#------------------------------------------------------------------------------ #$Date: 2020-06-05 13:20:13 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252738 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557908.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_1557908 loop_ _publ_author_name 'Doheny, Patrick W.' 'Clegg, Jack K.' 'Tuna, Floriana' 'Collison, David' 'Kepert, Cameron J.' 'D'Alessandro, Deanna M.' _publ_section_title ; Quantification of the mixed-valence and intervalence charge transfer properties of a cofacial metal--organic framework via single crystal electronic absorption spectroscopy ; _journal_issue 20 _journal_name_full 'Chemical Science' _journal_page_first 5213 _journal_paper_doi 10.1039/D0SC01521K _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C32 H18 Cd N4 O4 S3, 2(C1.5 H3.5 N0.5 O0.5), 0.5(C3 H7 N O)' _chemical_formula_sum 'C38 H32 Cd N6 O6 S3' _chemical_formula_weight 877.27 _chemical_name_systematic CdTzTz _space_group_crystal_system orthorhombic _space_group_IT_number 54 _space_group_name_Hall '-P 2a 2ac' _space_group_name_H-M_alt 'P c c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-03-05 deposited with the CCDC. 2020-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 19.0673(3) _cell_length_b 26.1197(6) _cell_length_c 15.5005(3) _cell_measurement_reflns_used 17681 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.409 _cell_measurement_theta_min 2.622 _cell_volume 7719.7(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)' _computing_molecular_graphics 'ShelXle-Rev929 (H\"ubschle et al., 2008)' _computing_publication_material 'ShelXle-Rev929 (H\"ubschle et al., 2008)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 300K' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_unetI/netI 0.0200 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 92102 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.274 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.510 _exptl_crystal_description Plate _exptl_crystal_F_000 3568 _exptl_crystal_size_max 0.183 _exptl_crystal_size_mid 0.164 _exptl_crystal_size_min 0.016 _refine_diff_density_max 6.132 _refine_diff_density_min -1.088 _refine_diff_density_rms 0.173 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 659 _refine_ls_number_reflns 6828 _refine_ls_number_restraints 706 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0804 _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^)+(0.1359P)^2^+38.6114P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2123 _refine_ls_wR_factor_ref 0.2173 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6136 _reflns_number_total 6828 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01521k2.cif _cod_data_source_block CdTzTz_a _cod_depositor_comments 'Adding full bibliography for 1557908--1557909.cif.' _cod_database_code 1557908 _shelx_shelxl_version_number 2018/3 _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 0.870 _shelx_estimated_absorpt_t_max 0.988 _shelx_res_file ; TITL Pcca_a.res in Pcca Pcca_a.res created by SHELXL-2018/3 at 14:07:38 on 24-Oct-2019 REM Old TITL Pcca in Pcca REM SHELXT solution in Pcca: R1 0.208, Rweak 0.004, Alpha 0.045 REM 2.830 for 738 systematic absences, Orientation as input REM Formula found by SHELXT: C74 N12 O13 S6 Cd2 CELL 0.71073 19.0673 26.1197 15.5005 90 90 90 ZERR 8 0.0003 0.0006 0.0003 0 0 0 LATT 1 SYMM 0.5-X,-Y,+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,-Y,0.5-Z SFAC C H Cd N O S UNIT 304 256 8 48 48 24 SADI S3A C21 S3 C21 S2A C18 S2 C18 SADI N2A C18 N2 C18 N3A C21 N3 C21 SADI S2 C20 S3A C19A S2A C20A S3 C19 SADI N2 C19 N3A C20A N3 C20 N2A C19A SADI C20A C19A C20 C19 SADI C27 C26 C27 C26A C25A C22 C25 C22 SADI C26 C25 C26A C25A SADI O5 C33 O6 C38 O7 C39 SADI N5 C33 N6 C38 N7 C39 SADI N5 C34 N5 C35 N6 C36 N6 C37 N7 C41 N7 C40 SADI C41 C39 C39 C40 C36 C38 C38 C37 C34 C33 C33 C35 SADI O5 N5 O6 N6 O7 N7 SADI C34 C35 C36 C37 C41 C40 SADI N6A C38A N6 C38 SADI O6A C38A O6 C38 SADI O6A N6A N6 O6 SADI C36 C38 C38 C37 SADI N6A C37A N6 C37 N6A C36A N6 C36 SADI C36A C38A C38A C37A SADI C36A C37A C37 C36 FLAT C38 O6 N6 C36 C37 FLAT C38A N6A O6A C37A C36A SIMU 0.01 0.02 2 N2 S2 S3 N3 C18 C19 C20 C21 N2A S2A S3A N3A C19A C20A SIMU 0.01 0.02 2 C25 C25A C26 C26A C27 C22 SIMU 0.01 0.02 2 C38A N6A O6A C37A C36A C38 O6 N6 C36 C37 RIGU N2 S2 S3 N3 C18 