#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/89/2238915.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2238915 loop_ _publ_author_name 'You, Ming-Hua' 'Li, Fo-Jun' 'Yang, Xiao-Ping' 'Lin, Xu-Xiang' 'Ye, Hua-Yan' _publ_section_title ; Poly[[(\m~2~-4,4'-bipyridyl-\k^2^N:N')bis{\m~2~-N-[2-(2-hydroxybenzoyl)carbamothioyl]acetamidato-\k^4^O,N,O':S}bis(nitrato-\k^2^O,O')dicadmium] dimethylformamide tetrasolvate] ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m647 _journal_page_last m648 _journal_paper_doi 10.1107/S1600536813030055 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac '[Cd2 (C10 H10 N3 O3 S)2 (C10 H8 N2) (N O3)2], 4C3 H7 N O' _chemical_formula_moiety 'C30 H28 Cd2 N10 O12 S2, 4(C3 H7 N O)' _chemical_formula_sum 'C42 H56 Cd2 N14 O16 S2' _chemical_formula_weight 1301.93 _chemical_name_systematic 'Poly[[(\m~2~-4,4'-bipyridyl-\k^2^N:N')bis{\m~2~-N-[2-(2-hydroxybenzoyl)carbamothioyl]acetamidato-\k^4^O,N,O':S}bis(nitrato-\k^2^O,O')dicadmium] dimethylformamide tetrasolvate]' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 110.55(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 13.831(3) _cell_length_b 15.280(3) _cell_length_c 14.363(3) _cell_measurement_reflns_used 10007 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.5126 _cell_measurement_theta_min 3.0294 _cell_volume 2842.3(12) _computing_cell_refinement 'CrystalClear (Rigaku, 2007)' _computing_data_collection 'CrystalClear (Rigaku, 2007)' _computing_data_reduction 'CrystalClear (Rigaku, 2007)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Rigaku Saturn 724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 18197 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 3.03 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2007)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1324 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.697 _refine_diff_density_min -0.626 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 349 _refine_ls_number_reflns 4980 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.276 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0599 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+4.0842P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1388 _refine_ls_wR_factor_ref 0.1410 _reflns_number_gt 4753 _reflns_number_total 4980 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL I in P2(1)/n CELL 0.71073 13.8312 15.2805 14.3626 90.000 110.549 90.000 ZERR 2.0000 