Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Long-Li Lai' _publ_contact_author_address ; Department of Applied Chemistry National Chi Nan University Puli, Nantou 545 TAIWAN ; _publ_contact_author_email LILAI@NCNU.EDU.TW _publ_section_title ; Polypseudorotaxane architecture of poly-bis[4 (N benzyl- pyridinium)]piperazine-hexa-thiocyanato-di-cadmium(II) with 2D honeycomb-like [Cd(SCN)3]nn- anionic polymeric framework ; loop_ _publ_author_name 'Long-Li Lai.' 'Kung-Lung Cheng.' 'Yi-Hung Liu.' 'Kuang-Lieh Lu.' ; D.V.Soldatov ; 'Yu Wang.' 'Yuh S.Wen' 'Chun-Han Wu.' 'Zhi Yu.' 'Kui Yu.' #CIF of hybrid 3 data_401d _database_code_depnum_ccdc_archive 'CCDC 288698' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Cd2 N10 S6' _chemical_formula_sum 'C34 H30 Cd2 N10 S6' _chemical_formula_weight 995.84 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 20.8688(6) _cell_length_b 18.5411(5) _cell_length_c 9.8944(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.9050(10) _cell_angle_gamma 90.00 _cell_volume 3814.42(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6728 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6728 _reflns_number_gt 5769 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker X8APEX' _computing_cell_refinement 'Bruker X8APEX' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ;WinGX publication routines (Farrugia, 1999) ; _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^)+(0.0203P)^2^+0.9125P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00009(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6728 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0429 _refine_ls_wR_factor_gt 0.0419 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.004 _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 0.262333(6) 0.660850(7) 0.772636(13) 0.01276(5) Uani 1 1 d . . . Cd2 Cd 0.246417(6) 0.342512(7) 0.828322(13) 0.01298(5) Uani 1 1 d . . . S51 S 0.35606(2) 0.56962(2) 0.68954(5) 0.01770(11) Uani 1 1 d . . . S52 S 0.33398(2) 0.35656(3) 1.04589(5) 0.01859(11) Uani 1 1 d . . . S53 S 0.15714(2) 0.43277(3) 0.92618(5) 0.01853(11) Uani 1 1 d . . . S54 S 0.34506(2) 0.77040(2) 0.74883(5) 0.01594(11) Uani 1 1 d . . . S55 S 0.14682(2) 0.34426(2) 0.62031(5) 0.01397(10) Uani 1 1 d . . . S56 S 0.16226(2) 0.74490(3) 0.83829(5) 0.01690(11) Uani 1 1 d . . . N1 N 0.17842(7) 0.95477(8) 0.77746(15) 0.0137(3) Uani 1 1 d . . . N4 N 0.29764(7) 1.02581(8) 0.86874(15) 0.0129(3) Uani 1 1 d . . . N11 N 0.01776(7) 0.83397(8) 0.65435(16) 0.0134(3) Uani 1 1 d . . . N21 N 0.46053(7) 1.15278(8) 0.92235(16) 0.0150(4) Uani 1 1 d . . . N51 N 0.30104(7) 0.43438(8) 0.73484(16) 0.0167(4) Uani 1 1 d . . . N52 N 0.29675(7) 0.25700(9) 0.70957(16) 0.0177(4) Uani 1 1 d . . . N53 N 0.20364(7) 