# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 # # Cambridge Crystallographic Data Centre # CCDC # data_njy1 _database_code_depnum_ccdc_archive 'CCDC 846086' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H34 As2 Cu4 Mo6 N8 O30' _chemical_formula_weight 1702.07 _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' As As 0.0499 2.0058 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.309(3) _cell_length_b 19.650(6) _cell_length_c 19.308(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.975(4) _cell_angle_gamma 90.00 _cell_volume 3826(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6453 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 5.897 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1767 _exptl_absorpt_correction_T_max 0.2622 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9230 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3356 _reflns_number_gt 3175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+116.8716P] 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 3356 _refine_ls_number_parameters 262 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 As1 As 0.08521(8) 0.25879(4) -0.03554(4) 0.0071(2) Uani 1 1 d U . . Mo1 Mo 0.19426(8) 0.23229(4) 0.15950(4) 0.0140(2) Uani 1 1 d . . . Mo2 Mo 0.20095(7) 0.09858(4) 0.05850(4) 0.0133(2) Uani 1 1 d . . . Mo3 Mo 0.24858(8) 0.11646(4) -0.10330(4) 0.0149(2) Uani 1 1 d . . . Cu2 Cu -0.19156(10) 0.34374(6) -0.10316(6) 0.0157(3) Uani 1 1 d . . . Cu1 Cu -0.24403(10) 0.19717(6) -0.05581(6) 0.0128(3) Uani 1 1 d . . . N1 N -0.1614(8) 0.1072(4) -0.0675(4) 0.0195(18) Uani 1 1 d . . . H1C H -0.0746 0.1078 -0.0470 0.023 Uiso 1 1 calc R . . H1D H -0.2011 0.0741 -0.0472 0.023 Uiso 1 1 calc R . . N2 N -0.3476(9) 0.1807(5) -0.1534(4) 0.0237(19) Uani 1 1 d . . . H2C H -0.4346 0.1859 -0.1542 0.028 Uiso 1 1 calc R . . H2D H -0.3243 0.2114 -0.1832 0.028 Uiso 1 1 calc R . . N3 N -0.0898(8) 0.3746(5) -0.1767(5) 0.0236(19) Uani 1 1 d . . . H3C H -0.0044 0.3822 -0.1561 0.028 Uiso 1 1 calc R . . H3D H -0.0925 0.3422 -0.2098 0.028 Uiso 1 1 calc R . . N4 N -0.3288(9) 0.4104(6) -0.1496(6) 0.037(3) Uani 1 1 d . . . H4C H -0.4093 0.3906 -0.1579 0.045 Uiso 1 1 calc R . . H4D H -0.3305 0.4462 -0.1208 0.045 Uiso 1 1 calc R . . O1 O 0.0494(7) 0.2000(4) 0.1757(4) 0.0282(18) Uani 1 1 d . . . O2 O 0.2891(8) 0.2478(4) 0.2426(4) 0.0329(19) Uani 1 1 d . . . O3 O 0.1287(6) 0.3215(3) 0.1325(3) 0.0155(13) Uani 1 1 d U . . O4 O 0.2812(6) 0.1511(3) 0.1399(3) 0.0166(14) Uani 1 1 d . . . O5 O 0.1015(6) 0.2077(3) 0.0370(3) 0.0142(13) Uani 1 1 d . . . O6 O 0.0632(7) 0.0695(4) 0.0846(4) 0.0299(18) Uani 1 1 d . . . O7 O 0.3082(7) 0.0315(4) 0.0703(4) 0.0257(17) Uani 1 1 d . . . O8 O 0.3518(6) 0.1625(3) 0.0123(3) 0.0102(12) Uani 1 1 d U . . O9 O 0.1321(6) 0.0954(3) -0.0416(3) 0.0163(14) Uani 1 1 d . . . O10 O 0.3557(7) 0.0487(4) -0.0823(4) 0.0263(17) Uani 1 1 d . . . O11 O 0.1477(8) 0.0954(5) -0.1821(4) 0.035(2) Uani 1 1 d . . . O12 O 0.1632(6) 0.2224(3) -0.0970(3) 0.0120(13) Uani 1 1 d U . . O13 O -0.0754(6) 0.2650(3) -0.0723(4) 0.0146(14) Uani 1 1 d . . . O14 O -0.3100(6) 0.2938(3) -0.0495(3) 0.0117(13) Uani 1 1 d . . . O1W O -0.1030(8) 0.4137(4) -0.0117(5) 0.041(2) Uani 1 1 d . . . C1 C -0.1789(10) 0.0949(6) -0.1442(6) 0.028(2) Uani 1 1 d . . . H1A H -0.1596 0.0478 -0.1531 0.033 Uiso 1 1 calc R . . H1B H -0.1197 0.1238 -0.1642 0.033 Uiso 1 1 calc R . . C2 C -0.3235(11) 0.1115(6) -0.1774(6) 0.026(2) Uani 1 1 d . . . H2A H -0.3379 0.1100 -0.2287 0.031 Uiso 1 1 calc R . . H2B H -0.3826 0.0792 -0.1620 0.031 Uiso 1 1 calc R . . C3 C -0.1502(11) 0.4373(5) -0.2095(5) 0.024(2) Uani 1 1 d . . . H3A H -0.1288 0.4430 -0.2558 0.029 Uiso 1 1 calc R . . H3B H -0.1154 0.4762 -0.1805 0.029 Uiso 1 1 calc R . . C4 C -0.2979(10) 0.4337(5) -0.2168(5) 0.023(2) Uani 1 1 d . . . H4A H -0.3367 0.4782 -0.2289 0.028 Uiso 1 1 calc R . . H4B H -0.3353 0.4023 -0.2545 0.028 Uiso 1 1 calc R . . _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 As1 0.0040(4) 0.0098(4) 0.0096(4) 0.0011(3) 0.0062(3) 0.0005(3) Mo1 0.0113(4) 0.0234(5) 0.0102(4) 0.0036(3) 0.0089(3) 0.0046(3) Mo2 0.0095(4) 0.0129(4) 0.0199(4) 0.0048(3) 0.0085(3) 0.0001(3) Mo3 0.0146(4) 0.0161(4) 0.0165(4) -0.0044(3) 0.0087(3) 0.0016(3) Cu2 0.0081(6) 0.0203(7) 0.0212(6) 0.0097(5) 0.0084(5) 0.0023(4) Cu1 0.0088(5) 0.0174(6) 0.0136(6) 0.0014(4) 0.0058(4) 0.0009(4) N1 0.020(4) 0.009(4) 0.027(5) 0.000(3) -0.003(4) -0.002(3) N2 0.020(4) 0.041(6) 0.010(4) 0.002(4) 0.003(3) 0.005(4) N3 0.020(4) 0.028(5) 0.025(5) 0.002(4) 0.010(4) -0.004(4) N4 0.019(5) 0.042(6) 0.058(7) 0.027(5) 0.024(5) 0.008(4) O1 0.018(4) 0.039(5) 0.032(4) 0.017(3) 0.016(3) 0.001(3) O2 0.032(4) 0.049(5) 0.017(4) -0.008(3) 0.003(3) 0.013(4) O3 0.0154(16) 0.0164(16) 0.0156(16) -0.0003(10) 0.0052(10) 0.0008(10) O4 0.014(3) 0.025(4) 0.012(3) 0.007(3) 0.006(3) 0.009(3) O5 0.014(3) 0.012(3) 0.018(3) 0.008(3) 0.008(3) 0.004(2) O6 0.024(4) 0.038(5) 0.033(4) 0.008(4) 0.016(3) -0.010(3) O7 0.013(3) 0.019(4) 0.047(5) 0.008(3) 0.012(3) 0.005(3) O8 0.0096(15) 0.0107(15) 0.0104(15) -0.0002(10) 0.0026(10) -0.0005(10) O9 0.013(3) 0.020(4) 0.017(3) -0.004(3) 0.004(3) -0.006(3) O10 0.026(4) 0.021(4) 0.033(4) -0.005(3) 0.008(3) 0.011(3) O11 0.027(4) 0.050(5) 0.026(4) -0.010(4) 0.001(3) -0.004(4) O12 0.0119(15) 0.0125(15) 0.0122(15) -0.0001(10) 0.0040(10) 0.0003(10) O13 0.004(3) 0.017(4) 0.022(4) 0.006(3) 0.003(3) -0.002(2) O14 0.009(3) 0.013(3) 0.015(3) 0.002(2) 0.009(2) 0.004(2) O1W 0.017(4) 0.039(5) 0.072(7) -0.019(4) 0.019(4) -0.005(3) C1 0.018(5) 0.035(6) 0.035(6) -0.006(5) 0.016(5) 0.006(4) C2 0.024(6) 0.030(6) 0.023(5) -0.007(4) 0.003(4) 0.003(4) C3 0.036(6) 0.022(6) 0.020(5) 0.002(4) 0.019(5) 0.001(4) C4 0.025(5) 0.023(6) 0.024(5) 0.007(4) 0.010(4) 0.002(4) _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. