#------------------------------------------------------------------------------ #$Date: 2019-04-16 02:04:50 +0300 (Tue, 16 Apr 2019) $ #$Revision: 214647 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/97/7049719.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_7049719 loop_ _publ_author_name 'Zhu, Li-Na' 'Deng, Zhaopeng' 'Ng, Seik Weng' 'Huo, Li-Hua' 'Gao, Shan' _publ_section_title ; Cd(II) coordination polymers constructed from bis(pyridyl) ligand with asymmetric spacer in chelating mode and diverse organic dicarboxylates: syntheses, structural evolutions and properties ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT00840C _journal_year 2019 _chemical_formula_moiety '[Cd3 (H2 O)6 (O4 S)2 (C15 H20 N4)2 (C8 H4 O4)], 4(H2 O)' _chemical_formula_sum 'C38 H64 Cd3 N8 O22 S2' _chemical_formula_weight 1386.29 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-04-01 deposited with the CCDC. 2019-04-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.834(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.4280(15) _cell_length_b 9.4270(11) _cell_length_c 26.416(3) _cell_measurement_reflns_used 2271 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 29.1450 _cell_measurement_theta_min 3.3220 _cell_volume 5158.2(9) _computing_cell_refinement ; CrysAlis Pro (Agilent, 2013) ; _computing_data_collection ; CrysAlis Pro (Agilent, 2013) ; _computing_data_reduction ; CrysAlis Pro (Agilent, 2013) ; _computing_molecular_graphics '(K. Brandenburg, Diamond 3.1, 2009)' _computing_publication_material '(K. Brandenburg, Diamond 3.1, 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 16.1954 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_unetI/netI 0.0502 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 9678 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.562 _diffrn_reflns_theta_min 3.292 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.392 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis Pro (Agilent, 2013) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.785 _exptl_crystal_description prism _exptl_crystal_F_000 2800 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.952 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.096 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 5889 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.250 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0800 _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^)+51.0473P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1166 _refine_ls_wR_factor_ref 0.1270 