0.0028 0.0031 0.0029 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O S CD UNIT 84 112 28 32 4 4 MERG 2 FMAP 2 GRID ACTA PLAN 20 TEMP 20 BOND $H EQIV $1 -x+2, -y, -z+1 EQIV $2 x+1/2, -y+1/2, z+1/2 HTAB N1 O7_$1 HTAB N3 O6 HTAB N3 S1 HTAB O6 O8_$2 OMIT -4 6 8 OMIT -3 5 6 OMIT 1 2 0 OMIT -3 50 MPLA 3 CD1 O1 O2 N2 O4 O3 MPLA 17 C1 C2 O1 N1 C3 S1 N2 N3 C4 O2 C5 C6 O6 C7 C8 C9 C10 L.S. 10 WGHT 0.047400 4.084200 FVAR 0.25040 CD1 6 0.930790 0.136190 0.356878 11.00000 0.03986 0.05414 = 0.05504 -0.00090 0.01226 0.00047 N4 3 0.960714 0.286310 0.395254 11.00000 0.04997 0.04897 = 0.07435 -0.00063 0.01227 -0.00069 O2 4 0.812916 0.154070 0.439987 11.00000 0.04404 0.07608 = 0.06300 0.00329 0.01585 0.00820 C4 1 0.842019 0.133875 0.529403 11.00000 0.03756 0.05092 = 0.06475 -0.01130 0.01449 -0.00124 N2 3 1.012033 0.105090 0.532892 11.00000 0.03563 0.04849 = 0.06190 -0.00345 0.01877 -0.00302 C6 1 0.798399 0.132418 0.689918 11.00000 0.05364 0.08560 = 0.08039 -0.01042 0.03399 -0.00044 O4 4 0.780987 0.191057 0.206535 11.00000 0.05703 0.10663 = 0.08285 0.00424 0.02379 -0.00372 C5 1 0.770516 0.140937 0.586960 11.00000 0.04866 0.06783 = 0.07616 -0.01245 0.02606 -0.00261 O6 4 0.898377 0.112641 0.744102 11.00000 0.05703 0.14500 = 0.07036 0.00971 0.02666 0.01265 AFIX 147 H6 2 0.904338 0.104928 0.802361 11.00000 -1.20000 AFIX 0 O5 4 0.803099 0.218013 0.067286 11.00000 0.08229 0.18096 = 0.07319 0.04683 0.00673 0.01248 N5 3 0.836068 0.195465 0.154964 11.00000 0.06437 0.08617 = 0.06446 0.01033 0.01141 0.00012 O3 4 0.930662 0.175173 0.195898 11.00000 0.05378 0.12578 = 0.06750 0.01611 0.01637 0.01334 C7 1 0.724004 0.142531 0.735418 11.00000 0.08169 0.13758 = 0.08871 -0.00622 0.05206 0.00827 AFIX 43 H7 2 0.743490 0.137536 0.804100 11.00000 -1.20000 AFIX 0 C10 1 0.667115 0.158278 0.531900 11.00000 0.04743 0.14692 = 0.09051 -0.01630 0.02604 0.00767 AFIX 43 H10 2 0.646458 0.164126 0.463216 11.00000 -1.20000 AFIX 0 C8 1 0.623792 0.159563 0.679622 11.00000 0.07381 0.21662 = 0.11821 -0.00820 0.06194 0.01437 AFIX 43 H8 2 0.574966 0.166226 0.710065 11.00000 -1.20000 AFIX 0 C9 1 0.594863 0.166912 0.577725 11.00000 0.04862 0.22840 = 0.11973 -0.01887 0.03416 0.02464 AFIX 43 H9 2 0.526181 0.177765 0.539548 11.00000 -1.20000 AFIX 0 O1 4 1.107455 0.122242 0.388819 11.00000 0.04311 0.08060 = 0.05863 0.00516 0.01477 0.00573 N1 3 1.181868 0.072459 0.548886 11.00000 0.03285 0.05620 = 0.06449 0.00055 0.01451 0.00508 AFIX 43 H1 2 1.240187 0.054093 0.589529 