# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Wang, Xiuli' _publ_contact_author_email wangxiuli@bhu.edu.cn _publ_section_title ; A 3D organopolymolybdate polymer with unusual topology functionalized by 1,4-bis(1,2,4-triazol-1-yl)butane through Mo-N bond ; loop_ _publ_author_name 'Xiuli Wang' 'Jin Li' 'Aixiang Tian' 'Guocheng Liu' 'Qiang Gao' ; Hongyan Lin ; 'Dan Zhao' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 793725' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 Mo4 N12 Ni O15' _chemical_formula_weight 1070.97 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' 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.599(5) _cell_length_b 12.238(5) _cell_length_c 13.468(5) _cell_angle_alpha 73.105(5) _cell_angle_beta 70.024(5) _cell_angle_gamma 88.139(5) _cell_volume 1566.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 25.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 2.233 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6636 _exptl_absorpt_correction_T_max 0.7305 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7907 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5423 _reflns_number_gt 4483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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^)+(0.0701P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5423 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Ni1 Ni 0.0000 0.5000 -0.5000 0.0190(3) Uani 1 2 d S . . Ni2 Ni 0.0000 0.0000 0.0000 0.0169(3) Uani 1 2 d S . . Mo1 Mo 0.16787(5) -0.21103(5) 0.40859(4) 0.01607(15) Uani 1 1 d . . . Mo2 Mo -0.08389(5) 0.18149(5) 0.34648(4) 0.01560(15) Uani 1 1 d . . . Mo3 Mo 0.17939(5) -0.00222(5) 0.19797(4) 0.01584(15) Uani 1 1 d . . . Mo4 Mo 0.16056(5) 0.06676(4) 0.42812(4) 0.01397(15) Uani 1 1 d . . . O1 O 0.2482(4) -0.0284(4) 0.3410(3) 0.0149(9) Uani 1 1 d . . . O2 O 0.1845(4) 0.0019(4) 0.5544(3) 0.0191(10) Uani 1 1 d . . . O3 O -0.0164(4) 0.1148(3) 0.4889(3) 0.0153(9) Uani 1 1 d . . . O4 O 0.0712(4) 0.0974(4) 0.2985(3) 0.0156(9) Uani 1 1 d . . . O5 O 0.0835(4) -0.1368(4) 0.2979(3) 0.0183(10) Uani 1 1 d . . . O6 O -0.2228(4) 0.2129(3) 0.4699(3) 0.0187(10) Uani 1 1 d . . . O7 O 0.3090(5) -0.2527(4) 0.3286(4) 0.0269(11) Uani 1 1 d . . . O8 O 