Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_shel _database_code_CSD 161607 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Lu, Shaofang' 'Chen, Jin' 'Chen, Zhong-Ning' 'Huang, Zi-Xiang' 'Lu, Can-Zhong' 'Yu, Rongmin' _publ_contact_author_name 'Shaofang Lu' _publ_contact_author_address ; The Chinese Academy of Sciences Fujian Institute of Research on the Structure of Matter Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email 'LSF@MS.FJIRSM.AC.CN' _publ_requested_journal 'Chemical Communications' _publ_section_title ; A Novel Compound with the Interpenetrating 2D Network Structure Constructed by [Mo5P2O23] and Ni-4, 4'-Bipyridine Components: Its Synthesis, Characterization and Magnetic Behaviour ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H98 Mo10 N12 Ni5 O70 P4' _chemical_formula_weight 3484.33 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(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 10.7192(2) _cell_length_b 31.0886(6) _cell_length_c 16.4690(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.3310(10) _cell_angle_gamma 90.00 _cell_volume 5317.43(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 25.02 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3444 _exptl_absorpt_coefficient_mu 2.172 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6522 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Scheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22337 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9299 _reflns_number_gt 6752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0441P)^2^+12.7069P] 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 9299 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.23349(6) 0.060683(18) 0.17222(3) 0.02155(14) Uani 1 1 d . . . Mo2 Mo 0.13859(6) 0.174392(18) 0.14694(4) 0.02726(16) Uani 1 1 d . . . Mo3 Mo 0.07404(7) 0.203631(19) 0.32715(4) 0.03186(17) Uani 1 1 d . . . Mo4 Mo 0.18894(6) 0.12723(2) 0.47242(4) 0.03028(17) Uani 1 1 d . . . Mo5 Mo 0.28789(6) 0.041898(19) 0.37788(4) 0.02631(16) Uani 1 1 d . . . Ni1 Ni 0.0000 0.0000 0.0000 0.0219(3) Uani 1 2 d S . . Ni2 Ni 0.38936(11) 0.22362(3) 0.05325(6) 0.0404(3) Uani 1 1 d . . . Ni3 Ni -0.21585(9) 0.06760(3) 0.35646(6) 0.0313(2) Uani 1 1 d . . . P1 P 0.01388(17) 0.09775(6) 0.26933(11) 0.0232(4) Uani 1 1 d . . . P2 P 0.35344(17) 0.14433(5) 0.32223(10) 0.0225(4) Uani 1 1 d . . . O1 O 0.1546(4) 0.02912(13) 0.0878(3) 0.0244(10) Uani 1 1 d . . . O2 O 0.3892(5) 0.05855(15) 0.1637(3) 0.0334(12) Uani 1 1 d . . . O3 O 0.1865(4) 0.11683(13) 0.1291(3) 0.0242(10) Uani 1 1 d . . . O4 O 0.2403(4) 0.02227(13) 