#------------------------------------------------------------------------------ #$Date: 2022-11-07 07:07:31 +0200 (Mon, 07 Nov 2022) $ #$Revision: 278962 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/13/07/7130757.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_7130757 loop_ _publ_author_name 'Mathoni\`ere, Corine' 'Mitcov, Dmitri' 'Koumousi, Evangelia' 'Amorin-Rosario, Daniel' 'Dechambenoit, Pierre' 'Fatima Jafri, Sadaf' 'Sainctavit, Philippe' 'Cartier Dit Moulin, Christophe' 'Toupet, Loic' 'Trzop, Elzbieta' 'Collet, Eric' 'Arrio, Marie-Anne' 'Rogalev, Andrei' 'Wilhelm, Fabrice' 'Cl\'erac, Rodolphe' _publ_section_title ; Metal-to-metal electron transfer in a cyanido-bridged {Fe2Co2} square complex followed by X-ray diffraction and absorption techniques. ; _journal_issue 86 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 12098 _journal_page_last 12101 _journal_paper_doi 10.1039/d2cc04246k _journal_volume 58 _journal_year 2022 _chemical_formula_moiety 'C42 H46 B Co Fe N13, C F3 O3 S, C3 H7 N O, 0.5(H2 O)' _chemical_formula_sum 'C46 H54 B Co F3 Fe N14 O4.5 S' _chemical_formula_weight 1089.68 _chemical_melting_point ? _chemical_properties_physical Light-sensitive,Photo-sensitive _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2022-06-29 deposited with the CCDC. 2022-09-22 downloaded from the CCDC. ; _cell_angle_alpha 69.246(7) _cell_angle_beta 89.144(7) _cell_angle_gamma 72.923(7) _cell_formula_units_Z 2 _cell_length_a 13.3992(11) _cell_length_b 13.9160(9) _cell_length_c 14.8696(12) _cell_measurement_reflns_used 1937 _cell_measurement_temperature 80.0 _cell_measurement_theta_max 22.0810 _cell_measurement_theta_min 3.0760 _cell_volume 2466.1(4) _computing_cell_refinement 'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.33.5 (Oxford Diffraction Ltd., 2008)' _computing_data_reduction 'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 80.0 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1852 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -104.00 -32.00 1.00 60.00 -- -21.92 179.00-180.00 72 2 \w -48.00 51.00 1.00 60.00 -- -21.92 38.00-150.00 99 3 \w -24.00 16.00 1.00 60.00 -- -21.92 -88.00 164.00 40 4 \w -87.00 9.00 1.00 60.00 -- -21.92 -38.00 30.00 96 5 \w -83.00 11.00 1.00 60.00 -- -21.92 -77.00 -30.00 94 6 \w 78.00 103.00 1.00 60.00 -- 23.80 179.00-180.00 25 7 \w -104.00 -32.00 1.00 60.00 -- -21.92 179.00-180.00 72 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0167132000 _diffrn_orient_matrix_UB_12 0.0537339000 _diffrn_orient_matrix_UB_13 -0.0341503000 _diffrn_orient_matrix_UB_21 0.0350039000 _diffrn_orient_matrix_UB_22 -0.0159723000 _diffrn_orient_matrix_UB_23 -0.0320152000 _diffrn_orient_matrix_UB_31 -0.0399109000 _diffrn_orient_matrix_UB_32 -0.0118673000 _diffrn_orient_matrix_UB_33 -0.0209057000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1235 _diffrn_reflns_av_unetI/netI 0.2378 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 19356 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.798 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_meas ? _exptl_crystal_density_method none _exptl_crystal_description prism _exptl_crystal_F_000 1130 _exptl_crystal_preparation 'Magnetic properties' _exptl_crystal_size_max 0.225 _exptl_crystal_size_mid 0.069 _exptl_crystal_size_min 0.027 _refine_diff_density_max 0.555 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 661 _refine_ls_number_reflns 8673 _refine_ls_number_restraints 54 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.1961 _refine_ls_R_factor_gt 0.0843 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1262 _refine_ls_wR_factor_ref 0.1785 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3953 _reflns_number_total 8673 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL mebipy80Klight CELL 0.71073 13.399155 13.916036 14.869647 69.2464 89.1441 72.9229 ZERR 2 0.001098 0.000935 0.001171 0.0067 0.0065 0.0066 LATT 1 SFAC C H B Co F Fe N O S UNIT 92 108 2 2 6 2 28 9 2 EQIV $1 1-X,1-Y,1-Z ISOR 0.005 0.01 O3 C39 C40 C42 C36 C33 C34 C32 C17 L.S. 6 0 0 PLAN 20 TEMP -193.15 HTAB O5 N8_$1 BOND $H CONF list 4 fmap 2 53 acta OMIT -4 50 WGHT 0.026600 FVAR 0.41151 CO1 4 0.733378 0.382756 0.395502 11.00000 0.02363 0.01497 = 0.02978 -0.00315 0.00480 -0.00607 FE1 6 0.456466 0.245045 0.594105 11.00000 0.02251 0.01595 = 0.03017 -0.00503 0.00541 -0.00668 S1 9 0.022196 0.183376 0.152057 11.00000 0.04035 0.02743 = 0.04642 -0.00859 0.01410 -0.01473 F1 5 -0.071448 0.038861 0.175830 11.00000 0.06219 0.05987 = 0.08907 -0.02466 0.01248 -0.04171 F2 5 0.002799 0.076943 0.045132 11.00000 0.10035 0.04843 = 0.03597 -0.01520 -0.00132 -0.01309 F3 5 -0.142354 0.186399 0.057345 11.00000 0.05411 0.07593 = 0.08712 -0.02334 -0.02337 0.00415 O1 8 0.370229 0.321357 1.057539 11.00000 0.05691 0.04213 = 0.04954 -0.00788 -0.00301 -0.02230 O2 8 0.119794 0.098867 0.188931 11.00000 0.02479 0.04829 = 0.07065 -0.02180 0.00281 0.00007 O3 8 0.027768 0.273435 0.067673 11.00000 0.10180 0.04122 = 0.05844 -0.00772 0.04013 -0.03547 O4 8 -0.041751 0.210537 0.223028 11.00000 0.04825 0.03756 = 0.04601 -0.01116 0.02444 -0.01021 O5 8 0.651537 0.575883 0.787625 10.50000 0.15390 0.14979 = 0.06005 -0.02527 0.01764 -0.07809 AFIX 3 H5D 2 0.674787 0.608793 0.733765 10.50000 -1.50000 H5E 2 0.685547 0.584253 0.834145 10.50000 -1.50000 AFIX 0 N1 7 0.371207 0.161772 0.681181 11.00000 0.03059 0.01434 = 0.02107 -0.00477 0.00740 -0.00930 N2 7 0.425774 0.062905 0.748346 11.00000 0.02944 0.01296 = 0.03611 -0.00386 0.01308 -0.00644 N3 7 0.552472 0.214802 0.708278 11.00000 0.02428 0.00972 = 0.03670 -0.00243 0.00273 0.00024 N4 7 0.583224 0.110026 0.777722 11.00000 0.03179 0.01807 = 0.03081 -0.00453 -0.00113 -0.00637 N5 7 0.540058 0.110142 0.579103 11.00000 0.02612 0.01980 = 0.02481 -0.00702 0.00791 -0.00646 N6 7 0.580596 0.019041 0.661067 11.00000 0.03103 0.01642 = 0.03245 -0.00662 0.00233 -0.00810 N7 7 0.325209 0.455983 0.615755 11.00000 0.02133 0.01598 = 0.03037 -0.00558 0.00458 0.00184 N8 7 0.296231 0.335088 0.415356 11.00000 0.03009 0.02435 = 0.04696 -0.01930 0.00448 -0.00545 N9 7 0.598149 0.353851 0.457666 11.00000 0.02431 0.01519 = 0.03941 -0.00756 0.01272 -0.00746 N10 7 0.806520 0.332459 0.537026 11.00000 0.02801 0.01398 = 0.03718 -0.00887 0.01196 -0.00866 N11 7 0.803351 0.211088 0.434899 11.00000 0.01795 0.01820 = 0.03203 -0.00762 0.01010 -0.00609 N12 7 0.862835 0.411716 0.320129 11.00000 0.02834 0.01315 = 0.03468 -0.00268 0.00644 -0.00243 N13 7 0.683074 0.409882 0.253213 11.00000 0.03639 0.01057 = 0.03098 0.00351 -0.00296 -0.00086 N14 7 0.299866 0.287971 0.937903 11.00000 0.04094 0.02746 = 0.02367 0.00816 -0.00047 -0.00389 C1 1 0.181315 0.272586 0.629057 11.00000 0.03014 0.03525 = 0.04205 -0.01863 0.00801 -0.01719 AFIX 137 H1A 2 0.195357 0.337124 0.630976 11.00000 -1.50000 H1B 2 0.114303 0.268934 0.655021 11.00000 -1.50000 H1C 2 0.177857 0.276235 0.562092 11.00000 -1.50000 AFIX 0 C2 1 0.267927 0.173529 0.689046 11.00000 0.02573 0.01453 = 0.02873 -0.00450 0.01256 -0.00558 C3 1 0.258301 0.079838 0.758606 11.00000 0.03112 0.02056 = 0.04095 -0.01080 0.01384 -0.01575 AFIX 43 H3 2 0.194502 0.065693 0.777769 11.00000 -1.20000 AFIX 0 C4 1 0.356634 0.012047 0.794312 11.00000 0.04910 0.01302 = 0.03649 -0.01295 0.00959 -0.01212 C5 1 0.393387 -0.100795 0.870976 11.00000 0.06173 0.01896 = 0.03383 -0.00106 0.02292 -0.01633 AFIX 137 H5A 2 0.442190 -0.149626 0.844764 11.00000 -1.50000 H5B 2 0.332770 -0.126430 0.890368 11.00000 -1.50000 H5C 2 0.428942 -0.099216 0.927316 11.00000 -1.50000 AFIX 0 C6 1 0.581300 0.390105 0.692760 11.00000 0.03285 0.01508 = 0.03713 -0.00833 0.00651 -0.00877 AFIX 137 H6A 2 0.588249 0.405549 0.623752 11.00000 -1.50000 H6B 2 0.634084 0.410903 0.720032 11.00000 -1.50000 H6C 2 0.511027 0.431267 0.701123 11.00000 -1.50000 AFIX 0 C7 1 0.597469 0.271361 0.743958 11.00000 0.02451 0.01692 = 0.03322 -0.00392 0.00055 -0.00228 C8 1 0.657310 0.205328 0.831498 11.00000 0.03145 0.02865 = 0.03727 -0.02206 0.01230 -0.01137 AFIX 43 H8 2 0.697474 0.225238 0.869958 11.00000 -1.20000 AFIX 0 C9 1 0.645971 0.104385 0.850756 11.00000 0.02224 0.02882 = 0.03358 -0.01286 -0.00252 0.00105 C10 1 0.695196 -0.000368 0.933105 11.00000 0.05231 0.02884 = 0.01305 -0.00106 0.00385 0.00174 AFIX 137 H10A 2 0.640161 -0.029717 0.964544 11.00000 -1.50000 H10B 2 0.735348 0.012193 0.980058 11.00000 -1.50000 H10C 2 0.742210 -0.051961 0.908468 11.00000 -1.50000 AFIX 0 C11 1 0.552709 0.154511 0.398731 11.00000 0.01361 0.02725 = 0.04017 -0.00928 0.00267 -0.00703 AFIX 137 H11A 2 0.480387 0.202752 0.387174 11.00000 -1.50000 H11B 2 0.561596 0.111146 0.357977 11.00000 -1.50000 H11C 2 0.601197 0.197555 0.382891 11.00000 -1.50000 AFIX 0 C12 1 0.575702 0.080788 0.503578 11.00000 0.02371 0.02258 = 0.03191 -0.00554 0.00252 -0.01439 C13 1 0.637390 -0.026643 0.536866 11.00000 0.01709 0.01533 = 0.04166 -0.00902 0.00888 -0.00054 AFIX 43 H13 2 0.671373 -0.066809 0.499009 11.00000 -1.20000 AFIX 0 C14 1 0.639249 -0.063277 0.636566 11.00000 0.01898 0.02047 = 0.04499 -0.01342 0.00833 -0.00339 C15 1 0.694588 -0.171365 0.712061 11.00000 0.04402 0.01695 = 0.03561 -0.01523 0.00755 -0.00465 AFIX 137 H15A 2 0.751868 -0.165426 0.747889 11.00000 -1.50000 H15B 2 0.723227 -0.223630 0.680906 11.00000 -1.50000 H15C 2 0.644859 -0.195725 0.756757 11.00000 -1.50000 AFIX 0 C16 1 0.373609 0.376773 0.607785 11.00000 0.02161 0.02453 = 0.02216 -0.01212 0.00365 -0.00947 C17 1 0.359767 0.295911 0.480938 11.00000 0.02694 0.01566 = 0.03211 -0.01131 0.00443 -0.00414 C18 1 0.542592 0.318009 0.507801 11.00000 0.02553 0.01789 = 0.01840 -0.01047 -0.00041 -0.00032 C19 1 0.813214 0.395378 0.584571 11.00000 0.02588 0.01009 = 0.03906 -0.00133 0.00338 -0.00384 AFIX 43 H19 2 0.787267 0.471337 0.551073 11.00000 -1.20000 AFIX 0 C20 1 0.854837 0.358497 0.678364 11.00000 0.03726 0.02850 = 0.03503 -0.00588 -0.00096 -0.01454 AFIX 43 H20 2 0.860262 0.407504 0.707747 11.00000 -1.20000 AFIX 0 C21 1 0.889032 0.247800 0.729789 11.00000 0.02343 0.02958 = 0.02730 0.00447 -0.00483 -0.00662 C22 1 0.879178 0.179993 0.683389 11.00000 0.04254 0.01496 = 0.03279 0.00140 0.00254 -0.00963 AFIX 43 H22 2 0.898251 0.104177 0.717627 11.00000 -1.20000 AFIX 0 C23 1 0.841187 0.223913 0.586450 11.00000 0.01882 0.02088 = 0.02463 0.00150 0.00102 -0.00144 C24 1 0.935376 0.205014 0.831553 11.00000 0.06330 0.02912 = 0.03871 -0.01114 -0.00259 -0.01441 AFIX 137 H24A 2 0.928971 0.132744 0.864824 11.00000 -1.50000 H24B 2 0.898108 0.253163 0.864183 11.00000 -1.50000 H24C 2 1.009655 0.200880 0.832852 11.00000 -1.50000 AFIX 0 C25 1 0.836937 0.156153 0.529671 11.00000 0.01844 0.02470 = 0.02372 -0.00153 0.00323 -0.01124 C26 1 0.872387 0.042724 0.568362 11.00000 0.02574 0.01814 = 0.02947 -0.00381 0.00362 -0.00091 AFIX 43 H26 2 0.893568 0.005004 0.635508 11.00000 -1.20000 AFIX 0 C27 1 0.876024 -0.013623 0.506835 11.00000 0.01704 0.01950 = 0.04685 -0.01424 0.01048 -0.00682 C28 1 0.844220 0.044190 0.410456 11.00000 0.02922 0.01391 = 0.03197 -0.00656 0.00299 -0.00587 AFIX 43 H28 2 0.846782 0.007660 0.366859 11.00000 -1.20000 AFIX 0 C29 1 0.808589 0.155296 0.377145 11.00000 0.02111 0.02237 = 0.02889 -0.00820 0.01044 -0.00966 AFIX 43 H29 2 0.786787 0.193956 0.310201 11.00000 -1.20000 AFIX 0 C30 1 0.913140 -0.136309 0.549675 11.00000 0.03657 0.01524 = 0.05310 -0.00925 0.00113 -0.01028 AFIX 137 H30A 2 0.853819 -0.162493 0.573518 11.00000 -1.50000 H30B 2 0.967523 -0.161104 0.603292 11.00000 -1.50000 H30C 2 0.942022 -0.164471 0.499849 11.00000 -1.50000 AFIX 0 C31 1 0.953922 0.410092 0.359428 11.00000 0.03022 0.01718 = 0.05022 -0.01017 0.00873 -0.00960 AFIX 43 H31 2 0.962304 0.393906 0.427053 11.00000 -1.20000 AFIX 0 C32 1 1.034714 0.430731 0.306153 11.00000 0.03290 0.02592 = 0.04344 -0.00741 0.00982 -0.01402 AFIX 43 H32 2 1.097425 0.428654 0.336806 11.00000 -1.20000 AFIX 0 C33 1 1.024451 0.454808 0.206688 11.00000 0.04347 0.03345 = 0.05068 -0.01381 0.01896 -0.01790 C34 1 0.933390 0.455124 0.168165 11.00000 0.05065 0.02442 = 0.04198 -0.01119 0.01396 -0.01225 AFIX 43 H34 2 0.923478 0.472325 0.100479 11.00000 -1.20000 AFIX 0 C35 1 0.854018 0.431088 0.224510 11.00000 0.03316 0.01308 = 0.04615 -0.01047 0.01588 -0.00746 C36 1 1.111550 0.479524 0.145941 11.00000 0.07440 0.05088 = 0.07220 -0.03517 0.04691 -0.03892 AFIX 137 H36A 2 1.131037 0.431230 0.109667 11.00000 -1.50000 H36B 2 1.172632 0.468691 0.188039 11.00000 -1.50000 H36C 2 1.087507 0.554689 0.100693 11.00000 -1.50000 AFIX 0 C37 1 0.757849 0.419797 0.188414 11.00000 0.03901 0.01202 = 0.02730 -0.00490 0.00763 -0.00111 C38 1 0.743108 0.415994 0.098841 11.00000 0.06021 0.02292 = 0.02382 -0.00470 0.00717 0.00150 AFIX 43 H38 2 0.795165 0.425257 0.055300 11.00000 -1.20000 AFIX 0 C39 1 0.653469 0.398849 0.070519 11.00000 0.05170 0.03972 = 0.04150 -0.02134 -0.00712 0.00208 C40 1 0.580331 0.387750 0.134516 11.00000 0.03685 0.02765 = 0.03412 -0.01423 -0.00752 0.00340 AFIX 43 H40 2 0.518466 0.374575 0.118615 11.00000 -1.20000 AFIX 0 C41 1 0.596522 0.395780 0.223448 11.00000 0.02629 0.01844 = 0.04067 -0.01068 -0.00329 0.00646 AFIX 43 H41 2 0.542765 0.390949 0.265668 11.00000 -1.20000 AFIX 0 C42 1 0.641769 0.388376 -0.024076 11.00000 0.08045 0.06110 = 0.05259 -0.03894 -0.01056 0.01546 AFIX 137 H42A 2 0.696360 0.324252 -0.025403 11.00000 -1.50000 H42B 2 0.648684 0.452758 -0.075747 11.00000 -1.50000 H42C 2 0.572517 0.381180 -0.033727 11.00000 -1.50000 AFIX 0 C43 1 0.301406 0.301333 1.020886 11.00000 0.04983 0.01929 = 0.03951 -0.00280 0.00918 -0.01226 AFIX 43 H43 2 0.242660 0.294739 1.056397 11.00000 -1.20000 AFIX 0 C44 1 0.387879 0.293186 0.881846 11.00000 0.04899 0.04349 = 0.05532 -0.00723 0.02636 -0.00321 AFIX 137 H44A 2 0.441209 0.306561 0.916071 11.00000 -1.50000 H44B 2 0.364535 0.351980 0.818830 11.00000 -1.50000 H44C 2 0.417859 0.224568 0.872442 11.00000 -1.50000 AFIX 0 C45 1 0.214995 0.265610 0.900012 11.00000 0.05729 0.02563 = 0.03572 -0.00678 -0.00385 -0.01029 AFIX 137 H45A 2 0.163016 0.257994 0.946979 11.00000 -1.50000 H45B 2 0.242033 0.198394 0.887678 11.00000 -1.50000 H45C 2 0.181968 0.325171 0.839499 11.00000 -1.50000 AFIX 0 C46 1 -0.051161 0.123273 0.106857 11.00000 0.04443 0.02931 = 0.02628 0.01815 -0.00118 -0.00100 B1 3 0.546170 0.024783 0.757603 11.00000 0.03314 0.01136 = 0.02435 0.00561 0.00366 0.00130 AFIX 13 H1 2 0.574647 -0.047300 0.810844 11.00000 -1.20000 AFIX 0 HKLF 