# Copyright The Royal Society of Chemistry, 1998 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H38 Cu Mo5 N6 O28 P2' _chemical_formula_weight 1247.60 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M ? 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' _cell_length_a 14.821(3) _cell_length_b 14.419(3) _cell_length_c 16.132(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.087(5) _cell_angle_gamma 90.00 _cell_volume 3258.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 4.99 _cell_measurement_theta_max 12.75 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.544 _exptl_crystal_density_method ? _exptl_crystal_F_000 2436 _exptl_absorpt_coefficient_mu 2.716 _exptl_absorpt_correction_type 'Semi-empirical from psi-scan' _exptl_absorpt_correction_T_min 0.8032 _exptl_absorpt_correction_T_max 0.9961 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.76 _diffrn_reflns_number 3522 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3235 _reflns_number_observed 3063 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0402P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.57(4) _refine_ls_number_reflns 3222 _refine_ls_number_parameters 414 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_obs 0.0267 _refine_ls_wR_factor_all 0.0696 _refine_ls_wR_factor_obs 0.0656 _refine_ls_goodness_of_fit_all 1.019 _refine_ls_goodness_of_fit_obs 1.042 _refine_ls_restrained_S_all 1.073 _refine_ls_restrained_S_obs 1.041 _refine_ls_shift/esd_max -0.011 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.11198(5) 0.83194(5) 0.34561(4) 0.0206(2) Uani 1 d . . Mo2 Mo 0.15861(5) 0.61072(5) 0.31287(4) 0.0195(2) Uani 1 d . . Mo3 Mo 0.31159(5) 0.60418(4) 0.19695(4) 0.01793(15) Uani 1 d . . Mo4 Mo 0.33655(5) 0.82180(5) 0.12915(4) 0.0204(2) Uani 1 d . . Mo5 Mo 0.18552(5) 0.96403(4) 0.18437(4) 0.0205(2) Uani 1 d . . Cu1 Cu 0.49331(10) 0.89632(6) 0.47685(6) 0.0194(2) Uani 1 d . . P1 P 0.32762(14) 0.78982(13) 0.33594(12) 0.0147(4) Uani 1 d . . P2 P 0.10930(15) 0.74778(13) 0.13151(12) 0.0157(4) Uani 1 d . . O1 O 0.1222(5) 0.8902(5) 0.4384(4) 0.035(2) Uani 1 d . . O2 O -0.0109(4) 0.8163(4) 0.2992(4) 0.0308(14) Uani 1 d . . O3 O 0.1322(4) 0.9269(4) 0.2710(4) 0.0245(12) Uani 1 d . . O4 O 0.2690(4) 0.8308(4) 0.3896(3) 0.0204(11) Uani 1 d . . O5 O 0.1437(5) 0.7069(4) 0.3879(4) 0.0244(12) Uani 1 d . . O6 O 0.1171(4) 0.7333(4) 0.2294(3) 0.0202(11) Uani 1 d . . O7 O 0.2205(5) 0.5358(4) 0.3940(4) 0.0313(14) Uani 1 d . . O8 O 0.0465(5) 0.5656(4) 0.2750(4) 0.0318(14) Uani 1 d . . O9 O 0.1977(4) 0.5642(4) 0.2172(3) 0.0204(12) Uani 1 d . . O10 O 0.3021(4) 0.6864(4) 0.3162(3) 0.0186(11) Uani 1 d . . O11 O 0.2895(5) 0.5536(4) 0.0965(4) 0.0308(14) Uani 1 d . . O12 O 0.3958(5) 0.5327(4) 0.2650(4) 0.0286(13) Uani 1 d . . O13 O 0.3892(4) 0.7075(4) 0.1910(4) 0.0214(12) Uani 1 d . . O14 O 0.2048(4) 0.7208(4) 0.1185(3) 0.0205(12) Uani 1 d . . O15 O 0.3221(5) 0.7875(5) 0.0239(4) 0.0339(15) Uani 1 d . . O16 O 0.4413(5) 0.8809(4) 0.1623(4) 0.036(2) Uani 1 d . . O17 O 0.2469(5) 0.9227(4) 0.1013(4) 0.0248(13) Uani 1 d . . O18 O 0.3008(4) 0.8458(3) 0.2488(3) 0.0190(11) Uani 1 d . . O19 O 0.2732(5) 1.0405(4) 0.2442(4) 0.0312(14) Uani 1 d . . O20 O 0.1023(5) 1.0384(4) 0.1231(4) 0.037(2) Uani 1 d . . O21 O 0.0896(4) 0.8514(4) 0.1126(3) 0.0206(12) Uani 1 d . . O22 O 0.4349(4) 0.7979(4) 0.3869(4) 0.0223(12) Uani 1 d . . O23 O 0.5253(4) 0.8078(4) 0.5733(3) 0.0232(12) Uani 1 d . . O24 O 0.6416(5) 0.8730(4) 0.4460(4) 0.0304(13) Uani 1 d . . H24A H 0.7335(5) 0.8399(4) 0.4610(4) 0.046 Uiso 1 d R . H24B H 0.6686(5) 0.8361(4) 0.5108(4) 0.046 Uiso 1 d R . O1W O -0.1598(5) 0.5570(5) 0.0321(4) 0.036(2) Uani 1 d . . H1WA H -0.2008(5) 0.5785(5) -0.0172(4) 0.054 Uiso 1 d R . H1WB H -0.2050(5) 0.5191(5) 0.0527(4) 0.054 Uiso 1 d R . O2W O 0.7071(8) 0.8665(5) 0.2463(7) 0.066(3) Uani 1 d . . H2WA H 0.7599(8) 0.8640(5) 0.2908(7) 0.099 Uiso 1 d R . H2WB H 0.6999(8) 0.9270(5) 0.2409(7) 0.099 Uiso 1 d R . O3W O -0.0732(7) 0.9929(7) -0.0191(6) 0.070(3) Uani 1 d . . H3WA H -0.1045(7) 0.9796(7) -0.0673(6) 0.106 Uiso 1 d R . H3WB H -0.0878(7) 0.9613(7) 0.0227(6) 0.106 Uiso 1 d R . O4W O 0.3613(8) 0.6686(7) -0.1022(7) 0.082(3) Uiso 1 d . . H4WA H 0.3334(8) 0.6992(7) -0.1372(7) 0.123 Uiso 1 d R . H4WB H 0.4266(8) 0.6842(7) -0.1188(7) 0.123 Uiso 1 d R . N1 N 0.4484(5) 0.9966(5) 0.3895(4) 0.0222(14) Uani 1 d . . H1C H 0.4811(5) 0.9946(5) 0.3514(4) 0.027 Uiso 1 calc R . H1D H 0.3862(5) 0.9881(5) 0.3593(4) 0.027 Uiso 1 calc R . N2 N 0.5455(5) 1.0001(5) 0.5616(4) 0.0237(15) Uani 1 d . . H2C H 0.5075(5) 1.0098(5) 0.5943(4) 0.028 Uiso 1 calc R . H2D H 0.6042(5) 0.9854(5) 0.5976(4) 0.028 Uiso 1 calc R . N3 N 0.5785(6) 0.7594(5) 0.2935(5) 0.033(2) Uani 1 d . . H3C H 0.6057(6) 0.7909(5) 0.2605(5) 0.049 Uiso 1 calc R . H3D H 0.5746(6) 0.7954(5) 0.3370(5) 0.049 Uiso 1 calc R . H3E H 0.5202(6) 0.7417(5) 0.2608(5) 0.049 Uiso 1 calc R . N4 N 0.5415(8) 0.6276(6) 0.4255(5) 0.049(2) Uani 1 d . . H4C H 0.5402(8) 0.5767(6) 0.4565(5) 0.073 Uiso 1 calc R . H4D H 0.4843(8) 0.6363(6) 0.3856(5) 0.073 Uiso 1 calc R . H4E H 0.5564(8) 0.6763(6) 