# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2061 data_CUDENT # paper complex no. 7 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [CuL](MeOSO3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H24 Cu N8 O10 S2' _chemical_formula_weight 544.03 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' '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 10.097(1) _cell_length_b 10.143(1) _cell_length_c 11.550(1) _cell_angle_alpha 114.325(2) _cell_angle_beta 98.612(2) _cell_angle_gamma 98.146(2) _cell_volume 1038.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4073 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.04 _exptl_crystal_description Rhomboid _exptl_crystal_colour Purple _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 562 _exptl_absorpt_coefficient_mu 1.321 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 10810 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 29.00 _reflns_number_total 4835 _reflns_number_gt 3707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^] 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 4835 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.005 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 0.68740(3) 0.40872(3) 0.35532(3) 0.01958(11) Uani 1 1 d . . . C101 C 0.7234(3) 0.1702(3) 0.1285(3) 0.0262(6) Uani 1 1 d . . . H10A H 0.8006 0.2121 0.1010 0.031 Uiso 1 1 calc R . . H10B H 0.6697 0.0769 0.0534 0.031 Uiso 1 1 calc R . . N102 N 0.6355(2) 0.2761(2) 0.1701(2) 0.0195(5) Uani 1 1 d . . . C103 C 0.5479(3) 0.2839(3) 0.0802(3) 0.0211(6) Uani 1 1 d . . . N104 N 0.4657(2) 0.3866(2) 0.1113(2) 0.0224(5) Uani 1 1 d . . . H104 H 0.4011 0.3775 0.0464 0.027 Uiso 1 1 calc R . . C105 C 0.4730(3) 0.5000(3) 0.2305(3) 0.0211(6) Uani 1 1 d . . . N106 N 0.5576(2) 0.5271(2) 0.3359(2) 0.0200(5) Uani 1 1 d . . . H106 H 0.5570 0.6067 0.4063 0.024 Uiso 1 1 calc R . . N131 N 0.5255(3) 0.1980(3) -0.0481(2) 0.0306(6) Uani 1 1 d . . . H13A H 0.5724 0.1291 -0.0777 0.037 Uiso 1 1 calc R . . H13B H 0.4639 0.2104 -0.1030 0.037 Uiso 1 1 calc R . . O151 O 0.3763(2) 0.5728(2) 0.21690(19) 0.0281(5) Uani 1 1 d . . . C152 C 0.3793(3) 0.7117(3) 0.3261(3) 0.0306(7) Uani 1 1 d . . . H15A H 0.3027 0.7530 0.3036 0.046 Uiso 1 1 calc R . . H15B H 0.4665 0.7819 0.3463 0.046 Uiso 1 1 calc R . . H15C H 0.3706 0.6944 0.4024 0.046 Uiso 1 1 calc R . . C201 C 0.7787(3) 0.1389(3) 0.2423(3) 0.0223(6) Uani 1 1 d . . . H20A H 0.7096 0.0626 0.2469 0.027 Uiso 1 1 calc R . . H20B H 0.8633 0.1011 0.2300 0.027 Uiso 1 1 calc R . . N202 N 0.8092(2) 0.2771(2) 0.3631(2) 0.0196(5) Uani 1 1 d . . . C203 C 0.8948(3) 0.2869(3) 0.4632(3) 0.0188(5) Uani 1 1 d . . . N204 N 0.9259(2) 0.4121(2) 0.5818(2) 0.0209(5) Uani 1 1 d . . . H204 H 0.9966 0.4194 0.6406 0.025 Uiso 1 1 calc R . . C205 C 0.8589(3) 0.5262(3) 0.6179(3) 0.0206(6) Uani 1 1 d . . . N206 N 0.7601(2) 0.5379(2) 0.5421(2) 0.0223(5) Uani 1 1 d . . . H206 H 0.7205 0.6121 0.5777 0.027 Uiso 1 1 calc R . . N231 N 0.9643(2) 0.1835(2) 0.4635(2) 0.0238(5) Uani 1 1 d . . . H23A H 0.9533 0.1012 0.3916 0.029 Uiso 1 1 calc R . . H23B H 1.0209 0.1981 0.5356 0.029 Uiso 1 1 calc R . . O251 O 0.9135(2) 0.6191(2) 0.74390(18) 0.0264(5) Uani 1 1 d . . . C252 C 0.8590(3) 0.7489(3) 0.8019(3) 0.0298(7) Uani 1 1 d . . . H25A H 0.9077 0.8071 0.8937 0.045 Uiso 1 1 calc R . . H25B H 0.7608 0.7184 0.7965 0.045 Uiso 1 1 calc R . . H25C H 0.8713 0.8095 0.7550 0.045 Uiso 1 1 calc R . . S1 S 0.40458(7) 0.10308(7) 0.31310(7) 0.02322(17) Uani 1 1 d . . . S2 S 0.83749(8) 0.70673(8) 0.19737(7) 0.02457(17) Uani 1 1 d . . . O11 O 0.4289(2) 0.2620(2) 0.39419(19) 0.0270(5) Uani 1 1 d . . . O12 O 0.3666(2) 0.0617(2) 0.1754(2) 0.0345(5) Uani 1 1 d . . . O13 O 0.5111(2) 0.0387(2) 0.3507(2) 0.0301(5) Uani 1 1 d . . . O14 O 0.2653(2) 0.0311(2) 0.3348(2) 0.0318(5) Uani 1 1 d . . . C141 C 0.2630(3) 0.0560(4) 0.4666(3) 0.0344(7) Uani 1 1 d . . . H14A H 0.1730 0.0063 0.4680 0.052 Uiso 1 1 calc R . . H14B H 0.2794 0.1628 0.5226 0.052 Uiso 1 1 calc R . . H14C H 0.3349 0.0157 0.4987 0.052 Uiso 1 1 calc R . . O21 O 0.8639(2) 0.5897(2) 0.2332(2) 0.0349(5) Uani 1 1 d . . . O22 O 0.6947(2) 0.6923(2) 0.1472(2) 0.0352(5) Uani 1 1 d . . . O23 O 0.9090(2) 0.8525(2) 0.29922(19) 0.0331(5) Uani 1 1 d . . . C241 