# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xian-Ming Zhang' _publ_contact_author_email ZHANGXM@DNS.SXNU.EDU.CN _publ_section_title ; Luminescent Boracite-Like Metal-Organic Frameworks Constructed by Cu-centered CuCu4 Tetrahedra and CuCu3 Triangles with Acentric Cubic Superlarge Cell ; loop_ _publ_author_name 'Xian-Ming Zhang' 'Cai-Hong Guo' 'Zheng-Ming Hao' 'Hai-Shun Wu' # Attachment 'zhangxm1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 731918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H72 Cl4 Cu31 N96 O32 S32' _chemical_formula_weight 5643.48 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 36.577(7) _cell_length_b 36.577(7) _cell_length_c 36.577(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 48936(17) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7633 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 19.74 _exptl_crystal_description cubic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 22136 _exptl_absorpt_coefficient_mu 3.005 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5848 _exptl_absorpt_correction_T_max 0.6449 _exptl_absorpt_process_details 'SADABS, sheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84715 _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4019 _reflns_number_gt 3734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0261P)^2^+295.6768P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.46(2) _refine_ls_number_reflns 4019 _refine_ls_number_parameters 190 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 505.3 165.7 2 0.500 0.000 0.000 505.4 168.9 3 0.000 0.000 0.500 505.2 168.9 4 0.500 0.000 0.500 505.4 165.7 5 0.250 0.250 0.250 1990.5 325.0 6 0.750 0.250 0.250 1990.6 324.2 7 0.250 0.250 0.750 1990.6 324.2 8 0.750 0.250 0.750 1990.5 325.0 9 0.000 0.500 0.000 505.2 168.9 10 0.500 0.500 0.000 505.3 165.7 11 1.000 0.500 0.500 505.3 165.7 12 0.500 0.500 0.500 505.1 168.9 13 0.250 0.750 0.250 1990.6 324.2 14 0.750 0.750 0.250 1990.5 325.0 15 0.250 0.750 0.750 1990.5 325.0 16 0.750 0.750 0.750 1990.6 324.2 _platon_squeeze_details ; ; 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 0.85210(2) 0.85210(2) 0.35210(2) 0.0429(3) Uani 1 3 d S . . Cu2 Cu 0.89121(2) 0.91401(2) 0.33118(3) 0.0457(2) Uani 1 1 d . . . Cu3 Cu 0.95348(2) 0.945189(19) 0.26875(2) 0.0376(2) Uani 1 1 d . . . Cu4 Cu 1.0000 1.0000 0.2500 0.0309(3) Uani 1 4 d S . . Cl1 Cl 0.90038(4) 0.90038(4) 0.40038(4) 0.0400(6) Uani 1 3 d S . . S1 S 0.95747(4) 0.96786(4) 0.21144(4) 0.0292(3) Uani 1 1 d . . . S2 S 0.89894(5) 0.81609(4) 0.33165(4) 0.0383(4) Uani 1 1 d . . . S3 S 1.0000 1.2500 0.2500 0.0337(6) Uani 1 4 d S . . S4 S 1.0000 1.0000 0.5000 0.0581(16) Uani 1 12 d S . . S5 S 0.91510(10) 1.08490(10) 0.41510(10) 0.0527(18) Uani 0.703(10) 3 d SPD A 1 O4 O 0.9385(3) 1.0615(3) 0.4385(3) 0.153(10) Uani 0.703(10) 3 d SPD A 1 S5' S 0.8943(2) 1.1057(2) 0.3943(2) 0.047(4) Uani 0.297(10) 3 d SPD A 2 O4' O 0.8705(4) 1.1295(4) 0.3705(4) 0.118(18) Uani 0.297(10) 3 d SPDU A 2 O1 O 1.02244(14) 1.23879(12) 0.28147(13) 0.0513(12) Uani 1 1 d . . . O2 O 0.97691(16) 0.97691(16) 0.47691(16) 0.077(3) Uani 1 3 d S . . O3 O 0.87712(18) 1.07040(19) 0.4112(2) 0.098(3) Uani 1 1 d . . . N1 N 1.02098(12) 0.93064(13) 0.19517(12) 0.0287(10) Uani 1 1 d . . . N2 N 1.03304(13) 0.90394(14) 0.16992(13) 0.0329(11) Uani 1 1 d . . . N3 N 0.97498(13) 0.91553(13) 0.16052(12) 0.0315(11) Uani 1 1 d . . . H3A H 0.9535 0.9147 0.1511 0.038 Uiso 1 1 calc R . . N4 N 1.00396(17) 0.87051(17) 0.12237(16) 0.0582(18) Uani 1 1 d . . . H4A H 1.0233 0.8582 0.1172 0.070 Uiso 1 1 calc R . . H4B H 0.9841 0.8669 0.1103 0.070 Uiso 1 1 calc R . . N5 N 0.92648(14) 0.88126(13) 0.30537(14) 0.0335(11) Uani 1 1 d . . . N6 N 0.95389(13) 0.89286(12) 0.28159(13) 0.0311(11) Uani 1 1 d . . . N7 N 0.95469(15) 0.83278(13) 0.28422(13) 0.0373(12) Uani 1 1 d . . . H7A H 0.9609 0.8104 0.2806 0.045 Uiso 1 1 calc R . . N8 N 0.99800(18) 0.86110(16) 0.24460(18) 0.063(2) Uani 1 1 d . . . H8A H 1.0068 0.8809 0.2355 0.076 Uiso 1 1 calc R . . H8B H 1.0068 0.8403 0.2381 0.076 Uiso 1 1 calc R . . C1 C 0.98606(15) 0.93668(15) 0.18903(14) 0.0273(12) Uani 1 1 d . . . C2 C 1.00478(17) 0.89606(17) 0.14992(16) 0.0360(14) Uani 1 1 d . . . C3 C 0.92726(16) 0.84509(15) 0.30629(16) 0.0324(13) Uani 1 1 d . . . C4 C 0.97000(17) 0.86266(17) 0.26927(17) 0.0365(14) 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 0.0429(3) 0.0429(3) 0.0429(3) 0.0064(4) 0.0064(4) 0.0064(4) Cu2 0.0468(5) 0.0286(4) 