4 REM mebipy80Klight REM R1 = 0.0843 for 3953 Fo > 4sig(Fo) and 0.1961 for all 8673 data REM 661 parameters refined using 54 restraints END WGHT 0.0266 0.0000 REM Highest difference peak 0.555, deepest hole -0.497, 1-sigma level 0.107 Q1 1 0.9210 0.0123 0.3790 11.00000 0.05 0.56 Q2 1 0.6389 0.3972 0.3756 11.00000 0.05 0.54 Q3 1 0.4590 0.2981 0.6430 11.00000 0.05 0.54 Q4 1 0.1751 0.0965 0.7961 11.00000 0.05 0.50 Q5 1 -0.0606 0.1841 0.1432 11.00000 0.05 0.49 Q6 1 0.8978 0.4747 0.1410 11.00000 0.05 0.48 Q7 1 0.4821 0.2820 0.6541 11.00000 0.05 0.48 Q8 1 0.9934 0.4752 0.1600 11.00000 0.05 0.47 Q9 1 0.5509 0.4388 0.3658 11.00000 0.05 0.46 Q10 1 0.3786 0.2437 0.5617 11.00000 0.05 0.45 Q11 1 0.6523 0.4329 0.4191 11.00000 0.05 0.45 Q12 1 0.5368 0.1965 0.5710 11.00000 0.05 0.45 Q13 1 0.3880 0.3453 0.4113 11.00000 0.05 0.44 Q14 1 -0.0029 0.1578 0.0821 11.00000 0.05 0.44 Q15 1 0.1068 0.2816 0.5987 11.00000 0.05 0.44 Q16 1 0.7825 0.1854 0.8631 11.00000 0.05 0.44 Q17 1 0.9534 0.2524 0.8811 11.00000 0.05 0.42 Q18 1 -0.1033 0.0795 0.0587 11.00000 0.05 0.42 Q19 1 0.6023 0.3601 -0.0388 11.00000 0.05 0.42 Q20 1 -0.0818 0.1606 0.1859 11.00000 0.05 0.42 REM The information below was added by Olex2. REM REM R1 = 0.0843 for 3953 Fo > 4sig(Fo) and 0.1961 for all 24526 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.56, deepest hole -0.50 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1961 REM R1_gt = 0.0843 REM wR_ref = 0.1785 REM GOOF = 1.019 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 24526 REM Reflections_gt = 3953 REM Parameters = n/a REM Hole = -0.50 REM Peak = 0.56 REM Flack = n/a ; _cod_data_source_file d2cc04246k2.cif _cod_data_source_block mebipy80Klight _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_melting_point' value 'not measured' was changed to '?' -- the value is undefined or not given. data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 7130756--7130758.cif. ; _cod_original_formula_sum 'C46 H54 B Co F3 Fe N14 O4.50 S' _cod_database_code 7130757 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula C46H53BCoF3FeN14O4.4S _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.87 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All B(H) groups, All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O3) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 3. Others Fixed Sof: O5(0.5) H5D(0.5) H5E(0.5) 4.a Riding coordinates: O5(H5D,H5E) 4.b Ternary CH refined with riding coordinates: B1(H1) 4.c Aromatic/amide H refined with riding coordinates: C3(H3), C8(H8), C13(H13), C19(H19), C20(H20), C22(H22), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C38(H38), C40(H40), C41(H41), C43(H43) 4.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C30(H30A,H30B, H30C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A, H45B,H45C) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.071 _oxdiff_exptl_absorpt_empirical_full_min 0.881 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -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 Co1 Co 0.73338(7) 0.38276(8) 0.39550(8) 0.0242(3) Uani 1 1 d . . . . . Fe1 Fe 0.45647(8) 0.24504(9) 0.59410(9) 0.0237(3) Uani 1 1 d . . . . . S1 S 0.02220(17) 0.18338(18) 0.15206(19) 0.0386(7) Uani 1 1 d . . . . . F1 F -0.0714(4) 0.0389(4) 0.1758(4) 0.0659(19) Uani 1 1 d . . . . . F2 F 0.0028(5) 0.0769(4) 0.0451(4) 0.0638(17) Uani 1 1 d . . . . . F3 F -0.1424(4) 0.1864(5) 0.0573(5) 0.080(2) Uani 1 1 d . . . . . O1 O 0.3702(5) 0.3214(5) 1.0575(5) 0.050(2) Uani 1 1 d . . . . . O2 O 0.1198(4) 0.0989(4) 0.1889(5) 0.051(2) Uani 1 1 d . . . . . O3 O 0.0278(5) 0.2734(5) 0.0677(5) 0.067(2) Uani 1 1 d . U . . . O4 O -0.0418(4) 0.2105(4) 0.2230(5) 0.0460(18) Uani 1 1 d . . . . . O5 O 0.6515(13) 0.5759(14) 0.7876(12) 0.118(7) Uani 0.5 1 d . . P . . H5D H 0.674787 0.608793 0.733765 0.177 Uiso 0.5 1 d R . P . . H5E H 0.685547 0.584253 0.834145 0.177 Uiso 0.5 1 d R . P . . N1 N 0.3712(4) 0.1618(5) 0.6812(5) 0.0220(16) Uani 1 1 d . . . . . N2 N 0.4258(4) 0.0629(5) 0.7483(5) 0.0278(18) Uani 1 1 d . . . . . N3 N 0.5525(4) 0.2148(5) 0.7083(5) 0.0266(18) Uani 1 1 d . . . . . N4 N 0.5832(5) 0.1100(5) 0.7777(5) 0.0284(18) Uani 1 1 d . . . . . N5 N 0.5401(4) 0.1101(5) 0.5791(5) 0.0241(17) Uani 1 1 d . . . . . N6 N 0.5806(5) 0.0190(5) 0.6611(5) 0.0271(18) Uani 1 1 d . . . . . N7 N 0.3252(4) 0.4560(5) 0.6158(5) 0.0252(17) Uani 1 1 d . . . . . N8 N 0.2962(5) 0.3351(5) 0.4154(5) 0.0327(19) Uani 1 1 d . . . . . N9 N 0.5981(4) 0.3539(5) 0.4577(5) 0.0268(18) Uani 1 1 d . . . . . N10 N 0.8065(4) 0.3325(5) 0.5370(5) 0.0261(18) Uani 1 1 d . . . . . N11 N 0.8034(4) 0.2111(5) 0.4349(5) 0.0231(17) Uani 1 1 d . . . . . N12 N 0.8628(5) 0.4117(5) 0.3201(5) 0.0281(18) Uani 1 1 d . . . . . N13 N 0.6831(5) 0.4099(5) 0.2532(5) 0.0306(19) Uani 1 1 d . . . . . N14 N 0.2999(5) 0.2880(5) 0.9379(6) 0.037(2) Uani 1 1 d . . . . . C1 C 0.1813(5) 0.2726(6) 0.6291(6) 0.033(2) Uani 1 1 d . . . . . H1A H 0.195357 0.337124 0.630976 0.049 Uiso 1 1 calc GR . . . . H1B H 0.114303 0.268934 0.655021 0.049 Uiso 1 1 calc GR . . . . H1C H 0.177857 0.276235 0.562092 0.049 Uiso 1 1 calc GR . . . . C2 C 0.2679(5) 0.1735(6) 0.6890(6) 0.024(2) Uani 1 1 d . . . . . C3 C 0.2583(6) 0.0798(6) 0.7586(6) 0.029(2) Uani 1 1 d . . . . . H3 H 0.194502 0.065693 0.777769 0.035 Uiso 1 1 calc R . . . . C4 C 0.3566(6) 0.0120(6) 0.7943(6) 0.031(2) Uani 1 1 d . . . . . C5 C 0.3934(6) -0.1008(6) 0.8710(6) 0.040(3) Uani 1 1 d . . . . . H5A H 0.442190 -0.149626 0.844764 0.060 Uiso 1 1 calc GR . . . . H5B H 0.332770 -0.126430 0.890368 0.060 Uiso 1 1 calc GR . . . . H5C H 0.428942 -0.099216 0.927316 0.060 Uiso 1 1 calc GR . . . . C6 C 0.5813(6) 0.3901(5) 0.6928(6) 0.028(2) Uani 1 1 d . . . . . H6A H 0.588249 0.405549 0.623752 0.043 Uiso 1 1 calc GR . . . . H6B H 0.634084 0.410903 0.720032 0.043 Uiso 1 1 calc GR . . . . H6C H 0.511027 0.431267 0.701123 0.043 Uiso 1 1 calc GR . . . . C7 C 0.5975(5) 0.2714(6) 0.7440(6) 0.027(2) Uani 1 1 d . . . . . C8 C 0.6573(6) 0.2053(6) 0.8315(6) 0.029(2) Uani 1 1 d . . . . . H8 H 0.697474 0.225238 0.869958 0.035 Uiso 1 1 calc R . . . . C9 C 0.6460(6) 0.1044(6) 0.8508(6) 0.030(2) Uani 1 1 d . . . . . C10 C 0.6952(6) -0.0004(6) 0.9331(6) 0.037(2) Uani 1 1 d . . . . . H10A H 0.640161 -0.029717 0.964544 0.055 Uiso 1 1 calc GR . . . . H10B H 0.735348 0.012193 0.980058 0.055 Uiso 1 1 calc GR . . . . H10C H 0.742210 -0.051961 0.908468 0.055 Uiso 1 1 calc GR . . . . C11 C 0.5527(5) 0.1545(6) 0.3987(6) 0.028(2) Uani 1 1 d . . . . . H11A H 0.480387 0.202752 0.387174 0.042 Uiso 1 1 calc GR . . . . H11B H 0.561596 0.111146 0.357977 0.042 Uiso 1 1 calc GR . . . . H11C H 0.601197 0.197555 0.382891 0.042 Uiso 1 1 calc GR . . . . C12 C 0.5757(5) 0.0808(6) 0.5036(6) 0.026(2) Uani 1 1 d . . . . . C13 C 0.6374(5) -0.0266(6) 0.5369(7) 0.026(2) Uani 1 1 d . . . . . H13 H 0.671373 -0.066809 0.499009 0.031 Uiso 1 1 calc R . . . . C14 C 0.6392(5) -0.0633(6) 0.6366(7) 0.028(2) Uani 1 1 d . . . . . C15 C 0.6946(6) -0.1714(6) 0.7121(6) 0.032(2) Uani 1 1 d . . . . . H15A H 0.751868 -0.165426 0.747889 0.048 Uiso 1 1 calc GR . . . . H15B H 0.723227 -0.223630 0.680906 0.048 Uiso 1 1 calc GR . . . . H15C