#------------------------------------------------------------------------------ #$Date: 2019-11-24 16:12:06 +0200 (Sun, 24 Nov 2019) $ #$Revision: 238504 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/53/1555335.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1555335 loop_ _publ_author_name 'Takeda, Takuya' 'Harada, Shinji' 'Nishida, Atsushi' _publ_section_title ; Catalytic Asymmetric Nazarov Cyclization of Heteroaryl Vinyl Ketones through a Crystallographically Defined Chiral Dinuclear Nickel Complex. ; _journal_issue 21 _journal_name_full 'Organic letters' _journal_page_first 5184 _journal_page_last 5187 _journal_paper_doi 10.1021/acs.orglett.5b02497 _journal_volume 17 _journal_year 2015 _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' _chemical_formula_moiety 'C51 H46 F12 N6 Ni O16 S4' _chemical_formula_sum 'C51 H46 F12 N6 Ni O16 S4' _chemical_formula_weight 1413.88 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 104.4654(11) _cell_angle_gamma 90.0000 _cell_formula_units_Z 4 _cell_length_a 13.6455(3) _cell_length_b 18.1359(5) _cell_length_c 24.9551(6) _cell_measurement_reflns_used 14246 _cell_measurement_temperature 93 _cell_measurement_theta_max 68.09 _cell_measurement_theta_min 3.04 _cell_volume 5979.9(3) _computing_cell_refinement 'RAPID AUTO' _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_data_reduction 'RAPID AUTO' _computing_molecular_graphics 'CrystalStructure 4.2' _computing_publication_material 'CrystalStructure 4.2 (Rigaku, 2015)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'SHELXT Version 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 93 _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_R_equivalents 0.1448 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 64005 _diffrn_reflns_point_group_measured_fraction_full 0.964 _diffrn_reflns_point_group_measured_fraction_max 0.960 _diffrn_reflns_theta_full 67.687 _diffrn_reflns_theta_max 68.217 _diffrn_reflns_theta_min 3.047 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.752 _exptl_absorpt_correction_T_max 0.759 _exptl_absorpt_correction_T_min 0.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2888.00 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.54 _refine_diff_density_min -0.70 _refine_ls_abs_structure_details ; Flack x determined using 1405 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 1678 _refine_ls_number_reflns 21038 _refine_ls_number_restraints 2020 _refine_ls_R_factor_all 0.3164 _refine_ls_R_factor_gt 0.1394 _refine_ls_shift/su_max 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3280 _refine_ls_wR_factor_ref 0.4540 _reflns_Friedel_coverage 0.863 _reflns_Friedel_fraction_full 0.927 _reflns_Friedel_fraction_max 0.921 _reflns_number_gt 5100 _reflns_number_total 21038 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ol5b02497_si_002.cif _cod_data_source_block 141114takeda04 _cod_original_cell_volume 5980.0(3) _cod_database_code 1555335 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL 141114takeda04 CELL 1.54187 13.64553 18.13592 24.95510 90.000 104.465 90.000 ZERR 4 0.00034 0.00046 0.00064 0.000 0.001 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H F N NI O S UNIT 204 184 48 24 4 64 16 L.S. 10 FMAP 2 PLAN -30 WPDB -2 HTAB LIST 4 TEMP -180.0 ACTA SIZE 0.100 0.100 0.150 SIMU DELU FLAT C15 C16 C17 C18 C19 C20 FLAT C36 C37 C38 C39 C40 C41 BOND $H CONF WGHT 0.200000 FVAR 0.65648 0.23530 NI1 5 0.578890 0.684592 0.252524 11.00000 0.10005 0.08527 = 0.13472 0.00231 0.05358 -0.00134 NI2 5 0.320559 0.904985 0.213197 11.00000 0.09790 0.07658 = 0.14746 0.00669 0.04441 0.00223 S1 7 0.935681 0.689780 0.132997 11.00000 0.10145 0.08607 = 0.16458 -0.00068 0.04860 -0.00752 S2 7 1.049821 0.557663 0.151570 11.00000 0.12502 0.09785 = 0.15502 -0.00105 0.04930 0.00457 S3 7 0.606766 0.915166 0.550939 11.00000 0.16423 0.11464 = 0.17165 0.00039 0.06854 -0.00115 S4 7 0.467223 0.812756 0.491627 11.00000 0.14973 0.11862 = 0.17143 -0.00834 0.06695 -0.00931 S5 7 0.559077 0.243392 0.024128 11.00000 0.16142 0.14212 = 0.15687 0.01342 0.05113 -0.00979 S6 7 0.588212 0.357120 0.101957 11.00000 0.15475 0.11561 = 0.20764 0.00588 0.05449 -0.00951 F1 3 0.959399 0.688611 0.032715 11.00000 0.14353 0.13809 = 0.16792 -0.01816 0.04536 -0.01115 F2 3 0.884106 0.784916 0.056647 11.00000 0.17511 0.07796 = 0.18446 0.00555 0.03510 -0.01055 F3 3 0.807369 0.679443 0.038658 11.00000 0.12501 0.06802 = 0.16579 -0.00574 0.02951 -0.00008 F4 3 1.016590 0.575663 0.248472 11.00000 0.16362 0.11930 = 0.17602 0.00897 0.07929 -0.00451 F5 3 0.955417 0.477491 0.207278 11.00000 0.13128 0.09626 = 0.21010 0.02564 0.05367 0.02042 F6 3 1.109079 0.482195 0.241985 11.00000 0.13452 0.14282 = 0.17415 0.04212 0.06996 0.01809 F7 3 0.747319 0.935684 0.503214 11.00000 0.28638 0.23533 = 0.20290 -0.09668 0.14519 -0.12309 F8 3 0.763684 0.839919 0.553626 11.00000 0.18138 0.18735 = 0.28771 -0.08423 0.03953 0.02844 F9 3 0.793223 0.946971 0.591259 11.00000 0.17628 0.20732 = 0.20668 -0.09762 0.10226 -0.03086 F10 3 0.595034 0.720165 0.555232 11.00000 0.24874 0.12072 = 0.13178 -0.01294 0.07916 0.02607 F11 3 0.461841 0.673673 0.505019 11.00000 0.24038 0.12922 = 0.19732 0.00473 0.09465 -0.00917 F12 3 0.578899 0.708888 0.469843 11.00000 0.21080 0.15571 = 0.13415 0.01942 0.06616 0.03140 F13 3 0.667274 0.122562 0.025237 11.00000 0.25430 0.16017 = 0.16194 0.01135 0.06945 0.03506 F14 3 0.727713 0.203234 0.085870 11.00000 0.16619 0.12598 = 0.21927 0.01481 0.05345 0.00164 F15 3 0.605111 0.137376 0.096104 11.00000 0.15084 0.11438 = 0.19470 0.01599 0.05826 0.01117 F16 3 0.650110 0.261843 0.181762 11.00000 0.17705 0.14866 = 0.22070 0.02698 0.08747 0.02663 F17 3 0.507564 0.313118 0.180520 11.00000 0.13918 0.15056 = 0.20457 -0.01222 0.05032 -0.00389 F18 3 0.640846 0.374010 0.206215 11.00000 0.21185 0.14408 = 0.22020 -0.02813 0.05497 -0.05583 O1 6 0.650730 0.617689 0.319135 11.00000 0.16422 0.09418 = 0.11442 0.00890 0.03325 0.00948 O2 6 0.677928 0.628816 0.214856 11.00000 0.09538 0.08963 = 0.14923 -0.00262 0.08135 0.00864 O3 6 0.734452 0.528916 0.186495 11.00000 0.12038 0.06614 = 0.15325 0.00621 0.06156 -0.00046 O4 6 0.798662 0.661012 0.513953 11.00000 0.26069 0.18795 = 0.17852 -0.03173 0.08437 -0.02114 O5 6 0.684351 0.468656 0.367014 11.00000 0.08976 0.10651 = 0.15692 0.01224 0.03125 0.00698 O6 6 0.908967 0.294853 0.478049 11.00000 0.16192 0.13153 = 0.15737 0.03139 0.04533 0.04851 O7 6 0.951832 0.376427 0.303451 11.00000 0.13379 0.13539 = 0.19097 0.04978 0.07184 0.05408 O8 6 0.340010 1.019054 0.205195 11.00000 0.11021 0.05133 = 0.17705 0.00767 0.04779 -0.00806 O9 6 0.169214 0.935347 0.205447 11.00000 0.07082 0.09601 = 0.18352 0.01463 0.05004 0.01586 O10 6 0.027160 0.992290 0.161496 11.00000 0.09006 0.09892 = 0.33295 0.04022 0.00982 -0.00255 O11 6 0.301731 1.142801 0.129754 11.00000 0.11346 0.10249 = 0.17986 0.01038 0.05301 -0.00221 O12 6 0.191659 1.384643 0.056409 11.00000 0.14997 0.08721 = 0.17411 -0.00039 0.05539 -0.00444 O13 6 -0.001382 1.239379 0.154443 11.00000 0.11298 0.09520 = 0.21636 0.02379 0.05899 0.02012 O14 6 0.571939 1.214465 0.296131 11.00000 0.15156 0.12375 = 0.15388 -0.00760 0.04911 -0.02901 O15 6 1.022685 0.731540 0.153695 11.00000 0.13005 0.07032 = 0.15518 0.00946 0.06024 -0.00696 O16 6 0.849713 0.700868 0.153550 11.00000 0.10577 0.10766 = 0.16818 -0.01409 0.03742 -0.00680 O17 6 1.139151 0.599561 0.166829 11.00000 0.11714 0.09149 = 0.14628 0.01809 0.04652 0.01856 O18 6 1.050877 0.495606 0.119652 11.00000 0.12406 0.11542 = 0.17395 -0.00880 0.05016 -0.00845 O19 6 0.605736 0.882223 0.604462 11.00000 0.21533 0.09293 = 0.16603 -0.01316 0.06575 -0.02969 O20 6 0.586661 0.991837 0.543344 11.00000 0.17745 0.10331 = 0.20196 0.01759 0.05834 -0.00651 O21 6 0.410458 0.819110 0.533820 11.00000 0.17170 0.10556 = 0.19835 -0.02945 0.09391 -0.03267 O22 6 0.412584 0.810239 0.435116 11.00000 0.15036 0.11640 = 0.17509 -0.01391 0.07196 -0.00685 O23 6 0.474011 0.195729 -0.004760 11.00000 0.18869 0.17847 = 0.15652 0.01154 0.05297 -0.05060 O24 6 0.611385 0.280871 -0.012754 11.00000 0.16886 0.19061 = 0.16717 0.01189 0.04181 -0.05897 O25 6 0.523286 0.418462 0.093650 11.00000 0.15025 0.11614 = 0.28467 0.01347 0.02692 0.00607 O26 6 0.690747 0.361700 0.096817 11.00000 0.14087 0.11143 = 0.18642 0.04229 0.02610 0.01243 O31 6 0.878289 0.096858 0.023582 11.00000 0.23134 O32 6 -0.018717 0.960006 0.055957 11.00000 0.22961 N1 4 0.479281 0.721331 0.298865 11.00000 0.11268 0.16261 = 0.10690 -0.01597 0.07273 0.00719 N2 4 0.671576 0.766083 0.303577 11.00000 0.09430 0.07364 = 0.13758 -0.00259 0.03584 0.02277 N3 4 0.290831 0.797762 0.228187 11.00000 0.12889 0.03696 = 0.16395 0.00225 0.06637 0.01382 N4 4 0.266035 0.867259 0.129066 11.00000 0.12108 0.06905 = 0.14234 -0.01295 0.04595 -0.00062 N5 4 0.472456 0.899632 0.214450 11.00000 0.07805 0.09446 = 0.17434 0.02864 0.04001 0.02627 N6 4 0.382249 0.932916 0.299854 11.00000 0.12257 0.09063 = 0.14183 -0.01011 0.03007 -0.00523 N7 4 0.541282 0.749914 0.183545 11.00000 0.10583 0.10089 = 0.12010 0.01997 0.04850 0.00625 N8 4 0.468898 0.615214 0.202493 11.00000 0.08549 0.07487 = 0.14618 -0.00478 0.03465 0.00364 N9 4 0.953071 0.599888 0.127643 11.00000 0.11668 0.09254 = 0.15897 -0.01311 0.01935 -0.01058 N10 4 0.556457 0.871340 0.499320 11.00000 0.14052 0.13249 = 0.17571 -0.01231 0.07497 -0.00202 N11 4 0.523767 0.294666 0.066657 11.00000 0.16753 0.13168 = 0.20184 -0.00317 0.05359 -0.00213 C1 1 0.724309 0.569744 0.225160 11.00000 0.09646 0.08269 = 0.15225 -0.00844 0.02116 0.01058 C2 1 0.754135 0.541630 0.281747 11.00000 0.10978 0.05148 = 0.15802 -0.00730 0.02082 -0.01493 C3 1 0.735000 0.582322 0.325928 11.00000 0.15636 0.04695 = 0.14960 0.01164 0.03775 -0.01398 C4 1 0.694704 0.554494 0.129284 11.00000 0.18599 0.11385 = 0.15196 0.03184 0.09655 -0.01089 AFIX 33 H4A 2 0.707963 0.517134 0.103605 11.00000 -1.20000 H4B 2 0.621597 0.562642 0.122265 11.00000 -1.20000 H4C 2 0.728054 0.600758 0.123842 11.00000 -1.20000 AFIX 0 C5 1 0.792748 0.473660 0.285822 11.00000 0.09791 0.06906 = 0.17581 0.00374 0.03290 -0.00108 AFIX 43 H5 2 0.801647 0.451979 0.252705 11.00000 -1.20000 AFIX 0 C6 1 0.823174 0.428553 0.336890 11.00000 0.09923 0.04777 = 0.16463 -0.01576 0.02215 0.00752 C7 1 0.764063 0.429951 0.382738 11.00000 0.09858 0.05991 = 0.17966 0.01074 0.03329 -0.00416 C8 1 0.792201 0.382944 0.429047 11.00000 0.14967 0.05052 = 0.18165 0.00661 0.04177 0.01706 AFIX 43 H8 2 0.751609 0.380665 0.454880 11.00000 -1.20000 AFIX 0 C9 1 0.879336 0.339733 0.437169 11.00000 0.14317 0.08770 = 0.15869 0.02017 0.03621 0.02566 C10 1 0.935416 0.335954 0.393657 11.00000 0.15845 0.06680 = 0.15904 0.01582 0.04017 0.03329 AFIX 43 H10 2 0.992227 0.304338 0.397360 11.00000 -1.20000 AFIX 0 C11 1 0.902903 0.379402 0.347940 11.00000 0.14416 0.06310 = 0.16386 0.01219 0.05337 0.03134 C12 1 0.621117 0.479925 0.409174 11.00000 0.13629 0.13740 = 0.19012 0.08619 0.06975 0.05733 AFIX 33 H12A 2 0.561933 0.510373 0.392689 11.00000 -1.20000 H12B 2 0.598699 0.431945 0.419730 11.00000 -1.20000 H12C 2 0.662265 0.504665 0.442075 11.00000 -1.20000 AFIX 0 C13 1 0.853839 0.293795 0.520491 11.00000 0.19152 0.14244 = 0.16268 0.02758 0.06092 0.02388 AFIX 33 H13A 2 0.884286 0.257438 0.548819 11.00000 -1.20000 H13B 2 0.856702 0.342726 0.537475 11.00000 -1.20000 H13C 2 0.783125 0.280502 0.503975 11.00000 -1.20000 AFIX 0 C14 1 1.026334 0.328766 0.309001 11.00000 0.23834 0.18168 = 0.19622 0.02516 0.09975 0.12672 AFIX 33 H14A 2 1.054294 0.331236 0.276490 11.00000 -1.20000 H14B 2 1.079427 0.340630 0.342283 11.00000 -1.20000 H14C 2 1.000800 0.278916 0.312364 11.00000 -1.20000 AFIX 0 C15 1 0.809081 0.600792 0.378842 11.00000 0.14708 0.09706 = 0.13865 0.00330 0.04888 0.00245 C16 1 0.778056 0.627296 0.424496 11.00000 0.16403 0.10505 = 0.15885 -0.00754 0.06611 -0.01286 AFIX 43 H16 2 0.708440 0.633864 0.423220 11.00000 -1.20000 AFIX 0 C17 1 0.849507 0.642883 0.469581 11.00000 0.20741 0.11491 = 0.15079 -0.00614 0.05294 -0.01265 C18 1 0.948064 0.636712 0.478830 11.00000 0.19333 0.15097 = 0.15298 -0.02753 0.03400 -0.05045 AFIX 43 H18 2 0.993178 0.648429 0.513384 11.00000 -1.20000 AFIX 0 C19 1 0.980560 0.611606 