# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email xiaojun_zhao15@yahoo.com.cn _publ_contact_author_name 'Xiao-Jun Zhao' loop_ _publ_author_name 'Xi Chen' 'Hong-Xi Li' 'Zhi-Yuan Zhang' 'Cheng Xu' 'Kai-Peng Hou' 'Li-Kuan Zhou' 'Jian-Ping Lang' 'Zhenrong Sun' data_100124b _database_code_depnum_ccdc_archive 'CCDC 860033' #TrackingRef '100124B.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H8 Cu2 N4 O7' _chemical_formula_weight 435.29 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' 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6447(17) _cell_length_b 7.2706(9) _cell_length_c 15.5079(14) _cell_angle_alpha 90.00 _cell_angle_beta 122.524(7) _cell_angle_gamma 90.00 _cell_volume 1297.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3442 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 27.81 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 3.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5279 _exptl_absorpt_correction_T_max 0.5856 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5913 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2290 _reflns_number_gt 1958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1260P)^2^+1.6931P] 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_number_reflns 2290 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1569 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.50528(5) 0.90294(9) 0.41201(5) 0.0217(3) Uani 1 1 d . . . Cu2 Cu 0.74219(6) 1.05881(10) 0.59070(5) 0.0244(3) Uani 1 1 d . . . O1 O 1.0915(4) 0.5388(8) 0.8319(3) 0.0416(12) Uani 1 1 d . . . O2 O 1.0818(4) 0.3150(7) 0.9243(4) 0.0455(12) Uani 1 1 d . . . O3 O 0.6053(5) 0.4978(6) 0.4799(3) 0.0431(12) Uani 1 1 d . . . O4 O 0.6421(3) 0.7872(5) 0.5307(3) 0.0297(9) Uani 1 1 d . . . O5 O 0.5871(4) 0.5588(6) 0.8421(3) 0.0332(10) Uani 1 1 d . . . O6 O 0.7397(4) 0.3977(6) 0.9633(3) 0.0303(9) Uani 1 1 d . . . O7 O 0.5829(3) 1.1410(5) 0.5258(3) 0.0221(8) Uani 1 1 d . . . H7 H 0.5686 1.2620 0.4933 0.027 Uiso 1 1 calc R . . N1 N 0.2536(4) 0.9602(7) 0.2795(4) 0.0270(10) Uani 1 1 d . . . N2 N 0.3551(4) 0.9606(7) 0.2806(4) 0.0276(10) Uani 1 1 d . . . N3 N 0.2119(5) 0.9786(7) 0.1249(4) 0.0315(11) Uani 1 1 d . . . N4 N 0.1405(5) 0.9688(9) 0.0157(4) 0.0455(15) Uani 1 1 d . . . H4' H 0.1256 1.0880 -0.0025 0.055 Uiso 1 1 d R . . H4" H 0.1932 0.9198 0.0043 0.055 Uiso 1 1 d R . . C1 C 0.3271(5) 0.9755(9) 0.1863(4) 0.0297(13) Uani 1 1 d . . . H1 H 0.3793 0.9827 0.1653 0.036 Uiso 1 1 calc R . . C2 C 0.1684(5) 0.9710(9) 0.1852(5) 0.0329(13) Uani 1 1 d . . . H2 H 0.0899 0.9733 0.1624 0.039 Uiso 1 1 calc R . . C3 C 0.9096(5) 0.4763(8) 0.8075(4) 0.0265(12) Uani 1 1 d . . . C4 C 0.8432(5) 0.5297(8) 0.7063(4) 0.0270(12) Uani 1 1 d . . . H4 H 0.8780 0.5464 0.6693 0.032 Uiso 1 1 calc R . . C5 C 0.7267(5) 0.5581(7) 0.6605(4) 0.0228(11) Uani 1 1 d . . . C6 C 0.6736(5) 0.5440(8) 0.7157(4) 0.0274(12) Uani 1 1 d . . . H6 H 0.5949 0.5702 0.6848 0.033 Uiso 1 1 calc R . . C7 C 0.7391(5) 0.4908(8) 0.8168(4) 0.0236(11) Uani 1 1 d . . . C8 C 0.8571(5) 0.4537(8) 0.8639(4) 0.0261(12) Uani 1 1 d . . . H8 H 0.9006 0.4146 0.9316 0.031 Uiso 1 1 calc R . . C9 C 1.0378(5) 0.4347(9) 0.8599(5) 0.0309(13) Uani 1 1 d . . . C10 C 0.6523(5) 0.6146(8) 0.5476(4) 0.0245(12) Uani 1 1 d . . . C11 C 0.6846(5) 0.4814(8) 0.8798(4) 0.0222(11) 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 0.0180(4) 0.0317(4) 0.0164(4) 0.0004(2) 0.0099(3) -0.0003(2) Cu2 0.0170(4) 0.0406(5) 0.0167(4) -0.0033(3) 0.0097(3) -0.0015(3) O1 0.016(2) 0.086(4) 0.023(2) 0.010(2) 0.0107(19) 0.000(2) O2 0.034(2) 0.054(3) 0.047(3) 0.014(2) 0.020(2) 0.011(2) O3 0.067(3) 0.028(2) 0.022(2) -0.0013(18) 0.016(2) -0.004(2) O4 0.028(2) 0.027(2) 0.023(2) 0.0010(15) 0.0066(18) -0.0009(16) O5 0.023(2) 0.059(3) 0.020(2) 0.0042(18) 0.0122(18) 0.0045(19) O6 0.029(2) 0.045(2) 0.021(2) 0.0013(17) 0.0170(19) 0.0016(18) O7 0.0209(18) 0.027(2) 0.0219(19) 0.0007(15) 0.0139(16) 0.0015(15) N1 0.020(2) 0.045(3) 0.018(2) -0.003(2) 0.011(2) 0.000(2) N2 0.024(2) 0.040(3) 0.021(3) -0.003(2) 0.014(2) -0.002(2) N3 0.029(3) 0.045(3) 0.016(2) 0.005(2) 0.010(2) 0.006(2) N4 0.041(3) 0.062(4) 0.022(3) 0.001(3) 0.010(3) 0.011(3) C1 0.028(3) 0.042(3) 0.021(3) 0.003(2) 0.015(3) 0.002(3) C2 0.022(3) 0.050(4) 0.024(3) 0.002(3) 0.010(3) 0.008(3) C3 0.024(3) 0.038(3) 0.022(3) 0.000(2) 0.015(3) -0.001(2) C4 0.025(3) 0.036(3) 0.023(3) 0.000(2) 0.016(3) -0.002(2) C5 0.024(3) 0.027(3) 0.017(3) 0.001(2) 0.011(2) 0.000(2) C6 0.020(3) 0.041(3) 0.020(3) 0.002(2) 0.009(2) 0.006(2) C7 0.025(3) 0.028(3) 0.019(3) -0.002(2) 0.013(2) -0.003(2) C8 0.024(3) 0.036(3) 0.020(3) -0.003(2) 0.013(3) 0.000(2) C9 0.024(3) 0.049(4) 0.019(3) -0.001(3) 0.011(3) 0.004(3) C10 0.023(3) 0.034(3) 0.019(3) 0.005(2) 0.013(2) 0.004(2) C11 0.018(3) 0.032(3) 0.018(3) -0.005(2) 0.011(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O7 1.930(3) 3_676 ? Cu1 O5 1.949(4) 4_575 ? Cu1 O4 1.971(4) . ? Cu1 N2 2.009(5) . ? Cu1 O7 2.285(4) . ? Cu2 O1 1.919(4) 2_756 ? Cu2 O7 1.935(4) . ? Cu2 O6 1.983(4) 4_575 ? Cu2 N1 1.987(5) 3_676 ? Cu2 O4 2.294(4) . ? O1 C9 1.280(8) . ? O1 Cu2 1.919(4) 2_746 ? O2 C9 1.214(8) . ? O3 C10 1.229(7) . ? O4 C10 1.274(7) . ? O5 C11 1.261(7) . ? O5 Cu1 1.949(4) 4_576 ? O6 C11 1.251(7) . ? O6 Cu2 1.983(4) 4_576 ? O7 Cu1 1.930(3) 3_676 ? O7 H7 0.9800 . ? N1 C2 1.292(8) . ? N1 N2 1.376(7) . ? N1 Cu2 1.987(5) 3_676 ? N2 C1 1.303(8) . ? N3 C1 1.329(8) . ? N3 C2 1.352(8) . ? N3 N4 1.431(7) . ? N4 H4' 0.9003 . ? N4 H4" 0.9009 . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.380(8) . ? C3 C8 1.407(8) . ? C3 C9 1.511(8) . ? C4 C5 1.363(8) . ? C4 H4 0.9300 . ? C5 C6 1.391(8) . ? C5 C10 1.534(7) . ? C6 C7 1.379(8) . ? C6 H6 0.9300 . ? C7 C8 1.391(8) . ? C7 C11 1.514(7) . ? C8 H8 0.9300 . ? 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 O7 Cu1 O5 176.77(16) 3_676 4_575 ? O7 Cu1 O4 89.69(16) 3_676 . ? O5 Cu1 O4 92.41(18) 4_575 . ? O7 Cu1 N2 88.36(17) 3_676 . ? O5 Cu1 N2 89.04(18) 4_575 . ? O4 Cu1 N2 166.77(19) . . ? O7 Cu1 O7 83.91(15) 3_676 . ? O5 Cu1 O7 98.93(16) 4_575 . ? O4 Cu1 O7 77.83(15) . . ? N2 Cu1 O7 114.93(18) . . ? O1 Cu2 O7 165.7(2) 2_756 . ? O1 Cu2 O6 90.91(18) 2_756 4_575 ? O7 Cu2 O6 91.16(16) . 