C 1.0470(4) 0.6923(4) 0.0919(4) 0.0472(9) Uani 1 1 d . . . H24A H 1.0739 0.6757 0.0098 0.071 Uiso 1 1 calc R . . H24B H 1.0702 0.6166 0.1184 0.071 Uiso 1 1 calc R . . H24C H 1.0962 0.7910 0.1598 0.071 Uiso 1 1 calc R . . O24 O 0.8996(2) 0.6826(2) 0.0736(2) 0.0364(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0250(2) 0.01748(18) 0.01317(17) 0.00356(13) 0.00028(13) 0.01018(13) C101 0.0330(17) 0.0295(15) 0.0133(13) 0.0039(11) 0.0034(12) 0.0183(13) N102 0.0218(12) 0.0206(11) 0.0145(11) 0.0058(9) 0.0009(9) 0.0096(9) C103 0.0244(15) 0.0181(13) 0.0178(13) 0.0049(11) 0.0034(11) 0.0068(11) N104 0.0231(12) 0.0232(12) 0.0159(11) 0.0046(9) -0.0037(9) 0.0115(9) C105 0.0231(14) 0.0158(13) 0.0253(14) 0.0087(11) 0.0056(12) 0.0079(10) N106 0.0268(13) 0.0172(11) 0.0129(10) 0.0037(9) 0.0011(9) 0.0081(9) N131 0.0398(16) 0.0329(14) 0.0138(11) 0.0038(10) -0.0016(11) 0.0212(12) O151 0.0317(12) 0.0226(10) 0.0221(10) 0.0023(8) -0.0024(9) 0.0153(9) C152 0.0345(18) 0.0200(14) 0.0301(16) 0.0039(12) 0.0008(13) 0.0139(12) C201 0.0269(15) 0.0200(14) 0.0168(13) 0.0044(11) 0.0012(11) 0.0111(11) N202 0.0238(12) 0.0189(11) 0.0145(10) 0.0052(9) 0.0024(9) 0.0092(9) C203 0.0188(14) 0.0196(13) 0.0187(13) 0.0078(11) 0.0050(11) 0.0078(10) N204 0.0235(12) 0.0223(12) 0.0132(11) 0.0053(9) -0.0032(9) 0.0098(9) C205 0.0249(15) 0.0180(13) 0.0180(13) 0.0065(11) 0.0061(11) 0.0054(11) N206 0.0277(13) 0.0201(12) 0.0156(11) 0.0038(9) 0.0010(10) 0.0121(10) N231 0.0298(13) 0.0213(12) 0.0182(11) 0.0060(9) -0.0001(10) 0.0136(10) O251 0.0308(11) 0.0242(10) 0.0165(9) 0.0019(8) -0.0017(8) 0.0135(8) C252 0.0381(18) 0.0241(15) 0.0188(14) -0.0003(12) 0.0034(13) 0.0156(13) S1 0.0289(4) 0.0198(3) 0.0192(3) 0.0052(3) 0.0066(3) 0.0101(3) S2 0.0286(4) 0.0247(4) 0.0172(3) 0.0073(3) -0.0018(3) 0.0103(3) O11 0.0392(12) 0.0184(10) 0.0203(10) 0.0040(8) 0.0073(9) 0.0111(9) O12 0.0505(15) 0.0296(12) 0.0188(10) 0.0039(9) 0.0063(10) 0.0189(10) O13 0.0304(12) 0.0303(11) 0.0315(12) 0.0127(9) 0.0076(9) 0.0159(9) O14 0.0277(12) 0.0335(12) 0.0322(12) 0.0137(10) 0.0045(9) 0.0058(9) C141 0.0352(18) 0.0377(18) 0.0335(17) 0.0166(15) 0.0120(14) 0.0102(14) O21 0.0307(12) 0.0356(12) 0.0404(13) 0.0225(11) -0.0049(10) 0.0092(9) O22 0.0314(12) 0.0425(13) 0.0279(11) 0.0134(10) -0.0047(9) 0.0161(10) O23 0.0394(13) 0.0258(11) 0.0230(11) 0.0027(9) -0.0019(9) 0.0089(9) C241 0.042(2) 0.052(2) 0.037(2) 0.0096(17) 0.0130(17) 0.0078(17) O24 0.0409(14) 0.0444(14) 0.0200(10) 0.0101(10) 0.0053(10) 0.0134(11) _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 N102 1.938(2) . y Cu1 N106 1.947(2) . y Cu1 N202 1.958(2) . y Cu1 N206 1.958(2) . y C101 N102 1.464(3) . ? C101 C201 1.521(4) . ? N102 C103 1.295(3) . ? C103 N131 1.337(3) . ? C103 N104 1.390(3) . ? N104 C105 1.366(3) . ? C105 N106 1.278(3) . ? C105 O151 1.333(3) . ? O151 C152 1.445(3) . ? C201 N202 1.464(3) . ? N202 C203 1.295(3) . ? C203 N231 1.342(3) . ? C203 N204 1.383(3) . ? N204 C205 1.371(3) . ? C205 N206 1.278(3) . ? C205 O251 1.339(3) . ? O251 C252 1.440(3) . ? S1 O13 1.436(2) . ? S1 O12 1.440(2) . ? S1 O11 1.4526(19) . ? S1 O14 1.594(2) . ? S2 O22 1.433(2) . ? S2 O23 1.450(2) . ? S2 O21 1.453(2) . ? S2 O24 1.587(2) . ? O14 C141 1.441(4) . ? C241 O24 1.455(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 N102 Cu1 N106 91.70(9) . . y N102 Cu1 N202 84.42(9) . . y N106 Cu1 N202 175.71(9) . . y N102 Cu1 N206 173.65(9) . . y N106 Cu1 N206 93.79(9) . . y N202 Cu1 N206 90.19(9) . . y N102 C101 C201 108.7(2) . . ? C103 N102 C101 117.8(2) . . ? C103 N102 Cu1 128.01(18) . . ? C101 N102 Cu1 113.49(16) . . ? N102 C103 N131 125.6(2) . . ? N102 C103 N104 121.3(2) . . ? N131 C103 N104 113.1(2) . . ? C105 N104 C103 127.7(2) . . ? N106 C105 O151 127.1(2) . . ? N106 C105 N104 124.6(2) . . ? O151 C105 N104 108.3(2) . . ? C105 N106 Cu1 126.09(18) . . ? C105 O151 C152 117.8(2) . . ? N202 C201 C101 108.6(2) . . ? C203 N202 C201 117.8(2) . . ? C203 N202 Cu1 128.80(18) . . ? C201 N202 Cu1 112.54(16) . . ? N202 C203 N231 125.2(2) . . ? N202 C203 N204 121.2(2) . . ? N231 C203 N204 113.5(2) . . ? C205 N204 C203 127.2(2) . . ? N206 C205 O251 127.0(2) . . ? N206 C205 N204 124.5(2) . . ? O251 C205 N204 108.5(2) . . ? C205 N206 Cu1 127.02(19) . . ? C205 O251 C252 117.8(2) . . ? O13 