data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Ya-guang Chen' _publ_contact_author_email chenyg146@nenu.edu.cn loop_ _publ_author_name 'Ya-Guang Chen' 'Chun-Jing Zhang' # Attachment '- compound 2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 769067' #TrackingRef '- compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H34 Cu4 Mo8 N12 O27' _chemical_formula_weight 1896.30 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.2950(10) _cell_length_b 20.1880(10) _cell_length_c 9.6130(10) _cell_angle_alpha 90.00 _cell_angle_beta 120.191(6) _cell_angle_gamma 90.00 _cell_volume 2230.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.1133 _exptl_crystal_size_mid 0.1121 _exptl_crystal_size_min 0.1110 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808.0 _exptl_absorpt_coefficient_mu 4.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.632 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4393 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.74 _reflns_number_total 2202 _reflns_number_gt 1439 _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. During the refinement, the command 'simu' was used to restrain the non-H atoms (C1 C1 C2 C3 C4 C5) with ADP or NPD problems. Furthermore, the command 'dfix' was used for C1 C3, and C1 C5 to restrain their bond distance in the rational range. ; _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^)+(0.0254P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2202 _refine_ls_number_parameters 174 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.049 _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 Mo1 Mo 0.74719(6) 0.0000 0.43499(9) 0.0211(2) Uani 1 2 d S . . Mo2 Mo 0.55633(5) -0.11277(2) 0.37461(7) 0.02032(15) Uani 1 1 d . . . Mo3 Mo 0.36607(6) 0.0000 0.30983(8) 0.01692(19) Uani 1 2 d S . . Cu1 Cu 0.5000 -0.27339(6) 0.5000 0.0472(4) Uani 1 2 d S . . Cu2 Cu 0.0000 -0.30402(6) 0.0000 0.0383(3) Uani 1 2 d S . . O1 O 0.7136(3) -0.09120(19) 0.4583(5) 0.0230(10) Uani 1 1 d . . . O1W O 0.5000 0.0000 0.0000 0.084(4) Uani 1 4 d S . . O2 O 0.5656(4) -0.1965(2) 0.4111(5) 0.0376(12) Uani 1 1 d . . . O3 O 0.5529(4) 0.0000 0.4066(6) 0.0178(13) Uani 1 2 d S . . O4 O 0.4053(3) 0.09331(18) 0.3655(5) 0.0190(9) Uani 1 1 d . . . O5 O 0.8944(5) 0.0000 0.5218(8) 0.0359(17) Uani 1 2 d S . . O6 O 0.5050(4) -0.1066(2) 0.1747(5) 0.0314(11) Uani 1 1 d . . . O7 O 0.3226(5) 0.0000 0.1120(7) 0.0306(16) Uani 1 2 d S . . O8 O 0.7634(5) 0.0000 0.6857(7) 0.0261(14) Uani 1 2 d S . . O9 O 0.6984(5) 0.0000 0.2338(7) 0.0356(16) Uani 1 2 d S . . N1 N 0.3535(4) -0.2991(3) 0.3113(7) 0.0343(14) Uani 1 1 d . . . N2 N 0.1658(4) -0.3042(3) 0.1185(6) 0.0333(14) Uani 1 1 d . . . N3 N 0.3340(4) -0.3532(3) 0.2223(6) 0.0316(13) Uani 1 1 d . . . C1 C 0.5023(8) -0.3788(5) 0.1933(12) 0.102(3) Uani 1 1 d DU . . H1A H 0.5290 -0.3344 0.2338 0.122 Uiso 1 1 calc R . . H1B H 0.5701 -0.4073 0.2372 0.122 Uiso 1 1 calc R . . C2 C 0.2511(6) -0.2706(4) 0.2466(8) 0.043(2) Uani 1 1 d . . . H2A H 0.2379 -0.2311 0.2846 0.051 Uiso 1 1 calc R . . C3 C 0.4246(6) -0.4019(4) 0.2536(9) 0.0462(19) Uani 1 1 d DU . . H3A H 0.3885 -0.4434 0.2016 0.055 Uiso 1 1 calc R . . H3B H 0.4708 -0.4100 0.3685 0.055 Uiso 1 1 calc R . . C4 C 0.2241(5) -0.3575(3) 0.1125(8) 0.0333(17) Uani 1 1 d . . . H4A H 0.1909 -0.3924 0.0404 0.040 Uiso 1 1 calc R . . C5 C 0.4491(10) -0.3778(6) 0.0198(13) 0.103(4) Uani 1 1 d DU . . H5A H 0.4014 -0.3384 -0.0241 0.123 Uiso 1 1 calc R . . H5B H 0.4001 -0.4164 -0.0268 0.123 Uiso 1 1 calc R . . 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 Mo1 0.0158(4) 0.0240(4) 0.0264(4) 0.000 0.0129(4) 0.000 Mo2 0.0184(3) 0.0202(3) 0.0234(3) -0.0044(3) 0.0114(2) -0.0018(3) Mo3 0.0125(4) 0.0194(4) 0.0154(4) 0.000 0.0044(3) 0.000 Cu1 0.0270(7) 0.0425(8) 0.0520(8) 0.000 0.0048(6) 0.000 Cu2 0.0157(6) 0.0504(8) 0.0391(7) 0.000 0.0065(5) 0.000 O1 0.014(2) 0.026(2) 0.029(2) 0.000(2) 0.0112(19) 0.0009(18) O1W 0.074(9) 0.082(10) 0.077(9) 0.000 0.023(8) 0.000 O2 0.034(3) 0.023(2) 0.057(3) -0.002(2) 0.025(2) 0.003(2) O3 0.010(3) 0.024(3) 0.015(3) 0.000 0.004(2) 0.000 O4 0.015(2) 0.018(2) 0.024(2) -0.0004(18) 0.0088(18) -0.0010(17) O5 0.018(3) 0.041(4) 0.049(4) 0.000 0.017(3) 0.000 O6 0.025(2) 0.042(3) 0.022(2) -0.010(2) 0.008(2) 0.003(2) O7 0.030(4) 0.035(4) 0.024(3) 0.000 0.012(3) 0.000 O8 0.023(3) 0.026(3) 0.031(4) 0.000 0.015(3) 0.000 O9 0.044(4) 0.041(4) 0.031(4) 0.000 0.026(3) 0.000 N1 0.017(3) 0.032(3) 0.045(4) -0.001(3) 0.009(3) 0.002(3) N2 0.014(3) 0.042(3) 0.032(3) -0.005(3) 0.003(2) -0.003(3) N3 0.020(3) 0.043(3) 0.029(3) 0.000(3) 0.010(3) 0.001(3) C1 0.079(6) 0.115(6) 0.098(6) 0.016(6) 0.035(5) 0.057(5) C2 0.027(4) 0.046(5) 0.045(4) -0.011(4) 0.010(4) 0.000(4) C3 0.039(4) 0.056(5) 0.047(4) 0.017(4) 0.024(4) 0.023(4) C4 0.021(4) 0.040(4) 0.032(4) -0.006(3) 0.008(3) -0.002(3) C5 0.099(7) 0.120(8) 0.115(8) 0.019(7) 0.072(6) 0.036(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O5 1.698(6) . ? Mo1 O9 1.703(6) . ? Mo1 O1 1.934(4) 6 ? Mo1 O1 1.934(4) . ? Mo1 O8 2.310(6) . ? Mo1 O3 2.457(5) . ? Mo2 O6 1.690(4) . ? Mo2 O2 1.718(4) . ? Mo2 O1 1.876(4) . ? Mo2 O4 2.005(4) 6 ? Mo2 O3 2.3008(9) . ? Mo2 O4 2.318(4) 5_656 ? Mo3 O7 1.687(6) . ? Mo3 O8 1.743(6) 5_656 ? Mo3 O4 1.956(4) . ? Mo3 O4 1.956(4) 6 ? Mo3 O3 2.171(5) . ? Mo3 O3 2.374(5) 5_656 ? Cu1 N1 1.949(5) . ? Cu1 N1 1.949(5) 2_656 ? Cu1 O2 2.156(5) 2_656 ? Cu1 O2 2.156(5) . ? Cu2 N2 1.906(5) . ? Cu2 N2 1.906(5) 2 ? O3 Mo2 2.3008(9) 6 ? O3 Mo3 2.374(5) 5_656 ? O4 Mo2 2.005(4) 6 ? O4 Mo2 2.318(4) 5_656 ? O8 Mo3 1.743(6) 5_656 ? N1 C2 1.311(8) . ? N1 N3 1.331(7) . ? N2 C4 1.344(8) . ? N2 C2 1.363(8) . ? N3 C4 1.305(7) . ? N3 C3 1.464(8) . ? C1 C5 1.448(9) . ? C1 C3 1.492(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9300 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9300 . ? C5 C5 1.58(2) 2_655 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? 