Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Manners, I.' 'Lough, Alan' 'McWilliams, Andrew R.' 'Rivard, Eric' _publ_contact_author_name 'Prof I Manners' _publ_contact_author_address ; Department of Chemistry University of Toronto 80 St. George Street Toronto M5S 1A1 CANADA ; _publ_contact_author_email 'IMANNERS@CHEM.UTORONTO.CA' _publ_section_title ; Synthesis and characterization of perhalogenated diazaphosphametalletidines containing transition metals from group 4 and 5 ; data_k0015 #(compound 2) _database_code_CSD 173273 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H26 Cl5 N2 O P Si2 Ti' _chemical_formula_weight 502.63 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(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 10.0677(3) _cell_length_b 14.8866(5) _cell_length_c 15.0835(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.576(2) _cell_angle_gamma 90.00 _cell_volume 2177.60(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 17345 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.54 _exptl_crystal_description 'block' _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7550 _exptl_absorpt_correction_T_max 0.8902 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 'none' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 17354 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4952 _reflns_number_gt 4256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2001)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXTL V5.1 (Sheldrick 1999)' _computing_structure_refinement 'SHELXTL V5.1 (Sheldrick 1999)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick 1999)' _computing_publication_material 'SHELXTL V5.1 (Sheldrick 1999)' _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^)+(0.0170P)^2^+1.2752P] 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 4952 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Ti1 Ti 0.39506(3) 0.20376(2) 0.25930(2) 0.01610(8) Uani 1 1 d . . . Cl1 Cl 0.26449(5) -0.03407(3) 0.09850(3) 0.02518(11) Uani 1 1 d . . . Cl2 Cl 0.09066(5) 0.13588(4) 0.02318(3) 0.02716(12) Uani 1 1 d . . . Cl3 Cl 0.59798(5) 0.27565(3) 0.27131(3) 0.02526(11) Uani 1 1 d . . . Cl4 Cl 0.36861(5) 0.21862(3) 0.40374(3) 0.02524(11) Uani 1 1 d . . . Cl5 Cl 0.26657(5) 0.32609(3) 0.20480(3) 0.02556(11) Uani 1 1 d . . . P1 P 0.25094(5) 0.09695(3) 0.12653(3) 0.01496(10) Uani 1 1 d . . . Si1 Si 0.44981(5) 0.18766(4) 0.03541(3) 0.01931(12) Uani 1 1 d . . . Si2 Si 0.07814(5) 0.09747(3) 0.26347(3) 0.01781(11) Uani 1 1 d . . . O1 O 0.52195(13) 0.08710(8) 0.31223(8) 0.0199(3) Uani 1 1 d . . . N1 N 0.38678(15) 0.15157(10) 0.12895(10) 0.0158(3) Uani 1 1 d . . . N2 N 0.22825(15) 0.11377(10) 0.22476(10) 0.0157(3) Uani 1 1 d . . . C1 C 0.6412(2) 0.18575(17) 0.06785(15) 0.0343(5) Uani 1 1 d . . . H1A H 0.6769 0.2257 0.1205 0.051 Uiso 1 1 calc R . . H1B H 0.6740 0.2061 0.0157 0.051 Uiso 1 1 calc R . . H1C H 0.6737 0.1244 0.0845 0.051 Uiso 1 1 calc R . . C2 C 0.3841(3) 0.30259(14) 0.00224(15) 0.0360(5) Uani 1 1 d . . . H2A H 0.4192 0.3436 0.0541 0.054 Uiso 1 1 calc R . . H2B H 0.2831 0.3022 -0.0143 0.054 Uiso 1 1 calc R . . H2C H 0.4154 0.3228 -0.0506 0.054 Uiso 1 1 calc R . . C3 C 0.3866(2) 0.10897(13) -0.06324(13) 0.0235(4) Uani 1 1 d . . . H3A H 0.4152 0.0476 -0.0435 0.035 Uiso 1 1 calc R . . H3B H 0.4257 0.1262 -0.1137 0.035 Uiso 1 1 calc R . . H3C H 0.2858 0.1118 -0.0843 0.035 Uiso 1 1 calc R . . C4 C -0.0385(2) 0.01777(13) 0.18464(14) 0.0247(4) Uani 1 1 d . . . H4A H 0.0114 -0.0380 0.1808 0.037 Uiso 1 1 calc R . . H4B H -0.0702 0.0447 0.1233 0.037 Uiso 1 1 calc R . . H4C H -0.1181 0.0046 0.2082 0.037 Uiso 1 1 calc R . . C5 C -0.0069(2) 0.20835(13) 0.26194(14) 0.0265(4) Uani 1 1 d . . . H5A H -0.0264 0.2341 0.2000 0.040 Uiso 1 1 calc R . . H5B H 0.0543 0.2488 0.3058 0.040 Uiso 1 1 calc R . . H5C H -0.0933 0.2007 0.2792 0.040 Uiso 1 1 calc R . . C6 C 0.1228(2) 0.04801(14) 0.38102(13) 0.0256(4) Uani 1 1 d . . . H6A H 0.1707 -0.0092 0.3807 0.038 Uiso 1 1 calc R . . H6B H 0.0382 0.0378 0.4000 0.038 Uiso 1 1 calc R . . H6C H 0.1829 0.0894 0.4243 0.038 Uiso 1 1 calc R . . C7 C 0.6363(2) 0.05376(14) 0.27818(14) 0.0271(4) Uani 1 1 d . . . H7A H 0.7060 0.1014 0.2815 0.032 Uiso 1 1 calc R . . H7B H 0.6023 0.0334 0.2135 0.032 Uiso 1 1 calc R . . C8 C 0.6971(2) -0.02360(15) 0.34007(16) 0.0343(5) Uani 1 1 d . . . H8A H 0.7711 -0.0030 0.3937 0.041 Uiso 1 1 calc R . . H8B H 0.7348 -0.0698 0.3063 0.041 Uiso 1 1 calc R . . C9 C 0.5751(2) -0.05925(15) 0.36953(17) 0.0357(5) Uani 1 1 d . . . H9A H 0.5180 -0.0995 0.3221 0.043 Uiso 1 1 calc R . . H9B H 0.6054 -0.0924 0.4284 0.043 Uiso 1 1 calc R . . C10 C 0.4975(2) 0.02387(14) 0.38023(15) 