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 O13 1.665(6) . ? As1 O8 1.702(6) 7 ? As1 O5 1.703(6) . ? As1 O12 1.720(6) . ? Mo1 O1 1.711(7) . ? Mo1 O2 1.723(7) . ? Mo1 O4 1.906(7) . ? Mo1 O3 1.912(7) . ? Mo1 O12 2.268(6) 7 ? Mo1 O5 2.409(7) . ? Mo2 O6 1.701(7) . ? Mo2 O7 1.704(7) . ? Mo2 O9 1.916(6) . ? Mo2 O4 1.918(7) . ? Mo2 O8 2.317(6) . ? Mo2 O5 2.376(6) . ? Mo3 O11 1.706(8) . ? Mo3 O10 1.723(7) . ? Mo3 O9 1.905(6) . ? Mo3 O3 1.923(6) 7 ? Mo3 O12 2.274(6) . ? Mo3 O8 2.438(6) . ? Cu2 O13 1.971(6) . ? Cu2 N4 1.998(9) . ? Cu2 O14 2.012(6) . ? Cu2 N3 2.025(8) . ? Cu2 O1W 2.275(9) . ? Cu1 N2 1.991(8) . ? Cu1 N1 1.996(8) . ? Cu1 O14 2.001(6) 7_455 ? Cu1 O14 2.030(6) . ? Cu1 O13 2.265(6) . ? Cu1 Cu1 3.013(2) 7_455 ? N1 C1 1.475(14) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C2 1.473(14) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 C3 1.464(14) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 C4 1.472(13) . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? O3 Mo3 1.923(6) 7 ? O8 As1 1.702(6) 7 ? O12 Mo1 2.268(6) 7 ? O14 Cu1 2.001(6) 7_455 ? C1 C2 1.531(15) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.502(15) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? _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 As1 O8 109.7(3) . 7 ? O13 As1 O5 108.3(3) . . ? O8 As1 O5 110.6(3) 7 . ? O13 As1 O12 107.6(3) . . ? O8 As1 O12 110.6(3) 7 . ? O5 As1 O12 110.0(3) . . ? O1 Mo1 O2 104.1(4) . . ? O1 Mo1 O4 101.0(3) . . ? O2 Mo1 O4 97.7(3) . . ? O1 Mo1 O3 96.8(3) . . ? O2 Mo1 O3 101.0(3) . . ? O4 Mo1 O3 150.1(3) . . ? O1 Mo1 O12 158.4(3) . 7 ? O2 Mo1 O12 96.9(3) . 7 ? O4 Mo1 O12 80.8(3) . 7 ? O3 Mo1 O12 74.1(2) . 7 ? O1 Mo1 O5 85.5(3) . . ? O2 Mo1 O5 169.2(3) . . ? O4 Mo1 O5 75.2(2) . . ? O3 Mo1 O5 82.5(2) . . ? O12 Mo1 O5 74.1(2) 7 . ? O6 Mo2 O7 105.0(4) . . ? O6 Mo2 O9 97.5(3) . . ? O7 Mo2 O9 101.8(3) . . ? O6 Mo2 O4 100.5(3) . . ? O7 Mo2 O4 98.6(3) . . ? O9 Mo2 O4 148.2(3) . . ? O6 Mo2 O8 164.7(3) . . ? O7 Mo2 O8 90.1(3) . . ? O9 Mo2 O8 76.5(2) . . ? O4 Mo2 O8 79.3(2) . . ? O6 Mo2 O5 89.9(3) . . ? O7 Mo2 O5 164.9(3) . . ? O9 Mo2 O5 78.3(3) . . ? O4 Mo2 O5 75.8(2) . . ? O8 Mo2 O5 75.1(2) . . ? O11 Mo3 O10 105.3(4) . . ? O11 Mo3 O9 99.1(3) . . ? O10 Mo3 O9 98.1(3) . . ? O11 Mo3 O3 102.1(4) . 7 ? O10 Mo3 O3 97.5(3) . 7 ? O9 Mo3 O3 149.2(3) . 7 ? O11 Mo3 O12 95.7(3) . . ? O10 Mo3 O12 158.6(3) . . ? O9 Mo3 O12 82.2(3) . . ? O3 Mo3 O12 73.8(2) 7 . ? O11 Mo3 O8 167.4(3) . . ? O10 Mo3 O8 86.2(3) . . ? O9 Mo3 O8 73.7(2) . . ? O3 Mo3 O8 81.0(2) 7 . ? O12 Mo3 O8 73.2(2) . . ? O13 Cu2 N4 168.2(4) . . ? O13 Cu2 O14 81.8(2) . . ? N4 Cu2 O14 95.8(3) . . ? O13 Cu2 N3 94.4(3) . . ? N4 Cu2 N3 84.9(4) . . ? O14 Cu2 N3 164.7(3) . . ? O13 Cu2 O1W 96.8(3) . . ? N4 Cu2 O1W 94.9(4) . . ? O14 Cu2 O1W 94.8(3) . . ? N3 Cu2 O1W 100.4(3) . . ? N2 Cu1 N1 84.6(4) . . ? N2 Cu1 O14 163.3(3) . 7_455 ? N1 Cu1 O14 99.1(3) . 7_455 ? N2 Cu1 O14 95.1(3) . . ? N1 Cu1 O14 172.8(3) . . ? O14 Cu1 O14 83.3(3) 7_455 . ? N2 Cu1 O13 103.8(3) . . ? N1 Cu1 O13 98.5(3) . . ? O14 Cu1 O13 91.8(2) 7_455 . ? O14 Cu1 O13 74.6(2) . . ? N2 Cu1 Cu1 134.1(3) . 7_455 ? N1 Cu1 Cu1 140.6(2) . 7_455 ? O14 Cu1 Cu1 41.99(17) 7_455 7_455 ? O14 Cu1 Cu1 41.26(18) . 7_455 ? O13 Cu1 Cu1 80.87(18) . 7_455 ? C1 N1 Cu1 107.0(6) . . ? C1 N1 H1C 110.3 . . ? Cu1 N1 H1C 110.3 . . ? C1 N1 H1D 110.3 . . ? Cu1 N1 H1D 110.3 . . ? H1C N1 H1D 108.6 . . ? C2 N2 Cu1 110.8(6) . . ? C2 N2 H2C 109.5 . . ? Cu1 N2 H2C 109.5 . . ? C2 N2 H2D 109.5 . . ? Cu1 N2 H2D 109.5 . . ? H2C N2 H2D 108.1 . . ? C3 N3 Cu2 108.7(6) . . ? C3 N3 H3C 110.0 . . ? Cu2 N3 H3C 110.0 . . ? C3 N3 H3D 110.0 . . ? Cu2 N3 H3D 110.0 . . ? H3C N3 H3D 108.3 . . ? C4 N4 Cu2 109.7(7) . . ? C4 N4 H4C 109.7 . . ? Cu2 N4 H4C 109.7 . . ? C4 N4 H4D 109.7 . . ? Cu2 N4 H4D 109.7 . . ? H4C N4 H4D 108.2 . . ? Mo1 O3 Mo3 116.4(3) . 7 ? Mo1 O4 Mo2 118.2(3) . . ? As1 O5 Mo2 129.9(3) . . ? As1 O5 Mo1 129.8(3) . . ? Mo2 O5 Mo1 86.6(2) . . ? As1 O8 Mo2 129.9(3) 7 . ? As1 O8 Mo3 130.5(3) 7 . ? Mo2 O8 Mo3 87.2(2) . . ? Mo3 O9 Mo2 118.3(3) . . ? As1 O12 Mo1 130.6(3) . 7 ? As1 O12 Mo3 131.2(3) . . ? Mo1 O12 Mo3 91.7(2) 7 . ? As1 O13 Cu2 132.4(4) . . ? As1 O13 Cu1 128.4(3) . . ? Cu2 O13 Cu1 93.9(2) . . ? Cu1 O14 Cu2 114.2(3) 7_455 . ? Cu1 O14 Cu1 96.7(3) 7_455 . ? Cu2 O14 Cu1 100.3(2) . . ? N1 C1 C2 107.0(8) . . ? N1 C1 H1A 110.3 . . ? C2 C1 H1A 110.3 . . ? N1 C1 H1B 110.3 . . ? C2 C1 H1B 110.3 . . ? H1A C1 H1B 108.6 . . ? N2 C2 C1 106.2(9) . . ? N2 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? N2 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? N3 C3 C4 109.4(8) . . ? N3 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N3 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N4 C4 C3 109.4(9) . . ? N4 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N4 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.369 _refine_diff_density_min -1.756 _refine_diff_density_rms 0.277 data_njy1_2 _database_code_depnum_ccdc_archive 'CCDC 846087' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H108 As4 Cu6 Mo18 N24 O74' _chemical_formula_weight 4445.28 _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' As As 0.0499 2.0058 '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 P2/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.7091(8) _cell_length_b 14.2336(7) _cell_length_c 22.3560(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.8803(8) _cell_angle_gamma 90.00 _cell_volume 5493.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9777 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.39 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4268 _exptl_absorpt_coefficient_mu 4.416 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2847 _exptl_absorpt_correction_T_max 0.5206 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26694 _diffrn_reflns_av_R_equivalents 0.2429 _diffrn_reflns_av_sigmaI/netI 0.1501 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9649 _reflns_number_gt 7599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1954P)^2^+13.2250P] 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 SHELXL _refine_ls_extinction_coef 0.0014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9649 _refine_ls_number_parameters 692 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1198 _refine_ls_R_factor_gt 0.1061 _refine_ls_wR_factor_ref 0.2922 _refine_ls_wR_factor_gt 0.2754 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 0.10324(6) 0.72775(8) 0.03760(6) 0.0276(3) Uani 1 1 d . . . Mo2 Mo 