0.3225(5) -0.0540(4) 0.1255(4) 0.0236(10) Uani 1 1 d . . . O9 O 0.0892(4) 0.0306(4) 0.1091(3) 0.0216(10) Uani 1 1 d . . . O10 O -0.1710(5) 0.1789(4) 0.2618(4) 0.0266(11) Uani 1 1 d . . . O11 O -0.0008(5) 0.3164(4) 0.2913(4) 0.0243(11) Uani 1 1 d . . . O12 O 0.2629(5) 0.1907(4) 0.3709(4) 0.0257(11) Uani 1 1 d . . . O13 O 0.0585(5) -0.3328(4) 0.4666(4) 0.0235(10) Uani 1 1 d . . . O1W O -0.1149(5) 0.5063(4) -0.3383(4) 0.0274(11) Uani 1 1 d . . . H1WA H -0.1222 0.4548 -0.2781 0.033 Uiso 1 1 d R . . H1WB H -0.1340 0.5623 -0.3117 0.033 Uiso 1 1 d R . . O2W O 0.5719(11) 0.2736(9) 0.2147(11) 0.156(5) Uani 1 1 d . . . N1 N 0.3071(5) 0.1643(5) 0.1157(4) 0.0219(12) Uani 1 1 d . . . N2 N 0.3712(6) 0.3516(5) 0.0470(5) 0.0357(16) Uani 1 1 d . . . N3 N 0.4563(5) 0.2917(5) -0.0132(4) 0.0235(13) Uani 1 1 d . . . N4 N 0.3180(6) 0.4492(5) -0.3794(5) 0.0312(14) Uani 1 1 d . . . N5 N 0.3308(7) 0.3547(6) -0.4117(6) 0.0439(18) Uani 1 1 d . . . N6 N 0.1590(5) 0.4504(4) -0.4464(4) 0.0215(12) Uani 1 1 d . . . N7 N 0.1862(6) 0.0274(5) -0.1287(4) 0.0230(13) Uani 1 1 d . . . N8 N 0.4063(7) 0.0344(8) -0.2059(6) 0.065(3) Uani 1 1 d . . . N9 N 0.3486(6) 0.0658(5) -0.2848(5) 0.0310(14) Uani 1 1 d . . . N10 N 0.0334(6) -0.1738(5) 0.0535(4) 0.0220(12) Uani 1 1 d . . . N11 N 0.0480(7) -0.3511(5) 0.1566(5) 0.0361(16) Uani 1 1 d . . . N12 N 0.1075(6) -0.3393(5) 0.0465(5) 0.0296(14) Uani 1 1 d . . . C1 C 0.4205(7) 0.1822(6) 0.0258(6) 0.0255(16) Uani 1 1 d . . . H1A H 0.4655 0.1259 -0.0034 0.031 Uiso 1 1 calc R . . C2 C 0.2817(7) 0.2714(6) 0.1232(6) 0.0293(17) Uani 1 1 d . . . H2A H 0.2075 0.2868 0.1774 0.035 Uiso 1 1 calc R . . C3 C 0.5700(7) 0.3483(7) -0.1121(5) 0.0283(17) Uani 1 1 d . . . H3A H 0.6158 0.2915 -0.1461 0.034 Uiso 1 1 calc R . . H3B H 0.6332 0.3839 -0.0910 0.034 Uiso 1 1 calc R . . C4 C 0.5269(7) 0.4384(6) -0.1955(6) 0.0328(18) Uani 1 1 d . . . H4A H 0.6061 0.4728 -0.2594 0.039 Uiso 1 1 calc R . . H4B H 0.4879 0.4982 -0.1630 0.039 Uiso 1 1 calc R . . C5 C 0.4258(7) 0.3938(6) -0.2344(6) 0.0308(17) Uani 1 1 d . . . H5A H 0.3384 0.3772 -0.1759 0.037 Uiso 1 1 calc R . . H5B H 0.4543 0.3236 -0.2522 0.037 Uiso 1 1 calc R . . C6 C 0.4157(9) 0.4835(8) -0.3363(7) 0.047(2) Uani 1 1 d . . . H6A H 0.3902 0.5540 -0.3180 0.057 