# 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 'Enbo Wang' _publ_contact_author_email WANGEB889@NENU.EDU.CN _publ_section_title ; Two new cantilever-type polyoxometalates constructed from {Mo2O4}2+ fragments and diphosphonates ; loop_ _publ_author_name 'Enbo Wang' 'Wei-Lin Chen' 'Yangguang Li' 'Ding Liu' 'Huaqiao Tan' # Attachment 'Crystal_structure_datas_1_and_2.cif' # Supplementary Material (ESI) for Dalton Transactions # This journal is ?The Royal Society of Chemistry 2009 data_web1 _database_code_depnum_ccdc_archive 'CCDC 736750' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H36 Mo4 N Na5 O39 P4 V' _chemical_formula_weight 1395.87 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.964(3) _cell_length_b 19.451(4) _cell_length_c 12.282(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2141.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2086 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 25.49 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1370 _exptl_absorpt_coefficient_mu 1.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 16144 _diffrn_reflns_av_R_equivalents 0.1192 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.49 _reflns_number_total 2086 _reflns_number_gt 1532 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+9.9447P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 2086 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1243 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Mo1 Mo 0.64502(9) 0.17377(4) 0.0000 0.0117(2) Uani 1 2 d S . . Mo2 Mo 0.34643(10) 0.26554(4) 0.0000 0.0138(2) Uani 1 2 d S . . V1 V 0.5000 0.0000 0.0000 0.0106(5) Uani 1 4 d S . . P1 P 0.31044(19) 0.11617(9) 0.12286(14) 0.0113(4) Uani 1 1 d . . . O1 O 0.2995(6) 0.3142(3) 0.1107(4) 0.0255(12) Uani 1 1 d . . . O2 O 0.4321(5) 0.1728(2) 0.1089(4) 0.0135(10) Uani 1 1 d . . . O3 O 0.7566(5) 0.1876(3) -0.1121(4) 0.0213(11) Uani 1 1 d . . . O4 O 0.2182(6) 0.1296(3) 0.2224(4) 0.0192(11) Uani 1 1 d . . . O5 O 0.3764(5) 0.0436(2) 0.1188(4) 0.0140(10) Uani 1 1 d . . . O6 O 0.6262(7) 0.0824(3) 0.0000 0.0129(14) Uani 1 2 d S . . O7 O 0.1743(7) 0.2037(3) 0.0000 0.0150(15) Uani 1 2 d S . . O8 O 0.5532(8) 0.2687(4) 0.0000 0.0179(15) Uani 1 2 d S . . C1 C 0.1974(10) 0.1305(5) 0.0000 0.0100(19) Uani 1 2 d S . . C2 C 0.0548(12) 0.0911(6) 0.0000 0.020(2) Uani 1 2 d S . . H2A H 0.0761 0.0428 0.0000 0.020 Uiso 1 2 calc SR . . H2B H -0.0018 0.1026 -0.0638 0.020 Uiso 0.50 1 calc PR . . H2C H -0.0018 0.1026 0.0638 0.020 Uiso 0.50 1 calc PR . . Na1 Na 0.5000 0.5000 0.0000 0.0322(15) Uani 1 4 d S . . O5W O 0.0215(7) 0.2444(3) 0.2064(5) 0.0363(15) Uiso 0.75 1 d P A 1 N1 N 0.0215(7) 0.2444(3) 0.2064(5) 0.0363(15) Uiso 0.25 1 d P B 2 O4W O 0.2487(11) 0.4601(5) 0.0000 0.044(2) Uani 1 2 d S . . Na2 Na 0.2187(9) 0.4359(4) 0.2422(6) 0.117(2) Uani 1 1 d . . . O3W O 0.5292(13) 0.4715(6) 0.1929(9) 0.034(3) Uani 0.50 1 d P . . O2W O -0.0402(11) 0.3902(7) 0.1113(7) 0.111(5) Uani 1 1 d . . . O1W O 0.6251(17) 0.4017(7) 0.0702(11) 0.049(4) 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 Mo1 0.0095(4) 0.0104(4) 0.0152(4) 0.000 0.000 -0.0004(3) Mo2 0.0136(4) 0.0086(4) 0.0193(4) 0.000 0.000 0.0018(3) V1 0.0119(11) 0.0095(11) 0.0104(11) 0.000 0.000 0.0028(9) P1 0.0128(8) 0.0098(8) 0.0112(8) 0.0004(7) 0.0027(7) -0.0004(7) O1 0.022(3) 0.021(3) 0.033(3) -0.014(2) 0.006(2) 0.002(2) O2 0.015(2) 0.013(2) 0.013(2) -0.0018(19) -0.0007(19) 0.0003(19) O3 0.018(3) 0.019(3) 0.027(3) 0.001(2) 0.011(2) -0.001(2) O4 0.023(3) 0.019(3) 0.016(2) 0.003(2) 0.007(2) 0.000(2) O5 0.016(2) 0.010(2) 0.016(2) 0.002(2) 0.0004(19) 