#------------------------------------------------------------------------------ #$Date: 2017-11-28 05:43:10 +0200 (Tue, 28 Nov 2017) $ #$Revision: 203658 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/48/7044867.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_7044867 loop_ _publ_author_name 'Jia, Hongli' 'Li, Qi' 'Bayaguud, Aruuhan' 'Huang, Yichao' 'She, Shan' 'Chen, Kun' 'Wei, Yongge' _publ_section_title ; Diversified polyoxovanadate derivatives obtained by copper(I)-catalysed azide--alkyne cycloaddition reaction: Their synthesis and structural characterization ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C7DT03822D _journal_year 2017 _chemical_formula_moiety 'C16 H24 N6 O21 V6, 2(C16 H36 N)' _chemical_formula_sum 'C48 H96 N8 O21 V6' _chemical_formula_weight 1426.96 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2017-05-09 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335) ; _audit_update_record ; 2017-07-05 deposited with the CCDC. 2017-11-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.715(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.1864(7) _cell_length_b 15.7148(5) _cell_length_c 25.1531(8) _cell_measurement_reflns_used 8664 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 75.8910 _cell_measurement_theta_min 4.0710 _cell_volume 6731.9(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2137 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.970 _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 -42.00 33.00 1.00 4.68 -- -40.81 38.00 -60.00 75 2 \w -46.00 -12.00 1.00 4.68 -- -40.81 125.00 -90.00 34 3 \w -55.00 32.00 1.00 4.68 -- -40.81 57.00 60.00 87 4 \w 31.00 97.00 1.00 4.68 -- 40.81-125.00 120.00 66 5 \w 37.00 97.00 1.00 18.72 -- 112.00 -95.00 150.00 60 6 \w 65.00 121.00 1.00 18.72 -- 112.00-125.00 90.00 56 7 \w 59.00 118.00 1.00 18.72 -- 112.00 -30.00-150.00 59 8 \w 90.00 141.00 1.00 18.72 -- 112.00 -61.00-150.00 51 9 \w 87.00 178.00 1.00 18.72 -- 112.00 61.00 0.00 91 10 \w 96.00 133.00 1.00 18.72 -- 112.00 125.00-120.00 37 11 \w 97.00 171.00 1.00 18.72 -- 112.00 125.00-150.00 74 12 \w 40.00 79.00 1.00 18.72 -- 112.00 -61.00-150.00 39 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0758333000 _diffrn_orient_matrix_UB_12 0.0454676000 _diffrn_orient_matrix_UB_13 -0.0107493000 _diffrn_orient_matrix_UB_21 0.0474526000 _diffrn_orient_matrix_UB_22 -0.0526150000 _diffrn_orient_matrix_UB_23 0.0448155000 _diffrn_orient_matrix_UB_31 0.0136561000 _diffrn_orient_matrix_UB_32 -0.0690989000 _diffrn_orient_matrix_UB_33 -0.0411461000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_unetI/netI 0.0595 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 27976 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.970 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.915 _diffrn_reflns_theta_min 3.546 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 7.317 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.20209 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.408 _exptl_crystal_description irregular _exptl_crystal_F_000 2984 _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.35 _refine_diff_density_max 0.781 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.089 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 815 _refine_ls_number_reflns 13792 _refine_ls_number_restraints 108 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0781 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1378P)^2^+0.6711P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2203 _refine_ls_wR_factor_ref 0.2381 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10418 _reflns_number_total 13792 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; exp_465.res created by SHELXL-2014/7 TITL CELL 1.54184 17.18639 15.71477 25.15311 90 97.7154 90 ZERR 4 0.00067 0.00047 0.0008 0 0.0033 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O V UNIT 192 384 32 84 24 SADI C15 C16C C15 C16B C15 C16A SADI O20C C16C O20A C16B O20B C16A DELU C46 C48A C47B C48B C47A DELU C31 C32A C32B DELU C43 C44A C44B DELU C1 O21A O21B SIMU 0.04 0.08 1.7 C46 C48A C47B C48B C47A SIMU 0.04 0.08 1.7 C31 C32A C32B SIMU 0.04 0.08 1.7 C43 C44A C44B SIMU 0.04 0.08 1.7 C1 O21A O21B EADP C16C C16B C16A EADP C16C O20C EADP C16B O20A EADP C16A O20B L.S. 10 PLAN 120 bond $H fmap 2 acta REM REM REM WGHT 0.137800 0.671100 FVAR 1.40617 V2 5 0.162619 0.731364 0.677576 11.00000 0.05409 0.05183 = 0.03736 -0.00104 0.00236 -0.00110 V3 5 0.276850 0.725844 0.793735 11.00000 0.05289 0.04434 = 0.05456 -0.00284 -0.01299 -0.00423 V6 5 0.265909 0.581338 0.713508 11.00000 0.04265 0.04955 = 0.06279 -0.00877 -0.00104 -0.00338 V5 5 0.073760 0.577280 0.709424 11.00000 0.04309 0.05560 = 0.05660 -0.00700 -0.00083 -0.00708 V1 5 0.083949 0.723293 0.789520 11.00000 0.06023 0.05310 = 0.04894 -0.00131 0.01401 -0.00311 V4 5 0.187065 0.572423 0.826129 11.00000 0.08019 0.04587 = 0.04622 0.00059 -0.00260 -0.00584 O0AA 4 0.175170 0.652306 0.751497 11.00000 0.04531 0.04587 = 0.04279 -0.00341 0.00072 -0.00113 O4 4 0.239001 0.658928 0.661020 11.00000 0.06131 0.05687 = 0.04849 -0.00840 0.00728 -0.00870 O15 4 0.258738 0.513175 0.780884 11.00000 0.05715 0.04323 = 0.06361 -0.00484 -0.01202 -0.00421 O14 4 0.019891 0.649517 0.747338 11.00000 0.04999 0.06363 = 0.07619 -0.00073 0.01296 -0.00789 O18 4 0.103330 0.509201 0.777179 11.00000 0.06746 0.04959 = 0.05561 -0.00240 0.00514 -0.01138 O12 4 0.167835 0.516539 0.686688 11.00000 0.04989 0.04876 = 0.05171 -0.01078 -0.00498 -0.00663 O5 4 0.083126 0.656020 0.656997 11.00000 0.05575 0.05797 = 0.05268 -0.00268 -0.00836 -0.00669 O10 4 0.330921 0.653786 0.756212 11.00000 0.04379 0.04879 = 0.07612 -0.00705 -0.01377 -0.00605 O16 4 0.265585 0.648075 0.846864 11.00000 0.08714 0.04685 = 0.04715 -0.00276 -0.01806 -0.00402 O17 4 0.108587 0.645078 0.841990 11.00000 0.10493 0.05499 = 0.04534 0.00403 0.01973 -0.00365 O11 4 0.325530 0.519065 0.689470 11.00000 0.04964 0.05723 = 0.08870 -0.01576 0.00035 -0.00211 O13 4 0.006219 0.513855 0.681625 11.00000 0.05130 0.06346 = 0.08497 -0.00857 -0.00550 -0.01288 O2 4 0.247600 0.793275 0.726368 11.00000 0.04684 0.04559 = 0.04711 -0.00283 -0.00085 -0.00252 O6 4 0.154396 0.800549 0.630271 11.00000 0.07621 0.06390 = 0.04116 0.00100 0.00598 -0.00146 O8 4 0.182428 0.787268 0.817192 11.00000 0.07240 0.04413 = 0.03898 -0.00113 0.00189 -0.00193 O7 4 0.022589 0.784571 0.813475 11.00000 0.08285 0.06148 = 0.06805 -0.00081 0.03045 0.00179 O9 4 0.341827 0.790916 0.821854 11.00000 0.06671 0.05208 = 0.07342 -0.00644 -0.02300 -0.00667 O19 4 0.194092 0.504782 0.874320 11.00000 0.12430 0.05017 = 0.05423 0.00478 -0.00077 -0.00048 O3 4 0.091306 0.792301 0.722834 11.00000 0.04816 0.05129 = 0.04425 0.00101 0.00522 -0.00008 C7 1 0.181001 0.878162 0.815575 11.00000 0.08247 0.04547 = 0.04456 -0.00214 0.00540 0.00018 AFIX 23 H7A 2 0.228707 0.900000 0.836004 11.00000 -1.20000 H7B 2 0.136898 0.898508 0.832360 11.00000 -1.20000 AFIX 0 C9 1 0.169182 0.425334 0.688293 11.00000 0.05786 0.04990 = 0.06533 -0.01395 -0.00288 -0.00620 AFIX 23 H9A 2 0.211923 0.404865 0.670165 11.00000 -1.20000 H9B 2 0.120485 0.403585 0.669151 11.00000 -1.20000 AFIX 0 C0AA 1 0.243345 0.883771 0.730563 11.00000 0.05873 0.04667 = 0.04837 0.00115 0.00302 -0.00474 AFIX 23 H0AA 2 0.238744 0.908416 0.694922 11.00000 -1.20000 H0AB 2 0.291586 0.904714 0.750771 11.00000 -1.20000 AFIX 0 C11 1 0.256630 0.421812 0.777185 11.00000 0.06592 0.04605 = 0.07179 -0.00670 -0.00940 -0.00305 AFIX 23 H11A 2 0.262367 0.397616 0.812975 11.00000 -1.20000 H11B 2 0.300235 0.402176 0.759622 11.00000 -1.20000 AFIX 0 C6 1 0.097215 0.883393 0.726710 11.00000 0.05994 0.05084 = 0.05021 0.00542 0.01055 0.00570 AFIX 23 H6A 2 0.054112 0.904921 0.744076 11.00000 -1.20000 H6B 2 0.092249 0.907333 0.690868 11.00000 -1.20000 AFIX 0 C5 1 0.174054 0.912535 0.757934 11.00000 0.06298 0.05227 = 0.04377 -0.00027 0.00503 0.00211 C12 1 0.179500 0.391297 0.745591 11.00000 0.06456 0.04433 = 0.06979 -0.00846 -0.00715 -0.00847 C10 1 0.110462 0.418237 0.773422 11.00000 0.07686 0.05318 = 0.06426 -0.00283 0.00232 -0.01242 AFIX 23 H10A 2 0.062522 0.395435 0.753838 11.00000 -1.20000 H10B 2 0.116550 0.394142 