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 O5 Mo1 O9 104.2(3) . . ? O5 Mo1 O1 102.66(12) . 6 ? O9 Mo1 O1 98.82(13) . 6 ? O5 Mo1 O1 102.66(12) . . ? O9 Mo1 O1 98.82(13) . . ? O1 Mo1 O1 144.4(2) 6 . ? O5 Mo1 O8 90.4(3) . . ? O9 Mo1 O8 165.4(3) . . ? O1 Mo1 O8 77.58(13) 6 . ? O1 Mo1 O8 77.58(13) . . ? O5 Mo1 O3 160.4(3) . . ? O9 Mo1 O3 95.5(2) . . ? O1 Mo1 O3 73.85(12) 6 . ? O1 Mo1 O3 73.85(12) . . ? O8 Mo1 O3 69.93(18) . . ? O6 Mo2 O2 104.6(2) . . ? O6 Mo2 O1 101.32(19) . . ? O2 Mo2 O1 100.99(19) . . ? O6 Mo2 O4 96.49(18) . 6 ? O2 Mo2 O4 99.75(19) . 6 ? O1 Mo2 O4 148.17(16) . 6 ? O6 Mo2 O3 93.15(19) . . ? O2 Mo2 O3 161.9(2) . . ? O1 Mo2 O3 78.78(17) . . ? O4 Mo2 O3 74.05(16) 6 . ? O6 Mo2 O4 163.17(17) . 5_656 ? O2 Mo2 O4 89.57(18) . 5_656 ? O1 Mo2 O4 84.52(16) . 5_656 ? O4 Mo2 O4 71.74(15) 6 5_656 ? O3 Mo2 O4 72.34(16) . 5_656 ? O7 Mo3 O8 104.2(3) . 5_656 ? O7 Mo3 O4 101.64(12) . . ? O8 Mo3 O4 97.10(12) 5_656 . ? O7 Mo3 O4 101.64(12) . 6 ? O8 Mo3 O4 97.10(12) 5_656 6 ? O4 Mo3 O4 148.7(2) . 6 ? O7 Mo3 O3 98.8(3) . . ? O8 Mo3 O3 157.0(2) 5_656 . ? O4 Mo3 O3 78.04(11) . . ? O4 Mo3 O3 78.04(11) 6 . ? O7 Mo3 O3 174.1(2) . 5_656 ? O8 Mo3 O3 81.7(2) 5_656 5_656 ? O4 Mo3 O3 77.36(12) . 5_656 ? O4 Mo3 O3 77.36(12) 6 5_656 ? O3 Mo3 O3 75.4(2) . 5_656 ? N1 Cu1 N1 149.1(3) . 2_656 ? N1 Cu1 O2 98.4(2) . 2_656 ? N1 Cu1 O2 103.7(2) 2_656 2_656 ? N1 Cu1 O2 103.7(2) . . ? N1 Cu1 O2 98.4(2) 2_656 . ? O2 Cu1 O2 87.9(2) 2_656 . ? N2 Cu2 N2 179.8(3) . 2 ? Mo2 O1 Mo1 116.36(19) . . ? Mo2 O2 Cu1 141.9(3) . . ? Mo3 O3 Mo2 92.17(13) . 6 ? Mo3 O3 Mo2 92.17(13) . . ? Mo2 O3 Mo2 163.4(3) 6 . ? Mo3 O3 Mo3 104.6(2) . 5_656 ? Mo2 O3 Mo3 97.21(12) 6 5_656 ? Mo2 O3 Mo3 97.21(12) . 5_656 ? Mo3 O3 Mo1 163.8(3) . . ? Mo2 O3 Mo1 85.67(13) 6 . ? Mo2 O3 Mo1 85.67(13) . . ? Mo3 O3 Mo1 91.61(17) 5_656 . ? Mo3 O4 Mo2 108.89(18) . 6 ? Mo3 O4 Mo2 110.02(17) . 5_656 ? Mo2 O4 Mo2 104.30(15) 6 5_656 ? Mo3 O8 Mo1 116.8(3) 5_656 . ? C2 N1 N3 103.6(5) . . ? C2 N1 Cu1 129.6(5) . . ? N3 N1 Cu1 126.7(4) . . ? C4 N2 C2 101.6(5) . . ? C4 N2 Cu2 119.6(4) . . ? C2 N2 Cu2 136.5(5) . . ? C4 N3 N1 110.6(5) . . ? C4 N3 C3 126.4(6) . . ? N1 N3 C3 123.0(5) . . ? C5 C1 C3 114.8(9) . . ? C5 C1 H1A 108.6 . . ? C3 C1 H1A 108.6 . . ? C5 C1 H1B 108.6 . . ? C3 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? N1 C2 N2 113.8(6) . . ? N1 C2 H2A 123.1 . . ? N2 C2 H2A 123.1 . . ? N3 C3 C1 111.6(6) . . ? N3 C3 H3A 109.3 . . ? C1 C3 H3A 109.3 . . ? N3 C3 H3B 109.3 . . ? C1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? N3 C4 N2 110.3(6) . . ? N3 C4 H4A 124.8 . . ? N2 C4 H4A 124.8 . . ? C1 C5 C5 107.2(11) . 2_655 ? C1 C5 H5A 110.3 . . ? C5 C5 H5A 110.3 2_655 . ? C1 C5 H5B 110.3 . . ? C5 C5 H5B 110.3 2_655 . ? H5A C5 H5B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.422 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.143 # Attachment '- compound 3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 769068' #TrackingRef '- compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 Cu2 Mo8 N24 O26' _chemical_formula_weight 2191.78 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' Mo Mo -1.6832 0.6857 '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 12.481(3) _cell_length_b 12.862(4) _cell_length_c 13.332(4) _cell_angle_alpha 100.001(2) _cell_angle_beta 105.253(2) _cell_angle_gamma 111.736(3) _cell_volume 1828.1(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.1131 _exptl_crystal_size_mid 0.1120 _exptl_crystal_size_min 0.1109 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1074.0 _exptl_absorpt_coefficient_mu 1.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12658 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.75 _reflns_number_total 7005 _reflns_number_gt 4718 _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. During the refinement, the command 'isor' was used to restrain the non-H atoms (C1 C4) with ADP or NPD problems. Furthermore, the command 'dfix' was used for C1 C4, and C1 C2 to restrain their bond distance in the rational range. ; _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^)+(0.0264P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7005 _refine_ls_number_parameters 454 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.985 _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 Mo1 Mo 1.48872(4) 0.62622(3) 0.57642(3) 0.02063(11) Uani 1 1 d . . . Mo2 Mo 1.56060(4) 0.41058(4) 0.71731(3) 0.02196(11) Uani 1 1 d . . . Mo3 Mo 1.73202(4) 0.68694(4) 0.44849(3) 0.02212(11) Uani 1 1 d . . . Mo4 Mo 1.79973(4) 0.61046(4) 