Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Lisa Berreau' 'Atta M. Arif' 'Brian Bennett' 'Amy L. Fuller' 'Makowska-Grzyska,Magdalena M.' 'Kyle J. Tubbs' _publ_contact_author_name 'Prof Lisa Berreau' _publ_contact_author_address ; Department of Chemistry and Biochemistry Utah State University 0300 Old Main Hill Logan UT 84322-0300 UNITED STATES OF AMERICA ; _publ_contact_author_email BERREAU@CC.USU.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Copper(II) Complexes of N3S(thioether) Ligands having Internal Hydrogen Bond Donors ; data_usu049 _database_code_CSD 209457 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [(pbnpa)Cu-Cl]ClO4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H43 Cl2 Cu N5 O4 S' _chemical_formula_weight 704.19 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.0077(2) _cell_length_b 14.5441(2) _cell_length_c 20.7276(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.4909(7) _cell_angle_gamma 90.00 _cell_volume 3290.11(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(1) _cell_measurement_reflns_used 7171 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour 'dark green-blue' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7803 _exptl_absorpt_correction_T_max 0.8355 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 200(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi plus Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 2.0' _diffrn_reflns_number 13782 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7509 _reflns_number_gt 4990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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^)+(0.0531P)^2^+1.3786P] 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 7509 _refine_ls_number_parameters 572 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _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 Cu1 Cu 0.40868(3) 0.20638(2) 0.518811(16) 0.02714(11) Uani 1 1 d . . . Cl1 Cl 0.23828(7) 0.14444(5) 0.55055(4) 0.03363(18) Uani 1 1 d . . . Cl2 Cl 0.81285(8) 0.33850(6) 0.29672(5) 0.0524(2) Uani 1 1 d . . . S1 S 0.40892(7) 0.36273(5) 0.45219(4) 0.03314(18) Uani 1 1 d . . . O1 O 0.7890(4) 0.3380(4) 0.3612(2) 0.1373(17) Uani 1 1 d . A . O2 O 0.7518(6) 0.4132(4) 0.2732(2) 0.124(3) Uani 0.805(7) 1 d PD A 1 O3 O 0.9368(4) 0.3338(5) 0.3004(3) 0.138(3) Uani 0.805(7) 1 d PD A 1 O4 O 0.7477(9) 0.2490(7) 0.2962(5) 0.105(3) Uiso 0.403(3) 1 d PD A 1 O4A O 0.7680(11) 0.2747(8) 0.2493(6) 0.107(3) Uiso 0.403(3) 1 d P A 2 O2' O 0.8666(16) 0.4338(10) 0.2754(8) 0.070(5) Uiso 0.195(7) 1 d PD A 2 O3' O 0.8632(17) 0.2741(10) 0.2542(8) 0.070(5) Uiso 0.195(7) 1 d PD A 2 O4' O 0.7028(15) 0.3415(13) 0.2384(9) 0.086(6) Uiso 0.195(7) 1 d PD A 2 N1 N 0.4513(2) 0.29395(16) 0.59433(11) 0.0293(5) Uani 1 1 d . . . N2 N 0.2568(2) 0.35244(19) 0.59572(14) 0.0390(7) Uani 1 1 d . . . N3 N 0.5945(2) 0.20520(15) 0.51952(12) 0.0295(5) Uani 1 1 d . . . N4 N 0.4128(2) 0.12300(15) 0.44155(11) 0.0276(5) Uani 1 1 d . . . N5 N 0.2110(2) 0.13950(17) 0.39574(13) 0.0319(6) Uani 1 1 d . . . C1 C 0.3777(3) 0.34265(18) 0.36707(14) 0.0298(6) Uani 1 1 d . . . C2 C 0.2559(3) 0.3487(2) 0.34077(17) 0.0361(7) Uani 1 1 d . . . C3 C 0.2215(4) 0.3351(2) 0.27524(18) 0.0440(8) Uani 1 1 d . . . C4 C 0.3097(4) 0.3151(2) 0.23528(18) 0.0472(9) Uani 1 1 d . . . C5 C 0.4303(4) 0.3083(2) 0.26097(17) 0.0440(8) Uani 1 1 d . . . C6 C 0.4662(3) 0.3223(2) 0.32678(15) 0.0356(7) Uani 1 1 d . . . C7 C 0.5745(3) 0.3658(2) 0.47026(17) 0.0359(7) Uani 1 1 d . . . C8 C 0.6386(3) 0.2723(2) 0.47336(17) 0.0358(7) Uani 1 1 d . . . C9 C 0.6449(3) 0.2214(2) 0.58801(16) 0.0367(7) Uani 1 1 d . . . C10 C 0.5738(3) 0.2968(2) 0.61602(14) 0.0315(6) Uani 1 1 d . . . C11 C 0.6251(3) 0.3617(2) 0.65849(16) 0.0384(8) Uani 1 1 d . . . C12 C 0.5499(3) 0.4295(2) 0.67877(17) 0.0440(8) Uani 1 1 d . . . C13 C 0.4275(3) 0.4294(2) 0.65834(16) 0.0396(8) Uani 1 1 d . . . C14 C 0.3766(3) 0.3591(2) 0.61619(14) 0.0317(7) Uani 1 1 d . . . C15 C 0.1635(4) 0.4171(3) 0.6123(3) 0.0582(11) Uani 1 1 d . . . C16 C 0.0346(3) 0.3793(2) 0.59761(18) 0.0432(8) Uani 1 1 d . . . C17 C 0.0060(6) 0.3513(6) 0.5266(3) 0.0898(19) Uani 1 1 d . . . C18 C -0.0530(5) 0.4559(4) 0.6121(3) 0.0693(13) Uani 1 1 d . . . C19 C 0.0196(4) 0.2980(3) 0.6421(3) 0.0753(15) Uani 1 1 d . . . C20 C 0.6189(3) 0.1107(2) 0.49713(17) 0.0350(7) Uani 1 1 d . . . C21 C 0.5271(3) 0.0879(2) 0.43888(15) 0.0321(7) Uani 1 1 d . . . C22 C 0.5558(3) 0.0345(2) 0.38851(17) 0.0410(8) Uani 1 1 d . . . C23 C 0.4626(3) 0.0134(2) 0.33938(17) 0.0438(8) Uani 1 1 d . . . C24 C 0.3478(3) 0.0468(2) 0.34053(16) 0.0383(7) Uani 1 1 d . . . C25 C 0.3222(3) 0.10334(18) 0.39243(14) 0.0289(6) Uani 1 1 d . . . C26 C 0.1009(3) 0.1263(2) 0.34837(16) 0.0354(7) Uani 1 1 d . . . C27 C 0.0080(3) 0.0571(2) 0.36884(15) 0.0352(7) Uani 1 1 d . . . C28 C -0.0491(4) 0.0945(3) 0.42677(19) 0.0465(9) Uani 1 1 d . . . C29 C -0.0922(4) 0.0451(3) 0.3113(2) 0.0550(10) Uani 1 1 d . . . C30 C 0.0688(4) -0.0352(3) 0.3869(3) 0.0521(10) Uani 1 1 d . . . H2 H 0.201(3) 0.359(2) 0.3675(17) 0.046(10) Uiso 1 1 d . . . H2N H 0.234(3) 0.305(2) 0.5739(15) 0.031(9) Uiso 1 1 d . . . H3 H 0.146(3) 0.339(2) 0.2587(17) 0.048(11) Uiso 1 1 d . . . H4 H 0.288(4) 0.303(3) 0.196(2) 0.062(12) Uiso 1 1 d . . . H5 H 0.490(3) 0.295(2) 0.2340(16) 0.037(9) Uiso 1 1 d . . . H6 H 0.549(4) 0.320(3) 0.3408(19) 0.058(11) Uiso 1 1 d . . . H7A H 0.605(3) 0.400(2) 0.4364(17) 0.048(10) Uiso 1 1 d . . . H7B H 0.593(3) 0.396(2) 0.514(2) 0.058(11) Uiso 1 1 d . . . H7N H 0.204(3) 0.1633(19) 0.4290(15) 0.020(8) Uiso 1 1 d . . . H8A H 0.629(3) 0.248(2) 0.4322(15) 0.027(8) Uiso 1 1 d . . . H8B H 0.726(3) 0.2854(19) 0.4858(15) 0.034(8) Uiso 1 1 d . . . H9A H 0.723(3) 0.236(2) 0.5930(16) 0.042(9) Uiso 1 1 d . . . H9B H 0.642(3) 0.167(2) 0.6129(15) 0.031(8) Uiso 1 1 d . . . H11 H 0.703(3) 0.360(2) 0.6689(16) 0.041(10) Uiso 1 1 d . . . H12 H 0.586(3) 0.474(2) 0.7077(16) 0.039(9) Uiso 1 1 d . . . H13 H 0.379(3) 0.479(2) 0.6701(17) 0.052(10) Uiso 1 1 d . . . H15A H 0.182(4) 0.427(3) 0.662(2) 0.088(15) Uiso 1 1 d . . . H15B H 0.172(3) 0.473(3) 0.5882(19) 0.063(12) Uiso 1 1 d . . . H17A H 0.051(5) 0.401(4) 0.510(3) 0.11(2) Uiso 1 1 d . . . H17B H -0.088(7) 0.334(5) 0.512(3) 0.16(3) Uiso 1 1 d . . . H17C H 0.056(5) 0.294(3) 0.514(3) 0.109(18) Uiso 1 1 d . . . H18A H -0.128(4) 0.429(3) 0.6002(19) 0.057(12) Uiso 1 1 d . . . H18B H -0.033(5) 0.480(4) 0.658(3) 0.105(19) Uiso 1 1 d . . . H18C H -0.038(4) 0.509(3) 0.588(2) 0.079(14) Uiso 1 1 d . . . H19A H 0.024(6) 0.322(5) 0.701(4) 0.18(3) Uiso 1 1 d . . . H19B H -0.066(6) 0.277(4) 0.628(3) 0.13(2) Uiso 1 1 d . . . H19C H 0.070(4) 0.247(3) 0.634(2) 0.079(14) Uiso 1 1 d . . . H20A H 0.699(3) 0.105(2) 0.4845(16) 0.044(9) Uiso 1 1 d . . . H20B H 0.609(3) 0.071(2) 0.5327(15) 0.030(8) Uiso 1 1 d . . . H22 H 0.634(3) 0.011(2) 0.3894(15) 0.035(8) Uiso 1 1 d . . . H23 H 0.476(3) -0.022(2) 0.3071(17) 0.041(9) Uiso 1 1 d . . . H24 H 0.286(3) 0.034(2) 0.3103(17) 0.042(10) Uiso 1 1 d . . . H26A H 0.061(3) 0.183(2) 0.3413(14) 0.030(8) Uiso 1 1 d . . . H26B H 0.129(3) 0.107(2) 0.3050(17) 0.041(9) Uiso 1 1 d . . . H28A H -0.090(3) 0.150(2) 0.4157(17) 0.044(10) Uiso 1 1 d . . . H28B H -0.113(3) 0.049(2) 0.4378(17) 0.052(10) Uiso 1 1 d . . . H28C H 0.012(3) 0.107(2) 0.4622(19) 0.051(10) Uiso 1 1 d . . . H29A H -0.059(4) 0.021(3) 0.276(2) 0.070(13) Uiso 1 1 d . . . H29B H -0.129(3) 0.105(3) 0.2997(18) 0.055(11) Uiso 1 1 d . . . H29C H -0.154(4) -0.001(3) 0.3252(18) 0.062(11) Uiso 1 1 d . . . H30A H 0.104(3) -0.059(2) 0.3555(19) 0.050(11) Uiso 1 1 d . . . H30B H 0.008(3) -0.080(2) 0.4022(18) 0.055(10) Uiso 1 1 d . . . H30C H 0.133(3) -0.031(2) 0.4218(17) 0.040(10) Uiso 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 Cu1 0.02351(19) 0.0313(2) 0.0276(2) -0.00174(14) 0.00702(14) -0.00200(14) Cl1 0.0302(4) 0.0409(4) 0.0312(4) -0.0021(3) 0.0097(3) -0.0092(3) Cl2 0.0412(5) 0.0550(5) 0.0614(6) -0.0079(4) 0.0083(4) 0.0101(4) S1 0.0370(4) 0.0346(4) 0.0287(4) -0.0003(3) 0.0076(3) 0.0028(3) O1 0.108(3) 0.215(5) 0.095(3) 0.045(3) 0.037(3) -0.012(3) O2 0.166(6) 0.111(4) 0.093(4) 0.032(3) 0.013(3) 0.098(4) O3 0.038(3) 0.189(6) 0.191(6) 0.040(5) 0.037(3) 0.026(3) N1 0.0277(13) 0.0347(13) 0.0263(13) 0.0012(10) 0.0073(10) -0.0052(10) N2 0.0311(15) 0.0392(15) 0.0490(18) -0.0160(13) 0.0140(13) -0.0056(12) N3 0.0240(13) 0.0330(13) 0.0320(14) 0.0039(10) 0.0055(10) -0.0015(10) N4 0.0274(13) 0.0282(12) 0.0289(13) 0.0013(10) 0.0097(11) -0.0014(10) N5 0.0331(15) 0.0376(14) 0.0252(14) -0.0050(11) 0.0047(11) -0.0012(11) C1 0.0360(17) 0.0243(14) 0.0294(16) 0.0043(12) 0.0050(13) -0.0011(12) C2 0.0350(19) 0.0366(17) 0.0381(19) 0.0041(14) 0.0098(15) 0.0028(13) C3 0.042(2) 0.047(2) 0.041(2) 0.0083(16) -0.0023(17) 0.0006(16) C4 0.062(3) 0.051(2) 0.0272(19) -0.0016(15) 0.0017(18) -0.0023(17) C5 0.053(2) 0.047(2) 0.0335(19) 0.0002(15) 0.0127(17) 0.0038(16) C6 0.0368(19) 0.0413(18) 0.0302(17) 0.0026(13) 0.0103(14) 0.0017(14) C7 0.0389(19) 0.0356(17) 0.0336(18) 0.0015(14) 0.0061(15) -0.0082(13) C8 0.0271(17) 0.0432(18) 0.0382(19) 0.0072(15) 0.0082(14) -0.0043(13) C9 0.0257(18) 0.048(2) 0.0355(18) 0.0042(15) 0.0010(14) -0.0040(14) C10 0.0284(16) 0.0405(17) 0.0257(15) 0.0049(13) 0.0043(12) -0.0056(12) C11 0.0333(19) 0.051(2) 0.0305(17) 0.0010(14) 0.0030(15) -0.0129(15) C12 0.051(2) 0.049(2) 0.0331(18) -0.0087(15) 0.0078(16) -0.0188(16) C13 0.042(2) 0.0414(19) 0.0380(19) -0.0082(15) 0.0140(15) -0.0098(15) C14 0.0323(17) 0.0363(16) 0.0283(16) -0.0010(12) 0.0109(13) -0.0081(12) C15 0.041(2) 0.046(2) 0.092(4) -0.019(2) 0.026(2) -0.0013(16) C16 0.0317(18) 0.0463(19) 0.053(2) 0.0038(16) 0.0112(16) 0.0056(14) C17 0.068(4) 0.127(5) 0.067(3) -0.025(4) -0.017(3) 0.033(4) C18 0.051(3) 0.064(3) 0.099(4) 0.005(3) 0.030(3) 0.016(2) C19 0.047(3) 0.067(3) 0.118(5) 0.031(3) 0.033(3) 0.011(2) C20 0.0281(17) 0.0374(17) 0.0417(19) 0.0031(14) 0.0121(14) 0.0052(13) C21 0.0309(16) 0.0333(16) 0.0336(17) 0.0075(13) 0.0106(13) 0.0038(12) C22 0.044(2) 0.0385(18) 0.045(2) 0.0021(14) 0.0219(17) 0.0097(15) C23 0.059(2) 