0.809245 11.00000 -1.20000 AFIX 0 N3 3 0.167974 1.056552 0.714046 11.00000 0.06529 0.04659 = 0.05437 0.00244 0.01052 0.00388 N2 3 0.233571 1.080358 0.693694 11.00000 0.06656 0.06146 = 0.07519 0.00882 0.01101 -0.00076 N7 3 0.215982 0.807126 0.987418 11.00000 0.07917 0.06790 = 0.03893 0.00180 0.00414 0.00697 N4 3 0.189239 0.245991 0.789315 11.00000 0.12560 0.04465 = 0.08926 -0.00588 -0.02054 -0.00918 PART 1 O20B 4 0.132341 0.042494 0.892815 10.50000 0.13964 0.04735 = 0.05987 0.00980 -0.02339 -0.02023 AFIX 143 H20B 2 0.160769 0.024994 0.871490 10.50000 -1.50000 AFIX 0 PART 0 C4 1 0.174600 1.009467 0.764256 11.00000 0.08137 0.05049 = 0.04864 -0.00071 0.00589 0.00193 AFIX 23 H4A 2 0.131436 1.025733 0.783312 11.00000 -1.20000 H4B 2 0.222978 1.026038 0.786216 11.00000 -1.20000 AFIX 0 C20 1 0.201536 0.724032 1.015174 11.00000 0.10137 0.07403 = 0.04497 0.01030 0.00975 0.01359 AFIX 23 H20D 2 0.246119 0.712779 1.042209 11.00000 -1.20000 H20E 2 0.155791 0.730887 1.033549 11.00000 -1.20000 AFIX 0 C29 1 0.237175 0.873954 1.030980 11.00000 0.08398 0.08228 = 0.04749 -0.00901 -0.00483 0.00523 AFIX 23 H29A 2 0.195887 0.875207 1.053745 11.00000 -1.20000 H29B 2 0.285052 0.856153 1.053052 11.00000 -1.20000 AFIX 0 C14 1 0.132199 0.219256 0.817060 11.00000 0.14693 0.05607 = 0.07707 -0.00680 -0.00972 -0.03415 AFIX 43 H14 2 0.078316 0.227258 0.808797 11.00000 -1.20000 AFIX 0 C13 1 0.179359 0.292982 0.739360 11.00000 0.08252 0.05070 = 0.07807 -0.00911 -0.00656 -0.01081 AFIX 23 H13A 2 0.130115 0.275967 0.718642 11.00000 -1.20000 H13B 2 0.221230 0.277108 0.719012 11.00000 -1.20000 AFIX 0 C30 1 0.248843 0.962637 1.011469 11.00000 0.12139 0.07398 = 0.07265 -0.01039 0.00315 -0.00855 AFIX 23 H30A 2 0.198716 0.985749 0.995614 11.00000 -1.20000 H30B 2 0.283294 0.961123 0.983935 11.00000 -1.20000 AFIX 0 C39 1 0.607930 0.312832 0.860154 11.00000 0.06724 0.06551 = 0.07209 0.00329 -0.00060 0.01227 AFIX 23 H39A 2 0.662406 0.313393 0.853902 11.00000 -1.20000 H39B 2 0.606054 0.331465 0.896725 11.00000 -1.20000 AFIX 0 C40 1 0.576916 0.223689 0.853717 11.00000 0.08262 0.07052 = 0.08117 0.00167 -0.00853 0.01228 AFIX 137 H40A 2 0.581198 0.203852 0.818128 11.00000 -1.50000 H40B 2 0.522821 0.222885 0.859471 11.00000 -1.50000 H40C 2 0.606879 0.187272 0.879431 11.00000 -1.50000 AFIX 0 C38 1 0.561581 0.374535 0.821884 11.00000 0.07026 0.06445 = 0.08945 -0.00517 -0.02885 0.01398 AFIX 23 H38A 2 0.567856 0.359286 0.785333 11.00000 -1.20000 H38B 2 0.506290 0.369798 0.825583 11.00000 -1.20000 AFIX 0 C37 1 0.587609 0.465329 0.832160 11.00000 0.05805 0.06216 = 0.08903 -0.00299 -0.02338 0.01131 AFIX 23 H37A 2 0.634418 0.474835 0.815302 11.00000 -1.20000 H37B 2 0.602028 0.472792 0.870498 11.00000 -1.20000 AFIX 0 N6 3 0.251297 0.181494 0.856628 11.00000 0.18397 0.06750 = 0.13683 0.00174 -0.05529 0.02098 PART 2 C16B 1 0.123838 0.133580 0.900776 10.30000 0.15417 0.09865 = 0.07976 0.01123 -0.04377 0.02008 AFIX 23 H16A 2 0.135227 0.159522 0.935953 10.30000 -1.20000 H16B 2 0.068096 0.139341 0.888607 10.30000 -1.20000 AFIX 0 PART 0 C18 1 0.168916 0.569873 1.010647 11.00000 0.15941 0.07579 = 0.10097 0.00759 0.00993 -0.01941 AFIX 23 H18A 2 0.121901 0.581806 1.026785 11.00000 -1.20000 H18B 2 0.157119 0.522918 0.985842 11.00000 -1.20000 AFIX 0 C17 1 0.230521 0.543651 1.052460 11.00000 0.28034 0.08097 = 0.09582 0.01398 -0.00946 0.00340 AFIX 137 H17A 2 0.276543 0.528623 1.036743 11.00000 -1.50000 H17B 2 0.213130 0.495330 1.071029 11.00000 -1.50000 H17C 2 0.242722 0.589619 1.077319 11.00000 -1.50000 AFIX 0 N1 3 0.209077 1.123202 0.649187 11.00000 0.08783 0.06006 = 0.06895 0.01462 0.01782 0.00654 C3 1 0.103231 1.083920 0.683198 11.00000 0.06566 0.05887 = 0.06114 0.00623 0.00917 0.02254 AFIX 43 H3 2 0.051287 1.076001 0.688710 11.00000 -1.20000 AFIX 0 C2 1 0.129949 1.125481 0.642395 11.00000 0.09340 0.05557 = 0.06028 0.00358 0.01070 0.02541 C1 1 0.082461 1.173369 0.597177 11.00000 0.11678 0.09186 = 0.07379 0.02129 0.01212 0.03740 PART 1 AFIX 23 H1AA 2 0.076421 1.231997 0.607970 10.80000 -1.20000 H1AB 2 0.110443 1.173390 0.566155 10.80000 -1.20000 AFIX 23 PART 0 PART 2 H1BC 2 0.030381 1.183031 0.606797 10.20000 -1.20000 H1BD 2 0.106589 1.228622 0.594041 10.20000 -1.20000 AFIX 0 PART 0 N0AA 3 0.527408 0.533002 0.812198 11.00000 0.05038 0.05639 = 0.08812 -0.00718 -0.02045 0.00603 C28 1 0.143295 0.834272 0.949622 11.00000 0.07644 0.06416 = 0.04125 -0.00057 -0.00176 0.00272 AFIX 23 H28A 2 0.154398 0.888121 0.933355 11.00000 -1.20000 H28B 2 0.133740 0.792581 0.921053 11.00000 -1.20000 AFIX 0 C8 1 0.568300 0.618555 0.824395 11.00000 0.06457 0.06619 = 0.10539 -0.01028 -0.02826 0.00299 AFIX 23 H8A 2 0.586990 0.621343 0.862496 11.00000 -1.20000 H8B 2 0.613770 0.621369 0.805410 11.00000 -1.20000 AFIX 0 C27 1 0.069213 0.844055 0.975183 11.00000 0.08197 0.06905 = 0.05473 -0.00159 0.01303 -0.00210 AFIX 23 H27A 2 0.049829 0.788348 0.983583 11.00000 -1.20000 H27B 2 0.080623 0.875720 1.008418 11.00000 -1.20000 AFIX 0 C36 1 0.500633 0.523537 0.752440 11.00000 0.06102 0.05860 = 0.08371 0.00376 -0.02366 0.00291 AFIX 23 H36A 2 0.459141 0.564467 0.741999 11.00000 -1.20000 H36B 2 0.478371 0.467177 0.745916 11.00000 -1.20000 AFIX 0 C21 1 0.282625 0.797807 0.953335 11.00000 0.07685 0.08346 = 0.04820 0.00506 0.00386 0.00329 AFIX 23 H21C 2 0.268052 0.754786 0.926165 11.00000 -1.20000 H21D 2 0.288682 0.851228 0.935011 11.00000 -1.20000 AFIX 0 C41 1 0.453734 0.525423 0.839160 11.00000 0.06136 0.07185 = 0.10038 -0.00141 -0.02014 0.01644 AFIX 23 H41A 2 0.418681 0.571836 0.826833 11.00000 -1.20000 H41B 2 0.427343 0.472713 0.827607 11.00000 -1.20000 AFIX 0 C26 1 0.007205 0.890185 0.937789 11.00000 0.08005 0.07596 = 0.06867 -0.01614 0.00202 0.00460 AFIX 23 H26A 2 -0.002989 0.858519 0.904480 11.00000 -1.20000 H26B 2 0.027345 0.945607 0.929523 11.00000 -1.20000 AFIX 0 C25 1 -0.069222 0.902096 0.960334 11.00000 0.08041 0.11884 = 0.09698 -0.03987 0.00503 0.00779 AFIX 137 H25A 2 -0.105260 0.933518 0.935214 11.00000 -1.50000 H25B 2 -0.059673 0.932871 0.993539 11.00000 -1.50000 H25C 2 -0.091302 0.847469 0.966577 11.00000 -1.50000 AFIX 0 C22 1 0.360577 0.773768 0.984602 11.00000 0.08281 0.14866 = 0.06295 0.00433 -0.00053 0.02639 AFIX 23 H22A 2 0.373824 0.814468 1.013388 11.00000 -1.20000 H22B 2 0.356019 0.718195 1.000682 11.00000 -1.20000 AFIX 0 C42 1 0.467387 0.526792 0.899753 11.00000 0.08146 0.12635 = 0.09708 0.00574 -0.01321 0.03629 AFIX 23 H42A 2 0.503940 0.481936 0.912554 11.00000 -1.20000 H42B 2 0.490810 0.580759 0.911844 11.00000 -1.20000 AFIX 0 C35 1 0.564512 0.536008 0.716697 11.00000 0.06485 0.10787 = 0.09427 0.01351 -0.01634 0.01259 AFIX 23 H35A 2 0.582084 0.594723 0.718424 11.00000 -1.20000 H35B 2 0.609133 0.499880 0.728848 11.00000 -1.20000 AFIX 0 C31 1 0.284208 1.019851 1.056967 11.00000 0.11099 0.10552 = 0.13686 -0.04306 -0.03210 0.00561 PART 1 AFIX 23 H31A 2 0.248868 1.020149 1.083966 10.60000 -1.20000 H31B 2 0.332987 0.994103 1.073172 10.60000 -1.20000 AFIX 23 PART 0 PART 2 H31C 2 0.276560 0.996909 1.091690 10.40000 -1.20000 H31D 2 0.262862 1.077015 1.053350 10.40000 -1.20000 AFIX 0 PART 0 PART 1 C32A 1 0.300658 1.107961 1.044355 10.60000 0.17634 0.10191 = 0.17818 -0.04587 -0.05486 -0.03489 AFIX 137 H32A 2 0.339508 1.109517 1.020282 10.60000 -1.50000 H32B 2 0.319952 1.137740 1.076782 10.60000 -1.50000 H32C 2 0.253356 1.134694 1.027689 10.60000 -1.50000 AFIX 0 PART 0 C46 1 0.516807 0.695257 0.809068 11.00000 0.09024 0.05858 = 0.13698 -0.00457 -0.03012 0.00079 PART 1 AFIX 23 H46A 2 0.484974 0.708199 0.837087 10.50000 -1.20000 H46B 2 0.482248 0.684499 0.775990 10.50000 -1.20000 AFIX 23 PART 0 PART 2 H46C 2 0.509241 0.700617 0.770298 10.50000 -1.20000 H46D 2 0.465731 0.685435 0.820305 10.50000 -1.20000 AFIX 0 PART 0 C23 1 0.425662 0.771549 0.950129 11.00000 0.08378 0.19431 = 0.07737 0.01734 0.00614 0.04183 AFIX 23 H23A 2 0.428641 0.826223 0.932617 11.00000 -1.20000 H23B 2 0.413880 0.728696 0.922463 11.00000 -1.20000 AFIX 0 PART 2 C48A 1 0.616465 0.796802 0.803072 10.50000 0.09591 0.07057 = 0.11543 0.00488 0.02992 -0.00322 AFIX 137 H48A 2 0.600395 0.792068 0.765135 10.50000 -1.50000 H48B 2 0.658676 0.757789 0.813708 10.50000 -1.50000 H48C 2 0.633850 