0.0616(5) -0.0024(4) 0.0211(4) 0.0022(3) Cu3 0.0488(5) 0.0271(4) 0.0370(4) 0.0006(3) 0.0151(4) 0.0034(3) Cu4 0.0298(4) 0.0298(4) 0.0331(7) 0.000 0.000 0.000 Cl1 0.0400(6) 0.0400(6) 0.0400(6) 0.0026(7) 0.0026(7) 0.0026(7) S1 0.0288(7) 0.0304(7) 0.0285(7) -0.0006(6) 0.0006(6) 0.0021(6) S2 0.0461(9) 0.0264(7) 0.0423(8) 0.0006(7) 0.0108(7) -0.0020(7) S3 0.0504(18) 0.0253(8) 0.0253(8) 0.000 0.000 0.000 S4 0.0581(16) 0.0581(16) 0.0581(16) 0.000 0.000 0.000 S5 0.0527(18) 0.0527(18) 0.0527(18) -0.0246(19) 0.0246(19) -0.0246(19) O4 0.153(10) 0.153(10) 0.153(10) 0.007(11) -0.007(11) 0.007(11) S5' 0.047(4) 0.047(4) 0.047(4) -0.017(4) 0.017(4) -0.017(4) O4' 0.118(18) 0.118(18) 0.118(18) -0.04(2) 0.04(2) -0.04(2) O1 0.075(3) 0.032(2) 0.046(3) -0.001(2) -0.013(3) 0.011(2) O2 0.077(3) 0.077(3) 0.077(3) -0.010(3) -0.010(3) -0.010(3) O3 0.092(4) 0.102(5) 0.101(5) -0.064(4) 0.061(4) -0.062(4) N1 0.027(2) 0.035(3) 0.024(2) -0.004(2) 0.0055(19) -0.002(2) N2 0.031(3) 0.042(3) 0.026(2) -0.006(2) -0.001(2) -0.001(2) N3 0.030(3) 0.041(3) 0.023(2) -0.010(2) -0.0060(19) 0.003(2) N4 0.043(3) 0.078(4) 0.054(4) -0.037(3) -0.017(3) 0.011(3) N5 0.038(3) 0.026(3) 0.037(3) -0.002(2) 0.010(2) 0.002(2) N6 0.038(3) 0.021(2) 0.034(3) 0.0040(19) 0.012(2) 0.008(2) N7 0.051(3) 0.022(2) 0.038(3) 0.000(2) 0.011(2) 0.008(2) N8 0.073(4) 0.030(3) 0.086(5) 0.006(3) 0.050(4) 0.012(3) C1 0.026(3) 0.030(3) 0.026(3) 0.004(2) 0.006(2) 0.002(2) C2 0.037(3) 0.040(3) 0.031(3) -0.006(3) 0.008(3) -0.001(3) C3 0.035(3) 0.032(3) 0.030(3) 0.000(2) 0.003(3) 0.009(3) C4 0.036(3) 0.036(3) 0.037(3) 0.003(3) 0.006(3) 0.002(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 Cu1 S2 2.2869(16) 33_554 ? Cu1 S2 2.2869(16) 53_554 ? Cu1 S2 2.2869(17) . ? Cu1 Cu2 2.7858(13) 53_554 ? Cu1 Cu2 2.7858(13) . ? Cu1 Cu2 2.7858(13) 33_554 ? Cu2 N2 1.992(5) 87_465 ? Cu2 N5 1.998(5) . ? Cu2 S2 2.314(2) 53_554 ? Cu2 Cl1 2.6015(18) . ? Cu3 N6 1.971(5) . ? Cu3 N1 1.993(5) 87_465 ? Cu3 S1 2.2592(16) . ? Cu3 Cu4 2.7175(9) . ? Cu4 S1 2.4065(15) 87_465 ? Cu4 S1 2.4065(15) . ? Cu4 S1 2.4065(15) 2_775 ? Cu4 S1 2.4065(15) 88_645 ? Cu4 Cu3 2.7175(9) 87_465 ? Cu4 Cu3 2.7175(9) 2_775 ? Cu4 Cu3 2.7175(9) 88_645 ? Cl1 Cu2 2.6015(18) 53_554 ? Cl1 Cu2 2.6015(18) 33_554 ? S1 C1 1.751(6) . ? S2 C3 1.749(6) . ? S2 Cu2 2.314(2) 33_554 ? S3 O1 1.472(5) 90_656 ? S3 O1 1.472(5) . ? S3 O1 1.472(5) 67_663 ? S3 O1 1.472(5) 28_575 ? S4 O2 1.463(10) 4_576 ? S4 O2 1.463(10) . ? S4 O2 1.463(10) 2_775 ? S4 O2 1.463(10) 3_756 ? S5 O4 1.486(16) . ? S5 O3 1.494(6) 54_576 ? S5 O3 1.494(6) . ? S5 O3 1.494(6) 36_764 ? S5' O4' 1.508(19) . ? S5' O3 1.562(9) . ? S5' O3 1.562(9) 54_576 ? S5' O3 1.562(9) 36_764 ? N1 C1 1.315(7) . ? N1 N2 1.415(6) . ? N1 Cu3 1.993(5) 88_645 ? N2 C2 1.299(7) . ? N2 Cu2 1.992(5) 88_645 ? N3 C2 1.359(7) . ? N3 C1 1.360(7) . ? N4 C2 1.374(7) . ? N5 C3 1.324(7) . ? N5 N6 1.393(6) . ? N6 C4 1.330(8) . ? N7 C4 1.344(8) . ? N7 C3 1.364(8) . ? N8 C4 1.366(8) . ? 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 S2 Cu1 S2 119.223(17) 33_554 53_554 ? S2 Cu1 S2 119.222(17) 33_554 . ? S2 Cu1 S2 119.222(17) 53_554 . ? S2 Cu1 Cu2 53.18(5) 33_554 53_554 ? S2 Cu1 Cu2 89.63(5) 53_554 53_554 ? S2 Cu1 Cu2 140.12(7) . 53_554 ? S2 Cu1 Cu2 140.12(7) 33_554 . ? S2 Cu1 Cu2 53.18(5) 53_554 . ? S2 Cu1 Cu2 89.63(5) . . ? Cu2 Cu1 Cu2 86.95(5) 53_554 . ? S2 Cu1 Cu2 89.63(5) 33_554 33_554 ? S2 Cu1 Cu2 140.12(7) 53_554 33_554 ? S2 Cu1 Cu2 53.18(5) . 33_554 ? Cu2 Cu1 Cu2 86.95(5) 53_554 33_554 ? Cu2 Cu1 Cu2 86.95(5) . 33_554 ? N2 Cu2 N5 115.0(2) 87_465 . ? N2 Cu2 S2 116.53(16) 87_465 53_554 ? N5 Cu2 S2 110.64(16) . 53_554 ? N2 Cu2 Cl1 100.13(15) 87_465 . ? N5 Cu2 Cl1 105.17(15) . . ? S2 Cu2 Cl1 107.92(6) 53_554 . ? N2 Cu2 Cu1 156.32(14) 87_465 . ? N5 Cu2 Cu1 88.51(14) . . ? S2 Cu2 Cu1 52.29(5) 53_554 . ? Cl1 Cu2 Cu1 69.10(6) . . ? N6 Cu3 N1 116.65(19) . 87_465 ? N6 Cu3 S1 125.24(14) . . ? N1 Cu3 S1 114.43(13) 87_465 . ? N6 Cu3 Cu4 140.53(14) . . ? N1 Cu3 Cu4 88.37(14) 87_465 . ? S1 Cu3 Cu4 56.94(4) . . ? S1 Cu4 S1 110.09(3) 87_465 . ? S1 Cu4 S1 110.09(3) 87_465 2_775 ? S1 Cu4 S1 108.24(7) . 2_775 ? S1 Cu4 S1 108.24(7) 87_465 88_645 ? S1 Cu4 S1 110.09(3) . 88_645 ? S1 Cu4 S1 110.09(3) 2_775 88_645 ? S1 Cu4 Cu3 51.89(4) 87_465 87_465 ? S1 Cu4 Cu3 71.40(4) . 87_465 ? S1 Cu4 Cu3 91.33(4) 2_775 87_465 ? S1 Cu4 Cu3 155.93(4) 88_645 87_465 ? S1 Cu4 Cu3 91.33(4) 87_465 . ? S1 Cu4 Cu3 51.89(4) . . ? S1 Cu4 Cu3 155.93(4) 2_775 . ? S1 Cu4 Cu3 71.40(4) 88_645 . ? Cu3 Cu4 Cu3 93.653(8) 87_465 . ? S1 Cu4 Cu3 71.40(4) 87_465 2_775 ? S1 Cu4 Cu3 155.93(4) . 