4_575 ? O1 Cu2 N1 88.90(19) 2_756 3_676 ? O7 Cu2 N1 87.76(17) . 3_676 ? O6 Cu2 N1 174.8(2) 4_575 3_676 ? O1 Cu2 O4 115.7(2) 2_756 . ? O7 Cu2 O4 78.31(15) . . ? O6 Cu2 O4 92.61(16) 4_575 . ? N1 Cu2 O4 92.16(18) 3_676 . ? C9 O1 Cu2 122.2(4) . 2_746 ? C10 O4 Cu1 123.8(4) . . ? C10 O4 Cu2 142.1(4) . . ? Cu1 O4 Cu2 94.01(16) . . ? C11 O5 Cu1 125.6(4) . 4_576 ? C11 O6 Cu2 129.2(4) . 4_576 ? Cu1 O7 Cu2 121.12(19) 3_676 . ? Cu1 O7 Cu1 96.09(15) 3_676 . ? Cu2 O7 Cu1 95.28(15) . . ? Cu1 O7 H7 113.7 3_676 . ? Cu2 O7 H7 113.7 . . ? Cu1 O7 H7 113.7 . . ? C2 N1 N2 107.5(5) . . ? C2 N1 Cu2 132.1(4) . 3_676 ? N2 N1 Cu2 120.4(4) . 3_676 ? C1 N2 N1 107.5(5) . . ? C1 N2 Cu1 132.8(4) . . ? N1 N2 Cu1 118.9(4) . . ? C1 N3 C2 107.0(5) . . ? C1 N3 N4 129.7(5) . . ? C2 N3 N4 122.9(5) . . ? N3 N4 H4' 102.6 . . ? N3 N4 H4" 98.2 . . ? H4' N4 H4" 112.8 . . ? N2 C1 N3 109.1(5) . . ? N2 C1 H1 125.5 . . ? N3 C1 H1 125.5 . . ? N1 C2 N3 108.9(5) . . ? N1 C2 H2 125.6 . . ? N3 C2 H2 125.6 . . ? C4 C3 C8 119.8(5) . . ? C4 C3 C9 122.0(5) . . ? C8 C3 C9 118.2(5) . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 121.0(5) . . ? C4 C5 C10 120.5(5) . . ? C6 C5 C10 118.5(5) . . ? C7 C6 C5 119.2(5) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 120.8(5) . . ? C6 C7 C11 120.2(5) . . ? C8 C7 C11 118.9(5) . . ? C7 C8 C3 118.9(5) . . ? C7 C8 H8 120.6 . . ? C3 C8 H8 120.6 . . ? O2 C9 O1 125.7(6) . . ? O2 C9 C3 120.2(6) . . ? O1 C9 C3 114.1(5) . . ? O3 C10 O4 123.8(5) . . ? O3 C10 C5 120.7(5) . . ? O4 C10 C5 115.5(5) . . ? O6 C11 O5 126.4(5) . . ? O6 C11 C7 117.3(5) . . ? O5 C11 C7 116.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Cu1 O4 C10 73.6(4) 3_676 . . . ? O5 Cu1 O4 C10 -103.9(4) 4_575 . . . ? N2 Cu1 O4 C10 -7.9(10) . . . . ? O7 Cu1 O4 C10 157.4(4) . . . . ? O7 Cu1 O4 Cu2 -109.64(16) 3_676 . . . ? O5 Cu1 O4 Cu2 72.82(18) 4_575 . . . ? N2 Cu1 O4 Cu2 168.9(7) . . . . ? O7 Cu1 O4 Cu2 -25.80(12) . . . . ? O1 Cu2 O4 C10 23.6(6) 2_756 . . . ? O7 Cu2 O4 C10 -153.5(6) . . . . ? O6 Cu2 O4 C10 115.8(6) 4_575 . . . ? N1 Cu2 O4 C10 -66.3(6) 3_676 . . . ? O1 Cu2 O4 Cu1 -152.04(17) 2_756 . . . ? O7 Cu2 O4 Cu1 30.87(15) . . . . ? O6 Cu2 O4 Cu1 -59.77(18) 4_575 . . . ? N1 Cu2 O4 Cu1 118.13(19) 3_676 . . . ? O1 Cu2 O7 Cu1 -95.3(7) 2_756 . . 3_676 ? O6 Cu2 O7 Cu1 166.5(2) 4_575 . . 3_676 ? N1 Cu2 O7 Cu1 -18.6(2) 3_676 . . 3_676 ? O4 Cu2 O7 Cu1 74.1(2) . . . 3_676 ? O1 Cu2 O7 Cu1 164.3(6) 2_756 . . . ? O6 Cu2 O7 Cu1 66.11(16) 4_575 . . . ? N1 Cu2 O7 Cu1 -118.99(18) 3_676 . . . ? O4 Cu2 O7 Cu1 -26.32(13) . . . . ? O7 Cu1 O7 Cu1 0.0 3_676 . . 3_676 ? O5 Cu1 O7 Cu1 178.45(17) 4_575 . . 3_676 ? O4 Cu1 O7 Cu1 -91.00(17) . . . 3_676 ? N2 Cu1 O7 Cu1 85.3(2) . . . 