# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr Enbo Wang' _publ_contact_author_email wangeb889@nenu.edu.cn loop_ _publ_author_name 'Enbo Wang' 'Hua-Qiao Tan' 'Yang-Guang Li' data_1 _database_code_depnum_ccdc_archive 'CCDC 782351' #TrackingRef '- revised compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H50 Mo6 N2 Na6 O47 P4' _chemical_formula_weight 1763.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.9198(7) _cell_length_b 12.9763(7) _cell_length_c 34.8821(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.3810(10) _cell_angle_gamma 90.00 _cell_volume 6248.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4944 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'block' _exptl_crystal_colour 'white' _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.765 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15450 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5504 _reflns_number_gt 4944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, all the non-H atoms were refined anisotropically. The 'omit -3 50' command was used to omit the weak reflections above 50 degree. The restraint command 'isor' was employed to restrain N1 so as to avoid some ADP and NPD problems on N atoms. In the crystal structure, there are a number of short connections between OW(H2O)...O(POM), indicating extensive H-bonding interactions among them. However, no H atoms on these O atoms could be found from the difference Fourier map because of the limited data quality. All H atoms on solvent water molecules were included into the formula directly. In the crystal, all positions of Na ions and solvent water molecules were firstly confirmed based on the distance references. Then, their site occupancies were determined as follows: For Na cations, only Na1 is well confirmed and fully occupied. The site occupancies of Na2, Na3, Na4, Na5 and Na6 were calculated by fixing their Ueq values, which are 1.2 times larger than Na1. Thus, the site occupancies of Na2¨CNa6 were determined. Then the crystal data was further refined with the free Ueq values. And the command DELU and ISOR was used for Na2, Na5 to avoid the ADP errors. Following the same method, the site occupancies of disordered solvent water molecules were also confirmed. ; _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^)+(0.1000P)^2^+150.0000P] 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 0.00191(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5504 _refine_ls_number_parameters 388 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1813 _refine_ls_wR_factor_gt 0.1753 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.980 _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 0.10613(4) 0.94957(5) 0.284548(17) 0.0276(2) Uani 1 1 d . . . Mo2 Mo 0.24766(5) 0.95717(6) 0.38409(2) 0.0407(3) Uani 1 1 d . . . Mo3 Mo 0.15045(6) 0.79574(8) 0.43653(2) 0.0561(3) Uani 1 1 d . . . P4 P -0.00064(14) 0.90035(19) 0.36681(6) 0.0387(5) Uani 1 1 d . . . P5 P 0.13107(16) 0.73536(16) 0.34348(7) 0.0412(5) Uani 1 1 d . . . O16 O 0.0000 0.9003(6) 0.2500 0.0317(16) Uani 1 2 d S . . O15 O 0.1263(4) 0.7904(4) 0.30472(16) 0.0366(12) Uani 1 1 d . . . O14 O 0.0031(4) 0.9482(4) 0.32766(15) 0.0336(12) Uani 1 1 d . . . O13 O 0.1967(4) 0.9716(4) 0.33432(15) 0.0373(13) Uani 1 1 d . . . O12 O 0.2065(4) 0.7852(5) 0.37524(17) 0.0456(14) Uani 1 1 d . . . O11 O 0.0845(5) 1.0782(4) 0.27875(17) 0.0445(14) Uani 1 1 d . . . O10 O 0.0906(4) 0.9310(5) 0.39587(15) 0.0431(14) Uani 1 1 d . . . O9 O 0.1984(4) 0.9299(5) 0.25776(18) 0.0494(15) Uani 1 1 d . . . O8 O 0.3678(5) 0.9322(7) 0.3806(2) 