C19 C20 C21 N2A S2A S3A N3A C19A C20A RIGU C22 C25A C25 C26 C26A C27 RIGU N6 O6 C38 C36 C37 RIGU C38 O6 N6 C36 C37 C38A N6A O6A C37A C36A TEMP -173 SIZE 0.183 0.164 0.016 L.S. 10 PLAN 20 BOND LIST 6 fmap 2 acta SHEL 100 0.84 WGHT 0.135900 38.611397 FVAR 0.08170 0.84176 0.43250 0.79363 CD1 3 0.556557 -0.120662 0.145137 11.00000 0.00787 0.04161 = 0.01417 0.00081 0.00092 0.00002 S1 6 0.691248 -0.127816 0.495753 11.00000 0.01042 0.05132 = 0.01492 0.00068 -0.00040 0.00038 N1 4 0.560830 -0.033236 0.155080 11.00000 0.01268 0.05206 = 0.01290 0.00395 0.00118 0.00010 O1 5 0.817240 -0.126443 0.611739 11.00000 0.01610 0.05480 = 0.01623 0.00058 -0.00161 0.00004 C1 1 0.833702 -0.127254 0.533947 11.00000 0.01763 0.03885 = 0.02331 0.00153 -0.00686 0.00056 PART 1 N2 4 0.521256 0.323258 0.136614 21.00000 0.02912 0.05094 = 0.03673 -0.00301 -0.00906 0.00015 PART 0 O2 5 0.896084 -0.125436 0.506629 11.00000 0.00745 0.07596 = 0.02100 -0.00276 -0.00062 0.00060 PART 1 S2 6 0.644253 0.330716 0.207309 21.00000 0.04778 0.04259 = 0.05482 -0.00389 -0.01418 0.00084 PART 0 C2 1 0.777542 -0.129623 0.467129 11.00000 0.01143 0.04243 = 0.02583 -0.00121 0.00060 0.00090 PART 1 S3 6 0.492731 0.428862 0.117531 21.00000 0.05395 0.04503 = 0.05088 -0.00072 -0.01342 0.00544 N3 4 0.615621 0.436967 0.184602 21.00000 0.05210 0.05380 = 0.06224 -0.00350 -0.01657 -0.00052 PART 0 O3 5 0.548524 -0.120461 0.432061 11.00000 0.01214 0.06416 = 0.01738 -0.00033 0.00157 0.00130 C3 1 0.785735 -0.130800 0.379578 11.00000 0.01107 0.06238 = 0.01958 -0.00157 0.00213 0.00228 AFIX 43 H3 2 0.830180 -0.132220 0.351981 11.00000 -1.20000 AFIX 0 N4 4 0.555573 0.791380 0.151088 11.00000 0.02251 0.04761 = 0.02504 -0.00171 0.00219 0.00155 O4 5 0.570177 -0.123144 0.292958 11.00000 0.01203 0.05328 = 0.02179 0.00018 -0.00192 -0.00138 C4 1 0.721936 -0.129702 0.334517 11.00000 0.01492 0.05428 = 0.01989 -0.00100 0.00100 0.00454 AFIX 43 H4 2 0.718144 -0.130035 0.273409 11.00000 -1.20000 AFIX 0 C5 1 0.665636 -0.128086 0.389744 11.00000 0.01582 0.04313 = 0.01479 0.00070 -0.00083 0.00121 C6 1 0.590474 -0.123752 0.369554 11.00000 0.01111 0.03123 = 0.01721 0.00066 -0.00108 0.00068 C7 1 0.610510 -0.007475 0.200919 11.00000 0.01638 0.05146 = 0.01987 0.00570 -0.00224 0.00166 AFIX 43 H7 2 0.644117 -0.026913 0.232134 11.00000 -1.20000 AFIX 0 C8 1 0.614799 0.044275 0.204601 11.00000 0.01775 0.05443 = 0.01724 -0.00086 -0.00095 -0.00235 AFIX 43 H8 2 0.650512 0.059846 0.238334 11.00000 -1.20000 AFIX 0 C9 1 0.515144 -0.003873 0.111010 11.00000 0.01768 0.05598 = 0.01956 0.00129 -0.00501 -0.00069 AFIX 43 H9 2 0.479788 -0.020466 0.078103 11.00000 -1.20000 AFIX 0 C10 1 0.516768 0.049021 0.110931 11.00000 0.01916 0.05351 = 0.01767 0.00254 -0.00601 0.00099 AFIX 43 H10 2 0.483404 0.067559 0.077824 11.00000 -1.20000 AFIX 0 C11 1 0.566806 0.075406 0.158883 11.00000 0.01618 0.05546 = 0.00821 -0.00126 0.00451 -0.00211 C12 1 0.568680 0.131671 0.161346 11.00000 0.01647 0.05632 = 0.01149 -0.00443 0.00166 -0.00233 C13 1 0.510144 0.160883 0.137939 11.00000 0.02463 0.05186 = 0.01207 -0.00156 0.00079 0.00066 AFIX 43 H13 2 0.468480 0.143956 0.120159 11.00000 -1.20000 AFIX 0 C14 1 0.511517 0.212945 0.140055 11.00000 0.02810 0.05371 = 0.01731 0.00141 -0.00024 0.00503 AFIX 43 H14 2 0.470951 0.231589 0.123346 11.00000 -1.20000 AFIX 0 C15 1 0.629344 0.158260 0.187540 11.00000 0.02187 0.05039 = 0.01601 -0.00086 0.00157 0.00111 AFIX 43 H15 2 0.670078 0.139535 0.203352 11.00000 -1.20000 AFIX 0 C16 1 0.630560 0.210782 0.190587 11.00000 0.02435 0.05659 = 0.02210 -0.00231 -0.00064 -0.00470 AFIX 43 H16 2 0.671803 0.227904 0.209295 11.00000 -1.20000 AFIX 0 C17 1 0.571354 0.239508 0.166290 11.00000 0.03716 0.04566 = 0.02193 -0.00216 0.00149 -0.00022 C18 1 0.571618 0.295306 0.167285 11.00000 0.03885 0.04733 = 0.03526 0.00068 -0.00464 0.00174 PART 1 C19 1 0.536081 0.373502 0.143472 21.00000 0.04603 0.04672 = 0.04496 -0.00280 -0.00639 0.00417 C20 1 0.600245 0.386286 0.178495 21.00000 0.04921 0.04752 = 0.04996 -0.00064 -0.00918 0.00435 PART 0 C21 1 0.565604 0.463884 0.156621 11.00000 0.05558 0.05028 = 0.05566 -0.00052 -0.00653 0.00369 C22 1 0.564254 0.519386 0.153928 11.00000 0.05683 0.05181 = 0.05649 -0.00509 -0.00300 0.00236 C23 1 0.506866 0.546293 0.122446 11.00000 0.06490 0.04756 = 0.05289 -0.00668 -0.01344 -0.00607 AFIX 43 H23 2 0.467456 0.527813 0.101558 11.00000 -1.20000 AFIX 