# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email JOHN.RIPMEESTER@NRC-CNRC.GC.CA _publ_contact_author_name 'Dr John Ripmeester' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; National Research Council Canada Steacie Institute for Molecular Sciences 100 Sussex Drive Ottawa Ontario K1A0R6 CANADA ; _publ_section_title ; Novel hybrid hetero-sandwich architectures via stoichiometric control of host-guest self-organization ; loop_ _publ_author_name 'John Ripmeester' 'H. Jurgen Meyer' 'Long-Li Lai' 'Markus Strobele' 'Jianqin Tao' 'Kostantin A. Udachin' ; X.-Z.You ; 'Zhi Yu' 'Kui Yu' 'Haoguo Zhu' data_yu1 _database_code_depnum_ccdc_archive 'CCDC 201155' _chemical_name_common "N,N'-dimethyl-4,4'-bipyridinium and cadmium-thiocyanate" _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H46 Cd7 N26 O2 S20' _chemical_formula_weight 2543.19 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' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4079(8) _cell_length_b 12.7469(10) _cell_length_c 15.7543(10) _cell_angle_alpha 86.738(10) _cell_angle_beta 71.983(9) _cell_angle_gamma 84.506(9) _cell_volume 2167.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 473(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 2.221 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 473(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37635 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.87 _reflns_number_total 9523 _reflns_number_gt 7993 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.1564P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9523 _refine_ls_number_parameters 563 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S14 S 0.59775(18) 0.41879(12) 0.42565(9) 0.0381(4) Uani 0.70 1 d PD A 1 C14 C 0.7110(4) 0.3217(4) 0.4067(3) 0.0322(9) Uani 0.70 1 d PD A 1 N14 N 0.7880(4) 0.2578(3) 0.4041(3) 0.0285(10) Uani 0.70 1 d PD A 1 S14A S 0.7581(4) 0.2415(3) 0.3987(2) 0.0381(4) Uani 0.30 1 d PD . 2 C14A C 0.6691(11) 0.3517(8) 0.4093(8) 0.0322(9) Uani 0.30 1 d PD B 2 N14A N 0.6143(13) 0.4357(8) 0.4120(9) 0.0285(10) Uani 0.30 1 d PD B 2 Cd1 Cd 0.61135(2) 0.544543(15) 0.275281(13) 0.02966(6) Uani 1 1 d . B 2 Cd2 Cd 1.10372(2) 0.318409(16) 0.143607(13) 0.03161(6) Uani 1 1 d . . 2 Cd3 Cd 1.5000 0.0000 0.0000 0.03366(8) Uani 1 2 d S . 2 Cd4 Cd 0.23040(2) 0.869033(16) 0.456809(15) 0.03541(6) Uani 1 1 d . . 2 S11 S 0.36752(7) 0.52829(5) 0.29655(5) 0.03230(15) Uani 1 1 d . B 2 S12 S 0.64564(7) 0.36780(6) 0.17973(5) 0.03471(16) Uani 1 1 d . B 2 S13 S 0.60922(8) 0.68240(6) 0.13931(5) 0.03868(17) Uani 1 1 d . B 2 S21 S 1.06673(7) 0.49572(5) 0.23649(5) 0.03311(15) Uani 1 1 d . B 2 S22 S 1.32482(8) 0.31279(6) 0.17593(5) 0.03798(17) Uani 1 1 d . C 2 S31 S 1.72630(8) 0.02123(6) 0.01473(5) 0.03819(17) Uani 1 1 d . D 2 S41 S 0.22469(8) 1.01076(6) 0.31539(5) 0.03980(18) Uani 1 1 d . . 