0.065(2) Uani 1 1 d . . . O7 O 0.0421(5) 0.7309(6) 0.40436(18) 0.061(2) Uani 1 1 d . . . O6 O 0.2483(6) 1.0807(6) 0.4007(2) 0.065(2) Uani 1 1 d . . . O5 O 0.2503(5) 0.8915(6) 0.43673(16) 0.0562(18) Uani 1 1 d . . . O4 O 0.1472(6) 0.6220(5) 0.3402(2) 0.070(2) Uani 1 1 d . . . O3 O -0.0928(5) 0.9217(8) 0.3832(2) 0.070(2) Uani 1 1 d . . . C4 C 0.0190(7) 0.7603(7) 0.3641(2) 0.046(2) Uani 1 1 d . . . O2 O 0.0917(6) 0.8347(8) 0.4735(2) 0.082(3) Uani 1 1 d . . . C3 C -0.0675(8) 0.6981(9) 0.3465(3) 0.062(3) Uani 1 1 d . . . H3A H -0.1184 0.7046 0.3629 0.074 Uiso 1 1 calc R . . H3B H -0.0490 0.6261 0.3463 0.074 Uiso 1 1 calc R . . O1 O 0.2103(7) 0.6863(7) 0.4529(2) 0.087(3) Uani 1 1 d . . . N1 N -0.2344(8) 0.6932(9) 0.2517(3) 0.086(3) Uani 1 1 d U . . H1A H -0.2797 0.6482 0.2424 0.104 Uiso 1 1 calc R . . H1B H -0.1905 0.6990 0.2354 0.104 Uiso 1 1 calc R . . H1C H -0.2616 0.7542 0.2546 0.104 Uiso 1 1 calc R . . C2 C -0.1873(8) 0.6572(10) 0.2891(3) 0.069(3) Uani 1 1 d . . . H2A H -0.1602 0.5892 0.2860 0.082 Uiso 1 1 calc R . . H2B H -0.2350 0.6515 0.3069 0.082 Uiso 1 1 calc R . . C1 C -0.1080(8) 0.7292(9) 0.3056(3) 0.065(3) Uani 1 1 d . . . H4A H -0.1333 0.7988 0.3058 0.078 Uiso 1 1 calc R . . H4B H -0.0564 0.7286 0.2894 0.078 Uiso 1 1 calc R . . Na1 Na 0.5000 1.0000 0.5000 0.113(3) Uani 1 2 d SU . . Na2 Na 0.0000 1.0000 0.5000 0.087(4) Uani 0.50 2 d SPU . . Na3 Na -0.3568(9) 0.5998(9) 0.1908(3) 0.135(4) Uani 0.72 1 d PU . . Na4 Na 0.3975(12) 0.8581(14) 0.3062(5) 0.172(6) Uani 0.66 1 d PU . . Na5 Na 0.0488(15) 0.5089(15) 0.2807(6) 0.149(6) Uani 0.48 1 d PU . . Na6 Na 0.5065(19) 0.7602(19) 0.4126(7) 0.149(8) Uani 0.39 1 d PU . . O1W O 0.4401(8) 0.8271(9) 0.4702(3) 0.106(3) Uani 1 1 d U A . O2W O 0.5140(10) 1.0291(10) 0.4322(4) 0.124(4) Uani 1 1 d U A . O3W O 0.313(2) 0.997(2) 0.5044(8) 0.111(7) Uani 0.50 1 d PU A 1 O4W O 0.336(2) 1.054(2) 0.4923(9) 0.133(10) Uani 0.50 1 d PU A 2 O5W O -0.2880(11) 0.9327(12) 0.3659(5) 0.118(5) Uani 0.75 1 d PU . . O6W O 0.0737(14) 1.0960(15) 0.4557(5) 0.086(5) Uani 0.50 1 d PU . . O7W O -0.1375(16) 0.9982(18) 0.4530(6) 0.133(7) Uani 0.65 1 d PU . . O8W O 0.4890(12) 0.7266(12) 0.2881(5) 0.138(5) Uani 0.85 1 d PU . . O9W O 0.1004(19) 1.214(2) 0.3567(7) 0.121(8) Uani 0.50 1 d PU . . O10W O -0.3882(11) 0.6718(12) 0.1123(5) 0.118(5) Uani 0.80 1 d PU . . O11W O 0.1264(15) 0.3148(17) 0.2831(7) 0.127(7) Uani 0.60 1 d PU . . O12W O 0.356(2) 1.245(2) 0.4456(7) 0.127(11) Uani 0.45 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 0.0253(4) 0.0318(4) 0.0243(4) 0.0029(2) -0.0019(2) -0.0052(2) Mo2 0.0356(4) 0.0533(5) 0.0298(4) 0.0061(3) -0.0092(3) -0.0204(3) Mo3 0.0536(5) 0.0761(6) 0.0334(4) 0.0230(4) -0.0146(3) -0.0292(4) P4 0.0273(10) 0.0591(13) 0.0290(10) 0.0054(9) 0.0014(8) -0.0060(9) P5 0.0431(12) 0.0318(11) 0.0434(12) 0.0086(9) -0.0145(9) -0.0042(9) O16 0.033(4) 0.033(4) 0.026(3) 0.000 -0.008(3) 0.000 O15 0.037(3) 0.034(3) 0.038(3) -0.001(2) -0.003(2) 0.001(2) O14 0.026(3) 0.042(3) 0.031(3) 0.005(2) 0.000(2) 0.001(2) O13 0.034(3) 0.045(3) 0.030(3) 0.005(2) -0.005(2) -0.016(2) O12 0.041(3) 0.048(3) 0.043(3) 0.010(3) -0.015(3) -0.007(3) O11 0.055(4) 0.034(3) 0.042(3) 0.007(2) -0.007(3) -0.011(3) O10 0.039(3) 0.062(4) 0.027(3) 0.000(3) -0.003(2) -0.011(3) O9 0.035(3) 0.073(4) 0.042(3) 0.003(3) 0.014(3) -0.006(3) O8 0.033(3) 0.099(6) 0.058(4) 0.011(4) -0.012(3) -0.020(4) O7 0.065(4) 0.075(5) 0.039(3) 0.029(3) -0.016(3) -0.039(4) O6 0.079(5) 0.066(4) 0.046(4) -0.008(3) -0.003(3) -0.033(4) O5 0.052(4) 0.083(5) 0.028(3) 0.014(3) -0.015(3) -0.029(3) O4 0.089(5) 0.033(3) 0.079(5) 0.010(3) -0.024(4) 0.005(3) O3 0.036(4) 0.128(7) 