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4120 _reflns_number_total 5889 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00840c2.cif _cod_data_source_block d6628 _cod_database_code 7049719 _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 0.788 _shelx_estimated_absorpt_t_max 0.851 _shelx_res_file ; TITL C2/c d6628.res created by SHELXL-2018/3 at 21:24:21 on 28-Mar-2019 CELL 0.71073 21.4280 9.4270 26.4159 90 104.834 90 ZERR 4 0.0015 0.00107 0.0027 0 0.009 0 LATT 7 SYMM -X,Y,0.5-Z SFAC C H N O S Cd UNIT 152 256 32 88 8 12 ACTA OMIT -10 2 1 OMIT -14 2 3 SIZE 0.18 0.16 0.12 FMAP 2 PLAN -1 EADP C7 C7' EADP C8 C8' SADI 0.01 N2 C7 N2 C7' SADI 0.01 N3 C8 N3 C8' SADI 0.01 C7 C8 C7' C8' SADI 0.01 C8 C9 C8' C9 L.S. 10 TEMP 22 WGHT 0.000000 51.047306 FVAR 1.34986 CD1 6 0.500000 0.500000 0.500000 10.50000 0.02297 0.06590 = 0.04084 0.00682 0.00422 -0.01514 CD2 6 0.846622 0.502809 0.707370 11.00000 0.03759 0.04712 = 0.04355 -0.00327 0.00178 -0.00500 S1 5 0.868830 0.206246 0.791788 11.00000 0.03364 0.03860 = 0.07729 0.01265 -0.00096 -0.00138 O1 4 0.591614 0.617857 0.502036 11.00000 0.02867 0.08875 = 0.07377 0.00746 0.01631 -0.01935 O2 4 0.618682 0.511237 0.435477 11.00000 0.04626 0.07837 = 0.07526 -0.00857 0.01248 -0.03450 O3 4 0.880555 0.291957 0.748402 11.00000 0.08177 0.05457 = 0.06397 0.01305 0.02272 0.01672 O4 4 0.821985 0.278600 0.814462 11.00000 0.06301 0.08115 = 0.09905 0.01850 0.03859 0.00880 O5 4 0.843698 0.068570 0.770555 11.00000 0.05300 0.04368 = 0.19901 -0.00542 -0.00087 -0.00646 O6 4 0.929278 0.189679 0.830483 11.00000 0.05173 0.09906 = 0.07334 0.02240 -0.01150 0.00622 O1W 4 0.492504 0.639844 0.571170 11.00000 0.03758 0.08699 = 0.05437 -0.00388 0.00650 -0.01888 AFIX 3 H11 2 0.458324 0.612853 0.578200 11.00000 -1.50000 H12 2 0.521674 0.624893 0.598650 11.00000 -1.50000 AFIX 0 O2W 4 0.782579 0.525800 0.764588 11.00000 0.04817 0.04862 = 0.05543 -0.00596 0.00724 0.00375 AFIX 3 H21 2 0.789399 0.453880 0.783998 11.00000 -1.50000 H22 2 0.743019 0.525870 0.749388 11.00000 -1.50000 AFIX 0 O3W 4 0.795185 0.711818 0.668700 11.00000 0.05062 0.06122 = 0.08467 0.01699 0.01471 0.01777 AFIX 3 H31 2 0.759495 0.723108 0.675840 11.00000 -1.50000 H32 2 0.820305 0.779798 0.679810 11.00000 -1.50000 AFIX 0 O4W 4 0.837545 0.976902 0.657703 11.00000 0.08862 0.07811 = 0.08841 -0.00094 0.02243 -0.03214 AFIX 3 H41 2 0.859773 1.002192 0.637303 11.00000 -1.50000 H42 2 0.850454 1.020482 0.686203 11.00000 -1.50000 AFIX 0 O5W 4 0.948280 1.177082 0.682023 11.00000 0.07096 0.11787 = 0.16181 -0.05248 0.02129 0.00088 AFIX 