#------------------------------------------------------------------------------ #$Date: 2021-06-24 04:27:47 +0300 (Thu, 24 Jun 2021) $ #$Revision: 266649 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/30/7243094.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_7243094 loop_ _publ_author_name 'Tseng, Tien-Wen' 'Luo, Tzuoo-Tsair' 'Tseng, Kuo-Yang' 'Huang, Guang-Cheng' 'Hong, Yu-Xian' _publ_section_title ; Bent-bis(triazolyl)-based coordination polymers tuned by the dicarboxylate ligands: syntheses, structures and properties ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D1CE00780G _journal_year 2021 _chemical_formula_sum 'C30 H24 Cd N6 O9 S' _chemical_formula_weight 757.01 _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' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-06-12 deposited with the CCDC. 2021-06-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.306(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.0668(4) _cell_length_b 25.6268(15) _cell_length_c 19.2630(12) _cell_measurement_reflns_used 9997 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 23.99 _cell_measurement_theta_min 2.26 _cell_volume 2989.9(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_unetI/netI 0.0428 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 74339 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.157 _diffrn_reflns_theta_min 1.910 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.867 _exptl_absorpt_correction_T_max 0.9952 _exptl_absorpt_correction_T_min 0.9337 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.682 _exptl_crystal_description needle _exptl_crystal_F_000 1528 _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.070 _refine_diff_density_max 1.494 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.115 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 436 _refine_ls_number_reflns 6628 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.201 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0450 _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^)+13.9731P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.1011 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5797 _reflns_number_total 6628 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce00780g2.cif _cod_data_source_block shelx_CCDC1 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7243094 _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 0.712 _shelx_estimated_absorpt_t_max 0.942 _shelx_res_file ; TITL SIR92 run in space group P 21/c shelx.res created by SHELXL-2018/3 at 16:08:24 on 27-Apr-2021 CELL 0.71073 6.0668 25.6268 19.2630 90.000 93.306 90.000 ZERR 4.00 0.0004 0.0015 0.0012 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC CD S C H N O UNIT 4 4 120 96 24 36 MERG 2 OMIT 0 1 1 DFIX 0.820 0.0020 H8A O8 H8B O8 DANG 1.2950 0.0040 H8A H8B DFIX 0.820 0.0020 H9A O9 H9B O9 DANG 1.2960 0.0040 H9A H9B FMAP 2 PLAN 5 SIZE 0.070 0.140 0.420 ACTA BOND $H CONF L.S. 80 TEMP -173.00 WGHT 0.000000 13.973100 FVAR 0.32809 CD1 1 0.865389 0.118985 0.817964 11.00000 0.00979 0.00974 = 0.01051 -0.00118 -0.00041 0.00057 S1 2 0.443641 0.440292 0.722701 11.00000 0.01359 0.01003 = 0.01143 -0.00006 0.00107 0.00172 C1 3 0.667844 0.272993 0.755626 11.00000 0.01837 0.01242 = 0.01174 0.00132 0.00946 0.00475 C2 3 0.818605 0.313604 