# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1204 data_ee _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H50 Mo8 N12 Na Ni2 O45 P V8' _chemical_formula_weight 2429.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 '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' '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 P4(3)22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' '-x, y, -z' 'x, -y, -z+1/2' 'y, x, -z+1/4' '-y, -x, -z+3/4' _cell_length_a 15.829(2) _cell_length_b 15.829(2) _cell_length_c 28.712(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7194.0(20) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 5.23 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.243 _exptl_crystal_density_method ? _exptl_crystal_F_000 4672 _exptl_absorpt_coefficient_mu 2.954 _exptl_absorpt_correction_type ; empirical via \y scans North,A.C.T., Phllips,D.C. & Mathews,F.S.(1968), Acta Cryst. A24, 351--359 ; _exptl_absorpt_correction_T_min 0.2649 _exptl_absorpt_correction_T_max 0.2970 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12486 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.05 _reflns_number_total 5048 _reflns_number_observed 3384 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure is disordered, the occupancy factor of major part is 0.8564(6). Two reflections were omited. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(6) _refine_ls_number_reflns 5046 _refine_ls_number_parameters 382 _refine_ls_number_restraints 250 _refine_ls_R_factor_all 0.1103 _refine_ls_R_factor_obs 0.0765 _refine_ls_wR_factor_all 0.2256 _refine_ls_wR_factor_obs 0.1987 _refine_ls_goodness_of_fit_all 1.161 _refine_ls_goodness_of_fit_obs 1.299 _refine_ls_restrained_S_all 1.166 _refine_ls_restrained_S_obs 1.255 _refine_ls_shift/esd_max 0.375 _refine_ls_shift/esd_mean 0.022 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.34078(7) -0.13376(7) -0.19721(4) 0.0298(3) Uani 0.8564(6) d P 1 Mo2 Mo 0.65555(7) -0.13771(7) -0.20036(3) 0.0260(3) Uani 0.8564(6) d P 1 Mo3 Mo 0.49559(8) -0.04643(6) -0.12590(3) 0.0309(3) Uani 0.8564(6) d P 1 Mo4 Mo 0.50095(9) 0.22573(6) -0.22890(3) 0.0306(3) Uani 0.8564(6) d P 1 V1 V 0.65942(12) 0.09263(12) -0.17682(6) 0.0225(5) Uani 0.8564(6) d P 1 V2 V 0.33768(13) 0.08860(12) -0.17428(6) 0.0239(6) Uani 0.8564(6) d P 1 V3 V 0.4962(2) 0.14424(12) -0.13326(6) 0.0334(5) Uani 0.8564(6) d P 1 O1 O 0.6995(4) -0.0220(4) -0.1924(2) 0.023(2) Uiso 0.8564(6) d P 1 O2 O 0.4128(5) 0.0494(5) -0.1257(3) 0.037(2) Uiso 0.8564(6) d P 1 O3 O 0.7109(6) 