0.56133(8) 0.82121(16) 0.0171(4) Uani 1 1 d . . . N54 N 0.21671(8) 0.67118(8) 0.55458(16) 0.0180(4) Uani 1 1 d . . . N55 N 0.19383(7) 0.25312(8) 0.93529(16) 0.0174(4) Uani 1 1 d . . . N56 N 0.30471(8) 0.66956(8) 0.99503(17) 0.0168(4) Uani 1 1 d . . . C2 C 0.23671(8) 0.94920(11) 0.70499(19) 0.0181(4) Uani 1 1 d . . . H2A H 0.2369 0.9874 0.6380 0.022 Uiso 1 1 calc R . . H2B H 0.2369 0.9034 0.6578 0.022 Uiso 1 1 calc R . . C3 C 0.29604(9) 0.95501(10) 0.8026(2) 0.0178(4) Uani 1 1 d . . . H3A H 0.2957 0.9173 0.8704 0.021 Uiso 1 1 calc R . . H3B H 0.3341 0.9489 0.7540 0.021 Uiso 1 1 calc R . . C5 C 0.23454(8) 1.05487(10) 0.8959(2) 0.0145(4) Uani 1 1 d . . . H5A H 0.2198 1.0880 0.8239 0.017 Uiso 1 1 calc R . . H5B H 0.2386 1.0816 0.9804 0.017 Uiso 1 1 calc R . . C6 C 0.18559(9) 0.99545(9) 0.90491(18) 0.0139(4) Uani 1 1 d . . . H6A H 0.1993 0.9633 0.9791 0.017 Uiso 1 1 calc R . . H6B H 0.1445 1.0161 0.9231 0.017 Uiso 1 1 calc R . . C7 C -0.03487(9) 0.78181(10) 0.61819(19) 0.0153(4) Uani 1 1 d . . . H7A H -0.0436 0.7804 0.5203 0.018 Uiso 1 1 calc R . . H7B H -0.0736 0.7980 0.6565 0.018 Uiso 1 1 calc R . . C8 C 0.51912(9) 1.19804(10) 0.9420(2) 0.0198(4) Uani 1 1 d . . . H8A H 0.5505 1.1804 0.8832 0.024 Uiso 1 1 calc R . . H8B H 0.5375 1.1929 1.0349 0.024 Uiso 1 1 calc R . . C12 C 0.06436(9) 0.84540(9) 0.56935(19) 0.0149(4) Uani 1 1 d . . . H12 H 0.0602 0.8245 0.4836 0.018 Uiso 1 1 calc R . . C13 C 0.11662(9) 0.88627(9) 0.60560(18) 0.0143(4) Uani 1 1 d . . . H13 H 0.1476 0.8931 0.5447 0.017 Uiso 1 1 calc R . . C14 C 0.12458(9) 0.91880(9) 0.73530(18) 0.0130(4) Uani 1 1 d . . . C15 C 0.07318(9) 0.90980(9) 0.81814(19) 0.0142(4) Uani 1 1 d . . . H15 H 0.0740 0.9334 0.9012 0.017 Uiso 1 1 calc R . . C16 C 0.02250(9) 0.86668(10) 0.77655(19) 0.0147(4) Uani 1 1 d . . . H16 H -0.0099 0.8596 0.8342 0.018 Uiso 1 1 calc R . . C22 C 0.46487(9) 1.08316(10) 0.88407(19) 0.0166(4) Uani 1 1 d . . . H22 H 0.5049 1.0649 0.8672 0.020 Uiso 1 1 calc R . . C23 C 0.41328(9) 1.03898(10) 0.86935(19) 0.0166(4) Uani 1 1 d . . . H23 H 0.4185 0.9911 0.8445 0.020 Uiso 1 1 calc R . . C24 C 0.35101(9) 1.06516(10) 0.89158(18) 0.0133(4) Uani 1 1 d . . . C25 C 0.34869(9) 1.13735(10) 0.93875(18) 0.0131(4) Uani 1 1 d . . . H25 H 0.3099 1.1567 0.9611 0.016 Uiso 1 1 calc R . . C26 C 0.40245(9) 1.17818(10) 0.95135(19) 0.0150(4) Uani 1 1 d . . . H26 H 0.3995 1.2255 0.9811 0.018 Uiso 1 1 calc R . . C31 C -0.01820(9) 0.70666(10) 0.66953(18) 0.0134(4) Uani 1 1 d . . . C32 C -0.06031(9) 0.66969(10) 0.74635(19) 0.0161(4) Uani 1 1 d . . . H32 H -0.0985 0.6914 0.7666 0.019 Uiso 1 1 calc R . . C33 C -0.04563(10) 0.60071(10) 0.7928(2) 0.0209(5) Uani 1 1 d . . . H33 H -0.0741 0.5762 0.8438 0.025 Uiso 1 1 calc R . . C34 C 0.01129(10) 