3 H51 2 0.936600 1.221372 0.705623 11.00000 -1.50000 H52 2 0.987460 1.194211 0.684713 11.00000 -1.50000 AFIX 0 N1 3 0.561282 0.323710 0.551974 11.00000 0.02700 0.05629 = 0.03867 0.00461 0.00025 -0.01321 N2 3 0.757419 0.403189 0.644978 11.00000 0.04630 0.12227 = 0.04943 -0.01011 0.00557 -0.02457 AFIX 13 0.8800 H2 2 0.732226 0.478190 0.641520 11.00000 -1.20000 AFIX 0 N3 3 0.885354 0.460230 0.632734 11.00000 0.04950 0.06660 = 0.06774 -0.01420 0.02126 -0.01585 AFIX 13 0.8800 PART 1 H3 2 0.912791 0.393031 0.646906 11.00000 -1.20000 AFIX 0 PART 0 N4 3 1.074239 0.619184 0.730935 11.00000 0.02685 0.04271 = 0.04586 0.00538 0.00717 0.00181 C1 1 0.614870 0.358602 0.589138 11.00000 0.03217 0.04582 = 0.05046 -0.00190 -0.00340 -0.01311 AFIX 43 H1 2 0.624314 0.454357 0.595212 11.00000 -1.20000 AFIX 0 C2 1 0.656613 0.260751 0.618752 11.00000 0.02942 0.06098 = 0.03792 0.00513 -0.00047 -0.00805 C3 1 0.641669 0.121602 0.609502 11.00000 0.04881 0.04999 = 0.05284 0.00752 0.00259 -0.00127 AFIX 43 H3A 2 0.668974 0.052081 0.628038 11.00000 -1.20000 AFIX 0 C4 1 0.586262 0.083138 0.572794 11.00000 0.05462 0.05600 = 0.05989 -0.00310 0.00718 -0.01423 AFIX 43 H4 2 0.574890 -0.011845 0.567121 11.00000 -1.20000 AFIX 0 C5 1 0.548735 0.186229 0.545171 11.00000 0.03716 0.07220 = 0.04328 0.00153 -0.00167 -0.02646 AFIX 43 H5 2 0.511887 0.159232 0.519862 11.00000 -1.20000 AFIX 0 C6 1 0.715746 0.309756 0.659916 11.00000 0.04573 0.06983 = 0.05034 0.01852 -0.01200 -0.01985 AFIX 23 H6A 2 0.701123 0.353756 0.688029 11.00000 -1.20000 H6B 2 0.740315 0.226193 0.674396 11.00000 -1.20000 AFIX 0 PART 1 C7 1 0.772914 0.415626 0.594517 10.50000 0.05725 0.06833 = 0.03753 0.01213 0.00387 -0.02410 AFIX 23 H7A 2 0.769273 0.514160 0.583575 10.50000 -1.20000 H7B 2 0.741970 0.361177 0.568545 10.50000 -1.20000 AFIX 0 PART 2 C7' 1 0.782880 0.335615 0.604565 10.50000 0.05725 0.06833 = 0.03753 0.01213 0.00387 -0.02410 AFIX 23 H7C 2 0.747475 0.311962 0.574710 10.50000 -1.20000 H7D 2 0.804740 0.248271 0.618213 10.50000 -1.20000 AFIX 0 PART 1 C8 1 0.838101 0.364812 0.596905 10.50000 0.04411 0.10195 = 0.06149 -0.03601 0.00425 0.00335 AFIX 13 H8 2 0.842862 0.268640 0.611476 10.50000 -1.20000 AFIX 0 PART 2 C8' 1 0.828229 0.430035 0.587696 10.50000 0.04411 0.10195 = 0.06149 -0.03601 0.00425 0.00335 AFIX 13 H8' 2 0.806180 0.519806 0.575972 10.50000 -1.20000 AFIX 0 PART 0 C9 1 0.844731 0.359025 0.540944 11.00000 0.10162 0.11503 = 0.08362 -0.02650 0.03512 -0.01621 AFIX 33 PART 1 H9A 2 0.887127 0.325960 0.541017 10.50000 -1.50000 H9B 2 0.812999 0.295349 0.520745 10.50000 -1.50000 H9C 2 0.838248 0.452116 0.525769 10.50000 -1.50000 PART 2 AFIX 33 H9D 2 0.874432 0.417597 0.528636 10.50000 -1.50000 H9E 2 0.864124 0.268263 0.551325 10.50000 -1.50000 H9F 2 0.806032 0.346478 0.513418 10.50000 -1.50000 AFIX 0 PART 0 C10 1 0.929885 0.544826 0.616730 11.00000 0.07852 0.17493 = 0.06229 0.00375 0.00259 -0.06317 AFIX 23 H10A 2 0.905876 0.615473 0.592815 11.00000 -1.20000 H10B 2 0.951867 0.485442 0.596756 11.00000 -1.20000 AFIX 0 C11 1 1.027354 0.551401 0.695535 11.00000 0.04186 0.04588 = 0.05770 -0.00087 0.00884 -0.00692 AFIX 43 H11A 2 1.026047 0.452869 0.696672 11.00000 -1.20000 AFIX 0 C12 1 0.980703 0.621440 0.657293 11.00000 0.03827 0.07563 = 0.04236 0.01281 0.01118 -0.00153 C13 1 0.985114 0.764389 0.655437 11.00000 0.04491 0.09834 = 0.06710 0.03328 0.00980 0.02550 AFIX 43 H13 2 0.955267 0.815266 0.630211 11.00000 -1.20000 AFIX 0 C14 1 1.032476 0.833182 0.689919 11.00000 0.08455 0.04420 = 0.09361 0.01366 0.01008 0.02319 AFIX 43 H14A 2 1.035281 0.931548 0.688962 11.00000 -1.20000 AFIX 0 C15 1 1.077115 0.755861 0.726939 11.00000 0.05052 0.04638 = 0.06238 0.00660 0.01384 0.00927 AFIX 43 H15 2 1.110530 0.804178 0.749866 11.00000 -1.20000 AFIX 0 C16 1 0.628925 0.593673 0.473787 11.00000 0.02485 0.04850 = 0.05183 0.01954 0.00023 -0.01060 C17 1 0.692230 0.672863 0.487083 11.00000 0.02384 0.04520 = 0.04935 0.01446 0.00110 -0.01105 C18 1 0.703502 0.774173 0.526340 11.00000 0.02038 0.06149 = 0.06604 0.00337 0.01909 -0.00828 AFIX 43 H18 2 0.672210 0.791703 0.544301 11.00000 -1.20000 AFIX 0 C19 1 0.738516 0.649468 0.460692 11.00000 0.03165 0.06428 = 0.06373 0.00199 0.01066 -0.01313 AFIX 43 H19 2 0.731428 0.582465 0.433985 11.00000 -1.20000 AFIX 0 HKLF 4 REM C2/c REM wR2 = 0.1270, GooF = S = 1.251, Restrained GooF = 1.250 for all data REM R1 = 0.0800 for 4120 Fo > 4sig(Fo) and 0.1114 for all 5889 data REM 337 parameters refined using 4 restraints END WGHT 0.0001 50.9497 REM Highest difference peak 0.952, deepest hole -0.969, 1-sigma level 0.096 Q1 1 0.8593 0.4146 0.7144 11.00000 0.05 0.95 ; _shelx_res_checksum 21853 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' '-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 Cd1 Cd 0.500000 0.500000 0.500000 0.0440(2) Uani 1 2 d S . P . . Cd2 Cd 0.84662(2) 0.50281(8) 0.70737(2) 0.04432(16) Uani 1 1 d . . . . . S1 S 0.86883(9) 0.2062(2) 0.79179(9) 0.0526(5) Uani 1 1 d . . . . . O1 O 0.5916(2) 0.6179(7) 0.5020(2) 0.0632(17) Uani 1 1 d . . . . . O2 O 0.6187(2) 0.5112(8) 0.4355(2) 0.0672(17) Uani 1 1 d . . . . . O3 O 0.8806(3) 0.2920(7) 