0.433778 11.00000 0.15946 0.14787 = 0.15314 0.00561 0.03594 -0.03720 AFIX 43 H19 2 1.051447 0.609869 0.437223 11.00000 -1.20000 AFIX 0 C20 1 0.915619 0.588192 0.382656 11.00000 0.15104 0.11357 = 0.15500 -0.02400 0.05001 -0.01372 AFIX 43 H20 2 0.939764 0.566390 0.353787 11.00000 -1.20000 AFIX 0 C21 1 0.875020 0.662346 0.579052 11.00000 0.33133 0.37725 = 0.17439 -0.08507 0.08093 -0.17559 AFIX 33 H21A 2 0.834977 0.674756 0.605384 11.00000 -1.20000 H21B 2 0.905971 0.613684 0.588070 11.00000 -1.20000 H21C 2 0.928208 0.699368 0.581296 11.00000 -1.20000 AFIX 0 C22 1 0.119913 0.991877 0.182804 11.00000 0.08839 0.10208 = 0.22213 0.01721 0.02873 0.00625 C23 1 0.178437 1.063058 0.185654 11.00000 0.11297 0.08827 = 0.18438 -0.01146 0.06101 -0.00341 C24 1 0.285018 1.071194 0.207573 11.00000 0.11952 0.05462 = 0.16780 0.00279 0.06059 -0.00415 PART 1 C25 1 -0.020172 0.928574 0.199068 10.50000 0.09273 0.11214 = 0.37176 0.06210 -0.01246 -0.03639 AFIX 33 H25A 2 -0.093786 0.925400 0.184811 10.50000 -1.50000 H25B 2 0.010154 0.880307 0.195866 10.50000 -1.50000 H25C 2 -0.003962 0.943561 0.238023 10.50000 -1.50000 AFIX 0 PART 2 C25A 1 -0.018623 0.913665 0.141682 10.50000 0.11778 0.08686 = 0.17561 0.09328 -0.00366 -0.01525 AFIX 33 H25D 2 -0.091565 0.918236 0.125426 10.50000 -1.50000 H25E 2 0.014116 0.894041 0.113931 10.50000 -1.50000 H25F 2 -0.006719 0.880118 0.173442 10.50000 -1.50000 AFIX 0 PART 0 C26 1 0.114288 1.119365 0.159443 11.00000 0.13291 0.09833 = 0.17216 -0.00945 0.05920 0.01301 AFIX 43 H26 2 0.043631 1.112625 0.154853 11.00000 -1.20000 AFIX 0 C27 1 0.148221 1.189634 0.137977 11.00000 0.14904 0.09410 = 0.10994 -0.02769 0.05860 0.01784 C28 1 0.237109 1.200263 0.120028 11.00000 0.14588 0.10269 = 0.14425 -0.00861 0.05588 0.01029 C29 1 0.251647 1.263755 0.092035 11.00000 0.13517 0.07079 = 0.16563 -0.03633 0.06344 0.00400 AFIX 43 H29 2 0.310322 1.270076 0.078533 11.00000 -1.20000 AFIX 0 C30 1 0.178643 1.316798 0.084590 11.00000 0.16629 0.08366 = 0.15043 -0.01719 0.08863 0.02353 C31 1 0.095473 1.313070 0.105566 11.00000 0.12839 0.07384 = 0.14140 -0.03408 0.05662 0.00121 AFIX 43 H31 2 0.055287 1.355585 0.106545 11.00000 -1.20000 AFIX 0 C32 1 0.071479 1.247709 0.124896 11.00000 0.14796 0.07623 = 0.16468 -0.01810 0.06073 0.00571 C33 1 0.395886 1.153617 0.112391 11.00000 0.15216 0.10299 = 0.15067 0.02118 0.07831 -0.00271 AFIX 33 H33A 2 0.437961 1.109295 0.121027 11.00000 -1.20000 H33B 2 0.379839 1.162832 0.072448 11.00000 -1.20000 H33C 2 0.432713 1.195946 0.132106 11.00000 -1.20000 AFIX 0 C34 1 0.280648 1.390283 0.036280 11.00000 0.21954 0.14565 = 0.22211 -0.02387 0.13545 -0.00881 AFIX 33 H34A 2 0.281358 1.438123 0.018122 11.00000 -1.20000 H34B 2 0.340730 1.385944 0.067295 11.00000 -1.20000 H34C 2 0.280883 1.350650 0.009619 11.00000 -1.20000 AFIX 0 C35 1 -0.075199 1.290842 0.150938 11.00000 0.11488 0.08658 = 0.14476 0.02654 0.02403 0.02309 AFIX 33 H35A 2 -0.119691 1.276067 0.174390 11.00000 -1.20000 H35B 2 -0.044283 1.338621 0.163438 11.00000 -1.20000 H35C 2 -0.114818 1.294923 0.112461 11.00000 -1.20000 AFIX 0 C36 1 0.321428 1.134292 0.246463 11.00000 0.14954 0.07707 = 0.13145 0.00552 0.05836 -0.01639 C37 1 0.423584 1.144760 0.254443 11.00000 0.14091 0.09129 = 0.12023 0.01059 0.03936 -0.00740 AFIX 43 H37 2 0.462221 1.115056 0.235956 11.00000 -1.20000 AFIX 0 C38 1 0.468310 1.200145 0.290388 11.00000 0.13973 0.12567 = 0.13255 -0.01008 0.05053 -0.01601 C39 1 0.410646 1.243412 0.317219 11.00000 0.16244 0.10295 = 0.14643 -0.00280 0.03634 0.01954 AFIX 43 H39 2 0.441580 1.282728 0.340538 11.00000 -1.20000 AFIX 0 C40 1 0.314282 1.230024 0.310372 11.00000 0.15952 0.11498 = 0.12465 -0.00203 0.05310 0.02554 AFIX 43 H40 2 0.277894 1.256221 0.332153 11.00000 -1.20000 AFIX 0 C41 1 0.261026 1.176193 0.270387 11.00000 0.16262 0.08083 = 0.13760 0.01284 0.04752 0.01759 AFIX 43 H41 2 0.189556 1.170639 0.261599 11.00000 -1.20000 AFIX 0 C42 1 0.624144 1.275135 0.333168 11.00000 0.14712 0.14924 = 0.13829 -0.01140 0.06785 -0.04669 AFIX 33 H42A 2 0.695411 1.277165 0.332123 11.00000 -1.20000 H42B 2 0.591436 1.322288 0.320455 11.00000 -1.20000 H42C 2 0.619742 1.265649 0.371157 11.00000 -1.20000 AFIX 0 C43 1 0.374799 0.695752 0.293996 11.00000 0.11608 0.07927 = 0.09975 -0.00557 0.04256 0.01740 AFIX 13 H43 2 0.355486 0.661336 0.261768 11.00000 -1.20000 AFIX 0 C44 1 0.369586 0.654361 0.345683 11.00000 0.12621 0.07775 = 0.12348 0.01343 0.03678 0.00466 AFIX 23 H44A 2 0.394991 0.686739 0.378122 11.00000 -1.20000 H44B 2 0.414972 0.611020 0.349818 11.00000 -1.20000 AFIX 0 C45 1 0.263868 0.628270 0.345785 11.00000 0.11935 0.09216 = 0.18137 0.01745 0.06157 0.01779 AFIX 23 H45A 2 0.239136 0.592936 0.315149 11.00000 -1.20000 H45B 2 0.265082 0.602995 0.381107 11.00000 -1.20000 AFIX 0 C46 1 0.196862 0.692043 0.339013 11.00000 0.13185 0.05758 = 0.20511 0.02848 0.06144 -0.00198 AFIX 23 H46A 2 0.221345 0.726604 0.370194 11.00000 -1.20000 H46B 2 0.127964 0.675774 0.339765 11.00000 -1.20000 AFIX 0 C47 1 0.192637 0.731674 0.284499 11.00000 0.10943 0.06173 = 0.16137 -0.00386 0.04412 -0.00783 AFIX 23 H47A 2 0.144291 0.773279 0.279990 11.00000 -1.20000 H47B 2 0.168540 0.697175 0.253236 11.00000 -1.20000 AFIX 0 C48 1 0.300188 0.761392 0.283778 11.00000 0.09582 0.06800 = 0.15454 0.01371 0.03642 0.00630 AFIX 13 H48 2 0.322433 0.798716 0.313859 11.00000 -1.20000 AFIX 0 C49 1 0.527439 0.765463 0.335938 11.00000 0.11270 0.08216 = 0.11117 0.03792 0.04685 0.01297 AFIX 43 H49 2 0.491293 0.784767 0.360768 11.00000 -1.20000 AFIX 0 C50 1 0.630734 0.789116 0.344139 11.00000 0.12052 0.04931 = 0.12501 0.03228 0.04426 0.01585 C51 1 0.674119 0.823476 0.387872 11.00000 0.10302 0.09698 = 0.11040 0.02301 0.03909 0.02773 AFIX 43 H51 2 0.636402 0.836146 0.413795 11.00000 -1.20000 AFIX 0 C52 1 0.773856 0.842661 0.398519 11.00000 0.11712 0.09575 = 0.13399 -0.00299 0.04075 0.00624 AFIX 43 H52 2 0.806141 0.869825 0.430629 11.00000 -1.20000 AFIX 0 C53 1 0.827373 0.819663 0.358691 11.00000 0.10741 0.04812 = 0.14637 -0.00667 0.04043 0.00962 C54 1 0.927629 0.837973 0.363505 11.00000 0.09961 0.11408 = 0.15171 -0.00066 0.03133 0.01059 AFIX 43 H54 2 0.962025 0.866945 0.394169 11.00000 -1.20000 AFIX 0 C55 1 0.977591 0.816528 0.326816 11.00000 0.10975 0.08420 = 0.14498 0.00027 0.04327 -0.01242 AFIX 43 H55 2 1.047408 0.828063 0.332825 11.00000 -1.20000 AFIX 0 C56 1 0.930476 0.778622 0.281188 11.00000 0.09761 0.10151 = 0.13058 0.01974 0.02316 -0.00293 AFIX 43 H56 2 0.966664 0.763402 0.255152 11.00000 -1.20000 AFIX 0 C57 1 0.827386 0.761932 0.272631 11.00000 0.09951 0.10381 = 0.11330 0.01565 0.02687 0.00652 AFIX 43 H57 2 0.790720 0.739895 0.239060 11.00000 -1.20000 AFIX 0 C58 1 0.777194 0.779478 0.317135 11.00000 0.10381 0.05961 = 0.14409 -0.00669 0.03380 0.01535 C59 1 0.254634 0.758447 0.184481 11.00000 0.08028 0.06197 = 0.16808 -0.00270 0.04433 0.01704 AFIX 43 H59 2 0.241679 0.707335 0.187440 11.00000 -1.20000 AFIX 0 C60 1 0.233569 0.795463 0.128971 11.00000 0.09416 0.06698 = 0.16284 -0.01234 0.05170 0.01948 C61 1 0.184755 0.761208 0.083273 11.00000 0.10622 0.09549 = 0.15804 -0.03124 0.07993 -0.03320 AFIX 43 H61 2 0.169417 0.710298 0.084970 11.00000 -1.20000 AFIX 0 C62 1 0.155258 0.797866 0.032721 11.00000 0.10172 0.12613 = 0.15943 -0.02938 0.05191 -0.02290 AFIX 43 H62 2 0.116950 0.774403 0.000156 11.00000 -1.20000 AFIX 0 C63 1 0.184817 0.869075 0.033124 11.00000 0.11072 0.12745 = 0.14774 -0.01353 0.04036 -0.03140 C64 1 0.151665 0.915603 -0.017015 11.00000 0.12032 0.14089 = 0.12663 -0.02857 0.03928 -0.02874 AFIX 43 H64 2 0.107487 0.897084 -0.049900 11.00000 -1.20000 AFIX 0 C65 1 0.186930 0.985303 -0.013906 11.00000 0.14117 0.13752 = 0.12252 -0.00311 0.03014 -0.01481 AFIX 43 H65 2 0.172325 1.014461 -0.046566 11.00000 -1.20000 AFIX 0 C66 1 0.242719 1.015922 0.034078 11.00000 0.12406 0.09970 = 0.13403 0.00609 0.03006 -0.02816 AFIX 43 H66 2 0.264131 1.065742 0.033877 11.00000 -1.20000 AFIX 0 C67 1 0.266729 0.979531 0.078967 11.00000 0.13129 0.09871 = 0.10448 -0.00221 0.04798 -0.00592 AFIX 43 H67 2 0.305707 1.000440 0.112440 11.00000 -1.20000 AFIX 0 C68 1 0.232503 0.907626 0.075951 11.00000 0.08914 0.09725 = 0.14189 -0.00292 0.02828 0.00162 C69 1 0.512578 0.882111 0.161312 11.00000 0.10373 0.10508 = 0.17038 0.04280 0.05684 0.02217 AFIX 13 H69 2 0.456014 0.867882 0.129053 11.00000 -1.20000 AFIX 0 C70 1 0.563027 0.954216 0.150275 11.00000 0.10605 0.09790 = 0.24291 0.04288 0.08846 0.03293 AFIX 23 H70A 2 0.511250 0.993532 0.140774 11.00000 -1.20000 H70B 2 0.613679 0.969383 0.184268 11.00000 -1.20000 AFIX 0 C71 1 0.613884 0.945541 0.103974 11.00000 0.14637 0.09152 = 0.22684 0.02194 0.09249 0.00121 AFIX 23 H71A 2 0.562198 0.935165 0.069201 11.00000 -1.20000 H71B 2 0.648098 0.992264 0.099021 11.00000 -1.20000 AFIX 0 C72 1 0.689534 0.884724 0.114989 11.00000 0.12170 0.11118 = 0.16400 0.00063 0.08360 -0.00019 AFIX 23 H72A 2 0.746827 0.898243 0.146417 11.00000 -1.20000 H72B 2 0.716284 0.876798 0.082036 11.00000 -1.20000 AFIX 0 C73 1 0.640633 0.814451 0.128484 11.00000 0.14035 0.09387 = 0.15602 0.01226 0.07380 0.01053 AFIX 23 H73A 2 0.692969 0.775503 0.137807 11.00000 -1.20000 H73B 2 0.589349 0.798237 0.095066 11.00000 -1.20000 AFIX 0 C74 1 0.589756 0.821857 0.176343 11.00000 0.10274 0.08909 = 0.14133 0.02128 0.05581 0.01192 AFIX 13 H74 2 0.641285 0.835033 0.211125 11.00000 -1.20000 AFIX 0 C75 1 0.528600 0.922023 0.259953 11.00000 0.09687 0.07870 = 0.16486 0.04357 0.02136 0.05203 AFIX 43 H75 2 0.599625 0.925527 0.264312 11.00000 -1.20000 AFIX 0 C76 1 0.484188 0.942956 0.306797 11.00000 0.10973 0.07869 = 0.16661 0.02200 0.02246 0.03813 C77 1 0.545071 0.978569 0.351567 11.00000 0.10320 0.07440 = 0.18582 0.01557 0.01870 0.02444 AFIX 43 H77 2 0.614513 0.988747 0.354523 11.00000 -1.20000 AFIX 0 C78 1 0.496255 0.998423 0.392172 11.00000 0.14144 0.08945 = 0.17106 0.00128 0.03394 -0.03268 AFIX 43 H78 2 0.535955 1.020901 0.424806 11.00000 -1.20000 AFIX 0 C79 1 0.398397 0.988383 0.388851 11.00000 0.14664 0.08223 = 0.17836 -0.03069 0.05613 -0.03280 C80 1 0.344203 1.010130 0.432969 11.00000 0.16939 0.10348 = 0.16953 -0.02171 0.05808 -0.03002 AFIX 43 H80 2 0.378389 1.031802 0.467193 11.00000 -1.20000 AFIX 0 C81 1 0.244984 0.996374 0.419807 11.00000 0.15326 0.13566 = 0.17432 -0.05931 0.05774 0.00838 AFIX 43 H81 2 0.208949 1.008542 0.446617 11.00000 -1.20000 AFIX 0 C82 1 0.189972 0.966039 0.370714 11.00000 0.15366 0.10943 = 0.16354 -0.04149 0.06927 -0.01432 AFIX 43 H82 2 0.118264 0.963489 0.362984 11.00000 -1.20000 AFIX 0 C83 1 0.236067 0.941500 0.335868 11.00000 0.12670 0.09596 = 0.12936 -0.01948 0.03575 0.00426 AFIX 43 H83 2 0.199662 0.912880 0.305497 11.00000 -1.20000 AFIX 0 C84 1 0.342525 0.956061 0.341303 11.00000 0.12764 0.07123 = 0.14422 0.01175 0.03936 0.00146 C85 1 0.474759 0.717629 0.147164 11.00000 0.08543 0.10545 = 0.16172 0.02184 0.04117 0.00761 AFIX 43 H85 2 0.451276 0.742171 0.112708 11.00000 -1.20000 AFIX 0 C86 1 0.429855 0.645037 0.153154 11.00000 0.07011 0.10875 = 0.15352 0.02118 0.05141 0.00091 C87 1 0.359608 0.618029 0.111153 11.00000 0.09606 0.11701 = 0.13055 0.00263 0.05420 0.00015 AFIX 43 H87 2 0.338670 0.643456 0.076911 11.00000 -1.20000 AFIX 0 C88 1 0.318280 0.550483 0.119960 11.00000 0.10491 0.10929 = 0.15820 -0.02484 0.06452 -0.00895 AFIX 43 H88 2 0.267709 0.527045 0.092027 11.00000 -1.20000 AFIX 0 C89 1 0.356889 0.517484 0.174559 11.00000 0.10718 0.06957 = 0.16959 -0.02198 0.04700 -0.00332 C90 1 0.310529 0.447104 0.185406 11.00000 0.11477 0.08694 = 0.17896 -0.02162 0.03381 -0.02151 AFIX 43 H90 2 0.256465 0.425946 0.158187 11.00000 -1.20000 AFIX 0 C91 1 0.346321 0.413559 0.234547 11.00000 0.10167 0.10979 = 0.17767 -0.00668 0.06422 -0.01238 AFIX 43 H91 2 0.319874 0.368247 0.243923 11.00000 -1.20000 AFIX 0 C92 1 0.425244 0.450760 0.270449 11.00000 0.12677 0.09798 = 0.15348 0.00855 0.04771 -0.00699 AFIX 43 H92 2 0.452511 0.427550 0.305096 11.00000 -1.20000 AFIX 0 C93 1 0.467381 0.514516 0.262542 11.00000 0.10130 0.07726 = 0.15903 -0.00450 0.05672 0.00513 AFIX 43 H93 2 0.521195 0.535360 0.290089 11.00000 -1.20000 AFIX 0 C94 1 0.428143 0.550025 0.210947 11.00000 0.10074 0.07421 = 0.16497 -0.00168 0.04943 -0.01119 C95 