0.0014(19) O6 0.007(3) 0.014(3) 0.018(3) 0.000 0.000 -0.001(3) O7 0.017(4) 0.008(3) 0.020(3) 0.000 0.000 0.008(3) O8 0.020(4) 0.013(4) 0.021(4) 0.000 0.000 -0.001(3) C1 0.008(4) 0.007(5) 0.015(4) 0.000 0.000 0.001(4) C2 0.017(5) 0.022(5) 0.020(5) 0.000 0.000 0.002(4) Na1 0.040(4) 0.028(4) 0.028(3) 0.000 0.000 -0.001(3) O4W 0.041(6) 0.050(6) 0.043(5) 0.000 0.000 -0.017(5) Na2 0.142(6) 0.097(5) 0.112(5) -0.009(4) 0.035(5) -0.001(5) O3W 0.035(7) 0.035(7) 0.033(6) 0.007(5) -0.008(6) 0.005(5) O2W 0.080(6) 0.212(14) 0.042(5) 0.019(6) -0.001(5) -0.065(8) O1W 0.075(10) 0.034(7) 0.039(8) 0.018(6) -0.005(7) -0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O3 1.723(5) 6 ? Mo1 O3 1.723(5) . ? Mo1 O6 1.786(7) . ? Mo1 O8 2.021(7) . ? Mo1 O2 2.330(5) 6 ? Mo1 O2 2.330(5) . ? Mo1 Mo2 3.2171(14) . ? Mo2 O1 1.708(5) 6 ? Mo2 O1 1.708(5) . ? Mo2 O8 1.855(7) . ? Mo2 O7 1.956(7) . ? Mo2 O2 2.373(5) 6 ? Mo2 O2 2.373(5) . ? V1 O6 1.961(6) 5_655 ? V1 O6 1.961(6) . ? V1 O5 2.019(5) 6 ? V1 O5 2.019(5) 5_655 ? V1 O5 2.019(5) . ? V1 O5 2.019(5) 2_655 ? P1 O4 1.499(5) . ? P1 O5 1.531(5) . ? P1 O2 1.560(5) . ? P1 C1 1.839(5) . ? O1 Na2 2.958(8) . ? O3 Na2 3.015(9) 8_665 ? O5 Na2 2.833(8) 4_545 ? O7 C1 1.438(11) . ? C1 C2 1.490(14) . ? C1 P1 1.839(5) 6 ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? Na1 O1W 2.378(13) 6 ? Na1 O1W 2.378(13) . ? Na1 O1W 2.378(13) 5_665 ? Na1 O1W 2.378(13) 2_665 ? Na1 O4W 2.383(9) . ? Na1 O4W 2.383(9) 5_665 ? Na1 O3W 2.447(11) 6 ? Na1 O3W 2.447(11) 5_665 ? Na1 O3W 2.447(11) . ? Na1 O3W 2.447(11) 2_665 ? Na1 Na2 4.094(7) 6 ? Na1 Na2 4.094(7) 2_665 ? Na2 O5 2.833(8) 4 ? Na2 O3W 2.931(15) . ? Na2 O3W 2.952(14) 2_665 ? Na2 O2W 2.960(12) . ? Na2 O3 3.015(9) 8_566 ? O3W O3W 1.23(2) 2_665 ? O3W Na2 2.952(14) 2_665 ? O1W O1W 1.72(3) 6 ? 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 O3 Mo1 O3 106.1(3) 6 . ? O3 Mo1 O6 102.1(2) 6 . ? O3 Mo1 O6 102.1(2) . . ? O3 Mo1 O8 95.4(2) 6 . ? O3 Mo1 O8 95.4(2) . . ? O6 Mo1 O8 150.5(3) . . ? O3 Mo1 O2 159.3(2) 6 6 ? O3 Mo1 O2 91.0(2) . 6 ? O6 Mo1 O2 85.1(2) . 6 ? O8 Mo1 O2 70.97(19) . 6 ? O3 Mo1 O2 91.0(2) 6 . ? O3 Mo1 O2 159.3(2) . . ? O6 Mo1 O2 85.1(2) . . ? O8 Mo1 O2 70.97(19) . . ? O2 Mo1 O2 70.0(2) 6 . ? O3 Mo1 Mo2 113.35(17) 6 . ? O3 Mo1 Mo2 113.35(17) . . ? O6 Mo1 Mo2 118.3(2) . . ? O8 Mo1 Mo2 32.3(2) . . ? O2 Mo1 Mo2 47.40(11) 6 . ? O2 Mo1 Mo2 47.40(11) . . ? O1 Mo2 O1 105.4(4) 6 . ? O1 Mo2 O8 103.2(2) 6 . ? O1 Mo2 O8 103.2(2) . . ? O1 Mo2 O7 98.4(2) 6 . ? O1 Mo2 O7 98.4(2) . . ? O8 Mo2 O7 143.9(3) . . ? O1 Mo2 O2 93.0(2) 6 6 ? O1 Mo2 O2 161.6(2) . 6 ? O8 Mo2 O2 72.6(2) . 6 ? O7 Mo2 O2 77.76(19) . 6 ? O1 Mo2 O2 161.6(2) 6 . ? O1 Mo2 O2 93.0(2) . . ? O8 Mo2 O2 72.6(2) . . ? O7 Mo2 O2 77.76(19) . . ? O2 Mo2 O2 68.6(2) 6 . ? O1 Mo2 Mo1 120.80(18) 6 . ? O1 Mo2 Mo1 120.80(18) . . ? O8 Mo2 Mo1 35.6(2) . . ? O7 Mo2 Mo1 108.36(19) . . ? O2 Mo2 Mo1 46.29(11) 6 . ? O2 Mo2 Mo1 46.29(11) . . ? O6 V1 O6 180.0(4) 5_655 . ? O6 V1 O5 91.55(18) 5_655 6 ? O6 V1 O5 88.45(18) . 6 ? O6 V1 O5 88.45(18) 5_655 5_655 ? O6 V1 O5 91.55(18) . 5_655 ? O5 V1 O5 87.5(3) 6 5_655 ? O6 V1 O5 91.55(18) 5_655 . ? O6 V1 O5 88.45(18) . . ? O5 V1 O5 92.5(3) 6 . ? O5 V1 O5 180.0(4) 5_655 . ? O6 V1 O5 88.45(18) 5_655 2_655 ? O6 V1 O5 91.55(18) . 2_655 ? O5 V1 O5 180.0(3) 6 2_655 ? O5 V1 O5 92.5(3) 5_655 2_655 ? O5 V1 O5 87.5(3) . 2_655 ? O4 P1 O5 113.6(3) . . ? O4 P1 O2 110.7(3) . . ? O5 P1 O2 112.2(3) . . ? O4 P1 C1 109.8(3) . . ? O5 P1 C1 109.0(3) . . ? O2 P1 C1 100.8(3) . . ? Mo2 O1 Na2 159.8(3) . . ? P1 O2 Mo1 129.9(3) . . ? P1 O2 Mo2 111.9(2) . . ? Mo1 O2 Mo2 86.31(15) . . ? Mo1 O3 Na2 106.5(3) . 