0.0317(5) Uani 1 1 d . . . H10A H 0.3979 0.0109 0.3684 0.038 Uiso 1 1 calc R . . H10B H 0.5319 0.0486 0.4432 0.038 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 Ti1 0.01680(17) 0.01534(17) 0.01665(17) -0.00297(12) 0.00536(13) -0.00226(13) Cl1 0.0321(3) 0.0164(2) 0.0301(3) -0.00615(19) 0.0137(2) -0.00266(19) Cl2 0.0195(2) 0.0382(3) 0.0202(2) 0.0041(2) -0.00072(18) 0.0023(2) Cl3 0.0213(2) 0.0235(2) 0.0319(3) -0.0056(2) 0.0088(2) -0.00792(19) Cl4 0.0294(3) 0.0286(3) 0.0196(2) -0.00798(19) 0.00987(19) -0.0056(2) Cl5 0.0275(2) 0.0173(2) 0.0336(3) 0.00091(19) 0.0113(2) 0.00319(19) P1 0.0150(2) 0.0150(2) 0.0147(2) -0.00123(17) 0.00366(17) -0.00029(17) Si1 0.0230(3) 0.0193(3) 0.0179(2) 0.0003(2) 0.0095(2) -0.0017(2) Si2 0.0169(2) 0.0175(3) 0.0209(3) -0.0013(2) 0.0084(2) -0.0014(2) O1 0.0194(7) 0.0217(7) 0.0201(6) 0.0037(5) 0.0081(5) 0.0018(5) N1 0.0153(7) 0.0168(8) 0.0147(7) -0.0013(6) 0.0031(6) -0.0004(6) N2 0.0157(7) 0.0149(8) 0.0165(7) -0.0013(6) 0.0045(6) -0.0008(6) C1 0.0289(11) 0.0509(15) 0.0276(11) -0.0086(10) 0.0154(9) -0.0096(10) C2 0.0604(16) 0.0232(11) 0.0325(12) 0.0059(9) 0.0265(11) 0.0023(10) C3 0.0265(10) 0.0255(11) 0.0198(9) 0.0013(8) 0.0083(8) 0.0018(8) C4 0.0215(10) 0.0250(11) 0.0291(11) -0.0026(8) 0.0093(8) -0.0048(8) C5 0.0228(10) 0.0250(11) 0.0344(11) -0.0015(9) 0.0124(9) 0.0023(8) C6 0.0258(10) 0.0269(11) 0.0267(10) 0.0025(8) 0.0118(8) -0.0017(8) C7 0.0248(10) 0.0277(11) 0.0336(11) 0.0046(9) 0.0164(9) 0.0063(9) C8 0.0305(12) 0.0358(13) 0.0392(13) 0.0087(10) 0.0136(10) 0.0092(10) C9 0.0332(12) 0.0305(12) 0.0465(14) 0.0144(10) 0.0160(10) 0.0049(10) C10 0.0353(12) 0.0320(12) 0.0331(12) 0.0140(9) 0.0183(10) 0.0053(10) _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 Ti1 N1 2.0947(14) . ? Ti1 N2 2.1016(15) . ? Ti1 O1 2.1766(13) . ? Ti1 Cl5 2.2570(6) . ? Ti1 Cl3 2.2699(5) . ? Ti1 Cl4 2.2755(5) . ? Ti1 P1 2.6615(5) . ? Cl1 P1 2.0081(6) . ? Cl2 P1 2.0047(6) . ? P1 N2 1.5787(14) . ? P1 N1 1.5830(15) . ? Si1 N1 1.7784(15) . ? Si1 C2 1.854(2) . ? Si1 C1 1.856(2) . ? Si1 C3 1.866(2) . ? Si2 N2 1.7769(15) . ? Si2 C5 1.857(2) . ? Si2 C4 1.857(2) . ? Si2 C6 1.860(2) . ? O1 C10 1.461(2) . ? O1 C7 1.467(2) . ? C7 C8 1.505(3) . ? C8 C9 1.510(3) . ? C9 C10 1.495(3) . ? 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 Ti1 N2 72.73(6) . . ? N1 Ti1 O1 85.41(5) . . ? N2 Ti1 O1 86.19(5) . . ? N1 Ti1 Cl5 94.76(4) . . ? N2 Ti1 Cl5 94.72(4) . . ? O1 Ti1 Cl5 179.08(4) . . ? N1 Ti1 Cl3 93.32(4) . . ? N2 Ti1 Cl3 164.25(4) . . ? O1 Ti1 Cl3 85.41(4) . . ? Cl5 Ti1 Cl3 93.68(2) . . ? N1 Ti1 Cl4 161.67(4) . . ? N2 Ti1 Cl4 90.46(4) . . ? O1 Ti1 Cl4 86.24(4) . . ? Cl5 Ti1 Cl4 93.86(2) . . ? Cl3 Ti1 Cl4 102.24(2) . . ? N1 Ti1 P1 36.48(4) . . ? N2 Ti1 P1 36.37(4) . . ? O1 Ti1 P1 86.96(4) . . ? Cl5 Ti1 P1 93.706(19) . . ? Cl3 Ti1 P1 129.70(2) . . ? Cl4 Ti1 P1 126.74(2) . . ? N2 P1 N1 103.81(8) . . ? N2 P1 Cl2 113.25(6) . . ? N1 P1 Cl2 112.31(6) . . ? N2 P1 Cl1 112.75(6) . . ? N1 P1 Cl1 113.37(6) . . ? Cl2 P1 Cl1 101.72(3) . . ? N2 P1 Ti1 52.13(5) . . ? N1 P1 Ti1 51.88(5) . . ? Cl2 P1 Ti1 125.08(3) . . ? Cl1 P1 Ti1 133.20(3) . . ? N1 Si1 C2 108.39(8) . . ? N1 Si1 C1 110.64(9) . . ? C2 Si1 C1 110.79(11) . . ? N1 Si1 C3 108.97(8) . . ? C2 Si1 C3 110.09(10) . . ? C1 Si1 C3 107.94(9) . . ? N2 Si2 C5 107.72(8) . . ? N2 Si2 C4 108.90(8) . . ? C5 Si2 C4 110.49(9) . . ? N2 Si2 C6 110.98(8) . . ? C5 Si2 C6 110.88(9) . . ? C4 Si2 C6 107.86(9) . . ? C10 O1 C7 108.88(14) . . ? C10 O1 Ti1 125.37(11) . . ? C7 O1 Ti1 125.44(11) . . ? P1 N1 Si1 128.82(9) . . ? P1 N1 Ti1 91.64(7) . . ? Si1 N1 Ti1 134.42(8) . . ? P1 N2 Si2 129.56(9) . . ? P1 N2 Ti1 91.51(7) . . ? Si2 N2 Ti1 134.36(8) . . ? O1 C7 C8 105.59(15) . . ? C7 C8 C9 102.91(17) . . ? C10 C9 C8 103.34(18) . . ? O1 C10 C9 105.45(15) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.374 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.063 #===END data_k99242 #(compound 3) _database_code_CSD 173274 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H26 Cl5 N2 O P Si2 Zr' _chemical_formula_weight 545.95 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(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 10.1372(4) _cell_length_b 15.1405(8) _cell_length_c 15.1927(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.642(3) _cell_angle_gamma 90.00 _cell_volume 2256.08(19) _cell_formula_units_Z 4 _cell_measurement_temperature 110(1) _cell_measurement_reflns_used 30447 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 30.10 _exptl_crystal_description 'block' _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7439 _exptl_absorpt_correction_T_max 0.7608 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 