H 0.644859 -0.195725 0.756757 0.048 Uiso 1 1 calc GR . . . . C16 C 0.3736(5) 0.3768(6) 0.6078(6) 0.0212(19) Uani 1 1 d . . . . . C17 C 0.3598(6) 0.2959(6) 0.4809(6) 0.025(2) Uani 1 1 d . U . . . C18 C 0.5426(5) 0.3180(6) 0.5078(6) 0.0210(19) Uani 1 1 d . . . . . C19 C 0.8132(5) 0.3954(6) 0.5846(7) 0.028(2) Uani 1 1 d . . . . . H19 H 0.787267 0.471337 0.551073 0.033 Uiso 1 1 calc R . . . . C20 C 0.8548(6) 0.3585(7) 0.6784(7) 0.034(2) Uani 1 1 d . . . . . H20 H 0.860262 0.407504 0.707747 0.041 Uiso 1 1 calc R . . . . C21 C 0.8890(6) 0.2478(7) 0.7298(6) 0.031(2) Uani 1 1 d . . . . . C22 C 0.8792(6) 0.1800(6) 0.6834(7) 0.033(2) Uani 1 1 d . . . . . H22 H 0.898251 0.104177 0.717627 0.039 Uiso 1 1 calc R . . . . C23 C 0.8412(5) 0.2239(6) 0.5865(6) 0.025(2) Uani 1 1 d . . . . . C24 C 0.9354(7) 0.2050(7) 0.8316(7) 0.044(3) Uani 1 1 d . . . . . H24A H 0.928971 0.132744 0.864824 0.066 Uiso 1 1 calc GR . . . . H24B H 0.898108 0.253163 0.864183 0.066 Uiso 1 1 calc GR . . . . H24C H 1.009655 0.200880 0.832852 0.066 Uiso 1 1 calc GR . . . . C25 C 0.8369(5) 0.1562(6) 0.5297(6) 0.023(2) Uani 1 1 d . . . . . C26 C 0.8724(5) 0.0427(6) 0.5684(6) 0.027(2) Uani 1 1 d . . . . . H26 H 0.893568 0.005004 0.635508 0.033 Uiso 1 1 calc R . . . . C27 C 0.8760(5) -0.0136(6) 0.5068(7) 0.027(2) Uani 1 1 d . . . . . C28 C 0.8442(5) 0.0442(6) 0.4105(6) 0.026(2) Uani 1 1 d . . . . . H28 H 0.846782 0.007660 0.366859 0.031 Uiso 1 1 calc R . . . . C29 C 0.8086(5) 0.1553(6) 0.3771(6) 0.024(2) Uani 1 1 d . . . . . H29 H 0.786787 0.193956 0.310201 0.029 Uiso 1 1 calc R . . . . C30 C 0.9131(6) -0.1363(6) 0.5497(7) 0.035(2) Uani 1 1 d . . . . . H30A H 0.853819 -0.162493 0.573518 0.053 Uiso 1 1 calc GR . . . . H30B H 0.967523 -0.161104 0.603292 0.053 Uiso 1 1 calc GR . . . . H30C H 0.942022 -0.164471 0.499849 0.053 Uiso 1 1 calc GR . . . . C31 C 0.9539(6) 0.4101(6) 0.3594(7) 0.033(2) Uani 1 1 d . . . . . H31 H 0.962304 0.393906 0.427053 0.039 Uiso 1 1 calc R . . . . C32 C 1.0347(6) 0.4307(6) 0.3062(7) 0.035(2) Uani 1 1 d . U . . . H32 H 1.097425 0.428654 0.336806 0.041 Uiso 1 1 calc R . . . . C33 C 1.0245(6) 0.4548(7) 0.2067(7) 0.042(3) Uani 1 1 d . U . . . C34 C 0.9334(6) 0.4551(6) 0.1682(7) 0.039(2) Uani 1 1 d . U . . . H34 H 0.923478 0.472325 0.100479 0.047 Uiso 1 1 calc R . . . . C35 C 0.8540(6) 0.4311(6) 0.2245(7) 0.031(2) Uani 1 1 d . . . . . C36 C 1.1116(7) 0.4795(7) 0.1459(8) 0.058(3) Uani 1 1 d . U . . . H36A H 1.131037 0.431230 0.109667 0.087 Uiso 1 1 calc GR . . . . H36B H 1.172632 0.468691 0.188039 0.087 Uiso 1 1 calc GR . . . . H36C H 1.087507 0.554689 0.100693 0.087 Uiso 1 1 calc GR . . . . C37 C 0.7578(6) 0.4198(6) 0.1884(7) 0.028(2) Uani 1 1 d . . . . . C38 C 0.7431(7) 0.4160(6) 0.0988(7) 0.040(2) Uani 1 1 d . . . . . H38 H 0.795165 0.425257 0.055300 0.048 Uiso 1 1 calc R . . . . C39 C 0.6535(7) 0.3988(7) 0.0705(7) 0.046(3) Uani 1 1 d . U . . . C40 C 0.5803(6) 0.3877(6) 0.1345(7) 0.035(2) Uani 1 1 d . U . . . H40 H 0.518466 0.374575 0.118615 0.042 Uiso 1 1 calc R . . . . C41 C 0.5965(6) 0.3958(6) 0.2234(7) 0.032(2) Uani 1 1 d . . . . . H41 H 0.542765 0.390949 0.265668 0.038 Uiso 1 1 calc R . . . . C42 C 0.6418(8) 0.3884(8) -0.0241(8) 0.068(3) Uani 1 1 d . U . . . H42A H 0.696360 0.324252 -0.025403 0.102 Uiso 1 1 calc GR . . . . H42B H 0.648684 0.452758 -0.075747 0.102 Uiso 1 1 calc GR . . . . H42C H 0.572517 0.381180 -0.033727 0.102 Uiso 1 1 calc GR . . . . C43 C 0.3014(7) 0.3013(6) 1.0209(7) 0.038(3) Uani 1 1 d . . . . . H43 H 0.242660 0.294739 1.056397 0.046 Uiso 1 1 calc R . . . . C44 C 0.3879(6) 0.2932(7) 0.8818(7) 0.055(3) Uani 1 1 d . . . . . H44A H 0.441209 0.306561 0.916071 0.083 Uiso 1 1 calc GR . . . . H44B H 0.364535 0.351980 0.818830 0.083 Uiso 1 1 calc GR . . . . H44C H 0.417859 0.224568 0.872442 0.083 Uiso 1 1 calc GR . . . . C45 C 0.2150(6) 0.2656(7) 0.9000(7) 0.041(3) Uani 1 1 d . . . . . H45A H 0.163016 0.257994 0.946979 0.062 Uiso 1 1 calc GR . . . . H45B H 0.242033 0.198394 0.887678 0.062 Uiso 1 1 calc GR . . . . H45C H 0.181968 0.325171 0.839499 0.062 Uiso 1 1 calc GR . . . . C46 C -0.0512(7) 0.1233(7) 0.1069(7) 0.044(3) Uani 1 1 d . . . . . B1 B 0.5462(7) 0.0248(7) 0.7576(7) 0.028(3) Uani 1 1 d . . . . . H1 H 0.574647 -0.047300 0.810844 0.034 Uiso 1 1 calc R . . . . 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 Co1 0.0236(6) 0.0150(6) 0.0298(8) -0.0032(5) 0.0048(5) -0.0061(4) Fe1 0.0225(6) 0.0159(7) 0.0302(8) -0.0050(6) 0.0054(5) -0.0067(5) S1 0.0403(14) 0.0274(14) 0.0464(18) -0.0086(12) 0.0141(12) -0.0147(10) F1 0.062(4) 0.060(4) 0.089(5) -0.025(4) 0.012(3) -0.042(3) F2 0.100(4) 0.048(4) 0.036(4) -0.015(3) -0.001(4) -0.013(3) F3 0.054(4) 0.076(4) 0.087(6) -0.023(4) -0.023(4) 0.004(3) O1 0.057(4) 0.042(4) 0.050(5) -0.008(4) -0.003(4) -0.022(3) O2 0.025(3) 0.048(4) 0.071(6) -0.022(4) 0.003(3) 0.000(3) O3 0.102(5) 0.041(4) 0.058(5) -0.008(4) 0.040(4) -0.035(3) O4 0.048(4) 0.038(4) 0.046(5) -0.011(3) 0.024(3) -0.010(3) O5 0.154(16) 0.150(17) 0.060(14) -0.025(12) 0.018(12) -0.078(14) N1 0.031(4) 0.014(4) 0.021(4) -0.005(3) 0.007(3) -0.009(3) N2 0.029(4) 0.013(4) 0.036(5) -0.004(3) 0.013(3) -0.006(3) N3 0.024(4) 0.010(4) 0.037(5) -0.002(3) 0.003(3) 0.000(3) N4 0.032(4) 0.018(4) 0.031(5) -0.005(3) -0.001(3) -0.006(3) N5 0.026(4) 0.020(4) 0.025(5) -0.007(4) 0.008(3) -0.006(3) N6 0.031(4) 0.016(4) 0.032(5) -0.007(4) 0.002(3) -0.008(3) N7 0.021(3) 0.016(4) 0.030(5) -0.006(3) 0.005(3) 0.002(3) N8 0.030(4) 0.024(4) 0.047(6) -0.019(4) 0.004(4) -0.005(3) N9 0.024(4) 0.015(4) 0.039(5) -0.008(3) 0.013(3) -0.007(3) N10 0.028(4) 0.014(4) 0.037(5) -0.009(4) 0.012(3) -0.009(3) N11 0.018(3) 0.018(4) 0.032(5) -0.008(4) 0.010(3) -0.006(3) N12 0.028(4) 0.013(4) 0.035(5) -0.003(4) 0.006(4) -0.002(3) N13 0.036(4) 0.011(4) 0.031(5) 0.004(3) -0.003(4) -0.001(3) N14 0.041(5) 0.027(5) 0.024(5) 0.008(4) 0.000(4) -0.004(3) C1 0.030(5) 0.035(5) 0.042(7) -0.019(5) 0.008(4) -0.017(4) C2 0.026(4) 0.015(4) 0.029(6) -0.005(4) 0.013(4) -0.006(3) C3 0.031(5) 0.021(5) 0.041(6) -0.011(4) 0.014(4) -0.016(4) C4 0.049(5) 0.013(5) 0.036(6) -0.013(4) 0.010(5) -0.012(4) C5 0.062(6) 0.019(5) 0.034(7) -0.001(5) 0.023(5) -0.016(4) C6 0.033(5) 0.015(5) 0.037(6) -0.008(4) 0.007(4) -0.009(3) C7 0.025(4) 0.017(5) 0.033(6) -0.004(4) 0.001(4) -0.002(4) C8 0.031(5) 0.029(5) 0.037(6) -0.022(5) 0.012(4) -0.011(4) C9 0.022(4) 0.029(5) 0.034(6) -0.013(4) -0.003(4) 0.001(4) C10 0.052(5) 0.029(5) 0.013(5) -0.001(4) 0.004(4) 0.002(4) C11 0.014(4) 0.027(5) 0.040(6) -0.009(4) 0.003(4) -0.007(3) C12 0.024(4) 0.023(5) 0.032(6) -0.006(4) 0.003(4) -0.014(4) C13 0.017(4) 0.015(5) 0.042(7) -0.009(4) 0.009(4) -0.001(3) C14 0.019(4) 0.020(5) 0.045(7) -0.013(5) 0.008(4) -0.003(3) C15 0.044(5) 0.017(5) 0.036(6) -0.015(4) 0.008(4) -0.005(4) C16 0.022(4) 0.025(5) 0.022(5) -0.012(4) 0.004(4) -0.009(4) C17 0.027(4) 0.016(4) 0.032(4) -0.011(3) 0.004(3) -0.004(3) C18 0.026(4) 0.018(5) 0.018(5) -0.010(4) 0.000(4) 0.000(3) C19 0.026(4) 0.010(5) 0.039(7) -0.001(4) 0.003(4) -0.004(3) C20 0.037(5) 0.028(6) 0.035(6) -0.006(5) -0.001(5) -0.015(4) C21 0.023(4) 0.030(6) 0.027(6) 0.004(5) -0.005(4) -0.007(4) C22 0.043(5) 0.015(5) 0.033(6) 0.001(4) 0.003(4) -0.010(4) C23 