8_665 ? P1 O5 V1 128.5(3) . . ? P1 O5 Na2 123.1(3) . 4_545 ? V1 O5 Na2 106.8(2) . 4_545 ? Mo1 O6 V1 150.2(4) . . ? C1 O7 Mo2 119.7(5) . . ? Mo2 O8 Mo1 112.1(3) . . ? O7 C1 C2 112.7(8) . . ? O7 C1 P1 103.3(4) . . ? C2 C1 P1 113.2(4) . . ? O7 C1 P1 103.3(4) . 6 ? C2 C1 P1 113.2(4) . 6 ? P1 C1 P1 110.3(5) . 6 ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1W Na1 O1W 42.5(7) 6 . ? O1W Na1 O1W 137.5(7) 6 5_665 ? O1W Na1 O1W 180.000(2) . 5_665 ? O1W Na1 O1W 180.000(2) 6 2_665 ? O1W Na1 O1W 137.5(7) . 2_665 ? O1W Na1 O1W 42.5(7) 5_665 2_665 ? O1W Na1 O4W 100.6(4) 6 . ? O1W Na1 O4W 100.6(4) . . ? O1W Na1 O4W 79.4(4) 5_665 . ? O1W Na1 O4W 79.4(4) 2_665 . ? O1W Na1 O4W 79.4(4) 6 5_665 ? O1W Na1 O4W 79.4(4) . 5_665 ? O1W Na1 O4W 100.6(4) 5_665 5_665 ? O1W Na1 O4W 100.6(4) 2_665 5_665 ? O4W Na1 O4W 180.0(4) . 5_665 ? O1W Na1 O3W 54.3(4) 6 6 ? O1W Na1 O3W 96.8(4) . 6 ? O1W Na1 O3W 83.2(4) 5_665 6 ? O1W Na1 O3W 125.7(4) 2_665 6 ? O4W Na1 O3W 91.6(3) . 6 ? O4W Na1 O3W 88.4(3) 5_665 6 ? O1W Na1 O3W 83.2(4) 6 5_665 ? O1W Na1 O3W 125.7(4) . 5_665 ? O1W Na1 O3W 54.3(4) 5_665 5_665 ? O1W Na1 O3W 96.8(4) 2_665 5_665 ? O4W Na1 O3W 88.4(3) . 5_665 ? O4W Na1 O3W 91.6(3) 5_665 5_665 ? O3W Na1 O3W 29.0(5) 6 5_665 ? O1W Na1 O3W 96.8(4) 6 . ? O1W Na1 O3W 54.3(4) . . ? O1W Na1 O3W 125.7(4) 5_665 . ? O1W Na1 O3W 83.2(4) 2_665 . ? O4W Na1 O3W 91.6(3) . . ? O4W Na1 O3W 88.4(3) 5_665 . ? O3W Na1 O3W 151.0(5) 6 . ? O3W Na1 O3W 180.0(5) 5_665 . ? O1W Na1 O3W 125.7(4) 6 2_665 ? O1W Na1 O3W 83.2(4) . 2_665 ? O1W Na1 O3W 96.8(4) 5_665 2_665 ? O1W Na1 O3W 54.3(4) 2_665 2_665 ? O4W Na1 O3W 88.4(3) . 2_665 ? O4W Na1 O3W 91.6(3) 5_665 2_665 ? O3W Na1 O3W 180.0(5) 6 2_665 ? O3W Na1 O3W 151.0(5) 5_665 2_665 ? O3W Na1 O3W 29.0(5) . 2_665 ? O1W Na1 Na2 77.4(4) 6 6 ? O1W Na1 Na2 108.0(3) . 6 ? O1W Na1 Na2 72.0(3) 5_665 6 ? O1W Na1 Na2 102.6(4) 2_665 6 ? O4W Na1 Na2 47.04(12) . 6 ? O4W Na1 Na2 132.96(12) 5_665 6 ? O3W Na1 Na2 45.0(3) 6 6 ? O3W Na1 Na2 45.5(3) 5_665 6 ? O3W Na1 Na2 134.5(3) . 6 ? O3W Na1 Na2 135.0(3) 2_665 6 ? O1W Na1 Na2 102.6(4) 6 2_665 ? O1W Na1 Na2 72.0(3) . 2_665 ? O1W Na1 Na2 108.0(3) 5_665 2_665 ? O1W Na1 Na2 77.4(4) 2_665 2_665 ? O4W Na1 Na2 132.96(12) . 2_665 ? O4W Na1 Na2 47.04(12) 5_665 2_665 ? O3W Na1 Na2 135.0(3) 6 2_665 ? O3W Na1 Na2 134.5(3) 5_665 2_665 ? O3W Na1 Na2 45.5(3) . 2_665 ? O3W Na1 Na2 45.0(3) 2_665 2_665 ? Na2 Na1 Na2 180.00(14) 6 2_665 ? O5 Na2 O3W 103.6(3) 4 . ? O5 Na2 O3W 84.4(3) 4 2_665 ? O3W Na2 O3W 24.0(4) . 2_665 ? O5 Na2 O1 174.3(3) 4 . ? O3W Na2 O1 81.0(3) . . ? O3W Na2 O1 100.9(3) 2_665 . ? O5 Na2 O2W 108.3(4) 4 . ? O3W Na2 O2W 134.7(4) . . ? O3W Na2 O2W 132.2(4) 2_665 . ? O1 Na2 O2W 69.8(3) . . ? O5 Na2 O3 105.4(3) 4 8_566 ? O3W Na2 O3 101.7(3) . 8_566 ? O3W Na2 O3 121.4(4) 2_665 8_566 ? O1 Na2 O3 70.0(2) . 8_566 ? O2W Na2 O3 99.9(3) . 8_566 ? O5 Na2 Na1 113.5(2) 4 . ? O3W Na2 Na1 36.2(2) . . ? O3W Na2 Na1 36.3(2) 2_665 . ? O1 Na2 Na1 72.29(17) . . ? O2W Na2 Na1 100.3(2) . . ? O3 Na2 Na1 127.2(2) 8_566 . ? O3W O3W Na1 75.5(3) 2_665 . ? O3W O3W Na2 79.0(11) 2_665 . ? Na1 O3W Na2 98.7(4) . . ? O3W O3W Na2 77.0(11) 2_665 2_665 ? Na1 O3W Na2 98.2(4) . 2_665 ? Na2 O3W Na2 145.9(5) . 2_665 ? O1W O1W Na1 68.7(3) 6 . ? 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 O3 Mo1 Mo2 O1 128.3(3) 6 . . 6 ? O3 Mo1 Mo2 O1 7.3(3) . . . 6 ? O6 Mo1 Mo2 O1 -112.2(2) . . . 6 ? O8 Mo1 Mo2 O1 67.8(2) . . . 6 ? O2 Mo1 Mo2 O1 -60.9(3) 6 . . 6 ? O2 Mo1 Mo2 O1 -163.4(3) . . . 