2 S42 S 0.18923(9) 1.03931(7) 0.56182(5) 0.04280(19) Uani 1 1 d . E 2 S43 S 0.46907(9) 0.89000(6) 0.43373(6) 0.04349(19) Uani 1 1 d . B 2 O24 O 1.0312(2) 0.20785(18) 0.27631(15) 0.0449(5) Uani 1 1 d . F 2 H23B H 0.9485 0.1938 0.2974 0.054 Uiso 1 1 calc R F 2 H23A H 1.0861 0.1795 0.3062 0.054 Uiso 1 1 calc R F 2 N11 N 0.2666(3) 0.7202(2) 0.3773(2) 0.0490(7) Uani 1 1 d . B 2 N12 N 0.9014(3) 0.3246(2) 0.14779(17) 0.0414(6) Uani 1 1 d . B 2 N13 N 0.8163(3) 0.6071(2) 0.00082(18) 0.0513(8) Uani 1 1 d . . 2 N21 N 0.8196(3) 0.5558(2) 0.2508(2) 0.0418(6) Uani 1 1 d . B 2 N22 N 1.4609(3) 0.1707(2) 0.04416(19) 0.0435(6) Uani 1 1 d . C 2 N41 N 0.4162(3) 0.9575(2) 0.15882(17) 0.0466(7) Uani 1 1 d . . 2 N42 N -0.0227(3) 1.1299(2) 0.5211(2) 0.0431(6) Uani 1 1 d . . 2 N43 N 0.5688(3) 0.69198(19) 0.36433(17) 0.0379(6) Uani 1 1 d . B 2 N50 N 0.7425(3) 0.68604(19) 0.55915(16) 0.0357(6) Uani 1 1 d . G 2 N60 N 1.2587(3) 0.66023(19) 0.08206(15) 0.0345(5) Uani 1 1 d . H 2 N70 N 0.7327(3) 1.01194(19) 0.23055(16) 0.0391(6) Uani 1 1 d . H 2 N73 N 1.1488(3) 0.1614(2) 0.0716(2) 0.0468(7) Uani 1 1 d . . 2 C11 C 0.3093(3) 0.6413(2) 0.34491(18) 0.0319(6) Uani 1 1 d . B 2 C12 C 0.7953(3) 0.3440(2) 0.16243(17) 0.0302(6) Uani 1 1 d . B 2 C13 C 0.7314(3) 0.6365(2) 0.05860(18) 0.0362(7) Uani 1 1 d . B 2 C21 C 0.9213(3) 0.5300(2) 0.24403(17) 0.0291(6) Uani 1 1 d . B 2 C22 C 1.4045(3) 0.2281(2) 0.09865(18) 0.0303(6) Uani 1 1 d . C 2 C31 C 1.7993(3) -0.0876(2) -0.03524(19) 0.0335(6) Uani 1 1 d . . 2 C41 C 0.3387(3) 0.9791(2) 0.22377(18) 0.0332(6) Uani 1 1 d . . 2 C42 C 0.0639(3) 1.0912(2) 0.53914(18) 0.0349(7) Uani 1 1 d . E 2 C43 C 0.5268(3) 0.7729(2) 0.39248(17) 0.0283(5) Uani 1 1 d . B 2 C51 C 0.6298(4) 0.7574(3) 0.5922(2) 0.0480(8) Uani 1 1 d . G 2 H51C H 0.6016(9) 0.7502(3) 0.6478(15) 0.072 Uiso 1 1 calc R G 2 H51B H 0.5767(15) 0.7428(5) 0.5689(7) 0.072 Uiso 1 1 calc R G 2 H51A H 0.6468(6) 0.8199(17) 0.5787(4) 0.072 Uiso 1 1 calc R G 2 C52 C 0.8389(3) 0.6956(2) 0.5881(2) 0.0384(7) Uani 1 1 d . G 2 H52 H 0.831(4) 0.743(3) 0.620(3) 0.052(11) Uiso 1 1 d . I 2 C53 C 0.9421(3) 0.6255(2) 0.5644(2) 0.0370(7) Uani 1 1 d . G 2 H53 H 1.007(4) 0.635(3) 0.583(2) 0.041(10) Uiso 1 1 d . J 2 C54 C 0.9462(3) 0.5402(2) 0.51064(17) 0.0311(6) Uani 1 1 d . . 2 C55 C 0.8462(4) 0.5348(3) 0.4803(2) 0.0435(8) Uani 1 1 d . G 2 H55 H 0.839(4) 0.488(3) 0.448(3) 0.060(12) Uiso 1 1 d . K 2 C56 C 0.7447(4) 0.6076(3) 0.5048(2) 0.0461(8) Uani 1 1 d . G 2 H56 H 0.682(5) 0.600(4) 0.495(4) 0.085(18) Uiso 1 1 d . L 2 C61 C 1.3689(3) 0.5863(3) 0.0506(2) 0.0434(7) Uani 1 1 d . H 2 H61C H 1.3491(6) 0.5225(17) 0.0660(4) 0.065 Uiso 1 1 calc R H 2 H61B H 1.4243(15) 0.6008(4) 0.0743(6) 0.065 Uiso 1 1 calc R H 2 H61A H 1.3983(8) 0.5919(3) -0.0070(15) 0.065 Uiso 1 1 calc R H 2 C62 C 1.2546(4) 0.7331(3) 0.1422(2) 0.0417(7) Uani 1 1 d . H 2 H62 H 1.320(3) 0.733(2) 0.1505(19) 0.020(8) Uiso 1 1 d . M 2 C63 C 1.1516(4) 0.8006(3) 0.1746(2) 0.0429(8) Uani 1 1 d . H 2 H63 H 1.152(4) 0.845(3) 0.218(3) 0.057(12) Uiso 1 1 d . N 2 C64 C 1.0500(3) 0.7960(2) 0.14482(18) 0.0331(6) Uani 1 1 d . H 2 C65 C 1.0567(3) 0.7196(2) 0.08307(19) 0.0352(6) Uani 1 1 d . H 2 H65 H 0.994(4) 0.718(2) 0.070(2) 0.028(8) Uiso 