Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email XJQ@MAIL.JLU.EDU.CN _publ_contact_author_name 'Prof Ji-Qing Xu' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Xu Ji-Qing' 'Cui Xiao-Bing' 'Li Guanghua' 'Lu Zheng-Laing' ; Pan Cheng-Ling ; data_m _database_code_CSD 187586 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H64 Cl K N12 Ni3 O50 V18' _chemical_formula_weight 2344.35 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 12.799(3) _cell_length_b 27.717(6) _cell_length_c 21.096(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.68(3) _cell_angle_gamma 90.00 _cell_volume 7475(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10114 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 27.47 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4616 _exptl_absorpt_coefficient_mu 3.054 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3891 _exptl_absorpt_correction_T_max 0.8215 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan ; _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 RAXIS-RAPID' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number None _diffrn_standards_interval_count None _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 16370 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8563 _reflns_number_gt 4810 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'Crystal Structure' _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^)+(0.0925P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8563 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1758 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.01307(7) 0.79820(4) 0.09588(5) 0.0228(2) Uani 1 1 d . . . Ni2 Ni 0.496(7) 0.998(4) 0.504(4) 0.024(4) Uani 0.50 1 d P . . Cl Cl 1.0000 0.34035(15) 0.2500 0.0619(11) Uani 1 2 d S . . V1 V 0.23604(9) 0.84139(5) 0.32601(6) 0.0188(3) Uani 1 1 d . . . V2 V 0.21764(9) 0.83305(5) 0.18761(6) 0.0204(3) Uani 1 1 d . . . V3 V 0.43868(9) 0.93150(5) 0.36523(6) 0.0207(3) Uani 1 1 d . . . V4 V 0.31871(9) 0.74266(5) 0.30165(6) 0.0209(3) Uani 1 1 d . . . V5 V 0.41098(9) 0.83256(5) 0.41775(6) 0.0206(3) Uani 1 1 d . . . V6 V 0.30521(9) 0.93189(5) 0.20824(6) 0.0205(3) Uani 1 1 d . . . V7 V 0.36264(9) 0.84172(5) 0.08803(6) 0.0239(3) Uani 1 1 d . . . V8 V 0.40599(9) 0.74261(5) 0.13753(6) 0.0230(3) Uani 1 1 d . . . V9 V 0.5000 0.97717(7) 0.2500 0.0284(5) Uani 1 2 d S . . V10 V 0.5000 0.69973(7) 0.2500 0.0338(5) Uani 1 2 d S . . O1 O 0.5000 1.0349(3) 0.2500 0.046(2) Uani 1 2 d S . . O2 O 0.5000 0.6420(3) 0.2500 0.056(3) Uani 1 2 d S . . O3 O 0.2205(4) 0.9728(2) 0.1881(3) 0.0370(15) Uani 1 1 d . . . O4 O 0.3684(4) 0.7011(2) 0.0885(3) 0.0339(14) Uani 1 1 d . . . O5 O 0.3739(4) 0.8308(2) 0.4897(3) 0.0293(13) Uani 1 1 d . . . O6 O 0.3028(4) 0.8450(2) 0.0196(3) 0.0403(15) Uani 1 1 d . . . O7 O 0.3654(4) 0.7229(2) 0.2203(3) 0.0273(12) Uani 1 1 d . . . O8 O 0.3742(4) 0.95282(19) 0.2862(2) 0.0251(12) Uani 1 1 d . . . O9 O 0.0968(4) 0.8304(2) 0.1596(3) 