0.0415(19) 0.0347(19) -0.0087(15) 0.0204(17) 0.0017(16) C24 0.046(2) 0.0402(18) 0.0293(18) -0.0042(14) 0.0068(16) -0.0010(15) C25 0.0358(17) 0.0263(14) 0.0258(15) 0.0028(11) 0.0089(13) -0.0016(12) C26 0.0370(18) 0.0364(18) 0.0315(18) 0.0033(14) -0.0010(14) -0.0021(14) C27 0.0337(17) 0.0374(17) 0.0350(17) -0.0026(13) 0.0057(14) -0.0033(13) C28 0.038(2) 0.058(2) 0.044(2) -0.0071(18) 0.0103(18) -0.0030(18) C29 0.048(2) 0.064(3) 0.050(2) -0.011(2) -0.0024(19) -0.014(2) C30 0.054(3) 0.039(2) 0.068(3) 0.0043(19) 0.022(2) -0.0024(17) _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 Cu1 N4 2.014(2) . ? Cu1 N1 2.025(2) . ? Cu1 N3 2.043(2) . ? Cu1 Cl1 2.2548(8) . ? Cu1 S1 2.6605(8) . ? Cl2 O2 1.336(4) . ? Cl2 O3 1.358(4) . ? Cl2 O4A 1.395(11) . ? Cl2 O1 1.395(4) . ? Cl2 O3' 1.446(15) . ? Cl2 O4 1.485(10) . ? Cl2 O2' 1.592(15) . ? Cl2 O4' 1.597(18) . ? S1 C1 1.777(3) . ? S1 C7 1.813(3) . ? O4A O3' 1.040(16) . ? O4A O4' 1.213(18) . ? N1 C10 1.365(4) . ? N1 C14 1.370(4) . ? N2 C14 1.335(4) . ? N2 C15 1.466(4) . ? N2 H2N 0.84(3) . ? N3 C9 1.474(4) . ? N3 C20 1.486(4) . ? N3 C8 1.492(4) . ? N4 C25 1.360(4) . ? N4 C21 1.366(4) . ? N5 C25 1.342(4) . ? N5 C26 1.469(4) . ? N5 H7N 0.78(3) . ? C1 C2 1.383(4) . ? C1 C6 1.395(4) . ? C2 C3 1.376(5) . ? C2 H2 0.89(4) . ? C3 C4 1.388(5) . ? C3 H3 0.86(4) . ? C4 C5 1.368(5) . ? C4 H4 0.84(4) . ? C5 C6 1.385(5) . ? C5 H5 0.94(3) . ? C6 H6 0.92(4) . ? C7 C8 1.528(4) . ? C7 H7A 0.96(4) . ? C7 H7B 1.01(4) . ? C8 H8A 0.92(3) . ? C8 H8B 0.99(3) . ? C9 C10 1.507(4) . ? C9 H9A 0.88(3) . ? C9 H9B 0.95(3) . ? C10 C11 1.363(4) . ? C11 C12 1.387(5) . ? C11 H11 0.86(3) . ? C12 C13 1.358(5) . ? C12 H12 0.93(3) . ? C13 C14 1.413(4) . ? C13 H13 0.95(4) . ? C15 C16 1.515(5) . ? C15 H15A 1.03(5) . ? C15 H15B 0.97(4) . ? C16 C17 1.521(6) . ? C16 C19 1.521(5) . ? C16 C18 1.529(5) . ? C17 H17A 0.96(6) . ? C17 H17B 1.07(7) . ? C17 H17C 1.05(5) . ? C18 H18A 0.92(4) . ? C18 H18B 1.01(5) . ? C18 H18C 0.95(5) . ? C19 H19A 1.26(8) . ? C19 H19B 1.00(6) . ? C19 H19C 0.96(5) . ? C20 C21 1.507(5) . ? C20 H20A 0.95(3) . ? C20 H20B 0.95(3) . ? C21 C22 1.370(4) . ? C22 C23 1.382(5) . ? C22 H22 0.92(3) . ? C23 C24 1.357(5) . ? C23 H23 0.87(3) . ? C24 C25 1.411(4) . ? C24 H24 0.88(3) . ? C26 C27 1.533(4) . ? C26 H26A 0.94(3) . ? C26 H26B 1.03(3) . ? C27 C30 1.524(5) . ? C27 C29 1.525(5) . ? C27 C28 1.527(5) . ? C28 H28A 0.94(3) . ? C28 H28B 1.01(4) . ? C28 H28C 0.95(4) . ? C29 H29A 0.93(4) . ? C29 H29B 0.98(4) . ? C29 H29C 1.02(4) . ? C30 H30A 0.87(4) . ? C30 H30B 1.01(4) . ? C30 H30C 0.95(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 165.08(9) . . ? N4 Cu1 N3 82.78(9) . . ? N1 Cu1 N3 82.46(9) . . ? N4 Cu1 Cl1 95.59(7) . . ? N1 Cu1 Cl1 98.26(7) . . ? N3 Cu1 Cl1 149.82(7) . . ? N4 Cu1 S1 95.76(7) . . ? N1 Cu1 S1 81.25(7) . . ? N3 Cu1 S1 86.68(7) . . ? Cl1 Cu1 S1 123.37(3) . . ? O2 Cl2 O3 121.0(4) . . ? O2 Cl2 O4A 99.7(5) . . ? O3 Cl2 O4A 105.5(6) . . ? O2 Cl2 O1 101.8(3) . . ? O3 Cl2 O1 105.0(3) . . ? O4A Cl2 O1 125.3(5) . . ? O2 Cl2 O3' 121.3(7) . . ? O3 Cl2 O3' 62.6(7) . . ? O4A Cl2 O3' 42.9(7) . . ? O1 Cl2 O3' 135.7(7) . . ? O2 Cl2 O4 119.4(5) . . ? O3 Cl2 O4 115.9(5) . . ? O4A Cl2 O4 44.4(5) . . ? O1 Cl2 O4 81.5(5) . . ? O3' Cl2 O4 69.6(8) . . ? O2 Cl2 O2' 51.5(6) . . ? O3 Cl2 O2' 69.6(7) . . ? O4A Cl2 O2' 119.6(8) . . ? O1 Cl2 O2' 113.1(6) . . ? O3' Cl2 O2' 102.1(8) . . ? O4 Cl2 O2' 163.3(7) . . ? O2 Cl2 O4' 53.5(7) . . ? O3 Cl2 O4' 134.6(7) . . ? O4A Cl2 O4' 47.2(7) . . ? O1 Cl2 O4' 120.4(7) . . ? O3' Cl2 O4' 82.5(9) . . ? O4 Cl2 O4' 72.6(8) . . ? O2' Cl2 O4' 92.2(8) . . ? C1 S1 C7 105.54(15) . . ? C1 S1 Cu1 111.21(9) . . ? C7 S1 Cu1 89.00(11) . . ? O3' O4A O4' 126.1(16) . . ? O3' O4A Cl2 71.2(11) . . ? O4' O4A Cl2 75.2(11) . . ? O4A O3' Cl2 65.9(11) . . ? O4A O4' Cl2 57.6(9) . . ? C10 N1 C14 118.7(2) . . ? C10 N1 Cu1 113.15(19) . . ? C14 N1 Cu1 127.00(19) . . ? C14 N2 C15 124.9(3) . . ? C14 N2 H2N 116(2) . . ? C15 N2 H2N 119(2) . . ? C9 N3 C20 112.8(2) . . ? C9 N3 C8 113.6(2) . . ? C20 N3 C8 108.5(2) . . ? C9 N3 Cu1 104.88(18) . . ? C20 N3 Cu1 103.16(17) . . ? C8 N3 Cu1 113.52(18) . . ? C25 N4 C21 118.8(2) . . ? C25 N4 Cu1 129.15(19) . . ? C21 N4 Cu1 111.97(19) . . ? C25 N5 C26 126.3(3) . . ? C25 N5 H7N 115(2) . . ? C26 N5 H7N 118(2) . . ? C2 C1 C6 119.6(3) . . ? C2 C1 S1 115.6(2) . . ? C6 C1 S1 124.7(2) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 121(2) . . ? C1 C2 H2 118(2) . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3 121(2) . . ? C4 C3 H3 119(2) . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4 120(3) . . ? C3 C4 H4 119(3) . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5 120(2) . . ? C6 C5 H5 119(2) . . ? C5 C6 C1 119.3(3) . . ? C5 C6 H6 117(2) . . ? C1 C6 H6 124(2) . . ? C8 C7 S1 115.6(2) . . ? C8 C7 H7A 107(2) . . ? S1 C7 H7A 108(2) . . ? C8 C7 H7B 108(2) . . ? S1 C7 H7B 106(2) . . ? H7A C7 H7B 113(3) . . ? N3 C8 C7 115.0(3) . . ? N3 C8 H8A 109.6(19) . . ? C7 C8 H8A 108.2(19) . . ? N3 C8 H8B 110.4(18) . . ? C7 C8 H8B 105.7(17) . . ? H8A C8 H8B 108(3) . . ? N3 C9 C10 109.7(2) . . ? N3 C9 H9A 113(2) . . ? C10 C9 H9A 109(2) . . ? N3 C9 H9B 110.9(18) . . ? C10 C9 H9B 110.3(18) . . ? H9A C9 H9B 104(3) . . ? C11 C10 N1 122.8(3) . . ? C11 C10 C9 124.1(3) . . ? N1 C10 C9 113.0(3) . . ? C10 C11 C12 118.3(3) . . ? C10 C11 H11 117(2) . . ? C12 C11 H11 124(2) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 122(2) . . ? C11 C12 H12 118(2) . . ? C12 C13 C14 119.4(3) . . ? C12 C13 H13 119(2) . . ? C14 C13 H13 121(2) . . ? N2 C14 N1 117.1(3) . . ? N2 C14 C13 123.0(3) . . ? N1 C14 C13 119.9(3) . . ? N2 C15 C16 112.7(3) . . ? N2 C15 H15A 106(3) . . ? C16 C15 H15A 108(3) . . ? N2 C15 H15B 108(2) . . ? C16 C15 H15B 111(2) . . ? H15A C15 H15B 112(3) . . ? C15 C16 C17 111.3(4) . . ? C15 C16 C19 109.4(4) . . ? C17 C16 C19 110.7(5) . . ? C15 C16 C18 107.1(3) . . ? C17 C16 C18 109.2(4) . . ? C19 C16 C18 109.1(4) . . ? C16 C17 H17A 95(4) . . ? C16 C17 H17B 114(4) . . ? H17A C17 H17B 127(5) . . ? C16 C17 H17C 114(3) . . ? H17A C17 H17C 101(4) . . ? H17B C17 H17C 105(4) . . ? C16 C18 H18A 102(2) . . ? C16 C18 H18B 112(3) . . ? H18A C18 H18B 119(4) . . ? C16 C18 H18C 110(3) . . ? H18A C18 H18C 114(4) . . ? H18B C18 H18C 101(4) . . ? C16 C19 H19A 112(3) . . ? C16 C19 H19B 104(3) . . ? H19A C19 H19B 107(4) . . ? C16 C19 H19C 112(3) . . ? H19A C19 H19C 116(4) . . ? H19B C19 H19C 105(4) . . ? N3 C20 C21 108.9(2) . . ? N3 C20 H20A 113(2) . . ? C21 C20 H20A 108(2) . . ? N3 C20 H20B 105.7(18) . . ? C21 C20 H20B 110.7(18) . . ? H20A C20 H20B 111(3) . . ? N4 C21 C22 123.2(3) . . ? N4 C21 C20 114.2(3) . . ? C22 C21 C20 122.6(3) . . ? C21 C22 C23 117.7(3) . . ? C21 C22 H22 120(2) . . ? C23 C22 H22 122.2(19) . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23 118(2) . . ? C22 C23 H23 121(2) . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 123(2) . . ? C25 C24 H24 117(2) . . ? N5 C25 N4 117.7(3) . . ? N5 C25 C24 122.8(3) . . ? N4 C25 C24 119.5(3) . . ? N5 C26 C27 115.0(3) . . ? N5 C26 H26A 108.4(18) . . ? C27 C26 H26A 108.0(18) . . ? N5 C26 H26B 107.6(18) . . ? C27 C26 H26B 110.6(18) . . ? H26A C26 H26B 107(3) . . ? C30 C27 C29 109.9(3) . . ? C30 C27 C28 109.5(3) . . ? C29 C27 C28 109.0(3) . . ? C30 C27 C26 111.0(3) . . ? C29 C27 C26 107.4(3) . . ? C28 C27 C26 110.0(3) . . ? C27 C28 H28A 110(2) . . ? C27 C28 H28B 108(2) . . ? H28A C28 H28B 107(3) . . ? C27 C28 H28C 111(2) . . ? H28A C28 H28C 107(3) . . ? H28B C28 H28C 113(3) . . ? C27 C29 H29A 110(3) . . ? C27 C29 H29B 109(2) . . ? H29A C29 H29B 109(3) . . ? C27 C29 H29C 107(2) . . ? H29A C29 H29C 109(3) . . ? H29B C29 H29C 113(3) . . ? C27 C30 H30A 113(2) . . ? C27 C30 H30B 111(2) . . ? H30A C30 H30B 111(3) . . ? C27 C30 H30C 113(2) . . ? H30A C30 H30C 104(3) . . ? H30B C30 H30C 105(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 S1 C1 13.18(13) . . . . ? N1 Cu1 S1 C1 178.44(13) . . . . ? N3 Cu1 S1 C1 95.57(13) . . . . ? Cl1 Cu1 S1 C1 -87.40(11) . . . . ? N4 Cu1 S1 C7 -93.12(13) . . . . ? N1 Cu1 S1 C7 72.14(13) . . . . ? N3 Cu1 S1 C7 -10.73(13) . . . . ? Cl1 Cu1 S1 C7 166.30(11) . . . . ? O2 Cl2 O4A O3' 126.1(11) . . . . ? O3 Cl2 O4A O3' -0.1(12) . . . . ? O1 Cl2 O4A O3' -121.8(11) . . . . ? O4 Cl2 O4A O3' -111.4(14) . . . . ? O2' Cl2 O4A O3' 75.0(13) . . . . ? O4' Cl2 O4A O3' 137.3(16) . . . . ? O2 Cl2 O4A O4' -11.2(11) . . . . ? O3 Cl2 O4A O4' -137.3(10) . . . . ? O1 Cl2 O4A O4' 100.9(11) . . . . ? O3' Cl2 O4A O4' -137.3(16) . . . . ? O4 Cl2 O4A O4' 111.3(14) . . . . ? O2' Cl2 O4A O4' -62.3(13) . . . . ? O4' O4A O3' Cl2 54.3(18) . . . . ? O2 Cl2 O3' O4A -68.7(12) . . . . ? O3 Cl2 O3' O4A 179.9(13) . . . . ? O1 Cl2 O3' O4A 96.5(12) . . . . ? O4 Cl2 O3' O4A 44.0(9) . . . . ? O2' Cl2 O3' O4A -120.8(11) . . . . ? O4' Cl2 O3' O4A -30.1(11) . . . . ? O3' O4A O4' Cl2 -52.7(18) . . . . ? O2 Cl2 O4' O4A 166.2(14) . . . . ? O3 Cl2 O4' O4A 66.4(13) . . . . ? O1 Cl2 O4' O4A -111.7(10) . . . . ? O3' Cl2 O4' O4A 27.8(11) . . . . ? O4 Cl2 O4' O4A -43.1(9) . . . . ? O2' Cl2 O4' O4A 129.7(11) . . . . ? N4 Cu1 N1 C10 -19.3(5) . . . . ? N3 Cu1 N1 C10 -10.89(19) . . . . ? Cl1 Cu1 N1 C10 138.63(18) . . . . ? S1 Cu1 N1 C10 -98.68(18) . . . . ? N4 Cu1 N1 C14 148.1(3) . . . . ? N3 Cu1 N1 C14 156.5(2) . . . . ? Cl1 Cu1 N1 C14 -54.0(2) . . . . ? S1 Cu1 N1 C14 68.7(2) . . . . ? N4 Cu1 N3 C9 -152.32(19) . . . . ? N1 Cu1 N3 C9 29.84(18) . . . . ? Cl1 Cu1 N3 C9 -63.6(2) . . . . ? S1 Cu1 N3 C9 111.44(18) . . . . ? N4 Cu1 N3 C20 -34.07(18) . . . . ? N1 Cu1 N3 C20 148.10(19) . . . . ? Cl1 Cu1 N3 C20 54.6(3) . . . . ? S1 Cu1 N3 C20 -130.31(18) . . . . ? N4 Cu1 N3 C8 83.1(2) . . . . ? N1 Cu1 N3 C8 -94.7(2) . . . . ? Cl1 Cu1 N3 C8 171.83(16) . . . . ? S1 Cu1 N3 C8 -13.1(2) . . . . ? N1 Cu1 N4 C25 -150.8(3) . . . . ? N3 Cu1 N4 C25 -159.2(2) . . . . ? Cl1 Cu1 N4 C25 51.1(2) . . . . ? S1 Cu1 N4 C25 -73.3(2) . . . . ? N1 Cu1 N4 C21 24.9(5) . . . . ? N3 Cu1 N4 C21 16.49(18) . . . . ? Cl1 Cu1 N4 C21 -133.18(18) . . . . ? S1 Cu1 N4 C21 102.39(18) . . . . ? C7 S1 C1 C2 -172.5(2) . . . . ? Cu1 S1 C1 C2 