0.047(4) 0.003(4) 0.011(3) 0.002(4) C4 0.045(5) 0.051(5) 0.037(4) 0.018(4) -0.013(4) -0.022(4) O2 0.081(5) 0.128(8) 0.034(4) 0.016(4) -0.003(3) -0.041(5) C3 0.058(6) 0.074(7) 0.048(5) 0.027(5) -0.016(4) -0.043(5) O1 0.085(6) 0.091(6) 0.073(5) 0.046(5) -0.038(4) -0.033(5) N1 0.074(6) 0.104(7) 0.074(6) 0.020(5) -0.017(5) -0.048(5) C2 0.055(6) 0.087(8) 0.057(6) 0.023(6) -0.019(5) -0.037(6) C1 0.050(6) 0.085(8) 0.053(6) 0.028(5) -0.021(5) -0.040(5) Na1 0.108(6) 0.133(6) 0.095(5) 0.011(5) -0.004(4) -0.037(5) Na2 0.089(8) 0.093(8) 0.081(7) -0.006(6) 0.015(6) -0.005(7) Na3 0.162(7) 0.131(7) 0.110(6) -0.003(5) 0.010(6) -0.066(6) Na4 0.159(9) 0.197(10) 0.162(9) -0.003(8) 0.031(7) -0.006(8) Na5 0.160(10) 0.132(9) 0.146(9) -0.021(8) -0.013(8) 0.003(8) Na6 0.158(11) 0.152(11) 0.145(11) 0.005(9) 0.049(9) 0.000(9) O1W 0.095(6) 0.112(7) 0.108(6) 0.033(5) 0.006(5) -0.011(5) O2W 0.138(8) 0.118(7) 0.108(7) 0.031(6) -0.019(6) -0.046(6) O3W 0.124(11) 0.102(10) 0.105(10) 0.002(8) 0.010(8) -0.010(9) O4W 0.128(12) 0.139(13) 0.132(13) -0.003(9) 0.010(9) 0.001(9) O5W 0.091(7) 0.108(8) 0.149(9) 0.026(7) -0.013(7) 0.001(7) O6W 0.097(9) 0.087(8) 0.079(8) -0.011(7) 0.029(7) 0.016(7) O7W 0.135(10) 0.154(10) 0.108(9) -0.008(8) 0.014(8) 0.002(8) O8W 0.117(8) 0.117(8) 0.181(10) -0.004(8) 0.024(8) 0.007(7) O9W 0.127(11) 0.122(11) 0.110(11) -0.006(8) 0.002(9) 0.024(9) O10W 0.112(8) 0.119(8) 0.122(8) 0.003(7) 0.007(7) -0.030(7) O11W 0.111(10) 0.120(10) 0.154(11) 0.025(8) 0.032(8) 0.013(8) O12W 0.13(2) 0.17(2) 0.096(17) -0.044(17) 0.075(16) -0.076(19) _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 O9 1.701(6) . ? Mo1 O11 1.704(6) . ? Mo1 O16 1.893(3) . ? Mo1 O13 2.031(5) . ? Mo1 O15 2.188(5) . ? Mo1 O14 2.208(5) . ? Mo2 O6 1.704(7) . ? Mo2 O8 1.722(7) . ? Mo2 O13 1.799(5) . ? Mo2 O5 2.021(6) . ? Mo2 O10 2.301(6) . ? Mo2 O12 2.315(6) . ? Mo2 Mo3 3.1940(10) . ? Mo3 O2 1.692(9) . ? Mo3 O1 1.707(9) . ? Mo3 O5 1.863(6) . ? Mo3 O7 1.951(6) . ? Mo3 O10 2.341(6) . ? Mo3 O12 2.372(7) . ? P4 O3 1.496(7) . ? P4 O14 1.507(5) . ? P4 O10 1.571(6) . ? P4 C4 1.842(10) . ? P5 O4 1.494(7) . ? P5 O15 1.523(6) . ? P5 O12 1.565(6) . ? P5 C4 1.829(10) . ? O16 Mo1 1.893(2) 2 ? O14 Na3 2.845(11) 4_455 ? O8 Na4 2.846(18) . ? O7 C4 1.451(10) . ? O4 Na5 2.76(2) . ? C4 C3 1.512(11) . ? O2 Na2 2.718(11) . ? C3 C1 1.518(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C2 1.457(13) . ? N1 Na3 2.821(14) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C2 C1 1.504(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H4A 0.9700 . ? C1 H4B 0.9700 . ? Na1 O4W 2.36(3) . ? Na1 O4W 2.36(3) 5_676 ? Na1 O2W 2.426(12) . ? Na1 O2W 2.426(12) 5_676 ? Na1 O1W 2.567(12) 5_676 ? Na1 O1W 2.567(12) . ? Na1 O3W 2.63(3) . ? Na1 O3W 2.63(3) 5_676 ? Na2 O6W 2.324(19) . ? Na2 O6W 2.324(19) 5_576 ? Na2 O7W 2.35(2) . ? Na2 O7W 2.35(2) 5_576 ? Na2 O2 2.718(11) 5_576 ? Na3 O8W 2.64(2) 2 ? Na3 O14 2.845(11) 4_445 ? Na3 O10W 2.872(19) . ? Na3 Na4 3.40(2) 2 ? Na4 O8W 2.27(2) . ? Na4 Na5 3.09(3) 3 ? Na4 Na3 3.40(2) 2 ? Na4 Na5 3.76(3) 4 ? Na5 Na5 2.38(4) 2 ? Na5 O11W 2.74(3) . ? Na5 Na4 3.09(3) 3_445 ? Na5 Na4 3.76(3) 4_545 ? Na6 O10W 2.10(3) 2 ? Na6 O1W 2.48(3) . ? Na6 O9W 2.55(3) 3_545 ? Na6 O6W 2.70(3) 3_545 ? O6W Na6 2.70(3) 3_455 ? O8W Na3 2.64(2) 2 ? O9W Na6 2.55(3) 3_455 ? O10W Na6 2.10(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Mo1 O11 102.5(3) . . ? O9 Mo1 O16 100.5(2) . . ? O11 Mo1 O16 98.2(3) . . ? O9 Mo1 O13 93.5(3) . . ? O11 Mo1 O13 92.6(3) . . ? O16 Mo1 O13 160.00(19) . . ? O9 Mo1 O15 87.7(3) . . ? O11 Mo1 O15 167.5(3) . . ? O16 Mo1 O15 86.8(2) . . ? O13 Mo1 O15 79.5(2) . . ? O9 Mo1 O14 