11.00000 -1.20000 AFIX 0 N3 3 0.938582 0.105632 0.579173 11.00000 0.04177 0.05816 = 0.05388 -0.00210 0.01784 0.00557 AFIX 43 H3 2 0.955063 0.087888 0.639590 11.00000 -1.20000 AFIX 0 C3 1 1.100660 0.071074 0.587056 11.00000 0.03839 0.04082 = 0.05817 -0.00902 0.01255 -0.00133 C13 1 0.992029 0.455870 0.477685 11.00000 0.04174 0.05074 = 0.06330 0.00221 0.01077 -0.00133 C2 1 1.183351 0.097808 0.459174 11.00000 0.04053 0.05211 = 0.06831 -0.00744 0.01719 -0.00456 N6 3 0.532114 0.112188 0.256738 11.00000 0.05637 0.10787 = 0.11010 0.02655 0.03170 0.02662 C15 1 0.883656 0.344128 0.375981 11.00000 0.04947 0.06144 = 0.08576 -0.00995 0.00191 0.00280 AFIX 43 H15 2 0.818196 0.327165 0.334289 11.00000 -1.20000 AFIX 0 C14 1 0.896200 0.427278 0.414584 11.00000 0.04786 0.05461 = 0.08633 -0.00367 0.00658 0.00571 AFIX 43 H14 2 0.839822 0.464885 0.398261 11.00000 -1.20000 AFIX 0 C16 1 0.613041 0.060084 0.286032 11.00000 0.03890 0.10224 = 0.06856 -0.00470 0.01230 0.00383 AFIX 43 H16 2 0.671874 0.079002 0.274722 11.00000 -1.20000 AFIX 0 C11 1 1.053868 0.313568 0.453265 11.00000 0.05127 0.05957 = 0.13338 -0.02434 0.00301 0.00717 AFIX 43 H11 2 1.109316 0.275219 0.466685 11.00000 -1.20000 AFIX 0 C12 1 1.071637 0.396552 0.494420 11.00000 0.04186 0.06374 = 0.14399 -0.03102 -0.00243 -0.00239 AFIX 43 H12 2 1.138274 0.412609 0.533982 11.00000 -1.20000 AFIX 0 C17 1 0.535283 0.197935 0.213710 11.00000 0.12638 0.11195 = 0.14962 0.02753 0.06122 0.04155 AFIX 137 H17A 2 0.602923 0.207974 0.211408 11.00000 -1.50000 H17B 2 0.519797 0.242208 0.253797 11.00000 -1.50000 H17C 2 0.485217 0.200164 0.147554 11.00000 -1.50000 AFIX 0 C18 1 0.439789 0.085953 0.272869 11.00000 0.06574 0.26196 = 0.35054 0.14838 0.10320 0.05510 AFIX 137 H18A 2 0.457509 0.050446 0.331634 11.00000 -1.50000 H18B 2 0.396963 0.052892 0.216690 11.00000 -1.50000 H18C 2 0.403034 0.136942 0.281093 11.00000 -1.50000 AFIX 0 O7 4 0.617992 -0.011450 0.327061 11.00000 0.05594 0.10227 = 0.09576 0.02161 0.01856 0.01414 C1 1 1.287966 0.095649 0.448385 11.00000 0.04177 0.08695 = 0.08120 0.00040 0.02768 -0.00007 AFIX 137 H1A 2 1.285716 0.057200 0.394803 11.00000 -1.50000 H1B 2 1.338526 0.074847 0.509056 11.00000 -1.50000 H1C 2 1.306224 0.153526 0.434432 11.00000 -1.50000 AFIX 0 S1 5 1.129072 0.023540 0.704115 11.00000 0.04638 0.06016 = 0.05161 -0.00564 0.00982 0.00134 N7 3 0.591972 0.399589 0.541863 11.00000 0.10481 0.30590 = 0.09755 0.00808 0.04286 -0.05197 C20 1 0.642503 0.410948 0.469009 11.00000 