0.766811 11.00000 0.01624 0.01771 = 0.01488 0.00493 0.00051 0.00408 AFIX 43 H2 4 0.968689 0.305971 0.779646 11.00000 -1.20000 AFIX 0 C3 3 0.750442 0.365375 0.759272 11.00000 0.01895 0.01485 = 0.01227 0.00181 0.00209 -0.00186 AFIX 43 H3 4 0.851532 0.393259 0.767879 11.00000 -1.20000 AFIX 0 C4 3 0.532265 0.375064 0.738979 11.00000 0.01841 0.01285 = 0.01114 0.00365 0.00459 0.00227 C5 3 0.378810 0.335094 0.726528 11.00000 0.01716 0.01439 = 0.01617 0.00177 -0.00011 0.00458 AFIX 43 H5 4 0.230230 0.342725 0.711720 11.00000 -1.20000 AFIX 0 C6 3 0.448806 0.283835 0.736338 11.00000 0.02214 0.00998 = 0.01792 0.00120 0.00075 -0.00307 AFIX 43 H6 4 0.346001 0.256059 0.729792 11.00000 -1.20000 AFIX 0 C7 3 0.744217 0.217306 0.767151 11.00000 0.02790 0.01309 = 0.00633 0.00077 0.00310 0.00479 C8 3 0.504587 0.446833 0.634338 11.00000 0.01797 0.00909 = 0.00992 0.00032 0.00059 0.00284 C9 3 0.351533 0.426808 0.584073 11.00000 0.01141 0.01302 = 0.01447 0.00156 -0.00010 0.00054 AFIX 43 H9 4 0.209816 0.415609 0.596490 11.00000 -1.20000 AFIX 0 C10 3 0.410720 0.423681 0.516215 11.00000 0.01399 0.01349 = 0.01406 -0.00132 -0.00371 -0.00086 AFIX 43 H10 4 0.309413 0.410342 0.481168 11.00000 -1.20000 AFIX 0 C11 3 0.620229 0.440195 0.499135 11.00000 0.01538 0.00788 = 0.01163 0.00097 0.00066 0.00191 C12 3 0.766504 0.461921 0.549567 11.00000 0.01399 0.01049 = 0.01360 0.00148 0.00017 -0.00026 AFIX 43 H12 4 0.906450 0.474304 0.537122 11.00000 -1.20000 AFIX 0 C13 3 0.707905 0.465456 0.617775 11.00000 0.01575 0.00907 = 0.01446 -0.00032 -0.00637 -0.00110 AFIX 43 H13 4 0.805981 0.480432 0.652486 11.00000 -1.20000 AFIX 0 C14 3 0.695153 0.430829 0.426831 11.00000 0.01679 0.01060 = 0.01241 0.00289 -0.00564 0.00508 C15 3 1.453445 0.249374 0.986623 11.00000 0.01772 0.01039 = 0.01267 -0.00015 -0.00300 -0.00137 C16 3 1.591834 0.263911 0.935733 11.00000 0.02025 0.02277 = 0.01078 -0.00374 0.00163 -0.00574 AFIX 43 H16 4 1.569125 0.250416 0.889945 11.00000 -1.20000 AFIX 0 C17 3 1.764539 0.298307 0.951432 11.00000 0.01841 0.02533 = 0.01393 -0.00003 0.00475 -0.00646 AFIX 43 H17 4 1.861731 0.308243 0.916816 11.00000 -1.20000 AFIX 0 C18 3 1.792749 0.317898 1.018450 11.00000 0.01361 0.01000 = 0.01559 0.00279 -0.00339 -0.00157 C19 3 1.658670 0.302179 1.069735 11.00000 0.03020 0.01792 = 0.01035 -0.00191 0.00225 -0.00738 AFIX 43 H19 4 1.683686 0.314883 1.115848 11.00000 -1.20000 AFIX 0 C20 3 1.486730 0.267693 1.053850 11.00000 0.02203 0.01928 = 0.01378 -0.00104 0.00468 -0.00741 AFIX 43 H20 4 1.392808 0.256788 1.088882 11.00000 -1.20000 AFIX 0 C21 3 1.207772 0.194861 0.906927 11.00000 0.01996 0.01516 = 0.01128 -0.00001 0.00212 -0.00260 AFIX 43 H21 4 1.283975 0.199054 0.865567 11.00000 -1.20000 AFIX 0 C22 3 0.981765 0.173134 0.980119 11.00000 0.01897 0.01596 = 0.01681 0.00050 0.00146 -0.00163 AFIX 43 H22 4 0.857624 0.157476 0.999653 11.00000 -1.20000 AFIX 0 C23 3 2.007860 0.393233 0.993033 11.00000 0.01788 0.01188 = 0.01090 0.00081 0.00055 -0.00349 C24 3 1.847188 0.416592 0.949819 11.00000 0.01059 0.01972 = 0.01852 0.00511 -0.00213 -0.00246 AFIX 43 H24 4 1.700489 0.403483 0.947848 11.00000 -1.20000 AFIX 0 C25 3 1.899134 0.459149 0.909246 11.00000 0.01379 0.01732 = 0.01446 0.00389 -0.00415 0.00233 AFIX 43 H25 4 1.789251 0.475411 0.879494 11.00000 -1.20000 AFIX 0 C26 3 2.114649 0.477440 0.913024 11.00000 0.01761 