# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Miguel Julve' _publ_contact_author_email MIGUEL.JULVE@UV.ES _publ_section_title ; Dinuclear, tetranuclear and one-dimensional pyrazine-based copper(II) complexes: preparation, X-ray structure and magnetic properties ; _publ_contact_author_address ; Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; loop_ _publ_author_name 'Miguel Julve' L.Canadillas-Delgado 'F Lloret' 'Catalina Ruiz-Perez' 'Consuelo Yuste' # Attachment 'Compound1.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 738678' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Cu2 F12 N6 O14 S4' _chemical_formula_weight 1147.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.3395(3) _cell_length_b 12.8704(3) _cell_length_c 20.5383(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.9750(10) _cell_angle_gamma 90.00 _cell_volume 4032.76(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 92 _cell_measurement_theta_min 6.25 _cell_measurement_theta_max 20.25 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7226 _exptl_absorpt_correction_T_max 0.8735 _exptl_absorpt_process_details ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22783 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4882 _reflns_number_gt 4351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0882P)^2^+18.5954P] 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 4882 _refine_ls_number_parameters 306 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1768 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Cu1 Cu 0.01658(3) 0.24097(3) 0.40959(2) 0.03030(16) Uani 1 1 d . . . F1 F -0.0895(3) -0.1508(4) 0.3043(2) 0.1096(15) Uani 1 1 d . . . F2 F -0.1535(2) -0.1017(4) 0.3874(2) 0.0919(13) Uani 1 1 d . . . F3 F -0.1452(2) 0.0019(4) 0.3060(2) 0.1018(15) Uani 1 1 d . . . F4 F 0.1509(4) 0.4791(4) 0.3080(3) 0.130(2) Uani 1 1 d . . . F5 F 0.1986(4) 0.5803(6) 0.3904(4) 0.180(3) Uani 1 1 d . . . F6 F 0.1027(5) 0.6334(4) 0.3116(3) 0.156(3) Uani 1 1 d . . . O1W O 0.0318(2) 0.2424(2) 0.50458(14) 0.0397(6) Uani 1 1 d D . . O1 O -0.0252(2) 0.0661(2) 0.41883(17) 0.0547(8) Uani 1 1 d . . . O2 O 0.0481(2) 0.0088(2) 0.32682(15) 0.0445(7) Uani 1 1 d . . . O3 O 0.0381(2) -0.1056(3) 0.41876(16) 0.0479(7) Uani 1 1 d . . . O4 O 0.0769(3) 0.4175(3) 0.4257(2) 0.0753(12) Uani 1 1 d . . . O5 O -0.0269(3) 0.4842(4) 0.3421(3) 0.108(2) Uani 1 1 d . . . O6 O 0.0218(4) 0.5934(4) 0.4317(3) 0.1034(19) Uani 1 1 d . . . S1 S 0.00133(6) -0.01939(7) 0.38064(5) 0.0329(2) Uani 1 1 d . . . S2 S 0.04692(10) 0.50979(9) 0.39707(7) 0.0616(4) Uani 1 1 d . . . C1 C -0.1654(3) 0.3076(4) 0.4345(2) 0.0437(9) Uani 1 1 d . . . H1 H -0.1463 0.3025 0.4789 0.052 Uiso 1 1 calc R . . C2 C -0.2484(3) 0.3456(4) 0.4158(2) 0.0506(11) Uani 1 1 d . . . H2 H -0.2853 0.3635 0.4472 0.061 Uiso 1 1 calc R . . C3 C -0.2758(3) 0.3566(4) 0.3506(2) 0.0466(10) Uani 1 1 d . . . H3 H -0.3306 0.3846 0.3372 0.056 Uiso 1 1 calc R . . C4 C -0.2207(2) 0.3254(3) 0.3048(2) 0.0370(8) Uani 1 1 d . . . H4 H -0.2381 0.3321 0.2603 0.044 Uiso 1 1 calc R . . C5 C -0.1399(2) 0.2845(3) 0.32627(17) 0.0296(7) Uani 1 1 d . . . C6 C -0.0732(2) 0.2538(2) 0.28272(17) 0.0260(6) Uani 1 1 d . . . C7 C 0.0811(2) 0.2356(2) 0.28508(16) 0.0255(6) Uani 1 1 d . . . C8 C 0.1568(2) 0.2013(3) 0.33105(17) 0.0287(6) Uani 1 1 d . . . C9 C 0.2331(2) 0.1599(3) 0.3125(2) 0.0365(8) Uani 1 1 d . . . H9 H 0.2426 0.1573 0.2685 0.044 Uiso 1 1 calc R . . C10 C 0.2959(3) 0.1222(4) 0.3602(2) 0.0462(10) Uani 1 1 d . . . H10 H 0.3482 0.0947 0.3485 0.055 Uiso 1 1 calc R . . C11 C 0.2804(3) 0.1259(4) 0.4245(2) 0.0477(10) Uani 1 1 d . . . H11 H 0.3222 0.1022 0.4571 0.057 Uiso 1 1 calc R . . C12 C 0.2011(3) 0.1658(3) 0.44002(19) 0.0405(9) Uani 1 1 d . . . H12 H 0.1898 0.1667 0.4836 0.049 Uiso 1 1 calc R . . C13 C -0.1020(3) -0.0710(5) 0.3424(3) 0.0627(14) Uani 1 1 d . . . C14 C 0.1253(6) 0.5526(6) 0.3451(4) 0.098(3) Uani 1 1 d . . . N1 N -0.1115(2) 0.2779(2) 0.39079(15) 0.0330(6) Uani 1 1 d . . . N2 N 0.00699(19) 0.2447(2) 0.31386(15) 0.0268(6) Uani 1 1 d . . . N3 N 0.14071(19) 0.2030(2) 0.39460(14) 0.0312(6) Uani 1 1 d . . . H1WA H 0.011(4) 0.187(3) 0.523(3) 0.08(2) Uiso 1 1 d D . . H1WB H 0.018(4) 0.306(2) 0.516(3) 0.070(18) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0314(3) 0.0356(3) 0.0243(2) -0.00117(15) 0.00502(17) 0.00385(16) F1 0.118(3) 0.096(3) 0.110(3) -0.042(3) -0.014(3) -0.041(3) F2 0.0462(17) 0.122(3) 0.107(3) 0.042(2) 0.0073(17) -0.0275(19) F3 0.0540(19) 0.144(4) 0.101(3) 0.057(3) -0.0208(19) -0.001(2) F4 0.125(4) 0.148(4) 0.133(4) -0.055(3) 0.089(3) -0.022(3) F5 0.097(4) 0.163(6) 0.275(9) -0.049(6) -0.009(5) -0.058(4) F6 0.236(7) 0.105(4) 0.139(5) 0.053(3) 0.073(5) -0.034(4) O1W 0.0560(18) 0.0365(15) 0.0270(13) -0.0020(10) 0.0070(12) 0.0001(12) O1 0.077(2) 0.0347(15) 0.0580(19) -0.0070(13) 0.0309(17) -0.0031(15) O2 0.0498(17) 0.0408(15) 0.0452(16) 0.0016(12) 0.0154(13) -0.0036(13) O3 0.0438(15) 0.0477(17) 0.0529(17) 0.0157(14) 0.0078(13) 0.0078(13) O4 0.102(3) 0.047(2) 0.076(3) 0.0069(18) 0.004(2) 0.003(2) O5 0.060(3) 0.089(4) 0.167(6) 0.001(4) -0.021(3) -0.004(2) O6 0.163(5) 0.062(3) 0.096(3) -0.024(2) 0.063(3) 0.023(3) S1 0.0335(4) 0.0291(4) 0.0368(5) -0.0002(3) 0.0064(3) -0.0016(3) S2 0.0814(9) 0.0380(6) 0.0733(8) 0.0123(5) 0.0452(7) 0.0194(6) C1 0.043(2) 0.054(2) 0.0371(19) -0.0032(17) 0.0161(16) 0.0080(18) C2 0.044(2) 0.060(3) 0.053(2) -0.005(2) 0.024(2) 0.012(2) C3 0.0333(19) 0.050(2) 0.058(3) 0.0014(19) 0.0145(18) 0.0140(17) C4 0.0304(17) 0.0401(19) 0.0414(19) 0.0015(15) 0.0076(15) 0.0088(15) C5 0.0287(16) 0.0282(16) 0.0331(17) 0.0011(13) 0.0084(13) 0.0026(13) C6 0.0241(15) 0.0241(14) 0.0302(16) 0.0018(11) 0.0044(12) 0.0021(11) C7 0.0238(15) 0.0246(14) 0.0285(15) -0.0032(11) 0.0051(12) -0.0005(11) C8 0.0264(15) 0.0269(15) 0.0323(16) -0.0019(13) 0.0009(12) -0.0006(12) C9 0.0259(16) 0.043(2) 0.0405(19) -0.0019(16) 0.0045(14) 0.0015(14) C10 0.0291(18) 0.051(2) 0.058(2) -0.001(2) 0.0001(17) 0.0080(17) C11 0.034(2) 0.051(2) 0.053(2) 0.0033(19) -0.0144(17) 0.0024(17) C12 0.039(2) 0.047(2) 0.0324(18) -0.0015(16) -0.0070(15) -0.0008(17) C13 0.049(3) 0.071(3) 0.065(3) 0.016(3) -0.005(2) -0.014(2) C14 0.124(7) 0.071(4) 0.108(6) -0.001(4) 0.051(5) -0.018(4) N1 0.0330(15) 0.0359(15) 0.0318(15) 0.0005(12) 0.0110(12) 0.0055(12) N2 0.0250(14) 0.0266(13) 0.0294(14) 0.0003(10) 0.0049(11) 0.0023(10) N3 0.0295(14) 0.0329(15) 0.0306(14) -0.0027(12) 0.0000(11) -0.0005(12) _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 O1W 1.941(3) . ? Cu1 N2 1.957(3) . ? Cu1 N1 2.019(3) . ? Cu1 N3 2.020(3) . ? Cu1 O1 2.353(3) . ? F1 C13 1.317(8) . ? F2 C13 1.337(6) . ? F3 C13 1.332(7) . ? F4 C14 1.301(9) . ? F5 C14 1.428(11) . ? F6 C14 1.275(10) . ? O1 S1 1.435(3) . ? O2 S1 1.427(3) . ? O3 S1 1.439(3) . ? O4 S2 1.383(4) . ? O5 S2 1.549(5) . ? O6 S2 1.367(4) . ? S1 C13 1.821(5) . ? S2 C14 1.776(8) . ? C1 N1 1.338(5) . ? C1 C2 1.381(6) . ? C2 C3 1.368(7) . ? C3 C4 1.387(5) . ? C4 C5 1.376(5) . ? C5 N1 1.354(5) . ? C5 C6 1.481(5) . ? C6 N2 1.331(4) . ? C6 C7 1.405(5) 2 ? C7 N2 1.340(4) . ? C7 C6 1.405(5) 2 ? C7 C8 1.485(5) . ? C8 N3 1.354(4) . ? C8 C9 1.376(5) . ? C9 C10 1.389(6) . ? C10 C11 1.366(7) . ? C11 C12 1.388(6) . ? C12 N3 1.334(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 O1W Cu1 N2 176.75(12) . . ? O1W Cu1 N1 101.71(13) . . ? N2 Cu1 N1 80.35(12) . . ? O1W Cu1 N3 97.96(13) . . ? N2 Cu1 N3 80.00(12) . . ? N1 Cu1 N3 160.32(12) . . ? O1W Cu1 O1 86.18(12) . . ? N2 Cu1 O1 96.42(12) . . ? N1 Cu1 O1 88.41(13) . . ? N3 Cu1 O1 92.88(12) . . ? S1 O1 Cu1 126.45(19) . . ? O2 S1 O1 115.00(18) . . ? O2 S1 O3 114.70(19) . . ? O1 S1 O3 114.3(2) . . ? O2 S1 C13 104.1(2) . . ? O1 S1 C13 103.4(3) . . ? O3 S1 C13 103.2(2) . . ? O6 S2 O4 123.7(3) . . ? O6 S2 O5 108.9(4) . . ? O4 S2 O5 108.2(3) . . ? O6 S2 C14 108.3(4) . . ? O4 S2 C14 107.8(4) . . ? O5 S2 C14 96.7(4) . . ? N1 C1 C2 122.0(4) . . ? C3 C2 C1 119.3(4) . . ? C2 C3 C4 119.1(4) . . ? C5 C4 C3 119.1(4) . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 113.7(3) . . ? C4 C5 C6 124.4(3) . . ? N2 C6 C7 116.2(3) . 2 ? N2 C6 C5 113.3(3) . . ? C7 C6 C5 130.5(3) 2 . ? N2 C7 C6 115.6(3) . 