0.4613(5) 0.073 Uiso 1 calc R . N5 N -0.0966(8) 0.8896(7) 0.1218(8) 0.063(3) Uani 1 d . . H5C H -0.0804(8) 0.9283(7) 0.0861(8) 0.094 Uiso 1 calc R . H5D H -0.0446(8) 0.8613(7) 0.1566(8) 0.094 Uiso 1 calc R . H5E H -0.1242(8) 0.9212(7) 0.1544(8) 0.094 Uiso 1 calc R . N6 N -0.1211(7) 0.6818(6) 0.1735(6) 0.043(2) Uani 1 d . . H6C H -0.1433(7) 0.6414(6) 0.2037(6) 0.064 Uiso 1 calc R . H6D H -0.0738(7) 0.7145(6) 0.2102(6) 0.064 Uiso 1 calc R . H6E H -0.0994(7) 0.6515(6) 0.1357(6) 0.064 Uiso 1 calc R . C1 C 0.4614(8) 1.0865(6) 0.4318(6) 0.036(2) Uani 1 d . . H1A H 0.4060(8) 1.1019(6) 0.4485(6) 0.043 Uiso 1 calc R . H1B H 0.4688(8) 1.1337(6) 0.3918(6) 0.043 Uiso 1 calc R . C2 C 0.5499(9) 1.0831(7) 0.5128(6) 0.040(2) Uani 1 d . . H2A H 0.6068(9) 1.0821(7) 0.4956(6) 0.048 Uiso 1 calc R . H2B H 0.5525(9) 1.1375(7) 0.5488(6) 0.048 Uiso 1 calc R . C3 C 0.6349(12) 0.6793(11) 0.3291(11) 0.078(4) Uiso 1 d . . H3A H 0.6404(12) 0.6442(11) 0.2797(11) 0.093 Uiso 1 calc R . H3B H 0.6985(12) 0.7015(11) 0.3613(11) 0.093 Uiso 1 calc R . C4 C 0.6108(14) 0.6169(13) 0.3829(13) 0.091(5) Uiso 1 d . . H4A H 0.6701(14) 0.6031(13) 0.4293(13) 0.109 Uiso 1 calc R . H4B H 0.5932(14) 0.5605(13) 0.3485(13) 0.109 Uiso 1 calc R . C5 C -0.1642(12) 0.8195(11) 0.0692(10) 0.073(4) Uiso 1 d . . H5A H -0.1339(12) 0.7869(11) 0.0328(10) 0.088 Uiso 1 calc R . H5B H -0.2196(12) 0.8514(11) 0.0304(10) 0.088 Uiso 1 calc R . C6 C -0.1993(8) 0.7457(9) 0.1245(9) 0.053(3) Uani 1 d . . H6A H -0.2235(8) 0.7778(9) 0.1657(9) 0.064 Uiso 1 calc R . H6B H -0.2512(8) 0.7098(9) 0.0854(9) 0.064 Uiso 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 0.0225(4) 0.0226(3) 0.0180(3) -0.0045(3) 0.0084(3) -0.0002(3) Mo2 0.0232(4) 0.0176(3) 0.0183(3) 0.0010(3) 0.0075(3) -0.0036(3) Mo3 0.0186(3) 0.0159(3) 0.0189(3) -0.0011(3) 0.0056(3) 0.0012(3) Mo4 0.0226(3) 0.0212(3) 0.0187(3) 0.0035(3) 0.0087(3) -0.0005(3) Mo5 0.0247(4) 0.0148(3) 0.0192(3) 0.0006(3) 0.0035(3) 0.0013(3) Cu1 0.0219(5) 0.0162(4) 0.0165(5) 0.0021(4) 0.0013(4) -0.0014(4) P1 0.0169(10) 0.0141(9) 0.0113(8) 0.0008(7) 0.0021(7) -0.0011(8) P2 0.0166(9) 0.0158(9) 0.0123(9) -0.0026(7) 0.0016(7) 0.0004(8) O1 0.040(4) 0.041(4) 0.025(3) -0.009(3) 0.012(3) 0.002(3) O2 0.027(3) 0.035(3) 0.030(3) -0.013(3) 0.009(3) -0.001(3) O3 0.032(3) 0.019(3) 0.024(3) -0.005(2) 0.011(3) 0.002(3) O4 0.029(3) 0.022(3) 0.011(2) -0.004(2) 0.007(2) -0.001(2) O5 0.032(3) 0.024(3) 0.019(3) 0.003(2) 0.012(3) -0.001(3) O6 0.028(3) 0.020(3) 0.013(2) -0.004(2) 0.009(2) 0.000(2) O7 0.040(4) 0.028(3) 0.024(3) 0.011(3) 0.009(3) 0.002(3) O8 0.030(3) 0.034(3) 0.037(3) -0.008(3) 0.017(3) -0.016(3) O9 0.020(3) 0.017(3) 0.023(3) 0.000(2) 0.005(2) -0.002(2) O10 0.018(3) 0.015(2) 0.019(3) -0.003(2) 0.000(2) -0.006(2) O11 0.041(4) 0.026(3) 0.029(3) -0.008(3) 0.016(3) 0.010(3) O12 0.027(3) 0.024(3) 0.031(3) -0.001(2) 0.003(3) 0.002(3) O13 0.018(3) 0.021(3) 0.025(3) 0.001(2) 0.007(2) 0.004(2) O14 0.023(3) 0.020(3) 0.018(3) 0.003(2) 0.006(2) 0.003(2) O15 0.040(4) 0.042(4) 0.023(3) 0.003(3) 0.014(3) 0.005(3) O16 0.037(4) 0.030(3) 0.044(4) 0.005(3) 0.015(3) -0.011(3) O17 0.039(3) 0.019(3) 0.019(3) 0.006(2) 0.012(3) -0.002(3) O18 0.025(3) 0.015(2) 0.017(3) 0.003(2) 0.008(2) 0.003(2) O19 0.029(3) 0.019(3) 0.038(3) -0.002(3) 0.000(3) -0.005(3) O20 0.041(4) 0.025(3) 0.038(4) 0.004(3) 0.005(3) 0.008(3) O21 0.024(3) 0.018(3) 0.019(3) -0.001(2) 0.006(2) 0.002(2) O22 0.022(3) 0.020(3) 0.021(3) -0.002(2) 0.003(2) -0.003(2) O23 0.018(3) 0.030(3) 0.018(3) 0.008(2) 0.000(2) 0.004(2) O24 0.031(3) 0.033(3) 0.025(3) 0.001(3) 0.006(3) -0.002(3) O1W 0.034(4) 0.038(4) 0.030(3) 0.014(3) 0.002(3) 0.005(3) O2W 0.098(8) 0.030(4) 0.086(6) 0.001(4) 0.053(6) 0.001(4) O3W 0.068(6) 0.077(6) 0.066(6) 0.006(5) 0.022(5) 0.005(5) N1 0.021(4) 0.022(3) 0.020(3) 0.005(3) 0.003(3) -0.003(3) N2 0.027(4) 0.022(3) 0.021(3) 0.006(3) 0.006(3) 0.003(3) N3 0.033(4) 0.030(4) 0.033(4) -0.002(3) 0.008(4) -0.004(4) N4 0.082(7) 0.033(4) 0.030(4) -0.007(4) 0.019(5) 0.002(5) N5 0.054(7) 0.068(7) 0.061(6) -0.011(5) 0.010(6) 0.015(6) N6 0.056(6) 0.035(4) 0.037(5) -0.002(4) 0.013(5) -0.001(4) C1 0.045(6) 0.025(5) 0.034(5) 0.007(4) 0.008(5) 0.013(4) C2 0.056(7) 0.029(5) 0.034(5) 0.000(4) 0.012(5) -0.012(5) C6 0.035(6) 0.057(7) 0.064(7) -0.012(6) 0.010(6) 0.005(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 O1 1.679(6) . ? Mo1 O2 1.742(6) . ? Mo1 O3 1.910(6) . ? Mo1 O5 1.932(5) . ? Mo1 O4 2.199(6) . ? Mo1 O6 2.374(5) . ? Mo2 O8 1.701(6) . ? Mo2 O7 1.714(6) . ? Mo2 O5 1.900(6) . ? Mo2 O9 1.937(6) . ? Mo2 O6 2.185(5) . ? Mo2 O10 2.376(5) . ? Mo3 O11 1.708(6) . ? Mo3 O12 1.711(6) . ? Mo3 O13 1.904(5) . ? Mo3 O9 1.910(6) . ? Mo3 O10 2.302(5) . ? Mo3 O14 2.371(5) . ? Mo4 O16 1.697(7) . ? Mo4 O15 1.714(6) . ? Mo4 O17 1.921(6) . ? Mo4 O13 1.952(5) . ? Mo4 O18 2.190(5) . ? Mo4 O14 2.397(6) . ? Mo5 O20 1.688(6) . ? Mo5 O19 1.737(6) . ? Mo5 O3 1.894(6) . ? Mo5 O17 1.944(6) . ? Mo5 O21 2.219(5) . ? Mo5 O18 2.397(5) . ? Cu1 O23 1.947(5) . ? Cu1 N1 1.976(6) . ? Cu1 N2 2.003(7) . ? Cu1 O22 2.012(5) . ? Cu1 O24 2.431(7) . ? P1 O4 1.532(6) . ? P1 O22 1.537(6) . ? P1 