# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email RCAO@MS.FJIRSM.AC.CN _publ_contact_author_name 'Prof Rong Cao' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; loop_ _publ_author_name 'Daofeng Sun' 'Rong Cao' 'Wenhua Bi' 'Daqiang Yuan' 'Qian Shi' 'Xing Li' data_(2) _database_code_CSD 205535 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu4(OH)2(SIPA)2(py)24H2O]n _chemical_formula_sum 'C6.50 H6.50 Cu N0.50 O5 S0.50' _chemical_formula_weight 251.19 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.5451(5) _cell_length_b 15.8535(6) _cell_length_c 10.8885(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2165.55(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 25.04 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max .45 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 2.105 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .6587 _exptl_absorpt_correction_T_max 1.0000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6367 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2014 _reflns_number_gt 1510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc #_refine_ls_weighting_details calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1146P)^2^+20.2544P] 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 2014 _refine_ls_number_parameters 162 _refine_ls_number_restraints 4 _refine_ls_r_factor_ref 0.1162 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2406 _refine_ls_wR_factor_gt 0.2142 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.153 _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 N N 0.7485(13) 0.2504(7) 0.5000 0.047(3) Uani 1 2 d S . . S S 0.5933(3) 0.1826(2) 1.0000 0.0287(8) Uani 1 2 d S . . Cu1 Cu 0.83888(14) 0.35388(10) 0.5000 0.0300(5) Uani 1 2 d S . . Cu2 Cu 1.0000 0.5000 0.63916(13) 0.0266(5) Uani 1 2 d S . . C1 C 0.8478(7) 0.3918(6) 0.7682(8) 0.027(2) Uani 1 1 d . . . C2 C 0.8038(7) 0.3600(6) 0.8891(8) 0.028(2) Uani 1 1 d . . . C3 C 0.7299(7) 0.2956(6) 0.8890(7) 0.027(2) Uani 1 1 d . . . H3A H 0.7060 0.2734 0.8150 0.032 Uiso 1 1 calc R . . C4 C 0.6910(11) 0.2635(8) 1.0000 0.028(3) Uani 1 2 d S . . C5 C 0.8406(10) 0.3934(8) 1.0000 0.024(3) Uani 1 2 d S . . H5A H 0.8894 0.4375 1.0000 0.028 Uiso 1 2 calc SR . . C11 C 0.657(2) 0.2470(17) 0.435(3) 0.078(9) Uani 0.50 1 d PD . . C12 C 0.585(3) 0.180(2) 0.451(4) 0.22(6) Uani 0.50 1 d PD . . C13 C 0.606(2) 0.1204(18) 0.542(2) 0.060(8) Uani 0.50 1 d PD . . C14 C 0.705(2) 0.1198(13) 0.599(3) 0.104(15) Uani 0.50 1 d PD . . C15 C 0.774(2) 