0.853850 0.811580 10.50000 -1.50000 AFIX 0 PART 0 C43 1 0.391974 0.514634 0.923245 11.00000 0.10998 0.20655 = 0.13261 0.05231 0.03056 0.06175 PART 1 AFIX 23 H43A 2 0.357184 0.561375 0.911136 10.50000 -1.20000 H43B 2 0.367370 0.462820 0.908269 10.50000 -1.20000 AFIX 23 PART 0 PART 2 H43C 2 0.349122 0.542086 0.900574 10.50000 -1.20000 H43D 2 0.396498 0.540512 0.958536 10.50000 -1.20000 AFIX 0 PART 0 C24 1 0.504048 0.751781 0.982555 11.00000 0.09718 0.30195 = 0.11727 0.01872 0.00794 0.02881 AFIX 137 H24A 2 0.543259 0.746386 0.958941 11.00000 -1.50000 H24B 2 0.500383 0.699394 1.001695 11.00000 -1.50000 H24C 2 0.518321 0.796997 1.007639 11.00000 -1.50000 AFIX 0 PART 1 C44A 1 0.396732 0.509665 0.979824 10.50000 0.12568 0.23174 = 0.12461 0.04515 0.02466 0.05686 AFIX 133 H44A 2 0.362278 0.465710 0.989246 10.50000 -1.50000 H44B 2 0.381445 0.563191 0.993627 10.50000 -1.50000 H44C 2 0.449698 0.496726 0.994940 10.50000 -1.50000 AFIX 0 PART 0 C34 1 0.531444 0.513309 0.659491 11.00000 0.10593 0.08661 = 0.09742 -0.00552 -0.00854 0.00734 AFIX 23 H34A 2 0.514292 0.454455 0.658411 11.00000 -1.20000 H34B 2 0.485795 0.548522 0.648387 11.00000 -1.20000 AFIX 0 PART 1 O21A 4 0.004789 1.135367 0.582438 10.80000 0.09930 0.16660 = 0.07007 0.00112 0.00352 0.03619 AFIX 143 H21A 2 0.000915 1.117717 0.551516 10.80000 -1.50000 AFIX 0 PART 0 C33 1 0.589870 0.525090 0.620214 11.00000 0.11423 0.19932 = 0.10977 0.01442 0.01398 0.01322 AFIX 137 H33A 2 0.565394 0.511123 0.584714 11.00000 -1.50000 H33B 2 0.634160 0.488407 0.629947 11.00000 -1.50000 H33C 2 0.607162 0.583220 0.621037 11.00000 -1.50000 AFIX 0 C19 1 0.188903 0.648171 0.979043 11.00000 0.10528 0.07433 = 0.06722 0.00432 -0.00092 -0.00154 AFIX 23 H19A 2 0.236052 0.637248 0.962839 11.00000 -1.20000 H19B 2 0.146383 0.659637 0.950505 11.00000 -1.20000 AFIX 0 N5 3 0.261597 0.224165 0.812676 11.00000 0.14192 0.07255 = 0.13808 0.00611 -0.04468 0.01970 C15 1 0.172180 0.177062 0.860773 11.00000 0.22644 0.05004 = 0.07919 0.00158 -0.03206 -0.02661 PART 2 C44B 1 0.374837 0.419105 0.927520 10.50000 0.21244 0.24488 = 0.19094 0.13912 -0.02964 0.02001 AFIX 33 H44D 2 0.326791 0.411426 0.942487 10.50000 -1.50000 H44E 2 0.369879 0.393884 0.892466 10.50000 -1.50000 H44F 2 0.417132 0.392314 0.950278 10.50000 -1.50000 AFIX 0 C32B 1 0.370142 1.017652 1.048443 10.40000 0.10819 0.14795 = 0.18330 -0.04116 -0.03175 0.00246 AFIX 33 H32D 2 0.400392 1.052124 1.075162 10.40000 -1.50000 H32E 2 0.388915 0.960082 1.051365 10.40000 -1.50000 H32F 2 0.375358 1.039361 1.013422 10.40000 -1.50000 AFIX 0 PART 0 PART 1 C47B 1 0.576946 0.775428 0.801160 10.50000 0.08371 0.05959 = 0.13042 0.00199 0.00990 -0.00063 AFIX 23 H47A 2 0.610555 0.759936 0.774652 10.50000 -1.20000 H47B 2 0.546344 0.824688 0.787831 10.50000 -1.20000 AFIX 0 C48B 1 0.624996 0.797272 0.850791 10.50000 0.13085 0.09307 = 0.11484 -0.00964 0.02811 -0.03582 AFIX 137 H48D 2 0.651114 0.850368 0.846590 10.50000 -1.50000 H48E 2 0.663384 0.753477 0.860007 10.50000 -1.50000 H48F 2 0.592462 0.802506 0.878803 10.50000 -1.50000 AFIX 0 PART 0 PART 2 O21B 4 0.075011 1.136304 0.549909 10.20000 0.14150 0.13757 = 0.07144 0.00949 -0.00346 0.04902 AFIX 147 H21B 2 0.101410 1.161906 0.530252 10.20000 -1.50000 AFIX 0 C47A 1 0.548361 0.775987 0.832477 10.50000 0.05942 0.06451 = 0.09700 -0.01428 0.00956 0.00010 AFIX 23 H47C 2 0.565630 0.769610 0.870593 10.50000 -1.20000 H47D 2 0.508913 0.820441 0.827305 10.50000 -1.20000 AFIX 0 PART 0 PART 1 C16A 1 0.155404 0.126433 0.909209 10.50000 0.13964 0.04735 = 0.05987 0.00980 -0.02339 -0.02023 AFIX 23 H16C 2 0.202030 0.124330 0.935595 10.50000 -1.20000 H16D 2 0.113823 0.153656 0.925526 10.50000 -1.20000 AFIX 0 PART 0 PART 2 O20A 4 0.145699 0.046182 0.903161 10.30000 0.15417 0.09865 = 0.07976 0.01123 -0.04377 0.02008 AFIX 143 H20A 2 0.119076 0.020097 0.878987 10.30000 -1.50000 AFIX 0 PART 0 PART 3 O20C 4 0.040689 0.172446 0.916096 10.20000 0.15417 0.09865 = 0.07976 0.01123 -0.04377 0.02008 AFIX 147 H20C 2 0.004871 0.156669 0.893382 10.20000 -1.50000 AFIX 0 C16C 1 0.115173 0.146751 0.900312 10.20000 0.15417 0.09865 = 0.07976 0.01123 -0.04377 0.02008 AFIX 23 H16E 2 0.105809 0.087750 0.890062 10.20000 -1.20000 H16F 2 0.149164 0.144477 0.934341 10.20000 -1.20000 AFIX 0 HKLF 4 REM REM R1 = 0.0781 for 10418 Fo > 4sig(Fo) and 0.0921 for all 13792 data REM 815 parameters refined using 108 restraints END WGHT 0.1372 0.7174 REM Highest difference peak 0.781, deepest hole -1.067, 1-sigma level 0.089 Q1 1 0.2990 0.7255 0.7583 11.00000 0.05 0.78 Q2 1 0.2025 0.7230 0.7404 11.00000 0.05 0.70 Q3 1 0.1876 0.7351 0.6404 11.00000 0.05 0.65 Q4 1 0.0523 0.5834 0.7447 11.00000 0.05 0.65 Q5 1 0.1297 0.5766 0.7691 11.00000 0.05 0.64 Q6 1 0.2910 0.5799 0.6779 11.00000 0.05 0.62 Q7 1 0.1307 0.7289 0.7181 11.00000 0.05 0.58 Q8 1 0.0538 0.7228 0.7281 11.00000 0.05 0.57 Q9 1 0.1129 0.6757 0.8047 11.00000 0.05 0.56 Q10 1 0.2167 0.5764 0.7895 11.00000 0.05 0.55 Q11 1 0.1430 0.7852 0.6646 11.00000 0.05 0.55 Q12 1 0.0574 0.7312 0.8276 11.00000 0.05 0.55 Q13 1 0.2915 0.5331 0.7298 11.00000 0.05 0.52 Q14 1 0.1947 0.8023 0.6823 11.00000 0.05 0.52 Q15 1 0.1261 0.8022 0.6767 11.00000 0.05 0.51 Q16 1 0.4070 0.3179 0.8839 11.00000 0.05 0.51 Q17 1 0.3001 0.6728 0.8087 11.00000 0.05 0.51 Q18 1 0.0968 0.5863 0.6752 11.00000 0.05 0.51 Q19 1 0.2965 0.5778 0.7755 11.00000 0.05 0.51 Q20 1 0.1649 0.5676 0.8633 11.00000 0.05 0.49 Q21 1 0.2129 0.5205 0.8399 11.00000 0.05 0.49 Q22 1 0.2997 0.5183 0.7200 11.00000 0.05 0.48 Q23 1 0.2393 0.6392 0.7020 11.00000 0.05 0.47 Q24 1 0.3658 0.3150 0.9070 11.00000 0.05 0.47 Q25 1 0.1860 0.7835 0.6887 11.00000 0.05 0.47 Q26 1 0.1100 0.7323 0.7479 11.00000 0.05 0.47 Q27 1 0.0502 0.5781 0.6457 11.00000 0.05 0.46 Q28 1 0.2402 0.5731 0.7514 11.00000 0.05 0.46 Q29 1 0.0524 0.6415 0.6967 11.00000 0.05 0.46 Q30 1 0.2261 0.5019 0.8241 11.00000 0.05 0.46 Q31 1 0.0555 0.7859 0.7781 11.00000 0.05 0.44 Q32 1 0.1953 0.6802 0.6916 11.00000 0.05 0.44 Q33 1 0.0675 0.6257 0.6902 11.00000 0.05 0.43 Q34 1 0.2340 0.5177 0.7083 11.00000 0.05 0.43 Q35 1 0.2573 0.7780 0.7831 11.00000 0.05 0.43 Q36 1 0.0458 0.6532 0.7108 11.00000 0.05 0.42 Q37 1 0.2203 0.5633 0.8882 11.00000 0.05 0.42 Q38 1 0.1688 0.6257 0.8102 11.00000 0.05 0.41 Q39 1 0.4465 0.8549 0.9543 11.00000 0.05 0.40 Q40 1 0.2942 0.6446 0.7207 11.00000 0.05 0.40 Q41 1 0.1532 0.6387 0.8191 11.00000 0.05 0.39 Q42 1 0.2495 0.7155 0.8347 11.00000 0.05 0.39 Q43 1 0.0958 0.7177 0.8538 11.00000 0.05 0.39 Q44 1 0.1206 0.7050 0.8506 11.00000 0.05 0.38 Q45 1 0.1249 0.7352 0.6166 11.00000 0.05 0.38 Q46 1 0.1005 1.2178 0.4797 11.00000 0.05 0.37 Q47 1 0.3324 0.6760 0.7368 11.00000 0.05 0.36 Q48 1 0.0400 0.5077 0.7016 11.00000 0.05 0.36 Q49 1 0.1064 1.1925 0.4883 11.00000 0.05 0.36 Q50 1 0.1005 0.6390 0.7183 11.00000 0.05 0.34 Q51 1 0.2999 0.7234 0.8552 11.00000 0.05 0.34 Q52 1 0.0295 0.4779 0.6893 11.00000 0.05 0.34 Q53 1 0.1937 0.9043 0.7703 11.00000 0.05 0.34 Q54 1 0.2754 0.7275 0.7217 11.00000 0.05 0.33 Q55 1 0.2483 0.6603 0.7835 11.00000 0.05 0.33 Q56 1 0.3089 0.8024 0.7929 11.00000 0.05 0.32 Q57 1 0.0816 0.5625 1.0430 11.00000 0.05 0.32 Q58 1 0.1034 0.5225 0.7222 11.00000 0.05 0.31 Q59 1 0.1114 0.5051 0.7131 11.00000 0.05 0.31 Q60 1 0.2023 0.7812 0.8085 11.00000 0.05 0.31 Q61 1 0.1762 0.8209 0.8041 11.00000 0.05 0.31 Q62 1 0.2245 0.5985 0.6522 11.00000 0.05 0.30 Q63 1 0.0974 0.7632 0.8025 11.00000 0.05 0.30 Q64 1 0.1484 0.4984 0.8253 11.00000 0.05 0.29 Q65 1 0.2660 0.7982 0.6989 11.00000 0.05 0.29 Q66 1 0.2122 0.6241 0.8394 11.00000 0.05 0.28 Q67 1 0.1210 0.7958 0.7817 11.00000 0.05 0.28 Q68 1 0.1633 0.9105 0.7889 11.00000 0.05 0.28 Q69 1 0.2047 0.5809 0.6564 11.00000 0.05 0.28 Q70 1 -0.0006 0.7864 0.8420 11.00000 0.05 0.28 Q71 1 0.4283 0.2995 0.9329 11.00000 0.05 0.28 Q72 1 0.1353 0.6773 0.6633 11.00000 0.05 0.27 Q73 1 0.2471 0.6629 0.6359 11.00000 0.05 0.27 Q74 1 0.1127 0.6837 0.6196 11.00000 0.05 0.27 Q75 1 0.1835 0.4764 0.6993 11.00000 0.05 0.27 Q76 1 0.0974 0.6426 0.8665 11.00000 0.05 0.26 Q77 1 0.1189 0.5876 0.6378 11.00000 0.05 0.26 Q78 1 0.1024 0.8170 0.7270 11.00000 0.05 0.26 Q79 1 0.3093 0.8418 0.8115 11.00000 0.05 0.26 Q80 1 0.3464 0.5223 0.6597 11.00000 0.05 