92.5(2) . . . . ? C7 S1 C1 C6 7.2(3) . . . . ? Cu1 S1 C1 C6 -87.9(3) . . . . ? C6 C1 C2 C3 -0.2(4) . . . . ? S1 C1 C2 C3 179.5(2) . . . . ? C1 C2 C3 C4 0.1(5) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 C1 0.6(5) . . . . ? C2 C1 C6 C5 -0.2(5) . . . . ? S1 C1 C6 C5 -179.8(2) . . . . ? C1 S1 C7 C8 -77.2(3) . . . . ? Cu1 S1 C7 C8 34.5(2) . . . . ? C9 N3 C8 C7 -79.2(3) . . . . ? C20 N3 C8 C7 154.6(3) . . . . ? Cu1 N3 C8 C7 40.5(3) . . . . ? S1 C7 C8 N3 -55.0(4) . . . . ? C20 N3 C9 C10 -155.1(3) . . . . ? C8 N3 C9 C10 81.0(3) . . . . ? Cu1 N3 C9 C10 -43.5(3) . . . . ? C14 N1 C10 C11 -0.1(4) . . . . ? Cu1 N1 C10 C11 168.5(2) . . . . ? C14 N1 C10 C9 -179.9(3) . . . . ? Cu1 N1 C10 C9 -11.4(3) . . . . ? N3 C9 C10 C11 -142.2(3) . . . . ? N3 C9 C10 N1 37.6(3) . . . . ? N1 C10 C11 C12 -2.2(5) . . . . ? C9 C10 C11 C12 177.7(3) . . . . ? C10 C11 C12 C13 2.0(5) . . . . ? C11 C12 C13 C14 0.3(5) . . . . ? C15 N2 C14 N1 -178.1(3) . . . . ? C15 N2 C14 C13 1.6(5) . . . . ? C10 N1 C14 N2 -177.8(3) . . . . ? Cu1 N1 C14 N2 15.4(4) . . . . ? C10 N1 C14 C13 2.4(4) . . . . ? Cu1 N1 C14 C13 -164.3(2) . . . . ? C12 C13 C14 N2 177.7(3) . . . . ? C12 C13 C14 N1 -2.6(5) . . . . ? C14 N2 C15 C16 -164.6(3) . . . . ? N2 C15 C16 C17 -56.4(6) . . . . ? N2 C15 C16 C19 66.3(5) . . . . ? N2 C15 C16 C18 -175.6(4) . . . . ? C9 N3 C20 C21 158.3(3) . . . . ? C8 N3 C20 C21 -75.0(3) . . . . ? Cu1 N3 C20 C21 45.7(3) . . . . ? C25 N4 C21 C22 0.9(4) . . . . ? Cu1 N4 C21 C22 -175.3(2) . . . . ? C25 N4 C21 C20 -177.6(2) . . . . ? Cu1 N4 C21 C20 6.2(3) . . . . ? N3 C20 C21 N4 -36.1(3) . . . . ? N3 C20 C21 C22 145.4(3) . . . . ? N4 C21 C22 C23 -2.1(5) . . . . ? C20 C21 C22 C23 176.3(3) . . . . ? C21 C22 C23 C24 1.8(5) . . . . ? C22 C23 C24 C25 -0.4(5) . . . . ? C26 N5 C25 N4 -179.4(3) . . . . ? C26 N5 C25 C24 0.7(5) . . . . ? C21 N4 C25 N5 -179.2(2) . . . . ? Cu1 N4 C25 N5 -3.8(4) . . . . ? C21 N4 C25 C24 0.6(4) . . . . ? Cu1 N4 C25 C24 176.0(2) . . . . ? C23 C24 C25 N5 179.0(3) . . . . ? C23 C24 C25 N4 -0.9(5) . . . . ? C25 N5 C26 C27 102.0(4) . . . . ? N5 C26 C27 C30 -54.0(4) . . . . ? N5 C26 C27 C29 -174.2(3) . . . . ? N5 C26 C27 C28 67.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.637 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.071 #===END data_usu074 _database_code_CSD 209458 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [(ebnpa)Cu-Cl]ClO4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H43 Cl2 Cu N5 O4 S' _chemical_formula_weight 656.15 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 8.4860(1) _cell_length_b 13.8394(2) _cell_length_c 14.3749(3) _cell_angle_alpha 101.7717(6) _cell_angle_beta 91.7414(6) _cell_angle_gamma 106.5561(11) _cell_volume 1577.11(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 5435 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7736 _exptl_absorpt_correction_T_max 0.8686 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi plus Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11542 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7142 _reflns_number_gt 6125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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^)+(0.0171P)^2^+0.9894P] 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 7142 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Cu1 Cu 0.42160(2) 0.186418(15) 0.761642(15) 0.01733(7) Uani 1 1 d . . . Cl1 Cl 0.38876(5) 0.20102(3) 0.60803(3) 0.02470(10) Uani 1 1 d . . . Cl2 Cl 0.93120(5) 0.20935(4) 1.12689(4) 0.02891(11) Uani 1 1 d . . . S1 S 0.13631(5) 0.16890(4) 0.76649(3) 0.02293(11) Uani 1 1 d . . . O1 O 0.95314(18) 0.26645(11) 1.05277(11) 0.0345(3) Uani 1 1 d . . . O2 O 0.9667(2) 0.11349(15) 1.09456(18) 0.0721(7) Uani 1 1 d . . . O3 O 0.76489(19) 0.18788(12) 1.15082(14) 0.0471(4) Uani 1 1 d . . . O4 O 1.0432(3) 0.26829(19) 1.20768(16) 0.0962(10) Uani 1 1 d . . . N1 N 0.57228(17) 0.33787(11) 0.84049(10) 0.0176(3) Uani 1 1 d . . . N2 N 0.5622(2) 0.43319(13) 0.72707(12) 0.0253(3) Uani 1 1 d . . . N3 N 0.41600(17) 0.16139(11) 0.89651(11) 0.0183(3) Uani 1 1 d . . . N4 N 0.56056(17) 0.08243(11) 0.74844(11) 0.0189(3) Uani 1 1 d . . . N5 N 0.70398(19) 0.11947(12) 0.61826(12) 0.0232(3) Uani 1 1 d . . . C1 C -0.0222(3) 0.32109(19) 0.80755(17) 0.0332(5) Uani 1 1 d . . . C2 C 0.1445(2) 0.30430(15) 0.78897(16) 0.0263(4) Uani 1 1 d . . . C3 C 0.1135(2) 0.13996(16) 0.88356(15) 0.0268(4) Uani 1 1 d . . . C4 C 0.2746(2) 0.18569(16) 0.94601(14) 0.0240(4) Uani 1 1 d . . . C5 C 0.5744(2) 0.22725(14) 0.95102(14) 0.0209(4) Uani 1 1 d . . . C6 C 0.6259(2) 0.33312(13) 0.92841(13) 0.0187(3) Uani 1 1 d . . . C7 C 0.7313(2) 0.41554(15) 0.99255(14) 0.0233(4) Uani 1 1 d . . . C8 C 0.7898(2) 0.50847(15) 0.96304(15) 0.0251(4) Uani 1 1 d . . . C9 C 0.7380(2) 0.51660(14) 0.87474(14) 0.0241(4) Uani 1 1 d . . . C10 C 0.6246(2) 0.43016(13) 0.81375(13) 0.0187(3) Uani 1 1 d . . . C11 C 0.6202(3) 0.51756(15) 0.67782(15) 0.0263(4) Uani 1 1 d . . . C12 C 0.5115(3) 0.58975(15) 0.68126(15) 0.0296(4) Uani 1 1 d . . . C13 C 0.3355(3) 0.5287(2) 0.6388(2) 0.0501(7) Uani 1 1 d . . . C14 C 0.5884(4) 0.66775(19) 0.6214(2) 0.0414(6) Uani 1 1 d . . . C15 C 0.5091(3) 0.64748(19) 0.78354(18) 0.0396(5) Uani 1 1 d . . . C16 C 0.4039(2) 0.05047(14) 0.88226(15) 0.0238(4) Uani 1 1 d . . . C17 C 0.5303(2) 0.02683(13) 0.81726(14) 0.0220(4) Uani 1 1 d . . . C18 C 0.6068(2) -0.04565(14) 0.82831(15) 0.0267(4) Uani 1 1 d . . . C19 C 0.7200(2) -0.06485(15) 0.76418(16) 0.0284(4) Uani 1 1 d . . . C20 C 0.7514(2) -0.01152(14) 0.69356(15) 0.0256(4) Uani 1 1 d . . . C21 C 0.6710(2) 0.06351(13) 0.68574(13) 0.0202(4) Uani 1 1 d . . . C22 C 0.8164(2) 0.10129(16) 0.54608(15) 0.0267(4) Uani 1 1 d . . . C23 C 0.8377(2) 0.17285(16) 0.47620(14) 0.0267(4) Uani 1 1 d . . . C24 C 0.8985(4) 0.2856(2) 0.5283(2) 0.0546(7) Uani 1 1 d . . . C25 C 0.6766(3) 0.1512(3) 0.41519(18) 0.0473(7) Uani 1 1 d . . . C26 C 0.9652(3) 0.1462(3) 0.4105(2) 0.0465(6) Uani 1 1 d . . . H1A H -0.062(3) 0.2990(18) 0.8682(18) 0.039(6) Uiso 1 1 d . . . H1B H -0.099(3) 0.2858(19) 0.7547(18) 0.040(7) Uiso 1 1 d . . . H1C H -0.007(3) 0.393(2) 0.8156(17) 0.039(7) Uiso 1 1 d . . . H2 H 0.511(3) 0.3787(18) 0.6938(16) 0.026(6) Uiso 1 1 d . . . H2A H 0.185(3) 0.3251(17) 0.7351(17) 0.031(6) Uiso 1 1 d . . . H2B H 0.227(3) 0.3442(16) 0.8425(15) 0.023(5) Uiso 1 1 d . . . H3A H 0.028(3) 0.1663(17) 0.9107(16) 0.034(6) Uiso 1 1 d . . . H3B H 0.076(3) 0.0653(19) 0.8718(16) 0.035(6) Uiso 1 1 d . . . H4A H 0.300(2) 0.2608(16) 0.9635(14) 0.021(5) Uiso 1 1 d . . . H4B H 0.270(3) 0.1612(17) 1.0050(16) 0.030(6) Uiso 1 1 d . . . H5 H 0.638(3) 0.1486(16) 0.6077(15) 0.022(5) Uiso 1 1 d . . . H5A H 0.654(2) 0.1934(15) 0.9324(14) 0.022(5) Uiso 1 1 d . . . H5B H 0.566(3) 0.2341(16) 1.0180(16) 0.028(6) Uiso 1 1 d . . . H7 H 0.765(2) 0.4081(15) 1.0472(16) 0.021(5) Uiso 1 1 d . . . H8 H 0.865(3) 0.5643(17) 1.0021(16) 0.028(5) Uiso 1 1 d . . . H9 H 0.773(3) 0.5767(17) 0.8522(15) 0.027(5) Uiso 1 1 d . . . H11A H 0.733(3) 0.5597(16) 0.7025(15) 0.024(5) Uiso 1 1 d . . . H11B H 0.625(3) 0.4885(16) 0.6140(17) 0.027(5) Uiso 1 1 d . . . H13A H 0.336(4) 0.486(2) 0.573(2) 0.066(9) Uiso 1 1 d . . . H13B H 0.282(3) 0.477(2) 0.676(2) 0.059(8) Uiso 1 1 d . . . H13C H 0.267(3) 0.575(2) 0.637(2) 0.060(8) Uiso 1 1 d . . . H14A H 0.590(3) 0.638(2) 0.556(2) 0.053(8) Uiso 1 1 d . . . H14B H 0.704(3) 0.706(2) 0.6454(19) 0.052(8) Uiso 1 1 d . . . H14C H 0.531(3) 0.720(2) 0.622(2) 0.059(8) Uiso 1 1 d . . . H15A H 0.469(3) 0.599(2) 0.8229(18) 0.044(7) Uiso 1 1 d . . . H15B H 0.621(3) 0.692(2) 0.8106(19) 0.049(7) Uiso 1 1 d . . . H15C H 0.440(3) 0.693(2) 0.7853(19) 0.055(8) Uiso 1 1 d . . . H16A H 0.422(2) 0.0324(16) 0.9442(16) 0.025(5) Uiso 1 1 d . . . H16B H 0.297(3) 0.0111(17) 0.8536(16) 0.029(6) Uiso 1 1 d . . . H18 H 0.579(2) -0.0808(16) 0.8751(15) 0.024(5) Uiso 1 1 d . . . H19 H 0.773(3) -0.1133(17) 0.7673(16) 0.030(6) Uiso 1 1 d . . . H20 H 0.825(3) -0.0235(16) 0.6500(15) 0.025(5) Uiso 1 1 d . . . H22A H 0.924(3) 0.1119(16) 0.5799(16) 0.030(6) Uiso 1 1 d . . . H22B H 0.778(3) 0.0302(18) 0.5087(16) 0.033(6) Uiso 1 1 d . . . H24A H 1.011(4) 0.297(2) 0.567(2) 0.071(9) Uiso 1 1 d . . . H24B H 0.826(4) 0.307(2) 0.569(2) 0.063(9) Uiso 1 1 d . . . H24C H 0.927(4) 0.333(2) 0.483(2) 0.075(9) Uiso 1 1 d . . . H25A H 0.634(4) 0.078(3) 0.388(3) 0.088(12) Uiso 1 1 d . . . H25B H 0.592(3) 0.167(2) 0.453(2) 0.054(8) Uiso 1 1 d . . . H25C H 0.689(3) 0.190(2) 0.368(2) 0.054(8) Uiso 1 1 d . . . H26A H 0.924(4) 0.069(3) 0.377(2) 0.069(9) Uiso 1 1 d . . . H26B H 1.073(4) 0.161(2) 0.447(2) 0.073(9) Uiso 1 1 d . . . H26C H 0.977(3) 0.185(2) 0.365(2) 0.061(9) Uiso 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 Cu1 0.01870(11) 0.01668(12) 0.01815(12) 0.00601(8) 0.00386(8) 0.00594(8) Cl1 0.0292(2) 0.0270(2) 0.0205(2) 0.00640(18) 0.00389(17) 0.01157(18) Cl2 0.0223(2) 0.0284(2) 0.0371(3) 0.0189(2) 0.00176(18) 0.00122(17) S1 0.0171(2) 0.0256(2) 0.0246(2) 0.00570(19) 0.00223(17) 0.00397(17) O1 0.0436(8) 0.0284(8) 0.0343(8) 0.0180(6) 0.0038(6) 0.0075(6) O2 0.0668(13) 0.0512(11) 0.133(2) 0.0599(13) 0.0583(13) 0.0398(10) O3 0.0339(8) 0.0413(9) 0.0730(12) 0.0231(9) 0.0254(8) 0.0129(7) O4 0.0882(16) 0.1004(18) 0.0595(14) 0.0503(13) -0.0423(12) -0.0532(13) N1 0.0185(7) 0.0153(7) 0.0194(8) 0.0054(6) 0.0031(6) 0.0047(5) N2 0.0350(9) 0.0145(8) 0.0236(9) 0.0070(7) -0.0036(7) 0.0016(7) N3 0.0193(7) 0.0155(7) 0.0218(8) 0.0069(6) 0.0051(6) 0.0054(5) N4 0.0204(7) 0.0149(7) 0.0219(8) 0.0051(6) 0.0040(6) 0.0052(5) N5 0.0227(8) 0.0238(8) 0.0279(9) 0.0087(7) 0.0087(6) 0.0115(6) C1 0.0247(10) 0.0415(13) 0.0343(13) 0.0016(10) 0.0002(9) 0.0160(9) C2 0.0222(9) 0.0295(11) 0.0302(11) 0.0090(9) 0.0045(8) 0.0106(8) C3 0.0209(9) 0.0303(11) 0.0313(11) 0.0132(9) 0.0095(8) 0.0056(8) C4 0.0255(9) 0.0279(11) 0.0216(10) 0.0091(8) 0.0083(7) 0.0093(8) C5 0.0232(9) 0.0200(9) 0.0203(10) 0.0068(7) 0.0004(7) 0.0061(7) C6 0.0168(8) 0.0206(9) 0.0206(9) 0.0068(7) 0.0041(7) 0.0070(6) C7 0.0246(9) 0.0251(10) 0.0195(10) 0.0049(8) -0.0008(7) 0.0068(7) C8 0.0223(9) 0.0184(9) 