6 ? O3 Mo1 Mo2 O1 -7.3(3) 6 . . . ? O3 Mo1 Mo2 O1 -128.3(3) . . . . ? O6 Mo1 Mo2 O1 112.2(2) . . . . ? O8 Mo1 Mo2 O1 -67.8(2) . . . . ? O2 Mo1 Mo2 O1 163.4(3) 6 . . . ? O2 Mo1 Mo2 O1 60.9(3) . . . . ? O3 Mo1 Mo2 O8 60.50(19) 6 . . . ? O3 Mo1 Mo2 O8 -60.50(19) . . . . ? O6 Mo1 Mo2 O8 180.0 . . . . ? O2 Mo1 Mo2 O8 -128.78(15) 6 . . . ? O2 Mo1 Mo2 O8 128.78(15) . . . . ? O3 Mo1 Mo2 O7 -119.50(19) 6 . . . ? O3 Mo1 Mo2 O7 119.50(19) . . . . ? O6 Mo1 Mo2 O7 0.0 . . . . ? O8 Mo1 Mo2 O7 180.0 . . . . ? O2 Mo1 Mo2 O7 51.22(15) 6 . . . ? O2 Mo1 Mo2 O7 -51.22(15) . . . . ? O3 Mo1 Mo2 O2 -170.7(2) 6 . . 6 ? O3 Mo1 Mo2 O2 68.3(2) . . . 6 ? O6 Mo1 Mo2 O2 -51.22(15) . . . 6 ? O8 Mo1 Mo2 O2 128.78(15) . . . 6 ? O2 Mo1 Mo2 O2 -102.4(3) . . . 6 ? O3 Mo1 Mo2 O2 -68.3(2) 6 . . . ? O3 Mo1 Mo2 O2 170.7(2) . . . . ? O6 Mo1 Mo2 O2 51.22(15) . . . . ? O8 Mo1 Mo2 O2 -128.78(15) . . . . ? O2 Mo1 Mo2 O2 102.4(3) 6 . . . ? O1 Mo2 O1 Na2 -17.1(11) 6 . . . ? O8 Mo2 O1 Na2 90.8(9) . . . . ? O7 Mo2 O1 Na2 -118.3(9) . . . . ? O2 Mo2 O1 Na2 165.3(7) 6 . . . ? O2 Mo2 O1 Na2 163.6(9) . . . . ? Mo1 Mo2 O1 Na2 124.4(9) . . . . ? O4 P1 O2 Mo1 164.6(3) . . . . ? O5 P1 O2 Mo1 36.7(4) . . . . ? C1 P1 O2 Mo1 -79.2(4) . . . . ? O4 P1 O2 Mo2 -91.2(3) . . . . ? O5 P1 O2 Mo2 140.9(2) . . . . ? C1 P1 O2 Mo2 25.0(3) . . . . ? O3 Mo1 O2 P1 -122.9(4) 6 . . . ? O3 Mo1 O2 P1 90.9(7) . . . . ? O6 Mo1 O2 P1 -20.8(3) . . . . ? O8 Mo1 O2 P1 141.8(4) . . . . ? O2 Mo1 O2 P1 65.7(4) 6 . . . ? Mo2 Mo1 O2 P1 115.6(4) . . . . ? O3 Mo1 O2 Mo2 121.5(2) 6 . . . ? O3 Mo1 O2 Mo2 -24.7(6) . . . . ? O6 Mo1 O2 Mo2 -136.44(16) . . . . ? O8 Mo1 O2 Mo2 26.13(15) . . . . ? O2 Mo1 O2 Mo2 -49.89(16) 6 . . . ? O1 Mo2 O2 P1 -80.8(7) 6 . . . ? O1 Mo2 O2 P1 96.9(3) . . . . ? O8 Mo2 O2 P1 -160.2(3) . . . . ? O7 Mo2 O2 P1 -1.0(2) . . . . ? O2 Mo2 O2 P1 -82.5(3) 6 . . . ? Mo1 Mo2 O2 P1 -131.8(3) . . . . ? O1 Mo2 O2 Mo1 51.0(7) 6 . . . ? O1 Mo2 O2 Mo1 -131.2(2) . . . . ? O8 Mo2 O2 Mo1 -28.38(15) . . . . ? O7 Mo2 O2 Mo1 130.79(16) . . . . ? O2 Mo2 O2 Mo1 49.30(16) 6 . . . ? O3 Mo1 O3 Na2 129.4(2) 6 . . 8_665 ? O6 Mo1 O3 Na2 22.8(3) . . . 8_665 ? O8 Mo1 O3 Na2 -133.4(3) . . . 8_665 ? O2 Mo1 O3 Na2 -62.4(3) 6 . . 8_665 ? O2 Mo1 O3 Na2 -85.9(6) . . . 8_665 ? Mo2 Mo1 O3 Na2 -105.5(2) . . . 8_665 ? O4 P1 O5 V1 177.3(3) . . . . ? O2 P1 O5 V1 -56.3(4) . . . . ? C1 P1 O5 V1 54.4(4) . . . . ? O4 P1 O5 Na2 13.4(4) . . . 4_545 ? O2 P1 O5 Na2 139.8(3) . . . 4_545 ? C1 P1 O5 Na2 -109.4(4) . . . 4_545 ? O6 V1 O5 P1 -131.0(3) 5_655 . . . ? O6 V1 O5 P1 49.0(3) . . . . ? O5 V1 O5 P1 -39.4(4) 6 . . . ? O5 V1 O5 P1 178(100) 5_655 . . . ? O5 V1 O5 P1 140.6(4) 2_655 . . . ? O6 V1 O5 Na2 34.8(3) 5_655 . . 4_545 ? O6 V1 O5 Na2 -145.2(3) . . . 4_545 ? O5 V1 O5 Na2 126.5(2) 6 . . 4_545 ? O5 V1 O5 Na2 -17(100) 5_655 . . 4_545 ? O5 V1 O5 Na2 -53.5(2) 2_655 . . 4_545 ? O3 Mo1 O6 V1 125.18(18) 6 . . . ? O3 Mo1 O6 V1 -125.18(18) . . . . ? O8 Mo1 O6 V1 0.0 . . . . ? O2 Mo1 O6 V1 -35.17(11) 6 . . . ? O2 Mo1 O6 V1 35.17(11) . . . . ? Mo2 Mo1 O6 V1 0.0 . . . . ? O6 V1 O6 Mo1 -107(100) 5_655 . . . ? O5 V1 O6 Mo1 46.29(13) 6 . . . ? O5 V1 O6 Mo1 133.71(13) 5_655 . . . ? O5 V1 O6 Mo1 -46.29(13) . . . . ? O5 V1 O6 Mo1 -133.71(13) 2_655 . . . ? O1 Mo2 O7 C1 126.47(19) 6 . . . ? O1 Mo2 O7 C1 -126.47(19) . . . . ? O8 Mo2 O7 C1 0.0 . . . . ? O2 Mo2 O7 C1 35.21(11) 6 . . . ? O2 Mo2 O7 C1 -35.21(11) . . . . ? Mo1 Mo2 O7 C1 0.0 . . . . ? O1 Mo2 O8 Mo1 -125.2(2) 6 . . . ? O1 Mo2 O8 Mo1 125.2(2) . . . . ? O7 Mo2 O8 Mo1 0.0 . . . . ? O2 Mo2 O8 Mo1 -36.18(12) 6 . . . ? O2 Mo2 O8 Mo1 36.18(12) . . . . ? O3 Mo1 O8 Mo2 -126.62(18) 6 . . . ? O3 Mo1 O8 Mo2 126.62(18) . . . . ? O6 Mo1 O8 Mo2 0.0 . . . . ? O2 Mo1 O8 Mo2 37.37(12) 6 . . . ? O2 Mo1 O8 Mo2 -37.37(12) . . . . ? Mo2 O7 C1 C2 180.0 . . . . ? Mo2 O7 C1 P1 57.5(3) . . . . ? Mo2 O7 C1 P1 -57.5(3) . . . 