0.1136(6) -0.2401(3) 0.055(3) Uiso 0.8564(6) d P 1 O4 O 0.2836(5) -0.0238(5) -0.1854(3) 0.032(2) Uiso 0.8564(6) d P 1 O5 O 0.5752(5) 0.0532(6) -0.1346(3) 0.039(2) Uiso 0.8564(6) d P 1 O6 O 0.5773(5) 0.1893(5) -0.1775(3) 0.031(2) Uiso 0.8564(6) d P 1 O7 O 0.5944(5) 0.2285(5) -0.2717(2) 0.021(2) Uiso 0.8564(6) d P 1 O8 O 0.4287(5) 0.1952(5) -0.2768(3) 0.039(2) Uiso 0.8564(6) d P 1 O9 O 0.4031(6) -0.1194(6) -0.1409(3) 0.054(3) Uiso 0.8564(6) d P 1 O10 O 0.2951(5) -0.1086(5) -0.2616(3) 0.039(2) Uiso 0.8564(6) d P 1 O11 O 0.5773(5) -0.1137(5) -0.1545(3) 0.035(2) Uiso 0.8564(6) d P 1 O12 O 0.2677(5) 0.1326(5) -0.1429(3) 0.036(2) Uiso 0.8564(6) d P 1 O13 O 0.5002(6) -0.0697(5) -0.0687(3) 0.046(2) Uiso 0.8564(6) d P 1 O14 O 0.2687(5) -0.2010(5) -0.1773(3) 0.038(2) Uiso 0.8564(6) d P 1 O15 O 0.4893(6) 0.3294(5) -0.2211(3) 0.044(2) Uiso 0.8564(6) d P 1 O16 O 0.7236(6) -0.1991(6) -0.1717(3) 0.054(3) Uiso 0.8564(6) d P 1 O17 O 0.7342(6) 0.1288(5) -0.1413(3) 0.038(2) Uiso 0.8564(6) d P 1 O18 O 0.4903(6) 0.2043(5) -0.0879(3) 0.048(2) Uiso 0.8564(6) d P 1 O19 O 0.4198(5) 0.1780(5) -0.1828(3) 0.032(2) Uiso 0.8564(6) d P 1 P P 0.4990(2) 0.0000 -0.2500 0.0144(7) Uani 1 d S 3 O22 O 0.4442(4) -0.0122(5) -0.2071(2) 0.035(2) Uiso 1 d . 3 O23 O 0.5544(4) -0.0773(4) -0.2558(2) 0.039(2) Uiso 1 d . 3 V4 V 0.75398(13) 0.0000 -0.2500 0.0304(6) Uani 1 d S . V5 V 0.24218(13) 0.0000 -0.2500 0.0333(6) Uani 1 d S . O20 O 0.1367(7) 0.0000 -0.2500 0.054(3) Uiso 1 d S . O21 O 0.8546(7) 0.0000 -0.2500 0.056(3) Uiso 1 d S . Na Na 0.4258(2) 0.5742(2) -0.1250 0.0356(13) Uani 1 d SU . OW1 O 0.6814(10) 0.3186(10) -0.1250 0.159(9) Uiso 1 d S . Ni Ni -0.02459(8) -0.22774(7) -0.25390(4) 0.0418(4) Uani 1 d D . N1 N 0.0309(4) -0.2646(5) -0.31303(13) 0.083(4) Uiso 1 d D . H1C H -0.0084(4) -0.2908(5) -0.33051(13) 0.100 Uiso 1 d R . H1D H 0.0723(4) -0.3019(5) -0.30687(13) 0.100 Uiso 1 d R . N2 N -0.0053(8) -0.1104(6) -0.2874(3) 0.067(3) Uiso 1 d . . H2C H 0.0439(8) -0.0865(6) -0.2788(3) 0.080 Uiso 1 d R . H2D H -0.0478(8) -0.0747(6) -0.2805(3) 0.080 Uiso 1 d R . N3 N 0.0886(2) -0.2190(10) -0.2234(2) 0.118(5) Uiso 1 d D . H3C H 0.1162(2) -0.1729(10) -0.2336(2) 0.142 Uiso 1 d R . H3D H 0.1204(2) -0.2650(10) -0.2291(2) 0.142 Uiso 1 d R . N4 N -0.0691(7) -0.1692(7) -0.1911(4) 0.065(3) Uiso 1 d U . H4C H -0.0994(7) -0.2063(7) -0.1742(4) 0.078 Uiso 1 d R . H4D H -0.1019(7) -0.1245(7) -0.1981(4) 0.078 Uiso 1 d R . N5 N -0.1500(4) -0.2492(2) -0.2854(2) 0.066(3) Uiso 1 d D . H5C H -0.1493(4) -0.2492(2) -0.3168(2) 0.080 Uiso 1 d R . H5D H -0.1850(4) -0.2081(2) -0.2757(2) 0.080 Uiso 1 d R . C1 C 0.0612(10) -0.1910(9) -0.3393(5) 0.073(4) Uiso 1 d . . H1A H 0.0738(10) -0.2065(9) -0.3709(5) 0.088 Uiso 1 d R . H1B H 0.1114(10) -0.1698(9) -0.3247(5) 0.088 Uiso 1 d R . C2 C -0.0016(8) -0.1272(6) -0.3369(3) 0.039(2) Uiso 1 d . . H2A H 0.0107(8) -0.0783(6) -0.3555(3) 0.047 Uiso 1 d R . H2B H -0.0544(8) -0.1512(6) -0.3467(3) 0.047 Uiso 1 d R . C3 C 0.0681(9) -0.2099(9) -0.1687(4) 0.069(3) Uiso 1 d U . H3A H 0.0478(9) -0.2629(9) -0.1570(4) 0.083 Uiso 1 d R . H3B H 0.1182(9) -0.1948(9) -0.1517(4) 0.083 Uiso 1 d R . C4 C 0.0006(9) -0.1463(7) -0.1645(4) 0.054(2) Uiso 1 d U . H4A H -0.0122(9) -0.1391(7) -0.1320(4) 0.065 Uiso 1 d R . H4B H 0.0208(9) -0.0935(7) -0.1765(4) 0.065 Uiso 1 d R . C5 C -0.1815(2) -0.3253(2) -0.2633(2) 0.098(6) Uiso 1 d D . H5A H -0.2135(2) -0.3526(2) -0.2874(2) 0.118 Uiso 1 d R . H5B H -0.2190(2) -0.3157(2) -0.2376(2) 0.118 Uiso 1 d R . C6 C -0.1142(2) -0.3687(4) -0.2387(2) 0.129(5) Uiso 0.43(3) d PDU . H6A H -0.0987(2) -0.4073(4) -0.2635(2) 0.155 Uiso 1 d R . H6B H -0.1387(2) -0.4029(4) -0.2142(2) 0.155 Uiso 1 d R . N6 N -0.0318(2) -0.3408(2) -0.2229(2) 0.120(5) Uiso 0.43(3) d PDU 1 H6C H -0.0343(2) -0.3421(2) -0.1916(2) 0.144 Uiso 1 d R 1 H6D H 0.0121(2) -0.3727(2) -0.2323(2) 0.144 Uiso 1 d R 1 C6' C -0.1199(2) -0.3892(3) -0.2509(3) 0.124(5) Uiso 0.57(3) d PDU 2 N6' N -0.0418(3) -0.3591(2) -0.2304(2) 0.111(5) Uiso 0.57(3) d PDU 2 Mo1' Mo 0.4873(3) 0.0409(3) -0.12494(13) 0.0160(9) Uani 0.1436(6) d PDU 2 Mo2' Mo 0.5065(4) 0.2257(2) -0.2684(2) 0.0188(9) Uani 0.1436(6) d PDU 2 Mo3' Mo 0.3381(3) 0.1222(2) -0.1901(2) 0.0104(10) Uani 0.1436(6) d PDU 2 Mo4' Mo 0.6533(3) 0.1384(3) -0.20066(13) 0.0102(9) Uani 0.1436(6) d PDU 2 V1' V 0.6548(5) -0.1058(6) -0.1812(2) 0.0079(13) Uani 0.1436(6) d PDU 2 V2' V 0.4956(3) -0.1487(3) -0.1336(2) 0.0182(13) Uani 0.1436(6) d PDU 2 V3' V 0.3352(4) -0.0834(5) -0.1756(3) 0.0089(12) Uani 0.1436(6) d PDU 2 O1' O 0.7390(5) 0.1640(15) -0.1671(4) 0.011(5) Uiso 0.1436(6) d PDU 2 O2' O 0.3946(24) 0.1236(24) -0.1337(12) 0.012(2) Uiso 0.1436(6) d PU 2 O3' O 0.7074(8) -0.1206(20) -0.1339(3) 0.014(5) Uiso 0.1436(6) d PDU 2 O4' O 0.4938(22) 0.3326(4) -0.2732(11) 0.016(5) Uiso 0.1436(6) d PDU 2 O5' O 0.4345(27) 0.1699(26) -0.3132(13) 0.018(3) Uiso 0.1436(6) d PU 2 O6' O 0.5700(25) -0.0443(26) -0.1335(13) 0.013(2) Uiso 0.1436(6) d PU 2 O7' O 0.5665(26) 0.1161(25) -0.1569(13) 0.013(2) Uiso 0.1436(6) d PU 2 O8' O 0.2672(7) -0.1454(8) -0.1517(6) 0.009(5) Uiso 0.1436(6) d PDU 2 O9' O 