0.0285(13) Uani 1 1 d . . . O10 O 0.4581(4) 0.7246(2) 0.3292(3) 0.0285(13) Uani 1 1 d . . . O11 O 0.2418(4) 0.7007(2) 0.3244(3) 0.0310(13) Uani 1 1 d . . . O12 O 0.4147(4) 0.9725(2) 0.4179(3) 0.0285(13) Uani 1 1 d . . . O13 O 0.2907(4) 0.88303(19) 0.1426(2) 0.0232(12) Uani 1 1 d . . . O14 O 0.5172(4) 0.88292(19) 0.4125(2) 0.0221(11) Uani 1 1 d . . . O15 O 0.3335(4) 0.88284(19) 0.3724(2) 0.0235(12) Uani 1 1 d . . . O16 O 0.5307(4) 0.79189(19) 0.4140(2) 0.0245(12) Uani 1 1 d . . . O17 O 0.2984(4) 0.79145(19) 0.1361(2) 0.0241(12) Uani 1 1 d . . . O18 O 0.2285(4) 0.88312(18) 0.2527(2) 0.0209(11) Uani 1 1 d . . . O19 O 0.2316(4) 0.79199(18) 0.2613(2) 0.0214(11) Uani 1 1 d . . . O20 O 0.5647(4) 0.95251(19) 0.3268(2) 0.0229(12) Uani 1 1 d . . . O21 O 0.3197(3) 0.79161(18) 0.3686(2) 0.0208(11) Uani 1 1 d . . . O22 O -0.1229(4) 0.84449(19) 0.1407(2) 0.0247(12) Uani 1 1 d . . . N1 N -0.0320(5) 0.7461(3) 0.1628(4) 0.0362(18) Uani 1 1 d . . . H1A H -0.0364 0.7596 0.2013 0.043 Uiso 1 1 calc R . . H1B H -0.0912 0.7294 0.1538 0.043 Uiso 1 1 calc R . . N2 N 0.0990(5) 0.7495(3) 0.0638(3) 0.0337(17) Uani 1 1 d . . . H2A H 0.0883 0.7444 0.0219 0.040 Uiso 1 1 calc R . . H2B H 0.1637 0.7617 0.0707 0.040 Uiso 1 1 calc R . . N3 N -0.1364(5) 0.7755(3) 0.0345(3) 0.0334(17) Uani 1 1 d . . . H3A H -0.1309 0.7437 0.0271 0.040 Uiso 1 1 calc R . . H3B H -0.1978 0.7810 0.0523 0.040 Uiso 1 1 calc R . . N4 N 0.0086(5) 0.8486(3) 0.0261(4) 0.0382(18) Uani 1 1 d . . . H4A H 0.0281 0.8770 0.0437 0.046 Uiso 1 1 calc R . . H4B H 0.0591 0.8388 0.0008 0.046 Uiso 1 1 calc R . . N5 N 0.4811(6) 1.0694(3) 0.4605(4) 0.0417(19) Uani 1 1 d . . . N6 N 0.6402(6) 1.0000(3) 0.4528(4) 0.045(2) Uani 1 1 d . . . C1 C 0.0599(8) 0.7131(4) 0.1625(5) 0.056(3) Uani 1 1 d . . . H1C H 0.1183 0.7275 0.1867 0.067 Uiso 1 1 calc R . . H1D H 0.0429 0.6828 0.1826 0.067 Uiso 1 1 calc R . . C2 C 0.0895(8) 0.7041(4) 0.0983(5) 0.049(3) Uani 1 1 d . . . H2C H 0.0372 0.6839 0.0767 0.058 Uiso 1 1 calc R . . H2D H 0.1558 0.6871 0.0991 0.058 Uiso 1 1 calc R . . C3 C -0.0914(8) 0.8542(4) -0.0112(5) 0.052(3) Uani 1 1 d . . . H3C H -0.0804 0.8711 -0.0506 0.063 Uiso 1 1 calc R . . H3D H -0.1411 0.8723 0.0127 0.063 Uiso 1 1 calc R . . C4 C -0.1323(7) 0.8020(4) -0.0247(4) 0.049(3) Uani 1 1 d . . . H4C H -0.2016 0.8034 -0.0454 0.059 Uiso 1 1 calc R . . H4D H -0.0862 0.7856 -0.0529 0.059 Uiso 1 1 calc R . . C5 C 0.5615(13) 1.0745(4) 0.4136(6) 0.082(4) Uani 1 1 d . . . H5A H 0.5753 1.1084 0.4062 0.099 Uiso 1 1 calc R . . H5B H 0.5372 1.0600 0.3737 0.099 Uiso 1 1 calc R . . C6 C 0.6617(10) 1.0493(5) 0.4386(6) 0.077(4) Uani 1 1 d . . . H6A H 0.7142 1.0510 0.4070 0.092 Uiso 1 1 calc R . . H6B H 0.6890 1.0656 0.4766 0.092 Uiso 1 1 calc R . . OW1 O 0.630(2) 0.4424(6) 0.0592(11) 0.156(13) Uani 0.50 1 d P . . OW2 O 0.5000 0.4080(9) 0.2500 0.168(9) Uani 1 2 d S . . OW3 O 0.7071(15) 0.4184(9) -0.0494(13) 0.147(12) Uani 0.50 1 d P . . OW4 O 0.5252(19) 0.5042(9) 0.1985(15) 0.177(14) Uani 