6 ? O4 P1 C1 O7 68.9(5) . . . . ? O5 P1 C1 O7 -166.0(4) . . . . ? O2 P1 C1 O7 -47.9(5) . . . . ? O4 P1 C1 C2 -53.2(7) . . . . ? O5 P1 C1 C2 71.8(6) . . . . ? O2 P1 C1 C2 -170.0(6) . . . . ? O4 P1 C1 P1 178.7(4) . . . 6 ? O5 P1 C1 P1 -56.2(5) . . . 6 ? O2 P1 C1 P1 61.9(5) . . . 6 ? Mo2 O1 Na2 O5 147(3) . . . 4 ? Mo2 O1 Na2 O3W -69.3(10) . . . . ? Mo2 O1 Na2 O3W -55.7(10) . . . 2_665 ? Mo2 O1 Na2 O2W 75.5(9) . . . . ? Mo2 O1 Na2 O3 -175.4(9) . . . 8_566 ? Mo2 O1 Na2 Na1 -33.1(9) . . . . ? O1W Na1 Na2 O5 162.4(4) 6 . . 4 ? O1W Na1 Na2 O5 132.5(4) . . . 4 ? O1W Na1 Na2 O5 -47.5(4) 5_665 . . 4 ? O1W Na1 Na2 O5 -17.6(4) 2_665 . . 4 ? O4W Na1 Na2 O5 -109.8(5) . . . 4 ? O4W Na1 Na2 O5 70.2(5) 5_665 . . 4 ? O3W Na1 Na2 O5 -140.3(4) 6 . . 4 ? O3W Na1 Na2 O5 -99.1(5) 5_665 . . 4 ? O3W Na1 Na2 O5 80.9(5) . . . 4 ? O3W Na1 Na2 O5 39.7(4) 2_665 . . 4 ? Na2 Na1 Na2 O5 -119.8(2) 6 . . 4 ? Na2 Na1 Na2 O5 60.2(2) 2_665 . . 4 ? O1W Na1 Na2 O3W 81.4(5) 6 . . . ? O1W Na1 Na2 O3W 51.5(5) . . . . ? O1W Na1 Na2 O3W -128.5(5) 5_665 . . . ? O1W Na1 Na2 O3W -98.6(5) 2_665 . . . ? O4W Na1 Na2 O3W 169.2(5) . . . . ? O4W Na1 Na2 O3W -10.8(5) 5_665 . . . ? O3W Na1 Na2 O3W 138.7(7) 6 . . . ? O3W Na1 Na2 O3W 180.0 5_665 . . . ? O3W Na1 Na2 O3W -41.3(7) 2_665 . . . ? Na2 Na1 Na2 O3W 159.3(4) 6 . . . ? Na2 Na1 Na2 O3W -20.7(4) 2_665 . . . ? O1W Na1 Na2 O3W 122.7(5) 6 . . 2_665 ? O1W Na1 Na2 O3W 92.8(5) . . . 2_665 ? O1W Na1 Na2 O3W -87.2(5) 5_665 . . 2_665 ? O1W Na1 Na2 O3W -57.3(5) 2_665 . . 2_665 ? O4W Na1 Na2 O3W -149.5(5) . . . 2_665 ? O4W Na1 Na2 O3W 30.5(5) 5_665 . . 2_665 ? O3W Na1 Na2 O3W 180.000(1) 6 . . 2_665 ? O3W Na1 Na2 O3W -138.7(7) 5_665 . . 2_665 ? O3W Na1 Na2 O3W 41.3(7) . . . 2_665 ? Na2 Na1 Na2 O3W -159.5(4) 6 . . 2_665 ? Na2 Na1 Na2 O3W 20.5(4) 2_665 . . 2_665 ? O1W Na1 Na2 O1 -17.6(4) 6 . . . ? O1W Na1 Na2 O1 -47.6(4) . . . . ? O1W Na1 Na2 O1 132.4(4) 5_665 . . . ? O1W Na1 Na2 O1 162.4(4) 2_665 . . . ? O4W Na1 Na2 O1 70.2(4) . . . . ? O4W Na1 Na2 O1 -109.8(4) 5_665 . . . ? O3W Na1 Na2 O1 39.7(4) 6 . . . ? O3W Na1 Na2 O1 80.9(4) 5_665 . . . ? O3W Na1 Na2 O1 -99.1(4) . . . . ? O3W Na1 Na2 O1 -140.3(4) 2_665 . . . ? Na2 Na1 Na2 O1 60.2(2) 6 . . . ? Na2 Na1 Na2 O1 -119.8(2) 2_665 . . . ? O1W Na1 Na2 O2W -82.4(5) 6 . . . ? O1W Na1 Na2 O2W -112.3(5) . . . . ? O1W Na1 Na2 O2W 67.7(5) 5_665 . . . ? O1W Na1 Na2 O2W 97.6(5) 2_665 . . . ? O4W Na1 Na2 O2W 5.4(4) . . . . ? O4W Na1 Na2 O2W -174.6(4) 5_665 . . . ? O3W Na1 Na2 O2W -25.1(5) 6 . . . ? O3W Na1 Na2 O2W 16.2(5) 5_665 . . . ? O3W Na1 Na2 O2W -163.8(5) . . . . ? O3W Na1 Na2 O2W 154.9(5) 2_665 . . . ? Na2 Na1 Na2 O2W -4.5(4) 6 . . . ? Na2 Na1 Na2 O2W 175.5(4) 2_665 . . . ? O1W Na1 Na2 O3 28.5(5) 6 . . 8_566 ? O1W Na1 Na2 O3 -1.4(4) . . . 8_566 ? O1W Na1 Na2 O3 178.6(4) 5_665 . . 8_566 ? O1W Na1 Na2 O3 -151.5(5) 2_665 . . 8_566 ? O4W Na1 Na2 O3 116.3(5) . . . 8_566 ? O4W Na1 Na2 O3 -63.7(5) 5_665 . . 8_566 ? O3W Na1 Na2 O3 85.8(5) 6 . . 8_566 ? O3W Na1 Na2 O3 127.1(5) 5_665 . . 8_566 ? O3W Na1 Na2 O3 -52.9(5) . . . 8_566 ? O3W Na1 Na2 O3 -94.2(5) 2_665 . . 8_566 ? Na2 Na1 Na2 O3 106.4(3) 6 . . 8_566 ? Na2 Na1 Na2 O3 -73.6(3) 2_665 . . 8_566 ? O1W Na1 O3W O3W 175.2(11) 6 . . 2_665 ? O1W Na1 O3W O3W 174.1(14) . . . 2_665 ? O1W Na1 O3W O3W -5.9(14) 5_665 . . 2_665 ? O1W Na1 O3W O3W -4.8(11) 2_665 . . 2_665 ? O4W Na1 O3W O3W -84.0(11) . . . 2_665 ? O4W Na1 O3W O3W 96.0(11) 5_665 . . 2_665 ? O3W Na1 O3W O3W 180.000(4) 6 . . 2_665 ? O3W Na1 O3W O3W 108(100) 5_665 . . 