3_676 ? O7 Cu1 O7 Cu2 122.1(2) 3_676 . . . ? O5 Cu1 O7 Cu2 -59.42(18) 4_575 . . . ? O4 Cu1 O7 Cu2 31.13(16) . . . . ? N2 Cu1 O7 Cu2 -152.54(17) . . . . ? C2 N1 N2 C1 1.3(7) . . . . ? Cu2 N1 N2 C1 -179.6(4) 3_676 . . . ? C2 N1 N2 Cu1 -169.8(4) . . . . ? Cu2 N1 N2 Cu1 9.3(6) 3_676 . . . ? O7 Cu1 N2 C1 -165.2(6) 3_676 . . . ? O5 Cu1 N2 C1 12.9(6) 4_575 . . . ? O4 Cu1 N2 C1 -83.6(10) . . . . ? O7 Cu1 N2 C1 112.3(6) . . . . ? O7 Cu1 N2 N1 3.2(4) 3_676 . . . ? O5 Cu1 N2 N1 -178.7(4) 4_575 . . . ? O4 Cu1 N2 N1 84.9(9) . . . . ? O7 Cu1 N2 N1 -79.3(4) . . . . ? N1 N2 C1 N3 -2.0(7) . . . . ? Cu1 N2 C1 N3 167.4(4) . . . . ? C2 N3 C1 N2 2.0(7) . . . . ? N4 N3 C1 N2 -170.8(6) . . . . ? N2 N1 C2 N3 -0.1(7) . . . . ? Cu2 N1 C2 N3 -179.0(4) 3_676 . . . ? C1 N3 C2 N1 -1.2(7) . . . . ? N4 N3 C2 N1 172.2(6) . . . . ? C8 C3 C4 C5 -0.9(9) . . . . ? C9 C3 C4 C5 177.1(6) . . . . ? C3 C4 C5 C6 3.6(9) . . . . ? C3 C4 C5 C10 -179.1(5) . . . . ? C4 C5 C6 C7 -3.6(9) . . . . ? C10 C5 C6 C7 179.1(5) . . . . ? C5 C6 C7 C8 0.8(9) . . . . ? C5 C6 C7 C11 177.7(5) . . . . ? C6 C7 C8 C3 1.7(9) . . . . ? C11 C7 C8 C3 -175.1(5) . . . . ? C4 C3 C8 C7 -1.7(9) . . . . ? C9 C3 C8 C7 -179.8(5) . . . . ? Cu2 O1 C9 O2 -14.1(9) 2_746 . . . ? Cu2 O1 C9 C3 163.7(4) 2_746 . . . ? C4 C3 C9 O2 -145.4(6) . . . . ? C8 C3 C9 O2 32.6(9) . . . . ? C4 C3 C9 O1 36.6(8) . . . . ? C8 C3 C9 O1 -145.4(6) . . . . ? Cu1 O4 C10 O3 28.2(8) . . . . ? Cu2 O4 C10 O3 -146.5(5) . . . . ? Cu1 O4 C10 C5 -150.7(4) . . . . ? Cu2 O4 C10 C5 34.6(8) . . . . ? C4 C5 C10 O3 90.6(7) . . . . ? C6 C5 C10 O3 -92.0(7) . . . . ? C4 C5 C10 O4 -90.4(7) . . . . ? C6 C5 C10 O4 87.0(6) . . . . ? Cu2 O6 C11 O5 -30.7(9) 4_576 . . . ? Cu2 O6 C11 C7 149.7(4) 4_576 . . . ? Cu1 O5 C11 O6 8.6(9) 4_576 . . . ? Cu1 O5 C11 C7 -171.7(4) 4_576 . . . ? C6 C7 C11 O6 165.8(5) . . . . ? C8 C7 C11 O6 -17.4(8) . . . . ? C6 C7 C11 O5 -13.9(8) . . . . ? C8 C7 C11 O5 162.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.935 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.194 data_1 _database_code_depnum_ccdc_archive 'CCDC 860434' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C17 H22 B Cu3 N8 S5 W), C4 H10 O' _chemical_formula_sum 'C38 H54 B2 Cu6 N16 O S10 W2 ' _chemical_formula_weight 1842.27 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.603(2) _cell_length_b 12.390(3) _cell_length_c 12.774(3) _cell_angle_alpha 80.25(3) _cell_angle_beta 70.91(3) _cell_angle_gamma 67.35(3) _cell_volume 1461.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'black red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 6.460 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.094 _exptl_absorpt_correction_T_max 0.524 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13232 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6722 _reflns_number_gt 5257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 constr _refine_ls_number_reflns 6583 _refine_ls_number_parameters 336 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 0.629 _refine_ls_restrained_S_all 0.631 _refine_ls_shift/su_max 0.010 _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 O1 O 0.0000 0.0000 0.5000 0.276(12) Uiso 1 2 d S . . C19 C 