1 1 d . O 2 C66 C 1.1618(3) 0.6524(2) 0.05371(19) 0.0354(6) Uani 1 1 d . H 2 H66 H 1.171(3) 0.600(2) 0.014(2) 0.030(8) Uiso 1 1 d . P 2 C71 C 0.6222(4) 1.0870(3) 0.2574(3) 0.0579(11) Uani 1 1 d . H 2 H71C H 0.6191(4) 1.1132(9) 0.3018(14) 0.087 Uiso 1 1 calc R H 2 H71B H 0.5630(19) 1.0571(10) 0.2647(4) 0.087 Uiso 1 1 calc R H 2 H71A H 0.6257(4) 1.1306(14) 0.2199(12) 0.087 Uiso 1 1 calc R H 2 C72 C 0.7196(4) 0.9100(2) 0.2195(2) 0.0403(8) Uani 1 1 d . H 2 H72 H 0.656(3) 0.898(3) 0.227(2) 0.025(9) Uiso 1 1 d . Q 2 C73 C 0.8206(3) 0.8380(2) 0.1932(2) 0.0388(7) Uani 1 1 d . H 2 H73 H 0.809(3) 0.773(3) 0.188(2) 0.039(9) Uiso 1 1 d . R 2 C74 C 0.9390(3) 0.8706(2) 0.17621(18) 0.0333(6) Uani 1 1 d . H 2 C75 C 0.9494(4) 0.9769(2) 0.1880(2) 0.0413(7) Uani 1 1 d . H 2 H75 H 1.021(4) 1.000(3) 0.180(2) 0.041(10) Uiso 1 1 d . S 2 C76 C 0.8453(4) 1.0451(3) 0.2146(2) 0.0443(8) Uani 1 1 d . H 2 H76 H 0.844(4) 1.113(3) 0.218(3) 0.050(11) Uiso 1 1 d . T 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 S14 0.0393(8) 0.0404(7) 0.0308(6) 0.0021(4) -0.0070(5) 0.0014(6) C14 0.021(3) 0.036(3) 0.0379(16) -0.0019(17) -0.0078(19) 0.0052(18) N14 0.020(2) 0.0285(18) 0.0446(19) 0.0040(13) -0.0208(16) -0.0056(15) S14A 0.0393(8) 0.0404(7) 0.0308(6) 0.0021(4) -0.0070(5) 0.0014(6) C14A 0.021(3) 0.036(3) 0.0379(16) -0.0019(17) -0.0078(19) 0.0052(18) N14A 0.020(2) 0.0285(18) 0.0446(19) 0.0040(13) -0.0208(16) -0.0056(15) Cd1 0.02605(12) 0.02867(9) 0.03377(10) -0.00300(7) -0.00904(8) 0.00100(7) Cd2 0.02519(13) 0.03469(10) 0.03245(10) -0.00552(7) -0.00597(8) 0.00292(8) Cd3 0.03351(19) 0.03109(14) 0.03090(13) -0.00754(10) -0.00313(11) 0.00556(11) Cd4 0.02951(14) 0.03152(10) 0.04403(11) -0.00961(8) -0.01127(9) 0.00832(8) S11 0.0267(4) 0.0287(3) 0.0398(3) -0.0085(2) -0.0068(3) -0.0008(3) S12 0.0280(4) 0.0337(3) 0.0431(4) -0.0072(3) -0.0114(3) 0.0001(3) S13 0.0345(5) 0.0417(4) 0.0399(4) 0.0080(3) -0.0128(3) -0.0040(3) S21 0.0269(4) 0.0337(3) 0.0384(3) -0.0030(3) -0.0106(3) 0.0017(3) S22 0.0296(4) 0.0431(4) 0.0415(4) -0.0170(3) -0.0111(3) 0.0059(3) S31 0.0386(5) 0.0347(3) 0.0404(4) -0.0094(3) -0.0112(3) 0.0031(3) S41 0.0450(5) 0.0387(4) 0.0292(3) -0.0003(3) -0.0059(3) 0.0101(3) S42 0.0440(5) 0.0488(4) 0.0372(4) -0.0142(3) -0.0173(3) 0.0123(4) S43 0.0363(5) 0.0333(4) 0.0625(5) -0.0177(3) -0.0176(4) 0.0072(3) O24 0.0380(15) 0.0484(12) 0.0475(12) 0.0077(10) -0.0148(10) 0.0001(10) N11 0.0309(18) 0.0461(15) 0.0731(19) -0.0234(14) -0.0202(14) 0.0089(12) N12 0.0373(18) 0.0443(14) 0.0428(13) -0.0113(11) -0.0141(11) 0.0074(12) N13 0.060(2) 0.0556(17) 0.0330(13) -0.0030(11) -0.0039(13) -0.0105(15) N21 0.0296(17) 0.0370(13) 0.0596(16) -0.0118(11) -0.0146(12) 0.0027(11) N22 0.0391(18) 0.0362(13) 0.0524(15) -0.0108(11) -0.0105(12) 0.0054(11) N41 0.0448(19) 0.0568(17) 0.0339(13) -0.0030(11) -0.0048(12) -0.0065(13) N42 0.0317(17) 0.0290(12) 0.0651(17) -0.0008(11) -0.0120(13) 0.0046(11) N43 0.0365(17) 0.0346(12) 0.0429(13) -0.0094(10) -0.0132(11) 0.0046(11) N50 0.0370(16) 0.0389(13) 0.0326(11) 