2_665 ? Na2 Na1 O3W O3W -105.8(11) 6 . . 2_665 ? Na2 Na1 O3W O3W 74.2(11) 2_665 . . 2_665 ? O1W Na1 O3W Na2 -108.7(5) 6 . . . ? O1W Na1 O3W Na2 -109.8(6) . . . . ? O1W Na1 O3W Na2 70.2(6) 5_665 . . . ? O1W Na1 O3W Na2 71.3(5) 2_665 . . . ? O4W Na1 O3W Na2 -7.9(4) . . . . ? O4W Na1 O3W Na2 172.1(4) 5_665 . . . ? O3W Na1 O3W Na2 -103.9(11) 6 . . . ? O3W Na1 O3W Na2 -176(100) 5_665 . . . ? O3W Na1 O3W Na2 76.1(11) 2_665 . . . ? Na2 Na1 O3W Na2 -29.7(5) 6 . . . ? Na2 Na1 O3W Na2 150.3(5) 2_665 . . . ? O1W Na1 O3W Na2 100.9(5) 6 . . 2_665 ? O1W Na1 O3W Na2 99.9(6) . . . 2_665 ? O1W Na1 O3W Na2 -80.1(6) 5_665 . . 2_665 ? O1W Na1 O3W Na2 -79.1(5) 2_665 . . 2_665 ? O4W Na1 O3W Na2 -158.2(4) . . . 2_665 ? O4W Na1 O3W Na2 21.8(4) 5_665 . . 2_665 ? O3W Na1 O3W Na2 105.8(11) 6 . . 2_665 ? O3W Na1 O3W Na2 33(100) 5_665 . . 2_665 ? O3W Na1 O3W Na2 -74.2(11) 2_665 . . 2_665 ? Na2 Na1 O3W Na2 180.0 6 . . 2_665 ? O5 Na2 O3W O3W -38.0(3) 4 . . 2_665 ? O1 Na2 O3W O3W 145.5(3) . . . 2_665 ? O2W Na2 O3W O3W 95.9(6) . . . 2_665 ? O3 Na2 O3W O3W -147.2(3) 8_566 . . 2_665 ? Na1 Na2 O3W O3W 73.2(3) . . . 2_665 ? O5 Na2 O3W Na1 -111.2(4) 4 . . . ? O3W Na2 O3W Na1 -73.2(3) 2_665 . . . ? O1 Na2 O3W Na1 72.3(3) . . . . ? O2W Na2 O3W Na1 22.7(7) . . . . ? O3 Na2 O3W Na1 139.5(3) 8_566 . . . ? O5 Na2 O3W Na2 7.8(9) 4 . . 2_665 ? O3W Na2 O3W Na2 45.7(8) 2_665 . . 2_665 ? O1 Na2 O3W Na2 -168.8(8) . . . 2_665 ? O2W Na2 O3W Na2 141.7(8) . . . 2_665 ? O3 Na2 O3W Na2 -101.5(7) 8_566 . . 2_665 ? Na1 Na2 O3W Na2 119.0(9) . . . 2_665 ? O1W Na1 O1W O1W -153(100) 5_665 . . 6 ? O1W Na1 O1W O1W 180.000(2) 2_665 . . 6 ? O4W Na1 O1W O1W 94.18(17) . . . 6 ? O4W Na1 O1W O1W -85.82(17) 5_665 . . 6 ? O3W Na1 O1W O1W 1.3(3) 6 . . 6 ? O3W Na1 O1W O1W -1.6(4) 5_665 . . 6 ? O3W Na1 O1W O1W 178.4(4) . . . 6 ? O3W Na1 O1W O1W -178.7(3) 2_665 . . 6 ? Na2 Na1 O1W O1W 46.10(15) 6 . . 6 ? Na2 Na1 O1W O1W -133.90(15) 2_665 . . 6 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.773 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.175 data_web2 _database_code_depnum_ccdc_archive 'CCDC 736751' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H46 Mo4 N6 O32 P4 V' _chemical_formula_weight 1297.09 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.056(2) _cell_length_b 17.233(3) _cell_length_c 11.722(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.27(3) _cell_angle_gamma 90.00 _cell_volume 2210.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3882 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.949 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1286 _exptl_absorpt_coefficient_mu 1.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 0.734 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 17042 _diffrn_reflns_av_R_equivalents 0.1151 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3882 _reflns_number_gt 2651 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+9.9308P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 3882 _refine_ls_number_parameters 277 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1951 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.107 _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 Mo1 Mo -0.23335(9) 0.67987(5) 0.76620(7) 0.0263(3) Uani 1 1 d . . . Mo2 Mo -0.14856(10) 0.68431(5) 0.51565(8) 0.0300(3) Uani 1 1 d . . . V1 V 0.0000 0.5000 0.5000 0.0234(6) Uani 1 2 d S . . P2 P 0.0126(3) 0.57886(15) 0.7485(2) 0.0214(6) Uani 1 1 d . . . P1 P -0.2280(3) 0.50856(15) 0.6432(2) 0.0239(6) Uani 1 1 d . . . O13 O 0.0744(6) 0.5374(4) 0.6575(5) 0.0245(16) Uani 1 1 d . . . O12 O 0.1566(7) 0.5309(4) 0.4437(5) 