0.09052(6) 0.78724(9) -0.12281(6) 0.0291(3) Uani 1 1 d . . . Mo3 Mo 0.12130(6) 0.56292(8) -0.06979(6) 0.0260(3) Uani 1 1 d . . . Mo4 Mo 0.28487(7) 0.78280(9) -0.18014(5) 0.0301(3) Uani 1 1 d . . . Mo5 Mo 0.30425(6) 0.55734(9) -0.13486(5) 0.0271(3) Uani 1 1 d . . . Mo6 Mo 0.31600(6) 0.49342(8) 0.03083(5) 0.0260(3) Uani 1 1 d . . . Mo7 Mo 0.30847(6) 0.66288(9) 0.13352(5) 0.0275(3) Uani 1 1 d . . . Mo8 Mo 0.28459(7) 0.91544(9) 0.08367(6) 0.0342(4) Uani 1 1 d . . . Mo9 Mo 0.27056(6) 0.97138(8) -0.06488(6) 0.0302(3) Uani 1 1 d . . . As1 As 0.27511(7) 0.72736(9) -0.02554(6) 0.0218(3) Uani 1 1 d . . . As2 As 0.10717(9) 0.92439(11) -0.01564(8) 0.0381(4) Uani 1 1 d . . . Cu1 Cu 0.5000 0.66103(18) 0.2500 0.0298(6) Uani 1 2 d S . . Cu2 Cu 0.12211(10) 0.65067(14) -0.37387(9) 0.0381(5) Uani 1 1 d . . . Cu3 Cu 0.0000 1.0979(2) -0.2500 0.0459(7) Uani 1 2 d S . . Cu4 Cu 0.4733(3) 0.2268(2) 0.05345(18) 0.1108(14) Uani 1 1 d D . . O1 O 0.0376(6) 0.7519(9) 0.0818(6) 0.050(3) Uani 1 1 d . . . O2 O 0.0153(5) 0.8461(9) -0.1698(5) 0.049(3) Uani 1 1 d . . . O3 O 0.0566(5) 0.4731(7) -0.0919(6) 0.043(3) Uani 1 1 d . . . O4 O 0.2470(7) 0.8255(9) -0.2516(5) 0.050(3) Uani 1 1 d . . . O5 O 0.2817(6) 0.4588(9) -0.1772(5) 0.047(3) Uani 1 1 d . . . O6 O 0.2960(6) 0.3743(7) 0.0341(5) 0.044(3) Uani 1 1 d . . . O7 O 0.2838(6) 0.6518(9) 0.2023(5) 0.050(3) Uani 1 1 d . . . O8 O 0.2540(8) 0.9790(8) 0.1376(6) 0.055(3) Uani 1 1 d . . . O9 O 0.2258(6) 1.0670(9) -0.1046(5) 0.048(3) Uani 1 1 d U . . O10 O 0.3815(7) 0.7859(9) -0.1748(6) 0.057(3) Uani 1 1 d . . . O11 O 0.4012(5) 0.5717(7) -0.1303(5) 0.035(2) Uani 1 1 d . . . O12 O 0.4151(5) 0.4930(8) 0.0567(5) 0.045(3) Uani 1 1 d . . . O13 O 0.4086(5) 0.6562(9) 0.1534(5) 0.045(3) Uani 1 1 d . . . O14 O 0.3782(7) 0.9470(8) 0.0923(6) 0.049(3) Uani 1 1 d . . . O15 O 0.3664(6) 1.0054(7) -0.0432(6) 0.045(3) Uani 1 1 d . . . O16 O 0.0518(5) 0.8143(8) -0.0401(5) 0.039(2) Uani 1 1 d . . . O17 O 0.0624(5) 0.6287(7) -0.0064(5) 0.032(2) Uani 1 1 d . . . O18 O 0.0515(5) 0.6687(7) -0.1221(4) 0.033(2) Uani 1 1 d U . . O19 O 0.1612(5) 0.7740(7) -0.1652(5) 0.035(2) Uani 1 1 d . . . O20 O 0.3138(5) 0.5104(8) -0.0536(4) 0.036(2) Uani 1 1 d . . . O21 O 0.2661(6) 0.6509(7) -0.1989(4) 0.035(2) Uani 1 1 d . . . O22 O 0.3000(6) 0.7951(8) 0.1196(5) 0.039(2) Uani 1 1 d . . . O23 O 0.1877(5) 0.5189(7) -0.0055(5) 0.037(2) Uani 1 1 d . . . O24 O 0.1626(5) 0.8521(7) 0.0441(5) 0.033(2) Uani 1 1 d . . . O25 O 0.2398(6) 0.9961(7) 0.0133(5) 0.040(2) Uani 1 1 d . . . O26 O 0.2899(5) 0.5318(7) 0.1066(4) 0.033(2) Uani 1 1 d . . . O27 O 0.2788(6) 0.8898(7) -0.1288(5) 0.036(2) Uani 1 1 d . . . O28 O 0.1825(5) 0.6784(8) 0.0880(5) 0.037(2) Uani 1 1 d . . . O29 O 0.1528(5) 0.9004(8) -0.0780(5) 0.039(2) Uani 1 1 d . . . O30 O 0.1806(6) 0.5625(7) -0.1235(5) 0.037(2) Uani 1 1 d . . . O31 O 0.1768(4) 0.7111(7) -0.0402(4) 0.0244(19) Uani 1 1 d . . . O32 O 0.3074(5) 0.7026(7) -0.0881(4) 0.028(2) Uani 1 1 d . . . O33 O 0.3166(4) 0.6544(6) 0.0313(4) 0.0240(19) Uani 1 1 d . . . O34 O 0.3005(5) 0.8381(8) -0.0057(4) 0.033(2) Uani 1 1 d . . . N1 N 0.4389(7) 0.7679(9) 0.2751(6) 0.036(3) Uani 1 1 d . . . N2 N 0.4358(6) 0.5570(9) 0.2738(6) 0.037(3) Uani 1 1 d . . . H2B H 0.4451 0.5513 0.3148 0.044 Uiso 1 1 calc R . . H2C H 0.3850 0.5687 0.2595 0.044 Uiso 1 1 calc R . . N3 N 0.1069(7) 0.6349(12) -0.2870(7) 0.053(4) Uani 1 1 d . . . H3B H 0.1515 0.6463 -0.2596 0.064 Uiso 1 1 calc R . . H3C H 0.0707 0.6752 -0.2800 0.064 Uiso 1 1 calc R . . N4 N 0.1110(8) 0.5092(9) -0.3795(7) 0.043(3) Uani 1 1 d . . . H4A H 0.0631 0.4930 -0.4000 0.052 Uiso 1 1 calc R . . H4B H 0.1458 0.4844 -0.3988 0.052 Uiso 1 1 calc R . . N5 N 0.1198(7) 0.6672(9) -0.4644(6) 0.040(3) Uani 1 1 d . . . H5A H 0.1553 0.6292 -0.4749 0.048 Uiso 1 1 calc R . . H5B H 0.0729 0.6506 -0.4866 0.048 Uiso 1 1 calc R . . N6 N 0.1370(9) 0.7900(11) -0.3712(7) 0.055(3) Uani 1 1 d U . . H6B H 0.0914 0.8191 -0.3732 0.066 Uiso 1 1 calc R . . H6C H 0.1697 0.8068 -0.3360 0.066 Uiso 1 1 calc R . . N7 N -0.0805(8) 1.0019(11) -0.2417(9) 0.058(4) Uani 1 1 d U . . H7C H -0.0906 0.9656 -0.2755 0.069 Uiso 1 1 calc R . . H7D H -0.0612 0.9646 -0.2094 0.069 Uiso 1 1 calc R . . N8 N -0.0762(9) 1.1900(11) -0.2313(9) 0.062(4) Uani 1 1 d . . . H8C H -0.0540 1.2238 -0.1980 0.074 Uiso 1 1 calc R . . H8D H -0.0907 1.2297 -0.2631 0.074 Uiso 1 1 calc R . . N9 N 0.5040(13) 0.1551(16) -0.0129(9) 0.098(7) Uiso 1 1 d D . . H9C H 0.5499 0.1274 0.0021 0.117 Uiso 1 1 calc R . . H9D H 0.4689 0.1095 -0.0257 0.117 Uiso 1 1 calc R . . N10 N 0.5032(9) 0.3369(11) 0.0089(7) 0.063(5) Uani 1 1 d D . . H10C H 0.4764 0.3880 0.0158 0.076 Uiso 1 1 calc R . . H10D H 0.5541 0.3489 0.0223 0.076 Uiso 1 1 calc R . . N11 N 0.4482(9) 0.2996(13) 0.1246(9) 0.068(5) Uani 1 1 d . . . H11C H 0.4895 0.3348 0.1418 0.082 Uiso 1 1 calc R . . H11D H 0.4086 0.3390 0.1098 0.082 Uiso 1 1 calc R . . N12 N 0.4585(17) 0.128(2) 0.1022(14) 0.131(7) Uiso 1 1 d U . . H12B H 0.4423 0.0776 0.0783 0.158 Uiso 1 1 calc R . . H12C H 0.5040 0.1128 0.1274 0.158 Uiso 1 1 calc R . . C1 C 0.3782(9) 0.7650(13) 0.3007(8) 0.044(4) Uani 1 1 d . . . H1A H 0.3604 0.7062 0.3093 0.053 Uiso 1 1 calc R . . C2 C 0.3395(11) 0.8426(16) 0.3155(10) 0.068(6) Uani 1 1 d . . . H2A H 0.2969 0.8379 0.3333 0.082 Uiso 1 1 calc R . . C3 C 0.3692(17) 0.9287(15) 0.3016(11) 0.077(7) Uani 1 1 d . . . H3A H 0.3437 0.9831 0.3090 0.093 Uiso 1 1 calc R . . C4 C 0.4343(15) 0.9382(14) 0.2773(13) 0.077(7) Uani 1 1 d . . . C5 C 0.4658(11) 0.8547(13) 0.2618(9) 0.053(4) Uani 1 1 d . . . C6 C 0.474(3) 1.0237(19) 0.2658(19) 0.143(16) Uani 1 1 d . . . H6A H 0.4607 1.0801 0.2819 0.172 Uiso 1 1 calc R . . C7 C 0.4577(9) 0.4732(11) 0.2468(7) 0.039(3) Uani 1 1 d . . . H7A H 0.4319 0.4704 0.2037 0.047 Uiso 1 1 calc R . . H7B H 0.4423 0.4186 0.2671 0.047 Uiso 1 1 calc R . . C8 C 0.0823(11) 0.5386(19) -0.2817(11) 0.073(7) Uani 1 1 d . . . H8A H 0.0271 0.5330 -0.2988 0.088 Uiso 1 1 calc R . . H8B H 0.0924 0.5203 -0.2389 0.088 Uiso 1 1 calc R . . C9 C 0.1255(11) 0.4766(15) -0.3155(9) 0.058(5) Uani 1 1 d . . . H9A H 0.1804 0.4791 -0.2969 0.069 Uiso 1 1 calc R . . H9B H 0.1081 0.4121 -0.3140 0.069 Uiso 1 1 calc R . . C10 