0 C24 1 0.505478 0.598936 0.120653 11.00000 0.05872 0.05494 = 0.04752 0.00102 -0.01199 0.00238 AFIX 43 H24 2 0.465392 0.616062 0.098474 11.00000 -1.20000 AFIX 0 PART 1 C25 1 0.627192 0.548292 0.164175 31.00000 0.05383 0.05128 = 0.05781 -0.00463 -0.00172 0.00539 AFIX 43 H25 2 0.670497 0.530788 0.171135 31.00000 -1.20000 AFIX 0 C26 1 0.626532 0.601678 0.164196 31.00000 0.04892 0.04967 = 0.05667 -0.00613 -0.00103 0.00543 AFIX 43 H26 2 0.668493 0.620571 0.173053 31.00000 -1.20000 AFIX 0 PART 0 C27 1 0.561530 0.627180 0.150639 11.00000 0.04367 0.04937 = 0.05247 -0.00496 -0.00224 0.00064 C28 1 0.560068 0.683935 0.149963 11.00000 0.03378 0.05356 = 0.03866 -0.00167 0.00002 0.00375 C29 1 0.522151 0.711527 0.088579 11.00000 0.04197 0.05357 = 0.03279 -0.00464 -0.00429 -0.00274 AFIX 43 H29 2 0.496782 0.694099 0.044763 11.00000 -1.20000 AFIX 0 C30 1 0.521791 0.763718 0.091968 11.00000 0.03483 0.05567 = 0.02445 -0.00115 -0.00246 0.00071 AFIX 43 H30 2 0.495688 0.781560 0.049291 11.00000 -1.20000 AFIX 0 C31 1 0.597062 0.712644 0.211441 11.00000 0.04684 0.04008 = 0.04768 0.00196 -0.01558 0.00688 AFIX 43 H31 2 0.624492 0.695863 0.254080 11.00000 -1.20000 AFIX 0 C32 1 0.593448 0.764507 0.209662 11.00000 0.03159 0.05075 = 0.04594 -0.00929 -0.01028 0.00551 AFIX 43 H32 2 0.618967 0.783098 0.251964 11.00000 -1.20000 AFIX 0 REM Begin 1st Disordered DMF O5 5 0.738106 0.735157 0.311829 11.00000 0.05356 0.12239 = 0.06701 -0.00960 0.00039 -0.00228 C33 1 0.769748 0.738212 0.383127 11.00000 0.06048 0.12042 = 0.06366 0.00029 -0.00319 -0.01066 AFIX 43 H33 2 0.818737 0.744807 0.382026 11.00000 -1.20000 AFIX 0 N5 4 0.739675 0.732915 0.458513 11.00000 0.06480 0.11016 = 0.05302 0.00025 -0.00199 -0.01523 C34 1 0.664348 0.725169 0.464868 11.00000 0.05439 0.15429 = 0.07885 0.01302 -0.00676 -0.02460 AFIX 137 H34A 2 0.643263 0.727966 0.407402 11.00000 -1.50000 H34B 2 0.644097 0.751241 0.502901 11.00000 -1.50000 H34C 2 0.654907 0.691079 0.488585 11.00000 -1.50000 AFIX 0 C35 1 0.777341 0.738408 0.538337 11.00000 0.06242 0.11123 = 0.06352 0.00902 -0.02002 -0.00875 AFIX 137 H35A 2 0.827829 0.739324 0.526599 11.00000 -1.50000 H35B 2 0.766694 0.709342 0.576110 11.00000 -1.50000 H35C 2 0.763174 0.770303 0.566710 11.00000 -1.50000 AFIX 0 REM End 1st Disordered DMF REM Begin 2nd Disordered DMF PART 1 O6 5 0.642247 0.570983 0.477979 40.50000 0.03917 0.24766 = 0.05413 0.03489 -0.00329 -0.00245 C38 1 0.706424 0.572048 0.493345 40.50000 0.04234 0.23756 = 0.05591 0.02382 0.00309 0.00123 AFIX 43 H38 2 0.722485 0.563949 0.549734 40.50000 -1.20000 AFIX 0 N6 4 0.752794 0.584184 0.433052 40.50000 0.03795 0.23441 = 0.05103 0.01802 0.00515 -0.00100 C36 1 0.727018 0.599291 0.348664 40.50000 0.05013 0.23755 = 0.05873 0.02081 0.00158 -0.00783 AFIX 137 H36A 2 0.679530 0.585809 0.340366 40.50000 -1.50000 H36B 2 0.758059 0.585528 0.303927 40.50000 -1.50000 H36C 2 0.726067 0.636732 0.344742 40.50000 -1.50000 AFIX 0 C37 1 0.825128 0.593059 0.450859 40.50000 0.04702 0.23473 = 0.06430 0.02189 -0.00383 -0.00613 AFIX 137 H37A 2 0.844010 0.617553 0.408976 40.50000 -1.50000 H37B 2 0.850972 0.560725 0.446608 40.50000 -1.50000 H37C 2 0.830130 0.606999 0.509233 40.50000 -1.50000 AFIX 0 PART 2 C38A 1 0.691630 0.604201 0.460058 -40.50000 0.04224 0.23791 = 0.05481 0.02225 0.00132 -0.00100 AFIX 43 H38A 2 0.674988 0.609292 0.517186 -40.50000 -1.20000 AFIX 0 N6A 4 0.743470 0.571729 0.449530 -40.50000 0.04058 0.23684 = 0.05411 0.02185 0.00187 -0.00211 C37A 1 0.772368 0.545008 0.522985 -40.50000 0.04614 0.23700 = 0.05889 0.02371 -0.00008 -0.00186 AFIX 137 H37D 2 0.791593 0.512040 0.504227 -40.50000 -1.50000 H37E 2 0.735352 0.539172 0.565732 -40.50000 -1.50000 H37F 2 0.809760 0.565684 0.548824 -40.50000 -1.50000 AFIX 0 C36A 1 0.770959 0.559432 0.365967 -40.50000 0.04135 0.23692 = 0.05593 0.02073 0.00175 -0.00477 AFIX 33 H36D 2 0.809188 0.534614 0.372039 -40.50000 -1.50000 H36E 2 0.733683 0.544664 0.330254 -40.50000 -1.50000 H36F 2 0.788797 0.590613 0.338489 -40.50000 -1.50000 AFIX 0 O6A 5 0.662328 0.628977 0.401281 -40.50000 0.04457 0.24461 = 0.06012 0.02542 -0.00791 -0.00493 REM Begin 3rd Disordered DMF SAME 0.02 0.04 O5 > C35 PART 0 PART -1 O7 5 0.745453 -0.005917 0.316728 10.50000 0.01357 0.03303 = 0.02441 -0.00129 0.00353 -0.01822 C39 1 0.772143 -0.000173 0.390865 10.50000 0.01377 0.03129 = 0.04010 0.00328 0.00500 0.00626 AFIX 43 H39 