0.67744(4) 0.03234(13) Uani 1 1 d . . . Cu1 Cu 1.5000 0.5000 1.0000 0.0239(2) Uani 1 2 d S . . Cu2 Cu 2.0000 0.0000 1.5000 0.0234(2) Uani 1 2 d S . . O1 O 1.8947(3) 0.7516(4) 0.7500(3) 0.0546(12) Uani 1 1 d . . . O2 O 1.8810(4) 0.5342(4) 0.7077(3) 0.0558(12) Uani 1 1 d . . . O3 O 1.6865(3) 0.5650(3) 0.7501(3) 0.0280(8) Uani 1 1 d . . . O4 O 1.8412(3) 0.8284(3) 0.5140(3) 0.0328(8) Uani 1 1 d . . . O5 O 1.7959(3) 0.6042(3) 0.5332(3) 0.0289(8) Uani 1 1 d . . . O6 O 1.3925(3) 0.5865(3) 0.4383(3) 0.0342(9) Uani 1 1 d . . . O7 O 1.4087(3) 0.2868(3) 0.6140(3) 0.0248(8) Uani 1 1 d . . . O8 O 1.7656(3) 0.6498(3) 0.3361(3) 0.0320(8) Uani 1 1 d . . . O9 O 1.6404(3) 0.3334(3) 0.7524(3) 0.0338(9) Uani 1 1 d . . . O10 O 1.4710(4) 0.7321(3) 0.6552(3) 0.0542(12) Uani 1 1 d . . . O11 O 1.4432(3) 0.4998(3) 0.6236(3) 0.0349(9) Uani 1 1 d . . . O12 O 1.5149(3) 0.4399(3) 0.8247(3) 0.0303(8) Uani 1 1 d . . . O13 O 1.6464(3) 0.6761(3) 0.5874(3) 0.0311(8) Uani 1 1 d . . . N1 N 2.0958(5) -0.1088(4) 1.2331(4) 0.0540(15) Uani 1 1 d . . . N2 N 1.2180(5) 0.1598(4) 0.8728(4) 0.0678(17) Uani 1 1 d . . . N3 N 1.2287(4) 0.1846(4) 0.9782(4) 0.0451(13) Uani 1 1 d . . . N4 N 1.6925(4) 0.0015(5) 1.2930(5) 0.0642(17) Uani 1 1 d . . . N5 N 1.2608(5) 0.6544(5) 0.9195(4) 0.0653(17) Uani 1 1 d . . . N6 N 1.3883(4) 0.5706(3) 0.9371(3) 0.0268(10) Uani 1 1 d . . . N7 N 1.8687(4) 0.0232(3) 1.3942(3) 0.0258(10) Uani 1 1 d . . . N8 N 2.0684(4) -0.2039(3) 1.2699(4) 0.0326(11) Uani 1 1 d . . . N9 N 1.7767(5) 0.0820(5) 1.2643(5) 0.0652(17) Uani 1 1 d . . . N10 N 1.3553(4) 0.3447(3) 0.9654(3) 0.0289(10) Uani 1 1 d . . . N11 N 1.2808(4) 0.6315(4) 0.8261(3) 0.0310(10) Uani 1 1 d . . . N12 N 2.0321(4) -0.0827(3) 1.3744(3) 0.0256(10) Uani 1 1 d . . . C1 C 1.5074(7) 0.0112(9) 1.1814(9) 0.130(4) Uani 1 1 d DU . . H1A H 1.5523 0.0446 1.1367 0.156 Uiso 1 1 calc R . . H1B H 1.5222 0.0764 1.2408 0.156 Uiso 1 1 calc R . . C2 C 1.3743(6) -0.0432(8) 1.1144(7) 0.100(3) Uani 1 1 d D . . H2A H 1.3597 -0.0942 1.0445 0.120 Uiso 1 1 calc R . . H2B H 1.3273 -0.0908 1.1507 0.120 Uiso 1 1 calc R . . C3 C 1.3103(5) 0.2938(5) 1.0317(5) 0.0458(16) Uani 1 1 d . . . H3A H 1.3328 0.3296 1.1057 0.055 Uiso 1 1 calc R . . C4 C 1.5601(8) -0.0537(9) 1.2261(10) 0.140(4) Uani 1 1 d DU . . H4A H 1.5458 -0.1186 1.1667 0.168 Uiso 1 1 calc R . . H4B H 1.5152 -0.0873 1.2707 0.168 Uiso 1 1 calc R . . C5 C 1.8801(5) 0.0917(5) 1.3283(5) 0.0413(15) Uani 1 1 d . . . H5A H 1.9564 0.1421 1.3287 0.050 Uiso 1 1 calc R . . C6 C 1.0527(5) 0.5574(5) 0.5395(4) 0.0363(13) Uani 1 1 d . . . H6A H 1.0207 0.6138 0.5559 0.044 Uiso 1 1 calc R . . H6B H 1.1122 0.5889 0.5055 0.044 Uiso 1 1 calc R . . C7 C 1.2173(5) 0.6544(5) 0.7286(4) 0.0414(14) Uani 1 1 d . . . H7A H 1.2765 0.6936 0.6969 0.050 Uiso 1 1 calc R . . H7B H 1.1810 0.7058 0.7491 0.050 Uiso 1 1 calc R . . C8 C 1.2933(6) 0.2581(5) 0.8684(5) 0.0584(19) Uani 1 1 d . . . H8A H 1.3044 0.2689 0.8041 0.070 Uiso 1 1 calc R . . C9 C 1.7484(5) -0.0324(5) 1.3686(5) 0.0390(14) Uani 1 1 d . . . H9A H 1.7092 -0.0875 1.3997 0.047 Uiso 1 1 calc R . . C10 C 1.3333(6) 0.0454(7) 1.0973(7) 0.082(2) Uani 1 1 d . . . H10A H 1.3864 0.0968 1.0674 0.099 Uiso 1 1 calc R . . H10B H 1.3435 0.0923 1.1674 0.099 Uiso 1 1 calc R . . C11 C 2.0114(6) -0.3655(5) 1.1033(5) 0.0494(16) Uani 1 1 d . . . H11A H 2.0297 -0.3112 1.0611 0.059 Uiso 1 1 calc R . . H11B H 1.9250 -0.3928 1.0948 0.059 Uiso 1 1 calc R . . C12 C 1.3272(6) 0.6174(6) 0.9836(5) 0.062(2) Uani 1 1 d . . . H12A H 1.3317 0.6230 1.0553 0.074 Uiso 1 1 calc R . . C13 C 1.1589(6) 0.0928(5) 1.0204(6) 0.070(2) Uani 1 1 d . . . H13A H 1.0721 0.0571 0.9751 0.084 Uiso 1 1 calc R . . H13B H 1.1669 0.1294 1.0937 0.084 Uiso 1 1 calc R . . C14 C 2.0350(6) -0.4697(5) 1.0604(4) 0.0446(15) Uani 1 1 d . . . H14A H 2.1227 -0.4427 1.0749 0.053 Uiso 1 1 calc R . . H14B H 2.0112 -0.5260 1.0997 0.053 Uiso 1 1 calc R . . C15 C 2.0719(6) -0.0374(5) 1.2990(5) 0.0505(17) Uani 1 1 d . . . H15A H 2.0814 0.0365 1.2940 0.061 Uiso 1 1 calc R . . C16 C 2.0316(4) -0.1862(4) 1.3522(4) 0.0279(12) Uani 1 1 d . . . H16A H 2.0082 -0.2401 1.3898 0.033 Uiso 1 1 calc R . . C17 C 1.2017(5) -0.0007(5) 1.0228(5) 0.0488(16) Uani 1 1 d . . . H17A H 1.1937 -0.0376 0.9495 0.059 Uiso 1 1 calc R . . H17B H 1.1490 -0.0604 1.0464 0.059 Uiso 1 1 calc R . . C18 C 1.3568(5) 0.5824(5) 0.8374(4) 0.0347(13) Uani 1 1 d . . . H18A H 1.3847 0.5590 0.7835 0.042 Uiso 1 1 calc R . . C19 C 1.1172(5) 0.5403(5) 0.6454(4) 0.0375(14) Uani 1 1 d . . . H19A H 1.0563 0.5037 0.6766 0.045 Uiso 1 1 calc R . . H19B H 1.1534 0.4875 0.6291 0.045 Uiso 1 1 calc R . . C20 C 2.0903(5) -0.3034(5) 1.2213(5) 0.0414(15) Uani 1 1 d . . . H20A H 2.0746 -0.3594 1.2621 0.050 Uiso 1 1 calc R . . H20B H 2.1765 -0.2743 1.2286 0.050 Uiso 1 1 calc R . . 