# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Key Lab for Polyoxometalate Science, Department of Chemistry, Northeast Normal University, Changchun 130024, People's Republic of China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_phone +86-431-85098620 _publ_contact_author_fax +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #=========================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 789618' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H50 Cu2 Mo8 N18 O30' _chemical_formula_sum 'C36 H50 Cu2 Mo8 N18 O30' _chemical_formula_weight 2109.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9897(10) _cell_length_b 11.2381(9) _cell_length_c 12.9222(15) _cell_angle_alpha 102.700(8) _cell_angle_beta 105.272(9) _cell_angle_gamma 91.721(7) _cell_volume 1495.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5843 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1026 _exptl_absorpt_coefficient_mu 2.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10117 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.1758 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 26.02 _reflns_number_total 5843 _reflns_number_gt 2632 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0252P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5843 _refine_ls_number_parameters 442 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1056 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 0.710 _refine_ls_restrained_S_all 0.710 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2271(7) 0.0898(6) -0.1467(6) 0.0204(19) Uani 1 1 d . . . H1 H -0.2026 0.0687 -0.2115 0.024 Uiso 1 1 calc R . . C2 C -0.2347(8) 0.1181(8) 0.0131(7) 0.048(3) Uani 1 1 d U . . H2 H -0.2125 0.1195 0.0880 0.057 Uiso 1 1 calc R . . C3 C -0.4337(6) 0.1728(7) -0.2247(6) 0.028(2) Uani 1 1 d . . . H3A H -0.5117 0.1257 -0.2309 0.033 Uiso 1 1 calc R . . H3B H -0.4152 0.1508 -0.2955 0.033 Uiso 1 1 calc R . . C4 C -0.2519(7) 0.3536(7) -0.2475(7) 0.035(2) Uani 1 1 d . . . H4A H -0.2455 0.2681 -0.2499 0.052 Uiso 1 1 calc R . . H4B H -0.1803 0.4008 -0.1925 0.052 Uiso 1 1 calc R . . H4C H -0.2536 0.3682 -0.3183 0.052 Uiso 1 1 calc R . . C5 C -0.6455(7) 0.2561(7) -0.1388(7) 0.036(2) Uani 1 1 d . . . H5A H -0.7238 0.2910 -0.1368 0.053 Uiso 1 1 calc R . . H5B H -0.6075 0.2368 -0.0693 0.053 Uiso 1 1 calc R . . H5C H -0.6618 0.1827 -0.1968 0.053 Uiso 1 1 calc R . . C6 C -0.5293(7) 0.6821(7) -0.1659(6) 0.036(2) Uani 1 1 d . . . H6A H -0.5838 0.6886 -0.2355 0.054 Uiso 1 1 calc R . . H6B H -0.4518 0.7333 -0.1493 0.054 Uiso 1 1 calc R . . H6C H -0.5706 0.7079 -0.1090 0.054 Uiso 1 1 calc R . . C7 C -0.4532(6) 0.3091(6) -0.1992(5) 0.0181(18) Uani 1 1 d . . . C8 C -0.3725(6) 0.3909(7) -0.2190(5) 0.0190(18) Uani 1 1 d . . . C9 C -0.3977(6) 0.5129(7) -0.2092(5) 0.0247(19) Uani 1 1 d . . . C10 C -0.5006(6) 0.5530(7) -0.1720(6) 0.0203(19) Uani 1 1 d . . . C11 C -0.5778(6) 0.4711(7) -0.1434(5) 0.0220(19) Uani 1 1 d . . . C12 C -0.5566(6) 0.3470(7) -0.1601(5) 0.0214(18) Uani 1 1 d . . . C13 C -0.3178(7) 0.5992(7) -0.2449(6) 0.027(2) Uani 1 1 d . . . H13A H -0.2737 0.5521 -0.2937 0.032 Uiso 1 1 calc R . . H13B H -0.3723 0.6496 -0.2856 0.032 Uiso 1 1 calc R . . C14 C -0.1853(7) 0.7926(7) -0.1367(6) 0.0268(19) Uani 1 1 d . . . H14 H -0.2169 0.8384 -0.1880 0.032 Uiso 1 1 calc R . . C15 C -0.0860(7) 0.7364(8) 0.0010(6) 0.033(2) Uani 1 1 d . . . H15 H -0.0310 0.7379 0.0698 0.040 Uiso 1 1 calc R . . C16 C -0.6816(6) 0.5187(8) -0.0946(5) 0.027(2) Uani 1 1 d . . . H16A H -0.7020 0.4649 -0.0510 0.033 Uiso 1 1 calc R . . H16B H -0.6539 0.5996 -0.0466 0.033 Uiso 1 1 calc R . . C17 C -0.8074(7) 0.5026(7) -0.2904(6) 0.029(2) Uani 1 1 d . . . H17 H -0.7444 0.4780 -0.3243 0.035 Uiso 1 1 calc R . . C18 C -0.9750(8) 0.5496(9) -0.2597(8) 0.053(3) Uani 1 1 d . . . H18 H -1.0598 0.5644 -0.2712 0.063 Uiso 1 1 calc R . . N1 N -0.9240(6) 0.5204(6) -0.3424(5) 0.0326(17) Uani 1 1 d . . . N2 N -0.9013(7) 0.5567(7) -0.1614(6) 0.051(2) Uani 1 1 d . . . N3 N -0.7943(5) 0.5246(5) -0.1845(5) 0.0244(16) Uani 1 1 d . . . N4 N -0.3295(5) 0.1391(5) -0.1397(5) 0.0218(15) Uani 1 1 d . . . N5 N -0.3389(6) 0.1601(7) -0.0344(5) 0.044(2) Uani 1 1 d . . . N6 N -0.1612(6) 0.0728(5) -0.0511(5) 0.0260(16) Uani 1 1 d . . . N7 N -0.2241(5) 0.6791(6) -0.1484(5) 0.0275(16) Uani 1 1 d . . . N8 N -0.0956(5) 0.8357(5) -0.0434(5) 0.0235(16) Uani 1 1 d . . . N9 N -0.1595(6) 0.6381(6) -0.0596(5) 0.0351(18) Uani 1 1 d . . . O1 O -0.2903(5) -0.1547(5) -0.3675(4) 0.0428(16) Uani 1 1 d . . . O2 O -0.1360(4) -0.2443(4) -0.6117(4) 0.0266(13) Uani 1 1 d . . . O3 O -0.0786(5) -0.2593(5) -0.4031(4) 0.0317(15) Uani 1 1 d . . . O4 O -0.0866(4) -0.0407(5) -0.4505(4) 0.0257(14) Uani 1 1 d . . . O5 O 0.0014(5) -0.0619(5) -0.2117(4) 0.0349(15) Uani 1 1 d . . . O6 O -0.0232(5) 0.1863(5) -0.2769(4) 0.0373(16) Uani 1 1 d . . . O7 O 0.1464(4) 0.0223(4) -0.3353(4) 0.0249(13) Uani 1 1 d . . . O8 O 0.1724(5) -0.2047(5) -0.2774(4) 0.0332(15) Uani 1 1 d . . . O9 O 0.1110(4) -0.1684(4) -0.4924(4) 0.0214(13) Uani 1 1 d . . . O10 O 0.3237(4) 0.1198(5) -0.4236(4) 0.0274(14) Uani 1 1 d . . . O11 O 0.3051(5) -0.0995(5) -0.5752(4) 0.0435(17) Uani 1 1 d . . . O12 O 0.3687(5) -0.1013(5) -0.3597(4) 0.0412(16) Uani 1 1 d . . . O13 O -0.3256(5) -0.3576(5) -0.5326(4) 0.0453(17) Uani 1 1 d . . . Cu1 Cu -1.0000 0.5000 -0.5000 0.0425(4) Uani 1 2 d S . . Cu2 Cu 0.0000 0.0000 0.0000 0.0289(4) Uani 1 2 d S . . Mo1 Mo 0.04976(6) -0.12764(7) -0.32669(6) 0.0256(2) Uani 1 1 d . . . Mo2 Mo 0.02477(6) 0.13194(6) -0.38878(5) 0.02218(19) Uani 1 1 d . . . Mo3 Mo -0.24104(7) -0.21755(7) -0.48025(6) 0.0297(2) Uani 1 1 d . . . Mo4 Mo 0.26347(6) -0.04638(7) -0.45623(6) 0.0273(2) Uani 1 1 d . . . O1W O -0.8466(6) 0.5865(6) -0.5181(5) 0.0567(19) Uani 1 1 d D . . O2W O 0.4198(8) -0.3625(8) -0.4604(9) 0.093(3) Uani 1 1 d D . . H1A H -0.773(6) 0.574(9) -0.479(9) 0.140 Uiso 1 1 d D . . H1B H -0.845(10) 0.665(3) -0.495(10) 0.140 Uiso 1 1 d D . . H2A H 0.469(11) -0.398(12) -0.497(10) 0.140 Uiso 1 1 d D . . H2B H 0.430(14) -0.285(2) -0.448(12) 0.140 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(4) 0.019(5) 0.023(4) 0.011(4) 0.010(4) 0.000(3) C2 0.046(5) 0.059(6) 0.025(4) 0.013(4) -0.016(4) 0.017(4) C3 0.019(4) 0.038(5) 0.020(4) 0.005(4) -0.004(3) 0.000(4) C4 0.027(5) 0.032(5) 0.044(5) 0.009(4) 0.007(4) -0.005(4) C5 0.040(5) 0.033(5) 0.039(5) 0.012(4) 0.016(4) 0.010(4) C6 0.034(5) 0.043(6) 0.028(5) 0.002(4) 0.006(4) 0.010(4) C7 0.016(4) 0.014(4) 0.017(4) 0.001(3) -0.006(3) 0.008(3) C8 0.017(4) 0.023(5) 0.015(4) 0.000(3) 0.003(3) 0.008(3) C9 0.020(4) 0.040(5) 0.011(4) 0.013(4) -0.005(3) -0.006(4) C10 0.017(4) 0.020(4) 0.017(4) -0.001(3) -0.002(3) 0.009(3) C11 0.024(4) 0.029(5) 0.010(4) 0.000(3) 0.002(3) 0.007(4) C12 0.018(4) 0.035(5) 0.007(4) 0.004(3) -0.003(3) 0.004(4) C13 0.027(4) 0.030(5) 0.016(4) -0.003(4) 0.000(3) 0.007(4) C14 0.033(5) 0.023(5) 0.026(5) 0.014(4) 0.004(4) 0.007(4) C15 0.042(5) 0.039(5) 0.016(4) 0.010(4) 0.000(4) 0.002(4) C16 0.027(4) 0.045(5) 0.011(4) 0.004(4) 0.008(3) 0.013(4) C17 0.023(4) 0.038(5) 0.025(5) 0.008(4) 0.002(4) -0.004(4) C18 0.024(5) 0.074(8) 0.072(7) 0.035(6) 0.016(5) 0.030(5) N1 0.029(4) 0.025(4) 0.040(4) 0.008(3) 0.002(3) 0.009(3) N2 0.039(4) 0.084(6) 0.040(5) 0.025(4) 0.014(4) 0.028(4) N3 0.026(4) 0.025(4) 0.032(4) 0.010(3) 0.019(3) 0.018(3) N4 0.020(3) 0.022(4) 0.022(4) 0.005(3) 0.002(3) 0.013(3) N5 0.049(5) 0.072(6) 0.016(4) 0.010(4) 0.011(3) 0.039(4) N6 0.025(4) 0.022(4) 0.023(4) 0.000(3) -0.001(3) 0.002(3) N7 0.027(4) 0.028(4) 0.023(4) 0.010(3) -0.003(3) 0.001(3) N8 0.026(4) 0.022(4) 0.028(4) 0.014(3) 0.009(3) 0.010(3) N9 0.045(4) 0.022(4) 0.032(4) 0.016(3) -0.006(3) 0.000(3) O1 0.059(4) 0.052(4) 0.020(3) 0.012(3) 0.012(3) 0.011(3) O2 0.032(3) 0.020(3) 0.028(3) 0.007(2) 0.007(2) 0.005(2) O3 0.032(3) 0.029(3) 0.029(3) 0.010(3) -0.002(3) -0.007(3) O4 0.025(3) 0.025(3) 0.017(3) 0.001(2) -0.006(2) -0.010(2) O5 0.042(3) 0.046(4) 0.024(3) 0.019(3) 0.014(3) 0.009(3) O6 0.045(4) 0.040(4) 0.023(3) -0.001(3) 0.010(3) 0.012(3) O7 0.027(3) 0.033(3) 0.014(3) 0.014(2) -0.002(2) 0.000(2) O8 0.040(3) 0.033(3) 0.024(3) 0.005(3) 0.006(3) 0.005(3) O9 0.022(3) 0.021(3) 0.022(3) 0.005(2) 0.008(2) 0.008(2) O10 0.031(3) 0.039(4) 0.013(3) 0.003(2) 0.010(2) 0.008(3) O11 0.047(4) 0.043(4) 0.044(4) -0.001(3) 0.029(3) -0.001(3) O12 0.036(3) 0.038(4) 0.044(3) 0.020(3) -0.006(3) 0.005(3) O13 0.047(4) 0.043(4) 0.038(3) 0.014(3) -0.004(3) -0.008(3) Cu1 0.0314(8) 0.0483(10) 0.0403(9) 0.0211(8) -0.0109(7) -0.0045(7) Cu2 0.0189(7) 0.0221(8) 0.0393(8) 0.0109(6) -0.0057(6) 0.0023(6) Mo1 0.0288(4) 0.0288(5) 0.0192(4) 0.0113(3) 0.0021(3) 0.0021(3) Mo2 0.0263(4) 0.0225(4) 0.0163(4) 0.0040(3) 0.0038(3) 0.0041(3) Mo3 0.0323(4) 0.0330(5) 0.0230(4) 0.0111(4) 0.0032(3) -0.0007(4) Mo4 0.0272(4) 0.0283(4) 0.0244(4) 0.0051(3) 0.0046(3) 0.0028(3) O1W 0.054(4) 0.055(4) 0.057(4) 0.018(4) 0.005(3) 0.002(3) O2W 0.059(5) 0.098(7) 0.114(7) 0.030(7) 0.005(5) 0.007(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N4 1.285(8) . ? C1 N6 1.315(9) . ? C2 N5 1.304(9) . ? C2 N6 1.338(10) . ? C3 N4 1.486(8) . ? C3 C7 1.528(9) . ? C4 C8 1.513(10) . ? C5 C12 1.510(11) . ? C6 C10 1.483(10) . ? C7 C8 1.369(10) . ? C7 C12 1.401(9) . ? C8 C9 1.392(10) . ? C9 C10 1.392(10) . ? C9 C13 1.511(11) . ? C10 C11 1.404(11) . ? C11 C12 1.400(10) . ? C11 C16 1.500(9) . ? C13 N7 1.482(8) . ? C14 N7 1.296(9) . ? C14 N8 1.323(8) . ? C15 N9 1.311(9) . ? C15 N8 1.358(9) . ? C16 N3 1.473(8) . ? C17 N3 1.304(9) . ? C17 N1 1.324(8) . ? C18 N2 1.299(10) . ? C18 N1 1.318(11) . ? N1 Cu1 1.945(6) . ? N2 N3 1.329(8) . ? N4 N5 1.362(8) . ? N6 Cu2 1.988(6) . ? N7 N9 1.362(8) . ? N8 Cu2 1.986(6) 1_565 ? O1 Mo3 1.703(6) . ? O2 Mo2 1.729(5) 2_554 ? O2 Mo3 2.266(5) . ? O3 Mo1 1.911(5) . ? O3 Mo3 1.929(5) . ? O4 Mo2 2.136(5) . ? O4 Mo1 2.296(5) . ? O4 Mo4 2.364(5) 2_554 ? O4 Mo2 2.382(5) 2_554 ? O4 Mo3 2.469(5) . ? O5 Mo1 1.731(5) . ? O6 Mo2 1.666(5) . ? O7 Mo2 1.942(5) . ? O7 Mo1 2.004(5) . ? O7 Mo4 2.299(5) . ? O8 Mo1 1.683(5) . ? O9 Mo2 1.964(4) 2_554 ? O9 Mo4 2.018(5) . ? O9 Mo1 2.366(5) . ? O10 Mo4 1.880(5) . ? O10 Mo3 1.908(5) 2_554 ? O11 Mo4 1.706(5) . ? O12 Mo4 1.701(5) . ? O13 Mo3 1.706(5) . ? Cu1 N1 1.945(6) 2_364 ? Cu1 O1W 2.013(7) . ? Cu1 O1W 2.013(7) 2_364 ? Cu2 N8 1.986(6) 2_565 ? Cu2 N8 1.986(6) 1_545 ? Cu2 N6 1.988(6) 2 ? Mo1 Mo2 3.1922(12) . ? Mo2 O2 1.729(5) 2_554 ? Mo2 O9 1.964(4) 2_554 ? Mo2 O4 2.382(5) 2_554 ? Mo3 O10 1.908(5) 2_554 ? Mo4 O4 2.364(5) 2_554 ? 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 N4 C1 N6 111.7(7) . . ? N5 C2 N6 116.8(7) . . ? N4 C3 C7 113.3(5) . . ? C8 C7 C12 121.4(7) . . ? C8 C7 C3 119.4(6) . . ? C12 C7 C3 119.2(7) . . ? C7 C8 C9 120.2(7) . . ? C7 C8 C4 121.6(7) . . ? C9 C8 C4 118.2(7) . . ? C8 C9 C10 119.6(7) . . ? C8 C9 C13 119.9(7) . . ? C10 C9 C13 120.3(7) . . ? C9 C10 C11 120.1(7) . . ? C9 C10 C6 119.1(7) . . ? C11 C10 C6 120.8(7) . . ? C12 C11 C10 119.8(7) . . ? C12 C11 C16 121.1(7) . . ? C10 C11 C16 119.1(7) . . ? C11 C12 C7 118.6(7) . . ? C11 C12 C5 120.3(7) . . ? C7 C12 C5 121.0(7) . . ? N7 C13 C9 111.1(6) . . ? N7 C14 N8 112.2(7) . . ? N9 C15 N8 115.5(6) . . ? N3 C16 C11 109.1(5) . . ? N3 C17 N1 109.7(8) . . ? N2 C18 N1 116.9(7) . . ? C18 N1 C17 101.4(7) . . ? C18 N1 Cu1 129.9(5) . . ? C17 N1 Cu1 128.7(6) . . ? C18 N2 N3 100.9(7) . . ? C17 N3 N2 111.1(6) . . ? C17 N3 C16 129.0(6) . . ? N2 N3 C16 119.9(6) . . ? C1 N4 N5 110.6(6) . . ? C1 N4 C3 131.3(7) . . ? N5 N4 C3 118.2(6) . . ? C2 N5 N4 100.1(7) . . ? C1 N6 C2 100.8(6) . . ? C1 N6 Cu2 134.5(6) . . ? C2 N6 Cu2 124.8(5) . . ? C14 N7 N9 109.7(6) . . ? C14 N7 C13 127.2(6) . . ? N9 N7 C13 123.0(6) . . ? C14 N8 C15 100.9(6) . . ? C14 N8 Cu2 125.0(5) . 1_565 ? C15 N8 Cu2 133.9(5) . 1_565 ? C15 N9 N7 101.7(6) . . ? Mo2 O2 Mo3 120.8(2) 2_554 . ? Mo1 O3 Mo3 117.3(3) . . ? Mo2 O4 Mo1 92.09(16) . . ? Mo2 O4 Mo4 92.6(2) . 2_554 ? Mo1 O4 Mo4 163.6(2) . 2_554 ? Mo2 O4 Mo2 103.9(2) . 2_554 ? Mo1 O4 Mo2 98.30(19) . 2_554 ? Mo4 O4 Mo2 95.85(17) 2_554 2_554 ? Mo2 O4 Mo3 164.2(2) . . ? Mo1 O4 Mo3 86.90(18) . . ? Mo4 O4 Mo3 84.38(14) 2_554 . ? Mo2 O4 Mo3 91.78(15) 2_554 . ? Mo2 O7 Mo1 108.0(2) . . ? Mo2 O7 Mo4 112.1(2) . . ? Mo1 O7 Mo4 105.5(2) . . ? Mo2 O9 Mo4 109.7(2) 2_554 . ? Mo2 O9 Mo1 109.3(2) 2_554 . ? Mo4 O9 Mo1 102.69(18) . . ? Mo4 O10 Mo3 118.0(2) . 2_554 ? N1 Cu1 N1 180.000(1) 2_364 . ? N1 Cu1 O1W 87.7(3) 2_364 . ? N1 Cu1 O1W 92.3(3) . . ? N1 Cu1 O1W 92.3(3) 2_364 2_364 ? N1 Cu1 O1W 87.7(3) . 2_364 ? O1W Cu1 O1W 180.000(1) . 2_364 ? N8 Cu2 N8 180.0(4) 2_565 1_545 ? N8 Cu2 N6 90.5(2) 2_565 . ? N8 Cu2 N6 89.5(2) 1_545 . ? N8 Cu2 N6 89.5(2) 2_565 2 ? N8 Cu2 N6 90.5(2) 1_545 2 ? N6 Cu2 N6 180.0(5) . 2 ? O8 Mo1 O5 104.1(2) . . ? O8 Mo1 O3 101.1(2) . . ? O5 Mo1 O3 103.0(2) . . ? O8 Mo1 O7 99.1(2) . . ? O5 Mo1 O7 97.4(2) . . ? O3 Mo1 O7 146.6(2) . . ? O8 Mo1 O4 158.1(2) . . ? O5 Mo1 O4 97.4(2) . . ? O3 Mo1 O4 77.78(19) . . ? O7 Mo1 O4 73.63(17) . . ? O8 Mo1 O9 86.0(2) . . ? O5 Mo1 O9 165.7(2) . . ? O3 Mo1 O9 84.5(2) . . ? O7 Mo1 O9 70.76(18) . . ? O4 Mo1 O9 72.12(17) . . ? O8 Mo1 Mo2 134.48(19) . . ? O5 Mo1 Mo2 86.55(19) . . ? O3 Mo1 Mo2 119.72(15) . . ? O7 Mo1 Mo2 35.34(13) . . ? O4 Mo1 Mo2 41.96(12) . . ? O9 Mo1 Mo2 79.20(12) . . ? O6 Mo2 O2 104.8(2) . 2_554 ? O6 Mo2 O7 101.0(2) . . ? O2 Mo2 O7 95.8(2) 2_554 . ? O6 Mo2 O9 102.7(2) . 2_554 ? O2 Mo2 O9 96.0(2) 2_554 2_554 ? O7 Mo2 O9 149.87(19) . 2_554 ? O6 Mo2 O4 100.1(2) . . ? O2 Mo2 O4 155.1(2) 2_554 . ? O7 Mo2 O4 78.61(19) . . ? O9 Mo2 O4 79.10(19) 2_554 . ? O6 Mo2 O4 176.0(2) . 2_554 ? O2 Mo2 O4 79.1(2) 2_554 2_554 ? O7 Mo2 O4 77.49(19) . 2_554 ? O9 Mo2 O4 77.67(18) 2_554 2_554 ? O4 Mo2 O4 76.1(2) . 2_554 ? O6 Mo2 Mo1 89.9(2) . . ? O2 Mo2 Mo1 132.43(16) 2_554 . ? O7 Mo2 Mo1 36.65(15) . . ? O9 Mo2 Mo1 125.05(14) 2_554 . ? O4 Mo2 Mo1 45.95(13) . . ? O4 Mo2 Mo1 86.72(13) 2_554 . ? O1 Mo3 O13 104.6(3) . . ? O1 Mo3 O10 98.7(2) . 2_554 ? O13 Mo3 O10 104.0(2) . 2_554 ? O1 Mo3 O3 97.7(2) . . ? O13 Mo3 O3 102.0(2) . . ? O10 Mo3 O3 144.4(2) 2_554 . ? O1 Mo3 O2 161.8(2) . . ? O13 Mo3 O2 93.7(2) . . ? O10 Mo3 O2 76.84(19) 2_554 . ? O3 Mo3 O2 77.8(2) . . ? O1 Mo3 O4 93.4(2) . . ? O13 Mo3 O4 161.9(2) . . ? O10 Mo3 O4 74.48(18) 2_554 . ? O3 Mo3 O4 73.21(19) . . ? O2 Mo3 O4 68.33(17) . . ? O12 Mo4 O11 104.3(3) . . ? O12 Mo4 O10 102.9(2) . . ? O11 Mo4 O10 100.2(3) . . ? O12 Mo4 O9 101.0(2) . . ? O11 Mo4 O9 96.5(2) . . ? O10 Mo4 O9 146.3(2) . . ? O12 Mo4 O7 91.7(2) . . ? O11 Mo4 O7 161.9(2) . . ? O10 Mo4 O7 83.86(19) . . ? O9 Mo4 O7 71.98(18) . . ? O12 Mo4 O4 163.2(2) . 2_554 ? O11 Mo4 O4 92.0(2) . 2_554 ? O10 Mo4 O4 77.61(18) . 2_554 ? O9 Mo4 O4 72.76(17) . 2_554 ? O7 Mo4 O4 71.60(16) . 2_554 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.660 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.141 #===================================================================================================end data_2 _database_code_depnum_ccdc_archive 'CCDC 789619' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H46 Cu4 Mo8 N18 O28' _chemical_formula_sum 'C36 H46 Cu4 Mo8 N18 O28' _chemical_formula_weight 2200.