Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name _publ_author_name_address 'Mallayan Palaniandavar' ; Department of Chemistry Bharathidasan University Tiruchirapalli 620 024 Tamil Nadu, INDIA ; 'Mathrubootham Vaidyanathan' ; Department of Chemistry Bharathidasan University Tiruchirapalli 620 024 Tamil Nadu, INDIA ; 'Ramalingam Balamurugan' ; Department of Chemistry Bharathidasan University Tiruchirapalli 620 024 Tamil Nadu, INDIA ; 'Usha Sivagnanam' ; Department of Chemistry Bharathidasan University Tiruchirapalli 620 024 Tamil Nadu, INDIA ; _publ_contact_author_name 'Dr Mallayan Palaniandavar' _publ_contact_author_address ; Dr Mallayan Palaniandavar Department of Chemistry Bharathidasan University Tiruchriappalli 620 024 Tamil Nadu INDIA ; _publ_contact_author_email 'palani@bdu.ernet.in' data_for_(1a) #[Cu(bbes)(H2O)Cl]Cl _database_code_CSD 156236 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Cl2 Cu N4 O S' _chemical_formula_weight 474.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' '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 9.466(3) _cell_length_b 9.480(3) _cell_length_c 11.519(2) _cell_angle_alpha 75.880(18) _cell_angle_beta 81.362(18) _cell_angle_gamma 80.03(2) _cell_volume 981.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 24.99 _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 1.508 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Noinus-CAD4' _diffrn_measurement_method 'w-2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3693 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3454 _reflns_number_gt 3028 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+0.6213P] 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 3454 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.21424(5) 0.25438(5) 0.72930(4) 0.0266(2) Uani 1 d . . . S1 S 0.17141(10) 0.41004(11) 0.87282(9) 0.0313(3) Uani 1 d . . . Cl1 Cl 0.31302(11) 0.22219(13) 0.54079(9) 0.0417(3) Uani 1 d . . . Cl2 Cl 0.84391(12) 0.24874(13) 0.98481(10) 0.0435(3) Uani 1 d . . . O1 O 0.1112(4) 0.0732(4) 0.8538(3) 0.0514(9) Uani 1 d . . . N1 N 0.4032(3) 0.1811(4) 0.7940(3) 0.0298(7) Uani 1 d . . . N2 N 0.6020(4) 0.1505(4) 0.8797(3) 0.0389(9) Uani 1 d . . . H2 H 0.654(5) 0.1663(15) 0.907(2) 0.050(3) Uiso 1 calc R . . N3 N 0.0245(3) 0.3343(4) 0.6722(3) 0.0301(7) Uani 1 d . . . N4 N -0.1698(4) 0.4912(4) 0.6200(3) 0.0387(9) Uani 1 d . . . H4 H -0.217(4) 0.555(5) 0.6101(9) 0.050(3) Uiso 1 calc R . . C1 C 0.4721(4) 0.0376(4) 0.7964(3) 0.0293(8) Uani 1 d . . . C2 C 0.4387(5) -0.0742(5) 0.7519(4) 0.0342(9) Uani 1 d . . . H2A H 0.353(5) -0.0625(8) 0.713(2) 0.050(3) Uiso 