0.19156 0.40186 = 0.21015 0.00069 0.13953 -0.07022 AFIX 137 H20A 2 0.598120 0.389608 0.405525 11.00000 -1.50000 H20B 2 0.706179 0.378793 0.489872 11.00000 -1.50000 H20C 2 0.656471 0.471919 0.463673 11.00000 -1.50000 AFIX 0 C21 1 0.653116 0.399676 0.649105 11.00000 0.09366 0.27865 = 0.11497 -0.01778 0.01211 -0.04013 AFIX 137 H21A 2 0.607848 0.392781 0.686221 11.00000 -1.50000 H21B 2 0.689671 0.454097 0.666822 11.00000 -1.50000 H21C 2 0.701645 0.352205 0.664108 11.00000 -1.50000 AFIX 0 O8 4 0.433337 0.383054 0.427175 11.00000 0.18198 0.72392 = 0.07089 0.05611 0.01462 -0.17660 C19 1 0.493118 0.383545 0.512472 11.00000 0.11870 0.51221 = 0.07046 0.03143 0.02807 -0.08726 AFIX 43 H19 2 0.465793 0.371289 0.561679 11.00000 -1.20000 HKLF 4 REM I in P2(1)/n REM R1 = 0.0599 for 4753 Fo > 4sig(Fo) and 0.0637 for all 4980 data REM 349 parameters refined using 0 restraints END WGHT 0.0475 4.0830 REM Highest difference peak 0.697, deepest hole -0.626, 1-sigma level 0.072 Q1 1 0.9552 0.1721 0.4128 11.00000 0.05 0.70 Q2 1 0.7112 0.3606 0.4351 11.00000 0.05 0.69 Q3 1 0.9237 0.1662 0.2977 11.00000 0.05 0.59 Q4 1 0.5712 0.0893 0.1433 11.00000 0.05 0.59 Q5 1 1.1218 0.0068 0.7651 11.00000 0.05 0.33 Q6 1 0.6390 0.2491 0.2147 11.00000 0.05 0.31 Q7 1 0.4426 0.4360 0.4312 11.00000 0.05 0.31 Q8 1 0.7682 0.5176 0.4882 11.00000 0.05 0.30 Q9 1 0.8691 0.2976 0.2957 11.00000 0.05 0.29 Q10 1 1.1013 0.0763 0.6451 11.00000 0.05 0.28 Q11 1 1.0097 0.1583 0.5223 11.00000 0.05 0.26 Q12 1 0.5059 0.3540 0.3781 11.00000 0.05 0.26 Q13 1 1.0992 -0.0333 0.6561 11.00000 0.05 0.26 Q14 1 0.7803 0.1671 0.6297 11.00000 0.05 0.25 Q15 1 1.0422 0.0484 0.7563 11.00000 0.05 0.23 Q16 1 0.7981 0.3548 0.2572 11.00000 0.05 0.23 Q17 1 1.1434 0.1141 0.7323 11.00000 0.05 0.23 Q18 1 0.9065 0.3123 0.4171 11.00000 0.05 0.23 Q19 1 1.1778 -0.0180 0.7342 11.00000 0.05 0.21 Q20 1 1.1237 0.1522 0.4330 11.00000 0.05 0.21 ; _cod_data_source_file rz5087.cif _cod_data_source_block I _cod_original_cell_volume 2842.4(12) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2238915 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity Cd Cd1 0.93079(3) 0.13619(3) 0.35688(3) 0.05085(16) Uani d . 1 1 N N4 0.9607(3) 0.2863(3) 0.3953(4) 0.0603(11) Uani d . 1 1 O O2 0.8129(3) 0.1541(3) 0.4400(3) 0.0618(10) Uani d . 1 1 C C4 0.8420(4) 0.1339(3) 0.5294(4) 0.0520(12) Uani d . 1 1 N N2 1.0120(3) 0.1051(3) 0.5329(3) 0.0482(10) Uani d . 1 1 C C6 0.7984(5) 0.1324(4) 0.6899(5) 0.0704(17) Uani d . 