'none' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 30447 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 30.07 _reflns_number_total 6514 _reflns_number_gt 5638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2001)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXTL V5.1 (Sheldrick 1999)' _computing_structure_refinement 'SHELXTL V5.1 (Sheldrick 1999)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick 1999)' _computing_publication_material 'SHELXTL V5.1 (Sheldrick 1999)' _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^)+1.3653P] 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 6514 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.003 _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 Zr1 Zr 0.602507(15) 0.207365(10) 0.237373(10) 0.01402(4) Uani 1 1 d . . . Cl1 Cl 0.73755(4) -0.03142(3) 0.40458(3) 0.02142(9) Uani 1 1 d . . . Cl2 Cl 0.90820(4) 0.13640(3) 0.47761(3) 0.02318(9) Uani 1 1 d . . . Cl3 Cl 0.38833(4) 0.28025(3) 0.22811(3) 0.02218(9) Uani 1 1 d . . . Cl4 Cl 0.63609(4) 0.21810(3) 0.08622(3) 0.02257(9) Uani 1 1 d . . . Cl5 Cl 0.73663(4) 0.33521(3) 0.29368(3) 0.02337(9) Uani 1 1 d . . . P1 P 0.75091(4) 0.09752(3) 0.37583(3) 0.01335(8) Uani 1 1 d . . . Si1 Si 0.55139(5) 0.18371(3) 0.46811(3) 0.01724(10) Uani 1 1 d . . . Si2 Si 0.92775(4) 0.09622(3) 0.24160(3) 0.01560(9) Uani 1 1 d . . . O1 O 0.47355(11) 0.08723(8) 0.18460(8) 0.0177(2) Uani 1 1 d . . . N1 N 0.61582(13) 0.15062(9) 0.37479(9) 0.0147(3) Uani 1 1 d . . . N2 N 0.77705(13) 0.11297(9) 0.27879(9) 0.0140(3) Uani 1 1 d . . . C1 C 0.36196(18) 0.18076(15) 0.43438(13) 0.0279(4) Uani 1 1 d . . . H1A H 0.3312 0.1206 0.4163 0.042 Uiso 1 1 calc R . . H1B H 0.3282 0.2211 0.3832 0.042 Uiso 1 1 calc R . . H1C H 0.3267 0.1991 0.4859 0.042 Uiso 1 1 calc R . . C2 C 0.6136(2) 0.29773(12) 0.50100(14) 0.0317(5) Uani 1 1 d . . . H2A H 0.7135 0.2981 0.5182 0.048 Uiso 1 1 calc R . . H2B H 0.5796 0.3174 0.5527 0.048 Uiso 1 1 calc R . . H2C H 0.5803 0.3377 0.4494 0.048 Uiso 1 1 calc R . . C3 C 0.61198(18) 0.10625(12) 0.56553(11) 0.0207(3) Uani 1 1 d . . . H3A H 0.5813 0.0462 0.5466 0.031 Uiso 1 1 calc R . . H3B H 0.5747 0.1244 0.6163 0.031 Uiso 1 1 calc R . . H3C H 0.7118 0.1075 0.5848 0.031 Uiso 1 1 calc R . . C4 C 1.04223(17) 0.01811(12) 0.31969(12) 0.0219(4) Uani 1 1 d . . . H4A H 1.0719 0.0446 0.3803 0.033 Uiso 1 1 calc R . . H4B H 1.1221 0.0055 0.2965 0.033 Uiso 1 1 calc R . . H4C H 0.9931 -0.0369 0.3234 0.033 Uiso 1 1 calc R . . C5 C 1.01114(18) 0.20586(12) 0.24295(13) 0.0235(4) Uani 1 1 d . . . H5A H 1.0292 0.2311 0.3042 0.035 Uiso 1 1 calc R . . H5B H 0.9509 0.2454 0.1997 0.035 Uiso 1 1 calc R . . H5C H 1.0973 0.1988 0.2256 0.035 Uiso 1 1 calc R . . C6 C 0.88573(18) 0.04772(12) 0.12499(12) 0.0216(4) Uani 1 1 d . . . H6A H 0.8389 -0.0089 0.1254 0.032 Uiso 1 1 calc R . . H6B H 0.9699 0.0383 0.1058 0.032 Uiso 1 1 calc R . . H6C H 0.8262 0.0883 0.0825 0.032 Uiso 1 1 calc R . . C7 C 0.35953(18) 0.05436(13) 0.21922(13) 0.0248(4) Uani 1 1 d . . . H7A H 0.2908 0.1013 0.2169 0.030 Uiso 1 1 calc R . . H7B H 0.3925 0.0337 0.2828 0.030 Uiso 1 1 calc R . . C8 C 0.2993(2) -0.02132(14) 0.15723(15) 0.0307(4) Uani 1 1 d . . . H8A H 0.2298 -0.0002 0.1032 0.037 Uiso 1 1 calc R . . H8B H 0.2576 -0.0658 0.1896 0.037 Uiso 1 1 calc R . . C9 C 0.4227(2) -0.05853(13) 0.13092(15) 0.0310(4) Uani 1 1 d . . . H9A H 0.4768 -0.0971 0.1794 0.037 Uiso 1 1 calc R . . H9B H 0.3956 -0.0926 0.0735 0.037 Uiso 1 1 calc R . . C10 C 0.5015(2) 0.02308(13) 0.11927(14) 0.0286(4) Uani 1 1 d . . . H10A H 0.6003 0.0101 0.1324 0.034 Uiso 1 1 calc R . . H10B H 0.4706 0.0460 0.0564 0.034 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 Zr1 0.01417(8) 0.01369(8) 0.01460(8) 0.00240(6) 0.00437(6) 0.00173(6) Cl1 0.0270(2) 0.01451(19) 0.0254(2) 0.00461(16) 0.01148(17) 0.00189(16) Cl2 0.01709(19) 0.0321(2) 0.01780(19) -0.00348(17) -0.00026(15) -0.00208(17) Cl3 0.01843(19) 0.0211(2) 0.0282(2) 0.00487(17) 0.00803(16) 0.00629(16) Cl4 0.0257(2) 0.0263(2) 0.01780(19) 0.00692(16) 0.00932(16) 0.00517(17) Cl5 0.0237(2) 0.01566(19) 0.0319(2) -0.00078(17) 0.00915(17) -0.00296(16) P1 0.01321(18) 0.01368(19) 0.01293(19) 0.00094(15) 0.00288(15) 0.00028(15) Si1 0.0206(2) 0.0169(2) 0.0160(2) 0.00003(17) 0.00797(17) 0.00204(19) Si2 0.0145(2) 0.0152(2) 0.0184(2) 0.00182(17) 0.00665(17) 0.00159(18) O1 0.0169(5) 0.0191(6) 0.0186(6) -0.0031(5) 0.0074(5) -0.0013(5) N1 0.0164(6) 0.0136(6) 0.0143(6) 0.0004(5) 0.0045(5) 0.0009(5) N2 0.0125(6) 0.0156(7) 0.0142(6) 0.0025(5) 0.0041(5) 0.0025(5) C1 0.0216(9) 0.0414(12) 0.0237(9) 0.0072(8) 0.0113(7) 0.0078(9) C2 0.0535(13) 0.0186(9) 0.0291(10) -0.0048(8) 0.0215(10) -0.0012(9) C3 0.0235(8) 0.0226(9) 