0.7484(2) 0.0660(17) Uani 1 1 d . . . . . O4 O 0.8220(3) 0.2786(8) 0.8145(3) 0.078(2) Uani 1 1 d . . . . . O5 O 0.8437(3) 0.0686(7) 0.7706(4) 0.105(3) Uani 1 1 d . . . . . O6 O 0.9293(3) 0.1897(8) 0.8305(2) 0.080(2) Uani 1 1 d . . . . . O1W O 0.4925(2) 0.6398(7) 0.5712(2) 0.0606(16) Uani 1 1 d . . . . . H11 H 0.458324 0.612853 0.578200 0.091 Uiso 1 1 d R U . . . H12 H 0.521674 0.624893 0.598650 0.091 Uiso 1 1 d R U . . . O2W O 0.7826(2) 0.5258(6) 0.76459(19) 0.0518(14) Uani 1 1 d . . . . . H21 H 0.789399 0.453880 0.783998 0.078 Uiso 1 1 d R U . . . H22 H 0.743019 0.525870 0.749388 0.078 Uiso 1 1 d R U . . . O3W O 0.7952(3) 0.7118(7) 0.6687(2) 0.0660(17) Uani 1 1 d . . . . . H31 H 0.759495 0.723108 0.675840 0.099 Uiso 1 1 d R U . . . H32 H 0.820305 0.779798 0.679810 0.099 Uiso 1 1 d R U . . . O4W O 0.8375(3) 0.9769(8) 0.6577(3) 0.085(2) Uani 1 1 d . . . . . H41 H 0.859773 1.002192 0.637303 0.128 Uiso 1 1 d R U . . . H42 H 0.850454 1.020482 0.686203 0.128 Uiso 1 1 d R U . . . O5W O 0.9483(3) 1.1771(9) 0.6820(3) 0.118(3) Uani 1 1 d . . . . . H51 H 0.936600 1.221372 0.705623 0.178 Uiso 1 1 d R U . . . H52 H 0.987460 1.194211 0.684713 0.178 Uiso 1 1 d R U . . . N1 N 0.5613(3) 0.3237(7) 0.5520(2) 0.0421(15) Uani 1 1 d . . . . . N2 N 0.7574(3) 0.4032(10) 0.6450(3) 0.074(3) Uani 1 1 d D . . . . H2 H 0.732226 0.478190 0.641520 0.089 Uiso 1 1 calc R U . A 1 N3 N 0.8854(3) 0.4602(8) 0.6327(3) 0.060(2) Uani 1 1 d D . . . . H3 H 0.912791 0.393031 0.646906 0.072 Uiso 1 1 calc R U . B 1 N4 N 1.0742(3) 0.6192(7) 0.7309(2) 0.0389(14) Uani 1 1 d . . . . . C1 C 0.6149(3) 0.3586(9) 0.5891(3) 0.0454(19) Uani 1 1 d . . . . . H1 H 0.624314 0.454357 0.595212 0.054 Uiso 1 1 calc R U . . . C2 C 0.6566(3) 0.2608(9) 0.6188(3) 0.0444(19) Uani 1 1 d . . . . . C3 C 0.6417(4) 0.1216(9) 0.6095(3) 0.052(2) Uani 1 1 d . . . . . H3A H 0.668974 0.052081 0.628038 0.063 Uiso 1 1 calc R U . . . C4 C 0.5863(4) 0.0831(10) 0.5728(3) 0.058(2) Uani 1 1 d . . . . . H4 H 0.574890 -0.011845 0.567121 0.070 Uiso 1 1 calc R U . . . C5 C 0.5487(4) 0.1862(10) 0.5452(3) 0.053(2) Uani 1 1 d . . . . . H5 H 0.511887 0.159232 0.519862 0.064 Uiso 1 1 calc R U . . . C6 C 0.7157(4) 0.3098(10) 0.6599(3) 0.060(2) Uani 1 1 d . . . . . H6A H 0.701123 0.353756 0.688029 0.072 Uiso 1 1 calc R U . . . H6B H 0.740315 0.226193 0.674396 0.072 Uiso 1 1 calc R U . . . C7 C 0.7729(8) 0.416(2) 0.5945(5) 0.056(4) Uani 0.5 1 d D . P C 1 H7A H 0.769273 0.514160 0.583575 0.067 Uiso 0.5 1 calc R U P C 1 H7B H 0.741970 0.361177 0.568545 0.067 Uiso 0.5 1 calc R U P C 1 C7' C 0.7829(9) 