0.01012 = 0.01033 0.00104 -0.00047 -0.00358 C27 3 2.275405 0.454675 0.957050 11.00000 0.01048 0.01967 = 0.01834 0.00260 -0.00322 -0.00201 AFIX 43 H27 4 2.421854 0.467950 0.959524 11.00000 -1.20000 AFIX 0 C28 3 2.221171 0.412398 0.997470 11.00000 0.01556 0.01663 = 0.01675 0.00574 -0.00759 -0.00193 AFIX 43 H28 4 2.330053 0.396645 1.028100 11.00000 -1.20000 AFIX 0 C29 3 2.080204 0.536410 0.809542 11.00000 0.01252 0.01070 = 0.01295 -0.00209 0.00061 -0.00199 AFIX 43 H29 4 1.946597 0.523063 0.788350 11.00000 -1.20000 AFIX 0 C30 3 2.372743 0.579477 0.832463 11.00000 0.01524 0.01542 = 0.01652 0.00060 0.00069 -0.00479 AFIX 43 H30 4 2.487926 0.604175 0.828157 11.00000 -1.20000 AFIX 0 N1 5 1.023680 0.167603 0.912209 11.00000 0.01602 0.01538 = 0.01317 0.00212 -0.00097 -0.00292 N2 5 1.269879 0.215600 0.968925 11.00000 0.01493 0.01278 = 0.01188 -0.00105 0.00309 -0.00248 N3 5 1.124696 0.201630 1.016965 11.00000 0.02036 0.01817 = 0.01308 -0.00115 0.00279 -0.00395 N4 5 2.201057 0.574529 0.783978 11.00000 0.01333 0.01045 = 0.01313 0.00117 0.00050 -0.00237 N5 5 2.176508 0.519963 0.869591 11.00000 0.01227 0.01042 = 0.01063 0.00032 -0.00058 -0.00105 N6 5 2.366523 0.547535 0.885431 11.00000 0.01361 0.01724 = 0.01345 0.00217 -0.00072 -0.00425 O1 6 0.946039 0.206881 0.763290 11.00000 0.02494 0.01972 = 0.01573 -0.00033 0.00163 0.00943 O2 6 0.601900 0.184388 0.782944 11.00000 0.03120 0.01163 = 0.02282 0.00293 0.00231 0.00229 O3 6 0.879621 0.447107 0.410907 11.00000 0.01816 0.01574 = 0.01641 -0.00218 0.00426 -0.00295 O4 6 0.575493 0.401483 0.387096 11.00000 0.01512 0.01958 = 0.01371 -0.00490 -0.00290 0.00091 O5 6 0.206673 0.441925 0.728385 11.00000 0.01779 0.01260 = 0.01687 0.00045 0.00278 0.00461 O6 6 0.583821 0.474763 0.764459 11.00000 0.02128 0.01272 = 0.01332 -0.00169 -0.00163 -0.00124 O7 6 1.965183 0.351968 1.037036 11.00000 0.02030 0.01829 = 0.01556 0.00772 -0.00548 -0.00980 O8 6 1.226133 0.099003 0.793586 11.00000 0.00935 0.02932 = 0.01539 0.00454 -0.00137 0.00331 O9 6 1.215300 0.162790 0.668983 11.00000 0.02628 0.03978 = 0.02723 -0.00427 0.00344 -0.00082 H8A 4 1.257982 0.117703 0.761119 11.00000 -1.50000 H8B 4 1.331478 0.101882 0.821955 11.00000 -1.50000 H9A 4 1.138859 0.181078 0.692980 11.00000 -1.50000 H9B 4 1.134040 0.155604 0.634793 11.00000 -1.50000 HKLF 4 REM SIR92 run in space group P 21/c REM wR2 = 0.1011, GooF = S = 1.202, Restrained GooF = 1.201 for all data REM R1 = 0.0450 for 5797 Fo > 4sig(Fo) and 0.0546 for all 6628 data REM 436 parameters refined using 6 restraints END WGHT 0.0000 14.0036 REM Highest difference peak 1.494, deepest hole -0.966, 1-sigma level 0.115 Q1 1 1.4780 0.1197 0.8191 11.00000 0.05 1.49 Q2 1 1.0596 0.1209 0.8192 11.00000 0.05 1.07 Q3 1 1.2231 0.1229 0.8201 11.00000 0.05 0.89 Q4 1 1.3450 0.1402 0.6837 11.00000 0.05 0.67 Q5 1 0.6711 0.1192 0.8198 11.00000 0.05 0.61 ; _shelx_res_checksum 63971 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 Cd1 Cd 0.86539(5) 0.11899(2) 0.81796(2) 0.01005(8) Uani 1 1 d . . . . . S1 S 0.44364(16) 0.44029(4) 0.72270(5) 0.01167(19) Uani 1 1 d . . . . . C1 C 0.6678(7) 0.27299(15) 0.7556(2) 0.0138(8) Uani 1 1 d . . . . . C2 C 0.8186(7) 0.31360(16) 0.7668(2) 0.0163(8) Uani 1 1 d . . . . . H2 H 0.968689 0.305971 0.779646 0.020 Uiso 1 1 calc R U . . . C3 C 0.7504(7) 0.36537(16) 0.7593(2) 0.0153(8) Uani 1 1 