#------------------------------------------------------------------------------ #$Date: 2024-12-06 19:28:55 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296456 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249365.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_7249365 loop_ _publ_author_name 'Xu, Li-Mei' 'Wang, Qian' 'Zhang, Lin' 'Shen, Jin-Qiu' 'Chen, Xiao-Lu' 'Zhang, Jian-Yong' 'Liu, Zhen-Jiang' _publ_section_title ; Controllable assembly over two CoII-based coordination polymers: structures and catalytic properties towards the alkene oxyalkylation reaction ; _journal_issue 43 _journal_name_full CrystEngComm _journal_page_first 6134 _journal_page_last 6142 _journal_paper_doi 10.1039/D4CE00857J _journal_volume 26 _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_sum 'C41 H33 Br2 Co3 N3 O13' _chemical_formula_weight 1112.31 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method ;FinalCif V118 by Daniel Kratzert, Freiburg 2024, https://dkratzert.de/finalcif.html ; _audit_update_record ; 2024-08-26 deposited with the CCDC. 2024-09-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 119.327(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.924(2) _cell_length_b 24.938(4) _cell_length_c 17.141(4) _cell_measurement_reflns_used 4968 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.3605 _cell_measurement_theta_min 2.8105 _cell_volume 6307(2) _computing_cell_refinement 'SAINT V8.40B' _computing_data_collection 'Bruker BIS 8.5.4.0/2024-05-04 && APEX5 2023.9-4' _computing_data_reduction 'SAINT V8.40B' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON III' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.878 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE dual wavelength Mo/Cu' _diffrn_measurement_method '\w and \f scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_unetI/netI 0.0879 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.878 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 10753 _diffrn_reflns_point_group_measured_fraction_full 0.500 _diffrn_reflns_point_group_measured_fraction_max 0.440 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.342 _diffrn_reflns_theta_min 2.505 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 2.093 _exptl_absorpt_process_details ;TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.171 _exptl_crystal_description block _exptl_crystal_F_000 2220 _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.915 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.105 _refine_ls_abs_structure_details ; No quotients, so Flack parameter determined by classical intensity fit ; _refine_ls_abs_structure_Flack 0.068(32) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 586 _refine_ls_number_reflns 10753 _refine_ls_number_restraints 634 _refine_ls_restrained_S_all 0.960 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0491 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0829P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1137 _refine_ls_wR_factor_ref 0.1249 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full 0.000 _reflns_Friedel_fraction_max 0.000 _reflns_number_gt 8057 _reflns_number_total 10753 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details 'The data was integrated as a 2-component twin.' _twin_individual_id 2 _twin_individual_twin_matrix_11 3e-05 _twin_individual_twin_matrix_12 0.01457 _twin_individual_twin_matrix_13 -0.99271 _twin_individual_twin_matrix_21 -1.0 _twin_individual_twin_matrix_22 0.00045 _twin_individual_twin_matrix_23 0.00016 _twin_individual_twin_matrix_31 0.00015 _twin_individual_twin_matrix_32 0.99271 _twin_individual_twin_matrix_33 0.99606 _cod_data_source_file d4ce00857j2.cif _cod_data_source_block mo_20240822a_0m_5_sq _cod_depositor_comments 'Adding full bibliography for 7249365--7249366.cif.' _cod_original_cell_volume 6307.4(19) _cod_original_sg_symbol_H-M 'C c' _cod_database_code 7249365 _shelx_shelxl_version_number 2019/2 _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. ; _shelx_estimated_absorpt_t_min 0.602 _shelx_estimated_absorpt_t_max 0.704 _diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800' _shelx_res_file ; TITL Cc_a.res in Cc mo_20240822a_0m_5_sq.res created by SHELXL-2019/2 at 09:21:57 on 26-Aug-2024 REM Old TITL Cc in Cc REM SHELXT solution in Cc: R1 0.248, Rweak 0.184, Alpha 0.036 REM 0.204 for 153 systematic absences, Orientation as input REM Flack x = 0.410 ( 0.009 ) from 3054 Parsons' quotients REM Formula found by SHELXT: C30 Br5 N16 O22 CELL 0.71073 16.9245 24.9380 17.1410 90.000 119.327 90.000 ZERR 4 0.0024 0.0041 0.0037 0.000 0.004 0.000 LATT -7 SYMM X, -Y, 1/2+Z SFAC C H BR CO N O UNIT 164 132 8 12 12 52 OMIT 0 4 1 OMIT -4 6 2 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173 SIZE 0.18 0.20 0.27 L.S. 5 0 273 isor 0.02 $C BOND ACTA SIMU 0.01 0.02 2 bump 0.01 