1 calc R . . C3 C 0.5349(5) -0.2044(5) 0.7652(4) 0.0422(11) Uani 1 d . . . H3 H 0.5160(12) -0.283(5) 0.7332(19) 0.050(3) Uiso 1 calc R . . C4 C 0.6577(5) -0.2234(6) 0.8235(5) 0.0497(12) Uani 1 d . . . H4A H 0.727(3) -0.327(5) 0.8338(7) 0.050(3) Uiso 1 calc R . . C5 C 0.6923(5) -0.1142(6) 0.8680(5) 0.0458(11) Uani 1 d . . . H5 H 0.772(5) -0.1269(10) 0.905(2) 0.050(3) Uiso 1 calc R . . C6 C 0.5990(4) 0.0171(5) 0.8525(4) 0.0339(9) Uani 1 d . . . C7 C 0.4866(4) 0.2427(5) 0.8448(4) 0.0331(9) Uani 1 d . . . C8 C 0.4627(5) 0.3962(5) 0.8635(4) 0.0413(10) Uani 1 d . . . H8A H 0.539(3) 0.4369(18) 0.8308(14) 0.050(3) Uiso 1 calc R . . H8B H 0.4550(5) 0.3914(5) 0.941(3) 0.050(3) Uiso 1 calc R . . C9 C 0.3329(5) 0.4953(5) 0.8140(4) 0.0391(10) Uani 1 d . . . H9A H 0.3452(7) 0.5132(9) 0.728(3) 0.050(3) Uiso 1 calc R . . H9B H 0.3232(6) 0.587(4) 0.8363(9) 0.050(3) Uiso 1 calc R . . C10 C 0.0330(5) 0.5616(5) 0.8256(4) 0.0372(10) Uani 1 d . . . H10A H -0.060(4) 0.5396(9) 0.8713(18) 0.050(3) Uiso 1 calc R . . H10B H 0.0552(9) 0.650(3) 0.8452(9) 0.050(3) Uiso 1 calc R . . C11 C 0.0176(5) 0.5944(5) 0.6908(4) 0.0381(10) Uani 1 d . . . H11A H -0.044(3) 0.681(4) 0.6702(10) 0.050(3) Uiso 1 calc R . . H11B H 0.106(4) 0.6068(8) 0.6471(19) 0.050(3) Uiso 1 calc R . . C12 C -0.0392(4) 0.4725(5) 0.6593(3) 0.0315(9) Uani 1 d . . . C13 C -0.1923(4) 0.3574(5) 0.6031(4) 0.0378(10) Uani 1 d . . . C14 C -0.3074(5) 0.3148(7) 0.5622(4) 0.0481(12) Uani 1 d . . . H14 H -0.396(5) 0.385(4) 0.5414(12) 0.050(3) Uiso 1 calc R . . C15 C -0.2932(5) 0.1738(7) 0.5523(4) 0.0533(14) Uani 1 d . . . H15 H -0.373(4) 0.140(2) 0.5226(17) 0.050(3) Uiso 1 calc R . . C16 C -0.1707(5) 0.0740(6) 0.5823(4) 0.0501(12) Uani 1 d . . . H16 H -0.1634(7) -0.033(6) 0.5723(7) 0.050(3) Uiso 1 calc R . . C17 C -0.0579(5) 0.1149(6) 0.6254(4) 0.0422(10) Uani 1 d . . . H17 H 0.029(5) 0.043(4) 0.6482(14) 0.050(3) Uiso 1 calc R . . C18 C -0.0706(4) 0.2596(5) 0.6357(3) 0.0321(9) Uani 1 d . . . H2W H 0.1414 -0.0214 0.8948 0.050 Uiso 1 d . . . H1W H 0.0246 0.1269 0.8816 0.050 Uiso 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 0.0229(3) 0.0340(3) 0.0229(3) -0.0066(2) -0.00530(19) -0.00168(19) S1 0.0304(5) 0.0391(6) 0.0253(5) -0.0089(4) -0.0028(4) -0.0054(4) Cl1 0.0363(6) 0.0583(7) 0.0245(5) -0.0083(5) -0.0047(4) 0.0091(5) Cl2 0.0409(6) 0.0509(7) 0.0445(6) -0.0159(5) -0.0042(5) -0.0158(5) O1 0.0421(18) 0.0470(19) 0.052(2) 0.0057(15) 0.0054(15) -0.0053(15) N1 0.0251(16) 0.0390(19) 0.0266(17) -0.0092(14) -0.0043(13) -0.0041(14) N2 0.0282(18) 0.056(2) 0.036(2) -0.0092(17) -0.0143(15) -0.0072(16) N3 0.0267(16) 0.0418(19) 