2_775 ? S1 Cu4 Cu3 51.89(4) 2_775 2_775 ? S1 Cu4 Cu3 91.33(4) 88_645 2_775 ? Cu3 Cu4 Cu3 93.653(8) 87_465 2_775 ? Cu3 Cu4 Cu3 150.76(3) . 2_775 ? S1 Cu4 Cu3 155.93(4) 87_465 88_645 ? S1 Cu4 Cu3 91.33(4) . 88_645 ? S1 Cu4 Cu3 71.40(4) 2_775 88_645 ? S1 Cu4 Cu3 51.89(4) 88_645 88_645 ? Cu3 Cu4 Cu3 150.76(3) 87_465 88_645 ? Cu3 Cu4 Cu3 93.653(8) . 88_645 ? Cu3 Cu4 Cu3 93.653(8) 2_775 88_645 ? Cu2 Cl1 Cu2 94.92(7) 53_554 . ? Cu2 Cl1 Cu2 94.92(7) 53_554 33_554 ? Cu2 Cl1 Cu2 94.92(7) . 33_554 ? C1 S1 Cu3 103.51(18) . . ? C1 S1 Cu4 101.91(19) . . ? Cu3 S1 Cu4 71.17(5) . . ? C3 S2 Cu1 105.55(19) . . ? C3 S2 Cu2 102.3(2) . 33_554 ? Cu1 S2 Cu2 74.53(6) . 33_554 ? O1 S3 O1 108.1(2) 90_656 . ? O1 S3 O1 112.2(4) 90_656 67_663 ? O1 S3 O1 108.1(2) . 67_663 ? O1 S3 O1 108.1(2) 90_656 28_575 ? O1 S3 O1 112.2(4) . 28_575 ? O1 S3 O1 108.1(2) 67_663 28_575 ? O2 S4 O2 109.471(2) 4_576 . ? O2 S4 O2 109.471(5) 4_576 2_775 ? O2 S4 O2 109.471(3) . 2_775 ? O2 S4 O2 109.471(2) 4_576 3_756 ? O2 S4 O2 109.471(1) . 3_756 ? O2 S4 O2 109.471(6) 2_775 3_756 ? O4 S5 O3 112.8(4) . 54_576 ? O4 S5 O3 112.8(4) . . ? O3 S5 O3 106.0(5) 54_576 . ? O4 S5 O3 112.8(4) . 36_764 ? O3 S5 O3 106.0(5) 54_576 36_764 ? O3 S5 O3 106.0(5) . 36_764 ? O4' S5' O3 118.2(5) . . ? O4' S5' O3 118.2(5) . 54_576 ? O3 S5' O3 99.5(7) . 54_576 ? O4' S5' O3 118.2(5) . 36_764 ? O3 S5' O3 99.5(7) . 36_764 ? O3 S5' O3 99.5(7) 54_576 36_764 ? S5 O3 S5' 51.0(5) . . ? C1 N1 N2 107.9(4) . . ? C1 N1 Cu3 130.2(4) . 88_645 ? N2 N1 Cu3 121.9(3) . 88_645 ? C2 N2 N1 105.8(5) . . ? C2 N2 Cu2 135.3(4) . 88_645 ? N1 N2 Cu2 118.5(3) . 88_645 ? C2 N3 C1 106.1(5) . . ? C3 N5 N6 107.7(5) . . ? C3 N5 Cu2 127.0(4) . . ? N6 N5 Cu2 125.2(3) . . ? C4 N6 N5 106.1(4) . . ? C4 N6 Cu3 136.8(4) . . ? N5 N6 Cu3 116.0(3) . . ? C4 N7 C3 106.2(5) . . ? N1 C1 N3 109.0(5) . . ? N1 C1 S1 127.5(4) . . ? N3 C1 S1 123.4(4) . . ? N2 C2 N3 111.2(5) . . ? N2 C2 N4 125.5(6) . . ? N3 C2 N4 123.2(6) . . ? N5 C3 N7 109.3(5) . . ? N5 C3 S2 127.4(4) . . ? N7 C3 S2 123.3(4) . . ? N6 C4 N7 110.7(5) . . ? N6 C4 N8 126.2(6) . . ? N7 C4 N8 123.1(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.545 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.088 #============================================================ data_2 _database_code_depnum_ccdc_archive 'CCDC 731919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H72 Br4 Cu31 N96 O32 S32' _chemical_formula_weight 5821.32 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' Br Br -0.2901 2.4595 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 36.3997(5) _cell_length_b 36.3997(5) _cell_length_c 36.3997(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 48227.4(11) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6143 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 22.79 _exptl_crystal_description cubic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 22712 _exptl_absorpt_coefficient_mu 3.668 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6277 _exptl_absorpt_correction_T_max 0.6673 _exptl_absorpt_process_details 'SADABS, sheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75603 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3952 _reflns_number_gt 3748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0546P)^2^+42.0491P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.238(12) _refine_ls_number_reflns 3952 _refine_ls_number_parameters 190 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.110 0.000 0.000 87.4 26.6 2 0.390 0.000 0.000 85.5 26.2 3 0.610 0.000 0.000 87.5 26.6 4 0.890 0.000 0.000 85.5 26.3 5 0.000 0.000 0.111 85.0 28.2 6 0.500 0.000 0.111 84.9 27.8 7 0.000 0.000 0.390 85.8 24.9 8 0.500 0.000 0.390 85.8 24.5 9 0.111 0.000 0.501 86.3 26.6 10 0.889 0.000 0.501 84.4 26.2 11 0.390 0.000 0.501 84.4 26.3 12 0.610 0.000 0.501 86.2 26.5 13 0.000 0.000 0.611 84.9 27.8 14 0.500 0.000 0.611 85.0 28.2 15 0.000 0.000 0.889 83.4 24.3 16 0.500 0.000 0.889 83.5 24.9 17 0.250 0.250 0.250 1932.4 352.5 18 0.750 0.250 0.250 1932.5 349.0 19 0.250 0.250 0.750 1932.5 349.0 20 0.750 0.250 0.750 1932.4 352.5 21 0.500 0.112 0.000 82.7 26.3 22 1.000 0.112 0.000 82.7 26.2 23 0.500 0.112 0.500 82.8 26.2 24 0.000 0.112 0.500 82.7 26.3 25 0.000 0.390 0.000 85.5 26.2 26 0.500 0.390 0.000 85.5 26.2 27 1.000 0.390 0.500 85.5 26.2 28 0.500 0.390 0.500 85.6 26.3 29 0.611 0.501 0.000 86.2 26.6 30 0.000 0.501 0.110 86.1 28.0 31 0.500 0.501 0.389 84.6 