0.4102(4) -0.0419(4) -0.1065(5) 0.016(2) Uiso 0.1436(6) d PDU 2 O10' O 0.5923(27) 0.2082(27) -0.3199(14) 0.019(3) Uiso 0.1436(6) d PU 2 O11' O 0.6788(23) 0.0150(25) -0.1926(12) 0.010(2) Uiso 0.1436(6) d PU 2 O12' O 0.3053(21) -0.0968(22) -0.2461(14) 0.006(3) Uiso 0.1436(6) d PU 2 O13' O 0.2876(8) 0.0338(5) -0.1892(13) 0.011(2) Uiso 0.1436(6) d PDU 2 O14' O 0.2815(7) 0.2031(6) -0.1657(6) 0.016(5) Uiso 0.1436(6) d PDU 2 O15' O 0.5244(12) -0.2125(7) -0.0928(4) 0.016(5) Uiso 0.1436(6) d PDU 2 O16' O 0.5680(26) 0.2102(26) -0.1940(14) 0.016(2) Uiso 0.1436(6) d PU 2 O17' O 0.5224(11) 0.0595(18) -0.0696(3) 0.016(5) Uiso 0.1436(6) d PDU 2 O18' O 0.7120(7) 0.1251(20) -0.2460(3) 0.011(3) Uiso 0.1436(6) d PDU 2 O19' O 0.4132(26) 0.2091(26) -0.2198(13) 0.015(2) Uiso 0.1436(6) d PU 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 Mo1 0.0239(5) 0.0270(6) 0.0384(6) 0.0089(5) 0.0067(5) -0.0037(5) Mo2 0.0222(5) 0.0240(6) 0.0317(5) 0.0054(5) -0.0011(5) 0.0020(5) Mo3 0.0411(6) 0.0312(5) 0.0203(4) 0.0012(4) 0.0020(6) -0.0003(7) Mo4 0.0400(6) 0.0192(4) 0.0325(5) -0.0014(4) -0.0028(6) -0.0016(7) V1 0.0216(10) 0.0224(10) 0.0234(9) 0.0044(9) -0.0092(9) -0.0091(9) V2 0.0284(11) 0.0177(10) 0.0256(10) 0.0040(9) 0.0111(9) 0.0026(9) V3 0.0502(12) 0.0269(10) 0.0232(9) -0.0068(8) -0.0013(12) 0.0041(14) P 0.0140(13) 0.0134(13) 0.0158(12) 0.0001(14) 0.000 0.000 V4 0.0174(10) 0.0297(12) 0.0442(13) -0.0114(15) 0.000 0.000 V5 0.0131(10) 0.0336(12) 0.0533(14) 0.028(2) 0.000 0.000 Na 0.038(2) 0.038(2) 0.030(2) 0.0002(14) 0.0002(14) 0.025(2) Ni 0.0607(9) 0.0348(7) 0.0298(6) -0.0005(7) 0.0012(8) 0.0017(6) Mo1' 0.011(2) 0.020(2) 0.017(2) -0.0029(14) 0.0062(15) -0.002(2) Mo2' 0.015(2) 0.023(2) 0.019(2) -0.0008(15) -0.001(2) 0.004(2) Mo3' 0.007(2) 0.013(2) 0.012(2) -0.001(2) 0.005(2) 0.005(2) Mo4' 0.007(2) 0.013(2) 0.011(2) -0.0021(15) -0.0045(14) -0.0031(15) V1' 0.006(2) 0.008(2) 0.011(2) 0.001(2) -0.002(2) 0.000(2) V2' 0.018(2) 0.020(2) 0.017(2) 0.002(2) 0.003(2) -0.001(2) V3' 0.007(2) 0.010(2) 0.010(2) 0.000(2) 0.001(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O14 1.661(9) . ? Mo1 O8 1.855(9) 6_554 ? Mo1 O9 1.908(9) . ? Mo1 O4 1.990(8) . ? Mo1 O10 2.024(8) . ? Mo1 V5 3.036(2) . ? Mo2 O16 1.668(10) . ? Mo2 O11 1.847(8) . ? Mo2 O7 1.910(7) 6_554 ? Mo2 O3 1.959(9) 6_554 ? Mo2 O1 1.972(7) . ? Mo2 V4 3.035(2) . ? Mo3 O13 1.684(8) . ? Mo3 O11 1.866(8) . ? Mo3 O9 1.913(10) . ? Mo3 O2 2.005(8) . ? Mo3 O5 2.034(9) . ? Mo3 V3 3.026(2) . ? Mo4 O15 1.667(8) . ? Mo4 O8 1.852(8) . ? Mo4 O7 1.923(7) . ? Mo4 O6 1.993(8) . ? Mo4 O19 