2 0.821565 0.003535 0.395480 10.50000 -1.20000 AFIX 0 N7 4 0.734057 0.000883 0.462216 10.50000 0.01157 0.04467 = 0.02695 0.00477 -0.00486 0.00236 C40 1 0.764665 -0.000497 0.546893 10.50000 0.04447 0.04891 = 0.02310 -0.00449 -0.00850 -0.00152 AFIX 137 H40A 2 0.747945 -0.030902 0.577702 10.50000 -1.50000 H40B 2 0.751057 0.030321 0.578834 10.50000 -1.50000 H40C 2 0.815867 -0.001852 0.541897 10.50000 -1.50000 AFIX 0 C41 1 0.657731 0.002773 0.457450 10.50000 0.01951 0.05598 = 0.02502 0.00688 0.00017 -0.00062 AFIX 137 H41A 2 0.641294 0.036264 0.477540 10.50000 -1.50000 H41B 2 0.637807 -0.024169 0.493994 10.50000 -1.50000 H41C 2 0.642791 -0.002505 0.397614 10.50000 -1.50000 AFIX 0 PART 0 REM Begin 3rd Disordered DMF REM Begin Disordered TzTz Moiety PART 2 N2A 4 0.625690 0.324271 0.173838 -21.00000 0.04759 0.04712 = 0.05061 -0.00419 -0.01241 0.00162 S2A 6 0.493164 0.326873 0.132906 -21.00000 0.04175 0.04617 = 0.04412 -0.00212 -0.00675 0.00606 S3A 6 0.644713 0.431302 0.199723 -21.00000 0.05667 0.04986 = 0.06458 -0.00403 -0.00867 -0.00572 N3A 4 0.516458 0.431944 0.141417 -21.00000 0.05296 0.04913 = 0.05032 -0.00141 -0.00735 0.00501 C19A 1 0.603959 0.373051 0.186384 -21.00000 0.04980 0.04742 = 0.05339 -0.00396 -0.01023 0.00044 C20A 1 0.536693 0.382801 0.157054 -21.00000 0.04652 0.04693 = 0.04785 -0.00208 -0.00741 0.00186 C25A 1 0.617913 0.547532 0.196082 -31.00000 0.05434 0.05152 = 0.05637 -0.00310 -0.00307 0.00420 AFIX 43 H25A 2 0.654748 0.530137 0.225134 -31.00000 -1.20000 AFIX 0 C26A 1 0.616200 0.600677 0.194566 -31.00000 0.05189 0.05030 = 0.05701 -0.00466 -0.00493 0.00508 AFIX 43 H26A 2 0.651882 0.619568 0.223138 -31.00000 -1.20000 PART 0 REM End Disordered TzTz Moiety AFIX 0 HKLF 4 REM Pcca_a.res in Pcca REM wR2 = 0.2173, GooF = S = 1.079, Restrained GooF = 1.036 for all data REM R1 = 0.0804 for 6136 Fo > 4sig(Fo) and 0.0852 for all 6828 data REM 659 parameters refined using 706 restraints END WGHT 0.1359 38.5592 REM Highest difference peak 6.132, deepest hole -1.088, 1-sigma level 0.173 Q1 1 0.5565 -0.0827 0.1437 11.00000 0.05 6.13 Q2 1 0.5564 -0.1577 0.1438 11.00000 0.05 6.04 Q3 1 0.6903 -0.0914 0.4965 11.00000 0.05 1.64 Q4 1 0.6905 -0.1649 0.4962 11.00000 0.05 1.42 Q5 1 0.4943 0.3913 0.1181 11.00000 0.05 1.05 Q6 1 0.5579 -0.1202 0.1974 11.00000 0.05 1.04 Q7 1 0.5552 -0.1196 0.0956 11.00000 0.05 1.03 Q8 1 0.4932 0.4673 0.1184 11.00000 0.05 1.01 Q9 1 0.7603 0.5610 0.4418 11.00000 0.05 0.96 Q10 1 0.6407 0.3674 0.2063 11.00000 0.05 0.96 Q11 1 0.6431 0.2934 0.2076 11.00000 0.05 0.95 Q12 1 0.7554 0.6915 0.4552 11.00000 0.05 0.74 Q13 1 0.5708 0.2666 0.1714 11.00000 0.05 0.68 Q14 1 0.7498 -0.0337 0.3172 11.00000 0.05 0.67 Q15 1 0.6546 0.6705 0.4133 11.00000 0.05 0.66 Q16 1 0.5750 -0.1597 0.2854 11.00000 0.05 0.65 Q17 1 0.8409 0.7347 0.4432 11.00000 0.05 0.64 Q18 1 0.5448 -0.1608 0.4256 11.00000 0.05 0.64 Q19 1 0.6846 0.5477 0.4712 11.00000 0.05 0.63 Q20 1 0.6604 0.5287 0.4553 11.00000 0.05 0.62 ; _shelx_res_checksum 48928 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, 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 Cd1 Cd 0.55656(2) -0.12066(2) 0.14514(2) 0.0212(2) Uani 1 1 d . . . . . S1 S 0.69125(6) -0.12782(6) 0.49575(8) 0.0256(3) Uani 1 1 d . . . . . N1 N 0.5608(2) -0.0332(2) 0.1551(3) 0.0259(11) Uani 1 1 d . . . . . O1 O 0.8172(2) -0.12644(16) 0.6117(3) 0.0290(9) Uani 1 1 d . . . . . C1 C 0.8337(3) -0.1273(2) 0.5339(4) 0.0266(12) Uani 1 1 d . . . . . N2 N 0.5213(5) 0.3233(3) 0.1366(6) 0.0389(15) Uani 0.842(5) 1 d D U P A 1 O2 O 0.8961(2) -0.12544(17) 0.5066(3) 0.0348(10) Uani 1 1 d . . . . . S2 S 0.64425(13) 0.33072(9) 0.20731(16) 0.0484(7) Uani 0.842(5) 1 d D U P A 1 C2 C 0.7775(3) -0.1296(2) 0.4671(4) 0.0266(12) Uani 1 1 d . . . . . S3 S 0.49273(15) 0.42886(9) 0.11753(17) 0.0500(7) Uani 0.842(5) 1 d D U P A 1 N3 N 0.6156(5) 0.4370(3) 0.1846(6) 0.0560(18) Uani 0.842(5) 1 d D U P A 1 O3 O 0.5485(2) -0.12046(16) 0.4321(3) 0.0312(10) Uani 1 1 d . . . . . C3 C 0.7857(3) -0.1308(3) 0.3796(4) 0.0310(13) Uani 1 1 d . . . . . H3 H 0.830180 -0.132220 0.351981 0.037 Uiso 1 1 calc R U . . . N4 N 0.5556(2) 0.7914(2) 0.1511(3) 0.0317(12) Uani 1 1 d . . . . . O4 O 0.5702(2) -0.12314(16) 0.2930(3) 0.0290(10) Uani 1 1 d . . . . . C4 C 0.7219(3) -0.1297(2) 0.3345(4) 0.0297(13) Uani 1 1 d . . . . . H4 H 0.718144 -0.130035 0.273409 0.036 Uiso 1 1 calc R U . . . C5 