S1 O12 114.94(13) . . ? O13 S1 O11 112.74(13) . . ? O12 S1 O11 113.32(12) . . ? O13 S1 O14 107.70(12) . . ? O12 S1 O14 100.84(13) . . ? O11 S1 O14 106.00(12) . . ? O22 S2 O23 115.08(13) . . ? O22 S2 O21 113.56(14) . . ? O23 S2 O21 111.69(13) . . ? O22 S2 O24 102.09(13) . . ? O23 S2 O24 106.76(13) . . ? O21 S2 O24 106.57(13) . . ? C141 O14 S1 116.66(19) . . ? C241 O24 S2 116.4(2) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.717 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.096 #===end data_CUOMCG # paper complex no. 8 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [CuL](EtOSO3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 Cu N8 O10 S2' _chemical_formula_weight 600.14 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' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.246(2) _cell_length_b 8.2144(11) _cell_length_c 21.292(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.214(2) _cell_angle_gamma 90.00 _cell_volume 2452.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4409 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.95 _exptl_crystal_description Lath _exptl_crystal_colour Purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 1.127 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD area detector' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 14319 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.6 _reflns_number_total 5521 _reflns_number_gt 3831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL; PLATON' _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^)+(0.0406P)^2^] 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 5520 _refine_ls_number_parameters 325 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.148 _refine_ls_shift/su_mean 0.007 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 0.60426(2) 0.30730(4) 0.062988(13) 0.01599(9) Uani 1 1 d . A . C111 C 0.7301(4) 0.4173(9) 0.1736(3) 0.0233(18) Uani 0.45 1 d PD A 1 H11B H 0.7684 0.3743 0.2136 0.028 Uiso 0.45 1 calc PR A 1 H11A H 0.7113 0.5303 0.1818 0.028 Uiso 0.45 1 calc PR A 1 C101 C 0.7472(3) 0.3416(8) 0.1751(3) 0.0207(15) Uani 0.55 1 d PD A 2 H10B H 0.7785 0.2356 0.1867 0.025 Uiso 0.55 1 calc PR A 2 H10A H 0.7592 0.4126 0.2132 0.025 Uiso 0.55 1 calc PR A 2 N102 N 0.64361(14) 0.3166(3) 0.15557(9) 0.0170(4) Uani 1 1 d D . . C103 C 0.60090(17) 0.2521(3) 0.19768(11) 0.0169(5) Uani 1 1 d . A . N104 N 0.50980(15) 0.1881(3) 0.18141(10) 0.0245(5) Uani 1 1 d . . . H104 H 0.4870 0.1398 0.2124 0.029 Uiso 1 1 calc R A . C105 C 0.45097(17) 0.1908(3) 0.12322(12) 0.0205(5) Uani 1 1 d . A . N106 N 0.47531(14) 0.2466(3) 0.07292(10) 0.0196(5) Uani 1 1 d . . . H106 H 0.4298 0.2592 0.0394 0.023 Uiso 1 1 calc R A . N131 N 0.63498(16) 0.2387(3) 0.26024(10) 0.0279(6) Uani 1 1 d . . . H13A H 0.6921 0.2763 0.2761 0.033 Uiso 1 1 calc R A . H13B H 0.6002 0.1923 0.2855 0.033 Uiso 1 1 calc R . . O151 O 0.36784(13) 0.1238(3) 0.12942(8) 0.0287(5) Uani 1 1 d . . . C152 C 0.29434(19) 0.1149(4) 0.07227(12) 0.0293(7) Uani 1 1 d . A . H15A H 0.3167 0.0471 0.0394 0.035 Uiso 1 1 calc R . . H15B H 0.2798 0.2252 0.0545 0.035 Uiso 1 1 calc R . . C153 C 0.2075(2) 0.0416(4) 0.09068(14) 0.0359(8) Uani 1 1 d . . . H15C H 0.1571 0.0335 0.0530 0.054 Uiso 1 1 calc R A . H15D H 0.1856 0.1103 0.1228 0.054 Uiso 1 1 calc R . . H15E H 0.2227 -0.0674 0.1084 0.054 Uiso 1 1 calc R . . C201 C 0.78939(18) 0.4180(4) 0.12255(11) 0.0235(6) Uani 1 1 d D . . H20B H 0.8198 0.5260 0.1214 0.028 Uiso 1 1 calc R A 1 H20A H 0.8407 0.3359 0.1328 0.028 Uiso 1 1 calc R A 1 N202 N 0.73294(14) 0.3822(3) 0.05941(9) 0.0173(5) Uani 1 1 d . A . C203 C 0.77014(17) 0.4096(3) 0.00958(11) 0.0180(5) Uani 1 1 d . . . N204 N 0.71827(14) 0.3911(3) -0.05179(10) 0.0204(5) Uani 1 1 d . A . H204 H 0.7500 0.4038 -0.0833 0.024 Uiso 1 1 calc R . . C205 C 0.62335(18) 0.3553(3) -0.06850(11) 0.0175(5) Uani 1 1 d . . . N206 N 0.56895(14) 0.3237(3) -0.02931(9) 0.0193(5) Uani 1 1 d . A . H206 H 0.5085 0.3073 -0.0455 0.023 Uiso 1 1 calc R . . N231 N 0.86021(15) 0.4569(3) 0.00987(11) 0.0331(6) Uani 1 1 d . A . H23A H 0.8993 0.4716 0.0463 0.040 Uiso 1 1 calc R . . H23B H 0.8803 0.4731 -0.0264 0.040 Uiso 1 1 calc R . . O251 O 0.59951(12) 0.3598(2) -0.13237(8) 0.0230(4) Uani 