FMAP 2 REM TWIN -1 0 0 0 -1 0 1 0 1 PLAN 200 ABIN DFIX 2.52 0.01 Co3 H13a Co3 H13B merg 0 sadi 0.01 C27 Br2 C27 Br2A sadi 0.01 C3 Br1 C3 Br1A WGHT 0.082900 BASF 0.45778 FVAR 0.26818 0.53199 0.78420 part 1 31 BR1 3 -0.317434 0.034789 0.384009 31.00000 0.01405 0.12731 = 0.08684 0.07985 0.01428 0.01163 part 2 -31 BR1A 3 -0.306702 0.053770 0.408044 -31.00000 0.02140 0.10484 = 0.09182 0.05469 0.02648 0.02370 part 0 part 1 21 BR2 3 0.613859 0.223188 0.357691 21.00000 0.06072 0.14443 = 0.09343 -0.08720 0.06505 -0.06287 part 2 -21 BR2A 3 0.580376 0.250262 0.324838 -21.00000 0.08231 0.14845 = 0.08976 -0.08169 0.07750 -0.07774 part 0 CO1 4 10.181405 10.127009 10.430428 11.00000 0.01490 0.01889 = 0.01358 0.00050 0.00649 -0.00109 CO2 4 0.671948 0.387668 0.724624 11.00000 0.01216 0.01627 = 0.01408 0.00099 0.00509 0.00002 CO3 4 -0.032426 0.133781 0.219259 11.00000 0.01063 0.02075 = 0.01429 0.00203 0.00422 0.00250 O1 6 0.080707 0.091572 0.447249 11.00000 0.02079 0.04399 = 0.02136 0.00561 0.01222 -0.00341 O2 6 0.077948 -0.058346 0.636603 11.00000 0.01803 0.04493 = 0.02270 0.02118 0.01015 0.00982 O3 6 -0.052371 0.108373 0.325506 11.00000 0.01651 0.03101 = 0.02235 0.00732 0.00918 0.00571 O4 6 0.106730 0.138513 0.295161 11.00000 0.01754 0.01885 = 0.00983 0.00092 0.00547 0.00431 AFIX 13 0.8500 H4X 2 0.113426 0.172170 0.293102 11.00000 -1.20000 AFIX 0 O5 6 0.291237 0.168188 0.438776 11.00000 0.03456 0.03609 = 0.02238 -0.00345 0.01549 -0.01681 O6 6 0.737431 0.448255 0.929639 11.00000 0.03362 0.02982 = 0.03005 -0.01103 0.01650 -0.00507 O7 6 0.742536 0.453177 0.800898 11.00000 0.04409 0.02345 = 0.02757 -0.01273 0.01716 -0.02182 O8 6 -0.033125 -0.057306 0.672640 11.00000 0.02200 0.02668 = 0.02796 0.01398 0.01352 0.00404 O9 6 0.277264 0.163876 0.302216 11.00000 0.03174 0.04463 = 0.02046 -0.02240 0.01772 -0.01987 O10 6 0.608655 0.323872 0.639542 11.00000 0.02958 0.03248 = 0.03558 -0.01855 0.02194 -0.01794 O11 6 0.462766 0.331249 0.605846 11.00000 0.02005 0.03797 = 0.03451 -0.00629 0.01984 -0.00913 DFIX 0.85 0.01 O12 H12a O12 H12B DFIX 1.34 0.01 H12a H12B O12 6 0.145528 0.207459 0.451596 11.00000 0.03416 0.02196 = 0.04180 -0.00116 0.02320 0.00070 H12A 2 0.129832 0.223908 0.402713 11.00000 -1.20000 H12B 2 0.176702 0.230210 0.491878 11.00000 -1.20000 DFIX 0.85 0.01 O13 H13a O13 H13B DFIX 1.34 0.01 H13a H13B O13 6 -0.046131 0.215846 0.252189 11.00000 0.02370 0.02515 = 0.04149 0.00504 0.01482 0.00591 AFIX 3 H13A 2 -0.074566 0.213424 0.281364 11.00000 -1.20000 H13B 2 -0.083189 0.230091 0.203111 11.00000 -1.20000 AFIX 0 N1 5 0.756197 0.377587 0.074708 11.00000 0.01430 0.02425 = 0.02059 0.00052 0.00589 0.00258 N2 5 0.741570 0.389959 0.647431 11.00000 0.02351 0.01728 = 0.02227 0.00200 0.01439 -0.00393 N3 5 1.322642 0.371201 0.646820 11.00000 0.01686 0.02549 = 0.02392 -0.00537 0.01002 -0.00472 C1 1 -0.050224 0.059426 0.443677 11.00000 0.01715 0.03677 = 0.02731 0.00331 0.01437 0.00564 C2 1 -0.147051 0.060498 0.403530 11.00000 0.02191 0.05155 = 0.03495 0.02388 0.00946 0.01036 AFIX 43 H2 2 -0.181670 0.082493 0.352736 11.00000 -1.20000 AFIX 0 C3 1 -0.189602 0.030168 0.437820 11.00000 0.01302 0.06870 = 0.04663 0.02592 0.01229 0.01303 C4 1 -0.143483 -0.001867 0.511794 11.00000 0.02227 0.05072 = 0.04559 0.02265 0.01988 0.01007 AFIX 43 H4 2 -0.175251 -0.022036 0.534677 11.00000 -1.20000 AFIX 0 C5 1 -0.046637 -0.004349 0.553868 11.00000 0.02702 0.03190 = 0.03380 0.01263 0.02065 0.00554 C6 1 -0.005746 0.025083 0.514396 11.00000 0.02114 0.03004 = 0.03544 0.00352 0.01605 -0.00007 AFIX 43 H6 2 0.057782 0.021066 0.538270 11.00000 -1.20000 AFIX 0 C7 1 -0.004208 0.089136 0.400108 11.00000 0.01498 0.02822 = 0.01947 0.00374 0.01016 0.00197 C8 1 0.798179 0.333470 0.127634 11.00000 0.03233 0.02844 = 0.01554 -0.00059 0.00481 0.00579 AFIX 43 H8 2 0.795384 0.299677 0.100811 11.00000 -1.20000 AFIX 0 C9 1 0.844214 0.338586 0.219601 11.00000 0.03467 0.02792 = 0.02033 0.00943 0.00361 0.00560 AFIX 43 H9 2 0.875877 0.308182 0.254206 11.00000 -1.20000 AFIX 0 C10 1 0.846986 0.384231 0.263431 11.00000 0.01520 0.02166 = 0.01968 0.00519 0.01091 0.00449 C11 1 0.800181 0.427564 0.209764 11.00000 0.02905 0.01392 = 0.01600 0.00306 0.00661 0.00788 AFIX 43 H11 2 0.796822 0.460361 0.236183 11.00000 -1.20000 AFIX 0 C12 1 0.758177 0.422736 0.117029 11.00000 0.03296 0.01352 = 0.02189 0.00193 0.01420 0.00786 AFIX 43 H12 2 0.729214 0.453502 0.081890 11.00000 -1.20000 AFIX 0 C13 1 0.003467 -0.041999 0.626198 11.00000 0.02201 0.03602 = 0.02926 0.01289 0.01574 0.01154 C14 1 0.754955 0.433970 0.612236 11.00000 0.03331 0.01917 = 0.02781 0.01056 0.01861 0.00460 AFIX 43 H14 2 0.728644 0.466231 0.618373 11.00000 -1.20000 AFIX 0 C15 1 0.803562 0.436944 0.567683 11.00000 0.03373 0.02683 = 0.02790 0.00195 0.02295 0.00439 AFIX 43 H15 2 0.813751 0.470569 0.548085 11.00000 -1.20000 AFIX 0 C16 1 0.837953 0.389748 0.551486 11.00000 0.01426 0.02039 = 0.02318 -0.00449 0.01101 0.00225 C17 1 0.822016 0.343146 0.587106 11.00000 0.02596 0.01910 = 0.02902 0.00240 0.01989 0.00522 AFIX 43 H17 2 0.843461 0.309544 0.579013 11.00000 -1.20000 AFIX 0 C18 1 0.775241 0.345973 0.633906 11.00000 0.02914 0.01476 = 0.02395 0.00539 0.02182 -0.00280 AFIX 43 H18 2 0.766815 0.313603 0.658138 11.00000 -1.20000 AFIX 0 C19 1 1.282902 0.419269 0.648614 11.00000 0.02177 0.02076 = 0.03212 -0.00479 0.01680 -0.00433 AFIX 43 H19 2 1.320482 0.448327 0.682214 11.00000 -1.20000 AFIX 0 C20 1 1.188053 0.426351 0.601907 11.00000 0.02169 0.02182 = 0.02940 -0.00525 0.01393 0.00020 AFIX 43 H20 2 1.162087 0.459582 0.604668 11.00000 -1.20000 AFIX 0 C21 1 1.132847 0.383892 0.551578 11.00000 0.01879 0.02379 = 0.02120 -0.00487 0.01145 0.00099 C22 1 1.175291 0.334709 0.553872 11.00000 0.02108 0.02391 = 0.02335 -0.00573 0.00646 0.00546 AFIX 43 H22 2 1.140316 0.303993 0.523988 11.00000 -1.20000 AFIX 0 C23 1 1.268125 0.332279 0.600204 11.00000 0.02831 0.02474 = 0.03236 -0.00908 0.01614 -0.00566 AFIX 43 H23 2 1.295286 0.299333 0.598256 11.00000 -1.20000 AFIX 0 C24 1 0.314050 0.178871 0.382106 11.00000 0.02902 0.02935 = 0.02371 -0.01138 0.01728 -0.01321 C25 1 0.398316 0.212381 0.413520 11.00000 0.03753 0.04348 = 0.02965 -0.01721 0.02541 -0.01532 C26 1 0.447690 0.208202 0.367669 11.00000 0.04883 0.07185 = 0.04723 -0.03746 0.03972 -0.03578 AFIX 43 H26 2 0.427192 0.186554 0.315703 11.00000 -1.20000 AFIX 0 C27 1 0.530861 0.238245 0.403038 11.00000 0.05784 0.10475 = 0.05603 -0.04103 0.04583 -0.04910 C28 1 0.553136 0.274613 0.474924 11.00000 0.04607 0.07861 = 0.04523 -0.04002 0.03429 -0.03604 AFIX 43 H28 2 0.605774 0.296390 0.496552 11.00000 -1.20000 AFIX 0 C29 1 0.497716 0.278112 0.513211 11.00000 0.03528 0.05374 = 0.03724 -0.01932 0.02360 -0.01973 C30 1 0.420149 0.248255 0.480753 11.00000 0.03120 0.02683 = 0.02677 -0.00400 0.02647 -0.00842 AFIX 43 H30 2 0.381109 0.252644 0.505479 11.00000 -1.20000 AFIX 0 C31 1 0.761831 0.467647 0.877964 11.00000 0.02868 0.02844 = 0.02614 -0.00172 0.01316 -0.00885 AFIX 43 H31 2 0.800818 0.497863 0.900393 11.00000 -1.20000 AFIX 0 C32 1 0.896099 0.387488 0.361653 11.00000 0.01841 0.02646 = 0.02063 -0.00092 0.01259 -0.00559 C33 1 0.987400 0.388543 0.408158 11.00000 0.02649 0.03289 = 0.02194 0.00508 0.01493 0.00035 C34 1 1.033900 0.388930 0.504515 11.00000 0.02655 0.02831 = 0.02118 0.00010 0.01508 0.00481 C35 1 0.984750 0.389309 0.551901 11.00000 0.02049 0.02729 = 0.02374 0.00154 0.01152 0.00193 C36 1 0.888530 0.390094 0.500591 11.00000 0.02105 0.02389 = 0.02273 -0.00084 0.00895 0.00154 C37 1 0.842017 0.388761 0.407912 11.00000 0.00699 0.03277 = 0.01730 0.00150 0.00769 0.00058 C38 1 0.525117 0.313575 0.593003 11.00000 0.02252 0.03892 = 0.03595 -0.01001 0.01950 -0.01278 C39 1 1.042216 0.391136 0.359907 11.00000 0.02259 0.05574 = 0.01693 -0.00009 0.01488 0.00547 AFIX 137 H39A 2 1.047569 0.355089 0.340201 11.00000 -1.50000 H39B 2 1.102781 0.405238 0.400582 11.00000 -1.50000 H39C 2 1.011715 0.414757 0.307762 11.00000 -1.50000 AFIX 0 C40 1 1.032074 0.388132 0.653752 11.00000 0.02903 0.05179 = 0.02437 -0.00442 0.01659 -0.00269 AFIX 137 H40A 2 1.011412 0.356829 0.673396 11.00000 -1.50000 H40B 2 1.017493 0.420899 0.675658 11.00000 -1.50000 H40C 2 1.097763 0.385910 0.677725 11.00000 -1.50000 AFIX 0 C41 1 0.740891 0.381581 0.355593 11.00000 0.01431 0.04449 = 0.01891 0.00888 0.00478 0.00691 AFIX 137 H41A 2 0.713309 0.413076 0.317649 11.00000 -1.50000 H41B 2 0.716994 0.377476 0.397045 11.00000 -1.50000 H41C 2 0.726475 0.349513 0.317994 11.00000 -1.50000 AFIX 0 HKLF 5 REM Cc_a.res in Cc REM wR2 = 0.1249, GooF = S = 0.974, Restrained GooF = 0.960 for all data REM R1 = 0.0491 for 8057 Fo > 4sig(Fo) and 0.0803 for all 10753 data REM 586 parameters refined using 634 restraints END WGHT 0.0759 0.0000 REM Highest difference peak 0.915, deepest hole -0.579, 1-sigma level 0.105 Q1 1 1.1803 0.3702 0.4292 11.00000 0.05 0.92 Q2 1 0.9668 0.3695 0.2218 11.00000 0.05 0.77 Q3 1 1.1701 0.3893 0.2236 11.00000 0.05 0.75 Q4 1 -0.0298 0.2324 0.4183 11.00000 0.05 0.69 Q5 1 0.5626 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4771.59 102.740 -2 -7 3 5 4771.59 102.740 1 5 3 0 4413.39 75.1474 -2 -5 3 5 4413.39 75.1474 1 3 3 2 2457.25 41.8605 -2 -3 3 5 2457.25 41.8605 1 1 3 4 1767.67 23.8392 -2 -1 3 5 1767.67 23.8392 1 -1 3 6 1109.82 19.4259 -2 1 3 5 1109.82 19.4259 1 -3 3 8 908.828 16.0442 -2 3 3 5 908.828 16.0442 1 -5 3 10 1073.10 14.8246 -2 5 3 5 1073.10 14.8246 1 -7 3 12 171.070 9.34949 -2 7 3 5 171.070 9.34949 1 -9 3 14 527.227 12.9010 -2 9 3 5 527.227 12.9010 1 -11 3 16 270.770 14.4599 -2 11 3 5 270.770 14.4599 1 -13 3 18 132.510 11.7131 -2 13 3 5 132.510 11.7131 1 -15 3 20 259.594 16.7745 -2 15 3 5 259.594 16.7745 1 -17 3 22 85.2750 17.8283 -2 17 3 5 85.2750 17.8283 1 19 3 5 12.9637 24.7207 1 -24 4 19 37.2004 18.2718 -2 -24 4 5 37.2004 18.2718 