C 0.1354(13) 0.7611(17) -0.4778(11) 0.073(6) Uani 1 1 d . . . H10A H 0.0878 0.7906 -0.4995 0.087 Uiso 1 1 calc R . . H10B H 0.1716 0.7616 -0.5046 0.087 Uiso 1 1 calc R . . C11 C 0.1681(13) 0.8157(17) -0.4223(10) 0.071(5) Uani 1 1 d U . . H11A H 0.2238 0.8069 -0.4117 0.086 Uiso 1 1 calc R . . H11B H 0.1581 0.8819 -0.4310 0.086 Uiso 1 1 calc R . . C12 C -0.1476(12) 1.0402(15) -0.2339(13) 0.073(5) Uani 1 1 d U . . H12A H -0.1636 1.0078 -0.2007 0.087 Uiso 1 1 calc R . . H12D H -0.1873 1.0301 -0.2709 0.087 Uiso 1 1 calc R . . C13 C -0.1428(12) 1.142(2) -0.2202(18) 0.114(12) Uani 1 1 d . . . H13A H -0.1887 1.1718 -0.2445 0.137 Uiso 1 1 calc R . . H13B H -0.1440 1.1502 -0.1774 0.137 Uiso 1 1 calc R . . C14 C 0.5103(14) 0.2147(13) -0.0666(8) 0.081(7) Uiso 1 1 d D . . H14A H 0.4779 0.1885 -0.1036 0.097 Uiso 1 1 calc R . . H14B H 0.5634 0.2144 -0.0713 0.097 Uiso 1 1 calc R . . C15 C 0.4856(15) 0.3144(13) -0.0586(7) 0.094(8) Uiso 1 1 d D . . H15A H 0.5133 0.3573 -0.0798 0.112 Uiso 1 1 calc R . . H15B H 0.4305 0.3214 -0.0759 0.112 Uiso 1 1 calc R . . C16 C 0.4282(12) 0.2437(14) 0.1701(11) 0.064(5) Uani 1 1 d . . . H16A H 0.3886 0.2747 0.1868 0.077 Uiso 1 1 calc R . . H16B H 0.4732 0.2335 0.2032 0.077 Uiso 1 1 calc R . . C17 C 0.398(2) 0.150(3) 0.1416(16) 0.118 Uiso 1 1 d U . . H17A H 0.3460 0.1560 0.1162 0.142 Uiso 1 1 calc R . . H17B H 0.3981 0.1023 0.1726 0.142 Uiso 1 1 calc R . . O1W O 0.2649(6) 0.6306(9) -0.3296(6) 0.050(3) Uani 1 1 d . . . O2W O -0.0583(8) 1.1002(12) -0.3694(7) 0.075(4) Uani 1 1 d . . . O3W O 0.346(2) 0.210(3) -0.018(2) 0.247(19) Uiso 1 1 d . . . _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 0.0193(5) 0.0236(7) 0.0439(7) 0.0042(5) 0.0155(5) 0.0020(5) Mo2 0.0199(5) 0.0252(7) 0.0423(7) 0.0068(5) 0.0074(5) 0.0015(5) Mo3 0.0188(5) 0.0189(7) 0.0409(7) 0.0012(5) 0.0079(4) -0.0029(4) Mo4 0.0315(6) 0.0282(7) 0.0345(7) 0.0021(5) 0.0161(5) -0.0017(5) Mo5 0.0279(6) 0.0222(7) 0.0344(7) -0.0049(5) 0.0137(5) 0.0031(5) Mo6 0.0229(5) 0.0187(7) 0.0382(7) 0.0052(5) 0.0107(4) 0.0047(4) Mo7 0.0226(5) 0.0306(7) 0.0302(6) 0.0017(5) 0.0082(4) -0.0016(5) Mo8 0.0358(6) 0.0248(7) 0.0464(8) -0.0088(5) 0.0188(5) -0.0043(5) Mo9 0.0300(6) 0.0162(7) 0.0499(8) 0.0019(5) 0.0206(5) -0.0033(5) As1 0.0187(6) 0.0164(8) 0.0326(7) -0.0001(5) 0.0109(5) -0.0005(5) As2 0.0356(7) 0.0244(9) 0.0610(10) 0.0035(7) 0.0251(7) 0.0081(6) Cu1 0.0232(10) 0.0268(14) 0.0444(14) 0.000 0.0179(9) 0.000 Cu2 0.0339(9) 0.0306(11) 0.0532(11) -0.0070(8) 0.0171(8) 0.0012(8) Cu3 0.0376(13) 0.0305(16) 0.075(2) 0.000 0.0248(13) 0.000 Cu4 0.182(4) 0.066(2) 0.102(3) -0.0216(17) 0.069(3) -0.047(2) O1 0.048(6) 0.052(8) 0.061(7) 0.004(6) 0.035(6) -0.002(6) O2 0.028(5) 0.067(8) 0.050(7) -0.001(6) 0.000(4) 0.015(5) O3 0.026(4) 0.027(6) 0.071(8) -0.006(5) -0.001(5) -0.002(4) O4 0.067(7) 0.040(7) 0.051(7) 0.013(5) 0.030(6) 0.000(6) O5 0.053(6) 0.050(7) 0.037(6) -0.020(5) 0.011(5) 0.000(6) O6 0.051(6) 0.017(5) 0.065(7) 0.007(5) 0.015(5) 0.009(5) O7 0.048(6) 0.068(9) 0.040(6) 0.009(5) 0.022(5) -0.005(6) O8 0.080(8) 0.036(7) 0.062(8) -0.008(5) 0.041(7) -0.006(6) O9 0.048(3) 0.048(3) 0.048(3) 0.0003(10) 0.0114(11) -0.0001(10) O10 0.062(7) 0.058(8) 0.065(8) 0.011(6) 0.043(6) 0.000(6) O11 0.029(4) 0.036(6) 0.045(6) -0.009(4) 0.016(4) 0.003(4) O12 0.030(5) 0.043(7) 0.060(7) 0.004(5) 0.006(5) 0.013(5) O13 0.028(5) 0.072(9) 0.036(6) 0.002(5) 0.011(4) 0.004(5) O14 0.056(6) 0.032(6) 0.060(7) -0.015(5) 0.013(6) -0.024(6) O15 0.047(6) 0.022(6) 0.074(8) -0.009(5) 0.031(6) -0.011(5) O16 0.029(5) 0.033(6) 0.058(7) 0.011(5) 0.014(4) 0.004(5) O17 0.025(4) 0.022(5) 0.053(6) 0.005(4) 0.016(4) 0.006(4) O18 0.033(2) 0.033(2) 0.033(2) 0.0005(10) 0.0072(11) -0.0003(10) O19 0.025(4) 0.031(6) 0.047(6) 0.001(4) 0.008(4) 0.000(4) O20 0.032(5) 0.042(6) 0.038(6) 0.001(4) 0.014(4) 0.010(5) O21 0.042(5) 0.034(6) 0.034(5) -0.002(4) 0.015(4) -0.009(5) O22 0.045(5) 0.032(6) 0.042(6) -0.005(5) 0.013(5) -0.001(5) O23 0.029(4) 0.034(6) 0.049(6) 0.003(5) 0.012(4) 0.005(4) O24 0.030(4) 0.027(6) 0.049(6) 0.004(4) 0.022(4) 0.002(4) O25 0.041(5) 0.018(5) 0.068(7) -0.001(5) 0.028(5) -0.008(4) O26 0.031(5) 0.031(6) 0.039(5) 0.001(4) 0.011(4) 0.000(4) O27 0.036(5) 0.028(6) 0.050(6) 0.005(4) 0.020(4) -0.002(5) O28 0.027(4) 0.034(6) 0.053(6) 0.005(5) 0.018(4) 0.001(4) O29 0.031(5) 0.033(6) 0.058(7) 0.007(5) 0.021(5) 0.004(5) O30 0.039(5) 0.031(6) 0.041(6) -0.006(4) 0.010(4) 0.006(5) O31 0.014(3) 0.030(5) 0.032(5) 0.002(4) 0.012(3) 0.003(4) O32 0.026(4) 0.030(5) 0.030(5) -0.003(4) 0.010(4) 0.003(4) O33 0.018(4) 0.013(5) 0.041(5) 0.002(4) 0.008(3) -0.005(3) O34 0.022(4) 0.047(7) 0.030(5) -0.014(4) 0.006(4) 0.004(4) N1 0.031(6) 0.038(8) 0.045(7) 0.002(5) 0.020(5) 0.005(5) N2 0.014(5) 0.041(8) 0.059(8) 0.009(6) 0.014(5) 0.003(5) N3 0.029(6) 0.074(12) 0.059(9) -0.020(8) 0.014(6) 0.003(7) N4 0.047(7) 0.025(7) 0.062(9) 0.005(6) 0.021(6) 0.003(6) N5 0.039(6) 0.024(7) 0.054(8) 0.000(6) 0.004(6) 0.005(6) N6 0.054(7) 0.048(8) 0.063(9) -0.005(7) 0.011(6) -0.002(7) N7 0.044(6) 0.038(8) 0.105(11) 0.009(7) 0.046(7) -0.009(6) N8 0.056(8) 0.032(9) 0.101(13) -0.010(8) 0.023(9) 0.014(7) N10 0.050(8) 0.043(10) 0.106(13) -0.021(9) 0.040(8) -0.016(7) N11 0.048(8) 0.053(10) 0.098(14) 0.008(9) 0.003(8) 0.012(8) C1 0.040(8) 0.042(10) 0.057(10) 0.002(7) 0.025(7) 0.004(7) C2 0.051(10) 0.071(16) 0.086(15) -0.032(12) 0.024(10) 0.022(10) C3 0.13(2) 0.042(12) 0.076(14) -0.002(10) 0.060(14) 0.020(13) C4 0.098(16) 0.031(11) 0.12(2) 0.009(11) 0.068(15) 0.005(11) C5 0.071(11) 0.035(10) 0.058(10) -0.004(8) 0.024(9) 0.000(9) C6 0.25(4) 0.045(15) 0.20(3) -0.012(18) 0.17(3) 0.01(2) C7 0.048(8) 0.034(9) 0.040(8) 0.008(6) 0.021(7) -0.007(7) C8 0.047(10) 0.098(19) 0.084(16) 0.023(13) 0.031(10) -0.003(11) C9 0.053(9) 0.056(12) 0.066(12) 0.011(9) 0.017(9) -0.014(9) C10 0.071(13) 0.082(17) 0.074(14) 0.002(12) 0.034(11) 0.007(12) C11 0.079(9) 0.059(10) 0.071(10) -0.003(8) 0.008(8) -0.011(9) C12 0.059(8) 0.046(9) 0.128(12) -0.006(9) 0.050(9) -0.008(8) C13 0.047(11) 0.10(2) 0.21(4) -0.05(2) 0.061(16) 0.002(13) C16 0.069(12) 0.039(11) 0.087(15) 0.008(10) 0.023(11) 0.016(10) O1W 0.039(5) 0.048(7) 0.066(8) -0.015(6) 0.018(5) 0.000(6) O2W 