1 0.889623 0.719341 0.059984 11.00000 0.13223 0.08834 = 0.17501 0.00962 0.04957 -0.02554 C96 1 1.034939 0.521905 0.220190 11.00000 0.15399 0.09180 = 0.17870 0.02386 0.07017 0.00572 C97 1 0.730994 0.912451 0.548144 11.00000 0.16752 0.16931 = 0.17296 -0.03586 0.06036 -0.00196 C98 1 0.532409 0.724693 0.509292 11.00000 0.16574 0.14077 = 0.18674 -0.00259 0.07019 0.01734 C99 1 0.641567 0.170174 0.057596 11.00000 0.17336 0.12502 = 0.18972 -0.00305 0.06646 -0.01065 C100 1 0.602861 0.323071 0.173366 11.00000 0.15415 0.10642 = 0.20438 -0.00674 0.05100 -0.02539 PART 1 AFIX 6 F19 3 0.687194 1.070458 0.261125 21.00000 0.19452 0.19919 = 0.25260 -0.10407 0.05635 0.03741 F20 3 0.795282 1.157588 0.281768 21.00000 0.25469 0.18097 = 0.24978 0.03343 -0.02314 0.01487 F21 3 0.788207 1.092198 0.209671 21.00000 0.22848 0.19721 = 0.22059 0.06486 0.01776 0.03597 F22 3 0.724542 1.042219 0.443421 21.00000 0.14446 0.19123 = 0.17426 0.06644 -0.01098 0.04895 F23 3 0.848183 1.073343 0.511500 21.00000 0.15854 0.22268 = 0.27486 -0.05048 0.02986 -0.06474 F24 3 0.799670 1.145949 0.441303 21.00000 0.23861 0.20212 = 0.34037 -0.01501 0.08398 0.00051 O27 6 0.961219 1.007058 0.445481 21.00000 0.22571 0.24575 = 0.28542 -0.00585 0.04960 0.05395 O28 6 0.900351 1.118641 0.400992 21.00000 0.24064 0.22910 = 0.30608 0.02282 0.11405 0.01640 O29 6 0.818614 0.942153 0.278929 21.00000 0.23637 0.18267 = 0.24687 0.07940 0.11129 -0.00685 O30 6 0.933296 1.041946 0.299293 21.00000 0.17817 0.19657 = 0.28694 0.07442 0.04197 0.01285 S7 7 0.880880 1.041720 0.406200 21.00000 0.21252 0.22213 = 0.28090 0.03415 0.07803 0.03376 S8 7 0.845661 1.011987 0.301336 21.00000 0.21245 0.18645 = 0.25186 0.09001 0.04968 0.00055 N12 4 0.823052 1.000366 0.356169 21.00000 0.22535 0.19413 = 0.24969 0.06654 0.06700 0.05110 C101 1 0.775101 1.091187 0.253124 21.00000 0.21251 0.18268 = 0.21861 0.04255 0.01221 0.01879 C102 1 0.814163 1.074004 0.455962 21.00000 0.17798 0.22506 = 0.27380 0.02339 0.06459 0.00771 PART 2 AFIX 6 F19A 3 0.713989 1.097879 0.219337 -21.00000 0.29272 0.13230 = 0.14657 -0.01271 0.02386 0.00346 F20A 3 0.858166 1.150840 0.242277 -21.00000 0.31116 0.21991 = 0.26611 0.06762 -0.06471 -0.03248 F21A 3 0.826614 1.073481 0.175580 -21.00000 0.33108 0.24105 = 0.22764 0.08450 0.07086 0.12520 F22A 3 0.712083 1.111066 0.398291 -21.00000 0.16438 0.24981 = 0.22592 -0.09782 0.06081 -0.02864 F23A 3 0.836115 1.121323 0.470449 21.00000 0.10545 0.13362 = 0.31188 -0.03130 0.01876 0.03475 F24A 3 0.836621 1.182739 0.396402 -21.00000 0.28733 0.17980 = 0.40980 0.02394 0.09116 -0.03496 O27A 6 0.916382 1.009040 0.417595 -21.00000 0.28558 0.18764 = 0.27462 0.05205 0.01089 0.08909 O28A 6 0.922227 1.116754 0.365616 -21.00000 0.28104 0.32258 = 0.28813 0.08855 0.13215 -0.04088 O29A 6 0.769186 0.946556 0.251131 21.00000 0.15141 0.24378 = 0.16012 0.11280 0.06715 0.01909 O30A 6 0.926142 1.009030 0.273654 -21.00000 0.17521 0.18218 = 0.20789 0.04242 0.03640 0.02678 S7A 7 0.863527 1.053807 0.372913 -21.00000 0.20880 0.19156 = 0.24724 0.09607 0.10811 0.06771 S8A 7 0.827950 1.008368 0.271202 -21.00000 0.21669 0.23472 = 0.23372 0.08091 0.05225 0.00993 N12A 4 0.793913 1.019562 0.322931 -21.00000 0.22702 0.17290 = 0.24419 0.09541 0.07346 0.08781 C103 1 0.808402 1.088404 0.216511 -21.00000 0.25965 0.18564 = 0.17240 0.05025 -0.00645 0.01475 C104 1 0.811290 1.116807 0.414801 -21.00000 0.16754 0.19465 = 0.30707 0.03335 0.07886 0.03453 AFIX 0 HKLF 4 REM 141114takeda04 REM R1 = 0.1394 for 5100 Fo > 4sig(Fo) and 0.3164 for all 21038 data REM 1678 parameters refined using 2020 restraints END WGHT 0.2000 0.0000 REM Instructions for potential hydrogen bonds HTAB C4 O16 EQIV $1 -x+1, y-1/2, -z+1 HTAB C8 O21_$1 HTAB C12 O21_$1 EQIV $2 -x+2, y-1/2, -z+1 HTAB C18 O28_$2 HTAB C18 S7_$2 HTAB C18 F23A_$2 HTAB C21 O28_$2 HTAB C21 O28A_$2 EQIV $3 x-1, y, z HTAB C25 O30_$3 EQIV $4 x-1, y+1, z HTAB C31 O18_$4 EQIV $5 x, y+1, z HTAB C33 O23_$5 HTAB C33 F17_$5 HTAB C34 O25_$5 EQIV $6 -x+1, y+1/2, -z+1 HTAB C39 O19_$6 HTAB C43 N8 HTAB C44 O22 HTAB C48 N6 HTAB C49 O22 HTAB C57 O2 HTAB C57 O16 HTAB C59 O17_$3 HTAB C67 O8 HTAB C67 O11 HTAB C69 N4 HTAB C70 O29A HTAB C73 O16 HTAB C74 N2 HTAB C75 O29A HTAB C77 F22 HTAB C83 O9 EQIV $7 -x+1, y+1/2, -z HTAB C85 O24_$7 HTAB C87 F13_$7 HTAB C93 O1 REM Highest difference peak 0.542, deepest hole -0.698, 1-sigma level 0.096 Q1 1 0.7447 1.1413 0.3280 11.00000 0.05 0.54 Q2 1 -0.0852 0.9702 0.2516 11.00000 0.05 0.46 Q3 1 -0.0712 1.0264 0.2578 11.00000 0.05 0.42 Q4 1 0.0425 1.0584 0.2699 11.00000 0.05 0.40 Q5 1 0.2549 1.1655 0.0485 11.00000 0.05 0.39 Q6 1 1.0933 0.5925 0.4235 11.00000 0.05 0.38 Q7 1 0.7354 0.9839 0.3233 11.00000 0.05 0.37 Q8 1 0.9731 0.0349 0.0138 11.00000 0.05 0.35 Q9 1 0.8572 1.1869 0.3240 11.00000 0.05 0.35 Q10 1 0.4236 0.9927 0.1373 11.00000 0.05 0.34 Q11 1 0.8467 0.6163 0.1858 11.00000 0.05 0.33 Q12 1 0.0430 1.1563 0.2793 11.00000 0.05 0.33 Q13 1 1.0377 0.4864 0.3026 11.00000 0.05 0.33 Q14 1 0.8640 1.0061 0.1474 11.00000 0.05 0.32 Q15 1 0.6796 0.2804 0.0748 11.00000 0.05 0.31 Q16 1 0.3597 0.3779 0.3079 11.00000 0.05 0.31 Q17 1 0.4252 0.9617 0.2774 11.00000 0.05 0.31 Q18 1 0.3453 0.5358 0.3804 11.00000 0.05 0.31 Q19 1 0.7031 1.0231 0.3482 11.00000 0.05 0.31 Q20 1 0.4569 0.6872 0.5703 11.00000 0.05 0.30 Q21 1 0.3775 0.9330 0.0837 11.00000 0.05 0.30 Q22 1 0.9455 0.4743 0.3205 11.00000 0.05 0.30 Q23 1 0.1592 0.8955 0.1725 11.00000 0.05 0.30 Q24 1 0.1897 0.5098 0.1275 11.00000 0.05 0.30 Q25 1 0.4017 0.6807 0.6121 11.00000 0.05 0.30 Q26 1 0.6346 0.9172 0.0202 11.00000 0.05 0.30 Q27 1 0.3920 0.8153 0.2009 11.00000 0.05 0.30 Q28 1 0.8732 0.6961 0.6510 11.00000 0.05 0.29 Q29 1 0.0988 1.0650 0.3376 11.00000 0.05 0.29 Q30 1 0.4063 1.2315 0.1687 11.00000 0.05 0.29 ; _shelx_res_checksum 34609 _shelx_hkl_file ; 0 -1 -1 6074.67 510.69 0 -1 1 6378.98 537.86 0 1 -1 6396.67 500.35 0 -1 -1 6325.46 705.87 0 1 -1 6454.49 542.46 0 -1 -1 6277.94 554.31 0 1 -1 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6.08 22.79 7 5 22 -2.44 23.50 -14 10 0 -0.80 39.10 14 10 0 -2.90 39.05 -5 9 27 14.17 45.80 -5 -9 27 -20.31 33.28 -4 21 2 -12.02 31.88 4 21 -2 38.63 39.02 4 -21 -2 5.95 29.12 3 0 27 10.11 30.67 -1 10 26 5.70 25.95 1 -10 -26 -4.09 24.25 -5 -6 -24 5.99 27.95 5 6 24 1.01 26.61 -2 7 28 -8.37 41.72 2 -7 -28 -13.47 34.65 10 -17 -2 -5.74 33.38 10 17 -2 -37.37 34.08 -10 -17 2 1.09 54.10 -10 -17 2 8.84 46.62 8 16 -17 19.92 45.37 -8 -16 17 -0.18 30.91 8 -16 -17 9.56 73.69 6 -20 -6 -25.68 37.23 -15 5 16 -18.18 38.21 15 -5 -16 -5.11 71.76 15 -5 -16 -16.79 36.56 9 18 -2 28.52 39.90 9 -18 -2 10.66 41.87 -9 -18 2 27.38 45.48 -13 -13 4 9.92 35.71 13 13 -4 3.24 40.21 4 21 -1 174.61 50.38 4 -21 -1 0.04 38.13 -4 21 1 -24.62 40.69 13 12 1 6.31 40.30 13 12 1 -1.24 24.74 4 6 25 4.39 29.01 -4 -6 -25 1.45 31.01 -7 -8 27 -10.27 44.17 -1 3 29 -0.66 33.17 1 -3 -29 9.83 36.23 -8 -10 25 -30.29 47.55 -8 10 25 -3.36 50.04 8 10 -25 -15.12 39.34 11 -16 -5 -1.77 29.36 -11 -16 5 0.76 41.06 -15 8 3 2.74 40.66 15 8 -3 -1.12 36.01 -16 4 9 -79.53 37.81 16 4 -9 -5.55 70.64 16 -4 -9 -4.57 60.70 -9 -11 -15 4.79 54.92 9 11 15 6.46 22.52 9 -11 15 1.84 27.81 -5 -19 13 31.89 45.33 5 -19 -13 -0.68 72.86 -9 -9 25 25.11 45.85 9 9 -25 -5.29 36.77 -9 9 25 -0.27 43.73 13 -13 -8 8.67 27.05 -13 -13 8 -3.90 39.57 -13 13 8 4.12 36.42 12 -1 -25 -3.89 32.86 12 1 -25 12.31 35.14 4 -21 -3 -4.11 29.46 4 21 -3 69.01 41.87 -4 21 3 1.12 51.74 -8 -18 -4 6.45 41.53 -8 18 -4 -42.11 41.48 -8 -18 -4 -8.59 64.41 8 18 4 -3.20 46.18 8 -18 4 3.25 24.78 -11 -16 6 18.28 45.12 11 -16 -6 -3.65 33.31 3 1 27 -31.00 33.24 3 -1 27 4.15 26.72 4 -16 -20 -2.86 52.58 -4 -16 20 1.67 36.56 -11 -16 4 -6.15 47.52 11 -16 -4 14.99 31.56 -10 -9 24 10.46 41.23 10 9 -24 -10.03 36.84 14 2 -21 -11.93 35.07 14 -2 -21 5.26 39.42 12 -9 10 28.06 58.98 12 9 10 0.91 36.61 -12 9 -10 -0.68 27.56 6 -2 24 29.41 31.93 6 2 24 -9.06 36.58 16 0 -13 -6.22 54.17 -14 11 4 -4.47 34.69 14 11 -4 5.47 37.54 -5 -11 -21 3.63 38.35 11 3 -26 -1.82 31.43 9 0 20 -6.35 35.86 -7 -3 29 -5.81 40.75 7 -3 -29 -10.95 23.66 -7 3 29 9.41 21.14 7 15 -20 -30.19 51.08 7 -15 -20 -3.86 63.74 -7 -15 20 -1.56 17.44 -13 -12 13 -3.95 38.42 13 -12 -13 19.21 39.58 13 -12 -13 0.11 48.55 -13 12 13 3.06 46.21 -7 -9 -20 1.52 27.79 -8 -15 19 1.20 30.27 8 15 -19 -15.89 45.86 8 -15 -19 11.24 65.54 -14 10 13 -0.19 47.15 14 -10 -13 -6.76 49.15 14 -10 -13 6.52 33.70 15 -6 -15 4.88 36.74 15 -6 -15 -3.60 70.59 -15 6 15 -50.42 42.75 10 10 14 -4.11 25.14 10 -10 14 2.95 29.35 -3 5 29 13.71 40.39 -3 -5 29 13.17 38.21 3 -5 -29 16.90 37.88 9 -10 16 -4.07 23.57 -9 -10 -16 3.93 23.99 -2 -5 -27 0.17 29.42 2 5 27 -2.44 33.79 -1 -16 -19 2.92 45.29 12 9 -21 -15.61 35.06 12 -9 -21 0.14 42.53 12 -9 -21 -10.61 33.78 -12 -9 21 -8.23 32.78 -12 9 21 60.15 43.11 -14 11 9 0.93 64.70 14 -11 -9 -58.28 33.84 -14 7 18 -4.23 44.84 14 -7 -18 -14.39 62.61 14 -7 -18 26.08 46.44 14 7 -18 -26.91 26.64 -14 8 -4 19.48 56.23 14 8 4 -0.27 34.76 14 8 4 58.83 37.94 -15 8 11 -8.69 48.08 15 -8 -11 -5.08 50.66 15 8 -11 -14.25 67.23 4 -21 0 4.61 41.54 -4 21 0 13.23 45.66 4 21 0 116.62 51.49 -5 -5 29 1.42 46.62 -5 5 29 -39.56 37.08 5 -5 -29 -2.93 29.74 16 4 -5 3.27 41.62 -16 4 5 1.23 28.77 -10 6 26 26.91 36.96 10 6 -26 -13.10 61.05 -10 -6 26 -1.48 77.66 12 -8 11 0.76 30.44 12 8 11 7.78 33.57 -12 8 -11 -7.87 28.37 -2 9 27 5.64 31.14 2 -9 -27 -4.55 23.38 0 -19 14 -10.31 39.99 0 -19 -14 -7.31 74.27 15 2 -18 -1.27 23.28 15 -2 -18 15.81 47.37 15 -2 -18 -26.91 73.76 16 1 -13 7.42 52.01 16 -1 -13 7.25 54.75 15 -4 -17 -1.00 52.88 15 -4 -17 -1.83 30.69 -3 -11 -23 -10.22 43.02 8 -4 21 -12.32 27.93 8 4 21 18.75 26.08 6 20 1 42.77 41.48 -6 20 -1 -2.94 37.23 6 -20 1 9.68 39.39 13 3 -23 15.64 39.84 13 -3 -23 -27.18 39.97 10 -11 13 4.02 31.67 10 11 13 1.82 27.28 -10 -11 -13 -0.67 31.08 0 -17 18 97.86 43.26 0 -17 -18 -20.05 90.07 9 1 20 -2.29 36.47 9 -1 20 -18.94 38.08 3 8 25 -3.74 26.20 -3 -8 -25 -0.27 38.37 8 13 -22 30.15 49.70 -8 -13 22 22.20 38.36 8 -13 -22 -0.72 56.77 -8 13 22 -2.09 35.27 16 3 -3 -0.41 36.30 -16 3 3 -5.61 28.14 14 -6 -19 -11.43 44.21 14 6 -19 17.93 29.08 -14 6 19 8.61 37.54 14 -6 -19 0.79 53.10 -11 3 -16 -14.85 34.78 11 3 16 1.57 23.80 11 -3 16 -2.79 24.23 -11 -3 -16 -1.31 23.85 -12 5 -13 -4.52 32.53 12 -5 13 -1.33 30.20 12 5 13 1.52 32.99 9 -18 -7 15.87 41.82 -9 -18 7 6.58 39.10 -2 -13 -22 2.69 31.20 9 -12 14 -3.04 29.22 -9 -12 -14 6.00 37.84 9 12 14 3.46 23.75 -8 5 28 36.42 39.30 -8 -5 28 -9.04 51.99 4 21 -4 21.03 31.46 4 -21 -4 -7.94 21.24 -5 -14 -18 6.02 38.66 11 -16 -7 -5.85 35.40 -11 -16 7 -5.12 47.36 14 -3 8 -79.70 34.22 -14 3 -8 18.92 37.25 14 3 8 42.64 40.78 13 -8 8 64.23 36.22 -13 8 -8 -6.52 41.75 13 8 8 -23.79 46.54 -6 -7 28 -11.58 40.72 -6 7 28 27.00 43.24 11 -16 -3 9.13 28.55 -11 -16 3 0.08 44.45 -12 -8 22 3.84 32.09 12 -8 -22 19.85 32.94 12 8 -22 -6.96 37.39 -12 8 22 -43.64 70.81 12 -8 -22 -2.79 36.55 16 2 -2 1.13 30.84 4 20 7 5.10 73.33 -4 20 -7 -124.47 58.52 -4 -20 -7 1.66 134.63 4 -20 7 -9.76 44.01 12 -2 14 2.15 31.27 -12 2 -14 3.66 35.53 12 2 14 2.79 31.11 -12 -2 -14 -27.10 25.50 6 -18 -15 6.72 65.47 -6 -18 15 1.76 39.47 10 -17 -8 5.22 39.49 -10 -17 8 -22.57 44.59 16 4 -10 7.12 46.92 16 -4 -10 -0.82 43.97 -5 -17 18 7.19 45.02 5 -17 -18 -5.56 67.42 -14 5 -7 23.89 38.53 14 5 7 -98.91 38.06 14 -5 7 61.02 29.53 13 13 -3 6.31 38.40 -13 -13 3 -0.05 31.21 -6 -8 -22 1.24 27.46 5 -3 25 4.72 22.59 5 3 25 -4.18 30.20 12 10 9 2.09 42.71 12 -10 9 -22.48 39.00 -12 5 24 -5.56 28.84 12 -5 -24 -29.44 36.14 12 5 -24 7.67 41.97 9 18 -1 -39.24 42.38 -9 -18 1 -25.38 44.34 9 -18 -1 -2.03 37.78 10 3 18 8.45 25.91 -10 3 -18 4.02 36.55 12 -12 6 1.54 34.31 12 12 6 54.09 45.16 -7 -16 -12 -3.80 48.79 -7 -16 -12 -2.57 63.46 7 16 12 -12.48 30.88 7 -16 12 -10.74 37.78 10 -16 -13 -3.47 49.05 10 -16 -13 3.04 31.97 -10 -16 13 3.92 40.39 4 -19 -14 -0.93 143.35 -4 -19 14 -28.31 50.30 10 -12 -21 -10.08 55.40 10 12 -21 -8.89 39.77 -10 -12 21 -4.37 40.47 -10 12 21 7.23 35.64 -9 13 21 5.42 37.17 9 -13 -21 -1.04 65.90 9 13 -21 11.46 50.51 -9 -13 21 40.53 45.12 15 3 4 -35.60 50.99 -15 3 -4 2.91 42.20 -13 13 9 6.79 38.17 13 -13 -9 10.23 29.16 -13 -13 9 -4.16 40.18 -10 -17 1 0.94 74.14 -10 -17 1 33.96 