1 1 d . A . C252 C 0.50184(18) 0.3147(4) -0.15948(12) 0.0251(6) Uani 1 1 d . . . H25A H 0.4565 0.3801 -0.1397 0.030 Uiso 1 1 calc R A . H25B H 0.4911 0.1982 -0.1512 0.030 Uiso 1 1 calc R . . C253 C 0.4862(2) 0.3457(4) -0.23017(12) 0.0308(7) Uani 1 1 d . A . H25C H 0.4209 0.3149 -0.2493 0.046 Uiso 1 1 calc R . . H25D H 0.5315 0.2809 -0.2494 0.046 Uiso 1 1 calc R . . H25E H 0.4959 0.4615 -0.2379 0.046 Uiso 1 1 calc R . . S1 S 0.41154(5) 0.00751(9) 0.34369(3) 0.02227(16) Uani 1 1 d . . . S2 S 0.68938(4) -0.12773(9) 0.09327(3) 0.01988(15) Uani 1 1 d . . . O11 O 0.35631(13) -0.1431(2) 0.30853(9) 0.0290(5) Uani 1 1 d . . . C12 C 0.2921(2) -0.1102(4) 0.24834(13) 0.0330(7) Uani 1 1 d . . . H1A H 0.2977 -0.1985 0.2176 0.040 Uiso 1 1 calc R . . H1B H 0.3108 -0.0068 0.2301 0.040 Uiso 1 1 calc R . . C13 C 0.1915(2) -0.0984(4) 0.25799(15) 0.0359(8) Uani 1 1 d . . . H1C H 0.1491 -0.0917 0.2164 0.054 Uiso 1 1 calc R . . H1D H 0.1837 -0.0007 0.2830 0.054 Uiso 1 1 calc R . . H1E H 0.1753 -0.1950 0.2809 0.054 Uiso 1 1 calc R . . O12 O 0.46393(14) -0.0660(3) 0.40091(9) 0.0338(5) Uani 1 1 d . . . O13 O 0.47163(13) 0.0717(3) 0.30161(9) 0.0294(5) Uani 1 1 d . . . O14 O 0.33973(13) 0.1219(3) 0.35607(9) 0.0282(5) Uani 1 1 d . . . O21 O 0.79611(13) -0.1521(2) 0.08109(9) 0.0281(5) Uani 1 1 d . . . C22 C 0.8601(2) -0.0161(4) 0.09789(15) 0.0373(8) Uani 1 1 d . . . H2A H 0.8593 0.0179 0.1424 0.045 Uiso 1 1 calc R . . H2B H 0.8394 0.0774 0.0694 0.045 Uiso 1 1 calc R . . C23 C 0.9582(2) -0.0671(5) 0.09109(18) 0.0534(10) Uani 1 1 d . . . H2C H 1.0022 0.0245 0.1019 0.080 Uiso 1 1 calc R . . H2D H 0.9583 -0.1010 0.0470 0.080 Uiso 1 1 calc R . . H2E H 0.9786 -0.1583 0.1200 0.080 Uiso 1 1 calc R . . O22 O 0.69462(13) -0.1298(3) 0.16179(8) 0.0331(5) Uani 1 1 d . . . O23 O 0.65587(14) 0.0239(2) 0.06388(9) 0.0319(5) Uani 1 1 d . . . O24 O 0.64195(13) -0.2680(2) 0.06104(8) 0.0240(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01283(15) 0.02376(18) 0.01111(14) 0.00059(13) 0.00139(11) -0.00186(14) C111 0.018(3) 0.032(5) 0.021(3) -0.007(4) 0.004(3) -0.004(3) C101 0.010(2) 0.036(4) 0.015(2) 0.002(3) 0.0005(19) 0.001(2) N102 0.0158(10) 0.0217(12) 0.0133(10) -0.0011(9) 0.0022(8) -0.0027(9) C103 0.0144(12) 0.0197(14) 0.0162(12) -0.0018(10) 0.0020(10) 0.0030(10) N104 0.0208(11) 0.0402(15) 0.0125(10) 0.0046(10) 0.0033(9) -0.0145(11) C105 0.0181(12) 0.0249(15) 0.0187(12) -0.0041(11) 0.0039(10) -0.0038(11) N106 0.0142(10) 0.0304(13) 0.0135(10) 0.0027(9) 0.0007(8) -0.0023(9) N131 0.0193(11) 0.0506(17) 0.0126(10) 0.0064(10) -0.0002(9) -0.0073(11) O151 0.0220(10) 0.0504(14) 0.0136(9) -0.0017(8) 0.0030(8) -0.0167(9) C152 0.0213(14) 0.048(2) 0.0161(13) -0.0022(12) -0.0025(11) -0.0107(13) C153 0.0238(15) 0.057(2) 0.0267(15) -0.0060(14) 0.0039(12) -0.0157(14) C201 0.0212(13) 0.0332(17) 0.0145(12) 0.0006(11) -0.0013(11) -0.0094(12) N202 0.0158(10) 0.0224(13) 0.0136(10) -0.0011(9) 0.0021(8) -0.0023(9) C203 0.0157(12) 0.0240(15) 0.0139(12) -0.0002(10) 0.0019(10) -0.0016(11) N204 0.0140(10) 0.0351(14) 0.0123(10) 0.0003(9) 0.0032(8) -0.0045(10) C205 0.0168(12) 0.0205(15) 0.0147(11) 0.0001(10) 0.0015(10) 0.0003(10) N206 0.0144(10) 0.0269(13) 0.0162(10) 0.0016(9) 0.0017(8) -0.0028(9) N231 0.0176(12) 0.068(2) 0.0145(11) -0.0008(11) 0.0036(9) -0.0149(12) O251 0.0169(9) 0.0395(12) 0.0116(8) 0.0004(8) 0.0001(7) -0.0047(8) C252 0.0150(12) 0.0401(18) 0.0190(13) 0.0010(12) -0.0005(10) -0.0019(12) C253 0.0207(14) 0.052(2) 0.0179(13) -0.0008(12) 0.0000(11) 0.0007(13) S1 0.0184(3) 0.0334(4) 0.0153(3) 0.0015(3) 0.0036(2) -0.0010(3) S2 0.0144(3) 0.0281(4) 0.0159(3) -0.0007(3) -0.0005(2) 0.0019(3) O11 0.0268(11) 0.0306(12) 0.0283(10) -0.0014(8) 0.0016(8) -0.0009(8) C12 0.0267(15) 0.047(2) 0.0229(14) -0.0064(14) -0.0013(12) -0.0050(14) C13 0.0266(15) 0.048(2) 0.0326(16) -0.0074(15) 0.0036(13) -0.0007(14) O12 0.0250(10) 0.0538(15) 0.0205(10) 0.0094(9) -0.0014(8) 0.0013(10) O13 0.0215(10) 0.0418(13) 0.0273(10) 0.0042(9) 0.0110(8) -0.0039(9) O14 0.0250(10) 0.0350(12) 0.0267(10) -0.0030(9) 0.0100(8) -0.0002(9) O21 0.0169(9) 0.0357(13) 0.0316(11) -0.0011(9) 0.0042(8) -0.0008(8) C22 0.0245(15) 0.049(2) 0.0359(17) 0.0056(15) -0.0010(13) -0.0121(15) C23 0.0232(17) 0.079(3) 0.056(2) 0.018(2) 