0.0226(16) -0.0106(14) -0.0012(13) -0.0037(14) N4 0.0301(18) 0.051(2) 0.0298(19) -0.0054(16) -0.0075(15) 0.0075(16) C1 0.0254(19) 0.035(2) 0.0222(18) -0.0007(16) 0.0002(15) -0.0020(16) C2 0.031(2) 0.036(2) 0.035(2) -0.0059(17) -0.0026(17) -0.0055(17) C3 0.041(3) 0.034(2) 0.047(3) -0.009(2) 0.005(2) -0.0046(19) C4 0.035(2) 0.043(3) 0.056(3) 0.001(2) 0.005(2) 0.009(2) C5 0.030(2) 0.053(3) 0.045(3) 0.002(2) -0.007(2) 0.003(2) C6 0.025(2) 0.045(2) 0.028(2) -0.0032(18) -0.0032(16) -0.0029(17) C7 0.028(2) 0.048(2) 0.026(2) -0.0089(18) -0.0041(16) -0.0124(18) C8 0.036(2) 0.048(3) 0.045(3) -0.017(2) -0.006(2) -0.010(2) C9 0.037(2) 0.038(2) 0.045(3) -0.014(2) 0.0015(19) -0.0128(19) C10 0.038(2) 0.041(2) 0.034(2) -0.0155(18) -0.0030(18) 0.0011(19) C11 0.040(2) 0.040(2) 0.029(2) -0.0020(18) -0.0005(18) -0.0009(19) C12 0.028(2) 0.045(2) 0.0180(18) -0.0042(16) -0.0002(15) -0.0013(17) C13 0.027(2) 0.062(3) 0.023(2) -0.0101(19) -0.0016(16) -0.0031(19) C14 0.026(2) 0.087(4) 0.032(2) -0.016(2) -0.0041(18) -0.005(2) C15 0.038(3) 0.092(4) 0.038(3) -0.018(3) -0.002(2) -0.027(3) C16 0.046(3) 0.070(3) 0.041(3) -0.018(2) -0.001(2) -0.023(2) C17 0.038(2) 0.054(3) 0.036(2) -0.011(2) -0.0053(19) -0.009(2) C18 0.0245(19) 0.051(3) 0.0204(19) -0.0081(17) -0.0010(15) -0.0061(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 N3 1.969(3) . ? Cu1 N1 1.988(3) . ? Cu1 O1 2.217(3) . ? Cu1 Cl1 2.3017(12) . ? Cu1 S1 2.4201(12) . ? S1 C10 1.805(4) . ? S1 C9 1.816(4) . ? N1 C7 1.332(5) . ? N1 C1 1.399(5) . ? N2 C7 1.322(6) . ? N2 C6 1.382(6) . ? N3 C12 1.327(5) . ? N3 C18 1.402(5) . ? N4 C12 1.348(5) . ? N4 C13 1.386(6) . ? C1 C2 1.384(6) . ? C1 C6 1.410(6) . ? C2 C3 1.391(6) . ? C3 C4 1.391(7) . ? C4 C5 1.367(8) . ? C5 C6 1.385(6) . ? C7 C8 1.496(6) . ? C8 C9 1.506(7) . ? C10 C11 1.532(6) . ? C11 C12 1.494(6) . ? C13 C18 1.385(6) . ? C13 C14 1.403(6) . ? C14 C15 1.352(8) . ? C15 C16 1.393(8) . ? C16 C17 1.390(7) . ? C17 C18 1.389(7) . ? 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 N1 176.64(13) . . ? N3 Cu1 O1 87.87(13) . . ? N1 Cu1 O1 92.28(14) . . ? N3 Cu1 Cl1 91.56(10) . . ? N1 Cu1 Cl1 91.33(10) . . ? O1 Cu1 Cl1 118.11(11) . . ? N3 Cu1 S1 91.09(10) . . ? N1 Cu1 S1 85.56(10) . . ? O1 Cu1 S1 94.32(10) . . ? Cl1 Cu1 S1 147.53(5) . . ? C10 S1 C9 100.7(2) . . ? C10 S1 Cu1 108.81(14) . . ? C9 S1 Cu1 93.79(15) . . ? C7 N1 C1 106.0(3) . . ? C7 N1 Cu1 132.3(3) . . ? C1 N1 Cu1 121.7(3) . . ? C7 N2 C6 109.3(4) . . ? C12 N3 C18 105.7(3) . . ? C12 N3 Cu1 126.4(3) . . ? C18 N3 Cu1 127.9(3) . . ? C12 N4 C13 107.9(4) . . ? C2 C1 N1 131.7(4) . . ? C2 C1 C6 120.1(4) . . ? N1 C1 C6 108.1(4) . . ? C1 C2 C3 117.2(4) . . ? C4 C3 C2 