0.2628(3) 0.0277(11) Uani 1 1 d . . . O5 O 0.3168(4) 0.09629(13) 0.2985(3) 0.0251(10) Uani 1 1 d . . . O6 O 0.0376(4) 0.06898(13) 0.1990(3) 0.0253(10) Uani 1 1 d . . . O7 O -0.0150(5) 0.17500(16) 0.0844(3) 0.0404(13) Uani 1 1 d . . . O8 O 0.2223(5) 0.20317(14) 0.0877(3) 0.0326(12) Uani 1 1 d . . . O9 O 0.1268(5) 0.21735(14) 0.2271(3) 0.0311(11) Uani 1 1 d . . . O10 O 0.0499(4) 0.14493(13) 0.2485(3) 0.0259(10) Uani 1 1 d . . . O11 O 0.3316(4) 0.16906(14) 0.2408(3) 0.0276(11) Uani 1 1 d . . . O12 O 0.1535(5) 0.24462(16) 0.3883(3) 0.0455(14) Uani 1 1 d . . . O13 O -0.0809(5) 0.22157(18) 0.2991(4) 0.0522(16) Uani 1 1 d . . . O14 O 0.2630(4) 0.16225(14) 0.3740(3) 0.0279(11) Uani 1 1 d . . . O15 O 0.0507(5) 0.16442(15) 0.4129(3) 0.0329(12) Uani 1 1 d . . . O16 O 0.2756(5) 0.16065(17) 0.5479(3) 0.0434(14) Uani 1 1 d . . . O17 O 0.0990(5) 0.09795(16) 0.5259(3) 0.0405(13) Uani 1 1 d . . . O18 O 0.3168(5) 0.08633(15) 0.4628(3) 0.0311(11) Uani 1 1 d . . . O19 O 0.1046(4) 0.08372(14) 0.3537(3) 0.0267(11) Uani 1 1 d . . . O20 O 0.2011(5) 0.00505(16) 0.4191(3) 0.0398(13) Uani 1 1 d . . . O21 O 0.4406(5) 0.02246(16) 0.4033(3) 0.0402(13) Uani 1 1 d . . . O22 O -0.1245(4) 0.09604(15) 0.2752(3) 0.0302(11) Uani 1 1 d . . . O23 O 0.4919(4) 0.14703(15) 0.3715(3) 0.0309(11) Uani 1 1 d . . . O24 O -0.1178(4) 0.03396(14) 0.0623(3) 0.0296(11) Uani 1 1 d . . . O25 O 0.4992(5) 0.18802(17) 0.1502(3) 0.0435(14) Uani 1 1 d . . . O26 O 0.5627(7) 0.2388(2) 0.0273(4) 0.080(2) Uani 1 1 d . . . O27 O 0.2612(12) 0.2600(2) -0.0376(4) 0.156(5) Uani 1 1 d . . . O28 O -0.3872(5) 0.09407(16) 0.2877(3) 0.0412(13) Uani 1 1 d . . . O29 O -0.0572(5) 0.03718(16) 0.4350(3) 0.0418(13) Uani 1 1 d . . . O30 O -0.1792(5) 0.12506(17) 0.4265(3) 0.0488(15) Uani 1 1 d . . . O31 O -0.3107(5) 0.04525(17) 0.4438(3) 0.0413(13) Uani 1 1 d . . . O32 O 0.7337(7) 0.1531(2) 0.1573(4) 0.075(2) Uiso 1 1 d . . . O33 O -0.0621(8) 0.2425(2) -0.0372(5) 0.092(2) Uiso 1 1 d . . . O34 O 0.1900(11) 0.3067(3) -0.1687(7) 0.140(4) Uiso 1 1 d . . . O35 O 0.7654(11) 0.2659(4) 0.1483(7) 0.147(4) Uiso 1 1 d . . . N1 N -0.0043(5) 0.04962(16) -0.0833(3) 0.0240(13) Uani 1 1 d . . . N2 N 0.3662(6) 0.17244(19) -0.0284(4) 0.0400(16) Uani 1 1 d . . . N3 N 0.4085(7) 0.27545(18) 0.1325(4) 0.0417(17) Uani 1 1 d . . . N4 N -0.2540(6) 0.0121(2) 0.2874(4) 0.0397(16) Uani 1 1 d . . . N5 N 0.5605(7) 0.1522(3) 0.5397(5) 0.059(2) Uani 1 1 d . . . N6 N 0.6845(8) 0.0824(3) 0.9581(5) 0.067(2) Uani 1 1 d . . . H6A H 0.7031 0.0733 1.0090 0.080 Uiso 1 1 calc R . . C11 C -0.0282(7) 0.0431(2) -0.1662(4) 0.0270(16) Uani 1 1 d . . . H11A H -0.0364 0.0150 -0.1860 