167.2(3) . . ? O11 Mo1 O14 88.2(3) . . ? O16 Mo1 O14 84.76(14) . . ? O13 Mo1 O14 78.8(2) . . ? O15 Mo1 O14 80.9(2) . . ? O6 Mo2 O8 103.8(4) . . ? O6 Mo2 O13 102.4(3) . . ? O8 Mo2 O13 102.6(3) . . ? O6 Mo2 O5 95.1(3) . . ? O8 Mo2 O5 94.6(3) . . ? O13 Mo2 O5 151.6(2) . . ? O6 Mo2 O10 92.4(3) . . ? O8 Mo2 O10 159.7(3) . . ? O13 Mo2 O10 85.5(2) . . ? O5 Mo2 O10 71.4(2) . . ? O6 Mo2 O12 160.5(3) . . ? O8 Mo2 O12 92.0(3) . . ? O13 Mo2 O12 84.9(2) . . ? O5 Mo2 O12 71.9(2) . . ? O10 Mo2 O12 69.9(2) . . ? O6 Mo2 Mo3 114.0(2) . . ? O8 Mo2 Mo3 113.8(3) . . ? O13 Mo2 Mo3 118.53(17) . . ? O5 Mo2 Mo3 33.10(17) . . ? O10 Mo2 Mo3 47.05(15) . . ? O12 Mo2 Mo3 47.80(16) . . ? O2 Mo3 O1 104.9(5) . . ? O2 Mo3 O5 103.4(4) . . ? O1 Mo3 O5 102.8(4) . . ? O2 Mo3 O7 98.9(4) . . ? O1 Mo3 O7 98.1(4) . . ? O5 Mo3 O7 144.2(2) . . ? O2 Mo3 O10 94.0(3) . . ? O1 Mo3 O10 161.1(4) . . ? O5 Mo3 O10 73.1(2) . . ? O7 Mo3 O10 77.7(2) . . ? O2 Mo3 O12 162.2(3) . . ? O1 Mo3 O12 92.9(4) . . ? O5 Mo3 O12 73.2(2) . . ? O7 Mo3 O12 77.1(3) . . ? O10 Mo3 O12 68.3(2) . . ? O2 Mo3 Mo2 121.5(3) . . ? O1 Mo3 Mo2 120.8(3) . . ? O5 Mo3 Mo2 36.32(17) . . ? O7 Mo3 Mo2 107.85(17) . . ? O10 Mo3 Mo2 46.01(14) . . ? O12 Mo3 Mo2 46.29(15) . . ? O3 P4 O14 113.6(4) . . ? O3 P4 O10 111.6(4) . . ? O14 P4 O10 111.2(3) . . ? O3 P4 C4 110.0(5) . . ? O14 P4 C4 109.7(4) . . ? O10 P4 C4 99.8(4) . . ? O4 P5 O15 112.6(4) . . ? O4 P5 O12 111.5(4) . . ? O15 P5 O12 112.5(3) . . ? O4 P5 C4 110.3(5) . . ? O15 P5 C4 108.9(3) . . ? O12 P5 C4 100.2(4) . . ? Mo1 O16 Mo1 140.6(4) 2 . ? P5 O15 Mo1 135.8(3) . . ? P4 O14 Mo1 136.2(3) . . ? P4 O14 Na3 112.5(4) . 4_455 ? Mo1 O14 Na3 110.4(3) . 4_455 ? Mo2 O13 Mo1 159.2(3) . . ? P5 O12 Mo2 128.7(3) . . ? P5 O12 Mo3 113.2(3) . . ? Mo2 O12 Mo3 85.9(2) . . ? P4 O10 Mo2 129.1(3) . . ? P4 O10 Mo3 113.4(3) . . ? Mo2 O10 Mo3 86.9(2) . . ? Mo2 O8 Na4 112.5(5) . . ? C4 O7 Mo3 120.1(5) . . ? Mo3 O5 Mo2 110.6(3) . . ? P5 O4 Na5 121.0(6) . . ? O7 C4 C3 108.6(7) . . ? O7 C4 P5 103.9(6) . . ? C3 C4 P5 114.9(8) . . ? O7 C4 P4 103.0(6) . . ? C3 C4 P4 115.6(7) . . ? P5 C4 P4 109.5(4) . . ? Mo3 O2 Na2 142.1(4) . . ? C4 C3 C1 114.9(7) . . ? C4 C3 H3A 108.6 . . ? C1 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? C1 C3 H3B 108.6 . . ? H3A C3 H3B 107.5 . . ? C2 N1 Na3 134.0(8) . . ? C2 N1 H1A 109.5 . . ? Na3 N1 H1A 27.3 . . ? C2 N1 H1B 109.5 . . ? Na3 N1 H1B 87.2 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? Na3 N1 H1C 104.1 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C2 C1 111.6(9) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C2 C1 C3 111.2(8) . . ? C2 C1 H4A 109.4 . . ? C3 C1 H4A 109.4 . . ? C2 C1 H4B 109.4 . . ? C3 C1 H4B 109.4 . . ? H4A C1 H4B 108.0 . . ? O4W Na1 O4W 180.000(8) . 5_676 ? O4W Na1 O2W 92.3(8) . . ? O4W Na1 O2W 87.7(8) 5_676 . ? O4W Na1 O2W 87.7(8) . 5_676 ? O4W Na1 O2W 92.3(8) 5_676 5_676 ? O2W Na1 O2W 180.000(3) . 5_676 ? O4W Na1 O1W 92.6(8) . 5_676 ? O4W Na1 O1W 87.4(8) 5_676 5_676 ? O2W Na1 O1W 101.3(4) . 5_676 ? O2W Na1 O1W 78.7(4) 5_676 5_676 ? O4W Na1 O1W 87.4(8) . . ? O4W Na1 O1W 92.6(8) 5_676 . ? O2W Na1 O1W 78.7(4) . . ? O2W Na1 O1W 101.3(4) 5_676 . ? O1W Na1 O1W 180.000(2) 5_676 . ? O4W Na1 O3W 20.6(8) . . ? O4W Na1 O3W 159.4(8) 5_676 . ? O2W Na1 O3W 105.2(7) . . ? O2W Na1 O3W 74.8(7) 5_676 . ? O1W Na1 O3W 105.2(6) 5_676 . ? O1W Na1 O3W 74.8(6) . . ? O4W Na1 O3W 159.4(8) . 5_676 ? O4W Na1 O3W 20.6(8) 5_676 5_676 ? O2W Na1 O3W 74.8(7) . 5_676 ? O2W Na1 O3W 105.2(7) 5_676 5_676 ? O1W Na1 O3W 74.8(6) 5_676 5_676 ? O1W Na1 O3W 105.2(6) . 5_676 ? O3W Na1 O3W 180.000(3) . 5_676 ? O6W Na2 O6W 180.000(4) . 