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 Mo1 0.0263(2) 0.0193(2) 0.0183(2) 0.00558(19) 0.0102(2) 0.01057(19) Mo2 0.0203(2) 0.0274(2) 0.0186(2) 0.0108(2) 0.0067(2) 0.00925(19) Mo3 0.0196(2) 0.0220(2) 0.0224(3) 0.0100(2) 0.0064(2) 0.00592(19) Mo4 0.0311(3) 0.0462(3) 0.0293(3) 0.0217(2) 0.0167(2) 0.0182(2) Cu1 0.0201(5) 0.0234(5) 0.0225(5) 0.0084(4) 0.0031(4) 0.0061(4) Cu2 0.0262(5) 0.0257(5) 0.0183(5) 0.0023(4) 0.0068(4) 0.0141(4) O1 0.036(2) 0.071(3) 0.042(3) 0.024(2) 0.014(2) 0.006(2) O2 0.059(3) 0.096(3) 0.051(3) 0.048(3) 0.035(2) 0.053(3) O3 0.0211(18) 0.031(2) 0.023(2) 0.0091(16) 0.0050(16) 0.0038(15) O4 0.028(2) 0.028(2) 0.031(2) 0.0095(17) 0.0043(18) 0.0036(16) O5 0.0240(19) 0.039(2) 0.035(2) 0.0212(18) 0.0157(18) 0.0170(16) O6 0.029(2) 0.054(2) 0.030(2) 0.0238(19) 0.0165(18) 0.0192(18) O7 0.0221(18) 0.0282(19) 0.025(2) 0.0095(16) 0.0088(16) 0.0105(15) O8 0.033(2) 0.038(2) 0.026(2) 0.0107(17) 0.0095(18) 0.0162(17) O9 0.033(2) 0.046(2) 0.031(2) 0.0190(18) 0.0114(18) 0.0227(18) O10 0.055(3) 0.043(2) 0.058(3) -0.009(2) 0.024(2) 0.023(2) O11 0.0243(19) 0.035(2) 0.039(2) 0.0215(18) 0.0041(18) 0.0071(16) O12 0.030(2) 0.035(2) 0.022(2) 0.0062(17) 0.0096(17) 0.0112(17) O13 0.0267(19) 0.041(2) 0.020(2) 0.0083(17) 0.0067(17) 0.0096(17) N1 0.094(4) 0.042(3) 0.044(3) 0.014(3) 0.043(3) 0.036(3) N2 0.077(4) 0.039(3) 0.039(4) 0.009(3) -0.002(3) -0.008(3) N3 0.036(3) 0.027(3) 0.070(4) 0.013(3) 0.033(3) 0.003(2) N4 0.023(3) 0.070(4) 0.096(5) 0.064(4) 0.005(3) 0.010(3) N5 0.083(4) 0.122(5) 0.044(4) 0.040(4) 0.036(3) 0.083(4) N6 0.028(2) 0.025(2) 0.026(3) 0.007(2) 0.007(2) 0.0124(19) N7 0.026(3) 0.023(2) 0.027(3) 0.009(2) 0.008(2) 0.011(2) N8 0.047(3) 0.023(2) 0.033(3) 0.005(2) 0.019(2) 0.019(2) N9 0.040(3) 0.071(4) 0.089(5) 0.062(4) 0.015(3) 0.019(3) N10 0.024(2) 0.024(2) 0.033(3) 0.010(2) 0.008(2) 0.0053(19) N11 0.032(3) 0.035(3) 0.025(3) 0.010(2) 0.005(2) 0.018(2) N12 0.030(2) 0.023(2) 0.021(2) -0.0011(19) 0.010(2) 0.0116(19) C1 0.067(5) 0.146(7) 0.162(8) 0.087(6) 0.024(5) 0.026(5) C2 0.028(4) 0.135(8) 0.126(8) 0.081(7) 0.001(5) 0.024(5) C3 0.054(4) 0.034(3) 0.038(4) -0.002(3) 0.028(3) 0.005(3) C4 0.079(6) 0.145(7) 0.184(8) 0.118(7) 0.019(6) 0.027(5) C5 0.029(3) 0.041(4) 0.055(4) 0.028(3) 0.013(3) 0.013(3) C6 0.036(3) 0.056(4) 0.024(3) 0.012(3) 0.007(3) 0.030(3) C7 0.040(3) 0.050(4) 0.031(4) 0.014(3) -0.001(3) 0.024(3) C8 0.076(5) 0.030(4) 0.028(4) 0.012(3) -0.004(3) -0.006(3) C9 0.030(3) 0.043(4) 0.046(4) 0.029(3) 0.008(3) 0.015(3) C10 0.047(5) 0.102(6) 0.071(6) 0.040(5) 0.005(4) 0.009(5) C11 0.063(4) 0.043(4) 0.038(4) -0.004(3) 0.009(3) 0.032(3) C12 0.077(5) 0.121(6) 0.032(4) 0.038(4) 0.032(4) 0.074(5) C13 0.067(5) 0.041(4) 0.104(6) 0.024(4) 0.058(5) 0.005(4) C14 0.056(4) 0.044(4) 0.038(4) 0.003(3) 0.017(3) 0.029(3) C15 0.091(5) 0.042(4) 0.039(4) 0.019(3) 0.035(4) 0.038(4) C16 0.032(3) 0.026(3) 0.023(3) 0.003(2) 0.014(3) 0.010(2) C17 0.038(4) 0.055(4) 0.056(4) 0.032(4) 0.018(3) 0.015(3) C18 0.053(4) 0.041(3) 0.020(3) 0.009(3) 0.011(3) 0.033(3) C19 0.038(3) 0.051(4) 0.032(3) 0.017(3) 0.009(3) 0.029(3) C20 0.058(4) 0.033(3) 0.041(4) 0.003(3) 0.022(3) 0.028(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 Mo1 O10 1.690(3) . ? Mo1 O6 1.775(4) . ? Mo1 O13 1.785(3) . ? Mo1 O11 1.795(3) . ? Mo2 O9 1.687(3) . ? Mo2 O12 1.708(3) . ? Mo2 O3 1.905(3) . ? Mo2 O7 1.912(3) . ? Mo2 O6 2.302(3) 2_866 ? Mo2 O11 2.409(3) . ? Mo3 O8 1.697(3) . ? Mo3 O4 1.708(3) . ? Mo3 O5 1.901(3) . ? Mo3 O7 1.913(3) 2_866 ? Mo3 O13 2.369(3) . ? Mo3 O11 2.383(3) 2_866 ? Mo4 O2 1.677(4) . ? Mo4 O1 1.682(4) . ? Mo4 O3 1.892(3) . ? Mo4 O5 1.898(3) . ? Mo4 O13 2.482(3) . ? Cu1 N10 2.008(4) . ? Cu1 N10 2.008(4) 2_867 ? Cu1 N6 2.014(4) 2_867 ? Cu1 N6 2.014(4) . ? Cu1 O12 2.409(3) . ? Cu1 O12 2.409(3) 2_867 ? Cu2 N7 2.014(4) 2_958 ? Cu2 N7 2.014(4) . ? Cu2 N12 2.036(3) . ? Cu2 N12 2.036(3) 2_958 ? Cu2 O4 2.436(3) 1_546 ? Cu2 O4 2.436(3) 2_967 ? O4 Cu2 2.436(3) 1_564 ? O6 Mo2 2.302(3) 2_866 ? O7 Mo3 1.913(3) 2_866 ? O11 Mo3 2.383(3) 2_866 ? N1 C15 1.329(6) . ? N1 N8 1.357(6) . ? N2 C8 1.288(7) . ? N2 N3 1.345(7) . ? N3 C3 1.315(6) . ? N3 C13 1.482(6) . ? N4 C9 1.304(7) . ? N4 N9 1.366(6) . ? N4 C4 1.471(10) . ? N5 C12 1.306(7) . ? N5 N11 1.338(6) . ? N6 C18 1.334(6) . ? N6 C12 1.338(6) . ? N7 C9 1.316(6) . ? N7 C5 1.345(6) . ? N8 C16 1.313(5) . ? N8 C20 1.482(6) . ? N9 C5 1.294(7) . ? N10 C3 1.310(6) . ? N10 C8 1.358(7) . ? N11 C18 1.313(6) . ? N11 C7 1.472(6) . ? N12 C16 1.309(6) . ? N12 C15 1.360(6) . ? C1 C4 1.363(8) . ? C1 C2 1.479(7) . ? C2 C10 1.439(11) . ? C6 C6 1.521(10) 2_766 ? C6 C19 1.526(7) . ? C7 C19 1.514(7) . ? C10 C17 1.501(9) . ? C11 C20 1.500(8) . ? C11 C14 1.524(7) . ? C13 C17 1.488(8) . ? C14 C14 1.512(11) 2_947 ? 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 O10 Mo1 O6 110.46(19) . . ? O10 Mo1 O13 110.07(17) . . ? O6 Mo1 O13 110.02(14) . . ? O10 Mo1 O11 107.93(18) . . ? O6 Mo1 O11 108.61(16) . . ? O13 Mo1 O11 109.72(15) . . ? O9 Mo2 O12 104.25(16) . . ? O9 Mo2 O3 103.50(15) . . ? O12 Mo2 O3 96.55(14) . . ? O9 Mo2 O7 100.29(15) . . ? O12 Mo2 O7 100.03(14) . . ? O3 Mo2 O7 146.54(14) . . ? O9 Mo2 O6 91.66(14) . 2_866 ? O12 Mo2 O6 163.46(14) . 2_866 ? O3 Mo2 O6 74.94(13) . 2_866 ? O7 Mo2 O6 81.23(12) . 2_866 ? O9 Mo2 O11 166.16(14) . . ? O12 Mo2 O11 88.82(14) . . ? O3 Mo2 O11 79.07(13) . . ? O7 Mo2 O11 72.46(12) . . ? O6 Mo2 O11 75.76(12) 2_866 . ? O8 Mo3 O4 103.19(15) . . ? O8 Mo3 O5 99.59(14) . . ? O4 Mo3 O5 101.48(16) . . ? O8 Mo3 O7 100.54(15) . 2_866 ? O4 Mo3 O7 100.23(15) . 2_866 ? O5 Mo3 O7 146.01(12) . 2_866 ? O8 Mo3 O13 162.42(14) . . ? O4 Mo3 O13 94.03(13) . . ? O5 Mo3 O13 73.14(12) . . ? O7 Mo3 O13 79.54(12) 2_866 . ? O8 Mo3 O11 87.25(14) . 