0.0293(11) 0.0004(8) -0.0010(8) 0.0017(7) C9 0.0229(9) 0.0169(9) 0.0306(11) 0.0060(8) 0.0018(7) 0.0024(7) C10 0.0189(8) 0.0169(9) 0.0221(9) 0.0062(7) 0.0039(7) 0.0066(6) C11 0.0372(11) 0.0213(10) 0.0217(10) 0.0101(8) 0.0048(8) 0.0068(8) C12 0.0361(11) 0.0232(10) 0.0319(11) 0.0133(8) 0.0005(8) 0.0078(8) C13 0.0419(14) 0.0416(15) 0.068(2) 0.0234(14) -0.0115(13) 0.0082(11) C14 0.0604(16) 0.0282(12) 0.0402(15) 0.0200(11) 0.0038(12) 0.0118(11) C15 0.0518(15) 0.0335(13) 0.0423(14) 0.0130(11) 0.0116(11) 0.0226(11) C16 0.0266(10) 0.0186(9) 0.0285(11) 0.0118(8) 0.0068(8) 0.0055(7) C17 0.0234(9) 0.0149(8) 0.0271(10) 0.0065(7) 0.0025(7) 0.0035(7) C18 0.0301(10) 0.0184(9) 0.0339(11) 0.0119(8) 0.0016(8) 0.0067(7) C19 0.0253(10) 0.0175(9) 0.0436(13) 0.0071(9) -0.0011(8) 0.0084(7) C20 0.0206(9) 0.0200(9) 0.0368(12) 0.0049(8) 0.0059(8) 0.0074(7) C21 0.0174(8) 0.0147(8) 0.0258(10) 0.0018(7) 0.0028(7) 0.0024(6) C22 0.0241(10) 0.0317(11) 0.0261(10) 0.0056(8) 0.0073(8) 0.0113(8) C23 0.0228(9) 0.0366(11) 0.0205(10) 0.0066(8) 0.0027(7) 0.0084(8) C24 0.078(2) 0.0355(14) 0.0425(16) 0.0143(12) 0.0135(15) -0.0006(13) C25 0.0330(12) 0.089(2) 0.0277(13) 0.0171(14) 0.0030(10) 0.0270(13) C26 0.0361(13) 0.077(2) 0.0376(14) 0.0235(14) 0.0163(11) 0.0255(13) _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 Cu1 N3 2.0374(15) . ? Cu1 N4 2.0897(14) . ? Cu1 N1 2.1744(14) . ? Cu1 Cl1 2.2740(5) . ? Cu1 S1 2.3681(5) . ? Cl2 O4 1.422(2) . ? Cl2 O3 1.4250(15) . ? Cl2 O2 1.4323(18) . ? Cl2 O1 1.4373(14) . ? S1 C3 1.811(2) . ? S1 C2 1.816(2) . ? N1 C6 1.351(2) . ? N1 C10 1.365(2) . ? N2 C10 1.353(2) . ? N2 C11 1.462(2) . ? N2 H2 0.80(2) . ? N3 C16 1.480(2) . ? N3 C5 1.483(2) . ? N3 C4 1.498(2) . ? N4 C17 1.360(2) . ? N4 C21 1.361(2) . ? N5 C21 1.349(2) . ? N5 C22 1.463(2) . ? N5 H5 0.80(2) . ? C1 C2 1.520(3) . ? C1 H1A 1.02(2) . ? C1 H1B 0.94(3) . ? C1 H1C 0.94(3) . ? C2 H2A 0.92(2) . ? C2 H2B 0.98(2) . ? C3 C4 1.508(3) . ? C3 H3A 0.96(2) . ? C3 H3B 0.97(2) . ? C4 H4A 0.98(2) . ? C4 H4B 0.97(2) . ? C5 C6 1.510(2) . ? C5 H5A 0.94(2) . ? C5 H5B 0.95(2) . ? C6 C7 1.375(3) . ? C7 C8 1.397(3) . ? C7 H7 0.86(2) . ? C8 C9 1.367(3) . ? C8 H8 0.92(2) . ? C9 C10 1.411(3) . ? C9 H9 0.93(2) . ? C11 C12 1.536(3) . ? C11 H11A 0.98(2) . ? C11 H11B 0.93(2) . ? C12 C13 1.527(3) . ? C12 C15 1.527(3) . ? C12 C14 1.531(3) . ? C13 H13A 1.00(3) . ? C13 H13B 0.99(3) . ? C13 H13C 0.98(3) . ? C14 H14A 0.94(3) . ? C14 H14B 0.98(3) . ? C14 H14C 0.98(3) . ? C15 H15A 0.96(3) . ? C15 H15B 0.99(3) . ? C15 H15C 0.97(3) . ? C16 C17 1.506(3) . ? C16 H16A 0.99(2) . ? C16 H16B 0.95(2) . ? C17 C18 1.372(3) . ? C18 C19 1.394(3) . ? C18 H18 0.91(2) . ? C19 C20 1.362(3) . ? C19 H19 0.92(2) . ? C20 C21 1.415(2) . ? C20 H20 0.92(2) . ? C22 C23 1.529(3) . ? C22 H22A 0.98(2) . ? C22 H22B 0.98(2) . ? C23 C24 1.518(3) . ? C23 C25 1.522(3) . ? C23 C26 1.531(3) . ? C24 H24A 1.04(3) . ? C24 H24B 0.93(3) . ? C24 H24C 1.01(3) . ? C25 H25A 0.97(4) . ? C25 H25B 0.96(3) . ? C25 H25C 0.94(3) . ? C26 H26A 1.03(3) . ? C26 H26B 0.99(3) . ? C26 H26C 0.92(3) . ? 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 Cu1 N4 81.12(6) . . ? N3 Cu1 N1 80.35(6) . . ? N4 Cu1 N1 109.59(6) . . ? N3 Cu1 Cl1 171.75(4) . . ? N4 Cu1 Cl1 101.48(4) . . ? N1 Cu1 Cl1 105.84(4) . . ? N3 Cu1 S1 86.01(4) . . ? N4 Cu1 S1 133.97(4) . . ? N1 Cu1 S1 111.45(4) . . ? Cl1 Cu1 S1 86.614(17) . . ? O4 Cl2 O3 110.88(14) . . ? O4 Cl2 O2 108.67(17) . . ? O3 Cl2 O2 108.77(10) . . ? O4 Cl2 O1 108.81(10) . . ? O3 Cl2 O1 109.93(10) . . ? O2 Cl2 O1 109.75(11) . . ? C3 S1 C2 102.78(10) . . ? C3 S1 Cu1 98.13(6) . . ? C2 S1 Cu1 99.50(6) . . ? C6 N1 C10 118.19(15) . . ? C6 N1 Cu1 110.71(11) . . ? C10 N1 Cu1 131.00(12) . . ? C10 N2 C11 125.59(16) . . ? C10 N2 H2 116.0(16) . . ? C11 N2 H2 115.5(16) . . ? C16 N3 C5 111.06(14) . . ? C16 N3 C4 111.79(14) . . ? C5 N3 C4 109.82(14) . . ? C16 N3 Cu1 103.56(11) . . ? C5 N3 Cu1 107.36(10) . . ? C4 N3 Cu1 113.05(11) . . ? C17 N4 C21 117.95(15) . . ? C17 N4 Cu1 110.48(11) . . ? C21 N4 Cu1 131.57(12) . . ? C21 N5 C22 121.80(16) . . ? C21 N5 H5 116.4(15) . . ? C22 N5 H5 118.6(15) . . ? C2 C1 H1A 111.1(13) . . ? C2 C1 H1B 109.8(14) . . ? H1A C1 H1B 111(2) . . ? C2 C1 H1C 106.7(14) . . ? H1A C1 H1C 108.8(19) . . ? H1B C1 H1C 109(2) . . ? C1 C2 S1 112.80(15) . . ? C1 C2 H2A 113.0(14) . . ? S1 C2 H2A 103.8(14) . . ? C1 C2 H2B 110.6(12) . . ? S1 C2 H2B 109.9(12) . . ? H2A C2 H2B 106.4(18) . . ? C4 C3 S1 110.91(13) . . ? C4 C3 H3A 111.7(14) . . ? S1 C3 H3A 107.9(14) . . ? C4 C3 H3B 112.3(14) . . ? S1 C3 H3B 105.0(14) . . ? H3A C3 H3B 108.7(18) . . ? N3 C4 C3 112.20(16) . . ? N3 C4 H4A 107.7(11) . . ? C3 C4 H4A 109.5(12) . . ? N3 C4 H4B 107.8(12) . . ? C3 C4 H4B 112.1(13) . . ? H4A C4 H4B 107.4(17) . . ? N3 C5 C6 111.54(15) . . ? N3 C5 H5A 106.5(12) . . ? C6 C5 H5A 109.2(12) . . ? N3 C5 H5B 110.6(13) . . ? C6 C5 H5B 109.6(13) . . ? H5A C5 H5B 109.3(17) . . ? N1 C6 C7 123.95(16) . . ? N1 C6 C5 115.70(15) . . ? C7 C6 C5 120.16(17) . . ? C6 C7 C8 117.43(18) . . ? C6 C7 H7 120.5(14) . . ? C8 C7 H7 121.9(14) . . ? C9 C8 C7 120.40(18) . . ? C9 C8 H8 119.2(14) . . ? C7 C8 H8 120.4(14) . . ? C8 C9 C10 119.29(17) . . ? C8 C9 H9 123.3(14) . . ? C10 C9 H9 117.4(14) . . ? N2 C10 N1 116.48(16) . . ? N2 C10 C9 122.88(16) . . ? N1 C10 C9 120.64(17) . . ? N2 C11 C12 115.21(16) . . ? N2 C11 H11A 111.1(12) . . ? C12 C11 H11A 108.4(12) . . ? N2 C11 H11B 107.9(13) . . ? C12 C11 H11B 107.8(13) . . ? H11A C11 H11B 106.0(17) . . ? C13 C12 C15 109.7(2) . . ? C13 C12 C14 109.6(2) . . ? C15 C12 C14 109.28(19) . . ? C13 C12 C11 110.59(19) . . ? C15 C12 C11 110.94(18) . . ? C14 C12 C11 106.59(18) . . ? C12 C13 H13A 110.7(17) . . ? C12 C13 H13B 111.7(16) . . ? H13A C13 H13B 104(2) . . ? C12 C13 H13C 111.1(17) . . ? H13A C13 H13C 111(2) . . ? H13B C13 H13C 108(2) . . ? C12 C14 H14A 113.9(17) . . ? C12 C14 H14B 111.1(16) . . ? H14A C14 H14B 106(2) . . ? C12 C14 H14C 112.5(16) . . ? H14A C14 H14C 106(2) . . ? H14B C14 H14C 107(2) . . ? C12 C15 H15A 110.0(15) . . ? C12 C15 H15B 111.2(15) . . ? H15A C15 H15B 109(2) . . ? C12 C15 H15C 110.6(16) . . ? H15A C15 H15C 110(2) . . ? H15B C15 H15C 106(2) . . ? N3 C16 C17 109.42(14) . . ? N3 C16 H16A 110.6(12) . . ? C17 C16 H16A 110.1(12) . . ? N3 C16 H16B 108.4(13) . . ? C17 C16 H16B 109.3(13) . . ? H16A C16 H16B 108.9(17) . . ? N4 C17 C18 123.89(17) . . ? N4 C17 C16 114.73(15) . . ? C18 C17 C16 121.38(17) . . ? C17 C18 C19 118.10(18) . . ? C17 C18 H18 119.1(13) . . ? C19 C18 H18 122.8(13) . . ? C20 C19 C18 119.47(18) . . ? C20 C19 H19 118.5(14) . . ? C18 C19 H19 122.0(14) . . ? C19 C20 C21 120.40(18) . . ? C19 C20 H20 120.8(13) . . ? C21 C20 H20 118.8(13) . . ? N5 C21 N4 118.43(16) . . ? N5 C21 C20 121.38(16) . . ? N4 C21 C20 120.17(17) . . ? N5 C22 C23 113.81(16) . . ? N5 C22 H22A 107.3(13) . . ? C23 C22 H22A 108.9(13) . . ? N5 C22 H22B 110.8(13) . . ? C23 C22 H22B 107.6(13) . . ? H22A C22 H22B 108.3(18) . . ? C24 C23 C25 110.4(2) . . ? C24 C23 C22 111.24(18) . . ? C25 C23 C22 110.57(19) . . ? C24 C23 C26 110.3(2) . . ? C25 C23 C26 108.17(19) . . ? C22 C23 C26 106.03(18) . . ? C23 C24 H24A 107.6(17) . . ? C23 C24 H24B 114.9(18) . . ? H24A C24 H24B 109(3) . . ? C23 C24 H24C 111.7(18) . . ? H24A C24 H24C 104(2) . . ? H24B C24 H24C 109(3) . . ? C23 C25 H25A 109(2) . . ? C23 C25 H25B 111.6(16) . . ? H25A C25 H25B 104(2) . . ? C23 C25 H25C 112.0(17) . . ? H25A C25 H25C 112(3) . . ? H25B C25 H25C 108(2) . . ? C23 C26 H26A 109.5(16) . . ? C23 C26 H26B 111.1(18) . . ? H26A C26 H26B 110(2) . . ? C23 C26 H26C 108.8(18) . . ? H26A C26 H26C 108(2) . . ? H26B C26 H26C 109(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 S1 C3 -2.49(8) . . . . ? N4 Cu1 S1 C3 71.11(9) . . . . ? N1 Cu1 S1 C3 -80.49(8) . . . . ? Cl1 Cu1 S1 C3 173.82(7) . . . . ? N3 Cu1 S1 C2 102.02(8) . . . . ? N4 Cu1 S1 C2 175.62(9) . . . . ? N1 Cu1 S1 C2 24.02(8) . . . . ? Cl1 Cu1 S1 C2 -81.68(7) . . . . ? N3 Cu1 N1 C6 17.33(11) . . . . ? N4 Cu1 N1 C6 -59.56(12) . . . . ? Cl1 Cu1 N1 C6 -168.25(10) . . . . ? S1 Cu1 N1 C6 99.14(11) . . . . ? N3 Cu1 N1 C10 -166.52(15) . . . . ? N4 Cu1 N1 C10 116.59(14) . . . . ? Cl1 Cu1 N1 C10 7.89(15) . . . . ? S1 Cu1 N1 C10 -84.72(14) . . . . ? N4 Cu1 N3 C16 -36.86(11) . . . . ? N1 Cu1 N3 C16 -148.62(11) . . . . ? Cl1 Cu1 N3 C16 72.2(3) . . . . ? S1 Cu1 N3 C16 98.82(10) . . . . ? N4 Cu1 N3 C5 80.70(11) . . . . ? N1 Cu1 N3 C5 -31.06(11) . . . . ? Cl1 Cu1 N3 C5 -170.3(2) . . . . ? S1 Cu1 N3 C5 -143.63(11) . . . . ? N4 Cu1 N3 C4 -158.03(12) . . . . ? N1 Cu1 N3 C4 90.21(12) . . . . ? Cl1 Cu1 N3 C4 -49.0(4) . . . . ? S1 Cu1 N3 C4 -22.36(11) . . . . ? N3 Cu1 N4 C17 20.53(12) . . . . ? N1 Cu1 N4 C17 96.90(12) . . . . ? Cl1 Cu1 N4 C17 -151.51(11) . . . . ? S1 Cu1 N4 C17 -55.07(14) . . . . ? N3 Cu1 N4 C21 -158.92(16) . . . . ? N1 Cu1 N4 C21 -82.55(16) . . . . ? Cl1 Cu1 N4 C21 29.04(16) . . . . ? S1 Cu1 N4 C21 125.48(14) . . . . ? C3 S1 C2 C1 -72.76(17) . . . . ? Cu1 S1 C2 C1 -173.42(15) . . . . ? C2 S1 C3 C4 -75.02(16) . . . . ? Cu1 S1 C3 C4 26.72(15) . . . . ? C16 N3 C4 C3 -69.5(2) . . . . ? C5 N3 C4 C3 166.80(15) . . . . ? Cu1 N3 C4 C3 46.93(18) . . . . ? S1 C3 C4 N3 -48.6(2) . . . . ? C16 N3 C5 C6 153.58(15) . . . . ? C4 N3 C5 C6 -82.26(18) . . . . ? Cu1 N3 C5 C6 41.02(16) . . . . ? C10 N1 C6 C7 -0.6(2) . . . . ? Cu1 N1 C6 C7 176.15(14) . . . . ? C10 N1 C6 C5 -175.47(15) . . . . ? Cu1 N1 C6 C5 1.23(17) . . . . ? N3 C5 C6 N1 -28.1(2) . . . . ? N3 C5 C6 C7 156.78(16) . . . . ? N1 C6 C7 C8 -2.1(3) . . . . ? C5 C6 C7 C8 172.60(16) . . . . ? C6 C7 C8 C9 2.3(3) . . . . ? C7 C8 C9 C10 0.1(3) . . . . ? C11 N2 C10 N1 -169.50(17) . . . . ? C11 N2 C10 C9 10.5(3) . . . . ? C6 N1 C10 N2 -176.93(15) . . . . ? Cu1 N1 C10 N2 7.2(2) . . . . ? C6 N1 C10 C9 3.0(2) . . . . ? Cu1 N1 C10 C9 -172.86(12) . . . . ? C8 C9 C10 N2 177.14(17) . . . . ? C8 C9 C10 N1 -2.8(3) . . . . ? C10 N2 C11 C12 -102.7(2) . . . . ? N2 C11 C12 C13 -57.8(3) . . . . ? N2 C11 C12 C15 64.2(2) . . . . ? N2 C11 C12 C14 -176.89(18) . . . . ? C5 N3 C16 C17 -67.1(2) . . . . ? C4 N3 C16 C17 169.85(15) . . . . ? Cu1 N3 C16 C17 47.82(17) . . . . ? C21 N4 C17 C18 1.3(3) . . . . ? Cu1 N4 C17 C18 -178.23(15) . . . . ? C21 N4 C17 C16 -178.62(15) . . . . ? Cu1 N4 C17 C16 1.84(19) . . . . ? N3 C16 C17 N4 -34.0(2) . . . . ? N3 C16 C17 C18 146.06(18) . . . . ? N4 C17 C18 C19 -1.2(3) . . . . ? C16 C17 C18 C19 178.71(18) . . . . ? C17 C18 C19 C20 0.2(3) . . . . ? C18 C19 C20 C21 0.6(3) . . . . ? C22 N5 C21 N4 -177.70(16) . . . . ? C22 N5 C21 C20 3.9(3) . . . . ? C17 N4 C21 N5 -178.86(16) . . . . ? Cu1 N4 C21 N5 0.6(3) . . . . ? C17 N4 C21 C20 -0.4(2) . . . . ? Cu1 N4 C21 C20 178.99(13) . . . . ? C19 C20 C21 N5 177.89(18) . . . . ? C19 C20 C21 N4 -0.5(3) . . . . ? C21 N5 C22 C23 -179.87(17) . . . . ? N5 C22 C23 C24 57.2(3) . . . . ? N5 C22 C23 C25 -65.9(2) . . . . ? N5 C22 C23 C26 177.04(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 Cl1 0.80(2) 2.42(2) 3.2135(17) 169(2) . N5 H5 Cl1 0.80(2) 2.43(2) 3.1961(17) 161(2) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.485 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.056 #===END data_usu071 _database_code_CSD 209459 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [(ebnpa)Cu-NCO]ClO4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H43 Cl Cu N6 O5 S' _chemical_formula_weight 710.76 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 7.2979(2) _cell_length_b 34.5443(14) _cell_length_c 13.0965(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.517(3) _cell_angle_gamma 90.00 _cell_volume 3300.