0.0051(9) -0.0125(10) -0.0077(11) N60 0.0327(16) 0.0414(13) 0.0313(11) 0.0047(9) -0.0116(10) -0.0094(10) N70 0.0513(19) 0.0305(12) 0.0362(12) 0.0008(9) -0.0138(11) -0.0067(11) N73 0.0307(17) 0.0438(15) 0.0604(17) -0.0136(12) -0.0040(12) -0.0019(12) C11 0.0263(17) 0.0336(13) 0.0360(13) -0.0052(10) -0.0098(11) -0.0003(11) C12 0.0323(18) 0.0287(12) 0.0300(12) -0.0062(9) -0.0111(11) 0.0039(11) C13 0.046(2) 0.0375(14) 0.0303(13) 0.0050(10) -0.0165(12) -0.0138(13) C21 0.0254(17) 0.0283(12) 0.0336(12) -0.0023(9) -0.0086(10) -0.0029(11) C22 0.0252(16) 0.0273(12) 0.0387(13) -0.0015(10) -0.0113(11) 0.0012(10) C31 0.0263(17) 0.0359(14) 0.0363(13) -0.0031(11) -0.0061(11) -0.0031(11) C41 0.0398(19) 0.0322(13) 0.0302(13) -0.0009(10) -0.0132(12) -0.0063(12) C42 0.0357(19) 0.0270(12) 0.0353(13) -0.0056(10) -0.0006(11) -0.0006(11) C43 0.0170(15) 0.0356(13) 0.0335(12) -0.0028(10) -0.0100(10) 0.0005(10) C51 0.048(2) 0.0456(17) 0.0528(18) -0.0011(14) -0.0195(16) -0.0003(15) C52 0.040(2) 0.0363(15) 0.0442(16) -0.0008(12) -0.0191(13) -0.0092(13) C53 0.034(2) 0.0392(15) 0.0449(15) 0.0006(12) -0.0200(13) -0.0106(13) C54 0.0297(18) 0.0401(14) 0.0250(11) 0.0038(10) -0.0094(10) -0.0097(11) C55 0.042(2) 0.0576(19) 0.0354(14) -0.0127(13) -0.0148(13) -0.0071(15) C56 0.041(2) 0.063(2) 0.0406(16) -0.0094(14) -0.0195(14) -0.0055(16) C61 0.035(2) 0.0539(19) 0.0451(16) 0.0016(13) -0.0173(14) -0.0058(15) C62 0.038(2) 0.0495(18) 0.0468(17) -0.0014(13) -0.0234(15) -0.0118(15) C63 0.045(2) 0.0460(17) 0.0432(16) -0.0047(13) -0.0181(14) -0.0134(15) C64 0.0330(18) 0.0365(14) 0.0326(13) 0.0036(10) -0.0122(11) -0.0119(12) C65 0.031(2) 0.0461(16) 0.0342(13) -0.0019(11) -0.0157(12) -0.0096(13) C66 0.0325(19) 0.0449(16) 0.0314(13) -0.0018(11) -0.0120(11) -0.0081(13) C71 0.066(3) 0.0355(16) 0.070(2) -0.0056(15) -0.018(2) 0.0005(16) C72 0.045(2) 0.0325(15) 0.0461(17) 0.0003(12) -0.0148(15) -0.0114(14) C73 0.047(2) 0.0282(14) 0.0427(15) -0.0006(11) -0.0137(13) -0.0101(13) C74 0.0373(19) 0.0366(14) 0.0291(12) 0.0015(10) -0.0121(11) -0.0125(12) C75 0.044(2) 0.0382(16) 0.0435(16) -0.0012(12) -0.0110(14) -0.0178(14) C76 0.060(3) 0.0318(15) 0.0424(16) -0.0006(12) -0.0146(15) -0.0166(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 S14 C14 1.669(4) . ? C14 N14 1.132(5) . ? S14A C14A 1.637(7) . ? S14A Cd4 2.639(4) 2_666 ? C14A N14A 1.183(8) . ? N14A Cd1 2.502(12) . ? Cd1 N21 2.304(3) . ? Cd1 N43 2.332(2) . ? Cd1 S13 2.6968(8) . ? Cd1 S12 2.7107(8) . ? Cd1 S11 2.7236(8) . ? Cd2 N12 2.282(3) . ? Cd2 N73 2.292(3) . ? Cd2 N13 2.355(3) 2_765 ? Cd2 O24 2.420(2) . ? Cd2 S21 2.6906(8) . ? Cd2 S22 2.7170(9) . ? Cd3 N22 2.283(3) 2_855 ? Cd3 N22 2.283(3) . ? Cd3 N41 2.436(3) 2_765 ? Cd3 N41 2.436(3) 1_645 ? Cd3 S31 2.7025(9) 2_855 ? Cd3 S31 2.7025(9) . ? Cd4 N11 2.267(3) . ? Cd4 N42 2.285(3) 2_576 ? Cd4 S14A 2.639(4) 2_666 ? Cd4 S43 2.6707(10) . ? Cd4 S42 2.7205(8) . ? Cd4 S41 2.8002(8) . ? S11 C11 1.651(3) . ? S12 C12 1.645(3) . ? S13 C13 1.653(3) . ? S21 C21 1.644(3) . ? S22 C22 1.658(3) . ? S31 C31 1.654(3) . ? S41 