0.50 1 d P . . OW5 O 0.681(4) 0.5846(9) 0.2106(17) 0.28(3) Uani 0.50 1 d P . . OW6 O 0.3421(19) 0.4586(9) 0.112(2) 0.26(3) Uani 0.50 1 d P . . OW7 O 0.6427(7) 0.5245(4) 0.2740(5) 0.094(3) Uani 1 1 d . . . K1 K 0.4818(10) 0.5741(2) 0.2233(3) 0.143(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 Ni1 0.0146(4) 0.0347(6) 0.0192(5) -0.0044(5) 0.0003(4) -0.0007(4) Ni2 0.027(10) 0.031(9) 0.014(13) -0.003(9) 0.005(7) -0.001(7) Cl 0.062(2) 0.065(3) 0.058(3) 0.000 0.001(2) 0.000 V1 0.0120(5) 0.0283(7) 0.0161(6) -0.0004(6) 0.0010(5) -0.0014(5) V2 0.0114(5) 0.0324(8) 0.0173(7) -0.0007(6) -0.0015(5) -0.0012(5) V3 0.0191(6) 0.0278(7) 0.0152(6) -0.0043(6) 0.0013(5) -0.0020(5) V4 0.0140(6) 0.0274(7) 0.0214(7) 0.0015(6) 0.0020(5) -0.0003(5) V5 0.0156(6) 0.0299(7) 0.0162(7) 0.0015(6) 0.0006(5) -0.0007(5) V6 0.0170(6) 0.0266(7) 0.0178(7) 0.0024(6) 0.0009(5) 0.0030(5) V7 0.0170(6) 0.0382(8) 0.0164(7) -0.0031(6) -0.0004(5) 0.0000(5) V8 0.0152(6) 0.0331(8) 0.0205(7) -0.0062(6) 0.0008(5) -0.0029(5) V9 0.0384(11) 0.0258(11) 0.0209(11) 0.000 -0.0001(9) 0.000 V10 0.0257(10) 0.0275(11) 0.0482(14) 0.000 0.0039(9) 0.000 O1 0.066(6) 0.035(5) 0.037(6) 0.000 -0.001(5) 0.000 O2 0.044(5) 0.026(5) 0.100(9) 0.000 0.003(6) 0.000 O3 0.028(3) 0.038(4) 0.045(4) 0.010(3) 0.001(3) 0.010(3) O4 0.023(3) 0.046(4) 0.033(3) -0.012(3) 0.000(2) -0.005(2) O5 0.027(3) 0.041(4) 0.020(3) 0.002(3) 0.003(2) 0.000(2) O6 0.033(3) 0.065(4) 0.023(3) -0.008(3) -0.006(3) 0.001(3) O7 0.022(3) 0.035(3) 0.025(3) -0.004(3) 0.007(2) -0.004(2) O8 0.030(3) 0.027(3) 0.018(3) -0.001(2) 0.000(2) 0.004(2) O9 0.014(2) 0.043(4) 0.027(3) -0.005(3) -0.003(2) 0.000(2) O10 0.016(2) 0.034(3) 0.035(3) 0.011(3) -0.002(2) -0.002(2) O11 0.021(3) 0.035(3) 0.037(4) 0.009(3) 0.006(2) -0.002(2) O12 0.028(3) 0.034(3) 0.023(3) -0.007(3) 0.000(2) -0.001(2) O13 0.017(2) 0.036(3) 0.016(3) -0.001(2) 0.002(2) -0.001(2) O14 0.017(2) 0.029(3) 0.021(3) 0.000(2) 0.002(2) -0.001(2) O15 0.019(2) 0.031(3) 0.021(3) -0.002(2) 0.002(2) 0.000(2) O16 0.018(2) 0.034(3) 0.021(3) 0.005(2) 0.003(2) 0.002(2) O17 0.017(2) 0.034(3) 0.022(3) -0.006(2) 0.001(2) -0.002(2) O18 0.018(2) 0.028(3) 0.017(3) 0.000(2) 0.002(2) -0.003(2) O19 0.018(2) 0.027(3) 0.019(3) 0.000(2) 0.000(2) 0.000(2) O20 0.018(2) 0.031(3) 0.019(3) -0.001(2) 0.003(2) -0.003(2) O21 0.016(2) 0.026(3) 0.020(3) 0.001(2) -0.002(2) 0.001(2) O22 0.018(2) 0.034(3) 0.023(3) -0.003(2) 0.004(2) 0.001(2) N1 0.023(3) 0.049(5) 0.037(4) 0.004(4) 0.005(3) 0.001(3) N2 0.025(3) 0.048(5) 0.029(4) -0.010(4) 0.003(3) 0.002(3) N3 0.022(3) 0.050(5) 0.028(4) -0.019(4) -0.002(3) 0.002(3) N4 0.036(4) 0.046(5) 0.033(4) -0.003(4) 0.001(3) -0.007(3) N5 0.067(5) 0.031(4) 0.028(4) -0.003(4) 0.002(4) 0.001(4) N6 0.034(4) 0.066(6) 0.036(5) -0.016(4) 0.008(3) -0.008(4) C1 0.060(7) 0.047(7) 0.060(8) 0.008(6) 0.008(6) 0.014(5) C2 0.049(6) 0.046(6) 0.051(7) -0.008(5) 0.011(5) 0.013(5) C3 0.056(6) 0.073(8) 0.027(5) 0.015(5) -0.007(5) 0.013(6) C4 0.032(5) 0.090(9) 