5_576 ? O6W Na2 O7W 86.1(7) . . ? O6W Na2 O7W 93.9(7) 5_576 . ? O6W Na2 O7W 93.9(7) . 5_576 ? O6W Na2 O7W 86.1(7) 5_576 5_576 ? O7W Na2 O7W 180.000(4) . 5_576 ? O6W Na2 O2 86.0(5) . . ? O6W Na2 O2 94.0(5) 5_576 . ? O7W Na2 O2 97.5(6) . . ? O7W Na2 O2 82.5(6) 5_576 . ? O6W Na2 O2 94.0(5) . 5_576 ? O6W Na2 O2 86.0(5) 5_576 5_576 ? O7W Na2 O2 82.5(6) . 5_576 ? O7W Na2 O2 97.5(6) 5_576 5_576 ? O2 Na2 O2 180.0(3) . 5_576 ? O8W Na3 N1 84.1(6) 2 . ? O8W Na3 O14 89.4(5) 2 4_445 ? N1 Na3 O14 144.4(5) . 4_445 ? O8W Na3 O10W 92.1(7) 2 . ? N1 Na3 O10W 125.6(5) . . ? O14 Na3 O10W 89.6(4) 4_445 . ? O8W Na3 Na4 41.7(5) 2 2 ? N1 Na3 Na4 69.0(4) . 2 ? O14 Na3 Na4 124.8(5) 4_445 2 ? O10W Na3 Na4 72.7(5) . 2 ? O8W Na4 O8 131.4(9) . . ? O8W Na4 Na5 88.2(7) . 3 ? O8 Na4 Na5 103.5(7) . 3 ? O8W Na4 Na3 50.9(6) . 2 ? O8 Na4 Na3 105.1(6) . 2 ? Na5 Na4 Na3 139.0(7) 3 2 ? O8W Na4 Na5 89.4(7) . 4 ? O8 Na4 Na5 128.8(7) . 4 ? Na5 Na4 Na5 39.2(7) 3 4 ? Na3 Na4 Na5 126.0(6) 2 4 ? Na5 Na5 O11W 101.8(8) 2 . ? Na5 Na5 O4 147.8(5) 2 . ? O11W Na5 O4 108.1(8) . . ? Na5 Na5 Na4 85.9(9) 2 3_445 ? O11W Na5 Na4 71.9(7) . 3_445 ? O4 Na5 Na4 114.2(8) . 3_445 ? Na5 Na5 Na4 55.0(8) 2 4_545 ? O11W Na5 Na4 55.1(7) . 4_545 ? O4 Na5 Na4 138.8(8) . 4_545 ? Na4 Na5 Na4 96.7(7) 3_445 4_545 ? O10W Na6 O1W 99.9(10) 2 . ? O10W Na6 O9W 90.4(11) 2 3_545 ? O1W Na6 O9W 169.5(14) . 3_545 ? O10W Na6 O6W 89.8(10) 2 3_545 ? O1W Na6 O6W 87.9(8) . 3_545 ? O9W Na6 O6W 93.8(10) 3_545 3_545 ? Na6 O1W Na1 120.0(7) . . ? Na2 O6W Na6 129.9(9) . 3_455 ? Na4 O8W Na3 87.4(7) . 2 ? Na6 O10W Na3 126.0(10) 2 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.250 _refine_diff_density_min -1.229 _refine_diff_density_rms 0.178 # Attachment 'revised_compound_2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 782352' #TrackingRef 'revised_compound_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H66 Mo12 N11 Na O61 P8' _chemical_formula_weight 2810.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.263(2) _cell_length_b 14.263(2) _cell_length_c 21.020(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4276.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4314 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 27.45 _exptl_crystal_description 'block' _exptl_crystal_colour 'white' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2724 _exptl_absorpt_coefficient_mu 1.956 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 0.731 _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 'Rotation anode' _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 20493 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4875 _reflns_number_gt 4314 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _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. During the refinement, all the non-H atoms were refined anisotropically. The restraint command 'isor' was employed to restrain N1 and N3 so as to avoid some ADP and NPD problems on N atoms. In the crystal structure, there are a number of short connections between N(NH4+)...O(POM) and N(NH4+)...N(NH4+), indicating extensive H-bonding interactions among them. However, no H atoms on these O and N atoms could be found from the difference Fourier map because of the limited data quality. All H atoms on solvent water molecules and NH4+ were included into the formula directly. ; _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^)+(0.1000P)^2^+0.0000P] 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 0.00059(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(7) _refine_ls_number_reflns 4875 _refine_ls_number_parameters 246 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.062 _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 Mo1 Mo 1.80146(5) -0.00495(4) 1.10133(3) 0.02784(18) Uani 1 1 d . . . Mo2 Mo 1.84105(5) 0.20514(5) 1.20098(3) 0.0361(2) Uani 1 1 d . . . Mo3 Mo 1.79845(7) 0.38393(5) 1.11547(4) 0.0448(2) Uani 1 1 d . . . P4 P 1.79838(13) -0.12715(13) 0.96593(9) 0.0239(4) Uani 1 1 d . . . P2 P 1.80538(15) -0.32511(14) 0.92224(11) 0.0315(4) Uani 1 1 d . . . O14 O 1.9049(4) -0.0642(4) 1.1007(3) 0.0377(13) Uani 1 1 d . . . O13 O 1.7503(4) -0.1072(4) 0.9015(3) 0.0307(11) Uani 1 1 d . . . O12 O 1.7577(4) -0.0614(4) 1.0163(3) 0.0306(12) Uani 1 1 d . . . O11 O 1.7605(4) 0.3423(4) 1.0313(3) 0.0377(13) Uani 1 1 d . . . O16 O 1.7733(6) 0.1944(5) 1.2671(3) 0.0524(19) Uani 1 1 d . . . O10 O 1.6881(4) 0.0892(4) 1.0799(3) 0.0325(12) Uani 1 1 d . . . O9 O 1.7294(6) -0.0763(5) 1.1450(3) 0.0482(17) Uani 1 1 d . . . O8 O 1.9052(4) -0.1239(4) 0.9632(3) 0.0267(11) Uani 1 1 d . . . O7 O 1.8363(5) 0.3427(4) 1.1968(4) 0.0460(16) Uani 1 1 d . . . O6 O 1.7753(5) -0.4231(4) 0.9353(4) 0.0494(17) Uani 1 1 d . . . C4 C 1.8683(7) -0.2992(6) 1.0724(5) 0.040(2) Uani 1 1 d . . . H4A H 1.8947 -0.3487 1.0463 0.048 Uiso 1 1 calc R . . H4B H 1.9052 -0.2430 1.0655 0.048 Uiso 1 1 calc R . . O5 O 1.8303(4) 0.0863(4) 1.1644(3) 0.0332(12) Uani 1 1 d . . . C3 C 1.7567(5) -0.2464(6) 0.9832(4) 0.0293(15) Uani 1 1 d . . . O4 O 1.7162(4) 0.2434(4) 1.1388(3) 0.0355(13) Uani 1 1 d . . . O3 O 1.7094(8) 0.4566(6) 1.1337(4) 0.072(3) Uani 1 1 d . . . O15 O 1.9543(6) 0.1974(6) 1.2279(4) 0.058(2) Uani 1 1 d . . . C2 C 1.7679(6) -0.2811(6) 1.0516(4) 0.0369(18) Uani 1 1 d . . . H2A H 1.7406 -0.2350 1.0800 0.044 Uiso 1 1 calc R . . H2B H 1.7325 -0.3387 1.0563 0.044 Uiso 1 1 calc R . . C1 C 1.8748(9) -0.3270(7) 1.1411(5) 0.048(2) Uani 1 1 d . . . H1A H 1.8249 -0.3704 1.1518 0.058 Uiso 1 1 calc R . . H1B H 1.9345 -0.3571 1.1495 0.058 Uiso 1 1 calc R . . O2 O 1.8901(6) 0.4577(5) 1.0944(5) 0.062(2) Uani 1 1 d . . . N3 N 1.9143(12) -0.5496(11) 0.9467(10) 0.111(5) Uani 1 1 d U . . N2 N 1.5807(16) 0.3360(17) 1.2268(11) 0.106(7) Uiso 0.75 1 d P A 1 OW1 O 1.535(3) 0.267(4) 1.214(2) 0.090(13) Uiso 0.25 1 d P B 2 N1 N 1.8658(11) -0.2382(10) 1.1796(7) 0.093(4) Uani 1 1 d U . . H1C H 1.8691 -0.2520 1.2208 0.112 Uiso 1 1 calc R . . H1D H 1.8109 -0.2111 1.1713 0.112 Uiso 1 1 calc R . . H1E H 1.9121 -0.1992 1.1694 0.112 Uiso 1 1 calc R . . Na1 Na 2.0001(11) -0.0002(10) 1.0004(7) 0.0344(14) Uani 1 4 d SR . . 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 0.0361(4) 0.0253(3) 0.0221(3) -0.0014(2) 0.0059(3) -0.0025(3) Mo2 0.0441(4) 0.0383(4) 0.0258(3) -0.0092(3) 0.0043(3) -0.0082(3) Mo3 0.0584(5) 0.0281(3) 0.0479(5) -0.0096(3) 0.0039(4) -0.0035(3) P4 0.0242(8) 0.0242(8) 0.0232(8) -0.0040(7) -0.0007(7) -0.0003(6) P2 0.0347(10) 0.0247(9) 0.0352(10) -0.0075(8) -0.0059(9) 0.0010(8) O14 0.044(3) 0.033(3) 0.036(3) 0.000(3) -0.002(3) 0.008(2) O13 0.035(3) 0.032(3) 0.025(3) -0.003(2) -0.005(2) 0.009(2) O12 0.033(3) 0.028(3) 0.031(3) -0.007(2) 0.003(2) -0.001(2) O11 0.043(3) 0.022(3) 0.048(3) -0.004(3) 0.002(3) 0.002(2) O16 0.069(5) 0.054(4) 0.034(3) -0.011(3) 0.021(3) -0.015(4) O10 0.026(3) 0.033(3) 0.039(3) -0.007(2) 0.011(2) -0.006(2) O9 0.066(5) 0.037(3) 0.042(4) 0.001(3) 0.020(3) -0.010(3) O8 0.024(2) 0.029(3) 0.026(3) -0.003(2) 0.000(2) -0.0010(19) O7 0.062(4) 0.030(3) 0.046(4) -0.018(3) 0.006(3) -0.009(3) O6 0.052(4) 0.029(3) 0.067(5) -0.002(3) -0.011(4) -0.007(3) C4 0.048(5) 0.033(4) 0.040(5) 0.004(4) 0.010(4) 0.006(4) O5 0.044(3) 0.033(3) 0.023(3) -0.005(2) -0.001(2) -0.004(2) C3 0.027(4) 0.029(4) 0.031(4) 0.001(3) -0.002(3) -0.003(3) O4 0.030(3) 0.037(3) 