O10 1.546(5) . ? P1 O18 1.555(5) . ? P2 O23 1.520(6) 4_464 ? P2 O21 1.533(5) . ? P2 O14 1.547(6) . ? P2 O6 1.559(5) . ? O23 P2 1.520(6) 4_565 ? N1 C1 1.447(12) . ? N2 C2 1.445(11) . ? N3 C3 1.43(2) . ? N4 C4 1.42(2) . ? N5 C5 1.48(2) . ? N6 C6 1.489(15) . ? C1 C2 1.519(14) . ? C3 C4 1.38(2) . ? C5 C6 1.58(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 102.9(3) . . ? O1 Mo1 O3 102.5(3) . . ? O2 Mo1 O3 100.3(3) . . ? O1 Mo1 O5 102.2(3) . . ? O2 Mo1 O5 97.5(3) . . ? O3 Mo1 O5 145.3(2) . . ? O1 Mo1 O4 86.5(3) . . ? O2 Mo1 O4 169.9(2) . . ? O3 Mo1 O4 80.9(2) . . ? O5 Mo1 O4 76.7(2) . . ? O1 Mo1 O6 170.6(3) . . ? O2 Mo1 O6 83.2(2) . . ? O3 Mo1 O6 83.1(2) . . ? O5 Mo1 O6 69.7(2) . . ? O4 Mo1 O6 87.0(2) . . ? O8 Mo2 O7 104.4(3) . . ? O8 Mo2 O5 101.8(3) . . ? O7 Mo2 O5 96.7(3) . . ? O8 Mo2 O9 95.4(3) . . ? O7 Mo2 O9 99.5(3) . . ? O5 Mo2 O9 152.6(2) . . ? O8 Mo2 O6 92.5(3) . . ? O7 Mo2 O6 162.4(3) . . ? O5 Mo2 O6 74.6(2) . . ? O9 Mo2 O6 83.5(2) . . ? O8 Mo2 O10 161.1(3) . . ? O7 Mo2 O10 91.2(3) . . ? O5 Mo2 O10 86.6(2) . . ? O9 Mo2 O10 71.2(2) . . ? O6 Mo2 O10 73.3(2) . . ? O11 Mo3 O12 103.0(3) . . ? O11 Mo3 O13 102.6(3) . . ? O12 Mo3 O13 100.2(3) . . ? O11 Mo3 O9 97.3(3) . . ? O12 Mo3 O9 102.1(3) . . ? O13 Mo3 O9 145.8(2) . . ? O11 Mo3 O10 165.3(3) . . ? O12 Mo3 O10 90.3(2) . . ? O13 Mo3 O10 80.9(2) . . ? O9 Mo3 O10 73.4(2) . . ? O11 Mo3 O14 84.8(2) . . ? O12 Mo3 O14 171.4(2) . . ? O13 Mo3 O14 74.2(2) . . ? O9 Mo3 O14 80.3(2) . . ? O10 Mo3 O14 82.4(2) . . ? O16 Mo4 O15 105.2(3) . . ? O16 Mo4 O17 100.7(3) . . ? O15 Mo4 O17 97.7(3) . . ? O16 Mo4 O13 95.2(3) . . ? O15 Mo4 O13 99.4(3) . . ? O17 Mo4 O13 152.7(2) . . ? O16 Mo4 O18 95.9(3) . . ? O15 Mo4 O18 158.7(3) . . ? O17 Mo4 O18 74.9(2) . . ? O13 Mo4 O18 81.6(2) . . ? O16 Mo4 O14 165.4(3) . . ? O15 Mo4 O14 85.3(3) . . ? O17 Mo4 O14 87.6(2) . . ? O13 Mo4 O14 72.8(2) . . ? O18 Mo4 O14 74.5(2) . . ? O20 Mo5 O19 101.1(3) . . ? O20 Mo5 O3 102.1(3) . . ? O19 Mo5 O3 100.7(3) . . ? O20 Mo5 O17 102.0(3) . . ? O19 Mo5 O17 98.3(3) . . ? O3 Mo5 O17 145.5(2) . . ? O20 Mo5 O21 86.5(3) . . ? O19 Mo5 O21 171.9(3) . . ? O3 Mo5 O21 80.0(2) . . ? O17 Mo5 O21 77.3(2) . . ? O20 Mo5 O18 170.5(3) . . ? O19 Mo5 O18 85.0(2) . . ? O3 Mo5 O18 83.6(2) . . ? O17 Mo5 O18 69.7(2) . . ? O21 Mo5 O18 87.1(2) . . ? O23 Cu1 N1 170.5(3) . . ? O23 Cu1 N2 90.3(3) . . ? N1 Cu1 N2 84.5(3) . . ? O23 Cu1 O22 92.8(2) . . ? N1 Cu1 O22 92.1(3) . . ? N2 Cu1 O22 176.3(3) . . ? O23 Cu1 O24 94.2(2) . . ? N1 Cu1 O24 94.1(3) . . ? N2 Cu1 O24 94.0(3) . . ? O22 Cu1 O24 87.6(2) . . ? O4 P1 O22 110.4(3) . . ? O4 P1 O10 110.1(3) . . ? O22 P1 O10 108.9(3) . . ? O4 P1 O18 106.6(3) . . ? O22 P1 O18 110.9(3) . . ? O10 P1 O18 109.9(3) . . ? O23 P2 O21 109.0(3) 4_464 . ? O23 P2 O14 112.6(3) 4_464 . ? O21 P2 O14 110.0(3) . . ? O23 P2 O6 109.3(3) 4_464 . ? O21 P2 O6 106.1(3) . . ? O14 P2 O6 109.6(3) . . ? Mo5 O3 Mo1 149.0(3) . . ? P1 O4 Mo1 123.8(3) . . ? Mo2 O5 Mo1 121.4(3) . . ? P2 O6 Mo2 130.2(3) . . ? P2 O6 Mo1 135.1(3) . . ? Mo2 O6 Mo1 94.2(2) . . ? Mo3 O9 Mo2 122.9(3) . . ? P1 O10 Mo3 126.3(3) . . ? P1 O10 Mo2 127.2(3) . . ? Mo3 O10 Mo2 92.5(2) . . ? Mo3 O13 Mo4 122.6(3) . . ? P2 O14 Mo3 126.0(3) . . ? P2 O14 Mo4 126.7(3) . . ? Mo3 O14 Mo4 90.4(2) . . ? Mo4 O17 Mo5 121.0(3) . . ? P1 O18 Mo4 130.6(3) . . ? P1 O18 Mo5 134.1(3) . . ? Mo4 O18 Mo5 94.2(2) . . ? P2 O21 Mo5 124.2(3) . . ? P1 O22 Cu1 124.4(3) . . ? P2 O23 Cu1 140.9(4) 4_565 . ? C1 N1 Cu1 110.9(5) . . ? C2 N2 Cu1 108.8(5) . . ? N1 C1 C2 108.7(8) . . ? N2 C2 C1 108.3(8) . . ? C4 C3 N3 122.9(15) . . ? C3 C4 N4 127.8(16) . . ? N5 C5 C6 114.9(12) . . ? N6 C6 C5 111.9(11) . . ? _refine_diff_density_max 0.977 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.113 #===END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H32 Cu Mo5 N6 O25 P2' _chemical_formula_weight 1193.56 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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 10.6813(14) _cell_length_b 11.176(2) _cell_length_c 12.852(2) _cell_angle_alpha 75.568(13) _cell_angle_beta 89.297(6) _cell_angle_gamma 86.545(8) _cell_volume 1483.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 4.79 _cell_measurement_theta_max 12.61 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.673 _exptl_crystal_density_method ? _exptl_crystal_F_000 1158 _exptl_absorpt_coefficient_mu 2.969 _exptl_absorpt_correction_type 'Semi-empirical from psi-scan' _exptl_absorpt_correction_T_min 0.6485 _exptl_absorpt_correction_T_max 0.9690 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.05 _diffrn_reflns_number 6085 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5180 _reflns_number_observed 4340 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 42 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+12.5553P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5138 _refine_ls_number_parameters 407 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_obs 0.0496 _refine_ls_wR_factor_all 0.1574 _refine_ls_wR_factor_obs 0.1306 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.075 _refine_ls_restrained_S_all 1.184 _refine_ls_restrained_S_obs 1.075 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo -0.38365(6) 0.76217(6) 0.26460(5) 0.0198(2) Uani 1 d . . Mo2 Mo -0.20102(7) 0.95026(6) 0.36095(5) 0.0206(2) Uani 1 d . . Mo3 Mo 0.12523(6) 0.82419(6) 0.34336(5) 0.0199(2) Uani 1 d . . Mo4 Mo 0.11005(7) 0.63399(6) 0.17901(5) 0.0213(2) Uani 1 d . . Mo5 Mo -0.19862(7) 0.58348(6) 0.14167(6) 0.0237(2) Uani 1 d . . Cu1 Cu -0.5000 0.5000 0.5000 0.0678(6) Uani 1 d SD . Cu2 Cu -0.5000 1.0000 0.0000 0.0255(3) Uani 1 d S . P1 P -0.1068(2) 0.8752(2) 0.13502(15) 0.0171(4) Uani 1 d . . P2 P -0.1092(2) 0.6244(2) 0.3923(2) 0.0218(4) Uani 1 d . . O1 O -0.4841(6) 0.8162(6) 0.1581(5) 0.0298(13) Uani 1 d . . O2 O -0.4803(7) 0.7053(7) 0.3715(5) 0.038(2) Uani 1 d . . O3 O -0.3271(6) 0.6020(5) 0.2420(5) 0.0262(13) Uani 1 d . . O4 O -0.2171(5) 0.7897(5) 0.1448(4) 0.0212(11) Uani 1 d . . O5 O -0.2065(6) 0.7340(5) 0.3637(4) 0.0244(12) Uani 1 d . . O6 O -0.3503(5) 0.9192(5) 0.2911(4) 0.0247(12) Uani 1 d . . O7 O -0.2459(6) 0.9061(6) 0.4918(5) 0.0328(14) Uani 1 d . . O8 O -0.2120(6) 1.1092(6) 0.3334(5) 0.0307(14) Uani 1 d . . O9 O -0.1432(5) 0.9835(5) 0.1837(4) 0.0197(11) Uani 1 d . . O10 O -0.0244(5) 0.9119(5) 0.3757(4) 0.0238(12) Uani 1 d . . O11 O 0.2001(6) 0.9413(6) 0.2594(5) 0.0359(15) Uani 1 d . . O12 O 0.2067(6) 0.7998(6) 0.4617(5) 0.0345(15) Uani 1 d . . O13 O 0.0081(5) 0.8035(5) 0.1987(4) 0.0215(12) Uani 1 d . . O14 O 0.0053(6) 0.6616(5) 0.4443(4) 0.0257(13) Uani 1 d . . O15 O 0.1879(5) 0.6806(5) 0.2962(5) 0.0255(12) Uani 1 d . . O16 O 0.2055(6) 0.6986(6) 0.0750(5) 0.0340(14) Uani 1 d . . O17 O 0.1579(6) 0.4801(6) 0.2174(5) 0.0328(14) Uani 1 d . . O18 O -0.0694(6) 0.5736(5) 0.2950(4) 0.0272(13) Uani 1 d . . O19 O -0.0352(6) 0.6292(5) 0.0903(5) 0.0272(13) Uani 1 d . . O20 O -0.2795(6) 0.6204(6) 0.0230(5) 0.036(2) Uani 1 d . . O21 O -0.1821(7) 0.4241(6) 0.1734(6) 0.039(2) Uani 1 d . . O22 O -0.0756(6) 0.9191(5) 0.0155(4) 0.0248(12) Uani 1 d . . O23 O -0.1740(7) 0.5217(6) 0.4782(5) 0.039(2) Uani 1 d . . H23A H -0.1401(7) 0.4579(6) 0.4973(5) 0.058 Uiso 1 d R . H23B H -0.2211(7) 0.5071(6) 0.4766(5) 0.058 Uiso 1 d R . N1 N -0.3838(11) 0.3999(12) 0.4251(11) 0.076(4) Uani 1 d . . H1A H -0.3343(11) 0.4509(12) 0.3796(11) 0.091 Uiso 1 calc R . H1B H -0.3343(11) 0.3471(12) 0.4742(11) 0.091 Uiso 1 calc R . N2A N -0.6289(16) 0.4728(16) 0.3945(13) 0.056(4) Uiso 0.70 d P . H2AC H -0.6779(16) 0.5425(16) 0.3713(13) 0.067 Uiso 0.70 d PR . H2AD H -0.6778(16) 0.4120(16) 0.4277(13) 0.067 Uiso 0.70 d PR . N2B N -0.5845(49) 0.5025(48) 0.3593(23) 0.083(14) Uiso 0.30 d PD . H2BC H -0.5413(49) 0.5399(48) 0.3008(23) 0.100 Uiso 0.30 d PR . H2BD H -0.6624(49) 0.5384(48) 0.3570(23) 0.100 Uiso 0.30 d PR . N3 N -0.6209(7) 0.8988(7) -0.0533(6) 0.031(2) Uani 1 d . . H3C H -0.6734(7) 0.8652(7) -0.0001(6) 0.038 Uiso 1 calc R . H3D H -0.6668(7) 0.9471(7) -0.1077(6) 0.038 Uiso 1 calc R . N4 N -0.3687(7) 0.9160(7) -0.0758(6) 0.031(2) Uani 1 d . . H4C H -0.3182(7) 0.9722(7) -0.1143(6) 0.037 Uiso 1 calc R . H4D H -0.3215(7) 0.8599(7) -0.0274(6) 0.037 Uiso 1 calc R . N5 N -0.0473(7) 0.2203(6) 0.1279(6) 0.026(2) Uani 1 d . . H5C H -0.0378(7) 0.2403(6) 0.0569(6) 0.039 Uiso 1 calc R . H5D H -0.1056(7) 0.2716(6) 0.1461(6) 0.039 Uiso 1 calc R . H5E H -0.0708(7) 0.1430(6) 0.1494(6) 0.039 Uiso 1 calc R . N6 N -0.0124(8) 0.2869(7) 0.3453(6) 0.034(2) Uani 1 d . . H6C H -0.0099(8) 0.2639(7) 0.4168(6) 0.051 Uiso 1 calc R . H6D H -0.0907(8) 0.2855(7) 0.3229(6) 0.051 Uiso 1 calc R . H6E H 0.0137(8) 0.3632(7) 0.3228(6) 0.051 Uiso 1 calc R . C1 C -0.4562(13) 0.3273(16) 0.3631(13) 0.074(4) Uani 1 d . . C2A C -0.5748(23) 0.4452(23) 0.3126(20) 0.078(6) Uiso 0.70 d P . H2AA H -0.5369(23) 0.5156(23) 0.2676(20) 0.094 Uiso 0.70 d PR . H2AB H -0.6338(23) 0.4158(23) 0.2704(20) 0.094 Uiso 0.70 d PR . C2B C -0.5917(21) 0.3545(21) 0.3782(19) 0.013(5) Uiso 0.30 d P . H2BA H -0.6411(21) 0.3344(21) 0.3237(19) 0.015 Uiso 0.30 d PR . H2BB H -0.6213(21) 0.3129(21) 0.4479(19) 0.015 Uiso 0.30 d PR . C3 C -0.5479(11) 0.7974(10) -0.0915(9) 0.045(3) Uani 1 d . . H3A H -0.5237(11) 0.7291(10) -0.0309(9) 0.054 Uiso 1 calc R . H3B H -0.5988(11) 0.7666(10) -0.1400(9) 0.054 Uiso 1 calc R . C4 C -0.4332(10) 0.8533(11) -0.1487(8) 0.042(2) Uani 1 d . . H4A H -0.3772(10) 0.7891(11) -0.1656(8) 0.051 Uiso 1 calc R . H4B H -0.4572(10) 0.9128(11) -0.2152(8) 0.051 Uiso 1 calc R . C5 C 0.0739(9) 0.2305(9) 0.1803(8) 0.034(2) Uani 1 d . . H5A H 0.0995(9) 0.3145(9) 0.1543(8) 0.041 Uiso 1 calc R . H5B H 0.1370(9) 0.1761(9) 0.1578(8) 0.041 Uiso 1 calc R . C6 C 0.0716(9) 0.1994(9) 0.3006(7) 0.031(2) Uani 1 d . . H6A H 0.1562(9) 0.1999(9) 0.3269(7) 0.037 Uiso 1 calc R . H6B H 0.0437(9) 0.1162(9) 0.3270(7) 0.037 Uiso 1 calc R . O1W O -0.5586(17) 0.4849(18) 0.1075(14) 0.061(4) Uani 0.50 d P . O2WA O -0.5000 1.0000 -0.5000 0.064(7) Uiso 0.50 d SP . O2WB O -0.4423(20) 1.0384(20) -0.4277(17) 0.020(4) Uiso 0.25 d P . O2WC O -0.4462(20) 0.1669(19) 0.4652(17) 0.020(4) Uiso 0.25 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0256(4) 0.0211(4) 0.0117(3) -0.0023(3) -0.0045(3) 0.0005(3) Mo2 