0.56804(10) 0.7635(2) 0.0210(5) Uani 1 1 d . . . H34 H 0.0214 0.5220 0.7959 0.025 Uiso 1 1 calc R . . C35 C 0.05285(9) 0.60430(10) 0.6861(2) 0.0201(4) Uani 1 1 d . . . H35 H 0.0910 0.5825 0.6658 0.024 Uiso 1 1 calc R . . C36 C 0.03804(9) 0.67296(10) 0.63874(19) 0.0170(4) Uani 1 1 d . . . H36 H 0.0661 0.6968 0.5857 0.020 Uiso 1 1 calc R . . C41 C 0.50697(9) 1.27705(10) 0.9127(2) 0.0159(4) Uani 1 1 d . . . C42 C 0.53583(9) 1.32787(11) 1.0006(2) 0.0205(4) Uani 1 1 d . . . H42 H 0.5593 1.3130 1.0799 0.025 Uiso 1 1 calc R . . C43 C 0.52992(10) 1.40064(11) 0.9712(2) 0.0251(5) Uani 1 1 d . . . H43 H 0.5509 1.4345 1.0285 0.030 Uiso 1 1 calc R . . C44 C 0.49301(10) 1.42297(11) 0.8570(2) 0.0244(5) Uani 1 1 d . . . H44 H 0.4887 1.4719 0.8378 0.029 Uiso 1 1 calc R . . C45 C 0.46244(9) 1.37275(11) 0.7710(2) 0.0213(5) Uani 1 1 d . . . H45 H 0.4365 1.3879 0.6951 0.026 Uiso 1 1 calc R . . C46 C 0.47039(9) 1.29990(10) 0.7977(2) 0.0182(4) Uani 1 1 d . . . H46 H 0.4510 1.2661 0.7379 0.022 Uiso 1 1 calc R . . C51 C 0.32371(9) 0.49005(10) 0.71747(18) 0.0134(4) Uani 1 1 d . . . C52 C 0.31060(9) 0.28996(10) 1.14178(19) 0.0139(4) Uani 1 1 d . . . C53 C 0.18466(9) 0.50815(10) 0.86300(19) 0.0144(4) Uani 1 1 d . . . C54 C 0.32133(9) 0.80418(10) 0.5981(2) 0.0137(4) Uani 1 1 d . . . C55 C 0.17423(8) 0.28653(10) 0.51187(19) 0.0136(4) Uani 1 1 d . . . C56 C 0.19536(9) 0.79323(10) 0.9657(2) 0.0138(4) Uani 1 1 d . . . 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 0.01601(8) 0.01116(8) 0.01111(8) 0.00028(6) 0.00110(6) -0.00050(5) Cd2 0.01617(8) 0.01050(8) 0.01247(8) 0.00091(6) 0.00240(6) -0.00048(5) S51 0.0170(3) 0.0121(2) 0.0248(3) -0.0005(2) 0.0068(2) -0.00188(19) S52 0.0225(3) 0.0169(3) 0.0160(3) 0.0020(2) -0.0003(2) -0.0062(2) S53 0.0235(3) 0.0125(2) 0.0210(3) -0.0005(2) 0.0105(2) -0.0017(2) S54 0.0182(3) 0.0144(2) 0.0147(3) 0.0021(2) -0.00127(19) -0.00193(19) S55 0.0143(2) 0.0145(2) 0.0134(2) -0.00083(19) 0.00293(19) 0.00115(19) S56 0.0169(3) 0.0165(2) 0.0167(3) -0.0036(2) -0.0019(2) 0.0029(2) N1 0.0151(8) 0.0131(8) 0.0133(8) -0.0034(7) 0.0033(7) -0.0018(7) N4 0.0128(8) 0.0113(8) 0.0148(8) -0.0027(7) 0.0027(6) 0.0008(6) N11 0.0133(8) 0.0116(8) 0.0151(8) 0.0007(7) 0.0002(7) -0.0013(6) N21 0.0134(8) 0.0144(8) 0.0172(9) 0.0014(7) 0.0012(7) -0.0005(6) N51 0.0173(9) 0.0141(9) 0.0194(9) 0.0007(7) 0.0059(7) -0.0003(7) N52 0.0192(9) 0.0193(9) 0.0140(9) -0.0005(8) -0.0028(7) 0.0020(7) N53 0.0170(9) 0.0142(9) 0.0204(9) -0.0009(7) 0.0045(7) 0.0020(7) N54 0.0253(10) 0.0140(8) 0.0143(9) 0.0005(7) -0.0005(7) -0.0014(7) N55 0.0163(9) 0.0183(9) 0.0171(9) 0.0032(7) -0.0023(7) -0.0028(7) N56 0.0184(9) 0.0173(9) 0.0148(9) 0.0026(7) 0.0019(7) 0.0021(7) C2 0.0156(10) 0.0211(10) 0.0185(11) -0.0070(9) 0.0062(8) -0.0005(8) C3 