0.0015(16) -0.0072(18) O22 0.0236(10) 0.0602(16) 0.0141(9) -0.0004(9) -0.0005(8) -0.0035(10) O23 0.0361(12) 0.0271(12) 0.0305(11) -0.0009(9) 0.0000(9) 0.0096(9) O24 0.0212(9) 0.0261(12) 0.0239(10) -0.0017(8) 0.0018(8) -0.0031(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N206 1.945(2) . Y Cu1 N202 1.948(2) . Y Cu1 N106 1.951(2) . Y Cu1 N102 1.9529(19) . Y C111 N102 1.478(5) . ? C111 C201 1.491(6) . ? C111 H11B 0.9900 . ? C111 H11A 0.9900 . ? C101 N102 1.475(4) . ? C101 C201 1.498(5) . ? C101 H10B 0.9900 . ? C101 H10A 0.9900 . ? N102 C103 1.284(3) . ? C103 N131 1.339(3) . ? C103 N104 1.386(3) . ? N104 C105 1.367(3) . ? N104 H104 0.8800 . ? C105 N106 1.269(3) . ? C105 O151 1.333(3) . ? N106 H106 0.8800 . ? N131 H13A 0.8800 . ? N131 H13B 0.8800 . ? O151 C152 1.460(3) . ? C152 C153 1.490(4) . ? C152 H15A 0.9900 . ? C152 H15B 0.9900 . ? C153 H15C 0.9800 . ? C153 H15D 0.9800 . ? C153 H15E 0.9800 . ? C201 N202 1.469(3) . ? C201 H20B 0.9900 . ? C201 H20A 0.9900 . ? N202 C203 1.287(3) . ? C203 N231 1.339(3) . ? C203 N204 1.391(3) . ? N204 C205 1.368(3) . ? N204 H204 0.8800 . ? C205 N206 1.262(3) . ? C205 O251 1.343(3) . ? N206 H206 0.8800 . ? N231 H23A 0.8800 . ? N231 H23B 0.8800 . ? O251 C252 1.456(3) . ? C252 C253 1.504(4) . ? C252 H25A 0.9900 . ? C252 H25B 0.9900 . ? C253 H25C 0.9800 . ? C253 H25D 0.9800 . ? C253 H25E 0.9800 . ? S1 O12 1.4435(19) . ? S1 O13 1.444(2) . ? S1 O14 1.447(2) . ? S1 O11 1.581(2) . ? S2 O23 1.437(2) . ? S2 O24 1.4458(19) . ? S2 O22 1.4477(19) . ? S2 O21 1.5997(19) . ? O11 C12 1.462(3) . ? C12 C13 1.486(4) . ? C12 H1A 0.9900 . ? C12 H1B 0.9900 . ? C13 H1C 0.9800 . ? C13 H1D 0.9800 . ? C13 H1E 0.9800 . ? O21 C22 1.446(4) . ? C22 C23 1.491(4) . ? C22 H2A 0.9900 . ? C22 H2B 0.9900 . ? C23 H2C 0.9800 . ? C23 H2D 0.9800 . ? C23 H2E 0.9800 . ? 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 N206 Cu1 N202 90.87(8) . . Y N206 Cu1 N106 92.72(8) . . Y N202 Cu1 N106 174.72(9) . . Y N206 Cu1 N102 173.58(9) . . Y N202 Cu1 N102 85.61(8) . . Y N106 Cu1 N102 90.45(8) . . Y N102 C111 C201 111.5(4) . . ? N102 C111 H11B 109.3 . . ? C201 C111 H11B 109.3 . . ? N102 C111 H11A 109.3 . . ? C201 C111 H11A 109.3 . . ? H11B C111 H11A 108.0 . . ? N102 C101 C201 111.2(3) . . ? N102 C101 H10B 109.4 . . ? C201 C101 H10B 109.4 . . ? N102 C101 H10A 109.4 . . ? C201 C101 H10A 109.4 . . ? H10B C101 H10A 108.0 . . ? C103 N102 C101 115.8(3) . . ? C103 N102 C111 121.7(3) . . ? C101 N102 C111 26.1(3) . . ? C103 N102 Cu1 127.02(17) . . ? C101 N102 Cu1 112.6(2) . . ? C111 N102 Cu1 111.2(3) . . ? N102 C103 N131 126.6(2) . . ? N102 C103 N104 121.4(2) . . ? N131 C103 N104 112.1(2) . . ? C105 N104 C103 128.1(2) . . ? C105 N104 H104 116.0 . . ? C103 N104 H104 116.0 . . ? N106 C105 O151 127.8(2) . . ? N106 C105 N104 123.7(2) . . ? O151 C105 N104 108.4(2) . . ? C105 N106 Cu1 125.98(17) . . ? C105 N106 H106 117.0 . . ? Cu1 N106 H106 117.0 . . ? C103 N131 H13A 120.0 . . ? C103 N131 H13B 120.0 . . ? H13A N131 H13B 120.0 . . ? C105 O151 C152 117.2(2) . . ? O151 C152 C153 107.9(2) . . ? O151 C152 H15A 110.1 . . ? C153 C152 H15A 110.1 . . ? O151 C152 H15B 110.1 . . ? C153 C152 H15B 110.1 . . ? H15A C152 H15B 108.4 . . ? C152 C153 H15C 109.5 . . ? C152 C153 H15D 109.5 . . ? H15C C153 H15D 109.5 . . ? C152 C153 H15E 109.5 . . ? H15C C153 H15E 109.5 . . ? H15D C153 H15E 109.5 . . ? N202 C201 C111 112.2(3) . . ? N202 C201 C101 111.9(3) . . ? C111 C201 C101 25.8(3) . . ? N202 C201 H20B 109.2 . . ? C111 C201 H20B 109.2 . . ? C101 C201 H20B 129.0 . . ? N202 C201 H20A 109.2 . . ? C111 C201 H20A 109.2 . . ? C101 C201 H20A 85.9 . . ? H20B C201 H20A 107.9 . . ? C203 N202 C201 118.7(2) . . ? C203 N202 Cu1 127.98(16) . . ? C201 N202 Cu1 113.19(16) . . ? N202 C203 N231 125.5(2) . . ? N202 C203 N204 121.8(2) . . ? N231 C203 N204 112.6(2) . . ? C205 N204 C203 127.2(2) . . ? C205 N204 H204 116.4 . . ? C203 N204 H204 116.4 . . ? N206 C205 O251 126.9(2) . . ? N206 C205 N204 124.5(2) . . ? O251 C205 N204 108.6(2) . . ? C205 N206 Cu1 127.09(17) . . ? C205 N206 H206 116.5 . . ? Cu1 N206 H206 116.5 . . ? C203 N231 H23A 120.0 . . ? C203 N231 H23B 120.0 . . ? H23A N231 H23B 120.0 . . ? C205 O251 C252 116.54(19) . . ? O251 C252 C253 108.4(2) . . ? O251 C252 H25A 110.0 . . ? C253 C252 