0.1886(15) 0.588(3) 0.080(9) Uani 0.50 1 d PD . . O1 O 0.4917(9) 0.2262(7) 1.0000 0.059(3) Uani 1 2 d S . . O2 O 0.6073(7) 0.1345(4) 0.8883(6) 0.047(2) Uani 1 1 d . . . O3 O 0.8174(7) 0.3528(5) 0.6758(6) 0.052(2) Uani 1 1 d . . . O4 O 0.9130(5) 0.4526(4) 0.7705(5) 0.0265(14) Uani 1 1 d . . . O5 O 0.9081(6) 0.4641(5) 0.5000 0.0213(18) Uani 1 2 d S . . O01 O 0.948(5) 0.131(6) 0.818(10) 0.51(7) Uani 0.50 1 d P . . O02 O 0.822(2) 0.005(3) 1.0000 0.32(3) Uani 1 2 d S . . 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 N 0.084(10) 0.029(6) 0.027(6) 0.000 0.000 -0.030(7) S 0.042(2) 0.0185(15) 0.0261(17) 0.000 0.000 -0.0155(14) Cu1 0.0504(11) 0.0223(9) 0.0172(8) 0.000 0.000 -0.0173(8) Cu2 0.0390(9) 0.0271(8) 0.0137(8) 0.000 0.000 -0.0176(7) C1 0.034(5) 0.031(5) 0.015(4) -0.003(4) 0.002(4) -0.005(4) C2 0.034(5) 0.031(5) 0.020(5) 0.000(4) 0.002(4) -0.012(4) C3 0.037(5) 0.027(5) 0.016(4) -0.005(4) 0.001(4) -0.018(4) C4 0.048(8) 0.015(6) 0.021(6) 0.000 0.000 -0.003(6) C5 0.031(7) 0.025(6) 0.015(6) 0.000 0.000 -0.012(6) C11 0.08(2) 0.08(2) 0.070(17) -0.025(15) 0.008(15) -0.062(17) C12 0.09(2) 0.057(19) 0.51(19) -0.02(5) 0.07(6) -0.05(2) C13 0.059(16) 0.054(16) 0.07(2) 0.010(12) 0.019(12) -0.015(13) C14 0.14(3) 0.013(11) 0.16(3) 0.023(15) 0.08(3) -0.003(15) C15 0.12(3) 0.052(16) 0.073(19) -0.008(15) 0.027(19) -0.001(17) O1 0.042(6) 0.035(6) 0.100(10) 0.000 0.000 -0.018(5) O2 0.075(5) 0.036(4) 0.029(4) -0.007(3) 0.007(4) -0.031(4) O3 0.087(6) 0.052(5) 0.017(3) -0.003(3) 0.003(4) -0.047(5) O4 0.035(3) 0.026(3) 0.018(3) 0.000(3) 0.000(3) -0.021(3) O5 0.027(4) 0.021(4) 0.016(4) 0.000 0.000 -0.007(4) O01 0.25(6) 0.55(13) 0.74(16) -0.17(12) -0.17(9) 0.31(8) O02 0.12(2) 0.27(5) 0.58(10) 0.000 0.000 0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N C11 1.35(3) 6_556 ? N C11 1.35(3) . ? N C15 1.41(3) 6_556 ? N C15 1.41(3) . ? N Cu1 1.995(12) . ? S O2 1.446(7) 6_557 ? S O2 1.446(7) . ? S O1 1.449(12) . ? S C4 1.774(13) . ? Cu1 O3 1.933(7) . ? Cu1 O3 1.933(7) 6_556 ? Cu1 O5 1.951(8) . ? Cu1 O1 2.299(10) 7_665 ? Cu2 O4 1.949(6) 2_765 ? Cu2 O4 1.949(6) . ? Cu2 O5 1.987(5) . ? Cu2 O5 1.987(5) 5_766 ? Cu2 Cu2 3.031(3) 5_766 ? C1 O3 1.240(11) . ? C1 O4 1.265(11) . ? C1 C2 1.514(12) . ? C2 C3 1.380(12) . ? C2 C5 1.396(10) . ? C3 C4 1.399(10) . ? C4 C3 1.399(10) 6_557 ? C5 C2 1.396(10) 6_557 ? C11 C12 1.398(10) . ? C11 C11 1.41(6) 6_556 ? C11 C15 1.76(4) 6_556 ? C11 C12 1.86(4) 6_556 ? C12 C13 0.99(4) 6_556 ? C12 C12 1.07(10) 6_556 ? C12 C13 1.397(10) . ? C12 C11 1.86(4) 6_556 ? C12 C14 1.87(6) 6_556 ? C13 C13 0.91(5) 6_556 ? C13 C12 0.99(4) 6_556 ? C13 C14 1.392(10) . ? C13 C14 1.97(3) 6_556 ? C14 C15 1.397(10) . ? C14 C12 1.87(6) 6_556 ? C14 C13 1.97(3) 6_556 ? C15 C11 1.76(4) 6_556 ? C15 C15 1.91(6) 6_556 ? O1 Cu1 2.299(10) 7_566 ? O5 Cu2 1.987(5) 5_766 ? 