0.032 Uiso 1 1 calc R . . C12 C -0.0412(7) 0.0757(2) -0.2228(4) 0.0313(17) Uani 1 1 d . . . H12A H -0.0587 0.0694 -0.2797 0.038 Uiso 1 1 calc R . . C13 C -0.0286(7) 0.1180(2) -0.1969(4) 0.0259(16) Uani 1 1 d . . . C14 C -0.0002(7) 0.1247(2) -0.1107(4) 0.0320(17) Uani 1 1 d . . . H14A H 0.0118 0.1525 -0.0894 0.038 Uiso 1 1 calc R . . C15 C 0.0101(7) 0.0905(2) -0.0572(4) 0.0299(16) Uani 1 1 d . . . H15A H 0.0279 0.0959 0.0001 0.036 Uiso 1 1 calc R . . C21 C 0.3641(9) 0.1324(2) 0.0015(5) 0.048(2) Uani 1 1 d . . . H21A H 0.3765 0.1287 0.0590 0.058 Uiso 1 1 calc R . . C22 C 0.3448(9) 0.0970(2) -0.0483(5) 0.049(2) Uani 1 1 d . . . H22A H 0.3452 0.0699 -0.0240 0.059 Uiso 1 1 calc R . . C23 C 0.3244(7) 0.1001(2) -0.1348(5) 0.0370(19) Uani 1 1 d . . . C24 C 0.3231(9) 0.1415(2) -0.1658(5) 0.047(2) Uani 1 1 d . . . H24A H 0.3073 0.1459 -0.2233 0.056 Uiso 1 1 calc R . . C25 C 0.3448(9) 0.1758(2) -0.1130(5) 0.048(2) Uani 1 1 d . . . H25A H 0.3450 0.2031 -0.1361 0.057 Uiso 1 1 calc R . . C31 C 0.4464(10) 0.3143(2) 0.1111(5) 0.053(3) Uani 1 1 d . . . H31A H 0.4581 0.3177 0.0573 0.064 Uiso 1 1 calc R . . C32 C 0.4687(9) 0.3489(3) 0.1639(5) 0.050(2) Uani 1 1 d . . . H32A H 0.4945 0.3750 0.1460 0.060 Uiso 1 1 calc R . . C33 C 0.4525(7) 0.3447(2) 0.2441(4) 0.0310(17) Uani 1 1 d . . . C34 C 0.4144(8) 0.3051(2) 0.2665(4) 0.0372(19) Uani 1 1 d . . . H34A H 0.4019 0.3009 0.3198 0.045 Uiso 1 1 calc R . . C35 C 0.3948(8) 0.2719(2) 0.2106(4) 0.040(2) Uani 1 1 d . . . H35A H 0.3707 0.2453 0.2278 0.048 Uiso 1 1 calc R . . C41 C -0.2472(9) -0.0273(3) 0.3224(5) 0.049(2) Uani 1 1 d . . . H41A H -0.2264 -0.0297 0.3805 0.059 Uiso 1 1 calc R . . C42 C -0.2703(8) -0.0646(3) 0.2744(5) 0.047(2) Uani 1 1 d . . . H42A H -0.2654 -0.0913 0.3002 0.057 Uiso 1 1 calc R . . C43 C -0.3005(7) -0.0615(2) 0.1890(5) 0.0357(18) Uani 1 1 d . . . C44 C -0.3091(9) -0.0206(2) 0.1545(5) 0.048(2) Uani 1 1 d . . . H44A H -0.3322 -0.0172 0.0966 0.057 Uiso 1 1 calc R . . C45 C -0.2840(9) 0.0145(3) 0.2048(5) 0.047(2) Uani 1 1 d . . . H45A H -0.2881 0.0415 0.1799 0.057 Uiso 1 1 calc R . . C51 C 0.5768(9) 0.1114(4) 0.5578(6) 0.071(3) Uani 1 1 d . . . H51A H 0.5714 0.0917 0.5146 0.086 Uiso 1 1 calc R . . C52 C 0.6023(9) 0.0964(3) 0.6407(5) 0.059(3) Uani 1 1 d . . . H52A H 0.6160 0.0673 0.6526 0.071 Uiso 1 1 calc R . . C53 C 0.6068(7) 0.1258(3) 0.7041(5) 0.041(2) Uani 1 1 d . . . C54 C 0.5897(9) 0.1686(3) 0.6822(5) 0.054(2) Uani 1 1 d . . . H54A H 0.5955 0.1895 0.7234 0.064 Uiso 1 1 calc R . . C55 C 0.5639(10) 0.1805(3) 0.5987(6) 0.068(3) Uani 1 1 d . . . H55A H 0.5486 0.2093 0.5843 0.081 Uiso 1 1 calc R . . C61 C 