Uiso 1 1 calc R . . H6B H 0.5037 0.4991 -0.3941 0.057 Uiso 1 1 calc R . . C7 C 0.2174(7) 0.5042(6) -0.4008(6) 0.0273(16) Uani 1 1 d . . . H7A H 0.1910 0.5725 -0.3856 0.033 Uiso 1 1 calc R . . C8 C 0.2319(8) 0.3599(7) -0.4516(7) 0.039(2) Uani 1 1 d . . . H8A H 0.2145 0.3046 -0.4810 0.046 Uiso 1 1 calc R . . C9 C 0.2162(7) 0.0587(6) -0.2360(6) 0.0249(15) Uani 1 1 d . . . H9A H 0.1542 0.0737 -0.2723 0.030 Uiso 1 1 calc R . . C10 C 0.3063(8) 0.0148(9) -0.1177(6) 0.049(2) Uani 1 1 d . . . H10A H 0.3158 -0.0073 -0.0487 0.059 Uiso 1 1 calc R . . C11 C 0.4282(7) 0.0929(7) -0.4027(5) 0.0309(17) Uani 1 1 d . . . H11A H 0.5079 0.1413 -0.4193 0.037 Uiso 1 1 calc R . . H11B H 0.3757 0.1349 -0.4459 0.037 Uiso 1 1 calc R . . C12 C 0.4696(7) -0.0144(6) -0.4348(6) 0.0309(17) Uani 1 1 d . . . H12A H 0.3920 -0.0691 -0.4057 0.037 Uiso 1 1 calc R . . H12B H 0.5362 -0.0487 -0.4030 0.037 Uiso 1 1 calc R . . C13 C 0.0981(8) -0.2333(6) -0.0157(6) 0.0330(18) Uani 1 1 d . . . H13A H 0.1306 -0.2064 -0.0926 0.040 Uiso 1 1 calc R . . C14 C 0.0062(8) -0.2497(6) 0.1565(6) 0.0312(17) Uani 1 1 d . . . H14A H -0.0384 -0.2306 0.2212 0.037 Uiso 1 1 calc R . . C15 C 0.1649(9) -0.4360(7) 0.0022(8) 0.046(2) Uani 1 1 d . . . H15A H 0.2516 -0.4098 -0.0559 0.055 Uiso 1 1 calc R A 1 H15B H 0.1792 -0.4974 0.0609 0.055 Uiso 1 1 calc R A 1 C16 C 0.0740(14) -0.4808(12) -0.0427(13) 0.037(3) Uani 0.599(14) 1 d P . 1 H16A H 0.1127 -0.5458 -0.0666 0.044 Uiso 0.599(14) 1 calc PR . 1 H16B H 0.0695 -0.4219 -0.1073 0.044 Uiso 0.599(14) 1 calc PR . 1 C16' C 0.047(2) -0.5257(18) 0.031(2) 0.037(3) Uani 0.401(14) 1 d P . 2 H16C H 0.0825 -0.5934 0.0113 0.044 Uiso 0.401(14) 1 calc PR . 2 H16D H -0.0026 -0.5482 0.1103 0.044 Uiso 0.401(14) 1 calc PR . 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 Ni1 0.0233(6) 0.0136(6) 0.0214(6) -0.0052(5) -0.0096(5) 0.0021(5) Ni2 0.0202(6) 0.0169(6) 0.0141(6) -0.0060(5) -0.0056(5) 0.0046(5) Mo1 0.0204(3) 0.0137(3) 0.0146(3) -0.0057(2) -0.0056(2) 0.0029(2) Mo2 0.0179(3) 0.0166(3) 0.0133(3) -0.0054(2) -0.0060(2) 0.0044(2) Mo3 0.0192(3) 0.0174(3) 0.0113(3) -0.0058(2) -0.0045(2) 0.0018(2) Mo4 0.0140(3) 0.0156(3) 0.0136(3) -0.0065(2) -0.0046(2) 0.0010(2) O1 0.012(2) 0.018(2) 0.012(2) -0.0043(18) -0.0014(17) 