121.7(5) . . ? C5 C4 C3 121.9(4) . . ? C4 C5 C6 116.8(5) . . ? N2 C6 C5 132.9(4) . . ? N2 C6 C1 104.8(4) . . ? C5 C6 C1 122.3(4) . . ? N2 C7 N1 111.8(4) . . ? N2 C7 C8 120.5(4) . . ? N1 C7 C8 127.6(4) . . ? C7 C8 C9 116.5(4) . . ? C8 C9 S1 109.8(3) . . ? C11 C10 S1 113.6(3) . . ? C12 C11 C10 111.1(4) . . ? N3 C12 N4 111.7(4) . . ? N3 C12 C11 126.1(4) . . ? N4 C12 C11 122.1(4) . . ? C18 C13 N4 105.7(4) . . ? C18 C13 C14 122.3(5) . . ? N4 C13 C14 132.0(4) . . ? C15 C14 C13 117.1(5) . . ? C14 C15 C16 121.8(5) . . ? C17 C16 C15 121.3(5) . . ? C18 C17 C16 117.6(5) . . ? C13 C18 C17 119.9(4) . . ? C13 C18 N3 108.9(4) . . ? C17 C18 N3 131.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.988 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.142 #===END data_(4) #[Cu(L4)](ClO4)2.2CH3CN _database_code_CSD 156237 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H28 Cl2 Cu N6 O8 S2' _chemical_formula_weight 715.07 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' 'Cl' 'Cl' 0.1484 0.1585 '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 'P21/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 10.9367(5) _cell_length_b 15.6280(6) _cell_length_c 17.6216(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.9692(15) _cell_angle_gamma 90.00 _cell_volume 2956.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 23.24 _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 1.117 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.308248 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens three-circle diffractometer' _diffrn_measurement_method 'w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11956 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.1118 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.24 _reflns_number_total 4217 _reflns_number_gt 2389 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+0.0000P] 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 4217 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1334 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.2132 _refine_ls_wR_factor_gt 0.1688 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.08452(9) 0.23221(6) 0.06626(6) 0.0426(4) Uani 1 d . . . S1 S 0.2890(2) 0.18663(14) 0.15315(13) 0.0553(7) Uani 1 d . . . S2 S -0.0574(2) 0.20735(15) 0.14748(14) 0.0574(7) Uani 1 d . . . Cl1 Cl -0.4554(2) -0.04766(15) 0.12122(14) 0.0599(7) Uani 1 d . . . Cl2 Cl 0.1945(2) 0.15306(19) 0.39668(17) 0.0734(8) Uani 1 d . . . N1 N 0.1960(6) 0.2590(4) -0.0071(4) 0.0413(16) Uani 1 d . . . N2 N 0.3692(7) 0.2567(5) -0.0526(4) 0.057(2) Uani 1 d . . . H2 H 0.436(8) 0.2493(10) -0.0546(5) 