0.024(5) -0.012(5) -0.004(4) 0.008(5) C5 0.156(14) 0.055(8) 0.037(7) 0.007(6) 0.012(8) -0.030(9) C6 0.083(9) 0.092(10) 0.058(8) -0.021(7) 0.030(7) -0.053(8) OW1 0.23(2) 0.064(12) 0.15(2) 0.066(13) -0.18(2) -0.095(14) OW2 0.038(7) 0.36(3) 0.112(14) 0.000 0.026(8) 0.000 OW3 0.079(14) 0.15(2) 0.21(3) 0.14(2) -0.029(15) -0.012(13) OW4 0.14(2) 0.13(2) 0.27(3) -0.10(2) 0.09(2) -0.110(17) OW5 0.49(6) 0.097(19) 0.26(4) 0.05(2) 0.28(4) 0.17(3) OW6 0.111(19) 0.11(2) 0.58(7) 0.15(3) 0.18(3) 0.055(16) OW7 0.093(7) 0.099(8) 0.086(7) -0.009(6) -0.017(6) 0.028(6) K1 0.308(12) 0.038(3) 0.088(6) 0.015(3) 0.056(8) 0.059(6) _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 Ni1 N1 2.043(7) . ? Ni1 N4 2.057(7) . ? Ni1 N3 2.090(6) . ? Ni1 O9 2.098(5) . ? Ni1 N2 2.104(7) . ? Ni1 O22 2.154(5) . ? Ni2 Ni2 0.21(12) 5_676 ? Ni2 N6 2.01(7) 5_676 ? Ni2 N5 2.04(10) 5_676 ? Ni2 O12 2.12(10) 5_676 ? Ni2 O12 2.17(10) . ? Ni2 N5 2.17(10) . ? Ni2 N6 2.18(7) . ? V1 O22 1.641(5) 2 ? V1 O15 1.928(5) . ? V1 O18 1.931(5) . ? V1 O19 1.932(5) . ? V1 O21 1.941(5) . ? V1 V5 2.9006(19) . ? V1 V2 2.9273(19) . ? V1 V4 2.9870(19) . ? V2 O9 1.631(5) . ? V2 O17 1.919(5) . ? V2 O19 1.928(5) . ? V2 O13 1.944(5) . ? V2 O18 1.952(5) . ? V2 V7 2.877(2) . ? V2 V6 2.9842(19) . ? V3 O12 1.630(5) . ? V3 O15 1.916(5) . ? V3 O8 1.919(5) . ? V3 O20 1.929(5) . ? V3 O14 1.929(5) . ? V3 V9 2.8820(17) . ? V3 V5 2.9849(19) . ? V4 O11 1.611(5) . ? V4 O10 1.917(5) . ? V4 O7 1.923(5) . ? V4 O19 1.936(5) . ? V4 O21 1.958(5) . ? V4 V10 2.8677(16) . ? V5 O5 1.613(6) . ? V5 O21 1.901(5) . ? V5 O16 1.907(5) . ? V5 O15 1.937(5) . ? V5 O14 1.955(5) . ? V5 V7 2.9168(18) 2_655 ? V6 O3 1.611(5) . ? V6 O8 1.919(5) . ? V6 O18 1.938(5) . ? V6 O20 1.939(5) 2_655 ? V6 O13 1.940(5) . ? V6 V9 2.8916(16) . ? V7 O6 1.606(6) . ? V7 O13 1.893(5) . ? V7 O14 1.916(5) 2_655 ? V7 O17 1.930(5) . ? V7 O16 1.943(5) 2_655 ? V7 V5 2.9168(18) 2_655 ? V7 V8 2.982(2) . ? V8 O4 1.605(6) . ? V8 O10 1.912(5) 2_655 ? V8 O7 1.925(6) . ? V8 O17 1.930(5) . ? V8 O16 1.946(5) 2_655 ? V8 V10 2.8675(17) . ? V9 O1 1.601(9) . ? V9 O20 1.910(5) . ? V9 O20 1.910(5) 2_655 ? V9 O8 1.935(5) . ? V9 O8 1.935(5) 2_655 ? V9 V3 2.8820(17) 2_655 ? V9 V6 2.8916(16) 2_655 ? V10 O2 1.601(9) . ? V10 O10 1.908(6) 2_655 ? V10 O10 1.908(6) . ? V10 O7 1.916(5) 2_655 ? V10 O7 1.916(5) . ? V10 V8 2.8675(17) 2_655 ? V10 V4 2.8677(16) 2_655 ? V10 K1 3.534(7) . ? V10 K1 3.534(7) 2_655 ? O2 K1 1.975(10) . ? O2 K1 1.975(10) 2_655 ? O10 V8 1.912(5) 2_655 ? O12 Ni2 2.12(10) 5_676 ? O14 V7 1.916(5) 2_655 ? O16 V7 1.943(5) 2_655 ? O16 V8 1.946(5) 2_655 ? O20 V6 1.939(5) 2_655 ? O22 V1 1.641(5) 2 ? N1 C1 1.489(11) . ? N2 C2 1.460(12) . ? N3 C4 1.452(12) . ? N4 C3 1.479(11) . ? N5 C5 1.468(15) . ? N5 Ni2 2.04(10) 5_676 ? N6 C6 1.428(15) . ? N6 Ni2 2.01(7) 5_676 ? C1 C2 1.446(14) . ? C3 C4 1.561(15) . ? C5 C6 1.532(18) . ? OW4 K1 2.09(3) . ? OW4 K1 2.55(2) 2_655 ? OW5 K1 2.58(3) 2_655 ? OW5 K1 2.59(4) . ? OW7 K1 2.108(14) 