0.26 Q81 1 0.3124 0.3420 0.9301 11.00000 0.05 0.26 Q82 1 0.1623 0.5176 0.8125 11.00000 0.05 0.26 Q83 1 0.1106 0.5488 1.0324 11.00000 0.05 0.25 Q84 1 0.1953 0.8350 0.8227 11.00000 0.05 0.25 Q85 1 -0.0407 0.5781 0.7491 11.00000 0.05 0.25 Q86 1 0.0701 0.5210 0.8100 11.00000 0.05 0.24 Q87 1 0.2525 0.7159 0.6682 11.00000 0.05 0.24 Q88 1 0.0855 0.5650 0.9512 11.00000 0.05 0.24 Q89 1 0.1411 1.2342 0.5877 11.00000 0.05 0.24 Q90 1 -0.0202 0.7284 0.7390 11.00000 0.05 0.24 Q91 1 -0.0088 1.0356 0.5807 11.00000 0.05 0.23 Q92 1 0.1371 0.5228 0.7024 11.00000 0.05 0.23 Q93 1 0.1792 0.4977 1.0088 11.00000 0.05 0.23 Q94 1 0.2262 0.1078 0.9139 11.00000 0.05 0.22 Q95 1 0.1552 0.9549 0.7540 11.00000 0.05 0.22 Q96 1 0.1535 0.4831 0.6726 11.00000 0.05 0.22 Q97 1 0.0231 0.2316 0.8214 11.00000 0.05 0.21 Q98 1 0.3691 0.5780 0.7612 11.00000 0.05 0.21 Q99 1 0.1762 0.7960 0.6013 11.00000 0.05 0.21 Q100 1 0.1818 0.9889 1.1028 11.00000 0.05 0.21 Q101 1 0.3755 0.7343 0.8425 11.00000 0.05 0.21 Q102 1 0.2326 0.9224 0.7092 11.00000 0.05 0.21 Q103 1 0.0527 0.6567 0.7765 11.00000 0.05 0.21 Q104 1 0.1282 0.4701 0.7889 11.00000 0.05 0.21 Q105 1 0.0973 0.8542 1.0831 11.00000 0.05 0.21 Q106 1 0.2248 0.8322 0.7075 11.00000 0.05 0.21 Q107 1 0.2020 0.7765 0.8803 11.00000 0.05 0.21 Q108 1 0.1484 1.0537 0.7499 11.00000 0.05 0.21 Q109 1 0.1556 0.9110 1.1065 11.00000 0.05 0.20 Q110 1 0.1777 0.1166 0.8827 11.00000 0.05 0.20 Q111 1 0.2704 0.4677 0.7892 11.00000 0.05 0.20 Q112 1 0.2620 0.0777 0.8952 11.00000 0.05 0.20 Q113 1 0.3701 0.5159 0.7422 11.00000 0.05 0.20 Q114 1 0.5642 0.4179 0.8334 11.00000 0.05 0.20 Q115 1 0.0712 0.0415 0.8737 11.00000 0.05 0.20 Q116 1 0.1299 1.0774 0.6514 11.00000 0.05 0.20 Q117 1 0.1628 0.4663 0.6796 11.00000 0.05 0.19 Q118 1 0.0095 1.0674 0.6938 11.00000 0.05 0.19 Q119 1 0.4687 0.5943 0.7617 11.00000 0.05 0.19 Q120 1 0.1334 0.6454 0.9803 11.00000 0.05 0.19 REM The information below was added by Olex2. REM REM R1 = 0.0781 for 10418 Fo > 4sig(Fo) and 0.0921 for all 27976 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.78, deepest hole -1.07 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0921 REM R1_gt = 0.0781 REM wR_ref = 0.2381 REM GOOF = 1.062 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 27976 REM Reflections_gt = 10418 REM Parameters = n/a REM Hole = -1.07 REM Peak = 0.78 REM Flack = n/a ; _cod_data_source_file c7dt03822d2.cif _cod_data_source_block exp_465 _cod_database_code 7044867 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula V6CHON _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 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances C15-C16C \\sim C15-C16B \\sim C15-C16A with sigma of 0.02 O20C-C16C \\sim O20A-C16B \\sim O20B-C16A with sigma of 0.02 3. Rigid bond restraints C46, C48A, C47B, C48B, C47A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C31, C32A, C32B with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C43, C44A, C44B with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C1, O21A, O21B with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints C46 \\sim C48A \\sim C47B \\sim C48B \\sim C47A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C31 \\sim C32A \\sim C32B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C43 \\sim C44A \\sim C44B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C1 \\sim O21A \\sim O21B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C16C) = Uanis(C16B) = Uanis(C16A) Uanis(C16C) = Uanis(O20C) Uanis(C16B) = Uanis(O20A) Uanis(C16A) = Uanis(O20B) 5. Others Fixed Sof: O20B(0.5) H20B(0.5) C16B(0.3) H16A(0.3) H16B(0.3) H1AA(0.8) H1AB(0.8) H1BC(0.2) H1BD(0.2) H31A(0.6) H31B(0.6) H31C(0.4) H31D(0.4) C32A(0.6) H32A(0.6) H32B(0.6) H32C(0.6) H46A(0.5) H46B(0.5) H46C(0.5) H46D(0.5) C48A(0.5) H48A(0.5) H48B(0.5) H48C(0.5) H43A(0.5) H43B(0.5) H43C(0.5) H43D(0.5) C44A(0.5) H44A(0.5) H44B(0.5) H44C(0.5) O21A(0.8) H21A(0.8) C44B(0.5) H44D(0.5) H44E(0.5) H44F(0.5) C32B(0.4) H32D(0.4) H32E(0.4) H32F(0.4) C47B(0.5) H47A(0.5) H47B(0.5) C48B(0.5) H48D(0.5) H48E(0.5) H48F(0.5) O21B(0.2) H21B(0.2) C47A(0.5) H47C(0.5) H47D(0.5) C16A(0.5) H16C(0.5) H16D(0.5) O20A(0.3) H20A(0.3) O20C(0.2) H20C(0.2) C16C(0.2) H16E(0.2) H16F(0.2) 6.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C9(H9A,H9B), C0AA(H0AA,H0AB), C11(H11A,H11B), C6(H6A,H6B), C10(H10A,H10B), C4(H4A,H4B), C20(H20D,H20E), C29(H29A,H29B), C13(H13A,H13B), C30(H30A,H30B), C39(H39A,H39B), C38(H38A,H38B), C37(H37A,H37B), C16B(H16A, H16B), C18(H18A,H18B), C1(H1AA,H1AB), C1(H1BC,H1BD), C28(H28A,H28B), C8(H8A, H8B), C27(H27A,H27B), C36(H36A,H36B), C21(H21C,H21D), C41(H41A,H41B), C26(H26A, H26B), C22(H22A,H22B), C42(H42A,H42B), C35(H35A,H35B), C31(H31A,H31B), C31(H31C,H31D), C46(H46A,H46B), C46(H46C,H46D), C23(H23A,H23B), C43(H43A,H43B), C43(H43C,H43D), C34(H34A,H34B), C19(H19A,H19B), C47B(H47A,H47B), C47A(H47C, H47D), C16A(H16C,H16D), C16C(H16E,H16F) 6.b Me refined with riding coordinates: C44B(H44D,H44E,H44F), C32B(H32D,H32E,H32F) 6.c Aromatic/amide H refined with riding coordinates: C14(H14), C3(H3) 6.d Idealised Me refined with riding coordinates: C44A(H44A,H44B,H44C) 6.e Idealised Me refined as rotating group: C40(H40A,H40B,H40C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C32A(H32A,H32B, H32C), C48A(H48A,H48B,H48C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C), C48B(H48D,H48E,H48F) 6.f Idealised tetrahedral OH refined with riding coordinates: O20B(H20B), O21A(H21A), O20A(H20A) 6.g Idealised tetrahedral OH refined as rotating group: O21B(H21B), O20C(H20C) ; _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 2.064 _oxdiff_exptl_absorpt_empirical_full_min 0.462 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 V2 V 0.16262(4) 0.73136(4) 0.67758(2) 0.04810(18) Uani 1 1 d . . . . . V3 V 0.27685(4) 0.72584(4) 0.79374(3) 0.05244(19) Uani 1 1 d . . . . . V6 V 0.26591(4) 0.58134(5) 0.71351(3) 0.05240(19) Uani 1 1 d . . . . . V5 V 0.07376(4) 0.57728(5) 0.70942(3) 0.05245(19) Uani 1 1 d . . . . . V1 V 0.08395(5) 0.72329(5) 0.78952(3) 0.05348(19) Uani 1 1 d . . . . . V4 V 0.18706(6) 0.57242(5) 0.82613(3) 0.0584(2) Uani 1 1 d . . . . . O0AA O 0.17517(15) 0.65231(16) 0.75150(10) 0.0451(5) Uani 1 1 d . . . . . O4 O 0.23900(19) 0.65893(19) 0.66102(11) 0.0556(7) Uani 1 1 d . . . . . O15 O 0.25874(19) 0.51318(18) 0.78088(12) 0.0565(7) Uani 1 1 d . . . . . O14 O 0.01989(19) 0.6495(2) 0.74734(14) 0.0629(7) Uani 1 1 d . . . . . O18 O 0.1033(2) 0.50920(19) 0.77718(12) 0.0578(7) Uani 1 1 d . . . . . O12 O 0.16783(17) 0.51654(18) 0.68669(11) 0.0512(6) Uani 1 1 d . . . . . O5 O 0.08313(18) 0.6560(2) 0.65700(12) 0.0569(7) Uani 1 1 d . . . . . O10 O 0.33092(17) 0.65379(19) 0.75621(13) 0.0582(7) Uani 1 1 d . . . . . O16 O 0.2656(2) 0.64807(19) 0.84686(12) 0.0628(8) Uani 1 1 d . . . . . O17 O 0.1086(2) 0.6451(2) 0.84199(12) 0.0675(9) Uani 1 1 d . . . . . O11 O 0.32553(19) 0.5191(2) 0.68947(15) 0.0660(8) Uani 1 1 d . . . . . O13 O 0.0062(2) 0.5139(2) 0.68163(15) 0.0679(8) Uani 1 1 d . . . . . O2 O 0.24760(16) 0.79327(17) 0.72637(10) 0.0472(6) Uani 1 1 d . . . . . O6 O 0.1544(2) 0.8005(2) 0.63027(11) 0.0606(7) Uani 1 1 d . . . . . O8 O 0.18243(19) 0.78727(17) 0.81719(10) 0.0523(6) Uani 1 1 d . . . . . O7 O 0.0226(2) 0.7846(2) 0.81347(14) 0.0689(9) Uani 1 1 d . . . . . O9 O 0.3418(2) 0.7909(2) 0.82185(14) 0.0670(9) Uani 1 1 d . . . . . O19 O 0.1941(3) 0.5048(2) 0.87432(13) 0.0774(11) Uani 1 1 d . . . . . O3 O 0.09131(17) 0.79230(18) 0.72283(10) 0.0480(6) Uani 1 1 d . . . . . C7 C 0.1810(3) 0.8782(3) 0.81558(16) 0.0578(10) Uani 1 1 d . . . . . H7A H 0.2287 0.9000 0.8360 0.069 Uiso 1 1 calc R . . . . H7B H 0.1369 0.8985 0.8324 0.069 Uiso 1 1 calc R . . . . C9 C 0.1692(3) 0.4253(3) 0.68829(19) 0.0587(10) Uani 1 1 d . . . . . H9A H 0.2119 0.4049 0.6702 0.070 Uiso 1 1 calc R . . . . H9B H 0.1205 0.4036 0.6692 0.070 Uiso 1 1 calc R . . . . C0AA C 0.2433(3) 0.8838(3) 0.73056(16) 0.0516(8) Uani 1 1 d . . . . . H0AA H 0.2387 0.9084 0.6949 0.062 Uiso 1 1 calc R . . . . H0AB H 0.2916 0.9047 0.7508 0.062 Uiso 1 1 calc R . . . . C11 C 0.2566(3) 0.4218(3) 0.7772(2) 0.0630(11) Uani 1 1 d . . . . . H11A H 0.2624 0.3976 0.8130 0.076 Uiso 1 1 calc R . . . . H11B H 0.3002 0.4022 0.7596 0.076 Uiso 1 1 calc R . . . . C6 C 0.0972(3) 0.8834(3) 0.72671(16) 0.0534(9) Uani 1 1 d . . . . . H6A H 0.0541 0.9049 0.7441 0.064 Uiso 1 1 calc R . . . . H6B H 0.0922 0.9073 0.6909 0.064 Uiso 1 1 calc R . . . . C5 C 0.1741(3) 0.9125(3) 0.75793(16) 0.0532(9) Uani 1 1 d . . . . . C12 C 0.1795(3) 0.3913(3) 0.7456(2) 0.0610(10) Uani 1 1 d . . . . . C10 C 0.1105(3) 0.4182(3) 0.7734(2) 0.0654(11) Uani 1 1 d . . . . . H10A H 0.0625 0.3954 0.7538 0.079 Uiso 1 1 calc R . . . . H10B H 0.1166 0.3941 0.8092 0.079 Uiso 1 1 calc R . . . . N3 N 0.1680(2) 1.0566(2) 0.71405(14) 0.0552(8) Uani 1 1 d . . . . . N2 N 0.2336(3) 1.0804(3) 0.69369(18) 0.0676(10) Uani 1 1 d . . . . . N7 N 0.2160(3) 0.8071(3) 0.98742(13) 0.0623(9) Uani 1 1 d . . . . . N4 N 0.1892(4) 0.2460(3) 0.7893(2) 0.0897(16) Uani 1 1 d . . . . . O20B O 0.1323(11) 0.0425(6) 0.8928(4) 0.086(3) Uani 0.5 1 d D . P A 1 H20B H 0.1608 0.0250 0.8715 0.128 Uiso 0.5 1 calc R . P A 1 C4 C 0.1746(3) 1.0095(3) 0.76426(17) 0.0604(10) Uani 1 1 d . . . . . H4A H 0.1314 1.0257 0.7833 0.073 Uiso 1 1 calc R . . . . H4B H 0.2230 1.0260 0.7862 0.073 Uiso 1 1 calc R . . . . C20 C 0.2015(4) 0.7240(3) 1.01517(18) 0.0735(14) Uani 1 1 d . . . . . H20D H 0.2461 0.7128 1.0422 0.088 Uiso 1 1 calc R . . . . H20E H 0.1558 0.7309 1.0335 0.088 Uiso 1 1 calc R . . . . C29 C 0.2372(4) 0.8740(4) 1.03098(19) 0.0725(13) Uani 1 1 d . . . . . H29A H 0.1959 0.8752 1.0537 0.087 Uiso 1 1 calc R . . . . H29B H 0.2851 0.8562 1.0531 0.087 Uiso 1 1 calc R . . . . C14 C 0.1322(5) 0.2193(4) 0.8171(3) 0.096(2) Uani 1 1 d . . . . . H14 H 0.0783 0.2273 0.8088 0.115 Uiso 1 1 calc R . . . . C13 C 0.1794(4) 0.2930(3) 0.7394(2) 0.0720(13) Uani 1 1 d . . . . . H13A H 0.1301 0.2760 0.7186 0.086 Uiso 1 1 calc R . . . . H13B H 0.2212 0.2771 0.7190 0.086 Uiso 1 1 calc R . . . . C30 C 0.2488(5) 0.9626(4) 1.0115(3) 0.0902(18) Uani 1 1 d . . . . . H30A H 0.1987 0.9857 0.9956 0.108 Uiso 1 1 calc R . . . . H30B H 0.2833 0.9611 0.9839 0.108 Uiso 1 1 calc R . . . . C39 C 0.6079(3) 0.3128(3) 0.8602(2) 0.0692(12) Uani 1 1 d . . . . . H39A H 0.6624 0.3134 0.8539 0.083 Uiso 1 1 calc R . . . . H39B H 0.6061 0.3315 0.8967 0.083 Uiso 1 1 calc R . . . . C40 C 0.5769(4) 0.2237(4) 0.8537(2) 0.0799(15) Uani 1 1 d . . . . . H40A H 0.5812 0.2039 0.8181 0.120 Uiso 1 1 calc GR . . . . H40B H 0.5228 0.2229 0.8595 0.120 Uiso 1 1 calc GR . . . . H40C H 0.6069 0.1873 0.8794 0.120 Uiso 1 1 calc GR . . . . C38 C 0.5616(4) 0.3745(3) 0.8219(3) 0.0783(15) Uani 1 1 d . . . . . H38A H 0.5679 0.3593 0.7853 0.094 Uiso 1 1 calc R . . . . H38B H 0.5063 0.3698 0.8256 0.094 Uiso 1 1 calc R . . . . C37 C 0.5876(3) 0.4653(3) 0.8322(2) 0.0728(13) Uani 1 1 d . . . . . H37A H 0.6344 0.4748 0.8153 0.087 Uiso 1 1 calc R . . . . H37B H 0.6020 0.4728 0.8705 0.087 Uiso 1 1 calc R . . . . N6 N 0.2513(6) 0.1815(4) 0.8566(4) 0.136(3) Uani 1 1 d . . . . . C16B C 0.124(2) 0.134(2) 0.9008(17) 0.116(6) Uani 0.3 1 d D . P B 2 H16A H 0.1352 0.1595 0.9360 0.140 Uiso 0.3 1 calc R . P B 2 H16B H 0.0681 0.1393 0.8886 0.140 Uiso 0.3 1 calc R . P B 2 C18 C 0.1689(6) 0.5699(5) 1.0106(3) 0.113(3) Uani 1 1 d . . . . . H18A H 0.1219 0.5818 1.0268 0.135 Uiso 1 1 calc R . . . . H18B H 0.1571 0.5229 0.9858 0.135 Uiso 1 1 calc R . . . . C17 C 0.2305(8) 0.5437(5) 1.0525(4) 0.156(5) Uani 1 1 d . . . . . H17A H 0.2765 0.5286 1.0367 0.233 Uiso 1 1 calc GR . . . . H17B H 0.2131 0.4953 1.0710 0.233 Uiso 1 1 calc GR . . . . H17C H 0.2427 0.5896 1.0773 0.233 Uiso 1 1 calc GR . . . . N1 N 0.2091(3) 1.1232(3) 0.64919(18) 0.0716(11) Uani 1 1 d . . . . . C3 C 0.1032(3) 1.0839(3) 0.68320(19) 0.0618(11) Uani 1 1 d . . . . . H3 H 0.0513 1.0760 0.6887 0.074 Uiso 1 1 calc R . . . . C2 C 0.1299(4) 1.1255(3) 0.6424(2) 0.0697(13) Uani 1 1 d . . . . . C1 C 0.0825(5) 1.1734(5) 0.5972(3) 0.0942(19) Uani 1 1 d . U . . . H1AA H 0.0764 1.2320 0.6080 0.113 Uiso 0.8 1 calc R . P C 1 H1AB H 0.1104 1.1734 0.5662 0.113 Uiso 0.8 1 calc R . P C 1 H1BC H 0.0304 1.1830 0.6068 0.113 Uiso 0.2 1 calc R . P D 2 H1BD H 0.1066 1.2286 0.5940 0.113 Uiso 0.2 1 calc R . P D 2 N0AA N 0.5274(2) 0.5330(3) 0.81220(19) 0.0677(10) Uani 1 1 d . . . . . C28 C 0.1433(3) 0.8343(3) 0.94962(16) 0.0615(11) Uani 1 1 d . . . . . H28A H 0.1544 0.8881 0.9334 0.074 Uiso 1 1 calc R . . . . H28B H 0.1337 0.7926 0.9211 0.074 Uiso 1 1 calc R . . . . C8 C 0.5683(4) 0.6186(4) 0.8244(3) 0.0823(16) Uani 1 1 d . . . . . H8A H 0.5870 0.6213 0.8625 0.099 Uiso 1 1 calc R . . . . H8B H 0.6138 0.6214 0.8054 0.099 Uiso 1 1 calc R . . . . C27 C 0.0692(3) 0.8441(3) 0.97518(19) 0.0682(12) Uani 1 1 d . . . . . H27A H 0.0498 0.7883 0.9836 0.082 Uiso 1 1 calc R . . . . H27B H 0.0806 0.8757 1.0084 0.082 Uiso 1 1 calc R . . . . C36 C 0.5006(3) 0.5235(3) 0.7524(2) 0.0708(13) Uani 1 1 d . . . . . H36A H 0.4591 0.5645 0.7420 0.085 Uiso 1 1 calc R . . . . H36B H 0.4784 0.4672 0.7459 0.085 Uiso 1 1 calc R . . . . C21 C 0.2826(3) 0.7978(4) 0.95334(18) 0.0699(12) Uani 1 1 d . . . . . H21C H 0.2681 0.7548 0.9262 0.084 Uiso 1 1 calc R . . . . H21D H 0.2887 0.8512 0.9350 0.084 Uiso 1 1 calc R . . . . C41 C 0.4537(3) 0.5254(4) 0.8392(3) 0.0807(16) Uani 1 1 d . . . . . H41A H 0.4187 0.5718 0.8268 0.097 Uiso 1 1 calc R . . . . H41B H 0.4273 0.4727 0.8276 0.097 Uiso 1 1 calc R . . . . C26 C 0.0072(4) 0.8902(4) 0.9378(2) 0.0756(14) Uani 1 1 d . . . . . H26A H -0.0030 0.8585 0.9045 0.091 Uiso 1 1 calc R . . . . H26B H 0.0273 0.9456 0.9295 0.091 Uiso 1 1 calc R . . . . C25 C -0.0692(4) 0.9021(5) 0.9603(3) 0.099(2) Uani 1 1 d . . . . . H25A H -0.1053 0.9335 0.9352 0.149 Uiso 1 1 calc GR . . . . H25B H -0.0597 0.9329 0.9935 0.149 Uiso 1 1 calc GR . . . . H25C H -0.0913 0.8475 0.9666 0.149 Uiso 1 1 calc GR . . . . C22 C 0.3606(4) 0.7738(6) 0.9846(2) 0.099(2) Uani 1 1 d . . . . . H22A H 0.3738 0.8145 1.0134 0.119 Uiso 1 1 calc R . . . . H22B H 0.3560 0.7182 1.0007 0.119 Uiso 1 1 calc R . . . . C42 C 0.4674(4) 0.5268(6) 0.8998(3) 0.104(2) Uani 1 1 d . . . . . H42A H 0.5039 0.4819 0.9126 0.125 Uiso 1 1 calc R . . . . H42B H 0.4908 0.5808 0.9118 0.125 Uiso 1 1 calc R . . . . C35 C 0.5645(4) 0.5360(5) 0.7167(3) 0.0915(18) Uani 1 1 d . . . . . H35A H 0.5821 0.5947 0.7184 0.110 Uiso 1 1 calc R . . . . H35B H 0.6091 0.4999 0.7288 0.110 Uiso 1 1 calc R . . . . C31 C 0.2842(6) 1.0199(6) 1.0570(4) 0.122(3) Uani 1 1 d . U . . . H31A H 0.2489 1.0201 1.0840 0.147 Uiso 0.6 1 calc R . P E 1 H31B H 0.3330 0.9941 1.0732 0.147 Uiso 0.6 1 calc R . P E 1 H31C H 0.2766 0.9969 1.0917 0.147 Uiso 0.4 1 calc R . P F 2 H31D H 0.2629 1.0770 1.0534 0.147 Uiso 0.4 1 calc R . P F 2 C32A C 0.3007(12) 1.1080(10) 1.0444(8) 0.159(8) Uani 0.6 1 d . U P G 1 H32A H 0.3395 1.1095 1.0203 0.239 Uiso 0.6 1 calc GR . P G 1 H32B H 0.3200 1.1377 1.0768 0.239 Uiso 0.6 1 calc GR . P G 1 H32C H 0.2534 1.1347 1.0277 0.239 Uiso 0.6 1 calc GR . P G 1 C46 C 0.5168(4) 0.6953(4) 0.8091(4) 0.099(2) Uani 1 1 d . U . . . H46A H 0.4850 0.7082 0.8371 0.119 Uiso 0.5 1 calc R . P H 1 H46B H 0.4822 0.6845 0.7760 0.119 Uiso 0.5 1 calc R . P H 1 H46C H 0.5092 0.7006 0.7703 0.119 Uiso 0.5 1 calc R . P I 2 H46D H 0.4657 0.6854 0.8203 0.119 Uiso 0.5 1 calc R . P I 2 C23 C 0.4257(4) 0.7715(7) 0.9501(3) 0.119(3) Uani 1 1 d . . . . . H23A H 0.4286 0.8262 0.9326 0.143 Uiso 1 1 calc R . . . . H23B H 0.4139 0.7287 0.9225 0.143 Uiso 1 1 calc R . . . . C48A C 0.6165(11) 0.7968(10) 0.8031(8) 0.093(4) Uani 0.5 1 d . U P J 2 H48A H 0.6004 0.7921 0.7651 0.139 Uiso 0.5 1 calc GR . P J 2 H48B H 0.6587 0.7578 0.8137 0.139 Uiso 0.5 1 calc GR . P J 2 H48C H 0.6338 0.8538 0.8116 0.139 Uiso 0.5 1 calc GR . P J 2 C43 C 0.3920(6) 0.5146(9) 0.9232(4) 0.148(4) Uani 1 1 d . U . . . H43A H 0.3572 0.5614 0.9111 0.178 Uiso 0.5 1 calc R . P K 1 H43B H 0.3674 0.4628 0.9083 0.178 Uiso 0.5 1 calc R . P K 1 H43C H 0.3491 0.5421 0.9006 0.178 Uiso 0.5 1 calc R . P L 2 H43D H 0.3965 0.5405 0.9585 0.178 Uiso 0.5 1 calc R . P L 2 C24 C 0.5040(6) 0.7518(10) 0.9826(4) 0.173(6) Uani 1 1 d . . . . . H24A H 0.5433 0.7464 0.9589 0.259 Uiso 1 1 calc GR . . . . H24B H 0.5004 0.6994 1.0017 0.259 Uiso 1 1 calc GR . . . . H24C H 0.5183 0.7970 1.0076 0.259 Uiso 1 1 calc GR . . . . C44A C 0.3967(13) 0.5097(19) 0.9798(9) 