24.9 32 0.889 0.501 0.500 84.4 26.2 33 0.111 0.501 0.500 86.2 26.6 34 0.500 0.501 0.610 86.1 28.0 35 1.000 0.501 0.889 84.6 24.9 36 0.389 0.501 1.000 84.4 26.2 37 0.112 0.501 0.000 83.9 26.4 38 0.500 0.501 0.112 83.8 28.2 39 1.000 0.501 0.388 82.3 24.4 40 0.388 0.501 0.500 82.0 26.1 41 0.612 0.501 0.500 83.9 26.4 42 0.000 0.501 0.612 83.8 28.2 43 0.500 0.501 0.888 82.3 24.4 44 0.888 0.501 1.000 82.0 26.1 45 0.250 0.750 0.250 1932.5 349.0 46 0.750 0.750 0.250 1932.4 352.5 47 0.250 0.750 0.750 1932.4 352.5 48 0.750 0.750 0.750 1932.5 349.0 49 1.000 0.612 0.000 82.7 26.3 50 0.500 0.612 0.000 82.7 26.2 51 0.000 0.612 0.500 82.8 26.2 52 0.500 0.612 0.500 82.7 26.3 53 0.000 0.888 0.000 80.9 26.1 54 0.500 0.888 0.000 80.9 26.1 55 0.500 0.888 0.500 80.9 26.1 56 1.000 0.888 0.500 80.9 26.1 _platon_squeeze_details ; ; 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 0.852066(17) 0.852066(17) 0.352066(17) 0.0348(2) Uani 1 3 d S . . Cu2 Cu 0.890118(17) 0.914182(15) 0.329467(18) 0.03759(16) Uani 1 1 d . . . Cu3 Cu 0.953157(16) 0.945333(14) 0.268419(15) 0.03244(14) Uani 1 1 d . . . Cu4 Cu 1.0000 1.0000 0.2500 0.0269(2) Uani 1 4 d S . . Br1 Br 0.901421(13) 0.901421(13) 0.401421(13) 0.03234(17) Uani 1 3 d S . . S1 S 0.95733(3) 0.96823(3) 0.21101(3) 0.0261(2) Uani 1 1 d . . . S2 S 0.89827(3) 0.81563(3) 0.33026(3) 0.0322(2) Uani 1 1 d . . . S3 S 1.0000 1.2500 0.2500 0.0283(5) Uani 1 4 d S . . S4 S 1.0000 1.0000 0.5000 0.0722(17) Uani 1 12 d S . . S5 S 0.91484(9) 1.08516(9) 0.41484(9) 0.0569(17) Uani 0.582(8) 3 d SPDU A 1 O4 O 0.9390(3) 1.0610(3) 0.4390(3) 0.127(6) Uani 0.582(8) 3 d SPDU A 1 S5' S 0.89247(9) 1.10753(9) 0.39247(9) 0.0329(16) Uani 0.418(8) 3 d SPD A 2 O4' O 0.8683(3) 1.1317(3) 0.3683(3) 0.084(7) Uani 0.418(8) 3 d SPDU A 2 O1 O 1.02252(10) 1.23922(9) 0.28141(10) 0.0434(9) Uani 1 1 d . . . O2 O 0.97643(17) 0.97643(17) 0.47643(17) 0.117(4) Uani 1 3 d S . . O3 O 0.87522(14) 1.07202(15) 0.40920(15) 0.093(2) Uani 1 1 d . . . N1 N 1.02054(9) 0.93023(10) 0.19552(9) 0.0257(7) Uani 1 1 d . . . N2 N 1.03238(9) 0.90299(10) 0.17102(10) 0.0293(8) Uani 1 1 d . . . N3 N 0.97489(9) 0.91491(10) 0.16055(9) 0.0297(8) Uani 1 1 d . . . H3A H 0.9534 0.9141 0.1509 0.036 Uiso 1 1 calc R . . N4 N 1.00366(13) 0.86909(13) 0.12337(12) 0.0501(12) Uani 1 1 d . . . H4A H 1.0230 0.8564 0.1186 0.060 Uiso 1 1 calc R . . H4B H 0.9839 0.8655 0.1110 0.060 Uiso 1 1 calc R . . N5 N 0.92534(10) 0.88093(10) 0.30433(10) 0.0295(8) Uani 1 1 d . . . N6 N 0.95362(10) 0.89275(9) 0.28059(10) 0.0297(8) Uani 1 1 d . . . N7 N 0.95441(11) 0.83301(10) 0.28403(11) 0.0335(9) Uani 1 1 d . . . H7A H 0.9605 0.8105 0.2804 0.040 Uiso 1 1 calc R . . N8 N 0.99919(13) 0.86154(13) 0.24583(13) 0.0559(14) Uani 1 1 d . . . H8A H 1.0080 0.8816 0.2369 0.067 Uiso 1 1 calc R . . H8B H 1.0087 0.8408 0.2398 0.067 Uiso 1 1 calc R . . C1 C 0.98587(11) 0.93660(12) 0.18909(10) 0.0246(8) Uani 1 1 d . . . C2 C 1.00439(12) 0.89497(12) 0.15052(12) 0.0302(9) Uani 1 1 d . . . C3 C 0.92696(12) 0.84503(11) 0.30555(12) 0.0278(9) Uani 1 1 d . . . C4 C 0.97060(14) 0.86263(12) 0.26920(13) 0.0344(10) 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 0.0348(2) 0.0348(2) 0.0348(2) 0.0042(3) 0.0042(3) 0.0042(3) Cu2 0.0390(3) 0.0252(3) 0.0485(4) -0.0020(2) 0.0171(3) 0.0014(2) Cu3 0.0410(3) 0.0231(3) 0.0332(3) 0.0010(2) 0.0131(2) 0.0028(2) Cu4 0.0264(3) 0.0264(3) 0.0279(5) 0.000 0.000 0.000 Br1 0.03234(17) 0.03234(17) 0.03234(17) 0.00240(19) 0.00240(19) 0.00240(19) S1 0.0241(5) 0.0293(5) 0.0248(5) -0.0019(4) 0.0008(4) 0.0000(4) S2 0.0379(6) 0.0221(5) 0.0367(6) 0.0007(4) 0.0085(5) -0.0014(4) S3 0.0446(13) 0.0201(6) 0.0201(6) 0.000 0.000 0.000 S4 0.0722(17) 0.0722(17) 0.0722(17) 0.000 0.000 0.000 S5 0.0569(17) 0.0569(17) 0.0569(17) -0.0269(17) 0.0269(17) -0.0269(17) O4 0.127(6) 0.127(6) 0.127(6) -0.013(7) 0.013(7) -0.013(7) S5' 0.0329(16) 0.0329(16) 0.0329(16) -0.0108(13) 0.0108(13) -0.0108(13) O4' 0.084(7) 0.084(7) 0.084(7) -0.032(9) 0.032(9) -0.032(9) O1 0.063(2) 0.0280(18) 0.0393(19) 0.0001(14) -0.0143(18) 0.0084(16) O2 0.117(4) 0.117(4) 0.117(4) -0.022(4) -0.022(4) -0.022(4) O3 0.088(3) 0.090(4) 0.102(4) -0.059(3) 0.062(3) -0.065(3) N1 0.0226(18) 0.035(2) 0.0200(17) -0.0084(15) 0.0033(14) -0.0013(14) N2 0.0232(18) 0.037(2) 0.0279(18) -0.0067(15) 0.0028(15) -0.0013(15) N3 0.0207(18) 0.044(2) 0.0243(19) -0.0100(16) -0.0042(13) -0.0020(15) N4 0.035(2) 0.064(3) 0.051(3) -0.035(2) -0.012(2) 0.012(2) N5 0.035(2) 0.0237(19) 0.0296(19) 0.0010(15) 0.0122(16) 