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9539(4) _cell_length_b 11.4171(4) _cell_length_c 12.3377(5) _cell_angle_alpha 85.654(3) _cell_angle_beta 72.963(3) _cell_angle_gamma 69.624(3) _cell_volume 1382.36(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6340 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 29.2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 3.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.66 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11456 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.19 _reflns_number_total 6340 _reflns_number_gt 3794 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0644P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6340 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.46390(10) 0.58259(9) 0.21593(8) 0.0413(2) Uani 1 1 d . . . Cu2 Cu 0.33559(12) 0.99728(13) 0.51701(9) 0.0661(4) Uani 1 1 d . . . C1 C 0.3233(7) 0.8555(6) 0.2278(6) 0.0289(15) Uani 1 1 d . . . H1 H 0.3071 0.8603 0.1574 0.035 Uiso 1 1 calc R . . C2 C 0.3936(9) 0.7889(7) 0.3683(6) 0.0446(19) Uani 1 1 d . . . H2 H 0.4365 0.7344 0.4165 0.054 Uiso 1 1 calc R . . C3 C 0.1933(7) 1.0835(6) 0.2964(5) 0.0299(15) Uani 1 1 d . . . H3A H 0.2475 1.1355 0.2946 0.036 Uiso 1 1 calc R . . H3B H 0.1172 1.1063 0.3646 0.036 Uiso 1 1 calc R . . C4 C 0.1392(6) 1.1099(6) 0.1933(5) 0.0248(14) Uani 1 1 d . . . C5 C 0.2114(6) 1.1519(6) 0.0948(5) 0.0248(14) Uani 1 1 d . . . C6 C 0.1503(7) 1.1959(6) 0.0073(5) 0.0273(15) Uani 1 1 d . . . C7 C 0.0249(7) 1.1884(6) 0.0141(5) 0.0271(15) Uani 1 1 d . . . C8 C -0.0425(6) 1.1363(6) 0.1101(6) 0.0266(15) Uani 1 1 d . . . C9 C 0.0118(7) 1.1000(6) 0.2015(5) 0.0281(15) Uani 1 1 d . . . C10 C -0.0614(8) 1.0512(8) 0.3111(6) 0.048(2) Uani 1 1 d . . . H10A H -0.0336 0.9618 0.3053 0.072 Uiso 1 1 calc R . . H10B H -0.1578 1.0868 0.3228 0.072 Uiso 1 1 calc R . . H10C H -0.0388 1.0744 0.3739 0.072 Uiso 1 1 calc R . . C11 C -0.1724(7) 1.1170(7) 0.1097(7) 0.0435(19) Uani 1 1 d . . . H11A H -0.1546 1.0672 0.0429 0.052 Uiso 1 1 calc R . . H11B H -0.1999 1.0702 0.1757 0.052 Uiso 1 1 calc R . . C12 C 0.3536(7) 1.1498(7) 0.0840(6) 0.0345(17) Uani 1 1 d . . . H12A H 0.3492 1.2103 0.1362 0.052 Uiso 1 1 calc R . . H12B H 0.3942 1.1695 0.0080 0.052 Uiso 1 1 calc R . . H12C H 0.4075 1.0680 0.1009 0.052 Uiso 1 1 calc R . . C13 C -0.3216(7) 1.3416(7) 0.1662(6) 0.0368(18) Uani 1 1 d . . . H13 H -0.2781 1.3567 0.2153 0.044 Uiso 1 1 calc R . . C14 C -0.4547(7) 1.3590(7) 0.0675(6) 0.0367(17) Uani 1 1 d . . . H14 H -0.5264 1.3931 0.0357 0.044 Uiso 1 1 calc R . . C15 C 0.2229(7) 1.2518(7) -0.0946(5) 0.0324(16) Uani 1 1 d . . . H15A H 0.1575 1.3233 -0.1180 0.039 Uiso 1 1 calc R . . H15B H 0.2870 1.2809 -0.0744 0.039 Uiso 1 1 calc R . . C16 C 0.2694(9) 1.1627(8) -0.2878(6) 0.048(2) Uani 1 1 d . . . H16 H 0.2060 1.2287 -0.3122 0.057 Uiso 1 1 calc R . . C17 C -0.0402(8) 1.2300(8) -0.0797(6) 0.046(2) Uani 1 1 d . . . H17A H -0.1001 1.3152 -0.0652 0.068 Uiso 1 1 calc R . . H17B H -0.0911 1.1777 -0.0838 0.068 Uiso 1 1 calc R . . H17C H 0.0288 1.2237 -0.1503 0.068 Uiso 1 1 calc R . . C18 C 0.4257(7) 0.9916(8) -0.2771(6) 0.0373(18) Uani 1 1 d . . . H18 H 0.4944 0.9144 -0.2967 0.045 Uiso 1 1 calc R . . N1 N 0.3952(6) 0.7535(5) 0.2685(5) 0.0303(13) Uani 1 1 d . . . N2 N 0.3255(7) 0.9094(6) 0.3938(5) 0.0434(16) Uani 1 1 d . . . N3 N 0.2772(6) 0.9506(5) 0.3016(4) 0.0266(12) Uani 1 1 d . . . N4 N -0.2850(5) 1.2347(5) 0.1105(5) 0.0283(12) Uani 1 1 d . . . N5 N -0.3692(6) 1.2443(6) 0.0448(5) 0.0392(15) Uani 1 1 d . . . N6 N -0.4292(6) 1.4239(5) 0.1419(5) 0.0346(14) Uani 1 1 d . . . N7 N 0.2956(6) 1.1601(5) -0.1888(5) 0.0295(13) Uani 1 1 d . . . N8 N 0.3905(6) 1.0533(6) -0.1776(5) 0.0414(16) Uani 1 1 d . . . N9 N 0.3474(7) 1.0567(6) -0.3469(5) 0.0418(16) Uani 1 1 d . . . O1 O 0.2411(5) 0.5951(5) 0.2333(4) 0.0365(12) Uani 1 1 d . . . O2 O 0.1634(5) 0.4385(4) 0.1417(4) 0.0347(11) Uani 1 1 d . . . O3 O -0.0224(4) 0.5960(4) 0.3336(3) 0.0235(10) Uani 1 1 d . . . O4 O -0.1273(5) 0.4671(5) 0.2136(4) 0.0370(12) Uani 1 1 d . . . O5 O -0.2194(5) 0.3457(5) 0.3969(4) 0.0399(12) Uani 1 1 d . . . O6 O 0.1320(4) 0.5015(4) 0.4661(3) 0.0233(10) Uani 1 1 d . . . O7 O 0.0397(4) 0.3603(4) 0.3610(3) 0.0253(10) Uani 1 1 d . . . O8 O 0.3136(5) 0.3473(4) 0.2968(3) 0.0292(10) Uani 1 1 d . . . O9 O -0.2159(5) 0.7488(4) 0.5105(3) 0.0288(10) Uani 1 1 d . . . O10 O 0.4278(5) 0.4809(5) 0.3898(4) 0.0359(12) Uani 1 1 d . . . O11 O 0.0357(5) 0.7704(4) 0.4428(4) 0.0339(11) Uani 1 1 d . . . O12 O -0.2982(5) 0.6048(4) 0.4093(4) 0.0291(10) Uani 1 1 d . . . O13 O 0.4994(5) 0.2299(5) 0.4217(4) 0.0448(13) Uani 1 1 d . . . Mo1 Mo 0.16798(6) 0.48285(5) 0.26685(5) 0.02578(15) Uani 1 1 d . . . Mo2 Mo -0.14738(6) 0.45717(5) 0.35492(5) 0.02631(15) Uani 1 1 d . . . Mo3 Mo -0.04079(6) 0.66296(5) 0.48076(4) 0.02394(15) Uani 1 1 d . . . Mo4 Mo 0.36199(6) 0.36317(6) 0.43092(5) 0.02894(16) Uani 1 1 d . . . O1W O 0.5000 1.0000 0.5000 0.110(4) Uani 1 2 d S . . O2W O 0.6348(18) 0.3428(14) 0.5250(12) 0.097(5) Uani 0.50 1 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 Cu1 0.0414(6) 0.0240(5) 0.0511(6) -0.0076(4) -0.0146(4) 0.0007(4) Cu2 0.0707(8) 0.1027(11) 0.0377(6) -0.0093(6) -0.0163(6) -0.0423(8) C1 0.035(4) 0.021(4) 0.032(4) -0.004(3) -0.017(3) -0.002(3) C2 0.057(5) 0.028(4) 0.043(5) 0.006(3) -0.027(4) 0.002(4) C3 0.033(4) 0.019(4) 0.031(4) -0.011(3) -0.007(3) 0.001(3) C4 0.027(4) 0.017(3) 0.027(3) -0.005(3) -0.013(3) 0.002(3) C5 0.025(3) 0.019(3) 0.029(4) -0.013(3) -0.010(3) -0.001(3) C6 0.030(4) 0.023(4) 0.028(4) -0.003(3) -0.009(3) -0.008(3) C7 0.030(4) 0.016(3) 0.032(4) -0.003(3) -0.016(3) 0.003(3) C8 0.022(3) 0.016(3) 0.037(4) -0.006(3) -0.007(3) -0.002(3) C9 0.026(4) 0.018(4) 0.029(4) -0.006(3) 0.000(3) 0.002(3) C10 0.043(5) 0.045(5) 0.054(5) 0.009(4) -0.006(4) -0.022(4) C11 0.031(4) 0.027(4) 0.068(6) 0.000(4) -0.016(4) -0.003(4) C12 0.032(4) 0.035(4) 0.033(4) -0.007(3) -0.013(3) -0.004(4) C13 0.032(4) 0.036(5) 0.046(4) -0.012(3) -0.022(3) -0.005(4) C14 0.030(4) 0.043(5) 0.034(4) -0.001(3) -0.014(3) -0.004(4) C15 0.036(4) 0.025(4) 0.034(4) -0.003(3) -0.011(3) -0.006(3) C16 0.070(6) 0.040(5) 0.036(4) 0.011(4) -0.024(4) -0.017(5) C17 0.041(5) 0.052(5) 0.046(5) 0.010(4) -0.024(4) -0.011(4) C18 0.032(4) 0.043(5) 0.039(4) -0.006(4) -0.007(3) -0.016(4) N1 0.032(3) 0.020(3) 0.039(3) -0.003(3) -0.016(3) -0.004(3) N2 0.060(5) 0.040(4) 0.028(3) 0.005(3) -0.021(3) -0.008(4) N3 0.032(3) 0.024(3) 0.023(3) 0.000(2) -0.012(2) -0.005(3) N4 0.022(3) 0.023(3) 0.038(3) -0.006(2) -0.010(2) -0.003(3) N5 0.038(4) 0.036(4) 0.048(4) -0.009(3) -0.022(3) -0.009(3) N6 0.029(3) 0.025(3) 0.046(4) -0.008(3) -0.012(3) -0.001(3) N7 0.031(3) 0.030(3) 0.031(3) 0.003(3) -0.011(3) -0.013(3) N8 0.033(4) 0.045(4) 0.041(4) -0.013(3) -0.019(3) 0.003(3) N9 0.062(5) 0.044(4) 0.020(3) 0.005(3) -0.013(3) -0.020(4) O1 0.037(3) 0.037(3) 0.038(3) 0.008(2) -0.017(2) -0.013(3) O2 0.044(3) 0.030(3) 0.029(3) -0.005(2) -0.018(2) -0.004(2) O3 0.030(2) 0.018(2) 0.022(2) -0.0023(18) -0.0137(19) -0.002(2) O4 0.044(3) 0.041(3) 0.030(3) -0.001(2) -0.018(2) -0.013(3) O5 0.048(3) 0.032(3) 0.044(3) 0.000(2) -0.020(2) -0.013(3) O6 0.027(2) 0.019(2) 0.021(2) -0.0002(18) -0.0103(19) -0.002(2) O7 0.033(3) 0.019(2) 0.024(2) -0.0031(18) -0.0124(19) -0.005(2) O8 0.032(3) 0.025(3) 0.025(2) -0.0054(19) -0.012(2) 0.002(2) O9 0.040(3) 0.018(2) 0.024(2) -0.0042(18) -0.015(2) 0.002(2) O10 0.036(3) 0.038(3) 0.034(3) -0.001(2) -0.012(2) -0.011(3) O11 0.045(3) 0.021(3) 0.038(3) 0.001(2) -0.016(2) -0.011(2) O12 0.033(3) 0.023(3) 0.032(3) -0.002(2) -0.018(2) -0.003(2) O13 0.044(3) 0.037(3) 0.043(3) -0.015(2) -0.020(2) 0.009(3) Mo1 0.0306(3) 0.0229(3) 0.0228(3) -0.0007(2) -0.0119(2) -0.0041(3) Mo2 0.0332(3) 0.0204(3) 0.0279(3) -0.0038(2) -0.0172(3) -0.0045(3) Mo3 0.0355(3) 0.0138(3) 0.0230(3) -0.0017(2) -0.0154(2) -0.0027(3) Mo4 0.0312(3) 0.0263(4) 0.0271(3) -0.0036(2) -0.0146(3) -0.0010(3) O1W 0.131(11) 0.145(12) 0.037(6) -0.010(6) 0.014(6) -0.055(10) O2W 0.138(15) 0.079(12) 0.081(10) 0.041(8) -0.031(10) -0.054(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 1.906(6) 1_645 ? Cu1 N1 1.917(5) . ? Cu1 O1 2.341(5) . ? Cu1 O10 2.356(5) . ? Cu2 O1W 1.7620(11) . ? Cu2 N9 1.912(6) 1_556 ? Cu2 N2 1.933(6) . ? C1 N1 1.317(9) . ? C1 N3 1.327(8) . ? C2 N1 1.319(9) . ? C2 N2 1.327(10) . ? C3 N3 1.483(9) . ? C3 C4 1.522(9) . ? C4 C5 1.395(9) . ? C4 C9 1.413(9) . ? C5 C6 1.405(9) . ? C5 C12 1.516(9) . ? C6 C7 1.383(9) . ? C6 C15 1.505(9) . ? C7 C8 1.410(9) . ? C7 C17 1.497(9) . ? C8 C9 1.396(9) . ? C8 C11 1.515(9) . ? C9 C10 1.531(9) . ? C11 N4 1.473(9) . ? C13 N4 1.322(8) . ? C13 N6 1.325(9) . ? C14 N5 1.310(9) . ? C14 N6 1.368(8) . ? C15 N7 1.464(8) . ? C16 N7 1.330(9) . ? C16 N9 1.332(10) . ? C18 N8 1.349(9) . ? C18 N9 1.386(10) . ? N2 N3 1.377(8) . ? N4 N5 1.368(7) . ? N6 Cu1 1.906(6) 1_465 ? N7 N8 1.328(8) . ? N9 Cu2 1.912(6) 1_554 ? O1 Mo1 1.702(4) . ? O2 Mo1 1.681(4) . ? O3 Mo3 1.952(4) . ? O3 Mo1 1.994(4) . ? O3 Mo2 2.385(4) . ? O4 Mo2 1.693(4) . ? O5 Mo2 1.694(5) . ? O6 Mo3 2.105(4) . ? O6 Mo2 2.358(4) 2_566 ? O6 Mo3 2.385(4) 2_566 ? O6 Mo1 2.387(4) . ? O6 Mo4 2.392(4) . ? O7 Mo3 1.954(4) 2_566 ? O7 Mo2 1.981(4) . ? O7 Mo1 2.334(4) . ? O8 Mo1 1.901(5) . ? O8 Mo4 1.918(4) . ? O9 Mo3 1.763(5) . ? O9 Mo4 2.307(4) 2_566 ? O10 Mo4 1.715(5) . ? O11 Mo3 1.681(4) . ? O12 Mo2 1.898(5) . ? O12 Mo4 1.905(4) 2_566 ? O13 Mo4 1.710(5) . ? Mo2 O6 2.358(4) 2_566 ? Mo2 Mo3 3.2092(8) 2_566 ? Mo3 O7 1.954(4) 2_566 ? Mo3 O6 2.385(4) 2_566 ? Mo3 Mo2 3.2092(8) 2_566 ? Mo4 O12 1.905(4) 2_566 ? Mo4 O9 2.307(4) 2_566 ? O1W Cu2 1.7620(11) 2_676 ? 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 N6 Cu1 N1 165.5(2) 1_645 . ? N6 Cu1 O1 103.3(2) 1_645 . ? N1 Cu1 O1 88.9(2) . . ? N6 Cu1 O10 88.9(2) 1_645 . ? N1 Cu1 O10 100.6(2) . . ? O1 Cu1 O10 82.99(16) . . ? O1W Cu2 N9 69.1(2) . 1_556 ? O1W Cu2 N2 112.9(2) . . ? N9 Cu2 N2 169.6(3) 1_556 . ? N1 C1 N3 110.3(6) . . ? N1 C2 N2 114.0(7) . . ? N3 C3 C4 113.0(5) . . ? C5 C4 C9 120.8(6) . . ? C5 C4 C3 119.6(6) . . ? C9 C4 C3 119.4(6) . . ? C4 C5 C6 119.1(6) . . ? C4 C5 C12 119.7(6) . . ? C6 C5 C12 121.2(6) . . ? C7 C6 C5 120.7(6) . . ? C7 C6 C15 120.2(6) . . ? C5 C6 C15 119.1(6) . . ? C6 C7 C8 119.7(6) . . ? C6 C7 C17 121.9(6) . . ? C8 C7 C17 118.4(6) . . ? C9 C8 C7 120.6(6) . . ? C9 C8 C11 121.0(6) . . ? C7 C8 C11 118.4(6) . . ? C8 C9 C4 118.7(6) . . ? C8 C9 C10 122.9(6) . . ? C4 C9 C10 118.4(6) . . ? N4 C11 C8 113.3(5) . . ? N4 C13 N6 110.0(6) . . ? N5 C14 N6 114.0(6) . . ? N7 C15 C6 111.1(5) . . ? N7 C16 N9 110.0(8) . . ? N8 C18 N9 112.0(7) . . ? C1 N1 C2 104.7(6) . . ? C1 N1 Cu1 130.6(4) . . ? C2 N1 Cu1 123.9(5) . . ? C2 N2 N3 102.7(6) . . ? C2 N2 Cu2 123.9(5) . . ? N3 N2 Cu2 132.2(5) . . ? C1 N3 N2 108.3(6) . . ? C1 N3 C3 131.4(6) . . ? N2 N3 C3 120.2(5) . . ? C13 N4 N5 110.1(6) . . ? C13 N4 C11 130.0(6) . . ? N5 N4 C11 120.0(5) . . ? C14 N5 N4 102.7(5) . . ? C13 N6 C14 103.2(6) . . ? C13 N6 Cu1 126.3(5) . 1_465 ? C14 N6 Cu1 129.7(5) . 1_465 ? N8 N7 C16 111.3(6) . . ? N8 N7 C15 121.0(6) . . ? C16 N7 C15 127.4(7) . . ? N7 N8 C18 103.5(6) . . ? C16 N9 C18 103.1(6) . . ? C16 N9 Cu2 128.5(6) . 1_554 ? C18 N9 Cu2 127.8(5) . 1_554 ? Mo1 O1 Cu1 129.8(3) . . ? Mo3 O3 Mo1 109.9(2) . . ? Mo3 O3 Mo2 110.87(18) . . ? Mo1 O3 Mo2 102.10(17) . . ? Mo3 O6 Mo2 91.77(15) . 2_566 ? Mo3 O6 Mo3 103.91(16) . 2_566 ? Mo2 O6 Mo3 98.03(15) 2_566 2_566 ? Mo3 O6 Mo1 91.74(15) . . ? Mo2 O6 Mo1 163.65(19) 2_566 . ? Mo3 O6 Mo1 96.61(13) 2_566 . ? Mo3 O6 Mo4 162.7(2) . . ? Mo2 O6 Mo4 86.22(14) 2_566 . ? Mo3 O6 Mo4 93.41(15) 2_566 . ? Mo1 O6 Mo4 85.69(13) . . ? Mo3 O7 Mo2 109.3(2) 2_566 . ? Mo3 O7 Mo1 112.11(17) 2_566 . ? Mo2 O7 Mo1 104.29(19) . . ? Mo1 O8 Mo4 116.6(2) . . ? Mo3 O9 Mo4 116.7(2) . 2_566 ? Mo4 O10 Cu1 130.7(2) . . ? Mo2 O12 Mo4 117.2(2) . 2_566 ? O2 Mo1 O1 104.3(2) . . ? O2 Mo1 O8 102.3(2) . . ? O1 Mo1 O8 100.7(2) . . ? O2 Mo1 O3 102.5(2) . . ? O1 Mo1 O3 97.5(2) . . ? O8 Mo1 O3 144.38(18) . . ? O2 Mo1 O7 90.07(19) . . ? O1 Mo1 O7 163.94(19) . . ? O8 Mo1 O7 82.92(17) . . ? O3 Mo1 O7 71.94(16) . . ? O2 Mo1 O6 161.10(19) . . ? O1 Mo1 O6 94.50(18) . . ? O8 Mo1 O6 75.92(16) . . ? O3 Mo1 O6 72.31(15) . . ? O7 Mo1 O6 71.03(13) . . ? O4 Mo2 O5 105.0(2) . . ? O4 Mo2 O12 100.9(2) . . ? O5 Mo2 O12 101.3(2) . . ? O4 Mo2 O7 102.1(2) . . ? O5 Mo2 O7 99.1(2) . . ? O12 Mo2 O7 143.90(17) . . ? O4 Mo2 O6 158.19(18) . 2_566 ? O5 Mo2 O6 96.81(19) . 2_566 ? O12 Mo2 O6 75.80(16) . 2_566 ? O7 Mo2 O6 72.46(15) . 2_566 ? O4 Mo2 O3 87.36(18) . . ? O5 Mo2 O3 165.9(2) . . ? O12 Mo2 O3 82.78(16) . . ? O7 Mo2 O3 70.99(16) . . ? O6 Mo2 O3 70.86(14) 2_566 . ? O4 Mo2 Mo3 137.21(18) . 2_566 ? O5 Mo2 Mo3 87.60(18) . 2_566 ? O12 Mo2 Mo3 116.76(13) . 2_566 ? O7 Mo2 Mo3 35.07(12) . 2_566 ? O6 Mo2 Mo3 40.98(11) 2_566 2_566 ? O3 Mo2 Mo3 78.52(10) . 2_566 ? O11 Mo3 O9 104.8(2) . . ? O11 Mo3 O3 101.81(19) . . ? O9 Mo3 O3 95.59(18) . . ? O11 Mo3 O7 101.14(19) . 2_566 ? O9 Mo3 O7 95.75(19) . 2_566 ? O3 Mo3 O7 150.80(17) . 2_566 ? O11 Mo3 O6 99.4(2) . . ? O9 Mo3 O6 155.80(18) . . ? O3 Mo3 O6 79.73(16) . . ? O7 Mo3 O6 78.93(17) 2_566 . ? O11 Mo3 O6 175.4(2) . 2_566 ? O9 Mo3 O6 79.71(17) . 2_566 ? O3 Mo3 O6 77.98(15) . 2_566 ? O7 Mo3 O6 77.71(15) 2_566 2_566 ? O6 Mo3 O6 76.09(16) . 2_566 ? O11 Mo3 Mo2 89.71(17) . 2_566 ? O9 Mo3 Mo2 131.40(14) . 2_566 ? O3 Mo3 Mo2 126.97(13) . 2_566 ? O7 Mo3 Mo2 35.65(13) 2_566 2_566 ? O6 Mo3 Mo2 47.25(10) . 2_566 ? O6 Mo3 Mo2 86.85(10) 2_566 2_566 ? O13 Mo4 O10 105.4(2) . . ? O13 Mo4 O12 100.8(2) . 2_566 ? O10 Mo4 O12 99.5(2) . 2_566 ? O13 Mo4 O8 101.8(2) . . ? O10 Mo4 O8 98.9(2) . . ? O12 Mo4 O8 145.75(19) 2_566 . ? O13 Mo4 O9 91.0(2) . 2_566 ? O10 Mo4 O9 163.5(2) . 2_566 ? O12 Mo4 O9 77.64(16) 2_566 2_566 ? O8 Mo4 O9 76.50(17) . 2_566 ? O13 Mo4 O6 161.1(2) . . ? O10 Mo4 O6 93.44(19) . . ? O12 Mo4 O6 74.82(17) 2_566 . ? O8 Mo4 O6 75.50(16) . . ? O9 Mo4 O6 70.14(15) 2_566 . ? Cu2 O1W Cu2 180.00(9) . 2_676 ? _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.717 _refine_diff_density_min -2.023 _refine_diff_density_rms 0.245 #======================================================================================================end data_3 _database_code_depnum_ccdc_archive 'CCDC 789620' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H61 Cu4 Mo8 N27 O26' _chemical_formula_sum 'C54 H61 Cu4 Mo8 N27 O26' _chemical_formula_weight 2525.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.5986(4) _cell_length_b 23.7671(6) _cell_length_c 23.6160(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.573(3) _cell_angle_gamma 90.00 _cell_volume 7632.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13590 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 67.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4936 _exptl_absorpt_coefficient_mu 12.