0.0165(8) -0.0002(7) 0.0059(7) -0.0010(7) C4 0.0182(8) 0.0230(9) 0.0258(9) 0.0035(7) 0.0079(7) 0.0056(7) C5 0.0198(8) 0.0208(9) 0.0323(10) 0.0016(7) 0.0109(7) -0.0021(7) C6 0.0225(8) 0.0229(9) 0.0220(9) -0.0009(7) 0.0103(7) 0.0026(7) C7 0.0238(9) 0.0247(9) 0.0307(10) -0.0041(8) 0.0154(8) -0.0061(8) C8 0.0272(10) 0.0291(10) 0.0384(11) -0.0101(9) 0.0130(9) -0.0080(8) C9 0.0294(10) 0.0244(10) 0.0430(12) -0.0125(9) 0.0162(9) -0.0059(8) C10 0.0304(10) 0.0279(10) 0.0323(10) -0.0130(8) 0.0168(8) -0.0034(8) _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 Zr1 N1 2.2299(13) . ? Zr1 N2 2.2375(13) . ? Zr1 O1 2.2651(12) . ? Zr1 Cl5 2.3957(5) . ? Zr1 Cl3 2.4077(4) . ? Zr1 Cl4 2.4107(5) . ? Zr1 P1 2.8025(4) . ? Cl1 P1 2.0124(6) . ? Cl2 P1 2.0084(6) . ? P1 N2 1.5798(14) . ? P1 N1 1.5847(14) . ? Si1 N1 1.7766(14) . ? Si1 C1 1.8586(19) . ? Si1 C2 1.8623(19) . ? Si1 C3 1.8664(18) . ? Si2 N2 1.7759(13) . ? Si2 C4 1.8592(18) . ? Si2 C5 1.8606(18) . ? Si2 C6 1.8649(18) . ? O1 C10 1.467(2) . ? O1 C7 1.472(2) . ? C7 C8 1.511(3) . ? C8 C9 1.515(3) . ? C9 C10 1.506(3) . ? 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 Zr1 N2 68.54(5) . . ? N1 Zr1 O1 85.12(5) . . ? N2 Zr1 O1 86.05(5) . . ? N1 Zr1 Cl5 94.73(4) . . ? N2 Zr1 Cl5 94.51(4) . . ? O1 Zr1 Cl5 179.32(3) . . ? N1 Zr1 Cl3 94.10(4) . . ? N2 Zr1 Cl3 161.17(4) . . ? O1 Zr1 Cl3 85.19(3) . . ? Cl5 Zr1 Cl3 94.159(16) . . ? N1 Zr1 Cl4 158.15(4) . . ? N2 Zr1 Cl4 91.08(4) . . ? O1 Zr1 Cl4 85.69(3) . . ? Cl5 Zr1 Cl4 94.682(17) . . ? Cl3 Zr1 Cl4 104.824(16) . . ? N1 Zr1 P1 34.38(3) . . ? N2 Zr1 P1 34.27(3) . . ? O1 Zr1 P1 86.64(3) . . ? Cl5 Zr1 P1 93.611(15) . . ? Cl3 Zr1 P1 128.383(15) . . ? Cl4 Zr1 P1 125.220(15) . . ? N2 P1 N1 105.30(7) . . ? N2 P1 Cl2 112.79(5) . . ? N1 P1 Cl2 112.01(6) . . ? N2 P1 Cl1 112.50(6) . . ? N1 P1 Cl1 112.89(6) . . ? Cl2 P1 Cl1 101.60(3) . . ? N2 P1 Zr1 52.88(5) . . ? N1 P1 Zr1 52.62(5) . . ? Cl2 P1 Zr1 125.10(2) . . ? Cl1 P1 Zr1 133.30(2) . . ? N1 Si1 C1 109.62(8) . . ? N1 Si1 C2 107.92(8) . . ? C1 Si1 C2 110.62(10) . . ? N1 Si1 C3 110.00(7) . . ? C1 Si1 C3 108.28(8) . . ? C2 Si1 C3 110.40(9) . . ? N2 Si2 C4 109.65(7) . . ? N2 Si2 C5 107.10(7) . . ? C4 Si2 C5 110.61(8) . . ? N2 Si2 C6 110.50(7) . . ? C4 Si2 C6 108.15(8) . . ? C5 Si2 C6 110.84(9) . . ? C10 O1 C7 108.75(13) . . ? C10 O1 Zr1 125.33(10) . . ? C7 O1 Zr1 125.45(10) . . ? P1 N1 Si1 128.78(8) . . ? P1 N1 Zr1 93.00(6) . . ? Si1 N1 Zr1 133.72(7) . . ? P1 N2 Si2 129.52(8) . . ? P1 N2 Zr1 92.85(6) . . ? Si2 N2 Zr1 133.20(7) . . ? O1 C7 C8 105.30(14) . . ? C7 C8 C9 102.47(15) . . ? C10 C9 C8 102.92(16) . . ? O1 C10 C9 105.36(14) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.418 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.074 #===END data_k0108 #(compound 5) _database_code_CSD 173275 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 Cl6 N2 Nb P Si2' _chemical_formula_weight 510.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Nb' 'Nb' -2.0727 0.6215 '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' 'P' 'P' 0.1023 0.0942 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3280(9) _cell_length_b 8.7650(8) _cell_length_c 12.4990(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.679(4) _cell_angle_gamma 90.00 _cell_volume 988.56(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 1766 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.03 _exptl_crystal_description 'needle' _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 1.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7187 _exptl_absorpt_correction_T_max 0.9097 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scan and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 'none' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 2963 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.06 _reflns_number_total 2963 _reflns_number_gt 2532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2001)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXTL V5.1 (Sheldrick 1999)' _computing_structure_refinement 'SHELXTL V5.1 (Sheldrick 1999)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick 1999)' _computing_publication_material 'SHELXTL V5.1 (Sheldrick 1999)' _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^)+0.0866P] 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 SHELXL _refine_ls_extinction_coef 0.0073(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(10) _refine_ls_number_reflns 2963 _refine_ls_number_parameters 171 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1083 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Nb1 Nb 0.38801(7) 0.33105(7) 0.27933(5) 0.0338(2) Uani 1 1 d . . . Cl1 Cl 0.5030(2) 0.1559(2) 0.41184(17) 