H25A 110.0 . . ? O251 C252 H25B 110.0 . . ? C253 C252 H25B 110.0 . . ? H25A C252 H25B 108.4 . . ? C252 C253 H25C 109.5 . . ? C252 C253 H25D 109.5 . . ? H25C C253 H25D 109.5 . . ? C252 C253 H25E 109.5 . . ? H25C C253 H25E 109.5 . . ? H25D C253 H25E 109.5 . . ? O12 S1 O13 113.69(12) . . ? O12 S1 O14 113.22(12) . . ? O13 S1 O14 113.08(12) . . ? O12 S1 O11 102.22(12) . . ? O13 S1 O11 106.96(12) . . ? O14 S1 O11 106.59(11) . . ? O23 S2 O24 113.12(11) . . ? O23 S2 O22 113.77(13) . . ? O24 S2 O22 113.89(12) . . ? O23 S2 O21 106.85(12) . . ? O24 S2 O21 101.59(11) . . ? O22 S2 O21 106.33(11) . . ? C12 O11 S1 116.87(19) . . ? O11 C12 C13 111.1(2) . . ? O11 C12 H1A 109.4 . . ? C13 C12 H1A 109.4 . . ? O11 C12 H1B 109.4 . . ? C13 C12 H1B 109.4 . . ? H1A C12 H1B 108.0 . . ? C12 C13 H1C 109.5 . . ? C12 C13 H1D 109.5 . . ? H1C C13 H1D 109.5 . . ? C12 C13 H1E 109.5 . . ? H1C C13 H1E 109.5 . . ? H1D C13 H1E 109.5 . . ? C22 O21 S2 116.00(19) . . ? O21 C22 C23 108.6(3) . . ? O21 C22 H2A 110.0 . . ? C23 C22 H2A 110.0 . . ? O21 C22 H2B 110.0 . . ? C23 C22 H2B 110.0 . . ? H2A C22 H2B 108.3 . . ? C22 C23 H2C 109.5 . . ? C22 C23 H2D 109.5 . . ? H2C C23 H2D 109.5 . . ? C22 C23 H2E 109.5 . . ? H2C C23 H2E 109.5 . . ? H2D C23 H2E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.595 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.093 #===end data_CUCGET # paper complex no. 9 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31 Cl Cu N8 O8 S' _chemical_formula_weight 546.50 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 8.3861(7) _cell_length_b 11.7910(10) _cell_length_c 12.5520(10) _cell_angle_alpha 93.835(2) _cell_angle_beta 108.332(2) _cell_angle_gamma 104.004(2) _cell_volume 1129.28(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7150 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.88 _exptl_crystal_description 'Rectangular block' _exptl_crystal_colour Purple _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 11690 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.89 _reflns_number_total 5213 _reflns_number_gt 4572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+0.0255P] 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 5213 _refine_ls_number_parameters 296 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.61118(3) 0.823497(16) 0.525201(16) 0.01635(7) Uani 1 1 d . . . C101 C 0.8791(2) 0.88265(15) 0.74522(14) 0.0210(4) Uani 1 1 d . . . H10A H 0.8362 0.9202 0.7995 0.025 Uiso 1 1 calc R . . H10B H 1.0082 0.9029 0.7780 0.025 Uiso 1 1 calc R . . N102 N 0.82685(19) 0.92642(12) 0.63678(12) 0.0172(3) Uani 1 1 d . . . C103 C 0.9228(2) 1.02723(14) 0.62756(14) 0.0166(3) Uani 1 1 d . . . N104 N 0.87788(19) 1.07600(12) 0.52832(12) 0.0178(3) Uani 1 1 d . . . H104 H 0.9547 1.1404 0.5253 0.021 Uiso 1 1 calc R . . C105 C 0.7299(2) 1.03696(14) 0.43480(14) 0.0173(3) Uani 1 1 d . . . N106 N 0.60863(18) 0.94179(12) 0.42268(12) 0.0179(3) Uani 1 1 d . . . H106 H 0.5144 0.9282 0.3620 0.021 Uiso 1 1 calc R . . N131 N 1.07264(19) 1.09245(12) 0.70643(12) 0.0203(3) Uani 1 1 d . . . H13A H 1.1139 1.0677 0.7715 0.024 Uiso 1 1 calc R . . H13B H 1.1297 1.1600 0.6932 0.024 Uiso 1 1 calc R . . O151 O 0.73374(16) 1.11372(10) 0.36212(10) 0.0200(3) Uani 1 1 d . . . C152 C 0.5912(2) 1.08470(15) 0.25377(15) 0.0227(4) Uani 1 1 d . . . H15A H 0.4779 1.0740 0.2661 0.027 Uiso 1 1 calc R . . H15B H 0.5888 1.0103 0.2110 0.027 Uiso 1 1 calc R . . C153 C 0.6215(3) 1.18522(16) 0.18863(16) 0.0288(4) Uani 1 1 d . . . H15C H 0.5276 1.1679 0.1147 0.043 Uiso 1 1 calc R . . H15D H 0.7341 1.1952 0.1772 0.043 Uiso 1 1 calc R . . H15E H 0.6224 1.2581 0.2314 0.043 Uiso 1 1 calc R . . C201 C 0.8019(2) 0.74888(15) 0.72537(15) 0.0237(4) Uani 1 1 d . . . H20A H 0.8773 0.7095 0.6988 0.028 Uiso 1 1 calc R . . H20B H 0.7954 0.7218 0.7972 0.028 Uiso 1 1 calc R . . N202 N 0.62589(19) 0.71771(12) 0.63944(12) 0.0185(3) Uani 1 1 d . . . C203 C 0.5229(2) 0.61285(14) 0.63094(14) 0.0186(3) Uani 1 1 d . . . N204 N 0.3618(2) 0.57374(12) 0.54510(12) 0.0211(3) Uani 1 1 d . . . H204 H 0.2929 0.5065 0.5502 0.025 Uiso 1 1 calc R . . C205 C 0.2956(2) 0.62589(15) 0.45331(14) 0.0189(3) Uani 1 1 d . . . N206 N 0.37510(19) 0.72597(12) 0.43486(12) 0.0188(3) Uani 1 1 d . . . H206 H 