0.058(7) 0.102(13) 0.064(9) 0.015(8) 0.009(7) -0.026(8) _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. ; _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 1.720(11) . ? Mo1 O28 1.740(10) . ? Mo1 O17 1.778(10) . ? Mo1 O24 2.047(10) . ? Mo1 O16 2.159(10) . ? Mo1 O31 2.405(8) . ? Mo1 As2 3.048(2) . ? Mo2 O2 1.719(10) . ? Mo2 O19 1.741(10) . ? Mo2 O18 1.825(10) . ? Mo2 O29 2.080(11) . ? Mo2 O16 2.145(11) . ? Mo2 O31 2.380(8) . ? Mo2 As2 3.053(2) . ? Mo3 O3 1.714(10) . ? Mo3 O23 1.756(10) . ? Mo3 O30 1.764(10) . ? Mo3 O18 2.125(10) . ? Mo3 O17 2.153(10) . ? Mo3 O31 2.358(9) . ? Mo4 O10 1.689(12) . ? Mo4 O4 1.701(11) . ? Mo4 O27 1.924(11) . ? Mo4 O21 1.936(10) . ? Mo4 O19 2.291(9) . ? Mo4 O32 2.309(9) . ? Mo5 O5 1.690(11) . ? Mo5 O11 1.709(9) . ? Mo5 O20 1.908(10) . ? Mo5 O21 1.963(10) . ? Mo5 O30 2.260(10) . ? Mo5 O32 2.311(10) . ? Mo6 O12 1.721(9) . ? Mo6 O6 1.737(11) . ? Mo6 O20 1.894(10) . ? Mo6 O26 1.932(10) . ? Mo6 O23 2.266(9) . ? Mo6 O33 2.291(9) . ? Mo7 O7 1.698(11) . ? Mo7 O13 1.731(9) . ? Mo7 O22 1.907(11) . ? Mo7 O26 1.966(11) . ? Mo7 O28 2.247(9) . ? Mo7 O33 2.324(9) . ? Mo8 O14 1.687(11) . ? Mo8 O8 1.689(12) . ? Mo8 O22 1.886(11) . ? Mo8 O25 1.966(11) . ? Mo8 O24 2.326(9) . ? Mo8 O34 2.352(9) . ? Mo9 O9 1.720(12) . ? Mo9 O15 1.727(11) . ? Mo9 O27 1.872(11) . ? Mo9 O25 1.975(11) . ? Mo9 O29 2.276(10) . ? Mo9 O34 2.307(11) . ? As1 O32 1.662(9) . ? As1 O34 1.672(11) . ? As1 O33 1.679(8) . ? As1 O31 1.715(8) . ? As2 O29 1.793(11) . ? As2 O24 1.795(10) . ? As2 O16 1.864(11) . ? Cu1 N2 2.009(12) 2_655 ? Cu1 N2 2.009(12) . ? Cu1 N1 2.017(12) 2_655 ? Cu1 N1 2.017(12) . ? Cu1 O13 2.394(10) 2_655 ? Cu1 O13 2.394(10) . ? Cu2 N6 1.999(16) . ? Cu2 N4 2.024(13) . ? Cu2 N5 2.028(14) . ? Cu2 N3 2.031(15) . ? Cu3 N8 1.990(14) 2_554 ? Cu3 N8 1.990(14) . ? Cu3 N7 2.014(13) . ? Cu3 N7 2.014(13) 2_554 ? Cu4 N12 1.84(3) . ? Cu4 N9 1.97(2) . ? Cu4 N10 1.990(17) . ? Cu4 N11 2.03(2) . ? N1 C1 1.33(2) . ? N1 C5 1.38(2) . ? N2 C7 1.43(2) . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? N3 C8 1.45(3) . ? N3 H3B 0.9000 . ? N3 H3C 0.9000 . ? N4 C9 1.47(2) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C10 1.41(3) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 C11 1.42(3) . ? N6 H6B 0.9000 . ? N6 H6C 0.9000 . ? N7 C12 1.35(2) . ? N7 H7C 0.9000 . ? N7 H7D 0.9000 . ? N8 C13 1.43(3) . ? N8 H8C 0.9000 . ? N8 H8D 0.9000 . ? N9 C14 1.494(10) . ? N9 H9C 0.9000 . ? N9 H9D 0.9000 . ? N10 C15 1.507(10) . ? N10 H10C 0.9000 . ? N10 H10D 0.9000 . ? N11 C16 1.40(3) . ? N11 H11C 0.9000 . ? N11 H11D 0.9000 . ? N12 C17 1.56(4) . ? N12 H12B 0.9000 . ? N12 H12C 0.9000 . ? C1 C2 1.38(2) . ? C1 H1A 0.9300 . ? C2 C3 1.40(3) . ? C2 H2A 0.9300 . ? C3 C4 1.39(3) . ? C3 H3A 0.9300 . ? C4 C5 1.39(3) . ? C4 C6 1.45(3) . ? C5 C5 1.43(4) 2_655 ? C6 C6 1.29(5) 2_655 ? C6 H6A 0.9300 . ? C7 C7 1.47(3) 2_655 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.48(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.47(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.48(3) . ? C12 H12A 0.9700 . ? C12 H12D 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.507(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.52(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? _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 O28 105.0(5) . . ? O1 Mo1 O17 103.4(5) . . ? O28 Mo1 O17 102.0(5) . . ? O1 Mo1 O24 100.9(5) . . ? O28 Mo1 O24 88.6(4) . . ? O17 Mo1 O24 149.8(4) . . ? O1 Mo1 O16 97.5(5) . . ? O28 Mo1 O16 152.4(4) . . ? O17 Mo1 O16 87.8(4) . . ? O24 Mo1 O16 71.4(4) . . ? O1 Mo1 O31 168.3(5) . . ? O28 Mo1 O31 86.5(4) . . ? O17 Mo1 O31 75.0(4) . . ? O24 Mo1 O31 77.5(4) . . ? O16 Mo1 O31 71.0(3) . . ? O1 Mo1 As2 96.8(4) . . ? O28 Mo1 As2 122.6(3) . . ? O17 Mo1 As2 123.7(3) . . ? O24 Mo1 As2 34.7(3) . . ? O16 Mo1 As2 37.3(3) . . ? O31 Mo1 As2 75.2(2) . . ? O2 Mo2 O19 105.8(5) . . ? O2 Mo2 O18 102.3(5) . . ? O19 Mo2 O18 103.0(5) . . ? O2 Mo2 O29 99.9(5) . . ? O19 Mo2 O29 88.7(4) . . ? O18 Mo2 O29 150.8(4) . . ? O2 Mo2 O16 95.0(5) . . ? O19 Mo2 O16 153.6(4) . . ? O18 Mo2 O16 87.9(4) . . ? O29 Mo2 O16 71.5(4) . . ? O2 Mo2 O31 166.5(4) . . ? O19 Mo2 O31 87.6(4) . . ? O18 Mo2 O31 75.5(4) . . ? O29 Mo2 O31 78.4(4) . . ? O16 Mo2 O31 71.7(3) . . ? O2 Mo2 As2 95.4(4) . . ? O19 Mo2 As2 122.8(3) . . ? O18 Mo2 As2 123.7(3) . . ? O29 Mo2 As2 34.8(3) . . ? O16 Mo2 As2 37.1(3) . . ? O31 Mo2 As2 75.5(2) . . ? O3 Mo3 O23 104.6(5) . . ? O3 Mo3 O30 105.2(5) . . ? O23 Mo3 O30 99.4(5) . . ? O3 Mo3 O18 95.8(4) . . ? O23 Mo3 O18 154.6(4) . . ? O30 Mo3 O18 89.4(4) . . ? O3 Mo3 O17 97.1(5) . . ? O23 Mo3 O17 87.2(4) . . ? O30 Mo3 O17 154.1(4) . . ? O18 Mo3 O17 75.3(4) . . ? O3 Mo3 O31 163.3(4) . . ? O23 Mo3 O31 85.9(4) . . ? O30 Mo3 O31 85.4(4) . . ? O18 Mo3 O31 71.1(3) . . ? O17 Mo3 O31 70.1(3) . . ? O10 Mo4 O4 103.8(6) . . ? O10 Mo4 O27 97.3(5) . . ? O4 Mo4 O27 102.4(5) . . ? O10 Mo4 O21 99.4(5) . . ? O4 Mo4 O21 97.5(5) . . ? O27 Mo4 O21 150.1(4) . . ? O10 Mo4 O19 167.8(5) . . ? O4 Mo4 O19 88.1(5) . . ? O27 Mo4 O19 76.9(4) . . ? O21 Mo4 O19 81.7(4) . . ? O10 Mo4 O32 88.8(5) . . ? O4 Mo4 O32 165.3(5) . . ? O27 Mo4 O32 83.2(4) . . ? O21 Mo4 O32 72.6(4) . . ? O19 Mo4 O32 79.9(3) . . ? O5 Mo5 O11 104.0(5) . . ? O5 Mo5 O20 101.7(5) . . ? O11 Mo5 O20 96.3(5) . . ? O5 Mo5 O21 98.9(5) . . ? O11 Mo5 O21 98.1(5) . . ? O20 Mo5 O21 151.2(4) . . ? O5 Mo5 O30 88.6(5) . . ? O11 Mo5 O30 167.0(4) . . ? O20 Mo5 O30 77.7(4) . . ? O21 Mo5 O30 82.8(4) . . ? O5 Mo5 O32 167.1(4) . . ? O11 Mo5 O32 86.8(4) . . ? O20 Mo5 O32 83.9(4) . . ? O21 Mo5 O32 72.1(4) . . ? O30 Mo5 O32 81.2(3) . . ? O12 Mo6 O6 100.7(5) . . ? O12 Mo6 O20 97.4(5) . . ? O6 Mo6 O20 102.0(5) . . ? O12 Mo6 O26 97.6(5) . . ? O6 Mo6 O26 98.5(5) . . ? O20 Mo6 O26 151.9(4) . . ? O12 Mo6 O23 170.8(5) . . ? O6 Mo6 O23 88.5(5) . . ? O20 Mo6 O23 80.0(4) . . ? O26 Mo6 O23 81.5(4) . . ? O12 Mo6 O33 89.9(4) . . ? O6 Mo6 O33 167.5(4) . . ? O20 Mo6 O33 82.9(4) . . ? O26 Mo6 O33 73.4(4) . . ? O23 Mo6 O33 81.1(3) . . ? O7 Mo7 O13 102.6(5) . . ? O7 Mo7 O22 102.3(6) . . ? O13 Mo7 O22 97.8(5) . . ? O7 Mo7 O26 97.5(5) . . ? O13 Mo7 O26 96.8(5) . . ? O22 Mo7 O26 152.2(4) . . ? O7 Mo7 O28 89.4(5) . . ? O13 