0.0242(16) Uani 1 1 d . . . O11 O -0.3847(8) 0.6803(5) 0.7781(7) 0.042(2) Uani 1 1 d . . . O10 O -0.0681(7) 0.6026(4) 0.4686(6) 0.0301(18) Uani 1 1 d . . . O9 O -0.0501(7) 0.6557(4) 0.6998(6) 0.0252(16) Uani 1 1 d . . . O8 O 0.0963(7) 0.5911(4) 0.8585(6) 0.0278(17) Uani 1 1 d . . . O7 O -0.0524(10) 0.7590(5) 0.4956(8) 0.053(3) Uani 1 1 d . . . O6 O -0.1854(7) 0.5812(4) 0.8387(5) 0.0269(17) Uani 1 1 d . . . O5 O -0.2597(7) 0.5953(4) 0.6082(6) 0.0267(16) Uani 1 1 d . . . C4 C -0.0412(11) 0.3840(6) 0.7998(9) 0.028(2) Uani 1 1 d . . . H4A H -0.1068 0.3554 0.7544 0.034 Uiso 1 1 calc R . . H4B H 0.0137 0.4020 0.7480 0.034 Uiso 1 1 calc R . . O4 O -0.1683(8) 0.7410(4) 0.8734(6) 0.038(2) Uani 1 1 d . . . O3 O -0.3376(7) 0.4639(5) 0.6652(6) 0.0372(19) Uani 1 1 d . . . O2 O -0.2296(7) 0.7410(4) 0.6347(6) 0.0306(18) Uani 1 1 d . . . N1 N -0.0473(8) 0.2992(5) 0.9724(7) 0.027(2) Uani 1 1 d . . . H1A H -0.0035 0.2649 1.0176 0.041 Uiso 1 1 calc R . . H1B H -0.1139 0.2763 0.9357 0.041 Uiso 1 1 calc R . . H1C H -0.0692 0.3380 1.0151 0.041 Uiso 1 1 calc R . . O1 O -0.2704(9) 0.6953(5) 0.4078(7) 0.050(2) Uani 1 1 d . . . C1 C -0.1224(10) 0.5246(6) 0.7776(8) 0.024(2) Uani 1 1 d . . . C2 C 0.0272(11) 0.3301(6) 0.8867(9) 0.032(3) Uani 1 1 d . . . H2A H 0.0579 0.2869 0.8464 0.039 Uiso 1 1 calc R . . H2B H 0.0970 0.3575 0.9275 0.039 Uiso 1 1 calc R . . C3 C -0.0946(10) 0.4535(6) 0.8535(8) 0.026(2) Uani 1 1 d . . . H3A H -0.0381 0.4688 0.9208 0.031 Uiso 1 1 calc R . . H3B H -0.1697 0.4373 0.8802 0.031 Uiso 1 1 calc R . . N3 N -0.4759(11) 0.3769(6) 0.4826(10) 0.055(3) Uani 1 1 d . . . N2 N -0.3019(12) 0.8148(7) 1.0330(10) 0.060(3) Uani 1 1 d . . . O5W O 0.3091(16) 0.6624(10) 0.7728(13) 0.041(4) Uani 0.50 1 d PU . . O6W O -0.5220(15) 0.5617(11) 0.7140(17) 0.049(5) Uani 0.50 1 d P . . O3W O -0.4202(18) 0.3777(10) 0.8297(16) 0.052(5) Uani 0.50 1 d PU . . O2W O 0.274(2) 0.4786(16) 0.9434(18) 0.082(8) Uani 0.50 1 d P . . O1W O 0.327(2) 0.4761(12) 0.6824(18) 0.068(6) Uani 0.50 1 d PU . . O4W O -0.668(2) 0.3303(15) 0.835(3) 0.100(9) 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 Mo1 0.0324(6) 0.0277(5) 0.0185(5) -0.0027(4) 0.0026(4) 0.0089(4) Mo2 0.0456(7) 0.0242(5) 0.0212(5) 0.0036(4) 0.0085(4) 0.0106(4) V1 0.0359(15) 0.0215(12) 0.0136(11) -0.0007(9) 0.0066(11) 0.0032(11) P2 0.0306(16) 0.0210(13) 0.0125(11) -0.0020(10) 0.0023(11) 0.0030(11) P1 0.0323(16) 0.0220(13) 0.0176(12) -0.0027(10) 0.0045(11) -0.0008(12) O13 0.029(4) 0.027(4) 0.018(3) -0.001(3) 0.002(3) 0.008(3) O12 0.038(4) 0.022(4) 0.014(3) 0.001(3) 0.007(3) -0.003(3) O11 0.039(5) 0.044(5) 0.046(5) -0.003(4) 0.011(4) 0.011(4) O10 0.050(5) 0.022(4) 0.019(3) 0.006(3) 0.007(3) 0.012(3) O9 0.037(4) 0.016(3) 0.024(4) 0.005(3) 0.009(3) 0.006(3) O8 0.028(4) 0.034(4) 0.020(3) -0.004(3) -0.002(3) 0.007(3) O7 0.083(7) 0.027(4) 0.056(5) 0.007(4) 0.032(6) -0.003(5) O6 0.039(5) 0.032(4) 0.011(3) -0.005(3) 0.009(3) 0.010(3) O5 0.034(4) 0.026(4) 0.019(3) -0.002(3) 0.002(3) 0.002(3) C4 0.043(7) 0.022(5) 0.020(5) 0.006(4) 0.005(5) 0.000(5) O4 0.054(6) 0.030(4) 0.029(4) -0.010(3) 0.003(4) 0.008(4) O3 0.036(5) 0.046(5) 0.031(4) -0.001(4) 0.010(4) -0.010(4) O2 0.039(5) 0.029(4) 0.023(4) -0.003(3) 0.002(3) 0.010(3) N1 0.031(5) 0.023(5) 0.027(5) 0.002(4) 0.003(4) -0.005(4) O1 0.069(7) 0.050(5) 0.031(4) 0.010(4) 0.004(4) 0.029(5) C1 0.031(6) 0.021(5) 0.021(5) -0.007(4) 0.011(5) 0.001(4) C2 0.046(7) 0.024(6) 0.028(6) 0.001(5) 0.007(5) 0.008(5) C3 0.035(6) 0.028(5) 0.013(4) 0.002(4) -0.001(4) -0.006(5) N3 0.046(7) 0.043(6) 0.069(8) -0.017(6) -0.018(6) 0.019(5) N2 0.068(9) 0.059(8) 0.057(7) 