0.0005(17) O2 0.019(2) 0.026(3) 0.016(2) -0.0088(19) -0.0079(19) 0.0005(19) O3 0.014(2) 0.017(2) 0.018(2) -0.0072(18) -0.0083(18) 0.0039(18) O4 0.018(2) 0.020(2) 0.008(2) -0.0061(18) -0.0006(17) 0.0027(18) O5 0.022(2) 0.020(2) 0.012(2) -0.0027(18) -0.0061(19) -0.0037(19) O6 0.021(2) 0.014(2) 0.022(2) -0.0057(19) -0.009(2) 0.0079(18) O7 0.028(3) 0.032(3) 0.019(2) -0.012(2) -0.003(2) 0.012(2) O8 0.027(3) 0.026(3) 0.016(2) -0.008(2) -0.004(2) 0.007(2) O9 0.025(3) 0.023(2) 0.017(2) -0.0063(19) -0.009(2) 0.003(2) O10 0.031(3) 0.037(3) 0.015(2) -0.010(2) -0.011(2) 0.008(2) O11 0.026(3) 0.023(3) 0.020(2) -0.007(2) -0.002(2) 0.001(2) O12 0.025(3) 0.023(3) 0.028(3) -0.009(2) -0.007(2) -0.002(2) O13 0.033(3) 0.016(2) 0.021(2) -0.0035(19) -0.010(2) -0.001(2) O1W 0.034(3) 0.025(3) 0.016(2) -0.004(2) -0.002(2) -0.001(2) O2W 0.101(8) 0.094(8) 0.212(13) 0.048(8) -0.056(8) 0.010(6) N1 0.023(3) 0.023(3) 0.014(3) -0.006(2) 0.002(2) 0.000(2) N2 0.031(4) 0.025(4) 0.044(4) -0.010(3) -0.005(3) 0.000(3) N3 0.020(3) 0.030(3) 0.011(3) -0.002(2) 0.002(2) -0.003(3) N4 0.037(4) 0.030(3) 0.026(3) -0.006(3) -0.013(3) 0.000(3) N5 0.045(4) 0.049(4) 0.055(5) -0.030(4) -0.028(4) 0.026(4) N6 0.025(3) 0.016(3) 0.023(3) -0.003(2) -0.011(3) 0.000(2) N7 0.024(3) 0.026(3) 0.021(3) -0.010(3) -0.008(3) 0.006(3) N8 0.030(4) 0.129(8) 0.049(5) -0.042(5) -0.018(4) 0.020(5) N9 0.028(3) 0.046(4) 0.023(3) -0.016(3) -0.010(3) 0.004(3) N10 0.033(3) 0.022(3) 0.011(3) -0.006(2) -0.007(2) 0.003(3) N11 0.063(5) 0.021(3) 0.033(4) -0.009(3) -0.025(3) 0.003(3) N12 0.041(4) 0.025(3) 0.032(3) -0.015(3) -0.019(3) 0.010(3) C1 0.017(3) 0.031(4) 0.029(4) -0.013(3) -0.005(3) 0.007(3) C2 0.031(4) 0.028(4) 0.021(4) -0.007(3) 0.000(3) 0.004(3) C3 0.018(4) 0.044(5) 0.014(3) -0.002(3) 0.002(3) -0.009(3) C4 0.029(4) 0.031(4) 0.038(4) -0.003(3) -0.017(4) -0.008(3) C5 0.028(4) 0.029(4) 0.035(4) -0.005(3) -0.014(3) -0.002(3) C6 0.043(5) 0.052(6) 0.050(5) -0.003(4) -0.028(4) -0.011(4) C7 0.039(4) 0.019(4) 0.024(4) -0.003(3) -0.014(3) 0.008(3) C8 0.045(5) 0.031(4) 0.059(6) -0.027(4) -0.032(4) 0.018(4) C9 0.020(4) 0.030(4) 0.024(4) -0.010(3) -0.006(3) -0.001(3) C10 0.030(5) 0.098(8) 0.017(4) -0.014(4) -0.007(4) 0.010(5) C11 0.027(4) 0.044(5) 0.013(3) -0.009(3) 