C 0.6656(3) -0.1281(2) 0.3897(3) 0.0246(12) Uani 1 1 d . . . . . C6 C 0.5905(3) -0.12375(19) 0.3696(3) 0.0198(11) Uani 1 1 d . . . . . C7 C 0.6105(3) -0.0075(2) 0.2009(3) 0.0292(13) Uani 1 1 d . . . . . H7 H 0.644117 -0.026913 0.232134 0.035 Uiso 1 1 calc R U . . . C8 C 0.6148(3) 0.0443(3) 0.2046(3) 0.0298(13) Uani 1 1 d . . . . . H8 H 0.650512 0.059846 0.238334 0.036 Uiso 1 1 calc R U . . . C9 C 0.5151(3) -0.0039(2) 0.1110(3) 0.0311(13) Uani 1 1 d . . . . . H9 H 0.479788 -0.020466 0.078103 0.037 Uiso 1 1 calc R U . . . C10 C 0.5168(3) 0.0490(2) 0.1109(3) 0.0301(13) Uani 1 1 d . . . . . H10 H 0.483404 0.067559 0.077824 0.036 Uiso 1 1 calc R U . . . C11 C 0.5668(3) 0.0754(3) 0.1589(3) 0.0266(13) Uani 1 1 d . . . . . C12 C 0.5687(3) 0.1317(3) 0.1613(4) 0.0281(13) Uani 1 1 d . . . . . C13 C 0.5101(3) 0.1609(3) 0.1379(3) 0.0295(13) Uani 1 1 d . . . . . H13 H 0.468480 0.143956 0.120159 0.035 Uiso 1 1 calc R U . . . C14 C 0.5115(3) 0.2129(3) 0.1401(3) 0.0330(14) Uani 1 1 d . . . . . H14 H 0.470951 0.231589 0.123346 0.040 Uiso 1 1 calc R U . . . C15 C 0.6293(3) 0.1583(2) 0.1875(3) 0.0294(13) Uani 1 1 d . . . . . H15 H 0.670078 0.139535 0.203352 0.035 Uiso 1 1 calc R U . . . C16 C 0.6306(3) 0.2108(3) 0.1906(4) 0.0343(14) Uani 1 1 d . . . . . H16 H 0.671803 0.227904 0.209295 0.041 Uiso 1 1 calc R U . . . C17 C 0.5714(4) 0.2395(3) 0.1663(4) 0.0349(13) Uani 1 1 d . . . . . C18 C 0.5716(3) 0.2953(3) 0.1673(5) 0.0405(13) Uani 1 1 d D U . . . C19 C 0.5361(6) 0.3735(4) 0.1435(8) 0.0459(17) Uani 0.842(5) 1 d D U P A 1 C20 C 0.6002(5) 0.3863(3) 0.1785(8) 0.0489(16) Uani 0.842(5) 1 d D U P A 1 C21 C 0.5656(4) 0.4639(3) 0.1566(6) 0.0538(16) Uani 1 1 d D U . . . C22 C 0.5643(4) 0.5194(3) 0.1539(6) 0.0550(19) Uani 1 1 d D U . . . C23 C 0.5069(5) 0.5463(3) 0.1224(5) 0.0551(19) Uani 1 1 d . . . . . H23 H 0.467456 0.527813 0.101558 0.066 Uiso 1 1 calc R U . . . C24 C 0.5055(5) 0.5989(3) 0.1207(5) 0.0537(19) Uani 1 1 d . . . . . H24 H 0.465392 0.616062 0.098474 0.064 Uiso 1 1 calc R U . . . C25 C 0.6272(10) 0.5483(8) 0.164(2) 0.054(3) Uani 0.43(4) 1 d D U P B 1 H25 H 0.670497 0.530788 0.171135 0.065 Uiso 0.43(4) 1 calc R U P B 1 C26 C 0.6265(10) 0.6017(8) 0.164(2) 0.052(3) Uani 0.43(4) 1 d D U P B 1 H26 H 0.668493 0.620571 0.173053 0.062 Uiso 0.43(4) 1 calc R U P B 1 C27 C 0.5615(4) 0.6272(3) 0.1506(5) 0.0485(19) Uani 1 1 d D U . . . C28 C 0.5601(3) 0.6839(3) 0.1500(4) 0.0420(17) Uani 1 1 d . . . . . C29 C 0.5222(4) 0.7115(3) 0.0886(4) 0.0428(16) Uani 1 1 d . . . . . H29 H 0.496782 0.694099 0.044763 0.051 Uiso 1 1 calc R U . . . C30 C 0.5218(3) 0.7637(3) 0.0920(4) 0.0383(15) Uani 1 1 d . . . . . H30 H 0.495688 0.781560 0.049291 0.046 Uiso 1 1 calc R U . . . C31 C 0.5971(4) 0.7126(3) 0.2114(5) 0.0449(16) Uani 1 1 d . . . . . H31 H 0.624492 0.695863 0.254080 0.054 Uiso 1 1 calc R U . . . C32 C 0.5934(3) 0.7645(3) 0.2097(5) 0.0428(16) Uani 1 1 d . . . . . H32 H 0.618967 0.783098 0.251964 0.051 Uiso 1 1 calc R U . . . O5 O 0.7381(3) 0.7352(3) 0.3118(4) 0.0810(19) Uani 1 1 d D . . . . C33 C 0.7697(5) 0.7382(5) 0.3831(6) 0.082(3) Uani 1 1 d D . . . . H33 H 0.818737 0.744807 0.382026 0.098 Uiso 1 1 calc R U . . . N5 N 0.7397(4) 0.7329(4) 0.4585(5) 0.076(2) Uani 1 1 d D . . . . C34 C 0.6643(4) 0.7252(5) 0.4649(7) 0.096(4) Uani 1 1 d D . . . . H34A H 0.643263 0.727966 0.407402 0.144 Uiso 1 1 calc R U . . . H34B H 0.644097 0.751241 0.502901 0.144 Uiso 1 1 calc R U . . . H34C H 0.654907 0.691079 0.488585 0.144 Uiso 1 1 calc R U . . . C35 C 0.7773(5) 0.7384(4) 0.5383(6) 0.079(3) Uani 1 1 d D . . . . H35A H 0.827829 0.739324 0.526599 0.119 Uiso 1 1 calc R U . . . H35B H 0.766694 0.709342 0.576110 0.119 Uiso 1 1 calc R U . . . H35C H 0.763174 0.770303 0.566710 0.119 Uiso 1 1 calc R U . . . O6 O 0.6422(7) 0.5710(10) 0.4780(11) 0.114(6) Uani 0.397(8) 1 d D U P C 1 C38 C 0.7064(8) 0.5720(11) 0.4933(12) 0.112(5) Uani 0.397(8) 1 d D U P C 1 H38 H 0.722485 0.563949 0.549734 0.134 Uiso 0.397(8) 1 calc R U P C 1 N6 N 0.7528(7) 0.5842(10) 0.4331(10) 0.108(5) Uani 0.397(8) 1 d D U P C 1 C36 C 0.7270(12) 0.5993(16) 0.3487(12) 0.115(6) Uani 0.397(8) 1 d D U P C 1 H36A H 0.679530 0.585809 0.340366 0.173 Uiso 0.397(8) 1 calc R U P C 1 H36B H 0.758059 0.585528 0.303927 0.173 Uiso 0.397(8) 1 calc R U P C 1 H36C H 0.726067 0.636732 0.344742 0.173 Uiso 0.397(8) 1 calc R U P C 1 C37 C 0.8251(8) 0.5931(15) 