0.145(2) -0.0795(17) 0.3224(16) 0.174(7) Uiso 1 1 d D . . H19A H 0.0510 -0.0774 0.3279 0.261 Uiso 1 1 calc R . . H19B H 0.2146 -0.1568 0.3025 0.261 Uiso 1 1 calc R . . H19C H 0.1693 -0.0217 0.2661 0.261 Uiso 1 1 calc R . . C20 C 0.146(3) -0.055(2) 0.422(2) 0.267(12) Uiso 1 1 d D . . H20A H 0.1991 -0.0016 0.4085 0.320 Uiso 1 1 calc R . . H20B H 0.1978 -0.1275 0.4573 0.320 Uiso 1 1 calc R . . W1 W -0.21757(2) 0.689509(16) 0.202935(15) 0.02317(8) Uani 1 1 d . . . C1 C -0.4178(6) 0.7197(5) 0.4648(4) 0.0304(11) Uani 1 1 d . . . C2 C -0.4511(6) 0.6508(5) 0.5594(5) 0.0357(12) Uani 1 1 d . . . H2 H -0.5142 0.6771 0.6289 0.043 Uiso 1 1 calc R . . C11 C 0.1096(6) 0.5455(5) 0.2384(4) 0.0310(11) Uani 1 1 d . . . C3 C -0.3748(6) 0.5376(5) 0.5323(4) 0.0300(11) Uani 1 1 d . . . C16 C -0.5921(7) 1.1440(5) 0.1736(4) 0.0333(12) Uani 1 1 d . . . C6 C -0.3139(6) 0.4960(5) 0.1202(4) 0.0315(11) Uani 1 1 d . . . C17 C -0.1633(6) 1.0804(5) -0.0104(4) 0.0312(11) Uani 1 1 d . . . C4 C -0.4803(7) 0.8493(5) 0.4571(5) 0.0413(14) Uani 1 1 d . . . H4A H -0.4089 0.8818 0.4534 0.062 Uiso 1 1 calc R . . H4B H -0.5610 0.8766 0.5220 0.062 Uiso 1 1 calc R . . H4C H -0.5120 0.8746 0.3909 0.062 Uiso 1 1 calc R . . C7 C -0.2969(6) 0.3778(5) 0.1394(5) 0.0355(13) Uani 1 1 d . . . H7 H -0.3238 0.3348 0.1021 0.043 Uiso 1 1 calc R . . C13 C 0.0842(7) 0.3935(5) 0.3492(5) 0.0395(13) Uani 1 1 d . . . C5 C -0.3693(7) 0.4272(5) 0.6042(5) 0.0395(13) Uani 1 1 d . . . H5A H -0.4400 0.4464 0.6757 0.059 Uiso 1 1 calc R . . H5B H -0.2751 0.3891 0.6146 0.059 Uiso 1 1 calc R . . H5C H -0.3894 0.3749 0.5686 0.059 Uiso 1 1 calc R . . C9 C -0.3773(7) 0.5744(5) 0.0342(5) 0.0411(14) Uani 1 1 d . . . H9A H -0.4564 0.6419 0.0688 0.062 Uiso 1 1 calc R . . H9B H -0.4113 0.5321 -0.0012 0.062 Uiso 1 1 calc R . . H9C H -0.3054 0.6003 -0.0210 0.062 Uiso 1 1 calc R . . C12 C 0.1802(6) 0.4469(5) 0.2946(5) 0.0380(13) Uani 1 1 d . . . H12 H 0.2757 0.4217 0.2950 0.046 Uiso 1 1 calc R . . C8 C -0.2330(6) 0.3360(5) 0.2234(5) 0.0346(12) Uani 1 1 d . . . C14 C 0.1760(6) 0.6310(5) 0.1703(5) 0.0395(13) Uani 1 1 d . . . H14A H 0.1662 0.6402 0.0961 0.059 Uiso 1 1 calc R . . H14B H 0.2764 0.6023 0.1662 0.059 Uiso 1 1 calc R . . H14C H 0.1286 0.7061 0.2043 0.059 Uiso 1 1 calc R . . C10 C -0.1809(8) 0.2146(5) 0.2697(6) 0.0501(16) Uani 1 1 d . . . H10A H -0.0782 0.1880 0.2552 0.075 Uiso 1 1 calc R . . H10B H -0.2046 0.1638 0.2352 0.075 Uiso 1 1 calc R . . H10C H -0.2257 0.2124 0.3491 0.075 Uiso 1 1 calc R . . C15 C 0.1016(8) 0.2880(6) 0.4257(7) 0.061(2) Uani 1 1 d . . . H15A H 0.0416 0.3102 0.5000 0.092 Uiso 1 1 calc R . . H15B H 0.2006 0.2521 0.4259 0.092 Uiso 1 1 calc R . . H15C H 0.0740 0.2326 0.4012 0.092 Uiso 1 1 calc R . . N5 N -0.0267(5) 0.5537(4) 0.2561(4) 0.0301(9) Uani 1 1 d . . . N6 N -0.0397(5) 0.4574(4) 0.3255(4) 0.0316(10) Uani 1 1 d . . . N1 N -0.3215(5) 0.6507(4) 0.3815(3) 0.0265(9) Uani 1 1 d . . . N2 N -0.2962(5) 0.5372(4) 0.4247(3) 0.0272(9) Uani 1 1 d . . . N3 N -0.2636(5) 0.5273(4) 0.1916(3) 0.0268(9) Uani 1 1 d . . . N4 N -0.2152(5) 0.4265(4) 0.2552(4) 0.0289(9) Uani 1 1 d . . . N7 N -0.6530(5) 1.1747(4) 0.1101(4) 0.0358(11) Uani 1 1 d . . . N8 N -0.0905(5) 1.1302(4) -0.0159(4) 0.0381(11) Uani 1 1 d . . . S1 S -0.44097(14) 0.79564(11) 0.18424(11) 0.0288(3) Uani 1 1 d . . . S3 S -0.06963(14) 0.65217(11) 0.02417(10) 0.0279(3) Uani 1 1 d . . . S2 S -0.15992(15) 0.82556(11) 0.26033(11) 0.0305(3) Uani 1 1 d . . . S4 S -0.5026(2) 1.10024(13) 0.26765(13) 0.0453(4) Uani 1 1 d . . . S5 S -0.26703(18) 1.00971(14) -0.00994(13) 0.0422(4) Uani 1 1 d . . . Cu1 Cu -0.28170(7) 0.77634(6) 0.01686(5) 0.03404(16) Uani 1 1 d . . . Cu3 Cu -0.34694(8) 0.92711(6) 0.19442(6) 0.03706(17) Uani 1 1 d . . . Cu2 Cu -0.05999(8) 0.81035(6) 0.07590(6) 0.03795(17) Uani 1 1 d . . . B1 B -0.1804(7) 0.4350(5) 0.3605(5) 0.0311(13) Uani 1 1 d . . . H1 H -0.177(6) 0.355(5) 0.411(4) 0.026(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02546(12) 0.02458(11) 0.02285(11) 0.00410(7) -0.01150(9) -0.01084(9) C1 0.035(3) 0.041(3) 0.019(2) -0.001(2) -0.012(2) -0.016(3) C2 0.035(3) 0.048(3) 0.027(3) 0.001(2) -0.013(2) -0.015(3) C11 0.030(3) 0.035(3) 0.031(3) 0.002(2) -0.017(2) -0.009(2) C3 0.030(3) 0.042(3) 0.025(2) 0.005(2) -0.012(2) -0.019(3) C16 0.045(3) 0.025(2) 0.030(3) -0.002(2) -0.016(3) -0.007(2) C6 0.034(3) 0.037(3) 0.029(3) -0.002(2) -0.004(2) -0.022(3) C17 0.034(3) 0.026(2) 0.031(3) 0.007(2) -0.008(2) -0.013(2) C4 0.051(4) 0.043(3) 0.027(3) -0.004(2) -0.012(3) -0.011(3) C7 0.038(3) 0.038(3) 0.037(3) -0.006(2) -0.003(3) -0.026(3) C13 0.036(3) 0.035(3) 0.045(3) 0.007(3) -0.021(3) -0.006(3) C5 0.045(4) 0.046(3) 0.032(3) 0.010(2) -0.016(3) -0.021(3) C9 0.055(4) 0.041(3) 0.040(3) -0.003(3) -0.026(3) -0.020(3) C12 0.034(3) 0.033(3) 0.047(3) 0.005(2) -0.024(3) -0.006(3) C8 0.038(3) 0.027(3) 0.036(3) -0.004(2) 0.002(2) -0.016(3) C14 0.030(3) 0.045(3) 0.047(3) 0.007(3) -0.016(3) -0.016(3) C10 0.061(4) 0.029(3) 0.057(4) 0.003(3) -0.015(4) -0.017(3) C15 0.043(4) 0.052(4) 0.079(5) 0.029(4) -0.030(4) -0.011(3) N5 0.032(2) 0.027(2) 0.030(2) 0.0043(18) -0.014(2) -0.006(2) N6 0.031(2) 0.031(2) 0.034(2) 0.0080(19) -0.016(2) -0.011(2) N1 0.037(3) 0.023(2) 0.022(2) 0.0072(16) -0.0143(19) -0.013(2) N2 0.034(2) 0.025(2) 0.024(2) 0.0058(16) -0.0103(19) -0.012(2) N3 0.028(2) 0.029(2) 0.028(2) 0.0037(17) -0.0083(19) -0.017(2) N4 0.035(3) 0.023(2) 0.028(2) 0.0025(17) -0.0086(19) -0.012(2) N7 0.043(3) 0.034(2) 0.030(2) 0.0051(19) -0.018(2) -0.010(2) N8 0.041(3) 0.032(2) 0.042(3) 0.008(2) -0.012(2) -0.018(2) S1 0.0268(7) 0.0320(6) 0.0293(6) -0.0005(5) -0.0129(5) -0.0087(6) S3 0.0288(7) 0.0294(6) 0.0252(6) 0.0022(5) -0.0084(5) -0.0111(6) S2 0.0338(7) 0.0299(6) 0.0357(7) 0.0020(5) -0.0191(6) -0.0138(6) S4 0.0626(11) 0.0338(7) 0.0452(8) -0.0062(6) -0.0385(8) -0.0022(8) S5 0.0517(9) 0.0444(8) 0.0453(8) 0.0144(7) -0.0242(7) -0.0311(8) Cu1 0.0338(4) 0.0415(4) 0.0260(3) 0.0030(3) -0.0161(3) -0.0081(3) Cu3 0.0380(4) 0.0285(3) 0.0499(4) -0.0016(3) -0.0246(3) -0.0075(3) Cu2 0.0411(4) 0.0378(4) 0.0408(4) 