2_866 ? O4 Mo3 O11 168.63(13) . 2_866 ? O5 Mo3 O11 80.87(13) . 2_866 ? O7 Mo3 O11 73.07(12) 2_866 2_866 ? O13 Mo3 O11 75.90(11) . 2_866 ? O2 Mo4 O1 106.2(2) . . ? O2 Mo4 O3 102.10(15) . . ? O1 Mo4 O3 103.47(15) . . ? O2 Mo4 O5 99.70(15) . . ? O1 Mo4 O5 103.86(16) . . ? O3 Mo4 O5 138.36(14) . . ? O2 Mo4 O13 164.28(18) . . ? O1 Mo4 O13 88.40(17) . . ? O3 Mo4 O13 79.53(12) . . ? O5 Mo4 O13 70.49(11) . . ? N10 Cu1 N10 180.0(2) . 2_867 ? N10 Cu1 N6 88.29(16) . 2_867 ? N10 Cu1 N6 91.71(16) 2_867 2_867 ? N10 Cu1 N6 91.71(16) . . ? N10 Cu1 N6 88.29(16) 2_867 . ? N6 Cu1 N6 180.000(2) 2_867 . ? N10 Cu1 O12 90.62(14) . . ? N10 Cu1 O12 89.38(14) 2_867 . ? N6 Cu1 O12 89.73(13) 2_867 . ? N6 Cu1 O12 90.27(13) . . ? N10 Cu1 O12 89.38(14) . 2_867 ? N10 Cu1 O12 90.62(14) 2_867 2_867 ? N6 Cu1 O12 90.27(13) 2_867 2_867 ? N6 Cu1 O12 89.73(13) . 2_867 ? O12 Cu1 O12 180.000(1) . 2_867 ? N7 Cu2 N7 180.000(3) 2_958 . ? N7 Cu2 N12 89.30(16) 2_958 . ? N7 Cu2 N12 90.70(16) . . ? N7 Cu2 N12 90.70(16) 2_958 2_958 ? N7 Cu2 N12 89.30(16) . 2_958 ? N12 Cu2 N12 180.000(2) . 2_958 ? N7 Cu2 O4 90.00(13) 2_958 1_546 ? N7 Cu2 O4 90.00(13) . 1_546 ? N12 Cu2 O4 98.26(13) . 1_546 ? N12 Cu2 O4 81.74(13) 2_958 1_546 ? N7 Cu2 O4 90.00(13) 2_958 2_967 ? N7 Cu2 O4 90.00(13) . 2_967 ? N12 Cu2 O4 81.74(13) . 2_967 ? N12 Cu2 O4 98.26(13) 2_958 2_967 ? O4 Cu2 O4 180.000(1) 1_546 2_967 ? Mo4 O3 Mo2 125.76(17) . . ? Mo3 O4 Cu2 145.79(18) . 1_564 ? Mo4 O5 Mo3 124.46(16) . . ? Mo1 O6 Mo2 131.03(16) . 2_866 ? Mo2 O7 Mo3 122.03(16) . 2_866 ? Mo1 O11 Mo3 133.26(18) . 2_866 ? Mo1 O11 Mo2 131.83(16) . . ? Mo3 O11 Mo2 88.56(11) 2_866 . ? Mo2 O12 Cu1 166.94(19) . . ? Mo1 O13 Mo3 129.47(17) . . ? Mo1 O13 Mo4 128.42(16) . . ? Mo3 O13 Mo4 87.72(10) . . ? C15 N1 N8 102.3(4) . . ? C8 N2 N3 102.6(5) . . ? C3 N3 N2 110.3(4) . . ? C3 N3 C13 128.9(6) . . ? N2 N3 C13 120.7(5) . . ? C9 N4 N9 110.4(5) . . ? C9 N4 C4 127.5(5) . . ? N9 N4 C4 120.7(6) . . ? C12 N5 N11 104.2(4) . . ? C18 N6 C12 102.4(4) . . ? C18 N6 Cu1 128.4(3) . . ? C12 N6 Cu1 129.2(4) . . ? C9 N7 C5 103.3(4) . . ? C9 N7 Cu2 127.1(3) . . ? C5 N7 Cu2 129.5(3) . . ? C16 N8 N1 110.0(4) . . ? C16 N8 C20 130.2(4) . . ? N1 N8 C20 119.6(4) . . ? C5 N9 N4 101.9(5) . . ? C3 N10 C8 102.5(4) . . ? C3 N10 Cu1 129.3(4) . . ? C8 N10 Cu1 127.4(3) . . ? C18 N11 N5 108.8(4) . . ? C18 N11 C7 129.0(4) . . ? N5 N11 C7 122.0(4) . . ? C16 N12 C15 103.0(4) . . ? C16 N12 Cu2 129.4(3) . . ? C15 N12 Cu2 127.3(3) . . ? C4 C1 C2 120.6(9) . . ? C10 C2 C1 110.7(8) . . ? N10 C3 N3 110.0(5) . . ? C1 C4 N4 120.1(8) . . ? N9 C5 N7 114.8(5) . . ? C6 C6 C19 111.6(5) 2_766 . ? N11 C7 C19 110.3(4) . . ? N2 C8 N10 114.7(5) . . ? N4 C9 N7 109.7(4) . . ? C2 C10 C17 115.0(7) . . ? C20 C11 C14 110.7(5) . . ? N5 C12 N6 114.0(5) . . ? N3 C13 C17 113.3(5) . . ? C14 C14 C11 113.0(6) 2_947 . ? N1 C15 N12 113.6(5) . . ? N12 C16 N8 111.1(4) . . ? C13 C17 C10 112.7(6) . . ? N11 C18 N6 110.7(4) . . ? C7 C19 C6 112.8(4) . . ? N8 C20 C11 113.7(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.390 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.112 data_compound1 _database_code_depnum_ccdc_archive 'CCDC 776980' #TrackingRef '- compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H64 Cu4 Mo8 N24 O26' _chemical_formula_weight 2318.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mo Mo -1.6832 0.6857 '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 10.850(1) _cell_length_b 12.843(1) _cell_length_c 14.740(1) _cell_angle_alpha 112.112(5) _cell_angle_beta 100.830(4) _cell_angle_gamma 98.902(4) _cell_volume 1810.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.1122 _exptl_crystal_size_mid 0.1116 _exptl_crystal_size_min 0.1110 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132.0 _exptl_absorpt_coefficient_mu 2.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 0.757 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12072 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.1997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 25.75 _reflns_number_total 6924 _reflns_number_gt 2722 _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. During the refinement, the command 'isor' was used to restrain the non-H atoms (C1 C2 C4' C5 C10 C17' C17 N3 N3') with ADP or NPD problems. The command 'Flat' was used to restrain the atoms (N3 C4 N1 C3 N2) in a plane, and the command 'Flat' was also used to restrain the atoms (N3' C4' N1 C3 N2') in a plane. Furthermore, the command 'dfix' was used for N1 C4', N12 C1, C1 C2, N4 C6, C2 C5, and C9 C6 to restrain their bond distance in the rational range. ; _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^)+(0.0105P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6924 _refine_ls_number_parameters 492 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.1646 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.043 _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 Mo1 Mo 0.33904(7) 0.47634(8) 0.50679(6) 0.0237(2) Uani 1 1 d . . . Mo2 Mo 0.55385(9) 0.49439(11) 0.69746(8) 0.0654(4) Uani 1 1 d . . . Mo3 Mo 0.63659(12) 0.27848(13) 0.53798(13) 0.0956(6) Uani 1 1 d . . . Mo4 Mo 0.58080(10) 0.73655(10) 0.65107(8) 0.0681(4) Uani 1 1 d . . . Cu1 Cu 0.99126(15) 0.37849(18) -0.47556(12) 0.0797(5) Uani 1 1 d . . . Cu2 Cu 0.70332(18) 1.00680(18) 0.59679(13) 0.1022(7) Uani 1 1 d . A . O1 O 0.5211(9) 0.1805(9) 0.5482(10) 0.141(5) Uani 1 1 d . . . O2 O 0.7716(10) 0.2291(11) 0.5473(11) 0.170(6) Uani 1 1 d . . . O3 O 0.6087(8) 0.8019(8) 0.7779(6) 0.115(4) Uani 1 1 d . . . O4 O 0.6738(7) 0.4042(10) 0.6681(8) 0.115(4) Uani 1 1 d . . . O5 O 0.4294(7) 0.7740(7) 0.6113(6) 0.080(3) Uani 1 1 d . . . O6 O 0.6312(7) 0.5966(9) 0.8171(5) 0.106(3) Uani 1 1 d . . . O7 O 0.5003(5) 0.4016(5) 0.5180(5) 0.0374(17) Uani 1 1 d . . . O8 O 0.4391(5) 0.5804(6) 0.6459(4) 0.043(2) Uani 1 1 d . . . O9 O 0.6907(7) 0.8235(6) 0.6222(6) 0.080(3) Uani 1 1 d . . . O10 O 0.4350(6) 0.4007(8) 0.7098(6) 0.080(3) Uani 1 1 d . . . O11 O 0.6742(5) 0.6112(6) 0.6363(4) 0.044(2) Uani 1 1 d . . . O12 O 0.7479(5) 0.4249(7) 0.5101(5) 0.051(2) Uani 1 1 d . . . O13 O 0.2359(6) 0.3839(6) 0.5297(4) 0.045(2) Uani 1 1 d . . . N1 N 0.7637(15) 0.9562(12) 0.4864(11) 0.159(7) Uani 1 1 d D . . N2 N 0.872(2) 0.850(2) 0.3813(16) 0.099(9) Uani 0.551(15) 1 d PD A 1 N2' N 0.766(2) 0.843(2) 0.3273(18) 0.069(7) Uiso 0.449(15) 1 d PD A 2 N3 N 0.946(2) 0.963(2) 0.4182(16) 0.096(8) Uani 0.551(15) 1 d PDU A 1 N3' N 0.736(3) 0.943(4) 0.317(3) 0.189(16) Uani 0.449(15) 1 d PDU A 2 N4 N 0.624(3) 1.2050(18) 0.8512(19) 0.216(13) Uani 1 1 d D . . N5 N 0.686(3) 1.1540(19) 0.8879(13) 0.179(10) Uani 1 1 d . . . N6 N 0.6768(13) 1.0887(10) 0.7252(9) 0.102(4) Uani 1 1 d . . . N7 N 1.1574(9) 0.6063(10) -0.1802(8) 0.086(4) Uani 1 1 d . . . N8 N 1.0407(8) 0.4871(9) -0.3389(6) 0.066(3) Uani 1 1 d . . . N9 N 1.0306(9) 0.6079(9) -0.1945(7) 0.060(3) Uani 1 1 d . . . N10 N 0.9419(9) 0.2659(9) -0.6081(7) 0.069(3) Uani 1 1 d . . . N11 N 0.9483(14) 0.1383(12) -0.7563(8) 0.113(4) Uani 1 1 d . . . N12 N 0.8308(11) 0.1615(16) -0.7591(12) 0.140(7) Uani 1 1 d D . . C1 C 0.7272(19) 0.132(2) -0.8576(12) 0.216(10) Uani 1 1 d DU . . H1A H 0.6684 0.1820 -0.8456 0.260 Uiso 1 1 calc R . . H1B H 0.7667 0.1392 -0.9094 0.260 Uiso 1 1 calc R . . C2 C 0.659(2) 0.011(2) -0.8883(15) 0.250(11) Uani 1 1 d DU . . H2A H 0.6209 0.0030 -0.8359 0.300 Uiso 1 1 calc R . . H2B H 0.7175 -0.0398 -0.9014 0.300 Uiso 1 1 calc R . . C3 C 0.7743(14) 0.8499(13) 0.4293(10) 0.104(5) Uani 1 1 d D A . H3 H 0.7208 0.7820 0.4228 0.125 Uiso 1 1 calc R B 1 C4 C 0.878(3) 1.019(2) 0.4780(17) 0.114(12) Uani 0.551(15) 1 d PD A 1 H4 H 0.9055 1.0996 0.5142 0.137 Uiso 0.551(15) 1 calc PR A 1 C4' C 0.738(3) 1.005(5) 0.424(4) 0.24(3) Uani 0.449(15) 1 d PDU A 2 H4' H 0.7216 1.0781 0.4467 0.291 Uiso 0.449(15) 1 calc PR A 2 C5 C 0.5525(14) -0.0192(16) -0.9866(13) 0.141(7) Uani 1 1 d DU . . H5A H 0.6020 -0.0132 -1.0335 0.170 Uiso 1 1 calc R . . H5B H 0.5164 -0.1017 -1.0098 0.170 Uiso 1 1 calc R . . C6 C 0.534(2) 1.2685(17) 0.903(2) 0.316(19) Uani 1 1 d D . . H6A H 0.4510 1.2508 0.8555 0.379 Uiso 1 1 calc R . . H6B H 0.5205 1.2469 0.9578 0.379 Uiso 1 1 calc R . . C7 C 0.7239(19) 1.0835(17) 0.8157(19) 0.137(7) Uani 1 1 d . A . H7 H 0.7768 1.0356 0.8245 0.165 Uiso 1 1 calc R . . C8 C 0.5287(17) 1.4667(15) 1.0126(12) 0.147(8) Uani 1 1 d . . . H8A H 0.4656 1.4161 1.0261 0.177 Uiso 1 1 calc R . . H8B H 0.5929 1.5145 1.0769 0.177 Uiso 1 1 calc R . . C9 C 0.5973(17) 1.3894(17) 0.9433(12) 0.134(7) Uani 1 1 d D . . H9A H 0.6002 1.4110 0.8872 0.160 Uiso 1 1 calc R . . H9B H 0.6858 1.4024 0.9812 0.160 Uiso 1 1 calc R . . C10 C 0.6124(15) 1.1596(15) 0.7549(14) 0.118(6) Uani 1 1 d U A . H10 H 0.5583 1.1792 0.7103 0.142 Uiso 1 1 calc R . . C11 C 0.912(2) 0.7792(15) 0.2316(15) 0.183(10) Uani 1 1 d . . . H11A H 0.9799 0.8492 0.2541 0.219 Uiso 1 1 calc R A 1 H11B H 0.8313 0.7968 0.2084 0.219 Uiso 1 1 calc R A 1 C12 C 0.9821(13) 0.6790(13) -0.1095(11) 0.109(5) Uani 1 1 d . . . H12A H 1.0390 0.7565 -0.0764 0.130 Uiso 1 1 calc R . . H12B H 0.8970 0.6856 -0.1380 0.130 Uiso 1 1 calc R . . C13 C 0.9663(11) 0.5423(12) -0.2871(9) 0.070(4) Uani 1 1 d . . . H13 H 0.8790 0.5347 -0.3140 0.084 Uiso 1 1 calc R . . C14 C 0.9285(15) 0.7138(12) 0.0499(12) 0.130(6) Uani 1 1 d . . . H14A H 0.9796 0.7923 0.0722 0.156 Uiso 1 1 calc R A . H14B H 0.8393 0.7122 0.0227 0.156 Uiso 1 1 calc R . . C15 C 0.9359(15) 0.6886(13) 0.1381(10) 0.129(7) Uani 1 1 d . A . H15A H 1.0212 0.6768 0.1581 0.155 Uiso 1 1 calc R . . H15B H 0.8734 0.6158 0.1180 0.155 Uiso 1 1 calc R . . C16 C 0.9728(14) 0.6356(13) -0.0339(10) 0.101(5) Uani 1 1 d . A . H16A H 1.0570 0.6268 -0.0060 0.122 Uiso 1 1 calc R . . H16B H 0.9127 0.5597 -0.0655 0.122 Uiso 1 1 calc R . . C17 C 0.905(3) 0.762(2) 0.309(2) 0.092(9) Uani 0.551(15) 1 d PU A 1 H17A H 0.9888 0.7535 0.3391 0.111 Uiso 0.551(15) 1 calc PR A 1 H17B H 0.8420 0.6893 0.2883 0.111 Uiso 0.551(15) 1 calc PR A 1 C17' C 0.797(3) 0.752(2) 0.248(2) 0.069(9) Uani 0.449(15) 1 d PU A 2 H17C H 0.7938 0.6856 0.2643 0.083 Uiso 0.449(15) 1 calc PR A 2 H17D H 0.7310 0.7285 0.1847 0.083 Uiso 0.449(15) 1 calc PR A 2 C18 C 1.0159(12) 0.2056(12) -0.6639(10) 0.085(5) Uani 1 1 d . . . H18 H 1.1033 0.2121 -0.6386 0.102 Uiso 1 1 calc R . . C19 C 1.1588(11) 0.5334(13) -0.2697(10) 0.083(5) Uani 1 1 d . . . H19 H 1.2340 0.5146 -0.2849 0.099 Uiso 1 1 calc R . . C20 C 0.8318(14) 0.2321(16) -0.6732(11) 0.103(6) Uani 1 1 d . . . H20 H 0.7595 0.2577 -0.6581 0.124 Uiso 1 1 calc R . . 