Mo7 O28 167.9(4) . . ? O22 Mo7 O28 78.2(4) . . ? O26 Mo7 O28 82.7(4) . . ? O7 Mo7 O33 166.1(5) . . ? O13 Mo7 O33 88.0(4) . . ? O22 Mo7 O33 84.9(4) . . ? O26 Mo7 O33 72.1(4) . . ? O28 Mo7 O33 80.3(3) . . ? O14 Mo8 O8 103.9(6) . . ? O14 Mo8 O22 98.5(5) . . ? O8 Mo8 O22 102.8(5) . . ? O14 Mo8 O25 98.4(5) . . ? O8 Mo8 O25 97.0(6) . . ? O22 Mo8 O25 150.0(4) . . ? O14 Mo8 O24 162.3(5) . . ? O8 Mo8 O24 93.5(5) . . ? O22 Mo8 O24 81.0(4) . . ? O25 Mo8 O24 75.4(4) . . ? O14 Mo8 O34 85.5(5) . . ? O8 Mo8 O34 167.0(5) . . ? O22 Mo8 O34 84.4(4) . . ? O25 Mo8 O34 72.4(4) . . ? O24 Mo8 O34 76.8(3) . . ? O9 Mo9 O15 103.5(5) . . ? O9 Mo9 O27 101.7(5) . . ? O15 Mo9 O27 98.6(5) . . ? O9 Mo9 O25 97.5(5) . . ? O15 Mo9 O25 98.6(5) . . ? O27 Mo9 O25 150.4(4) . . ? O9 Mo9 O29 88.9(5) . . ? O15 Mo9 O29 167.2(5) . . ? O27 Mo9 O29 81.5(4) . . ? O25 Mo9 O29 76.6(4) . . ? O9 Mo9 O34 165.5(4) . . ? O15 Mo9 O34 89.1(4) . . ? O27 Mo9 O34 83.1(4) . . ? O25 Mo9 O34 73.3(4) . . ? O29 Mo9 O34 78.2(3) . . ? O32 As1 O34 107.5(5) . . ? O32 As1 O33 109.4(4) . . ? O34 As1 O33 109.6(4) . . ? O32 As1 O31 109.6(4) . . ? O34 As1 O31 112.3(4) . . ? O33 As1 O31 108.3(4) . . ? O29 As2 O24 101.7(4) . . ? O29 As2 O16 84.9(5) . . ? O24 As2 O16 84.3(4) . . ? O29 As2 Mo1 100.5(3) . . ? O24 As2 Mo1 40.5(3) . . ? O16 As2 Mo1 44.5(3) . . ? O29 As2 Mo2 41.4(3) . . ? O24 As2 Mo2 99.1(3) . . ? O16 As2 Mo2 43.9(3) . . ? Mo1 As2 Mo2 73.30(5) . . ? N2 Cu1 N2 85.1(7) 2_655 . ? N2 Cu1 N1 96.4(5) 2_655 2_655 ? N2 Cu1 N1 178.0(5) . 2_655 ? N2 Cu1 N1 178.0(5) 2_655 . ? N2 Cu1 N1 96.4(5) . . ? N1 Cu1 N1 82.1(7) 2_655 . ? N2 Cu1 O13 84.7(5) 2_655 2_655 ? N2 Cu1 O13 92.8(5) . 2_655 ? N1 Cu1 O13 88.6(5) 2_655 2_655 ? N1 Cu1 O13 93.9(5) . 2_655 ? N2 Cu1 O13 92.8(5) 2_655 . ? N2 Cu1 O13 84.7(5) . . ? N1 Cu1 O13 93.9(5) 2_655 . ? N1 Cu1 O13 88.6(5) . . ? O13 Cu1 O13 176.7(6) 2_655 . ? N6 Cu2 N4 177.0(6) . . ? N6 Cu2 N5 83.6(6) . . ? N4 Cu2 N5 94.2(6) . . ? N6 Cu2 N3 97.2(7) . . ? N4 Cu2 N3 85.3(6) . . ? N5 Cu2 N3 171.5(5) . . ? N8 Cu3 N8 97.7(10) 2_554 . ? N8 Cu3 N7 173.3(8) 2_554 . ? N8 Cu3 N7 84.3(7) . . ? N8 Cu3 N7 84.3(7) 2_554 2_554 ? N8 Cu3 N7 173.3(8) . 2_554 ? N7 Cu3 N7 94.5(9) . 2_554 ? N12 Cu4 N9 98.6(11) . . ? N12 Cu4 N10 172.1(11) . . ? N9 Cu4 N10 83.2(7) . . ? N12 Cu4 N11 80.9(11) . . ? N9 Cu4 N11 176.7(8) . . ? N10 Cu4 N11 96.9(7) . . ? Mo7 O13 Cu1 132.6(5) . . ? As2 O16 Mo2 99.0(4) . . ? As2 O16 Mo1 98.2(5) . . ? Mo2 O16 Mo1 115.6(5) . . ? Mo1 O17 Mo3 120.8(5) . . ? Mo2 O18 Mo3 119.0(5) . . ? Mo2 O19 Mo4 154.2(6) . . ? Mo6 O20 Mo5 166.2(6) . . ? Mo4 O21 Mo5 119.0(5) . . ? Mo8 O22 Mo7 164.6(6) . . ? Mo3 O23 Mo6 141.8(6) . . ? As2 O24 Mo1 104.8(5) . . ? As2 O24 Mo8 111.6(5) . . ? Mo1 O24 Mo8 141.3(5) . . ? Mo8 O25 Mo9 117.5(5) . . ? Mo6 O26 Mo7 118.7(5) . . ? Mo9 O27 Mo4 166.0(6) . . ? Mo1 O28 Mo7 155.4(6) . . ? As2 O29 Mo2 103.8(5) . . ? As2 O29 Mo9 112.0(5) . . ? Mo2 O29 Mo9 141.1(5) . . ? Mo3 O30 Mo5 144.6(5) . . ? As1 O31 Mo3 121.1(4) . . ? As1 O31 Mo2 122.4(4) . . ? Mo3 O31 Mo2 92.0(3) . . ? As1 O31 Mo1 122.6(4) . . ? Mo3 O31 Mo1 91.9(3) . . ? Mo2 O31 Mo1 99.1(3) . . ? As1 O32 Mo4 128.4(5) . . ? As1 O32 Mo5 126.3(5) . . ? Mo4 O32 Mo5 93.3(3) . . ? As1 O33 Mo6 127.9(5) . . ? As1 O33 Mo7 126.9(5) . . ? Mo6 O33 Mo7 93.2(3) . . ? As1 O34 Mo9 127.5(5) . . ? As1 O34 Mo8 126.2(5) . . ? Mo9 O34 Mo8 92.7(4) . . ? C1 N1 C5 118.1(14) . . ? C1 N1 Cu1 129.3(11) . . ? C5 N1 Cu1 112.5(10) . . ? C7 N2 Cu1 106.3(9) . . ? C7 N2 H2B 110.5 . . ? Cu1 N2 H2B 110.5 . . ? C7 N2 H2C 110.5 . . ? Cu1 N2 H2C 110.5 . . ? H2B N2 H2C 108.7 . . ? C8 N3 Cu2 106.7(12) . . ? C8 N3 H3B 110.4 . . ? Cu2 N3 H3B 110.4 . . ? C8 N3 H3C 110.4 . . ? Cu2 N3 H3C 110.4 . . ? H3B N3 H3C 108.6 . . ? C9 N4 Cu2 105.1(11) . . ? C9 N4 H4A 110.7 . . ? Cu2 N4 H4A 110.7 . . ? C9 N4 H4B 110.7 . . ? Cu2 N4 H4B 110.7 . . ? H4A N4 H4B 108.8 . . ? C10 N5 Cu2 111.2(12) . . ? C10 N5 H5A 109.4 . . ? Cu2 N5 H5A 109.4 . . ? C10 N5 H5B 109.4 . . ? Cu2 N5 H5B 109.4 . . ? H5A N5 H5B 108.0 . . ? C11 N6 Cu2 107.7(13) . . ? C11 N6 H6B 110.2 . . ? Cu2 N6 H6B 110.2 . . ? C11 N6 H6C 110.2 . . ? Cu2 N6 H6C 110.2 . . ? H6B N6 H6C 108.5 . . ? C12 N7 Cu3 113.5(13) . . ? C12 N7 H7C 108.9 . . ? Cu3 N7 H7C 108.9 . . ? C12 N7 H7D 108.9 . . ? Cu3 N7 H7D 108.9 . . ? H7C N7 H7D 107.7 . . ? C13 N8 Cu3 110.1(13) . . ? C13 N8 H8C 109.6 . . ? Cu3 N8 H8C 109.6 . . ? C13 N8 H8D 109.6 . . ? Cu3 N8 H8D 109.6 . . ? H8C N8 H8D 108.1 . . ? C14 N9 Cu4 113.1(14) . . ? C14 N9 H9C 109.0 . . ? Cu4 N9 H9C 109.0 . . ? C14 N9 H9D 109.0 . . ? Cu4 N9 H9D 109.0 . . ? H9C N9 H9D 107.8 . . ? C15 N10 Cu4 108.4(11) . . ? C15 N10 H10C 110.0 . . ? Cu4 N10 H10C 110.0 . . ? C15 N10 H10D 110.0 . . ? Cu4 N10 H10D 110.0 . . ? H10C N10 H10D 108.4 . . ? C16 N11 Cu4 114.6(14) . . ? C16 N11 H11C 108.6 . . ? Cu4 N11 H11C 108.6 . . ? C16 N11 H11D 108.6 . . ? Cu4 N11 H11D 108.6 . . ? H11C N11 H11D 107.6 . . ? C17 N12 Cu4 113(2) . . ? C17 N12 H12B 109.1 . . ? Cu4 N12 H12B 109.1 . . ? C17 N12 H12C 109.1 . . ? Cu4 N12 H12C 109.1 . . ? H12B N12 H12C 107.8 . . ? N1 C1 C2 125.0(18) . . ? N1 C1 H1A 117.5 . . ? C2 C1 H1A 117.5 . . ? C1 C2 C3 114.6(19) . . ? C1 C2 H2A 122.7 . . ? C3 C2 H2A 122.7 . . ? C4 C3 C2 124.1(19) . . ? C4 C3 H3A 117.9 . . ? C2 C3 H3A 117.9 . . ? C3 C4 C5 115.4(19) . . ? C3 C4 C6 129(2) . . ? C5 C4 C6 116(2) . . ? N1 C5 C4 122.4(17) . . ? N1 C5 C5 116.2(9) . 2_655 ? C4 C5 C5 120.9(12) . 2_655 ? C6 C6 C4 122.1(15) 2_655 . ? C6 C6 H6A 119.0 2_655 . ? C4 C6 H6A 119.0 . . ? N2 C7 C7 109.0(10) . 