C41 1.656(3) . ? S42 C42 1.648(4) . ? S43 C43 1.656(3) . ? N11 C11 1.148(4) . ? N12 C12 1.165(4) . ? N13 C13 1.154(4) . ? N13 Cd2 2.355(3) 2_765 ? N21 C21 1.149(4) . ? N22 C22 1.151(4) . ? N41 C41 1.153(4) . ? N41 Cd3 2.436(3) 1_465 ? N42 C42 1.168(4) . ? N42 Cd4 2.285(3) 2_576 ? N43 C43 1.147(4) . ? N50 C52 1.333(4) . ? N50 C56 1.347(4) . ? N50 C51 1.473(4) . ? N60 C66 1.327(4) . ? N60 C62 1.352(4) . ? N60 C61 1.468(4) . ? N70 C76 1.336(5) . ? N70 C72 1.349(4) . ? N70 C71 1.473(5) . ? N73 C31 1.145(4) 2_855 ? C31 N73 1.145(4) 2_855 ? C52 C53 1.374(5) . ? C53 C54 1.404(4) . ? C54 C55 1.375(5) . ? C54 C54 1.488(6) 2_766 ? C55 C56 1.382(5) . ? C62 C63 1.366(5) . ? C63 C64 1.386(5) . ? C64 C65 1.395(4) . ? C64 C74 1.480(5) . ? C65 C66 1.375(5) . ? C72 C73 1.374(5) . ? C73 C74 1.393(5) . ? C74 C75 1.398(4) . ? C75 C76 1.371(5) . ? 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 N14 C14 S14 171.7(5) . . ? C14A S14A Cd4 119.4(5) . 2_666 ? N14A C14A S14A 173.8(14) . . ? C14A N14A Cd1 123.1(11) . . ? N21 Cd1 N43 89.41(10) . . ? N21 Cd1 N14A 86.4(4) . . ? N43 Cd1 N14A 87.2(3) . . ? N21 Cd1 S13 91.92(8) . . ? N43 Cd1 S13 85.94(7) . . ? N14A Cd1 S13 173.0(3) . . ? N21 Cd1 S12 94.01(7) . . ? N43 Cd1 S12 175.87(7) . . ? N14A Cd1 S12 90.6(3) . . ? S13 Cd1 S12 96.26(3) . . ? N21 Cd1 S11 177.42(7) . . ? N43 Cd1 S11 92.69(7) . . ? N14A Cd1 S11 95.2(4) . . ? S13 Cd1 S11 86.74(3) . . ? S12 Cd1 S11 83.96(2) . . ? N12 Cd2 N73 91.81(10) . . ? N12 Cd2 N13 97.99(11) . 2_765 ? N73 Cd2 N13 84.29(11) . 2_765 ? N12 Cd2 O24 82.35(9) . . ? N73 Cd2 O24 83.91(10) . . ? N13 Cd2 O24 168.20(9) 2_765 . ? N12 Cd2 S21 92.73(7) . . ? N73 Cd2 S21 174.42(9) . . ? N13 Cd2 S21 98.29(8) 2_765 . ? O24 Cd2 S21 93.48(6) . . ? N12 Cd2 S22 168.14(7) . . ? N73 Cd2 S22 94.43(8) . . ? N13 Cd2 S22 92.67(9) 2_765 . ? O24 Cd2 S22 88.28(6) . . ? S21 Cd2 S22 80.53(2) . . ? N22 Cd3 N22 180.00(14) 2_855 . ? N22 Cd3 N41 84.33(10) 2_855 2_765 ? N22 Cd3 N41 95.67(10) . 2_765 ? N22 Cd3 N41 95.67(10) 2_855 1_645 ? N22 Cd3 N41 84.33(10) . 1_645 ? N41 Cd3 N41 180.00(14) 2_765 1_645 ? N22 Cd3 S31 83.61(8) 2_855 2_855 ? N22 Cd3 S31 96.39(8) . 2_855 ? N41 Cd3 S31 92.01(8) 2_765 2_855 ? N41 Cd3 S31 87.99(8) 1_645 2_855 ? N22 Cd3 S31 96.39(8) 2_855 . ? N22 Cd3 S31 83.61(8) . . ? N41 Cd3 S31 87.99(8) 2_765 . ? N41 Cd3 S31 92.01(8) 1_645 . ? S31 Cd3 S31 180.0 2_855 . ? N11 Cd4 N42 90.93(11) . 2_576 ? N11 Cd4 S14A 91.01(12) . 2_666 ? N42 Cd4 S14A 98.56(12) 2_576 2_666 ? N11 Cd4 S43 94.66(8) . . ? N42 Cd4 S43 173.87(7) 2_576 . ? S14A Cd4 S43 83.86(10) 2_666 . ? N11 Cd4 S42 176.05(9) . . ? N42 Cd4 S42 89.95(7) 2_576 . ? S14A Cd4 S42 85.05(8) 2_666 . ? S43 Cd4 S42 84.63(3) . . ? N11 Cd4 S41 96.60(9) . . ? N42 Cd4 S41 84.13(7) 2_576 . ? S14A Cd4 S41 171.90(9) 2_666 . ? S43 Cd4 S41 92.72(3) . . ? S42 Cd4 S41 87.32(2) . . ? C11 S11 Cd1 99.33(11) . . ? C12 S12 Cd1 97.94(10) . . ? C13 S13 Cd1 102.03(10) . . ? C21 S21 Cd2 100.04(10) . . ? C22 S22 Cd2 98.29(11) . . ? C31 S31 Cd3 98.63(12) . . ? C41 S41 Cd4 111.04(10) . . ? C42 S42 Cd4 96.75(10) . . ? C43 S43 Cd4 98.54(11) . . ? C11 N11 Cd4 163.2(3) . . ? C12 N12 Cd2 165.9(2) . . ? C13 N13 Cd2 129.1(3) . 