0.3178 0.7537 0.3756 0.023 Uiso 1 1 calc R . . N231 N 0.5554(2) 0.53344(13) 0.69970(13) 0.0244(3) Uani 1 1 d . . . H23A H 0.6543 0.5501 0.7573 0.029 Uiso 1 1 calc R . . H23B H 0.4778 0.4643 0.6875 0.029 Uiso 1 1 calc R . . O251 O 0.14041(16) 0.55517(11) 0.38904(10) 0.0225(3) Uani 1 1 d . . . C252 C 0.0506(2) 0.59028(15) 0.28284(15) 0.0209(4) Uani 1 1 d . . . H25A H 0.1254 0.6023 0.2350 0.025 Uiso 1 1 calc R . . H25B H 0.0219 0.6651 0.2977 0.025 Uiso 1 1 calc R . . C253 C -0.1136(2) 0.49212(16) 0.22417(16) 0.0267(4) Uani 1 1 d . . . H25C H -0.1784 0.5124 0.1517 0.040 Uiso 1 1 calc R . . H25D H -0.1864 0.4813 0.2724 0.040 Uiso 1 1 calc R . . H25E H -0.0833 0.4187 0.2101 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.78566(6) 0.69504(3) 0.42002(4) 0.02142(10) Uani 1 1 d . . . S1 S 0.20247(6) 0.80988(4) 0.10943(4) 0.02076(11) Uani 1 1 d . . . O11 O 0.28876(16) 0.71050(10) 0.08064(11) 0.0241(3) Uani 1 1 d . . . O12 O 0.27078(16) 0.84313(11) 0.23167(10) 0.0235(3) Uani 1 1 d . . . O13 O 0.2525(2) 0.90637(12) 0.05140(12) 0.0349(3) Uani 1 1 d . . . O14 O 0.01775(18) 0.74757(12) 0.06540(13) 0.0338(3) Uani 1 1 d . . . C12 C 0.4804(2) 0.74534(16) 0.12076(17) 0.0267(4) Uani 1 1 d . . . H1A H 0.5274 0.7540 0.2047 0.032 Uiso 1 1 calc R . . H1B H 0.5247 0.8221 0.0977 0.032 Uiso 1 1 calc R . . C13 C 0.5374(3) 0.65053(17) 0.06881(19) 0.0316(4) Uani 1 1 d . . . H1C H 0.6654 0.6719 0.0943 0.047 Uiso 1 1 calc R . . H1E H 0.4904 0.6428 -0.0142 0.047 Uiso 1 1 calc R . . H1E H 0.4935 0.5751 0.0925 0.047 Uiso 1 1 calc R . . O1W O -0.1680(2) 0.54441(12) -0.08960(11) 0.0322(3) Uani 1 1 d D . . H1WB H -0.108(3) 0.5975(12) -0.0369(12) 0.038(7) Uiso 1 1 d D . . H1WA H -0.167(4) 0.4828(10) -0.0632(17) 0.068(10) Uiso 1 1 d D . . O2W O 0.19926(19) 1.09744(12) -0.05314(11) 0.0278(3) Uani 1 1 d D . . H2WB H 0.140(3) 1.1334(17) -0.0325(19) 0.047(8) Uiso 1 1 d D . . H2WA H 0.205(3) 1.0436(14) -0.0160(17) 0.043(7) Uiso 1 1 d 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 0.01608(12) 0.01320(11) 0.01630(11) 0.00387(8) 0.00341(8) 0.00019(8) C101 0.0218(9) 0.0172(8) 0.0178(8) 0.0054(7) 0.0025(7) -0.0007(7) N102 0.0174(7) 0.0135(6) 0.0175(7) 0.0040(5) 0.0039(5) 0.0005(5) C103 0.0166(8) 0.0158(7) 0.0171(8) 0.0016(6) 0.0057(6) 0.0045(6) N104 0.0175(7) 0.0125(6) 0.0185(7) 0.0045(5) 0.0036(5) -0.0015(5) C105 0.0202(8) 0.0146(7) 0.0179(8) 0.0037(6) 0.0065(6) 0.0061(6) N106 0.0154(7) 0.0160(7) 0.0175(7) 0.0032(5) 0.0016(5) 0.0012(5) N131 0.0187(7) 0.0173(7) 0.0190(7) 0.0053(6) 0.0024(6) -0.0012(6) O151 0.0198(6) 0.0163(6) 0.0180(6) 0.0061(5) 0.0018(5) -0.0002(5) C152 0.0213(9) 0.0204(8) 0.0187(8) 0.0051(7) -0.0006(7) 0.0013(7) C153 0.0316(11) 0.0262(10) 0.0240(9) 0.0110(8) 0.0040(8) 0.0050(8) C201 0.0218(9) 0.0179(8) 0.0236(9) 0.0079(7) -0.0006(7) 0.0012(7) N202 0.0177(7) 0.0162(7) 0.0169(7) 0.0039(5) 0.0029(6) 0.0001(5) C203 0.0204(9) 0.0172(8) 0.0166(8) 0.0019(6) 0.0063(7) 0.0026(7) N204 0.0206(7) 0.0155(7) 0.0214(7) 0.0063(6) 0.0042(6) -0.0024(6) C205 0.0165(8) 0.0180(8) 0.0203(8) 0.0024(7) 0.0061(6) 0.0020(6) N206 0.0176(7) 0.0161(7) 0.0201(7) 0.0068(6) 0.0040(6) 0.0021(6) N231 0.0240(8) 0.0162(7) 0.0225(8) 0.0063(6) -0.0004(6) -0.0027(6) O251 0.0174(6) 0.0201(6) 0.0224(6) 0.0068(5) 0.0016(5) -0.0028(5) C252 0.0189(9) 0.0202(8) 0.0208(8) 0.0040(7) 0.0040(7) 0.0039(7) C253 0.0197(9) 0.0254(9) 0.0279(9) 0.0012(8) 0.0028(7) 0.0010(7) Cl1 0.0227(2) 0.01485(19) 0.0250(2) 0.00359(16) 0.00953(17) 0.00016(15) S1 0.0221(2) 0.0167(2) 0.0203(2) 0.00238(16) 0.00166(17) 0.00724(17) O11 0.0224(7) 0.0174(6) 0.0292(7) 0.0003(5) 0.0041(5) 0.0065(5) O12 0.0225(7) 0.0226(6) 0.0215(6) 0.0019(5) 0.0047(5) 0.0036(5) O13 0.0505(9) 0.0272(7) 0.0321(7) 0.0145(6) 0.0133(7) 0.0186(7) O14 0.0223(7) 0.0299(7) 0.0390(8) -0.0065(6) -0.0018(6) 0.0081(6) C12 0.0213(9) 0.0232(9) 0.0336(10) 0.0020(8) 0.0073(8) 0.0061(7) C13 0.0294(11) 0.0240(9) 0.0458(12) 0.0073(9) 0.0167(9) 0.0096(8) O1W 0.0396(8) 0.0214(7) 0.0242(7) 0.0035(6) -0.0002(6) 0.0023(6) O2W 0.0314(8) 0.0264(7) 0.0270(7) 0.0112(6) 0.0079(6) 0.0113(6) _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 N102 1.9550(14) . y Cu1 N202 1.9569(14) . y Cu1 N206 1.9594(14) . y Cu1 N106 1.9594(14) . y C101 N102 1.463(2) . ? C101 C201 