0.160(10) Uani 0.5 1 d . U P M 1 H44A H 0.3623 0.4657 0.9892 0.240 Uiso 0.5 1 calc R . P M 1 H44B H 0.3814 0.5632 0.9936 0.240 Uiso 0.5 1 calc R . P M 1 H44C H 0.4497 0.4967 0.9949 0.240 Uiso 0.5 1 calc R . P M 1 C34 C 0.5314(5) 0.5133(5) 0.6595(3) 0.099(2) Uani 1 1 d . . . . . H34A H 0.5143 0.4545 0.6584 0.118 Uiso 1 1 calc R . . . . H34B H 0.4858 0.5485 0.6484 0.118 Uiso 1 1 calc R . . . . O21A O 0.0048(4) 1.1354(5) 0.5824(2) 0.113(2) Uani 0.8 1 d . U P N 1 H21A H 0.0009 1.1177 0.5515 0.169 Uiso 0.8 1 calc R . P N 1 C33 C 0.5899(6) 0.5251(8) 0.6202(4) 0.141(4) Uani 1 1 d . . . . . H33A H 0.5654 0.5111 0.5847 0.212 Uiso 1 1 calc GR . . . . H33B H 0.6342 0.4884 0.6299 0.212 Uiso 1 1 calc GR . . . . H33C H 0.6072 0.5832 0.6210 0.212 Uiso 1 1 calc GR . . . . C19 C 0.1889(4) 0.6482(4) 0.9790(2) 0.0834(16) Uani 1 1 d . . . . . H19A H 0.2361 0.6372 0.9628 0.100 Uiso 1 1 calc R . . . . H19B H 0.1464 0.6596 0.9505 0.100 Uiso 1 1 calc R . . . . N5 N 0.2616(5) 0.2242(4) 0.8127(3) 0.123(3) Uani 1 1 d . . . . . C15 C 0.1722(8) 0.1771(4) 0.8608(3) 0.123(4) Uani 1 1 d D . . . . C44B C 0.3748(19) 0.419(2) 0.9275(12) 0.221(14) Uani 0.5 1 d . U P M 2 H44D H 0.3268 0.4114 0.9425 0.332 Uiso 0.5 1 calc R . P M 2 H44E H 0.3699 0.3939 0.8925 0.332 Uiso 0.5 1 calc R . P M 2 H44F H 0.4171 0.3923 0.9503 0.332 Uiso 0.5 1 calc R . P M 2 C32B C 0.3701(15) 1.0177(19) 1.0484(13) 0.151(10) Uani 0.4 1 d . U P G 2 H32D H 0.4004 1.0521 1.0752 0.227 Uiso 0.4 1 calc R . P G 2 H32E H 0.3889 0.9601 1.0514 0.227 Uiso 0.4 1 calc R . P G 2 H32F H 0.3754 1.0394 1.0134 0.227 Uiso 0.4 1 calc R . P G 2 C47B C 0.5769(11) 0.7754(9) 0.8012(8) 0.092(4) Uani 0.5 1 d . U P O 1 H47A H 0.6106 0.7599 0.7747 0.110 Uiso 0.5 1 calc R . P O 1 H47B H 0.5463 0.8247 0.7878 0.110 Uiso 0.5 1 calc R . P O 1 C48B C 0.6250(11) 0.7973(10) 0.8508(7) 0.112(5) Uani 0.5 1 d . U P O 1 H48D H 0.6511 0.8504 0.8466 0.168 Uiso 0.5 1 calc GR . P O 1 H48E H 0.6634 0.7535 0.8600 0.168 Uiso 0.5 1 calc GR . P O 1 H48F H 0.5925 0.8025 0.8788 0.168 Uiso 0.5 1 calc GR . P O 1 O21B O 0.075(2) 1.136(2) 0.5499(9) 0.118(9) Uani 0.2 1 d . U P N 2 H21B H 0.1014 1.1619 0.5303 0.178 Uiso 0.2 1 calc GR . P N 2 C47A C 0.5484(7) 0.7760(7) 0.8325(6) 0.074(3) Uani 0.5 1 d . U P J 2 H47C H 0.5656 0.7696 0.8706 0.088 Uiso 0.5 1 calc R . P J 2 H47D H 0.5089 0.8204 0.8273 0.088 Uiso 0.5 1 calc R . P J 2 C16A C 0.1554(11) 0.1264(7) 0.9092(4) 0.086(3) Uani 0.5 1 d D . P A 1 H16C H 0.2020 0.1243 0.9356 0.103 Uiso 0.5 1 calc R . P A 1 H16D H 0.1138 0.1537 0.9255 0.103 Uiso 0.5 1 calc R . P A 1 O20A O 0.146(2) 0.0462(17) 0.9032(11) 0.116(6) Uani 0.3 1 d D . P B 2 H20A H 0.1191 0.0201 0.8790 0.174 Uiso 0.3 1 calc R . P B 2 O20C O 0.0407(17) 0.1724(18) 0.9161(9) 0.116(6) Uani 0.2 1 d D . P B 3 H20C H 0.0049 0.1567 0.8934 0.174 Uiso 0.2 1 calc GR . P B 3 C16C C 0.115(3) 0.147(4) 0.900(2) 0.116(6) Uani 0.2 1 d D . P B 3 H16E H 0.1058 0.0877 0.8901 0.140 Uiso 0.2 1 calc R . P B 3 H16F H 0.1492 0.1445 0.9343 0.140 Uiso 0.2 1 calc R . P B 3 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 V2 0.0541(4) 0.0518(4) 0.0374(3) -0.0010(2) 0.0024(2) -0.0011(3) V3 0.0529(4) 0.0443(3) 0.0546(4) -0.0028(3) -0.0130(3) -0.0042(3) V6 0.0427(4) 0.0496(4) 0.0628(4) -0.0088(3) -0.0010(3) -0.0034(3) V5 0.0431(4) 0.0556(4) 0.0566(4) -0.0070(3) -0.0008(3) -0.0071(3) V1 0.0602(4) 0.0531(4) 0.0489(4) -0.0013(3) 0.0140(3) -0.0031(3) V4 0.0802(5) 0.0459(4) 0.0462(4) 0.0006(3) -0.0026(3) -0.0058(3) O0AA 0.0453(13) 0.0459(13) 0.0428(12) -0.0034(10) 0.0007(10) -0.0011(11) O4 0.0613(17) 0.0569(16) 0.0485(14) -0.0084(12) 0.0073(12) -0.0087(13) O15 0.0571(17) 0.0432(14) 0.0636(16) -0.0048(12) -0.0120(13) -0.0042(12) O14 0.0500(16) 0.0636(18) 0.0762(19) -0.0007(15) 0.0130(14) -0.0079(14) O18 0.0675(19) 0.0496(15) 0.0556(15) -0.0024(12) 0.0051(13) -0.0114(13) O12 0.0499(15) 0.0488(14) 0.0517(14) -0.0108(11) -0.0050(11) -0.0066(12) O5 0.0558(16) 0.0580(16) 0.0527(14) -0.0027(12) -0.0084(12) -0.0067(13) O10 0.0438(14) 0.0488(15) 0.0761(19) -0.0070(13) -0.0138(13) -0.0061(12) O16 0.087(2) 0.0468(14) 0.0471(14) -0.0028(12) -0.0181(14) -0.0040(14) O17 0.105(3) 0.0550(16) 0.0453(14) 0.0040(12) 0.0197(16) -0.0037(17) O11 0.0496(16) 0.0572(17) 0.089(2) -0.0158(16) 0.0003(15) -0.0021(14) O13 0.0513(17) 0.0635(18) 0.085(2) -0.0086(16) -0.0055(15) -0.0129(15) O2 0.0468(14) 0.0456(13) 0.0471(13) -0.0028(10) -0.0009(10) -0.0025(11) O6 0.076(2) 0.0639(17) 0.0412(13) 0.0010(12) 0.0060(13) -0.0015(15) O8 0.0724(19) 0.0441(13) 0.0390(12) -0.0011(10) 0.0019(12) -0.0019(13) O7 0.083(2) 0.0615(18) 0.0681(19) -0.0008(15) 0.0304(17) 0.0018(16) O9 0.067(2) 0.0521(16) 0.0734(19) -0.0064(14) -0.0230(16) -0.0067(14) O19 0.124(3) 0.0502(16) 0.0542(16) 0.0048(14) -0.0008(18) -0.0005(19) O3 0.0482(14) 0.0513(14) 0.0443(12) 0.0010(11) 0.0052(11) -0.0001(11) C7 0.082(3) 0.045(2) 0.0446(19) -0.0021(15) 0.0054(19) 0.0002(19) C9 0.058(2) 0.050(2) 0.065(2) -0.0140(18) -0.0029(19) -0.0062(18) C0AA 0.059(2) 0.0467(19) 0.0484(18) 0.0011(15) 0.0030(16) -0.0047(17) C11 0.066(3) 0.046(2) 0.072(3) -0.0067(18) -0.009(2) -0.0030(19) C6 0.060(2) 0.051(2) 0.0502(19) 0.0054(16) 0.0106(17) 0.0057(18) C5 0.063(2) 0.052(2) 0.0438(18) -0.0003(15) 0.0050(17) 0.0021(18) C12 0.065(3) 0.044(2) 0.070(3) -0.0085(18) -0.007(2) -0.0085(18) C10 0.077(3) 0.053(2) 0.064(3) -0.0028(19) 0.002(2) -0.012(2) N3 0.065(2) 0.0466(17) 0.0544(18) 0.0024(14) 0.0105(16) 0.0039(15) N2 0.067(2) 0.061(2) 0.075(2) 0.0088(19) 0.011(2) -0.0008(18) N7 0.079(3) 0.068(2) 0.0389(15) 0.0018(15) 0.0041(16) 0.007(2) N4 0.126(5) 0.045(2) 0.089(3) -0.006(2) -0.021(3) -0.009(2) O20B 0.140(8) 0.047(4) 0.060(4) 0.010(3) -0.023(5) -0.020(4) C4 0.081(3) 0.050(2) 0.049(2) -0.0007(17) 0.0059(19) 0.002(2) C20 0.101(4) 0.074(3) 0.045(2) 0.010(2) 0.010(2) 0.014(3) C29 0.084(3) 0.082(3) 0.047(2) -0.009(2) -0.005(2) 0.005(3) C14 0.147(7) 0.056(3) 0.077(3) -0.007(2) -0.010(4) -0.034(4) C13 0.083(4) 0.051(2) 0.078(3) -0.009(2) -0.007(3) -0.011(2) C30 0.121(6) 0.074(3) 0.073(3) -0.010(3) 0.003(3) -0.009(3) C39 0.067(3) 0.066(3) 0.072(3) 0.003(2) -0.001(2) 0.012(2) C40 0.083(4) 0.071(3) 0.081(3) 0.002(3) -0.009(3) 0.012(3) C38 0.070(3) 0.064(3) 0.089(4) -0.005(3) -0.029(3) 0.014(2) C37 0.058(3) 0.062(3) 0.089(3) -0.003(2) -0.023(2) 0.011(2) N6 0.184(9) 0.067(3) 0.137(6) 0.002(4) -0.055(6) 0.021(5) C16B 0.154(13) 0.099(10) 0.080(7) 0.011(6) -0.044(8) 0.020(8) C18 0.159(8) 0.076(4) 0.101(5) 0.008(4) 0.010(5) -0.019(5) C17 0.280(16) 0.081(5) 0.096(5) 0.014(4) -0.009(7) 0.003(7) N1 0.088(3) 0.060(2) 0.069(2) 0.0146(19) 0.018(2) 0.007(2) C3 0.066(3) 0.059(2) 0.061(2) 0.0062(19) 0.009(2) 0.023(2) C2 0.093(4) 0.056(2) 0.060(2) 0.0036(19) 0.011(2) 0.025(2) C1 0.117(5) 0.092(4) 0.074(3) 0.021(3) 0.012(3) 0.037(4) N0AA 0.050(2) 0.056(2) 0.088(3) -0.0072(19) -0.0205(19) 0.0060(17) C28 0.076(3) 0.064(2) 0.0412(18) -0.0006(17) -0.0018(18) 0.003(2) C8 0.065(3) 0.066(3) 0.105(4) -0.010(3) -0.028(3) 0.003(3) C27 0.082(3) 0.069(3) 0.055(2) -0.002(2) 0.013(2) -0.002(2) C36 0.061(3) 0.059(3) 0.084(3) 0.004(2) -0.024(2) 0.003(2) C21 0.077(3) 0.083(3) 0.048(2) 0.005(2) 0.004(2) 0.003(3) C41 0.061(3) 0.072(3) 0.100(4) -0.001(3) -0.020(3) 0.016(3) C26 0.080(3) 0.076(3) 0.069(3) -0.016(2) 0.002(2) 0.005(3) C25 0.080(4) 0.119(5) 0.097(4) -0.040(4) 0.005(3) 0.008(4) C22 0.083(4) 0.149(7) 0.063(3) 0.004(4) -0.001(3) 0.026(4) C42 0.081(4) 0.126(6) 0.097(4) 0.006(4) -0.013(3) 0.036(4) C35 0.065(3) 0.108(5) 0.094(4) 0.014(4) -0.016(3) 0.013(3) C31 0.111(6) 0.106(5) 0.137(7) -0.043(5) -0.032(5) 0.006(5) C32A 0.176(17) 0.102(8) 0.178(16) -0.046(9) -0.055(14) -0.035(11) C46 0.090(4) 0.059(3) 0.137(6) -0.005(3) -0.030(4) 0.001(3) C23 0.084(5) 0.194(10) 0.077(4) 0.017(5) 0.006(3) 0.042(5) C48A 0.096(11) 0.071(8) 0.115(11) 0.005(7) 0.030(9) -0.003(7) C43 0.110(7) 0.207(11) 0.133(7) 0.052(8) 0.031(6) 0.062(8) C24 0.097(6) 0.302(19) 0.117(7) 0.019(10) 0.008(5) 0.029(9) C44A 0.126(15) 0.23(3) 0.125(10) 0.045(17) 0.025(12) 0.057(18) C34 0.106(5) 0.087(4) 0.097(4) -0.006(4) -0.009(4) 0.007(4) O21A 0.099(4) 0.167(7) 0.070(3) 0.001(4) 0.004(3) 0.036(4) C33 0.114(7) 0.199(11) 0.110(6) 0.014(7) 0.014(5) 0.013(8) C19 0.105(5) 