1 -22 4 17 9.85846 12.1651 -2 -22 4 5 9.85846 12.1651 1 -20 4 15 17.1299 8.11198 -2 -20 4 5 17.1299 8.11198 1 -18 4 13 40.1261 7.17286 -2 -18 4 5 40.1261 7.17286 1 -16 4 11 144.759 7.16502 -2 -16 4 5 144.759 7.16502 1 -14 4 9 107.516 4.98564 -2 -14 4 5 107.516 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5 5 296.989 8.32658 1 -15 5 10 577.336 9.11406 -2 -15 5 5 577.336 9.11406 1 -13 5 8 249.600 5.38496 -2 -13 5 5 249.600 5.38496 1 -11 5 6 314.772 4.84924 -2 -11 5 5 314.772 4.84924 1 -9 5 4 1208.61 22.1028 -2 -9 5 5 1208.61 22.1028 1 -7 5 2 2329.03 62.7958 -2 -7 5 5 2329.03 62.7958 1 5 5 0 2525.14 38.3660 -2 -5 5 5 2525.14 38.3660 1 3 5 2 1733.56 22.1110 -2 -3 5 5 1733.56 22.1110 1 1 5 4 1586.95 25.7640 -2 -1 5 5 1586.95 25.7640 1 -1 5 6 1253.59 21.5033 -2 1 5 5 1253.59 21.5033 1 -3 5 8 116.668 5.72125 -2 3 5 5 116.668 5.72125 1 -5 5 10 1157.32 15.4750 -2 5 5 5 1157.32 15.4750 1 -7 5 12 448.562 11.7147 -2 7 5 5 448.562 11.7147 1 -9 5 14 763.453 17.1089 -2 9 5 5 763.453 17.1089 1 -11 5 16 335.039 12.9942 -2 11 5 5 335.039 12.9942 1 -13 5 18 63.7223 12.4638 -2 13 5 5 63.7223 12.4638 1 -15 5 20 328.161 18.2039 -2 15 5 5 328.161 18.2039 1 -17 5 22 22.8759 27.3231 -2 17 5 5 22.8759 27.3231 1 19 5 5 87.1532 31.0821 1 -22 6 17 141.858 21.3085 -2 -22 6 5 141.858 21.3085 1 -20 6 15 513.857 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4 12 85.0453 13.6892 1 -20 4 8 199.137 12.8631 -2 -20 4 12 199.137 12.8631 1 -18 4 6 216.586 8.68789 -2 -18 4 12 216.586 8.68789 1 -16 4 4 666.542 11.2083 -2 -16 4 12 666.542 11.2083 1 -14 4 2 231.807 7.51701 -2 -14 4 12 231.807 7.51701 1 12 4 0 185.704 7.55819 -2 -12 4 12 185.704 7.55819 1 10 4 2 237.641 8.87264 -2 -10 4 12 237.641 8.87264 1 8 4 4 1140.06 15.5875 -2 -8 4 12 1140.06 15.5875 1 6 4 6 2044.08 33.3554 -2 -6 4 12 2044.08 33.3554 1 4 4 8 395.914 12.3383 -2 -4 4 12 395.914 12.3383 1 2 4 10 196.390 10.8780 -2 -2 4 12 196.390 10.8780 1 0 4 12 367.056 12.2007 -2 0 4 12 367.056 12.2007 1 -2 4 14 160.872 11.8775 -2 2 4 12 160.872 11.8775 1 -4 4 16 25.4844 15.4062 -2 4 4 12 25.4844 15.4062 1 -6 4 18 139.582 19.4797 -2 6 4 12 139.582 19.4797 1 -8 4 20 89.1155 21.0292 -2 8 4 12 89.1155 21.0292 1 -10 4 22 79.4114 33.3726 -2 10 4 12 79.4114 33.3726 1 12 4 12 30.5922 20.3349 1 14 4 12 -9.1567 17.6113 1 -25 5 13 93.5803 28.3210 -2 -25 5 12 93.5803 28.3210 1 -23 5 11 81.3862 24.5960 -2 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5.10 -7.39 -18 4 25 3.30 -3.71 -16 4 25 -2.37 3.75 -8 4 25 2.28 5.02 -6 4 25 -4.12 3.47 -19 5 25 3.23 -2.54 -17 5 25 -1.56 -2.24 -15 5 25 0.82 0.61 -11 5 25 -4.84 2.40 -5 5 25 1.76 6.77 -18 6 25 -2.61 -1.89 -16 6 25 -0.22 0.53 -12 6 25 -0.91 1.97 -10 6 25 -1.45 4.85 -8 6 25 -6.77 1.77 -6 6 25 -3.49 -0.66 -17 7 25 5.70 -0.60 -15 7 25 3.58 5.88 -13 7 25 -6.56 -4.04 -11 7 25 -8.27 -0.51 -18 8 25 -4.25 1.27 -16 8 25 -1.80 0.69 -10 8 25 -1.13 2.11 -8 8 25 -0.47 1.62 -6 8 25 3.78 7.43 -17 9 25 -3.22 0.73 -11 9 25 7.24 9.05 -9 9 25 1.42 3.12 -7 9 25 2.58 6.05 -16 10 25 -4.85 0.65 -12 10 25 -2.18 3.46 -10 10 25 -1.65 -3.64 -8 10 25 -1.51 3.52 -13 11 25 -1.47 4.36 -11 11 25 -1.78 -2.18 -9 11 25 -0.43 -3.17 -14 12 25 -1.08 -0.74 -12 12 25 2.64 -5.18 -10 12 25 4.97 -0.05 -13 13 25 1.94 -0.87 -11 13 25 -1.15 -1.00 -16 0 26 2.96 -1.12 -14 0 26 3.70 -3.23 -12 0 26 -1.91 -3.90 -8 0 26 -3.75 -11.32 -17 1 26 -1.54 1.48 -15 1 26 1.34 -4.15 -13 1 26 2.03 -4.73 -11 1 26 -2.91 2.73 -16 2 26 0.41 -1.25 -14 2 26 -0.50 1.22 -12 2 26 2.35 3.03 -8 2 26 -6.70 -0.74 -17 3 26 0.25 -2.57 -15 3 26 -0.85 0.34 -13 3 26 -4.34 9.13 -11 3 26 7.40 2.98 -9 3 26 -0.71 -0.38 -16 4 26 -1.94 -1.26 -14 4 26 -6.91 1.90 -12 4 26 -2.24 1.85 -10 4 26 -1.35 -1.07 -8 4 26 -1.33 -3.18 -15 5 26 -0.73 -5.53 -13 5 26 4.21 -5.24 -11 5 26 2.68 -1.23 -9 5 26 4.97 2.39 -16 6 26 -1.09 2.45 -14 6 26 2.55 -0.59 -10 6 26 -2.55 -4.82 -15 7 26 1.60 -1.52 -13 7 26 2.48 3.87 -11 7 26 -2.85 5.56 -14 8 26 4.10 -0.03 -12 8 26 -1.30 1.93 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 201118) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.149 0.446 0.013 2871 970 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 1 0 1.604 0 2 0 1.633 0 4 0 3.268 0 8 0 6.546 -1 1 1 1.608 0 2 1 2.127 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL mo_20240822A_0m_5C c R = 0.09 CELL 16.9240 24.9380 17.1410 90.00 119.33 90.00 SPGR Cc # Solvent Accessible Volume = 2881 # Electrons Found in S.A.V. = 948 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.473 0.265 0.924 ! 6.80 eA-3 Q102 0.189 0.271 0.361 ! 5.73 eA-3 C103 0.532 0.201 0.702 ! 5.47 eA-3 C104 0.184 0.384 0.237 ! 4.96 eA-3 C105 0.299 0.361 0.443 ! 4.34 eA-3 Q106 0.684 0.136 0.919 ! 4.04 eA-3 C107 0.425 0.288 0.948 ! 4.03 eA-3 C108 0.860 0.099 0.843 ! 3.99 eA-3 C109 0.486 0.427 0.363 ! 3.80 eA-3 C110 0.998 0.334 0.140 ! 3.74 eA-3 C111 0.450 0.307 0.031 ! 3.55 eA-3 Q112 0.474 0.123 0.722 ! 