0.057(6) Uiso 1 calc R . . N3 N -0.0203(6) 0.1466(4) -0.0003(4) 0.0411(16) Uani 1 d . . . N4 N -0.2031(7) 0.0882(5) -0.0477(4) 0.056(2) Uani 1 d . . . H4 H -0.290(7) 0.0727(14) -0.0523(6) 0.057(6) Uiso 1 calc R . . N5 N 0.1156(7) 0.3525(4) 0.1219(4) 0.0494(18) Uani 1 d . . . C1 C 0.1721(7) 0.2944(5) -0.0812(4) 0.041(2) Uani 1 d . . . C2 C 0.0623(9) 0.3274(6) -0.1245(5) 0.056(3) Uani 1 d . . . H2A H -0.012(7) 0.3270(6) -0.1062(17) 0.057(6) Uiso 1 calc R . . C3 C 0.0702(10) 0.3612(7) -0.1969(5) 0.071(3) Uani 1 d . . . H3 H 0.006(6) 0.384(2) -0.224(3) 0.057(6) Uiso 1 calc R . . C4 C 0.1802(12) 0.3592(7) -0.2260(6) 0.080(3) Uani 1 d . . . H4A H 0.1805(12) 0.381(2) -0.279(5) 0.057(6) Uiso 1 calc R . . C5 C 0.2874(12) 0.3273(8) -0.1829(6) 0.084(4) Uani 1 d . . . H5 H 0.356(7) 0.3274(8) -0.2000(18) 0.057(6) Uiso 1 calc R . . C6 C 0.2817(8) 0.2947(6) -0.1103(5) 0.053(2) Uani 1 d . . . C7 C 0.3159(8) 0.2356(5) 0.0068(5) 0.046(2) Uani 1 d . . . C8 C 0.3801(8) 0.1929(6) 0.0780(5) 0.057(3) Uani 1 d . . . H8A H 0.455(4) 0.2232(17) 0.0976(12) 0.057(6) Uiso 1 calc R . . H8B H 0.4022(16) 0.136(3) 0.0654(8) 0.057(6) Uiso 1 calc R . . C9 C 0.3133(9) 0.2900(6) 0.1978(5) 0.065(3) Uani 1 d . . . H9A H 0.2844(17) 0.2881(6) 0.245(3) 0.057(6) Uiso 1 calc R . . H9B H 0.400(5) 0.3005(8) 0.2097(9) 0.057(6) Uiso 1 calc R . . C10 C 0.2518(9) 0.3642(6) 0.1514(5) 0.064(3) Uani 1 d . . . H10A H 0.2644(12) 0.417(3) 0.1842(17) 0.057(6) Uiso 1 calc R . . H10B H 0.294(2) 0.3738(8) 0.107(2) 0.057(6) Uiso 1 calc R . . C11 C 0.0743(9) 0.4232(5) 0.0641(5) 0.068(3) Uani 1 d . . . H11A H 0.089(6) 0.479(3) 0.0903(16) 0.112(17) Uiso 1 calc R . . H11B H -0.016(5) 0.417(2) 0.042(3) 0.112(17) Uiso 1 calc R . . H11C H 0.123(5) 0.420(3) 0.022(3) 0.112(17) Uiso 1 calc R . . C12 C 0.0447(10) 0.3586(6) 0.1863(6) 0.069(3) Uani 1 d . . . H12A H 0.0366(10) 0.415(3) 0.1990(10) 0.057(6) Uiso 1 calc R . . H12B H 0.088(3) 0.3310(16) 0.229(3) 0.057(6) Uiso 1 calc R . . C13 C -0.0818(10) 0.3192(6) 0.1633(6) 0.082(4) Uani 1 d . . . H13A H -0.118(3) 0.3404(16) 0.126(3) 0.057(6) Uiso 1 calc R . . H13B H -0.120(3) 0.3252(8) 0.196(2) 0.057(6) Uiso 1 calc R . . C14 C -0.1873(8) 0.1766(6) 0.0737(6) 0.067(3) Uani 1 d . . . H14A H -0.238(3) 0.137(2) 0.0937(12) 0.057(6) Uiso 1 calc R . . H14B H -0.235(3) 0.225(3) 0.0558(11) 0.057(6) Uiso 1 calc R . . C15 C -0.1365(8) 0.1362(5) 0.0085(5) 0.050(2) Uani 1 d . . . C16 C -0.1270(8) 0.0648(5) -0.0976(5) 0.048(2) Uani 1 d . . . C17 C -0.1448(10) 0.0154(6) -0.1639(6) 0.063(3) Uani 1 d . . . H17 H -0.232(7) -0.012(2) -0.1865(18) 0.057(6) Uiso 1 calc R . . C18 C -0.0457(11) 0.0030(6) -0.1985(6) 0.070(3) Uani 