0.3356(17) 0.6046(6) 0.056(4) Uani 0.5 1 d D . P C 2 H7C H 0.747475 0.311962 0.574710 0.067 Uiso 0.5 1 calc R U P C 2 H7D H 0.804740 0.248271 0.618213 0.067 Uiso 0.5 1 calc R U P C 2 C8 C 0.8381(7) 0.365(3) 0.5969(5) 0.071(8) Uani 0.5 1 d D . P C 1 H8 H 0.842862 0.268640 0.611476 0.085 Uiso 0.5 1 calc R U P C 1 C8' C 0.8282(6) 0.430(3) 0.5877(5) 0.071(8) Uani 0.5 1 d D . P C 2 H8' H 0.806180 0.519806 0.575972 0.085 Uiso 0.5 1 calc R U P C 2 C9 C 0.8447(5) 0.3590(14) 0.5409(4) 0.098(4) Uani 1 1 d D . . . . H9A H 0.887127 0.325960 0.541017 0.147 Uiso 0.5 1 calc R U P C 1 H9B H 0.812999 0.295349 0.520745 0.147 Uiso 0.5 1 calc R U P C 1 H9C H 0.838248 0.452116 0.525769 0.147 Uiso 0.5 1 calc R U P C 1 H9D H 0.874432 0.417597 0.528636 0.147 Uiso 0.5 1 calc R U P C 2 H9E H 0.864124 0.268263 0.551325 0.147 Uiso 0.5 1 calc R U P C 2 H9F H 0.806032 0.346478 0.513418 0.147 Uiso 0.5 1 calc R U P C 2 C10 C 0.9299(5) 0.5448(15) 0.6167(4) 0.108(5) Uani 1 1 d . . . . . H10A H 0.905876 0.615473 0.592815 0.130 Uiso 1 1 calc R U . . . H10B H 0.951867 0.485442 0.596756 0.130 Uiso 1 1 calc R U . . . C11 C 1.0274(3) 0.5514(9) 0.6955(3) 0.0492(19) Uani 1 1 d . . . . . H11A H 1.026047 0.452869 0.696672 0.059 Uiso 1 1 calc R U . . . C12 C 0.9807(4) 0.6214(11) 0.6573(3) 0.052(2) Uani 1 1 d . . . . . C13 C 0.9851(4) 0.7644(13) 0.6554(4) 0.071(3) Uani 1 1 d . . . . . H13 H 0.955267 0.815266 0.630211 0.085 Uiso 1 1 calc R U . . . C14 C 1.0325(5) 0.8332(11) 0.6899(4) 0.076(3) Uani 1 1 d . . . . . H14A H 1.035281 0.931548 0.688962 0.092 Uiso 1 1 calc R U . . . C15 C 1.0771(4) 0.7559(9) 0.7269(3) 0.053(2) Uani 1 1 d . . . . . H15 H 1.110530 0.804178 0.749866 0.064 Uiso 1 1 calc R U . . . C16 C 0.6289(3) 0.5937(9) 0.4738(3) 0.0435(19) Uani 1 1 d . . . . . C17 C 0.6922(3) 0.6729(8) 0.4871(3) 0.0410(18) Uani 1 1 d . . . . . C18 C 0.7035(3) 0.7742(9) 0.5263(3) 0.048(2) Uani 1 1 d . . . . . H18 H 0.672210 0.791703 0.544301 0.057 Uiso 1 1 calc R U . . . C19 C 0.7385(3) 0.6495(10) 0.4607(3) 0.054(2) Uani 1 1 d . . . . . H19 H 0.731428 0.582465 0.433985 0.064 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 Cd1 0.0230(3) 0.0659(5) 0.0408(4) 0.0068(4) 0.0042(3) -0.0151(4) Cd2 0.0376(3) 0.0471(3) 0.0435(3) -0.0033(3) 0.0018(2) -0.0050(3) S1 0.0336(10) 0.0386(11) 0.0773(14) 0.0127(11) -0.0010(9) -0.0014(9) O1 0.029(3) 0.089(5) 0.074(4) 0.007(4) 0.016(3) -0.019(3) O2 0.046(3) 0.078(4) 0.075(4) -0.009(4) 0.012(3) -0.034(4) O3 0.082(4) 0.055(4) 0.064(4) 0.013(3) 0.023(3) 0.017(3) O4 0.063(4) 0.081(5) 0.099(5) 0.018(4) 0.039(4) 0.009(4) O5 