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 4501 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8147 _exptl_absorpt_correction_T_max 0.9348 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappCCD Diffractometer' _diffrn_measurement_method 'Phi plus Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10159 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.43 _reflns_number_total 6643 _reflns_number_gt 4838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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^)+(0.0157P)^2^+4.5269P] 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 6643 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _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 Cu1 Cu 0.46267(5) 0.082727(11) 0.26614(3) 0.01878(11) Uani 1 1 d . . . Cl1 Cl 0.06609(11) -0.04774(3) 0.15573(6) 0.0287(2) Uani 1 1 d . . . S1 S 0.79614(11) 0.11701(2) 0.25458(6) 0.02209(19) Uani 1 1 d . . . N1 N 0.5820(3) 0.04638(8) 0.36843(19) 0.0196(6) Uani 1 1 d . . . N2 N 0.5984(4) 0.08898(9) 0.5051(2) 0.0254(7) Uani 1 1 d . . . N3 N 0.5604(3) 0.04372(8) 0.16413(19) 0.0207(6) Uani 1 1 d . . . N4 N 0.3669(3) 0.10970(8) 0.13781(18) 0.0180(6) Uani 1 1 d . . . N5 N 0.2996(4) 0.16965(8) 0.2088(2) 0.0201(6) Uani 1 1 d . . . N6 N 0.2991(4) 0.10834(9) 0.3593(2) 0.0271(7) Uani 1 1 d . . . O1 O 0.0466(4) 0.09606(9) 0.4669(2) 0.0557(9) Uani 1 1 d . . . O2 O 0.0859(4) -0.01179(8) 0.2115(2) 0.0471(7) Uani 1 1 d . . . O3 O -0.0398(3) -0.04120(9) 0.06369(19) 0.0453(7) Uani 1 1 d . . . O4 O 0.2455(3) -0.06167(9) 0.13147(19) 0.0441(7) Uani 1 1 d . . . O5 O -0.0264(4) -0.07562(8) 0.2181(2) 0.0473(7) Uani 1 1 d . . . C1 C 0.7938(4) 0.15023(10) 0.1512(2) 0.0218(7) Uani 1 1 d . . . C2 C 0.8610(5) 0.14291(11) 0.0547(3) 0.0270(8) Uani 1 1 d . . . C3 C 0.8542(5) 0.17158(13) -0.0194(3) 0.0334(9) Uani 1 1 d . . . C4 C 0.7824(5) 0.20766(13) 0.0016(3) 0.0387(10) Uani 1 1 d . . . C5 C 0.7180(5) 0.21495(12) 0.0983(3) 0.0358(10) Uani 1 1 d . . . C6 C 0.7229(4) 0.18667(11) 0.1724(3) 0.0279(8) Uani 1 1 d . . . C7 C 0.8764(4) 0.07177(10) 0.2011(3) 0.0236(7) Uani 1 1 d . . . C8 C 0.7458(4) 0.05303(11) 0.1248(3) 0.0236(7) Uani 1 1 d . . . C9 C 0.5587(5) 0.00597(10) 0.2189(3) 0.0243(7) Uani 1 1 d . . . C10 C 0.6265(4) 0.01158(10) 0.3275(2) 0.0224(7) Uani 1 1 d . . . C11 C 0.7240(4) -0.01618(11) 0.3797(3) 0.0264(8) Uani 1 1 d . . . C12 C 0.7761(5) -0.00856(11) 0.4807(3) 0.0274(8) Uani 1 1 d . . . C13 C 0.7343(4) 0.02591(11) 0.5241(3) 0.0260(8) Uani 1 1 d . . . C14 C 0.6369(4) 0.05399(10) 0.4666(2) 0.0205(7) Uani 1 1 d . . . C15 C 0.6602(5) 0.10217(11) 0.6057(3) 0.0280(8) Uani 1 1 d . . . C16 C 0.6342(5) 0.14557(12) 0.6193(3) 0.0379(10) Uani 1 1 d . . . C17 C 0.7071(7) 0.15584(16) 0.7259(3) 0.0454(11) Uani 1 1 d . . . C18 C 0.4325(7) 0.1568(2) 0.6118(5) 0.0706(18) Uani 1 1 d . . . C19 C 0.7447(9) 0.16750(16) 0.5400(4) 0.0630(15) Uani 1 1 d . . . C20 C 0.4240(5) 0.04540(10) 0.0773(3) 0.0250(8) Uani 1 1 d . . . C21 C 0.3860(4) 0.08703(10) 0.0528(2) 0.0220(7) Uani 1 1 d . . . C22 C 0.3721(4) 0.10133(11) -0.0443(3) 0.0256(8) Uani 1 1 d . . . C23 C 0.3350(5) 0.14046(11) -0.0574(3) 0.0263(8) Uani 1 1 d . . . C24 C 0.3099(4) 0.16335(10) 0.0257(3) 0.0242(8) Uani 1 1 d . . . C25 C 0.3249(4) 0.14780(9) 0.1246(2) 0.0188(7) Uani 1 1 d . . . C26 C 0.2290(5) 0.20892(10) 0.2027(3) 0.0223(7) Uani 1 1 d . . . C27 C 0.2153(4) 0.22916(10) 0.3063(3) 0.0260(8) Uani 1 1 d . . . C28 C 0.0920(6) 0.20661(13) 0.3777(3) 0.0347(9) Uani 1 1 d . . . C29 C 0.4048(6) 0.23470(15) 0.3555(4) 0.0430(11) Uani 1 1 d . . . C30 C 0.1275(6) 0.26851(12) 0.2848(4) 0.0384(10) Uani 1 1 d . . . C31 C 0.1727(5) 0.10127(10) 0.4117(3) 0.0291(8) Uani 1 1 d . . . H2 H 0.914(5) 0.1191(11) 0.040(3) 0.029(10) Uiso 1 1 d . . . H2N H 0.532(5) 0.1003(11) 0.474(3) 0.028(11) Uiso 1 1 d . . . H3 H 0.901(4) 0.1642(10) -0.082(3) 0.024(9) Uiso 1 1 d . . . H4 H 0.773(5) 0.2251(13) -0.051(3) 0.052(13) Uiso 1 1 d . . . H5 H 0.669(5) 0.2381(13) 0.113(3) 0.047(12) Uiso 1 1 d . . . H5N H 0.289(4) 0.1593(9) 0.258(2) 0.008(9) Uiso 1 1 d . . . H6 H 0.677(5) 0.1914(10) 0.239(3) 0.033(10) Uiso 1 1 d . . . H7A H 0.908(4) 0.0569(10) 0.260(2) 0.017(8) Uiso 1 1 d . . . H7B H 0.986(5) 0.0775(10) 0.170(3) 0.029(9) Uiso 1 1 d . . . H8A H 0.798(4) 0.0291(11) 0.097(2) 0.029(9) Uiso 1 1 d . . . H8B H 0.725(4) 0.0687(10) 0.071(2) 0.015(8) Uiso 1 1 d . . . H9A H 0.632(5) -0.0128(10) 0.181(2) 0.031(10) Uiso 1 1 d . . . H9B H 0.430(4) -0.0033(9) 0.214(2) 0.023(9) Uiso 1 1 d . . . H11 H 0.758(4) -0.0388(10) 0.351(2) 0.025(9) Uiso 1 1 d . . . H12 H 0.846(5) -0.0264(11) 0.516(3) 0.030(10) Uiso 1 1 d . . . H13 H 0.770(4) 0.0305(9) 0.586(2) 0.018 Uiso 1 1 d . . . H15A H 0.597(4) 0.0888(9) 0.653(2) 0.018(9) Uiso 1 1 d . . . H15B H 0.799(4) 0.0955(9) 0.616(2) 0.016(8) Uiso 1 1 d . . . H17A H 0.647(7) 0.1429(15) 0.777(4) 0.073(17) Uiso 1 1 d . . . H17B H 0.832(6) 0.1501(12) 0.733(3) 0.045(12) Uiso 1 1 d . . . H17C H 0.693(5) 0.1844(14) 0.740(3) 0.052(13) Uiso 1 1 d . . . H18A H 0.373(7) 0.1507(16) 0.541(4) 0.096(18) Uiso 1 1 d . . . H18B H 0.353(5) 0.1360(11) 0.662(3) 0.031(10) Uiso 1 1 d . . . H18C H 0.419(7) 0.1844(17) 0.628(4) 0.093(19) Uiso 1 1 d . . . H19A H 0.699(6) 0.1611(13) 0.471(4) 0.057(13) Uiso 1 1 d . . . H19B H 0.899(7) 0.1577(15) 0.551(4) 0.088(18) Uiso 1 1 d . . . H19C H 0.738(7) 0.1943(18) 0.553(4) 0.091(19) Uiso 1 1 d . . . H20A H 0.474(4) 0.0332(10) 0.019(2) 0.021(9) Uiso 1 1 d . . . H20B H 0.315(5) 0.0320(10) 0.098(2) 0.027(9) Uiso 1 1 d . . . H22 H 0.385(4) 0.0859(10) -0.100(3) 0.029(10) Uiso 1 1 d . . . H23 H 0.321(5) 0.1508(11) -0.124(3) 0.032(10) Uiso 1 1 d . . . H24 H 0.280(4) 0.1869(9) 0.015(2) 0.012(8) Uiso 1 1 d . . . H26A H 0.308(4) 0.2241(9) 0.163(2) 0.017(8) Uiso 1 1 d . . . H26B H 0.107(5) 0.2087(10) 0.167(3) 0.034 Uiso 1 1 d . . . H28A H -0.033(7) 0.2018(13) 0.344(3) 0.071(15) Uiso 1 1 d . . . H28B H 0.140(6) 0.1830(13) 0.394(3) 0.052(13) Uiso 1 1 d . . . H28C H 0.076(5) 0.2210(11) 0.439(3) 0.037(11) Uiso 1 1 d . . . H29A H 0.457(5) 0.2101(14) 0.367(3) 0.049(13) Uiso 1 1 d . . . H29B H 0.399(6) 0.2474(13) 0.416(3) 0.055(13) Uiso 1 1 d . . . H29C H 0.481(7) 0.2511(15) 0.313(4) 0.075(16) Uiso 1 1 d . . . H30A H 0.194(6) 0.2829(13) 0.241(3) 0.060(14) Uiso 1 1 d . . . H30B H 0.119(5) 0.2848(11) 0.344(3) 0.033(10) Uiso 1 1 d . . . H30C H 0.000(6) 0.2653(12) 0.253(3) 0.051(12) Uiso 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 Cu1 0.01814(19) 0.0201(2) 0.0182(2) -0.00057(17) 0.00250(14) 0.00262(16) Cl1 0.0236(4) 0.0357(5) 0.0269(5) -0.0001(4) 0.0014(3) 0.0023(4) S1 0.0216(4) 0.0246(5) 0.0201(4) 0.0008(3) 0.0008(3) -0.0015(3) N1 0.0179(13) 0.0193(14) 0.0218(15) 0.0021(12) 0.0047(11) 0.0003(11) N2 0.0259(16) 0.0324(18) 0.0177(16) 0.0010(13) -0.0034(12) 0.0068(13) N3 0.0192(13) 0.0203(14) 0.0227(15) 0.0000(12) 0.0011(11) 0.0022(11) N4 0.0145(12) 0.0215(14) 0.0179(14) -0.0031(11) 0.0004(10) 0.0003(10) N5 0.0236(15) 0.0190(15) 0.0176(16) 0.0016(13) 0.0025(12) 0.0021(11) N6 0.0305(16) 0.0308(17) 0.0202(15) 0.0018(13) 0.0050(13) 0.0124(13) O1 0.0443(17) 0.059(2) 0.065(2) 0.0255(17) 0.0295(15) 0.0140(14) O2 0.0410(16) 0.0423(18) 0.0583(18) -0.0180(14) 0.0090(13) 0.0003(13) O3 0.0367(15) 0.062(2) 0.0362(16) 0.0134(14) -0.0133(12) -0.0073(13) O4 0.0295(14) 0.059(2) 0.0438(16) -0.0135(14) 0.0060(12) 0.0147(13) O5 0.0516(17) 0.0476(19) 0.0433(17) 0.0165(14) 0.0113(13) -0.0026(14) C1 0.0175(16) 0.0241(18) 0.0236(18) 0.0017(14) -0.0029(13) -0.0065(13) C2 0.0244(18) 0.029(2) 0.027(2) 0.0013(16) 0.0001(15) -0.0071(15) C3 0.0261(19) 0.051(3) 0.023(2) 0.0093(19) -0.0027(15) -0.0119(17) C4 0.0242(19) 0.046(3) 0.045(3) 0.026(2) -0.0078(18) -0.0074(17) C5 0.0198(18) 0.029(2) 0.059(3) 0.014(2) -0.0003(17) 0.0004(15) C6 0.0191(17) 0.029(2) 0.036(2) 0.0021(17) 0.0025(15) -0.0028(14) C7 0.0177(16) 0.0282(19) 0.025(2) 0.0032(15) 0.0030(14) 0.0011(14) C8 0.0236(17) 0.0220(18) 0.025(2) 0.0007(16) 0.0078(14) 0.0038(14) C9 0.0280(19) 0.0173(17) 0.028(2) -0.0008(15) 0.0057(15) -0.0012(14) C10 0.0168(15) 0.0227(18) 0.0280(19) 0.0027(15) 0.0069(13) -0.0024(13) C11 0.0224(17) 0.0221(19) 0.035(2) 0.0022(16) 0.0090(15) 0.0015(14) C12 0.0199(17) 0.028(2) 0.034(2) 0.0140(17) 0.0012(15) 0.0024(14) C13 0.0226(17) 0.033(2) 0.0220(19) 0.0075(16) -0.0001(14) -0.0016(15) C14 0.0160(15) 0.0250(18) 0.0206(18) 0.0017(14) 0.0049(13) 0.0001(13) C15 0.030(2) 0.036(2) 0.0182(19) 0.0025(16) 0.0001(15) -0.0032(16) C16 0.049(2) 0.041(2) 0.024(2) -0.0108(18) -0.0014(17) 0.0099(19) C17 0.056(3) 0.048(3) 0.031(3) -0.013(2) -0.008(2) 0.002(2) C18 