1 d . . . H18 H -0.0552(14) -0.025(3) -0.238(4) 0.057(6) Uiso 1 calc R . . C19 C 0.0695(10) 0.0355(6) -0.1699(5) 0.064(3) Uani 1 d . . . H19 H 0.134(6) 0.0248(11) -0.195(2) 0.057(6) Uiso 1 calc R . . C20 C 0.0899(9) 0.0843(5) -0.1037(5) 0.054(2) Uani 1 d . . . H20 H 0.170(7) 0.1065(19) -0.0837(18) 0.057(6) Uiso 1 calc R . . C21 C -0.0087(8) 0.1002(5) -0.0670(5) 0.043(2) Uani 1 d . . . N6 N 0.0838(16) 0.1546(11) 0.6091(13) 0.194(8) Uani 1 d . . . C22 C -0.152(2) -0.0096(12) 0.4165(13) 0.220(14) Uani 1 d . . . H22A H -0.169(6) -0.0121(17) 0.470(4) 0.112(17) Uiso 1 calc R . . H22B H -0.230(6) 0.005(2) 0.380(3) 0.112(17) Uiso 1 calc R . . H22C H -0.088(5) 0.034(3) 0.414(4) 0.112(17) Uiso 1 calc R . . C23 C 0.1083(16) 0.0913(15) 0.6037(12) 0.140(7) Uani 1 d . . . O1 O -0.5511(7) -0.0045(5) 0.1492(5) 0.112(3) Uani 1 d . . . O2 O -0.3804(7) -0.0962(5) 0.1780(5) 0.110(3) Uani 1 d . . . O3 O -0.5213(7) -0.1006(5) 0.0607(5) 0.102(3) Uani 1 d . . . O5 O 0.2436(13) 0.1309(9) 0.3328(8) 0.188(5) Uiso 1 d . . . O4 O -0.3741(17) -0.0174(13) 0.0737(11) 0.082(6) Uiso 0.40 d P . . O4A O -0.3852(11) 0.0228(8) 0.0987(7) 0.077(4) Uiso 0.60 d P . . O8 O 0.2870(16) 0.1328(12) 0.4639(10) 0.084(6) Uiso 0.50 d P . . O8A O 0.2961(17) 0.1715(12) 0.4538(11) 0.093(6) Uiso 0.50 d P . . O7 O 0.191(4) 0.220(3) 0.345(3) 0.166(14) Uiso 0.30 d P . . O7A O 0.1207(19) 0.2202(12) 0.4056(11) 0.182(7) Uiso 0.70 d P . . O6 O 0.167(4) 0.058(3) 0.407(2) 0.143(13) Uiso 0.30 d P . . O6A O 0.0939(16) 0.0941(11) 0.4015(9) 0.147(6) Uiso 0.70 d P . . 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 0.0437(6) 0.0451(6) 0.0394(7) -0.0014(5) 0.0092(5) -0.0041(5) S1 0.0599(15) 0.0514(14) 0.0496(15) 0.0089(11) -0.0025(12) 0.0008(11) S2 0.0627(16) 0.0648(16) 0.0490(15) 0.0055(11) 0.0215(12) 0.0026(12) Cl1 0.0531(14) 0.0648(16) 0.0620(17) 0.0097(13) 0.0120(12) 0.0056(12) Cl2 0.0578(16) 0.088(2) 0.078(2) -0.0122(15) 0.0209(15) -0.0057(14) N1 0.038(4) 0.048(4) 0.037(4) -0.003(3) 0.006(3) -0.003(3) N2 0.038(4) 0.079(6) 0.057(5) -0.001(4) 0.019(4) 0.006(4) N3 0.041(4) 0.043(4) 0.039(4) -0.004(3) 0.006(3) -0.001(3) N4 0.035(4) 0.068(5) 0.060(5) 0.008(4) 0.000(4) -0.011(4) N5 0.058(5) 0.047(4) 0.040(4) -0.006(3) 0.001(4) 0.006(3) C1 0.040(5) 0.050(5) 0.030(5) -0.011(4) 0.002(4) -0.004(4) C2 0.046(6) 0.068(6) 0.053(7) 0.001(5) 0.003(5) -0.007(4) C3 0.077(8) 0.089(8) 0.040(6) 0.008(5) -0.012(6) 0.003(6) C4 0.088(9) 0.125(10) 0.031(6) 0.009(6) 0.022(6) 0.007(7) C5 0.073(8) 0.129(10) 0.061(8) 0.005(7) 0.038(7) 0.008(7) C6 0.052(6) 0.064(6) 0.044(6) 0.005(5) 0.010(5) 0.006(5) C7 0.040(5) 0.051(5) 0.046(6) -0.006(4) 