0.0149(10) 0.0159(10) 0.0229(11) -0.0062(9) 0.0030(8) 0.0012(8) C5 0.0127(10) 0.0136(9) 0.0173(10) -0.0028(8) 0.0024(8) 0.0008(8) C6 0.0156(10) 0.0141(10) 0.0124(10) -0.0031(8) 0.0033(8) -0.0001(8) C7 0.0132(10) 0.0167(10) 0.0156(11) -0.0005(8) -0.0008(8) -0.0029(8) C8 0.0145(10) 0.0177(11) 0.0274(12) 0.0007(9) 0.0019(9) -0.0002(8) C12 0.0202(10) 0.0138(10) 0.0106(10) 0.0017(8) 0.0016(8) 0.0016(8) C13 0.0155(10) 0.0144(10) 0.0133(10) 0.0034(8) 0.0027(8) -0.0021(8) C14 0.0164(10) 0.0070(9) 0.0154(10) 0.0033(8) -0.0001(8) 0.0034(7) C15 0.0177(10) 0.0118(9) 0.0132(10) -0.0013(8) 0.0023(8) 0.0014(8) C16 0.0162(10) 0.0124(9) 0.0158(11) 0.0015(8) 0.0033(8) 0.0026(8) C22 0.0142(10) 0.0187(10) 0.0168(10) 0.0004(8) 0.0018(8) 0.0043(8) C23 0.0165(10) 0.0139(10) 0.0196(11) -0.0018(8) 0.0026(8) 0.0036(8) C24 0.0175(10) 0.0141(10) 0.0083(9) 0.0031(8) 0.0016(8) 0.0022(8) C25 0.0121(10) 0.0152(9) 0.0121(10) 0.0010(8) 0.0013(8) 0.0031(8) C26 0.0160(10) 0.0144(10) 0.0147(10) 0.0007(8) 0.0022(8) 0.0038(8) C31 0.0133(10) 0.0154(10) 0.0107(10) -0.0032(8) -0.0025(8) -0.0019(8) C32 0.0147(10) 0.0196(10) 0.0135(10) -0.0040(8) -0.0009(8) -0.0019(8) C33 0.0274(12) 0.0184(11) 0.0170(11) 0.0007(9) 0.0023(9) -0.0087(9) C34 0.0314(12) 0.0120(10) 0.0183(11) -0.0021(8) -0.0057(9) -0.0009(9) C35 0.0182(10) 0.0197(11) 0.0214(11) -0.0047(9) -0.0034(9) 0.0035(8) C36 0.0163(10) 0.0198(10) 0.0147(10) -0.0033(8) -0.0004(8) -0.0038(8) C41 0.0109(10) 0.0182(10) 0.0194(11) 0.0001(9) 0.0051(8) -0.0006(8) C42 0.0163(10) 0.0253(11) 0.0196(11) -0.0007(9) -0.0010(8) 0.0016(9) C43 0.0267(12) 0.0205(11) 0.0280(13) -0.0078(10) 0.0023(10) -0.0017(9) C44 0.0303(12) 0.0160(10) 0.0280(12) -0.0003(9) 0.0090(10) 0.0047(9) C45 0.0211(11) 0.0242(11) 0.0190(11) 0.0032(9) 0.0046(9) 0.0059(9) C46 0.0172(10) 0.0203(11) 0.0176(11) -0.0025(9) 0.0032(8) -0.0030(8) C51 0.0124(10) 0.0176(11) 0.0102(10) -0.0017(8) 0.0011(7) 0.0038(8) C52 0.0132(10) 0.0155(10) 0.0123(10) -0.0047(9) -0.0031(8) 0.0003(8) C53 0.0140(10) 0.0164(10) 0.0129(10) -0.0047(8) 0.0027(8) 0.0038(8) C54 0.0118(10) 0.0116(9) 0.0181(11) -0.0056(8) 0.0037(8) -0.0020(8) C55 0.0103(9) 0.0141(10) 0.0160(11) 0.0052(9) -0.0017(8) -0.0027(8) C56 0.0139(10) 0.0109(10) 0.0174(11) 0.0065(9) 0.0052(8) 0.0047(8) _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 N53 2.2885(16) . ? Cd1 N54 2.2906(17) . ? Cd1 N56 2.3060(17) . ? Cd1 S54 2.6891(5) . ? Cd1 S56 2.7283(5) . ? Cd1 S51 2.7637(5) . ? Cd2 N52 2.2823(16) . ? Cd2 N51 2.2883(15) . ? Cd2 N55 2.2957(16) . ? Cd2 S52 2.7145(5) . ? Cd2 S53 2.7418(5) . ? Cd2 S55 2.7974(5) . ? S51 C51 1.6554(19) . ? S52 C52 1.656(2) . ? S53 C53 1.654(2) . ? S54 C54 1.654(2) . ? S55 C55 1.652(2) . ? S56 C56 1.649(2) . ? N1 C14 1.342(2) . ? N1 C6 1.466(2) . ? N1 