0.0447(5) Uani 1 1 d . . . Cl2 Cl 0.4872(2) 0.2009(3) 0.14920(17) 0.0467(5) Uani 1 1 d . . . Cl3 Cl 0.1603(2) 0.2321(3) 0.17994(17) 0.0480(5) Uani 1 1 d . . . Cl4 Cl 0.2622(2) 0.4251(3) 0.40654(16) 0.0427(5) Uani 1 1 d . . . Cl5 Cl 0.5331(2) 0.8041(2) 0.30891(17) 0.0462(5) Uani 1 1 d . . . Cl6 Cl 0.6353(2) 0.6211(3) 0.12811(16) 0.0474(5) Uani 1 1 d . . . P1 P 0.5218(2) 0.5969(2) 0.24291(16) 0.0348(5) Uani 1 1 d . . . Si1 Si 0.2111(2) 0.6161(3) 0.08300(17) 0.0393(5) Uani 1 1 d . . . Si2 Si 0.7743(2) 0.4309(3) 0.40504(18) 0.0382(5) Uani 1 1 d . . . N1 N 0.3580(6) 0.5384(8) 0.1895(5) 0.0352(14) Uani 1 1 d . . . N2 N 0.5863(6) 0.4651(7) 0.3305(5) 0.0367(15) Uani 1 1 d . . . C1 C 0.0412(9) 0.6183(12) 0.1357(7) 0.053(2) Uani 1 1 d . . . H1A H 0.0318 0.5205 0.1713 0.079 Uiso 1 1 calc R . . H1B H -0.0460 0.6345 0.0739 0.079 Uiso 1 1 calc R . . H1C H 0.0484 0.7010 0.1896 0.079 Uiso 1 1 calc R . . C2 C 0.2617(10) 0.8158(12) 0.0529(7) 0.056(2) Uani 1 1 d . . . H2A H 0.3498 0.8135 0.0237 0.084 Uiso 1 1 calc R . . H2B H 0.2826 0.8761 0.1211 0.084 Uiso 1 1 calc R . . H2C H 0.1790 0.8621 -0.0019 0.084 Uiso 1 1 calc R . . C3 C 0.1944(9) 0.4951(11) -0.0407(7) 0.052(2) Uani 1 1 d . . . H3A H 0.2865 0.5004 -0.0646 0.078 Uiso 1 1 calc R . . H3B H 0.1118 0.5316 -0.1004 0.078 Uiso 1 1 calc R . . H3C H 0.1759 0.3893 -0.0227 0.078 Uiso 1 1 calc R . . C4 C 0.7876(9) 0.3834(11) 0.5513(6) 0.047(2) Uani 1 1 d . . . H4A H 0.7447 0.2822 0.5557 0.070 Uiso 1 1 calc R . . H4B H 0.7332 0.4595 0.5829 0.070 Uiso 1 1 calc R . . H4C H 0.8919 0.3832 0.5929 0.070 Uiso 1 1 calc R . . C5 C 0.8460(9) 0.2793(11) 0.3310(7) 0.053(2) Uani 1 1 d . . . H5A H 0.8055 0.1807 0.3462 0.080 Uiso 1 1 calc R . . H5B H 0.9543 0.2766 0.3562 0.080 Uiso 1 1 calc R . . H5C H 0.8162 0.2997 0.2514 0.080 Uiso 1 1 calc R . . C6 C 0.8795(9) 0.6130(11) 0.4031(7) 0.050(2) Uani 1 1 d . . . H6A H 0.8307 0.6962 0.4326 0.075 Uiso 1 1 calc R . . H6B H 0.8818 0.6368 0.3270 0.075 Uiso 1 1 calc R . . H6C H 0.9811 0.6010 0.4488 0.075 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 Nb1 0.0372(4) 0.0305(4) 0.0333(4) 0.0000(3) 0.0083(3) -0.0014(3) Cl1 0.0523(12) 0.0365(11) 0.0427(11) 0.0050(9) 0.0076(9) 0.0015(9) Cl2 0.0547(12) 0.0461(12) 0.0407(11) -0.0086(9) 0.0146(9) 0.0015(10) Cl3 0.0447(11) 0.0488(13) 0.0475(12) -0.0072(10) 0.0064(9) -0.0082(10) Cl4 0.0452(11) 0.0470(12) 0.0387(10) -0.0044(9) 0.0156(9) -0.0020(10) Cl5 0.0539(11) 0.0360(13) 0.0479(11) -0.0056(9) 0.0112(9) -0.0011(9) Cl6 0.0497(11) 0.0536(13) 0.0427(11) 0.0031(10) 0.0187(9) -0.0039(10) P1 0.0375(11) 0.0332(11) 0.0343(10) 0.0000(9) 0.0102(9) -0.0020(9) Si1 0.0426(13) 0.0362(12) 0.0387(12) 0.0030(11) 0.0093(10) 0.0026(10) Si2 0.0364(11) 0.0408(13) 0.0369(12) -0.0020(10) 0.0084(9) -0.0002(10) N1 0.032(3) 0.039(4) 0.032(3) -0.005(3) 0.005(3) -0.001(3) N2 0.038(3) 0.039(4) 0.035(3) 0.007(3) 0.011(3) -0.002(3) C1 0.049(5) 0.058(6) 0.053(5) 0.017(5) 0.014(4) 0.013(5) C2 0.059(5) 0.047(5) 0.058(5) 0.017(5) 0.009(4) 0.005(5) C3 0.052(5) 0.054(6) 0.049(5) 0.003(5) 0.012(4) 0.005(5) C4 0.038(4) 0.056(6) 0.042(4) 0.002(4) 0.002(4) 0.010(4) C5 0.046(5) 0.062(6) 0.051(5) 0.000(4) 0.010(4) 0.009(4) C6 0.043(5) 0.051(5) 0.052(5) -0.005(5) 0.005(4) -0.003(4) _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 Nb1 N1 2.117(7) . ? Nb1 N2 2.147(6) . ? Nb1 Cl1 2.313(2) . ? Nb1 Cl3 2.339(2) . ? Nb1 Cl4 2.3516(19) . ? Nb1 Cl2 2.359(2) . ? Nb1 P1 2.735(2) . ? Cl5 P1 1.987(3) . ? Cl6 P1 1.999(3) . ? P1 N1 1.589(6) . ? P1 N2 1.601(6) . ? Si1 N1 1.786(7) . ? Si1 C3 1.849(9) . ? Si1 C1 1.864(8) . ? Si1 C2 1.875(10) . ? Si2 N2 1.790(6) . ? Si2 C5 1.839(9) . ? Si2 C4 1.849(8) . ? Si2 C6 1.877(9) . ? 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 Nb1 N2 71.1(2) . . ? N1 Nb1 Cl1 157.58(17) . . ? N2 Nb1 Cl1 86.66(17) . . ? N1 Nb1 Cl3 93.25(17) . . ? N2 Nb1 Cl3 163.53(17) . . ? Cl1 Nb1 Cl3 109.15(8) . . ? N1 Nb1 Cl4 92.08(17) . . ? N2 Nb1 Cl4 98.42(17) . . ? Cl1 Nb1 Cl4 88.22(8) . . ? Cl3 Nb1 Cl4 86.99(7) . . ? N1 Nb1 Cl2 94.10(17) . . ? N2 Nb1 Cl2 90.65(17) . . ? Cl1 Nb1 Cl2 88.91(8) . . ? Cl3 Nb1 Cl2 85.21(7) . . ? Cl4 Nb1 Cl2 170.30(8) . . ? N1 Nb1 P1 35.41(17) . . ? N2 Nb1 P1 35.77(17) . . ? Cl1 Nb1 P1 122.43(7) . . ? Cl3 Nb1 P1 128.23(7) . . ? Cl4 Nb1 P1 98.09(7) . . ? Cl2 Nb1 P1 91.26(7) . . ? N1 P1 N2 102.1(3) . . ? N1 P1 Cl5 114.4(3) . . ? N2 P1 Cl5 113.9(3) . . ? N1 P1 Cl6 111.1(2) . . ? N2 P1 Cl6 113.1(2) . . ? Cl5 P1 Cl6 102.64(13) . . ? N1 P1 Nb1 50.6(2) . . ? N2 P1 Nb1 51.6(2) . . ? Cl5 P1 Nb1 133.50(11) . . ? Cl6 P1 Nb1 123.85(11) . . ? N1 Si1 C3 106.9(4) . . ? N1 Si1 C1 107.5(3) . . ? C3 Si1 C1 113.7(4) . . ? N1 Si1 C2 108.7(4) . . ? C3 Si1 C2 109.9(4) . . ? C1 Si1 C2 