3.41 eA-3 C113 0.421 0.297 0.985 ! 3.23 eA-3 C114 0.734 0.179 0.718 ! 3.22 eA-3 C115 0.424 0.416 0.353 ! 3.01 eA-3 C116 0.835 0.076 0.815 ! 2.99 eA-3 C117 1.001 0.195 0.575 ! 2.91 eA-3 C118 0.628 0.245 0.793 ! 2.82 eA-3 C119 0.266 0.344 0.376 ! 2.77 eA-3 C120 0.033 0.179 0.629 ! 2.76 eA-3 C121 0.653 0.149 0.697 ! 2.70 eA-3 C122 0.054 0.026 0.830 ! 2.70 eA-3 C123 0.090 0.379 0.064 ! 2.69 eA-3 C124 0.079 0.035 0.871 ! 2.60 eA-3 C125 0.051 0.187 0.591 ! 2.60 eA-3 C126 0.112 0.389 0.173 ! 2.59 eA-3 Q127 0.606 0.482 0.358 ! 2.56 eA-3 C128 0.997 0.442 0.029 ! 2.56 eA-3 C129 0.497 0.067 0.533 ! 2.54 eA-3 C130 0.090 0.415 0.081 ! 2.51 eA-3 C131 0.754 0.180 0.813 ! 2.47 eA-3 C132 0.254 0.680 0.813 ! 2.47 eA-3 C133 0.192 0.296 0.193 ! 2.45 eA-3 C134 0.861 0.179 0.533 ! 2.44 eA-3 Q135 0.157 0.398 0.312 ! 2.42 eA-3 C136 0.918 0.227 0.549 ! 2.42 eA-3 C137 0.766 0.155 0.781 ! 2.40 eA-3 C138 0.550 0.107 0.560 ! 2.40 eA-3 C139 0.329 0.388 0.391 ! 2.40 eA-3 Q140 0.811 0.168 0.903 ! 2.36 eA-3 C141 0.552 0.122 0.514 ! 2.36 eA-3 C142 0.544 0.123 0.625 ! 2.36 eA-3 Q143 0.295 0.319 0.361 ! 2.36 eA-3 C144 0.574 0.014 0.626 ! 2.35 eA-3 C145 0.308 0.330 0.265 ! 2.34 eA-3 C146 0.919 0.161 0.582 ! 2.32 eA-3 C147 0.028 0.419 0.032 ! 2.30 eA-3 C148 0.072 0.065 0.711 ! 2.30 eA-3 Q149 0.565 0.380 0.441 ! 2.28 eA-3 C150 0.499 0.382 0.205 ! 2.26 eA-3 Q151 0.447 0.271 0.860 ! 2.23 eA-3 C152 0.976 0.430 0.063 ! 2.22 eA-3 C153 0.065 0.115 0.934 ! 2.22 eA-3 C154 0.378 0.444 0.269 ! 2.22 eA-3 C155 0.097 0.324 0.140 ! 2.19 eA-3 C156 0.498 0.073 0.601 ! 2.15 eA-3 C157 0.391 0.344 0.018 ! 2.14 eA-3 C158 0.393 0.429 0.313 ! 2.14 eA-3 C159 0.111 0.329 0.187 ! 2.13 eA-3 C160 0.481 0.407 0.439 ! 2.12 eA-3 C161 0.134 0.334 0.155 ! 2.11 eA-3 C162 0.496 0.229 0.942 ! 2.11 eA-3 C163 0.061 0.086 0.938 ! 2.11 eA-3 C164 0.470 0.296 0.094 ! 2.11 eA-3 C165 0.703 0.143 0.623 ! 2.11 eA-3 C166 0.814 0.179 0.467 ! 2.10 eA-3 Q167 0.612 0.143 0.780 ! 2.10 eA-3 C168 0.888 0.052 0.832 ! 2.08 eA-3 C169 0.359 0.408 0.394 ! 2.08 eA-3 C170 0.766 0.198 0.659 ! 2.07 eA-3 C171 0.092 0.185 0.591 ! 2.07 eA-3 C172 0.279 0.391 0.342 ! 2.07 eA-3 C173 0.813 0.215 0.405 ! 2.07 eA-3 C174 0.249 0.363 0.296 ! 2.06 eA-3 C175 0.066 0.352 0.095 ! 2.05 eA-3 Q176 0.081 0.188 0.530 ! 2.05 eA-3 C177 0.156 0.366 0.109 ! 2.04 eA-3 C178 0.643 0.196 0.684 ! 2.03 eA-3 C179 0.973 0.101 0.795 ! 2.03 eA-3 C180 0.213 0.323 0.233 ! 2.01 eA-3 C181 0.282 0.369 0.342 ! 2.01 eA-3 C182 0.876 0.092 0.793 ! 2.01 eA-3 C183 0.970 0.075 0.894 ! 2.00 eA-3 C184 0.515 0.401 0.387 ! 2.00 eA-3 C185 0.361 0.267 0.906 ! 1.99 eA-3 Q186 0.454 0.045 0.453 ! 1.98 eA-3 C187 0.107 0.371 0.127 ! 1.97 eA-3 Q188 0.457 0.393 0.094 ! 1.97 eA-3 C189 0.375 0.352 0.111 ! 1.97 eA-3 Q190 0.377 0.017 0.408 ! 1.96 eA-3 C191 0.622 0.081 0.688 ! 1.96 eA-3 C192 0.568 0.307 0.173 ! 1.94 eA-3 Q193 1.004 0.461 0.716 ! 1.93 eA-3 C194 0.343 0.447 0.200 ! 1.93 eA-3 Q195 0.214 0.374-0.001 ! 1.93 eA-3 C196 0.793 0.154 0.842 ! 1.93 eA-3 C197 0.463 0.066 0.309 ! 1.92 eA-3 C198 0.609 0.253 0.170 ! 1.92 eA-3 C199 0.487 0.089 0.529 ! 1.92 eA-3 ) ; _shelx_fab_checksum 98969 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -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 Br1 Br -0.3174(2) 0.0348(5) 0.3840(7) 0.081(2) Uani 0.78(3) 1 d D U P A 1 Br1A Br -0.3067(13) 0.0538(13) 0.4080(19) 0.073(4) Uani 0.22(3) 1 d D U P A 2 Br2 Br 0.6139(5) 0.2232(5) 0.3577(7) 0.088(2) Uani 0.532(19) 1 d D U P B 1 Br2A Br 0.5804(8) 0.2503(5) 0.3248(7) 0.092(3) Uani 0.468(19) 1 d D U P B 2 Co1 Co 0.181405 0.127009 0.430428 0.01600(15) Uani 1 1 d . . . . . Co2 Co 0.67195(7) 0.38767(3) 0.72462(8) 0.01474(17) Uani 1 1 d . . . . . Co3 Co -0.03243(7) 0.13378(4) 0.21926(8) 0.01603(18) Uani 1 1 d D . . . . O1 O 0.0807(3) 0.0916(2) 0.4472(4) 0.0279(11) Uani 1 1 d . U . . . O2 O 0.0779(3) -0.0583(2) 0.6366(4) 0.0285(11) Uani 1 1 d . U . . . O3 O -0.0524(3) 0.1084(2) 0.3255(3) 0.0234(10) Uani 1 1 d . U . . . O4 O 0.1067(3) 0.13851(16) 0.2952(3) 0.0159(9) Uani 1 1 d . . . . . H4X H 0.113426 0.172170 0.293102 0.019 Uiso 1 1 calc R U . . . O5 O 0.2912(4) 0.1682(2) 0.4388(4) 0.0303(11) Uani 1 1 d . U . . . O6 O 0.7374(4) 0.4483(2) 0.9296(4) 0.0308(11) Uani 1 1 d . U . . . O7 O 0.7425(4) 0.4532(2) 0.8009(4) 0.0319(12) Uani 1 1 d . U . . . O8 O -0.0331(3) -0.05731(19) 0.6726(4) 0.0250(10) Uani 1 1 d . U . . . O9 O 0.2773(4) 0.1639(2) 0.3022(4) 0.0302(12) Uani 1 1 d . U . . . O10 O 0.6087(4) 0.3239(2) 0.6395(4) 0.0300(11) Uani 1 1 d . U . . . O11 O 0.4628(3) 0.3312(2) 0.6058(4) 0.0281(11) Uani 1 1 d . U . . . O12 O 0.1455(4) 0.2075(2) 0.4516(4) 0.0307(12) Uani 1 1 d D . . . . H12A H 0.130(6) 0.224(2) 0.4027(14) 0.037 Uiso 1 1 d D U . . . H12B H 0.1767(19) 0.2302(10) 0.4919(18) 0.037 Uiso 1 1 d D U . . . O13 O -0.0461(3) 0.21585(17) 0.2522(4) 0.0306(12) Uani 1 1 d D . . . . H13A H -0.074566 0.213424 0.281364 0.037 Uiso 1 1 d DR