C2 1.468(2) . ? N4 C24 1.334(2) . ? N4 C3 1.466(2) . ? N4 C5 1.469(2) . ? N11 C16 1.349(2) . ? N11 C12 1.356(2) . ? N11 C7 1.484(2) . ? N21 C22 1.350(2) . ? N21 C26 1.354(2) . ? N21 C8 1.482(2) . ? N51 C51 1.154(2) . ? N52 C52 1.151(2) 4_565 ? N53 C53 1.152(2) . ? N54 C56 1.158(2) 4_575 ? N55 C55 1.155(2) 4_566 ? N56 C54 1.156(2) 4_576 ? C2 C3 1.507(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.510(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C31 1.513(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C41 1.511(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C12 C13 1.351(3) . ? C12 H12 0.9300 . ? C13 C14 1.415(3) . ? C13 H13 0.9300 . ? C14 C15 1.415(3) . ? C15 C16 1.361(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C22 C23 1.351(3) . ? C22 H22 0.9300 . ? C23 C24 1.422(3) . ? C23 H23 0.9300 . ? C24 C25 1.420(2) . ? C25 C26 1.350(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C36 1.386(3) . ? C31 C32 1.391(3) . ? C32 C33 1.384(3) . ? C32 H32 0.9300 . ? C33 C34 1.386(3) . ? C33 H33 0.9300 . ? C34 C35 1.380(3) . ? C34 H34 0.9300 . ? C35 C36 1.382(3) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C46 1.382(3) . ? C41 C42 1.385(3) . ? C42 C43 1.384(3) . ? C42 H42 0.9300 . ? C43 C44 1.375(3) . ? C43 H43 0.9300 . ? C44 C45 1.380(3) . ? C44 H44 0.9300 . ? C45 C46 1.383(3) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C52 N52 1.151(2) 4_566 ? C54 N56 1.156(2) 4_575 ? C55 N55 1.155(2) 4_565 ? C56 N54 1.158(2) 4_576 ? 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 N53 Cd1 N54 94.50(6) . . ? N53 Cd1 N56 91.41(6) . . ? N54 Cd1 N56 170.96(5) . . ? N53 Cd1 S54 170.62(4) . . ? N54 Cd1 S54 94.16(4) . . ? N56 Cd1 S54 80.44(4) . . ? N53 Cd1 S56 88.64(4) . . ? N54 Cd1 S56 84.92(4) . . ? N56 Cd1 S56 88.38(4) . . ? S54 Cd1 S56 95.716(15) . . ? N53 Cd1 S51 88.52(4) . . ? N54 Cd1 S51 91.07(4) . . ? N56 Cd1 S51 95.93(4) . . ? S54 Cd1 S51 87.724(15) . . ? S56 Cd1 S51 174.891(15) . . ? N52 Cd2 N51 92.40(6) . . ? N52 Cd2 N55 89.71(6) . . ? N51 Cd2 N55 176.40(6) . . ? N52 Cd2 S52 99.60(4) . . ? N51 Cd2 S52 85.66(4) . . ? N55 Cd2 S52 91.12(4) . . ? N52 Cd2 S53 164.23(4) . . ? N51 Cd2 S53 93.75(4) . . ? N55 Cd2 S53 84.94(4) . . ? S52 Cd2 S53 95.340(16) . . ? N52 Cd2 S55 88.57(4) . . ? N51 Cd2 S55 93.35(4) . . ? N55 Cd2 S55 89.61(4) . . ? S52 Cd2 S55 171.807(15) . . ? S53 Cd2 S55 76.595(15) . . ? C51 S51 Cd1 100.76(6) . . ? C52 S52 Cd2 99.87(6) . . ? C53 S53 Cd2 96.54(6) . . ? C54 S54 Cd1 102.71(6) . . ? C55 S55 Cd2 101.16(6) . . ? C56 S56 Cd1 102.31(6) . . ? C14 N1 C6 122.98(15) . . ? C14 N1 C2 121.34(15) . . ? C6 N1 C2 115.37(14) . . ? C24 N4 C3 123.51(15) . . ? C24 N4 C5 121.13(15) . . ? C3 N4 C5 115.05(14) . . ? C16 N11 C12 118.97(16) . . ? C16 N11 C7 