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 C11 N C11 63(2) 6_556 . ? C11 N C15 121.5(17) 6_556 6_556 ? C11 N C15 79.1(17) . 6_556 ? C11 N C15 79.1(17) 6_556 . ? C11 N C15 121.5(17) . . ? C15 N C15 86(2) 6_556 . ? C11 N Cu1 121.1(13) 6_556 . ? C11 N Cu1 121.1(13) . . ? C15 N Cu1 116.3(13) 6_556 . ? C15 N Cu1 116.3(13) . . ? O2 S O2 114.5(6) 6_557 . ? O2 S O1 111.0(4) 6_557 . ? O2 S O1 111.0(4) . . ? O2 S C4 107.3(4) 6_557 . ? O2 S C4 107.3(4) . . ? O1 S C4 105.2(6) . . ? O3 Cu1 O3 164.0(5) . 6_556 ? O3 Cu1 O5 94.0(2) . . ? O3 Cu1 O5 94.0(2) 6_556 . ? O3 Cu1 N 85.1(2) . . ? O3 Cu1 N 85.1(2) 6_556 . ? O5 Cu1 N 171.8(5) . . ? O3 Cu1 O1 96.4(3) . 7_665 ? O3 Cu1 O1 96.4(3) 6_556 7_665 ? O5 Cu1 O1 97.1(4) . 7_665 ? N Cu1 O1 91.1(5) . 7_665 ? O4 Cu2 O4 85.6(3) 2_765 . ? O4 Cu2 O5 174.0(3) 2_765 . ? O4 Cu2 O5 97.1(2) . . ? O4 Cu2 O5 97.1(2) 2_765 5_766 ? O4 Cu2 O5 174.0(3) . 5_766 ? O5 Cu2 O5 80.6(3) . 5_766 ? O4 Cu2 Cu2 137.18(16) 2_765 5_766 ? O4 Cu2 Cu2 137.19(16) . 5_766 ? O5 Cu2 Cu2 40.31(17) . 5_766 ? O5 Cu2 Cu2 40.31(17) 5_766 5_766 ? O3 C1 O4 126.5(8) . . ? O3 C1 C2 115.3(8) . . ? O4 C1 C2 118.2(7) . . ? C3 C2 C5 120.2(8) . . ? C3 C2 C1 119.4(8) . . ? C5 C2 C1 120.4(8) . . ? C2 C3 C4 120.2(8) . . ? C3 C4 C3 119.4(11) 6_557 . ? C3 C4 S 120.3(6) 6_557 . ? C3 C4 S 120.3(6) . . ? C2 C5 C2 119.7(11) 6_557 . ? N C11 C12 121(3) . . ? N C11 C11 58.5(12) . 6_556 ? C12 C11 C11 83(2) . 6_556 ? N C11 C15 51.9(15) . 6_556 ? C12 C11 C15 99(3) . 6_556 ? C11 C11 C15 98.3(14) 6_556 6_556 ? N C11 C12 95(2) . 6_556 ? C12 C11 C12 35(3) . 6_556 ? C11 C11 C12 48.2(12) 6_556 6_556 ? C15 C11 C12 102(2) 6_556 6_556 ? C13 C12 C12 85(4) 6_556 6_556 ? C13 C12 C13 40(3) 6_556 . ? C12 C12 C13 45(2) 6_556 . ? C13 C12 C11 124(4) 6_556 . ? C12 C12 C11 97(2) 6_556 . ? C13 C12 C11 119(3) . . ? C13 C12 C11 111(3) 6_556 6_556 ? C12 C12 C11 48.2(12) 6_556 6_556 ? C13 C12 C11 80(2) . 6_556 ? C11 C12 C11 49(2) . 6_556 ? C13 C12 C14 47(3) 6_556 6_556 ? C12 C12 C14 106.9(17) 6_556 6_556 ? C13 C12 C14 73(2) . 6_556 ? C11 C12 C14 80(2) . 6_556 ? C11 C12 C14 95.5(19) 6_556 6_556 ? C13 C13 C12 95(4) 6_556 6_556 ? C13 C13 C14 116.8(18) 6_556 . ? C12 C13 C14 102(4) 6_556 . ? C13 C13 C12 45(2) 6_556 . ? C12 C13 C12 50(6) 6_556 . ? C14 C13 C12 119(3) . . ? C13 C13 C14 39.0(10) 6_556 6_556 ? C12 C13 C14 104(3) 6_556 6_556 ? C14 C13 C14 78(3) . 