0.004(3) -0.003(3) C12 0.019(4) 0.036(4) 0.042(5) -0.015(4) -0.013(3) 0.008(3) C13 0.045(5) 0.024(4) 0.028(4) -0.005(3) -0.015(4) 0.008(4) C14 0.046(5) 0.024(4) 0.025(4) -0.008(3) -0.014(4) 0.003(3) C15 0.052(5) 0.028(5) 0.078(7) -0.034(5) -0.033(5) 0.018(4) C16 0.041(7) 0.034(7) 0.039(7) -0.024(6) -0.008(8) 0.009(6) C16' 0.041(7) 0.034(7) 0.039(7) -0.024(6) -0.008(8) 0.009(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 O13 2.032(4) 1_564 ? Ni1 O13 2.032(4) 2 ? Ni1 N6 2.059(6) 2_564 ? Ni1 N6 2.059(6) . ? Ni1 O1W 2.124(4) . ? Ni1 O1W 2.124(4) 2_564 ? Ni2 N7 2.093(5) 2 ? Ni2 N7 2.093(5) . ? Ni2 N10 2.099(6) 2 ? Ni2 N10 2.099(6) . ? Ni2 O9 2.118(4) . ? Ni2 O9 2.118(4) 2 ? Mo1 O7 1.681(4) . ? Mo1 O13 1.730(4) . ? Mo1 O6 1.909(4) 2_556 ? Mo1 O5 1.979(4) . ? Mo1 O1 2.227(4) . ? Mo1 O3 2.276(4) 2_556 ? Mo1 Mo3 3.1878(12) . ? Mo2 O10 1.702(5) . ? Mo2 O11 1.728(5) . ? Mo2 O4 1.931(4) . ? Mo2 O6 1.935(4) . ? Mo2 O3 2.201(4) . ? Mo2 O2 2.323(4) 2_556 ? Mo3 O8 1.715(4) . ? Mo3 O9 1.728(4) . ? Mo3 O5 1.855(4) . ? Mo3 O4 2.108(4) . ? Mo3 O1 2.221(4) . ? Mo3 N1 2.248(5) . ? Mo4 O12 1.711(4) . ? Mo4 O2 1.757(4) . ? Mo4 O1 1.890(4) . ? Mo4 O3 1.921(4) . ? Mo4 O4 2.194(4) . ? Mo4 O3 2.476(4) 2_556 ? O2 Mo2 2.323(4) 2_556 ? O3 Mo1 2.276(4) 2_556 ? O3 Mo4 2.476(4) 2_556 ? O6 Mo1 1.909(4) 2_556 ? O13 Ni1 2.032(4) 1_546 ? N1 C1 1.352(8) . ? N1 C2 1.355(9) . ? N2 C2 1.313(9) . ? N2 N3 1.346(8) . ? N3 C1 1.305(9) . ? N3 C3 1.458(8) . ? N4 C7 1.313(9) . ? N4 N5 1.336(8) . ? N4 C6 1.472(9) . ? N5 C8 1.324(10) . ? N6 C7 1.310(9) . ? N6 C8 1.333(9) . ? N7 C9 1.307(8) . ? N7 C10 1.329(9) . ? N8 C10 1.258(10) . ? N8 N9 1.357(9) . ? N9 C9 1.324(9) . ? N9 C11 1.463(8) . ? N10 C13 1.340(9) . ? N10 C14 1.366(9) . ? N11 C14 1.304(9) . ? N11 N12 1.364(8) . ? N12 C13 1.346(9) . ? N12 C15 1.498(9) . ? C3 C4 1.511(10) . ? C4 C5 1.519(9) . ? C5 C6 1.522(11) . ? C11 C12 1.505(10) . ? C12 C12 1.584(14) 2_654 ? C15 C16 1.490(15) . ? C15 C16' 1.56(2) . ? C16 C16 1.58(3) 2_545 ? C16' C16' 1.52(5) 2_545 ? 