0.040(3) -0.013(3) 0.013(3) 0.000(2) O3 0.100(7) 0.052(4) 0.063(5) -0.023(4) 0.010(5) 0.027(5) O15 0.060(5) 0.071(5) 0.044(4) -0.005(4) -0.014(4) 0.001(4) C2 0.038(4) 0.037(4) 0.035(4) 0.000(4) 0.007(4) -0.004(3) C1 0.065(6) 0.045(5) 0.034(5) 0.001(4) 0.001(5) 0.016(4) O2 0.072(5) 0.037(3) 0.077(6) 0.002(4) -0.003(4) -0.019(3) N3 0.114(8) 0.078(7) 0.142(10) 0.029(7) 0.036(7) 0.008(6) N1 0.108(8) 0.089(7) 0.083(7) 0.010(6) 0.023(6) -0.003(6) Na1 0.0276(18) 0.0276(18) 0.048(4) 0.000 0.000 0.000 _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 O14 1.700(6) . ? Mo1 O9 1.713(7) . ? Mo1 O5 1.903(6) . ? Mo1 O12 2.057(6) . ? Mo1 O10 2.149(6) . ? Mo1 O8 2.235(5) 3_777 ? Mo1 Na1 3.541(15) . ? Mo2 O16 1.700(7) . ? Mo2 O15 1.715(8) . ? Mo2 O5 1.868(6) . ? Mo2 O7 1.965(6) . ? Mo2 O4 2.276(7) . ? Mo2 O13 2.365(6) 3_777 ? Mo2 Mo3 3.1786(13) . ? Mo3 O3 1.684(8) . ? Mo3 O2 1.735(8) . ? Mo3 O7 1.887(8) . ? Mo3 O11 1.943(7) . ? Mo3 O13 2.367(6) 3_777 ? Mo3 O4 2.373(6) . ? P4 O8 1.526(5) . ? P4 O12 1.529(6) . ? P4 O13 1.544(6) . ? P4 C3 1.838(8) . ? P4 Na1 3.476(15) . ? P2 O6 1.488(7) . ? P2 O10 1.516(6) 4_737 ? P2 O4 1.573(6) 4_737 ? P2 C3 1.840(8) . ? O14 Na1 2.670(16) . ? O13 Mo2 2.365(6) 4_737 ? O13 Mo3 2.367(6) 4_737 ? O11 C3 1.448(9) 3_777 ? O10 P2 1.516(6) 3_777 ? O8 Mo1 2.235(5) 4_737 ? O8 Na1 2.357(16) . ? C4 C1 1.500(13) . ? C4 C2 1.519(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3 O11 1.448(9) 4_737 ? C3 C2 1.527(12) . ? O4 P2 1.573(6) 3_777 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 N1 1.508(17) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? Na1 O8 2.356(16) 3_777 ? Na1 O8 2.351(16) 4_737 ? Na1 O8 2.359(14) 2_955 ? Na1 O14 2.680(16) 4_737 ? Na1 O14 2.684(16) 3_777 ? Na1 O14 2.670(17) 2_955 ? Na1 Mo1 3.547(15) 4_737 ? Na1 Mo1 3.551(14) 3_777 ? 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 O14 Mo1 O9 103.2(3) . . ? O14 Mo1 O5 99.1(3) . . ? O9 Mo1 O5 99.4(3) . . ? O14 Mo1 O12 93.5(3) . . ? O9 Mo1 O12 93.0(3) . . ? O5 Mo1 O12 159.8(2) . . ? O14 Mo1 O10 164.1(3) . . ? O9 Mo1 O10 91.9(3) . . ? O5 Mo1 O10 83.2(2) . . ? O12 Mo1 O10 80.5(2) . . ? O14 Mo1 O8 84.2(3) . 3_777 ? O9 Mo1 O8 171.5(3) . 3_777 ? O5 Mo1 O8 83.3(2) . 3_777 ? O12 Mo1 O8 82.3(2) . 3_777 ? O10 Mo1 O8 80.4(2) . 3_777 ? O14 Mo1 Na1 46.4(3) . . ? O9 Mo1 Na1 144.3(3) . . ? O5 Mo1 Na1 103.4(3) . . ? O12 Mo1 Na1 74.3(3) . . ? O10 Mo1 Na1 117.7(3) . . ? O8 Mo1 Na1 40.8(3) 3_777 . ? O16 Mo2 O15 105.0(4) . . ? O16 Mo2 O5 102.1(3) . . ? O15 Mo2 O5 98.9(4) . . ? O16 Mo2 O7 96.1(3) . . ? O15 Mo2 O7 96.4(4) . . ? O5 Mo2 O7 152.2(3) . . ? O16 Mo2 O4 92.7(3) . . ? O15 Mo2 O4 160.4(3) . . ? O5 Mo2 O4 85.2(2) . . ? O7 Mo2 O4 73.0(3) . . ? O16 Mo2 O13 161.2(3) . 3_777 ? O15 Mo2 O13 91.4(3) . 3_777 ? O5 Mo2 O13 83.9(2) . 3_777 ? O7 Mo2 O13 72.6(3) . 3_777 ? O4 Mo2 O13 69.9(2) . 3_777 ? O16 Mo2 Mo3 115.2(3) . . ? O15 Mo2 Mo3 114.7(3) . . ? O5 Mo2 Mo3 118.64(18) . . ? O7 Mo2 Mo3 33.6(2) . . ? O4 Mo2 Mo3 48.16(16) . . ? O13 Mo2 Mo3 47.84(14) 3_777 . ? O3 Mo3 O2 104.7(5) . . ? O3 Mo3 O7 101.6(4) . . ? O2 Mo3 O7 101.8(4) . . ? O3 Mo3 O11 100.7(4) . . ? O2 Mo3 O11 99.4(4) . . ? O7 Mo3 O11 144.0(2) . . ? O3 Mo3 O13 164.0(4) . 3_777 ? O2 Mo3 O13 91.4(3) . 3_777 ? O7 Mo3 O13 73.8(2) . 3_777 ? O11 Mo3 O13 76.9(2) . 3_777 ? O3 Mo3 O4 95.7(4) . . ? O2 Mo3 O4 159.6(3) . . ? O7 Mo3 O4 72.0(2) . . ? O11 Mo3 O4 78.0(2) . . ? O13 Mo3 O4 68.25(19) 3_777 . ? O3 Mo3 Mo2 120.6(4) . . ? O2 Mo3 Mo2 119.1(3) . . ? O7 Mo3 Mo2 35.19(18) . . ? O11 Mo3 Mo2 108.83(17) . . ? O13 Mo3 Mo2 47.76(14) 3_777 . ? O4 Mo3 Mo2 45.61(16) . . ? O8 P4 O12 112.7(3) . . ? O8 P4 O13 113.9(3) . . ? O12 P4 O13 109.0(3) . . ? O8 P4 C3 111.0(3) . . ? O12 P4 C3 108.0(3) . . ? O13 P4 C3 101.6(3) . . ? O8 P4 Na1 33.4(3) . . ? O12 P4 Na1 81.4(3) . . ? O13 P4 Na1 117.0(3) . . ? C3 P4 Na1 135.1(3) . . ? O6 P2 O10 114.1(4) . 