0.062(3) 0.084(5) 0.065(4) -0.039(3) -0.015(3) 0.031(3) C19 0.115(5) 0.034(3) 0.040(3) -0.003(2) 0.011(3) -0.006(3) C20 0.0271(18) 0.0236(19) 0.024(2) -0.0039(16) 0.0004(15) 0.0009(15) C21 0.0159(15) 0.0266(19) 0.0233(19) -0.0063(15) -0.0006(12) -0.0012(13) C22 0.0253(18) 0.036(2) 0.0158(19) -0.0079(16) -0.0013(14) 0.0019(15) C23 0.0292(19) 0.030(2) 0.0193(19) 0.0020(16) -0.0015(14) 0.0028(15) C24 0.0222(17) 0.0215(19) 0.029(2) 0.0040(16) 0.0024(14) 0.0027(14) C25 0.0110(14) 0.0243(18) 0.0211(18) -0.0014(14) -0.0006(12) -0.0002(12) C26 0.0221(17) 0.0206(18) 0.0243(19) 0.0027(15) 0.0025(14) 0.0026(14) C27 0.0249(17) 0.0242(19) 0.029(2) -0.0042(15) 0.0029(14) 0.0012(14) C28 0.044(2) 0.031(2) 0.030(2) -0.0035(19) 0.0109(18) 0.0034(19) C29 0.039(2) 0.046(3) 0.045(3) -0.024(2) -0.003(2) 0.001(2) C30 0.049(3) 0.021(2) 0.046(3) -0.0048(19) 0.017(2) 0.0077(18) C31 0.030(2) 0.026(2) 0.031(2) 0.0070(16) 0.0006(16) 0.0085(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 Cu1 N6 1.943(3) . ? Cu1 N1 2.017(3) . ? Cu1 N4 2.029(3) . ? Cu1 N3 2.040(3) . ? Cu1 S1 2.7143(9) . ? Cl1 O3 1.433(2) . ? Cl1 O4 1.438(2) . ? Cl1 O5 1.442(3) . ? Cl1 O2 1.446(3) . ? S1 C1 1.775(3) . ? S1 C7 1.816(3) . ? N1 C10 1.359(4) . ? N1 C14 1.362(4) . ? N2 C14 1.343(4) . ? N2 C15 1.455(4) . ? N2 H2N 0.74(4) . ? N3 C9 1.488(4) . ? N3 C20 1.492(4) . ? N3 C8 1.495(4) . ? N4 C25 1.361(4) . ? N4 C21 1.372(4) . ? N5 C25 1.353(4) . ? N5 C26 1.453(4) . ? N5 H5N 0.75(3) . ? N6 C31 1.189(4) . ? O1 C31 1.199(4) . ? C1 C2 1.390(5) . ? C1 C6 1.392(5) . ? C2 C3 1.386(5) . ? C2 H2 0.93(4) . ? C3 C4 1.382(6) . ? C3 H3 0.94(3) . ? C4 C5 1.385(6) . ? C4 H4 0.91(4) . ? C5 C6 1.378(5) . ? C5 H5 0.90(4) . ? C6 H6 0.95(3) . ? C7 C8 1.509(5) . ? C7 H7A 0.95(3) . ? C7 H7B 0.93(3) . ? C8 H8A 0.99(4) . ? C8 H8B 0.90(3) . ? C9 C10 1.506(5) . ? C9 H9A 0.98(4) . ? C9 H9B 0.99(3) . ? C10 C11 1.366(5) . ? C11 C12 1.392(5) . ? C11 H11 0.91(3) . ? C12 C13 1.358(5) . ? C12 H12 0.92(4) . ? C13 C14 1.409(5) . ? C13 H13 0.86(3) . ? C15 C16 1.522(5) . ? C15 H15A 0.91(3) . ? C15 H15B 1.04(3) . ? C16 C18 1.523(6) . ? C16 C17 1.523(5) . ? C16 C19 1.532(6) . ? C17 H17A 0.92(5) . ? C17 H17B 0.94(4) . ? C17 H17C 1.01(5) . ? C18 H18A 1.04(6) . ? C18 H18B 1.14(4) . ? C18 H18C 0.98(6) . ? C19 H19A 0.98(4) . ? C19 H19B 1.18(5) . ? C19 H19C 0.94(6) . ? C20 C21 1.498(5) . ? C20 H20A 0.95(3) . ? C20 H20B 0.96(3) . ? C21 C22 1.365(5) . ? C22 C23 1.388(5) . ? C22 H22 0.91(3) . ? C23 C24 1.361(5) . ? C23 H23 0.94(4) . ? C24 C25 1.404(5) . ? C24 H24 0.85(3) . ? C26 C27 1.532(5) . ? C26 H26A 0.95(3) . ? C26 H26B 1.00(3) . ? C27 C29 1.523(5) . ? C27 C30 1.526(5) . ? C27 C28 1.528(5) . ? C28 H28A 1.02(5) . ? C28 H28B 0.91(5) . ? C28 H28C 0.96(4) . ? C29 H29A 0.94(4) . ? C29 H29B 0.91(4) . ? C29 H29C 0.98(5) . ? C30 H30A 0.91(5) . ? C30 H30B 0.96(4) . ? C30 H30C 1.02(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Cu1 N1 97.34(11) . . ? N6 Cu1 N4 96.16(10) . . ? N1 Cu1 N4 165.70(10) . . ? N6 Cu1 N3 160.69(12) . . ? N1 Cu1 N3 82.61(10) . . ? N4 Cu1 N3 83.09(10) . . ? N6 Cu1 S1 113.76(9) . . ? N1 Cu1 S1 86.37(7) . . ? N4 Cu1 S1 92.48(7) . . ? N3 Cu1 S1 85.54(7) . . ? O3 Cl1 O4 109.94(16) . . ? O3 Cl1 O5 109.36(16) . . ? O4 Cl1 O5 110.11(17) . . ? O3 Cl1 O2 109.54(18) . . ? O4 Cl1 O2 108.65(16) . . ? O5 Cl1 O2 109.23(17) . . ? C1 S1 C7 105.00(16) . . ? C1 S1 Cu1 109.51(10) . . ? C7 S1 Cu1 86.84(11) . . ? C10 N1 C14 118.4(3) . . ? C10 N1 Cu1 113.1(2) . . ? C14 N1 Cu1 128.2(2) . . ? C14 N2 C15 124.0(3) . . ? C14 N2 H2N 114(3) . . ? C15 N2 H2N 121(3) . . ? C9 N3 C20 112.8(3) . . ? C9 N3 C8 111.9(3) . . ? C20 N3 C8 108.7(3) . . ? C9 N3 Cu1 104.83(19) . . ? C20 N3 Cu1 103.63(19) . . ? C8 N3 Cu1 114.8(2) . . ? C25 N4 C21 118.4(3) . . ? C25 N4 Cu1 128.4(2) . . ? C21 N4 Cu1 111.7(2) . . ? C25 N5 C26 122.1(3) . . ? C25 N5 H5N 117(3) . . ? C26 N5 H5N 117(2) . . ? C31 N6 Cu1 140.1(3) . . ? C2 C1 C6 119.2(3) . . ? C2 C1 S1 125.4(3) . . ? C6 C1 S1 115.3(3) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 H2 120(2) . . ? C1 C2 H2 120(2) . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3 125(2) . . ? C2 C3 H3 115(2) . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4 118(3) . . ? C5 C4 H4 123(3) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5 119(3) . . ? C4 C5 H5 120(3) . . ? C5 C6 C1 120.2(4) . . ? C5 C6 H6 121(2) . . ? C1 C6 H6 119(2) . . ? C8 C7 S1 114.8(2) . . ? C8 C7 H7A 116.2(19) . . ? S1 C7 H7A 102.9(19) . . ? C8 C7 H7B 110(2) . . ? S1 C7 H7B 106(2) . . ? H7A C7 H7B 106(3) . . ? N3 C8 C7 115.2(3) . . ? N3 C8 H8A 108(2) . . ? C7 C8 H8A 111.5(19) . . ? N3 C8 H8B 105.5(19) . . ? C7 C8 H8B 111(2) . . ? H8A C8 H8B 106(3) . . ? N3 C9 C10 109.6(3) . . ? N3 C9 H9A 109(2) . . ? C10 C9 H9A 113.3(19) . . ? N3 C9 H9B 105.8(19) . . ? C10 C9 H9B 112.6(17) . . ? H9A C9 H9B 106(3) . . ? N1 C10 C11 123.4(3) . . ? N1 C10 C9 114.2(3) . . ? C11 C10 C9 122.4(3) . . ? C10 C11 C12 117.9(3) . . ? C10 C11 H11 123(2) . . ? C12 C11 H11 119(2) . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 120(2) . . ? C11 C12 H12 119(2) . . ? C12 C13 C14 119.7(3) . . ? C12 C13 H13 120(2) . . ? C14 C13 H13 121(2) . . ? N2 C14 N1 118.0(3) . . ? N2 C14 C13 121.8(3) . . ? N1 C14 C13 120.2(3) . . ? N2 C15 C16 112.2(3) . . ? N2 C15 H15A 108(2) . . ? C16 C15 H15A 111(2) . . ? N2 C15 H15B 108.7(16) . . ? C16 C15 H15B 109.0(17) . . ? H15A C15 H15B 108(3) . . ? C15 C16 C18 111.5(4) . . ? C15 C16 C17 107.1(3) . . ? C18 C16 C17 108.2(4) . . ? C15 C16 C19 109.8(4) . . ? C18 C16 C19 110.9(5) . . ? C17 C16 C19 109.2(4) . . ? C16 C17 H17A 113(3) . . ? C16 C17 H17B 111(2) . . ? H17A C17 H17B 108(4) . . ? C16 C17 H17C 111(2) . . ? H17A C17 H17C 107(4) . . ? H17B C17 H17C 107(3) . . ? C16 C18 H18A 113(3) . . ? C16 C18 H18B 107.8(19) . . ? H18A C18 H18B 100(4) . . ? C16 C18 H18C 110(3) . . ? H18A C18 H18C 110(4) . . ? H18B C18 H18C 115(4) . . ? C16 C19 H19A 110(3) . . ? C16 C19 H19B 107(2) . . ? H19A C19 H19B 111(4) . . ? C16 C19 H19C 109(3) . . ? H19A C19 H19C 112(4) . . ? H19B C19 H19C 108(4) . . ? N3 C20 C21 108.5(3) . . ? N3 C20 H20A 109.2(19) . . ? C21 C20 H20A 109(2) . . ? N3 C20 H20B 107.9(19) . . ? C21 C20 H20B 112(2) . . ? H20A C20 H20B 110(3) . . ? C22 C21 N4 122.9(3) . . ? C22 C21 C20 123.8(3) . . ? N4 C21 C20 113.3(3) . . ? C21 C22 C23 118.4(3) . . ? C21 C22 H22 122(2) . . ? C23 C22 H22 120(2) . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H23 120(2) . . ? C22 C23 H23 120(2) . . ? C23 C24 C25 120.4(3) . . ? C23 C24 H24 118(2) . . ? C25 C24 H24 122(2) . . ? N5 C25 N4 118.1(3) . . ? N5 C25 C24 122.0(3) . . ? N4 C25 C24 119.9(3) . . ? N5 C26 C27 114.1(3) . . ? N5 C26 H26A 109.0(19) . . ? C27 C26 H26A 106.9(19) . . ? N5 C26 H26B 109(2) . . ? C27 C26 H26B 110(2) . . ? H26A C26 H26B 107(3) . . ? C29 C27 C30 109.8(3) . . ? C29 C27 C28 110.4(3) . . ? C30 C27 C28 108.4(3) . . ? C29 C27 C26 110.6(3) . . ? C30 C27 C26 106.2(3) . . ? C28 C27 C26 111.3(3) . . ? C27 C28 H28A 111(3) . . ? C27 C28 H28B 112(3) . . ? H28A C28 H28B 107(4) . . ? C27 C28 H28C 110(2) . . ? H28A C28 H28C 109(3) . . ? H28B C28 H28C 108(3) . . ? C27 C29 H29A 108(3) . . ? C27 C29 H29B 112(3) . . ? H29A C29 H29B 109(4) . . ? C27 C29 H29C 111(3) . . ? H29A C29 H29C 112(4) . . ? H29B C29 H29C 105(4) . . ? C27 C30 H30A 112(3) . . ? C27 C30 H30B 114(2) . . ? H30A C30 H30B 104(3) . . ? C27 C30 H30C 111(2) . . ? H30A C30 H30C 107(4) . . ? H30B C30 H30C 108(3) . . ? N6 C31 O1 176.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Cu1 S1 C1 -93.78(15) . . . . ? N1 Cu1 S1 C1 169.79(14) . . . . ? N4 Cu1 S1 C1 4.07(14) . . . . ? N3 Cu1 S1 C1 86.93(14) . . . . ? N6 Cu1 S1 C7 161.42(15) . . . . ? N1 Cu1 S1 C7 64.99(14) . . . . ? N4 Cu1 S1 C7 -100.74(14) . . . . ? N3 Cu1 S1 C7 -17.87(14) . . . . ? N6 Cu1 N1 C10 146.2(2) . . . . ? N4 Cu1 N1 C10 -14.6(5) . . . . ? N3 Cu1 N1 C10 -14.4(2) . . . . ? S1 Cu1 N1 C10 -100.3(2) . . . . ? N6 Cu1 N1 C14 -40.9(3) . . . . ? N4 Cu1 N1 C14 158.4(4) . . . . ? N3 Cu1 N1 C14 158.6(3) . . . . ? S1 Cu1 N1 C14 72.6(2) . . . . ? N6 Cu1 N3 C9 -60.3(4) . . . . ? N1 Cu1 N3 C9 30.78(19) . . . . ? N4 Cu1 N3 C9 -149.3(2) . . . . ? S1 Cu1 N3 C9 117.69(19) . . . . ? N6 Cu1 N3 C20 58.1(4) . . . . ? N1 Cu1 N3 C20 149.2(2) . . . . ? N4 Cu1 N3 C20 -30.8(2) . . . . ? S1 Cu1 N3 C20 -123.85(19) . . . . ? N6 Cu1 N3 C8 176.5(3) . . . . ? N1 Cu1 N3 C8 -92.4(2) . . . . ? N4 Cu1 N3 C8 87.5(2) . . . . ? S1 Cu1 N3 C8 -5.5(2) . . . . ? N6 Cu1 N4 C25 43.3(3) . . . . ? N1 Cu1 N4 C25 -155.9(4) . . . . ? N3 Cu1 N4 C25 -156.1(3) . . . . ? S1 Cu1 N4 C25 -70.9(2) . . . . ? N6 Cu1 N4 C21 -151.0(2) . . . . ? N1 Cu1 N4 C21 9.8(5) . . . . ? N3 Cu1 N4 C21 9.6(2) . . . . ? S1 Cu1 N4 C21 94.77(19) . . . . ? N1 Cu1 N6 C31 -63.8(4) . . . . ? N4 Cu1 N6 C31 111.5(4) . . . . ? N3 Cu1 N6 C31 24.8(6) . . . . ? S1 Cu1 N6 C31 -153.1(4) . . . . ? C7 S1 C1 C2 -6.7(3) . . . . ? Cu1 S1 C1 C2 -98.7(3) . . . . ? C7 S1 C1 C6 175.4(2) . . . . ? Cu1 S1 C1 C6 83.4(2) . . . . ? C6 C1 C2 C3 -1.0(5) . . . . ? S1 C1 C2 C3 -178.8(3) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 C1 0.2(5) . . . . ? C2 C1 C6 C5 0.6(5) . . . . ? S1 C1 C6 C5 178.7(3) . . . . ? C1 S1 C7 C8 -67.9(3) . . . . ? Cu1 S1 C7 C8 41.5(2) . . . . ? C9 N3 C8 C7 -83.9(4) . . . . ? C20 N3 C8 C7 150.9(3) . . . . ? Cu1 N3 C8 C7 35.4(4) . . . . ? S1 C7 C8 N3 -58.4(4) . . . . ? C20 N3 C9 C10 -154.0(3) . . . . ? C8 N3 C9 C10 83.1(3) . . . . ? Cu1 N3 C9 C10 -41.9(3) . . . . ? C14 N1 C10 C11 -0.1(4) . . . . ? Cu1 N1 C10 C11 173.6(2) . . . . ? C14 N1 C10 C9 179.7(3) . . . . ? Cu1 N1 C10 C9 -6.6(3) . . . . ? N3 C9 C10 N1 33.4(4) . . . . ? N3 C9 C10 C11 -146.8(3) . . . . ? N1 C10 C11 C12 1.5(5) . . . . ? C9 C10 C11 C12 -178.3(3) . . . . ? C10 C11 C12 C13 -1.6(5) . . . . ? C11 C12 C13 C14 0.2(5) . . . . ? C15 N2 C14 N1 -175.2(3) . . . . ? C15 N2 C14 C13 3.5(5) . . . . ? C10 N1 C14 N2 177.5(3) . . . . ? Cu1 N1 C14 N2 4.9(4) . . . . ? C10 N1 C14 C13 -1.3(4) . . . . ? Cu1 N1 C14 C13 -173.9(2) . . . . ? C12 C13 C14 N2 -177.5(3) . . . . ? C12 C13 C14 N1 1.2(5) . . . . ? C14 N2 C15 C16 