106.79 10 -17 -1 -0.38 39.80 6 6 23 2.10 22.32 -6 -19 12 -8.65 30.82 6 -19 -12 3.52 53.33 -15 7 0 -12.24 49.41 1 -16 -20 -11.06 52.44 12 -2 -25 -18.77 36.51 12 2 -25 -4.86 40.80 -3 -18 -14 -2.19 61.97 0 -11 -25 -4.57 31.63 12 -10 -20 -3.03 50.13 12 -10 -20 3.71 35.66 12 10 -20 0.73 33.52 -12 10 20 4.81 45.51 -12 -10 20 6.78 35.44 -12 12 17 -8.24 48.03 -12 -12 17 -15.42 42.96 12 -12 -17 -7.18 42.95 12 -12 -17 -6.38 61.47 -3 21 -4 8.69 39.35 3 -21 4 -12.15 33.00 3 21 4 -2.77 31.57 7 0 23 29.36 42.50 -2 -12 -23 22.04 43.05 13 -7 9 -102.85 39.31 13 7 9 70.77 47.66 -13 7 -9 -6.63 43.39 3 -2 27 26.09 25.55 3 2 27 -9.10 37.05 10 9 15 -4.33 25.42 10 -9 15 -4.21 29.29 4 -3 26 -26.99 24.58 4 3 26 4.77 38.01 -9 -3 28 -5.87 38.27 14 -8 -17 2.74 46.99 -14 8 17 42.25 52.84 14 -8 -17 0.75 65.02 -2 -14 -21 15.84 32.78 16 -3 -12 -2.44 49.99 16 3 -12 7.55 45.96 7 -19 -10 27.60 33.65 7 17 10 2.62 31.86 -7 -17 -10 -5.54 40.86 -7 -17 -10 -15.97 63.48 7 -17 10 1.42 35.99 14 11 -3 9.52 40.01 -14 11 3 -3.30 35.78 2 -18 15 314.15 58.91 -2 -18 -15 -7.07 161.19 0 0 -29 -0.85 33.03 0 0 29 -42.20 29.93 -4 21 -1 3.59 31.09 4 -21 1 -2.52 28.62 4 21 1 -0.13 32.46 6 -20 -7 -16.06 31.47 13 -9 7 12.21 74.50 -13 9 -7 4.27 52.97 13 9 7 104.15 52.04 -6 -12 -19 -2.46 36.82 -3 -6 -26 3.59 30.00 3 6 26 -12.91 32.72 -13 8 20 -15.48 40.83 13 -8 -20 -3.80 44.96 13 8 -20 10.78 27.79 13 -8 -20 1.03 38.77 -1 -4 -28 -8.76 33.32 1 4 28 -7.17 37.95 10 16 4 119.94 49.59 -10 -16 -4 -2.07 79.53 10 -16 4 -25.61 34.31 -10 -16 -4 5.30 53.97 12 13 4 -16.70 37.40 12 -13 4 3.33 24.46 -12 -13 -4 -6.69 33.15 -12 -14 -1 1.35 41.19 12 14 1 -34.68 34.77 12 14 1 4.23 50.93 5 -20 5 -10.73 31.40 5 20 5 -2.11 56.70 -5 -20 -5 3.69 50.36 -5 20 -5 4.48 39.53 -8 -16 -10 -12.50 46.20 8 -16 10 1.76 36.70 8 16 10 -0.85 33.72 -8 -16 -10 2.18 60.24 -1 21 -7 85.53 70.34 1 -21 7 13.87 65.05 1 21 7 140.26 24.35 -8 -19 4 -6.16 28.69 8 -19 -4 2.45 35.25 5 -18 -16 0.35 79.24 -5 -18 16 20.23 50.12 -2 -20 -10 4.22 87.65 2 -20 10 0.78 47.38 -2 20 -10 93.33 45.75 7 1 23 2.86 37.39 7 -1 23 -33.16 37.07 -9 6 27 34.51 40.57 -9 -6 27 -5.17 49.69 -10 -14 18 -10.60 37.95 10 -14 -18 8.75 63.54 10 14 -18 2.56 33.35 -8 -19 3 -0.14 32.97 8 19 -3 40.03 35.68 8 -19 -3 0.52 41.14 12 -14 -12 -5.80 35.65 12 -14 -12 -5.46 73.23 -12 -14 12 -2.89 44.81 -7 12 24 -5.65 35.78 -7 -12 24 9.77 33.38 7 12 -24 -22.44 36.30 -8 -11 -17 9.40 35.01 -16 4 4 -12.37 32.30 16 4 -4 1.53 43.81 12 -13 -15 -17.09 40.18 12 -13 -15 -0.45 52.71 -12 13 15 4.80 40.10 -12 -13 15 -3.90 43.40 16 2 -13 0.89 43.01 16 -2 -13 -4.90 48.92 11 6 -25 25.57 37.74 -11 6 25 8.11 32.52 -11 -6 25 -7.30 37.16 -14 11 10 12.74 55.19 14 -11 -10 59.35 31.62 14 -11 -10 -4.81 31.85 8 17 -15 -3.89 42.98 -8 -17 15 23.20 23.24 8 -17 -15 2.99 74.39 11 -15 -13 -7.50 36.40 11 -15 -13 -4.32 53.99 -11 -15 13 -5.34 46.16 9 2 20 2.59 28.27 9 -2 20 0.62 32.36 -3 -15 -19 4.85 29.28 0 8 27 -0.27 29.50 0 -8 -27 0.54 29.63 8 -12 16 -10.92 26.09 -8 -12 -16 1.48 37.44 -10 6 -17 5.39 24.94 10 -6 17 -3.60 19.30 -4 -15 -18 -7.52 33.74 -15 8 2 -21.43 50.99 -11 -16 8 18.16 41.95 11 -16 -8 -9.48 32.75 0 -1 -29 -14.67 33.12 0 1 29 -16.32 31.56 -4 12 25 3.86 43.25 3 21 -7 28.54 38.03 1 21 -8 -44.39 36.66 -1 -21 8 14.23 39.12 -3 -17 -16 -5.57 56.00 11 -16 -2 -2.24 24.25 -11 -16 2 -11.23 40.61 11 16 -2 -0.84 31.56 -8 0 29 -2.85 32.56 -6 -13 -18 3.17 37.51 4 21 -5 -78.21 51.68 2 -21 6 -5.44 32.26 2 21 6 2.16 24.93 -2 21 -6 9.38 36.69 -6 17 -12 -18.32 31.66 -6 -17 -12 19.31 34.25 -6 -17 -12 4.89 56.37 -11 -15 -3 -16.84 71.00 -11 -15 -3 -2.81 110.97 11 15 3 177.02 62.82 -8 -19 5 43.09 34.12 8 -19 -5 -15.99 43.88 9 -9 17 -48.95 24.48 -13 11 -4 -9.42 37.83 13 11 4 61.85 38.83 13 11 4 1.29 43.27 -15 7 14 27.87 44.83 15 -7 -14 2.87 62.20 15 -7 -14 2.07 33.05 10 -15 -16 2.51 25.80 -10 -15 16 -5.54 37.04 10 -15 -16 -3.11 60.74 10 15 -16 -3.39 27.20 10 -12 12 10.40 35.76 -10 -12 -12 12.65 38.13 10 12 12 1.59 31.80 -13 7 21 -5.14 43.90 13 -7 -21 -53.50 46.27 13 -7 -21 -3.25 48.06 13 7 -21 -4.76 38.16 -7 11 25 -0.42 46.24 -7 -11 25 21.84 40.30 7 11 -25 28.21 35.74 -8 9 26 -42.29 55.65 -8 -9 26 -19.01 97.03 -4 0 30 3.55 44.67 14 3 -21 -1.10 35.43 14 -3 -21 -12.77 40.39 6 -3 24 -10.34 26.52 6 3 24 -3.83 32.11 -1 -7 -27 8.85 34.77 1 7 27 1.40 34.18 14 5 -20 -3.29 29.91 14 -5 -20 -8.70 41.01 14 -5 -20 -1.96 43.38 -4 -10 -23 -14.74 43.97 12 7 12 4.98 35.89 12 -7 12 -0.35 32.60 -12 7 -12 9.11 31.74 -8 -19 2 9.76 30.40 8 -19 -2 14.21 36.90 8 19 -2 -45.34 34.76 -9 -18 8 3.31 38.51 9 -18 -8 -26.73 40.18 13 9 -19 11.43 25.29 13 -9 -19 -9.32 39.60 13 -9 -19 -4.45 49.55 -13 -9 19 -5.05 27.38 -13 9 19 5.76 44.44 11 6 15 4.35 25.51 -11 6 -15 -7.36 27.71 11 -6 15 0.35 24.80 4 -20 -11 -7.22 59.21 -4 -20 11 -19.00 37.11 1 -20 11 4.61 60.67 -1 -20 -11 4.30 63.42 -10 -8 25 -0.17 41.71 10 8 -25 -14.09 35.74 -10 8 25 24.71 37.90 16 -4 -11 -4.54 44.44 16 4 -11 0.21 43.87 -6 -11 -20 12.92 40.33 -8 -1 29 14.43 41.27 -11 -10 22 -3.89 47.26 11 10 -22 -5.33 45.90 11 -10 -22 -2.04 82.77 -11 10 22 -40.94 45.89 -10 -4 27 -1.86 31.31 -6 -9 27 11.85 34.45 -6 9 27 -0.19 43.21 -8 -15 -12 -8.22 50.88 -8 -15 -12 24.09 46.14 8 -15 12 -8.66 33.42 8 15 12 6.68 29.80 -4 -18 -13 0.19 57.63 13 4 11 -7.71 34.63 -13 4 -11 6.47 32.57 13 -4 11 2.33 29.29 12 -7 -23 -8.05 31.77 -12 7 23 12.73 31.58 -12 -7 23 0.39 30.91 6 20 2 -6.05 37.26 -6 20 -2 6.83 34.51 6 -20 2 15.89 34.10 13 13 -2 -4.61 41.57 -13 -13 2 -7.34 32.00 8 -18 -12 0.04 24.49 8 -18 -12 2.83 43.82 -7 -18 14 -27.15 39.97 7 -18 -14 -0.67 71.74 2 -20 -12 -0.18 61.93 -2 -20 12 8.68 39.09 -10 -14 -9 12.15 62.78 10 -14 9 108.42 48.77 -10 -14 -9 9.24 79.30 10 14 9 2.32 55.75 -5 -10 -22 -6.87 38.08 -2 -21 8 4.96 47.79 2 21 -8 126.45 46.03 4 -1 -30 -8.91 36.13 -4 -1 30 3.92 44.87 15 -8 -12 -0.69 47.54 -15 8 12 -2.68 42.18 6 -15 -21 -7.59 57.62 2 -5 -29 -12.47 33.30 -2 5 29 7.43 34.94 -7 13 23 9.64 29.76 -7 -13 23 -13.34 28.40 15 -3 -18 9.99 52.30 3 -20 9 14.61 36.94 -3 20 -9 13.62 40.60 -13 11 16 17.27 46.99 13 -11 -16 -2.08 54.95 -13 -11 16 -4.86 32.22 13 -11 -16 8.69 40.07 15 0 5 -46.77 33.60 9 -17 -13 -24.87 31.31 9 -17 -13 0.33 55.99 -9 -17 13 8.69 36.68 -9 -18 0 26.10 73.80 9 -18 0 4.64 57.09 1 -4 -29 -4.55 34.99 10 -17 -9 12.24 39.57 -10 -17 9 8.99 46.05 9 -15 -18 -4.02 64.28 -9 -15 18 3.54 32.88 -7 -19 -4 2.42 30.88 7 -19 4 -8.70 26.76 -4 -17 -15 -22.36 35.41 -13 -13 10 -0.94 35.32 -5 0 30 -3.86 44.95 5 -19 9 2.19 24.28 6 -5 -29 220.15 31.52 -9 -13 -13 18.96 50.43 -10 -15 -7 1.26 42.84 -1 -9 -26 10.32 36.67 -8 -10 -18 -1.77 26.81 ; _shelx_hkl_checksum 84282 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5789(3) 0.6846(3) 0.2525(2) 0.1024(14) Uani 1 1 d . U . . . Ni2 Ni 0.3206(3) 0.9050(2) 0.2132(2) 0.1049(15) Uani 1 1 d . U . . . S1 S 0.9357(6) 0.6898(4) 0.1330(4) 0.115(2) Uani 1 1 d . U . . . S2 S 1.0498(7) 0.5577(5) 0.1516(4) 0.123(3) Uani 1 1 d . U . . . S3 S 0.6068(9) 0.9152(6) 0.5509(5) 0.145(3) Uani 1 1 d . U . . . S4 S 0.4672(9) 0.8128(6) 0.4916(5) 0.142(3) Uani 1 1 d . U . . . S5 S 0.5591(9) 0.2434(7) 0.0241(5) 0.151(3) Uani 1 1 d . U . . . S6 S 0.5882(9) 0.3571(6) 0.1020(5) 0.158(3) Uani 1 1 d . U . . . F1 F 0.9594(14) 0.6886(12) 0.0327(9) 0.149(6) Uani 1 1 d . U . . . F2 F 0.8841(16) 0.7849(10) 0.0566(9) 0.148(6) Uani 1 1 d . U . . . F3 F 0.8074(12) 0.6794(8) 0.0387(8) 0.121(5) Uani 1 1 d . U . . . F4 F 1.0166(16) 0.5757(11) 0.2485(9) 0.146(6) Uani 1 1 d . U . . . F5 F 0.9554(14) 0.4775(10) 0.2073(9) 0.144(6) Uani 1 1 d . U . . . F6 F 1.1091(14) 0.4822(12) 0.2420(9) 0.145(6) Uani 1 1 d . U . . . F7 F 0.747(2) 0.9357(17) 0.5032(13) 0.227(11) Uani 1 1 d . U . . . F8 F 0.764(2) 0.8399(17) 0.5536(14) 0.222(10) Uani 1 1 d . U . . . F9 F 0.7932(18) 0.9470(15) 0.5913(11) 0.187(9) Uani 1 1 d . U . . . F10 F 0.595(2) 0.7202(12) 0.5552(10) 0.161(7) Uani 1 1 d . U . . . F11 F 0.462(2) 0.6737(13) 0.5050(11) 0.182(8) Uani 1 1 d . U . . . F12 F 0.5789(18) 0.7089(12) 0.4698(9) 0.163(7) Uani 1 1 d . U . . . F13 F 0.667(2) 0.1226(15) 0.0252(11) 0.189(8) Uani 1 1 d . U . . . F14 F 0.7277(17) 0.2032(12) 0.0859(11) 0.170(7) Uani 1 1 d . U . . . F15 F 0.6051(15) 0.1374(11) 0.0961(10) 0.151(6) Uani 1 1 d . U . . . F16 F 0.6501(18) 0.2618(14) 0.1818(11) 0.175(8) Uani 1 1 d . U . . . F17 F 0.5076(16) 0.3131(13) 0.1805(10) 0.163(7) Uani 1 1 d . U . . . F18 F 0.641(2) 0.3740(14) 0.2062(11) 0.192(8) Uani 1 1 d . U . . . O1 O 0.6507(19) 0.6177(12) 0.3191(9) 0.125(6) Uani 1 1 d . U . . . O2 O 0.6779(13) 0.6288(10) 0.2149(8) 0.102(5) Uani 1 1 d . U . . . O3 O 0.7345(14) 0.5289(10) 0.1865(10) 0.108(5) Uani 1 1 d . U . . . O4 O 0.799(3) 0.6610(19) 0.5140(14) 0.204(11) Uani 1 1 d . U . . . O5 O 0.6844(14) 0.4687(11) 0.3670(9) 0.118(6) Uani 1 1 d . U . . . O6 O 0.9090(19) 0.2949(14) 0.4780(11) 0.149(8) Uani 1 1 d . U . . . O7 O 0.9518(17) 0.3764(13) 0.3035(11) 0.148(8) Uani 1 1 d . U . . . O8 O 0.3400(14) 1.0191(9) 0.2052(9) 0.111(5) Uani 1 1 d . U . . . O9 O 0.1692(12) 0.9353(10) 0.2054(10) 0.114(6) Uani 1 1 d . U . . . O10 O 0.0272(17) 0.9923(13) 0.1615(15) 0.182(11) Uani 1 1 d . U . . . O11 O 0.3017(16) 1.1428(12) 0.1298(10) 0.129(7) Uani 1 1 d . U . . . O12 O 0.1917(17) 1.3846(11) 0.0564(10) 0.134(7) Uani 1 1 d . U . . . O13 O -0.0014(16) 1.2394(12) 0.1544(11) 0.138(7) Uani 1 1 d . U . . . O14 O 0.5719(19) 1.2145(13) 0.2961(10) 0.141(7) Uani 1 1 d . U . . . O15 O 1.0227(16) 0.7315(10) 0.1537(9) 0.114(6) Uani 1 1 d . U . . . O16 O 0.8497(15) 0.7009(11) 0.1536(10) 0.127(6) Uani 1 1 d . U . . . O17 O 1.1392(16) 0.5996(11) 0.1668(9) 0.116(6) Uani 1 1 d . U . . . O18 O 1.0509(16) 0.4956(14) 0.1197(11) 0.136(7) Uani 1 1 d . U . . . O19 O 0.606(2) 0.8822(12) 0.6045(11) 0.155(8) Uani 1 1 d . U . . . O20 O 0.587(2) 0.9918(14) 0.5433(12) 0.159(8) Uani 1 1 d . U . . . O21 O 0.4105(19) 0.8191(13) 0.5338(12) 0.150(8) Uani 1 1 d . U . . . O22 O 0.4126(19) 0.8102(13) 0.4351(12) 0.142(7) Uani 1 1 d . U . . . O23 O 0.474(2) 0.1957(17) -0.0048(11) 0.173(9) Uani 1 1 d . U . . . O24 O 0.611(2) 0.2809(17) -0.0128(12) 0.176(9) Uani 1 1 d . U . . . O25 O 0.523(2) 0.4185(15) 0.0937(15) 0.189(11) Uani 1 1 d . U . . . O26 O 0.6907(18) 0.3617(13) 0.0968(11) 0.149(8) Uani 1 1 d . U . . . O31 O 0.878(3) 0.097(2) 0.0236(16) 0.231(15) Uiso 1 1 d . . . . . O32 O -0.019(3) 0.960(2) 0.0560(16) 0.230(14) Uiso 1 1 d . . . . . N1 N 0.4793(19) 0.7213(17) 0.2989(11) 0.119(6) Uani 1 1 d . U . . . N2 N 0.6716(17) 0.7661(12) 0.3036(11) 0.101(5) Uani 1 1 d . U . . . N3 N 0.2908(19) 0.7978(10) 0.2282(12) 0.105(5) Uani 1 1 d . U . . . N4 N 0.2660(18) 0.8673(12) 0.1291(11) 0.109(5) Uani 1 1 d . U . . . N5 N 0.4725(17) 0.8996(14) 0.2144(13) 0.114(6) Uani 1 1 d . U . . . N6 N 0.382(2) 0.9329(14) 0.2999(12) 0.119(6) Uani 1 1 d . U . . . N7 N 0.5413(19) 0.7499(14) 0.1835(11) 0.105(5) Uani 1 1 d . U . . . N8 N 0.4689(16) 0.6152(12) 0.2025(11) 0.101(5) Uani 1 1 d . U . . . N9 N 0.953(2) 0.5999(14) 0.1276(12) 0.125(7) Uani 1 1 d . U . . . N10 N 0.556(2) 0.8713(18) 0.4993(13) 0.143(7) Uani 1 1 d . U . . . N11 N 0.524(3) 0.2947(19) 0.0667(16) 0.166(8) Uani 1 1 d . U . . . C1 C 0.724(2) 0.5697(18) 0.2252(17) 0.112(7) Uani 1 1 d . U . . . C2 C 0.754(2) 0.5416(15) 0.2817(16) 0.109(6) Uani 1 1 d . U . . . C3 C 0.735(3) 0.5823(15) 0.3259(16) 0.118(7) Uani 1 1 d . U . . . C4 C 0.695(3) 0.554(2) 0.1293(16) 0.141(11) Uani 1 1 d . U . . . H4A H 0.7080 0.5171 0.1036 0.169 Uiso 1 1 calc R U . . . H4B H 0.6216 0.5626 0.1223 0.169 Uiso 1 1 calc R U . . . H4C H 0.7281 0.6008 0.1238 0.169 Uiso 1 1 calc R U . . . C5 C 0.793(2) 0.4737(15) 0.2858(16) 0.114(7) Uani 1 1 d . U . . . H5 H 0.8016 0.4520 0.2527 0.137 Uiso 1 1 calc R U . . . C6 C 0.823(2) 0.4286(13) 0.3369(15) 0.106(7) Uani 1 1 d . U . . . C7 C 0.764(2) 0.4300(15) 0.3827(16) 0.113(7) Uani 1 1 d . U . . . C8 C 0.792(3) 0.3829(14) 0.4290(16) 0.127(8) Uani 1 1 d . U . . . H8 H 0.7516 0.3807 0.4549 0.153 Uiso 1 1 calc R U . . . C9 C 0.879(3) 0.3397(18) 0.4372(17) 0.130(9) Uani 1 1 d . U . . . C10 C 0.935(3) 0.3360(16) 0.3937(16) 0.128(9) Uani 1 1 d . U . . . H10 H 0.9922 0.3043 0.3974 0.154 Uiso 1 1 calc R U . . . C11 C 0.903(3) 0.3794(15) 0.3479(16) 0.121(8) Uani 1 1 d . U . . . C12 C 0.621(3) 0.480(2) 