2_655 ? N2 C7 H7A 109.9 . . ? C7 C7 H7A 109.9 2_655 . ? N2 C7 H7B 109.9 . . ? C7 C7 H7B 109.9 2_655 . ? H7A C7 H7B 108.3 . . ? N3 C8 C9 108.9(15) . . ? N3 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? N3 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N4 C9 C8 108.0(17) . . ? N4 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? N4 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N5 C10 C11 112.3(19) . . ? N5 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N5 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? N6 C11 C10 113.1(18) . . ? N6 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? N6 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N7 C12 C13 114.1(17) . . ? N7 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? N7 C12 H12D 108.7 . . ? C13 C12 H12D 108.7 . . ? H12A C12 H12D 107.6 . . ? N8 C13 C12 116.4(18) . . ? N8 C13 H13A 108.2 . . ? C12 C13 H13A 108.2 . . ? N8 C13 H13B 108.2 . . ? C12 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? N9 C14 C15 111.3(15) . . ? N9 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N9 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N10 C15 C14 108.5(14) . . ? N10 C15 H15A 110.0 . . ? C14 C15 H15A 110.0 . . ? N10 C15 H15B 110.0 . . ? C14 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? N11 C16 C17 108(2) . . ? N11 C16 H16A 110.0 . . ? C17 C16 H16A 110.0 . . ? N11 C16 H16B 110.0 . . ? C17 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? C16 C17 N12 101(3) . . ? C16 C17 H17A 111.6 . . ? N12 C17 H17A 111.6 . . ? C16 C17 H17B 111.6 . . ? N12 C17 H17B 111.6 . . ? H17A C17 H17B 109.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.430 _refine_diff_density_min -3.824 _refine_diff_density_rms 0.438 data_1 _database_code_depnum_ccdc_archive 'CCDC 846088' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H44 As6 Cu2 Mo6 N6 O40' _chemical_formula_weight 1992.71 _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' As As 0.0499 2.0058 '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 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2610(7) _cell_length_b 10.5615(8) _cell_length_c 12.3519(9) _cell_angle_alpha 76.1540(10) _cell_angle_beta 75.5670(10) _cell_angle_gamma 81.4200(10) _cell_volume 1130.85(15) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2793 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.42 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 950 _exptl_absorpt_coefficient_mu 7.003 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3496 _exptl_absorpt_correction_T_max 0.4629 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5713 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3917 _reflns_number_gt 3345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+1.6176P] 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 3917 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 0.59036(5) 0.50989(5) -0.28492(4) 0.01644(13) Uani 1 1 d . . . Mo2 Mo 0.57110(5) 0.22221(4) -0.09551(4) 0.01565(13) Uani 1 1 d . . . Mo3 Mo 0.47606(5) 0.21026(4) 0.18778(4) 0.01546(13) Uani 1 1 d . . . As1 As 0.86491(6) 0.40696(6) -0.12070(5) 0.01999(15) Uani 1 1 d . . . As2 As 0.21840(6) 0.60900(6) -0.15500(5) 0.01919(15) Uani 1 1 d . . . As3 As 0.20817(6) 0.32679(6) 0.02376(5) 0.01982(15) Uani 1 1 d . . . Cu1 Cu 0.5000 0.5000 0.0000 0.0133(2) Uani 1 2 d S . . Cu2 Cu 0.5000 0.0000 0.5000 0.0293(3) Uani 1 2 d S . . O1 O 0.4851(5) 0.5713(4) -0.3853(3) 0.0310(10) Uani 1 1 d . . . O2 O 0.6572(4) 0.6668(4) -0.2675(3) 0.0197(8) Uani 1 1 d . . . O3 O 0.7612(5) 0.4525(4) -0.3584(3) 0.0308(10) Uani 1 1 d . . . O4 O 0.4980(4) 0.3518(4) -0.2147(3) 0.0183(8) Uani 1 1 d . . . O5 O 0.4112(4) 0.6009(3) -0.1514(3) 0.0177(8) Uani 1 1 d . . . O6 O 0.6665(4) 0.4172(3) -0.1122(3) 0.0172(8) Uani 1 1 d . . . O7 O 0.7381(4) 0.1602(4) -0.1682(3) 0.0273(9) Uani 1 1 d . . . O8 O 0.4432(5) 0.1171(4) -0.0822(3) 0.0268(9) Uani 1 1 d . . . O9 O 0.6194(4) 0.1759(3) 0.0548(3) 0.0166(8) Uani 1 1 d . . . O10 O 0.3999(4) 0.3392(3) 0.0243(3) 0.0153(8) Uani 1 1 d . . . O11 O 0.5786(5) 0.1289(4) 0.2863(3) 0.0296(10) Uani 1 1 d . . . O12 O 0.3396(4) 0.1122(4) 0.2004(3) 0.0266(9) Uani 1 1 d . . . O13 O 0.8670(4) 0.3357(4) 0.0256(3) 0.0215(9) Uani 1 1 d . . . O14 O 0.8805(4) 0.5736(4) -0.1232(3) 0.0224(9) Uani 1 1 d . . . O15 O 0.1937(4) 0.4396(4) -0.1071(3) 0.0225(9) Uani 1 1 d . . . N1 N 0.8414(5) -0.0078(5) 0.1285(4) 0.0289(12) Uani 1 1 d . . . H1C H 0.8331 0.0730 0.1333 0.035 Uiso 1 1 calc R . . H1D H 0.7828 -0.0610 0.1771 0.035 Uiso 1 1 calc R . . N2 N 0.2794(6) 0.0344(6) 0.5008(5) 0.0369(13) Uani 1 1 d . . . H2A H 0.2286 0.0617 0.5646 0.044 Uiso 1 1 calc R . . H2B H 0.2644 0.0968 0.4397 0.044 Uiso 1 1 calc R . . N3 N 0.4887(6) -0.1651(5) 0.4534(4) 0.0361(13) Uani 1 1 d . . . H3C H 0.5658 -0.1770 0.3947 0.043 Uiso 1 1 calc R . . H3D H 0.4936 -0.2338 0.5122 0.043 Uiso 1 1 calc R . . O1W O -0.0539(5) 0.7370(5) -0.3679(4) 0.0540(14) Uani 1 1 d . . . O2W O 0.0224(6) 0.0525(6) 0.2593(5) 0.0622(16) Uani 1 1 d . . . O3W O 0.2616(5) 0.2421(5) -0.2701(4) 0.0409(12) Uani 1 1 d . . . O4W O 0.1806(8) 0.5302(7) -0.3967(6) 0.090(2) Uiso 1 1 d . . . O5W O 0.0328(10) 0.2667(9) -0.3955(7) 0.124(3) Uiso 1 1 d . . . C1 C 0.9552(7) -0.0545(6) 0.0376(6) 0.0342(16) Uani 1 1 d . . . H1A H 0.9070 -0.0900 -0.0085 0.041 Uiso 1 1 calc R . . H1B H 1.0217 -0.1242 0.0712 0.041 Uiso 1 1 calc R . . C3 C 0.3452(10) -0.1548(8) 0.4188(7) 0.055(2) Uani 1 1 d . . . H3A H 0.3542 -0.1050 0.3409 0.066 Uiso 1 1 calc R . . H3B H 0.3194 -0.2415 0.4219 0.066 Uiso 1 1 calc R . . C4 C 0.2274(8) -0.0890(9) 0.4967(7) 0.055(2) Uani 1 1 d . . . H4A H 0.1354 -0.0713 0.4694 0.066 Uiso 1 1 calc R . . H4B H 0.2079 -0.1447 0.5726 0.066 Uiso 1 1 calc R . . _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 0.0198(3) 0.0145(3) 0.0141(3) -0.00188(19) -0.00224(19) -0.00293(19) Mo2 0.0185(3) 0.0116(3) 0.0174(3) -0.00308(19) -0.00489(19) -0.00142(18) Mo3 0.0167(2) 0.0116(3) 0.0160(3) 0.00043(19) -0.00198(19) -0.00282(18) As1 0.0155(3) 0.0211(3) 0.0237(3) -0.0065(2) -0.0037(2) -0.0008(2) As2 0.0155(3) 0.0205(3) 0.0210(3) -0.0016(2) -0.0054(2) -0.0022(2) As3 0.0153(3) 0.0167(3) 0.0281(3) -0.0039(2) -0.0056(2) -0.0039(2) Cu1 0.0141(5) 0.0098(5) 0.0157(5) -0.0018(4) -0.0023(4) -0.0028(3) Cu2 0.0320(6) 0.0244(6) 0.0321(6) -0.0069(5) -0.0082(5) -0.0012(5) O1 0.042(3) 0.024(2) 0.029(2) 0.0026(18) -0.018(2) -0.0078(19) O2 0.0182(19) 0.016(2) 0.022(2) -0.0033(16) 0.0020(16) -0.0051(15) O3 0.027(2) 0.032(3) 0.029(2) -0.0122(19) 0.0071(18) -0.0022(19) O4 0.020(2) 0.019(2) 0.0174(19) -0.0021(16) -0.0066(16) -0.0022(16) O5 0.0142(18) 0.015(2) 0.023(2) -0.0037(16) -0.0025(15) -0.0031(15) O6 0.0146(19) 0.015(2) 0.023(2) -0.0033(16) -0.0061(16) -0.0019(15) O7 0.027(2) 0.027(2) 0.028(2) -0.0095(18) -0.0059(18) 0.0033(18) O8 0.036(2) 