6_556 ? C12 C13 C14 65(2) . 6_556 ? C13 C14 C15 121(2) . . ? C13 C14 C12 31.3(13) . 6_556 ? C15 C14 C12 94(2) . 6_556 ? C13 C14 C13 24.2(13) . 6_556 ? C15 C14 C13 109(2) . 6_556 ? C12 C14 C13 42.6(9) 6_556 6_556 ? C14 C15 N 118(3) . . ? C14 C15 C11 84.6(19) . 6_556 ? N C15 C11 49.0(15) . 6_556 ? C14 C15 C15 95.1(19) . 6_556 ? N C15 C15 47.1(12) . 6_556 ? C11 C15 C15 81.7(14) 6_556 6_556 ? S O1 Cu1 118.0(6) . 7_566 ? C1 O3 Cu1 139.1(6) . . ? C1 O4 Cu2 129.9(5) . . ? Cu1 O5 Cu2 121.0(3) . . ? Cu1 O5 Cu2 121.0(3) . 5_766 ? Cu2 O5 Cu2 99.4(3) . 5_766 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.929 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.205 data_(1) _database_code_CSD 205536 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu4(OH)2(SIPA)2(bipy)22H2O]n _chemical_formula_sum 'C9 H7 Cu N O4.50 S0.50' _chemical_formula_weight 280.73 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 10.9368(10) _cell_length_b 16.2104(16) _cell_length_c 10.7803(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1911.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.10 _exptl_crystal_description plate _exptl_crystal_colour 'deep blue' _exptl_crystal_size_max .40 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 2.394 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .8180 _exptl_absorpt_correction_T_max 1.0000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5971 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.10 _reflns_number_total 1802 _reflns_number_gt 1111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc #_refine_ls_weighting_details calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+16.0791P] 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 1802 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.1202 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _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 S S 0.2746(3) -0.09350(17) 0.0000 0.0401(8) Uani 1 2 d S . . Cu1 Cu 0.49380(15) -0.31834(6) 0.5000 0.0261(3) Uani 1 2 d S . . Cu2 Cu 0.5000 -0.5000 0.36457(10) 0.0325(4) Uani 1 2 d S . . O1 O 0.1974(13) -0.0918(7) -0.0987(7) 0.195(7) Uani 1 1 d . . . O2 O 0.3548(11) -0.0404(6) -0.0785(12) 0.050(3) Uani 0.50 1 d P . . O3 O 0.4561(6) -0.3058(3) 0.3242(4) 0.0446(17) Uani 1 1 d . . . O4 O 0.4414(5) -0.4296(3) 0.2332(4) 0.0388(14) Uani 1 1 d . . . O5 O 0.4337(7) -0.4320(4) 0.5000 0.0255(16) Uani 