1.993(8) . ? Mo4 V3 3.035(2) . ? V1 O17 1.665(8) . ? V1 O5 1.908(9) . ? V1 O1 1.973(7) . ? V1 O6 2.008(8) . ? V1 O3 2.017(9) . ? V1 V4 2.967(2) . ? V1 V3 2.985(3) . ? V2 O12 1.589(8) . ? V2 O2 1.935(8) . ? V2 O19 1.936(8) . ? V2 O10 1.987(8) 6_554 ? V2 O4 2.001(8) . ? V2 V3 2.908(3) . ? V2 V5 2.996(2) . ? V3 O18 1.616(8) . ? V3 O5 1.908(9) . ? V3 O6 1.942(8) . ? V3 O19 1.943(8) . ? V3 O2 2.010(9) . ? O1 V4 1.898(7) . ? O3 V4 1.945(10) . ? O3 Mo2 1.959(9) 6_554 ? O4 V5 2.002(7) . ? O7 Mo2 1.910(7) 6_554 ? O8 Mo1 1.855(9) 6_554 ? O10 V5 1.940(8) . ? O10 V2 1.987(8) 6_554 ? P O23 1.514(7) 6_554 ? P O23 1.514(7) . ? P O22 1.518(6) . ? P O22 1.518(6) 6_554 ? V4 O21 1.593(11) . ? V4 O1 1.898(7) 6_554 ? V4 O3 1.945(10) 6_554 ? V4 O11' 2.05(4) . ? V4 O11' 2.05(4) 6_554 ? V4 O18' 2.09(3) 6_554 ? V4 O18' 2.09(3) . ? V4 V1 2.967(2) 6_554 ? V4 V1' 3.029(8) . ? V5 O20 1.670(11) . ? V5 O12' 1.83(3) 6_554 ? V5 O12' 1.83(3) . ? V5 O10 1.940(8) 6_554 ? V5 O13' 1.96(3) . ? V5 O13' 1.96(3) 6_554 ? V5 O4 2.002(7) 6_554 ? V5 V3' 2.910(8) . ? V5 V3' 2.910(8) 6_554 ? Ni N1 1.999(4) . ? Ni N3 1.999(4) . ? Ni N6 2.003(3) . ? Ni N2 2.114(10) . ? Ni N4 2.146(10) . ? Ni N6' 2.203(3) . ? Ni N5 2.208(7) . ? N1 C1 1.47(2) . ? N1 H1C 0.90 . ? N1 H1D 0.90 . ? N2 C2 1.447(12) . ? N2 H2C 0.90 . ? N2 H2D 0.90 . ? N3 C3 1.609(14) . ? N3 H3C 0.90 . ? N3 H3D 0.90 . ? N4 C4 1.39(2) . ? N4 H4C 0.90 . ? N4 H4D 0.90 . ? N5 C5 1.450(4) . ? N5 H5C 0.90 . ? N5 H5D 0.90 . ? C1 C2 1.42(2) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C3 C4 1.47(2) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C5 C6' 1.449(4) . ? C5 C6 1.450(4) . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C6 N6' 1.181(5) . ? C6 N6 1.450(4) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? N6 H6C 0.90 . ? N6 H6D 0.90 . ? C6' N6' 1.451(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 O14 Mo1 O8 108.6(4) . 6_554 ? O14 Mo1 O9 98.1(4) . . ? O8 Mo1 O9 90.9(4) 6_554 . ? O14 Mo1 O4 100.9(4) . . ? O8 Mo1 O4 150.2(3) 6_554 . ? O9 Mo1 O4 89.3(4) . . ? O14 Mo1 O10 101.2(4) . . ? O8 Mo1 O10 90.2(3) 6_554 . ? O9 Mo1 O10 159.2(4) . . ? O4 Mo1 O10 79.7(3) . . ? O14 Mo1 V5 105.4(3) . . ? O8 Mo1 V5 123.4(3) 6_554 . ? O9 Mo1 V5 127.3(3) . . ? O4 Mo1 V5 40.7(2) . . ? O10 Mo1 V5 39.0(2) . . ? O16 Mo2 O11 101.6(4) . . ? O16 Mo2 O7 95.5(4) . 6_554 ? O11 Mo2 O7 96.5(3) . 6_554 ? O16 Mo2 O3 104.8(4) . 6_554 ? O11 Mo2 O3 151.9(4) . 