d . . . . . H3 H 0.851532 0.393259 0.767879 0.018 Uiso 1 1 calc R U . . . C4 C 0.5323(7) 0.37506(15) 0.7390(2) 0.0140(8) Uani 1 1 d . . . . . C5 C 0.3788(7) 0.33509(16) 0.7265(2) 0.0159(8) Uani 1 1 d . . . . . H5 H 0.230230 0.342725 0.711720 0.019 Uiso 1 1 calc R U . . . C6 C 0.4488(7) 0.28384(15) 0.7363(2) 0.0167(9) Uani 1 1 d . . . . . H6 H 0.346001 0.256059 0.729792 0.020 Uiso 1 1 calc R U . . . C7 C 0.7442(7) 0.21731(15) 0.7672(2) 0.0157(8) Uani 1 1 d . . . . . C8 C 0.5046(7) 0.44683(15) 0.6343(2) 0.0123(8) Uani 1 1 d . . . . . C9 C 0.3515(6) 0.42681(15) 0.5841(2) 0.0130(8) Uani 1 1 d . . . . . H9 H 0.209816 0.415609 0.596490 0.016 Uiso 1 1 calc R U . . . C10 C 0.4107(7) 0.42368(15) 0.5162(2) 0.0140(8) Uani 1 1 d . . . . . H10 H 0.309413 0.410342 0.481168 0.017 Uiso 1 1 calc R U . . . C11 C 0.6202(7) 0.44019(14) 0.4991(2) 0.0116(8) Uani 1 1 d . . . . . C12 C 0.7665(7) 0.46192(15) 0.5496(2) 0.0127(8) Uani 1 1 d . . . . . H12 H 0.906450 0.474304 0.537122 0.015 Uiso 1 1 calc R U . . . C13 C 0.7079(7) 0.46546(15) 0.6178(2) 0.0134(8) Uani 1 1 d . . . . . H13 H 0.805981 0.480432 0.652486 0.016 Uiso 1 1 calc R U . . . C14 C 0.6952(7) 0.43083(15) 0.4268(2) 0.0135(8) Uani 1 1 d . . . . . C15 C 1.4534(7) 0.24937(15) 0.9866(2) 0.0137(8) Uani 1 1 d . . . . . C16 C 1.5918(7) 0.26391(17) 0.9357(2) 0.0179(9) Uani 1 1 d . . . . . H16 H 1.569125 0.250416 0.889945 0.021 Uiso 1 1 calc R U . . . C17 C 1.7645(7) 0.29831(17) 0.9514(2) 0.0191(9) Uani 1 1 d . . . . . H17 H 1.861731 0.308243 0.916816 0.023 Uiso 1 1 calc R U . . . C18 C 1.7927(7) 0.31790(15) 1.0185(2) 0.0132(8) Uani 1 1 d . . . . . C19 C 1.6587(8) 0.30218(16) 1.0697(2) 0.0194(9) Uani 1 1 d . . . . . H19 H 1.683686 0.314883 1.115848 0.023 Uiso 1 1 calc R U . . . C20 C 1.4867(7) 0.26769(16) 1.0539(2) 0.0182(9) Uani 1 1 d . . . . . H20 H 1.392808 0.256788 1.088882 0.022 Uiso 1 1 calc R U . . . C21 C 1.2078(7) 0.19486(15) 0.9069(2) 0.0154(8) Uani 1 1 d . . . . . H21 H 1.283975 0.199054 0.865567 0.019 Uiso 1 1 calc R U . . . C22 C 0.9818(7) 0.17313(16) 0.9801(2) 0.0172(9) Uani 1 1 d . . . . . H22 H 0.857624 0.157476 0.999653 0.021 Uiso 1 1 calc R U . . . C23 C 2.0079(7) 0.39323(15) 0.9930(2) 0.0136(8) Uani 1 1 d . . . . . C24 C 1.8472(7) 0.41659(16) 0.9498(2) 0.0164(8) Uani 1 1 d . . . . . H24 H 1.700489 0.403483 0.947848 0.020 Uiso 1 1 calc R U . . . C25 C 1.8991(7) 0.45915(16) 0.9092(2) 0.0154(8) Uani 1 1 d . . . . . H25 H 1.789251 0.475411 0.879494 0.018 Uiso 1 1 calc R U . . . C26 C 2.1146(7) 0.47744(15) 0.9130(2) 0.0127(8) Uani 1 1 d . . . . . C27 C 2.2754(7) 0.45468(16) 0.9570(2) 0.0163(8) Uani 1 1 d . . . . . H27 H 2.421854 0.467950 0.959524 0.020 Uiso 1 1 calc R U . . . C28 C 2.2212(7) 0.41240(16) 0.9975(2) 0.0166(9) Uani 1 1 d . . . . . H28 H 2.330053 0.396645 1.028100 0.020 Uiso 1 1 calc R U . . . C29 C 2.0802(6) 0.53641(15) 0.8095(2) 0.0121(8) Uani 1 1 d . . . . . H29 H 1.946597 0.523063 0.788350 0.014 Uiso 1 1 calc R U . . . C30 C 2.3727(7) 0.57948(16) 0.8325(2) 0.0157(8) Uani 1 1 d . . . . . H30 H 2.487926 0.604175 0.828157 0.019 Uiso 1 1 calc R U . . . N1 N 1.0237(6) 0.16760(13) 0.91221(17) 0.0149(7) Uani 1 1 d . . . . . N2 N 1.2699(6) 0.21560(13) 0.96892(17) 0.0131(7) Uani 1 1 d . . . . . N3 N 1.1247(6) 0.20163(14) 1.01697(18) 0.0171(7) Uani 1 1 d . . . . . N4 N 2.2011(5) 0.57453(12) 0.78398(17) 