0.0032(15) N6 0.038(2) 0.0194(17) 0.0319(19) 0.0011(14) 0.0108(16) 0.0010(15) N7 0.043(2) 0.0176(17) 0.040(2) 0.0025(15) 0.0101(17) 0.0072(16) N8 0.064(3) 0.033(2) 0.071(3) 0.011(2) 0.044(3) 0.012(2) C1 0.022(2) 0.032(2) 0.019(2) 0.0012(16) 0.0001(15) -0.0057(17) C2 0.025(2) 0.036(2) 0.029(2) -0.0056(19) 0.0014(18) 0.0006(18) C3 0.038(2) 0.022(2) 0.024(2) -0.0016(17) 0.0021(19) 0.0031(18) C4 0.043(3) 0.026(2) 0.034(2) 0.0022(19) 0.009(2) 0.0033(19) _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 S2 2.2842(11) 53_554 ? Cu1 S2 2.2841(11) . ? Cu1 S2 2.2842(11) 33_554 ? Cu1 Cu2 2.7762(8) 53_554 ? Cu1 Cu2 2.7762(9) 33_554 ? Cu1 Cu2 2.7762(9) . ? Cu2 N5 1.986(4) . ? Cu2 N2 2.001(4) 87_465 ? Cu2 S2 2.3099(14) 53_554 ? Cu2 Br1 2.6916(8) . ? Cu3 N6 1.965(3) . ? Cu3 N1 1.990(3) 87_465 ? Cu3 S1 2.2548(12) . ? Cu3 Cu4 2.7049(6) . ? Cu4 S1 2.4010(10) 87_465 ? Cu4 S1 2.4010(10) . ? Cu4 S1 2.4010(10) 88_645 ? Cu4 S1 2.4010(11) 2_775 ? Cu4 Cu3 2.7049(6) 2_775 ? Cu4 Cu3 2.7049(6) 87_465 ? Cu4 Cu3 2.7049(6) 88_645 ? Br1 Cu2 2.6916(8) 53_554 ? Br1 Cu2 2.6916(8) 33_554 ? S1 C1 1.744(4) . ? S2 C3 1.745(5) . ? S2 Cu2 2.3099(14) 33_554 ? S3 O1 1.460(3) 90_656 ? S3 O1 1.460(3) . ? S3 O1 1.460(3) 67_663 ? S3 O1 1.460(3) 28_575 ? S4 O2 1.486(11) 4_576 ? S4 O2 1.486(11) 3_756 ? S4 O2 1.486(11) . ? S4 O2 1.486(11) 2_775 ? S5 O4 1.522(16) . ? S5 O3 1.533(5) 54_576 ? S5 O3 1.533(5) . ? S5 O3 1.533(5) 36_764 ? S5' O4' 1.521(17) . ? S5' O3 1.561(6) 54_576 ? S5' O3 1.561(6) . ? S5' O3 1.561(6) 36_764 ? N1 C1 1.304(5) . ? N1 N2 1.402(5) . ? N1 Cu3 1.990(3) 88_645 ? N2 C2 1.296(5) . ? N2 Cu2 2.001(4) 88_645 ? N3 C2 1.347(5) . ? N3 C1 1.364(5) . ? N4 C2 1.366(5) . ? N5 C3 1.309(5) . ? N5 N6 1.411(5) . ? N6 C4 1.325(6) . ? N7 C4 1.342(6) . ? N7 C3 1.343(6) . ? N8 C4 1.345(6) . ? 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 S2 Cu1 S2 118.791(15) 53_554 . ? S2 Cu1 S2 118.791(15) 53_554 33_554 ? S2 Cu1 S2 118.791(15) . 33_554 ? S2 Cu1 Cu2 90.15(3) 53_554 53_554 ? S2 Cu1 Cu2 142.26(5) . 53_554 ? S2 Cu1 Cu2 53.25(4) 33_554 53_554 ? S2 Cu1 Cu2 142.26(5) 53_554 33_554 ? S2 Cu1 Cu2 53.25(4) . 33_554 ? S2 Cu1 Cu2 90.15(3) 33_554 33_554 ? Cu2 Cu1 Cu2 89.02(3) 53_554 33_554 ? S2 Cu1 Cu2 53.25(4) 53_554 . ? S2 Cu1 Cu2 90.15(3) . . ? S2 Cu1 Cu2 142.26(5) 33_554 . ? Cu2 Cu1 Cu2 89.02(3) 53_554 . ? Cu2 Cu1 Cu2 89.02(3) 33_554 . ? N5 Cu2 N2 115.92(15) . 87_465 ? N5 Cu2 S2 110.83(12) . 53_554 ? N2 Cu2 S2 117.55(12) 87_465 53_554 ? N5 Cu2 Br1 104.14(11) . . ? N2 Cu2 Br1 98.09(11) 87_465 . ? S2 Cu2 Br1 108.24(4) 53_554 . ? N5 Cu2 Cu1 87.83(10) . . ? N2 Cu2 Cu1 155.67(10) 87_465 . ? S2 Cu2 Cu1 52.40(3) 53_554 . ? Br1 Cu2 Cu1 69.35(3) . . ? N6 Cu3 N1 117.57(14) . 87_465 ? N6 Cu3 S1 124.64(11) . . ? N1 Cu3 S1 114.12(10) 87_465 . ? N6 Cu3 Cu4 140.10(11) . . ? N1 Cu3 Cu4 88.20(10) 87_465 . ? S1 Cu3 Cu4 57.04(3) . . ? S1 Cu4 S1 110.45(3) 87_465 . ? S1 Cu4 S1 107.53(5) 87_465 88_645 ? S1 Cu4 S1 110.45(3) . 88_645 ? S1 Cu4 S1 110.45(3) 87_465 2_775 ? S1 Cu4 S1 107.53(5) . 2_775 ? S1 Cu4 S1 110.45(3) 88_645 2_775 ? S1 Cu4 Cu3 71.41(3) 87_465 2_775 ? S1 Cu4 Cu3 155.33(3) . 2_775 ? S1 Cu4 Cu3 91.48(3) 88_645 2_775 ? S1 Cu4 Cu3 52.00(3) 2_775 2_775 ? S1 Cu4 Cu3 91.48(3) 87_465 . ? S1 Cu4 Cu3 52.00(3) . . ? S1 Cu4 Cu3 71.41(3) 88_645 . ? S1 Cu4 Cu3 155.33(3) 2_775 . ? Cu3 Cu4 Cu3 151.30(2) 2_775 . ? S1 Cu4 Cu3 52.00(3) 87_465 87_465 ? S1 Cu4 Cu3 71.41(3) . 87_465 ? S1 Cu4 Cu3 155.33(3) 88_645 87_465 ? S1 Cu4 Cu3 91.48(3) 2_775 87_465 ? Cu3 Cu4 Cu3 93.522(6) 2_775 87_465 ? Cu3 Cu4 Cu3 93.522(6) . 87_465 ? S1 Cu4 Cu3 155.33(3) 87_465 88_645 ? S1 Cu4 Cu3 91.48(3) . 88_645 ? S1 Cu4 Cu3 52.00(3) 88_645 88_645 ? S1 Cu4 Cu3 71.41(3) 2_775 88_645 ? Cu3 Cu4 Cu3 93.522(6) 2_775 88_645 ? Cu3 Cu4 Cu3 93.522(6) . 88_645 ? Cu3 Cu4 Cu3 151.30(2) 87_465 88_645 ? Cu2 Br1 Cu2 92.61(3) 53_554 . ? Cu2 Br1 Cu2 92.61(3) 53_554 33_554 ? Cu2 Br1 Cu2 92.61(3) . 33_554 ? C1 S1 Cu3 102.72(14) . . ? C1 S1 Cu4 101.71(14) . . ? Cu3 S1 Cu4 70.96(3) . . ? C3 S2 Cu1 105.29(14) . . ? C3 S2 Cu2 101.68(15) . 33_554 ? Cu1 S2 Cu2 74.35(4) . 33_554 ? O1 S3 O1 108.37(16) 90_656 . ? O1 S3 O1 111.7(3) 90_656 67_663 ? O1 S3 O1 108.37(16) . 67_663 ? O1 S3 O1 108.37(16) 90_656 28_575 ? O1 S3 O1 111.7(3) . 28_575 ? O1 S3 O1 108.37(16) 67_663 28_575 ? O2 S4 O2 109.471(2) 4_576 3_756 ? O2 S4 O2 109.471(2) 4_576 . ? O2 S4 O2 109.471(3) 3_756 . ? O2 S4 O2 109.471(5) 4_576 2_775 ? O2 S4 O2 109.471(6) 3_756 2_775 ? O2 S4 O2 109.471(3) . 2_775 ? O4 S5 O3 116.1(3) . 