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.187 _exptl_absorpt_correction_T_max 0.358 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78037 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 67.35 _reflns_number_total 13590 _reflns_number_gt 9260 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^+34.5200P] 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 13590 _refine_ls_number_parameters 1118 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.09694(16) 0.04606(11) 0.42332(13) 0.1089(8) Uani 1 1 d . . . Cu2 Cu 0.63343(14) 0.03220(8) 0.01436(6) 0.0711(5) Uani 1 1 d . . . Cu3 Cu 0.91147(13) 0.31246(7) 0.05673(6) 0.0611(4) Uani 1 1 d . . . Cu4 Cu 0.49206(16) 0.30634(8) -0.40464(7) 0.0736(5) Uani 1 1 d . . . Mo1 Mo 1.29153(6) 0.18884(3) 0.11900(3) 0.03932(18) Uani 1 1 d . . . Mo2 Mo 1.19273(5) 0.31450(3) 0.10990(3) 0.03791(17) Uani 1 1 d . . . Mo3 Mo 1.36174(5) 0.27865(3) 0.00490(3) 0.03238(16) Uani 1 1 d . . . Mo4 Mo 1.41313(5) 0.36912(3) 0.12168(3) 0.03758(17) Uani 1 1 d . . . Mo5 Mo 1.57700(5) 0.33145(3) 0.01804(3) 0.03764(17) Uani 1 1 d . . . Mo6 Mo 1.45741(5) 0.15667(3) 0.00944(3) 0.03706(17) Uani 1 1 d . . . Mo7 Mo 1.50366(5) 0.24370(3) 0.13046(3) 0.03310(16) Uani 1 1 d . . . Mo8 Mo 1.68290(6) 0.20697(3) 0.02976(3) 0.04350(19) Uani 1 1 d . . . C3 C 0.7384(9) 0.1288(5) 0.3697(6) 0.067(3) Uani 1 1 d . . . C4 C 0.6531(7) 0.0922(4) 0.3486(4) 0.048(2) Uani 1 1 d . . . C5 C 0.6065(9) 0.0563(5) 0.3869(5) 0.061(3) Uani 1 1 d . . . C6 C 0.5280(8) 0.0231(4) 0.3677(4) 0.049(2) Uani 1 1 d . . . C7 C 0.4930(7) 0.0265(4) 0.3122(4) 0.045(2) Uani 1 1 d . . . C8 C 0.5350(7) 0.0654(4) 0.2752(4) 0.045(2) Uani 1 1 d . . . C9 C 0.6169(8) 0.0969(4) 0.2925(4) 0.047(2) Uani 1 1 d . . . C10 C 0.6656(10) 0.1372(6) 0.2509(5) 0.073(3) Uani 1 1 d . . . H10A H 0.6808 0.1174 0.2167 0.109 Uiso 1 1 calc R . . H10B H 0.7252 0.1517 0.2675 0.109 Uiso 1 1 calc R . . H10C H 0.6217 0.1677 0.2425 0.109 Uiso 1 1 calc R . . C11 C 0.6350(16) 0.0572(8) 0.4487(6) 0.125(8) Uani 1 1 d . . . H11A H 0.5778 0.0642 0.4711 0.188 Uiso 1 1 calc R . . H11B H 0.6824 0.0865 0.4552 0.188 Uiso 1 1 calc R . . H11C H 0.6631 0.0216 0.4591 0.188 Uiso 1 1 calc R . . C12 C 0.4085(9) -0.0104(5) 0.2916(4) 0.062(3) Uani 1 1 d . . . H12A H 0.4008 -0.0417 0.3169 0.093 Uiso 1 1 calc R . . H12B H 0.4225 -0.0241 0.2543 0.093 Uiso 1 1 calc R . . H12C H 0.3489 0.0112 0.2906 0.093 Uiso 1 1 calc R . . C13 C 0.4908(9) 0.0746(5) 0.2179(4) 0.056(3) Uani 1 1 d . . . H13A H 0.4216 0.0648 0.2193 0.067 Uiso 1 1 calc R . . H13B H 0.4950 0.1144 0.2089 0.067 Uiso 1 1 calc R . . C14 C 0.5726(9) 0.0639(5) 0.1247(4) 0.059(3) Uani 1 1 d . . . H14 H 0.5803 0.1020 0.1169 0.070 Uiso 1 1 calc R . . C15 C 0.5730(10) -0.0252(5) 0.1191(5) 0.069(3) Uani 1 1 d . . . H15 H 0.5812 -0.0613 0.1047 0.083 Uiso 1 1 calc R . . C16 C 0.4747(8) -0.0147(4) 0.4097(4) 0.055(3) Uani 1 1 d . . . H16A H 0.4604 -0.0507 0.3922 0.067 Uiso 1 1 calc R . . H16B H 0.5166 -0.0213 0.4426 0.067 Uiso 1 1 calc R . . C17 C 0.2929(9) -0.0018(5) 0.4164(5) 0.062(3) Uani 1 1 d . . . H17 H 0.2733 -0.0339 0.3967 0.075 Uiso 1 1 calc R . . C18 C 0.2949(9) 0.0734(5) 0.4620(5) 0.066(3) Uani 1 1 d . . . H18 H 0.2734 0.1057 0.4802 0.079 Uiso 1 1 calc R . . C19 C 0.6919(16) -0.0035(6) -0.0967(5) 0.119(8) Uani 1 1 d . . . H19 H 0.6850 -0.0411 -0.0864 0.143 Uiso 1 1 calc R . . C20 C 0.6925(9) 0.0836(5) -0.0926(4) 0.060(3) Uani 1 1 d . . . H20 H 0.6846 0.1207 -0.0810 0.072 Uiso 1 1 calc R . . C21 C 0.7472(10) 0.1002(5) -0.1939(4) 0.061(3) Uani 1 1 d . . . H21A H 0.7041 0.0891 -0.2249 0.073 Uiso 1 1 calc R . . H21B H 0.8142 0.0912 -0.2044 0.073 Uiso 1 1 calc R . . C22 C 0.7383(8) 0.1634(4) -0.1843(3) 0.045(2) Uani 1 1 d . . . C23 C 0.6466(8) 0.1891(4) -0.1863(3) 0.048(2) Uani 1 1 d . . . C24 C 0.6396(8) 0.2469(5) -0.1814(4) 0.054(3) Uani 1 1 d . . . C25 C 0.7255(9) 0.2803(5) -0.1771(4) 0.052(3) Uani 1 1 d . . . C26 C 0.8156(8) 0.2538(4) -0.1755(3) 0.045(2) Uani 1 1 d . . . C27 C 0.8229(7) 0.1951(4) -0.1769(3) 0.044(2) Uani 1 1 d . . . C28 C 0.9228(8) 0.1666(6) -0.1708(5) 0.070(3) Uani 1 1 d . . . H28A H 0.9140 0.1287 -0.1577 0.105 Uiso 1 1 calc R . . H28B H 0.9625 0.1870 -0.1439 0.105 Uiso 1 1 calc R . . H28C H 0.9550 0.1662 -0.2068 0.105 Uiso 1 1 calc R . . C29 C 0.5541(10) 0.1539(6) -0.1919(5) 0.073(4) Uani 1 1 d . . . H29A H 0.5260 0.1484 -0.1552 0.109 Uiso 1 1 calc R . . H29B H 0.5702 0.1180 -0.2080 0.109 Uiso 1 1 calc R . . H29C H 0.5077 0.1729 -0.2160 0.109 Uiso 1 1 calc R . . C30 C 0.7175(12) 0.3436(5) -0.1746(5) 0.082(4) Uani 1 1 d . . . H30A H 0.7463 0.3569 -0.1398 0.123 Uiso 1 1 calc R . . H30B H 0.6495 0.3544 -0.1763 0.123 Uiso 1 1 calc R . . H30C H 0.7516 0.3598 -0.2060 0.123 Uiso 1 1 calc R . . C31 C 0.9078(9) 0.2877(5) -0.1701(4) 0.062(3) Uani 1 1 d . . . H31A H 0.9592 0.2702 -0.1922 0.075 Uiso 1 1 calc R . . H31B H 0.8963 0.3251 -0.1853 0.075 Uiso 1 1 calc R . . C32 C 0.8864(8) 0.2923(5) -0.0648(4) 0.050(2) Uani 1 1 d . . . H32 H 0.8185 0.2878 -0.0643 0.061 Uiso 1 1 calc R . . C33 C 1.0336(8) 0.3029(5) -0.0412(4) 0.061(3) Uani 1 1 d . . . H33 H 1.0897 0.3075 -0.0189 0.074 Uiso 1 1 calc R . . C34 C 0.5379(10) 0.2737(7) -0.1798(4) 0.077(4) Uani 1 1 d . . . H34A H 0.4942 0.2498 -0.1582 0.092 Uiso 1 1 calc R . . H34B H 0.5423 0.3097 -0.1606 0.092 Uiso 1 1 calc R . . C35 C 0.5409(7) 0.2836(4) -0.2868(4) 0.048(2) Uani 1 1 d . . . H35 H 0.6080 0.2791 -0.2925 0.057 Uiso 1 1 calc R . . C36 C 0.3861(9) 0.2967(6) -0.2988(4) 0.066(3) Uani 1 1 d . . . H36 H 0.3257 0.3031 -0.3164 0.079 Uiso 1 1 calc R . . C37 C 0.9189(8) 0.3464(6) 0.1754(4) 0.066(3) Uani 1 1 d . . . H37 H 0.9859 0.3543 0.1742 0.079 Uiso 1 1 calc R . . C38 C 0.7761(8) 0.3235(6) 0.1503(4) 0.063(3) Uani 1 1 d . . . H38 H 0.7211 0.3124 0.1294 0.075 Uiso 1 1 calc R . . C39 C 0.6943(8) 0.3323(6) 0.2437(5) 0.069(4) Uani 1 1 d . . . H39A H 0.7019 0.2986 0.2664 0.083 Uiso 1 1 calc R . . H39B H 0.6339 0.3285 0.2219 0.083 Uiso 1 1 calc R . . C40 C 0.6846(7) 0.3816(5) 0.2823(4) 0.056(3) Uani 1 1 d . . . C41 C 0.6635(9) 0.4340(6) 0.2585(4) 0.069(3) Uani 1 1 d . . . C42 C 0.6446(11) 0.4779(6) 0.2941(5) 0.079(4) Uani 1 1 d . . . C43 C 0.6493(10) 0.4734(5) 0.3524(5) 0.066(3) Uani 1 1 d . . . C44 C 0.6773(8) 0.4211(5) 0.3763(4) 0.057(3) Uani 1 1 d . . . C45 C 0.6953(7) 0.3747(5) 0.3409(4) 0.053(3) Uani 1 1 d . . . C46 C 0.7271(10) 0.3190(6) 0.3662(5) 0.074(3) Uani 1 1 d . . . H46A H 0.6728 0.2932 0.3653 0.111 Uiso 1 1 calc R . . H46B H 0.7482 0.3247 0.4047 0.111 Uiso 1 1 calc R . . H46C H 0.7805 0.3038 0.3447 0.111 Uiso 1 1 calc R . . C47 C 0.6576(12) 0.4419(8) 0.1952(5) 0.105(6) Uani 1 1 d . . . H47A H 0.6123 0.4716 0.1864 0.157 Uiso 1 1 calc R . . H47B H 0.6354 0.4076 0.1777 0.157 Uiso 1 1 calc R . . H47C H 0.7215 0.4514 0.1811 0.157 Uiso 1 1 calc R . . C48 C 0.6239(14) 0.5237(7) 0.3894(6) 0.103(5) Uani 1 1 d . . . H48A H 0.6799 0.5481 0.3923 0.154 Uiso 1 1 calc R . . H48B H 0.6062 0.5108 0.4264 0.154 Uiso 1 1 calc R . . H48C H 0.5697 0.5438 0.3727 0.154 Uiso 1 1 calc R . . C49 C 0.6874(8) 0.4153(6) 0.4393(4) 0.069(3) Uani 1 1 d . . . H49A H 0.7465 0.3940 0.4479 0.082 Uiso 1 1 calc R . . H49B H 0.6952 0.4525 0.4558 0.082 Uiso 1 1 calc R . . C50 C 0.6039(9) 0.3470(6) 0.5028(5) 0.068(3) Uani 1 1 d . . . H50 H 0.6593 0.3262 0.5130 0.081 Uiso 1 1 calc R . . C51 C 0.4599(9) 0.3776(6) 0.4958(5) 0.069(3) Uani 1 1 d . . . H51 H 0.3927 0.3817 0.5017 0.083 Uiso 1 1 calc R . . C52 C 0.6153(18) 0.5307(11) 0.2698(11) 0.155(9) Uani 1 1 d U . . H52A H 0.6433 0.5336 0.2323 0.186 Uiso 1 1 calc R . . H52B H 0.6428 0.5608 0.2926 0.186 Uiso 1 1 calc R . . C53 C 0.431(2) 0.5056(13) 0.2284(14) 0.190(6) Uani 1 1 d U . . H53 H 0.4468 0.4764 0.2040 0.227 Uiso 1 1 calc R . . C54 C 0.349(2) 0.5669(12) 0.2860(13) 0.179(6) Uani 1 1 d U . . H54 H 0.2979 0.5853 0.3039 0.214 Uiso 1 1 calc R . . N4 N 0.5363(7) 0.0426(3) 0.1719(3) 0.053(2) Uani 1 1 d . . . N5 N 0.5369(9) -0.0140(4) 0.1704(4) 0.074(3) Uani 1 1 d . . . N6 N 0.5960(7) 0.0222(4) 0.0907(3) 0.056(2) Uani 1 1 d . . . N7 N 0.3829(7) 0.0121(4) 0.4275(3) 0.049(2) Uani 1 1 d . . . N8 N 0.3863(8) 0.0608(4) 0.4585(4) 0.069(3) Uani 1 1 d . . . N9 N 0.2321(7) 0.0369(4) 0.4377(4) 0.065(2) Uani 1 1 d . . . N10 N 0.7216(8) 0.0683(4) -0.1435(3) 0.059(2) Uani 1 1 d . . . N11 N 0.7178(12) 0.0124(4) -0.1479(4) 0.103(5) Uani 1 1 d . . . N12 N 0.6764(9) 0.0394(4) -0.0604(4) 0.068(3) Uani 1 1 d . . . N13 N 0.9406(7) 0.2922(4) -0.1106(3) 0.050(2) Uani 1 1 d . . . N14 N 1.0364(7) 0.2987(5) -0.0968(4) 0.069(3) Uani 1 1 d . . . N15 N 0.9430(6) 0.2998(4) -0.0197(3) 0.050(2) Uani 1 1 d . . . N16 N 0.4967(6) 0.2821(4) -0.2365(3) 0.053(2) Uani 1 1 d . . . N17 N 0.3981(8) 0.2905(5) -0.2429(4) 0.076(3) Uani 1 1 d . . . N18 N 0.4739(7) 0.2926(4) -0.3274(3) 0.052(2) Uani 1 1 d . . . N19 N 0.7765(6) 0.3356(4) 0.2045(3) 0.056(2) Uani 1 1 d . . . N20 N 0.8667(7) 0.3508(5) 0.2218(3) 0.066(3) Uani 1 1 d . . . N21 N 0.8664(7) 0.3295(4) 0.1297(3) 0.058(2) Uani 1 1 d . . . N22 N 0.6033(6) 0.3875(4) 0.4657(3) 0.055(2) Uani 1 1 d . . . N23 N 0.5097(8) 0.4079(5) 0.4597(4) 0.072(3) Uani 1 1 d . . . N24 N 0.5167(7) 0.3395(4) 0.5237(4) 0.060(2) Uani 1 1 d . . . N27 N 0.3410(17) 0.5255(10) 0.2379(11) 0.187(6) Uani 1 1 d U . . N26 N 0.4438(18) 0.5717(10) 0.2979(10) 0.184(7) Uani 1 1 d DU . . N25 N 0.5023(17) 0.5393(10) 0.2649(11) 0.185(6) Uani 1 1 d DU . . O1 O 1.0845(5) 0.3400(3) 0.0851(3) 0.0574(18) Uani 1 1 d . . . O3 O 1.1813(5) 0.2354(3) 0.0993(3) 0.0454(15) Uani 1 1 d . . . O2 O 1.1818(6) 0.3165(3) 0.1807(3) 0.0576(18) Uani 1 1 d . . . O21 O 1.3340(4) 0.2000(2) 0.0191(2) 0.0377(13) Uani 1 1 d . . . O26 O 1.6872(4) 0.2862(3) 0.0390(2) 0.0432(14) Uani 1 1 d . . . O10 O 1.4344(5) 0.3466(2) 0.0249(2) 0.0387(13) Uani 1 1 d . . . O5 O 1.2445(5) 0.3044(3) 0.0174(2) 0.0417(14) Uani 1 1 d . . . O15 O 1.6206(5) 0.2172(3) 0.1197(2) 0.0421(14) Uani 1 1 d . . . O4 O 1.2791(5) 0.3771(3) 0.1005(3) 0.0463(15) Uani 1 1 d . . . O9 O 1.5345(4) 0.3221(2) 0.1148(2) 0.0365(13) Uani 1 1 d . . . O12 O 1.4926(5) 0.2441(3) 0.2012(2) 0.0490(16) Uani 1 1 d . . . O11 O 1.3606(4) 0.2756(2) 0.1073(2) 0.0341(12) Uani 1 1 d . . . O19 O 1.3721(5) 0.2792(3) -0.0659(2) 0.0460(15) Uani 1 1 d . . . O20 O 1.5043(4) 0.2459(2) 0.0288(2) 0.0356(13) Uani 1 1 d . . . O23 O 1.4670(6) 0.1612(3) -0.0613(3) 0.0581(18) Uani 1 1 d . . . O18 O 1.5842(5) 0.3298(3) -0.0536(3) 0.0521(17) Uani 1 1 d . . . O14 O 1.4339(5) 0.1749(2) 0.1100(2) 0.0393(14) Uani 1 1 d . . . O6 O 1.2460(5) 0.1256(3) 0.0991(3) 0.0586(18) Uani 1 1 d . . . O7 O 1.4070(5) 0.3681(3) 0.1928(3) 0.0536(17) Uani 1 1 d . . . O22 O 1.4151(5) 0.0906(3) 0.0201(3) 0.0545(17) Uani 1 1 d . . . O8 O 1.4543(5) 0.4347(3) 0.1062(3) 0.0561(18) Uani 1 1 d . . . O24 O 1.7053(7) 0.2059(3) -0.0401(3) 0.075(3) Uani 1 1 d . . . O13 O 1.2858(5) 0.1882(3) 0.1902(3) 0.0561(18) Uani 1 1 d . . . O16 O 1.5923(5) 0.1463(3) 0.0322(3) 0.0456(15) Uani 1 1 d . . . O25 O 1.7873(5) 0.1818(4) 0.0606(4) 0.071(2) Uani 1 1 d . . . O17 O 1.6192(6) 0.3961(3) 0.0364(3) 0.063(2) Uani 1 1 d . . . C1 C 0.9070(9) 0.0990(6) 0.3965(7) 0.084(4) Uani 0.518(17) 1 d PD . 1 C2 C 0.8923(16) 0.0163(9) 0.4195(15) 0.104(12) Uani 0.518(17) 1 d PD . 1 N1 N 0.8163(13) 0.0898(7) 0.3889(11) 0.051(5) Uani 0.518(17) 1 d PD . 1 N2 N 0.8067(17) 0.0362(8) 0.4027(15) 0.120(12) Uani 0.518(17) 1 d PD . 1 N3 N 0.9577(16) 0.0581(9) 0.4154(13) 0.065(7) Uani 0.518(17) 1 d PD . 1 C1' C 0.9070(9) 0.0990(6) 0.3965(7) 0.084(4) Uani 0.482(17) 1 d P . 2 C2' C 0.967(2) 0.0693(15) 0.3203(19) 0.101(12) Uani 0.482(17) 1 d P . 2 N1' N 0.8397(19) 0.1045(12) 0.3612(14) 0.073(8) Uani 0.482(17) 1 d P . 2 N2' N 0.884(2) 0.0938(12) 0.3086(11) 0.088(8) Uani 0.482(17) 1 d P . 2 N3' N 0.985(2) 0.0683(13) 0.380(2) 0.096(12) Uani 0.482(17) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0645(13) 0.0955(16) 0.166(2) -0.0116(16) -0.0288(14) 0.0033(12) Cu2 0.0866(13) 0.0889(13) 0.0382(8) 0.0133(8) 0.0153(8) 0.0202(10) Cu3 0.0754(11) 0.0768(11) 0.0309(7) -0.0058(7) -0.0011(7) 0.0091(9) Cu4 0.1141(16) 0.0693(11) 0.0374(8) 0.0101(7) 0.0092(9) 0.0006(10) Mo1 0.0422(4) 0.0359(4) 0.0401(4) 0.0048(3) 0.0095(3) 0.0024(3) Mo2 0.0398(4) 0.0397(4) 0.0343(3) -0.0033(3) 0.0026(3) 0.0040(3) Mo3 0.0379(4) 0.0349(3) 0.0243(3) 0.0009(3) -0.0016(3) 0.0032(3) Mo4 0.0435(4) 0.0336(4) 0.0356(4) -0.0060(3) -0.0006(3) 0.0040(3) Mo5 0.0417(4) 0.0406(4) 0.0307(3) 0.0036(3) 0.0027(3) -0.0011(3) Mo6 0.0414(4) 0.0338(4) 0.0360(4) -0.0054(3) 0.0030(3) 0.0026(3) Mo7 0.0399(4) 0.0361(4) 0.0234(3) 0.0024(3) 0.0005(3) 0.0055(3) Mo8 0.0466(4) 0.0455(4) 0.0387(4) -0.0081(3) 0.0118(3) -0.0028(3) C3 0.052(7) 0.058(7) 0.091(9) -0.008(6) -0.018(6) 0.001(5) C4 0.041(5) 0.042(5) 0.062(6) 0.003(5) -0.003(5) -0.005(4) C5 0.064(7) 0.059(7) 0.059(6) 0.012(5) -0.018(5) -0.019(6) C6 0.060(6) 0.049(6) 0.039(5) 0.006(4) -0.006(4) -0.012(5) C7 0.053(6) 0.051(6) 0.031(4) 0.002(4) 0.002(4) -0.004(5) C8 0.053(6) 0.046(5) 0.036(5) 0.002(4) -0.003(4) 0.006(5) C9 0.057(6) 0.036(5) 0.048(5) -0.005(4) 0.007(5) -0.006(4) C10 0.072(8) 0.069(8) 0.076(8) 0.016(6) 0.003(7) -0.017(7) C11 0.20(2) 0.115(13) 0.057(8) 0.023(8) -0.056(10) -0.084(14) C12 0.072(8) 0.071(7) 0.043(5) -0.001(5) -0.006(5) -0.028(6) C13 0.074(7) 0.057(6) 0.036(5) -0.003(4) 0.002(5) 0.009(6) C14 0.080(8) 0.054(6) 0.042(5) 0.014(5) 0.006(5) 0.009(6) C15 0.100(10) 0.058(7) 0.050(6) -0.001(5) 0.018(6) 0.003(7) C16 0.068(7) 0.047(6) 0.052(6) 0.004(5) -0.001(5) -0.005(5) C17 0.067(8) 0.056(7) 0.064(7) -0.003(5) 0.000(6) -0.023(6) C18 0.067(8) 0.062(7) 0.068(7) -0.011(6) -0.001(6) -0.006(6) C19 0.25(2) 0.048(7) 0.059(8) 0.016(6) 0.061(11) 0.051(10) C20 0.099(9) 0.047(6) 0.033(5) -0.005(4) 0.015(5) 0.015(6) C21 0.104(9) 0.053(6) 0.026(4) -0.002(4) 0.010(5) -0.010(6) C22 0.063(7) 0.050(5) 0.023(4) 0.003(4) 0.001(4) -0.009(5) C23 0.061(6) 0.060(6) 0.023(4) 0.004(4) -0.007(4) -0.015(5) C24 0.058(6) 0.078(8) 0.024(4) -0.001(4) 0.001(4) 0.010(6) C25 0.078(8) 0.057(6) 0.022(4) 0.003(4) 0.002(4) -0.002(6) C26 0.056(6) 0.054(6) 0.025(4) -0.001(4) -0.001(4) -0.012(5) C27 0.055(6) 0.048(5) 0.028(4) -0.002(4) -0.007(4) -0.001(4) C28 0.051(7) 0.096(9) 0.063(7) -0.008(7) -0.004(5) 0.022(6) C29 0.076(8) 0.089(9) 0.054(6) 0.010(6) 0.004(6) -0.027(7) C30 0.137(13) 0.059(7) 0.049(6) -0.002(6) 0.003(7) 0.007(8) C31 0.081(8) 0.069(7) 0.037(5) 0.001(5) -0.003(5) -0.026(6) C32 0.058(6) 0.066(7) 0.027(4) -0.002(4) -0.001(4) -0.012(5) C33 0.052(6) 0.094(9) 0.039(5) -0.008(5) -0.013(5) -0.004(6) C34 0.093(9) 0.113(11) 0.025(5) -0.010(6) -0.005(5) 0.030(8) C35 0.044(5) 0.055(6) 0.044(5) 0.005(4) 0.012(4) 0.001(5) C36 0.064(7) 0.090(9) 0.043(6) 0.002(6) 0.006(5) 0.030(6) C37 0.043(6) 0.107(10) 0.046(6) -0.025(6) 0.003(5) 0.000(6) C38 0.046(6) 0.101(9) 0.041(5) -0.028(6) -0.016(5) -0.001(6) C39 0.044(6) 0.114(10) 0.049(6) -0.027(6) 0.009(5) -0.016(6) C40 0.041(6) 0.090(8) 0.038(5) -0.005(5) 0.008(4) -0.008(5) C41 0.072(8) 0.099(10) 0.036(5) 0.005(6) 0.007(5) 0.017(7) C42 0.104(11) 0.070(8) 0.064(8) 0.018(7) 0.004(7) 0.015(8) C43 0.079(8) 0.072(8) 0.049(6) -0.008(6) 0.004(6) -0.002(6) C44 0.047(6) 0.082(8) 0.041(5) -0.011(5) 0.004(4) -0.004(5) C45 0.043(6) 0.071(7) 0.046(5) -0.006(5) 0.006(4) -0.008(5) C46 0.069(8) 0.083(9) 0.070(8) 0.004(7) 0.005(6) 0.007(7) C47 0.106(12) 0.162(17) 0.046(7) 0.008(8) 0.003(7) 0.050(11) C48 0.135(15) 0.098(11) 0.076(9) -0.022(8) 0.015(9) 0.019(10) C49 0.054(7) 0.109(10) 0.043(6) -0.001(6) 0.006(5) -0.014(7) C50 0.065(8) 0.092(9) 0.046(6) 0.006(6) -0.006(5) 0.009(7) C51 