120.35(15) . . ? C12 N11 C7 120.51(16) . . ? C22 N21 C26 118.34(16) . . ? C22 N21 C8 120.24(15) . . ? C26 N21 C8 121.25(15) . . ? C51 N51 Cd2 161.87(15) . . ? C52 N52 Cd2 167.19(15) 4_565 . ? C53 N53 Cd1 166.37(15) . . ? C56 N54 Cd1 149.90(14) 4_575 . ? C55 N55 Cd2 166.35(15) 4_566 . ? C54 N56 Cd1 158.88(14) 4_576 . ? N1 C2 C3 110.60(16) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N4 C3 C2 109.65(15) . . ? N4 C3 H3A 109.7 . . ? C2 C3 H3A 109.7 . . ? N4 C3 H3B 109.7 . . ? C2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N4 C5 C6 111.40(15) . . ? N4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N1 C6 C5 110.13(15) . . ? N1 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N1 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N11 C7 C31 112.02(14) . . ? N11 C7 H7A 109.2 . . ? C31 C7 H7A 109.2 . . ? N11 C7 H7B 109.2 . . ? C31 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N21 C8 C41 113.63(15) . . ? N21 C8 H8A 108.8 . . ? C41 C8 H8A 108.8 . . ? N21 C8 H8B 108.8 . . ? C41 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C13 C12 N11 121.91(18) . . ? C13 C12 H12 119.0 . . ? N11 C12 H12 119.0 . . ? C12 C13 C14 120.63(17) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? N1 C14 C15 122.32(17) . . ? N1 C14 C13 121.61(16) . . ? C15 C14 C13 116.05(16) . . ? C16 C15 C14 120.15(17) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? N11 C16 C15 122.06(17) . . ? N11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C23 C22 N21 122.55(17) . . ? C23 C22 H22 118.7 . . ? N21 C22 H22 118.7 . . ? C22 C23 C24 120.46(17) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? N4 C24 C25 121.32(16) . . ? N4 C24 C23 123.21(17) . . ? C25 C24 C23 115.46(17) . . ? C26 C25 C24 120.49(17) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 N21 122.50(17) . . ? C25 C26 H26 118.7 . . ? N21 C26 H26 118.7 . . ? C36 C31 C32 118.97(17) . . ? C36 C31 C7 121.06(17) . . ? C32 C31 C7 119.96(16) . . ? C33 C32 C31 120.29(18) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 120.27(18) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 119.57(18) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.27(18) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 120.63(18) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C46 C41 C42 119.27(18) . . ? C46 C41 C8 121.83(17) . . ? C42 C41 C8 118.83(18) . . ? C43 C42 C41 120.31(19) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 120.02(19) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.01(19) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 119.96(19) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 120.36(19) . . ? C41 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? N51 C51 S51 178.96(18) . . ? N52 C52 S52 