U . . . H13B H -0.083189 0.230091 0.203111 0.037 Uiso 1 1 d DR U . . . N1 N 0.7562(4) 0.3776(2) 0.0747(4) 0.0209(10) Uani 1 1 d . U . . . N2 N 0.7416(4) 0.3900(2) 0.6474(4) 0.0197(11) Uani 1 1 d . U . . . N3 N 1.3226(4) 0.3712(2) 0.6468(5) 0.0221(12) Uani 1 1 d . U . . . C1 C -0.0502(4) 0.0594(3) 0.4437(5) 0.0256(13) Uani 1 1 d . U . . . C2 C -0.1471(5) 0.0605(4) 0.4035(6) 0.0381(17) Uani 1 1 d . U . . . H2 H -0.181670 0.082493 0.352736 0.046 Uiso 1 1 calc R U . . . C3 C -0.1896(5) 0.0302(4) 0.4378(7) 0.0438(18) Uani 1 1 d D U . . . C4 C -0.1435(5) -0.0019(4) 0.5118(6) 0.0381(17) Uani 1 1 d . U . . . H4 H -0.175251 -0.022036 0.534677 0.046 Uiso 1 1 calc R U . . . C5 C -0.0466(5) -0.0043(3) 0.5539(6) 0.0284(13) Uani 1 1 d . U . . . C6 C -0.0057(5) 0.0251(3) 0.5144(6) 0.0279(14) Uani 1 1 d . U . . . H6 H 0.057782 0.021066 0.538270 0.034 Uiso 1 1 calc R U . . . C7 C -0.0042(4) 0.0891(3) 0.4001(5) 0.0201(12) Uani 1 1 d . U . . . C8 C 0.7982(5) 0.3335(3) 0.1276(5) 0.0284(15) Uani 1 1 d . U . . . H8 H 0.795384 0.299677 0.100811 0.034 Uiso 1 1 calc R U . . . C9 C 0.8442(5) 0.3386(3) 0.2196(5) 0.0319(15) Uani 1 1 d . U . . . H9 H 0.875877 0.308182 0.254206 0.038 Uiso 1 1 calc R U . . . C10 C 0.8470(4) 0.3842(2) 0.2634(4) 0.0178(11) Uani 1 1 d . U . . . C11 C 0.8002(5) 0.4276(2) 0.2098(5) 0.0216(13) Uani 1 1 d . U . . . H11 H 0.796822 0.460361 0.236183 0.026 Uiso 1 1 calc R U . . . C12 C 0.7582(5) 0.4227(2) 0.1170(5) 0.0225(13) Uani 1 1 d . U . . . H12 H 0.729214 0.453502 0.081890 0.027 Uiso 1 1 calc R U . . . C13 C 0.0035(5) -0.0420(3) 0.6262(5) 0.0277(13) Uani 1 1 d . U . . . C14 C 0.7550(5) 0.4340(3) 0.6122(5) 0.0252(14) Uani 1 1 d . U . . . H14 H 0.728644 0.466231 0.618373 0.030 Uiso 1 1 calc R U . . . C15 C 0.8036(5) 0.4369(3) 0.5677(5) 0.0261(13) Uani 1 1 d . U . . . H15 H 0.813751 0.470569 0.548085 0.031 Uiso 1 1 calc R U . . . C16 C 0.8380(4) 0.3897(3) 0.5515(5) 0.0185(11) Uani 1 1 d . U . . . C17 C 0.8220(5) 0.3431(3) 0.5871(5) 0.0219(12) Uani 1 1 d . U . . . H17 H 0.843461 0.309544 0.579013 0.026 Uiso 1 1 calc R U . . . C18 C 0.7752(4) 0.3460(2) 0.6339(5) 0.0188(12) Uani 1 1 d . U . . . H18 H 0.766815 0.313603 0.658138 0.023 Uiso 1 1 calc R U . . . C19 C 1.2829(4) 0.4193(3) 0.6486(5) 0.0233(13) Uani 1 1 d . U . . . H19 H 1.320482 0.448327 0.682214 0.028 Uiso 1 1 calc R U . . . C20 C 1.1881(5) 0.4264(3) 0.6019(5) 0.0237(13) Uani 1 1 d . U . . . H20 H 1.162087 0.459582 0.604668 0.028 Uiso 1 1 calc R U . . . C21 C 1.1328(4) 0.3839(3) 0.5516(5) 0.0205(12) Uani 1 1 d . U . . . C22 C 1.1753(4) 0.3347(3) 0.5539(5) 0.0247(14) Uani 1 1 d . U . . . H22 H 1.140316 0.303993 0.523988 0.030 Uiso 1 1 calc R U . . . C23 C 1.2681(4) 0.3323(3) 0.6002(5) 0.0279(14) Uani 1 1 d . U . . . H23 H 1.295286 0.299333 0.598256 0.034 Uiso 1 1 calc R U . . . C24 C 0.3140(5) 0.1789(3) 0.3821(5) 0.0255(13) Uani 1 1 d . U . . . C25 C 0.3983(5) 0.2124(3) 0.4135(6) 0.0330(15) Uani 1 1 d . U . . . C26 C 0.4477(7) 0.2082(4) 0.3677(7) 0.049(2) Uani 1 1 d . U . . . H26 H 0.427192 0.186554 0.315703 0.059 Uiso 1 1 calc R U . . . C27 C 0.5309(7) 0.2382(5) 0.4030(8) 0.065(2) Uani 1 1 d D U . . . C28 C 0.5531(7) 0.2746(5) 0.4749(7) 0.052(2) Uani 1 1 d . U . . . H28 H 0.605774 0.296390 0.496552 0.062 Uiso 1 1 calc R U . . . C29 C 0.4977(6) 0.2781(4) 0.5132(6) 0.0396(16) Uani 1 1 d . U . . . C30 C 0.4201(5) 0.2483(3) 0.4808(5) 0.0230(12) Uani 1 1 d . U . . . H30 H 0.381109 0.252644 0.505479 0.028 Uiso 1 1 calc R U . . . C31 C 0.7618(5) 0.4676(3) 0.8780(5) 0.0279(14) Uani 1 1 d . U . . . H31 H 0.800818 0.497863 0.900393 0.033 Uiso 1 1 calc R U . . . C32 C 0.8961(4) 0.3875(2) 0.3617(5) 0.0205(11) Uani 1 1 d . U . . . C33 C 0.9874(5) 0.3885(3) 0.4082(5) 0.0258(13) Uani 1 1 d . U . . . C34 C 1.0339(5) 0.3889(3) 0.5045(5) 0.0239(12) Uani 1 1 d . U . . . C35 C 0.9847(5) 0.3893(3) 0.5519(5) 0.0235(13) Uani 1 1 d . U . . . C36 C 0.8885(5) 0.3901(3) 0.5006(5) 0.0233(12) Uani 1 1 d . U . . . C37 C 0.8420(4) 0.3888(3) 0.4079(4) 0.0183(11) Uani 1 1 d . U . . . C38 C 0.5251(5) 0.3136(3) 0.5930(6) 0.0302(14) Uani 1 1 d . U . . . C39 C 1.0422(4) 0.3911(3) 0.3599(4) 0.0295(15) Uani 1 1 d . U . . . H39A H 1.047569 0.355089 0.340201 0.044 Uiso 1 1 calc R U . . . H39B H 1.102781 0.405238 0.400582 0.044 Uiso 1 1 calc R U . . . H39C H 1.011715 0.414757 0.307762 0.044 Uiso 1 1 calc R U . . . C40 C 1.0321(5) 0.3881(3) 0.6538(5) 0.0336(18) Uani 1 1 d . U . . . H40A H 1.011412 0.356829 0.673396 0.050 Uiso 1 1 calc R U . . . H40B H 1.017493 0.420899 0.675658 0.050 Uiso 1 1 calc R U . . . H40C H 1.097763 0.385910 0.677725 0.050 Uiso 1 1 calc R U . . . C41 C 0.7409(4) 0.3816(3) 0.3556(5) 0.0273(15) Uani 1 1 d . U . . . H41A H 0.713309 0.413076 0.317649 0.041 Uiso 1 1 calc R U . . . H41B H 0.716994 0.377476 0.397045 0.041 Uiso 1 1 calc R U . . . H41C H 0.726475 0.349513 0.317994 0.041 Uiso 1 1 calc R U . . . 