54_576 ? O4 S5 O3 116.1(3) . . ? O3 S5 O3 102.1(4) 54_576 . ? O4 S5 O3 116.1(3) . 36_764 ? O3 S5 O3 102.1(4) 54_576 36_764 ? O3 S5 O3 102.1(4) . 36_764 ? O4' S5' O3 118.1(3) . 54_576 ? O4' S5' O3 118.1(3) . . ? O3 S5' O3 99.6(4) 54_576 . ? O4' S5' O3 118.1(3) . 36_764 ? O3 S5' O3 99.6(4) 54_576 36_764 ? O3 S5' O3 99.6(4) . 36_764 ? S5 O3 S5' 54.2(3) . . ? C1 N1 N2 108.0(3) . . ? C1 N1 Cu3 130.4(3) . 88_645 ? N2 N1 Cu3 121.6(3) . 88_645 ? C2 N2 N1 106.5(3) . . ? C2 N2 Cu2 134.9(3) . 88_645 ? N1 N2 Cu2 118.1(3) . 88_645 ? C2 N3 C1 106.6(3) . . ? C3 N5 N6 107.0(3) . . ? C3 N5 Cu2 128.5(3) . . ? N6 N5 Cu2 124.5(3) . . ? C4 N6 N5 106.2(3) . . ? C4 N6 Cu3 137.7(3) . . ? N5 N6 Cu3 115.4(3) . . ? C4 N7 C3 107.5(4) . . ? N1 C1 N3 108.5(4) . . ? N1 C1 S1 127.7(3) . . ? N3 C1 S1 123.8(3) . . ? N2 C2 N3 110.4(4) . . ? N2 C2 N4 126.0(4) . . ? N3 C2 N4 123.5(4) . . ? N5 C3 N7 109.8(4) . . ? N5 C3 S2 127.1(3) . . ? N7 C3 S2 123.1(3) . . ? N6 C4 N7 109.5(4) . . ? N6 C4 N8 125.7(4) . . ? N7 C4 N8 124.8(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.468 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.083 #========================================= data_3 _database_code_depnum_ccdc_archive 'CCDC 731920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H72 Cu31 I4 N96 O32 S32' _chemical_formula_weight 6009.28 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' I I -0.4742 1.8119 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 36.6289(11) _cell_length_b 36.6289(11) _cell_length_c 36.6289(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 49144(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7202 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.28 _exptl_crystal_description cubic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 23288 _exptl_absorpt_coefficient_mu 3.452 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5040 _exptl_absorpt_correction_T_max 0.6081 _exptl_absorpt_process_details 'SADABS, sheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86447 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4039 _reflns_number_gt 3906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0564P)^2^+142.2017P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.486(16) _refine_ls_number_reflns 4039 _refine_ls_number_parameters 190 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.111 0.000 0.000 87.4 31.2 2 0.389 0.000 0.000 85.5 31.3 3 0.611 0.000 0.000 87.4 31.6 4 0.889 0.000 0.000 85.6 31.0 5 0.000 0.000 0.112 85.0 32.5 6 0.500 0.000 0.112 84.9 32.8 7 0.000 0.000 0.389 85.8 29.7 8 0.500 0.000 0.389 85.8 29.4 9 0.111 0.000 0.501 86.2 31.6 10 0.889 0.000 0.501 84.3 31.3 11 0.389 0.000 0.501 84.4 30.9 12 0.611 0.000 0.501 86.0 31.1 13 0.000 0.000 0.612 84.8 32.8 14 0.500 0.000 0.612 85.0 32.5 15 0.000 0.000 0.888 83.3 29.3 16 0.500 0.000 0.888 83.4 29.8 17 0.250 0.250 0.250 1994.0 344.1 18 0.750 0.250 0.250 1994.4 344.0 19 0.250 0.250 0.750 1994.4 344.0 20 0.750 0.250 0.750 1994.0 344.1 21 0.500 0.113 0.000 82.6 31.4 22 1.000 0.113 0.000 82.6 31.1 23 0.500 0.113 0.500 82.6 31.1 24 0.000 0.113 0.500 82.6 31.4 25 0.000 0.389 0.000 85.7 31.3 26 0.500 0.389 0.000 85.7 31.0 27 1.000 0.389 0.500 85.7 31.0 28 0.500 0.389 0.500 85.7 31.3 29 0.611 0.501 0.000 86.2 31.2 30 0.000 0.501 0.111 86.1 32.9 31 0.500 0.501 0.389 84.6 29.7 32 0.889 0.501 0.500 84.4 31.0 33 0.111 0.501 0.500 86.2 31.2 34 0.500 0.501 0.611 86.1 32.9 35 1.000 0.501 0.889 84.6 29.7 36 0.389 0.501 1.000 84.4 31.0 37 0.113 0.501 0.000 83.7 31.5 38 0.500 0.501 0.113 83.6 32.5 39 1.000 0.501 0.387 82.1 29.3 40 0.387 0.501 0.500 81.8 31.4 41 0.613 0.501 0.500 83.7 31.5 42 0.000 0.501 0.613 83.6 32.5 43 0.500 0.501 0.887 82.1 29.3 44 0.887 0.501 1.000 81.8 31.4 45 0.250 0.750 0.250 1994.4 344.0 46 0.750 0.750 0.250 1994.0 344.1 47 0.250 0.750 0.750 1994.0 344.1 48 0.750 0.750 0.750 1994.4 344.0 49 1.000 0.613 0.000 82.6 31.4 50 0.500 0.613 0.000 82.6 31.1 51 0.000 0.613 0.500 82.6 31.1 52 0.500 0.613 0.500 82.6 31.4 53 0.000 0.887 0.000 80.8 31.0 54 0.500 0.887 0.000 80.8 31.4 55 0.500 0.887 0.500 80.8 31.0 56 1.000 0.887 0.500 80.8 31.4 _platon_squeeze_details ; ; 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 0.854189(18) 0.854189(18) 0.354189(18) 0.0393(2) Uani 1 3 d S . . Cu2 Cu 0.890824(17) 0.915142(15) 0.329433(17) 0.04018(15) Uani 1 1 d . . . Cu3 Cu 0.953174(16) 0.945451(14) 0.268424(16) 0.03605(14) Uani 1 1 d . . . Cu4 Cu 1.0000 1.0000 0.2500 0.0294(2) Uani 1 4 d S . . I1 I 0.903507(8) 0.903507(8) 0.403507(8) 0.03377(12) Uani 1 3 d S . . S1 S 0.95732(3) 0.96856(3) 0.21126(3) 0.0281(2) Uani 1 1 d . . . S2 S 0.89885(3) 0.81692(3) 0.33097(3) 0.0371(2) Uani 1 1 d . . . S3 S 1.0000 1.2500 0.2500 0.0332(5) Uani 1 4 d S . . S4 S 1.0000 1.0000 0.5000 0.0649(14) Uani 1 12 d S . . S5 S 0.91442(11) 1.08558(11) 0.41442(11) 0.0673(17) Uani 0.627(7) 3 d SPDU A 1 O4 O 0.9377(3) 1.0623(3) 0.4377(3) 0.165(11) Uani 0.627(7) 3 d SPD A 1 S5' S 0.89590(11) 1.10410(11) 0.39590(11) 0.0356(16) Uani 0.372(7) 3 d SPDU A 2 O4' O 0.8723(2) 1.1277(2) 0.3723(2) 0.061(5) Uani 0.372(7) 3 d SPDU A 2 O1 O 1.02292(11) 1.23841(10) 0.28112(10) 0.0497(9) Uani 1 1 d . . . O2 O 0.97644(14) 0.97644(14) 0.47644(14) 0.097(3) Uani 1 3 d S . . O3 O 0.87599(15) 1.07153(15) 0.41008(16) 0.095(2) Uani 1 1 d . . . N1 N 1.01997(9) 0.93046(10) 0.19639(9) 0.0300(7) Uani 1 1 d . . . N2 N 1.03156(10) 0.90285(10) 0.17220(9) 0.0324(7) Uani 1 1 d . . . N3 N 0.97385(10) 0.91510(11) 0.16213(9) 0.0337(8) Uani 1 1 d . . . H3A H 0.9522 0.9140 0.1531 0.040 Uiso 1 1 calc R . . N4 N 1.00242(13) 0.86874(13) 0.12535(12) 0.0538(12) Uani 1 1 d . . . H4A H 1.0214 0.8556 0.1209 0.065 Uiso 1 1 calc R . . H4B H 0.9827 0.8654 0.1131 0.065 Uiso 1 1 calc R . . N5 N 0.92559(10) 0.88157(9) 0.30408(10) 0.0322(8) Uani 1 1 d . . . N6 N 0.95339(10) 0.89261(10) 0.28040(10) 0.0337(8) Uani 1 1 d . . . N7 N 0.95413(10) 0.83340(10) 0.28426(10) 0.0346(8) Uani 1 1 d . . . H7A H 0.9602 0.8110 0.2807 0.042 Uiso 1 1 calc R . . N8 N 0.99779(14) 0.86117(12) 0.24514(13) 0.0583(14) Uani 1 1 d . . . H8A H 1.0064 0.8808 0.2356 0.070 Uiso 1 1 calc R . . H8B H 1.0069 0.8403 0.2394 0.070 Uiso 1 1 calc R . . C1 C 0.98572(11) 0.93712(12) 0.18958(10) 0.0279(8) Uani 1 1 d . . . C2 C 1.00372(12) 0.89514(13) 0.15207(11) 0.0355(9) Uani 1 1 d . . . C3 C 0.92690(12) 0.84560(11) 0.30605(11) 0.0312(8) Uani 1 1 d . . . C4 C 0.96991(12) 0.86309(12) 0.26916(12) 0.0343(9) 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 0.0393(2) 0.0393(2) 0.0393(2) 0.0067(3) 0.0067(3) 0.0067(3) Cu2 0.0455(3) 0.0276(3) 0.0474(3) 0.0002(2) 0.0183(3) 0.0029(2) Cu3 0.0464(3) 0.0268(3) 0.0350(3) 0.0005(2) 0.0138(2) 0.0032(2) Cu4 0.0294(3) 0.0294(3) 0.0296(5) 0.000 0.000 0.000 I1 0.03377(12) 0.03377(12) 0.03377(12) 0.00193(11) 0.00193(11) 0.00193(11) S1 0.0272(5) 0.0302(5) 0.0268(5) -0.0001(4) 0.0019(4) 0.0005(4) S2 0.0435(6) 0.0261(5) 0.0417(6) 0.0019(4) 0.0126(5) -0.0012(4) S3 0.0493(13) 0.0252(6) 0.0252(6) 0.000 0.000 0.000 S4 0.0649(14) 0.0649(14) 0.0649(14) 0.000 0.000 0.000 S5 0.0673(17) 0.0673(17) 0.0673(17) -0.0287(18) 0.0287(18) -0.0287(18) O4 0.165(11) 0.165(11) 0.165(11) 0.033(9) -0.033(9) 0.033(9) S5' 0.0356(16) 0.0356(16) 0.0356(16) -0.0154(15) 0.0154(15) -0.0154(15) O4' 0.061(5) 0.061(5) 0.061(5) 0.005(5) -0.005(5) 0.005(5) O1 0.064(2) 0.0391(19) 0.046(2) -0.0046(15) -0.0145(18) 0.0082(17) O2 0.097(3) 0.097(3) 0.097(3) -0.023(3) -0.023(3) -0.023(3) O3 0.099(4) 0.089(4) 0.096(4) -0.055(3) 0.062(3) -0.062(3) N1 0.0237(16) 0.0385(19) 0.0277(17) -0.0062(15) 0.0023(13) -0.0028(14) N2 0.0297(17) 0.041(2) 0.0264(16) -0.0072(15) -0.0007(14) -0.0020(15) N3 0.0275(17) 0.048(2) 0.0252(17) -0.0062(15) -0.0070(13) 0.0020(16) N4 0.037(2) 0.070(3) 0.054(3) -0.040(2) -0.008(2) 0.004(2) N5 0.038(2) 0.0260(17) 0.0326(18) 0.0011(14) 0.0117(15) 0.0006(15) N6 0.040(2) 0.0261(17) 0.0351(19) 0.0014(14) 0.0123(15) 0.0028(15) N7 0.040(2) 0.0232(17) 0.040(2) -0.0005(15) 0.0096(16) 0.0068(15) N8 0.066(3) 0.031(2) 0.078(3) 0.005(2) 0.043(3) 0.011(2) C1 0.028(2) 0.035(2) 0.0206(18) 0.0005(16) 0.0040(15) -0.0054(17) C2 0.032(2) 0.044(2) 0.030(2) -0.0091(19) 0.0024(17) -0.0031(18) C3 0.039(2) 0.0248(19) 0.030(2) -0.0002(17) -0.0005(18) 0.0034(17) C4 0.038(2) 0.031(2) 0.034(2) 0.0009(18) 0.0026(19) 0.0038(18) _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 S2 2.2942(11) 53_554 ? Cu1 S2 2.2942(11) . ? Cu1 S2 2.2942(11) 33_554 ? Cu1 Cu2 2.7582(8) 53_554 ? Cu1 Cu2 2.7582(8) . ? Cu1 Cu2 2.7582(8) 33_554 ? Cu2 N5 1.999(4) . ? Cu2 N2 2.002(4) 87_465 ? Cu2 S2 2.3178(14) 53_554 ? Cu2 I1 2.7855(7) . ? Cu3 N6 1.985(4) . ? Cu3 N1 1.989(3) 87_465 ? Cu3 S1 2.2635(12) . ? Cu3 Cu4 2.7184(6) . ? Cu4 S1 2.4050(10) 87_465 ? Cu4 S1 2.4050(11) . ? Cu4 S1 2.4050(11) 2_775 ? Cu4 S1 2.4050(11) 88_645 ? Cu4 Cu3 2.7184(6) 2_775 ? Cu4 Cu3 2.7184(6) 87_465 ? Cu4 Cu3 2.7184(6) 88_645 ? I1 Cu2 2.7855(7) 53_554 ? I1 Cu2 2.7855(7) 33_554 ? S1 C1 1.743(4) . ? S2 C3 1.730(5) . ? S2 Cu2 2.3178(14) 33_554 ? S3 O1 1.478(3) 90_656 ? S3 O1 1.478(3) 67_663 ? S3 O1 1.478(3) . ? S3 O1 1.478(3) 28_575 ? S4 O2 1.494(9) 4_576 ? S4 O2 1.495(9) . ? S4 O2 1.494(9) 3_756 ? S4 O2 1.494(9) 2_775 ? S5 O4 1.475(16) . ? S5 O3 1.507(6) 54_576 ? S5 O3 1.507(6) . ? S5 O3 1.507(6) 36_764 ? S5' O3 1.491(5) 54_576 ? S5' O3 1.491(5) 36_764 ? S5' O3 1.491(5) . ? S5' O4' 1.496(15) . ? N1 C1 1.302(5) . ? N1 N2 1.410(5) . ? N1 Cu3 1.989(3) 88_645 ? N2 C2 1.290(6) . ? N2 Cu2 2.002(4) 88_645 ? N3 C1 1.360(5) . ? N3 C2 1.367(6) . ? N4 C2 1.377(5) . ? N5 C3 1.320(5) . ? N5 N6 1.397(5) . ? N6 C4 1.306(6) . ? N7 C4 1.350(6) . ? N7 C3 1.353(6) . ? N8 C4 1.349(6) . ? 