0.4509(15) 0.115(6) Uani 0.397(8) 1 d D U P C 1 H37A H 0.844010 0.617553 0.408976 0.173 Uiso 0.397(8) 1 calc R U P C 1 H37B H 0.850972 0.560725 0.446608 0.173 Uiso 0.397(8) 1 calc R U P C 1 H37C H 0.830130 0.606999 0.509233 0.173 Uiso 0.397(8) 1 calc R U P C 1 C38A C 0.692(3) 0.604(3) 0.460(3) 0.112(6) Uani 0.103(8) 1 d D U P C 2 H38A H 0.674988 0.609292 0.517186 0.134 Uiso 0.103(8) 1 calc R U P C 2 N6A N 0.743(3) 0.572(3) 0.450(3) 0.111(6) Uani 0.103(8) 1 d D U P C 2 C37A C 0.772(4) 0.545(4) 0.523(4) 0.114(7) Uani 0.103(8) 1 d D U P C 2 H37D H 0.791593 0.512040 0.504227 0.171 Uiso 0.103(8) 1 calc R U P C 2 H37E H 0.735352 0.539172 0.565732 0.171 Uiso 0.103(8) 1 calc R U P C 2 H37F H 0.809760 0.565684 0.548824 0.171 Uiso 0.103(8) 1 calc R U P C 2 C36A C 0.771(4) 0.559(4) 0.366(4) 0.111(7) Uani 0.103(8) 1 d D U P C 2 H36D H 0.809188 0.534614 0.372039 0.167 Uiso 0.103(8) 1 calc R U P C 2 H36E H 0.733683 0.544664 0.330254 0.167 Uiso 0.103(8) 1 calc R U P C 2 H36F H 0.788797 0.590613 0.338489 0.167 Uiso 0.103(8) 1 calc R U P C 2 O6A O 0.662(3) 0.629(3) 0.401(4) 0.116(8) Uani 0.103(8) 1 d D U P C 2 O7 O 0.745(2) -0.0059(18) 0.3167(4) 0.024(6) Uani 0.5 1 d D . P D -1 C39 C 0.7721(5) -0.0002(4) 0.3909(6) 0.028(3) Uani 0.5 1 d D . P D -1 H39 H 0.821565 0.003535 0.395480 0.034 Uiso 0.5 1 calc R U P D -1 N7 N 0.7341(4) 0.0009(7) 0.4622(5) 0.028(3) Uani 0.5 1 d D . P D -1 C40 C 0.7647(7) -0.0005(17) 0.5469(6) 0.039(5) Uani 0.5 1 d D . P D -1 H40A H 0.747945 -0.030902 0.577702 0.058 Uiso 0.5 1 calc R U P D -1 H40B H 0.751057 0.030321 0.578834 0.058 Uiso 0.5 1 calc R U P D -1 H40C H 0.815867 -0.001852 0.541897 0.058 Uiso 0.5 1 calc R U P D -1 C41 C 0.6577(5) 0.0028(5) 0.4575(7) 0.034(3) Uani 0.5 1 d D . P D -1 H41A H 0.641294 0.036264 0.477540 0.050 Uiso 0.5 1 calc R U P D -1 H41B H 0.637807 -0.024169 0.493994 0.050 Uiso 0.5 1 calc R U P D -1 H41C H 0.642791 -0.002505 0.397614 0.050 Uiso 0.5 1 calc R U P D -1 N2A N 0.6257(14) 0.3243(11) 0.174(3) 0.048(3) Uani 0.158(5) 1 d D U P A 2 S2A S 0.4932(7) 0.3269(6) 0.1329(11) 0.044(2) Uani 0.158(5) 1 d D U P A 2 S3A S 0.6447(8) 0.4313(6) 0.1997(11) 0.057(3) Uani 0.158(5) 1 d D U P A 2 N3A N 0.5165(17) 0.4319(12) 0.141(3) 0.051(3) Uani 0.158(5) 1 d D U P A 2 C19A C 0.604(2) 0.3731(10) 0.186(5) 0.050(2) Uani 0.158(5) 1 d D U P A 2 C20A C 0.537(2) 0.3828(12) 0.157(5) 0.047(2) Uani 0.158(5) 1 d D U P A 2 C25A C 0.6179(10) 0.5475(6) 0.1961(16) 0.054(3) Uani 0.57(4) 1 d D U P B 2 H25A H 0.654748 0.530137 0.225134 0.065 Uiso 0.57(4) 1 calc R U P B 2 C26A C 0.6162(10) 0.6007(6) 0.1946(16) 0.053(3) Uani 0.57(4) 1 d D U P B 2 H26A H 0.651882 0.619568 0.223138 0.064 Uiso 0.57(4) 1 calc R U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0079(3) 0.0416(3) 0.0142(3) 0.00081(14) 0.00092(12) 0.00002(13) S1 0.0104(7) 0.0513(9) 0.0149(7) 0.0007(5) -0.0004(5) 0.0004(5) N1 0.013(2) 0.052(3) 0.013(2) 0.004(2) 0.0012(15) 0.0001(19) O1 0.016(2) 0.055(3) 0.016(2) 0.0006(16) -0.0016(16) 0.0000(16) C1 0.018(3) 0.039(3) 0.023(3) 0.002(2) -0.007(2) 0.001(2) N2 0.029(4) 0.051(3) 0.037(3) -0.003(2) -0.009(3) 0.000(3) O2 0.0075(19) 0.076(3) 0.021(2) -0.0028(18) -0.0006(16) 0.0006(17) S2 0.0478(13) 0.0426(12) 0.0548(14) -0.0039(10) -0.0142(10) 0.0008(9) C2 0.011(3) 0.042(3) 0.026(3) -0.001(2) 0.001(2) 0.001(2) S3 0.0540(15) 0.0450(12) 0.0509(15) -0.0007(10) -0.0134(11) 0.0054(10) N3 0.052(4) 0.054(3) 0.062(4) -0.003(3) -0.017(4) -0.001(3) O3 0.012(2) 0.064(3) 0.017(2) -0.0003(17) 0.0016(15) 0.0013(16) C3 0.011(3) 0.062(4) 0.020(3) -0.002(3) 0.002(2) 0.002(2) N4 0.023(3) 0.048(3) 0.025(3) -0.002(2) 0.0022(18) 0.002(2) O4 0.0120(18) 0.053(3) 0.022(2) 0.0002(16) -0.0019(16) -0.0014(16) C4 0.015(3) 0.054(4) 0.020(3) -0.001(2) 0.001(2) 0.005(2) C5 0.016(3) 0.043(3) 0.015(3) 0.001(2) -0.001(2) 0.001(2) C6 0.011(3) 0.031(3) 0.017(3) 0.0007(19) -0.001(2) 0.0007(19) C7 0.016(3) 0.051(4) 0.020(3) 0.006(2) -0.002(2) 0.002(2) C8 0.018(3) 0.054(4) 0.017(3) -0.001(2) -0.001(2) -0.002(2) C9 0.018(3) 0.056(4) 0.020(3) 0.001(3) -0.005(2) -0.001(2) C10 0.019(3) 0.054(4) 0.018(3) 0.003(2) -0.006(2) 0.001(2) C11 0.016(3) 0.055(4) 0.008(2) -0.001(2) 0.0045(19) -0.002(2) C12 0.016(3) 0.056(4) 0.011(2) -0.004(2) 0.002(2) -0.002(2) C13 0.025(3) 0.052(4) 0.012(3) -0.002(2) 0.001(2) 0.001(3) C14 0.028(3) 0.054(4) 0.017(3) 0.001(2) 0.000(2) 0.005(3) C15 0.022(3) 0.050(4) 0.016(3) -0.001(2) 