166.9(3) . . . . ? N2 C15 C16 C18 62.9(4) . . . . ? N2 C15 C16 C17 -178.8(3) . . . . ? N2 C15 C16 C19 -60.4(5) . . . . ? C9 N3 C20 C21 159.3(3) . . . . ? C8 N3 C20 C21 -76.0(3) . . . . ? Cu1 N3 C20 C21 46.5(3) . . . . ? C25 N4 C21 C22 2.8(4) . . . . ? Cu1 N4 C21 C22 -164.5(2) . . . . ? C25 N4 C21 C20 -177.5(3) . . . . ? Cu1 N4 C21 C20 15.3(3) . . . . ? N3 C20 C21 C22 137.2(3) . . . . ? N3 C20 C21 N4 -42.5(4) . . . . ? N4 C21 C22 C23 -0.8(5) . . . . ? C20 C21 C22 C23 179.5(3) . . . . ? C21 C22 C23 C24 -1.2(5) . . . . ? C22 C23 C24 C25 1.2(5) . . . . ? C26 N5 C25 N4 -171.0(3) . . . . ? C26 N5 C25 C24 9.4(4) . . . . ? C21 N4 C25 N5 177.6(3) . . . . ? Cu1 N4 C25 N5 -17.5(4) . . . . ? C21 N4 C25 C24 -2.7(4) . . . . ? Cu1 N4 C25 C24 162.1(2) . . . . ? C23 C24 C25 N5 -179.6(3) . . . . ? C23 C24 C25 N4 0.8(5) . . . . ? C25 N5 C26 C27 -178.5(3) . . . . ? N5 C26 C27 C29 64.6(4) . . . . ? N5 C26 C27 C30 -176.3(3) . . . . ? N5 C26 C27 C28 -58.5(4) . . . . ? Cu1 N6 C31 O1 167(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N N6 0.74(4) 2.25(4) 2.939(4) 155(4) . N5 H5N N6 0.75(3) 2.20(3) 2.894(4) 154(3) . _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.404 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.076 #===END data_usu065 _database_code_CSD 209460 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [(ebnpa)Cu-N3]ClO4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H43 Cl Cu N8 O4 S' _chemical_formula_weight 662.73 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 8.5866(2) _cell_length_b 13.7903(3) _cell_length_c 14.6773(4) _cell_angle_alpha 78.9526(9) _cell_angle_beta 89.4294(9) _cell_angle_gamma 73.8704(16) _cell_volume 1636.89(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 5722 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7539 _exptl_absorpt_correction_T_max 0.9193 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi plus Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2.0 _diffrn_reflns_number 11484 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7415 _reflns_number_gt 5850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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^)+(0.0494P)^2^+0.9490P] 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 7415 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Cu1 Cu 0.04692(3) 0.20192(2) 0.229059(18) 0.01994(9) Uani 1 1 d . . . Cl1 Cl 0.41920(7) 0.80126(5) 0.11423(4) 0.03411(15) Uani 1 1 d . . . S1 S 0.33540(6) 0.17573(5) 0.23247(4) 0.02531(13) Uani 1 1 d . . . O1 O 0.4458(2) 0.74023(14) 0.04378(13) 0.0396(4) Uani 1 1 d . . . O2 O 0.2597(3) 0.81672(19) 0.14558(18) 0.0611(6) Uani 1 1 d . . . O3 O 0.4458(4) 0.8984(2) 0.0799(3) 0.0979(12) Uani 1 1 d . . . O4 O 0.5357(4) 0.7511(3) 0.1886(2) 0.1226(16) Uani 1 1 d . . . N1 N 0.0697(2) 0.16788(14) 0.10074(13) 0.0230(4) Uani 1 1 d . . . N2 N -0.0818(2) 0.09141(14) 0.24693(13) 0.0210(4) Uani 1 1 d . . . N3 N -0.2166(2) 0.12682(16) 0.37950(14) 0.0262(4) Uani 1 1 d . . . H3 H -0.164(3) 0.161(2) 0.3832(18) 0.022(7) Uiso 1 1 d . . . N4 N -0.0928(2) 0.34775(14) 0.15053(13) 0.0240(4) Uani 1 1 d . . . N5 N -0.1017(3) 0.44662(18) 0.26206(17) 0.0398(6) Uani 1 1 d . . . H5 H -0.064(4) 0.392(3) 0.292(2) 0.040(9) Uiso 1 1 d . . . N6 N 0.0314(2) 0.23511(15) 0.35381(13) 0.0236(4) Uani 1 1 d . . . N7 N 0.1480(2) 0.20575(17) 0.40805(14) 0.0295(4) Uani 1 1 d . . . N8 N 0.2553(3) 0.1783(3) 0.46132(18) 0.0584(8) Uani 1 1 d . . . C1 C 0.5100(4) 0.3203(3) 0.1966(2) 0.0424(7) Uani 1 1 d . . . H1A H 0.560(4) 0.293(3) 0.139(2) 0.055(9) Uiso 1 1 d . . . H1B H 0.581(4) 0.283(3) 0.247(3) 0.060(10) Uiso 1 1 d . . . H1C H 0.500(4) 0.386(3) 0.188(2) 0.049(9) Uiso 1 1 d . . . C2 C 0.3406(3) 0.3092(2) 0.2120(2) 0.0328(6) Uani 1 1 d . . . H2A H 0.269(4) 0.344(3) 0.158(2) 0.054(9) Uiso 1 1 d . . . H2B H 0.297(3) 0.331(2) 0.260(2) 0.040(8) Uiso 1 1 d . . . C3 C 0.3678(3) 0.1431(2) 0.11858(18) 0.0315(5) Uani 1 1 d . . . H3A H 0.455(4) 0.169(2) 0.091(2) 0.041(8) Uiso 1 1 d . . . H3B H 0.396(3) 0.070(2) 0.1322(17) 0.024(6) Uiso 1 1 d . . . C4 C 0.2166(3) 0.1891(2) 0.05496(17) 0.0291(5) Uani 1 1 d . . . H4A H 0.233(3) 0.162(2) 0.000(2) 0.034(7) Uiso 1 1 d . . . H4B H 0.196(3) 0.267(2) 0.0365(17) 0.024(6) Uiso 1 1 d . . . C5 C 0.0774(3) 0.05725(19) 0.11467(18) 0.0279(5) Uani 1 1 d . . . H5A H 0.183(3) 0.015(2) 0.1422(18) 0.027(6) Uiso 1 1 d . . . H5B H 0.062(3) 0.041(2) 0.058(2) 0.039(7) Uiso 1 1 d . . . C6 C -0.0522(3) 0.03609(17) 0.17846(16) 0.0252(5) Uani 1 1 d . . . C7 C -0.1317(3) -0.03582(19) 0.16883(18) 0.0320(5) Uani 1 1 d . . . H7 H -0.106(3) -0.070(2) 0.1165(19) 0.034(7) Uiso 1 1 d . . . C8 C -0.2462(3) -0.0527(2) 0.23276(19) 0.0331(6) Uani 1 1 d . . . H8 H -0.303(4) -0.097(2) 0.228(2) 0.044(8) Uiso 1 1 d . . . C9 C -0.2762(3) 0.00022(18) 0.30362(18) 0.0283(5) Uani 1 1 d . . . H9 H -0.349(3) -0.0098(19) 0.3479(17) 0.024(6) Uiso 1 1 d . . . C10 C -0.1911(3) 0.07315(17) 0.31094(16) 0.0233(5) Uani 1 1 d . . . C11 C -0.3153(3) 0.1044(2) 0.45840(18) 0.0323(6) Uani 1 1 d . . . H11A H -0.281(4) 0.022(3) 0.485(2) 0.047(8) Uiso 1 1 d . . . H11B H -0.430(4) 0.125(2) 0.439(2) 0.043(8) Uiso 1 1 d . . . C12 C -0.2987(3) 0.1582(2) 0.53728(16) 0.0311(5) Uani 1 1 d . . . C13 C -0.4064(4) 0.1268(3) 0.6143(2) 0.0448(7) Uani 1 1 d . . . H13A H -0.375(5) 0.050(3) 0.633(3) 0.080(13) Uiso 1 1 d . . . H13B H -0.518(4) 0.150(2) 0.593(2) 0.046(8) Uiso 1 1 d . . . H13C H -0.400(4) 0.158(3) 0.665(2) 0.052(9) Uiso 1 1 d . . . C14 C -0.1251(4) 0.1251(4) 0.5758(2) 0.0652(11) Uani 1 1 d . . . H14A H -0.0552 0.1471 0.5277 0.098 Uiso 1 1 calc R . . H14B H -0.0891 0.0500 0.5951 0.098 Uiso 1 1 calc R . . H14C H -0.1184 0.1568 0.6294 0.098 Uiso 1 1 calc R . . C15 C -0.3558(6) 0.2740(3) 0.5049(3) 0.0610(10) Uani 1 1 d . . . H15A H -0.293(5) 0.305(3) 0.458(3) 0.074(12) Uiso 1 1 d . . . H15B H -0.463(5) 0.294(3) 0.478(3) 0.079(14) Uiso 1 1 d . . . H15C H -0.361(5) 0.308(4) 0.552(3) 0.093(14) Uiso 1 1 d . . . C16 C -0.0795(3) 0.23191(19) 0.04460(16) 0.0260(5) Uani 1 1 d . . . H16A H -0.161(3) 0.1963(19) 0.0616(17) 0.028(7) Uiso 1 1 d . . . H16B H -0.061(3) 0.236(2) -0.018(2) 0.035(7) Uiso 1 1 d . . . C17 C -0.1349(3) 0.33854(18) 0.06500(16) 0.0251(5) Uani 1 1 d . . . C18 C -0.2332(3) 0.4185(2) 0.00196(18) 0.0307(5) Uani 1 1 d . . . H18 H -0.253(3) 0.406(2) -0.0492(19) 0.025(7) Uiso 1 1 d . . . C19 C -0.2946(3) 0.5126(2) 0.02981(19) 0.0338(6) Uani 1 1 d . . . H19 H -0.367(3) 0.570(2) -0.009(2) 0.038(8) Uiso 1 1 d . . . C20 C -0.2544(3) 0.5251(2) 0.11549(19) 0.0335(6) Uani 1 1 d . . . H20 H -0.294(4) 0.591(3) 0.133(2) 0.063(10) Uiso 1 1 d . . . C21 C -0.1496(3) 0.44063(18) 0.17674(17) 0.0278(5) Uani 1 1 d . . . C22 C -0.1642(4) 0.5324(2) 0.3101(2) 0.0431(7) Uani 1 1 d . . . H22A H -0.265(3) 0.571(2) 0.2828(19) 0.033(7) Uiso 1 1 d . . . H22B H -0.180(3) 0.498(2) 0.379(2) 0.043(8) Uiso 1 1 d . . . C23 C -0.0519(4) 0.6001(2) 0.3135(2) 0.0493(7) Uani 1 1 d . . . C24 C 0.1112(5) 0.5356(3) 0.3604(3) 0.0808(13) Uani 1 1 d . . . H24A H 0.0939 0.4969 0.4211 0.121 Uiso 1 1 calc R . . H24B H 0.1778 0.5809 0.3687 0.121 Uiso 1 1 calc R . . H24C H 0.1670 0.4874 0.3214 0.121 Uiso 1 1 calc R . . C25 C -0.1349(6) 0.6810(3) 0.3701(3) 0.0637(10) Uani 1 1 d . . . H25A H -0.252(6) 0.716(4) 0.347(3) 0.101(16) Uiso 1 1 d . . . H25B H -0.139(4) 0.646(3) 0.438(3) 0.066(11) Uiso 1 1 d . . . H25C H -0.066(5) 0.728(3) 0.372(3) 0.079(12) Uiso 1 1 d . . . C26 C -0.0287(5) 0.6544(3) 0.2152(3) 0.0587(9) Uani 1 1 d . . . H26A H 0.015(4) 0.600(3) 0.176(2) 0.059(10) Uiso 1 1 d . . . H26B H 0.044(5) 0.695(3) 0.218(3) 0.088(13) Uiso 1 1 d . . . H26C H -0.137(5) 0.697(3) 0.179(3) 0.085(13) Uiso 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 Cu1 0.01969(14) 0.02042(15) 0.02022(15) -0.00536(11) 0.00319(10) -0.00560(10) Cl1 0.0294(3) 0.0321(3) 0.0415(4) -0.0178(3) 0.0013(2) -0.0027(2) S1 0.0190(3) 0.0278(3) 0.0271(3) -0.0041(2) 0.0039(2) -0.0045(2) O1 0.0479(11) 0.0354(10) 0.0373(10) -0.0167(9) 0.0026(8) -0.0081(9) O2 0.0505(13) 0.0623(15) 0.0829(17) -0.0336(13) 0.0347(12) -0.0242(11) O3 0.105(2) 0.0507(15) 0.166(3) -0.0607(18) 0.083(2) -0.0433(15) O4 0.109(2) 0.132(3) 0.088(2) -0.073(2) -0.0601(18) 0.066(2) N1 0.0242(9) 0.0227(10) 0.0228(10) -0.0055(8) 0.0047(7) -0.0072(8) N2 0.0195(9) 0.0196(9) 0.0232(9) -0.0043(8) 0.0016(7) -0.0042(7) N3 0.0239(10) 0.0297(11) 0.0291(11) -0.0088(9) 0.0080(8) -0.0125(9) N4 0.0251(9) 0.0210(10) 0.0245(10) -0.0025(8) 0.0021(7) -0.0053(8) N5 0.0608(15) 0.0191(12) 0.0330(13) -0.0076(10) -0.0050(11) 0.0012(11) N6 0.0210(9) 0.0255(10) 0.0248(10) -0.0066(8) 0.0011(7) -0.0062(8) N7 0.0252(10) 0.0396(12) 0.0276(11) -0.0149(9) 0.0065(8) -0.0103(9) N8 0.0317(13) 0.103(2) 0.0399(14) -0.0277(15) -0.0037(11) -0.0078(14) C1 0.0326(14) 0.0439(18) 0.0510(19) 0.0027(15) -0.0042(13) -0.0194(13) C2 0.0273(12) 0.0323(14) 0.0400(15) -0.0073(12) 0.0041(11) -0.0104(11) C3 0.0260(12) 0.0340(15) 0.0358(14) -0.0128(11) 0.0112(10) -0.0068(11) C4 0.0308(12) 0.0352(15) 0.0238(12) -0.0099(11) 0.0108(9) -0.0111(11) C5 0.0331(13) 0.0264(13) 0.0267(13) -0.0118(10) 0.0067(10) -0.0081(10) C6 0.0270(11) 0.0199(11) 0.0275(12) -0.0053(9) 0.0008(9) -0.0041(9) C7 0.0401(14) 0.0249(13) 0.0341(14) -0.0109(11) 0.0006(11) -0.0107(11) C8 0.0323(13) 0.0262(13) 0.0433(15) -0.0057(11) -0.0035(11) -0.0128(11) C9 0.0224(11) 0.0266(13) 0.0364(14) -0.0028(10) 0.0022(10) -0.0098(9) C10 0.0196(10) 0.0209(11) 0.0274(12) -0.0028(9) 0.0008(8) -0.0038(9) C11 0.0277(12) 0.0412(15) 0.0321(13) -0.0106(12) 0.0111(10) -0.0144(11) C12 0.0254(11) 0.0453(15) 0.0255(12) -0.0088(11) 0.0049(9) -0.0136(11) C13 0.0376(16) 0.073(2) 0.0312(15) -0.0145(16) 0.0126(12) -0.0246(16) C14 0.0335(15) 0.134(4) 0.0322(16) -0.0125(19) 0.0004(12) -0.0337(19) C15 0.092(3) 0.044(2) 0.053(2) -0.0216(17) 0.029(2) -0.021(2) C16 0.0282(12) 0.0301(13) 0.0199(12) -0.0046(10) -0.0002(9) -0.0085(10) C17 0.0222(11) 0.0278(12) 0.0256(12) -0.0019(10) 0.0031(9) -0.0096(9) C18 0.0317(13) 0.0329(14) 0.0261(13) -0.0011(11) -0.0026(10) -0.0097(11) C19 0.0326(13) 0.0255(13) 0.0364(15) 