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 Br1 0.0141(7) 0.127(4) 0.087(3) 0.080(3) 0.0143(12) 0.0116(13) Br1A 0.021(3) 0.105(8) 0.092(8) 0.055(7) 0.026(4) 0.024(4) Br2 0.061(2) 0.144(5) 0.093(4) -0.087(4) 0.065(3) -0.063(3) Br2A 0.082(4) 0.148(6) 0.090(3) -0.082(4) 0.077(3) -0.078(4) Co1 0.0149(4) 0.0189(3) 0.0136(4) 0.0005(4) 0.0065(4) -0.0011(3) Co2 0.0122(3) 0.0163(3) 0.0141(4) 0.0010(4) 0.0051(3) 0.0000(3) Co3 0.0106(4) 0.0207(4) 0.0143(5) 0.0020(4) 0.0042(4) 0.0025(3) O1 0.021(2) 0.044(3) 0.021(3) 0.006(2) 0.012(2) -0.003(2) O2 0.018(2) 0.045(3) 0.023(3) 0.021(2) 0.0102(19) 0.010(2) O3 0.0165(19) 0.031(2) 0.022(3) 0.007(2) 0.0092(18) 0.0057(18) O4 0.0175(19) 0.019(2) 0.010(2) 0.0009(15) 0.0055(17) 0.0043(16) O5 0.035(3) 0.036(2) 0.022(3) -0.003(2) 0.015(2) -0.017(2) O6 0.034(3) 0.030(2) 0.030(3) -0.011(2) 0.017(2) -0.005(2) O7 0.044(3) 0.023(2) 0.028(3) -0.013(2) 0.017(2) -0.022(2) O8 0.022(2) 0.027(2) 0.028(3) 0.014(2) 0.014(2) 0.0040(18) O9 0.032(3) 0.045(3) 0.020(3) -0.022(2) 0.018(2) -0.020(2) O10 0.030(2) 0.032(2) 0.036(3) -0.019(2) 0.022(2) -0.018(2) O11 0.020(2) 0.038(3) 0.035(3) -0.006(2) 0.020(2) -0.0091(19) O12 0.034(3) 0.022(2) 0.042(4) -0.001(2) 0.023(3) 0.001(2) O13 0.024(2) 0.025(2) 0.041(3) 0.005(2) 0.015(2) 0.0059(18) N1 0.014(2) 0.024(2) 0.021(2) 0.001(2) 0.006(2) 0.0026(19) N2 0.024(2) 0.017(2) 0.022(3) 0.002(2) 0.014(2) -0.004(2) N3 0.017(2) 0.025(2) 0.024(3) -0.005(2) 0.010(2) -0.005(2) C1 0.017(2) 0.037(3) 0.027(3) 0.003(3) 0.014(2) 0.006(2) C2 0.022(3) 0.052(4) 0.035(4) 0.024(3) 0.009(3) 0.010(3) C3 0.013(3) 0.069(4) 0.047(4) 0.026(4) 0.012(3) 0.013(3) C4 0.022(3) 0.051(4) 0.046(4) 0.023(3) 0.020(3) 0.010(3) C5 0.027(3) 0.032(3) 0.034(3) 0.013(3) 0.021(3) 0.006(2) C6 0.021(3) 0.030(3) 0.035(4) 0.004(3) 0.016(3) 0.000(2) C7 0.015(2) 0.028(3) 0.019(3) 0.004(2) 0.010(2) 0.002(2) C8 0.032(3) 0.028(3) 0.016(3) -0.001(3) 0.005(3) 0.006(3) C9 0.035(3) 0.028(3) 0.020(3) 0.009(3) 0.004(3) 0.006(3) C10 0.015(2) 0.022(3) 0.020(3) 0.005(2) 0.011(2) 0.004(2) C11 0.029(3) 0.014(2) 0.016(3) 0.003(2) 0.007(2) 0.008(2) C12 0.033(3) 0.014(2) 0.022(3) 0.002(2) 0.014(3) 0.008(2) C13 0.022(3) 0.036(3) 0.029(3) 0.013(3) 0.016(2) 0.012(2) C14 0.033(3) 0.019(3) 0.028(3) 0.011(3) 0.019(3) 0.005(2) C15 0.034(3) 0.027(3) 0.028(3) 0.002(3) 0.023(3) 0.004(3) C16 0.014(2) 0.020(2) 0.023(3) -0.004(2) 0.011(2) 0.002(2) C17 0.026(3) 0.019(3) 0.029(3) 0.002(3) 0.020(3) 0.005(2) C18 0.029(3) 0.015(2) 0.024(3) 0.005(2) 0.022(3) -0.003(2) C19 0.022(3) 0.021(3) 0.032(3) -0.005(3) 0.017(3) -0.004(2) C20 0.022(3) 0.022(3) 0.029(3) -0.005(3) 0.014(3) 0.000(2) C21 0.019(2) 0.024(3) 0.021(3) -0.005(2) 0.011(2) 0.001(2) C22 0.021(3) 0.024(3) 0.023(3) -0.006(3) 0.006(2) 0.005(2) C23 0.028(3) 0.025(3) 0.032(3) -0.009(3) 0.016(3) -0.006(2) C24 0.029(3) 0.029(3) 0.024(3) -0.011(3) 0.017(2) -0.013(2) C25 0.038(3) 0.043(3) 0.030(3) -0.017(3) 0.025(3) -0.015(3) C26 0.049(4) 0.072(5) 0.047(4) -0.037(4) 0.040(3) -0.036(4) C27 0.058(4) 0.105(5) 0.056(5) -0.041(4) 0.046(4) -0.049(4) C28 0.046(4) 0.079(5) 0.045(4) -0.040(4) 0.034(3) -0.036(4) C29 0.035(3) 0.054(4) 0.037(4) -0.019(3) 0.024(3) -0.020(3) C30 0.031(3) 0.027(3) 0.027(3) -0.004(2) 0.026(3) -0.008(2) C31 0.029(3) 0.028(3) 0.026(3) -0.002(3) 0.013(3) -0.009(2) C32 0.018(2) 0.026(3) 0.021(3) -0.001(2) 0.013(2) -0.006(2) C33 0.026(3) 0.033(3) 0.022(3) 0.005(3) 0.015(2) 0.000(3) C34 0.027(3) 0.028(3) 0.021(3) 0.000(3) 0.015(2) 0.005(2) C35 0.020(3) 0.027(3) 0.024(3) 0.002(2) 0.012(2) 0.002(2) C36 0.021(2) 0.024(2) 0.023(3) -0.001(3) 0.009(2) 0.002(2) C37 0.007(2) 0.033(3) 0.017(3) 0.001(2) 0.008(2) 0.001(2) C38 0.023(3) 0.039(3) 0.036(3) -0.010(3) 0.020(3) -0.013(2) C39 0.023(3) 0.056(4) 0.017(3) 0.000(3) 0.015(3) 0.005(3) C40 0.029(3) 0.052(5) 0.024(4) -0.004(3) 0.017(3) -0.003(3) C41 0.014(3) 0.044(4) 0.019(4) 0.009(3) 0.005(3) 0.007(3) 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' Br Br -0.2901 2.4595 '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' 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' 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 O4 Co1 O1 97.2(2) . . ? O4 Co1 O5 92.5(2) . . ? O1 Co1 O5 168.7(2) . . ? O4 Co1 O6 98.50(19) . 4_454 ? O1 Co1 O6 91.4(2) . 4_454 ? O5 Co1 O6 92.9(2) . 4_454 ? O4 Co1 N1 174.5(2) . 4_455 ? O1 Co1 N1 83.0(2) . 4_455 ? O5 Co1 N1 86.8(2) . 4_455 ? O6 Co1 N1 87.0(2) 4_454 4_455 ? O4 Co1 O12 89.5(2) . . ? O1 Co1 O12 93.1(2) . . ? O5 Co1 O12 81.1(2) . . ? O6 Co1 O12 170.2(2) 4_454 . ? N1 Co1 O12 85.0(2) 4_455 . ? O2 Co2 O10 92.2(3) 3 . ? O2 Co2 O7 86.9(2) 3 . ? O10 Co2 O7 173.3(2) . . ? O2 Co2 O9 171.0(2) 3 4 ? O10 Co2 O9 87.8(2) . 4 ? O7 Co2 O9 92.0(2) . 4 ? O2 Co2 O4 100.90(18) 3 4 ? O10 Co2 O4 85.99(19) . 4 ? O7 Co2 O4 100.7(2) . 4 ? O9 Co2 O4 88.11(19) 4 4 ? O2 Co2 N2 89.5(2) 3 . ? O10 Co2 N2 80.7(2) . . ? O7 Co2 N2 92.7(2) . . ? O9 Co2 N2 81.6(2) 4 . ? O4 Co2 N2 163.4(2) 4 . ? O4 Co3 O8 94.89(18) . 