0.053(4) 0.044(4) 0.199(8) -0.005(5) -0.001(5) -0.006(3) O6 0.052(4) 0.099(6) 0.073(4) 0.022(4) -0.011(3) 0.006(4) O1W 0.038(3) 0.087(5) 0.054(3) -0.004(3) 0.007(2) -0.019(3) O2W 0.048(3) 0.049(4) 0.055(3) -0.006(3) 0.007(2) 0.004(3) O3W 0.051(3) 0.061(4) 0.085(4) 0.017(4) 0.015(3) 0.018(3) O4W 0.089(5) 0.078(5) 0.088(5) -0.001(4) 0.022(4) -0.032(4) O5W 0.071(5) 0.118(7) 0.162(8) -0.052(6) 0.021(5) 0.001(5) N1 0.027(3) 0.056(4) 0.039(3) 0.005(3) 0.000(2) -0.013(3) N2 0.046(4) 0.122(8) 0.049(4) -0.010(5) 0.006(3) -0.025(5) N3 0.050(4) 0.067(5) 0.068(4) -0.014(4) 0.021(3) -0.016(4) N4 0.027(3) 0.043(4) 0.046(3) 0.005(3) 0.007(3) 0.002(3) C1 0.032(4) 0.046(5) 0.050(4) -0.002(4) -0.003(3) -0.013(3) C2 0.029(4) 0.061(5) 0.038(4) 0.005(4) 0.000(3) -0.008(4) C3 0.049(5) 0.050(5) 0.053(5) 0.008(4) 0.003(4) -0.001(4) C4 0.055(5) 0.056(6) 0.060(5) -0.003(4) 0.007(4) -0.014(4) C5 0.037(4) 0.072(6) 0.043(4) 0.002(4) -0.002(3) -0.026(4) C6 0.046(4) 0.070(6) 0.050(5) 0.019(4) -0.012(4) -0.020(4) C7 0.057(7) 0.068(12) 0.038(6) 0.012(7) 0.004(6) -0.024(9) C7' 0.057(7) 0.068(12) 0.038(6) 0.012(7) 0.004(6) -0.024(9) C8 0.044(7) 0.10(2) 0.061(8) -0.036(11) 0.004(6) 0.003(10) C8' 0.044(7) 0.10(2) 0.061(8) -0.036(11) 0.004(6) 0.003(10) C9 0.102(9) 0.115(11) 0.084(8) -0.027(8) 0.035(7) -0.016(8) C10 0.079(7) 0.175(15) 0.062(6) 0.004(7) 0.003(5) -0.063(9) C11 0.042(4) 0.046(5) 0.058(5) -0.001(4) 0.009(4) -0.007(4) C12 0.038(4) 0.076(7) 0.042(4) 0.013(4) 0.011(3) -0.002(4) C13 0.045(5) 0.098(9) 0.067(6) 0.033(6) 0.010(4) 0.026(5) C14 0.085(7) 0.044(6) 0.094(7) 0.014(5) 0.010(6) 0.023(5) C15 0.051(5) 0.046(5) 0.062(5) 0.007(4) 0.014(4) 0.009(4) C16 0.025(3) 0.048(5) 0.052(4) 0.020(4) 0.000(3) -0.011(3) C17 0.024(3) 0.045(5) 0.049(4) 0.014(4) 0.001(3) -0.011(3) C18 0.020(3) 0.061(5) 0.066(5) 0.003(4) 0.019(3) -0.008(4) C19 0.032(4) 0.064(6) 0.064(5) 0.002(4) 0.011(4) -0.013(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' 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' Cd Cd -0.8075 1.2024 '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 O1 Cd1 O1 180.00(12) 5_666 . O1 Cd1 N1 91.1(2) 5_666 . O1 Cd1 N1 88.9(2) . . O1 Cd1 N1 88.9(2) 5_666 5_666 O1 Cd1 N1 91.1(2) . 5_666 N1 Cd1 N1 180.0(2) . 5_666 O1 Cd1 O1W 86.6(2) 5_666 5_666 O1 Cd1 O1W 93.4(2) . 5_666 N1 Cd1 O1W 85.8(2) . 5_666 N1 Cd1 O1W 94.2(2) 5_666 5_666 O1 Cd1 O1W 93.4(2) 5_666 . O1 Cd1 O1W 86.6(2) . . N1 Cd1 O1W 94.2(2) . . N1 Cd1 O1W 85.8(2) 5_666 . O1W Cd1 O1W 180.0 5_666 . O3 Cd2 O2W 86.6(2) . . O3 Cd2 N4 89.5(2) . 2_756 O2W Cd2 N4 86.86(19) . 