4_737 ? O6 P2 O4 112.0(4) . 4_737 ? O10 P2 O4 111.6(4) 4_737 4_737 ? O6 P2 C3 109.6(4) . . ? O10 P2 C3 108.6(3) 4_737 . ? O4 P2 C3 99.9(3) 4_737 . ? Mo1 O14 Na1 106.1(4) . . ? P4 O13 Mo2 128.5(3) . 4_737 ? P4 O13 Mo3 112.7(3) . 4_737 ? Mo2 O13 Mo3 84.40(18) 4_737 4_737 ? P4 O12 Mo1 136.6(4) . . ? C3 O11 Mo3 120.6(5) 3_777 . ? P2 O10 Mo1 136.0(3) 3_777 . ? P4 O8 Mo1 130.1(3) . 4_737 ? P4 O8 Na1 125.7(5) . . ? Mo1 O8 Na1 101.1(4) 4_737 . ? Mo3 O7 Mo2 111.2(3) . . ? C1 C4 C2 112.4(8) . . ? C1 C4 H4A 109.1 . . ? C2 C4 H4A 109.1 . . ? C1 C4 H4B 109.1 . . ? C2 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? Mo2 O5 Mo1 157.8(4) . . ? O11 C3 C2 108.9(7) 4_737 . ? O11 C3 P4 102.2(5) 4_737 . ? C2 C3 P4 116.9(6) . . ? O11 C3 P2 105.2(5) 4_737 . ? C2 C3 P2 114.7(6) . . ? P4 C3 P2 107.7(4) . . ? P2 O4 Mo2 130.9(3) 3_777 . ? P2 O4 Mo3 113.0(3) 3_777 . ? Mo2 O4 Mo3 86.2(2) . . ? C4 C2 C3 115.2(7) . . ? C4 C2 H2A 108.5 . . ? C3 C2 H2A 108.5 . . ? C4 C2 H2B 108.5 . . ? C3 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N1 C1 C4 106.9(9) . . ? N1 C1 H1A 110.3 . . ? C4 C1 H1A 110.3 . . ? N1 C1 H1B 110.3 . . ? C4 C1 H1B 110.3 . . ? H1A C1 H1B 108.6 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? O8 Na1 O8 96.1(6) . 3_777 ? O8 Na1 O8 96.3(5) . 4_737 ? O8 Na1 O8 142.0(8) 3_777 4_737 ? O8 Na1 O8 141.3(8) . 2_955 ? O8 Na1 O8 96.1(5) 3_777 2_955 ? O8 Na1 O8 96.2(6) 4_737 2_955 ? O8 Na1 O14 63.6(4) . 4_737 ? O8 Na1 O14 143.6(7) 3_777 4_737 ? O8 Na1 O14 73.3(5) 4_737 4_737 ? O8 Na1 O14 85.5(5) 2_955 4_737 ? O8 Na1 O14 85.4(5) . 3_777 ? O8 Na1 O14 73.1(5) 3_777 3_777 ? O8 Na1 O14 143.7(7) 4_737 3_777 ? O8 Na1 O14 63.5(4) 2_955 3_777 ? O14 Na1 O14 75.2(5) 4_737 3_777 ? O8 Na1 O14 73.4(4) . . ? O8 Na1 O14 63.8(4) 3_777 . ? O8 Na1 O14 85.9(5) 4_737 . ? O8 Na1 O14 144.1(7) 2_955 . ? O14 Na1 O14 128.8(6) 4_737 . ? O14 Na1 O14 128.6(6) 3_777 . ? O8 Na1 O14 144.2(6) . 2_955 ? O8 Na1 O14 85.8(5) 3_777 2_955 ? O8 Na1 O14 63.8(4) 4_737 2_955 ? O8 Na1 O14 73.3(5) 2_955 2_955 ? O14 Na1 O14 128.8(6) 4_737 2_955 ? O14 Na1 O14 128.6(5) 3_777 2_955 ? O14 Na1 O14 75.6(5) . 2_955 ? O8 Na1 P4 20.9(2) . . ? O8 Na1 P4 75.3(4) 3_777 . ? O8 Na1 P4 113.0(5) 4_737 . ? O8 Na1 P4 142.7(6) 2_955 . ? O14 Na1 P4 81.6(4) 4_737 . ? O14 Na1 P4 79.4(4) 3_777 . ? O14 Na1 P4 64.2(3) . . ? O14 Na1 P4 139.8(5) 2_955 . ? O8 Na1 Mo1 38.2(3) . 4_737 ? O8 Na1 Mo1 132.0(6) 3_777 4_737 ? O8 Na1 Mo1 74.0(4) 4_737 4_737 ? O8 Na1 Mo1 112.8(5) 2_955 4_737 ? O14 Na1 Mo1 27.5(2) 4_737 4_737 ? O14 Na1 Mo1 86.2(4) 3_777 4_737 ? O14 Na1 Mo1 102.3(4) . 4_737 ? O14 Na1 Mo1 137.8(5) 2_955 4_737 ? P4 Na1 Mo1 58.3(2) . 4_737 ? O8 Na1 Mo1 74.0(4) . . ? O8 Na1 Mo1 38.3(3) 3_777 . ? O8 Na1 Mo1 113.2(5) 4_737 . ? O8 Na1 Mo1 132.1(6) 2_955 . ? O14 Na1 Mo1 137.6(5) 4_737 . ? O14 Na1 Mo1 102.1(5) 3_777 . ? O14 Na1 Mo1 27.5(2) . . ? O14 Na1 Mo1 86.5(4) 2_955 . ? P4 Na1 Mo1 56.8(2) . . ? Mo1 Na1 Mo1 111.2(4) 4_737 . ? O8 Na1 Mo1 112.7(6) . 3_777 ? O8 Na1 Mo1 73.8(4) 3_777 3_777 ? O8 Na1 Mo1 132.0(5) 4_737 3_777 ? O8 Na1 Mo1 38.1(3) 2_955 3_777 ? O14 Na1 Mo1 86.2(4) 4_737 3_777 ? O14 Na1 Mo1 27.41(18) 3_777 3_777 ? O14 Na1 Mo1 137.6(5) . 3_777 ? O14 Na1 Mo1 102.2(4) 2_955 3_777 ? P4 Na1 Mo1 105.9(4) . 3_777 ? Mo1 Na1 Mo1 105.9(4) 4_737 3_777 ? Mo1 Na1 Mo1 111.1(4) . 3_777 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.572 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.183