0.002(2) 0.001(2) C16 0.024(3) 0.057(4) 0.022(3) -0.002(3) -0.001(2) -0.005(3) C17 0.037(3) 0.046(4) 0.022(3) -0.002(3) 0.001(3) 0.000(3) C18 0.039(3) 0.047(3) 0.035(3) 0.001(3) -0.005(3) 0.002(2) C19 0.046(3) 0.047(3) 0.045(4) -0.003(3) -0.006(3) 0.004(3) C20 0.049(3) 0.048(3) 0.050(4) -0.001(3) -0.009(3) 0.004(3) C21 0.056(4) 0.050(3) 0.056(4) -0.001(3) -0.007(3) 0.004(3) C22 0.057(4) 0.052(4) 0.056(4) -0.005(3) -0.003(3) 0.002(3) C23 0.065(5) 0.048(4) 0.053(4) -0.007(4) -0.013(4) -0.006(4) C24 0.059(5) 0.055(5) 0.048(4) 0.001(4) -0.012(4) 0.002(4) C25 0.054(5) 0.051(4) 0.058(7) -0.005(6) -0.002(5) 0.005(4) C26 0.049(5) 0.050(4) 0.057(7) -0.006(6) -0.001(5) 0.005(4) C27 0.044(4) 0.049(4) 0.052(5) -0.005(3) -0.002(3) 0.001(3) C28 0.034(4) 0.054(4) 0.039(4) -0.002(3) 0.000(3) 0.004(3) C29 0.042(4) 0.054(4) 0.033(3) -0.005(3) -0.004(3) -0.003(3) C30 0.035(3) 0.056(4) 0.024(3) -0.001(3) -0.002(3) 0.001(3) C31 0.047(4) 0.040(4) 0.048(4) 0.002(3) -0.016(3) 0.007(3) C32 0.032(3) 0.051(4) 0.046(4) -0.009(3) -0.010(3) 0.006(3) O5 0.054(4) 0.122(6) 0.067(4) -0.010(4) 0.000(3) -0.002(4) C33 0.060(6) 0.120(9) 0.064(6) 0.000(6) -0.003(5) -0.011(6) N5 0.065(5) 0.110(6) 0.053(4) 0.000(4) -0.002(4) -0.015(4) C34 0.054(6) 0.154(11) 0.079(7) 0.013(7) -0.007(5) -0.025(6) C35 0.062(6) 0.111(8) 0.064(6) 0.009(5) -0.020(5) -0.009(6) O6 0.039(6) 0.248(17) 0.054(8) 0.035(9) -0.003(6) -0.002(9) C38 0.042(6) 0.238(16) 0.056(8) 0.024(9) 0.003(6) 0.001(9) N6 0.038(6) 0.234(16) 0.051(7) 0.018(9) 0.005(5) -0.001(8) C36 0.050(9) 0.238(17) 0.059(9) 0.021(10) 0.002(7) -0.008(11) C37 0.047(8) 0.235(18) 0.064(10) 0.022(12) -0.004(8) -0.006(11) C38A 0.042(7) 0.238(16) 0.055(8) 0.022(9) 0.001(7) -0.001(9) N6A 0.041(7) 0.237(16) 0.054(8) 0.022(9) 0.002(7) -0.002(9) C37A 0.046(11) 0.237(18) 0.059(11) 0.024(12) 0.000(10) -0.002(12) C36A 0.041(11) 0.237(19) 0.056(10) 0.021(12) 0.002(10) -0.005(12) O6A 0.045(12) 0.245(19) 0.060(12) 0.025(12) -0.008(11) -0.005(12) O7 0.014(9) 0.033(19) 0.024(3) -0.001(5) 0.004(5) -0.018(8) C39 0.014(6) 0.031(6) 0.040(8) 0.003(5) 0.005(4) 0.006(6) N7 0.012(8) 0.045(5) 0.027(5) 0.005(5) -0.005(3) 0.002(9) C40 0.044(16) 0.049(6) 0.023(5) -0.004(8) -0.009(5) -0.002(18) C41 0.020(5) 0.056(8) 0.025(6) 0.007(5) 0.000(5) -0.001(5) N2A 0.048(5) 0.047(5) 0.051(6) -0.004(5) -0.012(5) 0.002(4) S2A 0.042(5) 0.046(4) 0.044(4) -0.002(4) -0.007(5) 0.006(4) S3A 0.057(5) 0.050(4) 0.065(5) -0.004(4) -0.009(5) -0.006(4) N3A 0.053(5) 0.049(5) 0.050(6) -0.001(5) -0.007(5) 0.005(4) C19A 0.050(4) 0.047(4) 0.053(4) -0.004(4) -0.010(4) 0.000(4) C20A 0.047(4) 0.047(4) 0.048(4) -0.002(4) -0.007(4) 0.002(4) C25A 0.054(5) 0.052(4) 0.056(6) -0.003(5) -0.003(5) 0.004(4) C26A 0.052(5) 0.050(4) 0.057(6) -0.005(5) -0.005(5) 0.005(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 N1 Cd1 N4 173.64(18) . 1_545 ? N1 Cd1 O4 87.55(15) . . ? N4 Cd1 O4 86.16(16) 1_545 . ? N1 Cd1 O2 95.82(15) . 8_755 ? N4 Cd1 O2 89.24(16) 1_545 8_755 ? O4 Cd1 O2 150.36(14) . 8_755 ? N1 Cd1 O3 93.60(15) . 3_655 ? N4 Cd1 O3 90.91(16) 1_545 3_655 ? O4 Cd1 O3 127.30(15) . 3_655 ? O2 Cd1 O3 81.98(14) 8_755 3_655 ? N1 Cd1 O1 92.32(14) . 8_755 ? N4 Cd1 O1 87.43(15) 1_545 8_755 ? O4 Cd1 O1 95.56(14) . 8_755 ? O2 Cd1 O1 54.95(13) 8_755 8_755 ? O3 Cd1 O1 136.91(14) 3_655 8_755 ? N1 Cd1 O4 91.90(14) . 3_655 ? N4 Cd1 O4 87.29(15) 1_545 3_655 ? O4 Cd1 O4 74.78(16) . 3_655 ? O2 Cd1 O4 134.26(13) 8_755 3_655 ? O3 Cd1 O4 52.52(14) 3_655 3_655 ? O1 Cd1 O4 169.28(13) 8_755 3_655 ? N1 Cd1 C1 94.50(16) . 8_755 ? N4 Cd1 C1 88.19(17) 1_545 8_755 ? O4 Cd1 C1 122.80(16) . 8_755 ? O2 Cd1 C1 27.67(16) 8_755 8_755 ? O3 Cd1 C1 109.64(17) 3_655 8_755 ? O1 Cd1 C1 27.28(16) 8_755 8_755 ? O4 Cd1 C1 161.48(16) 3_655 8_755 ? C2 S1 C5 91.5(3) . . ? C9 N1 C7 115.7(6) . . ? C9 N1 Cd1 120.7(4) . . ? C7 N1 Cd1 123.5(4) . . ? C1 O1 Cd1 87.6(3) . 8_756 ? O1 C1 O2 124.1(5) . . ? O1 C1 C2 119.5(5) . . ? O2 C1 C2 116.4(5) . . ? O1 C1 Cd1 65.1(3) . 8_756 ? O2 C1 Cd1 59.0(3) . 8_756 ? C2 C1 Cd1 175.3(4) . 8_756 ? C18 N2 C19 111.4(8) . . ? C1 O2 Cd1 93.3(3) . 8_756 ? C20 S2 C18 88.2(4) . . ? C3 C2 C1 127.5(5) . . ? C3 C2 S1 111.7(4) . . ? C1 C2 S1 120.7(5) . . ? C19 S3 C21 88.7(4) . . ? C21 N3 C20 110.8(8) . . ? C6 O3 Cd1 98.7(3) . 3_655 ? C2 C3 C4 113.3(5) . . ? C30 N4 C32 115.9(6) . . ? C30 N4 Cd1 121.2(4) . 1_565 ? C32 N4 Cd1 122.7(4) . 