0.4092(16) 0.149(14) Uani 1 1 d . U . . . H12A H 0.5619 0.5104 0.3927 0.179 Uiso 1 1 calc R U . . . H12B H 0.5987 0.4319 0.4197 0.179 Uiso 1 1 calc R U . . . H12C H 0.6623 0.5047 0.4421 0.179 Uiso 1 1 calc R U . . . C13 C 0.854(3) 0.294(2) 0.5205(18) 0.163(14) Uani 1 1 d . U . . . H13A H 0.8843 0.2574 0.5488 0.195 Uiso 1 1 calc R U . . . H13B H 0.8567 0.3427 0.5375 0.195 Uiso 1 1 calc R U . . . H13C H 0.7831 0.2805 0.5040 0.195 Uiso 1 1 calc R U . . . C14 C 1.026(4) 0.329(3) 0.3090(19) 0.20(2) Uani 1 1 d . U . . . H14A H 1.0543 0.3312 0.2765 0.237 Uiso 1 1 calc R U . . . H14B H 1.0794 0.3406 0.3423 0.237 Uiso 1 1 calc R U . . . H14C H 1.0008 0.2789 0.3124 0.237 Uiso 1 1 calc R U . . . C15 C 0.809(3) 0.6008(17) 0.3788(16) 0.125(8) Uani 1 1 d . U . . . C16 C 0.778(3) 0.6273(16) 0.4245(17) 0.138(9) Uani 1 1 d . U . . . H16 H 0.7084 0.6339 0.4232 0.166 Uiso 1 1 calc R U . . . C17 C 0.850(4) 0.6429(19) 0.470(2) 0.156(10) Uani 1 1 d . U . . . C18 C 0.948(4) 0.637(2) 0.479(2) 0.167(12) Uani 1 1 d . U . . . H18 H 0.9932 0.6484 0.5134 0.201 Uiso 1 1 calc R U . . . C19 C 0.981(3) 0.612(2) 0.4338(18) 0.154(11) Uani 1 1 d . U . . . H19 H 1.0514 0.6099 0.4372 0.185 Uiso 1 1 calc R U . . . C20 C 0.916(3) 0.5882(19) 0.3827(17) 0.138(10) Uani 1 1 d . U . . . H20 H 0.9398 0.5664 0.3538 0.165 Uiso 1 1 calc R U . . . C21 C 0.875(5) 0.662(4) 0.579(2) 0.29(3) Uani 1 1 d . U . . . H21A H 0.8350 0.6748 0.6054 0.349 Uiso 1 1 calc R U . . . H21B H 0.9060 0.6137 0.5881 0.349 Uiso 1 1 calc R U . . . H21C H 0.9282 0.6994 0.5813 0.349 Uiso 1 1 calc R U . . . C22 C 0.120(3) 0.992(2) 0.1828(18) 0.139(10) Uani 1 1 d . U . . . C23 C 0.178(2) 1.0631(18) 0.1857(17) 0.124(8) Uani 1 1 d . U . . . C24 C 0.285(2) 1.0712(15) 0.2076(15) 0.110(7) Uani 1 1 d . U . . . C25 C -0.020(5) 0.929(4) 0.199(5) 0.20(3) Uani 0.5 1 d . U P A 1 H25A H -0.0938 0.9254 0.1848 0.307 Uiso 0.5 1 calc R U P A 1 H25B H 0.0102 0.8803 0.1959 0.307 Uiso 0.5 1 calc R U P A 1 H25C H -0.0040 0.9436 0.2380 0.307 Uiso 0.5 1 calc R U P A 1 C25A C -0.019(5) 0.914(3) 0.142(3) 0.13(2) Uani 0.5 1 d . U P A 2 H25D H -0.0916 0.9182 0.1254 0.201 Uiso 0.5 1 calc R U P A 2 H25E H 0.0141 0.8940 0.1139 0.201 Uiso 0.5 1 calc R U P A 2 H25F H -0.0067 0.8801 0.1734 0.201 Uiso 0.5 1 calc R U P A 2 C26 C 0.114(3) 1.1194(19) 0.1594(16) 0.131(9) Uani 1 1 d . U . . . H26 H 0.0436 1.1126 0.1549 0.157 Uiso 1 1 calc R U . . . C27 C 0.148(3) 1.1896(18) 0.1380(13) 0.113(7) Uani 1 1 d . U . . . C28 C 0.237(3) 1.200(2) 0.1200(16) 0.127(8) Uani 1 1 d . U . . . C29 C 0.252(3) 1.2638(16) 0.0920(15) 0.119(8) Uani 1 1 d . U . . . H29 H 0.3103 1.2701 0.0785 0.143 Uiso 1 1 calc R U . . . C30 C 0.179(3) 1.3168(18) 0.0846(15) 0.125(8) Uani 1 1 d . U . . . C31 C 0.095(2) 1.3131(16) 0.1056(13) 0.110(8) Uani 1 1 d . U . . . H31 H 0.0553 1.3556 0.1065 0.133 Uiso 1 1 calc R U . . . C32 C 0.071(3) 1.2477(18) 0.1249(16) 0.126(8) Uani 1 1 d . U . . . C33 C 0.396(2) 1.1536(18) 0.1124(15) 0.128(10) Uani 1 1 d . U . . . H33A H 0.4380 1.1093 0.1210 0.154 Uiso 1 1 calc R U . . . H33B H 0.3798 1.1628 0.0724 0.154 Uiso 1 1 calc R U . . . H33C H 0.4327 1.1959 0.1321 0.154 Uiso 1 1 calc R U . . . C34 C 0.281(3) 1.390(2) 0.0363(19) 0.182(17) Uani 1 1 d . U . . . H34A H 0.2814 1.4381 0.0181 0.218 Uiso 1 1 calc R U . . . H34B H 0.3407 1.3859 0.0673 0.218 Uiso 1 1 calc R U . . . H34C H 0.2809 1.3507 0.0096 0.218 Uiso 1 1 calc R U . . . C35 C -0.075(2) 1.2908(16) 0.1509(14) 0.117(10) Uani 1 1 d . U . . . H35A H -0.1197 1.2761 0.1744 0.140 Uiso 1 1 calc R U . . . H35B H -0.0443 1.3386 0.1634 0.140 Uiso 1 1 calc R U . . . H35C H -0.1148 1.2949 0.1125 0.140 Uiso 1 1 calc R U . . . C36 C 0.321(3) 1.1343(16) 0.2465(13) 0.115(8) Uani 1 1 d . U . . . C37 C 0.424(3) 1.1448(17) 0.2544(12) 0.116(8) Uani 1 1 d . U . . . H37 H 0.4622 1.1151 0.2360 0.140 Uiso 1 1 calc R U . . . C38 C 0.468(3) 1.2001(19) 0.2904(14) 0.130(9) Uani 1 1 d . U . . . C39 C 0.411(3) 1.243(2) 0.3172(16) 0.138(10) Uani 1 1 d . U . . . H39 H 0.4416 1.2827 0.3405 0.165 Uiso 1 1 calc R U . . . C40 C 0.314(3) 1.230(2) 0.3104(15) 0.130(9) Uani 1 1 d . U . . . H40 H 0.2779 1.2562 0.3322 0.156 Uiso 1 1 calc R U . . . C41 C 0.261(3) 1.1762(17) 0.2704(14) 0.125(9) Uani 1 1 d . U . . . H41 H 0.1896 1.1706 0.2616 0.150 Uiso 1 1 calc R U . . . C42 C 0.624(3) 1.275(2) 0.3332(15) 0.139(12) Uani 1 1 d . U . . . H42A H 0.6954 1.2772 0.3321 0.167 Uiso 1 1 calc R U . . . H42B H 0.5914 1.3223 0.3205 0.167 Uiso 1 1 calc R U . . . H42C H 0.6197 1.2656 0.3712 0.167 Uiso 1 1 calc R U . . . C43 C 0.375(2) 0.6958(15) 0.2940(12) 0.096(6) Uani 1 1 d . U . . . H43 H 0.3555 0.6613 0.2618 0.115 Uiso 1 1 calc R U . . . C44 C 0.370(2) 0.6544(16) 0.3457(13) 0.108(8) Uani 1 1 d . U . . . H44A H 0.3950 0.6867 0.3781 0.130 Uiso 1 1 calc R U . . . H44B H 0.4150 0.6110 0.3498 0.130 Uiso 1 1 calc R U . . . C45 C 0.264(2) 0.6283(18) 0.3458(16) 0.127(9) Uani 1 1 d . U . . . H45A H 0.2391 0.5929 0.3151 0.152 Uiso 1 1 calc R U . . . H45B H 0.2651 0.6030 0.3811 0.152 Uiso 1 1 calc R U . . . C46 C 0.197(2) 0.6920(15) 0.3390(16) 0.128(9) Uani 1 1 d . U . . . H46A H 0.2213 0.7266 0.3702 0.154 Uiso 1 1 calc R U . . . H46B H 0.1280 0.6758 0.3398 0.154 Uiso 1 1 calc R U . . . C47 C 0.193(2) 0.7317(15) 0.2845(14) 0.109(7) Uani 1 1 d . U . . . H47A H 0.1443 0.7733 0.2800 0.131 Uiso 1 1 calc R U . . . H47B H 0.1685 0.6972 0.2532 0.131 Uiso 1 1 calc R U . . . C48 C 0.300(2) 0.7614(15) 0.2838(14) 0.105(6) Uani 1 1 d . U . . . H48 H 0.3224 0.7987 0.3139 0.126 Uiso 1 1 calc R U . . . C49 C 0.527(2) 0.7655(16) 0.3359(14) 0.099(6) Uani 1 1 d . U . . . H49 H 0.4913 0.7848 0.3608 0.118 Uiso 1 1 calc R U . . . C50 C 0.631(2) 0.7891(14) 0.3441(15) 0.096(6) Uani 1 1 d . U . . . C51 C 0.674(2) 0.8235(17) 0.3879(13) 0.101(7) Uani 1 1 d . U . . . H51 H 0.6364 0.8361 0.4138 0.122 Uiso 1 1 calc R U . . . C52 C 0.774(2) 0.8427(17) 0.3985(14) 0.114(8) Uani 1 1 d . U . . . H52 H 0.8061 0.8698 0.4306 0.137 Uiso 1 1 calc R U . . . C53 C 0.827(2) 0.8197(14) 0.3587(14) 0.099(7) Uani 1 1 d . U . . . C54 C 0.928(2) 0.8380(19) 0.3635(15) 0.122(9) Uani 1 1 d . U . . . H54 H 0.9620 0.8669 0.3942 0.146 Uiso 1 1 calc R U . . . C55 C 0.978(3) 0.8165(17) 0.3268(15) 0.111(8) Uani 1 1 d . U . . . H55 H 1.0474 0.8281 0.3328 0.133 Uiso 1 1 calc R U . . . C56 C 0.930(2) 0.7786(17) 0.2812(15) 0.111(8) Uani 1 1 d . U . . . H56 H 0.9667 0.7634 0.2552 0.133 Uiso 1 1 calc R U . . . C57 C 0.827(2) 0.7619(16) 0.2726(14) 0.105(7) Uani 1 1 d . U . . . H57 H 0.7907 0.7399 0.2391 0.127 Uiso 1 1 calc R U . . . C58 C 0.777(2) 0.7795(14) 0.3171(15) 0.102(7) Uani 1 1 d . U . . . C59 C 0.2546(19) 0.7584(16) 0.1845(15) 0.101(6) Uani 1 1 d . U . . . H59 H 0.2417 0.7073 0.1874 0.121 Uiso 1 1 calc R U . . . C60 C 0.234(2) 0.7955(16) 0.1290(15) 0.105(6) Uani 1 1 d . U . . . C61 C 0.185(2) 0.7612(17) 0.0833(15) 0.112(7) Uani 1 1 d . U . . . H61 H 0.1694 0.7103 0.0850 0.134 Uiso 1 1 calc R U . . . C62 C 0.155(2) 0.798(2) 0.0327(17) 0.126(8) Uani 1 1 d . U . . . H62 H 0.1170 0.7744 0.0002 0.151 Uiso 1 1 calc R U . . . C63 C 0.185(3) 0.869(2) 0.0331(17) 0.127(8) Uani 1 1 d . U . . . C64 C 0.152(3) 0.916(2) -0.0170(16) 0.128(9) Uani 1 1 d . U . . . H64 H 0.1075 0.8971 -0.0499 0.153 Uiso 1 1 calc R U . . . C65 C 0.187(3) 0.985(2) -0.0139(16) 0.134(10) Uani 1 1 d . U . . . H65 H 0.1723 1.0145 -0.0466 0.161 Uiso 1 1 calc R U . . . C66 C 0.243(2) 1.0159(19) 0.0341(16) 0.120(9) Uani 1 1 d . U . . . H66 H 0.2641 1.0657 0.0339 0.144 Uiso 1 1 calc R U . . . C67 C 0.267(2) 0.9795(18) 0.0790(14) 0.108(8) Uani 1 1 d . U . . . H67 H 0.3057 1.0004 0.1124 0.130 Uiso 1 1 calc R U . . . C68 C 0.233(2) 0.9076(19) 0.0760(15) 0.110(7) Uani 1 1 d . U . . . C69 C 0.513(2) 0.8821(17) 0.1613(15) 0.122(7) Uani 1 1 d . U . . . H69 H 0.4560 0.8679 0.1291 0.147 Uiso 1 1 calc R U . . . C70 C 0.563(2) 0.9542(18) 0.1503(18) 0.141(10) Uani 1 1 d . U . . . H70A H 0.5113 0.9935 0.1408 0.169 Uiso 1 1 calc R U . . . H70B H 0.6137 0.9694 0.1843 0.169 Uiso 1 1 calc R U . . . C71 C 0.614(3) 0.9455(19) 0.1040(18) 0.147(10) Uani 1 1 d . U . . . H71A H 0.5622 0.9352 0.0692 0.176 Uiso 1 1 calc R U . . . H71B H 0.6481 0.9923 0.0990 0.176 Uiso 1 1 calc R U . . . C72 C 0.690(2) 0.8847(17) 0.1150(15) 0.124(9) Uani 1 1 d . U . . . H72A H 0.7468 0.8982 0.1464 0.149 Uiso 1 1 calc R U . . . H72B H 0.7163 0.8768 0.0820 0.149 Uiso 1 1 calc R U . . . C73 C 0.641(3) 0.8145(17) 0.1285(15) 0.124(9) Uani 1 1 d . U . . . H73A H 0.6930 0.7755 0.1378 0.148 Uiso 1 1 calc R U . . . H73B H 0.5893 0.7982 0.0951 0.148 Uiso 1 1 calc R U . . . C74 C 0.590(2) 0.8219(16) 0.1763(14) 0.107(7) Uani 1 1 d . U . . . H74 H 0.6413 0.8350 0.2111 0.128 Uiso 1 1 calc R U . . . C75 C 0.529(2) 0.9220(16) 0.2600(16) 0.115(7) Uani 1 1 d . U . . . H75 H 0.5996 0.9255 0.2643 0.139 Uiso 1 1 calc R U . . . C76 C 0.484(3) 0.9430(17) 0.3068(17) 0.120(7) Uani 1 1 d . U . . . C77 C 0.545(3) 0.9786(17) 0.3516(18) 0.124(8) Uani 1 1 d . U . . . H77 H 0.6145 0.9887 0.3545 0.149 Uiso 1 1 calc R U . . . C78 C 0.496(3) 0.9984(19) 0.3922(18) 0.135(9) Uani 1 1 d . U . . . H78 H 0.5360 1.0209 0.4248 0.162 Uiso 1 1 calc R U . . . C79 C 0.398(3) 0.9884(18) 0.3889(18) 0.133(9) Uani 1 1 d . U . . . C80 C 0.344(3) 1.010(2) 0.4330(18) 0.145(10) Uani 1 1 d . U . . . H80 H 0.3784 1.0318 0.4672 0.174 Uiso 1 1 calc R U . . . C81 C 0.245(3) 0.996(2) 0.4198(18) 0.151(11) Uani 1 1 d . U . . . H81 H 0.2089 1.0085 0.4466 0.182 Uiso 1 1 calc R U . . . C82 C 0.190(3) 0.9660(19) 0.3707(17) 0.137(10) Uani 1 1 d . U . . . H82 H 0.1183 0.9635 0.3630 0.164 Uiso 1 1 calc R U . . . C83 C 0.236(3) 0.9415(17) 0.3359(15) 0.117(8) Uani 1 1 d . U . . . H83 H 0.1997 0.9129 0.3055 0.140 Uiso 1 1 calc R U . . . C84 C 0.343(3) 0.9561(16) 0.3413(16) 0.113(7) Uani 1 1 d . U . . . C85 C 0.475(2) 0.7176(19) 0.1472(17) 0.116(8) Uani 1 1 d . U . . . H85 H 0.4513 0.7422 0.1127 0.139 Uiso 1 1 calc R U . . . C86 C 0.430(2) 0.6450(18) 0.1532(16) 0.107(7) Uani 1 1 d . U . . . C87 C 0.360(2) 0.6180(18) 0.1112(15) 0.110(7) Uani 1 1 d . U . . . H87 H 0.3387 0.6435 0.0769 0.132 Uiso 1 1 calc R U . . . C88 C 0.318(2) 0.5505(19) 0.1200(16) 0.119(8) Uani 1 1 d . U . . . H88 H 0.2677 0.5270 0.0920 0.142 Uiso 1 1 calc R U . . . C89 C 0.357(2) 0.5175(16) 0.1746(16) 0.113(8) Uani 1 1 d . U . . . C90 C 0.311(3) 0.4471(18) 0.1854(18) 0.127(9) Uani 1 1 d . U . . . H90 H 0.2565 0.4259 0.1582 0.153 Uiso 1 1 calc R U . . . C91 C 0.346(2) 0.414(2) 0.2345(17) 0.125(9) Uani 1 1 d . U . . . H91 H 0.3199 0.3682 0.2439 0.149 Uiso 1 1 calc R U . . . C92 C 0.425(3) 0.4508(19) 0.2704(16) 0.124(9) Uani 1 1 d . U . . . H92 H 0.4525 0.4275 0.3051 0.149 Uiso 1 1 calc R U . . . C93 C 0.467(2) 0.5145(16) 0.2625(15) 0.108(7) Uani 1 1 d . U . . . H93 H 0.5212 0.5354 0.2901 0.130 Uiso 1 1 calc R U . . . C94 C 0.428(2) 0.5500(17) 0.2109(16) 0.110(7) Uani 1 1 d . U . . . C95 C 0.890(3) 0.719(2) 0.0600(17) 0.130(7) Uani 1 1 d . U . . . C96 C 1.035(4) 0.522(2) 0.220(2) 0.136(7) Uani 1 1 d . U . . . C97 C 0.731(4) 0.912(3) 0.548(2) 0.167(9) Uani 1 1 d . U . . . C98 C 0.532(4) 0.725(3) 0.509(3) 0.160(9) Uani 1 1 d . U . . . C99 C 0.642(4) 0.170(3) 0.058(2) 0.159(9) Uani 1 1 d . U . . . C100 C 0.603(4) 0.323(3) 0.173(2) 0.154(8) Uani 1 1 d . U . . . F19 F 0.687(4) 1.070(4) 0.261(2) 0.22(2) Uani 0.235(14) 1 d G U P B 1 F20 F 0.795(6) 1.158(3) 0.282(2) 0.24(3) Uani 0.235(14) 1 d G U P B 1 F21 F 0.788(6) 1.092(4) 0.210(2) 0.22(2) Uani 0.235(14) 1 d G U P B 1 F22 F 0.725(4) 1.042(4) 0.443(2) 0.18(2) Uani 0.235(14) 1 d G U P B 1 F23 F 0.848(5) 1.073(4) 0.511(2) 0.22(3) Uani 0.235(14) 1 d G U P B 1 F24 F 0.800(5) 1.146(3) 0.441(2) 0.26(2) Uani 0.235(14) 1 d G U P B 1 O27 O 0.961(4) 1.007(4) 0.445(2) 0.25(3) Uani 0.235(14) 1 d G U P B 1 O28 O 0.900(4) 1.119(3) 0.401(2) 0.25(2) Uani 0.235(14) 1 d G U P B 1 O29 O 0.819(6) 0.942(3) 0.279(2) 0.21(2) Uani 0.235(14) 1 d G U P B 1 O30 O 0.933(4) 1.042(4) 0.299(2) 0.22(3) Uani 0.235(14) 1 d G U P B 1 S7 S 0.881(3) 1.042(3) 0.406(2) 0.236(14) Uani 0.235(14) 1 d G U P B 1 S8 S 0.846(4) 1.012(3) 0.301(2) 0.218(13) Uani 0.235(14) 1 d G U P B 1 N12 N 0.823(4) 1.000(2) 0.356(2) 0.222(15) Uani 0.235(14) 1 d G U P B 1 C101 C 0.775(5) 1.091(3) 