0.062(7) 0.095(9) 0.050(6) 0.019(6) 0.004(5) -0.003(7) C52 0.147(11) 0.162(12) 0.156(12) 0.002(9) 0.012(9) -0.002(9) C53 0.164(13) 0.166(12) 0.239(15) -0.061(11) -0.003(12) 0.044(10) C54 0.161(13) 0.152(12) 0.223(14) -0.051(10) 0.000(13) 0.046(12) N4 0.081(6) 0.047(5) 0.030(4) 0.002(3) 0.007(4) 0.005(4) N5 0.117(9) 0.049(5) 0.056(5) 0.001(4) 0.020(6) 0.003(6) N6 0.066(6) 0.063(6) 0.039(4) 0.012(4) 0.001(4) 0.009(5) N7 0.061(6) 0.049(5) 0.037(4) 0.005(3) 0.001(4) -0.008(4) N8 0.075(7) 0.054(6) 0.076(7) -0.014(5) -0.006(5) -0.012(5) N9 0.059(6) 0.061(6) 0.074(6) -0.004(5) -0.005(5) -0.003(5) N10 0.097(7) 0.044(5) 0.035(4) 0.000(4) 0.020(4) 0.001(5) N11 0.209(15) 0.042(5) 0.060(6) 0.002(5) 0.056(8) 0.022(7) N12 0.111(8) 0.047(5) 0.047(5) 0.006(4) 0.017(5) 0.018(5) N13 0.064(5) 0.062(5) 0.024(4) -0.004(3) 0.002(3) -0.025(4) N14 0.059(6) 0.104(8) 0.044(5) -0.009(5) 0.004(4) -0.010(6) N15 0.047(5) 0.062(5) 0.041(4) 0.002(4) -0.005(4) -0.002(4) N16 0.057(5) 0.067(6) 0.034(4) 0.006(4) 0.007(4) 0.025(4) N17 0.079(7) 0.107(8) 0.041(5) 0.006(5) 0.010(5) 0.039(6) N18 0.058(5) 0.053(5) 0.046(4) 0.001(4) -0.002(4) 0.005(4) N19 0.048(5) 0.085(7) 0.037(4) -0.015(4) -0.006(4) 0.002(5) N20 0.049(5) 0.109(8) 0.038(4) -0.017(5) -0.006(4) -0.011(5) N21 0.053(5) 0.091(7) 0.031(4) -0.006(4) -0.004(4) 0.001(5) N22 0.052(5) 0.079(6) 0.033(4) 0.007(4) 0.004(4) 0.001(5) N23 0.062(6) 0.093(8) 0.060(6) 0.027(5) 0.001(5) 0.014(6) N24 0.069(6) 0.070(6) 0.043(4) 0.009(4) 0.009(4) -0.003(5) N27 0.159(12) 0.167(12) 0.234(14) -0.043(10) -0.004(12) 0.041(10) N26 0.175(14) 0.155(12) 0.221(15) -0.058(11) 0.001(14) 0.041(13) N25 0.158(14) 0.161(13) 0.236(16) -0.062(12) -0.004(12) 0.048(11) O1 0.052(4) 0.064(5) 0.057(4) -0.011(4) 0.004(3) 0.013(4) O3 0.045(4) 0.045(4) 0.046(3) -0.001(3) 0.010(3) 0.003(3) O2 0.067(5) 0.060(4) 0.045(4) -0.010(3) 0.005(3) -0.006(4) O21 0.045(3) 0.040(3) 0.028(3) -0.001(2) -0.002(2) -0.001(3) O26 0.039(3) 0.055(4) 0.035(3) -0.007(3) 0.004(3) -0.004(3) O10 0.052(4) 0.036(3) 0.027(3) 0.003(2) -0.002(3) 0.000(3) O5 0.047(4) 0.048(4) 0.030(3) -0.001(3) -0.001(3) 0.005(3) O15 0.044(3) 0.059(4) 0.022(3) 0.003(3) 0.002(2) 0.007(3) O4 0.052(4) 0.040(3) 0.047(4) -0.003(3) 0.005(3) 0.007(3) O9 0.042(3) 0.041(3) 0.026(3) -0.003(2) 0.000(2) -0.002(3) O12 0.055(4) 0.062(4) 0.030(3) 0.004(3) 0.000(3) 0.004(3) O11 0.040(3) 0.036(3) 0.027(3) -0.001(2) 0.004(2) 0.007(3) O19 0.060(4) 0.049(4) 0.029(3) 0.000(3) -0.003(3) 0.001(3) O20 0.042(3) 0.039(3) 0.026(3) 0.002(2) 0.005(2) 0.004(3) O23 0.074(5) 0.057(4) 0.044(4) -0.014(3) 0.005(3) 0.008(4) O18 0.054(4) 0.061(4) 0.042(3) 0.011(3) 0.003(3) 0.001(3) O14 0.048(4) 0.039(3) 0.031(3) 0.004(2) 0.006(3) 0.003(3) O6 0.060(5) 0.041(4) 0.075(5) 0.005(3) 0.017(4) -0.006(3) O7 0.063(5) 0.057(4) 0.040(3) -0.011(3) 0.000(3) 0.007(4) O22 0.056(4) 0.036(3) 0.071(5) -0.003(3) 0.005(4) -0.004(3) O8 0.062(4) 0.040(4) 0.066(4) -0.008(3) -0.003(4) 0.001(3) O24 0.103(7) 0.064(5) 0.059(4) -0.019(4) 0.042(4) -0.024(5) O13 0.058(4) 0.065(4) 0.046(4) 0.014(3) 0.016(3) 0.006(4) O16 0.054(4) 0.040(3) 0.043(3) -0.002(3) 0.007(3) 0.006(3) O25 0.043(4) 0.076(5) 0.094(6) -0.016(5) 0.012(4) 0.008(4) O17 0.072(5) 0.050(4) 0.066(5) -0.001(4) 0.017(4) -0.010(4) C1 0.063(8) 0.076(9) 0.112(11) -0.035(8) -0.022(8) 0.008(7) C2 0.049(16) 0.12(3) 0.14(3) 0.03(2) 0.000(16) 0.029(18) N1 0.040(11) 0.039(11) 0.075(15) -0.005(9) -0.011(10) -0.004(8) N2 0.094(19) 0.054(14) 0.21(3) 0.031(17) 0.03(2) -0.012(13) N3 0.039(13) 0.045(11) 0.11(2) -0.028(12) 0.010(12) -0.003(9) C1' 0.063(8) 0.076(9) 0.112(11) -0.035(8) -0.022(8) 0.008(7) C2' 0.060(19) 0.09(2) 0.15(4) -0.05(2) 0.02(2) 0.007(17) N1' 0.046(14) 0.060(16) 0.11(2) -0.009(16) -0.011(15) -0.007(11) N2' 0.084(18) 0.094(18) 0.087(17) -0.009(14) 0.017(14) -0.010(15) N3' 0.044(17) 0.068(17) 0.17(4) -0.05(2) -0.02(2) -0.002(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N9 1.878(10) . ? Cu1 N3' 1.90(3) 1_455 ? Cu1 N3 1.92(2) 1_455 ? Cu2 N12 1.872(9) . ? Cu2 N6 1.893(8) . ? Cu3 N21 1.880(8) . ? Cu3 N15 1.882(8) . ? Cu4 N18 1.872(8) . ? Cu4 N24 1.900(8) 1_554 ? Mo1 O13 1.685(7) . ? Mo1 O6 1.690(7) . ? Mo1 O3 1.917(7) . ? Mo1 O14 1.977(6) . ? Mo1 O11 2.284(6) . ? Mo1 O21 2.448(5) . ? Mo1 Mo7 3.1747(10) . ? Mo2 O2 1.681(7) . ? Mo2 O1 1.690(7) . ? Mo2 O3 1.903(6) . ? Mo2 O4 1.909(7) . ? Mo2 O5 2.314(6) . ? Mo2 O11 2.464(6) . ? Mo3 O19 1.679(6) . ? Mo3 O5 1.736(6) . ? Mo3 O21 1.936(6) . ? Mo3 O10 1.948(6) . ? Mo3 O20 2.158(6) . ? Mo3 O11 2.420(5) . ? Mo3 Mo6 3.1790(10) . ? Mo3 Mo5 3.1971(10) . ? Mo4 O7 1.682(6) . ? Mo4 O8 1.697(7) . ? Mo4 O4 1.894(7) . ? Mo4 O9 2.001(6) . ? Mo4 O11 2.358(6) . ? Mo4 O10 2.369(5) . ? Mo5 O17 1.695(7) . ? Mo5 O18 1.696(6) . ? Mo5 O26 1.906(7) . ? Mo5 O10 1.981(6) . ? Mo5 O20 2.275(6) . ? Mo5 O9 2.374(5) . ? Mo6 O23 1.680(7) . ? Mo6 O22 1.691(7) . ? Mo6 O16 1.922(7) . ? Mo6 O21 1.984(6) . ? Mo6 O20 2.261(6) . ? Mo6 O14 2.439(5) . ? Mo7 O12 1.678(6) . ? Mo7 O15 1.732(6) . ? Mo7 O9 1.946(6) . ? Mo7 O14 1.949(6) . ? Mo7 O11 2.154(6) . ? Mo7 O20 2.402(5) . ? Mo8 O24 1.680(7) . ? Mo8 O25 1.698(8) . ? Mo8 O16 1.897(7) . ? Mo8 O26 1.897(7) . ? Mo8 O15 2.308(5) . ? C3 N1 1.48(2) . ? C3 N1' 1.51(3) . ? C3 C4 1.530(15) . ? C4 C5 1.400(15) . ? C4 C9 1.414(14) . ? C5 C6 1.399(15) . ? C5 C11 1.506(16) . ? C6 C7 1.393(13) . ? C6 C16 1.526(14) . ? C7 C8 1.399(13) . ? C7 C12 1.522(14) . ? C8 C9 1.400(14) . ? C8 C13 1.491(13) . ? C9 C10 1.525(15) . ? C13 N4 1.468(12) . ? C14 N6 1.317(14) . ? C14 N4 1.324(13) . ? C15 N5 1.339(14) . ? C15 N6 1.349(15) . ? C16 N7 1.466(14) . ? C17 N7 1.292(14) . ? C17 N9 1.339(15) . ? C18 N8 1.282(16) . ? C18 N9 1.341(15) . ? C19 N11 1.318(15) . ? C19 N12 1.351(15) . ? C20 N12 1.317(14) . ? C20 N10 1.320(12) . ? C21 N10 1.455(12) . ? C21 C22 1.524(15) . ? C22 C27 1.386(14) . ? C22 C23 1.389(15) . ? C23 C24 1.382(16) . ? C23 C29 1.514(15) . ? C24 C25 1.416(16) . ? C24 C34 1.523(16) . ? C25 C26 1.378(15) . ? C25 C30 1.510(16) . ? C26 C27 1.398(14) . ? C26 C31 1.495(15) . ? C27 C28 1.524(15) . ? C31 N13 1.474(12) . ? C32 N13 1.315(12) . ? C32 N15 1.320(12) . ? C33 N14 1.317(13) . ? C33 N15 1.340(14) . ? C34 N16 1.462(13) . ? C35 N18 1.334(13) . ? C35 N16 1.336(12) . ? C36 N17 1.337(14) . ? C36 N18 1.381(14) . ? C37 N20 1.316(13) . ? C37 N21 1.350(13) . ? C38 N19 1.312(12) . ? C38 N21 1.333(14) . ? C39 N19 1.459(13) . ? C39 C40 1.493(16) . ? C40 C41 1.395(18) . ? C40 C45 1.398(14) . ? C41 C42 1.366(19) . ? C41 C47 1.508(15) . ? C42 C43 1.381(17) . ? C42 C52 1.44(3) . ? C43 C44 1.415(18) . ? C43 C48 1.521(18) . ? C44 C45 1.408(16) . ? C44 C49 1.500(14) . ? C45 C46 1.514(17) . ? C49 N22 1.466(14) . ? C50 N22 1.300(15) . ? C50 N24 1.302(15) . ? C51 N23 1.311(15) . ? C51 N24 1.356(15) . ? C52 N25 1.55(3) . ? C53 N27 1.33(3) . ? C53 N25 1.52(3) . ? C54 N26 1.32(3) . ? C54 N27 1.51(3) . ? N4 N5 1.345(13) . ? N7 N8 1.371(12) . ? N10 N11 1.334(13) . ? N13 N14 1.349(13) . ? N16 N17 1.362(13) . ? N19 N20 1.339(12) . ? N22 N23 1.369(13) . ? N24 Cu4 1.900(8) 1_556 ? N26 N25 1.359(16) . ? C1 N1 1.264(16) . ? C1 N3 1.27(3) . ? C2 N2 1.314(18) . ? C2 N3 1.336(18) . ? N1 N2 1.322(17) . ? N3 Cu1 1.92(2) 1_655 ? C2' N2' 1.30(4) . ? C2' N3' 1.43(5) . ? N1' N2' 1.41(4) . ? N3' Cu1 1.90(3) 1_655 ? 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 N9 Cu1 N3' 155.1(16) . 1_455 ? N9 Cu1 N3 174.9(9) . 1_455 ? N3' Cu1 N3 28.7(13) 1_455 1_455 ? N12 Cu2 N6 176.8(4) . . ? N21 Cu3 N15 173.1(4) . . ? N18 Cu4 N24 165.1(4) . 1_554 ? O13 Mo1 O6 104.4(4) . . ? O13 Mo1 O3 101.8(3) . . ? O6 Mo1 O3 99.4(3) . . ? O13 Mo1 O14 99.2(3) . . ? O6 Mo1 O14 100.2(3) . . ? O3 Mo1 O14 146.6(3) . . ? O13 Mo1 O11 98.7(3) . . ? O6 Mo1 O11 156.8(3) . . ? O3 Mo1 O11 76.7(2) . . ? O14 Mo1 O11 74.6(2) . . ? O13 Mo1 O21 167.6(3) . . ? O6 Mo1 O21 85.3(3) . . ? O3 Mo1 O21 83.9(2) . . ? O14 Mo1 O21 71.0(2) . . ? O11 Mo1 O21 71.59(19) . . ? O13 Mo1 Mo7 88.3(3) . . ? O6 Mo1 Mo7 136.0(3) . . ? O3 Mo1 Mo7 119.4(2) . . ? O14 Mo1 Mo7 35.76(17) . . ? O11 Mo1 Mo7 42.70(14) . . ? O21 Mo1 Mo7 79.32(14) . . ? O2 Mo2 O1 104.4(4) . . ? O2 Mo2 O3 98.7(3) . . ? O1 Mo2 O3 103.8(3) . . ? O2 Mo2 O4 98.9(3) . . ? O1 Mo2 O4 102.4(3) . . ? O3 Mo2 O4 143.5(3) . . ? O2 Mo2 O5 166.6(3) . . ? O1 Mo2 O5 89.0(3) . . ? O3 Mo2 O5 78.3(2) . . ? O4 Mo2 O5 77.2(2) . . ? O2 Mo2 O11 97.3(3) . . ? O1 Mo2 O11 158.3(3) . . ? O3 Mo2 O11 72.6(2) . . ? O4 Mo2 O11 73.6(2) . . ? O5 Mo2 O11 69.31(19) . . ? O19 Mo3 O5 104.7(3) . . ? O19 Mo3 O21 101.5(3) . . ? O5 Mo3 O21 97.5(3) . . ? O19 Mo3 O10 100.8(3) . . ? O5 Mo3 O10 97.5(3) . . ? O21 Mo3 O10 149.0(2) . . ? O19 Mo3 O20 100.3(3) . . ? O5 Mo3 O20 155.0(2) . . ? O21 Mo3 O20 77.5(2) . . ? O10 Mo3 O20 77.5(2) . . ? O19 Mo3 O11 175.4(3) . . ? O5 Mo3 O11 79.9(2) . . ? O21 Mo3 O11 78.1(2) . . ? O10 Mo3 O11 77.9(2) . . ? O20 Mo3 O11 75.11(19) . . ? O19 Mo3 Mo6 90.1(2) . . ? O5 Mo3 Mo6 133.8(2) . . ? O21 Mo3 Mo6 36.34(18) . . ? O10 Mo3 Mo6 122.77(18) . . ? O20 Mo3 Mo6 45.29(16) . . ? O11 Mo3 Mo6 86.89(13) . . ? O19 Mo3 Mo5 90.4(2) . . ? O5 Mo3 Mo5 133.4(2) . . ? O21 Mo3 Mo5 122.80(18) . . ? O10 Mo3 Mo5 35.88(18) . . ? O20 Mo3 Mo5 45.33(16) . . ? O11 Mo3 Mo5 85.97(14) . . ? Mo6 Mo3 Mo5 88.89(3) . . ? O7 Mo4 O8 104.4(3) . . ? O7 Mo4 O4 102.0(3) . . ? O8 Mo4 O4 99.8(3) . . ? O7 Mo4 O9 97.0(3) . . ? O8 Mo4 O9 102.8(3) . . ? O4 Mo4 O9 145.7(2) . . ? O7 Mo4 O11 96.4(3) . . ? O8 Mo4 O11 159.2(3) . . ? O4 Mo4 O11 76.5(2) . . ? O9 Mo4 O11 73.2(2) . . ? O7 Mo4 O10 165.4(3) . . ? O8 Mo4 O10 87.5(3) . . ? O4 Mo4 O10 83.9(2) . . ? O9 Mo4 O10 71.8(2) . . ? O11 Mo4 O10 71.79(19) . . ? O17 Mo5 O18 104.7(4) . . ? O17 Mo5 O26 100.4(3) . . ? O18 Mo5 O26 101.1(3) . . ? O17 Mo5 O10 98.3(3) . . ? O18 Mo5 O10 98.7(3) . . ? O26 Mo5 O10 148.1(2) . . ? O17 Mo5 O20 158.1(3) . . ? O18 Mo5 O20 96.9(3) . . ? O26 Mo5 O20 79.0(2) . . ? O10 Mo5 O20 74.1(2) . . ? O17 Mo5 O9 85.6(3) . . ? O18 Mo5 O9 167.3(3) . . ? O26 Mo5 O9 84.0(2) . . ? O10 Mo5 O9 72.0(2) . . ? O20 Mo5 O9 72.47(19) . . ? O17 Mo5 Mo3 133.5(3) . . ? O18 Mo5 Mo3 87.5(2) . . ? O26 Mo5 Mo3 121.38(19) . . ? O10 Mo5 Mo3 35.19(17) . . ? O20 Mo5 Mo3 42.42(15) . . ? O9 Mo5 Mo3 79.94(14) . . ? O23 Mo6 O22 103.7(4) . . ? O23 Mo6 O16 101.7(3) . . ? O22 Mo6 O16 99.5(3) . . ? O23 Mo6 O21 99.0(3) . . ? O22 Mo6 O21 100.1(3) . . ? O16 Mo6 O21 147.1(2) . . ? O23 Mo6 O20 96.7(3) . . ? O22 Mo6 O20 159.5(3) . . ? O16 Mo6 O20 78.3(2) . . ? O21 Mo6 O20 74.1(2) . . ? O23 Mo6 O14 165.8(3) . . ? O22 Mo6 O14 88.4(3) . . ? O16 Mo6 O14 83.4(2) . . ? O21 Mo6 O14 71.1(2) . . ? O20 Mo6 O14 71.12(19) . . ? O23 Mo6 Mo3 86.8(2) . . ? O22 Mo6 Mo3 135.4(2) . . ? O16 Mo6 Mo3 121.00(19) . . ? O21 Mo6 Mo3 35.32(17) . . ? O20 Mo6 Mo3 42.73(15) . . ? O14 Mo6 Mo3 79.26(14) . . ? O12 Mo7 O15 103.9(3) . . ? O12 Mo7 O9 101.8(3) . . ? O15 Mo7 O9 96.9(3) . . ? O12 Mo7 O14 101.7(3) . . ? O15 Mo7 O14 96.0(3) . . ? O9 Mo7 O14 149.5(2) . . ? O12 Mo7 O11 99.2(3) . . ? O15 Mo7 O11 156.9(2) . . ? O9 Mo7 O11 79.1(2) . . ? O14 Mo7 O11 78.3(2) . . ? O12 Mo7 O20 174.8(3) . . ? O15 Mo7 O20 81.3(2) . . ? O9 Mo7 O20 77.7(2) . . ? O14 Mo7 O20 77.2(2) . . ? O11 Mo7 O20 75.55(19) . . ? O12 Mo7 Mo1 89.8(2) . . ? O15 Mo7 Mo1 132.3(2) . . ? O9 Mo7 Mo1 125.07(18) . . ? O14 Mo7 Mo1 36.35(18) . . ? O11 Mo7 Mo1 46.00(15) . . ? O20 Mo7 Mo1 86.34(14) . . ? O24 Mo8 O25 104.9(4) . . ? O24 Mo8 O16 98.2(3) . . ? O25 Mo8 O16 105.1(4) . . ? O24 Mo8 O26 97.0(3) . . ? O25 Mo8 O26 106.0(3) . . ? O16 Mo8 O26 140.4(3) . . ? O24 Mo8 O15 167.7(4) . . ? O25 Mo8 O15 87.4(3) . . ? O16 Mo8 O15 78.9(2) . . ? O26 Mo8 O15 78.5(2) . . ? N1 C3 N1' 31.5(11) . . ? N1 C3 C4 106.4(11) . . ? N1' C3 C4 115.4(14) . . ? C5 C4 C9 119.9(9) . . ? C5 C4 C3 118.9(10) . . ? C9 C4 C3 121.1(9) . . ? C6 C5 C4 118.9(10) . . ? C6 C5 C11 120.7(11) . . ? C4 C5 C11 120.2(10) . . ? C7 C6 C5 121.7(9) . . ? C7 C6 C16 119.1(9) . . ? C5 C6 C16 119.1(9) . . ? C6 C7 C8 119.2(9) . . ? C6 C7 C12 121.2(9) . . ? C8 C7 C12 119.5(8) . . ? C7 C8 C9 120.1(9) . . ? C7 C8 C13 120.0(9) . . ? C9 C8 C13 119.9(9) . . ? C8 C9 C4 119.9(9) . . ? C8 C9 C10 119.8(9) . . ? C4 C9 C10 120.2(9) . . ? N4 C13 C8 115.2(9) . . ? N6 C14 N4 108.7(10) . . ? N5 C15 N6 111.9(10) . . ? N7 C16 C6 110.0(8) . . ? N7 C17 N9 109.6(10) . . ? N8 C18 N9 115.8(11) . . ? N11 C19 N12 114.2(11) . . ? N12 C20 N10 111.2(9) . . ? N10 C21 C22 111.8(8) . . ? C27 C22 C23 120.6(9) . . ? C27 C22 C21 119.2(10) . . ? C23 C22 C21 120.1(10) . . ? C24 C23 C22 119.8(10) . . ? C24 C23 C29 119.9(11) . . ? C22 C23 C29 120.3(10) . . ? C23 C24 C25 120.4(10) . . ? C23 C24 C34 118.8(11) . . ? C25 C24 C34 120.8(11) . . ? C26 C25 C24 118.6(10) . . ? C26 C25 C30 121.3(11) . . ? C24 C25 C30 120.2(11) . . ? C25 C26 C27 121.2(9) . . ? C25 C26 C31 120.0(10) . . ? C27 C26 C31 118.7(10) . . ? C22 C27 C26 119.2(9) . . ? C22 C27 C28 120.6(10) . . ? C26 C27 C28 120.3(10) . . ? N13 C31 C26 111.4(8) . . ? N13 C32 N15 109.7(9) . . ? N14 C33 N15 114.2(9) . . ? N16 C34 C24 112.0(8) . . ? N18 C35 N16 109.4(9) . . ? N17 C36 N18 112.2(10) . . ? N20 C37 N21 113.8(10) . . ? N19 C38 N21 109.7(9) . . ? N19 C39 C40 114.7(10) . . ? C41 C40 C45 121.6(11) . . ? C41 C40 C39 118.2(10) . . ? C45 C40 C39 120.2(11) . . ? C42 C41 C40 118.2(10) . . ? C42 C41 C47 120.5(13) . . ? C40 C41 C47 121.3(12) . . ? C41 C42 C43 123.3(12) . . ? C41 C42 C52 118.3(15) . . ? C43 C42 C52 118.4(16) . . ? C42 C43 C44 118.3(11) . . ? C42 C43 C48 120.3(13) . . ? C44 C43 C48 121.5(11) . . ? C45 C44 C43 120.0(10) . . ? C45 C44 C49 120.2(11) . . ? C43 C44 C49 119.8(11) . . ? C40 C45 C44 118.5(11) . . ? C40 C45 C46 121.4(11) . . ? C44 C45 C46 120.1(10) . . ? N22 C49 C44 113.6(9) . . ? N22 C50 N24 110.9(11) . . ? N23 C51 N24 112.8(11) . . ? C42 C52 N25 115(2) . . ? N27 C53 N25 107(2) . . ? N26 C54 N27 106(2) . . ? C14 N4 N5 111.0(9) . . ? C14 N4 C13 126.0(9) . . ? N5 N4 C13 122.7(8) . . ? C15 N5 N4 103.0(9) . . ? C14 N6 C15 105.4(9) . . ? C14 N6 Cu2 123.8(7) . . ? C15 N6 Cu2 130.1(8) . . ? C17 N7 N8 110.5(10) . . ? C17 N7 C16 129.7(9) . . ? N8 N7 C16 119.7(9) . . ? C18 N8 N7 101.8(9) . . ? C17 N9 C18 102.2(10) . . ? C17 N9 Cu1 128.2(8) . . ? C18 N9 Cu1 128.3(9) . . ? C20 N10 N11 109.4(9) . . ? C20 N10 C21 132.7(9) . . ? N11 N10 C21 117.7(8) . . ? C19 N11 N10 103.0(9) . . ? C20 N12 C19 101.9(9) . . ? C20 N12 Cu2 132.4(7) . . ? C19 N12 Cu2 125.6(8) . . ? C32 N13 N14 110.4(8) . . ? C32 N13 C31 128.2(9) . . ? N14 N13 C31 121.4(8) . . ? C33 N14 N13 102.3(9) . . ? C32 N15 C33 103.4(8) . . ? C32 N15 Cu3 131.2(7) . . ? C33 N15 Cu3 125.1(7) . . ? C35 N16 N17 110.5(8) . . ? C35 N16 C34 130.3(9) . . ? N17 N16 C34 119.3(8) . . ? C36 N17 N16 103.6(9) . . ? C35 N18 C36 104.3(8) . . ? C35 N18 Cu4 129.3(7) . . ? C36 N18 Cu4 126.0(7) . . ? C38 N19 N20 110.6(9) . . ? C38 N19 C39 127.6(9) . . ? N20 N19 C39 121.7(8) . . ? C37 N20 N19 103.0(8) . . ? C38 N21 C37 102.9(8) . . ? C38 N21 Cu3 128.4(7) . . ? C37 N21 Cu3 128.5(8) . . ? C50 N22 N23 109.4(9) . . ? C50 N22 C49 128.4(10) . . ? N23 N22 C49 121.6(9) . . ? C51 N23 N22 102.9(9) . . ? C50 N24 C51 104.0(10) . . ? C50 N24 Cu4 124.4(8) . 1_556 ? C51 N24 Cu4 127.2(8) . 