1 1 O O4 0.7810(3) 0.1911(3) 0.2065(3) 0.0824(13) Uani d . 1 1 C C5 0.7705(4) 0.1409(4) 0.5870(5) 0.0631(15) Uani d . 1 1 O O6 0.8984(3) 0.1126(4) 0.7441(3) 0.0897(15) Uani d . 1 1 H H6 0.9043 0.1049 0.8024 0.108 Uiso calc R 1 1 O O5 0.8031(4) 0.2180(5) 0.0673(4) 0.118(2) Uani d . 1 1 N N5 0.8361(4) 0.1955(4) 0.1550(4) 0.0747(14) Uani d . 1 1 O O3 0.9307(3) 0.1752(4) 0.1959(3) 0.0837(13) Uani d . 1 1 C C7 0.7240(6) 0.1425(6) 0.7354(6) 0.097(2) Uani d . 1 1 H H7 0.7435 0.1375 0.8041 0.116 Uiso calc R 1 1 C C10 0.6671(5) 0.1583(6) 0.5319(6) 0.094(2) Uani d . 1 1 H H10 0.6465 0.1641 0.4632 0.113 Uiso calc R 1 1 C C8 0.6238(7) 0.1596(8) 0.6796(8) 0.129(4) Uani d . 1 1 H H8 0.5750 0.1662 0.7101 0.154 Uiso calc R 1 1 C C9 0.5949(6) 0.1669(8) 0.5777(8) 0.131(4) Uani d . 1 1 H H9 0.5262 0.1778 0.5395 0.157 Uiso calc R 1 1 O O1 1.1075(3) 0.1222(3) 0.3888(3) 0.0616(10) Uani d . 1 1 N N1 1.1819(3) 0.0725(3) 0.5489(3) 0.0519(10) Uani d . 1 1 H H1 1.2402 0.0541 0.5895 0.062 Uiso calc R 1 1 N N3 0.9386(3) 0.1056(3) 0.5792(3) 0.0510(10) Uani d . 1 1 H H3 0.9551 0.0879 0.6396 0.061 Uiso calc R 1 1 C C3 1.1007(4) 0.0711(3) 0.5871(4) 0.0470(11) Uani d . 1 1 C C13 0.9920(4) 0.4559(3) 0.4777(4) 0.0540(12) Uani d . 1 1 C C2 1.1834(4) 0.0978(4) 0.4592(4) 0.0542(13) Uani d . 1 1 N N6 0.5321(4) 0.1122(4) 0.2567(5) 0.0908(18) Uani d . 1 1 C C15 0.8837(5) 0.3441(4) 0.3760(5) 0.0714(17) Uani d . 1 1 H H15 0.8182 0.3272 0.3343 0.086 Uiso calc R 1 1 C C14 0.8962(4) 0.4273(4) 0.4146(5) 0.0675(16) Uani d . 1 1 H H14 0.8398 0.4649 0.3983 0.081 Uiso calc R 1 1 C C16 0.6130(4) 0.0601(5) 0.2860(5) 0.0717(17) Uani d . 1 1 H H16 0.6719 0.0790 0.2747 0.086 Uiso calc R 1 1 C C11 1.0539(5) 0.3136(4) 0.4533(6) 0.089(2) Uani d . 1 1 H H11 1.1093 0.2752 0.4667 0.107 Uiso calc R 1 1 C C12 1.0716(5) 0.3966(4) 0.4944(6) 0.093(2) Uani d . 1 1 H H12 1.1383 0.4126 0.5340 0.111 Uiso calc R 1 1 C C17 0.5353(8) 0.1979(6) 0.2137(8) 0.126(3) Uani d . 1 1 H H17A 0.6029 0.2080 0.2114 0.189 Uiso calc R 1 1 H H17B 0.5198 0.2422 0.2538 0.189 Uiso calc R 1 1 H H17C 0.4852 0.2002 0.1476 0.189 Uiso calc R 1 1 C C18 0.4398(7) 0.0860(10) 0.2729(12) 0.218(8) Uani d . 1 1 H H18A 0.4575 0.0504 0.3316 0.327 Uiso calc R 1 1 H H18B 0.3970 0.0529 0.2167 0.327 Uiso calc R 1 1 H H18C 0.4030 0.1369 0.2811 0.327 Uiso calc R 1 1 O O7 0.6180(3) -0.0114(4) 0.3271(4) 0.0868(14) Uani d . 1 1 C C1 1.2880(4) 0.0956(5) 0.4484(5) 0.0683(16) Uani d . 