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 O13 Ni1 O13 180.000(1) 1_564 2 ? O13 Ni1 N6 89.7(2) 1_564 2_564 ? O13 Ni1 N6 90.3(2) 2 2_564 ? O13 Ni1 N6 90.3(2) 1_564 . ? O13 Ni1 N6 89.7(2) 2 . ? N6 Ni1 N6 180.0(3) 2_564 . ? O13 Ni1 O1W 86.31(18) 1_564 . ? O13 Ni1 O1W 93.69(18) 2 . ? N6 Ni1 O1W 91.1(2) 2_564 . ? N6 Ni1 O1W 88.9(2) . . ? O13 Ni1 O1W 93.69(18) 1_564 2_564 ? O13 Ni1 O1W 86.31(18) 2 2_564 ? N6 Ni1 O1W 88.9(2) 2_564 2_564 ? N6 Ni1 O1W 91.1(2) . 2_564 ? O1W Ni1 O1W 180.0 . 2_564 ? N7 Ni2 N7 180.0(4) 2 . ? N7 Ni2 N10 89.7(2) 2 2 ? N7 Ni2 N10 90.3(2) . 2 ? N7 Ni2 N10 90.3(2) 2 . ? N7 Ni2 N10 89.7(2) . . ? N10 Ni2 N10 180.0(4) 2 . ? N7 Ni2 O9 88.25(19) 2 . ? N7 Ni2 O9 91.75(19) . . ? N10 Ni2 O9 91.50(19) 2 . ? N10 Ni2 O9 88.50(19) . . ? N7 Ni2 O9 91.75(19) 2 2 ? N7 Ni2 O9 88.25(19) . 2 ? N10 Ni2 O9 88.50(19) 2 2 ? N10 Ni2 O9 91.50(19) . 2 ? O9 Ni2 O9 180.0(3) . 2 ? O7 Mo1 O13 103.8(2) . . ? O7 Mo1 O6 99.0(2) . 2_556 ? O13 Mo1 O6 100.41(19) . 2_556 ? O7 Mo1 O5 101.0(2) . . ? O13 Mo1 O5 94.51(19) . . ? O6 Mo1 O5 151.38(17) 2_556 . ? O7 Mo1 O1 92.09(19) . . ? O13 Mo1 O1 162.03(19) . . ? O6 Mo1 O1 85.13(16) 2_556 . ? O5 Mo1 O1 73.90(16) . . ? O7 Mo1 O3 164.3(2) . 2_556 ? O13 Mo1 O3 91.29(19) . 2_556 ? O6 Mo1 O3 73.31(16) 2_556 2_556 ? O5 Mo1 O3 82.13(16) . 2_556 ? O1 Mo1 O3 73.82(15) . 2_556 ? O7 Mo1 Mo3 88.05(16) . . ? O13 Mo1 Mo3 126.79(15) . . ? O6 Mo1 Mo3 129.16(13) 2_556 . ? O5 Mo1 Mo3 32.54(12) . . ? O1 Mo1 Mo3 44.14(11) . . ? O3 Mo1 Mo3 86.55(11) 2_556 . ? O10 Mo2 O11 104.1(2) . . ? O10 Mo2 O4 104.2(2) . . ? O11 Mo2 O4 97.1(2) . . ? O10 Mo2 O6 101.4(2) . . ? O11 Mo2 O6 96.49(19) . . ? O4 Mo2 O6 146.96(18) . . ? O10 Mo2 O3 156.2(2) . . ? O11 Mo2 O3 99.63(19) . . ? O4 Mo2 O3 73.49(16) . . ? O6 Mo2 O3 74.61(17) . . ? O10 Mo2 O2 85.22(19) . 2_556 ? O11 Mo2 O2 170.49(19) . 2_556 ? O4 Mo2 O2 82.09(16) . 2_556 ? O6 Mo2 O2 79.64(16) . 2_556 ? O3 Mo2 O2 71.01(15) . 2_556 ? O8 Mo3 O9 103.5(2) . . ? O8 Mo3 O5 101.2(2) . . ? O9 Mo3 O5 100.0(2) . . ? O8 Mo3 O4 154.49(19) . . ? O9 Mo3 O4 95.13(19) . . ? O5 Mo3 O4 92.44(17) . . ? O8 Mo3 O1 91.70(19) . . ? O9 Mo3 O1 164.80(18) . . ? O5 Mo3 O1 76.36(16) . . ? O4 Mo3 O1 70.50(16) . . ? O8 Mo3 N1 82.3(2) . . ? O9 Mo3 N1 93.3(2) . . ? O5 Mo3 N1 164.91(19) . . ? O4 Mo3 N1 79.32(17) . . ? O1 Mo3 N1 88.92(18) . . ? O8 Mo3 Mo1 87.32(15) . . ? O9 Mo3 Mo1 134.83(15) . . ? O5 Mo3 Mo1 35.01(13) . . ? O4 Mo3 Mo1 91.81(12) . . ? O1 Mo3 Mo1 44.30(11) . . ? N1 Mo3 Mo1 131.77(15) . . ? O12 Mo4 O2 104.7(2) . . ? O12 Mo4 O1 104.1(2) . . ? O2 Mo4 O1 102.80(19) . . ? O12 Mo4 O3 104.4(2) . . ? O2 Mo4 O3 97.06(19) . . ? O1 Mo4 O3 139.53(17) . . ? O12 Mo4 O4 96.09(19) . . ? O2 Mo4 O4 158.86(17) . . ? O1 Mo4 O4 75.09(17) . . ? O3 Mo4 O4 73.85(16) . . ? O12 Mo4 O3 178.86(19) . 