0.0026(3) -0.0080(3) -0.0253(4) B1 0.038(4) 0.029(3) 0.030(3) 0.008(2) -0.016(3) -0.015(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 O1 C20 1.51(3) . ? O1 C20 1.51(3) 2_556 ? C19 C20 1.357(16) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? W1 N1 2.245(4) . ? W1 N3 2.280(4) . ? W1 S2 2.2930(13) . ? W1 S1 2.2938(15) . ? W1 N5 2.297(4) . ? W1 S3 2.3120(16) . ? W1 Cu1 2.6262(10) . ? W1 Cu2 2.6452(11) . ? W1 Cu3 2.7275(11) . ? C1 N1 1.354(7) . ? C1 C2 1.385(8) . ? C1 C4 1.482(8) . ? C2 C3 1.360(8) . ? C2 H2 0.9400 . ? C11 N5 1.354(7) . ? C11 C12 1.385(7) . ? C11 C14 1.495(8) . ? C3 N2 1.354(7) . ? C3 C5 1.505(7) . ? C16 N7 1.126(7) . ? C16 S4 1.663(5) . ? C6 N3 1.364(6) . ? C6 C7 1.393(7) . ? C6 C9 1.491(8) . ? C17 N8 1.139(7) . ? C17 S5 1.647(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C7 C8 1.376(8) . ? C7 H7 0.9400 . ? C13 N6 1.350(7) . ? C13 C12 1.363(8) . ? C13 C15 1.483(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C12 H12 0.9400 . ? C8 N4 1.352(6) . ? C8 C10 1.480(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? N5 N6 1.385(6) . ? N6 B1 1.530(8) . ? N1 N2 1.377(5) . ? N2 B1 1.510(8) . ? N3 N4 1.385(6) . ? N4 B1 1.536(7) . ? N7 Cu1 1.886(4) 2_475 ? N8 Cu2 1.895(5) 2_575 ? S1 Cu1 2.2319(17) . ? S1 Cu3 2.2519(15) . ? S3 Cu1 2.2037(17) . ? S3 Cu2 2.2193(15) . ? S2 Cu3 2.2441(16) . ? S2 Cu2 2.2522(17) . ? S4 Cu3 2.268(2) . ? S5 Cu3 2.6261(19) . ? Cu1 N7 1.886(4) 2_475 ? Cu1 Cu2 2.8813(11) . ? Cu1 Cu3 2.9199(13) . ? Cu3 Cu2 2.8251(17) . ? Cu2 N8 1.895(5) 2_575 ? B1 H1 1.09(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 O1 C20 180(3) . 2_556 ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 C20 O1 114(2) . . ? C19 C20 H20A 108.7 . . ? O1 C20 H20A 108.7 . . ? C19 C20 H20B 108.7 . . ? O1 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? N1 W1 N3 78.29(15) . . ? N1 W1 S2 88.40(11) . . ? N3 W1 S2 163.75(11) . . ? N1 W1 S1 88.22(12) . . ? N3 W1 S1 86.36(12) . . ? S2 W1 S1 102.68(5) . . ? N1 W1 N5 78.52(16) . . ? N3 W1 N5 82.85(16) . . ? S2 W1 N5 85.40(12) . . ? S1 W1 N5 164.34(12) . . ? N1 W1 S3 157.88(11) . . ? N3 W1 S3 85.12(12) . . ? S2 W1 S3 105.04(5) . . ? S1 W1 S3 105.37(6) . . ? N5 W1 S3 85.03(12) . . ? N1 W1 Cu1 140.69(11) . . ? N3 W1 Cu1 89.69(11) . . ? S2 W1 Cu1 106.56(4) . . ? S1 W1 Cu1 53.43(5) . . ? N5 W1 Cu1 137.45(12) . . ? S3 W1 Cu1 52.54(4) . . ? N1 W1 Cu2 141.77(10) . . ? N3 W1 Cu2 137.79(11) . . ? S2 W1 Cu2 53.70(4) . . ? S1 W1 Cu2 103.50(5) . . ? N5 W1 Cu2 92.11(12) . . ? S3 W1 Cu2 52.67(4) . . ? Cu1 W1 Cu2 66.27(3) . . ? N1 W1 Cu3 99.26(12) . . ? N3 W1 Cu3 138.76(11) . . ? S2 W1 Cu3 52.23(4) . . ? S1 W1 Cu3 52.43(4) . . ? N5 W1 Cu3 137.60(11) . . ? S3 W1 Cu3 102.87(5) . . ? Cu1 W1 Cu3 66.07(4) . . ? Cu2 W1 Cu3 63.43(4) . . ? N1 C1 C2 109.6(5) . . ? N1 C1 C4 125.8(5) . . ? C2 C1 C4 124.6(5) . . ? C3 C2 C1 106.7(5) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? N5 C11 C12 110.3(5) . . ? N5 C11 C14 125.7(5) . . ? C12 C11 C14 124.0(5) . . ? N2 C3 C2 108.1(5) . . ? N2 C3 C5 