0.0123(7) Uani 1 1 d . . . . . N5 N 2.1765(5) 0.51996(12) 0.86959(17) 0.0112(7) Uani 1 1 d . . . . . N6 N 2.3665(6) 0.54753(13) 0.88543(17) 0.0148(7) Uani 1 1 d . . . . . O1 O 0.9460(5) 0.20688(12) 0.76329(15) 0.0201(6) Uani 1 1 d . . . . . O2 O 0.6019(5) 0.18439(11) 0.78294(16) 0.0219(7) Uani 1 1 d . . . . . O3 O 0.8796(5) 0.44711(11) 0.41091(15) 0.0166(6) Uani 1 1 d . . . . . O4 O 0.5755(5) 0.40148(11) 0.38710(14) 0.0163(6) Uani 1 1 d . . . . . O5 O 0.2067(5) 0.44192(11) 0.72839(15) 0.0157(6) Uani 1 1 d . . . . . O6 O 0.5838(5) 0.47476(11) 0.76446(14) 0.0159(6) Uani 1 1 d . . . . . O7 O 1.9652(5) 0.35197(11) 1.03704(15) 0.0183(6) Uani 1 1 d . . . . . O8 O 1.2261(5) 0.09900(12) 0.79359(15) 0.0181(6) Uani 1 1 d D . . . . O9 O 1.2153(6) 0.16279(15) 0.66898(18) 0.0310(8) Uani 1 1 d D . . . . H8A H 1.258(7) 0.1177(17) 0.7611(16) 0.047 Uiso 1 1 d D U . . . H8B H 1.331(5) 0.102(2) 0.8220(17) 0.047 Uiso 1 1 d D U . . . H9A H 1.139(6) 0.1811(18) 0.693(2) 0.047 Uiso 1 1 d D U . . . H9B H 1.134(6) 0.156(2) 0.6348(16) 0.047 Uiso 1 1 d D 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 Cd1 0.00979(13) 0.00974(13) 0.01051(13) -0.00118(11) -0.00041(9) 0.00057(11) S1 0.0136(5) 0.0100(4) 0.0114(4) -0.0001(4) 0.0011(4) 0.0017(4) C1 0.018(2) 0.0124(19) 0.0117(19) 0.0013(15) 0.0095(16) 0.0048(16) C2 0.016(2) 0.018(2) 0.015(2) 0.0049(16) 0.0005(16) 0.0041(16) C3 0.019(2) 0.0149(19) 0.0123(19) 0.0018(15) 0.0021(16) -0.0019(16) C4 0.018(2) 0.0128(19) 0.0111(18) 0.0037(15) 0.0046(15) 0.0023(16) C5 0.017(2) 0.0144(19) 0.016(2) 0.0018(16) -0.0001(16) 0.0046(16) C6 0.022(2) 0.0100(19) 0.018(2) 0.0012(15) 0.0007(17) -0.0031(16) C7 0.028(2) 0.0131(19) 0.0063(18) 0.0008(15) 0.0031(16) 0.0048(17) C8 0.018(2) 0.0091(18) 0.0099(18) 0.0003(14) 0.0006(15) 0.0028(15) C9 0.0114(19) 0.0130(19) 0.0145(19) 0.0016(15) -0.0001(15) 0.0005(15) C10 0.0140(19) 0.0135(19) 0.0141(19) -0.0013(15) -0.0037(16) -0.0009(15) C11 0.0154(19) 0.0079(17) 0.0116(19) 0.0010(14) 0.0007(15) 0.0019(15) C12 0.0140(19) 0.0105(18) 0.0136(19) 0.0015(15) 0.0002(15) -0.0003(15) C13 0.016(2) 0.0091(18) 0.0145(19) -0.0003(15) -0.0064(16) -0.0011(15) C14 0.017(2) 0.0106(18) 0.0124(19) 0.0029(15) -0.0056(16) 0.0051(15) C15 0.018(2) 0.0104(18) 0.0127(19) -0.0001(15) -0.0030(16) -0.0014(16) C16 0.020(2) 0.023(2) 0.0108(19) -0.0037(16) 0.0016(16) -0.0057(17) C17 0.018(2) 0.025(2) 0.014(2) 0.0000(17) 0.0047(17) -0.0065(18) C18 0.0136(19) 0.0100(18) 0.016(2) 0.0028(15) -0.0034(15) -0.0016(15) C19 0.030(2) 0.018(2) 0.0104(19) -0.0019(16) 0.0023(17) -0.0074(18) C20 0.022(2) 0.019(2) 0.014(2) -0.0010(16) 0.0047(17) -0.0074(17) C21 0.020(2) 0.015(2) 0.0113(19) 0.0000(15) 0.0021(16) -0.0026(16) C22 0.019(2) 0.016(2) 0.017(2) 0.0005(16) 0.0015(17) -0.0016(17) C23 0.018(2) 0.0119(19) 0.0109(18) 0.0008(15) 0.0006(15) -0.0035(15) C24 0.0106(19) 0.020(2) 0.019(2) 0.0051(17) -0.0021(16) -0.0025(16) C25 0.014(2) 0.017(2) 0.0145(19) 0.0039(16) -0.0042(16) 0.0023(16) C26 0.018(2) 0.0101(18) 0.0103(18) 0.0010(15) -0.0005(15) -0.0036(15) C27 0.0105(19) 0.020(2) 0.018(2) 0.0026(17) -0.0032(16) -0.0020(16) C28 0.016(2) 0.017(2) 0.017(2) 0.0057(16) -0.0076(16) -0.0019(16) C29 0.0125(19) 0.0107(18) 0.0130(19) -0.0021(15) 0.0006(15) -0.0020(15) C30 0.015(2) 0.0154(19) 0.017(2) 0.0006(16) 0.0007(16) -0.0048(16) N1 0.0160(17) 0.0154(17) 