0.007(4) -0.003(4) C8 0.052(6) 0.057(6) 0.059(7) -0.003(5) 0.005(5) 0.007(4) C9 0.066(6) 0.078(7) 0.043(6) -0.005(5) -0.012(5) 0.005(5) C10 0.089(8) 0.046(6) 0.050(6) -0.010(5) -0.003(6) -0.009(5) C11 0.093(8) 0.039(5) 0.067(7) 0.004(5) 0.004(6) 0.008(5) C12 0.087(8) 0.053(6) 0.066(7) -0.018(5) 0.017(6) -0.001(5) C13 0.098(10) 0.088(8) 0.065(8) -0.009(6) 0.032(7) 0.021(7) C14 0.046(6) 0.079(7) 0.078(8) 0.006(6) 0.021(5) -0.004(5) C15 0.037(5) 0.056(6) 0.057(6) 0.013(5) 0.011(5) 0.000(4) C16 0.036(5) 0.046(5) 0.055(6) 0.010(5) -0.010(5) -0.006(4) C17 0.066(7) 0.057(6) 0.055(7) 0.004(5) -0.017(6) -0.008(5) C18 0.085(9) 0.067(7) 0.048(7) -0.021(5) -0.016(6) 0.011(6) C19 0.073(7) 0.062(6) 0.052(7) -0.016(5) 0.003(6) -0.002(5) C20 0.046(6) 0.053(6) 0.065(7) -0.007(5) 0.012(5) -0.005(4) C21 0.049(5) 0.036(5) 0.041(5) 0.001(4) -0.001(4) -0.002(4) N6 0.163(14) 0.136(14) 0.29(2) 0.032(15) 0.068(13) 0.075(12) C22 0.21(2) 0.136(19) 0.32(3) 0.09(2) 0.08(2) 0.011(16) C23 0.097(12) 0.130(16) 0.203(18) 0.048(16) 0.051(11) 0.012(11) O1 0.088(6) 0.118(7) 0.135(7) -0.014(5) 0.034(5) 0.036(5) O2 0.084(5) 0.147(7) 0.094(6) 0.058(5) 0.008(5) 0.033(5) O3 0.085(5) 0.103(6) 0.111(7) -0.025(5) 0.001(5) 0.005(5) _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 N1 1.982(6) . ? Cu1 N3 1.993(6) . ? Cu1 N5 2.118(6) . ? Cu1 S2 2.335(3) . ? Cu1 S1 2.559(2) . ? S1 C9 1.794(9) . ? S1 C8 1.804(9) . ? S2 C13 1.798(10) . ? S2 C14 1.799(9) . ? Cl1 O2 1.392(7) . ? Cl1 O1 1.411(7) . ? Cl1 O4 1.414(19) . ? Cl1 O3 1.431(7) . ? Cl1 O4A 1.441(12) . ? Cl2 O7A 1.352(19) . ? Cl2 O8A 1.380(18) . ? Cl2 O5 1.380(14) . ? Cl2 O7 1.38(4) . ? Cl2 O8 1.439(17) . ? Cl2 O6A 1.451(17) . ? Cl2 O6 1.54(4) . ? N1 C7 1.339(10) . ? N1 C1 1.397(10) . ? N2 C7 1.333(10) . ? N2 C6 1.390(10) . ? N3 C15 1.319(10) . ? N3 C21 1.406(10) . ? N4 C15 1.341(11) . ? N4 C16 1.370(11) . ? N5 C10 1.493(11) . ? N5 C12 1.494(11) . ? N5 C11 1.513(10) . ? C1 C6 1.391(11) . ? C1 C2 1.393(11) . ? C2 C3 1.399(12) . ? C3 C4 1.394(14) . ? C4 C5 1.364(14) . ? C5 C6 1.390(12) . ? C7 C8 1.476(11) . ? C9 C10 1.503(11) . ? C12 C13 1.498(13) . ? C14 C15 1.506(12) . ? C16 C17 1.383(12) . ? C16 C21 1.416(11) . ? C17 C18 1.355(13) . ? C18 C19 1.363(13) . ? C19 C20 1.376(12) . ? C20 C21 1.382(11) . ? N6 C23 1.03(2) . ? C22 C23 1.43(2) 3_556 ? C23 C22 1.43(2) 3_556 ? O5 O7 1.53(4) . ? O4 O4A 0.789(19) . ? O8 O8A 0.64(2) . ? O7 O7A 1.43(4) . ? O6 O6A 0.97(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 N1 Cu1 N3 96.6(3) . . ? N1 Cu1 N5 92.9(3) . . ? N3 Cu1 N5 153.2(3) . . ? N1 Cu1 S2 175.8(2) . . ? N3 Cu1 S2 82.8(2) . . ? N5 Cu1 S2 86.0(2) . . ? N1 Cu1 S1 