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 S2 Cu1 S2 117.91(2) 53_554 . ? S2 Cu1 S2 117.91(2) 53_554 33_554 ? S2 Cu1 S2 117.91(2) . 33_554 ? S2 Cu1 Cu2 90.74(3) 53_554 53_554 ? S2 Cu1 Cu2 145.48(5) . 53_554 ? S2 Cu1 Cu2 53.66(4) 33_554 53_554 ? S2 Cu1 Cu2 53.66(4) 53_554 . ? S2 Cu1 Cu2 90.74(3) . . ? S2 Cu1 Cu2 145.48(5) 33_554 . ? Cu2 Cu1 Cu2 91.85(3) 53_554 . ? S2 Cu1 Cu2 145.48(5) 53_554 33_554 ? S2 Cu1 Cu2 53.66(4) . 33_554 ? S2 Cu1 Cu2 90.74(3) 33_554 33_554 ? Cu2 Cu1 Cu2 91.85(3) 53_554 33_554 ? Cu2 Cu1 Cu2 91.85(3) . 33_554 ? N5 Cu2 N2 116.47(14) . 87_465 ? N5 Cu2 S2 110.62(11) . 53_554 ? N2 Cu2 S2 116.95(12) 87_465 53_554 ? N5 Cu2 Cu1 87.97(10) . . ? N2 Cu2 Cu1 154.98(10) 87_465 . ? S2 Cu2 Cu1 52.88(3) 53_554 . ? N5 Cu2 I1 104.60(11) . . ? N2 Cu2 I1 98.14(10) 87_465 . ? S2 Cu2 I1 108.12(3) 53_554 . ? Cu1 Cu2 I1 68.72(3) . . ? N6 Cu3 N1 118.64(14) . 87_465 ? N6 Cu3 S1 124.68(11) . . ? N1 Cu3 S1 112.91(10) 87_465 . ? N6 Cu3 Cu4 140.29(11) . . ? N1 Cu3 Cu4 87.52(10) 87_465 . ? S1 Cu3 Cu4 56.85(3) . . ? S1 Cu4 S1 110.37(2) 87_465 . ? S1 Cu4 S1 110.37(2) 87_465 2_775 ? S1 Cu4 S1 107.69(5) . 2_775 ? S1 Cu4 S1 107.69(5) 87_465 88_645 ? S1 Cu4 S1 110.37(2) . 88_645 ? S1 Cu4 S1 110.37(2) 2_775 88_645 ? S1 Cu4 Cu3 71.21(3) 87_465 2_775 ? S1 Cu4 Cu3 155.31(3) . 2_775 ? S1 Cu4 Cu3 52.00(3) 2_775 2_775 ? S1 Cu4 Cu3 91.67(3) 88_645 2_775 ? S1 Cu4 Cu3 52.00(3) 87_465 87_465 ? S1 Cu4 Cu3 71.21(3) . 87_465 ? S1 Cu4 Cu3 91.67(3) 2_775 87_465 ? S1 Cu4 Cu3 155.31(3) 88_645 87_465 ? Cu3 Cu4 Cu3 93.533(6) 2_775 87_465 ? S1 Cu4 Cu3 91.67(3) 87_465 . ? S1 Cu4 Cu3 52.00(3) . . ? S1 Cu4 Cu3 155.31(3) 2_775 . ? S1 Cu4 Cu3 71.21(3) 88_645 . ? Cu3 Cu4 Cu3 151.25(2) 2_775 . ? Cu3 Cu4 Cu3 93.533(6) 87_465 . ? S1 Cu4 Cu3 155.31(3) 87_465 88_645 ? S1 Cu4 Cu3 91.67(3) . 88_645 ? S1 Cu4 Cu3 71.21(3) 2_775 88_645 ? S1 Cu4 Cu3 52.00(3) 88_645 88_645 ? Cu3 Cu4 Cu3 93.533(6) 2_775 88_645 ? Cu3 Cu4 Cu3 151.25(2) 87_465 88_645 ? Cu3 Cu4 Cu3 93.533(6) . 88_645 ? Cu2 I1 Cu2 90.69(2) . 53_554 ? Cu2 I1 Cu2 90.69(2) . 33_554 ? Cu2 I1 Cu2 90.69(2) 53_554 33_554 ? C1 S1 Cu3 102.38(14) . . ? C1 S1 Cu4 101.38(14) . . ? Cu3 S1 Cu4 71.15(3) . . ? C3 S2 Cu1 104.93(15) . . ? C3 S2 Cu2 103.07(14) . 33_554 ? Cu1 S2 Cu2 73.46(4) . 33_554 ? O1 S3 O1 110.8(3) 90_656 67_663 ? O1 S3 O1 108.83(17) 90_656 . ? O1 S3 O1 108.83(17) 67_663 . ? O1 S3 O1 108.83(17) 90_656 28_575 ? O1 S3 O1 108.83(17) 67_663 28_575 ? O1 S3 O1 110.8(3) . 28_575 ? O2 S4 O2 109.5 4_576 . ? O2 S4 O2 109.471(3) 4_576 3_756 ? O2 S4 O2 109.5 . 3_756 ? O2 S4 O2 109.471(4) 4_576 2_775 ? O2 S4 O2 109.471(2) . 2_775 ? O2 S4 O2 109.471(5) 3_756 2_775 ? O4 S5 O3 113.8(4) . 54_576 ? O4 S5 O3 113.8(4) . . ? O3 S5 O3 104.9(4) 54_576 . ? O4 S5 O3 113.8(4) . 36_764 ? O3 S5 O3 104.9(4) 54_576 36_764 ? O3 S5 O3 104.9(4) . 36_764 ? O3 S5' O3 106.4(4) 54_576 36_764 ? O3 S5' O3 106.4(4) 54_576 . ? O3 S5' O3 106.4(4) 36_764 . ? O3 S5' O4' 112.4(4) 54_576 . ? O3 S5' O4' 112.4(4) 36_764 . ? O3 S5' O4' 112.4(4) . . ? S5' O3 S5 46.1(3) . . ? C1 N1 N2 107.7(3) . . ? C1 N1 Cu3 131.2(3) . 88_645 ? N2 N1 Cu3 121.0(3) . 88_645 ? C2 N2 N1 106.2(3) . . ? C2 N2 Cu2 134.9(3) . 88_645 ? N1 N2 Cu2 118.0(2) . 88_645 ? C1 N3 C2 105.1(3) . . ? C3 N5 N6 107.2(3) . . ? C3 N5 Cu2 127.7(3) . . ? N6 N5 Cu2 125.1(3) . . ? C4 N6 N5 107.1(4) . . ? C4 N6 Cu3 137.7(3) . . ? N5 N6 Cu3 114.6(3) . . ? C4 N7 C3 106.9(4) . . ? N1 C1 N3 109.8(4) . . ? N1 C1 S1 127.7(3) . . ? N3 C1 S1 122.5(3) . . ? N2 C2 N3 111.2(4) . . ? N2 C2 N4 126.0(4) . . ? N3 C2 N4 122.7(4) . . ? N5 C3 N7 108.9(4) . . ? N5 C3 S2 127.8(3) . . ? N7 C3 S2 123.3(3) . . ? N6 C4 N8 126.8(4) . . ? N6 C4 N7 109.8(4) . . ? N8 C4 N7 123.3(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.690 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.089 #=========================================