2_655 ? OW7 K1 2.658(13) . ? K1 K1 1.200(16) 2_655 ? K1 OW7 2.108(14) 2_655 ? K1 OW4 2.55(2) 2_655 ? K1 OW5 2.58(3) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N4 177.6(3) . . ? N1 Ni1 N3 96.0(3) . . ? N4 Ni1 N3 83.4(3) . . ? N1 Ni1 O9 87.5(3) . . ? N4 Ni1 O9 93.5(3) . . ? N3 Ni1 O9 171.2(2) . . ? N1 Ni1 N2 82.7(3) . . ? N4 Ni1 N2 95.1(3) . . ? N3 Ni1 N2 96.6(3) . . ? O9 Ni1 N2 91.8(2) . . ? N1 Ni1 O22 91.0(2) . . ? N4 Ni1 O22 91.3(3) . . ? N3 Ni1 O22 87.8(2) . . ? O9 Ni1 O22 84.1(2) . . ? N2 Ni1 O22 172.6(2) . . ? Ni2 Ni2 N6 143(10) 5_676 5_676 ? Ni2 Ni2 N5 126(10) 5_676 5_676 ? N6 Ni2 N5 88(3) 5_676 5_676 ? Ni2 Ni2 O12 99(10) 5_676 5_676 ? N6 Ni2 O12 95(3) 5_676 5_676 ? N5 Ni2 O12 90(4) 5_676 5_676 ? Ni2 Ni2 O12 76(10) 5_676 . ? N6 Ni2 O12 90(4) 5_676 . ? N5 Ni2 O12 93(4) 5_676 . ? O12 Ni2 O12 175(3) 5_676 . ? Ni2 Ni2 N5 50(10) 5_676 . ? N6 Ni2 N5 96(4) 5_676 . ? N5 Ni2 N5 176(4) 5_676 . ? O12 Ni2 N5 91(4) 5_676 . ? O12 Ni2 N5 85(3) . . ? Ni2 Ni2 N6 33(10) 5_676 . ? N6 Ni2 N6 177(5) 5_676 . ? N5 Ni2 N6 95(4) 5_676 . ? O12 Ni2 N6 86(3) 5_676 . ? O12 Ni2 N6 89(3) . . ? N5 Ni2 N6 81(2) . . ? O22 V1 O15 108.4(2) 2 . ? O22 V1 O18 107.4(2) 2 . ? O15 V1 O18 93.2(2) . . ? O22 V1 O19 110.0(2) 2 . ? O15 V1 O19 141.0(2) . . ? O18 V1 O19 81.9(2) . . ? O22 V1 O21 108.5(2) 2 . ? O15 V1 O21 81.9(2) . . ? O18 V1 O21 143.4(2) . . ? O19 V1 O21 79.7(2) . . ? O22 V1 V5 112.86(19) 2 . ? O15 V1 V5 41.50(16) . . ? O18 V1 V5 126.39(15) . . ? O19 V1 V5 114.08(15) . . ? O21 V1 V5 40.47(15) . . ? O22 V1 V2 113.52(19) 2 . ? O15 V1 V2 124.95(16) . . ? O18 V1 V2 41.34(15) . . ? O19 V1 V2 40.63(15) . . ? O21 V1 V2 115.01(16) . . ? V5 V1 V2 133.03(6) . . ? O22 V1 V4 116.6(2) 2 . ? O15 V1 V4 114.02(16) . . ? O18 V1 V4 114.56(16) . . ? O19 V1 V4 39.50(15) . . ? O21 V1 V4 40.22(15) . . ? V5 V1 V4 76.64(5) . . ? V2 V1 V4 76.63(5) . . ? O9 V2 O17 107.1(2) . . ? O9 V2 O19 108.4(3) . . ? O17 V2 O19 94.0(2) . . ? O9 V2 O13 108.9(3) . . ? O17 V2 O13 82.4(2) . . ? O19 V2 O13 141.8(2) . . ? O9 V2 O18 108.8(2) . . ? O17 V2 O18 143.4(2) . . ? O19 V2 O18 81.5(2) . . ? O13 V2 O18 79.4(2) . . ? O9 V2 V7 111.8(2) . . ? O17 V2 V7 41.78(16) . . ? O19 V2 V7 126.81(15) . . ? O13 V2 V7 40.74(16) . . ? O18 V2 V7 115.24(15) . . ? O9 V2 V1 113.3(2) . . ? O17 V2 V1 126.26(17) . . ? O19 V2 V1 40.75(15) . . ? O13 V2 V1 114.39(16) . . ? O18 V2 V1 40.80(15) . . ? V7 V2 V1 134.19(5) . . ? O9 V2 V6 115.9(2) . . ? O17 V2 V6 115.20(16) . . ? O19 V2 V6 113.85(16) . . ? O13 V2 V6 39.74(16) . . ? O18 V2 V6 39.72(15) . . ? V7 V2 V6 77.24(5) . . ? V1 V2 V6 76.70(5) . . ? O12 V3 O15 106.4(3) . . ? O12 V3 O8 106.9(3) . . ? O15 V3 O8 90.6(2) . . ? O12 V3 O20 105.3(3) . . ? O15 V3 O20 148.2(2) . . ? O8 V3 O20 82.8(2) . . ? O12 V3 O14 104.1(3) . . ? O15 V3 O14 79.6(2) . . ? O8 V3 O14 148.9(2) . . ? O20 V3 O14 90.2(2) . . ? O12 V3 V9 109.6(2) . . ? O15 V3 V9 126.54(17) . . ? O8 V3 V9 41.80(16) . . ? O20 V3 V9 41.10(15) . . ? O14 V3 V9 125.93(16) . . ? O12 