1.523(2) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? N102 C103 1.299(2) . ? C103 N131 1.341(2) . ? C103 N104 1.389(2) . ? N104 C105 1.366(2) . ? N104 H104 0.8800 . ? C105 N106 1.282(2) . ? C105 O151 1.329(2) . ? N106 H106 0.8800 . ? N131 H13A 0.8800 . ? N131 H13B 0.8800 . ? O151 C152 1.453(2) . ? C152 C153 1.501(2) . ? C152 H15A 0.9900 . ? C152 H15B 0.9900 . ? C153 H15C 0.9800 . ? C153 H15D 0.9800 . ? C153 H15E 0.9800 . ? C201 N202 1.470(2) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? N202 C203 1.301(2) . ? C203 N231 1.334(2) . ? C203 N204 1.384(2) . ? N204 C205 1.368(2) . ? N204 H204 0.8800 . ? C205 N206 1.282(2) . ? C205 O251 1.328(2) . ? N206 H206 0.8800 . ? N231 H23A 0.8800 . ? N231 H23B 0.8800 . ? O251 C252 1.452(2) . ? C252 C253 1.502(2) . ? C252 H25A 0.9900 . ? C252 H25B 0.9900 . ? C253 H25C 0.9800 . ? C253 H25D 0.9800 . ? C253 H25E 0.9800 . ? S1 O13 1.4397(15) . ? S1 O12 1.4471(13) . ? S1 O14 1.4495(14) . ? S1 O11 1.5955(13) . ? O11 C12 1.466(2) . ? C12 C13 1.503(3) . ? C12 H1A 0.9900 . ? C12 H1B 0.9900 . ? C13 H1C 0.9800 . ? C13 H1E 0.9800 . ? C13 H1E 0.9800 . ? O1W H1WB 0.816(5) . ? O1W H1WA 0.818(5) . ? O2W H2WB 0.816(5) . ? O2W H2WA 0.814(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N102 Cu1 N202 84.63(6) . . y N102 Cu1 N206 169.18(6) . . y N202 Cu1 N206 90.70(6) . . y N102 Cu1 N106 90.56(6) . . y N202 Cu1 N106 174.59(5) . . y N206 Cu1 N106 93.62(6) . . y N102 C101 C201 108.96(13) . . ? N102 C101 H10A 109.9 . . ? C201 C101 H10A 109.9 . . ? N102 C101 H10B 109.9 . . ? C201 C101 H10B 109.9 . . ? H10A C101 H10B 108.3 . . ? C103 N102 C101 117.75(14) . . ? C103 N102 Cu1 128.72(12) . . ? C101 N102 Cu1 113.50(10) . . ? N102 C103 N131 125.91(16) . . ? N102 C103 N104 120.86(15) . . ? N131 C103 N104 113.20(14) . . ? C105 N104 C103 128.36(14) . . ? C105 N104 H104 115.8 . . ? C103 N104 H104 115.8 . . ? N106 C105 O151 127.08(16) . . ? N106 C105 N104 124.01(16) . . ? O151 C105 N104 108.90(14) . . ? C105 N106 Cu1 126.81(12) . . ? C105 N106 H106 116.6 . . ? Cu1 N106 H106 116.6 . . ? C103 N131 H13A 120.0 . . ? C103 N131 H13B 120.0 . . ? H13A N131 H13B 120.0 . . ? C105 O151 C152 117.39(13) . . ? O151 C152 C153 107.53(14) . . ? O151 C152 H15A 110.2 . . ? C153 C152 H15A 110.2 . . ? O151 C152 H15B 110.2 . . ? C153 C152 H15B 110.2 . . ? H15A C152 H15B 108.5 . . ? C152 C153 H15C 109.5 . . ? C152 C153 H15D 109.5 . . ? H15C C153 H15D 109.5 . . ? C152 C153 H15E 109.5 . . ? H15C C153 H15E 109.5 . . ? H15D C153 H15E 109.5 . . ? N202 C201 C101 108.97(14) . . ? N202 C201 H20A 109.9 . . ? C101 C201 H20A 109.9 . . ? N202 C201 H20B 109.9 . . ? C101 C201 H20B 109.9 . . ? H20A C201 H20B 108.3 . . ? C203 N202 C201 117.79(14) . . ? C203 N202 Cu1 127.84(12) . . ? C201 N202 Cu1 111.45(11) . . ? N202 C203 N231 126.16(16) . . ? N202 C203 N204 120.76(16) . . ? N231 C203 N204 113.08(15) . . ? C205 N204 C203 128.47(15) . . ? C205 N204 H204 115.8 . . ? C203 N204 H204 115.8 . . ? N206 C205 O251 127.36(16) . . ? N206 C205 N204 124.11(15) . . ? O251 C205 N204 108.52(14) . . ? C205 N206 Cu1 126.61(12) . . ? C205 N206 H206 116.7 . . ? Cu1 N206 H206 116.7 . . ? C203 N231 H23A 120.0 . . ? C203 N231 H23B 120.0 . . ? H23A N231 H23B 120.0 . . ? C205 O251 C252 117.82(13) . . ? O251 C252 C253 106.85(14) . . ? O251 C252 H25A 110.4 . . ? C253 C252 H25A 110.4 . . ? O251 C252 H25B 110.4 . . ? C253 C252 H25B 110.4 . . ? H25A C252 H25B 108.6 . . ? C252 C253 H25C 109.5 . . ? C252 C253 H25D 109.5 . . ? H25C C253 H25D 109.5 . . ? C252 C253 H25E 109.5 . . ? H25C C253 H25E 109.5 . . ? H25D C253 H25E 109.5 . . ? O13 S1 O12 112.51(8) . . ? O13 S1 O14 114.26(9) . . ? O12 S1 O14 113.53(9) . . ? O13 S1 O11 106.78(8) . . ? O12 S1 O11 106.61(7) . . ? O14 S1 O11 102.04(7) . . ? C12 O11 S1 115.34(10) . . ? O11 C12 C13 107.89(15) . . ? O11 C12 H1A 110.1 . . ? C13 C12 H1A 110.1 . . ? O11 C12 H1B 110.1 . . ? C13 C12 H1B 110.1 . . ? H1A C12 H1B 108.4 . . ? C12 C13 H1C 109.5 . . ? C12 C13 H1E 109.5 . . ? H1C C13 H1E 109.5 . . ? C12 C13 H1E 109.5 . . ? H1C C13 H1E 109.5 . . ? H1E C13 H1E 109.5 . . ? H1WB O1W H1WA 105.7(8) . . ? H2WB O2W H2WA 106.1(9) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.410 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.073 #===end