0.6865(9) 0.1242(3) 0.9410(6) 0.057(2) Uani 1 1 d . . . H61A H 0.7072 0.1437 0.9852 0.069 Uiso 1 1 calc R . . C62 C 0.6590(8) 0.1398(3) 0.8596(5) 0.050(2) Uani 1 1 d . . . H62A H 0.6599 0.1692 0.8495 0.060 Uiso 1 1 calc R . . C63 C 0.6305(7) 0.1111(3) 0.7939(5) 0.0394(19) Uani 1 1 d . . . C64 C 0.6261(8) 0.0680(3) 0.8126(5) 0.051(2) Uani 1 1 d . . . H64A H 0.6051 0.0478 0.7699 0.061 Uiso 1 1 calc R . . C65 C 0.6531(9) 0.0553(3) 0.8946(6) 0.058(3) Uani 1 1 d . . . H5A H 0.6491 0.0262 0.9062 0.069 Uiso 1 1 calc R . . 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 0.0254(3) 0.0224(3) 0.0167(3) -0.0026(2) 0.0049(2) -0.0003(3) Mo2 0.0353(4) 0.0241(3) 0.0205(3) -0.0015(2) 0.0034(3) 0.0031(3) Mo3 0.0391(4) 0.0283(3) 0.0310(4) -0.0078(3) 0.0141(3) 0.0015(3) Mo4 0.0343(4) 0.0379(4) 0.0203(3) -0.0064(3) 0.0099(3) -0.0046(3) Mo5 0.0308(4) 0.0290(3) 0.0186(3) 0.0028(2) 0.0050(3) -0.0007(3) Ni1 0.0297(7) 0.0209(6) 0.0151(6) 0.0002(5) 0.0054(5) -0.0013(5) Ni2 0.0759(8) 0.0263(5) 0.0215(5) -0.0020(4) 0.0167(5) -0.0057(5) Ni3 0.0317(6) 0.0347(5) 0.0281(5) -0.0046(4) 0.0084(4) -0.0019(4) P1 0.0231(10) 0.0268(9) 0.0198(9) -0.0038(7) 0.0055(8) -0.0012(8) P2 0.0257(10) 0.0254(9) 0.0168(8) -0.0027(7) 0.0060(8) -0.0026(8) O1 0.030(3) 0.025(2) 0.017(2) -0.0045(19) 0.004(2) -0.001(2) O2 0.031(3) 0.040(3) 0.030(3) -0.006(2) 0.008(2) -0.001(2) O3 0.032(3) 0.023(2) 0.016(2) -0.0024(18) 0.003(2) -0.001(2) O4 0.037(3) 0.021(2) 0.023(3) -0.0041(19) 0.005(2) -0.002(2) O5 0.033(3) 0.024(2) 0.019(2) -0.0011(19) 0.008(2) -0.003(2) O6 0.027(3) 0.025(3) 0.023(2) -0.0039(19) 0.005(2) 0.001(2) O7 0.041(3) 0.040(3) 0.034(3) 0.006(2) -0.003(3) 0.007(3) O8 0.045(3) 0.029(3) 0.023(3) 0.002(2) 0.006(2) 0.004(2) O9 0.042(3) 0.023(2) 0.028(3) -0.003(2) 0.009(2) 0.003(2) O10 0.030(3) 0.025(3) 0.022(2) -0.0029(19) 0.007(2) 0.000(2) O11 0.035(3) 0.026(3) 0.025(3) -0.001(2) 0.011(2) -0.006(2) O12 0.066(4) 0.036(3) 0.040(3) -0.017(2) 0.024(3) -0.012(3) O13 0.040(4) 0.050(4) 0.069(4) 0.003(3) 0.020(3) 0.012(3) O14 0.033(3) 0.028(3) 0.025(3) -0.007(2) 0.010(2) -0.003(2) O15 0.039(3) 0.036(3) 0.026(3) -0.009(2) 0.013(2) -0.005(2) O16 0.044(3) 0.056(3) 0.030(3) -0.017(3) 0.009(3) -0.009(3) O17 0.051(4) 0.051(3) 0.024(3) -0.001(2) 0.018(3) -0.006(3) O18 0.036(3) 0.039(3) 0.016(2) -0.003(2) 0.002(2) -0.004(2) O19 0.031(3) 0.029(3) 0.020(2) -0.002(2) 0.007(2) 0.000(2) O20 0.044(3) 0.043(3) 0.032(3) 0.010(2) 0.009(3) -0.006(3) O21 0.038(3) 0.044(3) 0.035(3) 0.001(2) 0.003(3) 0.004(3) O22 0.026(3) 0.035(3) 0.029(3) 0.000(2) 0.006(2) -0.001(2) O23 0.027(3) 0.040(3) 0.022(3) -0.007(2) -0.001(2) -0.004(2) O24 