0.0132(17) 0.0021(13) -0.0010(13) -0.0029(14) N2 0.0149(17) 0.0128(16) 0.0119(16) -0.0011(13) 0.0031(13) -0.0025(13) N3 0.0204(18) 0.0182(18) 0.0131(17) -0.0012(14) 0.0028(14) -0.0040(15) N4 0.0133(16) 0.0104(16) 0.0131(16) 0.0012(13) 0.0005(13) -0.0024(13) N5 0.0123(16) 0.0104(15) 0.0106(16) 0.0003(12) -0.0006(13) -0.0011(13) N6 0.0136(17) 0.0172(17) 0.0134(17) 0.0022(14) -0.0007(13) -0.0043(14) O1 0.0249(17) 0.0197(15) 0.0157(15) -0.0003(12) 0.0016(12) 0.0094(13) O2 0.0312(18) 0.0116(14) 0.0228(16) 0.0029(12) 0.0023(14) 0.0023(13) O3 0.0182(15) 0.0157(14) 0.0164(15) -0.0022(11) 0.0043(12) -0.0029(12) O4 0.0151(14) 0.0196(15) 0.0137(14) -0.0049(12) -0.0029(11) 0.0009(12) O5 0.0178(15) 0.0126(14) 0.0169(14) 0.0005(11) 0.0028(12) 0.0046(11) O6 0.0213(15) 0.0127(14) 0.0133(14) -0.0017(11) -0.0016(12) -0.0012(12) O7 0.0203(15) 0.0183(15) 0.0156(15) 0.0077(12) -0.0055(12) -0.0098(12) O8 0.0094(14) 0.0293(17) 0.0154(15) 0.0045(13) -0.0014(11) 0.0033(12) O9 0.0263(18) 0.040(2) 0.0272(19) -0.0043(16) 0.0034(15) -0.0008(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cd Cd -0.8075 1.2024 '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' 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' 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 N4 Cd1 O8 80.67(11) 2_846 . ? N4 Cd1 O4 106.12(11) 2_846 4_566 ? O8 Cd1 O4 144.94(10) . 4_566 ? N4 Cd1 N1 165.41(12) 2_846 . ? O8 Cd1 N1 85.73(11) . . ? O4 Cd1 N1 88.06(11) 4_566 . ? N4 Cd1 O2 91.44(11) 2_846 . ? O8 Cd1 O2 136.18(11) . . ? O4 Cd1 O2 78.70(10) 4_566 . ? N1 Cd1 O2 94.75(11) . . ? N4 Cd1 O3 106.19(11) 2_846 4_566 ? O8 Cd1 O3 90.08(10) . 4_566 ? O4 Cd1 O3 54.88(9) 4_566 4_566 ? N1 Cd1 O3 78.94(11) . 4_566 ? O2 Cd1 O3 133.11(10) . 4_566 ? N4 Cd1 O1 96.55(11) 2_846 . ? O8 Cd1 O1 84.58(10) . . ? O4 Cd1 O1 127.30(10) 4_566 . ? N1 Cd1 O1 76.81(10) . . ? O2 Cd1 O1 53.36(10) . . ? O3 Cd1 O1 155.48(10) 4_566 . ? N4 Cd1 C14 111.95(11) 2_846 4_566 ? O8 Cd1 C14 117.28(11) . 4_566 ? O4 Cd1 C14 27.92(11) 4_566 4_566 ? N1 Cd1 C14 79.03(11) . 4_566 ? O2 Cd1 C14 105.70(12) . 4_566 ? O3 Cd1 C14 27.42(11) 4_566 4_566 ? O1 Cd1 C14 145.88(11) . 4_566 ? O6 S1 O5 119.80(17) . . ? O6 S1 C8 109.25(18) . . ? O5 S1 C8 109.46(18) . . ? O6 S1 C4 108.39(18) . . ? O5 S1 C4 107.76(18) . . ? C8 S1 C4 100.41(18) . . ? C6 C1 C2 120.1(4) . . ? C6 C1 C7 120.6(4) . . ? C2 C1 C7 119.3(4) . . ? C1 C2 C3 120.4(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 118.3(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 122.4(4) . . ? C3 C4 S1 119.6(3) . . ? C5 C4 S1 117.9(3) . . ? C6 C5 C4 118.3(4) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C1 C6 C5 120.4(4) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O2 C7 O1 123.8(4) . . ? O2 C7 C1 117.4(4) . . ? O1 C7 C1 118.8(4) . . ? C13 C8 C9 122.3(4) . . ? C13 C8 S1 119.7(3) . . ? C9 C8 S1 117.6(3) . . ? C10 C9 C8 118.6(4) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.6(4) . . ? C12 C11 C14 119.6(4) . . ? C10 C11 C14 119.7(4) . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C8 C13 C12 118.7(4) . . ? C8 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? O3 C14 O4 122.6(4) . . ? O3 C14 C11 119.7(3) . . ? O4 C14 C11 117.3(4) . . ? O3 C14 Cd1 65.2(2) . 4_565 ? O4 C14 Cd1 59.0(2) . 4_565 ? C11 C14 Cd1 159.7(3) . 4_565 ? C16 C15 C20 120.9(4) . . ? C16 C15 N2 119.3(4) . . ? C20 C15 N2 119.8(4) . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 118.9(4) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 121.1(4) . . ? C19 C18 O7 117.7(4) . . ? C17 C18 O7 121.1(4) . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C15 C20 C19 119.4(4) . . ? C15 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? N1 C21 N2 109.6(4) . . ? N1 C21 H21 125.2 . . ? N2 C21 H21 125.2 . . ? N3 C22 N1 115.2(4) . . ? N3 C22 H22 122.4 . . ? N1 C22 H22 122.4 . . ? C24 C23 C28 120.6(4) . . ? C24 C23 O7 123.2(4) . . ? C28 C23 O7 116.1(3) . . ? C23 C24 C25 120.3(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 118.7(4) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C27 C26 C25 121.2(4) . . ? C27 C26 N5 118.6(4) . . ? C25 C26 N5 120.2(4) . . ? C26 C27 C28 119.5(4) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C23 C28 C27 119.7(4) . . ? C23 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? N4 C29 N5 109.2(3) . . ? N4 C29 H29 125.4 . . ? N5 C29 H29 125.4 . . ? N6 C30 N4 114.8(4) . . ? N6 C30 H30 122.6 . . ? N4 C30 H30 122.6 . . ? C21 N1 C22 103.0(3) . . ? C21 N1 Cd1 121.7(3) . . ? C22 N1 Cd1 135.0(3) . . ? C21 N2 N3 110.0(3) . . ? C21 N2 C15 128.6(3) . . ? N3 N2 C15 121.4(3) . . ? C22 N3 N2 102.2(3) . . ? C29 N4 C30 103.3(3) . . ? C29 N4 Cd1 127.5(3) . 2_856 ? C30 N4 Cd1 129.2(3) . 2_856 ? C29 N5 N6 110.5(3) . . ? C29 N5 C26 128.9(3) . . ? N6 N5 C26 120.4(3) . . ? C30 N6 N5 102.1(3) . . ? C7 O1 Cd1 87.3(2) . . ? C7 O2 Cd1 94.7(3) . . ? C14 O3 Cd1 87.4(2) . 4_565 ? C14 O4 Cd1 93.1(2) . 4_565 ? C23 O7 C18 118.9(3) . . ? Cd1 O8 H8A 107(4) . . ? Cd1 O8 H8B 124(4) . . ? H8A O8 H8B 104.3(5) . . ? H9A O9 H9B 104.3(5) . . ? 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 N4 2.286(3) 2_846 ? Cd1 O8 2.322(3) . ? Cd1 O4 2.326(3) 4_566 ? Cd1 N1 2.360(3) . ? Cd1 O2 2.386(3) . ? Cd1 O3 2.462(3) 4_566 ? Cd1 O1 2.546(3) . ? Cd1 C14 2.710(4) 4_566 ? S1 O6 1.439(3) . ? S1 O5 1.449(3) . ? S1 C8 1.770(4) . ? S1 C4 1.778(4) . ? C1 C6 1.387(6) . ? C1 C2 1.394(6) . ? C1 C7 1.513(5) . ? C2 C3 1.395(6) . ? C2 H2 0.9500 . ? C3 C4 1.381(6) . ? C3 H3 0.9500 . ? C4 C5 1.396(6) . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O2 1.257(5) . ? C7 O1 1.260(5) . ? C8 C13 1.377(6) . ? C8 C9 1.400(5) . ? C9 C10 1.378(6) . ? C9 H9 0.9500 . ? C10 C11 1.397(6) . ? C10 H10 0.9500 . ? C11 C12 1.394(5) . ? C11 C14 1.509(5) . ? C12 C13 1.384(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O3 1.249(5) . ? C14 O4 1.271(5) . ? C15 C16 1.378(6) . ? C15 C20 1.381(6) . ? C15 N2 1.436(5) . ? C16 C17 1.389(6) . ? C16 H16 0.9500 . ? C17 C18 1.387(6) . ? C17 H17 0.9500 . ? C18 C19 1.376(6) . ? C18 O7 1.393(5) . ? C19 C20 1.388(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 N1 1.326(5) . ? C21 N2 1.341(5) . ? C21 H21 0.9500 . ? C22 N3 1.311(5) . ? C22 N1 1.354(5) . ? C22 H22 0.9500 . ? C23 C24 1.381(6) . ? C23 C28 1.382(6) . ? C23 O7 1.389(5) . ? C24 C25 1.389(6) . ? C24 H24 0.9500 . ? C25 C26 1.387(6) . ? C25 H25 0.9500 . ? C26 C27 1.384(6) . ? C26 N5 1.437(5) . ? C27 C28 1.385(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 N4 1.333(5) . ? C29 N5 1.334(5) . ? C29 H29 0.9500 . ? C30 N6 1.310(5) . ? C30 N4 1.364(5) . ? C30 H30 0.9500 . ? N2 N3 1.362(5) . ? N5 N6 1.371(5) . ? O8 H8A 0.820(2) . ? O8 H8B 0.820(2) . ? O9 H9A 0.820(2) . ? O9 H9B 