2_756 O3 Cd2 O3W 170.4(2) . . O2W Cd2 O3W 85.10(19) . . N4 Cd2 O3W 94.9(2) 2_756 . O3 Cd2 N3 96.4(2) . . O2W Cd2 N3 164.2(2) . . N4 Cd2 N3 108.6(2) 2_756 . O3W Cd2 N3 90.3(2) . . O3 Cd2 N2 95.0(3) . . O2W Cd2 N2 89.1(2) . . N4 Cd2 N2 173.8(3) 2_756 . O3W Cd2 N2 80.0(3) . . N3 Cd2 N2 75.3(2) . . O6 S1 O5 110.7(4) . . O6 S1 O4 110.3(4) . . O5 S1 O4 110.3(4) . . O6 S1 O3 108.1(4) . . O5 S1 O3 107.9(5) . . O4 S1 O3 109.5(4) . . C16 O1 Cd1 125.9(5) . . S1 O3 Cd2 138.2(4) . . C5 N1 C1 116.3(7) . . C5 N1 Cd1 123.5(5) . . C1 N1 Cd1 120.1(5) . . C6 N2 C7 128.8(10) . . C6 N2 C7' 108.6(10) . . C6 N2 Cd2 121.2(5) . . C7 N2 Cd2 105.7(8) . . C7' N2 Cd2 107.1(8) . . C10 N3 C8 124.0(9) . . C10 N3 C8' 110.6(10) . . C10 N3 Cd2 124.9(7) . . C8 N3 Cd2 107.7(6) . . C8' N3 Cd2 107.7(6) . . C15 N4 C11 117.3(7) . . C15 N4 Cd2 119.3(6) . 2_756 C11 N4 Cd2 123.2(5) . 2_756 N1 C1 C2 123.9(7) . . C3 C2 C1 117.1(7) . . C3 C2 C6 122.6(7) . . C1 C2 C6 120.3(8) . . C2 C3 C4 120.2(8) . . C5 C4 C3 118.6(8) . . N1 C5 C4 123.9(7) . . N2 C6 C2 118.2(7) . . N2 C7 C8 111.9(11) . . N2 C7' C8' 110.9(11) . . C7 C8 N3 108.3(14) . . C7 C8 C9 107.2(12) . . N3 C8 C9 114.8(11) . . C7' C8' N3 110.1(15) . . C7' C8' C9 106.8(13) . . N3 C8' C9 114.5(10) . . N3 C10 C12 119.2(8) . . N4 C11 C12 123.3(8) . . C13 C12 C11 117.1(8) . . C13 C12 C10 119.8(9) . . C11 C12 C10 123.0(10) . . C14 C13 C12 120.2(9) . . C13 C14 C15 119.3(9) . . N4 C15 C14 122.8(9) . . O1 C16 O2 126.3(7) . . O1 C16 C17 116.5(7) . . O2 C16 C17 117.2(7) . . C19 C17 C18 118.8(6) . . C19 C17 C16 121.8(7) . . C18 C17 C16 119.3(7) . . C17 C18 C19 120.8(7) . 7_666 C17 C19 C18 120.4(8) . 7_666 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cd1 O1 2.244(5) 5_666 Cd1 O1 2.244(5) . Cd1 N1 2.334(6) . Cd1 N1 2.334(6) 5_666 Cd1 O1W 2.335(6) 5_666 Cd1 O1W 2.335(6) . Cd2 O3 2.291(6) . Cd2 O2W 2.297(5) . Cd2 N4 2.307(6) 2_756 Cd2 O3W 2.359(6) . Cd2 N3 2.361(6) . Cd2 N2 2.375(7) . S1 O6 1.438(6) . S1 O5 1.461(7) . S1 O4 1.463(6) . S1 O3 1.475(6) . O1 C16 1.246(9) . O2 C16 1.250(9) . N1 C5 1.326(10) . N1 C1 1.347(8) . N2 C6 1.382(10) . N2 C7 1.459(12) . N2 C7' 1.463(12) . N3 C10 1.390(11) . N3 C8 1.496(13) . N3 C8' 1.500(12) . N4 C15 1.296(10) . N4 C11 1.346(9) . C1 C2 1.380(10) . C2 C3 1.358(11) . C2 C6 1.515(9) . C3 C4 1.375(10) . C4 C5 1.350(11) . C7 C8 1.463(17) . C7' C8' 1.469(17) . C8 C9 1.522(14) . C8' C9 1.524(14) . C10 C12 1.503(12) . C11 C12 1.392(10) . C12 C13 1.353(13) . C13 C14 1.344(13) . C14 C15 1.387(11) . C16 C17 1.509(9) . C17 C19 1.368(10) . C17 C18 1.385(11) . C18 C19 1.400(10) 7_666