0.035(3) 0.035(3) 0.019(2) -0.001(2) 0.009(2) 0.003(2) O25 0.055(4) 0.049(3) 0.031(3) 0.012(2) 0.019(3) 0.000(3) O26 0.122(6) 0.082(5) 0.053(4) -0.017(4) 0.056(4) -0.055(4) O27 0.345(15) 0.056(5) 0.038(4) 0.000(4) -0.009(6) 0.088(7) O28 0.034(3) 0.049(3) 0.041(3) -0.005(3) 0.010(3) 0.006(3) O29 0.034(3) 0.044(3) 0.046(3) 0.011(3) 0.007(3) -0.006(3) O30 0.044(4) 0.055(4) 0.050(4) -0.028(3) 0.017(3) -0.010(3) O31 0.037(3) 0.054(3) 0.036(3) 0.006(3) 0.013(3) 0.000(3) N1 0.029(3) 0.024(3) 0.019(3) -0.002(2) 0.006(3) -0.001(2) N2 0.059(5) 0.031(4) 0.035(4) -0.004(3) 0.020(3) -0.005(3) N3 0.072(5) 0.027(3) 0.029(4) -0.003(3) 0.017(3) -0.011(3) N4 0.046(4) 0.035(4) 0.036(4) -0.002(3) 0.007(3) -0.003(3) N5 0.041(5) 0.091(7) 0.041(5) -0.002(5) 0.004(4) 0.002(5) N6 0.065(6) 0.096(7) 0.033(4) 0.010(5) 0.000(4) 0.030(5) C11 0.035(4) 0.024(4) 0.022(4) 0.000(3) 0.008(3) 0.000(3) C12 0.044(5) 0.032(4) 0.020(4) -0.003(3) 0.014(3) 0.001(3) C13 0.028(4) 0.028(4) 0.024(4) 0.004(3) 0.010(3) 0.001(3) C14 0.047(5) 0.016(3) 0.031(4) -0.002(3) 0.006(4) -0.004(3) C15 0.041(5) 0.029(4) 0.017(3) 0.001(3) 0.004(3) 0.000(3) C21 0.077(7) 0.031(4) 0.043(5) -0.002(4) 0.025(5) -0.001(4) C22 0.088(7) 0.025(4) 0.040(5) -0.002(4) 0.030(5) -0.005(4) C23 0.040(5) 0.031(4) 0.045(5) -0.009(4) 0.021(4) -0.009(4) C24 0.076(7) 0.039(5) 0.031(4) -0.005(4) 0.023(4) -0.003(4) C25 0.085(7) 0.027(4) 0.035(5) -0.001(3) 0.023(5) -0.004(4) C31 0.106(8) 0.036(5) 0.029(4) -0.003(4) 0.038(5) -0.010(5) C32 0.088(7) 0.035(5) 0.033(4) -0.010(4) 0.028(5) -0.026(4) C33 0.044(5) 0.029(4) 0.020(4) -0.004(3) 0.007(3) -0.004(3) C34 0.056(6) 0.037(4) 0.023(4) -0.004(3) 0.020(4) -0.013(4) C35 0.075(6) 0.025(4) 0.024(4) -0.005(3) 0.021(4) -0.018(4) C41 0.071(7) 0.044(5) 0.029(4) 0.001(4) 0.008(4) 0.000(4) C42 0.061(6) 0.030(4) 0.046(5) 0.001(4) 0.006(4) 0.003(4) C43 0.039(5) 0.034(4) 0.037(4) -0.004(3) 0.016(4) 0.002(4) C44 0.075(7) 0.034(5) 0.034(5) -0.006(4) 0.013(4) -0.008(4) C45 0.072(7) 0.034(5) 0.036(5) 0.000(4) 0.012(5) -0.003(4) C51 0.052(7) 0.122(10) 0.038(6) -0.036(6) 0.010(5) 0.007(7) C52 0.077(7) 0.065(6) 0.031(5) -0.015(4) 0.008(5) 0.003(5) C53 0.032(5) 0.056(5) 0.035(5) -0.002(4) 0.006(4) 0.002(4) C54 0.063(6) 0.064(6) 0.030(5) -0.006(4) 0.004(4) 0.001(5) C55 0.077(8) 0.069(7) 0.052(6) 0.009(5) 0.007(6) -0.003(6) C61 0.062(7) 0.070(7) 0.035(5) -0.003(5) 0.002(5) 0.009(5) C62 0.051(6) 0.058(6) 0.036(5) -0.006(4) 0.002(4) 0.000(4) C63 0.029(5) 0.049(5) 0.038(5) -0.005(4) 0.004(4) 0.013(4) C64 0.050(6) 0.059(6) 0.040(5) -0.002(4) 0.005(4) 0.012(4) C65 0.049(6) 0.068(6) 0.056(6) 0.009(5) 0.013(5) 