0.019(4) 0.021(5) 0.025(6) 0.002(4) 0.001(4) -0.001(3) C24 0.063(6) 0.029(6) 0.039(7) -0.011(5) -0.003(5) -0.014(5) C25 0.018(4) 0.025(5) 0.024(6) -0.002(4) 0.003(4) -0.011(3) C26 0.026(4) 0.018(5) 0.029(6) -0.004(4) 0.004(4) -0.001(3) C27 0.017(4) 0.020(5) 0.047(7) -0.014(5) 0.010(4) -0.007(3) C28 0.029(4) 0.014(5) 0.032(6) -0.007(4) 0.003(4) -0.006(3) C29 0.021(4) 0.022(5) 0.029(6) -0.008(4) 0.010(4) -0.010(3) C30 0.037(5) 0.015(5) 0.053(7) -0.009(5) 0.001(5) -0.010(4) C31 0.030(5) 0.017(5) 0.050(7) -0.010(4) 0.009(4) -0.010(4) C32 0.033(4) 0.026(4) 0.043(5) -0.007(3) 0.010(3) -0.014(3) C33 0.043(4) 0.033(4) 0.051(5) -0.014(3) 0.019(4) -0.018(3) C34 0.051(4) 0.024(4) 0.042(5) -0.011(3) 0.014(3) -0.012(3) C35 0.033(5) 0.013(5) 0.046(7) -0.010(5) 0.016(5) -0.007(4) C36 0.074(6) 0.051(6) 0.072(7) -0.035(5) 0.047(5) -0.039(5) C37 0.039(5) 0.012(5) 0.027(6) -0.005(4) 0.008(4) -0.001(4) C38 0.060(6) 0.023(5) 0.024(6) -0.005(5) 0.007(5) 0.002(4) C39 0.052(4) 0.040(4) 0.041(5) -0.021(4) -0.007(4) 0.002(3) C40 0.037(4) 0.028(4) 0.034(4) -0.014(3) -0.008(3) 0.003(3) C41 0.026(5) 0.018(5) 0.041(7) -0.011(4) -0.003(4) 0.006(4) C42 0.080(6) 0.061(6) 0.053(7) -0.039(5) -0.011(5) 0.015(5) C43 0.050(6) 0.019(5) 0.040(7) -0.003(5) 0.009(5) -0.012(4) C44 0.049(6) 0.043(6) 0.055(8) -0.007(6) 0.026(5) -0.003(5) C45 0.057(6) 0.026(5) 0.036(7) -0.007(5) -0.004(5) -0.010(4) C46 0.044(6) 0.029(6) 0.026(7) 0.018(5) -0.001(5) -0.001(4) B1 0.033(5) 0.011(5) 0.024(7) 0.006(5) 0.004(5) 0.001(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -16 -12 -11 0.0585 15 -1 8 0.0416 16 11 11 0.0616 3 -17 -2 0.1004 18 0 -2 0.0272 -18 0 2 0.0002 1 -15 -17 0.0815 -4 0 19 0.0332 4 0 -19 0.0332 -11 1 -14 0.0087 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Co1 N9 89.8(2) 2_666 . ? N7 Co1 N10 92.5(3) 2_666 . ? N7 Co1 N11 169.1(3) 2_666 . ? N7 Co1 N12 91.6(2) 2_666 . ? N7 Co1 N13 96.3(2) 2_666 . ? N9 Co1 N10 88.3(2) . . ? N9 Co1 N11 88.8(2) . . ? N9 Co1 N12 174.2(3) . . ? N10 Co1 N11 76.6(3) . . ? N12 Co1 N10 97.2(3) . . ? N12 Co1 N11 90.8(2) . . ? N13 Co1 N9 97.0(3) . . ? N13 Co1 N10 169.8(3) . . ? N13 Co1 N11 94.6(3) . . ? N13 Co1 N12 77.3(3) . . ? N3 Fe1 N1 89.6(3) . . ? N5 Fe1 N1 88.4(3) . . ? N5 Fe1 N3 91.0(3) . . ? C16 Fe1 N1 91.4(3) . . ? C16 Fe1 N3 89.6(3) . . ? C16 Fe1 N5 179.3(3) . . ? C16 Fe1 C18 91.9(3) . . ? C17 Fe1 N1 94.4(3) . . ? C17 Fe1 N3 171.7(3) . . ? C17 Fe1 N5 96.3(3) . . ? C17 Fe1 C16 83.0(3) . . ? C17 Fe1 C18 85.3(3) . . ? C18 Fe1 N1 176.5(3) . . ? C18 Fe1 N3 91.1(3) . . ? C18 Fe1 N5 88.2(3) . . ? O2 S1 O3 114.7(4) . . ? O2 S1 O4 115.9(4) . . ? O2 S1 C46 102.9(4) . . ? O3 S1 C46 103.1(4) . . ? O4 S1 O3 115.9(4) . . ? O4 S1 C46 101.4(4) . . ? H5D O5 H5E 105.6 . . ? N2 N1 Fe1 116.4(4) . . ? C2 N1 Fe1 136.4(5) . . ? C2 N1 N2 107.0(5) . . ? N1 N2 B1 120.0(6) . . ? C4 N2 N1 109.1(6) . . ? C4 N2 B1 130.8(6) . . ? N4 N3 Fe1 117.7(5) . . ? C7 N3 Fe1 137.3(5) . . ? C7 N3 N4 104.9(6) . . ? N3 N4 B1 117.7(6) . . ? C9 N4 N3 109.9(6) . . ? C9 N4 B1 132.3(7) . . ? N6 N5 Fe1 118.7(6) . . ? C12 N5 Fe1 135.5(5) . . ? C12 N5 N6 105.6(6) . . ? N5 N6 B1 117.6(7) . . ? C14 N6 N5 110.1(8) . . ? C14 N6 B1 132.1(7) . . ? C16 N7 Co1 163.8(6) . 2_666 ? C18 N9 Co1 163.3(6) . . ? C19 N10 Co1 126.8(5) . . ? C19 N10 C23 117.2(8) . . ? C23 N10 Co1 115.6(6) . . ? C25 N11 Co1 114.8(6) . . ? C29 N11 Co1 126.4(6) . . ? C29 N11 C25 118.6(7) . . ? C31 N12 Co1 125.9(6) . . ? C35 N12 Co1 116.6(5) . . ? C35 N12 C31 117.5(7) . . ? C37 N13 Co1 115.4(5) . . ? C41 N13 Co1 126.9(6) . . ? C41 N13 C37 116.1(8) . . ? C43 N14 C44 119.4(8) . . ? C43 N14 C45 123.3(8) . . ? C45 N14 C44 117.2(9) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C2 C1 123.8(6) . . ? N1 C2 C3 108.4(6) . . ? C3 C2 C1 127.7(6) . . ? C2 C3 H3 126.2 . . ? C4 C3 C2 107.6(7) . . ? C4 C3 H3 126.2 . . ? N2 C4 C5 121.6(7) . . ? C3 C4 N2 107.7(7) . . ? C3 C4 C5 130.6(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? N3 C7 C6 122.5(7) . . ? N3 C7 C8 111.1(6) . . ? C8 C7 C6 126.4(7) . . ? C7 C8 H8 127.3 . . ? C9 C8 C7 105.4(7) . . ? C9 C8 H8 127.3 . . ? N4 C9 C8 108.6(7) . . ? N4 C9 C10 121.4(7) . . ? C8 C9 C10 129.9(8) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? N5 C12 C11 125.0(7) . . ? N5 C12 C13 110.3(7) . . ? C13 C12 C11 124.7(9) . . ? C12 C13 H13 127.1 . . ? C14 C13 C12 105.9(8) . . ? C14 C13 H13 127.1 . . ? N6 C14 C13 108.1(7) . . ? N6 C14 C15 121.2(9) . . ? C13 C14 C15 130.6(8) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 Fe1 179.1(7) . . ? N8 C17 Fe1 173.2(7) . . ? N9 C18 Fe1 175.0(7) . . ? N10 C19 H19 117.7 . . ? N10 C19 C20 124.5(7) . . ? C20 C19 H19 117.7 . . ? C19 C20 H20 120.7 . . ? C19 C20 C21 118.5(9) . . ? C21 C20 H20 120.7 . . ? C20 C21 C24 119.9(9) . . ? C22 C21 C20 118.3(8) . . ? C22 C21 C24 121.8(7) . . ? C21 C22 H22 120.3 . . ? C21 C22 C23 119.4(7) . . ? C23 C22 H22 120.3 . . ? N10 C23 C22 121.8(8) . . ? N10 C23 C25 115.7(7) . . ? C22 C23 C25 122.5(7) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C23 115.2(7) . . ? N11 C25 C26 121.3(8) . . ? C26 C25 C23 123.3(8) . . ? C25 C26 H26 120.5 . . ? C27 C26 C25 119.0(8) . . ? C27 C26 H26 120.5 . . ? C26 C27 C30 118.6(8) . . ? C28 C27 C26 118.5(7) . . ? C28 C27 C30 122.9(8) . . ? C27 C28 H28 120.1 . . ? C27 C28 C29 119.8(8) . . ? C29 C28 H28 120.1 . . ? N11 C29 C28 122.8(8) . . ? N11 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N12 C31 H31 118.5 . . ? N12 C31 C32 123.0(9) . . ? C32 C31 H31 118.5 . . ? C31 C32 H32 120.2 . . ? C31 C32 C33 119.7(8) . . ? C33 C32 H32 120.2 . . ? C32 C33 C36 120.8(8) . . ? C34 C33 C32 116.9(8) . . ? C34 C33 C36 122.3(10) . . ? C33 C34 H34 119.0 . . ? C33 C34 C35 122.1(9) . . ? C35 C34 H34 119.0 . . ? N12 C35 C34 120.8(8) . . ? N12 C35 C37 114.7(7) . . ? C34 C35 C37 124.5(9) . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N13 C37 C35 114.9(8) . . ? C38 C37 N13 121.5(8) . . ? C38 C37 C35 123.6(8) . . ? C37 C38 H38 119.4 . . ? C37 C38 C39 121.3(9) . . ? C39 C38 H38 119.4 . . ? C38 C39 C42 120.5(10) . . ? C40 C39 C38 117.4(10) . . ? C40 C39 C42 122.1(9) . . ? C39 C40 H40 120.2 . . ? C39 C40 C41 119.7(8) . . ? C41 C40 H40 120.2 . . ? N13 C41 C40 124.1(8) . . ? N13 C41 H41 118.0 . . ? C40 C41 H41 118.0 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O1 C43 N14 127.1(9) . . ? O1 C43 H43 116.4 . . ? N14 C43 H43 116.4 . . ? N14 C44 H44A 109.5 . . ? N14 C44 H44B 109.5 . . ? N14 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N14 C45 H45A 109.5 . . ? N14 C45 H45B 109.5 . . ? N14 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? F1 C46 S1 113.3(7) . . ? F1 C46 F2 102.9(8) . . ? F2 C46 S1 111.7(6) . . ? F3 C46 S1 116.9(7) . . ? F3 C46 F1 106.0(7) . . ? F3 C46 F2 104.8(8) . . ? N2 B1 H1 110.8 . . ? N4 B1 N2 107.5(7) . . ? N4 B1 H1 110.8 . . ? N6 B1 N2 107.7(7) . . ? N6 B1 N4 109.2(6) . . ? N6 B1 H1 110.8 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N7 2.094(7) 2_666 ? Co1 N9 2.101(6) . ? Co1 N10 2.120(7) . ? Co1 N11 2.154(6) . ? Co1 N12 2.112(6) . ? Co1 N13 2.098(7) . ? Fe1 N1 1.999(6) . ? Fe1 N3 1.989(7) . ? Fe1 N5 1.971(7) . ? Fe1 C16 1.923(8) . ? Fe1 C17 1.922(8) . ? Fe1 C18 1.931(8) . ? S1 O2 1.434(5) . ? S1 