2_556 ? O2 Mo4 O3 74.65(17) . 2_556 ? O1 Mo4 O3 75.23(15) . 2_556 ? O3 Mo4 O3 76.62(17) . 2_556 ? O4 Mo4 O3 84.59(14) . 2_556 ? Mo4 O1 Mo3 110.52(19) . . ? Mo4 O1 Mo1 115.22(18) . . ? Mo3 O1 Mo1 91.55(15) . . ? Mo4 O2 Mo2 117.3(2) . 2_556 ? Mo4 O3 Mo2 104.86(18) . . ? Mo4 O3 Mo1 153.5(2) . 2_556 ? Mo2 O3 Mo1 92.53(15) . 2_556 ? Mo4 O3 Mo4 103.38(17) . 2_556 ? Mo2 O3 Mo4 96.55(15) . 2_556 ? Mo1 O3 Mo4 94.12(15) 2_556 2_556 ? Mo2 O4 Mo3 150.2(2) . . ? Mo2 O4 Mo4 104.81(17) . . ? Mo3 O4 Mo4 103.71(18) . . ? Mo3 O5 Mo1 112.4(2) . . ? Mo1 O6 Mo2 114.7(2) 2_556 . ? Mo3 O9 Ni2 155.8(3) . . ? Mo1 O13 Ni1 156.5(3) . 1_546 ? C1 N1 C2 103.0(6) . . ? C1 N1 Mo3 124.0(4) . . ? C2 N1 Mo3 131.6(4) . . ? C2 N2 N3 102.5(6) . . ? C1 N3 N2 111.9(5) . . ? C1 N3 C3 126.5(6) . . ? N2 N3 C3 121.5(6) . . ? C7 N4 N5 109.9(6) . . ? C7 N4 C6 129.0(7) . . ? N5 N4 C6 120.9(7) . . ? C8 N5 N4 101.7(6) . . ? C7 N6 C8 102.0(6) . . ? C7 N6 Ni1 127.6(5) . . ? C8 N6 Ni1 130.4(5) . . ? C9 N7 C10 102.8(6) . . ? C9 N7 Ni2 130.9(5) . . ? C10 N7 Ni2 126.3(5) . . ? C10 N8 N9 102.5(7) . . ? C9 N9 N8 108.9(6) . . ? C9 N9 C11 129.1(6) . . ? N8 N9 C11 121.8(6) . . ? C13 N10 C14 104.4(6) . . ? C13 N10 Ni2 123.3(4) . . ? C14 N10 Ni2 132.2(4) . . ? C14 N11 N12 102.5(6) . . ? C13 N12 N11 111.4(6) . . ? C13 N12 C15 125.0(6) . . ? N11 N12 C15 123.4(6) . . ? N3 C1 N1 108.6(6) . . ? N2 C2 N1 114.0(6) . . ? N3 C3 C4 112.3(6) . . ? C3 C4 C5 114.4(6) . . ? C4 C5 C6 109.5(6) . . ? N4 C6 C5 113.7(7) . . ? N6 C7 N4 111.2(6) . . ? N5 C8 N6 115.1(7) . . ? N7 C9 N9 109.4(6) . . ? N8 C10 N7 116.4(7) . . ? N9 C11 C12 111.1(6) . . ? C11 C12 C12 110.2(7) . 2_654 ? N10 C13 N12 107.4(6) . . ? N11 C14 N10 114.3(6) . . ? C16 C15 N12 111.6(8) . . ? C16 C15 C16' 35.6(8) . . ? N12 C15 C16' 108.0(9) . . ? C15 C16 C16 114.1(14) . 2_545 ? C16' C16' C15 110(2) 2_545 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.728 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.201