0.026(5) _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 O2 1.711(5) . ? Mo1 O1 1.741(4) . ? Mo1 O4 1.898(4) . ? Mo1 O3 1.905(4) . ? Mo1 O6 2.265(4) . ? Mo1 O5 2.330(4) . ? Mo2 O7 1.712(5) . ? Mo2 O8 1.729(5) . ? Mo2 O9 1.904(4) . ? Mo2 O3 1.905(4) . ? Mo2 O11 2.261(5) . ? Mo2 O10 2.308(4) . ? Mo3 O13 1.703(5) . ? Mo3 O12 1.714(5) . ? Mo3 O9 1.918(5) . ? Mo3 O15 1.928(5) . ? Mo3 O10 2.216(4) . ? Mo3 O14 2.362(5) . ? Mo4 O16 1.707(5) . ? Mo4 O17 1.719(5) . ? Mo4 O18 1.905(5) . ? Mo4 O15 1.943(5) . ? Mo4 O14 2.254(4) . ? Mo4 O19 2.365(4) . ? Mo5 O21 1.697(5) . ? Mo5 O20 1.717(5) . ? Mo5 O18 1.935(4) . ? Mo5 O4 1.936(4) . ? Mo5 O5 2.206(4) . ? Mo5 O19 2.307(4) . ? Ni1 N1 2.058(5) 3 ? Ni1 N1 2.058(5) . ? Ni1 O24 2.098(4) 3 ? Ni1 O24 2.098(4) . ? Ni1 O1 2.114(4) 3 ? Ni1 O1 2.114(4) . ? Ni2 N3 2.052(6) . ? Ni2 O25 2.057(5) . ? Ni2 N2 2.059(6) . ? Ni2 O26 2.061(6) . ? Ni2 O27 2.095(8) . ? Ni2 O8 2.107(5) . ? Ni3 O22 2.045(4) . ? Ni3 N4 2.051(6) . ? Ni3 O28 2.074(5) . ? Ni3 O31 2.075(5) . ? Ni3 O29 2.090(5) . ? Ni3 O30 2.110(5) . ? P1 O22 1.511(5) . ? P1 O6 1.533(4) . ? P1 O19 1.549(5) . ? P1 O10 1.576(5) . ? P2 O23 1.508(5) . ? P2 O11 1.514(5) . ? P2 O14 1.545(4) . ? P2 O5 1.569(4) . ? N1 C15 1.338(8) . ? N1 C11 1.340(8) . ? N2 C21 1.341(9) . ? N2 C25 1.359(9) . ? N3 C35 1.334(9) . ? N3 C31 1.348(9) . ? N4 C45 1.321(9) . ? N4 C41 1.348(10) . ? N5 C51 1.303(13) . ? N5 C55 1.305(12) . ? N6 C65 1.320(12) . ? N6 C61 1.331(11) . ? C11 C12 1.362(9) . ? C12 C13 1.378(9) . ? C13 C14 1.392(9) . ? C13 C33 1.493(9) 4_565 ? C14 C15 1.369(9) . ? C21 C22 1.359(10) . ? C22 C23 1.389(11) . ? C23 C24 1.383(10) . ? C23 C43 1.479(10) 3 ? C24 C25 1.358(10) . ? C31 C32 1.367(10) . ? C32 C33 1.380(10) . ? C33 C34 1.377(9) . ? C33 C13 1.493(9) 4_666 ? C34 C35 1.364(9) . ? C41 C42 1.390(11) . ? C42 C43 1.367(11) . ? C43 C44 1.387(10) . ? C43 C23 1.479(10) 3 ? C44 C45 1.356(10) . ? C51 C52 1.404(13) . ? C52 C53 1.380(11) . ? C53 C54 1.380(11) . ? C53 C63 1.508(11) . ? C54 C55 1.383(12) . ? C61 C62 1.387(12) . ? C62 C63 1.377(11) . ? C63 C64 1.379(11) . ? C64 C65 1.367(12) . ? 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 O2 Mo1 O1 101.8(2) . . ? O2 Mo1 O4 101.0(2) . . ? O1 Mo1 O4 100.92(19) . . ? O2 Mo1 O3 100.3(2) . . ? O1 Mo1 O3 100.79(19) . . ? O4 Mo1 O3 145.60(18) . . ? O2 Mo1 O6 172.29(19) . . ? O1 Mo1 O6 85.94(18) . . ? O4 Mo1 O6 77.03(18) . . ? O3 Mo1 O6 78.26(17) . . ? O2 Mo1 O5 85.73(19) . . ? O1 Mo1 O5 169.73(17) . . ? O4 Mo1 O5 70.48(16) . . ? O3 Mo1 O5 84.56(16) . . ? O6 Mo1 O5 86.59(15) . . ? O7 Mo2 O8 102.2(2) . . ? O7 Mo2 O9 101.0(2) . . ? O8 Mo2 O9 99.3(2) . . ? O7 