2_554 ? O4 Co3 O11 94.29(18) . 4_454 ? O8 Co3 O11 92.0(2) 2_554 4_454 ? O4 Co3 O3 95.10(18) . . ? O8 Co3 O3 94.8(2) 2_554 . ? O11 Co3 O3 167.87(18) 4_454 . ? O4 Co3 N3 177.0(2) . 4_354 ? O8 Co3 N3 86.2(2) 2_554 4_354 ? O11 Co3 N3 88.5(2) 4_454 4_354 ? O3 Co3 N3 82.0(2) . 4_354 ? O4 Co3 O13 90.95(17) . . ? O8 Co3 O13 172.9(2) 2_554 . ? O11 Co3 O13 83.6(2) 4_454 . ? O3 Co3 O13 88.6(2) . . ? N3 Co3 O13 88.1(2) 4_354 . ? C7 O1 Co1 133.9(5) . . ? C13 O2 Co2 132.7(5) . 3_445 ? C7 O3 Co3 135.4(4) . . ? Co1 O4 Co3 126.0(2) . . ? Co1 O4 Co2 113.7(2) . 4_454 ? Co3 O4 Co2 112.3(2) . 4_454 ? C24 O5 Co1 132.0(5) . . ? C31 O6 Co1 131.2(5) . 4 ? C31 O7 Co2 131.9(5) . . ? C13 O8 Co3 127.0(5) . 2 ? C24 O9 Co2 134.4(5) . 4_454 ? C38 O10 Co2 129.4(5) . . ? C38 O11 Co3 130.8(5) . 4 ? C12 N1 C8 116.6(6) . . ? C12 N1 Co1 120.9(5) . 4_554 ? C8 N1 Co1 122.3(5) . 4_554 ? C18 N2 C14 115.3(6) . . ? C18 N2 Co2 120.1(4) . . ? C14 N2 Co2 124.5(5) . . ? C23 N3 C19 116.9(6) . . ? C23 N3 Co3 125.2(5) . 4_655 ? C19 N3 Co3 118.0(4) . 4_655 ? C6 C1 C2 116.1(6) . . ? C6 C1 C7 123.4(6) . . ? C2 C1 C7 119.9(6) . . ? C3 C2 C1 120.3(7) . . ? C2 C3 C4 122.7(7) . . ? C2 C3 Br1A 114.8(9) . . ? C4 C3 Br1A 118.6(9) . . ? C2 C3 Br1 118.4(6) . . ? C4 C3 Br1 118.8(6) . . ? C3 C4 C5 118.9(7) . . ? C6 C5 C4 116.8(7) . . ? C6 C5 C13 122.3(6) . . ? C4 C5 C13 120.2(6) . . ? C1 C6 C5 124.9(6) . . ? O3 C7 O1 128.0(6) . . ? O3 C7 C1 117.8(5) . . ? O1 C7 C1 114.2(6) . . ? C9 C8 N1 119.8(7) . . ? C10 C9 C8 124.0(7) . . ? C9 C10 C11 115.7(6) . . ? C9 C10 C32 122.0(6) . . ? C11 C10 C32 122.3(6) . . ? C10 C11 C12 119.7(6) . . ? N1 C12 C11 123.9(6) . . ? O2 C13 O8 125.0(6) . . ? O2 C13 C5 117.3(6) . . ? O8 C13 C5 117.7(6) . . ? N2 C14 C15 125.6(7) . . ? C14 C15 C16 119.1(7) . . ? C17 C16 C15 115.1(6) . . ? C17 C16 C36 123.3(6) . . ? C15 C16 C36 121.6(6) . . ? C18 C17 C16 120.0(6) . . ? N2 C18 C17 124.8(6) . . ? N3 C19 C20 121.8(6) . . ? C21 C20 C19 119.1(6) . . ? C20 C21 C22 117.7(6) . . ? C20 C21 C34 120.9(6) . . ? C22 C21 C34 121.2(6) . . ? C23 C22 C21 118.5(6) . . ? N3 C23 C22 125.9(7) . . ? O5 C24 O9 128.0(6) . . ? O5 C24 C25 116.3(6) . . ? O9 C24 C25 115.7(6) . . ? C30 C25 C26 122.3(7) . . ? C30 C25 C24 119.0(6) . . ? C26 C25 C24 118.5(6) . . ? C25 C26 C27 116.9(8) . . ? C28 C27 C26 119.0(8) . . ? C28 C27 Br2A 118.9(7) . . ? C26 C27 Br2A 117.3(7) . . ? C28 C27 Br2 122.1(7) . . ? C26 C27 Br2 118.6(7) . . ? C29 C28 C27 119.7(8) . . ? C30 C29 C28 120.7(7) . . ? C30 C29 C38 119.9(7) . . ? C28 C29 C38 119.4(7) . . ? C25 C30 C29 120.7(6) . . ? O6 C31 O7 129.4(6) . . ? C33 C32 C10 121.3(6) . . ? C33 C32 C37 121.0(6) . . ? C10 C32 C37 117.7(5) . . ? C32 C33 C34 120.2(6) . . ? C32 C33 C39 120.6(6) . . ? C34 C33 C39 119.2(6) . . ? C35 C34 C33 120.8(6) . . ? C35 C34 C21 121.2(6) . . ? C33 C34 C21 117.8(6) . . ? C34 C35 C36 117.4(6) . . ? C34 C35 C40 122.0(6) . . ? C36 C35 C40 120.6(6) . . ? C37 C36 C35 123.0(6) . . ? C37 C36 C16 120.3(6) . . ? C35 C36 C16 116.7(6) . . ? C36 C37 C32 117.6(5) . . ? C36 C37 C41 121.9(6) . . ? C32 C37 C41 120.1(6) . . ? O11 C38 O10 126.4(7) . . ? O11 C38 C29 117.1(7) . . ? O10 C38 C29 116.5(6) . . ? 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 Br1 C3 1.895(7) . ? Br1A C3 1.882(10) . ? Br2 C27 1.946(10) . ? Br2A C27 1.921(10) . ? Co1 O4 2.046(4) . ? Co1 O1 2.062(5) . ? Co1 O5 2.066(5) . ? Co1 O6 2.106(5) 4_454 ? Co1 N1 2.160(6) 4_455 ? Co1 O12 2.177(5) . ? Co2 O2 2.066(5) 3 ? Co2 O10 2.068(5) . ? Co2 O7 2.068(5) . ? Co2 O9 2.068(5) 4 ? Co2 O4 2.101(4) 4 ? Co2 N2 2.161(6) . ? Co3 O4 2.062(5) . ? Co3 O8 2.066(5) 2_554 ? Co3 O11 2.095(6) 4_454 ? Co3 O3 2.106(5) . ? Co3 N3 2.143(6) 4_354 ? Co3 O13 2.165(4) . ? O1 C7 1.259(8) . ? O2 C13 1.252(8) . ? O3 C7 1.228(9) . ? O5 C24 1.237(9) . ? O6 C31 1.244(9) . ? O7 C31 1.249(9) . ? O8 C13 1.283(8) . ? O9 C24 1.252(9) . ? O10 C38 1.263(9) . ? O11 C38 1.259(8) . ? N1 C12 1.331(9) . ? N1 C8 1.381(9) . ? N2 C18 1.308(9) . ? N2 C14 1.324(8) . ? N3 C23 1.308(9) . ? N3 C19 1.382(9) . ? C1 C6 1.370(11) . ? C1 C2 1.434(9) . ? C1 C7 1.511(9) . ? C2 C3 1.360(12) . ? C3 C4 1.373(12) . ? C4 C5 1.433(10) . ? C5 C6 1.391(9) . ? C5 C13 1.452(10) . ? C8 C9 1.380(11) . ? C9 C10 1.352(10) . ? C10 C11 1.388(8) . ? C10 C32 1.470(9) . ? C11 C12 1.393(10) . ? C14 C15 1.371(9) . ? C15 C16 1.400(9) . ? C16 C17 1.399(9) . ? C16 C36 1.492(9) . ? C17 C18 1.377(8) . ? C19 C20 1.411(9) . ? C20 C21 1.396(9) . ? C21 C22 1.412(9) . ? C21 C34 1.465(9) . ? C22 C23 1.371(9) . ? C24 C25 1.507(10) . ? C25 C30 1.359(10) . ? C25 C26 1.404(10) . ? C26 C27 1.440(12) . ? C27 C28 1.424(14) . ? C28 C29 1.386(11) . ? C29 C30 1.368(10) . ? C29 C38 1.499(11) . ? C32 C33 1.348(9) . ? C32 C37 1.476(8) . ? C33 C34 1.440(11) . ? C33 C39 1.517(9) . ? C34 C35 1.419(9) . ? C35 C36 1.422(9) . ? C35 C40 1.523(11) . ? C36 C37 1.385(10) . ? C37 C41 1.504(9) . ?