1_556 ? C53 N27 C54 107(2) . . ? C54 N26 N25 114(2) . . ? N26 N25 C53 104(2) . . ? N26 N25 C52 128(2) . . ? C53 N25 C52 127(2) . . ? Mo2 O3 Mo1 118.4(3) . . ? Mo3 O21 Mo6 108.3(3) . . ? Mo3 O21 Mo1 108.7(2) . . ? Mo6 O21 Mo1 105.2(2) . . ? Mo8 O26 Mo5 120.4(3) . . ? Mo3 O10 Mo5 108.9(3) . . ? Mo3 O10 Mo4 110.8(3) . . ? Mo5 O10 Mo4 104.4(2) . . ? Mo3 O5 Mo2 119.1(3) . . ? Mo7 O15 Mo8 121.3(3) . . ? Mo4 O4 Mo2 118.9(3) . . ? Mo7 O9 Mo4 109.9(3) . . ? Mo7 O9 Mo5 109.1(2) . . ? Mo4 O9 Mo5 103.5(2) . . ? Mo7 O11 Mo1 91.3(2) . . ? Mo7 O11 Mo4 91.4(2) . . ? Mo1 O11 Mo4 163.3(2) . . ? Mo7 O11 Mo3 104.4(2) . . ? Mo1 O11 Mo3 98.9(2) . . ? Mo4 O11 Mo3 96.4(2) . . ? Mo7 O11 Mo2 163.8(3) . . ? Mo1 O11 Mo2 87.34(19) . . ? Mo4 O11 Mo2 85.55(18) . . ? Mo3 O11 Mo2 91.66(19) . . ? Mo3 O20 Mo6 92.0(2) . . ? Mo3 O20 Mo5 92.3(2) . . ? Mo6 O20 Mo5 159.7(3) . . ? Mo3 O20 Mo7 104.9(2) . . ? Mo6 O20 Mo7 100.2(2) . . ? Mo5 O20 Mo7 97.9(2) . . ? Mo7 O14 Mo1 107.9(3) . . ? Mo7 O14 Mo6 108.8(2) . . ? Mo1 O14 Mo6 105.8(3) . . ? Mo8 O16 Mo6 120.9(3) . . ? N1 C1 N3 116.3(15) . . ? N2 C2 N3 107.4(19) . . ? C1 N1 N2 103.3(18) . . ? C1 N1 C3 129.2(16) . . ? N2 N1 C3 127.5(17) . . ? C2 N2 N1 109.3(19) . . ? C1 N3 C2 103.6(18) . . ? C1 N3 Cu1 132.7(15) . 1_655 ? C2 N3 Cu1 122.5(19) . 1_655 ? N2' C2' N3' 111(3) . . ? N2' N1' C3 126(3) . . ? C2' N2' N1' 106(3) . . ? C2' N3' Cu1 131(3) . 1_655 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 67.35 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.303 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.150 #=================================================================================end data_4 _database_code_depnum_ccdc_archive 'CCDC 789621' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H56 Mo8 N18 Ni2 O34' _chemical_formula_sum 'C36 H56 Mo8 N18 Ni2 O34' _chemical_formula_weight 2169.93 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' Ni Ni 0.3393 1.1124 '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 'P 21/n' _symmetry_space_group_name_hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4938(5) _cell_length_b 16.1953(5) _cell_length_c 15.3550(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.354(5) _cell_angle_gamma 90.00 _cell_volume 3202.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7444 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 29.2 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 2.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.67 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14493 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.1346 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 29.20 _reflns_number_total 7444 _reflns_number_gt 3794 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7444 _refine_ls_number_parameters 473 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0448 _refine_ls_wR_factor_gt 0.0418 _refine_ls_goodness_of_fit_ref 0.729 _refine_ls_restrained_S_all 0.729 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4994(4) 0.1975(3) 1.1706(4) 0.0508(15) Uani 1 1 d . . . H1 H 0.4275 0.1923 1.1530 0.061 Uiso 1 1 calc R . . C2 C 0.6579(3) 0.2116(3) 1.2585(3) 0.0325(12) Uani 1 1 d . . . H2 H 0.7156 0.2182 1.3094 0.039 Uiso 1 1 calc R . . C3 C 0.5273(4) 0.2059(3) 1.3395(3) 0.0404(13) Uani 1 1 d . . . H3A H 0.4848 0.2540 1.3402 0.048 Uiso 1 1 calc R . . H3B H 0.5892 0.2098 1.3916 0.048 Uiso 1 1 calc R . . C4 C 0.4678(3) 0.1292(2) 1.3490(3) 0.0287(11) Uani 1 1 d . . . C5 C 0.5219(3) 0.0546(3) 1.3680(3) 0.0296(11) Uani 1 1 d . . . C6 C 0.4678(3) -0.0176(2) 1.3747(3) 0.0277(11) Uani 1 1 d . . . C7 C 0.3614(3) -0.0159(2) 1.3641(3) 0.0326(12) Uani 1 1 d . . . C8 C 0.3082(3) 0.0605(3) 1.3457(3) 0.0297(11) Uani 1 1 d . . . C9 C 0.3610(3) 0.1318(2) 1.3349(3) 0.0289(11) Uani 1 1 d . . . C10 C 0.3030(4) 0.2130(2) 1.3089(4) 0.0512(15) Uani 1 1 d . . . H10A H 0.2919 0.2375 1.3622 0.077 Uiso 1 1 calc R . . H10B H 0.2372 0.2028 1.2643 0.077 Uiso 1 1 calc R . . H10C H 0.3432 0.2498 1.2839 0.077 Uiso 1 1 calc R . . C11 C 0.6370(3) 0.0509(3) 1.3774(4) 0.0496(15) Uani 1 1 d . . . H11A H 0.6709 0.0143 1.4264 0.074 Uiso 1 1 calc R . . H11B H 0.6664 0.1051 1.3901 0.074 Uiso 1 1 calc R . . H11C H 0.6464 0.0309 1.3215 0.074 Uiso 1 1 calc R . . C12 C 0.5267(3) -0.0986(2) 1.3889(3) 0.0369(12) Uani 1 1 d . . . H12A H 0.5915 -0.0920 1.4373 0.044 Uiso 1 1 calc R . . H12B H 0.4861 -0.1405 1.4079 0.044 Uiso 1 1 calc R . . C13 C 0.6285(4) -0.1789(3) 1.2231(4) 0.0535(16) Uani 1 1 d . . . H13 H 0.6804 -0.2038 1.2037 0.064 Uiso 1 1 calc R . . C14 C 0.4870(3) -0.1277(3) 1.2203(3) 0.0375(12) Uani 1 1 d . . . H14 H 0.4193 -0.1077 1.2009 0.045 Uiso 1 1 calc R . . C15 C 0.3038(3) -0.0950(2) 1.3687(4) 0.0518(15) Uani 1 1 d . . . H15A H 0.2400 -0.0961 1.3198 0.078 Uiso 1 1 calc R . . H15B H 0.2890 -0.0978 1.4261 0.078 Uiso 1 1 calc R . . H15C H 0.3459 -0.1414 1.3633 0.078 Uiso 1 1 calc R . . C16 C 0.1928(3) 0.0638(3) 1.3313(3) 0.0360(12) Uani 1 1 d . . . H16A H 0.1597 0.0851 1.2705 0.043 Uiso 1 1 calc R . . H16B H 0.1680 0.0078 1.3333 0.043 Uiso 1 1 calc R . . C17 C 0.1424(4) 0.1495(3) 1.5194(4) 0.0616(17) Uani 1 1 d . . . H17 H 0.1476 0.1513 1.5811 0.074 Uiso 1 1 calc R . . C18 C 0.1027(3) 0.1797(3) 1.3824(4) 0.0425(14) Uani 1 1 d . . . H18 H 0.0752 0.2051 1.3260 0.051 Uiso 1 1 calc R . . N1 N 0.5554(3) 0.1966(2) 1.1133(3) 0.0482(11) Uani 1 1 d . . . N2 N 0.6555(4) 0.2053(3) 1.1727(4) 0.0843(17) Uani 1 1 d . . . N3 N 0.5577(3) 0.2065(2) 1.2558(3) 0.0418(11) Uani 1 1 d . . . N4 N 0.5484(3) -0.1256(2) 1.3068(3) 0.0353(10) Uani 1 1 d . . . N5 N 0.6421(3) -0.1582(3) 1.3081(3) 0.0549(13) Uani 1 1 d . . . N6 N 0.5352(3) -0.1619(2) 1.1662(3) 0.0365(10) Uani 1 1 d . . . N7 N 0.1595(3) 0.1122(2) 1.3943(3) 0.0356(10) Uani 1 1 d . . . N8 N 0.1851(3) 0.0921(3) 1.4835(3) 0.0613(14) Uani 1 1 d . . . N9 N 0.0887(3) 0.2074(2) 1.4576(3) 0.0353(10) Uani 1 1 d . . . O1 O 0.7460(2) 0.01106(18) 1.1391(2) 0.0504(10) Uani 1 1 d . . . O2 O 0.8809(3) -0.0679(2) 1.2800(2) 0.0613(10) Uani 1 1 d . . . O3 O 1.0334(2) -0.07256(16) 1.1860(2) 0.0344(8) Uani 1 1 d . . . O4 O 0.8404(2) -0.12440(16) 1.0964(2) 0.0359(8) Uani 1 1 d . . . O5 O 0.9445(2) 0.07210(16) 1.2004(2) 0.0365(8) Uani 1 1 d . . . O6 O 1.0345(2) 0.21335(16) 1.1606(2) 0.0366(8) Uani 1 1 d . . . O7 O 0.8382(2) 0.17808(17) 1.0593(2) 0.0417(9) Uani 1 1 d . . . O8 O 0.91687(18) 0.00907(15) 1.0356(2) 0.0237(7) Uani 1 1 d . . . O9 O 0.79602(19) 0.09362(15) 0.8713(2) 0.0350(8) Uani 1 1 d . . . O10 O 0.99482(19) 0.14009(14) 0.9842(2) 0.0265(7) Uani 1 1 d . . . O11 O 0.88765(18) -0.06332(15) 0.87945(18) 0.0247(7) Uani 1 1 d . . . O12 O 0.8037(2) -0.21004(17) 0.9351(2) 0.0500(10) Uani 1 1 d . . . O13 O 0.7093(2) -0.06411(18) 0.9332(2) 0.0438(9) Uani 1 1 d . . . Ni1 Ni 0.51281(4) 0.18508(3) 0.97291(5) 0.03673(17) Uani 1 1 d . . . Mo1 Mo 0.95889(3) 0.13645(2) 1.10163(3) 0.02884(11) Uani 1 1 d . . . Mo2 Mo 0.91668(3) 0.05381(2) 0.90463(3) 0.02431(10) Uani 1 1 d . . . Mo3 Mo 0.82821(3) -0.11151(2) 0.97141(3) 0.03086(11) Uani 1 1 d . . . Mo4 Mo 0.86871(3) -0.02960(2) 1.17527(3) 0.03754(12) Uani 1 1 d . . . O4W O 0.4214(6) 0.4027(6) 1.0561(9) 0.117(7) Uani 0.518(12) 1 d P A 1 O4W' O 0.3926(8) 0.4212(7) 0.9244(15) 0.191(11) Uani 0.482(12) 1 d P A 2 O1W O 0.3767(3) 0.2521(2) 0.9651(3) 0.0578(11) Uani 1 1 d D . . O2W O 0.6429(2) 0.1130(2) 0.9820(2) 0.0499(10) Uani 1 1 d D . . O3W O 0.4383(3) 0.0744(2) 0.9855(3) 0.0611(12) Uani 1 1 d D . . H1A H 0.387(4) 0.3026(16) 0.953(4) 0.092 Uiso 1 1 d D . . H1B H 0.325(3) 0.225(3) 0.937(4) 0.092 Uiso 1 1 d D . . H2B H 0.694(3) 0.143(3) 0.995(3) 0.092 Uiso 1 1 d D . . H2A H 0.621(4) 0.104(3) 0.9263(15) 0.092 Uiso 1 1 d D . . H4B H 0.387(3) 0.065(3) 1.007(4) 0.092 Uiso 1 1 d D . . H4A H 0.471(4) 0.054(3) 0.952(3) 0.092 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(3) 0.060(3) 0.055(4) 0.001(3) 0.025(3) -0.010(3) C2 0.019(2) 0.056(3) 0.020(3) -0.002(3) 0.003(2) -0.005(2) C3 0.057(3) 0.032(3) 0.037(3) -0.002(2) 0.021(3) 0.001(2) C4 0.046(3) 0.019(2) 0.026(3) -0.005(2) 0.018(2) -0.007(2) C5 0.031(2) 0.032(3) 0.024(3) -0.004(2) 0.006(2) 0.002(2) C6 0.034(3) 0.024(2) 0.024(3) -0.001(2) 0.008(2) 0.003(2) C7 0.051(3) 0.024(2) 0.021(3) -0.001(2) 0.008(2) -0.002(2) C8 0.034(3) 0.034(3) 0.021(3) -0.004(2) 0.007(2) 0.003(2) C9 0.044(3) 0.020(2) 0.024(3) -0.002(2) 0.011(2) 0.004(2) C10 0.060(3) 0.034(3) 0.066(4) 0.005(3) 0.028(3) 0.015(2) C11 0.040(3) 0.045(3) 0.059(4) 0.004(3) 0.007(3) -0.003(2) C12 0.047(3) 0.034(3) 0.030(3) -0.003(2) 0.010(3) 0.005(2) C13 0.036(3) 0.072(4) 0.048(4) -0.011(3) 0.007(3) 0.018(3) C14 0.033(3) 0.043(3) 0.035(3) 0.000(3) 0.008(3) 0.004(2) C15 0.057(3) 0.034(3) 0.071(4) 0.008(3) 0.028(3) -0.009(2) C16 0.035(3) 0.036(3) 0.034(3) -0.014(3) 0.005(2) 0.000(2) C17 0.077(4) 0.076(4) 0.032(3) -0.001(3) 0.015(3) 0.030(3) C18 0.044(3) 0.047(3) 0.038(4) 0.006(3) 0.013(3) 0.013(3) N1 0.042(3) 0.066(3) 0.038(3) 0.004(2) 0.016(2) -0.010(2) N2 0.076(4) 0.077(4) 0.094(5) 0.009(4) 0.017(4) -0.009(3) N3 0.050(3) 0.042(2) 0.037(3) 0.000(2) 0.018(2) -0.009(2) N4 0.037(2) 0.028(2) 0.040(3) 0.002(2) 0.009(2) 0.0043(18) N5 0.032(2) 0.074(3) 0.053(3) -0.007(3) 0.005(2) 0.014(2) N6 0.028(2) 0.039(2) 0.040(3) -0.007(2) 0.007(2) 0.0009(18) N7 0.038(2) 0.041(2) 0.030(3) 0.000(2) 0.012(2) 0.010(2) N8 0.083(3) 0.062(3) 0.041(3) 0.007(3) 0.022(3) 0.038(3) N9 0.034(2) 0.043(2) 0.031(3) 0.000(2) 0.012(2) 0.0053(19) O1 0.0426(19) 0.049(2) 0.065(3) -0.0072(19) 0.0238(18) 0.0033(16) O2 0.073(2) 0.078(3) 0.045(2) 0.009(2) 0.036(2) -0.003(2) O3 0.0363(17) 0.0344(18) 0.033(2) 0.0065(15) 0.0108(15) 0.0009(14) O4 0.0428(18) 0.0303(17) 0.043(2) 0.0019(16) 0.0260(16) -0.0053(14) O5 0.0401(18) 0.0390(18) 0.035(2) -0.0020(16) 0.0179(16) 0.0000(14) O6 0.0382(17) 0.0278(17) 0.042(2) -0.0103(16) 0.0099(16) 0.0008(14) O7 0.0310(17) 0.0423(19) 0.051(2) -0.0085(18) 0.0115(17) 0.0088(14) O8 0.0226(15) 0.0206(14) 0.0293(18) 0.0016(14) 0.0100(13) 0.0000(12) O9 0.0304(16) 0.0277(16) 0.045(2) 0.0062(15) 0.0075(16) 0.0052(13) O10 0.0296(15) 0.0168(14) 0.0320(19) 0.0019(14) 0.0075(14) -0.0023(12) O11 0.0278(15) 0.0236(15) 0.0232(18) -0.0006(14) 0.0086(13) 0.0001(12) O12 0.053(2) 0.0301(18) 0.071(3) -0.0136(18) 0.0249(19) -0.0182(15) O13 0.0239(16) 0.052(2) 0.057(2) 0.0048(18) 0.0145(16) 0.0007(14) Ni1 0.0304(3) 0.0400(3) 0.0434(4) -0.0001(3) 0.0164(3) -0.0033(3) Mo1 0.0269(2) 0.0264(2) 0.0343(3) -0.0057(2) 0.01081(19) 0.00194(18) Mo2 0.0243(2) 0.0212(2) 0.0272(2) 0.00213(19) 0.00736(18) 0.00200(17) Mo3 0.0262(2) 0.0269(2) 0.0421(3) -0.0016(2) 0.0142(2) -0.00522(17) Mo4 0.0372(2) 0.0424(3) 0.0394(3) 0.0013(2) 0.0211(2) -0.0009(2) O4W 0.055(5) 0.098(8) 0.198(16) -0.084(9) 0.039(7) 0.007(5) O4W' 0.080(7) 0.155(11) 0.34(3) 0.131(13) 0.071(11) 0.069(7) O1W 0.040(2) 0.055(2) 0.082(3) -0.003(2) 0.024(2) 0.0012(19) O2W 0.0272(19) 0.061(2) 0.060(3) -0.007(2) 0.0096(18) -0.0037(16) O3W 0.053(3) 0.052(2) 0.098(4) 0.004(2) 0.051(2) -0.0061(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N3 1.318(6) . ? C1 N1 1.321(6) . ? C1 H1 0.9300 . ? C2 N2 1.313(7) . ? C2 N3 1.343(5) . ? C2 H2 0.9300 . ? C3 N3 1.461(6) . ? C3 C4 1.510(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.392(5) . ? C4 C5 1.397(5) . ? C5 C6 1.398(5) . ? C5 C11 1.518(6) . ? C6 C7 1.396(5) . ? C6 C12 1.515(5) . ? C7 C8 1.415(5) . ? C7 C15 1.512(5) . ? C8 C9 1.393(5) . ? C8 C16 1.508(5) . ? C9 C10 1.521(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.445(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N5 1.306(6) . ? C13 N6 1.330(5) . ? C13 H13 0.9300 . ? C14 N6 1.319(6) . ? C14 N4 1.341(5) . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N7 1.419(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N8 1.299(6) . ? C17 N9 1.376(6) . ? C17 H17 0.9300 . ? C18 N9 1.303(6) . ? C18 N7 1.316(5) . ? C18 H18 0.9300 . ? N1 N2 1.393(6) . ? N1 Ni1 2.067(4) . ? N4 N5 1.364(5) . ? N6 Ni1 2.074(4) 3_657 ? N7 N8 1.348(5) . ? N9 Ni1 2.069(4) 4_566 ? O1 Mo4 1.714(3) . ? O2 Mo4 1.685(4) . ? O3 Mo2 1.744(3) 3_757 ? O3 Mo4 2.287(3) . ? O4 Mo3 1.888(3) . ? O4 Mo4 1.922(3) . ? O5 Mo1 1.898(3) . ? O5 Mo4 1.916(3) . ? O6 Mo1 1.692(3) . ? O7 Mo1 1.702(3) . ? O8 Mo2 2.137(3) . ? O8 Mo1 2.294(2) . ? O8 Mo3 2.348(2) . ? O8 Mo2 2.386(2) 3_757 ? O8 Mo4 2.499(3) . ? O9 Mo2 1.683(2) . ? O10 Mo2 1.946(2) . ? O10 Mo1 2.003(3) . ? O10 Mo3 2.326(2) 3_757 ? O11 Mo2 1.952(2) . ? O11 Mo3 1.980(3) . ? O11 Mo1 2.327(2) 3_757 ? O12 Mo3 1.690(3) . ? O13 Mo3 1.717(3) . ? Ni1 N9 2.069(4) 4_665 ? Ni1 N6 2.074(4) 3_657 ? Ni1 O2W 2.078(4) . ? Ni1 O3W 2.092(4) . ? Ni1 O1W 2.105(3) . ? Mo1 O11 2.327(2) 3_757 ? Mo1 Mo2 3.1997(6) . ? Mo2 O3 1.744(3) 3_757 ? Mo2 O8 2.386(2) 3_757 ? Mo3 O10 2.326(2) 3_757 ? O1W H1A 0.859(19) . ? O1W H1B 0.83(5) . ? O2W H2B 0.82(5) . ? O2W H2A 0.831(19) . ? O3W H4B 0.87(5) . ? O3W H4A 0.84(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 C1 N1 111.8(5) . . ? N3 C1 H1 124.1 . . ? N1 C1 H1 124.1 . . ? N2 C2 N3 103.9(4) . . ? N2 C2 H2 128.0 . . ? N3 C2 H2 128.0 . . ? N3 C3 C4 112.8(4) . . ? N3 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N3 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C9 C4 C5 120.7(4) . . ? C9 C4 C3 121.1(4) . . ? C5 C4 C3 118.2(4) . . ? C4 C5 C6 119.2(4) . . ? C4 C5 C11 120.7(4) . . ? C6 C5 C11 120.1(4) . . ? C7 C6 C5 121.1(4) . . ? C7 C6 C12 120.7(4) . . ? C5 C6 C12 118.1(4) . . ? C6 C7 C8 118.9(4) . . ? C6 C7 C15 120.2(4) . . ? C8 C7 C15 120.8(4) . . ? C9 C8 C7 120.1(4) . . ? C9 C8 C16 119.7(4) . . ? C7 C8 C16 120.1(4) . . ? C4 C9 C8 119.9(4) . . ? C4 C9 C10 119.7(4) . . ? C8 C9 C10 120.4(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C6 111.8(4) . . ? N4 C12 H12A 109.3 . . ? C6 C12 H12A 109.3 . . ? N4 C12 H12B 109.3 . . ? C6 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? N5 C13 N6 115.2(5) . . ? N5 C13 H13 122.4 . . ? N6 C13 H13 122.4 . . ? N6 C14 N4 111.0(4) . . ? N6 C14 H14 124.5 . . ? N4 C14 H14 124.5 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 C8 116.3(3) . . ? N7 C16 H16A 108.2 . . ? C8 C16 H16A 108.2 . . ? N7 C16 H16B 108.2 . . ? C8 C16 H16B 108.2 . . ? H16A C16 H16B 107.4 . . ? N8 C17 N9 113.8(5) . . ? N8 C17 H17 123.1 . . ? N9 C17 H17 123.1 . . ? N9 C18 N7 113.3(5) . . ? N9 C18 H18 123.4 . . ? N7 C18 H18 123.4 . . ? C1 N1 N2 101.4(5) . . ? C1 N1 Ni1 131.3(4) . . ? N2 N1 Ni1 127.3(4) . . ? C2 N2 N1 113.2(5) . . ? C1 N3 C2 109.6(5) . . ? C1 N3 C3 129.1(4) . . ? C2 N3 C3 121.1(4) . . ? C14 N4 N5 107.5(4) . . ? C14 N4 C12 130.2(4) . . ? N5 N4 C12 122.2(4) . . ? C13 N5 N4 103.4(4) . . ? C14 N6 C13 102.8(4) . . ? C14 N6 Ni1 131.6(3) . 3_657 ? C13 N6 Ni1 125.6(4) . 3_657 ? C18 N7 N8 107.7(4) . . ? C18 N7 C16 130.9(4) . . ? N8 N7 C16 121.5(4) . . ? C17 N8 N7 104.3(4) . . ? C18 N9 C17 101.0(4) . . ? C18 N9 Ni1 126.7(3) . 4_566 ? C17 N9 Ni1 132.2(4) . 4_566 ? Mo2 O3 Mo4 119.20(13) 3_757 . ? Mo3 O4 Mo4 119.53(14) . . ? Mo1 O5 Mo4 119.11(15) . . ? Mo2 O8 Mo1 92.39(9) . . ? Mo2 O8 Mo3 91.69(10) . . ? Mo1 O8 Mo3 164.01(12) . . ? Mo2 O8 Mo2 104.08(11) . 3_757 ? Mo1 O8 Mo2 97.68(9) . 3_757 ? Mo3 O8 Mo2 96.30(9) . 3_757 ? Mo2 O8 Mo4 164.79(11) . . ? Mo1 O8 Mo4 86.52(10) . . ? Mo3 O8 Mo4 85.50(8) . . ? Mo2 O8 Mo4 91.09(9) 3_757 . ? Mo2 O10 Mo1 108.23(12) . . ? Mo2 O10 Mo3 110.95(12) . 