177.41(17) 4_566 . ? N53 C53 S53 178.72(17) . . ? N56 C54 S54 177.32(17) 4_575 . ? N55 C55 S55 179.11(18) 4_565 . ? N54 C56 S56 177.53(17) 4_576 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.313 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.055 #Hybrid 4 data_ic10629 _database_code_depnum_ccdc_archive 'CCDC 628691' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 N6 O2 S2' _chemical_formula_weight 574.75 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 41.0460(8) _cell_length_b 4.5649(5) _cell_length_c 7.978(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.000(2) _cell_angle_gamma 90.00 _cell_volume 1494.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 15158 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5152 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 24.94 _reflns_number_total 1339 _reflns_number_gt 940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV)' _computing_cell_refinement 'HKL Denzo & Scalepack (Otwinowski & Minor)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinowski & Minor)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.1114P)^2^+0.4535P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.45(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1339 _refine_ls_number_parameters 107 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2333 _refine_ls_wR_factor_gt 0.2074 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.002 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 N1 N 0.03380(8) 0.4338(9) 0.5000 0.0882(13) Uani 1 2 d S . . N2 N 0.12047(7) -0.0353(7) 0.5000 0.0691(10) Uani 1 2 d S . . C1 C 0.01753(7) 0.5395(9) 0.6516(6) 0.0999(13) Uani 1 1 d . . . H1A H 0.0197 0.7507 0.6584 0.120 Uiso 1 1 calc R . . H1B H 0.0280 0.4549 0.7493 0.120 Uiso 1 1 calc R . . C2 C 0.06252(8) 0.2909(9) 0.5000 0.0747(13) Uani 1 2 d S . . C3 C 0.07845(7) 0.2069(8) 0.6489(5) 0.0915(12) Uani 1 1 d . . . H3A H 0.0697 0.2612 0.7520 0.110 Uiso 1 1 calc R . . C4 C 0.10645(7) 0.0471(8) 0.6434(5) 0.0870(11) Uani 1 1 d . . . H4A H 0.1162 -0.0070 0.7440 0.104 Uiso 1 1 calc R . . C5 C 0.15175(9) -0.2024(9) 0.5000 0.0768(13) Uani 1 2 d S . . H5A H 0.1527 -0.3254 0.4025 0.092 Uiso 0.50 1 d PR . . C6 C 0.18033(9) 0.0041(8) 0.5000 0.0667(11) Uani 1 2 d S . . C7 C 0.19320(7) 0.1022(7) 0.6494(4) 0.0783(10) Uani 1 1 d . . . H7A H 0.1845 0.0372 0.7505 0.094 Uiso 1 1 calc R . . C8 C 0.21893(8) 0.2970(8) 0.6490(5) 0.0913(11) Uani 1 1 d . . . H8A H 0.2276 0.3644 0.7496 0.110 Uiso 1 1 calc R . . C9 C 0.23161(11) 0.3898(12) 0.5000 0.0926(16) Uani 1 2 d S . . H9A H 0.2492 0.5186 0.5000 0.111 Uiso 2.00 2 calc SPR . . S1 S 0.14616(4) -0.4596(4) 1.0000 0.1098(9) Uani 1 2 d S . . N3 N 0.07952(14) -0.3434(16) 1.0000 0.134(2) Uani 1 2 d S . . C10 C 0.10781(15) -0.3925(13) 1.0000 0.0957(16) Uani 1 2 d S . . O1 O 0.03170(10) 0.0964(13) 1.0000 0.1358(17) Uani 1 2 d SD . . H1 H 0.0264 0.0275 1.0830 0.204 Uiso 1 1 d RD . . 