0.0278(4) 0.0228(4) 0.0132(3) -0.0094(3) -0.0039(3) 0.0037(3) Mo3 0.0259(4) 0.0201(4) 0.0152(3) -0.0077(3) -0.0061(3) 0.0013(3) Mo4 0.0282(4) 0.0196(4) 0.0177(4) -0.0087(3) -0.0066(3) 0.0053(3) Mo5 0.0322(4) 0.0197(4) 0.0213(4) -0.0099(3) -0.0124(3) 0.0054(3) Cu1 0.0674(15) 0.079(2) 0.0586(14) -0.0202(12) -0.0037(11) -0.0017(12) Cu2 0.0238(7) 0.0331(8) 0.0191(7) -0.0067(6) -0.0039(5) 0.0032(6) P1 0.0254(10) 0.0170(10) 0.0089(9) -0.0040(7) -0.0046(7) 0.0030(8) P2 0.0356(12) 0.0164(10) 0.0123(9) -0.0022(8) -0.0109(8) 0.0032(8) O1 0.030(3) 0.035(3) 0.024(3) -0.006(3) -0.010(2) 0.001(3) O2 0.046(4) 0.046(4) 0.023(3) -0.010(3) 0.003(3) -0.004(3) O3 0.034(3) 0.025(3) 0.020(3) -0.006(2) 0.001(2) -0.001(2) O4 0.027(3) 0.021(3) 0.016(3) -0.006(2) -0.008(2) 0.001(2) O5 0.037(3) 0.021(3) 0.015(3) -0.007(2) -0.009(2) 0.007(2) O6 0.030(3) 0.024(3) 0.022(3) -0.009(2) -0.007(2) 0.004(2) O7 0.040(4) 0.049(4) 0.011(3) -0.010(3) 0.000(2) 0.001(3) O8 0.035(3) 0.028(3) 0.034(3) -0.017(3) -0.007(3) 0.008(3) O9 0.030(3) 0.014(3) 0.014(3) -0.004(2) -0.003(2) 0.004(2) O10 0.029(3) 0.024(3) 0.021(3) -0.011(2) -0.005(2) 0.001(2) O11 0.042(4) 0.028(3) 0.039(4) -0.010(3) 0.006(3) -0.007(3) O12 0.039(4) 0.041(4) 0.028(3) -0.017(3) -0.015(3) 0.003(3) O13 0.026(3) 0.021(3) 0.020(3) -0.010(2) -0.014(2) 0.007(2) O14 0.036(3) 0.023(3) 0.016(3) -0.002(2) -0.014(2) 0.004(2) O15 0.030(3) 0.022(3) 0.025(3) -0.009(2) -0.010(2) 0.009(2) O16 0.038(4) 0.044(4) 0.022(3) -0.013(3) -0.001(3) 0.002(3) O17 0.040(4) 0.023(3) 0.038(4) -0.014(3) -0.013(3) 0.009(3) O18 0.043(4) 0.026(3) 0.012(3) -0.008(2) -0.016(2) 0.011(3) O19 0.035(3) 0.030(3) 0.018(3) -0.011(2) -0.006(2) 0.007(3) O20 0.043(4) 0.041(4) 0.028(3) -0.017(3) -0.018(3) 0.008(3) O21 0.052(4) 0.023(3) 0.044(4) -0.015(3) -0.015(3) 0.004(3) O22 0.038(3) 0.027(3) 0.010(3) -0.005(2) 0.000(2) 0.002(3) O23 0.052(4) 0.025(3) 0.029(3) 0.011(3) -0.014(3) -0.003(3) N1 0.055(7) 0.084(9) 0.075(8) 0.005(7) -0.015(6) -0.005(6) N3 0.028(4) 0.035(4) 0.028(4) -0.005(3) -0.008(3) 0.006(3) N4 0.027(4) 0.038(4) 0.023(4) 0.001(3) -0.005(3) 0.006(3) N5 0.041(4) 0.020(3) 0.021(3) -0.013(3) 0.001(3) 0.001(3) N6 0.059(5) 0.029(4) 0.017(4) -0.010(3) -0.008(3) -0.002(4) C1 0.057(8) 0.103(12) 0.084(10) -0.063(9) -0.005(7) 0.000(8) C3 0.051(6) 0.041(6) 0.048(6) -0.019(5) -0.010(5) 0.005(5) C4 0.051(6) 0.055(6) 0.025(5) -0.020(4) -0.015(4) 0.017(5) C5 0.035(5) 0.041(5) 0.030(5) -0.015(4) 0.006(4) -0.006(4) C6 0.037(5) 0.032(5) 0.027(5) -0.012(4) -0.014(4) 0.004(4) O1W 0.065(11) 0.076(12) 0.049(10) -0.032(9) -0.004(8) -0.006(9) _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 O1 1.713(6) . ? Mo1 O2 1.722(6) . ? Mo1 O6 1.924(6) . ? Mo1 O3 1.944(6) . ? Mo1 O5 2.255(6) . ? Mo1 O4 2.323(6) . ? Mo2 O7 1.702(6) . ? Mo2 O8 1.719(6) . ? Mo2 O10 1.911(6) . ? Mo2 O6 1.930(6) . ? Mo2 O9 2.298(5) . ? Mo2 O5 2.413(6) . ? Mo3 O11 1.708(6) . ? Mo3 O12 1.715(6) . ? Mo3 O10 1.920(6) . ? Mo3 O15 1.933(6) . ? Mo3 O13 2.320(5) . ? Mo3 O14 2.386(6) . ? Mo4 O16 1.710(6) . ? Mo4 O17 1.714(6) . ? Mo4 O15 1.925(6) . ? Mo4 O19 1.947(6) . ? Mo4 O13 2.196(5) . ? Mo4 O18 2.436(7) . ? Mo5 O20 1.708(6) . ? Mo5 O21 1.724(6) . ? Mo5 O3 1.908(6) . ? Mo5 O19 1.912(6) . ? Mo5 O4 2.311(6) . ? Mo5 O18 2.396(5) . ? Cu1 N1 2.014(14) . ? Cu1 N1 2.014(14) 2_466 ? Cu1 N2B 2.024(5) 2_466 ? Cu1 N2B 2.024(5) . ? Cu1 N2A 2.03(2) . ? Cu1 N2A 2.03(2) 2_466 ? Cu1 O2 2.490(6) . ? Cu1 O2 2.490(6) . ? Cu2 N3 2.000(8) . ? Cu2 N3 2.000(8) 2_475 ? Cu2 N4 2.015(8) 2_475 ? Cu2 N4 2.015(8) . ? Cu2 O1 2.503(6) . ? Cu2 O1 2.503(6) . ? P1 O9 1.525(5) . ? P1 O22 1.531(5) . ? P1 O4 1.545(6) . ? P1 O13 1.548(5) . ? P2 O14 1.527(6) . ? P2 O5 1.533(6) . ? P2 O18 1.542(6) . ? P2 O23 1.568(6) . ? N1 C1 1.52(2) . ? N2A N2B 0.69(5) . ? N2A C2A 1.29(3) . ? N2A C2B 1.42(3) . ? N2B C2A 0.98(4) . ? N2B C2B 1.62(6) . ? N3 C3 1.515(13) . ? N4 C4 1.497(13) . ? N5 C5 1.489(12) . ? N6 C6 1.501(12) . ? C1 C2B 1.48(3) . ? C1 C2A 1.78(3) . ? C2A C2B 1.17(3) . ? C3 C4 1.51(2) . ? C5 C6 1.498(13) . ? O2WA O2WB 1.29(2) 2_474 ? O2WA O2WB 1.29(2) . ? O2WB O2WC 1.72(3) 1_564 ? O2WC O2WB 1.72(3) 1_546 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 104.3(3) . . ? O1 Mo1 O6 97.8(3) . . ? O2 Mo1 O6 100.2(3) . . ? O1 Mo1 O3 100.9(3) . . ? O2 Mo1 O3 96.0(3) . . ? O6 Mo1 O3 151.2(3) . . ? O1 Mo1 O5 159.7(3) . . ? O2 Mo1 O5 95.2(3) . . ? O6 Mo1 O5 72.7(2) . . ? O3 Mo1 O5 82.4(2) . . ? O1 Mo1 O4 88.8(2) . . ? O2 Mo1 O4 163.6(3) . . ? O6 Mo1 O4 87.5(2) . . ? O3 Mo1 O4 71.4(2) . . ? O5 Mo1 O4 73.1(2) . . ? O7 Mo2 O8 103.4(3) . . ? O7 Mo2 O10 100.3(3) . . ? O8 Mo2 O10 102.8(3) . . ? O7 Mo2 O6 100.1(3) . . ? O8 Mo2 O6 101.1(3) . . ? O10 Mo2 O6 143.8(2) . . ? O7 Mo2 O9 172.5(3) . . ? O8 Mo2 O9 83.9(2) . . ? O10 Mo2 O9 79.4(2) . . ? O6 Mo2 O9 76.5(2) . . ? O7 Mo2 O5 85.3(3) . . ? O8 Mo2 O5 168.1(2) . . ? O10 Mo2 O5 83.3(2) . . ? O6 Mo2 O5 69.0(2) . . ? O9 Mo2 O5 87.2(2) . . ? O11 Mo3 O12 103.3(3) . . ? O11 Mo3 O10 101.0(3) . . ? O12 Mo3 O10 101.0(3) . . ? O11 Mo3 O15 102.6(3) . . ? O12 Mo3 O15 99.7(3) . . ? O10 Mo3 O15 143.9(2) . . ? O11 Mo3 O13 89.3(3) . . ? O12 