0.0023(11) -0.0016(11) -0.0027(10) C20 0.0348(13) 0.0229(13) 0.0383(15) -0.0029(11) 0.0006(11) -0.0030(10) C21 0.0287(12) 0.0200(12) 0.0328(13) -0.0036(10) 0.0020(9) -0.0046(9) C22 0.065(2) 0.0260(14) 0.0339(16) -0.0099(12) 0.0049(14) -0.0034(13) C23 0.068(2) 0.0307(15) 0.0478(18) -0.0170(14) -0.0024(15) -0.0055(14) C24 0.081(3) 0.065(3) 0.096(3) -0.042(2) -0.029(2) -0.001(2) C25 0.106(3) 0.0344(18) 0.050(2) -0.0207(16) 0.000(2) -0.010(2) C26 0.076(3) 0.053(2) 0.059(2) -0.0226(18) 0.0147(19) -0.030(2) _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 Cu1 N6 1.9652(19) . ? Cu1 N1 2.0214(18) . ? Cu1 N2 2.0950(17) . ? Cu1 N4 2.1474(19) . ? Cu1 S1 2.4015(6) . ? Cl1 O2 1.413(2) . ? Cl1 O3 1.417(3) . ? Cl1 O4 1.421(3) . ? Cl1 O1 1.4323(19) . ? S1 C3 1.812(3) . ? S1 C2 1.821(3) . ? N1 C5 1.483(3) . ? N1 C16 1.488(3) . ? N1 C4 1.497(3) . ? N2 C6 1.356(3) . ? N2 C10 1.360(3) . ? N3 C10 1.341(3) . ? N3 C11 1.464(3) . ? N3 H3 0.74(3) . ? N4 C17 1.348(3) . ? N4 C21 1.365(3) . ? N5 C21 1.346(3) . ? N5 C22 1.464(3) . ? N5 H5 0.78(3) . ? N6 N7 1.212(3) . ? N7 N8 1.145(3) . ? C1 C2 1.515(4) . ? C1 H1A 1.03(4) . ? C1 H1B 0.93(4) . ? C1 H1C 0.87(3) . ? C2 H2A 0.97(3) . ? C2 H2B 0.86(3) . ? C3 C4 1.516(4) . ? C3 H3A 0.97(3) . ? C3 H3B 0.95(3) . ? C4 H4A 0.95(3) . ? C4 H4B 1.02(3) . ? C5 C6 1.502(3) . ? C5 H5A 0.97(3) . ? C5 H5B 0.93(3) . ? C6 C7 1.379(3) . ? C7 C8 1.388(4) . ? C7 H7 0.97(3) . ? C8 C9 1.364(4) . ? C8 H8 0.90(3) . ? C9 C10 1.417(3) . ? C9 H9 0.92(3) . ? C11 C12 1.518(3) . ? C11 H11A 1.08(3) . ? C11 H11B 0.97(3) . ? C12 C14 1.514(4) . ? C12 C15 1.515(5) . ? C12 C13 1.527(3) . ? C13 H13A 1.00(4) . ? C13 H13B 0.96(3) . ? C13 H13C 0.93(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.97(4) . ? C15 H15B 0.95(4) . ? C15 H15C 0.90(5) . ? C16 C17 1.502(3) . ? C16 H16A 0.97(3) . ? C16 H16B 0.93(3) . ? C17 C18 1.376(3) . ? C18 C19 1.395(4) . ? C18 H18 0.83(3) . ? C19 C20 1.362(4) . ? C19 H19 0.95(3) . ? C20 C21 1.417(3) . ? C20 H20 0.96(4) . ? C22 C23 1.525(4) . ? C22 H22A 0.93(3) . ? C22 H22B 1.06(3) . ? C23 C24 1.523(5) . ? C23 C25 1.530(4) . ? C23 C26 1.531(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 1.01(5) . ? C25 H25B 1.02(4) . ? C25 H25C 1.00(4) . ? C26 H26A 1.02(4) . ? C26 H26B 0.96(4) . ? C26 H26C 1.04(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Cu1 N1 178.33(7) . . ? N6 Cu1 N2 99.60(7) . . ? N1 Cu1 N2 81.66(7) . . ? N6 Cu1 N4 99.18(8) . . ? N1 Cu1 N4 81.31(7) . . ? N2 Cu1 N4 112.24(7) . . ? N6 Cu1 S1 91.85(5) . . ? N1 Cu1 S1 86.50(5) . . ? N2 Cu1 S1 128.59(5) . . ? N4 Cu1 S1 115.04(5) . . ? O2 Cl1 O3 108.93(15) . . ? O2 Cl1 O4 111.0(2) . . ? O3 Cl1 O4 106.6(3) . . ? O2 Cl1 O1 111.30(13) . . ? O3 Cl1 O1 110.49(15) . . ? O4 Cl1 O1 108.42(14) . . ? C3 S1 C2 102.98(13) . . ? C3 S1 Cu1 96.62(8) . . ? C2 S1 Cu1 99.52(8) . . ? C5 N1 C16 110.40(18) . . ? C5 N1 C4 111.63(18) . . ? C16 N1 C4 109.98(18) . . ? C5 N1 Cu1 105.16(14) . . ? C16 N1 Cu1 107.01(14) . . ? C4 N1 Cu1 112.46(14) . . ? C6 N2 C10 118.71(18) . . ? C6 N2 Cu1 110.89(14) . . ? C10 N2 Cu1 130.28(15) . . ? C10 N3 C11 122.7(2) . . ? C10 N3 H3 118(2) . . ? C11 N3 H3 118(2) . . ? C17 N4 C21 119.0(2) . . ? C17 N4 Cu1 110.82(15) . . ? C21 N4 Cu1 129.98(16) . . ? C21 N5 C22 126.6(2) . . ? C21 N5 H5 111(2) . . ? C22 N5 H5 118(2) . . ? N7 N6 Cu1 121.00(15) . . ? N8 N7 N6 178.1(2) . . ? C2 C1 H1A 112.7(18) . . ? C2 C1 H1B 111(2) . . ? H1A C1 H1B 106(3) . . ? C2 C1 H1C 106(2) . . ? H1A C1 H1C 109(3) . . ? H1B C1 H1C 112(3) . . ? C1 C2 S1 112.8(2) . . ? C1 C2 H2A 110.9(19) . . ? S1 C2 H2A 106.1(19) . . ? C1 C2 H2B 114.2(19) . . ? S1 C2 H2B 103.7(19) . . ? H2A C2 H2B 109(3) . . ? C4 C3 S1 111.85(17) . . ? C4 C3 H3A 108.8(17) . . ? S1 C3 H3A 108.6(17) . . ? C4 C3 H3B 111.7(15) . . ? S1 C3 H3B 102.7(15) . . ? H3A C3 H3B 113(2) . . ? N1 C4 C3 111.88(19) . . ? N1 C4 H4A 109.6(16) . . ? C3 C4 H4A 109.3(17) . . ? N1 C4 H4B 108.4(14) . . ? C3 C4 H4B 109.7(14) . . ? H4A C4 H4B 108(2) . . ? N1 C5 C6 109.47(19) . . ? N1 C5 H5A 109.9(15) . . ? C6 C5 H5A 109.2(15) . . ? N1 C5 H5B 109.1(18) . . ? C6 C5 H5B 110.0(17) . . ? H5A C5 H5B 109(2) . . ? N2 C6 C7 123.0(2) . . ? N2 C6 C5 114.74(19) . . ? C7 C6 C5 122.2(2) . . ? C6 C7 C8 118.3(2) . . ? C6 C7 H7 117.4(16) . . ? C8 C7 H7 124.3(16) . . ? C9 C8 C7 120.1(2) . . ? C9 C8 H8 118.5(19) . . ? C7 C8 H8 121.4(19) . . ? C8 C9 C10 119.6(2) . . ? C8 C9 H9 122.7(16) . . ? C10 C9 H9 117.7(16) . . ? N3 C10 N2 118.12(19) . . ? N3 C10 C9 121.7(2) . . ? N2 C10 C9 120.2(2) . . ? N3 C11 C12 113.6(2) . . ? N3 C11 H11A 109.2(16) . . ? C12 C11 H11A 108.7(16) . . ? N3 C11 H11B 110.7(18) . . ? C12 C11 H11B 107.2(17) . . ? H11A C11 H11B 107(2) . . ? C14 C12 C15 110.4(3) . . ? C14 C12 C11 110.8(2) . . ? C15 C12 C11 110.6(3) . . ? C14 C12 C13 108.6(2) . . ? C15 C12 C13 108.7(3) . . ? C11 C12 C13 107.7(2) . . ? C12 C13 H13A 110(2) . . ? C12 C13 H13B 110.5(18) . . ? H13A C13 H13B 108(3) . . ? C12 C13 H13C 111(2) . . ? H13A C13 H13C 111(3) . . ? H13B C13 H13C 106(3) . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 118(2) . . ? C12 C15 H15B 110(3) . . ? H15A C15 H15B 105(3) . . ? C12 C15 H15C 113(3) . . ? H15A C15 H15C 105(3) . . ? H15B C15 H15C 105(4) . . ? N1 C16 C17 112.06(18) . . ? N1 C16 H16A 105.5(15) . . ? C17 C16 H16A 110.0(15) . . ? N1 C16 H16B 110.0(17) . . ? C17 C16 H16B 109.3(17) . . ? H16A C16 H16B 110(2) . . ? N4 C17 C18 123.2(2) . . ? N4 C17 C16 115.7(2) . . ? C18 C17 C16 120.9(2) . . ? C17 C18 C19 117.6(2) . . ? C17 C18 H18 117.0(19) . . ? C19 C18 H18 125.3(19) . . ? C20 C19 C18 120.9(2) . . ? C20 C19 H19 116.8(17) . . ? C18 C19 H19 122.2(17) . . ? C19 C20 C21 119.0(2) . . ? C19 C20 H20 120(2) . . ? C21 C20 H20 121(2) . . ? N5 C21 N4 116.9(2) . . ? N5 C21 C20 122.9(2) . . ? N4 C21 C20 120.2(2) . . ? N5 C22 C23 115.1(3) . . ? N5 C22 H22A 108.2(18) . . ? C23 C22 H22A 111.1(17) . . ? N5 C22 H22B 105.6(16) . . ? C23 C22 H22B 107.7(16) . . ? H22A C22 H22B 109(2) . . ? C24 C23 C22 110.2(3) . . ? C24 C23 C25 110.0(3) . . ? C22 C23 C25 106.9(3) . . ? C24 C23 C26 110.4(3) . . ? C22 C23 C26 110.2(3) . . ? C25 C23 C26 109.2(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 111(3) . . ? C23 C25 H25B 110(2) . . ? H25A C25 H25B 106(3) . . ? C23 C25 H25C 109(2) . . ? H25A C25 H25C 115(4) . . ? H25B C25 H25C 105(3) . . ? C23 C26 H26A 109.1(19) . . ? C23 C26 H26B 109(2) . . ? H26A C26 H26B 111(3) . . ? C23 C26 H26C 114(2) . . ? H26A C26 H26C 101(3) . . ? H26B C26 H26C 112(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Cu1 S1 C3 179.77(11) . . . . ? N1 Cu1 S1 C3 -0.50(11) . . . . ? N2 Cu1 S1 C3 75.93(11) . . . . ? N4 Cu1 S1 C3 -79.21(11) . . . . ? N6 Cu1 S1 C2 -75.83(11) . . . . ? N1 Cu1 S1 C2 103.91(11) . . . . ? N2 Cu1 S1 C2 -179.67(12) . . . . ? N4 Cu1 S1 C2 25.19(12) . . . . ? N6 Cu1 N1 C5 106(3) . . . . ? N2 Cu1 N1 C5 -32.95(14) . . . . ? N4 Cu1 N1 C5 -147.12(15) . . . . ? S1 Cu1 N1 C5 96.88(14) . . . . ? N6 Cu1 N1 C16 -137(3) . . . . ? N2 Cu1 N1 C16 84.47(14) . . . . ? N4 Cu1 N1 C16 -29.70(13) . . . . ? S1 Cu1 N1 C16 -145.69(13) . . . . ? N6 Cu1 N1 C4 -16(3) . . . . ? N2 Cu1 N1 C4 -154.65(16) . . . . ? N4 Cu1 N1 C4 91.18(16) . . . . ? S1 Cu1 N1 C4 -24.81(15) . . . . ? N6 Cu1 N2 C6 -163.59(15) . . . . ? N1 Cu1 N2 C6 15.30(15) . . . . ? N4 Cu1 N2 C6 92.29(16) . . . . ? S1 Cu1 N2 C6 -63.40(16) . . . . ? N6 Cu1 N2 C10 20.5(2) . . . . ? N1 Cu1 N2 C10 -160.6(2) . . . . ? N4 Cu1 N2 C10 -83.6(2) . . . . ? S1 Cu1 N2 C10 120.68(17) . . . . ? N6 Cu1 N4 C17 -164.75(14) . . . . ? N1 Cu1 N4 C17 16.87(14) . . . . ? N2 Cu1 N4 C17 -60.36(15) . . . . ? S1 Cu1 N4 C17 98.84(14) . . . . ? N6 Cu1 N4 C21 10.6(2) . . . . ? N1 Cu1 N4 C21 -167.8(2) . . . . ? N2 Cu1 N4 C21 115.01(19) . . . . ? S1 Cu1 N4 C21 -85.78(19) . . . . ? N1 Cu1 N6 N7 -32(3) . . . . ? N2 Cu1 N6 N7 106.84(18) . . . . ? N4 Cu1 N6 N7 -138.56(18) . . . . ? S1 Cu1 N6 N7 -22.83(18) . . . . ? Cu1 N6 N7 N8 -157(8) . . . . ? C3 S1 C2 C1 -72.8(2) . . . . ? Cu1 S1 C2 C1 -171.9(2) . . . . ? C2 S1 C3 C4 -76.1(2) . . . . ? Cu1 S1 C3 C4 25.34(19) . . . . ? C5 N1 C4 C3 -69.0(3) . . . . ? C16 N1 C4 C3 168.13(19) . . . . ? Cu1 N1 C4 C3 49.0(2) . . . . ? S1 C3 C4 N1 -49.2(3) . . . . ? C16 N1 C5 C6 -69.6(2) . . . . ? C4 N1 C5 C6 167.77(19) . . . . ? Cu1 N1 C5 C6 45.5(2) . . . . ? C10 N2 C6 C7 2.1(3) . . . . ? Cu1 N2 C6 C7 -174.36(19) . . . . ? C10 N2 C6 C5 -176.5(2) . . . . ? Cu1 N2 C6 C5 7.1(2) . . . . ? N1 C5 C6 N2 -35.7(3) . . . . ? N1 C5 C6 C7 145.7(2) . . . . ? N2 C6 C7 C8 -0.5(4) . . . . ? C5 C6 C7 C8 178.0(2) . . . . ? C6 C7 C8 C9 -0.9(4) . . . . ? C7 C8 C9 C10 0.7(4) . . . . ? C11 N3 C10 N2 -172.0(2) . . . . ? C11 N3 C10 C9 8.9(4) . . . . ? C6 N2 C10 N3 178.6(2) . . . . ? Cu1 N2 C10 N3 -5.8(3) . . . . ? C6 N2 C10 C9 -2.3(3) . . . . ? Cu1 N2 C10 C9 173.40(16) . . . . ? C8 C9 C10 N3 -180.0(2) . . . . ? C8 C9 C10 N2 0.9(3) . . . . ? C10 N3 C11 C12 167.5(2) . . . . ? N3 C11 C12 C14 -60.8(3) . . . . ? N3 C11 C12 C15 61.9(3) . . . . ? N3 C11 C12 C13 -179.5(2) . . . . ? C5 N1 C16 C17 153.06(19) . . . . ? C4 N1 C16 C17 -83.3(2) . . . . ? Cu1 N1 C16 C17 39.1(2) . . . . ? C21 N4 C17 C18 -0.1(3) . . . . ? Cu1 N4 C17 C18 175.88(18) . . . . ? C21 N4 C17 C16 -174.92(19) . . . . ? Cu1 N4 C17 C16 1.0(2) . . . . ? N1 C16 C17 N4 -26.8(3) . . . . ? N1 C16 C17 C18 158.2(2) . . . . ? N4 C17 C18 C19 -1.6(3) . . . . ? C16 C17 C18 C19 172.9(2) . . . . ? C17 C18 C19 C20 1.8(4) . . . . ? C18 C19 C20 C21 -0.4(4) . . . . ? C22 N5 C21 N4 -170.6(2) . . . . ? C22 N5 C21 C20 9.0(4) . . . . ? C17 N4 C21 N5 -178.7(2) . . . . ? Cu1 N4 C21 N5 6.2(3) . . . . ? C17 N4 C21 C20 1.6(3) . . . . ? Cu1 N4 C21 C20 -173.46(17) . . . . ? C19 C20 C21 N5 179.0(2) . . . . ? C19 C20 C21 N4 -1.4(4) . . . . ? C21 N5 C22 C23 -104.9(3) . . . . ? N5 C22 C23 C24 -57.8(4) . . . . ? N5 C22 C23 C25 -177.3(3) . . . . ? N5 C22 C23 C26 64.2(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 N6 0.74(3) 2.20(3) 2.906(3) 160(3) . N5 H5 N6 0.78(3) 2.11(3) 2.881(3) 170(3) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.711 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.067 #===END