3_757 ? Mo1 O10 Mo3 103.51(11) . 3_757 ? Mo2 O11 Mo3 109.98(13) . . ? Mo2 O11 Mo1 110.57(11) . 3_757 ? Mo3 O11 Mo1 104.18(10) . 3_757 ? N1 Ni1 N9 92.84(16) . 4_665 ? N1 Ni1 N6 174.29(15) . 3_657 ? N9 Ni1 N6 92.78(16) 4_665 3_657 ? N1 Ni1 O2W 90.78(16) . . ? N9 Ni1 O2W 92.53(14) 4_665 . ? N6 Ni1 O2W 88.02(14) 3_657 . ? N1 Ni1 O3W 88.45(18) . . ? N9 Ni1 O3W 178.12(16) 4_665 . ? N6 Ni1 O3W 85.91(17) 3_657 . ? O2W Ni1 O3W 86.08(14) . . ? N1 Ni1 O1W 88.83(17) . . ? N9 Ni1 O1W 90.70(14) 4_665 . ? N6 Ni1 O1W 92.06(16) 3_657 . ? O2W Ni1 O1W 176.76(14) . . ? O3W Ni1 O1W 90.69(14) . . ? O6 Mo1 O7 105.58(13) . . ? O6 Mo1 O5 99.53(14) . . ? O7 Mo1 O5 102.01(14) . . ? O6 Mo1 O10 101.02(13) . . ? O7 Mo1 O10 96.07(14) . . ? O5 Mo1 O10 147.76(11) . . ? O6 Mo1 O8 158.25(11) . . ? O7 Mo1 O8 96.05(11) . . ? O5 Mo1 O8 77.80(11) . . ? O10 Mo1 O8 73.91(10) . . ? O6 Mo1 O11 86.30(11) . 3_757 ? O7 Mo1 O11 164.48(13) . 3_757 ? O5 Mo1 O11 85.43(11) . 3_757 ? O10 Mo1 O11 71.46(10) . 3_757 ? O8 Mo1 O11 72.00(8) . 3_757 ? O6 Mo1 Mo2 136.30(11) . . ? O7 Mo1 Mo2 85.68(11) . . ? O5 Mo1 Mo2 119.62(8) . . ? O10 Mo1 Mo2 35.29(7) . . ? O8 Mo1 Mo2 41.86(7) . . ? O11 Mo1 Mo2 78.81(7) 3_757 . ? O9 Mo2 O3 105.03(14) . 3_757 ? O9 Mo2 O10 102.12(12) . . ? O3 Mo2 O10 96.32(12) 3_757 . ? O9 Mo2 O11 101.14(11) . . ? O3 Mo2 O11 96.52(12) 3_757 . ? O10 Mo2 O11 149.43(10) . . ? O9 Mo2 O8 98.39(13) . . ? O3 Mo2 O8 156.57(10) 3_757 . ? O10 Mo2 O8 78.71(10) . . ? O11 Mo2 O8 78.51(11) . . ? O9 Mo2 O8 174.20(13) . 3_757 ? O3 Mo2 O8 80.66(11) 3_757 3_757 ? O10 Mo2 O8 78.08(9) . 3_757 ? O11 Mo2 O8 76.80(9) . 3_757 ? O8 Mo2 O8 75.92(11) . 3_757 ? O9 Mo2 Mo1 90.62(11) . . ? O3 Mo2 Mo1 132.78(9) 3_757 . ? O10 Mo2 Mo1 36.47(9) . . ? O11 Mo2 Mo1 124.22(8) . . ? O8 Mo2 Mo1 45.75(7) . . ? O8 Mo2 Mo1 86.17(7) 3_757 . ? O12 Mo3 O13 103.79(14) . . ? O12 Mo3 O4 100.36(15) . . ? O13 Mo3 O4 100.73(15) . . ? O12 Mo3 O11 102.59(14) . . ? O13 Mo3 O11 96.67(13) . . ? O4 Mo3 O11 146.85(11) . . ? O12 Mo3 O10 89.51(12) . 3_757 ? O13 Mo3 O10 164.25(12) . 3_757 ? O4 Mo3 O10 84.82(11) . 3_757 ? O11 Mo3 O10 71.85(10) . 3_757 ? O12 Mo3 O8 161.58(12) . . ? O13 Mo3 O8 94.54(11) . . ? O4 Mo3 O8 77.66(10) . . ? O11 Mo3 O8 73.00(10) . . ? O10 Mo3 O8 72.09(8) 3_757 . ? O2 Mo4 O1 105.12(17) . . ? O2 Mo4 O5 103.27(15) . . ? O1 Mo4 O5 98.11(12) . . ? O2 Mo4 O4 104.58(15) . . ? O1 Mo4 O4 96.40(13) . . ? O5 Mo4 O4 143.85(13) . . ? O2 Mo4 O3 90.15(14) . . ? O1 Mo4 O3 164.72(15) . . ? O5 Mo4 O3 78.38(10) . . ? O4 Mo4 O3 78.97(11) . . ? O2 Mo4 O8 159.17(13) . . ? O1 Mo4 O8 95.69(13) . . ? O5 Mo4 O8 72.42(11) . . ? O4 Mo4 O8 73.32(10) . . ? O3 Mo4 O8 69.04(9) . . ? Ni1 O1W H1A 108(4) . . ? Ni1 O1W H1B 110(4) . . ? H1A O1W H1B 123(6) . . ? Ni1 O2W H2B 109(4) . . ? Ni1 O2W H2A 90(4) . . ? H2B O2W H2A 112(3) . . ? Ni1 O3W H4B 130(4) . . ? Ni1 O3W H4A 85(4) . . ? H4B O3W H4A 143(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C9 -105.6(5) . . . . ? N3 C3 C4 C5 71.4(5) . . . . ? C9 C4 C5 C6 -1.3(7) . . . . ? C3 C4 C5 C6 -178.3(4) . . . . ? C9 C4 C5 C11 176.1(4) . . . . ? C3 C4 C5 C11 -0.9(6) . . . . ? C4 C5 C6 C7 -1.0(7) . . . . ? C11 C5 C6 C7 -178.4(4) . . . . ? C4 C5 C6 C12 175.9(4) . . . . ? C11 C5 C6 C12 -1.5(6) . . . . ? C5 C6 C7 C8 0.4(7) . . . . ? C12 C6 C7 C8 -176.4(4) . . . . ? C5 C6 C7 C15 178.2(4) . . . . ? C12 C6 C7 C15 1.3(7) . . . . ? C6 C7 C8 C9 2.6(7) . . . . ? C15 C7 C8 C9 -175.2(4) . . . . ? C6 C7 C8 C16 178.2(4) . . . . ? C15 C7 C8 C16 0.5(7) . . . . ? C5 C4 C9 C8 4.3(7) . . . . ? C3 C4 C9 C8 -178.8(4) . . . . ? C5 C4 C9 C10 -176.5(4) . . . . ? C3 C4 C9 C10 0.4(7) . . . . ? C7 C8 C9 C4 -4.9(7) . . . . ? C16 C8 C9 C4 179.4(4) . . . . ? C7 C8 C9 C10 175.9(4) . . . . ? C16 C8 C9 C10 0.2(7) . . . . ? C7 C6 C12 N4 103.4(5) . . . . ? C5 C6 C12 N4 -73.6(5) . . . . ? C9 C8 C16 N7 -65.8(6) . . . . ? C7 C8 C16 N7 118.5(5) . . . . ? N3 C1 N1 N2 0.5(6) . . . . ? N3 C1 N1 Ni1 -179.7(3) . . . . ? N3 C2 N2 N1 0.3(6) . . . . ? C1 N1 N2 C2 -0.5(6) . . . . ? Ni1 N1 N2 C2 179.7(4) . . . . ? N1 C1 N3 C2 -0.4(6) . . . . ? N1 C1 N3 C3 -176.2(4) . . . . ? N2 C2 N3 C1 0.0(6) . . . . ? N2 C2 N3 C3 176.2(4) . . . . ? C4 C3 N3 C1 54.3(7) . . . . ? C4 C3 N3 C2 -121.1(4) . . . . ? N6 C14 N4 N5 1.6(5) . . . . ? N6 C14 N4 C12 -176.0(4) . . . . ? C6 C12 N4 C14 -44.8(6) . . . . ? C6 C12 N4 N5 137.9(4) . . . . ? N6 C13 N5 N4 0.9(6) . . . . ? C14 N4 N5 C13 -1.5(5) . . . . ? C12 N4 N5 C13 176.4(4) . . . . ? N4 C14 N6 C13 -1.1(5) . . . . ? N4 C14 N6 Ni1 179.7(3) . . . 3_657 ? N5 C13 N6 C14 0.1(6) . . . . ? N5 C13 N6 Ni1 179.4(4) . . . 3_657 ? N9 C18 N7 N8 0.7(6) . . . . ? N9 C18 N7 C16 -179.5(4) . . . . ? C8 C16 N7 C18 115.7(5) . . . . ? C8 C16 N7 N8 -64.5(6) . . . . ? N9 C17 N8 N7 0.2(6) . . . . ? C18 N7 N8 C17 -0.5(6) . . . . ? C16 N7 N8 C17 179.7(4) . . . . ? N7 C18 N9 C17 -0.5(5) . . . . ? N7 C18 N9 Ni1 175.9(3) . . . 4_566 ? N8 C17 N9 C18 0.2(6) . . . . ? N8 C17 N9 Ni1 -175.9(3) . . . 4_566 ? C1 N1 Ni1 N9 125.4(5) . . . 4_665 ? N2 N1 Ni1 N9 -54.9(4) . . . 4_665 ? C1 N1 Ni1 O2W -142.0(5) . . . . ? N2 N1 Ni1 O2W 37.7(4) . . . . ? C1 N1 Ni1 O3W -55.9(5) . . . . ? N2 N1 Ni1 O3W 123.7(4) . . . . ? C1 N1 Ni1 O1W 34.8(5) . . . . ? N2 N1 Ni1 O1W -145.5(4) . . . . ? Mo4 O5 Mo1 O6 -177.30(16) . . . . ? Mo4 O5 Mo1 O7 74.39(18) . . . . ? Mo4 O5 Mo1 O10 -48.3(3) . . . . ? Mo4 O5 Mo1 O8 -19.29(13) . . . . ? Mo4 O5 Mo1 O11 -91.83(15) . . . 3_757 ? Mo4 O5 Mo1 Mo2 -17.46(18) . . . . ? Mo2 O10 Mo1 O6 179.13(13) . . . . ? Mo3 O10 Mo1 O6 61.34(12) 3_757 . . . ? Mo2 O10 Mo1 O7 -73.66(14) . . . . ? Mo3 O10 Mo1 O7 168.55(12) 3_757 . . . ? Mo2 O10 Mo1 O5 50.5(2) . . . . ? Mo3 O10 Mo1 O5 -67.3(2) 3_757 . . . ? Mo2 O10 Mo1 O8 20.91(10) . . . . ? Mo3 O10 Mo1 O8 -96.89(10) 3_757 . . . ? Mo2 O10 Mo1 O11 96.87(12) . . . 3_757 ? Mo3 O10 Mo1 O11 -20.93(8) 3_757 . . 3_757 ? Mo3 O10 Mo1 Mo2 -117.80(15) 3_757 . . . ? Mo2 O8 Mo1 O6 -97.3(4) . . . . ? Mo3 O8 Mo1 O6 158.1(4) . . . . ? Mo2 O8 Mo1 O6 7.3(4) 3_757 . . . ? Mo4 O8 Mo1 O6 97.9(4) . . . . ? Mo2 O8 Mo1 O7 76.60(14) . . . . ? Mo3 O8 Mo1 O7 -28.0(5) . . . . ? Mo2 O8 Mo1 O7 -178.84(14) 3_757 . . . ? Mo4 O8 Mo1 O7 -88.21(13) . . . . ? Mo2 O8 Mo1 O5 177.62(12) . . . . ? Mo3 O8 Mo1 O5 73.0(5) . . . . ? Mo2 O8 Mo1 O5 -77.82(11) 3_757 . . . ? Mo4 O8 Mo1 O5 12.81(9) . . . . ? Mo2 O8 Mo1 O10 -18.00(9) . . . . ? Mo3 O8 Mo1 O10 -122.6(5) . . . . ? Mo2 O8 Mo1 O10 86.56(11) 3_757 . . . ? Mo4 O8 Mo1 O10 177.19(10) . . . . ? Mo2 O8 Mo1 O11 -93.27(10) . . . 3_757 ? Mo3 O8 Mo1 O11 162.1(5) . . . 3_757 ? Mo2 O8 Mo1 O11 11.29(9) 3_757 . . 3_757 ? Mo4 O8 Mo1 O11 101.92(9) . . . 3_757 ? Mo3 O8 Mo1 Mo2 -104.6(5) . . . . ? Mo2 O8 Mo1 Mo2 104.56(12) 3_757 . . . ? Mo4 O8 Mo1 Mo2 -164.81(11) . . . . ? Mo1 O10 Mo2 O9 74.23(15) . . . . ? Mo3 O10 Mo2 O9 -172.85(14) 3_757 . . . ? Mo1 O10 Mo2 O3 -178.87(13) . . . 3_757 ? Mo3 O10 Mo2 O3 -65.95(14) 3_757 . . 3_757 ? Mo1 O10 Mo2 O11 -64.5(3) . . . . ? Mo3 O10 Mo2 O11 48.4(3) 3_757 . . . ? Mo1 O10 Mo2 O8 -22.04(10) . . . . ? Mo3 O10 Mo2 O8 90.88(12) 3_757 . . . ? Mo1 O10 Mo2 O8 -99.84(12) . . . 3_757 ? Mo3 O10 Mo2 O8 13.08(12) 3_757 . . 3_757 ? Mo3 O10 Mo2 Mo1 112.92(16) 3_757 . . . ? Mo3 O11 Mo2 O9 -73.70(16) . . . . ? Mo1 O11 Mo2 O9 171.79(14) 3_757 . . . ? Mo3 O11 Mo2 O3 179.53(13) . . . 3_757 ? Mo1 O11 Mo2 O3 65.02(13) 3_757 . . 3_757 ? Mo3 O11 Mo2 O10 65.2(3) . . . . ? Mo1 O11 Mo2 O10 -49.3(3) 3_757 . . . ? Mo3 O11 Mo2 O8 22.72(11) . . . . ? Mo1 O11 Mo2 O8 -91.79(12) 3_757 . . . ? Mo3 O11 Mo2 O8 100.75(13) . . . 3_757 ? Mo1 O11 Mo2 O8 -13.76(11) 3_757 . . 3_757 ? Mo3 O11 Mo2 Mo1 24.77(14) . . . . ? Mo1 O11 Mo2 Mo1 -89.74(12) 3_757 . . . ? Mo1 O8 Mo2 O9 -82.63(11) . . . . ? Mo3 O8 Mo2 O9 81.91(11) . . . . ? Mo2 O8 Mo2 O9 178.84(11) 3_757 . . . ? Mo4 O8 Mo2 O9 2.9(5) . . . . ? Mo1 O8 Mo2 O3 97.9(3) . . . 3_757 ? Mo3 O8 Mo2 O3 -97.6(3) . . . 3_757 ? Mo2 O8 Mo2 O3 -0.7(3) 3_757 . . 3_757 ? Mo4 O8 Mo2 O3 -176.6(4) . . . 3_757 ? Mo1 O8 Mo2 O10 18.15(9) . . . . ? Mo3 O8 Mo2 O10 -177.31(11) . . . . ? Mo2 O8 Mo2 O10 -80.38(10) 3_757 . . . ? Mo4 O8 Mo2 O10 103.7(5) . . . . ? Mo1 O8 Mo2 O11 177.63(10) . . . . ? Mo3 O8 Mo2 O11 -17.83(9) . . . . ? Mo2 O8 Mo2 O11 79.10(11) 3_757 . . . ? Mo4 O8 Mo2 O11 -96.8(5) . . . . ? Mo1 O8 Mo2 O8 98.53(10) . . . 3_757 ? Mo3 O8 Mo2 O8 -96.93(11) . . . 3_757 ? Mo2 O8 Mo2 O8 0.0 3_757 . . 3_757 ? Mo4 O8 Mo2 O8 -175.9(5) . . . 3_757 ? Mo3 O8 Mo2 Mo1 164.54(12) . . . . ? Mo2 O8 Mo2 Mo1 -98.53(10) 3_757 . . . ? Mo4 O8 Mo2 Mo1 85.5(5) . . . . ? O6 Mo1 Mo2 O9 -111.01(16) . . . . ? O7 Mo1 Mo2 O9 -2.91(14) . . . . ? O5 Mo1 Mo2 O9 98.46(13) . . . . ? O10 Mo1 Mo2 O9 -109.78(15) . . . . ? O8 Mo1 Mo2 O9 101.14(13) . . . . ? O11 Mo1 Mo2 O9 176.58(12) 3_757 . . . ? O6 Mo1 Mo2 O3 0.30(17) . . . 3_757 ? O7 Mo1 Mo2 O3 108.41(15) . . . 3_757 ? O5 Mo1 Mo2 O3 -150.23(15) . . . 3_757 ? O10 Mo1 Mo2 O3 1.53(17) . . . 3_757 ? O8 Mo1 Mo2 O3 -147.55(14) . . . 3_757 ? O11 Mo1 Mo2 O3 -72.11(13) 3_757 . . 3_757 ? O6 Mo1 Mo2 O10 -1.23(18) . . . . ? O7 Mo1 Mo2 O10 106.88(16) . . . . ? O5 Mo1 Mo2 O10 -151.76(15) . . . . ? O8 Mo1 Mo2 O10 -149.08(14) . . . . ? O11 Mo1 Mo2 O10 -73.64(14) 3_757 . . . ? O6 Mo1 Mo2 O11 145.04(16) . . . . ? O7 Mo1 Mo2 O11 -106.86(14) . . . . ? O5 Mo1 Mo2 O11 -5.49(13) . . . . ? O10 Mo1 Mo2 O11 146.27(14) . . . . ? O8 Mo1 Mo2 O11 -2.81(12) . . . . ? O11 Mo1 Mo2 O11 72.63(13) 3_757 . . . ? O6 Mo1 Mo2 O8 147.85(15) . . . . ? O7 Mo1 Mo2 O8 -104.04(14) . . . . ? O5 Mo1 Mo2 O8 -2.68(13) . . . . ? O10 Mo1 Mo2 O8 149.08(14) . . . . ? O11 Mo1 Mo2 O8 75.44(11) 3_757 . . . ? O6 Mo1 Mo2 O8 73.83(14) . . . 3_757 ? O7 Mo1 Mo2 O8 -178.06(12) . . . 3_757 ? O5 Mo1 Mo2 O8 -76.70(11) . . . 3_757 ? O10 Mo1 Mo2 O8 75.06(13) . . . 3_757 ? O8 Mo1 Mo2 O8 -74.02(12) . . . 3_757 ? O11 Mo1 Mo2 O8 1.42(9) 3_757 . . 3_757 ? Mo4 O4 Mo3 O12 -179.79(16) . . . . ? Mo4 O4 Mo3 O13 -73.45(18) . . . . ? Mo4 O4 Mo3 O11 47.0(3) . . . . ? Mo4 O4 Mo3 O10 91.66(15) . . . 3_757 ? Mo4 O4 Mo3 O8 18.89(13) . . . . ? Mo2 O11 Mo3 O12 177.39(14) . . . . ? Mo1 O11 Mo3 O12 -64.09(13) 3_757 . . . ? Mo2 O11 Mo3 O13 71.61(14) . . . . ? Mo1 O11 Mo3 O13 -169.87(13) 3_757 . . . ? Mo2 O11 Mo3 O4 -49.8(2) . . . . ? Mo1 O11 Mo3 O4 68.7(2) 3_757 . . . ? Mo2 O11 Mo3 O10 -97.33(12) . . . 3_757 ? Mo1 O11 Mo3 O10 21.19(9) 3_757 . . 3_757 ? Mo2 O11 Mo3 O8 -21.11(10) . . . . ? Mo1 O11 Mo3 O8 97.41(10) 3_757 . . . ? Mo2 O8 Mo3 O12 96.7(5) . . . . ? Mo1 O8 Mo3 O12 -158.6(5) . . . . ? Mo2 O8 Mo3 O12 -7.7(5) 3_757 . . . ? Mo4 O8 Mo3 O12 -98.3(5) . . . . ? Mo2 O8 Mo3 O13 -77.58(14) . . . . ? Mo1 O8 Mo3 O13 27.2(5) . . . . ? Mo2 O8 Mo3 O13 178.05(14) 3_757 . . . ? Mo4 O8 Mo3 O13 87.45(13) . . . . ? Mo2 O8 Mo3 O4 -177.59(12) . . . . ? Mo1 O8 Mo3 O4 -72.8(5) . . . . ? Mo2 O8 Mo3 O4 78.04(12) 3_757 . . . ? Mo4 O8 Mo3 O4 -12.55(9) . . . . ? Mo2 O8 Mo3 O11 18.02(9) . . . . ? Mo1 O8 Mo3 O11 122.8(5) . . . . ? Mo2 O8 Mo3 O11 -86.35(11) 3_757 . . . ? Mo4 O8 Mo3 O11 -176.95(10) . . . . ? Mo2 O8 Mo3 O10 93.92(11) . . . 3_757 ? Mo1 O8 Mo3 O10 -161.3(5) . . . 3_757 ? Mo2 O8 Mo3 O10 -10.45(10) 3_757 . . 3_757 ? Mo4 O8 Mo3 O10 -101.04(9) . . . 3_757 ? Mo1 O5 Mo4 O2 176.95(18) . . . . ? Mo1 O5 Mo4 O1 -75.33(19) . . . . ? Mo1 O5 Mo4 O4 37.4(3) . . . . ? Mo1 O5 Mo4 O3 89.58(16) . . . . ? Mo1 O5 Mo4 O8 18.11(13) . . . . ? Mo3 O4 Mo4 O2 -176.54(18) . . . . ? Mo3 O4 Mo4 O1 75.98(19) . . . . ? Mo3 O4 Mo4 O5 -37.2(3) . . . . ? Mo3 O4 Mo4 O3 -89.29(16) . . . . ? Mo3 O4 Mo4 O8 -18.07(13) . . . . ? Mo2 O3 Mo4 O2 -179.97(18) 3_757 . . . ? Mo2 O3 Mo4 O1 1.6(5) 3_757 . . . ? Mo2 O3 Mo4 O5 -76.45(16) 3_757 . . . ? Mo2 O3 Mo4 O4 75.20(16) 3_757 . . . ? Mo2 O3 Mo4 O8 -1.01(13) 3_757 . . . ? Mo2 O8 Mo4 O2 179.6(5) . . . . ? Mo1 O8 Mo4 O2 -94.1(4) . . . . ? Mo3 O8 Mo4 O2 99.8(4) . . . . ? Mo2 O8 Mo4 O2 3.6(4) 3_757 . . . ? Mo2 O8 Mo4 O1 -2.6(5) . . . . ? Mo1 O8 Mo4 O1 83.72(12) . . . . ? Mo3 O8 Mo4 O1 -82.42(11) . . . . ? Mo2 O8 Mo4 O1 -178.66(11) 3_757 . . . ? Mo2 O8 Mo4 O5 -99.3(5) . . . . ? Mo1 O8 Mo4 O5 -13.01(9) . . . . ? Mo3 O8 Mo4 O5 -179.14(11) . . . . ? Mo2 O8 Mo4 O5 84.62(10) 3_757 . . . ? Mo2 O8 Mo4 O4 92.4(5) . . . . ? Mo1 O8 Mo4 O4 178.71(12) . . . . ? Mo3 O8 Mo4 O4 12.58(9) . . . . ? Mo2 O8 Mo4 O4 -83.66(10) 3_757 . . . ? Mo2 O8 Mo4 O3 176.7(5) . . . . ? Mo1 O8 Mo4 O3 -96.98(9) . . . . ? Mo3 O8 Mo4 O3 96.88(9) . . . . ? Mo2 O8 Mo4 O3 0.64(8) 3_757 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3W H4B O13 0.87(5) 1.80(5) 2.653(5) 168(6) 3_657 O2W H2A O9 0.831(19) 2.74(5) 3.059(5) 105(4) . O2W H2B O7 0.82(5) 1.98(2) 2.757(4) 158(5) . O1W H1A O4W 0.859(19) 2.22(5) 2.786(8) 124(5) . _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.582 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.107 #=========================================================================================end data_5 _database_code_depnum_ccdc_archive 'CCDC 789622' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H46 Mo8 N18 O28 Zn2' _chemical_formula_sum 'C36 H46 Mo8 N18 O28 Zn2' _chemical_formula_weight 2077.17 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' Zn Zn 0.2839 1.4301 '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 'P 21/n' _symmetry_space_group_name_hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5822(4) _cell_length_b 13.0529(4) _cell_length_c 19.6111(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.749(3) _cell_angle_gamma 90.00 _cell_volume 2954.65(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6852 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 29.1 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 2.