1 1 H H1A 1.2857 0.0572 0.3948 0.103 Uiso calc R 1 1 H H1B 1.3385 0.0748 0.5091 0.103 Uiso calc R 1 1 H H1C 1.3062 0.1535 0.4344 0.103 Uiso calc R 1 1 S S1 1.12907(10) 0.02354(9) 0.70412(10) 0.0547(3) Uani d . 1 1 N N7 0.5920(7) 0.3996(9) 0.5419(6) 0.167(4) Uani d . 1 1 C C20 0.6425(12) 0.4109(13) 0.4690(11) 0.249(9) Uani d . 1 1 H H20A 0.5981 0.3896 0.4055 0.374 Uiso calc R 1 1 H H20B 0.7062 0.3788 0.4899 0.374 Uiso calc R 1 1 H H20C 0.6565 0.4719 0.4637 0.374 Uiso calc R 1 1 C C21 0.6531(8) 0.3997(10) 0.6491(8) 0.169(5) Uani d . 1 1 H H21A 0.6078 0.3928 0.6862 0.253 Uiso calc R 1 1 H H21B 0.6897 0.4541 0.6668 0.253 Uiso calc R 1 1 H H21C 0.7016 0.3522 0.6641 0.253 Uiso calc R 1 1 O O8 0.4333(8) 0.3831(12) 0.4272(6) 0.334(11) Uani d . 1 1 C C19 0.4931(10) 0.3835(13) 0.5125(8) 0.235(10) Uani d . 1 1 H H19 0.4658 0.3713 0.5617 0.282 Uiso calc R 1 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 0.0399(2) 0.0541(3) 0.0550(3) 0.00047(16) 0.01226(17) -0.00090(17) N4 0.050(3) 0.049(3) 0.074(3) -0.001(2) 0.012(2) -0.001(2) O2 0.044(2) 0.076(3) 0.063(2) 0.0082(18) 0.0158(18) 0.003(2) C4 0.038(3) 0.051(3) 0.065(3) -0.001(2) 0.014(2) -0.011(3) N2 0.036(2) 0.048(2) 0.062(3) -0.0030(18) 0.0188(19) -0.003(2) C6 0.054(3) 0.086(4) 0.080(4) 0.000(3) 0.034(3) -0.010(3) O4 0.057(2) 0.107(4) 0.083(3) -0.004(2) 0.024(2) 0.004(3) C5 0.049(3) 0.068(4) 0.076(4) -0.003(3) 0.026(3) -0.012(3) O6 0.057(3) 0.145(5) 0.070(3) 0.013(3) 0.027(2) 0.010(3) O5 0.082(3) 0.181(6) 0.073(3) 0.012(4) 0.007(3) 0.047(4) N5 0.064(3) 0.086(4) 0.064(3) 0.000(3) 0.011(3) 0.010(3) O3 0.054(3) 0.126(4) 0.068(3) 0.013(3) 0.016(2) 0.016(3) C7 0.082(5) 0.138(7) 0.089(5) 0.008(5) 0.052(4) -0.006(5) C10 0.047(4) 0.147(7) 0.091(5) 0.008(4) 0.026(3) -0.016(5) C8 0.074(6) 0.217(12) 0.118(7) 0.014(6) 0.062(5) -0.008(7) C9 0.049(4) 0.228(12) 0.120(7) 0.025(6) 0.034(4) -0.019(8) O1 0.043(2) 0.081(3) 0.059(2) 0.0057(18) 0.0148(18) 0.0052(19) N1 0.033(2) 0.056(3) 0.064(3) 0.0051(18) 0.0145(19) 0.001(2) N3 0.042(2) 0.058(3) 0.054(2) 0.0056(19) 0.0178(19) -0.002(2) C3 0.038(2) 0.041(3) 0.058(3) -0.001(2) 0.013(2) -0.009(2) C13 0.042(3) 0.051(3) 0.063(3) -0.001(2) 0.011(2) 0.002(2) C2 0.041(3) 0.052(3) 0.068(3) -0.005(2) 0.017(3) -0.007(3) N6 0.056(3) 0.108(5) 0.110(5) 0.027(3) 0.032(3) 0.027(4) C15 0.049(3) 0.061(4) 0.086(4) 0.003(3) 0.002(3) -0.010(3) C14 0.048(3) 0.055(3) 0.086(4) 0.006(3) 0.007(3) -0.004(3) C16 0.039(3) 0.102(5) 0.069(4) 0.004(3) 0.012(3) -0.005(4) C11 0.051(4) 0.060(4) 0.133(6) 0.007(3) 