6_554 ? O7 Mo2 O3 90.4(3) 6_554 6_554 ? O16 Mo2 O1 104.9(4) . . ? O11 Mo2 O1 87.9(3) . . ? O7 Mo2 O1 157.9(3) 6_554 . ? O3 Mo2 O1 76.3(3) 6_554 . ? O16 Mo2 V4 108.6(3) . . ? O11 Mo2 V4 122.1(3) . . ? O7 Mo2 V4 127.1(2) 6_554 . ? O3 Mo2 V4 38.8(3) 6_554 . ? O1 Mo2 V4 37.5(2) . . ? O13 Mo3 O11 105.9(4) . . ? O13 Mo3 O9 96.9(4) . . ? O11 Mo3 O9 95.0(4) . . ? O13 Mo3 O2 101.0(4) . . ? O11 Mo3 O2 152.4(3) . . ? O9 Mo3 O2 87.6(4) . . ? O13 Mo3 O5 105.2(4) . . ? O11 Mo3 O5 87.7(4) . . ? O9 Mo3 O5 156.1(4) . . ? O2 Mo3 O5 79.5(3) . . ? O13 Mo3 V3 106.6(3) . . ? O11 Mo3 V3 122.5(3) . . ? O9 Mo3 V3 126.1(3) . . ? O2 Mo3 V3 41.2(2) . . ? O5 Mo3 V3 38.4(2) . . ? O15 Mo4 O8 106.8(4) . . ? O15 Mo4 O7 98.5(4) . . ? O8 Mo4 O7 90.4(3) . . ? O15 Mo4 O6 104.6(4) . . ? O8 Mo4 O6 148.0(4) . . ? O7 Mo4 O6 90.8(3) . . ? O15 Mo4 O19 102.3(4) . . ? O8 Mo4 O19 89.7(3) . . ? O7 Mo4 O19 158.2(3) . . ? O6 Mo4 O19 77.9(3) . . ? O15 Mo4 V3 107.1(3) . . ? O8 Mo4 V3 123.0(3) . . ? O7 Mo4 V3 127.4(2) . . ? O6 Mo4 V3 38.9(2) . . ? O19 Mo4 V3 38.9(2) . . ? O17 V1 O5 102.7(4) . . ? O17 V1 O1 103.1(4) . . ? O5 V1 O1 93.9(3) . . ? O17 V1 O6 101.8(4) . . ? O5 V1 O6 78.6(3) . . ? O1 V1 O6 155.0(3) . . ? O17 V1 O3 102.0(4) . . ? O5 V1 O3 155.3(4) . . ? O1 V1 O3 79.5(3) . . ? O6 V1 O3 97.3(3) . . ? O17 V1 V4 104.2(3) . . ? O5 V1 V4 129.9(3) . . ? O1 V1 V4 39.0(2) . . ? O6 V1 V4 134.1(2) . . ? O3 V1 V4 40.6(3) . . ? O17 V1 V3 105.3(3) . . ? O5 V1 V3 38.5(3) . . ? O1 V1 V3 128.7(2) . . ? O6 V1 V3 40.1(2) . . ? O3 V1 V3 133.0(3) . . ? V4 V1 V3 150.30(9) . . ? O12 V2 O2 99.2(4) . . ? O12 V2 O19 102.7(4) . . ? O2 V2 O19 85.0(3) . . ? O12 V2 O10 102.7(4) . 6_554 ? O2 V2 O10 158.1(4) . 6_554 ? O19 V2 O10 89.6(3) . 6_554 ? O12 V2 O4 100.5(4) . . ? O2 V2 O4 95.3(3) . . ? O19 V2 O4 156.5(3) . . ? O10 V2 O4 81.3(3) 6_554 . ? O12 V2 V3 103.8(3) . . ? O2 V2 V3 43.5(3) . . ? O19 V2 V3 41.5(2) . . ? O10 V2 V3 128.3(3) 6_554 . ? O4 V2 V3 134.7(2) . . ? O12 V2 V5 105.4(3) . . ? O2 V2 V5 133.1(3) . . ? O19 V2 V5 126.0(2) . . ? O10 V2 V5 39.7(2) 6_554 . ? O4 V2 V5 41.6(2) . . ? V3 V2 V5 150.56(9) . . ? O18 V3 O5 119.9(4) . . ? O18 V3 O6 110.4(4) . . ? O5 V3 O6 80.3(4) . . ? O18 V3 O19 113.2(4) . . ? O5 V3 O19 126.9(3) . . ? O6 V3 O19 80.3(3) . . ? O18 V3 O2 108.3(4) . . ? O5 V3 O2 82.5(3) . . ? O6 V3 O2 141.2(3) . . ? O19 V3 O2 82.8(3) . . ? O18 V3 V2 117.1(4) . . ? O5 V3 V2 109.2(3) . . ? O6 V3 V2 114.6(2) . . ? O19 V3 V2 41.4(2) . . ? O2 V3 V2 41.5(2) . . ? O18 V3 V1 123.3(4) . . ? O5 V3 V1 38.5(3) . . ? O6 V3 V1 41.7(2) . . ? O19 V3 V1 107.9(2) . . ? O2 V3 V1 114.2(3) . . ? V2 V3 V1 119.62(8) . . ? O18 V3 Mo3 122.1(3) . . ? O5 V3 Mo3 41.4(3) . . ? O6 V3 Mo3 114.5(2) . . ? O19 