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13616 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.1074 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 29.14 _reflns_number_total 6852 _reflns_number_gt 3833 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6852 _refine_ls_number_parameters 424 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0476 _refine_ls_wR_factor_gt 0.0451 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0982(4) 0.1455(4) 0.6679(2) 0.0491(15) Uani 1 1 d . . . H1 H 1.1190 0.0800 0.6549 0.059 Uiso 1 1 calc R . . C2 C 1.0309(4) 0.2680(4) 0.7197(2) 0.0496(14) Uani 1 1 d . . . H2 H 0.9939 0.3059 0.7516 0.059 Uiso 1 1 calc R . . C3 C 1.1799(4) 0.2402(3) 0.5726(2) 0.0409(13) Uani 1 1 d . . . H3A H 1.2010 0.1729 0.5567 0.049 Uiso 1 1 calc R . . H3B H 1.2509 0.2789 0.5823 0.049 Uiso 1 1 calc R . . C4 C 1.1369(4) 0.3897(3) 0.4946(2) 0.0286(11) Uani 1 1 d . . . C5 C 1.0745(4) 0.4352(3) 0.4381(2) 0.0280(11) Uani 1 1 d . . . C6 C 0.9864(4) 0.3822(3) 0.4022(2) 0.0334(11) Uani 1 1 d . . . C7 C 0.9496(4) 0.2888(3) 0.4277(2) 0.0333(12) Uani 1 1 d . . . C8 C 1.0104(4) 0.2425(3) 0.4836(2) 0.0370(12) Uani 1 1 d . . . C9 C 1.1066(4) 0.2932(3) 0.5163(2) 0.0300(11) Uani 1 1 d . . . C10 C 1.2385(4) 0.4472(3) 0.5312(2) 0.0433(13) Uani 1 1 d . . . H10A H 1.2452 0.4290 0.5788 0.065 Uiso 1 1 calc R . . H10B H 1.2257 0.5196 0.5267 0.065 Uiso 1 1 calc R . . H10C H 1.3086 0.4292 0.5112 0.065 Uiso 1 1 calc R . . C11 C 0.9763(5) 0.1374(3) 0.5088(3) 0.0615(17) Uani 1 1 d . . . H11A H 0.9363 0.1450 0.5495 0.092 Uiso 1 1 calc R . . H11B H 1.0447 0.0967 0.5189 0.092 Uiso 1 1 calc R . . H11C H 0.9265 0.1042 0.4741 0.092 Uiso 1 1 calc R . . C12 C 0.9303(4) 0.4221(3) 0.3350(2) 0.0515(14) Uani 1 1 d . . . H12A H 0.8778 0.4766 0.3437 0.077 Uiso 1 1 calc R . . H12B H 0.8884 0.3676 0.3112 0.077 Uiso 1 1 calc R . . H12C H 0.9890 0.4473 0.3076 0.077 Uiso 1 1 calc R . . C13 C 0.8432(4) 0.2376(3) 0.3932(2) 0.0450(13) Uani 1 1 d . . . H13A H 0.8084 0.1944 0.4261 0.054 Uiso 1 1 calc R . . H13B H 0.7871 0.2897 0.3780 0.054 Uiso 1 1 calc R . . C14 C 0.9615(4) 0.1184(3) 0.3246(3) 0.0404(12) Uani 1 1 d . . . H14 H 1.0287 0.1147 0.3540 0.048 Uiso 1 1 calc R . . C15 C 0.8359(4) 0.0945(4) 0.2418(3) 0.0568(15) Uani 1 1 d . . . H15 H 0.7988 0.0691 0.2015 0.068 Uiso 1 1 calc R . . C16 C 1.1039(4) 0.5418(3) 0.4158(2) 0.0355(12) Uani 1 1 d . . . H16A H 1.0339 0.5750 0.3962 0.043 Uiso 1 1 calc R . . H16B H 1.1331 0.5810 0.4555 0.043 Uiso 1 1 calc R . . C17 C 1.2571(4) 0.4685(3) 0.3462(2) 0.0329(12) Uani 1 1 d . . . H17 H 1.2557 0.4011 0.3614 0.039 Uiso 1 1 calc R . . C18 C 1.2975(4) 0.6031(3) 0.2954(2) 0.0389(12) Uani 1 1 d . . . H18 H 1.3336 0.6484 0.2674 0.047 Uiso 1 1 calc R . . N1 N 1.0393(3) 0.1656(3) 0.72177(18) 0.0364(10) Uani 1 1 d . . . N2 N 1.0799(3) 0.3101(3) 0.66817(19) 0.0419(10) Uani 1 1 d . . . N3 N 1.1231(3) 0.2287(3) 0.63559(19) 0.0373(10) Uani 1 1 d . . . N4 N 0.8694(3) 0.1756(3) 0.3348(2) 0.0412(10) Uani 1 1 d . . . N5 N 0.7888(4) 0.1622(4) 0.2820(2) 0.0659(13) Uani 1 1 d . . . N6 N 0.9429(3) 0.0674(3) 0.2662(2) 0.0368(10) Uani 1 1 d . . . N7 N 1.1902(3) 0.5422(2) 0.36547(18) 0.0310(9) Uani 1 1 d . . . N8 N 1.3266(3) 0.5043(3) 0.30196(17) 0.0316(9) Uani 1 1 d . . . N9 N 1.2135(3) 0.6299(2) 0.3323(2) 0.0408(10) Uani 1 1 d . . . O1 O 1.1045(3) 0.1598(2) 0.98010(16) 0.0515(9) Uani 1 1 d . . . O2 O 1.0016(3) 0.1701(2) 1.09875(16) 0.0594(10) Uani 1 1 d . . . O3 O 0.8947(2) 0.26731(19) 0.98639(13) 0.0307(7) Uani 1 1 d . . . O4 O 1.1682(2) 0.3205(2) 1.06971(14) 0.0360(8) Uani 1 1 d . . . O5 O 0.9207(2) 0.2291(2) 0.84854(14) 0.0366(8) Uani 1 1 d . . . O6 O 0.7211(2) 0.3098(2) 0.88620(16) 0.0458(9) Uani 1 1 d . . . O7 O 1.0575(2) 0.37319(19) 0.94080(16) 0.0382(8) Uani 1 1 d . . . O8 O 0.8892(2) 0.44037(19) 0.84128(13) 0.0312(7) Uani 1 1 d . . . O9 O 0.8398(3) 0.4729(2) 0.96582(15) 0.0438(9) Uani 1 1 d . . . O10 O 0.6836(3) 0.5522(2) 0.84941(16) 0.0478(9) Uani 1 1 d . . . O11 O 1.0262(2) 0.5923(2) 0.91035(16) 0.0449(9) Uani 1 1 d . . . O12 O 0.8621(3) 0.6395(2) 0.79165(15) 0.0448(9) Uani 1 1 d . . . O13 O 1.2473(3) 0.4967(2) 0.90595(17) 0.0531(10) Uani 1 1 d . . . Zn1 Zn 0.97067(5) 0.05659(4) 0.77388(3) 0.04829(17) Uani 1 1 d D . . Mo1 Mo 1.04162(4) 0.24345(3) 1.03232(2) 0.03656(11) Uani 1 1 d . . . Mo2 Mo 0.86719(3) 0.32502(3) 0.896517(19) 0.02790(10) Uani 1 1 d . . . Mo3 Mo 1.12245(3) 0.49697(3) 0.946675(19) 0.02605(10) Uani 1 1 d . . . Mo4 Mo 0.82987(4) 0.57425(3) 0.86167(2) 0.03340(11) Uani 1 1 d . . . O1W O 1.0641(3) 0.0381(3) 0.86650(19) 0.0547(10) Uani 1 1 d D . . H1A H 1.113(3) 0.087(3) 0.8728(16) 0.082 Uiso 1 1 d D . . H1B H 1.016(4) -0.003(3) 0.877(3) 0.082 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.068(4) 0.034(3) 0.048(3) 0.009(3) 0.023(3) -0.001(3) C2 0.059(4) 0.060(4) 0.033(3) 0.012(3) 0.022(3) 0.011(3) C3 0.038(3) 0.044(3) 0.043(3) 0.001(3) 0.017(3) 0.008(2) C4 0.031(3) 0.024(2) 0.034(3) -0.007(2) 0.016(2) 0.001(2) C5 0.026(3) 0.027(2) 0.033(3) 0.004(2) 0.017(2) 0.000(2) C6 0.029(3) 0.034(3) 0.038(3) -0.002(2) 0.009(2) 0.010(2) C7 0.024(3) 0.039(3) 0.038(3) -0.006(2) 0.009(2) 0.000(2) C8 0.043(3) 0.029(2) 0.042(3) -0.006(2) 0.022(3) -0.002(2) C9 0.026(3) 0.036(3) 0.030(3) 0.002(2) 0.017(2) 0.006(2) C10 0.044(3) 0.040(3) 0.046(3) 0.001(2) 0.006(3) -0.007(2) C11 0.075(4) 0.039(3) 0.072(4) 0.006(3) 0.015(4) -0.019(3) C12 0.055(4) 0.045(3) 0.055(4) -0.007(3) 0.004(3) 0.006(3) C13 0.039(3) 0.047(3) 0.051(3) -0.013(3) 0.015(3) -0.004(3) C14 0.021(3) 0.050(3) 0.050(4) 0.002(3) 0.004(3) -0.001(2) C15 0.039(3) 0.079(4) 0.051(4) -0.018(3) -0.007(3) 0.018(3) C16 0.042(3) 0.031(3) 0.036(3) -0.002(2) 0.019(3) 0.004(2) C17 0.037(3) 0.023(2) 0.040(3) 0.001(2) 0.011(2) 0.005(2) C18 0.035(3) 0.042(3) 0.041(3) 0.002(2) 0.004(3) -0.006(2) N1 0.040(2) 0.033(2) 0.038(2) 0.0011(19) 0.016(2) 0.0026(19) N2 0.050(3) 0.038(2) 0.039(3) -0.002(2) 0.005(2) 0.010(2) N3 0.035(2) 0.040(2) 0.039(2) 0.010(2) 0.014(2) 0.0067(19) N4 0.033(3) 0.044(2) 0.047(3) -0.006(2) -0.001(2) -0.004(2) N5 0.044(3) 0.094(4) 0.057(3) -0.014(3) -0.014(3) 0.018(3) N6 0.031(3) 0.043(2) 0.036(3) -0.002(2) 0.002(2) 0.0006(19) N7 0.034(2) 0.0218(19) 0.038(2) 0.0039(18) 0.010(2) 0.0032(17) N8 0.029(2) 0.033(2) 0.034(2) -0.0015(19) 0.0089(18) -0.0062(19) N9 0.035(2) 0.033(2) 0.055(3) 0.014(2) 0.014(2) -0.0026(18) O1 0.054(2) 0.045(2) 0.053(2) -0.0148(17) -0.0046(19) 0.0046(17) O2 0.057(2) 0.070(2) 0.048(2) 0.0203(19) -0.0102(19) -0.009(2) O3 0.0315(18) 0.0343(17) 0.0261(17) 0.0041(14) 0.0005(15) -0.0017(14) O4 0.041(2) 0.0310(17) 0.0353(19) -0.0049(15) -0.0042(16) 0.0072(15) O5 0.044(2) 0.0337(17) 0.0330(18) -0.0015(14) 0.0078(16) -0.0004(15) O6 0.030(2) 0.055(2) 0.053(2) 0.0132(17) 0.0071(17) -0.0016(16) O7 0.0264(18) 0.0328(17) 0.054(2) 0.0028(15) -0.0018(16) -0.0053(14) O8 0.0345(18) 0.0309(16) 0.0284(18) 0.0036(14) 0.0039(15) -0.0041(14) O9 0.064(2) 0.0338(18) 0.0327(19) -0.0009(14) 0.0004(17) 0.0050(16) O10 0.037(2) 0.051(2) 0.055(2) -0.0025(17) 0.0015(18) 0.0020(16) O11 0.0331(19) 0.0368(18) 0.062(2) 0.0130(16) -0.0149(17) -0.0017(15) O12 0.061(2) 0.0388(18) 0.033(2) 0.0039(15) -0.0028(18) 0.0063(16) O13 0.045(2) 0.0427(18) 0.077(3) -0.0030(19) 0.040(2) -0.0034(17) Zn1 0.0382(4) 0.0553(4) 0.0540(4) 0.0168(3) 0.0196(3) 0.0035(3) Mo1 0.0336(2) 0.0423(2) 0.0329(3) 0.0011(2) -0.0023(2) 0.0005(2) Mo2 0.0277(2) 0.0304(2) 0.0257(2) 0.00159(19) 0.00253(18) -0.00089(18) Mo3 0.0227(2) 0.0296(2) 0.0265(2) 0.00135(18) 0.00656(17) 0.00068(18) Mo4 0.0389(3) 0.0314(2) 0.0290(2) -0.0002(2) -0.0029(2) 0.0015(2) O1W 0.053(3) 0.056(3) 0.053(2) -0.0072(19) -0.008(2) 0.0003(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N3 1.303(5) . ? C1 N1 1.329(5) . ? C1 H1 0.9300 . ? C2 N2 1.319(5) . ? C2 N1 1.342(5) . ? C2 H2 0.9300 . ? C3 N3 1.455(5) . ? C3 C9 1.505(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.385(5) . ? C4 C5 1.402(6) . ? C4 C10 1.525(6) . ? C5 C6 1.377(6) . ? C5 C16 1.506(5) . ? C6 C7 1.398(6) . ? C6 C12 1.512(6) . ? C7 C8 1.391(6) . ? C7 C13 1.512(6) . ? C8 C9 1.404(6) . ? C8 C11 1.521(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N4 1.455(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N6 1.328(5) . ? C14 N4 1.330(5) . ? C14 H14 0.9300 . ? C15 N5 1.331(6) . ? C15 N6 1.338(6) . ? C15 H15 0.9300 . ? C16 N7 1.462(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N7 1.310(4) . ? C17 N8 1.316(4) . ? C17 H17 0.9300 . ? C18 N9 1.307(5) . ? C18 N8 1.336(5) . ? C18 H18 0.9300 . ? N1 Zn1 1.958(3) . ? N2 N3 1.356(4) . ? N4 N5 1.346(5) . ? N6 Zn1 2.091(4) 3_756 ? N7 N9 1.355(4) . ? N8 Zn1 1.968(3) 4_665 ? O1 Mo1 1.701(3) . ? O2 Mo1 1.711(3) . ? O3 Mo1 1.885(3) . ? O3 Mo2 1.919(3) . ? O4 Mo1 1.876(3) . ? O4 Mo4 1.922(3) 3_767 ? O5 Mo2 1.713(3) . ? O6 Mo2 1.699(3) . ? O7 Mo3 1.782(3) . ? O7 Mo2 2.386(3) . ? O7 Mo1 2.486(3) . ? O8 Mo2 1.885(2) . ? O8 Mo4 1.932(3) . ? O9 Mo3 1.780(3) 3_767 ? O9 Mo2 2.397(3) . ? O9 Mo4 2.428(3) . ? O10 Mo4 1.715(3) . ? O11 Mo3 1.780(3) . ? O11 Mo4 2.404(3) . ? O12 Mo4 1.684(3) . ? O13 Mo3 1.709(2) . ? Zn1 N8 1.968(3) 4_566 ? Zn1 O1W 2.050(4) . ? Zn1 N6 2.091(4) 3_756 ? Mo3 O9 1.780(3) 3_767 ? Mo4 O4 1.922(3) 3_767 ? O1W H1A 0.86(4) . ? O1W H1B 0.81(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 C1 N1 111.8(4) . . ? N3 C1 H1 124.1 . . ? N1 C1 H1 124.1 . . ? N2 C2 N1 113.8(4) . . ? N2 C2 H2 123.1 . . ? N1 C2 H2 123.1 . . ? N3 C3 C9 113.8(3) . . ? N3 C3 H3A 108.8 . . ? C9 C3 H3A 108.8 . . ? N3 C3 H3B 108.8 . . ? C9 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C9 C4 C5 120.0(4) . . ? C9 C4 C10 120.5(4) . . ? C5 C4 C10 119.4(4) . . ? C6 C5 C4 120.2(4) . . ? C6 C5 C16 119.4(4) . . ? C4 C5 C16 120.4(4) . . ? C5 C6 C7 119.3(4) . . ? C5 C6 C12 121.3(4) . . ? C7 C6 C12 119.3(4) . . ? C8 C7 C6 120.8(4) . . ? C8 C7 C13 120.1(4) . . ? C6 C7 C13 119.1(5) . . ? C7 C8 C9 119.0(4) . . ? C7 C8 C11 121.3(5) . . ? C9 C8 C11 119.6(5) . . ? C4 C9 C8 120.0(4) . . ? C4 C9 C3 120.1(4) . . ? C8 C9 C3 119.8(4) . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C7 112.6(4) . . ? N4 C13 H13A 109.1 . . ? C7 C13 H13A 109.1 . . ? N4 C13 H13B 109.1 . . ? C7 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N6 C14 N4 109.6(4) . . ? N6 C14 H14 125.2 . . ? N4 C14 H14 125.2 . . ? N5 C15 N6 112.1(5) . . ? N5 C15 H15 123.9 . . ? N6 C15 H15 123.9 . . ? N7 C16 C5 112.5(3) . . ? N7 C16 H16A 109.1 . . ? C5 C16 H16A 109.1 . . ? N7 C16 H16B 109.1 . . ? C5 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N7 C17 N8 109.8(3) . . ? N7 C17 H17 125.1 . . ? N8 C17 H17 125.1 . . ? N9 C18 N8 113.5(4) . . ? N9 C18 H18 123.3 . . ? N8 C18 H18 123.3 . . ? C1 N1 C2 102.3(4) . . ? C1 N1 Zn1 121.9(3) . . ? C2 N1 Zn1 135.1(3) . . ? C2 N2 N3 103.5(4) . . ? C1 N3 N2 108.6(4) . . ? C1 N3 C3 129.3(4) . . ? N2 N3 C3 122.0(3) . . ? C14 N4 N5 109.1(4) . . ? C14 N4 C13 130.7(4) . . ? N5 N4 C13 120.0(4) . . ? C15 N5 N4 104.4(4) . . ? C14 N6 C15 104.8(4) . . ? C14 N6 Zn1 131.6(3) . 3_756 ? C15 N6 Zn1 121.9(3) . 3_756 ? C17 N7 N9 109.6(3) . . ? C17 N7 C16 130.2(3) . . ? N9 N7 C16 120.1(3) . . ? C17 N8 C18 104.0(3) . . ? C17 N8 Zn1 128.3(3) . 4_665 ? C18 N8 Zn1 125.2(3) . 4_665 ? C18 N9 N7 103.0(3) . . ? Mo1 O3 Mo2 125.33(13) . . ? Mo1 O4 Mo4 128.34(15) . 3_767 ? Mo3 O7 Mo2 129.40(14) . . ? Mo3 O7 Mo1 128.84(16) . . ? Mo2 O7 Mo1 87.81(9) . . ? Mo2 O8 Mo4 122.44(13) . . ? Mo3 O9 Mo2 133.72(15) 3_767 . ? Mo3 O9 Mo4 132.96(14) 3_767 . ? Mo2 O9 Mo4 87.77(9) . . ? Mo3 O11 Mo4 129.15(14) . . ? N1 Zn1 N8 146.10(15) . 4_566 ? N1 Zn1 O1W 109.90(15) . . ? N8 Zn1 O1W 95.88(14) 4_566 . ? N1 Zn1 N6 97.94(13) . 3_756 ? N8 Zn1 N6 103.66(14) 4_566 3_756 ? O1W Zn1 N6 90.45(15) . 3_756 ? O1 Mo1 O2 104.83(16) . . ? O1 Mo1 O4 102.67(14) . . ? O2 Mo1 O4 104.75(15) . . ? O1 Mo1 O3 103.49(14) . . ? O2 Mo1 O3 99.51(14) . . ? O4 Mo1 O3 138.06(12) . . ? O1 Mo1 O7 86.63(12) . . ? O2 Mo1 O7 166.36(13) . . ? O4 Mo1 O7 79.33(11) . . ? O3 Mo1 O7 70.14(10) . . ? O6 Mo2 O5 104.55(14) . . ? O6 Mo2 O8 101.89(13) . . ? O5 Mo2 O8 101.29(12) . . ? O6 Mo2 O3 98.69(13) . . ? O5 Mo2 O3 100.23(12) . . ? O8 Mo2 O3 145.24(12) . . ? O6 Mo2 O7 162.80(13) . . ? O5 Mo2 O7 91.54(12) . . ? O8 Mo2 O7 80.42(11) . . ? O3 Mo2 O7 72.02(11) . . ? O6 Mo2 O9 89.11(13) . . ? O5 Mo2 O9 166.19(12) . . ? O8 Mo2 O9 73.32(10) . . ? O3 Mo2 O9 79.34(11) . . ? O7 Mo2 O9 75.12(10) . . ? O13 Mo3 O11 109.91(15) . . ? O13 Mo3 O9 107.51(16) . 3_767 ? O11 Mo3 O9 109.12(14) . 3_767 ? O13 Mo3 O7 109.70(14) . . ? O11 Mo3 O7 111.16(13) . . ? O9 Mo3 O7 109.36(13) 3_767 . ? O12 Mo4 O10 104.70(15) . . ? O12 Mo4 O4 102.62(13) . 3_767 ? O10 Mo4 O4 99.91(13) . 3_767 ? O12 Mo4 O8 100.50(12) . . ? O10 Mo4 O8 100.58(13) . . ? O4 Mo4 O8 143.89(12) 3_767 . ? O12 Mo4 O11 90.45(13) . . ? O10 Mo4 O11 164.32(13) . . ? O4 Mo4 O11 72.30(11) 3_767 . ? O8 Mo4 O11 80.19(11) . . ? O12 Mo4 O9 164.43(14) . . ? O10 Mo4 O9 90.22(13) . . ? O4 Mo4 O9 78.67(10) 3_767 . ? O8 Mo4 O9 71.85(10) . . ? O11 Mo4 O9 75.05(10) . . ? Zn1 O1W H1A 109.5(19) . . ? Zn1 O1W H1B 89(4) . . ? H1A O1W H1B 156(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C4 C5 C6 -2.9(6) . . . . ? C10 C4 C5 C6 176.6(4) . . . . ? C9 C4 C5 C16 177.6(3) . . . . ? C10 C4 C5 C16 -2.9(5) . . . . ? C4 C5 C6 C7 8.4(6) . . . . ? C16 C5 C6 C7 -172.1(3) . . . . ? C4 C5 C6 C12 -170.4(4) . . . . ? C16 C5 C6 C12 9.2(6) . . . . ? C5 C6 C7 C8 -8.6(6) . . . . ? C12 C6 C7 C8 170.2(4) . . . . ? C5 C6 C7 C13 172.4(4) . . . . ? C12 C6 C7 C13 -8.9(6) . . . . ? C6 C7 C8 C9 3.1(6) . . . . ? C13 C7 C8 C9 -177.8(4) . . . . ? C6 C7 C8 C11 -175.7(4) . . . . ? C13 C7 C8 C11 3.4(6) . . . . ? C5 C4 C9 C8 -2.7(6) . . . . ? C10 C4 C9 C8 177.9(4) . . . . ? C5 C4 C9 C3 174.3(3) . . . . ? C10 C4 C9 C3 -5.2(5) . . . . ? C7 C8 C9 C4 2.5(6) . . . . ? C11 C8 C9 C4 -178.7(4) . . . . ? C7 C8 C9 C3 -174.5(3) . . . . ? C11 C8 C9 C3 4.3(6) . . . . ? N3 C3 C9 C4 112.0(4) . . . . ? N3 C3 C9 C8 -71.0(5) . . . . ? C8 C7 C13 N4 -94.3(5) . . . . ? C6 C7 C13 N4 84.8(5) . . . . ? C6 C5 C16 N7 -89.2(5) . . . . ? C4 C5 C16 N7 90.3(5) . . . . ? N3 C1 N1 C2 -0.2(6) . . . . ? N3 C1 N1 Zn1 171.6(3) . . . . ? N2 C2 N1 C1 0.4(6) . . . . ? N2 C2 N1 Zn1 -169.7(3) . . . . ? N1 C2 N2 N3 -0.4(6) . . . . ? N1 C1 N3 N2 0.0(6) . . . . ? N1 C1 N3 C3 -176.1(4) . . . . ? C2 N2 N3 C1 0.2(5) . . . . ? C2 N2 N3 C3 176.7(4) . . . . ? C9 C3 N3 C1 119.7(5) . . . . ? C9 C3 N3 N2 -55.9(6) . . . . ? N6 C14 N4 N5 -0.1(5) . . . . ? N6 C14 N4 C13 174.0(4) . . . . ? C7 C13 N4 C14 35.8(7) . . . . ? C7 C13 N4 N5 -150.7(4) . . . . ? N6 C15 N5 N4 -1.6(6) . . . . ? C14 N4 N5 C15 1.0(6) . . . . ? C13 N4 N5 C15 -173.8(4) . . . . ? N4 C14 N6 C15 -0.8(5) . . . . ? N4 C14 N6 Zn1 -165.8(3) . . . 3_756 ? N5 C15 N6 C14 1.5(6) . . . . ? N5 C15 N6 Zn1 168.3(3) . . . 3_756 ? N8 C17 N7 N9 1.3(5) . . . . ? N8 C17 N7 C16 -176.6(4) . . . . ? C5 C16 N7 C17 -12.3(7) . . . . ? C5 C16 N7 N9 169.9(4) . . . . ? N7 C17 N8 C18 -0.3(5) . . . . ? N7 C17 N8 Zn1 162.2(3) . . . 4_665 ? N9 C18 N8 C17 -0.8(5) . . . . ? N9 C18 N8 Zn1 -164.0(3) . . . 4_665 ? N8 C18 N9 N7 1.5(5) . . . . ? C17 N7 N9 C18 -1.7(5) . . . . ? C16 N7 N9 C18 176.5(4) . . . . ? C1 N1 Zn1 N8 -115.8(4) . . . 4_566 ? C2 N1 Zn1 N8 52.8(6) . . . 4_566 ? C1 N1 Zn1 O1W 107.0(4) . . . . ? C2 N1 Zn1 O1W -84.4(5) . . . . ? C1 N1 Zn1 N6 13.6(4) . . . 3_756 ? C2 N1 Zn1 N6 -177.8(5) . . . 3_756 ? Mo4 O4 Mo1 O1 -175.78(19) 3_767 . . . ? Mo4 O4 Mo1 O2 -66.5(2) 3_767 . . . ? Mo4 O4 Mo1 O3 56.8(3) 3_767 . . . ? Mo4 O4 Mo1 O7 100.17(19) 3_767 . . . ? Mo2 O3 Mo1 O1 -60.6(2) . . . . ? Mo2 O3 Mo1 O2 -168.50(18) . . . . ? Mo2 O3 Mo1 O4 66.6(2) . . . . ? Mo2 O3 Mo1 O7 20.71(14) . . . . ? Mo3 O7 Mo1 O1 -126.1(2) . . . . ? Mo2 O7 Mo1 O1 92.21(13) . . . . ? Mo3 O7 Mo1 O2 86.3(6) . . . . ? Mo2 O7 Mo1 O2 -55.4(6) . . . . ? Mo3 O7 Mo1 O4 -22.52(18) . . . . ? Mo2 O7 Mo1 O4 -164.22(11) . . . . ? Mo3 O7 Mo1 O3 128.3(2) . . . . ? Mo2 O7 Mo1 O3 -13.43(10) . . . . ? Mo4 O8 Mo2 O6 65.1(2) . . . . ? Mo4 O8 Mo2 O5 172.78(17) . . . . ? Mo4 O8 Mo2 O3 -60.0(3) . . . . ? Mo4 O8 Mo2 O7 -97.55(17) . . . . ? Mo4 O8 Mo2 O9 -20.34(16) . . . . ? Mo1 O3 Mo2 O6 173.53(17) . . . . ? Mo1 O3 Mo2 O5 66.92(19) . . . . ? Mo1 O3 Mo2 O8 -60.6(3) . . . . ? Mo1 O3 Mo2 O7 -21.37(15) . . . . ? Mo1 O3 Mo2 O9 -99.04(17) . . . . ? Mo3 O7 Mo2 O6 -69.1(5) . . . . ? Mo1 O7 Mo2 O6 72.3(4) . . . . ? Mo3 O7 Mo2 O5 131.4(2) . . . . ? Mo1 O7 Mo2 O5 -87.23(11) . . . . ? Mo3 O7 Mo2 O8 30.25(19) . . . . ? Mo1 O7 Mo2 O8 171.58(11) . . . . ? Mo3 O7 Mo2 O3 -128.3(2) . . . . ? Mo1 O7 Mo2 O3 13.03(9) . . . . ? Mo3 O7 Mo2 O9 -44.90(19) . . . . ? Mo1 O7 Mo2 O9 96.43(10) . . . . ? Mo3 O9 Mo2 O6 115.8(2) 3_767 . . . ? Mo4 O9 Mo2 O6 -89.19(12) . . . . ? Mo3 O9 Mo2 O5 -72.8(5) 3_767 . . . ? Mo4 O9 Mo2 O5 82.3(5) . . . . ? Mo3 O9 Mo2 O8 -141.5(2) 3_767 . . . ? Mo4 O9 Mo2 O8 13.50(10) . . . . ? Mo3 O9 Mo2 O3 16.8(2) 3_767 . . . ? Mo4 O9 Mo2 O3 171.80(12) . . . . ? Mo3 O9 Mo2 O7 -57.3(2) 3_767 . . . ? Mo4 O9 Mo2 O7 97.76(10) . . . . ? Mo4 O11 Mo3 O13 124.1(2) . . . . ? Mo4 O11 Mo3 O9 -118.26(19) . . . 