0.003(4) -0.024(4) C12 0.042(3) 0.064(4) 0.144(7) -0.002(3) -0.002(4) -0.031(4) C17 0.126(8) 0.112(7) 0.150(9) 0.042(6) 0.061(7) 0.028(7) C18 0.066(6) 0.262(16) 0.35(2) 0.055(8) 0.103(9) 0.148(15) O7 0.056(3) 0.102(4) 0.096(3) 0.014(2) 0.019(2) 0.022(3) C1 0.042(3) 0.087(4) 0.081(4) 0.000(3) 0.028(3) 0.000(3) S1 0.0464(7) 0.0602(8) 0.0516(7) 0.0013(6) 0.0098(6) -0.0056(6) N7 0.105(6) 0.306(14) 0.098(6) -0.052(8) 0.043(5) 0.008(7) C20 0.192(15) 0.40(3) 0.210(15) -0.070(17) 0.140(13) 0.001(17) C21 0.094(7) 0.279(16) 0.115(8) -0.040(9) 0.012(6) -0.018(9) O8 0.182(9) 0.72(3) 0.071(5) -0.177(13) 0.015(5) 0.056(9) C19 0.119(9) 0.51(3) 0.070(6) -0.087(13) 0.028(6) 0.031(11) 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_site_symmetry_3 _geom_angle O1 Cd1 O2 . 140.93(13) O1 Cd1 N4 . 87.55(15) O2 Cd1 N4 . 82.21(15) O1 Cd1 O3 . 81.83(14) O2 Cd1 O3 . 134.28(14) N4 Cd1 O3 . 85.65(18) O1 Cd1 N2 . 72.96(13) O2 Cd1 N2 . 69.13(13) N4 Cd1 N2 . 88.16(15) O3 Cd1 N2 . 154.27(14) O1 Cd1 O4 . 132.81(14) O2 Cd1 O4 . 83.67(14) N4 Cd1 O4 . 84.38(16) O3 Cd1 O4 . 51.27(14) N2 Cd1 O4 . 152.53(14) O1 Cd1 S1 3_756 99.58(10) O2 Cd1 S1 3_756 94.80(10) N4 Cd1 S1 3_756 171.58(11) O3 Cd1 S1 3_756 90.91(14) N2 Cd1 S1 3_756 98.16(10) O4 Cd1 S1 3_756 87.47(12) C11 N4 C15 . 116.7(5) C11 N4 Cd1 . 120.1(4) C15 N4 Cd1 . 122.1(4) C4 O2 Cd1 . 117.7(3) O2 C4 N3 . 122.0(5) O2 C4 C5 . 121.0(5) N3 C4 C5 . 117.0(5) C3 N2 N3 . 114.0(4) C3 N2 Cd1 . 133.8(3) N3 N2 Cd1 . 110.3(3) O6 C6 C5 . 118.2(5) O6 C6 C7 . 121.3(7) C5 C6 C7 . 120.4(6) N5 O4 Cd1 . 92.1(3) C10 C5 C6 . 117.7(6) C10 C5 C4 . 116.4(6) C6 C5 C4 . 125.9(5) C6 O6 H6 . 109.5 O5 N5 O4 . 123.0(6) O5 N5 O3 . 119.6(6) O4 N5 O3 . 117.4(5) N5 O3 Cd1 . 99.2(3) C8 C7 C6 . 120.5(8) C8 C7 H7 . 119.8 C6 C7 H7 . 119.8 C9 C10 C5 . 121.1(8) C9 C10 H10 . 119.4 C5 C10 H10 . 119.4 C7 C8 C9 . 119.8(7) C7 C8 H8 . 120.1 C9 C8 H8 . 120.1 C8 C9 C10 . 120.6(8) C8 C9 H9 . 119.7 C10 C9 H9 . 119.7 C2 O1 Cd1 . 136.2(4) C2 N1 C3 . 130.9(4) C2 N1 H1 . 114.6 C3 N1 H1 . 114.6 C4 N3 N2 . 120.1(4) C4 N3 H3 . 119.9 N2 N3 H3 . 119.9 N2 C3 N1 . 118.1(5) N2 C3 S1 . 125.9(4) N1 C3 S1 . 116.1(3) C12 C13 C14 . 115.3(5) C12 C13 C13 3_766 122.4(6) C14 C13 C13 3_766 122.3(6) O1 C2 N1 . 125.1(5) O1 C2 C1 . 119.6(5) N1 C2 C1 . 115.3(5) C16 N6 C18 . 119.0(8) C16 N6 C17 . 122.1(7) C18 N6 C17 . 118.8(7) N4 C15 C14 . 123.3(5) N4 C15 H15 . 118.3 C14 C15 H15 . 118.3 C15 C14 C13 . 120.8(5) C15 C14 H14 . 119.6 C13 C14 H14 . 119.6 O7 C16 N6 . 