2 ? N2 C7 C8 112.9(3) . . ? C6 C7 C8 131.4(3) 2 . ? N3 C8 C9 121.3(3) . . ? N3 C8 C7 113.5(3) . . ? C9 C8 C7 124.8(3) . . ? C8 C9 C10 119.2(4) . . ? C11 C10 C9 119.5(4) . . ? C10 C11 C12 118.7(4) . . ? N3 C12 C11 122.3(4) . . ? F1 C13 F3 108.2(5) . . ? F1 C13 F2 108.3(5) . . ? F3 C13 F2 107.6(5) . . ? F1 C13 S1 111.5(4) . . ? F3 C13 S1 110.2(4) . . ? F2 C13 S1 111.0(4) . . ? F6 C14 F4 110.9(8) . . ? F6 C14 F5 107.4(7) . . ? F4 C14 F5 107.3(8) . . ? F6 C14 S2 114.5(7) . . ? F4 C14 S2 113.0(5) . . ? F5 C14 S2 102.9(6) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 Cu1 126.5(3) . . ? C5 N1 Cu1 114.2(2) . . ? C6 N2 C7 125.4(3) . . ? C6 N2 Cu1 117.0(2) . . ? C7 N2 Cu1 117.6(2) . . ? C12 N3 C8 119.0(3) . . ? C12 N3 Cu1 125.3(3) . . ? C8 N3 Cu1 114.9(2) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.699 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.161 # Attachment 'Compound2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 738679' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 Cr Cu N6 O7' _chemical_formula_weight 622.02 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' Cr Cr 0.3209 0.6236 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.5171(7) _cell_length_b 27.088(2) _cell_length_c 7.8068(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.576(7) _cell_angle_gamma 90.00 _cell_volume 2434.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 105 _cell_measurement_theta_min 7.67 _cell_measurement_theta_max 20.25 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 1.379 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8095 _exptl_absorpt_correction_T_max 0.8977 _exptl_absorpt_process_details ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25322 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 30.20 _reflns_number_total 7206 _reflns_number_gt 5465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0242P)^2^+3.5399P] 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 7206 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Cr1 Cr 0.25574(3) 0.167570(14) -0.32626(5) 0.01026(9) Uani 1 1 d . . . Cu1 Cu 0.24142(3) 0.218444(10) 0.10378(4) 0.00964(7) Uani 1 1 d . . . C1 C 0.4848(2) 0.23820(9) 0.0107(3) 0.0167(5) Uani 1 1 d . . . H1 H 0.4590 0.2702 -0.0111 0.020 Uiso 1 1 calc R . . C2 C 0.5977(2) 0.22593(10) -0.0271(4) 0.0211(6) Uani 1 1 d . . . H2 H 0.6477 0.2494 -0.0710 0.025 Uiso 1 1 calc R . . C3 C 0.6350(2) 0.17801(10) 0.0017(4) 0.0197(6) Uani 1 1 d . . . H3 H 0.7103 0.1687 -0.0242 0.024 Uiso 1 1 calc R . . C4 C 0.5588(2) 0.14388(9) 0.0696(3) 0.0154(5) Uani 1 1 d . . . H4 H 0.5823 0.1115 0.0889 0.019 Uiso 1 1 calc R . . C5 C 0.4473(2) 0.15886(9) 0.1082(3) 0.0110(5) Uani 1 1 d . . . C6 C 0.0581(2) 0.16543(9) 0.2572(3) 0.0114(5) Uani 1 1 d . . . C7 C -0.0434(2) 0.15502(9) 0.3412(3) 0.0144(5) Uani 1 1 d . . . H7 H -0.0550 0.1242 0.3906 0.017 Uiso 1 1 calc R . . C8 C -0.1274(2) 0.19166(10) 0.3498(3) 0.0182(5) Uani 1 1 d . . . H8 H -0.1970 0.1855 0.4036 0.022 Uiso 1 1 calc R . . C9 C -0.1069(2) 0.23713(10) 0.2781(4) 0.0187(5) Uani 1 1 d . . . H9 H -0.1630 0.2618 0.2806 0.022 Uiso 1 1 calc R . . C10 C -0.0013(2) 0.24577(9) 0.2019(3) 0.0142(5) Uani 1 1 d . . . H10 H 0.0135 0.2768 0.1564 0.017 Uiso 1 1 calc R . . C11 C 0.4542(2) 0.04244(9) 0.2477(3) 0.0122(5) Uani 1 1 d . . . C12 C 0.4442(2) -0.00691(9) 0.2012(3) 0.0159(5) Uani 1 1 d . . . H12 H 0.3801 -0.0179 0.1368 0.019 Uiso 1 1 calc R . . C13 C 0.5312(2) -0.03949(10) 0.2523(3) 0.0193(6) Uani 1 1 d . . . H13 H 0.5272 -0.0726 0.2216 0.023 Uiso 1 1 calc R . . C14 C 0.6235(2) -0.02178(10) 0.3494(3) 0.0198(6) Uani 1 1 d . . . H14 H 0.6814 -0.0430 0.3900 0.024 Uiso 1 1 calc R . . C15 C 0.6289(2) 0.02821(10) 0.3859(3) 0.0190(5) Uani 1 1 d . . . H15 H 0.6931 0.0400 0.4481 0.023 Uiso 1 1 calc R . . C16 C -0.1299(2) 0.03316(11) 0.0919(4) 0.0223(6) Uani 1 1 d . . . H16 H -0.1907 0.0440 0.0206 0.027 Uiso 1 1 calc R . . C17 C -0.1367(3) -0.01364(11) 0.1608(4) 0.0244(6) Uani 1 1 d . . . H17 H -0.2002 -0.0338 0.1346 0.029 Uiso 1 1 calc R . . C18 C -0.0488(3) -0.03017(10) 0.2682(4) 0.0231(6) Uani 1 1 d . . . H18 H -0.0524 -0.0613 0.3182 0.028 Uiso 1 1 calc R . . C19 C 0.0455(2) 0.00045(9) 0.3006(3) 0.0172(5) Uani 1 1 d . . . H19 H 0.1070 -0.0098 0.3718 0.021 Uiso 1 1 calc R . . C20 C 0.0464(2) 0.04649(9) 0.2248(3) 0.0125(5) Uani 1 1 d . . . C21 C 0.3545(2) 0.12682(9) 0.1782(3) 0.0103(4) Uani 1 1 d . . . C22 C 0.3538(2) 0.07608(9) 0.2181(3) 0.0107(4) Uani 1 1 d . . . C23 C 0.1519(2) 0.07786(9) 0.2360(3) 0.0114(5) Uani 1 1 d . . . C24 C 0.1538(2) 0.12974(9) 0.2320(3) 0.0102(4) Uani 1 1 d . . . N1 N 0.41168(18) 0.20578(7) 0.0774(3) 0.0117(4) Uani 1 1 d . . . N2 N 0.07972(17) 0.21058(7) 0.1924(2) 0.0105(4) Uani 1 1 d . . . N3 N 0.54630(18) 0.06050(8) 0.3360(3) 0.0146(4) Uani 1 1 d . . . N4 N -0.04050(19) 0.06363(8) 0.1223(3) 0.0160(4) Uani 1 1 d . . . N5 N 0.25376(17) 0.15115(7) 0.1928(2) 0.0091(4) Uani 1 1 d . . . N6 N 0.25156(18) 0.05317(7) 0.2361(3) 0.0116(4) Uani 1 1 d . . . O1 O 0.18718(15) 0.18024(7) -0.1472(2) 0.0153(4) Uani 1 1 d . . . O2 O 0.20278(17) 0.11797(6) -0.4136(2) 0.0176(4) Uani 1 1 d . . . O1W O -0.0478(2) 0.14507(8) -0.1192(3) 0.0241(5) Uani 1 1 d . . . O3 O 0.39420(16) 0.16066(7) -0.2841(2) 0.0205(4) Uani 1 1 d . . . O2W O 0.59736(19) 0.14988(8) -0.4708(3) 0.0239(5) Uani 1 1 d . . . O4 O 0.23515(15) 0.21487(6) -0.4681(2) 0.0137(3) Uani 1 1 d . . . O3W O 0.2086(3) -0.09737(10) 0.3362(5) 0.0564(9) Uani 1 1 d . . . H1WA H -0.040(3) 0.1225(15) -0.045(5) 0.045(12) Uiso 1 1 d . . . H2WA H 0.581(3) 0.1279(15) -0.529(5) 0.040(12) Uiso 1 1 d . . . H2WB H 0.541(4) 0.1523(15) -0.418(5) 0.048(13) Uiso 1 1 d . . . H1WB H 0.013(3) 0.1531(15) -0.136(5) 0.040(12) Uiso 1 1 d . . . H3WA H 0.261(4) -0.1150(16) 0.358(5) 0.052(13) Uiso 1 1 d . . . H3WB H 0.167(4) -0.1131(17) 0.286(6) 0.060(15) 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 Cr1 0.01232(19) 0.00802(16) 0.01034(18) -0.00083(15) -0.00131(14) 0.00049(15) Cu1 0.00919(14) 0.00709(13) 0.01263(14) 0.00045(11) -0.00009(10) -0.00002(11) C1 0.0181(13) 0.0111(11) 0.0210(13) 0.0016(10) 0.0021(10) -0.0031(10) C2 0.0165(13) 0.0195(13) 0.0276(15) 0.0018(11) 0.0072(11) -0.0056(11) C3 0.0101(12) 0.0244(14) 0.0248(14) 0.0031(12) 0.0023(10) -0.0006(10) C4 0.0111(12) 0.0163(12) 0.0190(12) 0.0027(10) 0.0009(9) 0.0006(10) C5 0.0111(11) 0.0111(11) 0.0108(11) 0.0006(9) -0.0012(9) -0.0011(9) C6 0.0121(11) 0.0112(11) 0.0108(11) -0.0024(9) -0.0026(9) -0.0009(9) C7 0.0129(12) 0.0159(11) 0.0144(11) -0.0009(10) 0.0014(9) 0.0003(9) C8 0.0144(13) 0.0199(13) 0.0206(13) -0.0039(11) 0.0041(10) 0.0002(10) C9 0.0126(12) 0.0179(12) 0.0256(14) -0.0054(11) 0.0001(10) 0.0034(10) C10 0.0133(12) 0.0119(11) 0.0173(12) -0.0012(10) -0.0028(10) 0.0016(9) C11 0.0129(12) 0.0122(11) 0.0116(11) 0.0021(9) 0.0015(9) 0.0019(9) C12 0.0152(13) 0.0141(12) 0.0183(13) 0.0006(10) 0.0012(10) 0.0010(10) C13 0.0235(14) 0.0118(11) 0.0229(13) 0.0036(11) 0.0075(11) 0.0068(10) C14 0.0155(13) 0.0243(13) 0.0199(13) 0.0083(11) 0.0056(10) 0.0114(11) C15 0.0130(12) 0.0256(14) 0.0184(13) 0.0033(11) 0.0000(10) 0.0045(11) C16 0.0127(13) 0.0320(15) 0.0222(14) -0.0098(12) 0.0013(10) -0.0031(11) C17 0.0210(15) 0.0283(15) 0.0244(14) -0.0133(12) 0.0112(12) -0.0128(12) C18 0.0284(16) 0.0157(13) 0.0260(15) -0.0044(11) 0.0134(12) -0.0073(11) C19 0.0181(13) 0.0143(12) 0.0194(13) -0.0007(10) 0.0050(10) -0.0017(10) C20 0.0122(12) 0.0129(11) 0.0124(11) -0.0030(9) 0.0030(9) -0.0020(9) C21 0.0101(11) 0.0115(10) 0.0091(10) -0.0003(9) -0.0018(8) 0.0003(9) C22 0.0112(11) 0.0118(11) 0.0088(10) -0.0001(9) -0.0018(8) 0.0011(9) C23 0.0128(12) 0.0125(11) 0.0088(11) 0.0009(9) -0.0003(9) -0.0006(9) C24 0.0100(11) 0.0116(11) 0.0091(10) 0.0014(9) -0.0009(8) -0.0009(9) N1 0.0115(10) 0.0101(9) 0.0135(10) 0.0001(8) -0.0012(8) -0.0010(8) N2 0.0101(10) 0.0104(9) 0.0108(9) -0.0011(8) -0.0022(7) 0.0006(8) N3 0.0107(10) 0.0173(10) 0.0157(10) 0.0006(9) -0.0002(8) 0.0014(8) N4 0.0118(10) 0.0191(11) 0.0172(11) -0.0021(9) 0.0004(8) -0.0013(8) N5 0.0097(9) 0.0095(8) 0.0080(9) 0.0003(7) -0.0004(7) 0.0004(8) N6 0.0120(10) 0.0097(9) 0.0131(10) 0.0001(8) -0.0011(8) 0.0006(8) O1 