3_767 ? Mo4 O11 Mo3 O7 2.4(2) . . . . ? Mo2 O7 Mo3 O13 -124.1(2) . . . . ? Mo1 O7 Mo3 O13 109.19(19) . . . . ? Mo2 O7 Mo3 O11 -2.3(2) . . . . ? Mo1 O7 Mo3 O11 -129.04(18) . . . . ? Mo2 O7 Mo3 O9 118.23(19) . . . 3_767 ? Mo1 O7 Mo3 O9 -8.5(2) . . . 3_767 ? Mo2 O8 Mo4 O12 -173.78(18) . . . . ? Mo2 O8 Mo4 O10 -66.5(2) . . . . ? Mo2 O8 Mo4 O4 57.1(3) . . . 3_767 ? Mo2 O8 Mo4 O11 97.60(18) . . . . ? Mo2 O8 Mo4 O9 20.23(16) . . . . ? Mo3 O11 Mo4 O12 -130.3(2) . . . . ? Mo3 O11 Mo4 O10 64.5(5) . . . . ? Mo3 O11 Mo4 O4 126.6(2) . . . 3_767 ? Mo3 O11 Mo4 O8 -29.69(19) . . . . ? Mo3 O11 Mo4 O9 43.99(19) . . . . ? Mo3 O9 Mo4 O12 79.6(5) 3_767 . . . ? Mo2 O9 Mo4 O12 -75.8(4) . . . . ? Mo3 O9 Mo4 O10 -116.9(2) 3_767 . . . ? Mo2 O9 Mo4 O10 87.79(12) . . . . ? Mo3 O9 Mo4 O4 -16.8(2) 3_767 . . 3_767 ? Mo2 O9 Mo4 O4 -172.14(13) . . . 3_767 ? Mo3 O9 Mo4 O8 142.1(2) 3_767 . . . ? Mo2 O9 Mo4 O8 -13.28(10) . . . . ? Mo3 O9 Mo4 O11 57.7(2) 3_767 . . . ? Mo2 O9 Mo4 O11 -97.65(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1B O2 0.81(4) 2.24(4) 2.918(4) 141(5) 3_757 O1W H1A O1 0.86(4) 2.32(4) 2.745(5) 111(3) . _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.992 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.112 #===========================================================================================end data_6 _database_code_depnum_ccdc_archive 'CCDC 789623' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H42 Ag4 Mo8 N18 O26' _chemical_formula_sum 'C36 H42 Ag4 Mo8 N18 O26' _chemical_formula_weight 2341.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4063(14) _cell_length_b 11.8303(16) _cell_length_c 12.2270(14) _cell_angle_alpha 115.199(12) _cell_angle_beta 93.897(10) _cell_angle_gamma 101.029(11) _cell_volume 1444.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5139 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 67.2 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 25.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.10 _exptl_absorpt_correction_T_max 0.24 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16362 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 67.21 _reflns_number_total 5139 _reflns_number_gt 3739 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5139 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1441 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3223(11) 0.0026(10) 0.4931(10) 0.045(3) Uani 1 1 d . . . H1 H 0.2812 -0.0812 0.4384 0.054 Uiso 1 1 calc R . . C2 C 0.3878(9) 0.1727(9) 0.6577(9) 0.037(2) Uani 1 1 d . . . H2 H 0.4035 0.2342 0.7393 0.044 Uiso 1 1 calc R . . C3 C 0.5173(9) 0.3061(9) 0.5751(8) 0.035(2) Uani 1 1 d . . . H3A H 0.6006 0.3011 0.5878 0.042 Uiso 1 1 calc R . . H3B H 0.5064 0.3806 0.6453 0.042 Uiso 1 1 calc R . . C4 C 0.4936(8) 0.3232(8) 0.4609(9) 0.032(2) Uani 1 1 d . . . C5 C 0.3804(8) 0.3400(8) 0.4300(9) 0.032(2) Uani 1 1 d . . . C6 C 0.3534(8) 0.3466(8) 0.3187(8) 0.0275(18) Uani 1 1 d . . . C7 C 0.4417(8) 0.3450(9) 0.2432(9) 0.0297(19) Uani 1 1 d . . . C8 C 0.5569(7) 0.3324(8) 0.2792(8) 0.0246(17) Uani 1 1 d . . . C9 C 0.5808(7) 0.3183(8) 0.3859(8) 0.0267(18) Uani 1 1 d . . . C10 C 0.7028(9) 0.2986(12) 0.4222(9) 0.043(2) Uani 1 1 d . . . H10A H 0.7274 0.3462 0.5095 0.065 Uiso 1 1 calc R . . H10B H 0.7621 0.3286 0.3823 0.065 Uiso 1 1 calc R . . H10C H 0.6959 0.2087 0.3978 0.065 Uiso 1 1 calc R . . C11 C 0.4134(10) 0.3554(11) 0.1258(10) 0.043(2) Uani 1 1 d . . . H11A H 0.3439 0.2880 0.0745 0.064 Uiso 1 1 calc R . . H11B H 0.4817 0.3470 0.0837 0.064 Uiso 1 1 calc R . . H11C H 0.3967 0.4376 0.1446 0.064 Uiso 1 1 calc R . . C12 C 0.2259(9) 0.3476(11) 0.2782(12) 0.047(3) Uani 1 1 d . . . H12A H 0.2042 0.4215 0.3398 0.057 Uiso 1 1 calc R . . H12B H 0.2216 0.3553 0.2022 0.057 Uiso 1 1 calc R . . C13 C 0.2869(9) 0.3480(9) 0.5126(10) 0.037(2) Uani 1 1 d . . . H13A H 0.2353 0.2638 0.4869 0.056 Uiso 1 1 calc R . . H13B H 0.2391 0.4049 0.5079 0.056 Uiso 1 1 calc R . . H13C H 0.3267 0.3805 0.5955 0.056 Uiso 1 1 calc R . . C14 C 0.6537(9) 0.3315(10) 0.2009(9) 0.037(2) Uani 1 1 d . . . H14A H 0.6451 0.3883 0.1640 0.044 Uiso 1 1 calc R . . H14B H 0.7325 0.3654 0.2529 0.044 Uiso 1 1 calc R . . C15 C 0.0252(9) 0.2162(10) 0.2807(9) 0.037(2) Uani 1 1 d . . . H15 H -0.0145 0.2824 0.3089 0.045 Uiso 1 1 calc R . . C16 C 0.0715(11) 0.0358(11) 0.2258(14) 0.064(4) Uani 1 1 d . . . H16 H 0.0672 -0.0489 0.2110 0.076 Uiso 1 1 calc R . . C17 C 0.6843(14) 0.0204(12) 0.0191(13) 0.063(3) Uani 1 1 d . . . H17 H 0.7108 -0.0533 0.0061 0.075 Uiso 1 1 calc R . . C18 C 0.6058(10) 0.1529(11) -0.0120(10) 0.045(2) Uani 1 1 d . . . H18 H 0.5666 0.1925 -0.0495 0.055 Uiso 1 1 calc R . . N1 N 0.4354(7) 0.1885(7) 0.5668(7) 0.0286(16) Uani 1 1 d . . . N2 N 0.3939(8) 0.0824(8) 0.4621(7) 0.0395(19) Uani 1 1 d . . . N3 N 0.3162(8) 0.0581(9) 0.6144(8) 0.045(2) Uani 1 1 d . . . N4 N 0.6489(7) 0.2041(8) 0.1042(7) 0.0359(18) Uani 1 1 d . . . N5 N 0.7012(11) 0.1217(11) 0.1293(9) 0.059(3) Uani 1 1 d . . . N6 N 0.6256(10) 0.0354(9) -0.0705(9) 0.050(2) Uani 1 1 d . . . N7 N 0.1392(7) 0.2284(7) 0.2597(7) 0.0324(17) Uani 1 1 d . . . N8 N 0.1693(8) 0.1145(9) 0.2212(10) 0.056(3) Uani 1 1 d . . . N9 N -0.0221(8) 0.0947(8) 0.2550(9) 0.043(2) Uani 1 1 d . . . O1 O 0.0130(5) -0.3933(5) 0.1118(5) 0.0253(12) Uani 1 1 d . . . O2 O 0.1795(5) -0.3954(5) -0.0235(5) 0.0268(12) Uani 1 1 d . . . O3 O 0.2299(7) -0.1786(7) 0.2020(7) 0.0471(18) Uani 1 1 d . . . O4 O 0.3694(6) -0.3469(8) 0.1637(6) 0.0461(18) Uani 1 1 d . . . O5 O 0.1824(6) -0.3523(8) 0.2974(6) 0.0430(17) Uani 1 1 d . . . O6 O 0.0191(7) -0.3603(13) 0.4628(7) 0.079(3) Uani 1 1 d . . . O7 O 0.0454(8) -0.1770(10) 0.3833(11) 0.087(4) Uani 1 1 d . . . O8 O -0.1457(6) -0.3891(7) 0.2631(6) 0.0358(15) Uani 1 1 d . . . O9 O -0.3405(6) -0.4374(7) 0.0912(7) 0.0419(16) Uani 1 1 d . . . O10 O -0.1632(7) -0.2256(7) 0.1533(7) 0.0498(19) Uani 1 1 d . . . O11 O -0.1594(5) -0.4394(6) -0.0609(6) 0.0294(13) Uani 1 1 d . . . O12 O 0.0071(6) -0.4461(7) -0.2182(6) 0.0354(14) Uani 1 1 d . . . O13 O 0.0319(6) -0.2260(6) -0.0121(7) 0.0403(16) Uani 1 1 d . . . Mo1 Mo 0.02144(7) -0.33839(9) 0.33418(7) 0.0455(3) Uani 1 1 d . . . Mo2 Mo -0.18765(6) -0.38464(7) 0.11162(6) 0.02754(19) Uani 1 1 d . . . Mo3 Mo 0.01482(6) -0.38491(6) -0.05961(6) 0.02485(19) Uani 1 1 d . . . Mo4 Mo 0.22252(6) -0.33725(7) 0.15626(6) 0.0291(2) Uani 1 1 d . . . Ag1 Ag 0.17519(8) -0.01196(8) 0.69283(9) 0.0585(3) Uani 1 1 d . . . Ag2 Ag 0.36767(8) 0.05671(8) 0.26648(7) 0.0517(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.057(6) 0.029(5) 0.037(5) 0.009(4) 0.008(5) -0.004(4) C2 0.033(5) 0.033(5) 0.031(5) 0.010(4) 0.009(4) -0.009(4) C3 0.040(5) 0.033(5) 0.029(5) 0.020(4) -0.002(4) -0.010(4) C4 0.029(5) 0.023(4) 0.039(5) 0.012(4) 0.005(4) -0.003(3) C5 0.030(5) 0.016(4) 0.045(5) 0.012(4) 0.009(4) -0.003(3) C6 0.024(4) 0.020(4) 0.039(5) 0.015(4) 0.004(4) 0.002(3) C7 0.032(5) 0.031(5) 0.036(5) 0.024(4) 0.007(4) 0.007(4) C8 0.019(4) 0.026(4) 0.032(4) 0.016(4) 0.004(3) 0.004(3) C9 0.021(4) 0.027(4) 0.030(4) 0.012(4) 0.000(3) 0.005(3) C10 0.032(5) 0.066(7) 0.034(5) 0.024(5) 0.006(4) 0.016(5) C11 0.043(6) 0.055(7) 0.046(6) 0.032(5) 0.010(5) 0.019(5) C12 0.026(5) 0.052(7) 0.079(8) 0.041(6) 0.010(5) 0.010(4) C13 0.037(5) 0.028(5) 0.046(6) 0.014(4) 0.020(4) 0.011(4) C14 0.040(5) 0.037(5) 0.039(5) 0.023(4) 0.014(4) 0.004(4) C15 0.036(5) 0.043(6) 0.044(5) 0.029(5) 0.013(4) 0.009(4) C16 0.049(7) 0.023(5) 0.092(10) 0.005(6) 0.011(6) 0.001(5) C17 0.088(10) 0.046(7) 0.066(8) 0.027(6) 0.029(7) 0.033(7) C18 0.044(6) 0.046(6) 0.045(6) 0.019(5) 0.006(5) 0.008(5) N1 0.032(4) 0.022(4) 0.025(4) 0.009(3) 0.002(3) -0.002(3) N2 0.051(5) 0.028(4) 0.025(4) 0.005(3) 0.000(3) -0.004(4) N3 0.051(5) 0.042(5) 0.037(5) 0.017(4) 0.015(4) -0.002(4) N4 0.044(5) 0.036(4) 0.032(4) 0.017(4) 0.013(3) 0.013(4) N5 0.080(7) 0.059(6) 0.044(5) 0.023(5) 0.012(5) 0.028(5) N6 0.065(6) 0.035(5) 0.042(5) 0.010(4) 0.013(4) 0.014(4) N7 0.026(4) 0.032(4) 0.036(4) 0.015(3) 0.001(3) 0.002(3) N8 0.035(5) 0.040(5) 0.072(7) 0.005(5) 0.014(4) 0.010(4) N9 0.038(4) 0.032(4) 0.057(5) 0.015(4) 0.017(4) 0.009(4) O1 0.022(3) 0.024(3) 0.029(3) 0.011(2) 0.005(2) 0.002(2) O2 0.027(3) 0.021(3) 0.032(3) 0.014(3) 0.007(2) 0.001(2) O3 0.042(4) 0.039(4) 0.041(4) 0.006(3) 0.003(3) -0.001(3) O4 0.024(3) 0.070(5) 0.037(4) 0.021(4) -0.003(3) 0.007(3) O5 0.033(3) 0.062(5) 0.022(3) 0.013(3) 0.000(3) 0.002(3) O6 0.039(4) 0.156(10) 0.032(4) 0.036(5) 0.006(3) 0.015(5) O7 0.050(5) 0.058(6) 0.091(7) -0.019(5) 0.020(5) -0.003(4) O8 0.033(3) 0.042(4) 0.029(3) 0.012(3) 0.013(3) 0.010(3) O9 0.032(3) 0.052(4) 0.045(4) 0.024(3) 0.011(3) 0.010(3) O10 0.064(5) 0.032(4) 0.059(5) 0.018(4) 0.029(4) 0.022(3) O11 0.024(3) 0.037(3) 0.034(3) 0.021(3) 0.009(2) 0.009(3) O12 0.034(3) 0.047(4) 0.036(3) 0.028(3) 0.007(3) 0.011(3) O13 0.046(4) 0.030(3) 0.053(4) 0.026(3) 0.018(3) 0.010(3) Mo1 0.0293(4) 0.0610(6) 0.0263(4) 0.0049(4) 0.0046(3) 0.0023(4) Mo2 0.0274(4) 0.0272(4) 0.0296(4) 0.0124(3) 0.0108(3) 0.0087(3) Mo3 0.0232(3) 0.0276(4) 0.0299(4) 0.0181(3) 0.0073(3) 0.0062(3) Mo4 0.0240(4) 0.0308(4) 0.0241(4) 0.0079(3) 0.0014(3) -0.0005(3) Ag1 0.0594(5) 0.0457(5) 0.0678(6) 0.0268(4) 0.0258(4) -0.0018(4) Ag2 0.0686(6) 0.0396(4) 0.0370(4) 0.0109(3) 0.0126(4) 0.0049(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.324(14) . ? C1 N3 1.356(14) . ? C2 N3 1.301(13) . ? C2 N1 1.335(13) . ? C3 N1 1.480(11) . ? C3 C4 1.508(14) . ? C4 C9 1.391(13) . ? C4 C5 1.394(14) . ? C5 C6 1.413(14) . ? C5 C13 1.506(13) . ? C6 C7 1.409(13) . ? C6 C12 1.508(14) . ? C7 C8 1.412(13) . ? C7 C11 1.511(13) . ? C8 C9 1.399(13) . ? C8 C14 1.508(12) . ? C9 C10 1.522(13) . ? C12 N7 1.477(13) . ? C14 N4 1.454(13) . ? C15 N9 1.323(14) . ? C15 N7 1.335(12) . ? C16 N8 1.330(16) . ? C16 N9 1.372(15) . ? C17 N5 1.338(17) . ? C17 N6 1.338(17) . ? C18 N4 1.299(14) . ? C18 N6 1.338(15) . ? N1 N2 1.327(11) . ? N2 Ag2 2.270(8) . ? N3 Ag1 2.137(9) . ? N4 N5 1.361(14) . ? N6 Ag2 2.184(9) 2_655 ? N7 N8 1.347(13) . ? N8 Ag2 2.577(10) . ? N9 Ag1 2.107(9) 2_556 ? O1 Mo3 2.141(6) . ? O1 Mo2 2.310(5) . ? O1 Mo4 2.315(5) . ? O1 Mo3 2.371(6) 2_545 ? O1 Mo1 2.503(6) . ? O2 Mo3 1.939(6) . ? O2 Mo4 1.996(6) . ? O2 Mo2 2.380(6) 2_545 ? O3 Mo4 1.698(8) . ? O4 Mo4 1.700(7) . ? O5 Mo4 1.886(7) . ? O5 Mo1 1.940(7) . ? O6 Mo1 1.701(9) . ? O7 Mo1 1.698(11) . ? O8 Mo2 1.906(7) . ? O8 Mo1 1.908(6) . ? O9 Mo2 1.698(7) . ? O10 Mo2 1.685(7) . ? O11 Mo3 1.965(6) . ? O11 Mo2 1.995(6) . ? O11 Mo4 2.322(6) 2_545 ? O12 Mo3 1.746(7) . ? O12 Mo1 2.272(7) 2_545 ? O13 Mo3 1.680(7) . ? Mo1 O12 2.272(7) 2_545 ? Mo2 O2 2.380(6) 2_545 ? Mo3 O1 2.371(6) 2_545 ? Mo3 Mo4 3.2045(11) . ? Mo4 O11 2.322(6) 2_545 ? Ag1 N9 2.107(9) 2_556 ? Ag2 N6 2.184(9) 2_655 ? 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 N2 C1 N3 111.7(9) . . ? N3 C2 N1 109.5(8) . . ? N1 C3 C4 111.9(7) . . ? C9 C4 C5 120.7(9) . . ? C9 C4 C3 121.0(8) . . ? C5 C4 C3 118.3(9) . . ? C4 C5 C6 119.1(8) . . ? C4 C5 C13 120.7(9) . . ? C6 C5 C13 120.3(9) . . ? C7 C6 C5 120.9(8) . . ? C7 C6 C12 120.3(9) . . ? C5 C6 C12 118.7(8) . . ? C6 C7 C8 118.6(8) . . ? C6 C7 C11 120.7(8) . . ? C8 C7 C11 120.7(8) . . ? C9 C8 C7 120.3(8) . . ? C9 C8 C14 119.9(8) . . ? C7 C8 C14 119.8(8) . . ? C4 C9 C8 120.4(8) . . ? C4 C9 C10 119.0(9) . . ? C8 C9 C10 120.6(8) . . ? N7 C12 C6 110.9(8) . . ? N4 C14 C8 113.4(8) . . ? N9 C15 N7 109.1(9) . . ? N8 C16 N9 111.8(10) . . ? N5 C17 N6 113.5(11) . . ? N4 C18 N6 110.7(10) . . ? N2 N1 C2 109.7(8) . . ? N2 N1 C3 123.0(7) . . ? C2 N1 C3 127.2(8) . . ? C1 N2 N1 104.3(8) . . ? C1 N2 Ag2 120.2(7) . . ? N1 N2 Ag2 130.1(6) . . ? C2 N3 C1 104.7(9) . . ? C2 N3 Ag1 128.9(7) . . ? C1 N3 Ag1 123.6(7) . . ? C18 N4 N5 110.0(9) . . ? C18 N4 C14 129.8(9) . . ? N5 N4 C14 120.1(8) . . ? C17 N5 N4 102.6(10) . . ? C18 N6 C17 103.2(10) . . ? C18 N6 Ag2 123.3(8) . 2_655 ? C17 N6 Ag2 128.2(8) . 2_655 ? C15 N7 N8 110.4(8) . . ? C15 N7 C12 127.2(8) . . ? N8 N7 C12 122.4(8) . . ? C16 N8 N7 103.8(9) . . ? C16 N8 Ag2 112.8(9) . . ? N7 N8 Ag2 131.6(6) . . ? C15 N9 C16 104.6(9) . . ? C15 N9 Ag1 130.6(7) . 2_556 ? C16 N9 Ag1 121.1(8) . 2_556 ? Mo3 O1 Mo2 92.6(2) . . ? Mo3 O1 Mo4 91.9(2) . . ? Mo2 O1 Mo4 162.4(3) . . ? Mo3 O1 Mo3 104.5(2) . 2_545 ? Mo2 O1 Mo3 98.0(2) . 2_545 ? Mo4 O1 Mo3 97.3(2) . 2_545 ? Mo3 O1 Mo1 164.5(3) . . ? Mo2 O1 Mo1 85.75(18) . . ? Mo4 O1 Mo1 85.36(19) . . ? Mo3 O1 Mo1 91.0(2) 2_545 . ? Mo3 O2 Mo4 109.1(3) . . ? Mo3 O2 Mo2 109.3(2) . 2_545 ? Mo4 O2 Mo2 103.5(2) . 2_545 ? Mo4 O5 Mo1 117.3(4) . . ? Mo2 O8 Mo1 118.5(3) . . ? Mo3 O11 Mo2 108.8(3) . . ? Mo3 O11 Mo4 110.0(3) . 2_545 ? Mo2 O11 Mo4 105.6(3) . 2_545 ? Mo3 O12 Mo1 119.3(3) . 2_545 ? O7 Mo1 O6 105.6(6) . . ? O7 Mo1 O8 99.0(4) . . ? O6 Mo1 O8 103.4(3) . . ? O7 Mo1 O5 97.1(4) . . ? O6 Mo1 O5 103.3(4) . . ? O8 Mo1 O5 143.7(3) . . ? O7 Mo1 O12 164.3(5) . 2_545 ? O6 Mo1 O12 90.1(5) . 2_545 ? O8 Mo1 O12 77.9(3) . 2_545 ? O5 Mo1 O12 77.9(3) . 2_545 ? O7 Mo1 O1 95.4(5) . . ? O6 Mo1 O1 159.0(5) . . ? O8 Mo1 O1 73.0(2) . . ? O5 Mo1 O1 73.3(2) . . ? O12 Mo1 O1 68.9(2) 2_545 . ? O10 Mo2 O9 104.7(4) . . ? O10 Mo2 O8 102.8(4) . . ? O9 Mo2 O8 99.1(3) . . ? O10 Mo2 O11 97.3(3) . . ? O9 Mo2 O11 101.6(3) . . ? O8 Mo2 O11 146.3(3) . . ? O10 Mo2 O1 96.3(3) . . ? O9 Mo2 O1 158.8(3) . . ? O8 Mo2 O1 77.8(2) . . ? O11 Mo2 O1 73.3(2) . . ? O10 Mo2 O2 164.8(3) . 2_545 ? O9 Mo2 O2 87.4(3) . 2_545 ? O8 Mo2 O2 84.0(2) . 2_545 ? O11 Mo2 O2 70.8(2) . 2_545 ? O1 Mo2 O2 71.5(2) . 2_545 ? O13 Mo3 O12 103.5(3) . . ? O13 Mo3 O2 102.1(3) . . ? O12 Mo3 O2 96.6(3) . . ? O13 Mo3 O11 100.8(3) . . ? O12 Mo3 O11 96.9(3) . . ? O2 Mo3 O11 149.8(2) . . ? O13 Mo3 O1 100.3(3) . . ? O12 Mo3 O1 156.2(3) . . ? O2 Mo3 O1 79.0(2) . . ? O11 Mo3 O1 77.8(2) . . ? O13 Mo3 O1 175.6(3) . 2_545 ? O12 Mo3 O1 80.7(3) . 2_545 ? O2 Mo3 O1 78.3(2) . 2_545 ? O11 Mo3 O1 77.4(2) . 2_545 ? O1 Mo3 O1 75.5(2) . 2_545 ? O13 Mo3 Mo4 92.1(3) . . ? O12 Mo3 Mo4 132.6(2) . . ? O2 Mo3 Mo4 36.06(17) . . ? O11 Mo3 Mo4 123.96(18) . . ? O1 Mo3 Mo4 46.21(14) . . ? O1 Mo3 Mo4 85.69(14) 2_545 . ? O3 Mo4 O4 104.7(4) . . ? O3 Mo4 O5 100.2(4) . . ? O4 Mo4 O5 101.6(3) . . ? O3 Mo4 O2 97.2(3) . . ? O4 Mo4 O2 99.5(3) . . ? O5 Mo4 O2 148.1(3) . . ? O3 Mo4 O1 92.8(3) . . ? O4 Mo4 O1 162.0(3) . . ? O5 Mo4 O1 78.9(2) . . ? O2 Mo4 O1 73.7(2) . . ? O3 Mo4 O11 163.3(3) . 2_545 ? O4 Mo4 O11 89.9(3) . 2_545 ? O5 Mo4 O11 84.3(3) . 2_545 ? O2 Mo4 O11 72.0(2) . 2_545 ? O1 Mo4 O11 72.1(2) . 2_545 ? O3 Mo4 Mo3 85.0(3) . . ? O4 Mo4 Mo3 134.4(2) . . ? O5 Mo4 Mo3 120.8(2) . . ? O2 Mo4 Mo3 34.88(16) . . ? O1 Mo4 Mo3 41.89(14) . . ? O11 Mo4 Mo3 78.90(15) 2_545 . ? N9 Ag1 N3 171.9(4) 2_556 . ? N6 Ag2 N2 155.9(4) 2_655 . ? N6 Ag2 N8 90.0(4) 2_655 . ? N2 Ag2 N8 109.4(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 67.21 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.279 _refine_diff_density_min -1.981 _refine_diff_density_rms 0.236