2_765 ? C21 N21 Cd1 159.7(2) . . ? C22 N22 Cd3 146.4(3) . . ? C41 N41 Cd3 144.9(3) . 1_465 ? C42 N42 Cd4 147.3(2) . 2_576 ? C43 N43 Cd1 160.0(2) . . ? C52 N50 C56 120.5(3) . . ? C52 N50 C51 119.3(3) . . ? C56 N50 C51 120.0(3) . . ? C66 N60 C62 120.4(3) . . ? C66 N60 C61 119.6(3) . . ? C62 N60 C61 119.9(3) . . ? C76 N70 C72 120.2(3) . . ? C76 N70 C71 120.3(3) . . ? C72 N70 C71 119.5(3) . . ? C31 N73 Cd2 162.7(3) 2_855 . ? N11 C11 S11 178.2(3) . . ? N12 C12 S12 177.5(3) . . ? N13 C13 S13 178.0(3) . . ? N21 C21 S21 178.3(3) . . ? N22 C22 S22 178.8(3) . . ? N73 C31 S31 178.3(3) 2_855 . ? N41 C41 S41 178.4(3) . . ? N42 C42 S42 177.9(3) . . ? N43 C43 S43 178.6(3) . . ? N50 C52 C53 121.1(3) . . ? C52 C53 C54 120.2(3) . . ? C55 C54 C53 116.8(3) . . ? C55 C54 C54 122.5(3) . 2_766 ? C53 C54 C54 120.7(3) . 2_766 ? C54 C55 C56 121.3(3) . . ? N50 C56 C55 120.0(4) . . ? N60 C62 C63 121.0(3) . . ? C62 C63 C64 119.9(3) . . ? C63 C64 C65 117.8(3) . . ? C63 C64 C74 121.1(3) . . ? C65 C64 C74 121.1(3) . . ? C66 C65 C64 120.0(3) . . ? N60 C66 C65 120.9(3) . . ? N70 C72 C73 121.2(4) . . ? C72 C73 C74 119.7(3) . . ? C73 C74 C75 117.7(3) . . ? C73 C74 C64 121.1(3) . . ? C75 C74 C64 121.1(3) . . ? C76 C75 C74 120.0(3) . . ? N70 C76 C75 121.1(3) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 2.029 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.108 data_ll3 _database_code_depnum_ccdc_archive 'CCDC 201156' _chemical_name_common "N,N'-dimethyl-4,4'-bipyridinium cadmium-thiocyanate" _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 Cd N6 S4' _chemical_formula_weight 530.97 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7284(6) _cell_length_b 13.2940(7) _cell_length_c 13.2404(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.7850(10) _cell_angle_gamma 90.00 _cell_volume 2059.91(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17230 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0126 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3620 _reflns_number_gt 3350 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+5.4687P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3620 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.07110(2) 0.282593(19) 0.237940(19) 0.03342(8) Uani 1 1 d . . . S1 S -0.02941(11) 0.27657(11) 0.40960(10) 0.0643(4) Uani 1 1 d . . . S2 S -0.32447(8) 0.26781(8) 0.06455(8) 0.0404(2) Uani 1 1 d . . . S3 S 0.44913(9) 0.22154(8) 0.38597(9) 0.0479(3) Uani 1 1 d . . . S4 S 0.14772(9) 0.09009(8) 0.25864(10) 0.0524(3) Uani 1 1 d . . . N1 N 0.1495(3) 0.2259(2) 0.5645(2) 0.0346(5) Uani 1 1 d . . . N2 N -0.1138(3) 0.2528(2) 0.1761(2) 0.0346(5) Uani 1 1 d . . . N3 N 0.2515(3) 0.3143(3) 0.3033(3) 0.0413(8) Uani 1 1 d . . . N4 N -0.0316(3) -0.0459(3) 0.2704(3) 0.0562(10) Uani 1 1 d . . . N5 N 0.2765(3) -0.0032(3) 0.0554(2) 0.0446(8) Uani 1 1 d . . . N6 N 0.7445(3) 0.0167(2) 0.4112(2) 0.0409(8) Uani 