V3 V5 111.0(2) . . ? O15 V3 V5 39.49(15) . . ? O8 V3 V5 123.49(17) . . ? O20 V3 V5 123.35(17) . . ? O14 V3 V5 40.10(15) . . ? V9 V3 V5 139.32(6) . . ? O11 V4 O10 107.1(3) . . ? O11 V4 O7 106.2(3) . . ? O10 V4 O7 82.7(2) . . ? O11 V4 O19 107.1(2) . . ? O10 V4 O19 145.8(2) . . ? O7 V4 O19 90.3(2) . . ? O11 V4 O21 105.6(3) . . ? O10 V4 O21 89.3(2) . . ? O7 V4 O21 148.2(2) . . ? O19 V4 O21 79.2(2) . . ? O11 V4 V10 109.3(2) . . ? O10 V4 V10 41.32(18) . . ? O7 V4 V10 41.57(16) . . ? O19 V4 V10 125.84(16) . . ? O21 V4 V10 125.71(14) . . ? O11 V4 V1 112.6(2) . . ? O10 V4 V1 121.28(18) . . ? O7 V4 V1 122.84(18) . . ? O19 V4 V1 39.41(15) . . ? O21 V4 V1 39.79(14) . . ? V10 V4 V1 138.15(6) . . ? O5 V5 O21 107.2(3) . . ? O5 V5 O16 107.1(3) . . ? O21 V5 O16 95.7(2) . . ? O5 V5 O15 108.7(3) . . ? O21 V5 O15 82.7(2) . . ? O16 V5 O15 143.0(2) . . ? O5 V5 O14 108.1(3) . . ? O21 V5 O14 143.8(2) . . ? O16 V5 O14 81.8(2) . . ? O15 V5 O14 78.4(2) . . ? O5 V5 V1 112.25(19) . . ? O21 V5 V1 41.50(15) . . ? O16 V5 V1 128.26(17) . . ? O15 V5 V1 41.26(15) . . ? O14 V5 V1 114.77(16) . . ? O5 V5 V7 112.25(19) . 2_655 ? O21 V5 V7 128.00(16) . 2_655 ? O16 V5 V7 41.22(16) . 2_655 ? O15 V5 V7 113.78(16) . 2_655 ? O14 V5 V7 40.62(15) . 2_655 ? V1 V5 V7 134.59(6) . 2_655 ? O5 V5 V3 115.0(2) . . ? O21 V5 V3 115.26(16) . . ? O16 V5 V3 114.71(16) . . ? O15 V5 V3 38.98(15) . . ? O14 V5 V3 39.47(15) . . ? V1 V5 V3 77.07(5) . . ? V7 V5 V3 76.65(5) 2_655 . ? O3 V6 O8 106.9(3) . . ? O3 V6 O18 105.6(3) . . ? O8 V6 O18 91.1(2) . . ? O3 V6 O20 105.7(3) . 2_655 ? O8 V6 O20 82.4(2) . 2_655 ? O18 V6 O20 148.6(2) . 2_655 ? O3 V6 O13 105.2(3) . . ? O8 V6 O13 147.9(2) . . ? O18 V6 O13 79.9(2) . . ? O20 V6 O13 89.4(2) 2_655 . ? O3 V6 V9 109.6(2) . . ? O8 V6 V9 41.58(16) . . ? O18 V6 V9 127.18(15) . . ? O20 V6 V9 40.93(15) 2_655 . ? O13 V6 V9 124.95(15) . . ? O3 V6 V2 111.3(2) . . ? O8 V6 V2 123.86(17) . . ? O18 V6 V2 40.07(15) . . ? O20 V6 V2 122.58(16) 2_655 . ? O13 V6 V2 39.84(15) . . ? V9 V6 V2 139.06(6) . . ? O6 V7 O13 106.7(3) . . ? O6 V7 O14 108.0(3) . 2_655 ? O13 V7 O14 93.2(2) . 2_655 ? O6 V7 O17 108.5(3) . . ? O13 V7 O17 83.4(2) . . ? O14 V7 O17 142.7(2) 2_655 . ? O6 V7 O16 109.1(3) . 2_655 ? O13 V7 O16 143.7(2) . 2_655 ? O14 V7 O16 81.9(2) 2_655 2_655 ? O17 V7 O16 79.4(2) . 2_655 ? O6 V7 V2 111.4(2) . . ? O13 V7 V2 42.09(16) . . ? O14 V7 V2 126.84(17) 2_655 . ? O17 V7 V2 41.46(16) . . ? O16 V7 V2 115.76(17) 2_655 . ? O6 V7 V5 113.6(2) . 2_655 ? O13 V7 V5 126.20(16) . 2_655 ? O14 V7 V5 41.61(15) 2_655 2_655 ? O17 V7 V5 114.06(16) . 2_655 ? O16 V7 V5 40.30(15) 2_655 2_655 ? V2 V7 V5 134.36(6) . 2_655 ? O6 V7 V8 116.2(2) . . ? O13 V7 V8 115.61(17) . . ? O14 V7 V8 114.51(16) 2_655 . ? O17 V7 V8 39.44(15) . . ? O16 V7 V8 39.99(16) 2_655 . ? V2 V7 V8 77.48(5) . . ? V5 V7 V8 76.44(5) 2_655 . ? O4 V8 O10 106.8(3) . 2_655 ? O4 V8 O7 107.2(3) . . ? O10 V8 O7 82.7(2) 2_655 . ? O4 V8 O17 107.5(3) . . ? O10 V8 O17 145.6(2) 2_655 . ? O7 V8 O17 89.5(2) . . ? O4 V8 O16 105.2(3) . 