1 2 d S . . N1 N 0.5623(8) -0.2015(5) 0.5000 0.027(2) Uani 1 2 d S . . N2 N 0.7942(9) 0.2085(6) 0.5000 0.043(3) Uani 1 2 d S . . C1 C 0.4377(7) -0.3529(4) 0.2331(7) 0.0302(18) Uani 1 1 d . . . C2 C 0.4125(7) -0.3116(4) 0.1115(6) 0.0245(17) Uani 1 1 d . . . C3 C 0.3711(7) -0.2304(4) 0.1101(7) 0.0276(18) Uani 1 1 d . . . H3 H 0.368(7) -0.204(4) 0.181(7) 0.04(2) Uiso 1 1 d . . . C4 C 0.3478(10) -0.1904(5) 0.0000 0.023(2) Uani 1 2 d S . . C5 C 0.4279(10) -0.3534(6) 0.0000 0.023(2) Uani 1 2 d S . . H5 H 0.452(10) -0.409(7) 0.0000 0.05(3) Uiso 1 2 d S . . C11 C 0.5855(9) -0.1609(5) 0.3951(8) 0.044(2) Uani 1 1 d . . . H11 H 0.576(8) -0.186(5) 0.323(8) 0.05(3) Uiso 1 1 d . . . C12 C 0.6314(9) -0.0819(5) 0.3923(8) 0.043(2) Uani 1 1 d . . . H12 H 0.638(7) -0.056(4) 0.319(7) 0.04(2) Uiso 1 1 d . . . C13 C 0.6557(11) -0.0384(6) 0.5000 0.031(3) Uani 1 2 d S . . C14 C 0.7067(10) 0.0457(6) 0.5000 0.029(3) Uani 1 2 d S . . C15 C 0.7319(9) 0.0867(5) 0.6091(8) 0.043(2) Uani 1 1 d . . . H15 H 0.720(8) 0.061(5) 0.679(8) 0.05(3) Uiso 1 1 d . . . C16 C 0.7745(9) 0.1670(5) 0.6035(9) 0.051(3) Uani 1 1 d . . . H16 H 0.804(7) 0.195(5) 0.672(7) 0.04(2) Uiso 1 1 d . . . O01 O 0.2034(11) -0.3794(6) 0.4491(12) 0.063(4) Uani 0.50 1 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 S 0.058(2) 0.0171(13) 0.0448(18) 0.000 0.000 0.0154(14) Cu1 0.0518(9) 0.0131(6) 0.0133(6) 0.000 0.000 -0.0006(7) Cu2 0.0703(10) 0.0146(6) 0.0126(5) 0.000 0.000 0.0098(7) O1 0.324(16) 0.201(11) 0.060(5) -0.061(7) -0.081(8) 0.232(12) O2 0.051(7) 0.027(6) 0.070(8) 0.020(6) 0.013(7) 0.004(6) O3 0.100(5) 0.017(2) 0.017(3) 0.000(2) -0.013(3) -0.003(3) O4 0.085(4) 0.015(3) 0.016(3) 0.001(2) -0.008(3) 0.008(3) O5 0.051(5) 0.009(3) 0.016(3) 0.000 0.000 0.003(3) N1 0.045(6) 0.013(4) 0.022(5) 0.000 0.000 0.003(4) N2 0.030(6) 0.033(5) 0.065(7) 0.000 0.000 -0.002(5) C1 0.047(5) 0.026(4) 0.018(4) 0.002(3) 0.000(4) 0.002(4) C2 0.040(5) 0.017(4) 0.016(4) 0.006(3) 0.003(3) -0.001(3) C3 0.044(5) 0.015(3) 0.024(4) -0.002(3) 0.004(4) 0.002(3) C4 0.037(6) 0.010(5) 0.024(5) 0.000 0.000 0.006(4) C5 0.030(6) 0.016(5) 0.021(5) 0.000 0.000 0.007(5) C11 0.081(7) 0.028(4) 0.025(5) -0.004(4) 0.009(5) -0.004(5) C12 0.073(7) 0.029(4) 0.027(5) 0.003(4) 0.010(4) -0.013(4) C13 0.035(7) 0.021(5) 0.037(7) 0.000 0.000 0.004(5) C14 0.037(7) 0.012(5) 0.039(7) 0.000 0.000 0.007(5) C15 0.063(6) 0.029(4) 0.037(5) 0.000(4) 0.014(5) -0.009(4) C16 0.062(6) 0.042(5) 0.050(6) -0.019(5) 0.018(5) -0.022(5) O01 0.057(8) 0.034(6) 0.098(13) -0.004(6) 0.003(7) 