0.0162(9) 0.0175(9) 0.0123(8) -0.0028(7) 0.0002(7) 0.0006(7) O2 0.0277(11) 0.0089(8) 0.0161(9) -0.0005(7) -0.0023(8) -0.0030(7) O1W 0.0213(12) 0.0222(11) 0.0281(11) 0.0063(9) -0.0098(9) -0.0037(9) O3 0.0155(9) 0.0246(10) 0.0213(9) 0.0002(8) -0.0018(7) 0.0060(8) O2W 0.0193(11) 0.0207(10) 0.0318(12) -0.0053(9) 0.0027(9) -0.0006(9) O4 0.0176(9) 0.0100(8) 0.0133(8) -0.0005(7) -0.0010(7) -0.0006(7) O3W 0.0464(18) 0.0281(13) 0.092(2) -0.0189(15) -0.0454(17) 0.0115(13) _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 Cr1 O2 1.6183(18) . ? Cr1 O3 1.6302(19) . ? Cr1 O1 1.6604(17) . ? Cr1 O4 1.7056(17) . ? Cu1 O4 1.8923(17) 4_566 ? Cu1 N5 1.9546(19) . ? Cu1 N1 2.007(2) . ? Cu1 N2 2.016(2) . ? Cu1 O1 2.2873(17) . ? C1 N1 1.333(3) . ? C1 C2 1.382(4) . ? C2 C3 1.384(4) . ? C3 C4 1.390(4) . ? C4 C5 1.388(3) . ? C5 N1 1.355(3) . ? C5 C21 1.491(3) . ? C6 N2 1.349(3) . ? C6 C7 1.385(3) . ? C6 C24 1.483(3) . ? C7 C8 1.389(3) . ? C8 C9 1.376(4) . ? C9 C10 1.388(4) . ? C10 N2 1.337(3) . ? C11 N3 1.341(3) . ? C11 C12 1.389(3) . ? C11 C22 1.486(3) . ? C12 C13 1.386(4) . ? C13 C14 1.375(4) . ? C14 C15 1.385(4) . ? C15 N3 1.342(3) . ? C16 N4 1.336(3) . ? C16 C17 1.380(4) . ? C17 C18 1.373(4) . ? C18 C19 1.384(4) . ? C19 C20 1.380(3) . ? C20 N4 1.347(3) . ? C20 C23 1.484(3) . ? C21 N5 1.342(3) . ? C21 C22 1.409(3) . ? C22 N6 1.341(3) . ? C23 N6 1.328(3) . ? C23 C24 1.406(3) . ? C24 N5 1.332(3) . ? O4 Cu1 1.8923(17) 4_565 ? 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 O2 Cr1 O3 110.19(10) . . ? O2 Cr1 O1 110.11(9) . . ? O3 Cr1 O1 109.80(9) . . ? O2 Cr1 O4 107.83(9) . . ? O3 Cr1 O4 109.59(9) . . ? O1 Cr1 O4 109.29(9) . . ? O4 Cu1 N5 175.93(8) 4_566 . ? O4 Cu1 N1 99.34(8) 4_566 . ? N5 Cu1 N1 79.36(8) . . ? O4 Cu1 N2 100.05(8) 4_566 . ? N5 Cu1 N2 80.69(8) . . ? N1 Cu1 N2 158.71(8) . . ? O4 Cu1 O1 99.83(7) 4_566 . ? N5 Cu1 O1 84.15(7) . . ? N1 Cu1 O1 94.54(7) . . ? N2 Cu1 O1 90.75(7) . . ? N1 C1 C2 122.3(2) . . ? C1 C2 C3 118.7(2) . . ? C2 C3 C4 119.3(2) . . ? C5 C4 C3 119.1(2) . . ? N1 C5 C4 120.8(2) . . ? N1 C5 C21 113.3(2) . . ? C4 C5 C21 125.9(2) . . ? N2 C6 C7 121.9(2) . . ? N2 C6 C24 113.3(2) . . ? C7 C6 C24 124.7(2) . . ? C6 C7 C8 118.4(2) . . ? C9 C8 C7 119.5(2) . . ? C8 C9 C10 119.2(2) . . ? N2 C10 C9 121.6(2) . . ? N3 C11 C12 123.0(2) . . ? N3 C11 C22 117.2(2) . . ? C12 C11 C22 119.4(2) . . ? C13 C12 C11 118.9(2) . . ? C14 C13 C12 118.6(2) . . ? C13 C14 C15 119.0(2) . . ? N3 C15 C14 123.4(3) . . ? N4 C16 C17 123.4(3) . . ? C18 C17 C16 119.3(3) . . ? C17 C18 C19 118.6(3) . . ? C20 C19 C18 118.6(3) . . ? N4 C20 C19 123.5(2) . . ? N4 C20 C23 115.6(2) . . ? C19 C20 C23 120.5(2) . . ? N5 C21 C22 116.7(2) . . ? N5 C21 C5 112.0(2) . . ? C22 C21 C5 131.1(2) . . ? N6 C22 C21 119.0(2) . . ? N6 C22 C11 112.4(2) . . ? C21 C22 C11 128.5(2) . . ? N6 C23 C24 119.3(2) . . ? N6 C23 C20 114.7(2) . . ? C24 C23 C20 125.8(2) . . ? N5 C24 C23 117.0(2) . . ? N5 C24 C6 113.4(2) . . ? C23 C24 C6 129.5(2) . . ? C1 N1 C5 119.7(2) . . ? C1 N1 Cu1 123.88(17) . . ? C5 N1 Cu1 115.71(16) . . ? C10 N2 C6 119.3(2) . . ? C10 N2 Cu1 126.59(17) . . ? C6 N2 Cu1 113.95(16) . . ? C11 N3 C15 117.1(2) . . ? C16 N4 C20 116.7(2) . . ? C24 N5 C21 124.1(2) . . ? C24 N5 Cu1 115.66(16) . . ? C21 N5 Cu1 118.84(16) . . ? C23 N6 C22 121.8(2) . . ? Cr1 O1 Cu1 133.61(10) . . ? Cr1 O4 Cu1 121.41(10) . 4_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.574 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.101 # Attachment 'Compound3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 738680' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H94 Cu4 F12 Mo2 N24 O31 S4' _chemical_formula_weight 2930.27 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0125(3) _cell_length_b 17.3925(3) _cell_length_c 22.2506(5) _cell_angle_alpha 79.4340(10) _cell_angle_beta 85.6220(10) _cell_angle_gamma 89.8420(10) _cell_volume 5694.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 6.20 _cell_measurement_theta_max 20.17 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2964 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8057 _exptl_absorpt_correction_T_max 0.9778 _exptl_absorpt_process_details ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123321 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.0986 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.60 _reflns_number_total 28233 _reflns_number_gt 20099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+26.9562P] 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 28233 _refine_ls_number_parameters 1594 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1254 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.1860 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.005 _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 C1 C 0.6275(5) 0.4361(5) 0.5070(4) 0.048(2) Uani 1 1 d . . . C2 C 0.3243(5) 0.1997(4) 0.6235(3) 0.0350(17) Uani 1 1 d . . . C3 C 0.1178(8) 0.2934(6) 0.8912(4) 0.075(4) Uani 1 1 d . . . C4 C 0.8283(10) 0.0554(11) 0.9846(5) 0.41(3) Uani 1 1 d D . . F1 F 0.6357(4) 0.4943(4) 0.4599(3) 0.0820(19) Uani 1 1 d . . . F2 F 0.5851(4) 0.4693(4) 0.5511(3) 0.088(2) Uani 1 1 d . . . F3 F 0.5777(5) 0.3819(4) 0.4987(5) 0.139(4) Uani 1 1 d . . . F4 F 0.2556(3) 0.1616(3) 0.6589(2) 0.0490(12) Uani 1 1 d . . . F5 F 0.3729(3) 0.2321(3) 0.6564(2) 0.0450(11) Uani 1 1 d . . . F6 F 0.2871(3) 0.2564(3) 0.5833(2) 0.0475(11) Uani 1 1 d . . . F7 F 0.0413(5) 0.2980(5) 0.8633(3) 0.103(3) Uani 1 1 d . . . F8 F 0.1168(8) 0.2343(4) 0.9354(3) 0.157(5) Uani 1 1 d . . . F9 F 0.1844(5) 0.2839(3) 0.8504(3) 0.087(2) Uani 1 1 d . . . F10 F 0.7785(7) 0.0430(4) 0.9347(3) 0.152(4) Uani 1 1 d D . . F11 F 0.9265(7) 0.0488(12) 0.9676(4) 0.319(12) Uani 1 1 d D . . F12 F 0.8067(6) -0.0141(3) 1.0302(3) 0.118(3) Uani 1 1 d D . . S1 S 0.73486(13) 0.40107(11) 0.53097(9) 0.0355(4) Uani 1 1 d . . . S2 S 0.38663(12) 0.13119(12) 0.58168(8) 0.0351(4) Uani 1 1 d . . . S3 S 0.13413(13) 0.38589(11) 0.91872(9) 0.0361(4) Uani 1 1 d . . . S4 S 0.84389(18) 0.13299(13) 1.00005(12) 0.0573(6) Uani 1 1 d D . . O9 O 0.7844(4) 0.4680(4) 0.5390(4) 0.086(3) Uani 1 1 d . . . O10 O 0.7167(4) 0.3458(4) 0.5857(3) 0.0674(19) Uani 1 1 d . . . O11 O 0.7699(4) 0.3669(4) 0.4804(3) 0.0581(17) Uani 1 1 d . . . O12 O 0.4568(4) 0.1843(4) 0.5469(3) 0.0514(15) Uani 1 1 d . . . O13 O 0.4148(5) 0.0729(4) 0.6289(3) 0.0626(19) Uani 1 1 d . . . O14 O 0.3210(4) 0.1084(3) 0.5455(3) 0.0474(14) Uani 1 1 d . . . O15 O 0.0590(5) 0.3890(5) 0.9623(3) 0.084(2) Uani 1 1 d . . . O16 O 0.2172(4) 0.3739(3) 0.9457(3) 0.0568(17) Uani 1 1 d . . . O17 O 0.1356(4) 0.4441(3) 0.8646(3) 0.0504(15) Uani 1 1 d . . . O18 O 0.7311(7) 0.1251(9) 1.0159(5) 0.250(10) Uani 1 1 d D . . O19 O 0.8763(5) 0.1269(4) 1.0580(3) 0.078(2) Uani 1 1 d D . . O20 O 0.8529(9) 0.1914(4) 0.9507(3) 0.153(5) Uani 1 1 d D . . O2W O 0.3271(3) 0.4759(3) 0.2483(2) 0.0319(11) Uani 1 1 d . . . O3W O 0.1540(3) 0.0457(2) 0.26526(19) 0.0251(10) Uani 1 1 d . . . O5W O 0.3353(4) 0.7336(3) 0.2147(3) 0.0515(15) Uani 1 1 d . . . O6W O 0.2157(4) 0.9104(4) 0.2322(4) 0.077(2) Uani 1 1 d . . . O7W O 0.3905(4) 0.8681(3) 0.2639(3) 0.0472(14) Uani 1 1 d . . . O8W O 0.5919(4) 0.2252(3) 0.6222(3) 0.0538(15) Uani 1 1 d . . . O9W O 0.7342(4) 0.3968(3) 0.7040(3) 0.0464(14) Uani 1 1 d . . . O10W O 0.8961(4) 0.3555(4) 0.7569(3) 0.0588(17) Uani 1 1 d . . . O11W O 0.8284(4) 0.2179(3) 0.8275(3) 0.0460(14) Uani 1 1 d . . . C101 C 0.3187(4) 0.5273(3) -0.0621(3) 0.0186(12) Uani 1 1 d . . . C102 C 0.2718(4) 0.5471(3) -0.0057(3) 0.0185(12) Uani 1 1 d . . . C103 C 0.1953(4) 0.5907(4) -0.0032(3) 0.0269(15) Uani 1 1 d . . . H103 H 0.1669 0.6088 -0.0387 0.032 Uiso 1 1 calc R . . C104 C 0.1611(5) 0.6075(4) 0.0525(3) 0.0282(15) Uani 1 1 d . . . H104 H 0.1102 0.6377 0.0547 0.034 Uiso 1 1 calc R . . C105 C 0.2032(4) 0.5789(4) 0.1047(3) 0.0257(14) Uani 1 1 d . . . H105 H 0.1827 0.5911 0.1423 0.031 Uiso 1 1 calc R . . C106 C 0.2772(4) 0.5312(3) 0.1002(3) 0.0206(13) Uani 1 1 d . . . H106 H 0.3043 0.5099 0.1356 0.025 Uiso 1 1 calc R . . C107 C 0.3075(4) 0.5566(3) -0.1238(3) 0.0179(12) Uani 1 1 d . . . C108 C 0.2546(4) 0.6271(3) -0.1485(3) 0.0198(13) Uani 1 1 d . . . C109 