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 Mo1 0.0165(4) 0.0320(7) 0.0219(5) 0.0109(4) 0.0060(4) 0.0044(4) Mo2 0.0381(6) 0.1225(12) 0.0483(7) 0.0533(8) 0.0114(5) 0.0099(7) Mo3 0.0743(9) 0.1091(13) 0.1823(16) 0.1131(13) 0.0742(11) 0.0564(9) Mo4 0.0579(7) 0.0455(9) 0.0767(8) -0.0039(7) 0.0394(7) -0.0034(6) Cu1 0.0594(8) 0.1214(14) 0.0406(8) 0.0244(9) 0.0072(7) 0.0060(9) Cu2 0.1242(15) 0.1017(18) 0.0755(12) 0.0168(12) 0.0566(12) 0.0301(13) O1 0.143(8) 0.124(10) 0.276(13) 0.149(10) 0.141(10) 0.090(8) O2 0.142(9) 0.190(13) 0.325(17) 0.210(13) 0.116(11) 0.117(10) O3 0.114(7) 0.087(8) 0.078(6) -0.035(6) 0.065(6) -0.026(6) O4 0.046(5) 0.252(13) 0.178(10) 0.191(11) 0.069(6) 0.084(7) O5 0.077(6) 0.073(7) 0.114(7) 0.037(6) 0.068(6) 0.039(5) O6 0.078(6) 0.180(10) 0.032(5) 0.043(6) -0.002(4) -0.024(6) O7 0.026(3) 0.025(5) 0.050(4) 0.012(4) 0.003(3) -0.006(3) O8 0.037(4) 0.059(6) 0.020(4) 0.005(4) 0.007(3) 0.002(4) O9 0.064(5) 0.035(6) 0.112(7) -0.001(5) 0.047(5) -0.012(4) O10 0.053(5) 0.133(9) 0.083(6) 0.080(6) 0.028(4) 0.007(5) O11 0.030(4) 0.060(6) 0.018(4) -0.002(4) 0.003(3) -0.006(4) O12 0.027(4) 0.081(6) 0.057(5) 0.036(5) 0.015(4) 0.018(4) O13 0.044(4) 0.058(6) 0.030(4) 0.017(4) 0.014(3) 0.009(4) N1 0.271(18) 0.065(11) 0.189(14) 0.052(11) 0.185(15) 0.023(12) N2 0.083(17) 0.094(19) 0.091(17) 0.003(14) 0.060(16) -0.012(14) N3 0.096(11) 0.090(12) 0.096(11) 0.023(8) 0.050(8) 0.021(8) N3' 0.220(19) 0.193(19) 0.175(18) 0.110(12) 0.049(11) 0.031(10) N4 0.42(3) 0.15(2) 0.21(2) 0.107(17) 0.26(2) 0.156(19) N5 0.32(3) 0.087(16) 0.079(13) -0.006(11) 0.080(15) -0.027(15) N6 0.154(11) 0.084(10) 0.078(9) 0.014(8) 0.075(9) 0.057(9) N7 0.049(6) 0.139(12) 0.058(7) 0.031(8) 0.018(6) 0.015(7) N8 0.029(5) 0.126(10) 0.034(6) 0.026(6) 0.003(5) 0.019(6) N9 0.057(6) 0.079(8) 0.039(6) 0.016(6) 0.019(6) 0.019(6) N10 0.050(6) 0.094(9) 0.028(6) 0.011(6) -0.008(5) -0.023(6) N11 0.116(11) 0.136(13) 0.029(7) -0.004(8) 0.008(7) -0.009(9) N12 0.031(6) 0.27(2) 0.102(12) 0.097(14) -0.017(7) -0.020(9) C1 0.229(13) 0.227(13) 0.181(12) 0.075(9) 0.065(10) 0.037(9) C2 0.276(14) 0.272(15) 0.205(13) 0.110(10) 0.089(10) 0.022(9) C3 0.146(13) 0.063(12) 0.095(12) 0.003(10) 0.083(11) 0.014(10) C4 0.18(3) 0.05(2) 0.10(2) 0.010(17) 0.08(3) 0.01(2) C4' 0.24(3) 0.24(3) 0.24(3) 0.087(16) 0.079(13) 0.059(13) C5 0.138(10) 0.156(11) 0.107(9) 0.050(8) 0.010(8) 0.010(8) C6 0.44(4) 0.11(2) 0.40(4) 0.01(3) 0.35(4) 0.05(3) C7 0.187(19) 0.095(17) 0.111(17) 0.049(15) 0.007(15) 0.008(14) C8 0.24(2) 0.18(2) 0.135(14) 0.109(13) 0.126(15) 0.166(16) C9 0.22(2) 0.130(17) 0.111(14) 0.072(13) 0.093(15) 0.095(17) C10 0.132(9) 0.118(10) 0.121(9) 0.038(7) 0.081(8) 0.049(8) C11 0.28(2) 0.086(15) 0.179(19) 0.002(14) 0.184(19) 0.013(15) C12 0.090(10) 0.117(14) 0.105(12) 0.021(11) 0.044(10) 0.031(10) C13 0.056(8) 0.099(12) 0.049(8) 0.027(9) 0.007(8) 0.024(8) C14 0.184(15) 0.092(13) 0.156(15) 0.041(12) 0.144(14) 0.059(12) C15 0.190(16) 0.122(15) 0.090(12) 0.026(11) 0.105(13) 0.042(13) C16 0.140(13) 0.117(13) 0.074(9) 0.041(9) 0.080(10) 0.043(10) C17 0.100(12) 0.090(13) 0.085(12) 0.033(9) 0.030(9) 0.018(9) C17' 0.067(11) 0.066(12) 0.071(12) 0.013(8) 0.039(9) 0.026(9) C18 0.064(8) 0.116(14) 0.038(8) 0.007(9) 0.013(8) -0.013(9) C19 0.053(8) 0.144(15) 0.053(9) 0.038(10) 0.028(8) 0.023(9) C20 0.077(11) 0.184(19) 0.024(8) 0.037(11) 0.000(8) -0.004(11) _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 Mo1 O13 1.676(7) . ? Mo1 O12 1.755(6) 2_666 ? Mo1 O11 1.945(5) 2_666 ? Mo1 O8 1.955(6) . ? Mo1 O7 2.130(6) . ? Mo1 O7 2.336(6) 2_666 ? Mo1 Mo2 3.2039(16) . ? Mo1 Mo4 3.2175(15) 2_666 ? Mo2 O6 1.702(8) . ? Mo2 O10 1.708(7) . ? Mo2 O4 1.877(8) . ? Mo2 O8 2.012(6) . ? Mo2 O7 2.364(6) . ? Mo2 O11 2.371(7) . ? Mo3 O2 1.686(8) . ? Mo3 O1 1.703(9) . ? Mo3 O4 1.904(11) . ? Mo3 O5 1.988(8) 2_666 ? Mo3 O12 2.287(7) . ? Mo3 O7 2.385(6) . ? Mo3 Mo4 3.217(2) 2_666 ? Mo4 O3 1.679(8) . ? Mo4 O9 1.728(7) . ? Mo4 O5 1.835(7) . ? Mo4 O11 1.998(6) . ? Mo4 O8 2.298(7) . ? Mo4 O7 2.345(6) 2_666 ? Mo4 Mo3 3.217(2) 2_666 ? Mo4 Mo1 3.2175(15) 2_666 ? Cu1 N10 1.854(9) . ? Cu1 N8 1.881(9) . ? Cu2 N1 1.798(11) . ? Cu2 N6 1.890(9) . ? O5 Mo3 1.988(8) 2_666 ? O7 Mo1 2.336(6) 2_666 ? O7 Mo4 2.345(6) 2_666 ? O11 Mo1 1.945(5) 2_666 ? O12 Mo1 1.755(6) 2_666 ? N1 C4' 1.311(10) . ? N1 C3 1.344(16) . ? N1 C4 1.43(3) . ? N2 C3 1.378(19) . ? N2 N3 1.39(3) . ? N2 C17 1.39(3) . ? N2' N3' 1.43(4) . ? N2' C17' 1.45(3) . ? N2' C3 1.46(2) . ? N3 C4 1.32(2) . ? N3' C4' 1.47(6) . ? N4 N5 1.20(2) . ? N4 C10 1.29(2) . ? N4 C6 1.508(10) . ? N5 C7 1.30(2) . ? N6 C10 1.234(15) . ? N6 C7 1.367(19) . ? N7 C19 1.302(13) . ? N7 N9 1.358(10) . ? N8 C13 1.318(11) . ? N8 C19 1.361(13) . ? N9 C13 1.286(13) . ? N9 C12 1.489(13) . ? N10 C20 1.277(14) . ? N10 C18 1.371(12) . ? N11 C18 1.298(14) . ? N11 N12 1.349(14) . ? N12 C20 1.246(17) . ? N12 C1 1.534(10) . ? C1 C2 1.468(10) . ? C2 C5 1.547(10) . ? C5 C5 1.36(2) 2_653 ? C6 C9 1.435(10) . ? C7 C10 1.96(2) . ? C8 C8 1.26(2) 2_687 ? C8 C9 1.528(16) . ? C11 C17 1.25(3) . ? C11 C17' 1.33(3) . ? C11 C15 1.531(16) . ? C12 C16 1.434(16) . ? C14 C15 1.444(17) . ? C14 C16 1.485(14) . ? 