0.821(2) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.5(6) . . . . ? C7 C1 C2 C3 -177.4(4) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? C2 C3 C4 S1 -175.5(3) . . . . ? O6 S1 C4 C3 -27.8(4) . . . . ? O5 S1 C4 C3 -158.9(3) . . . . ? C8 S1 C4 C3 86.6(4) . . . . ? O6 S1 C4 C5 155.9(3) . . . . ? O5 S1 C4 C5 24.9(4) . . . . ? C8 S1 C4 C5 -89.6(3) . . . . ? C3 C4 C5 C6 1.2(6) . . . . ? S1 C4 C5 C6 177.4(3) . . . . ? C2 C1 C6 C5 1.4(6) . . . . ? C7 C1 C6 C5 179.3(4) . . . . ? C4 C5 C6 C1 -2.3(6) . . . . ? C6 C1 C7 O2 -24.5(6) . . . . ? C2 C1 C7 O2 153.4(4) . . . . ? C6 C1 C7 O1 158.3(4) . . . . ? C2 C1 C7 O1 -23.8(5) . . . . ? O6 S1 C8 C13 23.1(4) . . . . ? O5 S1 C8 C13 156.0(3) . . . . ? C4 S1 C8 C13 -90.8(3) . . . . ? O6 S1 C8 C9 -164.4(3) . . . . ? O5 S1 C8 C9 -31.4(4) . . . . ? C4 S1 C8 C9 81.8(3) . . . . ? C13 C8 C9 C10 2.8(6) . . . . ? S1 C8 C9 C10 -169.5(3) . . . . ? C8 C9 C10 C11 0.2(6) . . . . ? C9 C10 C11 C12 -2.8(6) . . . . ? C9 C10 C11 C14 172.7(4) . . . . ? C10 C11 C12 C13 2.5(6) . . . . ? C14 C11 C12 C13 -173.0(3) . . . . ? C9 C8 C13 C12 -3.1(6) . . . . ? S1 C8 C13 C12 169.1(3) . . . . ? C11 C12 C13 C8 0.5(6) . . . . ? C12 C11 C14 O3 -6.8(5) . . . . ? C10 C11 C14 O3 177.7(4) . . . . ? C12 C11 C14 O4 165.7(3) . . . . ? C10 C11 C14 O4 -9.8(5) . . . . ? C12 C11 C14 Cd1 91.8(8) . . . 4_565 ? C10 C11 C14 Cd1 -83.8(9) . . . 4_565 ? C20 C15 C16 C17 -1.4(7) . . . . ? N2 C15 C16 C17 177.3(4) . . . . ? C15 C16 C17 C18 -0.7(7) . . . . ? C16 C17 C18 C19 2.7(7) . . . . ? C16 C17 C18 O7 179.1(4) . . . . ? C17 C18 C19 C20 -2.5(7) . . . . ? O7 C18 C19 C20 -179.1(4) . . . . ? C16 C15 C20 C19 1.6(7) . . . . ? N2 C15 C20 C19 -177.1(4) . . . . ? C18 C19 C20 C15 0.4(7) . . . . ? C28 C23 C24 C25 1.2(6) . . . . ? O7 C23 C24 C25 177.3(4) . . . . ? C23 C24 C25 C26 0.1(6) . . . . ? C24 C25 C26 C27 -1.1(6) . . . . ? C24 C25 C26 N5 177.3(4) . . . . ? C25 C26 C27 C28 0.9(6) . . . . ? N5 C26 C27 C28 -177.6(4) . . . . ? C24 C23 C28 C27 -1.5(6) . . . . ? O7 C23 C28 C27 -177.8(4) . . . . ? C26 C27 C28 C23 0.4(6) . . . . ? N2 C21 N1 C22 -0.3(4) . . . . ? N2 C21 N1 Cd1 -175.6(2) . . . . ? N3 C22 N1 C21 0.1(5) . . . . ? N3 C22 N1 Cd1 174.5(3) . . . . ? N1 C21 N2 N3 0.4(5) . . . . ? N1 C21 N2 C15 -177.4(4) . . . . ? C16 C15 N2 C21 -0.2(6) . . . . ? C20 C15 N2 C21 178.5(4) . . . . ? C16 C15 N2 N3 -177.8(4) . . . . ? C20 C15 N2 N3 0.9(6) . . . . ? N1 C22 N3 N2 0.1(5) . . . . ? C21 N2 N3 C22 -0.3(4) . . . . ? C15 N2 N3 C22 177.7(4) . . . . ? N5 C29 N4 C30 -0.1(4) . . . . ? N5 C29 N4 Cd1 178.8(2) . . . 2_856 ? N6 C30 N4 C29 0.0(5) . . . . ? N6 C30 N4 Cd1 -178.9(3) . . . 2_856 ? N4 C29 N5 N6 0.2(4) . . . . ? N4 C29 N5 C26 -175.3(4) . . . . ? C27 C26 N5 C29 155.6(4) . . . . ? C25 C26 N5 C29 -22.9(6) . . . . ? C27 C26 N5 N6 -19.5(5) . . . . ? C25 C26 N5 N6 162.0(4) . . . . ? N4 C30 N6 N5 0.1(5) . . . . ? C29 N5 N6 C30 -0.2(4) . . . . ? C26 N5 N6 C30 175.7(3) . . . . ? O2 C7 O1 Cd1 -9.7(4) . . . . ? C1 C7 O1 Cd1 167.2(3) . . . . ? O1 C7 O2 Cd1 10.4(4) . . . . ? C1 C7 O2 Cd1 -166.6(3) . . . . ? O4 C14 O3 Cd1 -14.3(4) . . . 4_565 ? C11 C14 O3 Cd1 157.8(3) . . . 4_565 ? O3 C14 O4 Cd1 15.2(4) . . . 4_565 ? C11 C14 O4 Cd1 -157.1(3) . . . 4_565 ? C24 C23 O7 C18 28.8(6) . . . . ? C28 C23 O7 C18 -155.0(4) . . . . ? C19 C18 O7 C23 -137.9(4) . . . . ? C17 C18 O7 C23 45.5(5) . . . . ?