V3 Mo3 108.9(2) . . ? O2 V3 Mo3 41.0(2) . . ? V2 V3 Mo3 73.95(7) . . ? V1 V3 Mo3 76.04(7) . . ? O18 V3 Mo4 118.7(3) . . ? O5 V3 Mo4 106.7(3) . . ? O6 V3 Mo4 40.2(2) . . ? O19 V3 Mo4 40.2(2) . . ? O2 V3 Mo4 115.5(2) . . ? V2 V3 Mo4 77.51(7) . . ? V1 V3 Mo4 73.47(6) . . ? Mo3 V3 Mo4 119.16(6) . . ? V4 O1 Mo2 103.3(3) . . ? V4 O1 V1 100.0(3) . . ? Mo2 O1 V1 140.1(4) . . ? V2 O2 Mo3 130.0(4) . . ? V2 O2 V3 95.0(4) . . ? Mo3 O2 V3 97.8(4) . . ? V4 O3 Mo2 102.0(4) . 6_554 ? V4 O3 V1 97.0(4) . . ? Mo2 O3 V1 129.6(5) 6_554 . ? Mo1 O4 V2 127.6(4) . . ? Mo1 O4 V5 99.0(3) . . ? V2 O4 V5 96.9(3) . . ? V1 O5 V3 102.9(4) . . ? V1 O5 Mo3 139.8(5) . . ? V3 O5 Mo3 100.2(4) . . ? V3 O6 Mo4 100.9(4) . . ? V3 O6 V1 98.2(3) . . ? Mo4 O6 V1 128.3(4) . . ? Mo2 O7 Mo4 129.9(4) 6_554 . ? Mo4 O8 Mo1 154.0(5) . 6_554 ? Mo1 O9 Mo3 131.2(5) . . ? V5 O10 V2 99.5(4) . 6_554 ? V5 O10 Mo1 99.9(3) . . ? V2 O10 Mo1 139.2(4) 6_554 . ? Mo2 O11 Mo3 153.6(5) . . ? V2 O19 V3 97.1(4) . . ? V2 O19 Mo4 142.6(4) . . ? V3 O19 Mo4 100.9(4) . . ? O23 P O23 109.2(5) 6_554 . ? O23 P O22 110.1(4) 6_554 . ? O23 P O22 108.5(4) . . ? O23 P O22 108.5(4) 6_554 6_554 ? O23 P O22 110.1(4) . 6_554 ? O22 P O22 110.3(5) . 6_554 ? O21 V4 O1 117.0(2) . . ? O21 V4 O1 117.0(2) . 6_554 ? O1 V4 O1 125.9(4) . 6_554 ? O21 V4 O3 110.5(3) . . ? O1 V4 O3 83.2(3) . . ? O1 V4 O3 78.4(3) 6_554 . ? O21 V4 O3 110.5(3) . 6_554 ? O1 V4 O3 78.4(3) . 6_554 ? O1 V4 O3 83.2(3) 6_554 6_554 ? O3 V4 O3 138.9(5) . 6_554 ? O21 V4 V1 120.29(5) . . ? O1 V4 V1 40.9(2) . . ? O1 V4 V1 107.3(2) 6_554 . ? O3 V4 V1 42.4(3) . . ? O3 V4 V1 112.6(3) 6_554 . ? O21 V4 V1 120.29(5) . 6_554 ? O1 V4 V1 107.3(2) . 6_554 ? O1 V4 V1 40.9(2) 6_554 6_554 ? O3 V4 V1 112.6(3) . 6_554 ? O3 V4 V1 42.4(3) 6_554 6_554 ? V1 V4 V1 119.41(10) . 6_554 ? O20 V5 O10 115.6(2) . 6_554 ? O20 V5 O10 115.6(2) . . ? O10 V5 O10 128.8(5) 6_554 . ? O20 V5 O4 109.1(2) . 6_554 ? O10 V5 O4 81.4(3) 6_554 6_554 ? O10 V5 O4 82.4(3) . 6_554 ? O20 V5 O4 109.1(2) . . ? O10 V5 O4 82.4(3) 6_554 . ? O10 V5 O4 81.4(3) . . ? O4 V5 O4 141.8(5) 6_554 . ? O20 V5 V2 120.30(5) . . ? O10 V5 V2 40.8(2) 6_554 . ? O10 V5 V2 108.7(2) . . ? O4 V5 V2 114.7(2) 6_554 . ? O4 V5 V2 41.5(2) . . ? N1 Ni N3 89.9(3) . . ? N1 Ni N6 98.1(3) . . ? N3 Ni N6 85.3(4) . . ? N1 Ni N2 78.9(4) . . ? N3 Ni N2 90.5(5) . . ? N6 Ni N2 174.9(4) . . ? N1 Ni N4 169.7(4) . . ? N3 Ni N4 84.0(4) . . ? N6 Ni N4 89.6(3) . . ? N2 Ni N4 92.9(4) . . ? N1 Ni N6' 92.3(3) . . ? N3 Ni N6' 92.4(5) . . ? N2 Ni N6' 170.7(3) . . ? N4 Ni N6' 96.3(3) . . ? N1 Ni N5 