O3 1.445(6) . ? S1 O4 1.434(7) . ? S1 C46 1.737(10) . ? F1 C46 1.353(9) . ? F2 C46 1.381(12) . ? F3 C46 1.321(9) . ? O1 C43 1.224(9) . ? O5 H5D 0.8744 . ? O5 H5E 0.8930 . ? N1 N2 1.372(7) . ? N1 C2 1.353(8) . ? N2 C4 1.360(9) . ? N2 B1 1.535(10) . ? N3 N4 1.398(8) . ? N3 C7 1.360(9) . ? N4 C9 1.349(10) . ? N4 B1 1.531(11) . ? N5 N6 1.381(8) . ? N5 C12 1.360(11) . ? N6 C14 1.349(10) . ? N6 B1 1.523(12) . ? N7 C16 1.149(9) . ? N8 C17 1.161(9) . ? N9 C18 1.139(9) . ? N10 C19 1.327(10) . ? N10 C23 1.360(9) . ? N11 C25 1.351(9) . ? N11 C29 1.336(10) . ? N12 C31 1.352(9) . ? N12 C35 1.350(11) . ? N13 C37 1.382(10) . ? N13 C41 1.338(9) . ? N14 C43 1.313(12) . ? N14 C44 1.438(10) . ? N14 C45 1.435(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.504(9) . ? C2 C3 1.388(9) . ? C3 H3 0.9500 . ? C3 C4 1.358(10) . ? C4 C5 1.517(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6 C7 1.503(9) . ? C7 C8 1.390(10) . ? C8 H8 0.9500 . ? C8 C9 1.385(10) . ? C9 C10 1.501(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 C12 1.508(10) . ? C12 C13 1.388(10) . ? C13 H13 0.9500 . ? C13 C14 1.384(12) . ? C14 C15 1.499(10) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C19 H19 0.9500 . ? C19 C20 1.367(11) . ? C20 H20 0.9500 . ? C20 C21 1.389(10) . ? C21 C22 1.386(12) . ? C21 C24 1.484(11) . ? C22 H22 0.9500 . ? C22 C23 1.388(11) . ? C23 C25 1.484(12) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.404(10) . ? C26 H26 0.9500 . ? C26 C27 1.392(12) . ? C27 C28 1.372(11) . ? C27 C30 1.519(10) . ? C28 H28 0.9500 . ? C28 C29 1.376(10) . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C31 C32 1.370(10) . ? C32 H32 0.9500 . ? C32 C33 1.395(13) . ? C33 C34 1.354(11) . ? C33 C36 1.510(11) . ? C34 H34 0.9500 . ? C34 C35 1.389(11) . ? C35 C37 1.474(11) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.371(12) . ? C38 H38 0.9500 . ? C38 C39 1.390(11) . ? C39 C40 1.359(12) . ? C39 C42 1.480(13) . ? C40 H40 0.9500 . ? C40 C41 1.391(12) . ? C41 H41 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? B1 H1 1.0000 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O5 H5D N8 0.87 2.15 2.988(18) 161.8 2_666 yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co1 N10 C19 C20 175.2(6) . . . . ? Co1 N10 C23 C22 -172.2(6) . . . . ? Co1 N10 C23 C25 8.5(8) . . . . ? Co1 N11 C25 C23 -12.5(8) . . . . ? Co1 N11 C25 C26 172.1(5) . . . . ? Co1 N11 C29 C28 -172.6(5) . . . . ? Co1 N12 C31 C32 -179.3(6) . . . . ? Co1 N12 C35 C34 177.5(6) . . . . ? Co1 N12 C35 C37 -5.0(9) . . . . ? Co1 N13 C37 C35 -11.4(8) . . . . ? Co1 N13 C37 C38 166.8(6) . . . . ? Co1 N13 C41 C40 -162.6(6) . . . . ? Fe1 N1 N2 C4 -173.5(6) . . . . ? Fe1 N1 N2 B1 3.6(10) . . . . ? Fe1 N1 C2 C1 -6.3(14) . . . . ? Fe1 N1 C2 C3 172.6(6) . . . . ? Fe1 N3 N4 C9 -178.6(5) . . . . ? Fe1 N3 N4 B1 3.7(9) . . . . ? Fe1 N3 C7 C6 -1.4(13) . . . . ? Fe1 N3 C7 C8 178.2(6) . . . . ? Fe1 N5 N6 C14 -177.1(5) . . . . ? Fe1 N5 N6 B1 7.8(8) . . . . ? Fe1 N5 C12 C11 -2.7(11) . . . . ? Fe1 N5 C12 C13 176.6(5) . . . . ? O2 S1 C46 F1 63.9(8) . . . . ? O2 S1 C46 F2 -51.7(6) . . . . ? O2 S1 C46 F3 -172.3(7) . . . . ? O3 S1 C46 F1 -176.5(7) . . . . ? O3 S1 C46 F2 67.9(6) . . . . ? O3 S1 C46 F3 -52.8(9) . . . . ? O4 S1 C46 F1 -56.3(7) . . . . ? O4 S1 C46 F2 -171.9(5) . . . . ? O4 S1 C46 F3 67.5(8) . . . . ? N1 N2 C4 C3 -1.9(10) . . . . ? N1 N2 C4 C5 178.2(8) . . . . ? N1 N2 B1 N4 56.9(10) . . . . ? N1 N2 B1 N6 -60.7(9) . . . . ? N1 C2 C3 C4 1.3(11) . . . . ? N2 N1 C2 C1 178.7(8) . . . . ? N2 N1 C2 C3 -2.4(10) . . . . ? N3 N4 C9 C8 0.5(9) . . . . ? N3 N4 C9 C10 -176.8(7) . . . . ? N3 N4 B1 N2 -60.7(9) . . . . ? N3 N4 B1 N6 55.9(9) . . . . ? N3 C7 C8 C9 -1.4(9) . . . . ? N4 N3 C7 C6 -177.9(7) . . . . ? N4 N3 C7 C8 1.6(9) . . . . ? N5 N6 C14 C13 -0.3(8) . . . . ? N5 N6 C14 C15 178.7(6) . . . . ? N5 N6 B1 N2 53.3(8) . . . . ? N5 N6 B1 N4 -63.2(8) . . . . ? N5 C12 C13 C14 -0.2(8) . . . . ? N6 N5 C12 C11 -179.2(6) . . . . ? N6 N5 C12 C13 0.1(8) . . . . ? N10 C19 C20 C21 -2.7(12) . . . . ? N10 C23 C25 N11 2.8(9) . . . . ? N10 C23 C25 C26 178.1(6) . . . . ? N11 C25 C26 C27 2.1(10) . . . . ? N12 C31 C32 C33 0.1(13) . . . . ? N12 C35 C37 N13 10.8(10) . . . . ? N12 C35 C37 C38 -167.3(8) . . . . ? N13 C37 C38 C39 -1.9(13) . . . . ? C1 C2 C3 C4 -179.9(9) . . . . ? C2 N1 N2 C4 2.7(9) . . . . ? C2 N1 N2 B1 179.8(8) . . . . ? C2 C3 C4 N2 0.4(11) . . . . ? C2 C3 C4 C5 -179.7(10) . . . . ? C4 N2 B1 N4 -126.7(9) . . . . ? C4 N2 B1 N6 115.7(9) . . . . ? C6 C7 C8 C9 178.1(8) . . . . ? C7 N3 N4 C9 -1.3(9) . . . . ? C7 N3 N4 B1 -178.9(7) . . . . ? C7 C8 C9 N4 0.5(9) . . . . ? C7 C8 C9 C10 177.5(9) . . . . ? C9 N4 B1 N2 122.3(9) . . . . ? C9 N4 B1 N6 -121.1(9) . . . . ? C11 C12 C13 C14 179.1(6) . . . . ? C12 N5 N6 C14 0.1(8) . . . . ? C12 N5 N6 B1 -175.0(6) . . . . ? C12 C13 C14 N6 0.3(8) . . . . ? C12 C13 C14 C15 -178.5(7) . . . . ? C14 N6 B1 N2 -120.5(8) . . . . ? C14 N6 B1 N4 123.0(8) . . . . ? C19 N10 C23 C22 1.9(10) . . . . ? C19 N10 C23 C25 -177.3(6) . . . . ? C19 C20 C21 C22 0.0(12) . . . . ? C19 C20 C21 C24 179.5(8) . . . . ? C20 C21 C22 C23 3.5(12) . . . . ? C21 C22 C23 N10 -4.5(12) . . . . ? C21 C22 C23 C25 174.6(7) . . . . ? C22 C23 C25 N11 -176.5(7) . . . . ? C22 C23 C25 C26 -1.1(11) . . . . ? C23 N10 C19 C20 1.8(11) . . . . ? C23 C25 C26 C27 -172.9(7) . . . . ? C24 C21 C22 C23 -176.1(8) . . . . ? C25 N11 C29 C28 1.7(10) . . . . ? C25 C26 C27 C28 -0.3(11) . . . . ? C25 C26 C27 C30 -179.2(6) . . . . ? C26 C27 C28 C29 -0.8(10) . . . . ? C27 C28 C29 N11 0.1(11) . . . . ? C29 N11 C25 C23 172.6(6) . . . . ? C29 N11 C25 C26 -2.8(10) . . . . ? C30 C27 C28 C29 178.1(6) . . . . ? C31 N12 C35 C34 -4.0(11) . . . . ? C31 N12 C35 C37 173.5(6) . . . . ? C31 C32 C33 C34 -0.7(13) . . . . ? C31 C32 C33 C36 179.1(8) . . . . ? C32 C33 C34 C35 -1.0(13) . . . . ? C33 C34 C35 N12 3.4(13) . . . . ? C33 C34 C35 C37 -173.8(8) . . . . ? C34 C35 C37 N13 -171.8(7) . . . . ? C34 C35 C37 C38 10.0(12) . . . . ? C35 N12 C31 C32 2.3(11) . . . . ? C35 C37 C38 C39 176.1(7) . . . . ? C36 C33 C34 C35 179.2(8) . . . . ? C37 N13 C41 C40 1.9(11) . . . . ? C37 C38 C39 C40 1.0(13) . . . . ? C37 C38 C39 C42 -176.3(8) . . . . ? C38 C39 C40 C41 1.2(12) . . . . ? C39 C40 C41 N13 -2.8(13) . . . . ? C41 N13 C37 C35 -177.8(6) . . . . ? C41 N13 C37 C38 0.4(11) . . . . ? C42 C39 C40 C41 178.4(9) . . . . ? C44 N14 C43 O1 2.1(14) . . . . ? C45 N14 C43 O1 -179.4(8) . . . . ? B1 N2 C4 C3 -178.6(9) . . . . ? B1 N2 C4 C5 1.5(15) . . . . ? B1 N4 C9 C8 177.7(8) . . . . ? B1 N4 C9 C10 0.4(14) . . . . ? B1 N6 C14 C13 173.9(7) . . . . ? B1 N6 C14 C15 -7.2(12) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 2 9.1 9.01 0 0 -2 6.88 8.38 0 0 3 196.5 31.65 0 0 -3 207.04 31.5 0 0 4 1389.16 94.67 0 0 5 1064.07 94.05 0 0 6 949.22 96.98 0 0 7 28.56 20.68 0 0 8 28.99 21.6 0 0 9 761.49 109.57 0 0 10 150.16 53.45 0 0 11 699.36 118.59 0 0 12 -4.85 26.93 0 0 13 118.28 59.27 0 0 14 175.56 71.71 0 0 15 -52.99 55.86 0 0 16 14.16 25.96 0 0 16 17.35 29.89 0 0 17 52.11 48.1 0 0 17 -20.94 30.15 0 0 18 94.12 72.79 0 0 18 -65.09 51.81 0 -1 17 32.14 37.95 0 -1 17 -33.42 38.11 0 -1 16 -162.56 87.08 0 -1 16 -43.66 39.78 0 -1 15 156.98 73.92 0 -1 15 