1 1 d . . . C1 C 0.0621(3) 0.2472(3) 0.4941(3) 0.0464(10) Uani 1 1 d . . . C2 C -0.2005(3) 0.2604(3) 0.1309(3) 0.0323(8) Uani 1 1 d . . . C3 C 0.3327(3) 0.2747(3) 0.3366(3) 0.0337(8) Uani 1 1 d . . . C4 C 0.0397(3) 0.0112(3) 0.2624(3) 0.0353(8) Uani 1 1 d . . . C5 C 0.2960(4) -0.0802(3) 0.1197(3) 0.0516(11) Uani 1 1 d . . . H5 H 0.2467 -0.1370 0.1153 0.062 Uiso 1 1 calc R . . C6 C 0.3857(4) -0.0785(3) 0.1916(3) 0.0452(10) Uani 1 1 d . . . H6 H 0.3977 -0.1334 0.2370 0.054 Uiso 1 1 calc R . . C7 C 0.4585(3) 0.0031(3) 0.1978(3) 0.0375(8) Uani 1 1 d . . . C8 C 0.4348(4) 0.0831(3) 0.1307(3) 0.0490(10) Uani 1 1 d . . . H8 H 0.4823 0.1410 0.1334 0.059 Uiso 1 1 calc R . . C9 C 0.3435(4) 0.0777(3) 0.0616(3) 0.0506(11) Uani 1 1 d . . . H9 H 0.3275 0.1326 0.0170 0.061 Uiso 1 1 calc R . . C10 C 0.1769(4) -0.0044(4) -0.0186(4) 0.0588(12) Uani 1 1 d . . . H10F H 0.1843 -0.0603 -0.0659 0.088 Uiso 0.50 1 calc PR . . H10E H 0.1734 0.0592 -0.0561 0.088 Uiso 0.50 1 calc PR . . H10D H 0.1069 -0.0127 0.0170 0.088 Uiso 0.50 1 calc PR . . H10C H 0.1254 0.0511 -0.0041 0.088 Uiso 0.50 1 calc PR . . H10B H 0.1363 -0.0684 -0.0138 0.088 Uiso 0.50 1 calc PR . . H10A H 0.2028 0.0035 -0.0870 0.088 Uiso 0.50 1 calc PR . . C11 C 0.5583(3) 0.0067(3) 0.2728(3) 0.0369(8) Uani 1 1 d . . . C12 C 0.6514(3) 0.0690(3) 0.2571(3) 0.0432(9) Uani 1 1 d . . . H12 H 0.6511 0.1090 0.1977 0.052 Uiso 1 1 calc R . . C13 C 0.7428(3) 0.0729(3) 0.3265(3) 0.0438(9) Uani 1 1 d . . . H13 H 0.8057 0.1155 0.3149 0.053 Uiso 1 1 calc R . . C14 C 0.6569(4) -0.0440(3) 0.4281(3) 0.0456(10) Uani 1 1 d . . . H14 H 0.6598 -0.0837 0.4879 0.055 Uiso 1 1 calc R . . C15 C 0.5636(3) -0.0501(3) 0.3616(3) 0.0435(10) Uani 1 1 d . . . H15 H 0.5019 -0.0931 0.3757 0.052 Uiso 1 1 calc R . . C16 C 0.8438(4) 0.0235(3) 0.4851(3) 0.0496(10) Uani 1 1 d . . . H16F H 0.9130 0.0034 0.4527 0.074 Uiso 0.50 1 calc PR . . H16E H 0.8323 -0.0213 0.5423 0.074 Uiso 0.50 1 calc PR . . H16D H 0.8521 0.0929 0.5094 0.074 Uiso 0.50 1 calc PR . . H16C H 0.8186 0.0466 0.5503 0.074 Uiso 0.50 1 calc PR . . H16B H 0.8993 0.0713 0.4606 0.074 Uiso 0.50 1 calc PR . . H16A H 0.8795 -0.0429 0.4935 0.074 Uiso 0.50 1 calc PR . . 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 0.03472(15) 0.03316(15) 0.03100(15) 0.00124(9) -0.00832(11) -0.00055(9) S1 0.0542(7) 0.0936(10) 0.0455(6) 0.0030(6) 0.0065(5) 0.0034(6) S2 0.0309(4) 0.0470(5) 0.0419(5) 0.0068(4) -0.0078(4) -0.0020(4) S3 0.0330(5) 0.0513(6) 0.0584(6) 0.0061(5) -0.0042(5) 0.0037(4) S4 0.0421(5) 0.0348(5) 0.0816(7) 0.0126(5) 0.0139(5) 0.0026(4) N1 0.0481(12) 0.0346(11) 0.0192(9) -0.0012(8) -0.0127(9) 0.0048(9) N2 0.0481(12) 0.0346(11) 0.0192(9) -0.0012(8) -0.0127(9) 0.0048(9) N3 0.0351(16) 0.0436(17) 0.0438(18) 0.0005(15) -0.0074(14) 0.0004(14) N4 0.0496(19) 0.0382(19) 0.079(3) -0.0037(18) -0.0085(18) -0.0056(17) N5 0.0524(18) 0.0420(18) 0.0381(17) -0.0047(14) -0.0067(14) 0.0090(15) N6 0.0425(16) 0.0385(17) 0.0415(16) 0.0007(14) 0.0010(13) 0.0094(14) C1 0.048(2) 0.0335(19) 0.060(3) -0.012(2) 