2_655 ? O10 V8 O16 89.6(2) 2_655 2_655 ? O7 V8 O16 147.6(2) . 2_655 ? O17 V8 O16 79.3(2) . 2_655 ? O4 V8 V10 109.7(2) . . ? O10 V8 V10 41.31(18) 2_655 . ? O7 V8 V10 41.57(15) . . ? O17 V8 V10 125.08(17) . . ? O16 V8 V10 125.74(15) 2_655 . ? O4 V8 V7 112.9(2) . . ? O10 V8 V7 121.37(18) 2_655 . ? O7 V8 V7 121.75(17) . . ? O17 V8 V7 39.44(16) . . ? O16 V8 V7 39.92(15) 2_655 . ? V10 V8 V7 137.37(7) . . ? O1 V9 O20 110.96(16) . . ? O1 V9 O20 110.96(16) . 2_655 ? O20 V9 O20 138.1(3) . 2_655 ? O1 V9 O8 110.41(16) . . ? O20 V9 O8 82.9(2) . . ? O20 V9 O8 82.8(2) 2_655 . ? O1 V9 O8 110.41(16) . 2_655 ? O20 V9 O8 82.8(2) . 2_655 ? O20 V9 O8 82.9(2) 2_655 2_655 ? O8 V9 O8 139.2(3) . 2_655 ? O1 V9 V3 116.05(4) . . ? O20 V9 V3 41.59(15) . . ? O20 V9 V3 115.70(17) 2_655 . ? O8 V9 V3 41.40(15) . . ? O8 V9 V3 116.34(17) 2_655 . ? O1 V9 V3 116.05(4) . 2_655 ? O20 V9 V3 115.70(17) . 2_655 ? O20 V9 V3 41.59(14) 2_655 2_655 ? O8 V9 V3 116.34(17) . 2_655 ? O8 V9 V3 41.40(15) 2_655 2_655 ? V3 V9 V3 127.89(9) . 2_655 ? O1 V9 V6 115.72(4) . . ? O20 V9 V6 115.87(16) . . ? O20 V9 V6 41.69(15) 2_655 . ? O8 V9 V6 41.18(16) . . ? O8 V9 V6 116.74(17) 2_655 . ? V3 V9 V6 78.55(5) . . ? V3 V9 V6 79.48(5) 2_655 . ? O1 V9 V6 115.72(4) . 2_655 ? O20 V9 V6 41.69(15) . 2_655 ? O20 V9 V6 115.87(16) 2_655 2_655 ? O8 V9 V6 116.74(16) . 2_655 ? O8 V9 V6 41.18(16) 2_655 2_655 ? V3 V9 V6 79.48(5) . 2_655 ? V3 V9 V6 78.55(5) 2_655 2_655 ? V6 V9 V6 128.56(9) . 2_655 ? O2 V10 O10 111.17(17) . 2_655 ? O2 V10 O10 111.17(17) . . ? O10 V10 O10 137.7(3) 2_655 . ? O2 V10 O7 109.56(17) . 2_655 ? O10 V10 O7 83.1(2) 2_655 2_655 ? O10 V10 O7 83.0(2) . 2_655 ? O2 V10 O7 109.56(17) . . ? O10 V10 O7 83.0(2) 2_655 . ? O10 V10 O7 83.1(2) . . ? O7 V10 O7 140.9(3) 2_655 . ? O2 V10 V8 114.49(5) . 2_655 ? O10 V10 V8 116.80(17) 2_655 2_655 ? O10 V10 V8 41.39(15) . 2_655 ? O7 V10 V8 41.81(16) 2_655 2_655 ? O7 V10 V8 117.89(17) . 2_655 ? O2 V10 V8 114.49(5) . . ? O10 V10 V8 41.39(15) 2_655 . ? O10 V10 V8 116.80(17) . . ? O7 V10 V8 117.89(17) 2_655 . ? O7 V10 V8 41.81(16) . . ? V8 V10 V8 131.02(9) 2_655 . ? O2 V10 V4 114.52(5) . 2_655 ? O10 V10 V4 41.55(15) 2_655 2_655 ? O10 V10 V4 116.66(17) . 2_655 ? O7 V10 V4 41.77(16) 2_655 2_655 ? O7 V10 V4 117.91(17) . 2_655 ? V8 V10 V4 80.02(5) 2_655 2_655 ? V8 V10 V4 80.17(5) . 2_655 ? O2 V10 V4 114.52(5) . . ? O10 V10 V4 116.66(17) 2_655 . ? O10 V10 V4 41.55(15) . . ? O7 V10 V4 117.91(17) 2_655 . ? O7 V10 V4 41.77(16) . . ? V8 V10 V4 80.17(5) 2_655 . ? V8 V10 V4 80.02(5) . . ? V4 V10 V4 130.96(9) 2_655 . ? O2 V10 K1 9.77(13) . . ? O10 V10 K1 103.6(2) 2_655 . ? O10 V10 K1 118.5(2) . . ? O7 V10 K1 115.7(3) 2_655 . ? O7 V10 K1 103.1(3) . . ? V8 V10 K1 124.23(15) 2_655 . ? V8 V10 K1 104.75(14) . . ? V4 V10 K1 113.37(19) 2_655 . ? V4 V10 K1 114.9(2) . . ? O2 V10 K1 9.77(13) . 2_655 ? O10 V10 K1 118.5(2) 2_655 2_655 ? O10 V10 K1 103.6(2) . 2_655 ? O7 V10 K1 103.1(3) 2_655 2_655 ? O7 V10 K1 115.7(3) . 