Mo3 O13 165.4(3) . . ? O10 Mo3 O13 83.6(2) . . ? O15 Mo3 O13 69.9(2) . . ? O11 Mo3 O14 173.6(3) . . ? O12 Mo3 O14 83.1(3) . . ? O10 Mo3 O14 77.4(2) . . ? O15 Mo3 O14 76.2(2) . . ? O13 Mo3 O14 84.4(2) . . ? O16 Mo4 O17 105.9(3) . . ? O16 Mo4 O15 100.8(3) . . ? O17 Mo4 O15 96.3(3) . . ? O16 Mo4 O19 95.9(3) . . ? O17 Mo4 O19 101.0(3) . . ? O15 Mo4 O19 151.5(2) . . ? O16 Mo4 O13 98.8(3) . . ? O17 Mo4 O13 154.5(3) . . ? O15 Mo4 O13 72.8(2) . . ? O19 Mo4 O13 82.0(2) . . ? O16 Mo4 O18 164.7(3) . . ? O17 Mo4 O18 84.9(3) . . ? O15 Mo4 O18 88.5(2) . . ? O19 Mo4 O18 70.9(2) . . ? O13 Mo4 O18 72.1(2) . . ? O20 Mo5 O21 103.8(3) . . ? O20 Mo5 O3 101.9(3) . . ? O21 Mo5 O3 98.6(3) . . ? O20 Mo5 O19 99.9(3) . . ? O21 Mo5 O19 102.3(3) . . ? O3 Mo5 O19 145.1(3) . . ? O20 Mo5 O4 89.0(3) . . ? O21 Mo5 O4 165.7(3) . . ? O3 Mo5 O4 72.3(2) . . ? O19 Mo5 O4 81.2(2) . . ? O20 Mo5 O18 168.1(3) . . ? O21 Mo5 O18 86.9(3) . . ? O3 Mo5 O18 81.1(2) . . ? O19 Mo5 O18 72.4(2) . . ? O4 Mo5 O18 80.9(2) . . ? N1 Cu1 N1 180.000(2) . 2_466 ? N1 Cu1 N2B 106.1(16) . 2_466 ? N1 Cu1 N2B 73.9(16) 2_466 2_466 ? N1 Cu1 N2B 73.9(16) . . ? N1 Cu1 N2B 106.1(16) 2_466 . ? N2B Cu1 N2B 180.000(8) 2_466 . ? N1 Cu1 N2A 83.6(6) . . ? N1 Cu1 N2A 96.4(6) 2_466 . ? N2B Cu1 N2A 160.4(15) 2_466 . ? N2B Cu1 N2A 19.6(15) . . ? N1 Cu1 N2A 96.4(6) . 2_466 ? N1 Cu1 N2A 83.6(6) 2_466 2_466 ? N2B Cu1 N2A 19.6(15) 2_466 2_466 ? N2B Cu1 N2A 160.4(15) . 2_466 ? N2A Cu1 N2A 180.000(2) . 2_466 ? N3 Cu2 N3 180.000(1) . 2_475 ? N3 Cu2 N4 94.8(3) . 2_475 ? N3 Cu2 N4 85.2(3) 2_475 2_475 ? N3 Cu2 N4 85.2(3) . . ? N3 Cu2 N4 94.8(3) 2_475 . ? N4 Cu2 N4 180.0 2_475 . ? O9 P1 O22 111.6(3) . . ? O9 P1 O4 110.0(3) . . ? O22 P1 O4 107.3(3) . . ? O9 P1 O13 107.2(3) . . ? O22 P1 O13 110.6(3) . . ? O4 P1 O13 110.1(3) . . ? O14 P2 O5 109.8(3) . . ? O14 P2 O18 110.5(4) . . ? O5 P2 O18 113.0(3) . . ? O14 P2 O23 108.3(3) . . ? O5 P2 O23 105.4(4) . . ? O18 P2 O23 109.6(4) . . ? Mo5 O3 Mo1 122.5(3) . . ? P1 O4 Mo5 125.1(3) . . ? P1 O4 Mo1 130.0(3) . . ? Mo5 O4 Mo1 93.6(2) . . ? P2 O5 Mo1 131.0(3) . . ? P2 O5 Mo2 133.2(3) . . ? Mo1 O5 Mo2 93.7(2) . . ? Mo1 O6 Mo2 124.3(3) . . ? P1 O9 Mo2 120.8(3) . . ? Mo2 O10 Mo3 150.6(3) . . ? P1 O13 Mo4 128.7(3) . . ? P1 O13 Mo3 135.1(3) . . ? Mo4 O13 Mo3 96.1(2) . . ? P2 O14 Mo3 119.2(3) . . ? Mo4 O15 Mo3 121.2(3) . . ? P2 O18 Mo5 125.0(3) . . ? P2 O18 Mo4 126.0(3) . . ? Mo5 O18 Mo4 90.7(2) . . ? Mo5 O19 Mo4 125.9(3) . . ? C1 N1 Cu1 111.5(8) . . ? N2B N2A C2A 48.6(36) . . ? N2B N2A C2B 93.3(49) . . ? C2A N2A C2B 50.7(15) . . ? N2B N2A Cu1 79.6(15) . . ? C2A N2A Cu1 110.9(16) . . ? C2B N2A Cu1 104.1(13) . . ? N2A N2B C2A 99.4(57) . . ? N2A N2B C2B 61.4(43) . . ? C2A N2B C2B 45.8(28) . . ? N2A N2B Cu1 80.8(16) . . ? C2A N2B Cu1 130.8(40) . . ? C2B N2B Cu1 97.4(19) . . ? C3 N3 Cu2 108.9(6) . . ? C4 N4 Cu2 108.7(6) . . ? C2B C1 N1 107.8(13) . . ? C2B C1 C2A 40.7(12) . . ? N1 C1 C2A 96.7(13) . . ? N2B C2A C2B 97.2(38) . . ? N2B C2A N2A 32.0(33) . . ? C2B C2A N2A 70.5(19) . . ? N2B C2A C1 110.6(32) . . ? C2B C2A C1 55.9(16) . . ? N2A C2A C1 107.0(18) . . ? C2A C2B N2A 58.7(17) . . ? C2A C2B C1 83.3(19) . . ? N2A C2B C1 117.4(18) . . ? C2A C2B N2B 37.0(18) . . ? N2A C2B N2B 25.3(19) . . ? C1 C2B N2B 96.4(25) . . ? C4 C3 N3 107.1(9) . . ? N4 C4 C3 108.0(8) . . ? N5 C5 C6 115.3(8) . . ? C5 C6 N6 113.5(7) . . ? O2WB O2WA O2WB 180.000(4) 2_474 . ? O2WA O2WB O2WC 78.1(13) . 1_564 ? _refine_diff_density_max 1.842 _refine_diff_density_min -3.897 _refine_diff_density_rms 0.230 #===END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H20 Cu Mo2.50 N4 O13 P' _chemical_formula_weight 666.60 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' _cell_length_a 11.478(4) _cell_length_b 39.171(8) _cell_length_c 15.226(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6845.4(38) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.93 _cell_measurement_theta_max 12.54 _exptl_crystal_description ? _exptl_crystal_colour 'DARK_BLUE ' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.587 _exptl_crystal_density_method ? _exptl_crystal_F_000 5200 _exptl_absorpt_coefficient_mu 3.190 _exptl_absorpt_correction_type 'Semi-empirical from psi-scan' _exptl_absorpt_correction_T_min 0.4740 _exptl_absorpt_correction_T_max 0.9874 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.43 _diffrn_reflns_number 6556 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3035 _reflns_number_observed 2813 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 29 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+18.9322P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00053(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3006 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_obs 0.0246 _refine_ls_wR_factor_all 0.0694 _refine_ls_wR_factor_obs 0.0603 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_goodness_of_fit_obs 1.123 _refine_ls_restrained_S_all 1.252 _refine_ls_restrained_S_obs 1.123 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo -0.11793(3) 0.059003(7) 0.56809(2) 0.02047(10) Uani 1 d . . Mo2 Mo -0.02886(2) 