110.0(5) . . ? N2 Si2 C5 107.0(3) . . ? N2 Si2 C4 111.3(3) . . ? C5 Si2 C4 113.1(4) . . ? N2 Si2 C6 107.3(3) . . ? C5 Si2 C6 110.5(4) . . ? C4 Si2 C6 107.5(4) . . ? P1 N1 Si1 131.7(4) . . ? P1 N1 Nb1 94.0(3) . . ? Si1 N1 Nb1 134.1(3) . . ? P1 N2 Si2 128.7(4) . . ? P1 N2 Nb1 92.6(3) . . ? Si2 N2 Nb1 136.0(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.521 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.099 #===END data_k99256 #(compound 6) _database_code_CSD 173276 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Cl11 N6 Nb2 P3 Si4' _chemical_formula_weight 1045.51 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 '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 26.3658(9) _cell_length_b 10.4749(5) _cell_length_c 16.1779(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.783(2) _cell_angle_gamma 90.00 _cell_volume 4056.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 58454 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 26.08 _exptl_crystal_description 'block' _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7475 _exptl_absorpt_correction_T_max 0.8608 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 'none' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 58454 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.06 _reflns_number_total 4004 _reflns_number_gt 3427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2001)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXTL V5.1 (Sheldrick 1999)' _computing_structure_refinement 'SHELXTL V5.1 (Sheldrick 1999)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick 1999)' _computing_publication_material 'SHELXTL V5.1 (Sheldrick 1999)' _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^)+(0.0299P)^2^+6.4126P] 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 SHELXL _refine_ls_extinction_coef 0.00042(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4004 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.003 _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 Nb1 Nb 0.407408(10) 0.15936(3) 0.141505(17) 0.02367(10) Uani 1 1 d . . . Cl1 Cl 0.27972(3) 0.38618(9) 0.17663(6) 0.0405(2) Uani 1 1 d . . . Cl2 Cl 0.39927(4) 0.45949(8) 0.31600(5) 0.0358(2) Uani 1 1 d . . . Cl3 Cl 0.5000 0.27362(10) 0.2500 0.0263(2) Uani 1 2 d S . . Cl4 Cl 0.32415(3) 0.06844(9) 0.03914(6) 0.0369(2) Uani 1 1 d . . . Cl5 Cl 0.43357(3) 0.20818(8) 0.02323(5) 0.03324(19) Uani 1 1 d . . . Cl6 Cl 0.51686(4) -0.18610(9) 0.16773(6) 0.0432(2) Uani 1 1 d . . . P1 P 0.5000 -0.06916(11) 0.2500 0.0278(3) Uani 1 2 d S . . P2 P 0.35982(3) 0.34449(8) 0.20869(5) 0.02472(18) Uani 1 1 d . . . Si1 Si 0.36344(4) 0.10279(9) 0.31922(6) 0.0286(2) Uani 1 1 d . . . Si2 Si 0.36905(4) 0.49170(9) 0.05368(6) 0.0311(2) Uani 1 1 d . . . N1 N 0.37436(10) 0.1985(2) 0.23663(17) 0.0244(5) Uani 1 1 d . . . N2 N 0.37754(10) 0.3632(2) 0.12890(17) 0.0258(5) Uani 1 1 d . . . N3 N 0.44591(10) 0.0111(2) 0.19095(17) 0.0259(5) Uani 1 1 d . . . C1 C 0.30741(15) 0.1758(3) 0.3458(3) 0.0398(8) Uani 1 1 d . . . H1A H 0.2719 0.1738 0.2914 0.060 Uiso 1 1 calc R . . H1B H 0.3173 0.2645 0.3653 0.060 Uiso 1 1 calc R . . H1C H 0.3036 0.1275 0.3948 0.060 Uiso 1 1 calc R . . C2 C 0.43018(15) 0.1025(3) 0.4224(2) 0.0399(8) Uani 1 1 d . . . H2A H 0.4579 0.0519 0.4111 0.060 Uiso 1 1 calc R . . H2B H 0.4243 0.0652 0.4733 0.060 Uiso 1 1 calc R . . H2C H 0.4437 0.1903 0.4376 0.060 Uiso 1 1 calc R . . C3 C 0.34056(13) -0.0576(3) 0.2693(2) 0.0343(8) Uani 1 1 d . . . H3A H 0.3672 -0.0912 0.2470 0.051 Uiso 1 1 calc R . . H3C H 0.3035 -0.0514 0.2186 0.051 Uiso 1 1 calc R . . H3D H 0.3389 -0.1150 0.3159 0.051 Uiso 1 1 calc R . . C4 C 0.3406(2) 0.6314(4) 0.0914(3) 0.0612(12) Uani 1 1 d . . . H4A H 0.3027 0.6120 0.0848 0.092 Uiso 1 1 calc R . . H4B H 0.3395 0.7057 0.0538 0.092 Uiso 1 1 calc R . . H4C H 0.3646 0.6502 0.1553 0.092 Uiso 1 1 calc R . . C5 C 0.43892(15) 0.5347(4) 0.0593(2) 0.0425(9) Uani 1 1 d . . . H5A H 0.4521 0.4664 0.0318 0.064 Uiso 1 1 calc R . . H5B H 0.4654 0.5459 0.1230 0.064 Uiso 1 1 calc R . . H5C H 0.4361 0.6145 0.0260 0.064 Uiso 1 1 calc R . . C6 C 0.31849(13) 0.4387(3) -0.0611(2) 0.0353(8) Uani 1 1 d . . . H6A H 0.2843 0.4081 -0.0577 0.053 Uiso 1 1 calc R . . H6B H 0.3350 0.3694 -0.0824 0.053 Uiso 1 1 calc R . . H6C H 0.3095 0.5105 -0.1037 0.053 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 Nb1 0.02400(15) 0.02745(17) 0.01823(15) -0.00042(11) 0.00754(11) 0.00261(11) Cl1 0.0314(4) 0.0546(5) 0.0387(5) 0.0103(4) 0.0177(4) 0.0152(4) Cl2 0.0482(5) 0.0359(4) 0.0268(4) -0.0050(3) 0.0191(4) -0.0006(4) Cl3 0.0250(5) 0.0264(5) 0.0258(5) 0.000 0.0090(4) 0.000 Cl4 0.0275(4) 0.0462(5) 0.0295(4) -0.0072(4) 0.0045(3) -0.0009(3) Cl5 