2_655 ? V8 V10 K1 104.75(14) 2_655 2_655 ? V8 V10 K1 124.23(15) . 2_655 ? V4 V10 K1 114.9(2) 2_655 2_655 ? V4 V10 K1 113.37(19) . 2_655 ? K1 V10 K1 19.5(3) . 2_655 ? V10 O2 K1 162.3(2) . . ? V10 O2 K1 162.3(2) . 2_655 ? K1 O2 K1 35.4(5) . 2_655 ? V10 O7 V4 96.7(2) . . ? V10 O7 V8 96.6(2) . . ? V4 O7 V8 146.8(3) . . ? V6 O8 V3 144.4(3) . . ? V6 O8 V9 97.2(2) . . ? V3 O8 V9 96.8(2) . . ? V2 O9 Ni1 147.9(3) . . ? V10 O10 V8 97.3(2) . 2_655 ? V10 O10 V4 97.1(2) . . ? V8 O10 V4 149.4(3) 2_655 . ? V3 O12 Ni2 133(3) . 5_676 ? V3 O12 Ni2 135(3) . . ? Ni2 O12 Ni2 5(3) 5_676 . ? V7 O13 V6 145.4(3) . . ? V7 O13 V2 97.2(2) . . ? V6 O13 V2 100.4(2) . . ? V7 O14 V3 144.2(3) 2_655 . ? V7 O14 V5 97.8(2) 2_655 . ? V3 O14 V5 100.4(2) . . ? V3 O15 V1 145.0(3) . . ? V3 O15 V5 101.5(2) . . ? V1 O15 V5 97.2(2) . . ? V5 O16 V7 98.5(2) . 2_655 ? V5 O16 V8 142.6(3) . 2_655 ? V7 O16 V8 100.1(2) 2_655 2_655 ? V2 O17 V8 144.7(3) . . ? V2 O17 V7 96.8(2) . . ? V8 O17 V7 101.1(2) . . ? V1 O18 V6 143.0(3) . . ? V1 O18 V2 97.9(2) . . ? V6 O18 V2 100.2(2) . . ? V2 O19 V1 98.6(2) . . ? V2 O19 V4 143.2(3) . . ? V1 O19 V4 101.1(2) . . ? V9 O20 V3 97.3(2) . . ? V9 O20 V6 97.4(2) . 2_655 ? V3 O20 V6 145.2(3) . 2_655 ? V5 O21 V1 98.0(2) . . ? V5 O21 V4 142.2(3) . . ? V1 O21 V4 100.0(2) . . ? V1 O22 Ni1 139.8(3) 2 . ? C1 N1 Ni1 108.1(6) . . ? C2 N2 Ni1 108.6(5) . . ? C4 N3 Ni1 108.9(5) . . ? C3 N4 Ni1 108.1(6) . . ? C5 N5 Ni2 104(2) . 5_676 ? C5 N5 Ni2 109(2) . . ? Ni2 N5 Ni2 4(4) 5_676 . ? C6 N6 Ni2 105(3) . 5_676 ? C6 N6 Ni2 107(3) . . ? Ni2 N6 Ni2 3(5) 5_676 . ? C2 C1 N1 110.6(9) . . ? C1 C2 N2 110.5(8) . . ? N4 C3 C4 105.9(8) . . ? N3 C4 C3 109.7(7) . . ? N5 C5 C6 109.0(9) . . ? N6 C6 C5 110.0(9) . . ? K1 OW4 K1 27.8(5) . 2_655 ? K1 OW5 K1 26.9(5) 2_655 . ? K1 OW7 K1 26.0(3) 2_655 . ? K1 K1 O2 72.3(2) 2_655 . ? K1 K1 OW4 98.0(11) 2_655 . ? O2 K1 OW4 157.8(9) . . ? K1 K1 OW7 103.6(9) 2_655 2_655 ? O2 K1 OW7 133.9(6) . 2_655 ? OW4 K1 OW7 67.2(7) . 2_655 ? K1 K1 OW4 54.2(9) 2_655 2_655 ? O2 K1 OW4 123.1(8) . 2_655 ? OW4 K1 OW4 58.3(15) . 2_655 ? OW7 K1 OW4 55.7(8) 2_655 2_655 ? K1 K1 OW5 77.2(15) 2_655 2_655 ? O2 K1 OW5 79.9(6) . 2_655 ? OW4 K1 OW5 118.1(9) . 2_655 ? OW7 K1 OW5 55.1(7) 2_655 2_655 ? OW4 K1 OW5 71.4(10) 2_655 2_655 ? K1 K1 OW5 76.0(15) 2_655 . ? O2 K1 OW5 79.6(7) . . ? OW4 K1 OW5 78.7(9) . . ? OW7 K1 OW5 145.6(7) 2_655 . ? OW4 K1 OW5 102.5(9) 2_655 . ? OW5 K1 OW5 150.1(5) 2_655 . ? K1 K1 OW7 50.4(8) 2_655 . ? O2 K1 OW7 107.4(5) . . ? OW4 K1 OW7 53.9(9) . . ? OW7 K1 OW7 102.9(5) 2_655 . ? OW4 K1 OW7 52.9(6) 2_655 . ? OW5 K1 OW7 118.1(11) 2_655 . ? OW5 K1 OW7 49.7(7) . . ? K1 K1 V10 80.23(13) 2_655 . ? O2 K1 V10 7.91(12) . . ? OW4 K1 V10 159.7(8) . . ? OW7 K1 V10 133.1(5) 2_655 . ? OW4 K1 V10 130.5(8) 2_655 . ? OW5 K1 V10 81.4(5) 2_655 . ? OW5 K1 V10 81.2(6) . . ? OW7 K1 V10 113.7(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.792 _refine_diff_density_min -1.774 _refine_diff_density_rms 0.182