0.253(2) 0.212(17) Uani 0.235(14) 1 d G U P B 1 C102 C 0.814(4) 1.074(3) 0.456(2) 0.224(17) Uani 0.235(14) 1 d G U P B 1 F19A F 0.7140(15) 1.0979(11) 0.2193(7) 0.196(11) Uani 0.765(14) 1 d G U P B 2 F20A F 0.8582(19) 1.1508(10) 0.2423(7) 0.29(2) Uani 0.765(14) 1 d G U P B 2 F21A F 0.827(2) 1.0735(13) 0.1756(6) 0.266(16) Uani 0.765(14) 1 d G U P B 2 F22A F 0.7121(14) 1.1111(14) 0.3983(9) 0.211(13) Uani 0.765(14) 1 d G U P B 2 F23A F 0.8361(19) 1.1213(14) 0.4704(7) 0.190(18) Uani 0.235(14) 1 d G U P B 2 F24A F 0.8366(18) 1.1827(9) 0.3964(8) 0.292(17) Uani 0.765(14) 1 d G U P B 2 O27A O 0.9164(18) 1.0090(11) 0.4176(6) 0.260(19) Uani 0.765(14) 1 d G U P B 2 O28A O 0.9222(11) 1.1168(10) 0.3656(7) 0.286(18) Uani 0.765(14) 1 d G U P B 2 O29A O 0.769(2) 0.9466(8) 0.2511(8) 0.180(19) Uani 0.235(14) 1 d G U P B 2 O30A O 0.9261(15) 1.0090(12) 0.2737(7) 0.190(13) Uani 0.765(14) 1 d G U P B 2 S7A S 0.8635(12) 1.0538(8) 0.3729(6) 0.207(7) Uani 0.765(14) 1 d G U P B 2 S8A S 0.8279(15) 1.0084(8) 0.2712(6) 0.229(8) Uani 0.765(14) 1 d G U P B 2 N12A N 0.7939(13) 1.0196(7) 0.3229(7) 0.212(11) Uani 0.765(14) 1 d G U P B 2 C103 C 0.8084(17) 1.0884(10) 0.2165(6) 0.217(14) Uani 0.765(14) 1 d G U P B 2 C104 C 0.8113(14) 1.1168(10) 0.4148(7) 0.220(12) Uani 0.765(14) 1 d G U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.100(3) 0.085(3) 0.135(4) 0.002(3) 0.054(3) -0.001(3) Ni2 0.098(3) 0.077(3) 0.147(4) 0.007(3) 0.044(3) 0.002(2) S1 0.101(5) 0.086(5) 0.165(7) -0.001(5) 0.049(5) -0.008(4) S2 0.125(6) 0.098(6) 0.155(8) -0.001(5) 0.049(6) 0.005(5) S3 0.164(8) 0.115(7) 0.172(9) 0.000(6) 0.069(7) -0.001(6) S4 0.150(8) 0.119(7) 0.171(9) -0.008(7) 0.067(7) -0.009(6) S5 0.161(9) 0.142(8) 0.157(9) 0.013(6) 0.051(7) -0.010(6) S6 0.155(8) 0.116(7) 0.208(10) 0.006(7) 0.054(8) -0.010(7) F1 0.144(12) 0.138(14) 0.168(14) -0.018(14) 0.045(12) -0.011(12) F2 0.175(17) 0.078(10) 0.184(17) 0.006(10) 0.035(14) -0.011(10) F3 0.125(10) 0.068(9) 0.166(13) -0.006(10) 0.030(9) 0.000(8) F4 0.164(16) 0.119(13) 0.176(15) 0.009(11) 0.079(14) -0.005(11) F5 0.131(12) 0.096(12) 0.210(19) 0.026(11) 0.054(11) 0.020(9) F6 0.135(12) 0.143(16) 0.174(16) 0.042(12) 0.070(11) 0.018(11) F7 0.29(3) 0.24(2) 0.203(19) -0.097(17) 0.145(19) -0.12(2) F8 0.181(18) 0.187(18) 0.29(3) -0.084(17) 0.04(2) 0.028(16) F9 0.176(14) 0.21(2) 0.207(19) -0.098(18) 0.102(14) -0.031(17) F10 0.25(2) 0.121(14) 0.132(14) -0.013(11) 0.079(13) 0.026(12) F11 0.24(2) 0.129(12) 0.20(2) 0.005(15) 0.095(16) -0.009(15) F12 0.211(19) 0.156(17) 0.134(13) 0.019(13) 0.066(13) 0.031(13) F13 0.25(3) 0.160(18) 0.162(18) 0.011(13) 0.069(16) 0.035(15) F14 0.166(14) 0.126(16) 0.22(2) 0.015(13) 0.053(13) 0.002(12) F15 0.151(15) 0.114(14) 0.195(19) 0.016(11) 0.058(14) 0.011(11) F16 0.177(17) 0.149(16) 0.22(2) 0.027(14) 0.087(17) 0.027(14) F17 0.139(13) 0.151(17) 0.205(19) -0.012(15) 0.050(14) -0.004(12) F18 0.21(2) 0.144(17) 0.220(15) -0.028(16) 0.055(18) -0.056(16) O1 0.164(15) 0.094(12) 0.114(11) 0.009(10) 0.033(10) 0.009(10) O2 0.095(10) 0.090(11) 0.149(13) -0.003(9) 0.081(10) 0.009(8) O3 0.120(13) 0.066(11) 0.153(14) 0.006(10) 0.062(13) 0.000(10) O4 0.26(3) 0.19(3) 0.179(19) -0.03(2) 0.084(19) -0.02(2) O5 0.090(12) 0.107(15) 0.157(18) 0.012(12) 0.031(11) 0.007(10) O6 0.162(19) 0.132(18) 0.16(2) 0.031(14) 0.045(15) 0.049(15) O7 0.134(16) 0.135(18) 0.19(2) 0.050(16) 0.072(14) 0.054(13) O8 0.110(11) 0.051(7) 0.177(16) 0.008(9) 0.048(12) -0.008(7) O9 0.071(8) 0.096(11) 0.184(17) 0.015(11) 0.050(9) 0.016(7) O10 0.090(11) 0.099(14) 0.33(3) 0.040(18) 0.010(16) -0.003(10) O11 0.113(13) 0.102(13) 0.18(2) 0.010(13) 0.053(13) -0.002(10) O12 0.150(17) 0.087(12) 0.17(2) 0.000(12) 0.055(13) -0.004(12) O13 0.113(14) 0.095(14) 0.22(2) 0.024(15) 0.059(14) 0.020(11) O14 0.152(14) 0.124(17) 0.154(19) -0.008(13) 0.049(15) -0.029(13) O15 0.130(12) 0.070(10) 0.155(16) 0.009(11) 0.060(11) -0.007(9) O16 0.106(11) 0.108(15) 0.168(17) -0.014(13) 0.037(12) -0.007(11) O17 0.117(11) 0.091(13) 0.146(18) 0.018(11) 0.047(12) 0.019(9) O18 0.124(15) 0.115(14) 0.174(18) -0.009(12) 0.050(15) -0.008(11) O19 0.22(2) 0.093(15) 0.166(15) -0.013(12) 0.066(17) -0.030(15) O20 0.177(19) 0.103(11) 0.20(2) 0.018(13) 0.058(18) -0.007(13) O21 0.172(19) 0.106(15) 0.198(19) -0.029(16) 0.094(16) -0.033(13) O22 0.150(17) 0.116(16) 0.175(14) -0.014(14) 0.072(12) -0.007(13) O23 0.189(18) 0.18(2) 0.16(2) 0.012(14) 0.053(14) -0.051(15) O24 0.17(2) 0.19(2) 0.17(2) 0.012(16) 0.042(15) -0.059(17) O25 0.150(18) 0.116(16) 0.28(3) 0.013(17) 0.03(2) 0.006(12) O26 0.141(12) 0.111(16) 0.19(2) 0.042(16) 0.026(14) 0.012(13) N1 0.113(11) 0.16(2) 0.107(16) -0.016(11) 0.073(12) 0.007(10) N2 0.094(10) 0.074(10) 0.138(14) -0.003(10) 0.036(9) 0.023(9) N3 0.129(15) 0.037(8) 0.164(12) 0.002(8) 0.066(14) 0.014(8) N4 0.121(14) 0.069(11) 0.142(9) -0.013(8) 0.046(11) -0.001(11) N5 0.078(9) 0.094(14) 0.174(16) 0.029(14) 0.040(10) 0.026(10) N6 0.123(12) 0.091(14) 0.142(10) -0.010(10) 0.030(9) -0.005(14) N7 0.106(16) 0.101(11) 0.120(12) 0.020(10) 0.048(10) 0.006(9) N8 0.085(11) 0.075(11) 0.146(14) -0.005(8) 0.035(10) 0.004(9) N9 0.117(12) 0.093(10) 0.159(18) -0.013(12) 0.019(14) -0.011(9) N10 0.141(15) 0.132(14) 0.176(16) -0.012(14) 0.075(14) -0.002(12) N11 0.168(19) 0.132(17) 0.202(18) -0.003(14) 0.054(15) -0.002(13) C1 0.096(17) 0.083(16) 0.152(14) -0.008(12) 0.021(17) 0.011(12) C2 0.110(17) 0.051(12) 0.158(13) -0.007(10) 0.021(15) -0.015(11) C3 0.156(18) 0.047(13) 0.150(14) 0.012(11) 0.038(13) -0.014(11) C4 0.19(3) 0.11(2) 0.152(16) 0.032(19) 0.10(2) -0.01(2) C5 0.098(18) 0.069(14) 0.18(2) 0.004(12) 0.033(16) -0.001(12) C6 0.099(16) 0.048(13) 0.165(19) -0.016(12) 0.022(13) 0.008(10) C7 0.099(16) 0.060(15) 0.18(2) 0.011(13) 0.033(14) -0.004(11) C8 0.15(2) 0.051(15) 0.18(2) 0.007(14) 0.042(17) 0.017(13) C9 0.14(2) 0.088(19) 0.16(2) 0.020(16) 0.036(16) 0.026(15) C10 0.16(2) 0.067(17) 0.16(2) 0.016(15) 0.040(17) 0.033(16) C11 0.14(2) 0.063(16) 0.16(2) 0.012(14) 0.053(15) 0.031(13) C12 0.14(3) 0.14(3) 0.19(3) 0.09(3) 0.07(2) 0.06(2) C13 0.19(4) 0.14(3) 0.16(3) 0.03(3) 0.06(2) 0.02(3) C14 0.24(4) 0.18(4) 0.20(4) 0.03(3) 0.10(3) 0.13(3) C15 0.147(15) 0.097(19) 0.139(17) 0.003(16) 0.049(13) 0.002(18) C16 0.16(2) 0.11(2) 0.159(19) -0.01(2) 0.066(16) -0.01(2) C17 0.21(2) 0.11(2) 0.151(19) -0.01(2) 0.053(18) -0.01(3) C18 0.19(2) 0.15(3) 0.15(2) -0.03(2) 0.03(2) -0.05(3) C19 0.159(19) 0.15(3) 0.15(3) 0.01(2) 0.036(15) -0.04(2) C20 0.151(16) 0.11(2) 0.16(2) -0.02(2) 0.050(16) -0.01(2) C21 0.33(6) 0.38(7) 0.17(2) -0.09(5) 0.08(3) -0.18(6) C22 0.088(11) 0.102(14) 0.22(3) 0.017(18) 0.029(18) 0.006(9) C23 0.113(12) 0.088(13) 0.18(2) -0.011(14) 0.061(16) -0.003(10) C24 0.120(13) 0.055(10) 0.17(2) 0.003(12) 0.061(15) -0.004(10) C25 0.09(3) 0.11(5) 0.37(7) 0.06(5) -0.01(5) -0.04(4) C25A 0.12(4) 0.09(3) 0.18(5) 0.09(3) 0.00(4) -0.02(3) C26 0.133(18) 0.098(14) 0.17(3) -0.009(17) 0.059(17) 0.013(14) C27 0.149(17) 0.094(13) 0.110(19) -0.028(13) 0.059(15) 0.018(13) C28 0.146(18) 0.103(17) 0.14(2) -0.009(16) 0.056(17) 0.010(13) C29 0.135(19) 0.071(14) 0.17(3) -0.036(13) 0.063(17) 0.004(12) C30 0.17(2) 0.084(14) 0.15(2) -0.017(14) 0.089(17) 0.024(14) C31 0.128(19) 0.074(13) 0.14(2) -0.034(14) 0.057(15) 0.001(13) C32 0.148(19) 0.076(13) 0.16(2) -0.018(15) 0.061(16) 0.006(13) C33 0.15(2) 0.10(2) 0.15(3) 0.02(2) 0.08(2) -0.003(18) C34 0.22(4) 0.15(3) 0.22(4) -0.02(3) 0.14(3) -0.01(3) C35 0.11(2) 0.087(19) 0.14(3) 0.027(19) 0.024(19) 0.023(14) C36 0.150(16) 0.077(15) 0.13(2) 0.006(12) 0.058(16) -0.016(14) C37 0.141(16) 0.091(18) 0.12(2) 0.011(13) 0.039(17) -0.007(15) C38 0.140(16) 0.13(2) 0.13(2) -0.010(15) 0.051(17) -0.016(15) C39 0.162(19) 0.10(2) 0.15(2) -0.003(16) 0.04(2) 0.02(2) C40 0.16(2) 0.11(2) 0.12(2) -0.002(14) 0.05(2) 0.03(2) C41 0.16(2) 0.081(18) 0.14(2) 0.013(13) 0.048(18) 0.018(16) C42 0.15(2) 0.15(3) 0.14(3) -0.011(19) 0.07(2) -0.05(2) C43 0.116(11) 0.079(15) 0.100(16) -0.006(11) 0.043(12) 0.017(10) C44 0.126(15) 0.078(16) 0.12(2) 0.013(13) 0.037(16) 0.005(13) C45 0.119(18) 0.092(19) 0.18(3) 0.017(16) 0.062(18) 0.018(14) C46 0.132(18) 0.058(15) 0.21(2) 0.028(17) 0.061(19) -0.002(13) C47 0.109(13) 0.062(15) 0.16(2) -0.004(13) 0.044(16) -0.008(12) C48 0.096(12) 0.068(13) 0.155(15) 0.014(12) 0.036(15) 0.006(10) C49 0.113(14) 0.082(17) 0.111(19) 0.038(10) 0.047(13) 0.013(12) C50 0.121(13) 0.049(14) 0.125(18) 0.032(10) 0.044(13) 0.016(11) C51 0.103(14) 0.10(2) 0.110(18) 0.023(13) 0.039(14) 0.028(14) C52 0.117(15) 0.096(19) 0.13(2) -0.003(15) 0.041(14) 0.006(16) C53 0.107(13) 0.048(14) 0.146(19) -0.007(13) 0.040(12) 0.010(12) C54 0.100(14) 0.11(2) 0.15(2) -0.001(17) 0.031(14) 0.011(15) C55 0.110(18) 0.084(19) 0.14(2) 0.000(16) 0.043(14) -0.012(15) C56 0.098(15) 0.10(2) 0.13(2) 0.020(15) 0.023(15) -0.003(16) C57 0.100(13) 0.104(19) 0.113(18) 0.016(15) 0.027(13) 0.007(15) C58 0.104(11) 0.060(15) 0.144(19) -0.007(13) 0.034(12) 0.015(12) C59 0.080(16) 0.062(11) 0.168(14) -0.003(10) 0.044(16) 0.017(12) C60 0.094(17) 0.067(12) 0.163(14) -0.012(10) 0.052(15) 0.019(12) C61 0.11(2) 0.095(17) 0.158(16) -0.031(12) 0.080(17) -0.033(15) C62 0.10(2) 0.126(17) 0.159(17) -0.029(15) 0.052(19) -0.023(17) C63 0.11(2) 0.127(17) 0.148(15) -0.014(13) 0.040(17) -0.031(17) C64 0.12(2) 0.14(2) 0.127(16) -0.029(15) 0.039(17) -0.029(19) C65 0.14(3) 0.14(2) 0.123(19) -0.003(17) 0.030(18) -0.01(2) C66 0.12(2) 0.100(18) 0.13(2) 0.006(13) 0.030(19) -0.028(17) C67 0.13(2) 0.099(15) 0.104(18) -0.002(12) 0.048(17) -0.006(16) C68 0.089(17) 0.097(14) 0.142(12) -0.003(11) 0.028(15) 0.002(14) C69 0.104(16) 0.105(14) 0.170(18) 0.043(16) 0.057(14) 0.022(12) C70 0.106(19) 0.098(15) 0.24(3) 0.04(2) 0.088(18) 0.033(15) C71 0.15(2) 0.092(17) 0.23(3) 0.02(2) 0.09(2) 0.001(16) C72 0.12(2) 0.111(19) 0.16(2) 0.001(18) 0.084(17) 0.000(14) C73 0.14(2) 0.094(16) 0.16(2) 0.012(17) 0.074(17) 0.011(15) C74 0.103(16) 0.089(12) 0.14(2) 0.021(12) 0.056(13) 0.012(9) C75 0.097(11) 0.079(18) 0.165(18) 0.044(16) 0.021(11) 0.052(14) C76 0.110(13) 0.079(18) 0.167(17) 0.022(15) 0.022(11) 0.038(15) C77 0.103(16) 0.074(19) 0.19(2) 0.016(17) 0.019(13) 0.024(14) C78 0.141(17) 0.09(2) 0.17(2) 0.001(17) 0.034(16) -0.033(19) C79 0.147(17) 0.082(18) 0.178(19) -0.031(17) 0.056(15) -0.033(18) C80 0.17(2) 0.10(2) 0.17(2) -0.022(19) 0.058(18) -0.03(2) C81 0.15(2) 0.14(3) 0.17(3) -0.06(2) 0.06(2) 0.01(2) C82 0.15(2) 0.11(2) 0.16(3) -0.04(2) 0.069(17) -0.01(2) C83 0.127(15) 0.096(19) 0.13(2) -0.019(16) 0.036(15) 0.004(17) C84 0.128(14) 0.071(16) 0.144(15) 0.012(15) 0.039(13) 0.001(15) C85 0.085(18) 0.105(17) 0.162(17) 0.022(14) 0.041(13) 0.008(12) C86 0.070(16) 0.109(16) 0.154(17) 0.021(13) 0.051(12) 0.001(12) C87 0.096(19) 0.117(18) 0.131(17) 0.003(14) 0.054(12) 0.000(13) C88 0.105(19) 0.109(18) 0.158(19) -0.025(14) 0.065(15) -0.009(14) C89 0.107(19) 0.070(15) 0.17(2) -0.022(13) 0.047(15) -0.003(12) C90 0.11(2) 0.087(18) 0.18(2) -0.022(15) 0.034(19) -0.022(15) C91 0.10(2) 0.11(2) 0.18(3) -0.007(15) 0.064(18) -0.012(15) C92 0.13(2) 0.098(19) 0.15(2) 0.009(16) 0.048(17) -0.007(15) C93 0.101(18) 0.077(15) 0.16(2) -0.005(13) 0.057(15) 0.005(13) C94 0.101(18) 0.074(15) 0.165(19) -0.002(12) 0.049(15) -0.011(12) C95 0.13(2) 0.088(13) 0.175(14) 0.010(16) 0.050(12) -0.026(14) C96 0.15(2) 0.09(2) 0.179(18) 0.024(12) 0.070(17) 0.006(13) C97 0.168(14) 0.17(2) 0.17(2) -0.04(2) 0.060(18) -0.002(18) C98 0.17(3) 0.141(16) 0.19(2) 0.00(2) 0.070(16) 0.017(12) C99 0.17(2) 0.13(2) 0.19(3) -0.003(13) 0.066(16) -0.011(14) C100 0.15(2) 0.106(19) 0.204(16) -0.007(15) 0.05(2) -0.025(17) F19 0.19(4) 0.20(6) 0.25(7) -0.10(5) 0.06(4) 0.04(3) F20 0.25(6) 0.18(3) 0.25(6) 0.03(4) -0.02(6) 0.01(4) F21 0.23(5) 0.20(5) 0.22(3) 0.06(3) 0.02(4) 0.04(5) F22 0.14(3) 0.19(5) 0.17(5) 0.07(5) -0.01(3) 0.05(4) F23 0.16(5) 0.22(7) 0.27(3) -0.05(4) 0.03(4) -0.06(6) F24 0.24(5) 0.20(3) 0.34(5) -0.02(4) 0.08(4) 0.00(3) O27 0.23(6) 0.25(6) 0.29(7) -0.01(5) 0.05(4) 0.05(5) O28 0.24(5) 0.23(3) 0.31(5) 0.02(4) 0.11(4) 0.02(4) O29 0.24(5) 0.18(2) 0.25(4) 0.08(3) 0.11(5) -0.01(3) O30 0.18(3) 0.20(5) 0.29(6) 0.07(6) 0.04(4) 0.01(3) S7 0.21(3) 0.22(3) 0.28(3) 0.03(2) 0.08(2) 0.03(2) S8 0.21(2) 0.19(2) 0.25(2) 0.09(2) 0.05(2) 