Mo2 O3 100.0(2) . . ? O8 Mo2 O3 101.61(19) . . ? O9 Mo2 O3 146.41(19) . . ? O7 Mo2 O11 173.1(2) . . ? O8 Mo2 O11 84.75(19) . . ? O9 Mo2 O11 77.54(18) . . ? O3 Mo2 O11 78.49(17) . . ? O7 Mo2 O10 86.2(2) . . ? O8 Mo2 O10 168.07(19) . . ? O9 Mo2 O10 70.49(17) . . ? O3 Mo2 O10 85.10(16) . . ? O11 Mo2 O10 86.98(16) . . ? O13 Mo3 O12 103.0(3) . . ? O13 Mo3 O9 99.7(2) . . ? O12 Mo3 O9 97.5(2) . . ? O13 Mo3 O15 96.4(2) . . ? O12 Mo3 O15 100.1(2) . . ? O9 Mo3 O15 152.76(19) . . ? O13 Mo3 O10 98.4(2) . . ? O12 Mo3 O10 157.6(2) . . ? O9 Mo3 O10 72.38(17) . . ? O15 Mo3 O10 83.69(17) . . ? O13 Mo3 O14 165.1(2) . . ? O12 Mo3 O14 87.2(2) . . ? O9 Mo3 O14 89.45(17) . . ? O15 Mo3 O14 70.88(18) . . ? O10 Mo3 O14 73.09(16) . . ? O16 Mo4 O17 102.9(2) . . ? O16 Mo4 O18 101.2(2) . . ? O17 Mo4 O18 101.3(2) . . ? O16 Mo4 O15 102.4(2) . . ? O17 Mo4 O15 96.9(2) . . ? O18 Mo4 O15 146.09(18) . . ? O16 Mo4 O14 90.3(2) . . ? O17 Mo4 O14 165.1(2) . . ? O18 Mo4 O14 82.76(18) . . ? O15 Mo4 O14 73.13(18) . . ? O16 Mo4 O19 167.8(2) . . ? O17 Mo4 O19 88.43(19) . . ? O18 Mo4 O19 71.64(17) . . ? O15 Mo4 O19 80.54(17) . . ? O14 Mo4 O19 79.19(15) . . ? O21 Mo5 O20 104.4(2) . . ? O21 Mo5 O18 96.0(2) . . ? O20 Mo5 O18 101.3(2) . . ? O21 Mo5 O4 97.7(2) . . ? O20 Mo5 O4 98.0(2) . . ? O18 Mo5 O4 152.73(19) . . ? O21 Mo5 O5 98.7(2) . . ? O20 Mo5 O5 156.2(2) . . ? O18 Mo5 O5 81.97(17) . . ? O4 Mo5 O5 72.71(17) . . ? O21 Mo5 O19 166.3(2) . . ? O20 Mo5 O19 85.6(2) . . ? O18 Mo5 O19 72.51(18) . . ? O4 Mo5 O19 90.12(17) . . ? O5 Mo5 O19 72.79(16) . . ? N1 Ni1 N1 180.0(3) 3 . ? N1 Ni1 O24 91.84(19) 3 3 ? N1 Ni1 O24 88.16(19) . 3 ? N1 Ni1 O24 88.16(19) 3 . ? N1 Ni1 O24 91.84(19) . . ? O24 Ni1 O24 180.0(3) 3 . ? N1 Ni1 O1 91.11(19) 3 3 ? N1 Ni1 O1 88.89(19) . 3 ? O24 Ni1 O1 85.10(17) 3 3 ? O24 Ni1 O1 94.90(17) . 3 ? N1 Ni1 O1 88.89(19) 3 . ? N1 Ni1 O1 91.11(19) . . ? O24 Ni1 O1 94.90(17) 3 . ? O24 Ni1 O1 85.10(17) . . ? O1 Ni1 O1 180.0(4) 3 . ? N3 Ni2 O25 88.9(2) . . ? N3 Ni2 N2 178.5(3) . . ? O25 Ni2 N2 92.6(2) . . ? N3 Ni2 O26 90.0(3) . . ? O25 Ni2 O26 85.0(3) . . ? N2 Ni2 O26 90.6(2) . . ? N3 Ni2 O27 88.5(3) . . ? O25 Ni2 O27 173.3(4) . . ? N2 Ni2 O27 90.0(3) . . ? O26 Ni2 O27 101.2(4) . . ? N3 Ni2 O8 91.3(2) . . ? O25 Ni2 O8 89.39(19) . . ? N2 Ni2 O8 88.3(2) . . ? O26 Ni2 O8 174.2(3) . . ? O27 Ni2 O8 84.5(4) . . ? O22 Ni3 N4 93.6(2) . . ? O22 Ni3 O28 88.52(19) . . ? N4 Ni3 O28 90.2(2) . . ? O22 Ni3 O31 173.9(2) . . ? N4 Ni3 O31 92.1(2) . . ? O28 Ni3 O31 89.5(2) . . ? O22 Ni3 O29 98.79(19) . . ? N4 Ni3 O29 89.0(2) . . ? O28 Ni3 O29 172.7(2) . . ? O31 Ni3 O29 83.3(2) . . ? O22 Ni3 O30 86.4(2) . . ? N4 