122.8(5) . . ? C2 C3 C5 129.0(5) . . ? N7 C16 S4 179.3(5) . . ? N3 C6 C7 109.5(5) . . ? N3 C6 C9 126.1(5) . . ? C7 C6 C9 124.4(5) . . ? N8 C17 S5 176.8(5) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C7 C6 106.8(5) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? N6 C13 C12 107.6(5) . . ? N6 C13 C15 123.2(6) . . ? C12 C13 C15 129.2(5) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C13 C12 C11 106.7(5) . . ? C13 C12 H12 126.6 . . ? C11 C12 H12 126.6 . . ? N4 C8 C7 107.6(5) . . ? N4 C8 C10 123.1(6) . . ? C7 C8 C10 129.1(5) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 N5 N6 104.8(4) . . ? C11 N5 W1 133.8(4) . . ? N6 N5 W1 121.4(3) . . ? C13 N6 N5 110.6(5) . . ? C13 N6 B1 129.7(5) . . ? N5 N6 B1 119.7(4) . . ? C1 N1 N2 105.9(4) . . ? C1 N1 W1 132.8(3) . . ? N2 N1 W1 121.1(3) . . ? C3 N2 N1 109.6(4) . . ? C3 N2 B1 128.3(4) . . ? N1 N2 B1 121.6(4) . . ? C6 N3 N4 105.5(4) . . ? C6 N3 W1 133.7(3) . . ? N4 N3 W1 120.0(3) . . ? C8 N4 N3 110.5(4) . . ? C8 N4 B1 128.7(4) . . ? N3 N4 B1 119.5(4) . . ? C16 N7 Cu1 168.3(5) . 2_475 ? C17 N8 Cu2 159.3(5) . 2_575 ? Cu1 S1 Cu3 81.27(6) . . ? Cu1 S1 W1 70.93(5) . . ? Cu3 S1 W1 73.73(5) . . ? Cu1 S3 Cu2 81.30(6) . . ? Cu1 S3 W1 71.08(5) . . ? Cu2 S3 W1 71.40(5) . . ? Cu3 S2 Cu2 77.85(6) . . ? Cu3 S2 W1 73.90(5) . . ? Cu2 S2 W1 71.17(5) . . ? C16 S4 Cu3 97.4(2) . . ? C17 S5 Cu3 106.6(2) . . ? N7 Cu1 S3 126.78(16) 2_475 . ? N7 Cu1 S1 119.08(16) 2_475 . ? S3 Cu1 S1 111.35(6) . . ? N7 Cu1 W1 171.05(15) 2_475 . ? S3 Cu1 W1 56.39(5) . . ? S1 Cu1 W1 55.64(4) . . ? N7 Cu1 Cu2 131.71(16) 2_475 . ? S3 Cu1 Cu2 49.59(4) . . ? S1 Cu1 Cu2 98.08(5) . . ? W1 Cu1 Cu2 57.18(3) . . ? N7 Cu1 Cu3 124.94(15) 2_475 . ? S3 Cu1 Cu3 99.89(5) . . ? S1 Cu1 Cu3 49.67(4) . . ? W1 Cu1 Cu3 58.63(3) . . ? Cu2 Cu1 Cu3 58.28(4) . . ? S2 Cu3 S1 105.62(6) . . ? S2 Cu3 S4 119.26(6) . . ? S1 Cu3 S4 116.75(7) . . ? S2 Cu3 S5 111.84(7) . . ? S1 Cu3 S5 105.54(6) . . ? S4 Cu3 S5 96.88(7) . . ? S2 Cu3 W1 53.87(4) . . ? S1 Cu3 W1 53.84(4) . . ? S4 Cu3 W1 153.56(6) . . ? S5 Cu3 W1 109.37(6) . . ? S2 Cu3 Cu2 51.20(5) . . ? S1 Cu3 Cu2 99.22(5) . . ? S4 Cu3 Cu2 143.33(6) . . ? S5 Cu3 Cu2 64.99(6) . . ? W1 Cu3 Cu2 56.87(4) . . ? S2 Cu3 Cu1 98.89(5) . . ? S1 Cu3 Cu1 49.07(4) . . ? S4 Cu3 Cu1 141.69(5) . . ? S5 Cu3 Cu1 63.08(4) . . ? W1 Cu3 Cu1 55.30(3) . . ? Cu2 Cu3 Cu1 60.18(4) . . ? N8 Cu2 S3 126.17(16) 2_575 . ? N8 Cu2 S2 114.61(16) 2_575 . ? S3 Cu2 S2 109.62(6) . . ? N8 Cu2 W1 161.18(16) 2_575 . ? S3 Cu2 W1 55.93(4) . . ? S2 Cu2 W1 55.13(4) . . ? N8 Cu2 Cu3 129.01(15) 2_575 . ? S3 Cu2 Cu3 102.37(5) . . ? S2 Cu2 Cu3 50.95(5) . . ? W1 Cu2 Cu3 59.71(3) . . ? N8 Cu2 Cu1 141.17(16) 2_575 . ? S3 Cu2 Cu1 49.11(5) . . ? S2 Cu2 Cu1 99.81(5) . . ? W1 Cu2 Cu1 56.55(3) . . ? Cu3 Cu2 Cu1 61.54(3) . . ? N2 B1 N6 108.4(4) . . ? N2 B1 N4 109.5(5) . . ? N6 B1 N4 108.2(4) . . ? N2 B1 H1 109(3) . . ? N6 B1 H1 114(3) . . ? N4 B1 H1 108(3) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.244 _refine_diff_density_min -1.603 _refine_diff_density_rms 0.169