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 N1 0.060(2) 0.088(3) 0.116(3) 0.000 0.000 0.0129(17) N2 0.0623(19) 0.0558(19) 0.089(2) 0.000 0.000 0.0020(14) C1 0.0680(18) 0.097(2) 0.135(3) -0.013(2) -0.0038(17) 0.0209(16) C2 0.0508(19) 0.064(2) 0.110(3) 0.000 0.000 -0.0026(17) C3 0.0683(17) 0.106(3) 0.101(2) 0.001(2) 0.0084(15) 0.0156(16) C4 0.0697(17) 0.098(2) 0.093(2) 0.0130(18) 0.0042(15) 0.0135(15) C5 0.067(2) 0.055(2) 0.108(3) 0.000 0.000 0.0097(17) C6 0.065(2) 0.058(2) 0.078(2) 0.000 0.000 0.0157(17) C7 0.0784(18) 0.0759(19) 0.0805(19) 0.0075(15) -0.0053(14) 0.0088(15) C8 0.090(2) 0.084(2) 0.100(3) -0.0058(19) -0.0214(18) 0.0041(17) C9 0.073(3) 0.076(3) 0.128(5) 0.000 0.000 -0.007(2) S1 0.1197(13) 0.1136(14) 0.0962(12) 0.000 0.000 0.0189(8) N3 0.120(4) 0.193(6) 0.091(3) 0.000 0.000 0.020(4) C10 0.128(4) 0.104(4) 0.055(2) 0.000 0.000 0.007(3) O1 0.124(3) 0.178(4) 0.105(3) 0.000 0.000 0.020(3) _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 N1 C2 1.347(5) . ? N1 C1 1.463(4) 6_556 ? N1 C1 1.463(4) . ? N2 C4 1.335(4) . ? N2 C4 1.335(4) 6_556 ? N2 C5 1.493(5) . ? C1 C1 1.483(6) 2_565 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.409(4) . ? C2 C3 1.409(4) 6_556 ? C3 C4 1.362(4) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.505(6) . ? C5 H5A 0.9600 . ? C6 C7 1.379(4) 6_556 ? C6 C7 1.379(4) . ? C7 C8 1.381(5) . ? C7 H7A 0.9300 . ? C8 C9 1.365(4) . ? C8 H8A 0.9300 . ? C9 C8 1.365(4) 6_556 ? C9 H9A 0.9300 . ? S1 C10 1.604(6) . ? N3 C10 1.183(7) . ? O1 H1 0.7647 . ? 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 C2 N1 C1 123.99(17) . 6_556 ? C2 N1 C1 123.99(17) . . ? C1 N1 C1 111.5(4) 6_556 . ? C4 N2 C4 118.0(3) . 6_556 ? C4 N2 C5 120.96(17) . . ? C4 N2 C5 120.97(17) 6_556 . ? N1 C1 C1 111.3(3) . 2_565 ? N1 C1 H1A 109.4 . . ? C1 C1 H1A 109.4 2_565 . ? N1 C1 H1B 109.4 . . ? C1 C1 H1B 109.4 2_565 . ? H1A C1 H1B 108.0 . . ? N1 C2 C3 122.52(18) . . ? N1 C2 C3 122.52(18) . 6_556 ? C3 C2 C3 114.9(4) . 6_556 ? C4 C3 C2 120.7(3) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? N2 C4 C3 122.8(3) . . ? N2 C4 H4A 118.6 . . ? C3 C4 H4A 118.6 . . ? N2 C5 C6 110.5(3) . . ? N2 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C7 C6 C7 119.7(4) 6_556 . ? C7 C6 C5 120.14(19) 6_556 . ? C7 C6 C5 120.15(19) . . ? C6 C7 C8 120.0(3) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C8 C9 C8 121.1(5) 6_556 . ? C8 C9 H9A 119.4 6_556 . ? C8 C9 H9A 119.4 . . ? N3 C10 S1 179.9(6) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.249 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.033