Ni3 O30 179.2(3) . . ? O28 Ni3 O30 89.0(2) . . ? O31 Ni3 O30 87.8(2) . . ? O29 Ni3 O30 91.8(2) . . ? O22 P1 O6 112.1(3) . . ? O22 P1 O19 110.0(3) . . ? O6 P1 O19 109.2(2) . . ? O22 P1 O10 110.1(3) . . ? O6 P1 O10 106.4(2) . . ? O19 P1 O10 108.9(3) . . ? O23 P2 O11 111.4(3) . . ? O23 P2 O14 110.6(3) . . ? O11 P2 O14 109.0(3) . . ? O23 P2 O5 109.9(3) . . ? O11 P2 O5 106.8(2) . . ? O14 P2 O5 109.1(2) . . ? Mo1 O1 Ni1 158.7(2) . . ? Mo2 O3 Mo1 149.3(2) . . ? Mo1 O4 Mo5 121.4(2) . . ? P2 O5 Mo5 130.2(2) . . ? P2 O5 Mo1 133.8(2) . . ? Mo5 O5 Mo1 94.93(16) . . ? P1 O6 Mo1 123.3(3) . . ? Mo2 O8 Ni2 154.5(3) . . ? Mo2 O9 Mo3 121.6(2) . . ? P1 O10 Mo3 129.7(2) . . ? P1 O10 Mo2 134.0(2) . . ? Mo3 O10 Mo2 95.02(16) . . ? P2 O11 Mo2 123.9(3) . . ? P2 O14 Mo4 127.1(3) . . ? P2 O14 Mo3 128.4(3) . . ? Mo4 O14 Mo3 94.12(16) . . ? Mo3 O15 Mo4 121.7(2) . . ? Mo4 O18 Mo5 123.2(2) . . ? P1 O19 Mo5 129.2(2) . . ? P1 O19 Mo4 127.4(2) . . ? Mo5 O19 Mo4 92.58(16) . . ? P1 O22 Ni3 133.9(3) . . ? C15 N1 C11 116.7(5) . . ? C15 N1 Ni1 121.0(4) . . ? C11 N1 Ni1 122.2(4) . . ? C21 N2 C25 115.7(6) . . ? C21 N2 Ni2 119.2(5) . . ? C25 N2 Ni2 125.0(5) . . ? C35 N3 C31 116.0(6) . . ? C35 N3 Ni2 122.0(5) . . ? C31 N3 Ni2 121.7(5) . . ? C45 N4 C41 117.7(7) . . ? C45 N4 Ni3 119.2(5) . . ? C41 N4 Ni3 123.1(5) . . ? C51 N5 C55 120.6(9) . . ? C65 N6 C61 118.0(8) . . ? N1 C11 C12 123.1(6) . . ? C11 C12 C13 120.9(6) . . ? C12 C13 C14 116.0(6) . . ? C12 C13 C33 123.5(6) . 4_565 ? C14 C13 C33 120.5(6) . 4_565 ? C15 C14 C13 120.2(6) . . ? N1 C15 C14 123.1(6) . . ? N2 C21 C22 123.0(8) . . ? C21 C22 C23 121.6(7) . . ? C24 C23 C22 115.4(7) . . ? C24 C23 C43 123.2(7) . 3 ? C22 C23 C43 121.4(7) . 3 ? C25 C24 C23 120.6(7) . . ? C24 C25 N2 123.7(7) . . ? N3 C31 C32 123.7(7) . . ? C31 C32 C33 119.5(7) . . ? C34 C33 C32 117.1(6) . . ? C34 C33 C13 121.5(6) . 4_666 ? C32 C33 C13 121.4(6) . 4_666 ? C35 C34 C33 120.2(6) . . ? N3 C35 C34 123.6(6) . . ? N4 C41 C42 122.1(7) . . ? C43 C42 C41 119.5(7) . . ? C42 C43 C44 117.3(7) . . ? C42 C43 C23 121.8(7) . 3 ? C44 C43 C23 120.9(7) . 3 ? C45 C44 C43 120.4(8) . . ? N4 C45 C44 123.0(8) . . ? N5 C51 C52 121.9(9) . . ? C53 C52 C51 118.5(9) . . ? C54 C53 C52 117.6(8) . . ? C54 C53 C63 121.9(7) . . ? C52 C53 C63 120.5(8) . . ? C53 C54 C55 119.9(9) . . ? N5 C55 C54 121.5(10) . . ? N6 C61 C62 122.4(9) . . ? C63 C62 C61 119.1(9) . . ? C62 C63 C64 117.8(8) . . ? C62 C63 C53 121.7(8) . . ? C64 C63 C53 120.5(7) . . ? C65 C64 C63 119.4(9) . . ? N6 C65 C64 123.3(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.797 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.137