0.003(6) 0.021(7) 0.024(7) O5W 0.049(8) 0.047(8) 0.027(6) -0.024(6) 0.007(6) -0.012(6) O6W 0.017(9) 0.059(12) 0.072(12) 0.001(10) 0.013(9) 0.003(8) O3W 0.062(9) 0.036(7) 0.064(8) 0.030(7) 0.033(7) 0.011(7) O2W 0.065(15) 0.13(2) 0.051(12) 0.004(13) 0.014(11) 0.052(15) O1W 0.068(9) 0.067(9) 0.064(9) -0.014(7) -0.008(8) 0.025(8) O4W 0.066(17) 0.10(2) 0.12(2) 0.054(18) -0.017(16) -0.014(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O11 1.699(9) . ? Mo1 O4 1.716(8) . ? Mo1 O2 1.872(7) . ? Mo1 O6 1.940(7) . ? Mo1 O9 2.311(7) . ? Mo1 O5 2.341(7) . ? Mo1 Mo2 3.2097(14) . ? Mo2 O7 1.707(9) . ? Mo2 O1 1.720(9) . ? Mo2 O10 1.794(7) . ? Mo2 O2 2.016(7) . ? Mo2 O9 2.327(7) . ? Mo2 O5 2.328(7) . ? V1 O10 1.937(7) 3_566 ? V1 O10 1.937(7) . ? V1 O12 2.012(7) 3_566 ? V1 O12 2.012(7) . ? V1 O13 2.016(7) 3_566 ? V1 O13 2.016(7) . ? P2 O8 1.490(7) . ? P2 O13 1.526(7) . ? P2 O9 1.563(7) . ? P2 C1 1.834(11) . ? P1 O3 1.489(8) . ? P1 O12 1.535(7) 3_566 ? P1 O5 1.577(7) . ? P1 C1 1.841(11) . ? O12 P1 1.535(7) 3_566 ? O6 C1 1.448(11) . ? C4 C2 1.499(14) . ? C4 C3 1.512(14) . ? N1 C2 1.485(14) . ? C1 C3 1.520(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Mo1 O4 104.6(4) . . ? O11 Mo1 O2 101.8(4) . . ? O4 Mo1 O2 101.6(4) . . ? O11 Mo1 O6 100.2(4) . . ? O4 Mo1 O6 99.1(3) . . ? O2 Mo1 O6 144.8(3) . . ? O11 Mo1 O9 161.8(3) . . ? O4 Mo1 O9 93.5(3) . . ? O2 Mo1 O9 72.6(3) . . ? O6 Mo1 O9 78.0(3) . . ? O11 Mo1 O5 93.2(3) . . ? O4 Mo1 O5 162.2(4) . . ? O2 Mo1 O5 73.4(3) . . ? O6 Mo1 O5 78.3(3) . . ? O9 Mo1 O5 68.7(3) . . ? O11 Mo1 Mo2 119.7(3) . . ? O4 Mo1 Mo2 120.6(3) . . ? O2 Mo1 Mo2 35.8(2) . . ? O6 Mo1 Mo2 108.94(18) . . ? O9 Mo1 Mo2 46.41(17) . . ? O5 Mo1 Mo2 46.41(18) . . ? O7 Mo2 O1 104.7(5) . . ? O7 Mo2 O10 101.7(4) . . ? O1 Mo2 O10 103.3(4) . . ? O7 Mo2 O2 94.5(4) . . ? O1 Mo2 O2 94.4(4) . . ? O10 Mo2 O2 151.9(3) . . ? O7 Mo2 O9 94.0(4) . . ? O1 Mo2 O9 156.6(4) . . ? O10 Mo2 O9 86.1(3) . . ? O2 Mo2 O9 69.9(3) . . ? O7 Mo2 O5 160.3(4) . . ? O1 Mo2 O5 90.3(4) . . ? O10 Mo2 O5 86.9(3) . . ? O2 Mo2 O5 71.3(3) . . ? O9 Mo2 O5 68.7(2) . . ? O7 Mo2 Mo1 114.4(3) . . ? O1 Mo2 Mo1 112.0(3) . . ? O10 Mo2 Mo1 119.1(2) . . ? O2 Mo2 Mo1 32.9(2) . . ? O9 Mo2 Mo1 46.00(18) . . ? O5 Mo2 Mo1 46.74(17) . . ? O10 V1 O10 180.000(2) 3_566 . ? O10 V1 O12 91.4(3) 3_566 3_566 ? O10 V1 O12 88.6(3) . 3_566 ? O10 V1 O12 88.6(3) 3_566 . ? O10 V1 O12 91.4(3) . . ? O12 V1 O12 180.000(1) 3_566 . ? O10 V1 O13 88.8(3) 3_566 3_566 ? O10 V1 O13 91.2(3) . 3_566 ? O12 V1 O13 87.6(3) 3_566 3_566 ? O12 V1 O13 92.4(3) . 3_566 ? O10 V1 O13 91.2(3) 3_566 . ? O10 V1 O13 88.8(3) . . ? O12 V1 O13 92.4(3) 3_566 . ? O12 V1 O13 87.6(3) . . ? O13 V1 O13 180.000(1) 3_566 . ? O8 P2 O13 112.7(4) . . ? O8 P2 O9 112.5(4) . . ? O13 P2 O9 111.2(4) . . ? O8 P2 C1 109.4(5) . . ? O13 P2 C1 110.4(4) . . ? O9 P2 C1 99.8(5) . . ? O3 P1 O12 113.3(4) . 3_566 ? O3 P1 O5 112.3(5) . . ? O12 P1 O5 111.3(4) 3_566 . ? O3 P1 C1 111.2(4) . . ? O12 P1 C1 108.1(4) 3_566 . ? O5 P1 C1 99.8(4) . . ? P2 O13 V1 128.7(4) . . ? P1 O12 V1 130.5(4) 3_566 . ? Mo2 O10 V1 148.7(4) . . ? P2 O9 Mo1 113.2(4) . . ? P2 O9 Mo2 130.0(4) . . ? Mo1 O9 Mo2 87.6(3) . . ? C1 O6 Mo1 119.6(5) . . ? P1 O5 Mo2 129.3(4) . . ? P1 O5 Mo1 112.7(4) . . ? Mo2 O5 Mo1 86.8(2) . . ? C2 C4 C3 113.3(9) . . ? Mo1 O2 Mo2 111.2(3) . . ? O6 C1 C3 109.0(7) . . ? O6 C1 P2 102.1(6) . . ? C3 C1 P2 114.7(8) . . ? O6 C1 P1 103.5(7) . . ? C3 C1 P1 115.5(7) . . ? P2 C1 P1 110.5(5) . . ? N1 C2 C4 114.0(10) . . ? C4 C3 C1 117.0(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.430 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.197