1_565 ? C6 O4 Cd1 168.4(4) . . ? C6 O4 Cd1 86.4(3) . 3_655 ? Cd1 O4 Cd1 105.14(16) . 3_655 ? C5 C4 C3 111.6(5) . . ? C4 C5 C6 129.1(5) . . ? C4 C5 S1 112.0(4) . . ? C6 C5 S1 118.8(4) . . ? O4 C6 O3 122.3(5) . . ? O4 C6 C5 120.3(5) . . ? O3 C6 C5 117.4(5) . . ? C8 C7 N1 123.8(5) . . ? C7 C8 C11 120.9(5) . . ? N1 C9 C10 123.7(5) . . ? C9 C10 C11 120.7(5) . . ? C10 C11 C8 115.2(6) . . ? C10 C11 C12 121.7(5) . . ? C8 C11 C12 123.1(5) . . ? C13 C12 C15 117.4(6) . . ? C13 C12 C11 121.2(6) . . ? C15 C12 C11 121.3(5) . . ? C14 C13 C12 121.5(6) . . ? C13 C14 C17 121.3(6) . . ? C16 C15 C12 121.1(6) . . ? C15 C16 C17 120.7(6) . . ? C14 C17 C16 118.0(6) . . ? C14 C17 C18 120.2(6) . . ? C16 C17 C18 121.8(6) . . ? N2A C18 C17 126.4(17) . . ? N2 C18 C17 123.8(7) . . ? N2 C18 S2 114.3(6) . . ? C17 C18 S2 121.8(5) . . ? N2A C18 S2A 115.1(18) . . ? C17 C18 S2A 117.0(7) . . ? N2 C19 C20 116.9(9) . . ? N2 C19 S3 134.6(8) . . ? C20 C19 S3 108.4(8) . . ? N3 C20 C19 117.0(8) . . ? N3 C20 S2 133.8(8) . . ? C19 C20 S2 109.1(8) . . ? N3 C21 C22 125.5(8) . . ? N3A C21 C22 129.4(19) . . ? N3 C21 S3 115.0(7) . . ? C22 C21 S3 119.5(6) . . ? N3A C21 S3A 111.3(19) . . ? C22 C21 S3A 118.9(7) . . ? C23 C22 C25A 117.9(10) . . ? C23 C22 C25 115.7(12) . . ? C23 C22 C21 122.0(7) . . ? C25A C22 C21 119.4(10) . . ? C25 C22 C21 120.7(12) . . ? C24 C23 C22 121.9(8) . . ? C23 C24 C27 120.9(8) . . ? C26 C25 C22 121.4(19) . . ? C25 C26 C27 118.4(19) . . ? C24 C27 C26 118.3(12) . . ? C24 C27 C26A 117.9(10) . . ? C24 C27 C28 121.2(7) . . ? C26 C27 C28 119.0(11) . . ? C26A C27 C28 120.2(9) . . ? C29 C28 C31 116.6(7) . . ? C29 C28 C27 122.1(7) . . ? C31 C28 C27 121.3(7) . . ? C30 C29 C28 119.5(6) . . ? N4 C30 C29 124.4(6) . . ? C32 C31 C28 119.6(6) . . ? N4 C32 C31 123.9(6) . . ? O5 C33 N5 124.5(8) . . ? C33 N5 C35 122.6(7) . . ? C33 N5 C34 120.5(7) . . ? C35 N5 C34 116.7(7) . . ? O6 C38 N6 121.7(15) . . ? C38 N6 C37 123.2(12) . . ? C38 N6 C36 118.3(11) . . ? C37 N6 C36 117.2(13) . . ? O6A C38A N6A 126(3) . . ? C38A N6A C36A 122.2(16) . . ? C38A N6A C37A 120.1(16) . . ? C36A N6A C37A 118(2) . . ? O7 C39 N7 122.7(17) . . ? C39 N7 C40 122.7(8) . . ? C39 N7 C41 120.4(8) . . ? C40 N7 C41 116.9(8) . . ? C18 N2A C19A 109(2) . . ? C20A S2A C18 85.6(15) . . ? C19A S3A C21 89.7(15) . . ? C21 N3A C20A 112(2) . . ? N2A C19A C20A 114(3) . . ? N2A C19A S3A 135(3) . . ? C20A C19A S3A 107(2) . . ? N3A C20A C19A 120(3) . . ? N3A C20A S2A 129(2) . . ? C19A C20A S2A 111(3) . . ? C26A C25A C22 119.5(15) . . ? C25A C26A C27 120.7(14) . . ? 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 Cd1 N1 2.290(6) . ? Cd1 N4 2.299(6) 1_545 ? Cd1 O4 2.307(4) . ? Cd1 O2 2.332(4) 8_755 ? Cd1 O3 2.334(4) 3_655 ? Cd1 O1 2.466(4) 8_755 ? Cd1 O4 2.601(4) 3_655 ? Cd1 C1 2.716(6) 8_755 ? S1 C2 1.705(6) . ? S1 C5 1.714(5) . ? N1 C9 1.347(8) . ? N1 C7 1.362(7) . ? O1 C1 1.246(8) . ? C1 O2 1.263(7) . ? C1 C2 1.491(8) . ? N2 C18 1.297(10) . ? N2 C19 1.347(12) . ? S2 C20 1.735(8) . ? S2 C18 1.777(7) . ? C2 C3 1.366(9) . ? S3 C19 1.713(10) . ? S3 C21 1.770(8) . ? N3 C21 1.262(10) . ? N3 C20 1.359(12) . ? O3 C6 1.259(7) . ? C3 C4 1.403(8) . ? N4 C30 1.333(8) . ? N4 C32 1.356(9) . ? O4 C6 1.249(7) . ? C4 C5 1.374(8) . ? C5 C6 1.471(7) . ? C7 C8 1.355(9) . ? C8 C11 1.414(8) . ? C9 C10 1.382(9) . ? C10 C11 1.392(8) . ? C11 C12 1.471(9) . ? C12 C13 1.400(9) . ? C12 C15 1.409(8) . ? C13 C14 1.361(9) . ? C14 C17 1.396(9) . ? C15 C16 1.373(9) . ? C16 C17 1.407(9) . ? C17 C18 1.458(10) . ? C18 N2A 1.283(18) . ? C18 S2A 1.789(12) . ? C19 C20 1.379(13) . ? C21 N3A 1.277(19) . ? C21 C22 1.451(12) . ? C21 S3A 1.856(13) . ? C22 C23 1.389(12) . ? C22 C25A 1.419(13) . ? C22 C25 1.427(15) . ? C23 C24 1.376(11) . ? C24 C27 1.379(11) . ? C25 C26 1.394(18) . ? C26 C27 1.423(15) . ? C27 C26A 1.425(13) . ? C27 C28 1.483(11) . ? C28 C29 1.395(10) . ? C28 C31 1.403(10) . ? C29 C30 1.364(10) . ? C31 C32 1.357(10) . ? O5 C33 1.262(10) . ? C33 N5 1.309(11) . ? N5 C35 1.438(9) . ? N5 C34 1.454(9) . ? O6 C38 1.247(16) . ? C38 N6 1.325(15) . ? N6 C37 1.426(13) . ? N6 C36 1.452(14) . ? C38A O6A 1.25(2) . ? C38A N6A 1.313(19) . ? N6A C36A 1.434(17) . ? N6A C37A 1.445(17) . ? O7 C39 1.266(17) . ? C39 N7 1.323(11) . ? N7 C40 1.437(10) . ? N7 C41 1.458(10) . ? N2A C19A 1.35(2) . ? S2A C20A 1.721(19) . ? S3A C19A 1.721(19) . ? N3A C20A 1.36(2) . ? C19A C20A 1.38(2) . ? C25A C26A 1.389(15) . ?