126.0(6) O7 C16 H16 . 117.0 N6 C16 H16 . 117.0 N4 C11 C12 . 122.8(6) N4 C11 H11 . 118.6 C12 C11 H11 . 118.6 C13 C12 C11 . 121.1(5) C13 C12 H12 . 119.5 C11 C12 H12 . 119.5 N6 C17 H17A . 109.5 N6 C17 H17B . 109.5 H17A C17 H17B . 109.5 N6 C17 H17C . 109.5 H17A C17 H17C . 109.5 H17B C17 H17C . 109.5 N6 C18 H18A . 109.5 N6 C18 H18B . 109.5 H18A C18 H18B . 109.5 N6 C18 H18C . 109.5 H18A C18 H18C . 109.5 H18B C18 H18C . 109.5 C2 C1 H1A . 109.5 C2 C1 H1B . 109.5 H1A C1 H1B . 109.5 C2 C1 H1C . 109.5 H1A C1 H1C . 109.5 H1B C1 H1C . 109.5 C3 S1 Cd1 3_756 97.32(16) C19 N7 C20 . 120.1(10) C19 N7 C21 . 119.3(9) C20 N7 C21 . 120.4(10) N7 C20 H20A . 109.5 N7 C20 H20B . 109.5 H20A C20 H20B . 109.5 N7 C20 H20C . 109.5 H20A C20 H20C . 109.5 H20B C20 H20C . 109.5 N7 C21 H21A . 109.5 N7 C21 H21B . 109.5 H21A C21 H21B . 109.5 N7 C21 H21C . 109.5 H21A C21 H21C . 109.5 H21B C21 H21C . 109.5 O8 C19 N7 . 126.4(11) O8 C19 H19 . 116.8 N7 C19 H19 . 116.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Cd1 O1 . 2.332(4) Cd1 O2 . 2.350(4) Cd1 N4 . 2.362(5) Cd1 O3 . 2.387(4) Cd1 N2 . 2.426(4) Cd1 O4 . 2.553(5) Cd1 S1 3_756 2.6270(15) N4 C11 . 1.332(7) N4 C15 . 1.336(7) O2 C4 . 1.242(7) C4 N3 . 1.346(6) C4 C5 . 1.499(8) N2 C3 . 1.307(6) N2 N3 . 1.396(5) C6 O6 . 1.361(8) C6 C5 . 1.397(9) C6 C7 . 1.408(9) O4 N5 . 1.237(6) C5 C10 . 1.395(9) O6 H6 . 0.8200 O5 N5 . 1.229(7) N5 O3 . 1.270(6) C7 C8 . 1.361(12) C7 H7 . 0.9300 C10 C9 . 1.382(10) C10 H10 . 0.9300 C8 C9 . 1.380(12) C8 H8 . 0.9300 C9 H9 . 0.9300 O1 C2 . 1.232(6) N1 C2 . 1.352(7) N1 C3 . 1.412(6) N1 H1 . 0.8600 N3 H3 . 0.8600 C3 S1 . 1.745(5) C13 C12 . 1.381(8) C13 C14 . 1.388(7) C13 C13 3_766 1.476(10) C2 C1 . 1.509(7) N6 C16 . 1.317(8) N6 C18 . 1.433(10) N6 C17 . 1.456(10) C15 C14 . 1.373(8) C15 H15 . 0.9300 C14 H14 . 0.9300 C16 O7 . 1.232(8) C16 H16 . 0.9300 C11 C12 . 1.384(9) C11 H11 . 0.9300 C12 H12 . 0.9300 C17 H17A . 0.9600 C17 H17B . 0.9600 C17 H17C . 0.9600 C18 H18A . 0.9600 C18 H18B . 0.9600 C18 H18C . 0.9600 C1 H1A . 0.9600 C1 H1B . 0.9600 C1 H1C . 0.9600 S1 Cd1 3_756 2.6270(15) N7 C19 . 1.305(14) N7 C20 . 1.458(13) N7 C21 . 1.474(12) C20 H20A . 0.9600 C20 H20B . 0.9600 C20 H20C . 0.9600 C21 H21A . 0.9600 C21 H21B . 0.9600 C21 H21C . 0.9600 O8 C19 . 1.214(13) C19 H19 . 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 O7 3_756 0.86 2.01 2.871(6) 174.1 y N3 H3 O6 . 0.86 1.96 2.619(6) 132.6 y N3 H3 S1 . 0.86 2.46 2.901(4) 112.6 n O6 H6 O8 4_666 0.82 1.70 2.502(9) 163.8 y