0.0391(4) 0.0397(5) 0.0254(4) 0.0013(3) 0.0179(3) 0.0070(3) Cl6 0.0389(5) 0.0370(5) 0.0442(5) -0.0149(4) 0.0081(4) 0.0060(4) P1 0.0256(5) 0.0249(6) 0.0268(6) 0.000 0.0049(5) 0.000 P2 0.0267(4) 0.0289(4) 0.0207(4) 0.0028(3) 0.0120(3) 0.0051(3) Si1 0.0302(4) 0.0317(5) 0.0240(4) 0.0040(4) 0.0115(4) -0.0035(4) Si2 0.0419(5) 0.0295(5) 0.0250(5) 0.0056(4) 0.0171(4) 0.0045(4) N1 0.0240(12) 0.0270(13) 0.0216(13) 0.0036(10) 0.0090(10) 0.0014(10) N2 0.0313(13) 0.0289(13) 0.0190(12) 0.0032(10) 0.0122(10) 0.0052(11) N3 0.0265(12) 0.0256(13) 0.0233(13) -0.0007(11) 0.0083(10) -0.0006(11) C1 0.050(2) 0.041(2) 0.040(2) 0.0042(16) 0.0310(17) -0.0058(16) C2 0.0437(19) 0.041(2) 0.0274(18) 0.0099(15) 0.0078(15) -0.0058(16) C3 0.0300(16) 0.0349(18) 0.0370(19) 0.0030(15) 0.0131(14) -0.0043(14) C4 0.108(4) 0.041(2) 0.052(3) 0.013(2) 0.050(3) 0.023(2) C5 0.046(2) 0.041(2) 0.034(2) 0.0043(16) 0.0100(16) -0.0151(17) C6 0.0315(17) 0.043(2) 0.0281(18) 0.0128(15) 0.0089(14) 0.0005(15) _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 Nb1 N3 1.844(2) . ? Nb1 N1 2.102(3) . ? Nb1 N2 2.255(3) . ? Nb1 Cl4 2.3281(8) . ? Nb1 Cl5 2.3463(8) . ? Nb1 Cl3 2.6231(5) . ? Nb1 P2 2.7676(8) . ? Cl1 P2 2.0005(11) . ? Cl2 P2 2.0082(11) . ? Cl3 Nb1 2.6231(5) 2_655 ? Cl6 P1 1.9913(11) . ? P1 N3 1.585(2) 2_655 ? P1 N3 1.585(2) . ? P1 Cl6 1.9913(11) 2_655 ? P2 N2 1.558(3) . ? P2 N1 1.595(3) . ? Si1 N1 1.788(3) . ? Si1 C2 1.850(3) . ? Si1 C3 1.852(3) . ? Si1 C1 1.867(4) . ? Si2 N2 1.765(3) . ? Si2 C4 1.860(4) . ? Si2 C6 1.860(3) . ? Si2 C5 1.861(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 N3 Nb1 N1 99.70(11) . . ? N3 Nb1 N2 160.79(10) . . ? N1 Nb1 N2 69.22(9) . . ? N3 Nb1 Cl4 98.48(8) . . ? N1 Nb1 Cl4 92.52(7) . . ? N2 Nb1 Cl4 97.67(7) . . ? N3 Nb1 Cl5 103.93(8) . . ? N1 Nb1 Cl5 155.25(7) . . ? N2 Nb1 Cl5 86.03(7) . . ? Cl4 Nb1 Cl5 91.20(3) . . ? N3 Nb1 Cl3 84.57(8) . . ? N1 Nb1 Cl3 88.64(7) . . ? N2 Nb1 Cl3 79.65(7) . . ? Cl4 Nb1 Cl3 176.50(3) . . ? Cl5 Nb1 Cl3 86.39(2) . . ? N3 Nb1 P2 132.64(8) . . ? N1 Nb1 P2 34.97(7) . . ? N2 Nb1 P2 34.26(6) . . ? Cl4 Nb1 P2 96.81(3) . . ? Cl5 Nb1 P2 120.28(3) . . ? Cl3 Nb1 P2 82.27(2) . . ? Nb1 Cl3 Nb1 125.71(4) . 2_655 ? N3 P1 N3 115.93(19) 2_655 . ? N3 P1 Cl6 109.43(10) 2_655 . ? N3 P1 Cl6 108.66(9) . . ? N3 P1 Cl6 108.66(9) 2_655 2_655 ? N3 P1 Cl6 109.43(10) . 2_655 ? Cl6 P1 Cl6 104.07(8) . 2_655 ? N2 P2 N1 103.60(14) . . ? N2 P2 Cl1 114.10(10) . . ? N1 P2 Cl1 112.64(10) . . ? N2 P2 Cl2 114.48(11) . . ? N1 P2 Cl2 110.74(10) . . ? Cl1 P2 Cl2 101.60(5) . . ? N2 P2 Nb1 54.54(10) . . ? N1 P2 Nb1 49.07(9) . . ? Cl1 P2 Nb1 130.86(5) . . ? Cl2 P2 Nb1 127.16(4) . . ? N1 Si1 C2 106.58(14) . . ? N1 Si1 C3 107.96(14) . . ? C2 Si1 C3 113.88(16) . . ? N1 Si1 C1 109.47(14) . . ? C2 Si1 C1 109.73(18) . . ? C3 Si1 C1 109.11(16) . . ? N2 Si2 C4 109.04(16) . . ? N2 Si2 C6 106.93(14) . . ? C4 Si2 C6 110.1(2) . . ? N2 Si2 C5 108.31(15) . . ? C4 Si2 C5 108.7(2) . . ? C6 Si2 C5 113.68(16) . . ? P2 N1 Si1 130.90(16) . . ? P2 N1 Nb1 95.95(12) . . ? Si1 N1 Nb1 133.12(14) . . ? P2 N2 Si2 132.18(17) . . ? P2 N2 Nb1 91.20(12) . . ? Si2 N2 Nb1 136.31(14) . . ? P1 N3 Nb1 154.26(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.577 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.088 data_k01281 #(compound 6) _database_code_CSD 179458 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Cl11 N6 Nb2 P3 Si4' _chemical_formula_weight 1045.51 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Nb' 'Nb' -2.0727 0.6215 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.1891(2) _cell_length_b 24.4588(6) _cell_length_c 18.0989(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.50(3) _cell_angle_gamma 90.00 _cell_volume 4023.07(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8050 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'plate' _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6356 _exptl_absorpt_correction_T_max 0.8114 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28732 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.44 _reflns_number_total 9011 _reflns_number_gt 6806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2001)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXTL V6.12 (Sheldrick 2001)' _computing_structure_refinement 'SHELXTL V6.12 (Sheldrick 2001)' _computing_molecular_graphics 'SHELXTL V6.12 (Sheldrick 2001)' _computing_publication_material 'SHELXTL V6.12 (Sheldrick 2001)' _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^)+12.4054P] 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 SHELXL _refine_ls_extinction_coef 0.00128(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9011 