C 0.2040(4) 0.6261(4) -0.1983(3) 0.0265(14) Uani 1 1 d . . . H109 H 0.2014 0.5819 -0.2162 0.032 Uiso 1 1 calc R . . C110 C 0.1580(5) 0.6926(4) -0.2203(3) 0.0333(17) Uani 1 1 d . . . H110 H 0.1227 0.6938 -0.2530 0.040 Uiso 1 1 calc R . . C111 C 0.1646(5) 0.7564(4) -0.1936(3) 0.0345(18) Uani 1 1 d . . . H111 H 0.1339 0.8019 -0.2079 0.041 Uiso 1 1 calc R . . C112 C 0.2174(5) 0.7529(4) -0.1450(3) 0.0329(17) Uani 1 1 d . . . H112 H 0.2217 0.7971 -0.1274 0.040 Uiso 1 1 calc R . . C113 C 0.4011(4) 0.4602(3) -0.1539(3) 0.0179(12) Uani 1 1 d . . . C114 C 0.4318(4) 0.4260(4) -0.2080(3) 0.0209(13) Uani 1 1 d . . . C115 C 0.4530(4) 0.4760(4) -0.2632(3) 0.0259(14) Uani 1 1 d . . . H115 H 0.4484 0.5299 -0.2663 0.031 Uiso 1 1 calc R . . C116 C 0.4815(5) 0.4436(4) -0.3140(3) 0.0329(16) Uani 1 1 d . . . H116 H 0.4974 0.4754 -0.3516 0.040 Uiso 1 1 calc R . . C117 C 0.4855(5) 0.3631(4) -0.3071(3) 0.0333(16) Uani 1 1 d . . . H117 H 0.5045 0.3398 -0.3402 0.040 Uiso 1 1 calc R . . C118 C 0.4608(4) 0.3178(4) -0.2505(3) 0.0288(15) Uani 1 1 d . . . H118 H 0.4630 0.2637 -0.2467 0.035 Uiso 1 1 calc R . . C119 C 0.4262(4) 0.4391(3) -0.0930(3) 0.0171(12) Uani 1 1 d . . . C120 C 0.4960(4) 0.3839(3) -0.0672(3) 0.0171(12) Uani 1 1 d . . . C121 C 0.5573(4) 0.3452(4) -0.1002(3) 0.0231(13) Uani 1 1 d . . . H121 H 0.5579 0.3527 -0.1427 0.028 Uiso 1 1 calc R . . C122 C 0.6176(4) 0.2952(4) -0.0696(3) 0.0268(15) Uani 1 1 d . . . H122 H 0.6592 0.2691 -0.0914 0.032 Uiso 1 1 calc R . . C123 C 0.6158(5) 0.2843(4) -0.0068(3) 0.0296(15) Uani 1 1 d . . . H123 H 0.6553 0.2502 0.0145 0.036 Uiso 1 1 calc R . . C124 C 0.5542(4) 0.3249(4) 0.0243(3) 0.0275(15) Uani 1 1 d . . . H124 H 0.5533 0.3180 0.0668 0.033 Uiso 1 1 calc R . . C201 C 0.1544(4) 0.3803(3) 0.3868(3) 0.0160(12) Uani 1 1 d . . . C202 C 0.2466(4) 0.3586(3) 0.4027(3) 0.0161(12) Uani 1 1 d . . . C203 C 0.2821(4) 0.3660(3) 0.4572(3) 0.0206(13) Uani 1 1 d . . . H203 H 0.2468 0.3832 0.4882 0.025 Uiso 1 1 calc R . . C204 C 0.3704(4) 0.3476(4) 0.4645(3) 0.0227(13) Uani 1 1 d . . . H204 H 0.3946 0.3509 0.5012 0.027 Uiso 1 1 calc R . . C205 C 0.4228(4) 0.3243(4) 0.4177(3) 0.0271(15) Uani 1 1 d . . . H205 H 0.4826 0.3119 0.4222 0.032 Uiso 1 1 calc R . . C206 C 0.3840(4) 0.3196(3) 0.3635(3) 0.0223(13) Uani 1 1 d . . . H206 H 0.4189 0.3036 0.3318 0.027 Uiso 1 1 calc R . . C207 C 0.0768(4) 0.3903(3) 0.4247(3) 0.0161(12) Uani 1 1 d . . . C208 C 0.0592(4) 0.3618(3) 0.4918(3) 0.0178(12) Uani 1 1 d . . . C209 C -0.0052(4) 0.3973(3) 0.5251(3) 0.0215(13) Uani 1 1 d . . . H209 H -0.0377 0.4388 0.5054 0.026 Uiso 1 1 calc R . . C210 C -0.0211(5) 0.3709(4) 0.5877(3) 0.0260(14) Uani 1 1 d . . . H210 H -0.0626 0.3953 0.6109 0.031 Uiso 1 1 calc R . . C211 C 0.0262(4) 0.3078(4) 0.6143(3) 0.0265(14) Uani 1 1 d . . . H211 H 0.0175 0.2886 0.6561 0.032 Uiso 1 1 calc R . . C212 C 0.0865(4) 0.2733(4) 0.5784(3) 0.0233(13) Uani 1 1 d . . . H212 H 0.1165 0.2293 0.5968 0.028 Uiso 1 1 calc R . . C213 C 0.0045(4) 0.4474(3) 0.3378(3) 0.0189(12) Uani 1 1 d . . . C214 C -0.0759(4) 0.4933(4) 0.3190(3) 0.0194(12) Uani 1 1 d . . . C215 C -0.1598(4) 0.4634(4) 0.3439(3) 0.0335(16) Uani 1 1 d . . . H215 H -0.1658 0.4149 0.3698 0.040 Uiso 1 1 calc R . . C216 C -0.2336(5) 0.5086(5) 0.3287(4) 0.046(2) Uani 1 1 d . . . H216 H -0.2908 0.4904 0.3433 0.055 Uiso 1 1 calc R . . C217 C -0.2212(5) 0.5804(5) 0.2916(3) 0.0368(18) Uani 1 1 d . . . H217 H -0.2699 0.6116 0.2807 0.044 Uiso 1 1 calc R . . C218 C -0.1358(5) 0.6060(4) 0.2709(3) 0.0294(15) Uani 1 1 d . . . H218 H -0.1282 0.6558 0.2472 0.035 Uiso 1 1 calc R . . C219 C 0.0744(4) 0.4238(3) 0.2996(3) 0.0177(12) Uani 1 1 d . . . C220 C 0.0780(4) 0.4219(3) 0.2327(3) 0.0176(12) Uani 1 1 d . . . C221 C 0.0128(4) 0.4485(4) 0.1936(3) 0.0209(13) Uani 1 1 d . . . H221 H -0.0378 0.4731 0.2075 0.025 Uiso 1 1 calc R . . C222 C 0.0240(4) 0.4378(4) 0.1332(3) 0.0246(14) Uani 1 1 d . . . H222 H -0.0198 0.4543 0.1064 0.030 Uiso 1 1 calc R . . C223 C 0.0999(4) 0.4030(4) 0.1129(3) 0.0231(13) Uani 1 1 d . . . H223 H 0.1079 0.3952 0.0726 0.028 Uiso 1 1 calc R . . C224 C 0.1638(4) 0.3801(3) 0.1535(3) 0.0191(12) Uani 1 1 d . . . H224 H 0.2162 0.3581 0.1395 0.023 Uiso 1 1 calc R . . C301 C 0.3116(4) 0.1314(3) 0.1310(3) 0.0179(12) Uani 1 1 d . . . C302 C 0.2194(4) 0.1565(3) 0.1188(3) 0.0190(12) Uani 1 1 d . . . C303 C 0.1763(4) 0.1442(4) 0.0687(3) 0.0281(15) Uani 1 1 d . . . H303 H 0.2070 0.1231 0.0378 0.034 Uiso 1 1 calc R . . C304 C 0.0878(5) 0.1633(4) 0.0647(3) 0.0350(17) Uani 1 1 d . . . H304 H 0.0571 0.1529 0.0322 0.042 Uiso 1 1 calc R . . C305 C 0.0454(4) 0.1982(4) 0.1100(3) 0.0290(15) Uani 1 1 d . . . H305 H -0.0136 0.2142 0.1072 0.035 Uiso 1 1 calc R . . C306 C 0.0912(4) 0.2090(4) 0.1593(3) 0.0225(13) Uani 1 1 d . . . H306 H 0.0621 0.2318 0.1899 0.027 Uiso 1 1 calc R . . C307 C 0.3811(4) 0.1134(4) 0.0905(3) 0.0204(13) Uani 1 1 d . . . C308 C 0.3822(4) 0.1317(4) 0.0224(3) 0.0217(13) Uani 1 1 d . . . C309 C 0.4102(6) 0.0766(4) -0.0116(3) 0.041(2) Uani 1 1 d . . . H309 H 0.4253 0.0266 0.0072 0.049 Uiso 1 1 calc R . . C310 C 0.4151(7) 0.0984(5) -0.0755(3) 0.054(3) Uani 1 1 d . . . H310 H 0.4352 0.0632 -0.1002 0.065 Uiso 1 1 calc R . . C311 C 0.3899(6) 0.1721(4) -0.1010(3) 0.041(2) Uani 1 1 d . . . H311 H 0.3910 0.1873 -0.1434 0.049 Uiso 1 1 calc R . . C312 C 0.3632(4) 0.2229(4) -0.0634(3) 0.0261(14) Uani 1 1 d . . . H312 H 0.3473 0.2731 -0.0812 0.031 Uiso 1 1 calc R . . C313 C 0.4677(4) 0.0702(3) 0.1718(3) 0.0157(12) Uani 1 1 d . . . C314 C 0.5553(4) 0.0318(3) 0.1863(3) 0.0179(12) Uani 1 1 d . . . C315 C 0.6342(4) 0.0675(4) 0.1603(3) 0.0292(15) Uani 1 1 d . . . H315 H 0.6340 0.1172 0.1363 0.035 Uiso 1 1 calc R . . C316 C 0.7134(4) 0.0290(4) 0.1701(3) 0.0319(16) Uani 1 1 d . . . H316 H 0.7677 0.0523 0.1537 0.038 Uiso 1 1 calc R . . C317 C 0.7096(4) -0.0456(4) 0.2052(3) 0.0294(15) Uani 1 1 d . . . H317 H 0.7618 -0.0737 0.2122 0.035 Uiso 1 1 calc R . . C318 C 0.6291(4) -0.0776(4) 0.2295(3) 0.0258(14) Uani 1 1 d . . . H318 H 0.6282 -0.1275 0.2534 0.031 Uiso 1 1 calc R . . C319 C 0.4036(4) 0.0957(3) 0.2122(3) 0.0168(12) Uani 1 1 d . . . C320 C 0.4086(4) 0.1007(3) 0.2783(3) 0.0175(12) Uani 1 1 d . . . C321 C 0.4778(4) 0.0742(4) 0.3134(3) 0.0215(13) Uani 1 1 d . . . H321 H 0.5253 0.0480 0.2973 0.026 Uiso 1 1 calc R . . C322 C 0.4758(4) 0.0870(4) 0.3738(3) 0.0237(14) Uani 1 1 d . . . H322 H 0.5230 0.0712 0.3978 0.028 Uiso 1 1 calc R . . C323 C 0.4030(4) 0.1235(4) 0.3969(3) 0.0218(13) Uani 1 1 d . . . H323 H 0.4001 0.1330 0.4368 0.026 Uiso 1 1 calc R . . C324 C 0.3337(4) 0.1461(3) 0.3596(3) 0.0188(12) Uani 1 1 d . . . H324 H 0.2836 0.1693 0.3756 0.023 Uiso 1 1 calc R . . C401 C 0.1820(4) -0.0284(3) 0.5704(3) 0.0152(11) Uani 1 1 d . . . C402 C 0.2298(4) -0.0376(3) 0.5109(3) 0.0163(12) Uani 1 1 d . . . C403 C 0.3108(4) -0.0744(3) 0.5040(3) 0.0209(13) Uani 1 1 d . . . H403 H 0.3414 -0.0951 0.5380 0.025 Uiso 1 1 calc R . . C404 C 0.3450(4) -0.0797(4) 0.4454(3) 0.0260(14) Uani 1 1 d . . . H404 H 0.3988 -0.1049 0.4398 0.031 Uiso 1 1 calc R . . C405 C 0.2995(4) -0.0476(4) 0.3954(3) 0.0232(13) Uani 1 1 d . . . H405 H 0.3206 -0.0532 0.3560 0.028 Uiso 1 1 calc R . . C406 C 0.2225(4) -0.0072(3) 0.4048(3) 0.0174(12) Uani 1 1 d . . . H406 H 0.1930 0.0166 0.3711 0.021 Uiso 1 1 calc R . . C407 C 0.1965(4) -0.0654(3) 0.6302(3) 0.0185(12) Uani 1 1 d . . . C408 C 0.2500(4) -0.1373(3) 0.6463(3) 0.0194(12) Uani 1 1 d . . . C409 C 0.3054(4) -0.1456(4) 0.6941(3) 0.0244(14) Uani 1 1 d . . . H409 H 0.3104 -0.1059 0.7166 0.029 Uiso 1 1 calc R . . C410 C 0.3533(4) -0.2143(4) 0.7076(3) 0.0300(16) Uani 1 1 d . . . H410 H 0.3911 -0.2217 0.7394 0.036 Uiso 1 1 calc R . . C411 C 0.3432(5) -0.2712(4) 0.6729(3) 0.0330(17) Uani 1 1 d . . . H411 H 0.3740 -0.3180 0.6808 0.040 Uiso 1 1 calc R . . C412 C 0.2870(5) -0.2578(4) 0.6266(3) 0.0325(16) Uani 1 1 d . . . H412 H 0.2810 -0.2969 0.6037 0.039 Uiso 1 1 calc R . . C413 C 0.0987(4) 0.0215(3) 0.6699(3) 0.0183(12) Uani 1 1 d . . . C414 C 0.0698(4) 0.0505(3) 0.7265(3) 0.0180(12) Uani 1 1 d . . . C415 C 0.0574(4) -0.0013(4) 0.7817(3) 0.0225(13) Uani 1 1 d . . . H415 H 0.0648 -0.0548 0.7836 0.027 Uiso 1 1 calc R . . C416 C 