0.000(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 S O1 1.359(9) . ? S O1 1.359(9) 6 ? S O2 1.492(11) 6 ? S O2 1.492(11) . ? S C4 1.762(9) . ? Cu1 O5 1.956(6) . ? Cu1 O3 1.950(5) . ? Cu1 O3 1.950(5) 6_556 ? Cu1 N1 2.036(8) . ? Cu2 O4 1.929(5) . ? Cu2 O4 1.929(5) 2_645 ? Cu2 O5 1.968(4) . ? Cu2 O5 1.968(4) 5_646 ? Cu2 Cu2 2.920(2) 5_646 ? O2 O2 1.69(3) 6 ? O3 C1 1.260(8) . ? O4 C1 1.243(8) . ? O5 Cu2 1.968(4) 5_646 ? N1 C11 1.333(9) 6_556 ? N1 C11 1.333(9) . ? N2 C16 1.321(10) 6_556 ? N2 C16 1.321(10) . ? C1 C2 1.497(9) . ? C2 C5 1.391(8) . ? C2 C3 1.391(9) . ? C3 C4 1.377(8) . ? C4 C3 1.377(8) 6 ? C5 C2 1.391(8) 6 ? C11 C12 1.375(11) . ? C12 C13 1.385(10) . ? C13 C12 1.385(10) 6_556 ? C13 C14 1.472(13) . ? C14 C15 1.379(10) . ? C14 C15 1.379(10) 6_556 ? C15 C16 1.384(11) . ? O01 O01 1.10(3) 6_556 ? 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 O1 S O1 103.1(11) . 6 ? O1 S O2 143.0(8) . 6 ? O1 S O2 84.8(8) 6 6 ? O1 S O2 84.8(8) . . ? O1 S O2 143.0(8) 6 . ? O2 S O2 69.1(10) 6 . ? O1 S C4 107.5(4) . . ? O1 S C4 107.5(4) 6 . ? O2 S C4 104.3(5) 6 . ? O2 S C4 104.3(5) . . ? O5 Cu1 O3 91.56(15) . . ? O5 Cu1 O3 91.56(15) . 6_556 ? O3 Cu1 O3 152.7(4) . 6_556 ? O5 Cu1 N1 178.0(4) . . ? O3 Cu1 N1 88.91(16) . . ? O3 Cu1 N1 88.91(16) 6_556 . ? O4 Cu2 O4 85.5(3) . 2_645 ? O4 Cu2 O5 95.23(19) . . ? O4 Cu2 O5 177.2(3) 2_645 . ? O4 Cu2 O5 177.2(3) . 5_646 ? O4 Cu2 O5 95.23(19) 2_645 5_646 ? O5 Cu2 O5 84.2(3) . 5_646 ? O4 Cu2 Cu2 137.26(15) . 5_646 ? O4 Cu2 Cu2 137.26(15) 2_645 5_646 ? O5 Cu2 Cu2 42.10(14) . 5_646 ? O5 Cu2 Cu2 42.10(14) 5_646 5_646 ? S O2 O2 55.4(5) . 6 ? C1 O3 Cu1 136.7(5) . . ? C1 O4 Cu2 127.1(5) . . ? Cu1 O5 Cu2 113.8(3) . . ? Cu1 O5 Cu2 113.8(3) . 5_646 ? Cu2 O5 Cu2 95.8(3) . 5_646 ? C11 N1 C11 116.0(9) 6_556 . ? C11 N1 Cu1 122.0(5) 6_556 . ? C11 N1 Cu1 122.0(5) . . ? C16 N2 C16 115.3(11) 6_556 . ? O4 C1 O3 126.9(7) . . ? O4 C1 C2 117.0(6) . . ? O3 C1 C2 116.1(6) . . ? C5 C2 C3 119.4(7) . . ? C5 C2 C1 121.1(6) . . ? C3 C2 C1 119.5(6) . . ? C4 C3 C2 121.0(7) . . ? C3 C4 C3 119.1(9) 6 . ? C3 C4 S 120.3(4) 6 . ? C3 C4 S 120.3(4) . . ? C2 C5 C2 119.7(9) 6 . ? N1 C11 C12 123.3(8) . . ? C11 C12 C13 121.8(8) . . ? C12 C13 C12 113.9(10) . 6_556 ? C12 C13 C14 123.0(5) . . ? C12 C13 C14 123.0(5) 6_556 . ? C15 C14 C15 117.1(10) . 6_556 ? C15 C14 C13 121.5(5) . . ? C15 C14 C13 121.5(5) 6_556 . ? C14 C15 C16 119.0(9) . . ? N2 C16 C15 124.8(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.022 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.127