0.016(2) 0.032(2) -0.0027(17) -0.0118(19) -0.0072(17) O9 0.0176(19) 0.012(2) 0.019(2) -0.0029(15) -0.0045(15) 0.0013(15) O10 0.0128(18) 0.0131(19) 0.0192(19) -0.0019(15) -0.0026(15) -0.0025(14) O11 0.037(2) 0.025(2) 0.023(2) 0.0007(18) -0.0092(19) 0.0019(19) O12 0.023(2) 0.017(2) 0.038(2) -0.0066(18) 0.0009(18) -0.0080(17) O13 0.017(2) 0.021(2) 0.025(2) -0.0050(17) -0.0041(16) 0.0010(16) O14 0.017(2) 0.024(2) 0.026(2) -0.0044(17) -0.0012(16) -0.0065(16) O15 0.020(2) 0.020(2) 0.032(2) -0.0066(17) -0.0113(17) -0.0039(16) N1 0.020(3) 0.025(3) 0.037(3) -0.010(2) 0.003(2) 0.000(2) N2 0.035(3) 0.041(4) 0.034(3) -0.008(3) -0.005(2) -0.001(3) N3 0.050(4) 0.029(3) 0.026(3) -0.004(2) -0.003(3) -0.004(3) O1W 0.038(3) 0.066(4) 0.049(3) 0.006(3) -0.001(2) -0.024(3) O2W 0.040(3) 0.100(5) 0.055(3) -0.031(3) -0.013(3) -0.007(3) O3W 0.046(3) 0.038(3) 0.036(3) -0.004(2) -0.008(2) -0.005(2) C1 0.031(4) 0.028(4) 0.040(4) -0.011(3) 0.002(3) -0.004(3) C3 0.074(6) 0.043(5) 0.061(5) -0.007(4) -0.033(5) -0.023(4) C4 0.034(4) 0.075(6) 0.058(5) -0.014(4) -0.007(4) -0.017(4) _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. ; _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 1.714(4) . ? Mo1 O3 1.719(4) . ? Mo1 O4 1.907(4) . ? Mo1 O2 1.929(4) . ? Mo1 O5 2.306(3) . ? Mo1 O6 2.357(4) . ? Mo2 O8 1.694(4) . ? Mo2 O7 1.707(4) . ? Mo2 O4 1.937(3) . ? Mo2 O9 1.949(3) . ? Mo2 O6 2.305(4) . ? Mo2 O10 2.313(3) . ? Mo3 O12 1.705(4) . ? Mo3 O11 1.719(4) . ? Mo3 O9 1.910(3) . ? Mo3 O2 1.925(4) 2_665 ? Mo3 O5 2.286(4) 2_665 ? Mo3 O10 2.353(3) . ? As1 O14 1.780(4) . ? As1 O13 1.787(4) . ? As1 O6 1.802(3) . ? As2 O15 1.775(4) . ? As2 O5 1.786(4) . ? As2 O13 1.789(4) 2_665 ? As3 O14 1.774(4) 2_665 ? As3 O15 1.785(4) . ? As3 O10 1.802(3) . ? Cu1 O10 1.980(4) . ? Cu1 O10 1.980(4) 2_665 ? Cu1 O6 2.043(3) . ? Cu1 O6 2.043(3) 2_665 ? Cu1 O5 2.204(4) . ? Cu1 O5 2.204(4) 2_665 ? Cu2 N3 1.986(5) . ? Cu2 N3 1.986(5) 2_656 ? Cu2 N2 2.019(5) 2_656 ? Cu2 N2 2.019(5) . ? O2 Mo3 1.925(4) 2_665 ? O5 Mo3 2.286(4) 2_665 ? O13 As2 1.789(4) 2_665 ? O14 As3 1.774(4) 2_665 ? N1 C1 1.461(7) . ? N1 H1C 0.8600 . ? N1 H1D 0.8600 . ? N2 C4 1.471(9) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C3 1.476(9) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? C1 C1 1.505(12) 2_755 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.473(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? _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 O3 105.7(2) . . ? O1 Mo1 O4 98.49(18) . . ? O3 Mo1 O4 101.83(18) . . ? O1 Mo1 O2 101.84(18) . . ? O3 Mo1 O2 95.76(18) . . ? O4 Mo1 O2 148.31(15) . . ? O1 Mo1 O5 90.31(17) . . ? O3 Mo1 O5 161.10(17) . . ? O4 Mo1 O5 85.23(14) . . ? O2 Mo1 O5 70.70(14) . . ? O1 Mo1 O6 163.49(17) . . ? O3 Mo1 O6 89.12(17) . . ? O4 Mo1 O6 70.84(13) . . ? O2 Mo1 O6 83.41(14) . . ? O5 Mo1 O6 76.54(12) . . ? O8 Mo2 O7 107.1(2) . . ? O8 Mo2 O4 94.17(17) . . ? O7 Mo2 O4 102.55(17) . . ? O8 Mo2 O9 102.41(17) . . ? O7 Mo2 O9 96.59(17) . . ? O4 Mo2 O9 149.71(15) . . ? O8 Mo2 O6 158.94(16) . . ? O7 Mo2 O6 91.38(17) . . ? O4 Mo2 O6 71.55(14) . . ? O9 Mo2 O6 84.86(14) . . ? O8 Mo2 O10 90.78(16) . . ? O7 Mo2 O10 160.46(16) . . ? O4 Mo2 O10 83.35(14) . . ? O9 Mo2 O10 71.39(13) . . ? O6 Mo2 O10 72.63(12) . . ? O12 Mo3 O11 105.5(2) . . ? O12 Mo3 O9 102.97(17) . . ? O11 Mo3 O9 97.05(17) . . ? O12 Mo3 O2 94.16(17) . 2_665 ? O11 Mo3 O2 102.46(17) . 2_665 ? O9 Mo3 O2 149.51(15) . 2_665 ? O12 Mo3 O5 158.34(16) . 2_665 ? O11 Mo3 O5 93.46(17) . 2_665 ? O9 Mo3 O5 84.53(14) . 2_665 ? O2 Mo3 O5 71.22(14) 2_665 2_665 ? O12 Mo3 O10 87.48(16) . . ? O11 Mo3 O10 164.36(17) . . ? O9 Mo3 O10 71.10(13) . . ? O2 Mo3 O10 84.86(14) 2_665 . ? O5 Mo3 O10 75.64(13) 2_665 . ? O14 As1 O13 100.09(17) . . ? O14 As1 O6 98.91(17) . . ? O13 As1 O6 99.27(17) . . ? O15 As2 O5 98.59(17) . . ? O15 As2 O13 99.70(18) . 2_665 ? O5 As2 O13 99.88(17) . 2_665 ? O14 As3 O15 100.10(18) 2_665 . ? O14 As3 O10 98.40(17) 2_665 . ? O15 As3 O10 99.73(17) . . ? O10 Cu1 O10 180.00(9) . 2_665 ? O10 Cu1 O6 85.66(14) . . ? O10 Cu1 O6 94.34(14) 2_665 . ? O10 Cu1 O6 94.34(14) . 2_665 ? O10 Cu1 O6 85.66(14) 2_665 2_665 ? O6 Cu1 O6 180.0 . 2_665 ? O10 Cu1 O5 94.49(14) . . ? O10 Cu1 O5 85.51(14) 2_665 . ? O6 Cu1 O5 85.60(13) . . ? O6 Cu1 O5 94.40(13) 2_665 . ? O10 Cu1 O5 85.51(14) . 2_665 ? O10 Cu1 O5 94.49(14) 2_665 2_665 ? O6 Cu1 O5 94.40(13) . 2_665 ? O6 Cu1 O5 85.60(13) 2_665 2_665 ? O5 Cu1 O5 180.00(11) . 2_665 ? N3 Cu2 N3 180.000(1) . 2_656 ? N3 Cu2 N2 94.9(2) . 2_656 ? N3 Cu2 N2 85.1(2) 2_656 2_656 ? N3 Cu2 N2 85.1(2) . . ? N3 Cu2 N2 94.9(2) 2_656 . ? N2 Cu2 N2 180.0 2_656 . ? Mo3 O2 Mo1 121.80(18) 2_665 . ? Mo1 O4 Mo2 121.87(18) . . ? As2 O5 Cu1 122.93(18) . . ? As2 O5 Mo3 119.87(18) . 2_665 ? Cu1 O5 Mo3 97.16(14) . 2_665 ? As2 O5 Mo1 119.07(17) . . ? Cu1 O5 Mo1 97.37(13) . . ? Mo3 O5 Mo1 94.34(13) 2_665 . ? As1 O6 Cu1 126.54(19) . . ? As1 O6 Mo2 115.81(17) . . ? Cu1 O6 Mo2 100.01(14) . . ? As1 O6 Mo1 115.45(17) . . ? Cu1 O6 Mo1 100.47(14) . . ? Mo2 O6 Mo1 92.22(12) . . ? Mo3 O9 Mo2 121.37(18) . . ? As3 O10 Cu1 128.01(19) . . ? As3 O10 Mo2 113.25(17) . . ? Cu1 O10 Mo2 101.69(14) . . ? As3 O10 Mo3 113.57(16) . . ? Cu1 O10 Mo3 101.68(14) . . ? Mo2 O10 Mo3 92.28(12) . . ? As1 O13 As2 132.0(2) . 2_665 ? As3 O14 As1 130.8(2) 2_665 . ? As2 O15 As3 132.2(2) . . ? C1 N1 H1C 120.0 . . ? C1 N1 H1D 120.0 . . ? H1C N1 H1D 120.0 . . ? C4 N2 Cu2 107.6(4) . . ? C4 N2 H2A 110.2 . . ? Cu2 N2 H2A 110.2 . . ? C4 N2 H2B 110.2 . . ? Cu2 N2 H2B 110.2 . . ? H2A N2 H2B 108.5 . . ? C3 N3 Cu2 108.0(4) . . ? C3 N3 H3C 110.1 . . ? Cu2 N3 H3C 110.1 . . ? C3 N3 H3D 110.1 . . ? Cu2 N3 H3D 110.1 . . ? H3C N3 H3D 108.4 . . ? N1 C1 C1 111.1(6) . 2_755 ? N1 C1 H1A 109.4 . . ? C1 C1 H1A 109.4 2_755 . ? N1 C1 H1B 109.4 . . ? C1 C1 H1B 109.4 2_755 . ? H1A C1 H1B 108.0 . . ? C4 C3 N3 109.0(6) . . ? C4 C3 H3A 109.9 . . ? N3 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? N3 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N2 C4 C3 108.2(6) . . ? N2 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N2 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.242 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.151