90.1(2) . . ? N3 Ni N5 174.9(5) . . ? N6 Ni N5 89.7(2) . . ? N2 Ni N5 94.5(3) . . ? N4 Ni N5 96.6(3) . . ? N6' Ni N5 82.5(2) . . ? C1 N1 Ni 110.4(7) . . ? C1 N1 H1C 107.7(6) . . ? Ni N1 H1C 107.7(2) . . ? C1 N1 H1D 112.6(6) . . ? Ni N1 H1D 110.2(2) . . ? H1C N1 H1D 108.1 . . ? C2 N2 Ni 106.9(7) . . ? C2 N2 H2C 108.2(7) . . ? Ni N2 H2C 111.6(3) . . ? C2 N2 H2D 111.2(7) . . ? Ni N2 H2D 110.1(3) . . ? H2C N2 H2D 108.9 . . ? C3 N3 Ni 104.7(6) . . ? C3 N3 H3C 110.1(7) . . ? Ni N3 H3C 110.3(4) . . ? C3 N3 H3D 111.3(7) . . ? Ni N3 H3D 111.5(4) . . ? H3C N3 H3D 108.9 . . ? C4 N4 Ni 108.3(8) . . ? C4 N4 H4C 107.3(7) . . ? Ni N4 H4C 110.3(3) . . ? C4 N4 H4D 112.0(7) . . ? Ni N4 H4D 110.0(3) . . ? H4C N4 H4D 108.9 . . ? C5 N5 Ni 104.9(4) . . ? C5 N5 H5C 116.3(3) . . ? Ni N5 H5C 113.6(2) . . ? C5 N5 H5D 104.6(3) . . ? Ni N5 H5D 108.37(14) . . ? H5C N5 H5D 108.6 . . ? C2 C1 N1 108.2(11) . . ? C2 C1 H1A 111.9(7) . . ? N1 C1 H1A 110.6(6) . . ? C2 C1 H1B 108.0(8) . . ? N1 C1 H1B 108.9(6) . . ? H1A C1 H1B 109.1 . . ? C1 C2 N2 102.0(10) . . ? C1 C2 H2A 113.9(7) . . ? N2 C2 H2A 113.9(6) . . ? C1 C2 H2B 108.2(8) . . ? N2 C2 H2B 109.0(7) . . ? H2A C2 H2B 109.4 . . ? C4 C3 N3 106.8(10) . . ? C4 C3 H3A 109.0(8) . . ? N3 C3 H3A 109.3(7) . . ? C4 C3 H3B 112.8(7) . . ? N3 C3 H3B 110.6(6) . . ? H3A C3 H3B 108.4 . . ? N4 C4 C3 110.6(10) . . ? N4 C4 H4A 113.3(7) . . ? C3 C4 H4A 108.4(7) . . ? N4 C4 H4B 107.0(7) . . ? C3 C4 H4B 109.0(8) . . ? H4A C4 H4B 108.4 . . ? C6' C5 C6 19.3(3) . . ? C6' C5 N5 117.1(4) . . ? C6 C5 N5 110.8(4) . . ? C6' C5 H5A 102.6(3) . . ? C6 C5 H5A 121.6(3) . . ? N5 C5 H5A 103.8(3) . . ? C6' C5 H5B 109.8(3) . . ? C6 C5 H5B 98.9(3) . . ? N5 C5 H5B 114.8(3) . . ? H5A C5 H5B 107.4 . . ? N6' C6 C5 138.6(5) . . ? C5 C6 N6 132.0(4) . . ? N6' C6 H6A 89.1(4) . . ? C5 C6 H6A 97.3(3) . . ? N6 C6 H6A 101.2(3) . . ? N6' C6 H6B 108.2(4) . . ? C5 C6 H6B 108.9(2) . . ? N6 C6 H6B 107.6(3) . . ? H6A C6 H6B 106.3 . . ? C6 N6 Ni 100.5(3) . . ? C6 N6 H6C 105.5(3) . . ? Ni N6 H6C 117.8(2) . . ? C6 N6 H6D 115.5(3) . . ? Ni N6 H6D 108.85(14) . . ? H6C N6 H6D 108.8 . . ? C5 C6' N6' 116.3(3) . . ? C5 C6' H6A 126.3(10) . . ? N6' C6' H6A 85.5(6) . . ? C5 C6' H6B 100.8(4) . . ? N6' C6' H6B 84.7(5) . . ? H6A C6' H6B 131.0(9) . . ? C6 N6' C6' 17.8(4) . . ? C6 N6' Ni 100.3(3) . . ? C6' N6' Ni 106.9(3) . . ? C6 N6' H6C 109.1(6) . . ? Ni N6' H6C 93.6(2) . . ? C6 N6' H6D 153.5(7) . . ? Ni N6' H6D 95.3(3) . . ? H6C N6' H6D 91.1(6) . . ? _refine_diff_density_max 3.443 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.268