0.00(2) N12 0.23(3) 0.19(3) 0.25(2) 0.07(2) 0.07(2) 0.05(3) C101 0.21(3) 0.18(3) 0.22(3) 0.04(2) 0.01(3) 0.02(3) C102 0.18(3) 0.23(3) 0.27(3) 0.02(3) 0.06(3) 0.01(3) F19A 0.29(3) 0.13(2) 0.15(2) -0.013(17) 0.02(2) 0.003(19) F20A 0.31(4) 0.22(3) 0.27(4) 0.07(2) -0.06(3) -0.03(3) F21A 0.33(4) 0.24(3) 0.23(3) 0.08(2) 0.07(3) 0.13(3) F22A 0.164(17) 0.25(3) 0.23(3) -0.10(3) 0.061(19) -0.03(2) F23A 0.11(4) 0.13(5) 0.31(3) -0.03(3) 0.02(3) 0.03(4) F24A 0.29(3) 0.18(2) 0.41(5) 0.02(3) 0.09(4) -0.03(3) O27A 0.29(4) 0.19(3) 0.27(4) 0.05(2) 0.01(3) 0.09(3) O28A 0.28(4) 0.32(4) 0.29(4) 0.09(3) 0.13(3) -0.04(3) O29A 0.15(4) 0.24(4) 0.16(4) 0.11(2) 0.07(4) 0.02(4) O30A 0.175(19) 0.18(3) 0.21(3) 0.04(3) 0.04(2) 0.03(2) S7A 0.209(15) 0.192(14) 0.247(18) 0.096(12) 0.108(13) 0.068(11) S8A 0.217(15) 0.235(16) 0.234(17) 0.081(14) 0.052(16) 0.010(15) N12A 0.23(3) 0.17(2) 0.24(2) 0.095(18) 0.073(17) 0.09(2) C103 0.26(3) 0.19(3) 0.17(3) 0.05(2) -0.01(2) 0.01(2) C104 0.168(19) 0.19(2) 0.31(3) 0.03(2) 0.08(2) 0.03(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; F F 0.0727 0.0534 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni -3.0029 0.5091 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0492 0.0322 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.3331 0.5567 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N7 Ni1 O2 87.5(9) N7 Ni1 O1 166.6(10) O2 Ni1 O1 81.3(9) N7 Ni1 N1 102.6(10) O2 Ni1 N1 168.8(10) O1 Ni1 N1 89.2(10) N7 Ni1 N8 81.7(11) O2 Ni1 N8 83.7(8) O1 Ni1 N8 104.3(9) N1 Ni1 N8 93.0(11) N7 Ni1 N2 95.0(10) O2 Ni1 N2 104.4(8) O1 Ni1 N2 80.7(9) N1 Ni1 N2 79.7(10) N8 Ni1 N2 171.2(8) N3 Ni2 N5 101.4(10) N3 Ni2 O9 91.8(8) N5 Ni2 O9 166.7(9) N3 Ni2 O8 172.5(9) N5 Ni2 O8 84.1(9) O9 Ni2 O8 83.0(7) N3 Ni2 N4 80.8(10) N5 Ni2 N4 95.8(11) O9 Ni2 N4 84.3(9) O8 Ni2 N4 103.9(9) N3 Ni2 N6 94.9(11) N5 Ni2 N6 81.9(12) O9 Ni2 N6 99.1(10) O8 Ni2 N6 80.7(9) N4 Ni2 N6 174.6(10) O15 S1 O16 119.8(13) O15 S1 N9 116.0(13) O16 S1 N9 108.6(14) O15 S1 C95 104.8(15) O16 S1 C95 102.0(16) N9 S1 C95 103.0(17) O18 S2 O17 117.6(14) O18 S2 N9 108.6(16) O17 S2 N9 116.4(13) O18 S2 C96 105.2(18) O17 S2 C96 102.8(18) N9 S2 C96 104.5(19) O20 S3 O19 118.3(17) O20 S3 N10 111.5(19) O19 S3 N10 116.9(17) O20 S3 C97 101(2) O19 S3 C97 105(2) N10 S3 C97 101(2) O22 S4 O21 118.5(17) O22 S4 N10 109.7(17) O21 S4 N10 112.9(15) O22 S4 C98 108(2) O21 S4 C98 102(2) N10 S4 C98 104(2) O24 S5 O23 114.2(17) O24 S5 N11 115(2) O23 S5 N11 109.8(19) O24 S5 C99 107(2) O23 S5 C99 97(2) N11 S5 C99 113(2) O25 S6 O26 122.2(17) O25 S6 N11 104.2(18) O26 S6 N11 114.5(19) O25 S6 C100 109(2) O26 S6 C100 103(2) N11 S6 C100 102(2) C3 O1 Ni1 128(2) C1 O2 Ni1 133(2) C1 O3 C4 119(3) C17 O4 C21 115(4) C7 O5 C12 117(3) C9 O6 C13 118(3) C14 O7 C11 116(3) C24 O8 Ni2 131.7(18) C22 O9 Ni2 130(2) C22 O10 C25A 114(3) C22 O10 C25 104(4) C28 O11 C33 115(3) C34 O12 C30 117(3) C35 O13 C32 121(3) C38 O14 C42 121(3) C49 N1 C43 125(2) C49 N1 Ni1 108(2) C43 N1 Ni1 127(2) C50 N2 C58 111(3) C50 N2 Ni1 112(2) C58 N2 Ni1 132.3(18) C59 N3 C48 117(2) C59 N3 Ni2 115(2) C48 N3 Ni2 127.5(19) C60 N4 C68 116(3) C60 N4 Ni2 110(2) C68 N4 Ni2 131.9(19) C75 N5 C69 124(3) C75 N5 Ni2 112(2) C69 N5 Ni2 123(2) C84 N6 C76 117(3) C84 N6 Ni2 135(2) C76 N6 Ni2 107(2) C85 N7 C74 126(3) C85 N7 Ni1 109(2) C74 N7 Ni1 126(2) C86 N8 C94 115(3) C86 N8 Ni1 112(2) C94 N8 Ni1 134(2) S2 N9 S1 126.4(17) S3 N10 S4 128(2) S6 N11 S5 126(2) O2 C1 O3 120(4) O2 C1 C2 120(3) O3 C1 C2 119(3) C5 C2 C3 125(3) C5 C2 C1 114(3) C3 C2 C1 121(3) O1 C3 C2 119(3) O1 C3 C15 113(3) C2 C3 C15 127(4) O3 C4 H4A 109.5 O3 C4 H4B 109.5 H4A C4 H4B 109.5 O3 C4 H4C 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 C2 C5 C6 127(3) C2 C5 H5 116.7 C6 C5 H5 116.7 C11 C6 C5 124(3) C11 C6 C7 113(3) C5 C6 C7 123(2) O5 C7 C8 129(3) O5 C7 C6 110(3) C8 C7 C6 121(3) C9 C8 C7 120(4) C9 C8 H8 119.8 C7 C8 H8 119.8 O6 C9 C8 124(4) O6 C9 C10 116(3) C8 C9 C10 120(3) C11 C10 C9 118(3) C11 C10 H10 121.1 C9 C10 H10 121.1 C10 C11 C6 128(4) C10 C11 O7 121(3) C6 C11 O7 111(3) O5 C12 H12A 109.5 O5 C12 H12B 109.5 H12A C12 H12B 109.5 O5 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 O6 C13 H13A 109.5 O6 C13 H13B 109.5 H13A C13 H13B 109.5 O6 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 O7 C14 H14A 109.5 O7 C14 H14B 109.5 H14A C14 H14B 109.5 O7 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C16 C15 C20 120(4) C16 C15 C3 122(4) C20 C15 C3 118(4) C17 C16 C15 117(4) C17 C16 H16 121.4 C15 C16 H16 121.4 C18 C17 C16 130(5) C18 C17 O4 123(5) C16 C17 O4 107(5) C17 C18 C19 114(5) C17 C18 H18 123.0 C19 C18 H18 123.0 C18 C19 C20 125(5) C18 C19 H19 117.6 C20 C19 H19 117.6 C19 C20 C15 114(4) C19 C20 H20 123.2 C15 C20 H20 123.2 O4 C21 H21A 109.5 O4 C21 H21B 109.5 H21A C21 H21B 109.5 O4 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 O9 C22 O10 124(3) O9 C22 C23 117(3) O10 C22 C23 119(3) C26 C23 C24 124(3) C26 C23 C22 110(3) C24 C23 C22 126(3) O8 C24 C23 119(3) O8 C24 C36 121(3) C23 C24 C36 118(3) O10 C25 H25A 109.5 O10 C25 H25B 109.5 H25A C25 H25B 109.5 O10 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 O10 C25A H25D 109.5 O10 C25A H25E 109.5 H25D C25A H25E 109.5 O10 C25A H25F 109.5 H25D C25A H25F 109.5 H25E C25A H25F 109.5 C23 C26 C27 125(3) C23 C26 H26 117.4 C27 C26 H26 117.4 C28 C27 C32 117(3) C28 C27 C26 127(3) C32 C27 C26 115(3) O11 C28 C29 124(3) O11 C28 C27 114(3) C29 C28 C27 121(3) C30 C29 C28 118(3) C30 C29 H29 121.2 C28 C29 H29 121.2 C29 C30 C31 124(3) C29 C30 O12 119(3) C31 C30 O12 116(3) C32 C31 C30 119(3) C32 C31 H31 120.7 C30 C31 H31 120.7 C31 C32 O13 124(3) C31 C32 C27 119(3) O13 C32 C27 112(3) O11 C33 H33A 109.5 O11 C33 H33B 109.5 H33A C33 H33B 109.5 O11 C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 O12 C34 H34A 109.5 O12 C34 H34B 109.5 H34A C34 H34B 109.5 O12 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 O13 C35 H35A 109.5 O13 C35 H35B 109.5 H35A C35 H35B 109.5 O13 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 C41 C36 C37 124(3) C41 C36 C24 125(3) C37 C36 C24 111(3) C36 C37 C38 118(3) C36 C37 H37 121.2 C38 C37 H37 121.2 C37 C38 C39 121(4) C37 C38 O14 118(3) C39 C38 O14 121(4) C40 C39 C38 120(4) C40 C39 H39 119.9 C38 C39 H39 119.9 C39 C40 C41 122(4) C39 C40 H40 119.0 C41 C40 H40 119.0 C36 C41 C40 115(3) C36 C41 H41 122.5 C40 C41 H41 122.5 O14 C42 H42A 109.5 O14 C42 H42B 109.5 H42A C42 H42B 109.5 O14 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 N1 C43 C44 110(2) N1 C43 C48 111(2) C44 C43 C48 111(2) N1 C43 H43 108.5 C44 C43 H43 108.5 C48 C43 H43 108.5 C43 C44 C45 114(3) C43 C44 H44A 108.8 C45 C44 H44A 108.8 C43 C44 H44B 108.8 C45 C44 H44B 108.8 H44A C44 H44B 107.7 C46 C45 C44 109(3) C46 C45 H45A 109.9 C44 C45 H45A 109.9 C46 C45 H45B 109.9 C44 C45 H45B 109.9 H45A C45 H45B 108.3 C45 C46 C47 111(3) C45 C46 H46A 109.4 C47 C46 H46A 109.4 C45 C46 H46B 109.4 C47 C46 H46B 109.4 H46A C46 H46B 108.0 C46 C47 C48 110(3) C46 C47 H47A 109.6 C48 C47 H47A 109.6 C46 C47 H47B 109.6 C48 C47 H47B 109.6 H47A C47 H47B 108.1 N3 C48 C43 113(2) N3 C48 C47 107(2) C43 C48 C47 108(2) N3 C48 H48 109.5 C43 C48 H48 109.5 C47 C48 H48 109.5 N1 C49 C50 127(3) N1 C49 H49 116.6 C50 C49 H49 116.6 C51 C50 N2 128(3) C51 C50 C49 120(3) N2 C50 C49 112(3) C50 C51 C52 121(3) C50 C51 H51 119.3 C52 C51 H51 119.3 C51 C52 C53 117(3) C51 C52 H52 121.7 C53 C52 H52 121.7 C58 C53 C54 121(3) C58 C53 C52 117(3) C54 C53 C52 122(3) C55 C54 C53 122(4) C55 C54 H54 118.8 C53 C54 H54 118.8 C54 C55 C56 121(3) C54 C55 H55 119.6 C56 C55 H55 119.6 C55 C56 C57 119(3) C55 C56 H56 120.4 C57 C56 H56 120.4 C56 C57 C58 118(3) C56 C57 H57 120.8 C58 C57 H57 120.8 C53 C58 N2 126(3) C53 C58 C57 118(3) N2 C58 C57 115(3) N3 C59 C60 118(3) N3 C59 H59 120.8 C60 C59 H59 120.8 C61 C60 N4 123(3) C61 C60 C59 122(3) N4 C60 C59 116(3) C60 C61 C62 122(3) C60 C61 H61 119.1 C62 C61 H61 119.1 C63 C62 C61 116(4) C63 C62 H62 122.2 C61 C62 H62 122.2 C68 C63 C62 127(4) C68 C63 C64 112(3) C62 C63 C64 121(4) C65 C64 C63 117(3) C65 C64 H64 121.4 C63 C64 H64 121.4 C64 C65 C66 123(4) C64 C65 H65 118.5 C66 C65 H65 118.5 C67 C66 C65 122(4) C67 C66 H66 119.1 C65 C66 H66 119.1 C66 C67 C68 116(3) C66 C67 H67 122.2 C68 C67 H67 122.2 C63 C68 C67 130(4) C63 C68 N4 117(3) C67 C68 N4 113(3) C74 C69 C70 110(2) C74 C69 N5 108(2) C70 C69 N5 104(3) C74 C69 H69 111.5 C70 C69 H69 111.5 N5 C69 H69 111.5 C71 C70 C69 111(3) C71 C70 H70A 109.4 C69 C70 H70A 109.4 C71 C70 H70B 109.4 C69 C70 H70B 109.4 H70A C70 H70B 108.0 C72 C71 C70 112(3) C72 C71 H71A 109.3 C70 C71 H71A 109.3 C72 C71 H71B 109.3 C70 C71 H71B 109.3 H71A C71 H71B 108.0 C71 C72 C73 110(3) C71 C72 H72A 109.7 C73 C72 H72A 109.7 C71 C72 H72B 109.7 C73 C72 H72B 109.7 H72A C72 H72B 108.2 C72 C73 C74 114(3) C72 C73 H73A 108.7 C74 C73 H73A 108.7 C72 C73 H73B 108.7 C74 C73 H73B 108.7 H73A C73 H73B 107.6 N7 C74 C69 111(2) N7 C74 C73 109(2) C69 C74 C73 107(3) N7 C74 H74 109.9 C69 C74 H74 109.9 C73 C74 H74 109.9 N5 C75 C76 121(3) N5 C75 H75 119.7 C76 C75 H75 119.7 N6 C76 C77 124(4) N6 C76 C75 118(3) C77 C76 C75 118(4) C76 C77 C78 114(4) C76 C77 H77 122.9 C78 C77 H77 122.9 C79 C78 C77 125(4) C79 C78 H78 117.4 C77 C78 H78 117.4 C78 C79 C84 116(4) C78 C79 C80 126(4) C84 C79 C80 118(4) C81 C80 C79 115(4) C81 C80 H80 122.6 C79 C80 H80 122.6 C80 C81 C82 126(4) C80 C81 H81 117.1 C82 C81 H81 117.1 C83 C82 C81 120(4) C83 C82 H82 120.2 C81 C82 H82 120.2 C82 C83 C84 122(4) C82 C83 H83 119.1 C84 C83 H83 119.1 N6 C84 C79 124(3) N6 C84 C83 117(3) C79 C84 C83 119(4) N7 C85 C86 126(4) N7 C85 H85 117.1 C86 C85 H85 117.1 C87 C86 N8 129(3) C87 C86 C85 119(4) N8 C86 C85 112(3) C86 C87 C88 116(3) C86 C87 H87 121.9 C88 C87 H87 121.9 C87 C88 C89 116(3) C87 C88 H88 121.9 C89 C88 H88 121.9 C94 C89 C88 120(3) C94 C89 C90 123(4) C88 C89 C90 117(3) C91 C90 C89 119(3) C91 C90 H90 120.6 C89 C90 H90 120.6 C90 C91 C92 114(4) C90 C91 H91 122.8 C92 C91 H91 122.8 C93 C92 C91 128(4) C93 C92 H92 115.8 C91 C92 H92 115.8 C92 C93 C94 117(3) C92 C93 H93 121.6 C94 C93 H93 121.6 C89 C94 N8 124(4) C89 C94 C93 118(3) N8 C94 C93 118(3) F2 C95 F3 119(4) F2 C95 F1 113(3) F3 C95 F1 101(3) F2 C95 S1 111(3) F3 C95 S1 106(2) F1 C95 S1 105(3) F6 C96 F4 117(4) F6 C96 F5 106(3) F4 C96 F5 110(4) F6 C96 S2 109(3) F4 C96 S2 109(3) F5 C96 S2 105(3) F7 C97 F9 110(5) F7 C97 F8 106(4) F9 C97 F8 104(4) F7 C97 S3 115(4) F9 C97 S3 113(4) F8 C97 S3 109(4) F10 C98 F11 110(5) F10 C98 F12 109(4) F11 C98 F12 105(4) F10 C98 S4 117(4) F11 C98 S4 107(3) F12 C98 S4 108(4) F13 C99 F15 111(4) F13 C99 F14 107(4) F15 C99 F14 105(4) F13 C99 S5 116(4) F15 C99 S5 111(3) F14 C99 S5 106(3) F18 C100 F16 115(5) F18 C100 F17 105(4) F16 C100 F17 109(4) F18 C100 S6 108(3) F16 C100 S6 112(4) F17 C100 S6 107(3) O27 S7 O28 111.4 O27 S7 N12 120.5 O28 S7 N12 118.8 O27 S7 C102 95.9 O28 S7 C102 83.3 N12 S7 C102 118.8 O30 S8 O29 120.5 O30 S8 N12 119.2 O29 S8 N12 98.3 O30 S8 C101 89.2 O29 S8 C101 112.2 N12 S8 C101 118.9 S8 N12 S7 120.4 F21 C101 F19 120.81(5) F21 C101 F20 114.6 F19 C101 F20 103.9 F21 C101 S8 115.1 F19 C101 S8 91.4 F20 C101 S8 108.3 F22 C102 F23 107.5 F22 C102 F24 107.0 F23 C102 F24 106.0 F22 C102 S7 107.0 F23 C102 S7 126.8 F24 C102 S7 101.0 O27A S7A O28A 111.4 O27A S7A N12A 120.5 O28A S7A N12A 118.8 O27A S7A C104 95.9 O28A S7A C104 83.3 N12A S7A C104 118.8 O30A S8A O29A 120.5 O30A S8A N12A 119.2 O29A S8A N12A 98.3 O30A S8A C103 89.2 O29A S8A C103 112.2 N12A S8A C103 118.9 S8A N12A S7A 120.4 F21A C103 F19A 120.8 F21A C103 F20A 114.6 F19A C103 F20A 103.9 F21A C103 S8A 115.1 F19A C103 S8A 91.4 F20A C103 S8A 108.3 F22A C104 F23A 107.5 F22A C104 F24A 107.0 F23A C104 F24A 106.0 F22A C104 S7A 107.0 F23A C104 S7A 126.8 F24A C104 S7A 101.