0.074(3) 0.067(3) 0.004(3) -0.001(3) -0.002(3) N5 0.142(6) 0.073(3) 0.138(6) 0.006(4) -0.045(5) 0.020(4) C15 0.226(12) 0.050(3) 0.079(4) 0.002(3) -0.032(6) -0.027(5) C44B 0.21(3) 0.245(18) 0.19(2) 0.14(2) -0.03(2) 0.02(2) C32B 0.108(11) 0.15(2) 0.18(2) -0.04(2) -0.032(14) 0.002(16) C47B 0.084(10) 0.060(7) 0.130(11) 0.002(7) 0.010(9) -0.001(6) C48B 0.131(13) 0.093(9) 0.115(10) -0.010(8) 0.028(8) -0.036(9) O21B 0.14(2) 0.14(2) 0.071(10) 0.009(11) -0.003(13) 0.049(18) C47A 0.059(6) 0.065(5) 0.097(8) -0.014(5) 0.010(5) 0.000(4) C16A 0.140(8) 0.047(4) 0.060(4) 0.010(3) -0.023(5) -0.020(4) O20A 0.154(13) 0.099(10) 0.080(7) 0.011(6) -0.044(8) 0.020(8) O20C 0.154(13) 0.099(10) 0.080(7) 0.011(6) -0.044(8) 0.020(8) C16C 0.154(13) 0.099(10) 0.080(7) 0.011(6) -0.044(8) 0.020(8) 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 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.0687 2.1097 'International Tables 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 V6 V2 V5 65.98(2) O0AA V2 V6 47.56(7) O0AA V2 V5 47.72(7) O4 V2 V6 33.84(9) O4 V2 V5 88.02(10) O4 V2 O0AA 81.40(12) O4 V2 O5 93.69(14) O4 V2 O2 87.46(13) O4 V2 O3 158.66(12) O5 V2 V6 88.05(10) O5 V2 V5 34.22(10) O5 V2 O0AA 81.94(12) O5 V2 O2 158.83(13) O5 V2 O3 88.84(13) O2 V2 V6 81.17(8) O2 V2 V5 124.89(8) O2 V2 O0AA 77.32(10) O6 V2 V6 137.89(13) O6 V2 V5 137.82(13) O6 V2 O0AA 171.31(13) O6 V2 O4 104.34(16) O6 V2 O5 103.93(16) O6 V2 O2 96.22(15) O6 V2 O3 95.56(14) O3 V2 V6 125.33(8) O3 V2 V5 82.21(8) O3 V2 O0AA 77.99(10) O3 V2 O2 82.74(12) V6 V3 V4 66.07(2) O0AA V3 V6 47.33(7) O0AA V3 V4 47.52(7) O10 V3 V6 34.19(9) O10 V3 V4 87.60(10) O10 V3 O0AA 81.51(11) O10 V3 O16 94.28(16) O10 V3 O2 88.74(13) O10 V3 O8 158.51(13) O16 V3 V6 89.01(9) O16 V3 V4 33.89(10) O16 V3 O0AA 81.40(12) O16 V3 O2 157.83(14) O16 V3 O8 86.50(14) O2 V3 V6 81.20(8) O2 V3 V4 124.65(8) O2 V3 O0AA 77.33(10) O2 V3 O8 82.85(11) O8 V3 V6 124.51(9) O8 V3 V4 81.11(9) O8 V3 O0AA 77.37(11) O9 V3 V6 138.45(15) O9 V3 V4 137.43(14) O9 V3 O0AA 171.46(15) O9 V3 O10 104.64(17) O9 V3 O16 103.75(17) O9 V3 O2 96.68(15) O9 V3 O8 95.99(17) V2 V6 V3 66.09(2) O0AA V6 V2 47.25(7) O0AA V6 V3 47.52(7) O4 V6 V2 34.19(9) O4 V6 V3 88.16(9) O4 V6 O0AA 81.44(12) O4 V6 O15 158.30(14) O4 V6 O12 88.62(13) O4 V6 O10 94.86(14) O15 V6 V2 124.44(10) O15 V6 V3 81.03(9) O15 V6 O0AA 77.37(12) O12 V6 V2 82.06(9) O12 V6 V3 125.38(9) O12 V6 O0AA 78.11(11) O12 V6 O15 82.53(12) O10 V6 V2 88.74(10) O10 V6 V3 33.59(10) O10 V6 O0AA 81.10(12) O10 V6 O15 86.50(14) O10 V6 O12 158.16(14) O11 V6 V2 138.50(15) O11 V6 V3 136.72(12) O11 V6 O0AA 172.04(15) O11 V6 O4 104.54(18) O11 V6 O15 96.16(17) O11 V6 O12 96.59(15) O11 V6 O10 103.34(16) V2 V5 V1 65.53(2) O0AA V5 V2 47.02(7) O0AA V5 V1 47.21(7) O14 V5 V2 87.12(10) O14 V5 V1 33.73(11) O14 V5 O0AA 80.94(13) O14 V5 O18 88.64(15) O14 V5 O12 157.88(14) O14 V5 O5 93.22(15) O18 V5 V2 124.65(9) O18 V5 V1 81.67(9) O18 V5 O0AA 77.82(11) O18 V5 O12 82.45(13) O12 V5 V2 81.49(9) O12 V5 V1 124.42(8) O12 V5 O0AA 77.42(10) O5 V5 V2 34.18(9) O5 V5 V1 87.96(10) O5 V5 O0AA 81.20(12) O5 V5 O18 158.38(14) O5 V5 O12 87.96(14) O13 V5 V2 137.50(14) O13 V5 V1 136.52(14) O13 V5 O0AA 173.56(16) O13 V5 O14 103.05(18) O13 V5 O18 97.08(17) O13 V5 O12 98.13(16) O13 V5 O5 103.45(17) V4 V1 V5 65.81(2) O0AA V1 V5 47.41(7) O0AA V1 V4 47.59(7) O14 V1 V5 33.30(10) O14 V1 V4 87.84(11) O14 V1 O0AA 80.71(12) O14 V1 O8 158.07(13) O14 V1 O3 87.62(14) O17 V1 V5 87.58(10) O17 V1 V4 34.65(11) O17 V1 O0AA 82.22(13) O17 V1 O14 93.21(16) O17 V1 O8 89.06(15) O17 V1 O3 159.50(15) O8 V1 V5 125.25(9) O8 V1 V4 81.67(9) O8 V1 O0AA 78.00(11) O8 V1 O3 82.83(12) O7 V1 V5 135.98(15) O7 V1 V4 138.00(13) O7 V1 O0AA 172.86(14) O7 V1 O14 102.87(18) O7 V1 O17 103.58(17) O7 V1 O8 97.76(17) O7 V1 O3 96.17(15) O3 V1 V5 81.90(8) O3 V1 V4 125.08(8) O3 V1 O0AA 77.70(10) V1 V4 V3 66.04(2) O0AA V4 V3 47.40(7) O0AA V4 V1 47.47(7) O15 V4 V3 81.01(9) O15 V4 V1 124.57(9) O15 V4 O0AA 77.28(11) O15 V4 O18 82.43(13) O18 V4 V3 124.93(9) O18 V4 V1 81.96(10) O18 V4 O0AA 77.78(11) O16 V4 V3 34.29(9) O16 V4 V1 87.53(11) O16 V4 O0AA 81.68(12) O16 V4 O15 88.72(15) O16 V4 O18 158.96(13) O16 V4 O17 93.95(17) O17 V4 V3 88.81(11) O17 V4 V1 33.81(9) O17 V4 O0AA 81.26(11) O17 V4 O15 157.76(13) O17 V4 O18 87.41(16) O19 V4 V3 137.76(16) O19 V4 V1 136.88(17) O19 V4 O0AA 172.50(14) O19 V4 O15 97.52(18) O19 V4 O18 96.29(17) O19 V4 O16 103.79(18) O19 V4 O17 103.23(19) V2 O0AA V3 95.18(10) V2 O0AA V6 85.19(9) V2 O0AA V5 85.26(9) V2 O0AA V1 94.81(10) V2 O0AA V4 179.66(14) V3 O0AA V5 179.41(15) V3 O0AA V1 94.97(10) V3 O0AA V4 85.08(9) V6 O0AA V3 85.15(9) V6 O0AA V5 94.50(10) V6 O0AA V1 179.87(16) V6 O0AA V4 95.06(10) V1 O0AA V5 85.38(9) V1 O0AA V4 84.94(9) V4 O0AA V5 94.49(10) V6 O4 V2 111.98(15) V4 O15 V6 109.84(14) C11 O15 V6 118.6(3) C11 O15 V4 119.1(3) V5 O14 V1 112.97(17) V5 O18 V4 109.34(14) C10 O18 V5 119.0(3) C10 O18 V4 117.9(3) V6 O12 V5 109.41(13) C9 O12 V6 119.2(3) C9 O12 V5 118.3(3) V2 O5 V5 111.60(15) V3 O10 V6 112.22(16) V4 O16 V3 111.82(15) V1 O17 V4 111.55(16) V3 O2 V2 109.68(13) C0AA O2 V2 118.9(3) C0AA O2 V3 118.2(2) V1 O8 V3 109.16(13) C7 O8 V3 118.4(3) C7 O8 V1 118.6(3) V1 O3 V2 108.91(13) C6 O3 V2 117.8(2) C6 O3 V1 119.4(2) O8 C7 H7A 109.2 O8 C7 H7B 109.2 O8 C7 C5 112.1(3) H7A C7 H7B 107.9 C5 C7 H7A 109.2 C5 C7 H7B 109.2 O12 C9 H9A 109.2 O12 C9 H9B 109.2 O12 C9 C12 112.1(3) H9A C9 H9B 107.9 C12 C9 H9A 109.2 C12 C9 H9B 109.2 O2 C0AA H0AA 109.1 O2 C0AA H0AB 109.1 O2 C0AA C5 112.3(3) H0AA C0AA H0AB 107.9 C5 C0AA H0AA 109.1 C5 C0AA H0AB 109.1 O15 C11 H11A 109.4 O15 C11 H11B 109.4 O15 C11 C12 111.1(4) H11A C11 H11B 108.0 C12 C11 H11A 109.4 C12 C11 H11B 109.4 O3 C6 H6A 109.1 O3 C6 H6B 109.1 O3 C6 C5 112.7(4) H6A C6 H6B 107.8 C5 C6 H6A 109.1 C5 C6 H6B 109.1 C0AA C5 C7 110.9(4) C0AA C5 C4 110.4(4) C6 C5 C7 109.6(4) C6 C5 C0AA 110.9(3) C6 C5 C4 110.3(4) C4 C5 C7 104.7(3) C9 C12 C11 111.3(4) C9 C12 C13 104.8(4) C11 C12 C13 110.7(4) C10 C12 C9 109.8(4) C10 C12 C11 110.5(4) C10 C12 C13 109.5(4) O18 C10 C12 112.7(4) O18 C10 H10A 109.0 O18 C10 H10B 109.0 C12 C10 H10A 109.0 C12 C10 H10B 109.0 H10A C10 H10B 107.8 N2 N3 C4 119.8(4) C3 N3 N2 111.2(4) C3 N3 C4 128.9(4) N1 N2 N3 105.9(4) C20 N7 C29 107.5(4) C20 N7 C28 110.9(4) C20 N7 C21 110.9(4) C29 N7 C21 110.1(4) C28 N7 C29 110.6(4) C28 N7 C21 106.9(3) C14 N4 C13 126.9(6) C14 N4 N5 112.9(7) N5 N4 C13 120.2(7) C16A O20B H20B 109.5 C5 C4 H4A 108.6 C5 C4 H4B 108.6 N3 C4 C5 114.6(3) N3 C4 H4A 108.6 N3 C4 H4B 108.6 H4A C4 H4B 107.6 N7 C20 H20D 108.5 N7 C20 H20E 108.5 H20D C20 H20E 107.5 C19 C20 N7 115.2(4) C19 C20 H20D 108.5 C19 C20 H20E 108.5 N7 C29 H29A 108.4 N7 C29 H29B 108.4 H29A C29 H29B 107.4 C30 C29 N7 115.7(4) C30 C29 H29A 108.4 C30 C29 H29B 108.4 N4 C14 H14 128.0 N4 C14 C15 104.1(9) C15 C14 H14 128.0 C12 C13 H13A 108.5 C12 C13 H13B 108.5 N4 C13 C12 114.9(4) N4 C13 H13A 108.5 N4 C13 H13B 108.5 H13A C13 H13B 107.5 C29 C30 H30A 109.4 C29 C30 H30B 109.4 C29 C30 C31 111.2(6) H30A C30 H30B 108.0 C31 C30 H30A 109.4 C31 C30 H30B 109.4 H39A C39 H39B 107.9 C40 C39 H39A 109.1 C40 C39 H39B 109.1 C40 C39 C38 112.3(5) C38 C39 H39A 109.1 C38 C39 H39B 109.1 C39 C40 H40A 109.5 C39 C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40B 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 C39 C38 H38A 109.2 C39 C38 H38B 109.2 H38A C38 H38B 107.9 C37 C38 C39 112.2(4) C37 C38 H38A 109.2 C37 C38 H38B 109.2 C38 C37 H37A 108.4 C38 C37 H37B 108.4 C38 C37 N0AA 115.6(4) H37A C37 H37B 107.4 N0AA C37 H37A 108.4 N0AA C37 H37B 108.4 N5 N6 C15 109.4(7) H16A C16B H16B 108.6 C15 C16B H16A 110.3 C15 C16B H16B 110.3 O20A C16B H16A 110.3 O20A C16B H16B 110.3 O20A C16B C15 107(3) H18A C18 H18B 107.6 C17 C18 H18A 108.7 C17 C18 H18B 108.7 C17 C18 C19 114.4(8) C19 C18 H18A 108.7 C19 C18 H18B 108.7 C18 C17 H17A 109.5 C18 C17 H17B 109.5 C18 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 N2 N1 C2 108.7(4) N3 C3 H3 127.6 N3 C3 C2 104.8(5) C2 C3 H3 127.6 N1 C2 C3 109.4(4) N1 C2 C1 122.9(5) C3 C2 C1 127.6(6) C2 C1 H1AA 109.3 C2 C1 H1AB 109.3 C2 C1 H1BC 108.3 C2 C1 H1BD 108.3 H1AA C1 H1AB 107.9 H1BC C1 H1BD 107.4 O21A C1 C2 111.7(6) O21A C1 H1AA 109.3 O21A C1 H1AB 109.3 O21B C1 C2 116.0(14) O21B C1 H1BC 108.3 