0.0337(4) 0.0289(4) 0.8343(3) 0.0292(15) Uani 1 1 d . . . H416 H 0.0239 -0.0043 0.8720 0.035 Uiso 1 1 calc R . . C417 C 0.0249(5) 0.1085(4) 0.8300(3) 0.0312(16) Uani 1 1 d . . . H417 H 0.0093 0.1300 0.8646 0.037 Uiso 1 1 calc R . . C418 C 0.0398(4) 0.1556(4) 0.7731(3) 0.0285(15) Uani 1 1 d . . . H418 H 0.0339 0.2093 0.7705 0.034 Uiso 1 1 calc R . . C419 C 0.0704(4) 0.0478(3) 0.6108(3) 0.0148(11) Uani 1 1 d . . . C420 C -0.0060(4) 0.0993(3) 0.5912(3) 0.0172(12) Uani 1 1 d . . . C421 C -0.0728(4) 0.1242(3) 0.6288(3) 0.0201(13) Uani 1 1 d . . . H421 H -0.0748 0.1070 0.6710 0.024 Uiso 1 1 calc R . . C422 C -0.1367(4) 0.1746(4) 0.6037(3) 0.0229(13) Uani 1 1 d . . . H422 H -0.1812 0.1926 0.6289 0.027 Uiso 1 1 calc R . . C423 C -0.1342(4) 0.1983(3) 0.5402(3) 0.0233(14) Uani 1 1 d . . . H423 H -0.1766 0.2325 0.5225 0.028 Uiso 1 1 calc R . . C424 C -0.0679(4) 0.1703(3) 0.5043(3) 0.0209(13) Uani 1 1 d . . . H424 H -0.0662 0.1858 0.4620 0.025 Uiso 1 1 calc R . . Cu1 Cu 0.40019(5) 0.43132(4) 0.03646(3) 0.01732(16) Uani 1 1 d . . . Cu2 Cu 0.24096(5) 0.35303(4) 0.27484(3) 0.01769(16) Uani 1 1 d . . . Cu3 Cu 0.24184(5) 0.17083(4) 0.24310(3) 0.01731(16) Uani 1 1 d . . . Cu4 Cu 0.09291(5) 0.07457(4) 0.48039(3) 0.01625(15) Uani 1 1 d . . . Mo1 Mo 0.43249(3) 0.32940(3) 0.18495(2) 0.01711(12) Uani 1 1 d . . . Mo2 Mo 0.05249(3) 0.18306(3) 0.33457(2) 0.01586(11) Uani 1 1 d . . . N1 N 0.3103(3) 0.5152(3) 0.0466(2) 0.0179(10) Uani 1 1 d . . . N2 N 0.3811(3) 0.4716(3) -0.0500(2) 0.0181(10) Uani 1 1 d . . . N3 N 0.4955(3) 0.3741(3) -0.0049(2) 0.0188(10) Uani 1 1 d . . . N4 N 0.2627(4) 0.6891(3) -0.1220(2) 0.0270(12) Uani 1 1 d . . . N5 N 0.3455(3) 0.5204(3) -0.1673(2) 0.0192(11) Uani 1 1 d . . . N6 N 0.4342(4) 0.3475(3) -0.2011(2) 0.0250(12) Uani 1 1 d . . . N7 N 0.1536(3) 0.3880(3) 0.2121(2) 0.0173(10) Uani 1 1 d . . . N8 N 0.1466(3) 0.3944(3) 0.3263(2) 0.0157(10) Uani 1 1 d . . . N9 N 0.2982(3) 0.3373(3) 0.3555(2) 0.0186(10) Uani 1 1 d . . . N10 N -0.0629(3) 0.5628(3) 0.2829(2) 0.0238(12) Uani 1 1 d . . . N11 N 0.0071(3) 0.4271(3) 0.3986(2) 0.0167(10) Uani 1 1 d . . . N12 N 0.1048(3) 0.2996(3) 0.5178(2) 0.0214(11) Uani 1 1 d . . . N13 N 0.1766(3) 0.1875(3) 0.1643(2) 0.0172(10) Uani 1 1 d . . . N14 N 0.3276(3) 0.1239(3) 0.1904(2) 0.0161(10) Uani 1 1 d . . . N15 N 0.3366(3) 0.1357(3) 0.3020(2) 0.0153(10) Uani 1 1 d . . . N16 N 0.3586(3) 0.2041(3) -0.0023(2) 0.0194(11) Uani 1 1 d . . . N17 N 0.4557(3) 0.0808(3) 0.1120(2) 0.0205(11) Uani 1 1 d . . . N18 N 0.5505(3) -0.0408(3) 0.2206(2) 0.0219(11) Uani 1 1 d . . . N19 N 0.1886(3) -0.0013(3) 0.4616(2) 0.0171(10) Uani 1 1 d . . . N20 N 0.1170(3) 0.0243(3) 0.5637(2) 0.0161(10) Uani 1 1 d . . . N21 N -0.0052(3) 0.1211(3) 0.5286(2) 0.0193(11) Uani 1 1 d . . . N22 N 0.2401(4) -0.1923(3) 0.6118(2) 0.0267(12) Uani 1 1 d . . . N23 N 0.1594(3) -0.0365(3) 0.6778(2) 0.0191(10) Uani 1 1 d . . . N24 N 0.0622(3) 0.1289(3) 0.7214(2) 0.0218(11) Uani 1 1 d . . . O1 O 0.4316(3) 0.4073(2) 0.11944(18) 0.0222(9) Uani 1 1 d . . . O2 O 0.3224(3) 0.3032(2) 0.22314(18) 0.0173(8) Uani 1 1 d . . . O1W O 0.2999(3) 0.3323(2) 0.04919(19) 0.0242(10) Uani 1 1 d . . . O3 O 0.4785(3) 0.2468(3) 0.1635(2) 0.0345(12) Uani 1 1 d . . . O4 O 0.4977(3) 0.3587(3) 0.2375(2) 0.0304(11) Uani 1 1 d . . . O5 O 0.1624(3) 0.2160(2) 0.29799(19) 0.0193(9) Uani 1 1 d . . . O4W O 0.1902(3) 0.1757(2) 0.47185(19) 0.0224(9) Uani 1 1 d . . . O6 O 0.0564(3) 0.1052(2) 0.39975(18) 0.0225(9) Uani 1 1 d . . . O7 O -0.0006(3) 0.2629(3) 0.3560(2) 0.0319(11) Uani 1 1 d . . . O8 O -0.0075(3) 0.1489(3) 0.2812(2) 0.0262(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 C1 0.032(4) 0.054(5) 0.060(6) -0.019(5) -0.002(4) 0.007(4) C2 0.037(4) 0.028(4) 0.036(4) 0.004(3) -0.005(3) 0.003(3) C3 0.113(10) 0.066(7) 0.038(6) 0.025(5) -0.037(6) -0.047(7) C4 0.77(7) 0.42(4) 0.054(10) -0.130(17) 0.15(2) -0.49(5) F1 0.086(4) 0.102(5) 0.051(3) 0.008(3) -0.011(3) 0.047(4) F2 0.059(4) 0.116(5) 0.082(4) -0.013(4) 0.029(3) 0.032(4) F3 0.083(5) 0.089(5) 0.269(11) -0.054(6) -0.111(6) -0.001(4) F4 0.040(3) 0.059(3) 0.043(3) 0.004(2) 0.001(2) 0.001(2) F5 0.046(3) 0.045(3) 0.046(3) -0.009(2) -0.013(2) -0.001(2) F6 0.047(3) 0.046(3) 0.047(3) 0.001(2) -0.009(2) 0.014(2) F7 0.101(5) 0.164(7) 0.045(3) -0.021(4) -0.012(3) -0.089(5) F8 0.351(14) 0.060(4) 0.054(4) 0.028(3) -0.067(6) -0.099(6) F9 0.147(6) 0.063(4) 0.059(4) -0.019(3) -0.043(4) 0.044(4) F10 0.322(13) 0.075(5) 0.064(5) -0.024(4) -0.026(6) -0.081(6) F11 0.155(11) 0.67(4) 0.089(8) 0.014(13) 0.071(7) 0.124(16) F12 0.257(10) 0.041(3) 0.052(4) -0.010(3) 0.025(5) -0.035(5) S1 0.0416(11) 0.0308(9) 0.0326(10) -0.0020(8) -0.0028(8) 0.0021(8) S2 0.0316(10) 0.0511(11) 0.0227(9) -0.0046(8) -0.0081(7) 0.0120(8) S3 0.0330(10) 0.0415(10) 0.0362(10) -0.0072(8) -0.0173(8) -0.0025(8) S4 0.0726(17) 0.0392(12) 0.0646(16) -0.0114(11) -0.0307(13) 0.0028(11) O9 0.053(4) 0.049(4) 0.169(8) -0.042(5) -0.039(5) 0.019(3) O10 0.055(4) 0.072(4) 0.063(4) 0.015(4) 0.001(3) -0.004(3) O11 0.076(4) 0.061(4) 0.037(3) -0.010(3) 0.006(3) 0.034(3) O12 0.034(3) 0.076(4) 0.037(3) 0.008(3) 0.003(2) 0.005(3) O13 0.096(5) 0.055(4) 0.036(3) -0.006(3) -0.012(3) 0.043(4) O14 0.052(4) 0.052(3) 0.042(3) -0.012(3) -0.017(3) -0.005(3) O15 0.058(4) 0.154(8) 0.047(4) -0.031(5) -0.006(3) -0.006(5) O16 0.055(4) 0.049(3) 0.073(4) -0.012(3) -0.043(3) 0.008(3) O17 0.061(4) 0.037(3) 0.052(4) 0.003(3) -0.023(3) 0.012(3) O18 0.234(15) 0.41(2) 0.092(8) -0.008(11) -0.010(9) 0.274(17) O19 0.099(6) 0.104(6) 0.031(3) -0.007(3) -0.014(3) -0.052(5) O20 0.356(17) 0.047(5) 0.050(5) 0.010(4) -0.016(7) -0.063(7) O2W 0.036(3) 0.031(3) 0.029(3) -0.003(2) -0.006(2) -0.006(2) O3W 0.029(2) 0.024(2) 0.022(2) -0.0015(18) -0.0020(19) -0.0022(19) O5W 0.050(4) 0.059(4) 0.049(4) -0.018(3) -0.004(3) 0.008(3) O6W 0.059(4) 0.065(4) 0.127(7) -0.062(5) -0.020(4) 0.023(3) O7W 0.037(3) 0.055(4) 0.050(4) -0.015(3) 0.002(3) -0.014(3) O8W 0.067(4) 0.044(3) 0.050(4) -0.004(3) -0.012(3) -0.001(3) O9W 0.043(3) 0.056(4) 0.046(3) -0.020(3) -0.012(3) 0.006(3) O10W 0.037(3) 0.078(4) 0.057(4) 0.000(3) -0.005(3) -0.014(3) O11W 0.043(3) 0.045(3) 0.053(4) -0.013(3) -0.009(3) 0.011(3) C101 0.018(3) 0.017(3) 0.021(3) -0.004(2) -0.002(2) 0.004(2) C102 0.018(3) 0.015(3) 0.020(3) 0.001(2) 0.002(2) 0.000(2) C103 0.027(4) 0.026(3) 0.024(3) 0.002(3) 0.004(3) 0.007(3) C104 0.028(4) 0.024(3) 0.031(4) -0.004(3) 0.006(3) 0.008(3) C105 0.028(4) 0.027(3) 0.020(3) -0.006(3) 0.009(3) -0.003(3) C106 0.023(3) 0.023(3) 0.015(3) -0.002(2) 0.003(2) -0.001(2) C107 0.017(3) 0.020(3) 0.017(3) -0.005(2) -0.001(2) -0.002(2) C108 0.018(3) 0.023(3) 0.016(3) -0.001(2) 0.003(2) 0.001(2) C109 0.020(3) 0.031(4) 0.026(4) 0.000(3) -0.003(3) 0.002(3) C110 0.026(4) 0.038(4) 0.030(4) 0.008(3) -0.004(3) 0.004(3) C111 0.025(4) 0.032(4) 0.038(4) 0.014(3) 0.005(3) 0.012(3) C112 0.034(4) 0.018(3) 0.042(4) 0.003(3) 0.009(3) 0.003(3) C113 0.014(3) 0.023(3) 0.017(3) -0.004(2) 0.000(2) -0.004(2) C114 0.017(3) 0.025(3) 0.024(3) -0.012(3) -0.005(2) 0.003(2) C115 0.026(3) 0.031(4) 0.020(3) -0.004(3) 0.000(3) -0.001(3) C116 0.030(4) 0.047(4) 0.024(4) -0.012(3) 0.002(3) 0.000(3) C117 0.030(4) 0.044(4) 0.031(4) -0.021(3) -0.001(3) 0.002(3) C118 0.030(4) 0.028(3) 0.032(4) -0.014(3) -0.007(3) 0.004(3) C119 0.016(3) 0.018(3) 0.018(3) -0.005(2) 0.000(2) 0.000(2) C120 0.018(3) 0.014(3) 0.020(3) -0.004(2) -0.003(2) -0.002(2) C121 0.019(3) 0.028(3) 0.025(3) -0.011(3) -0.003(3) 0.003(3) C122 0.016(3) 0.032(4) 0.035(4) -0.012(3) -0.003(3) 0.009(3) C123 0.030(4) 0.029(4) 0.028(4) 0.001(3) -0.007(3) 0.008(3) C124 0.029(4) 0.029(4) 0.022(3) 0.001(3) -0.002(3) 0.011(3) C201 0.015(3) 0.015(3) 0.018(3) -0.003(2) -0.002(2) 0.000(2) C202 0.014(3) 0.017(3) 0.018(3) -0.003(2) -0.003(2) 0.000(2) C203 0.021(3) 0.021(3) 0.021(3) -0.004(2) -0.002(2) 0.000(2) C204 0.021(3) 0.027(3) 0.021(3) -0.005(3) -0.008(3) -0.001(3) C205 0.018(3) 0.029(3) 0.034(4) -0.002(3) -0.009(3) 0.003(3) C206 0.015(3) 0.022(3) 0.029(3) -0.004(3) -0.002(3) 0.001(2) C207 0.018(3) 0.015(3) 0.016(3) -0.004(2) -0.006(2) 0.004(2) C208 0.020(3) 0.017(3) 0.015(3) 0.000(2) -0.003(2) 0.000(2) C209 0.028(3) 0.015(3) 0.022(3) -0.004(2) 