0.141518(7) 0.56663(2) 0.01749(10) Uani 1 d . . Mo3 Mo -0.2500 0.191535(10) 0.5000 0.01905(11) Uani 1 d S . Cu1 Cu 0.06493(3) 0.145830(11) 0.31871(3) 0.02424(12) Uani 1 d . . P1 P -0.18009(7) 0.11770(2) 0.38683(5) 0.0156(2) Uani 1 d . . O1 O -0.2500 0.04648(9) 0.5000 0.0257(7) Uani 1 d S . O2 O -0.1194(2) 0.03042(7) 0.6536(2) 0.0351(6) Uani 1 d . . O3 O -0.2565(2) 0.08573(6) 0.64563(14) 0.0198(5) Uani 1 d . . O4 O -0.0102(2) 0.04262(7) 0.5029(2) 0.0350(6) Uani 1 d . . O5 O -0.0320(2) 0.09590(6) 0.61991(15) 0.0215(5) Uani 1 d . . O6 O -0.1153(2) 0.10765(6) 0.47255(14) 0.0203(5) Uani 1 d . . O7 O -0.0961(2) 0.12982(6) 0.31680(15) 0.0231(5) Uani 1 d . . O8 O 0.1052(2) 0.14066(7) 0.5180(2) 0.0321(6) Uani 1 d . . O9 O -0.0067(2) 0.16309(7) 0.6628(2) 0.0290(6) Uani 1 d . . O10 O -0.0908(2) 0.17729(6) 0.49394(14) 0.0199(5) Uani 1 d . . O11 O -0.2285(2) 0.14586(6) 0.59448(15) 0.0183(5) Uani 1 d . . O12 O -0.2463(3) 0.21837(7) 0.5883(2) 0.0370(6) Uani 1 d . . N1 N 0.2289(3) 0.16455(10) 0.3201(3) 0.0408(9) Uani 1 d . . H1A H 0.2637(3) 0.16002(10) 0.2684(3) 0.049 Uiso 0.80 d PR . H1B H 0.2699(3) 0.15421(10) 0.3628(3) 0.049 Uiso 0.80 d PR . H1C H 0.2712(3) 0.15454(10) 0.2775(3) 0.049 Uiso 0.20 d PR . H1D H 0.2627(3) 0.16006(10) 0.3721(3) 0.049 Uiso 0.20 d PR . N2 N 0.0195(3) 0.19453(8) 0.3336(2) 0.0270(7) Uani 1 d . . H2A H -0.0221(3) 0.19663(8) 0.3834(2) 0.032 Uiso 0.80 d PR . H2B H -0.0268(3) 0.20065(8) 0.2886(2) 0.032 Uiso 0.80 d PR . H2C H -0.0398(3) 0.19609(8) 0.3721(2) 0.032 Uiso 0.20 d PR . H2D H -0.0044(3) 0.20316(8) 0.2819(2) 0.032 Uiso 0.20 d PR . N3 N 0.1187(3) 0.09701(8) 0.3132(2) 0.0287(7) Uani 1 d . . H3A H 0.1329(3) 0.09111(8) 0.2571(2) 0.034 Uiso 0.80 d PR . H3B H 0.0627(3) 0.08320(8) 0.3343(2) 0.034 Uiso 0.80 d PR . H3C H 0.1578(3) 0.09421(8) 0.2625(2) 0.034 Uiso 0.20 d PR . H3D H 0.0548(3) 0.08374(8) 0.3103(2) 0.034 Uiso 0.20 d PR . N4A N 0.3464(3) 0.05627(10) 0.2976(3) 0.0317(9) Uiso 0.80 d P . H4AA H 0.3791(3) 0.03608(10) 0.2838(3) 0.048 Uiso 0.80 d PR . H4AB H 0.3138(3) 0.06545(10) 0.2493(3) 0.048 Uiso 0.80 d PR . H4AC H 0.4014(3) 0.07048(10) 0.3185(3) 0.048 Uiso 0.80 d PR . N4B N 0.2668(16) 0.0318(5) 0.2935(12) 0.042(4) Uiso 0.20 d P . H4BA H 0.2813(16) 0.0098(5) 0.3070(12) 0.063 Uiso 0.20 d PR . H4BB H 0.2000(16) 0.0331(5) 0.2627(12) 0.063 Uiso 0.20 d PR . H4BC H 0.3258(16) 0.0401(5) 0.2610(12) 0.063 Uiso 0.20 d PR . C1A C 0.2251(5) 0.20170(15) 0.3090(4) 0.0386(14) Uiso 0.80 d P . H1AA H 0.2090(5) 0.20685(15) 0.2486(4) 0.046 Uiso 0.80 d PR . H1AB H 0.2970(5) 0.21241(15) 0.3257(4) 0.046 Uiso 0.80 d PR . C1B C 0.2280(17) 0.2007(5) 0.3435(16) 0.027(4) Uiso 0.20 d P . H1BA H 0.2739(17) 0.2112(5) 0.2982(16) 0.032 Uiso 0.20 d PR . H1BB H 0.2665(17) 0.2050(5) 0.3983(16) 0.032 Uiso 0.20 d PR . C2A C 0.1209(5) 0.21458(14) 0.3630(4) 0.0351(12) Uiso 0.80 d P . H2AA H 0.1367(5) 0.20923(14) 0.4234(4) 0.042 Uiso 0.80 d PR . H2AB H 0.1080(5) 0.23870(14) 0.3577(4) 0.042 Uiso 0.80 d PR . C2B C 0.1191(17) 0.2186(5) 0.3265(15) 0.028(4) Uiso 0.20 d P . H2BA H 0.1141(17) 0.2318(5) 0.3794(15) 0.034 Uiso 0.20 d PR . H2BB H 0.1146(17) 0.2341(5) 0.2778(15) 0.034 Uiso 0.20 d PR . C3A C 0.1925(5) 0.08339(14) 0.3842(3) 0.0323(12) Uiso 0.80 d P . H3AA H 0.1452(5) 0.08083(14) 0.4358(3) 0.039 Uiso 0.80 d PR . H3AB H 0.2510(5) 0.10017(14) 0.3971(3) 0.039 Uiso 0.80 d PR . C3B C 0.2295(18) 0.0912(5) 0.3633(13) 0.028(4) Uiso 0.20 d P . H3BA H 0.2241(18) 0.1007(5) 0.4214(13) 0.033 Uiso 0.20 d PR . H3BB H 0.2932(18) 0.1021(5) 0.3333(13) 0.033 Uiso 0.20 d PR . C4 C 0.2521(4) 0.05104(11) 0.3669(3) 0.0379(9) Uani 1 d . . H4A H 0.2868(4) 0.04270(11) 0.4201(3) 0.045 Uiso 0.80 d PR . H4B H 0.1968(4) 0.03443(11) 0.3467(3) 0.045 Uiso 0.80 d PR . H4C H 0.3199(4) 0.04751(11) 0.4027(3) 0.045 Uiso 0.20 d PR . H4D H 0.1873(4) 0.04155(11) 0.3984(3) 0.045 Uiso 0.20 d PR . O1W O 0.0000 0.2500 0.1634(4) 0.087(2) Uani 1 d S . H1WA H 0.0379 0.2667 0.1322(4) 0.131 Uiso 1 d R . O2W O -0.0602(4) -0.01689(10) 0.1646(2) 0.0627(10) Uani 1 d . . H2WA H -0.0190(4) -0.03184(10) 0.1644(2) 0.094 Uiso 1 d R . H2WB H -0.0990(4) -0.01894(10) 0.1192(2) 0.094 Uiso 1 d 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 0.0206(2) 0.0203(2) 0.0205(2) -0.00160(11) -0.00545(11) 0.00484(11) Mo2 0.0133(2) 0.0236(2) 0.0155(2) -0.00277(11) -0.00177(10) -0.00083(11) Mo3 0.0199(2) 0.0175(2) 0.0197(2) 0.000 0.0003(2) 0.000 Cu1 0.0165(2) 0.0274(2) 0.0289(2) -0.0076(2) 0.0040(2) -0.0023(2) P1 0.0133(4) 0.0204(4) 0.0131(4) -0.0020(3) -0.0003(3) 0.0001(3) O1 0.026(2) 0.022(2) 0.029(2) 0.000 -0.0129(15) 0.000 O2 0.045(2) 0.0280(14) 0.0326(14) 0.0066(11) -0.0115(13) 0.0060(12) O3 0.0183(11) 0.0238(12) 0.0173(11) 0.0043(9) -0.0020(9) 0.0020(9) O4 0.0304(13) 0.038(2) 0.0362(14) -0.0106(13) -0.0018(12) 0.0128(12) O5 0.0188(11) 0.0261(12) 0.0197(11) -0.0005(9) -0.0060(9) 0.0009(9) O6 0.0196(11) 0.0239(12) 0.0175(11) -0.0020(9) -0.0053(9) 0.0021(9) O7 0.0183(11) 0.0320(13) 0.0191(11) -0.0023(10) 0.0040(10) -0.0050(10) O8 0.0169(12) 0.044(2) 0.0349(14) -0.0016(12) 0.0050(11) 0.0010(11) O9 0.0308(13) 0.0355(15) 0.0207(12) -0.0070(11) -0.0073(11) 