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 O13 Mo1 O12 104.8(3) . 2_666 ? O13 Mo1 O11 101.9(3) . 2_666 ? O12 Mo1 O11 96.4(3) 2_666 2_666 ? O13 Mo1 O8 100.0(3) . . ? O12 Mo1 O8 95.0(3) 2_666 . ? O11 Mo1 O8 151.8(2) 2_666 . ? O13 Mo1 O7 97.8(3) . . ? O12 Mo1 O7 157.3(3) 2_666 . ? O11 Mo1 O7 79.4(2) 2_666 . ? O8 Mo1 O7 80.2(2) . . ? O13 Mo1 O7 174.1(3) . 2_666 ? O12 Mo1 O7 80.7(3) 2_666 2_666 ? O11 Mo1 O7 79.0(2) 2_666 2_666 ? O8 Mo1 O7 77.5(2) . 2_666 ? O7 Mo1 O7 76.6(3) . 2_666 ? O13 Mo1 Mo2 87.8(2) . . ? O12 Mo1 Mo2 131.7(2) 2_666 . ? O11 Mo1 Mo2 126.89(18) 2_666 . ? O8 Mo1 Mo2 36.74(19) . . ? O7 Mo1 Mo2 47.53(17) . . ? O7 Mo1 Mo2 87.06(15) 2_666 . ? O13 Mo1 Mo4 90.7(2) . 2_666 ? O12 Mo1 Mo4 132.2(2) 2_666 2_666 ? O11 Mo1 Mo4 35.87(19) 2_666 2_666 ? O8 Mo1 Mo4 126.96(17) . 2_666 ? O7 Mo1 Mo4 46.76(17) . 2_666 ? O7 Mo1 Mo4 86.74(15) 2_666 2_666 ? Mo2 Mo1 Mo4 92.98(5) . 2_666 ? O6 Mo2 O10 106.3(4) . . ? O6 Mo2 O4 102.4(4) . . ? O10 Mo2 O4 101.2(4) . . ? O6 Mo2 O8 100.9(4) . . ? O10 Mo2 O8 97.2(3) . . ? O4 Mo2 O8 144.7(3) . . ? O6 Mo2 O7 158.2(3) . . ? O10 Mo2 O7 95.4(3) . . ? O4 Mo2 O7 74.9(3) . . ? O8 Mo2 O7 73.6(2) . . ? O6 Mo2 O11 87.5(3) . . ? O10 Mo2 O11 163.6(3) . . ? O4 Mo2 O11 84.0(3) . . ? O8 Mo2 O11 70.9(2) . . ? O7 Mo2 O11 70.70(19) . . ? O6 Mo2 Mo1 136.5(3) . . ? O10 Mo2 Mo1 85.4(2) . . ? O4 Mo2 Mo1 116.5(3) . . ? O8 Mo2 Mo1 35.54(18) . . ? O7 Mo2 Mo1 41.67(14) . . ? O11 Mo2 Mo1 78.37(15) . . ? O2 Mo3 O1 105.4(5) . . ? O2 Mo3 O4 101.9(5) . . ? O1 Mo3 O4 100.7(5) . . ? O2 Mo3 O5 102.2(5) . 2_666 ? O1 Mo3 O5 96.1(5) . 2_666 ? O4 Mo3 O5 145.7(3) . 2_666 ? O2 Mo3 O12 88.5(4) . . ? O1 Mo3 O12 165.7(3) . . ? O4 Mo3 O12 79.3(3) . . ? O5 Mo3 O12 77.2(3) 2_666 . ? O2 Mo3 O7 158.7(4) . . ? O1 Mo3 O7 95.9(3) . . ? O4 Mo3 O7 73.9(2) . . ? O5 Mo3 O7 74.8(2) 2_666 . ? O12 Mo3 O7 70.19(19) . . ? O2 Mo3 Mo4 133.4(5) . 2_666 ? O1 Mo3 Mo4 86.0(4) . 2_666 ? O4 Mo3 Mo4 120.5(2) . 2_666 ? O5 Mo3 Mo4 31.26(17) 2_666 2_666 ? O12 Mo3 Mo4 81.80(16) . 2_666 ? O7 Mo3 Mo4 46.62(15) . 2_666 ? O3 Mo4 O9 105.0(4) . . ? O3 Mo4 O5 100.1(4) . . ? O9 Mo4 O5 101.9(4) . . ? O3 Mo4 O11 101.2(4) . . ? O9 Mo4 O11 96.8(3) . . ? O5 Mo4 O11 146.8(3) . . ? O3 Mo4 O8 90.2(3) . . ? O9 Mo4 O8 163.2(3) . . ? O5 Mo4 O8 82.0(3) . . ? O11 Mo4 O8 72.8(2) . . ? O3 Mo4 O7 161.4(3) . 2_666 ? O9 Mo4 O7 93.4(3) . 2_666 ? O5 Mo4 O7 78.5(3) . 2_666 ? O11 Mo4 O7 73.3(2) . 2_666 ? O8 Mo4 O7 71.2(2) . 2_666 ? O3 Mo4 Mo3 134.2(3) . 2_666 ? O9 Mo4 Mo3 88.2(3) . 2_666 ? O5 Mo4 Mo3 34.2(2) . 2_666 ? O11 Mo4 Mo3 120.92(17) . 2_666 ? O8 Mo4 Mo3 86.13(16) . 2_666 ? O7 Mo4 Mo3 47.66(15) 2_666 2_666 ? O3 Mo4 Mo1 135.9(3) . 2_666 ? O9 Mo4 Mo1 85.3(2) . 2_666 ? O5 Mo4 Mo1 119.9(3) . 2_666 ? O11 Mo4 Mo1 34.78(16) . 2_666 ? O8 Mo4 Mo1 78.71(14) . 2_666 ? O7 Mo4 Mo1 41.44(14) 2_666 2_666 ? Mo3 Mo4 Mo1 87.92(5) 2_666 2_666 ? N10 Cu1 N8 177.3(5) . . ? N1 Cu2 N6 166.2(6) . . ? Mo2 O4 Mo3 119.6(4) . . ? Mo4 O5 Mo3 114.5(3) . 2_666 ? Mo1 O7 Mo1 103.4(2) . 2_666 ? Mo1 O7 Mo4 91.8(2) . 2_666 ? Mo1 O7 Mo4 97.6(2) 2_666 2_666 ? Mo1 O7 Mo2 90.8(2) . . ? Mo1 O7 Mo2 98.0(2) 2_666 . ? Mo4 O7 Mo2 163.0(3) 2_666 . ? Mo1 O7 Mo3 163.2(3) . . ? Mo1 O7 Mo3 93.35(19) 2_666 . ? Mo4 O7 Mo3 85.7(2) 2_666 . ? Mo2 O7 Mo3 87.0(2) . . ? Mo1 O8 Mo2 107.7(3) . . ? Mo1 O8 Mo4 111.6(3) . . ? Mo2 O8 Mo4 104.3(2) . . ? Mo1 O11 Mo4 109.4(3) 2_666 . ? Mo1 O11 Mo2 110.2(3) 2_666 . ? Mo4 O11 Mo2 102.2(2) . . ? Mo1 O12 Mo3 115.7(3) 2_666 . ? C4' N1 C3 106(3) . . ? C4' N1 C4 67.5(14) . . ? C3 N1 C4 96.6(14) . . ? C4' N1 Cu2 115(3) . . ? C3 N1 Cu2 130.8(11) . . ? C4 N1 Cu2 122.9(13) . . ? C3 N2 N3 108.8(17) . . ? C3 N2 C17 132(2) . . ? N3 N2 C17 119.2(19) . . ? N3' N2' C17' 123(3) . . ? N3' N2' C3 112(2) . . ? C17' N2' C3 125(2) . . ? C4 N3 N2 100(2) . . ? N2' N3' C4' 95(3) . . ? N5 N4 C10 107.7(17) . . ? N5 N4 C6 121(3) . . ? C10 N4 C6 126(3) . . ? N4 N5 C7 106.6(19) . . ? C10 N6 C7 97.7(13) . . ? C10 N6 Cu2 133.0(14) . . ? C7 N6 Cu2 129.2(15) . . ? C19 N7 N9 101.9(10) . . ? C13 N8 C19 101.9(10) . . ? C13 N8 Cu1 127.2(8) . . ? C19 N8 Cu1 130.8(8) . . ? C13 N9 N7 110.7(9) . . ? C13 N9 C12 128.3(10) . . ? N7 N9 C12 121.0(10) . . ? C20 N10 C18 102.5(11) . . ? C20 N10 Cu1 128.2(11) . . ? C18 N10 Cu1 129.2(9) . . ? C18 N11 N12 103.4(11) . . ? C20 N12 N11 109.4(12) . . ? C20 N12 C1 124.8(17) . . ? N11 N12 C1 124.0(16) . . ? C2 C1 N12 104.4(16) . . ? C1 C2 C5 104.7(17) . . ? N1 C3 N2 114.0(15) . . ? N1 C3 N2' 107.1(15) . . ? N2 C3 N2' 51.4(10) . . ? N3 C4 N1 120(2) . . ? N1 C4' N3' 119(5) . . ? C5 C5 C2 137(2) 2_653 . ? C9 C6 N4 105.4(15) . . ? N5 C7 N6 111.4(18) . . ? N5 C7 C10 72.8(14) . . ? N6 C7 C10 38.6(7) . . ? C8 C8 C9 121.6(17) 2_687 . ? C6 C9 C8 112.5(13) . . ? N6 C10 N4 116.1(17) . . ? N6 C10 C7 43.7(9) . . ? N4 C10 C7 72.6(13) . . ? C17 C11 C17' 60.2(15) . . ? C17 C11 C15 122(2) . . ? C17' C11 C15 115.2(18) . . ? C16 C12 N9 115.6(12) . . ? N9 C13 N8 110.9(10) . . ? C15 C14 C16 116.7(12) . . ? C14 C15 C11 117.1(14) . . ? C12 C16 C14 112.1(12) . . ? C11 C17 N2 113(2) . . ? C11 C17' N2' 116(2) . . ? N11 C18 N10 111.3(12) . . ? N7 C19 N8 114.3(10) . . ? N12 C20 N10 113.4(14) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.300 _refine_diff_density_min -1.370 _refine_diff_density_rms 0.136