O21B C1 H1BD 108.3 C37 N0AA C8 105.9(4) C36 N0AA C37 111.1(4) C36 N0AA C8 110.8(4) C36 N0AA C41 105.9(4) C41 N0AA C37 111.6(5) C41 N0AA C8 111.6(5) N7 C28 H28A 108.4 N7 C28 H28B 108.4 H28A C28 H28B 107.5 C27 C28 N7 115.5(4) C27 C28 H28A 108.4 C27 C28 H28B 108.4 N0AA C8 H8A 108.7 N0AA C8 H8B 108.7 H8A C8 H8B 107.6 C46 C8 N0AA 114.3(5) C46 C8 H8A 108.7 C46 C8 H8B 108.7 C28 C27 H27A 109.6 C28 C27 H27B 109.6 H27A C27 H27B 108.1 C26 C27 C28 110.4(4) C26 C27 H27A 109.6 C26 C27 H27B 109.6 N0AA C36 H36A 108.5 N0AA C36 H36B 108.5 N0AA C36 C35 115.2(4) H36A C36 H36B 107.5 C35 C36 H36A 108.5 C35 C36 H36B 108.5 N7 C21 H21C 108.7 N7 C21 H21D 108.7 H21C C21 H21D 107.6 C22 C21 N7 114.3(4) C22 C21 H21C 108.7 C22 C21 H21D 108.7 N0AA C41 H41A 108.5 N0AA C41 H41B 108.5 H41A C41 H41B 107.5 C42 C41 N0AA 115.0(5) C42 C41 H41A 108.5 C42 C41 H41B 108.5 C27 C26 H26A 108.8 C27 C26 H26B 108.8 C27 C26 C25 113.7(5) H26A C26 H26B 107.7 C25 C26 H26A 108.8 C25 C26 H26B 108.8 C26 C25 H25A 109.5 C26 C25 H25B 109.5 C26 C25 H25C 109.5 H25A C25 H25B 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C21 C22 H22A 109.1 C21 C22 H22B 109.1 H22A C22 H22B 107.8 C23 C22 C21 112.5(5) C23 C22 H22A 109.1 C23 C22 H22B 109.1 C41 C42 H42A 109.3 C41 C42 H42B 109.3 H42A C42 H42B 108.0 C43 C42 C41 111.6(7) C43 C42 H42A 109.3 C43 C42 H42B 109.3 C36 C35 H35A 109.9 C36 C35 H35B 109.9 H35A C35 H35B 108.3 C34 C35 C36 108.8(6) C34 C35 H35A 109.9 C34 C35 H35B 109.9 C30 C31 H31A 107.8 C30 C31 H31B 107.8 C30 C31 H31C 111.7 C30 C31 H31D 111.7 C30 C31 C32B 100.3(12) H31A C31 H31B 107.2 H31C C31 H31D 109.5 C32A C31 C30 118.0(10) C32A C31 H31A 107.8 C32A C31 H31B 107.8 C32B C31 H31C 111.7 C32B C31 H31D 111.7 C31 C32A H32A 109.5 C31 C32A H32B 109.5 C31 C32A H32C 109.5 H32A C32A H32B 109.5 H32A C32A H32C 109.5 H32B C32A H32C 109.5 C8 C46 H46A 110.4 C8 C46 H46B 110.4 C8 C46 H46C 108.7 C8 C46 H46D 108.7 C8 C46 C47B 106.4(8) H46A C46 H46B 108.6 H46C C46 H46D 107.6 C47B C46 H46A 110.4 C47B C46 H46B 110.4 C47A C46 C8 114.4(7) C47A C46 H46C 108.7 C47A C46 H46D 108.7 C22 C23 H23A 109.3 C22 C23 H23B 109.3 C22 C23 C24 111.8(7) H23A C23 H23B 107.9 C24 C23 H23A 109.3 C24 C23 H23B 109.3 H48A C48A H48B 109.5 H48A C48A H48C 109.5 H48B C48A H48C 109.5 C47A C48A H48A 109.5 C47A C48A H48B 109.5 C47A C48A H48C 109.5 C42 C43 H43A 107.9 C42 C43 H43B 107.9 C42 C43 H43C 109.8 C42 C43 H43D 109.8 C42 C43 C44B 109.5(16) H43A C43 H43B 107.2 H43C C43 H43D 108.2 C44A C43 C42 117.7(13) C44A C43 H43A 107.9 C44A C43 H43B 107.9 C44B C43 H43C 109.8 C44B C43 H43D 109.8 C23 C24 H24A 109.5 C23 C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C43 C44A H44A 109.5 C43 C44A H44B 109.5 C43 C44A H44C 109.5 H44A C44A H44B 109.5 H44A C44A H44C 109.5 H44B C44A H44C 109.5 C35 C34 H34A 108.9 C35 C34 H34B 108.9 H34A C34 H34B 107.8 C33 C34 C35 113.2(7) C33 C34 H34A 108.9 C33 C34 H34B 108.9 C1 O21A H21A 109.5 C34 C33 H33A 109.5 C34 C33 H33B 109.5 C34 C33 H33C 109.5 H33A C33 H33B 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C20 C19 C18 110.5(5) C20 C19 H19A 109.6 C20 C19 H19B 109.6 C18 C19 H19A 109.6 C18 C19 H19B 109.6 H19A C19 H19B 108.1 N6 N5 N4 105.9(9) C14 C15 C16B 118(2) C14 C15 C16A 139.7(14) C14 C15 C16C 111(2) N6 C15 C14 107.8(8) N6 C15 C16B 133.8(18) N6 C15 C16A 112.5(11) N6 C15 C16C 141(2) C43 C44B H44D 109.5 C43 C44B H44E 109.5 C43 C44B H44F 109.5 H44D C44B H44E 109.5 H44D C44B H44F 109.5 H44E C44B H44F 109.5 C31 C32B H32D 109.5 C31 C32B H32E 109.5 C31 C32B H32F 109.5 H32D C32B H32E 109.5 H32D C32B H32F 109.5 H32E C32B H32F 109.5 C46 C47B H47A 109.3 C46 C47B H47B 109.3 H47A C47B H47B 107.9 C48B C47B C46 111.7(15) C48B C47B H47A 109.3 C48B C47B H47B 109.3 C47B C48B H48D 109.5 C47B C48B H48E 109.5 C47B C48B H48F 109.5 H48D C48B H48E 109.5 H48D C48B H48F 109.5 H48E C48B H48F 109.5 C1 O21B H21B 109.5 C46 C47A C48A 105.1(11) C46 C47A H47C 110.7 C46 C47A H47D 110.7 C48A C47A H47C 110.7 C48A C47A H47D 110.7 H47C C47A H47D 108.8 O20B C16A C15 109.2(10) O20B C16A H16C 109.8 O20B C16A H16D 109.8 C15 C16A H16C 109.8 C15 C16A H16D 109.8 H16C C16A H16D 108.3 C16B O20A H20A 109.5 C16C O20C H20C 109.5 C15 C16C H16E 102.6 C15 C16C H16F 102.6 O20C C16C C15 138(4) O20C C16C H16E 102.6 O20C C16C H16F 102.6 H16E C16C H16F 105.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance V2 V6 3.0159(10) V2 V5 3.0275(10) V2 O0AA 2.223(3) V2 O4 1.827(3) V2 O5 1.829(3) V2 O2 2.026(3) V2 O6 1.604(3) V2 O3 2.022(3) V3 V6 3.0270(10) V3 V4 3.0324(11) V3 O0AA 2.240(3) V3 O10 1.809(3) V3 O16 1.840(3) V3 O2 2.005(3) V3 O8 2.042(3) V3 O9 1.607(3) V6 O0AA 2.234(3) V6 O4 1.811(3) V6 O15 2.023(3) V6 O12 2.007(3) V6 O10 1.837(3) V6 O11 1.594(3) V5 V1 3.0430(10) V5 O0AA 2.248(3) V5 O14 1.814(3) V5 O18 2.019(3) V5 O12 2.025(3) V5 O5 1.831(3) V5 O13 1.616(3) V1 V4 3.0284(11) V1 O0AA 2.240(3) V1 O14 1.835(3) V1 O17 1.812(3) V1 O8 2.011(3) V1 O7 1.604(3) V1 O3 2.016(3) V4 O0AA 2.245(3) V4 O15 2.014(3) V4 O18 2.024(3) V4 O16 1.821(3) V4 O17 1.851(4) V4 O19 1.605(3) O15 C11 1.439(5) O18 C10 1.439(6) O12 C9 1.434(5) O2 C0AA 1.429(5) O8 C7 1.429(5) O3 C6 1.437(5) C7 H7A 0.9700 C7 H7B 0.9700 C7 C5 1.537(5) C9 H9A 0.9700 C9 H9B 0.9700 C9 C12 1.525(7) C0AA H0AA 0.9700 C0AA H0AB 0.9700 C0AA C5 1.522(6) C11 H11A 0.9700 C11 H11B 0.9700 C11 C12 1.528(6) C6 H6A 0.9700 C6 H6B 0.9700 C6 C5 1.514(6) C5 C4 1.531(6) C12 C10 1.517(7) C12 C13 1.553(6) C10 H10A 0.9700 C10 H10B 0.9700 N3 N2 1.352(6) N3 C4 1.455(5) N3 C3 1.339(6) N2 N1 1.326(6) N7 C20 1.517(6) N7 C29 1.526(6) N7 C28 1.526(6) N7 C21 1.527(6) N4 C14 1.345(10) N4 C13 1.448(8) N4 N5 1.347(9) O20B H20B 0.8200 O20B C16A 1.422(14) C4 H4A 0.9700 C4 H4B 0.9700 C20 H20D 0.9700 C20 H20E 0.9700 C20 C19 1.497(8) C29 H29A 0.9700 C29 H29B 0.9700 C29 C30 1.500(9) C14 H14 0.9300 C14 C15 1.385(10) C13 H13A 0.9700 C13 H13B 0.9700 C30 H30A 0.9700 C30 H30B 0.9700 C30 C31 1.517(9) C39 H39A 0.9700 C39 H39B 0.9700 C39 C40 1.500(8) C39 C38 1.515(7) C40 H40A 0.9600 C40 H40B 0.9600 C40 H40C 0.9600 C38 H38A 0.9700 C38 H38B 0.9700 C38 C37 1.507(7) C37 H37A 0.9700 C37 H37B 0.9700 C37 N0AA 1.521(6) N6 N5 1.325(12) N6 C15 1.379(14) C16B H16A 0.9700 C16B H16B 0.9700 C16B C15 1.547(18) C16B O20A 1.42(2) C18 H18A 0.9700 C18 H18B 0.9700 C18 C17 1.448(13) C18 C19 1.529(9) C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 N1 C2 1.348(8) C3 H3 0.9300 C3 C2 1.348(7) C2 C1 1.509(7) C1 H1AA 0.9700 C1 H1AB 0.9700 C1 H1BC 0.9700 C1 H1BD 0.9700 C1 O21A 1.464(11) C1 O21B 1.31(3) N0AA C8 1.529(7) N0AA C36 1.519(7) N0AA C41 1.519(8) C28 H28A 0.9700 C28 H28B 0.9700 C28 C27 1.509(7) C8 H8A 0.9700 C8 H8B 0.9700 C8 C46 1.514(8) C27 H27A 0.9700 C27 H27B 0.9700 C27 C26 1.509(8) C36 H36A 0.9700 C36 H36B 0.9700 C36 C35 1.522(9) C21 H21C 0.9700 C21 H21D 0.9700 C21 C22 1.508(8) C41 H41A 0.9700 C41 H41B 0.9700 C41 C42 1.511(9) C26 H26A 0.9700 C26 H26B 0.9700 C26 C25 1.511(9) C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C22 H22A 0.9700 C22 H22B 0.9700 C22 C23 1.505(10) C42 H42A 0.9700 C42 H42B 0.9700 C42 C43 1.507(12) C35 H35A 0.9700 C35 H35B 0.9700 C35 C34 1.517(9) C31 H31A 0.9700 C31 H31B 0.9700 C31 H31C 0.9700 C31 H31D 0.9700 C31 C32A 1.457(19) C31 C32B 1.52(3) C32A H32A 0.9600 C32A H32B 0.9600 C32A H32C 0.9600 C46 H46A 0.9700 C46 H46B 0.9700 C46 H46C 0.9700 C46 H46D 0.9700 C46 C47B 1.658(18) C46 C47A 1.471(12) C23 H23A 0.9700 C23 H23B 0.9700 C23 C24 1.511(12) C48A H48A 0.9600 C48A H48B 0.9600 C48A H48C 0.9600 C48A C47A 1.502(18) C43 H43A 0.9700 C43 H43B 0.9700 C43 H43C 0.9700 C43 H43D 0.9700 C43 C44A 1.42(2) C43 C44B 1.54(3) C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C44A H44A 0.9600 C44A H44B 0.9600 C44A H44C 0.9600 C34 H34A 0.9700 C34 H34B 0.9700 C34 C33 1.512(12) O21A H21A 0.8200 C33 H33A 0.9600 C33 H33B 0.9600 C33 H33C 0.9600 C19 H19A 0.9700 C19 H19B 0.9700 C15 C16A 1.515(13) C15 C16C 1.561(19) C44B H44D 0.9600 C44B H44E 0.9600 C44B H44F 0.9600 C32B H32D 0.9600 C32B H32E 0.9600 C32B H32F 0.9600 C47B H47A 0.9700 C47B H47B 0.9700 C47B C48B 1.44(2) C48B H48D 0.9600 C48B H48E 0.9600 C48B H48F 0.9600 O21B H21B 0.8200 C47A H47C 0.9700 C47A H47D 0.9700 C16A H16C 0.9700 C16A H16D 0.9700 O20A H20A 0.8200 O20C H20C 0.8200 O20C C16C 1.45(2) C16C H16E 0.9700 C16C H16F 0.9700