82.71(19) . . ? N3 Cu1 S1 120.31(19) . . ? N5 Cu1 S1 85.70(19) . . ? S2 Cu1 S1 101.19(9) . . ? C9 S1 C8 102.5(4) . . ? C9 S1 Cu1 93.0(3) . . ? C8 S1 Cu1 95.0(3) . . ? C13 S2 C14 104.6(5) . . ? C13 S2 Cu1 93.9(4) . . ? C14 S2 Cu1 97.3(3) . . ? O2 Cl1 O1 112.6(5) . . ? O2 Cl1 O4 104.9(8) . . ? O1 Cl1 O4 129.7(9) . . ? O2 Cl1 O3 111.4(5) . . ? O1 Cl1 O3 103.6(5) . . ? O4 Cl1 O3 92.1(9) . . ? O2 Cl1 O4A 110.0(6) . . ? O1 Cl1 O4A 101.6(7) . . ? O4 Cl1 O4A 32.1(8) . . ? O3 Cl1 O4A 117.1(6) . . ? O7A Cl2 O8A 99.8(11) . . ? O7A Cl2 O5 128.5(10) . . ? O8A Cl2 O5 105.3(9) . . ? O7A Cl2 O7 63.3(18) . . ? O8A Cl2 O7 104.1(19) . . ? O5 Cl2 O7 67.3(18) . . ? O7A Cl2 O8 114.7(11) . . ? O8A Cl2 O8 26.3(9) . . ? O5 Cl2 O8 107.2(9) . . ? O7 Cl2 O8 129.7(19) . . ? O7A Cl2 O6A 90.6(11) . . ? O8A Cl2 O6A 127.2(11) . . ? O5 Cl2 O6A 107.8(9) . . ? O7 Cl2 O6A 126.2(18) . . ? O8 Cl2 O6A 103.6(10) . . ? O7A Cl2 O6 127.3(17) . . ? O8A Cl2 O6 105.4(16) . . ? O5 Cl2 O6 88.0(15) . . ? O7 Cl2 O6 145(2) . . ? O8 Cl2 O6 79.3(16) . . ? O6A Cl2 O6 37.9(14) . . ? C7 N1 C1 106.3(7) . . ? C7 N1 Cu1 121.7(6) . . ? C1 N1 Cu1 131.6(5) . . ? C7 N2 C6 109.7(7) . . ? C15 N3 C21 106.1(7) . . ? C15 N3 Cu1 118.2(6) . . ? C21 N3 Cu1 134.8(5) . . ? C15 N4 C16 108.2(7) . . ? C10 N5 C12 110.8(7) . . ? C10 N5 C11 107.2(7) . . ? C12 N5 C11 109.5(7) . . ? C10 N5 Cu1 109.4(5) . . ? C12 N5 Cu1 110.3(5) . . ? C11 N5 Cu1 109.6(5) . . ? C6 C1 C2 120.7(8) . . ? C6 C1 N1 109.0(7) . . ? C2 C1 N1 130.3(8) . . ? C1 C2 C3 116.3(9) . . ? C4 C3 C2 122.3(10) . . ? C5 C4 C3 120.9(10) . . ? C4 C5 C6 117.5(10) . . ? N2 C6 C5 133.2(9) . . ? N2 C6 C1 104.5(7) . . ? C5 C6 C1 122.3(9) . . ? N2 C7 N1 110.4(7) . . ? N2 C7 C8 124.9(8) . . ? N1 C7 C8 124.7(8) . . ? C7 C8 S1 114.2(6) . . ? C10 C9 S1 116.3(6) . . ? N5 C10 C9 114.1(8) . . ? N5 C12 C13 110.7(8) . . ? C12 C13 S2 106.6(7) . . ? C15 C14 S2 108.0(6) . . ? N3 C15 N4 112.4(8) . . ? N3 C15 C14 122.8(8) . . ? N4 C15 C14 124.8(8) . . ? N4 C16 C17 133.3(8) . . ? N4 C16 C21 105.9(8) . . ? C17 C16 C21 120.8(9) . . ? C18 C17 C16 117.6(9) . . ? C17 C18 C19 122.9(10) . . ? C18 C19 C20 120.5(10) . . ? C19 C20 C21 118.9(9) . . ? C20 C21 N3 133.4(8) . . ? C20 C21 C16 119.2(8) . . ? N3 C21 C16 107.4(8) . . ? N6 C23 C22 169(3) . 3_556 ? Cl2 O5 O7 56.4(18) . . ? O4A O4 Cl1 75.8(19) . . ? O4 O4A Cl1 72.1(19) . . ? O8A O8 Cl2 72(3) . . ? O8 O8A Cl2 82(3) . . ? Cl2 O7 O7A 57(2) . . ? Cl2 O7 O5 56.3(17) . . ? O7A O7 O5 112(3) . . ? Cl2 O7A O7 59.4(19) . . ? O6A O6 Cl2 66(3) . . ? O6 O6A Cl2 76(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.739 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.138 #===END