0.0008(11) O10 0.0170(10) 0.0250(12) 0.0178(11) 0.0020(9) 0.0016(9) -0.0034(10) O11 0.0152(11) 0.0224(11) 0.0175(10) 0.0005(9) 0.0001(9) -0.0014(9) O12 0.0420(15) 0.0311(14) 0.0380(15) -0.0131(12) -0.0030(13) 0.0055(13) N1 0.021(2) 0.046(2) 0.055(2) -0.011(2) 0.002(2) -0.004(2) N2 0.0236(15) 0.032(2) 0.0253(15) -0.0040(13) 0.0061(13) -0.0049(13) N3 0.0238(15) 0.033(2) 0.030(2) -0.0057(13) -0.0006(13) 0.0018(13) C4 0.036(2) 0.037(2) 0.041(2) 0.010(2) -0.003(2) 0.001(2) O1W 0.091(4) 0.082(5) 0.088(4) 0.000 0.000 -0.016(4) O2W 0.087(3) 0.061(2) 0.040(2) -0.013(2) 0.022(2) -0.025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O4 1.711(3) . ? Mo1 O2 1.717(3) . ? Mo1 O1 1.9008(10) . ? Mo1 O5 1.919(2) . ? Mo1 O3 2.240(2) . ? Mo1 O6 2.398(2) . ? Mo2 O8 1.708(2) . ? Mo2 O9 1.710(2) . ? Mo2 O10 1.922(2) . ? Mo2 O5 1.963(2) . ? Mo2 O6 2.190(2) . ? Mo2 O11 2.337(2) . ? Mo3 O12 1.707(3) . ? Mo3 O12 1.707(3) 7_445 ? Mo3 O10 1.912(2) 7_445 ? Mo3 O10 1.912(2) . ? Mo3 O11 2.309(2) 7_445 ? Mo3 O11 2.309(2) . ? Cu1 O7 1.952(2) . ? Cu1 N2 1.991(3) . ? Cu1 N3 2.011(3) . ? Cu1 N1 2.020(3) . ? Cu1 O9 2.557(2) . ? P1 O7 1.514(2) . ? P1 O3 1.531(2) 7_445 ? P1 O11 1.549(2) 7_445 ? P1 O6 1.553(2) . ? O1 Mo1 1.9008(10) 7_445 ? O3 P1 1.531(2) 7_445 ? O11 P1 1.549(2) 7_445 ? N1 C1B 1.46(2) . ? N1 C1A 1.466(7) . ? N2 C2A 1.474(6) . ? N2 C2B 1.49(2) . ? N3 C3A 1.473(6) . ? N3 C3B 1.50(2) . ? N4A N4B 1.33(2) . ? N4A C4 1.524(6) . ? N4B C4 1.36(2) . ? C1A C1B 0.53(2) . ? C1A C2B 1.41(2) . ? C1A C2A 1.536(8) . ? C1B C2A 1.38(2) . ? C1B C2B 1.46(3) . ? C2A C2B 0.58(2) . ? C3A C3B 0.61(2) . ? C3A C4 1.465(7) . ? C3B C4 1.60(2) . ? 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 O4 Mo1 O2 101.69(14) . . ? O4 Mo1 O1 99.37(10) . . ? O2 Mo1 O1 103.72(12) . . ? O4 Mo1 O5 98.62(12) . . ? O2 Mo1 O5 100.64(12) . . ? O1 Mo1 O5 145.92(12) . . ? O4 Mo1 O3 173.84(11) . . ? O2 Mo1 O3 84.16(11) . . ? O1 Mo1 O3 80.91(8) . . ? O5 Mo1 O3 78.24(9) . . ? O4 Mo1 O6 86.38(11) . . ? O2 Mo1 O6 168.07(11) . . ? O1 Mo1 O6 83.34(10) . . ? O5 Mo1 O6 69.18(9) . . ? O3 Mo1 O6 87.54(8) . . ? O8 Mo2 O9 104.31(13) . . ? O8 Mo2 O10 95.64(12) . . ? O9 Mo2 O10 100.82(11) . . ? O8 Mo2 O5 100.24(12) . . ? O9 Mo2 O5 95.67(11) . . ? O10 Mo2 O5 153.49(9) . . ? O8 Mo2 O6 96.48(11) . . ? O9 Mo2 O6 157.96(11) . . ? O10 Mo2 O6 84.11(9) . . ? O5 Mo2 O6 73.17(9) . . ? O8 Mo2 O11 164.50(11) . . ? O9 Mo2 O11 87.38(11) . . ? O10 Mo2 O11 71.85(9) . . ? O5 Mo2 O11 88.46(9) . . ? O6 Mo2 O11 73.64(8) . . ? O12 Mo3 O12 104.0(2) . 7_445 ? O12 Mo3 O10 99.52(12) . 7_445 ? O12 Mo3 O10 101.17(12) 7_445 7_445 ? O12 Mo3 O10 101.17(12) . . ? O12 Mo3 O10 99.52(12) 7_445 . ? O10 Mo3 O10 146.08(13) 7_445 . ? O12 Mo3 O11 166.03(11) . 7_445 ? O12 Mo3 O11 89.06(12) 7_445 7_445 ? O10 Mo3 O11 72.66(8) 7_445 7_445 ? O10 Mo3 O11 81.13(9) . 7_445 ? O12 Mo3 O11 89.06(12) . . ? O12 Mo3 O11 166.03(11) 7_445 . ? O10 Mo3 O11 81.13(9) 7_445 . ? O10 Mo3 O11 72.66(8) . . ? O11 Mo3 O11 78.41(12) 7_445 . ? O7 Cu1 N2 93.52(11) . . ? O7 Cu1 N3 89.13(12) . . ? N2 Cu1 N3 175.09(13) . . ? O7 Cu1 N1 177.44(13) . . ? N2 Cu1 N1 83.98(14) . . ? N3 Cu1 N1 93.41(14) . . ? O9 Cu1 N2 75.5(11) . . ? O9 Cu1 O7 79.8(12) . . ? O9 Cu1 N1 99.0(11) . . ? O9 Cu1 N3 107.0(13) . . ? O7 P1 O3 109.40(13) . 7_445 ? O7 P1 O11 109.71(14) . 7_445 ? O3 P1 O11 108.66(13) 7_445 7_445 ? O7 P1 O6 111.53(13) . . ? O3 P1 O6 106.96(13) 7_445 . ? O11 P1 O6 110.50(13) 7_445 . ? Mo1 O1 Mo1 150.1(2) . 7_445 ? P1 O3 Mo1 123.36(12) 7_445 . ? Mo1 O5 Mo2 121.68(11) . . ? P1 O6 Mo2 127.82(14) . . ? P1 O6 Mo1 134.87(13) . . ? Mo2 O6 Mo1 95.18(8) . . ? P1 O7 Cu1 133.88(14) . . ? Mo3 O10 Mo2 122.58(11) . . ? P1 O11 Mo3 126.45(13) 7_445 . ? P1 O11 Mo2 130.23(13) 7_445 . ? Mo3 O11 Mo2 92.75(8) . . ? C1B N1 C1A 20.8(9) . . ? C1B N1 Cu1 110.4(8) . . ? C1A N1 Cu1 109.4(3) . . ? C2A N2 C2B 22.5(8) . . ? C2A N2 Cu1 109.8(3) . . ? C2B N2 Cu1 113.4(8) . . ? C3A N3 C3B 23.8(8) . . ? C3A N3 Cu1 119.4(3) . . ? C3B N3 Cu1 112.5(8) . . ? N4B N4A C4 56.4(8) . . ? N4A N4B C4 69.2(9) . . ? C1B C1A C2B 84.4(27) . . ? C1B C1A N1 79.0(25) . . ? C2B C1A N1 118.0(9) . . ? C1B C1A C2A 62.7(25) . . ? C2B C1A C2A 22.1(9) . . ? N1 C1A C2A 106.7(5) . . ? C1A C1B C2A 97.4(28) . . ? C1A C1B C2B 74.5(26) . . ? C2A C1B C2B 23.4(9) . . ? C1A C1B N1 80.3(25) . . ? C2A C1B N1 116.3(14) . . ? C2B C1B N1 115.5(16) . . ? C2B C2A C1B 86.0(24) . . ? C2B C2A N2 79.9(22) . . ? C1B C2A N2 115.4(9) . . ? C2B C2A C1A 66.5(21) . . ? C1B C2A C1A 19.9(9) . . ? N2 C2A C1A 106.1(4) . . ? C2A C2B C1A 91.4(24) . . ? C2A C2B C1B 70.7(23) . . ? C1A C2B C1B 21.1(9) . . ? C2A C2B N2 77.6(22) . . ? C1A C2B N2 112.4(13) . . ? C1B C2B N2 110.0(15) . . ? C3B C3A C4 90.9(19) . . ? C3B C3A N3 80.5(19) . . ? C4 C3A N3 116.7(4) . . ? C3A C3B N3 75.7(19) . . ? C3A C3B C4 66.5(18) . . ? N3 C3B C4 107.7(12) . . ? N4B C4 C3A 133.4(9) . . ? N4B C4 N4A 54.4(8) . . ? C3A C4 N4A 109.9(4) . . ? N4B C4 C3B 122.7(11) . . ? C3A C4 C3B 22.6(7) . . ? N4A C4 C3B 87.7(9) . . ? _refine_diff_density_max 0.451 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.102 #===END