21.99 24.66 0 -1 14 107.15 59.49 0 -1 14 107.22 48.19 0 -1 13 154.62 64.52 0 -1 13 245.84 74.78 0 -1 12 24.32 27.63 0 -1 11 18.6 20.99 0 -1 10 394.35 86.89 0 -1 9 182.56 57.4 0 -1 8 129.26 45.26 0 -1 7 12.07 17.28 0 -1 6 993.72 105.76 0 -1 5 28.64 20.49 0 -1 4 89.49 25.79 0 -1 3 44.37 18.66 0 -1 3 54.68 10.13 0 -1 2 1390.57 64.97 0 -1 2 1356.84 47.98 0 1 -2 1315.1 75.62 0 -1 2 1382.59 77.64 0 1 2 1408.64 63.87 0 1 3 2002.84 93.54 0 -1 -3 2231.94 99.02 0 -1 -4 520.23 29.49 0 1 4 564.53 58.36 0 1 5 219.49 42.9 0 1 6 180.51 43.95 0 1 7 44.51 27.49 0 1 8 -1.71 10.9 0 1 9 15.07 22.4 0 1 10 91.44 41.79 0 1 11 8.65 18.38 0 1 12 6.23 19.86 0 1 13 -2.47 15.24 0 1 14 -3.33 18.16 0 1 15 40.19 52.3 0 1 16 -38.98 38.31 0 1 17 -10.17 37.57 0 1 18 22.41 52.19 0 1 18 -53.6 48.12 0 1 19 -2.59 31.02 0 -2 17 -70.5 56.44 0 -2 16 7.44 29.62 0 -2 15 12.52 30.17 0 -2 15 -16.85 35.9 0 -2 14 115.63 62.91 0 -2 14 10.85 15.16 0 -2 13 228.64 83.56 0 -2 13 30.51 22.13 0 -2 12 65.53 48.95 0 -2 12 64.18 35.96 0 -2 11 37 34.82 0 -2 11 93.17 41.39 0 -2 10 121.4 50.38 0 -2 10 32.35 27.12 0 -2 9 328.02 78.68 0 -2 9 395.21 73.84 0 -2 8 14.48 17.1 0 -2 8 37.06 26.54 0 -2 7 52.67 30.03 0 -2 7 107.98 36.01 0 -2 6 159.26 50.25 0 -2 6 126.65 19.66 0 -2 6 160.83 41.88 0 -2 5 128.87 47.61 0 -2 5 27.44 11.3 0 -2 5 37.34 20.74 0 -2 4 495.6 56.25 0 -2 4 555.9 70.42 0 -2 4 532.73 42.71 0 -2 3 88.73 21.53 0 -2 3 107.11 27.08 0 2 -2 144.44 26.61 0 -2 2 287.78 44.97 0 -2 2 250.02 35.43 0 -2 2 505.9 60.93 0 -2 2 191.93 29.8 0 -2 1 651 46.98 0 2 -1 671.01 49.15 0 2 -1 739.61 58.52 0 -2 1 683.3 55.93 0 -2 0 719.86 46.02 0 2 0 659.48 44.41 0 2 0 766.32 52.78 0 -2 0 702.62 50.11 0 2 1 2112.22 83.5 0 -2 -1 1903.05 77.22 0 -2 -1 2070.7 82.52 0 2 1 1994.47 82.18 0 2 2 1978.01 85.87 0 -2 -2 1960.86 85.24 0 2 3 1302.58 76.15 0 2 3 1222.88 75.95 0 -2 -3 1293.7 77.82 0 2 4 12.48 11.73 0 -2 -5 348.13 34.94 0 2 5 300.59 46.87 0 -2 -6 420.78 38.15 0 2 6 663.56 78.48 0 -2 -7 1304.75 64.35 0 2 7 1323.1 116.59 0 -2 -8 4.22 5.33 0 2 8 -0.86 17.79 0 2 9 -23.86 25.67 0 2 10 3.76 16.67 0 2 11 26.89 27.01 0 2 12 258.49 72.92 0 2 13 29.06 33.77 0 2 14 -11.02 23.6 0 2 15 50.17 43.86 0 2 16 68.98 48 0 2 17 49.23 50.9 0 2 18 23.11 47.25 0 -3 17 28.71 50.31 0 -3 16 -15.08 32.49 0 -3 16 -9.2 24.54 0 -3 15 81.21 51.69 0 -3 14 61.82 42.24 0 -3 14 36.2 40.8 0 -3 13 90.41 48.09 0 -3 13 80.13 59.6 0 -3 12 1.36 24.82 0 -3 12 -75.23 51.43 0 -3 11 86.43 45.75 0 -3 11 71.29 44.98 0 -3 10 -7.63 17.5 0 -3 10 -23.12 24.89 0 -3 9 218.65 53.66 0 -3 9 220.29 67.32 0 -3 8 317.35 62.86 0 -3 8 331.23 77.87 0 -3 7 1055.82 69.14 0 -3 7 1103.9 110.21 0 -3 7 1159.8 136.12 0 -3 6 -11.09 16.41 0 -3 6 3.62 11.91 0 -3 6 8.69 8.97 0 -3 5 26.53 18.24 0 -3 5 61.58 18.08 0 -3 5 24.65 18.56 0 -3 4 52.61 29.5 0 -3 4 39.1 16.19 0 -3 4 91.61 31.17 0 -3 4 58.91 31.67 0 -3 3 2130.61 76.27 0 -3 3 2049.36 116.46 0 3 -3 1988.95 72.66 0 -3 3 2142.74 106.79 0 -3 3 2209.84 77.05 0 -3 3 1972 131.21 0 -3 2 1454.94 103.45 0 -3 2 1577.72 91.7 0 3 -2 1471.82 88.32 0 -3 2 1508.14 89.63 0 -3 1 2480.81 124.8 0 3 -1 2379.16 107.25 0 -3 1 2154.29 101.27 0 3 0 173.59 30.39 0 -3 0 188.99 30.8 0 -3 0 185.97 33.18 0 -3 -1 6839.97 177.89 0 3 1 7482.7 183.32 0 -3 -1 7066.46 187.79 0 3 1 7239.4 189.14 0 3 2 2572.79 114.97 0 -3 -2 2510.81 112.09 0 -3 -3 627.04 59.37 0 3 4 969.72 79.92 0 -3 -4 1297.13 91.48 0 3 5 461.62 60.6 0 3 6 857.55 89.45 0 3 7 25.78 22.47 0 3 8 45.61 22.7 0 -3 -8 72.08 20.17 0 3 9 150.73 47.44 0 -3 -9 131.07 25.54 0 3 10 139.67 48.76 0 -3 -10 112.26 21.65 0 3 11 115.73 45.38 0 3 12 18.98 26.01 0 3 13 270.92 77.59 0 3 14 79.66 49.89 0 3 15 186.58 73.61 0 3 16 -121.12 65.16 0 3 17 144.97 71.09 0 3 18 -0.58 26.18 0 3 19 32.98 44.1 0 -4 16 28.9 39.41 0 -4 15 122.12 72.29 0 -4 15 -60.63 51.23 0 -4 14 37.67 34.66 0 -4 14 12.26 30.03 0 -4 13 40.51 37.41 0 -4 13 33.41 30.39 0 -4 13 80.66 55.81 0 -4 12 60.94 46.28 0 -4 12 116.94 51.5 0 -4 12 127.54 66.34 0 -4 11 53.28 33.57 0 -4 11 110.74 46.91 0 -4 11 97.3 53.89 0 -4 10 34.68 31.65 0 -4 10 14.98 20.69 0 -4 10 7.76 18.84 0 -4 9 111.72 47.76 0 -4 9 57.7 24.17 0 -4 9 109.72 49.79 0 -4 8 44.15 31 0 -4 8 2.96 12.04 0 -4 8 -4.42 13.77 0 -4 7 132.08 47.5 0 -4 7 106.6 44.92 0 -4 7 120.43 39.54 0 -4 6 -6.32 16.95 0 -4 6 87.75 41.2 0 -4 6 64.6 37.25 0 -4 5 10.19 12.53 0 -4 5 41.38 15.73 0 -4 5 30.39 13.34 0 4 -5 12.09 9.1 0 -4 5 30.43 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-4 3 264.28 100.16 -16 -4 3 118.2 69.92 -16 -4 2 174.2 88.09 -16 -4 2 144.6 85.67 -16 -4 1 50.92 46.23 -16 -4 1 6.84 26.18 -16 -4 0 -49.38 53.65 -16 -4 0 -13.46 28.77 -16 -4 -1 16.69 24.54 -16 -4 -1 -35.93 45.07 -16 -4 -2 -35.75 44.8 -16 -4 -2 19.35 27.53 16 4 3 -25.9 38.94 -16 -4 -3 65.34 54.49 -16 -4 -3 3.59 30.09 16 4 4 -62.39 45.63 -16 -4 -4 14.66 48.34 -16 -4 -4 36.01 37.32 -16 -4 -5 -64.26 58.26 16 4 5 67.61 53.16 -16 -4 -5 -35.82 49.29 -16 -4 -6 -24.44 46.39 16 4 6 50.12 44.43 -16 -4 -6 59.68 55.36 -16 -4 -7 21.17 37.34 16 4 7 21.2 33.21 -16 -4 -7 -51.09 56.16 16 4 8 -70.65 66.57 -16 -5 8 -32.83 51.53 -16 -5 8 -37.14 54.01 -16 -5 7 55.36 55.26 -16 -5 7 44.8 47.4 -16 -5 6 -19.23 30.55 -16 -5 6 148.5 88.28 -16 -5 5 166.08 81.94 -16 -5 5 293.54 109.64 -16 -5 4 0.67 26.93 -16 -5 4 -19.04 40.04 -16 -5 3 78.23 57.97 -16 -5 3 -105.54 67.84 -16 -5 2 -34.43 45.45 -16 -5 2 53.05 43.73 -16 -5 1 18.12 42.08 -16 -5 1 -30.52 48.69 -16 -5 0 12.39 33.44 -16 -5 0 17.65 40.96 -16 -5 -1 28.07 38.63 -16 -5 -1 43.43 45.52 -16 -5 -2 315.83 111.39 -16 -5 -2 258.91 102.59 -16 -5 -3 131.51 75.97 -16 -5 -3 -43.07 52 -16 -5 -4 229.27 99.97 -16 -5 -4 217.04 90.02 -16 -5 -5 14.26 28.81 16 5 5 -31.84 44.42 -16 -5 -5 52.71 51.21 -16 -5 -6 118.88 74.38 16 5 6 -30.39 40.82 -16 -5 -6 91.92 63.77 -16 -5 -7 5.05 23.45 -16 -5 -7 -24.41 30.56 16 5 8 -18.7 32.45 16 5 9 -42.04 46.01 -16 -6 8 85.16 62.35 -16 -6 8 -89.78 63.67 -16 -6 7 -41.22 50.91 -16 -6 7 45.43 48.05 -16 -6 6 133.91 71.88 -16 -6 6 10.13 35.72 -16 -6 5 38.56 47.68 -16 -6 5 -1.94 31.96 -16 -6 4 7.16 21.6 -16 -6 4 103.08 65.9 -16 -6 3 -70.21 63.2 -16 -6 3 7.75 26.39 -16 -6 2 -34.83 43.16 -16 -6 2 -30.26 37.16 -16 -6 1 26.28 41.09 -16 -6 1 -11.05 36.56 -16 -6 0 282.27 104.43 -16 -6 0 48.85 53.23 -16 -6 -1 88.77 64.55 -16 -6 -1 126.65 71.62 -16 -6 -2 -29.03 23.51 -16 -6 -2 29.41 45.77 -16 -6 -3 -40.55 52.79 -16 -6 -3 51.63 50.25 -16 -6 -4 7.11 27.79 -16 -6 -4 141.93 80.51 -16 -6 -5 13.13 29.44 -16 -6 -5 32.63 44.76 -16 -6 -6 -10.75 43.18 16 6 6 89.42 65.38 -16 -6 -6 41.99 56.81 -16 -6 -7 36.37 52.14 16 6 7 41.93 36.46 16 6 8 -89.96 66.62 16 6 9 -80.44 61.18 -16 -7 7 19.81 23.2 -16 -7 7 96.49 64.78 -16 -7 6 18.31 31.65 -16 -7 6 27.99 47.24 -16 -7 5 24.41 35.92 -16 -7 5 -0.07 19.9 -16 -7 4 67.32 50.92 -16 -7 4 17.33 22.01 -16 -7 3 2.55 22.13 -16 -7 3 8.04 29.96 -16 -7 2 -46.59 51.66 -16 -7 2 -53.46 47.37 -16 -7 1 49.57 50.84 -16 -7 1 8.22 28.07 -16 -7 0 87.88 58.94 -16 -7 0 1.17 21.97 -16 -7 -1 -55.41 58.88 -16 -7 -1 -60.93 63.4 -16 -7 -2 153.16 84.24 -16 -7 -2 119.61 72.95 -16 -7 -3 -41.25 49.72 -16 -7 -3 46.7 43.24 -16 -7 -4 82.34 65.56 -16 -7 -4 27.22 40.56 -16 -7 -5 63.59 53.63 -16 -7 -5 71.72 59.87 -16 -7 -6 191.22 95.06 -16 -7 -6 114.14 78.69 -16 -7 -7 19.39 28.68 -16 -7 -7 71.67 48.43 16 7 8 0.56 35.53 16 7 9 13.51 34.06 16 7 10 2.51 31.14 16 8 -7 -69.07 58.22 -16 -8 6 -41.67 46.35 16 8 -6 15.29 40.77 -16 -8 6 25.18 34.23 -16 -8 5 10.29 31.85 -16 -8 5 38.76 41.94 -16 -8 4 165.86 78.34 -16 -8 4 10.93 32.97 -16 -8 3 271.89 99.32 -16 -8 3 120.43 72.93 -16 -8 2 23.05 45.76 -16 -8 2 16.98 40.39 -16 -8 1 80.27 61.66 -16 -8 1 -36.78 57.02 -16 -8 0 -4.57 22.11 -16 -8 0 11.32 23.51 -16 -8 -1 73.79 47.72 -16 -8 -1 23.04 32.96 -16 -8 -2 33.98 40.28 -16 -8 -2 32.13 43.73 -16 -8 -3 151.73 75.59 -16 -8 -3 108.25 61.62 -16 -8 -4 42.16 40.66 -16 -8 -4 116.55 72.73 -16 -8 -5 94.31 67.49 -16 -8 -5 -1.83 23.62 -16 -8 -6 77.27 58.65 -16 -8 -6 73.69 62.99 -16 -8 -7 51.28 44.95 -16 -8 -7 143.24 77.39 16 8 9 66.8 62.55 16 8 10 -18.05 43.69 16 9 -5 58.91 47.81 -16 -9 4 -11.88 26.51 16 9 -4 76.26 62.56 -16 -9 4 96.02 62.45 -16 -9 3 68.8 49.99 16 9 -3 30.87 56.78 -16 -9 3 36.54 45.18 -16 -9 2 15.48 27.41 16 9 -2 106.38 70.19 -16 -9 2 18.28 31.44 -16 -9 1 104.47 65.2 -16 -9 1 39.2 38.55 -16 -9 0 -44.08 46.68 -16 -9 0 -14.56 34.7 -16 -9 -1 -129.06 78.99 -16 -9 -1 -42.98 54.12 -16 -9 -2 67.62 55.62 -16 -9 -2 39.51 47.83 -16 -9 -3 115.24 61.33 -16 -9 -3 63.96 58.85 -16 -9 -4 -15.74 30.92 -16 -9 -4 -73.58 63.99 -16 -9 -5 -134 77 -16 -9 -5 -27.42 55.56 -16 -9 -6 184.22 85.32 16 9 6 -79.89 57.44 -16 -9 -6 71.82 61.75 16 9 7 -18.78 41.81 16 9 8 -31.35 41.76 16 9 9 44.51 54.55 16 9 10 26.62 43.96 16 10 -3 -58.72 55.6 -16 -10 2 6.5 25.63 16 10 -2 -15.77 31.69 -16 -10 2 -34.11 32.85 -16 -10 1 105.64 65.86 16 10 -1 8.71 40.88 -16 -10 1 21.02 33.91 -16 -10 0 -78.75 59 16 10 0 10.34 24.06 -16 -10 0 -25.65 47.67 -16 -10 -1 61.35 50.63 -16 -10 -1 82.57 52.99 16 10 1 80.16 65.14 -16 -10 -2 23.55 37 16 10 2 13.09 41.65 -16 -10 -2 70.45 60.63 -16 -10 -3 136.18 75.17 16 10 3 150.85 82.54 -16 -10 -3 222.09 87.38 -16 -10 -4 140.44 74.32 16 10 4 319.36 117.45 -16 -10 -4 192.63 85.21 -16 -10 -5 147.3 78.93 16 10 5 58.38 57.73 -16 -10 -6 -17.68 35.65 16 10 6 60.75 67.33 -16 -10 -6 100.03 68.18 16 10 7 -53.06 52.15 16 10 8 0.08 42.54 16 10 9 76.35 57.92 16 10 10 6.31 28.62 -16 -11 0 93.42 65.22 16 11 0 68.59 59.25 -16 -11 0 -10.68 32.73 -16 -11 -1 137.98 80.41 16 11 1 66.77 50.76 -16 -11 -1 161.03 79.86 -16 -11 -2 26.6 37.99 16 11 2 94.05 82.2 -16 -11 -2 -39.17 40.62 -16 -11 -3 71.2 51.55 -16 -11 -3 8.11 31.03 -16 -11 -4 36.8 48.04 16 11 4 -34.7 51.37 -16 -11 -4 21.78 36.93 -16 -11 -5 198.35 95.34 16 11 5 2.97 26.19 -16 -11 -5 143.51 72.86 16 11 6 -54.07 61.1 16 11 7 -15.64 33.3 16 11 8 37.83 40.17 -16 -12 -2 54.76 46.13 -16 -12 -2 159.55 82.17 -16 -12 -3 -25.39 34.54 -16 -12 -3 -110.27 66.62 -16 -12 -4 49.59 47.24 -16 -12 -4 44.77 34.22 17 -2 -3 -46.94 65.74 17 -2 -2 100.32 75.33 17 -1 -2 75.57 64.41 17 -1 -1 28.19 31.92 17 -1 0 65.99 67.63 17 0 0 -68.53 64.27 17 0 1 -46.28 67.87 17 0 2 -70.21 60.26 17 1 1 -32.73 44.63 17 1 2 49.2 47.02 17 1 3 -54.35 59.27 -17 -2 2 -54.6 52.61 -17 -2 2 -17.32 31.28 -17 -2 1 53.86 62.07 -17 -2 1 -61.04 54.64 -17 -2 0 8.29 32.72 -17 -2 0 -65.33 64.13 17 2 2 10.09 32.34 17 2 3 11.42 27.97 17 2 4 -28.61 49.4 17 2 5 -13.83 36.98 -17 -3 4 4.26 28.25 -17 -3 4 68.44 60.52 -17 -3 3 -92.56 58.74 -17 -3 3 42.28 46.18 -17 -3 2 105.7 64.49 -17 -3 2 -21.47 49.64 -17 -3 1 64.04 62.09 -17 -3 1 6.61 25.5 -17 -3 0 -6.03 32.03 -17 -3 0 42.59 44.13 -17 -3 -1 22.65 51.07 -17 -3 -1 0.17 34.57 -17 -3 -2 58.43 61.74 -17 -3 -2 -49.23 52.39 17 3 3 -5.09 28.54 17 3 4 -68.4 58.22 17 3 5 137.46 79.23 17 3 6 -16.56 39.79 -17 -4 4 -24.67 49.28 -17 -4 4 71.8 66.12 -17 -4 3 -21.9 52.04 -17 -4 3 45.42 39.65 -17 -4 2 -18.02 45.75 -17 -4 2 51.55 62.23 -17 -4 1 -0.9 29.29 -17 -4 1 19.21 25.18 -17 -4 0 -65.16 69.72 -17 -4 0 187.1 87.24 -17 -4 -1 -13.78 37.23 -17 -4 -1 14.86 29.04 -17 -4 -2 78.31 60.97 -17 -4 -2 -16.99 37.78 -17 -4 -3 4.28 33.25 -17 -4 -3 72.58 51.23 17 4 5 -51.63 43.68 17 4 6 -44.09 50.15 -17 -5 5 -45.83 50.24 -17 -5 5 168.88 91.25 -17 -5 4 -24.4 35.52 -17 -5 4 32.42 41.23 -17 -5 3 -30.44 51.2 -17 -5 3 -55.59 50.88 -17 -5 2 25.88 36.72 -17 -5 2 23.5 41.47 -17 -5 1 15.68 35.53 -17 -5 1 -5.43 30.11 -17 -5 0 -41.11 60.06 -17 -5 0 115.09 69.43 -17 -5 -1 -46.64 50.74 -17 -5 -1 -96.22 65.86 -17 -5 -2 -10.06 60.2 -17 -5 -2 53.02 52.3 -17 -5 -3 121.71 75.16 -17 -5 -3 -15.25 38.34 17 5 6 -42.46 52.53 17 5 7 -10.33 39.22 -17 -6 5 61.99 61.96 -17 -6 5 -11.3 42.82 -17 -6 4 151.6 80.62 -17 -6 4 104.66 60.11 -17 -6 3 35.14 39.32 -17 -6 3 48.49 45.56 -17 -6 2 122.4 71.88 -17 -6 2 147.96 82.94 -17 -6 1 49.44 44.42 -17 -6 1 -8 26.45 -17 -6 0 -40.49 51.48 -17 -6 0 -22.17 47.62 -17 -6 -1 -16.61 39.22 -17 -6 -1 29.15 43.01 -17 -6 -2 13.84 25.92 -17 -6 -2 30.52 47.38 -17 -6 -3 110.8 77.86 -17 -6 -3 265.1 104.47 -17 -6 -4 36.2 43.49 -17 -6 -4 -9.01 37.2 17 6 8 44 48.66 -17 -7 5 -89.31 63.41 -17 -7 5 48.52 53.69 -17 -7 4 69.73 56.35 -17 -7 4 -38.28 57.15 -17 -7 3 39.02 43.71 -17 -7 3 73.72 61.67 -17 -7 2 31.16 43.94 -17 -7 2 89.71 66.01 -17 -7 1 67.6 55.73 -17 -7 1 19.17 39.1 -17 -7 0 57.72 51.66 -17 -7 0 -55.4 58.82 -17 -7 -1 135.63 82.54 -17 -7 -1 -42.76 54.3 -17 -7 -2 56.5 49.69 -17 -7 -2 56.23 50.05 -17 -7 -3 65.83 62.03 -17 -7 -3 41.93 49.96 -17 -7 -4 39.19 59.86 -17 -7 -4 -8.09 25.87 -17 -8 5 -46.18 40.74 -17 -8 5 34.86 46.44 -17 -8 4 14.31 26.66 -17 -8 4 56.61 45.75 -17 -8 3 -17.43 44.96 -17 -8 3 -1.73 32.38 -17 -8 2 80.66 67.51 -17 -8 2 -36.39 55.6 -17 -8 1 3.8 45.2 -17 -8 1 29.62 52.43 -17 -8 0 -51.63 55.54 -17 -8 0 38.85 44.29 -17 -8 -1 143.92 78.47 -17 -8 -1 46.16 26.72 -17 -8 -2 41.72 48.78 -17 -8 -2 45.83 60.11 -17 -8 -3 -39.28 49.71 -17 -8 -3 23.37 37.57 -17 -8 -4 -4.34 31 -17 -8 -4 -84.55 62.46 -17 -9 4 -15.74 25.66 -17 -9 4 110.02 64.29 -17 -9 3 17.27 27.25 -17 -9 3 -59.96 52.53 -17 -9 2 42.24 52.66 -17 -9 2 45.73 46.63 -17 -9 1 -41.36 38.45 -17 -9 1 -101.72 70.18 -17 -9 0 40.17 55.27 -17 -9 0 2.05 23.7 -17 -9 -1 15.5 28.69 -17 -9 -1 -69.95 57.02 -17 -9 -2 -67.2 68 -17 -9 -2 -18.81 50.12 -17 -9 -3 84.02 68.15 -17 -9 -3 34.03 49.74 -17 -9 -4 205.21 95.61 -17 -9 -4 172.05 85.86 -17 -10 2 2.7 30.42 -17 -10 2 50.14 52.8 -17 -10 1 65.05 59 -17 -10 1 53.77 52.08 -17 -10 0 43.91 39.49 -17 -10 0 41.81 46.91 -17 -10 -1 -43.73 51.33 -17 -10 -1 29.58 48.73 -17 -10 -2 -34.69 54.08 -17 -10 -2 124.9 77.73 -17 -10 -3 -16.87 43.06 -17 -10 -3 14.65 29.44 -17 -10 -4 32.23 48.46 -17 -10 -4 108.19 74.28 -17 -11 0 22.78 43.94 -17 -11 0 59.2 56.11 -17 -11 -1 39.68 55.33 -17 -11 -1 27.22 36.06 -17 -11 -2 134.53 78.61 -17 -11 -2 60.11 54.05 -17 -11 -3 2.46 26.66 -17 -11 -3 68.38 58.05 -17 -12 -2 84.19 61.97 -17 -12 -2 -5.95 24.36 -17 -12 -3 99.08 71 -17 -12 -3 -61.35 60.42 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -15.8062 -11.9834 -10.8487 -0.0093 -0.0146 0.9999 15.1322 -0.6699 8.3896 -0.5754 0.2718 -0.7714 15.8942 11.0181 11.1518 -0.0544 0.0233 -0.9982 3.2194 -16.6792 -1.5158 -0.8983 0.4276 0.1011 18.1720 0.4318 -2.1745 -0.2062 0.6988 -0.6849 -18.1720 -0.4318 2.1745 0.2062 -0.6988 0.6849 0.5691 -15.3489 -17.2741 -0.2444 0.8181 0.5206 -4.1855 0.0688 19.4507 -0.5906 -0.7703 -0.2404 4.1855 -0.0688 -19.4507 0.5906 0.7703 0.2404 -10.5794 1.0921 -13.9313 0.7113 0.0583 0.7005