0.001(3) 0.001(2) C210 0.034(4) 0.025(3) 0.019(3) -0.009(3) 0.005(3) -0.005(3) C211 0.036(4) 0.029(4) 0.013(3) -0.001(3) -0.002(3) -0.002(3) C212 0.031(4) 0.018(3) 0.021(3) -0.002(2) -0.008(3) 0.001(3) C213 0.019(3) 0.020(3) 0.017(3) 0.000(2) -0.003(2) -0.001(2) C214 0.016(3) 0.028(3) 0.014(3) -0.005(2) -0.002(2) 0.000(2) C215 0.019(3) 0.048(4) 0.030(4) 0.003(3) -0.001(3) 0.001(3) C216 0.017(4) 0.080(6) 0.036(4) 0.002(4) 0.000(3) 0.007(4) C217 0.032(4) 0.053(5) 0.026(4) -0.006(3) -0.011(3) 0.022(4) C218 0.031(4) 0.030(4) 0.026(4) -0.002(3) -0.008(3) 0.011(3) C219 0.016(3) 0.019(3) 0.019(3) -0.003(2) -0.006(2) 0.000(2) C220 0.025(3) 0.015(3) 0.013(3) -0.002(2) -0.001(2) 0.000(2) C221 0.016(3) 0.027(3) 0.019(3) -0.004(3) -0.002(2) 0.003(2) C222 0.025(3) 0.028(3) 0.021(3) -0.003(3) -0.007(3) 0.005(3) C223 0.029(4) 0.027(3) 0.013(3) -0.004(2) 0.001(3) -0.002(3) C224 0.022(3) 0.021(3) 0.014(3) -0.003(2) -0.002(2) 0.006(2) C301 0.022(3) 0.018(3) 0.016(3) -0.006(2) -0.007(2) 0.006(2) C302 0.021(3) 0.016(3) 0.019(3) -0.001(2) 0.000(2) -0.002(2) C303 0.027(4) 0.039(4) 0.017(3) -0.003(3) -0.004(3) -0.003(3) C304 0.031(4) 0.050(5) 0.023(4) -0.001(3) -0.008(3) -0.004(3) C305 0.022(3) 0.040(4) 0.021(3) 0.005(3) -0.004(3) 0.001(3) C306 0.021(3) 0.025(3) 0.019(3) 0.003(3) -0.002(2) 0.000(3) C307 0.021(3) 0.026(3) 0.015(3) -0.003(2) -0.005(2) 0.003(3) C308 0.023(3) 0.030(3) 0.014(3) -0.005(3) -0.005(2) 0.002(3) C309 0.068(6) 0.035(4) 0.021(4) -0.010(3) -0.006(4) 0.023(4) C310 0.108(8) 0.040(5) 0.016(4) -0.014(3) -0.003(4) 0.022(5) C311 0.076(6) 0.037(4) 0.009(3) 0.000(3) -0.006(3) 0.011(4) C312 0.035(4) 0.023(3) 0.019(3) -0.002(3) -0.003(3) 0.002(3) C313 0.019(3) 0.016(3) 0.012(3) -0.003(2) -0.001(2) 0.000(2) C314 0.018(3) 0.022(3) 0.015(3) -0.007(2) -0.003(2) 0.004(2) C315 0.028(4) 0.027(3) 0.030(4) 0.001(3) -0.005(3) 0.002(3) C316 0.019(3) 0.034(4) 0.042(4) -0.006(3) -0.004(3) 0.003(3) C317 0.025(4) 0.032(4) 0.031(4) -0.003(3) -0.007(3) 0.011(3) C318 0.034(4) 0.026(3) 0.017(3) -0.001(3) -0.006(3) 0.008(3) C319 0.019(3) 0.020(3) 0.011(3) -0.003(2) -0.001(2) -0.001(2) C320 0.018(3) 0.021(3) 0.014(3) -0.002(2) -0.003(2) 0.000(2) C321 0.021(3) 0.026(3) 0.017(3) -0.002(2) 0.000(2) 0.002(3) C322 0.026(3) 0.029(3) 0.017(3) -0.003(3) -0.010(3) 0.003(3) C323 0.027(3) 0.026(3) 0.013(3) -0.004(2) -0.005(2) 0.004(3) C324 0.022(3) 0.021(3) 0.011(3) 0.001(2) 0.002(2) -0.002(2) C401 0.013(3) 0.013(3) 0.020(3) -0.003(2) -0.005(2) 0.003(2) C402 0.021(3) 0.013(3) 0.015(3) -0.001(2) -0.004(2) 0.000(2) C403 0.016(3) 0.024(3) 0.020(3) 0.001(3) 0.000(2) 0.001(2) C404 0.020(3) 0.028(3) 0.028(4) -0.003(3) 0.007(3) 0.007(3) C405 0.022(3) 0.025(3) 0.024(3) -0.009(3) 0.006(3) 0.001(3) C406 0.020(3) 0.017(3) 0.014(3) -0.001(2) 0.002(2) -0.004(2) C407 0.020(3) 0.018(3) 0.017(3) -0.004(2) -0.001(2) -0.002(2) C408 0.019(3) 0.024(3) 0.014(3) 0.000(2) -0.001(2) 0.005(2) C409 0.021(3) 0.030(3) 0.020(3) 0.002(3) -0.002(3) 0.002(3) C410 0.022(3) 0.035(4) 0.028(4) 0.006(3) -0.001(3) 0.008(3) C411 0.030(4) 0.024(3) 0.038(4) 0.008(3) 0.006(3) 0.011(3) C412 0.038(4) 0.023(3) 0.036(4) -0.006(3) 0.003(3) 0.002(3) C413 0.020(3) 0.017(3) 0.016(3) -0.001(2) 0.004(2) -0.002(2) C414 0.015(3) 0.025(3) 0.014(3) -0.008(2) 0.003(2) -0.002(2) C415 0.025(3) 0.025(3) 0.017(3) -0.003(3) -0.004(2) -0.001(3) C416 0.028(4) 0.043(4) 0.015(3) -0.003(3) 0.004(3) -0.004(3) C417 0.034(4) 0.039(4) 0.025(4) -0.015(3) 0.000(3) 0.003(3) C418 0.031(4) 0.026(3) 0.033(4) -0.013(3) -0.006(3) 0.000(3) C419 0.015(3) 0.016(3) 0.013(3) -0.003(2) 0.002(2) -0.002(2) C420 0.019(3) 0.017(3) 0.016(3) -0.004(2) -0.003(2) -0.001(2) C421 0.021(3) 0.020(3) 0.019(3) -0.005(2) 0.004(2) 0.002(2) C422 0.018(3) 0.025(3) 0.027(3) -0.009(3) 0.000(3) 0.003(2) C423 0.018(3) 0.017(3) 0.035(4) -0.006(3) -0.006(3) 0.005(2) C424 0.022(3) 0.016(3) 0.023(3) 0.000(2) -0.001(3) 0.002(2) Cu1 0.0191(4) 0.0184(4) 0.0141(4) -0.0025(3) -0.0007(3) 0.0032(3) Cu2 0.0166(4) 0.0221(4) 0.0146(4) -0.0037(3) -0.0023(3) 0.0041(3) Cu3 0.0169(4) 0.0219(4) 0.0129(3) -0.0027(3) -0.0011(3) 0.0039(3) Cu4 0.0171(4) 0.0176(4) 0.0132(4) -0.0011(3) -0.0007(3) 0.0026(3) Mo1 0.0157(3) 0.0165(2) 0.0184(3) -0.0015(2) -0.0003(2) 0.00082(19) Mo2 0.0148(2) 0.0167(2) 0.0156(3) -0.00196(19) -0.00094(19) 0.00073(19) N1 0.016(2) 0.020(3) 0.016(3) -0.001(2) 0.0013(19) 0.000(2) N2 0.019(3) 0.019(3) 0.015(2) 0.000(2) -0.004(2) 0.001(2) N3 0.019(3) 0.019(2) 0.017(3) -0.001(2) 0.001(2) 0.004(2) N4 0.029(3) 0.025(3) 0.026(3) 0.000(2) -0.002(2) 0.003(2) N5 0.018(3) 0.021(3) 0.019(3) -0.004(2) -0.003(2) 0.002(2) N6 0.026(3) 0.026(3) 0.026(3) -0.011(2) -0.011(2) 0.009(2) N7 0.016(2) 0.018(2) 0.017(3) -0.002(2) -0.0013(19) 0.0029(19) N8 0.016(2) 0.017(2) 0.014(2) -0.0029(19) -0.0027(19) 0.0023(19) N9 0.019(3) 0.020(3) 0.017(3) -0.003(2) -0.002(2) 0.002(2) N10 0.022(3) 0.023(3) 0.024(3) 0.000(2) -0.003(2) 0.005(2) N11 0.019(3) 0.018(2) 0.014(2) -0.0036(19) -0.0019(19) 0.000(2) N12 0.022(3) 0.023(3) 0.020(3) -0.004(2) -0.007(2) -0.002(2) N13 0.017(2) 0.017(2) 0.016(2) 0.0012(19) -0.0027(19) -0.0009(19) N14 0.015(2) 0.018(2) 0.015(2) -0.0037(19) -0.0010(19) 0.0023(19) N15 0.015(2) 0.016(2) 0.014(2) -0.0018(19) -0.0011(19) 0.0028(19) N16 0.021(3) 0.018(2) 0.020(3) -0.006(2) -0.002(2) 0.002(2) N17 0.024(3) 0.024(3) 0.015(3) -0.007(2) -0.004(2) 0.003(2) N18 0.026(3) 0.024(3) 0.015(3) -0.002(2) 0.000(2) 0.002(2) N19 0.019(3) 0.015(2) 0.017(2) -0.0029(19) 0.001(2) -0.0020(19) N20 0.015(2) 0.021(2) 0.012(2) -0.0031(19) 0.0019(18) 0.0009(19) N21 0.016(3) 0.018(2) 0.024(3) -0.003(2) -0.004(2) 0.003(2) N22 0.034(3) 0.018(3) 0.027(3) -0.002(2) 0.001(2) 0.003(2) N23 0.015(2) 0.024(3) 0.018(3) -0.003(2) 0.000(2) 0.001(2) N24 0.028(3) 0.019(3) 0.020(3) -0.007(2) -0.002(2) 0.002(2) O1 0.025(2) 0.026(2) 0.016(2) -0.0049(18) -0.0034(17) 0.0021(18) O2 0.016(2) 0.020(2) 0.017(2) -0.0058(17) -0.0009(16) 0.0012(16) O1W 0.025(2) 0.027(2) 0.022(2) -0.0091(19) 0.0040(18) -0.0028(18) O3 0.031(3) 0.023(2) 0.046(3) -0.004(2) 0.015(2) 0.001(2) O4 0.026(3) 0.037(3) 0.025(2) 0.005(2) -0.007(2) -0.009(2) O5 0.016(2) 0.022(2) 0.021(2) -0.0054(17) -0.0015(17) 0.0006(17) O4W 0.024(2) 0.020(2) 0.022(2) -0.0028(18) 0.0008(18) -0.0031(18) O6 0.027(2) 0.025(2) 0.014(2) 0.0001(17) -0.0032(17) -0.0004(18) O7 0.028(3) 0.023(2) 0.044(3) -0.007(2) 0.008(2) -0.0013(19) O8 0.022(2) 0.033(3) 0.022(2) 0.0001(19) -0.0042(18) -0.0086(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 C1 F3 1.254(10) . ? C1 F1 1.315(10) . ? C1 F2 1.345(10) . ? C1 S1 1.805(8) . ? C2 F5 1.273(9) . ? C2 F4 1.346(8) . ? C2 F6 1.354(8) . ? C2 S2 1.851(8) . ? C3 F8 1.284(10) . ? C3 F9 1.329(14) . ? C3 F7 1.343(12) . ? C3 S3 1.846(12) . ? C4 F10 1.433(11) . ? C4 F12 1.449(14) . ? C4 S4 1.475(18) . ? C4 F11 1.503(15) . ? F11 S4 2.108(16) . ? S1 O10 1.415(6) . ? S1 O9 1.429(7) . ? S1 O11 1.432(6) . ? S2 O13 1.409(6) . ? S2 O14 1.420(5) . ? S2 O12 1.476(6) . ? S3 O17 1.422(6) . ? S3 O16 1.423(5) . ? S3 O15 1.437(7) . ? S4 O20 1.351(7) . ? S4 O19 1.398(6) . ? S4 O18 1.704(11) . ? C101 N2 1.351(7) . ? C101 C107 1.397(8) . ? C101 C102 1.488(8) . ? C102 N1 1.364(8) . ? C102 C103 1.377(8) . ? C103 C104 1.387(9) . ? C103 H103 0.9300 . ? C104 C105 1.376(9) . ? C104 H104 0.9300 . ? C105 C106 1.392(9) . ? C105 H105 0.9300 . ? C106 N1 1.332(7) . ? C106 H106 0.9300 . ? C107 N5 1.339(7) . ? C107 C108 1.500(8) . ? C108 N4 1.330(8) . ? C108 C109 1.394(9) . ? C109 C110 1.375(9) . ? C109 H109 0.9300 . ? C110 C111 1.359(11) . ? C110 H110 0.9300 . ? C111 C112 1.381(11) . ? C111 H111 0.9300 . ? C112 N4 1.341(8) . ? C112 H112 0.9300 . ? C113 N5 1.342(7) . ? C113 C119 1.416(8) . ? C113 C114 1.482(8) . ? C114 N6 1.345(8) . ? C114 C115 1.384(9) . ? C115 C116 1.390(9) . ? C115 H115 0.9300 . ? C116 C117 1.381(10) . ? C116 H116 0.9300 . ? C117 C118 1.384(10) . ? C117 H117 0.9300 . ? C118 N6 1.333(8) . ? C118 H118 0.9300 . ? C119 N2 1.340(7) . ? C119 C120 1.495(8) . ? C120 N3 1.365(7) . ? C120 C121 1.384(8) . ? C121 C122 1.382(9) . ? C121 H121 0.9300 . ? C122 C123 1.373(9) . ? C122 H122 0.9300 . ? C123 C124 1.381(9) . ? C123 H123 0.9300 . ? C124 N3 1.345(8) . ? C124 H124 0.9300 . ? C201 N8 1.338(7) . ? C201 C207 1.415(8) . ? C201 C202 1.485(8) . ? C202 N9 1.362(7) . ? C202 C203 1.389(8) . ? C203 C204 1.378(8) . ? C203 H203 0.9300 . ? C204 C205 1.377(9) . ? C204 H204 0.9300 . ? C205 C206 1.395(9) . ? C205 H205 0.9300 . ? C206 N9 1.341(7) . ? C206 H206 0.9300 . ? C207 N11 1.339(7) . ? C207 C208 1.488(8) . ? C208 N12 1.341(7) . ? C208 C209 1.385(8) . ? C209 C210 1.387(9) . ? C209 H209 0.9300 . ? C210 C211 1.373(9) . ? C210 H210 0.9300 . ? C211 C212 1.370(9) . ? C211 H211 0.9300 . ? C212 N12 1.349(8) . ? C212 H212 0.9300 . ? C213 N11 1.338(7) . ? C213 C219 1.406(8) . ? C213 C214 1.489(8) . ? C214 N10 1.329(8) . ? C214 C215 1.399(9) . ? C215 C216 1.385(10) . ? C215 H215 0.9300 . ? C216 C217 1.369(11) . ? C216 H216 0.9300 . ? C217 C218 1.376(10) . ? C217 H217 0.9300 . ? C218 N10 1.342(8) . ? C218 H218 0.9300 . ? C219 N8 1.332(7) . ? C219 C220 1.493(8) . ? C220 N7 1.365(7) . ? C220 C221 1.381(8) . ? C221 C222 1.388(9) . ? C221 H221 0.9300 . ? C222 C223 1.373(9) . ? C222 H222 0.9300 . ? C223 C224 1.376(8) . ? C223 H223 0.9300 . ? C224 N7 1.334(7) . ? C224 H224 0.9300 . ? C301 N14 1.343(7) . ? C301 C307 1.399(8) . ? C301 C302 1.480(8) . ? C302 N13 1.353(7) . ? C302 C303 1.379(9) . ? C303 C304 1.373(10) . ? C303 H303 0.9300 . ? C304 C305 1.384(10) . ? C304 H304 0.9300 . ? C305 C306 1.380(9) . ? C305 H305 0.9300 . ? C306 N13 1.341(8) . ? C306 H306 0.9300 . ? C307 N17 1.336(7) . ? C307 C308 1.489(8) . ? C308 N16 1.337(8) . ? C308 C309 1.372(9) . ? C309 C310 1.398(10) . ? C309 H309 0.9300 . ? C310 C311 1.368(10) . ? C310 H310 0.9300 . ? C311 C312 1.365(9) . ? C311 H311 0.9300 . ? C312 N16 1.334(8) . ? C312 H312 0.9300 . ? C313 N17 1.336(7) . ? C313 C319 1.394(8) . ? C313 C314 1.504(8) . ? C314 N18 1.349(8) . ? C314 C315 1.375(9) . ? C315 C316 1.374(9) . ? C315 H315 0.9300 . ? C316 C317 1.386(10) . ? C316 H316 0.9300 . ? C317 C318 1.362(9) . ? C317 H317 0.9300 . ? C318 N18 1.352(8) . ? C318 H318 0.9300 . ? C319 N14 1.332(7) . ? C319 C320 1.497(8) . ? C320 N15 1.357(7) . ? C320 C321 1.376(8) . ? C321 C322 1.399(8) . ? C321 H321 0.9300 . ? C322 C323 1.377(9) . ? C322 H322 0.9300 . ? C323 C324 1.391(8) . ? C323 H323 0.9300 . ? C324 N15 1.325(7) . ? C324 H324 0.9300 . ? C401 N20 1.335(7) . ? C401 C407 1.400(8) . ? C401 C402 1.493(8) . ? C402 N19 1.352(7) . ? C402 C403 1.384(8) . ? C403 C404 1.383(9) . ? C403 H403 0.9300 . ? C404 C405 1.379(9) . ? C404 H404 0.9300 . ? C405 C406 1.374(8) . ? C405 H405 0.9300 . ? C406 N19 1.349(7) . ? C406 H406 0.9300 . ? C407 N23 1.336(7) . ? C407 C408 1.488(8) . ? C408 N22 1.346(8) . ? C408 C409 1.385(8) . ? C409 C410 1.391(9) . ? C409 H409 0.9300 . ? C410 C411 1.379(10) . ? C410 H410 0.9300 . ? C411 C412 1.366(10) . ? C411 H411 0.9300 . ? C412 N22 1.341(8) . ? C412 H412 0.9300 . ? C413 N23 1.353(7) . ? C413 C419 1.407(8) . ? C413 C414 1.475(8) . ? C414 N24 1.354(7) . ? C414 C415 1.385(8) . ? C415 C416 1.390(9) . ? C415 H415 0.9300 . ? C416 C417 1.376(10) . ? C416 H416 0.9300 . ? C417 C418 1.380(10) . ? C417 H417 0.9300 . ? C418 N24 1.336(8) . ? C418 H418 0.9300 . ? C419 N20 1.340(7) . ? C419 C420 1.495(8) . ? C420 N21 1.375(7) . ? C420 C421 1.378(8) . ? C421 C422 1.378(8) . ? C421 H421 0.9300 . ? C422 C423 1.396(9) . ? C422 H422 0.9300 . ? C423 C424 1.372(8) . ? C423 H423 0.9300 . ? C424 N21 1.345(7) . ? C424 H424 0.9300 . ? Cu1 O1 1.912(4) . ? Cu1 N2 1.965(5) . ? Cu1 N3 2.002(5) . ? Cu1 N1 2.016(5) . ? Cu1 O1W 2.255(4) . ? Cu2 O2 1.927(4) . ? Cu2 N8 1.971(5) . ? Cu2 N7 2.001(5) . ? Cu2 N9 2.022(5) . ? Cu3 O5 1.912(4) . ? Cu3 N14 1.953(5) . ? Cu3 N15 2.024(5) . ? Cu3 N13 2.047(5) . ? Cu4 O6 1.898(4) . ? Cu4 N20 1.960(5) . ? Cu4 N21 2.011(5) . ? Cu4 N19 2.019(5) . ? Cu4 O4W 2.260(4) . ? Mo1 O3 1.721(4) . ? Mo1 O4 1.727(5) . ? Mo1 O1 1.800(4) . ? Mo1 O2 1.819(4) . ? Mo2 O7 1.724(4) . ? Mo2 O8 1.732(4) . ? Mo2 O6 1.798(4) . ? Mo2 O5 1.828(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 C1 F1 113.2(9) . . ? F3 C1 F2 106.7(8) . . ? F1 C1 F2 102.7(7) . . ? F3 C1 S1 112.3(6) . . ? F1 C1 S1 111.8(6) . . ? F2 C1 S1 109.5(6) . . ? F5 C2 F4 109.6(6) . . ? F5 C2 F6 108.4(6) . . ? F4 C2 F6 105.8(6) . . ? F5 C2 S2 113.1(5) . . ? F4 C2 S2 109.6(5) . . ? F6 C2 S2 110.1(5) . . ? F8 C3 F9 107.9(12) . . ? F8 C3 F7 111.2(9) . . ? F9 C3 F7 108.3(8) . . ? F8 C3 S3 111.4(7) . . ? F9 C3 S3 109.8(7) . . ? F7 C3 S3 108.3(9) . . ? F10 C4 F12 102.4(10) . . ? F10 C4 S4 123.9(13) . . ? F12 C4 S4 123.4(9) . . ? F10 C4 F11 109.5(12) . . ? F12 C4 F11 104.4(14) . . ? S4 C4 F11 90.1(11) . . ? C4 F11 S4 44.4(8) . . ? O10 S1 O9 113.8(5) . . ? O10 S1 O11 113.4(4) . . ? O9 S1 O11 113.5(5) . . ? O10 S1 C1 105.9(4) . . ? O9 S1 C1 106.6(4) . . ? O11 S1 C1 102.5(4) . . ? O13 S2 O14 116.4(4) . . ? O13 S2 O12 116.4(4) . . ? O14 S2 O12 114.6(3) . . ? O13 S2 C2 103.6(3) . . ? O14 S2 C2 102.2(3) . . ? O12 S2 C2 100.2(4) . . ? O17 S3 O16 115.1(4) . . ? O17 S3 O15 115.1(4) . . ? O16 S3 O15 113.8(4) . . ? O17 S3 C3 104.0(4) . . ? O16 S3 C3 102.4(5) . . ? O15 S3 C3 104.3(5) . . ? O20 S4 O19 130.3(5) . . ? O20 S4 C4 113.7(6) . . ? O19 S4 C4 111.7(6) . . ? O20 S4 O18 103.1(6) . . ? O19 S4 O18 103.3(5) . . ? C4 S4 O18 80.2(8) . . ? O20 S4 F11 99.6(6) . . ? O19 S4 F11 98.1(5) . . ? C4 S4 F11 45.5(7) . . ? O18 S4 F11 125.7(7) . . ? N2 C101 C107 116.9(5) . . ? N2 C101 C102 112.9(5) . . ? C107 C101 C102 130.3(5) . . ? N1 C102 C103 120.8(6) . . ? N1 C102 C101 113.3(5) . . ? C103 C102 C101 125.8(6) . . ? C102 C103 C104 119.5(6) . . ? C102 C103 H103 120.3 . . ? C104 C103 H103 120.3 . . ? C105 C104 C103 119.3(6) . . ? C105 C104 H104 120.3 . . ? C103 C104 H104 120.3 . . ? C104 C105 C106 118.7(6) . . ? C104 C105 H105 120.6 . . ? C106 C105 H105 120.6 . . ? N1 C106 C105 122.0(6) . . ? N1 C106 H106 119.0 . . ? C105 C106 H106 119.0 . . ? N5 C107 C101 119.9(5) . . ? N5 C107 C108 113.8(5) . . ? C101 C107 C108 126.3(5) . . ? N4 C108 C109 123.8(6) . . ? N4 C108 C107 116.3(5) . . ? C109 C108 C107 119.9(6) . . ? C110 C109 C108 118.0(7) . . ? C110 C109 H109 121.0 . . ? C108 C109 H109 121.0 . . ? C111 C110 C109 119.3(7) . . ? C111 C110 H110 120.3 . . ? C109 C110 H110 120.3 . . ? C110 C111 C112 119.0(6) . . ? C110 C111 H111 120.5 . . ? C112 C111 H111 120.5 . . ? N4 C112 C111 123.5(7) . . ? N4 C112 H112 118.3 . . ? C111 C112 H112 118.3 . . ? N5 C113 C119 118.8(5) . . ? N5 C113 C114 113.0(5) . . ? C119 C113 C114 128.1(5) . . ? N6 C114 C115 123.7(6) . . ? N6 C114 C113 117.7(6) . . ? C115 C114 C113 118.5(5) . . ? C114 C115 C116 118.3(6) . . ? C114 C115 H115 120.9 . . ? C116 C115 H115 120.9 . . ? C117 C116 C115 118.5(7) . . ? C117 C116 H116 120.8 . . ? C115 C116 H116 120.8 . . ? C116 C117 C118 119.1(6) . . ? C116 C117 H117 120.4 . . ? C118 C117 H117 120.4 . . ? N6 C118 C117 123.5(6) . . ? N6 C118 H118 118.3 . . ? C117 C118 H118 118.3 . . ? N2 C119 C113 117.3(5) . . ? N2 C119 C120 112.3(5) . . ? C113 C119 C120 130.4(5) . . ? N3 C120 C121 120.6(5) . . ? N3 C120 C119 113.1(5) . . ? C121 C120 C119 126.3(5) . . ? C122 C121 C120 119.6(6) . . ? C122 C121 H121 120.2 . . ? C120 C121 H121 120.2 . . ? C123 C122 C121 119.7(6) . . ? C123 C122 H122 120.1 . . ? C121 C122 H122 120.1 . . ? C122 C123 C124 118.8(6) . . ? C122 C123 H123 120.6 . . ? C124 C123 H123 120.6 . . ? N3 C124 C123 122.2(6) . . ? N3 C124 H124 118.9 . . ? C123 C124 H124 118.9 . . ? N8 C201 C207 116.7(5) . . ? N8 C201 C202 112.6(5) . . ? C207 C201 C202 130.6(5) . . ? N9 C202 C203 121.5(5) . . ? N9 C202 C201 113.2(5) . . ? C203 C202 C201 124.9(5) . . ? C204 C203 C202 118.8(6) . . ? C204 C203 H203 120.6 . . ? C202 C203 H203 120.6 . . ? C205 C204 C203 120.3(6) . . ? C205 C204 H204 119.9 . . ? C203 C204 H204 119.9 . . ? C204 C205 C206 118.3(6) . . ? C204 C205 H205 120.9 . . ? C206 C205 H205 120.9 . . ? N9 C206 C205 122.4(6) . . ? N9 C206 H206 118.8 . . ? C205 C206 H206 118.8 . . ? N11 C207 C201 118.4(5) . . ? N11 C207 C208 113.3(5) . . ? C201 C207 C208 128.2(5) . . ? N12 C208 C209 121.9(5) . . ? N12 C208 C207 118.0(5) . . ? C209 C208 C207 120.0(5) . . ? C208 C209 C210 119.9(6) . . ? C208 C209 H209 120.0 . . ? C210 C209 H209 120.0 . . ? C211 C210 C209 117.9(6) . . ? C211 C210 H210 121.0 . . ? C209 C210 