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 N7 2.05(2) Ni1 O2 2.090(16) Ni1 O1 2.09(2) Ni1 N1 2.10(2) Ni1 N8 2.11(2) Ni1 N2 2.15(2) Ni2 N3 2.04(2) Ni2 N5 2.07(2) Ni2 O9 2.099(16) Ni2 O8 2.102(17) Ni2 N4 2.16(3) Ni2 N6 2.18(3) S1 O15 1.39(2) S1 O16 1.41(2) S1 N9 1.66(3) S1 C95 1.85(4) S2 O18 1.38(3) S2 O17 1.41(2) S2 N9 1.51(3) S2 C96 1.89(4) S3 O20 1.42(3) S3 O19 1.47(3) S3 N10 1.52(3) S3 C97 1.71(5) S4 O22 1.42(3) S4 O21 1.46(2) S4 N10 1.59(3) S4 C98 1.83(5) S5 O24 1.47(3) S5 O23 1.48(3) S5 N11 1.57(4) S5 C99 1.81(5) S6 O25 1.40(3) S6 O26 1.44(3) S6 N11 1.56(4) S6 C100 1.85(5) F1 C95 1.42(4) F2 C95 1.19(4) F3 C95 1.33(4) F4 C96 1.26(4) F5 C96 1.32(4) F6 C96 1.25(4) F7 C97 1.27(5) F8 C97 1.38(5) F9 C97 1.35(5) F10 C98 1.25(5) F11 C98 1.32(5) F12 C98 1.33(5) F13 C99 1.29(5) F14 C99 1.35(5) F15 C99 1.33(5) F16 C100 1.27(5) F17 C100 1.37(5) F18 C100 1.26(5) O1 C3 1.29(4) O2 C1 1.24(3) O3 C1 1.25(4) O3 C4 1.47(4) O4 C17 1.48(5) O4 C21 1.70(6) O5 C7 1.27(3) O5 C12 1.53(4) O6 C9 1.29(4) O6 C13 1.44(4) O7 C14 1.32(4) O7 C11 1.43(4) O8 C24 1.22(3) O9 C22 1.28(4) O10 C22 1.24(3) O10 C25A 1.59(7) O10 C25 1.71(10) O11 C28 1.35(4) O11 C33 1.47(3) O12 C34 1.43(4) O12 C30 1.45(4) O13 C35 1.36(3) O13 C32 1.39(4) O14 C38 1.41(4) O14 C42 1.50(4) N1 C49 1.27(4) N1 C43 1.48(4) N2 C50 1.34(4) N2 C58 1.42(4) N3 C59 1.29(4) N3 C48 1.51(4) N4 C60 1.38(4) N4 C68 1.48(4) N5 C75 1.27(4) N5 C69 1.59(4) N6 C84 1.35(4) N6 C76 1.37(4) N7 C85 1.26(4) N7 C74 1.49(4) N8 C86 1.33(4) N8 C94 1.35(3) C1 C2 1.46(5) C2 C5 1.33(4) C2 C3 1.40(5) C3 C15 1.49(5) C4 H4A 0.9800 C4 H4B 0.9800 C4 H4C 0.9800 C5 C6 1.48(4) C5 H5 0.9500 C6 C11 1.38(4) C6 C7 1.56(4) C7 C8 1.41(4) C8 C9 1.40(4) C8 H8 0.9500 C9 C10 1.48(5) C10 C11 1.37(4) C10 H10 0.9500 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 C16 1.40(5) C15 C20 1.45(5) C16 C17 1.32(5) C16 H16 0.9500 C17 C18 1.31(6) C18 C19 1.38(6) C18 H18 0.9500 C19 C20 1.42(5) C19 H19 0.9500 C20 H20 0.9500 C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 C23 1.51(4) C23 C26 1.40(5) C23 C24 1.43(4) C24 C36 1.50(4) C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C25A H25D 0.9800 C25A H25E 0.9800 C25A H25F 0.9800 C26 C27 1.50(4) C26 H26 0.9500 C27 C28 1.41(4) C27 C32 1.46(4) C28 C29 1.39(4) C29 C30 1.36(4) C29 H29 0.9500 C30 C31 1.37(4) C31 C32 1.35(4) C31 H31 0.9500 C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 C41 1.36(4) C36 C37 1.37(4) C37 C38 1.38(4) C37 H37 0.9500 C38 C39 1.40(5) C39 C40 1.31(5) C39 H39 0.9500 C40 C41 1.45(5) C40 H40 0.9500 C41 H41 0.9500 C42 H42A 0.9800 C42 H42B 0.9800 C42 H42C 0.9800 C43 C44 1.51(4) C43 C48 1.55(4) C43 H43 1.0000 C44 C45 1.52(4) C44 H44A 0.9900 C44 H44B 0.9900 C45 C46 1.46(4) C45 H45A 0.9900 C45 H45B 0.9900 C46 C47 1.53(4) C46 H46A 0.9900 C46 H46B 0.9900 C47 C48 1.57(4) C47 H47A 0.9900 C47 H47B 0.9900 C48 H48 1.0000 C49 C50 1.44(4) C49 H49 0.9500 C50 C51 1.27(4) C51 C52 1.36(4) C51 H51 0.9500 C52 C53 1.43(4) C52 H52 0.9500 C53 C58 1.31(4) C53 C54 1.38(4) C54 C55 1.33(4) C54 H54 0.9500 C55 C56 1.35(4) C55 H55 0.9500 C56 C57 1.40(4) C56 H56 0.9500 C57 C58 1.48(4) C57 H57 0.9500 C59 C60 1.50(4) C59 H59 0.9500 C60 C61 1.32(4) C61 C62 1.39(5) C61 H61 0.9500 C62 C63 1.35(5) C62 H62 0.9500 C63 C68 1.31(4) C63 C64 1.48(5) C64 C65 1.35(5) C64 H64 0.9500 C65 C66 1.37(4) C65 H65 0.9500 C66 C67 1.27(4) C66 H66 0.9500 C67 C68 1.38(4) C67 H67 0.9500 C69 C74 1.50(4) C69 C70 1.53(4) C69 H69 1.0000 C70 C71 1.50(5) C70 H70A 0.9900 C70 H70B 0.9900 C71 C72 1.49(4) C71 H71A 0.9900 C71 H71B 0.9900 C72 C73 1.51(4) C72 H72A 0.9900 C72 H72B 0.9900 C73 C74 1.53(4) C73 H73A 0.9900 C73 H73B 0.9900 C74 H74 1.0000 C75 C76 1.49(5) C75 H75 0.9500 C76 C77 1.38(4) C77 C78 1.39(5) C77 H77 0.9500 C78 C79 1.33(5) C78 H78 0.9500 C79 C84 1.37(5) C79 C80 1.52(5) C80 C81 1.33(5) C80 H80 0.9500 C81 C82 1.38(5) C81 H81 0.9500 C82 C83 1.27(4) C82 H82 0.9500 C83 C84 1.45(4) C83 H83 0.9500 C85 C86 1.48(4) C85 H85 0.9500 C86 C87 1.32(4) C87 C88 1.39(4) C87 H87 0.9500 C88 C89 1.46(5) C88 H88 0.9500 C89 C94 1.30(4) C89 C90 1.48(4) C90 C91 1.35(4) C90 H90 0.9500 C91 C92 1.39(4) C91 H91 0.9500 C92 C93 1.33(4) C92 H92 0.9500 C93 C94 1.42(4) C93 H93 0.9500 F19 C101 1.3190 F20 C101 1.3923 F21 C101 1.1424 F22 C102 1.3170 F23 C102 1.3472 F24 C102 1.3562 O27 S7 1.4216 O28 S7 1.4321 O29 S8 1.3964 O30 S8 1.3260 S7 N12 1.5006 S7 C102 1.8107 S8 N12 1.4909 S8 C101 1.9644 F19A C103 1.3190 F20A C103 1.3923 F21A C103 1.1424 F22A C104 1.3170 F23A C104 1.3472 F24A C104 1.3562 O27A S7A 1.4216 O28A S7A 1.4321 O29A S8A 1.3964 O30A S8A 1.3260 S7A N12A 1.5006 S7A C104 1.8107 S8A N12A 1.4909 S8A C103 1.9644 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O18 S2 N9 S1 -153(2) O17 S2 N9 S1 -18(3) C96 S2 N9 S1 95(3) O15 S1 N9 S2 11(3) O16 S1 N9 S2 -127(2) C95 S1 N9 S2 125(2) O20 S3 N10 S4 -114(3) O19 S3 N10 S4 27(3) C97 S3 N10 S4 140(3) O22 S4 N10 S3 153(2) O21 S4 N10 S3 19(3) C98 S4 N10 S3 -91(3) O25 S6 N11 S5 131(3) O26 S6 N11 S5 -5(4) C100 S6 N11 S5 -116(3) O24 S5 N11 S6 -44(4) O23 S5 N11 S6 -175(2) C99 S5 N11 S6 79(3) Ni1 O2 C1 O3 142(3) Ni1 O2 C1 C2 -28(4) C4 O3 C1 O2 3(4) C4 O3 C1 C2 174(3) O2 C1 C2 C5 172(3) O3 C1 C2 C5 2(4) O2 C1 C2 C3 -3(5) O3 C1 C2 C3 -174(3) Ni1 O1 C3 C2 -45(4) Ni1 O1 C3 C15 125(3) C5 C2 C3 O1 -136(3) C1 C2 C3 O1 39(4) C5 C2 C3 C15 56(4) C1 C2 C3 C15 -129(3) C3 C2 C5 C6 0(5) C1 C2 C5 C6 -176(3) C2 C5 C6 C11 -146(3) C2 C5 C6 C7 36(4) C12 O5 C7 C8 15(4) C12 O5 C7 C6 -176(2) C11 C6 C7 O5 -172(3) C5 C6 C7 O5 6(3) C11 C6 C7 C8 -1(4) C5 C6 C7 C8 176(3) O5 C7 C8 C9 175(3) C6 C7 C8 C9 6(4) C13 O6 C9 C8 -6(5) C13 O6 C9 C10 -177(3) C7 C8 C9 O6 -179(3) C7 C8 C9 C10 -8(5) O6 C9 C10 C11 176(3) C8 C9 C10 C11 4(5) C9 C10 C11 C6 1(5) C9 C10 C11 O7 -178(3) C5 C6 C11 C10 -180(3) C7 C6 C11 C10 -2(5) C5 C6 C11 O7 -1(4) C7 C6 C11 O7 177(2) C14 O7 C11 C10 2(5) C14 O7 C11 C6 -177(3) O1 C3 C15 C16 25(4) C2 C3 C15 C16 -166(3) O1 C3 C15 C20 -157(3) C2 C3 C15 C20 12(4) C20 C15 C16 C17 3(3) C3 C15 C16 C17 -179(3) C15 C16 C17 C18 -1(4) C15 C16 C17 O4 -173(3) C21 O4 C17 C18 -8(5) C21 O4 C17 C16 166(4) C16 C17 C18 C19 2(6) O4 C17 C18 C19 173(3) C17 C18 C19 C20 -5(6) C18 C19 C20 C15 7(5) C16 C15 C20 C19 -5(4) C3 C15 C20 C19 177(3) Ni2 O9 C22 O10 151(3) Ni2 O9 C22 C23 -33(5) C25A O10 C22 O9 -24(7) C25 O10 C22 O9 31(7) C25A O10 C22 C23 160(4) C25 O10 C22 C23 -146(5) O9 C22 C23 C26 -180(3) O10 C22 C23 C26 -3(5) O9 C22 C23 C24 5(6) O10 C22 C23 C24 -178(4) Ni2 O8 C24 C23 -36(5) Ni2 O8 C24 C36 126(3) C26 C23 C24 O8 -145(3) C22 C23 C24 O8 29(5) C26 C23 C24 C36 52(5) C22 C23 C24 C36 -134(3) C24 C23 C26 C27 16(6) C22 C23 C26 C27 -159(3) C23 C26 C27 C28 27(6) C23 C26 C27 C32 -165(3) C33 O11 C28 C29 5(5) C33 O11 C28 C27 -179(3) C32 C27 C28 O11 -176(3) C26 C27 C28 O11 -8(5) C32 C27 C28 C29 1(5) C26 C27 C28 C29 168(3) O11 C28 C29 C30 179(3) C27 C28 C29 C30 3(5) C28 C29 C30 C31 4(5) C28 C29 C30 O12 179(3) C34 O12 C30 C29 2(5) C34 O12 C30 C31 178(3) C29 C30 C31 C32 -14(6) O12 C30 C31 C32 170(3) C30 C31 C32 O13 170(3) C30 C31 C32 C27 18(5) C35 O13 C32 C31 21(5) C35 O13 C32 C27 175(3) C28 C27 C32 C31 -12(5) C26 C27 C32 C31 180(3) C28 C27 C32 O13 -167(3) C26 C27 C32 O13 24(4) O8 C24 C36 C41 -150(3) C23 C24 C36 C41 13(4) O8 C24 C36 C37 31(4) C23 C24 C36 C37 -167(3) C41 C36 C37 C38 2(3) C24 C36 C37 C38 -179(2) C36 C37 C38 C39 0(3) C36 C37 C38 O14 -176(3) C42 O14 C38 C37 178(2) C42 O14 C38 C39 2(4) C37 C38 C39 C40 3(5) O14 C38 C39 C40 179(3) C38 C39 C40 C41 -7(5) C37 C36 C41 C40 -6(4) C24 C36 C41 C40 175(3) C39 C40 C41 C36 8(5) C49 N1 C43 C44 -61(4) Ni1 N1 C43 C44 112(3) C49 N1 C43 C48 61(4) Ni1 N1 C43 C48 -125(2) N1 C43 C44 C45 178(2) C48 C43 C44 C45 55(3) C43 C44 C45 C46 -58(4) C44 C45 C46 C47 60(4) C45 C46 C47 C48 -62(3) C59 N3 C48 C43 63(3) Ni2 N3 C48 C43 -121(2) C59 N3 C48 C47 -56(3) Ni2 N3 C48 C47 120(2) N1 C43 C48 N3 67(3) C44 C43 C48 N3 -171(2) N1 C43 C48 C47 -175(2) C44 C43 C48 C47 -53(3) C46 C47 C48 N3 178(2) C46 C47 C48 C43 56(3) C43 N1 C49 C50 177(3) Ni1 N1 C49 C50 2(4) C58 N2 C50 C51 5(4) Ni1 N2 C50 C51 163(2) C58 N2 C50 C49 -170(2) Ni1 N2 C50 C49 -12(3) N1 C49 C50 C51 -168(3) N1 C49 C50 N2 7(4) N2 C50 C51 C52 1(5) C49 C50 C51 C52 176(3) C50 C51 C52 C53 -2(4) C51 C52 C53 C58 -3(4) C51 C52 C53 C54 177(3) C58 C53 C54 C55 0(5) C52 C53 C54 C55 180(3) C53 C54 C55 C56 3(5) C54 C55 C56 C57 0(5) C55 C56 C57 C58 -7(4) C54 C53 C58 N2 -171(3) C52 C53 C58 N2 10(4) C54 C53 C58 C57 -7(4) C52 C53 C58 C57 174(3) C50 N2 C58 C53 -11(4) Ni1 N2 C58 C53 -163(2) C50 N2 C58 C57 -175(2) Ni1 N2 C58 C57 33(4) C56 C57 C58 C53 10(4) C56 C57 C58 N2 175(2) C48 N3 C59 C60 173(2) Ni2 N3 C59 C60 -3(3) C68 N4 C60 C61 7(4) Ni2 N4 C60 C61 171(2) C68 N4 C60 C59 -171(2) Ni2 N4 C60 C59 -7(3) N3 C59 C60 C61 -171(3) N3 C59 C60 N4 7(4) N4 C60 C61 C62 -6(4) C59 C60 C61 C62 173(3) C60 C61 C62 C63 4(5) C61 C62 C63 C68 -4(6) C61 C62 C63 C64 -175(3) C68 C63 C64 C65 10(5) C62 C63 C64 C65 -178(3) C63 C64 C65 C66 -6(5) C64 C65 C66 C67 1(6) C65 C66 C67 C68 0(5) C62 C63 C68 C67 178(3) C64 C63 C68 C67 -10(5) C62 C63 C68 N4 6(5) C64 C63 C68 N4 178(2) C66 C67 C68 C63 5(5) C66 C67 C68 N4 178(3) C60 N4 C68 C63 -7(4) Ni2 N4 C68 C63 -167(2) C60 N4 C68 C67 179(2) Ni2 N4 C68 C67 20(4) C75 N5 C69 C74 61(4) Ni2 N5 C69 C74 -130(2) C75 N5 C69 C70 -57(4) Ni2 N5 C69 C70 113(3) C74 C69 C70 C71 60(4) N5 C69 C70 C71 175(3) C69 C70 C71 C72 -57(4) C70 C71 C72 C73 53(4) C71 C72 C73 C74 -55(4) C85 N7 C74 C69 59(4) Ni1 N7 C74 C69 -125(3) C85 N7 C74 C73 -58(4) Ni1 N7 C74 C73 117(3) C70 C69 C74 N7 -176(3) N5 C69 C74 N7 71(3) C70 C69 C74 C73 -58(4) N5 C69 C74 C73 -171(3) C72 C73 C74 N7 178(3) C72 C73 C74 C69 57(4) C69 N5 C75 C76 175(2) Ni2 N5 C75 C76 5(4) C84 N6 C76 C77 -4(5) Ni2 N6 C76 C77 163(3) C84 N6 C76 C75 -176(3) Ni2 N6 C76 C75 -9(3) N5 C75 C76 N6 4(4) N5 C75 C76 C77 -169(3) N6 C76 C77 C78 5(5) C75 C76 C77 C78 178(3) C76 C77 C78 C79 -3(5) C77 C78 C79 C84 0(6) C77 C78 C79 C80 -180(3) C78 C79 C80 C81 178(4) C84 C79 C80 C81 -1(5) C79 C80 C81 C82 -1(6) C80 C81 C82 C83 7(7) C81 C82 C83 C84 -11(6) C76 N6 C84 C79 0(5) Ni2 N6 C84 C79 -162(3) C76 N6 C84 C83 -176(3) Ni2 N6 C84 C83 21(4) C78 C79 C84 N6 2(5) C80 C79 C84 N6 -178(3) C78 C79 C84 C83 178(3) C80 C79 C84 C83 -2(5) C82 C83 C84 N6 -175(3) C82 C83 C84 C79 9(5) C74 N7 C85 C86 177(2) Ni1 N7 C85 C86 1(4) C94 N8 C86 C87 -3(4) Ni1 N8 C86 C87 180(3) C94 N8 C86 C85 178(2) Ni1 N8 C86 C85 0(3) N7 C85 C86 C87 180(3) N7 C85 C86 N8 -1(4) N8 C86 C87 C88 2(5) C85 C86 C87 C88 -178(3) C86 C87 C88 C89 0(4) C87 C88 C89 C94 -2(4) C87 C88 C89 C90 177(3) C94 C89 C90 C91 -3(5) C88 C89 C90 C91 178(3) C89 C90 C91 C92 0(5) C90 C91 C92 C93 1(5) C91 C92 C93 C94 0(5) C88 C89 C94 N8 2(5) C90 C89 C94 N8 -178(3) C88 C89 C94 C93 -177(3) C90 C89 C94 C93 4(5) C86 N8 C94 C89 0(4) Ni1 N8 C94 C89 177(2) C86 N8 C94 C93 179(3) Ni1 N8 C94 C93 -4(4) C92 C93 C94 C89 -2(4) C92 C93 C94 N8 179(3) O15 S1 C95 F2 -51(3) O16 S1 C95 F2 75(3) N9 S1 C95 F2 -172(3) O15 S1 C95 F3 179(2) O16 S1 C95 F3 -55(3) N9 S1 C95 F3 57(3) O15 S1 C95 F1 72(2) O16 S1 C95 F1 -162(2) N9 S1 C95 F1 -50(2) O18 S2 C96 F6 62(3) O17 S2 C96 F6 -62(3) N9 S2 C96 F6 176(3) O18 S2 C96 F4 -169(3) O17 S2 C96 F4 67(3) N9 S2 C96 F4 -55(4) O18 S2 C96 F5 -52(3) O17 S2 C96 F5 -176(2) N9 S2 C96 F5 62(3) O20 S3 C97 F7 -60(4) O19 S3 C97 F7 177(4) N10 S3 C97 F7 55(5) O20 S3 C97 F9 67(4) O19 S3 C97 F9 -57(4) N10 S3 C97 F9 -179(4) O20 S3 C97 F8 -179(4) O19 S3 C97 F8 58(4) N10 S3 C97 F8 -64(4) O22 S4 C98 F10 171(4) O21 S4 C98 F10 -63(5) N10 S4 C98 F10 54(5) O22 S4 C98 F11 -65(4) O21 S4 C98 F11 61(4) N10 S4 C98 F11 178(3) O22 S4 C98 F12 48(4) O21 S4 C98 F12 174(3) N10 S4 C98 F12 -69(4) O24 S5 C99 F13 -58(4) O23 S5 C99 F13 60(4) N11 S5 C99 F13 175(4) O24 S5 C99 F15 174(3) O23 S5 C99 F15 -68(4) N11 S5 C99 F15 46(4) O24 S5 C99 F14 60(4) O23 S5 C99 F14 178(3) N11 S5 C99 F14 -67(4) O25 S6 C100 F18 -61(4) O26 S6 C100 F18 71(4) N11 S6 C100 F18 -170(3) O25 S6 C100 F16 172(3) O26 S6 C100 F16 -57(4) N11 S6 C100 F16 62(4) O25 S6 C100 F17 52(3) O26 S6 C100 F17 -177(3) N11 S6 C100 F17 -57(3) O30 S8 N12 S7 18.8 O29 S8 N12 S7 150.8 C101 S8 N12 S7 -88.1 O27 S7 N12 S8 -100.7 O28 S7 N12 S8 43.2 C102 S7 N12 S8 141.9 O27 S7 C102 F22 -118.3 O28 S7 C102 F22 130.8 N12 S7 C102 F22 11.5 O27 S7 C102 F23 10.2 O28 S7 C102 F23 -100.7 N12 S7 C102 F23 140.0 O27 S7 C102 F24 130.0 O28 S7 C102 F24 19.0 N12 S7 C102 F24 -100.3 O30A S8A N12A S7A 18.8 O29A S8A N12A S7A 150.8 C103 S8A N12A S7A -88.1 O27A S7A N12A S8A -100.7 O28A S7A N12A S8A 43.2 C104 S7A N12A S8A 141.9 O27A S7A C104 F22A -118.3 O28A S7A C104 F22A 130.8 N12A S7A C104 F22A 11.5 O27A S7A C104 F23A 10.2 O28A S7A C104 F23A -100.7 N12A S7A C104 F23A 140.0 O27A S7A C104 F24A 130.0 O28A S7A C104 F24A 19.0 N12A S7A C104 F24A -100.3