0.017(2) -0.0030(18) C2 0.0366(18) 0.0355(17) 0.0247(16) 0.0013(14) 0.0022(14) -0.0024(15) C3 0.0359(18) 0.0315(17) 0.0334(18) -0.0044(14) 0.0008(15) -0.0073(14) C4 0.0448(19) 0.0313(18) 0.0299(16) -0.0017(14) 0.0026(15) 0.0066(16) C5 0.065(3) 0.0301(19) 0.057(2) -0.0051(18) -0.014(2) 0.0019(18) C6 0.057(2) 0.0321(19) 0.045(2) 0.0029(16) -0.0101(18) 0.0081(17) C7 0.0408(18) 0.0357(19) 0.0361(18) 0.0012(15) 0.0050(15) 0.0066(16) C8 0.048(2) 0.050(2) 0.047(2) 0.0169(19) -0.0044(18) -0.0032(19) C9 0.056(2) 0.050(2) 0.044(2) 0.0145(19) -0.0068(18) -0.001(2) C10 0.068(3) 0.050(2) 0.055(3) -0.002(2) -0.021(2) 0.004(2) C11 0.0397(18) 0.0344(18) 0.0369(18) 0.0024(15) 0.0041(15) 0.0082(15) C12 0.042(2) 0.043(2) 0.045(2) 0.0110(17) 0.0043(17) 0.0087(17) C13 0.042(2) 0.042(2) 0.048(2) 0.0073(18) 0.0045(17) 0.0062(17) C14 0.050(2) 0.048(2) 0.039(2) 0.0102(17) 0.0017(17) 0.0027(18) C15 0.043(2) 0.043(2) 0.045(2) 0.0084(17) 0.0037(17) -0.0001(17) C16 0.047(2) 0.051(2) 0.049(2) -0.0051(19) -0.0114(18) 0.0078(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 2.272(3) . ? Cd1 N2 2.302(3) . ? Cd1 N4 2.328(4) 2 ? Cd1 N1 2.532(3) 4_565 ? Cd1 S1 2.6297(13) . ? Cd1 S4 2.7202(11) . ? S1 C1 1.549(5) . ? S2 C2 1.651(4) . ? S3 C3 1.635(4) . ? S4 C4 1.648(4) . ? N1 C1 1.369(5) . ? N1 Cd1 2.532(3) 4_566 ? N2 C2 1.150(5) . ? N3 C3 1.151(5) . ? N4 C4 1.139(5) . ? N4 Cd1 2.328(4) 2_545 ? N5 C9 1.331(6) . ? N5 C5 1.341(5) . ? N5 C10 1.475(5) . ? N6 C14 1.337(5) . ? N6 C13 1.346(5) . ? N6 C16 1.474(5) . ? C5 C6 1.372(6) . ? C6 C7 1.380(6) . ? C7 C8 1.402(5) . ? C7 C11 1.485(5) . ? C8 C9 1.363(6) . ? C11 C15 1.396(5) . ? C11 C12 1.397(6) . ? C12 C13 1.367(6) . ? C14 C15 1.360(6) . ? 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 N3 Cd1 N2 178.17(11) . . ? N3 Cd1 N4 90.76(13) . 2 ? N2 Cd1 N4 88.39(12) . 2 ? N3 Cd1 N1 88.24(11) . 4_565 ? N2 Cd1 N1 93.44(10) . 4_565 ? N4 Cd1 N1 94.81(13) 2 4_565 ? N3 Cd1 S1 97.79(9) . . ? N2 Cd1 S1 80.58(8) . . ? N4 Cd1 S1 88.37(11) 2 . ? N1 Cd1 S1 173.16(7) 4_565 . ? N3 Cd1 S4 80.98(9) . . ? N2 Cd1 S4 99.87(8) . . ? N4 Cd1 S4 171.74(10) 2 . ? N1 Cd1 S4 84.96(7) 4_565 . ? S1 Cd1 S4 92.76(4) . . ? C1 S1 Cd1 107.68(16) . . ? C4 S4 Cd1 110.64(13) . . ? C1 N1 Cd1 109.0(3) . 4_566 ? C2 N2 Cd1 161.9(3) . . ? C3 N3 Cd1 142.0(3) . . ? C4 N4 Cd1 142.4(3) . 2_545 ? C9 N5 C5 120.2(3) . . ? C9 N5 C10 119.2(4) . . ? C5 N5 C10 120.5(4) . . ? C14 N6 C13 120.4(3) . . ? C14 N6 C16 120.5(3) . . ? C13 N6 C16 119.1(4) . . ? N1 C1 S1 175.1(4) . . ? N2 C2 S2 178.3(4) . . ? N3 C3 S3 178.2(3) . . ? N4 C4 S4 175.7(4) . . ? N5 C5 C6 121.2(4) . . ? C5 C6 C7 119.8(4) . . ? C6 C7 C8 117.6(4) . . ? C6 C7 C11 121.5(3) . . ? C8 C7 C11 120.9(3) . . ? C9 C8 C7 120.0(4) . . ? N5 C9 C8 121.1(4) . . ? C15 C11 C12 117.0(3) . . ? C15 C11 C7 122.4(3) . . ? C12 C11 C7 120.6(3) . . ? C13 C12 C11 120.6(4) . . ? N6 C13 C12 120.4(4) . . ? N6 C14 C15 121.4(4) . . ? C14 C15 C11 120.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.350 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.113