H210 121.0 . . ? C212 C211 C210 119.3(6) . . ? C212 C211 H211 120.4 . . ? C210 C211 H211 120.4 . . ? N12 C212 C211 123.5(6) . . ? N12 C212 H212 118.2 . . ? C211 C212 H212 118.2 . . ? N11 C213 C219 118.8(5) . . ? N11 C213 C214 113.5(5) . . ? C219 C213 C214 127.7(5) . . ? N10 C214 C215 124.0(6) . . ? N10 C214 C213 117.7(5) . . ? C215 C214 C213 118.2(6) . . ? C216 C215 C214 117.6(7) . . ? C216 C215 H215 121.2 . . ? C214 C215 H215 121.2 . . ? C217 C216 C215 119.0(7) . . ? C217 C216 H216 120.5 . . ? C215 C216 H216 120.5 . . ? C216 C217 C218 119.2(6) . . ? C216 C217 H217 120.4 . . ? C218 C217 H217 120.4 . . ? N10 C218 C217 123.5(6) . . ? N10 C218 H218 118.3 . . ? C217 C218 H218 118.3 . . ? N8 C219 C213 117.1(5) . . ? N8 C219 C220 113.5(5) . . ? C213 C219 C220 129.3(5) . . ? N7 C220 C221 120.9(5) . . ? N7 C220 C219 113.0(5) . . ? C221 C220 C219 126.1(5) . . ? C220 C221 C222 118.8(6) . . ? C220 C221 H221 120.6 . . ? C222 C221 H221 120.6 . . ? C223 C222 C221 120.0(6) . . ? C223 C222 H222 120.0 . . ? C221 C222 H222 120.0 . . ? C222 C223 C224 118.6(6) . . ? C222 C223 H223 120.7 . . ? C224 C223 H223 120.7 . . ? N7 C224 C223 122.5(5) . . ? N7 C224 H224 118.7 . . ? C223 C224 H224 118.7 . . ? N14 C301 C307 117.4(5) . . ? N14 C301 C302 113.1(5) . . ? C307 C301 C302 129.4(5) . . ? N13 C302 C303 121.4(6) . . ? N13 C302 C301 113.7(5) . . ? C303 C302 C301 124.6(6) . . ? C304 C303 C302 119.9(6) . . ? C304 C303 H303 120.1 . . ? C302 C303 H303 120.1 . . ? C303 C304 C305 118.5(7) . . ? C303 C304 H304 120.7 . . ? C305 C304 H304 120.7 . . ? C306 C305 C304 119.4(6) . . ? C306 C305 H305 120.3 . . ? C304 C305 H305 120.3 . . ? N13 C306 C305 121.9(6) . . ? N13 C306 H306 119.1 . . ? C305 C306 H306 119.1 . . ? N17 C307 C301 120.3(5) . . ? N17 C307 C308 114.6(5) . . ? C301 C307 C308 125.1(5) . . ? N16 C308 C309 123.4(6) . . ? N16 C308 C307 116.5(5) . . ? C309 C308 C307 120.0(6) . . ? C308 C309 C310 117.7(7) . . ? C308 C309 H309 121.1 . . ? C310 C309 H309 121.1 . . ? C311 C310 C309 119.0(7) . . ? C311 C310 H310 120.5 . . ? C309 C310 H310 120.5 . . ? C312 C311 C310 119.0(6) . . ? C312 C311 H311 120.5 . . ? C310 C311 H311 120.5 . . ? N16 C312 C311 123.4(6) . . ? N16 C312 H312 118.3 . . ? C311 C312 H312 118.3 . . ? N17 C313 C319 120.1(5) . . ? N17 C313 C314 112.0(5) . . ? C319 C313 C314 127.8(5) . . ? N18 C314 C315 123.5(5) . . ? N18 C314 C313 116.3(5) . . ? C315 C314 C313 120.0(5) . . ? C316 C315 C314 119.4(6) . . ? C316 C315 H315 120.3 . . ? C314 C315 H315 120.3 . . ? C315 C316 C317 117.8(6) . . ? C315 C316 H316 121.1 . . ? C317 C316 H316 121.1 . . ? C318 C317 C316 119.7(6) . . ? C318 C317 H317 120.2 . . ? C316 C317 H317 120.2 . . ? N18 C318 C317 123.5(6) . . ? N18 C318 H318 118.3 . . ? C317 C318 H318 118.3 . . ? N14 C319 C313 118.1(5) . . ? N14 C319 C320 112.5(5) . . ? C313 C319 C320 129.3(5) . . ? N15 C320 C321 121.3(5) . . ? N15 C320 C319 113.2(5) . . ? C321 C320 C319 125.5(5) . . ? C320 C321 C322 119.2(6) . . ? C320 C321 H321 120.4 . . ? C322 C321 H321 120.4 . . ? C323 C322 C321 118.8(6) . . ? C323 C322 H322 120.6 . . ? C321 C322 H322 120.6 . . ? C322 C323 C324 118.9(6) . . ? C322 C323 H323 120.5 . . ? C324 C323 H323 120.5 . . ? N15 C324 C323 122.2(6) . . ? N15 C324 H324 118.9 . . ? C323 C324 H324 118.9 . . ? N20 C401 C407 117.3(5) . . ? N20 C401 C402 112.9(5) . . ? C407 C401 C402 129.8(5) . . ? N19 C402 C403 121.3(5) . . ? N19 C402 C401 113.0(5) . . ? C403 C402 C401 125.6(5) . . ? C404 C403 C402 118.3(6) . . ? C404 C403 H403 120.8 . . ? C402 C403 H403 120.8 . . ? C405 C404 C403 120.3(6) . . ? C405 C404 H404 119.9 . . ? C403 C404 H404 119.9 . . ? C406 C405 C404 118.7(6) . . ? C406 C405 H405 120.7 . . ? C404 C405 H405 120.7 . . ? N19 C406 C405 121.7(6) . . ? N19 C406 H406 119.2 . . ? C405 C406 H406 119.2 . . ? N23 C407 C401 119.6(5) . . ? N23 C407 C408 115.5(5) . . ? C401 C407 C408 124.9(5) . . ? N22 C408 C409 123.6(6) . . ? N22 C408 C407 115.5(5) . . ? C409 C408 C407 120.9(6) . . ? C408 C409 C410 118.6(6) . . ? C408 C409 H409 120.7 . . ? C410 C409 H409 120.7 . . ? C411 C410 C409 118.3(6) . . ? C411 C410 H410 120.9 . . ? C409 C410 H410 120.9 . . ? C412 C411 C410 118.9(6) . . ? C412 C411 H411 120.5 . . ? C410 C411 H411 120.5 . . ? N22 C412 C411 124.7(7) . . ? N22 C412 H412 117.6 . . ? C411 C412 H412 117.6 . . ? N23 C413 C419 118.8(5) . . ? N23 C413 C414 114.1(5) . . ? C419 C413 C414 127.2(5) . . ? N24 C414 C415 123.3(5) . . ? N24 C414 C413 116.5(5) . . ? C415 C414 C413 120.1(5) . . ? C414 C415 C416 118.1(6) . . ? C414 C415 H415 121.0 . . ? C416 C415 H415 121.0 . . ? C417 C416 C415 119.5(6) . . ? C417 C416 H416 120.3 . . ? C415 C416 H416 120.3 . . ? C416 C417 C418 118.3(6) . . ? C416 C417 H417 120.8 . . ? C418 C417 H417 120.8 . . ? N24 C418 C417 124.2(6) . . ? N24 C418 H418 117.9 . . ? C417 C418 H418 117.9 . . ? N20 C419 C413 117.4(5) . . ? N20 C419 C420 112.8(5) . . ? C413 C419 C420 129.8(5) . . ? N21 C420 C421 120.5(5) . . ? N21 C420 C419 112.8(5) . . ? C421 C420 C419 126.7(5) . . ? C420 C421 C422 119.8(6) . . ? C420 C421 H421 120.1 . . ? C422 C421 H421 120.1 . . ? C421 C422 C423 119.5(6) . . ? C421 C422 H422 120.3 . . ? C423 C422 H422 120.3 . . ? C424 C423 C422 118.8(6) . . ? C424 C423 H423 120.6 . . ? C422 C423 H423 120.6 . . ? N21 C424 C423 122.1(6) . . ? N21 C424 H424 119.0 . . ? C423 C424 H424 119.0 . . ? O1 Cu1 N2 170.3(2) . . ? O1 Cu1 N3 100.66(19) . . ? N2 Cu1 N3 79.6(2) . . ? O1 Cu1 N1 97.91(19) . . ? N2 Cu1 N1 80.1(2) . . ? N3 Cu1 N1 158.24(19) . . ? O1 Cu1 O1W 93.65(17) . . ? N2 Cu1 O1W 95.99(18) . . ? N3 Cu1 O1W 94.13(18) . . ? N1 Cu1 O1W 95.92(18) . . ? O2 Cu2 N8 172.92(19) . . ? O2 Cu2 N7 96.57(18) . . ? N8 Cu2 N7 80.18(19) . . ? O2 Cu2 N9 103.59(18) . . ? N8 Cu2 N9 79.82(19) . . ? N7 Cu2 N9 159.83(19) . . ? O5 Cu3 N14 176.96(19) . . ? O5 Cu3 N15 97.54(18) . . ? N14 Cu3 N15 79.45(19) . . ? O5 Cu3 N13 102.79(18) . . ? N14 Cu3 N13 80.23(19) . . ? N15 Cu3 N13 159.66(19) . . ? O6 Cu4 N20 168.79(19) . . ? O6 Cu4 N21 100.44(19) . . ? N20 Cu4 N21 80.12(19) . . ? O6 Cu4 N19 97.86(19) . . ? N20 Cu4 N19 79.75(19) . . ? N21 Cu4 N19 158.5(2) . . ? O6 Cu4 O4W 94.18(17) . . ? N20 Cu4 O4W 96.90(18) . . ? N21 Cu4 O4W 96.03(18) . . ? N19 Cu4 O4W 93.74(17) . . ? O3 Mo1 O4 108.5(2) . . ? O3 Mo1 O1 110.2(2) . . ? O4 Mo1 O1 108.4(2) . . ? O3 Mo1 O2 107.9(2) . . ? O4 Mo1 O2 107.9(2) . . ? O1 Mo1 O2 113.86(18) . . ? O7 Mo2 O8 109.4(2) . . ? O7 Mo2 O6 110.1(2) . . ? O8 Mo2 O6 107.5(2) . . ? O7 Mo2 O5 107.5(2) . . ? O8 Mo2 O5 108.26(19) . . ? O6 Mo2 O5 113.93(19) . . ? C106 N1 C102 119.4(5) . . ? C106 N1 Cu1 125.1(4) . . ? C102 N1 Cu1 114.6(4) . . ? C119 N2 C101 123.8(5) . . ? C119 N2 Cu1 118.4(4) . . ? C101 N2 Cu1 117.6(4) . . ? C124 N3 C120 119.1(5) . . ? C124 N3 Cu1 125.0(4) . . ? C120 N3 Cu1 115.8(4) . . ? C108 N4 C112 116.4(6) . . ? C107 N5 C113 121.7(5) . . ? C118 N6 C114 116.9(6) . . ? C224 N7 C220 119.2(5) . . ? C224 N7 Cu2 125.2(4) . . ? C220 N7 Cu2 115.6(4) . . ? C219 N8 C201 124.7(5) . . ? C219 N8 Cu2 117.7(4) . . ? C201 N8 Cu2 116.9(4) . . ? C206 N9 C202 118.7(5) . . ? C206 N9 Cu2 125.8(4) . . ? C202 N9 Cu2 114.7(4) . . ? C214 N10 C218 116.6(6) . . ? C213 N11 C207 122.5(5) . . ? C208 N12 C212 117.3(5) . . ? C306 N13 C302 118.8(5) . . ? C306 N13 Cu3 126.0(4) . . ? C302 N13 Cu3 113.4(4) . . ? C319 N14 C301 122.9(5) . . ? C319 N14 Cu3 119.3(4) . . ? C301 N14 Cu3 117.2(4) . . ? C324 N15 C320 119.5(5) . . ? C324 N15 Cu3 125.1(4) . . ? C320 N15 Cu3 115.4(4) . . ? C312 N16 C308 117.4(5) . . ? C307 N17 C313 120.5(5) . . ? C314 N18 C318 116.1(5) . . ? C406 N19 C402 119.4(5) . . ? C406 N19 Cu4 124.8(4) . . ? C402 N19 Cu4 114.8(4) . . ? C401 N20 C419 123.7(5) . . ? C401 N20 Cu4 118.1(4) . . ? C419 N20 Cu4 118.1(4) . . ? C424 N21 C420 119.4(5) . . ? C424 N21 Cu4 125.4(4) . . ? C420 N21 Cu4 115.2(4) . . ? C412 N22 C408 115.9(6) . . ? C407 N23 C413 121.2(5) . . ? C418 N24 C414 116.7(5) . . ? Mo1 O1 Cu1 142.9(2) . . ? Mo1 O2 Cu2 133.5(2) . . ? Mo2 O5 Cu3 130.5(2) . . ? Mo2 O6 Cu4 146.2(3) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.60 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 2.569 _refine_diff_density_min -1.301 _refine_diff_density_rms 0.242