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.003 _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 Nb1 Nb 0.20030(4) 0.162225(16) 0.94200(2) 0.02134(11) Uani 1 1 d . . . Nb2 Nb 0.29496(4) 0.295283(16) 0.93905(2) 0.02214(11) Uani 1 1 d . . . Cl1 Cl -0.01867(12) 0.17471(5) 0.85683(6) 0.0316(3) Uani 1 1 d . . . Cl2 Cl 0.14343(14) 0.06724(5) 0.94607(7) 0.0352(3) Uani 1 1 d . . . Cl3 Cl 0.41110(13) 0.14812(5) 1.03055(7) 0.0343(3) Uani 1 1 d . . . Cl4 Cl 0.33597(16) 0.20382(6) 0.72438(7) 0.0451(3) Uani 1 1 d . . . Cl5 Cl 0.59945(13) 0.19291(6) 0.85274(9) 0.0475(4) Uani 1 1 d . . . Cl6 Cl 0.15432(14) 0.24501(6) 1.15122(6) 0.0391(3) Uani 1 1 d . . . Cl7 Cl -0.11934(12) 0.26376(5) 1.03113(7) 0.0385(3) Uani 1 1 d . . . Cl8 Cl 0.42376(14) 0.33814(6) 0.85016(8) 0.0437(3) Uani 1 1 d . . . Cl9 Cl 0.51123(13) 0.28238(5) 1.02161(8) 0.0447(3) Uani 1 1 d . . . Cl10 Cl 0.18184(15) 0.46339(5) 0.91013(7) 0.0425(3) Uani 1 1 d . . . Cl11 Cl -0.04144(14) 0.40931(6) 0.99942(8) 0.0454(3) Uani 1 1 d . . . P1 P 0.07187(12) 0.22370(5) 1.04691(6) 0.0232(2) Uani 1 1 d . . . P2 P 0.38187(13) 0.18501(5) 0.83255(7) 0.0272(3) Uani 1 1 d . . . P3 P 0.13805(12) 0.39040(5) 0.95330(7) 0.0251(3) Uani 1 1 d . . . Si1 Si -0.04351(15) 0.11024(6) 1.07310(8) 0.0330(3) Uani 1 1 d . . . Si2 Si 0.36394(15) 0.06216(5) 0.82020(7) 0.0297(3) Uani 1 1 d . . . Si3 Si -0.02051(13) 0.34177(6) 0.80842(7) 0.0286(3) Uani 1 1 d . . . Si4 Si 0.38287(16) 0.40308(6) 1.08386(8) 0.0348(3) Uani 1 1 d . . . N1 N 0.3212(4) 0.12816(16) 0.8545(2) 0.0269(8) Uani 1 1 d . . . N2 N 0.0605(4) 0.16069(15) 1.0323(2) 0.0253(8) Uani 1 1 d . . . N3 N 0.3037(4) 0.22576(15) 0.8831(2) 0.0247(8) Uani 1 1 d . . . N4 N 0.1759(4) 0.24377(15) 0.98955(19) 0.0215(8) Uani 1 1 d . . . N5 N 0.1081(4) 0.34375(15) 0.89253(19) 0.0225(8) Uani 1 1 d . . . N6 N 0.2715(4) 0.36816(15) 1.0093(2) 0.0265(8) Uani 1 1 d . . . C1 C 0.4887(8) 0.0717(2) 0.7483(4) 0.067(2) Uani 1 1 d . . . H1A H 0.5815 0.0881 0.7717 0.101 Uiso 1 1 calc R . . H1B H 0.4414 0.0959 0.7086 0.101 Uiso 1 1 calc R . . H1C H 0.5086 0.0362 0.7268 0.101 Uiso 1 1 calc R . . C2 C 0.4617(6) 0.0202(2) 0.8967(3) 0.0440(13) Uani 1 1 d . . . H2A H 0.4080 0.0213 0.9396 0.066 Uiso 1 1 calc R . . H2B H 0.5611 0.0348 0.9114 0.066 Uiso 1 1 calc R . . H2C H 0.4678 -0.0176 0.8797 0.066 Uiso 1 1 calc R . . C3 C 0.1930(6) 0.0303(2) 0.7716(3) 0.0463(14) Uani 1 1 d . . . H3A H 0.1143 0.0344 0.8023 0.069 Uiso 1 1 calc R . . H3B H 0.2105 -0.0087 0.7636 0.069 Uiso 1 1 calc R . . H3C H 0.1641 0.0483 0.7233 0.069 Uiso 1 1 calc R . . C4 C -0.1444(8) 0.1454(3) 1.1414(4) 0.066(2) Uani 1 1 d . . . H4A H -0.2133 0.1720 1.1151 0.099 Uiso 1 1 calc R . . H4B H -0.0740 0.1644 1.1787 0.099 Uiso 1 1 calc R . . H4C H -0.1990 0.1184 1.1663 0.099 Uiso 1 1 calc R . . C5 C 0.0872(6) 0.0603(2) 1.1249(3) 0.0493(15) Uani 1 1 d . . . H5A H 0.1689 0.0537 1.0968 0.074 Uiso 1 1 calc R . . H5B H 0.0358 0.0258 1.1308 0.074 Uiso 1 1 calc R . . H5C H 0.1256 0.0752 1.1742 0.074 Uiso 1 1 calc R . . C6 C -0.1840(5) 0.0818(2) 1.0006(3) 0.0408(13) Uani 1 1 d . . . H6A H -0.1376 0.0701 0.9579 0.061 Uiso 1 1 calc R . . H6B H -0.2580 0.1099 0.9844 0.061 Uiso 1 1 calc R . . H6C H -0.2313 0.0505 1.0209 0.061 Uiso 1 1 calc R . . C7 C -0.0361(7) 0.4103(3) 0.7649(4) 0.0624(18) Uani 1 1 d . . . H7A H 0.0618 0.4233 0.7580 0.094 Uiso 1 1 calc R . . H7B H -0.0795 0.4358 0.7974 0.094 Uiso 1 1 calc R . . H7C H -0.0991 0.4082 0.7163 0.094 Uiso 1 1 calc R . . C8 C -0.1995(5) 0.3210(3) 0.8348(3) 0.0504(16) Uani 1 1 d . . . H8A H -0.2298 0.3476 0.8700 0.076 Uiso 1 1 calc R . . H8B H -0.1898 0.2848 0.8583 0.076 Uiso 1 1 calc R . . H8C H -0.2737 0.3195 0.7899 0.076 Uiso 1 1 calc R . . C9 C 0.0501(5) 0.2931(2) 0.7436(3) 0.0376(12) Uani 1 1 d . . . H9A H 0.1494 0.3040 0.7361 0.056 Uiso 1 1 calc R . . H9B H -0.0150 0.2933 0.6955 0.056 Uiso 1 1 calc R . . H9C H 0.0530 0.2562 0.7650 0.056 Uiso 1 1 calc R . . C10 C 0.5581(6) 0.4218(3) 1.0511(3) 0.0543(16) Uani 1 1 d . . . H10A H 0.6207 0.3893 1.0515 0.081 Uiso 1 1 calc R . . H10B H 0.6090 0.4496 1.0842 0.081 Uiso 1 1 calc R . . H10C H 0.5374 0.4362 1.0001 0.081 Uiso 1 1 calc R . . C11 C 0.4067(8) 0.3590(3) 1.1674(3) 0.0600(18) Uani 1 1 d . . . H11A H 0.4510 0.3242 1.1557 0.090 Uiso 1 1 calc R . . H11B H 0.3107 0.3522 1.1830 0.090 Uiso 1 1 calc R . . H11C H 0.4713 0.3773 1.2079 0.090 Uiso 1 1 calc R . . C12 C 0.2881(7) 0.4669(2) 1.1080(3) 0.0513(15) Uani 1 1 d . . . H12A H 0.2774 0.4919 1.0653 0.077 Uiso 1 1 calc R . . H12B H 0.3466 0.4845 1.1511 0.077 Uiso 1 1 calc R . . H12C H 0.1906 0.4576 1.1202 0.077 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 Nb1 0.0231(2) 0.0173(2) 0.0254(2) 0.00023(16) 0.00979(16) -0.00187(16) Nb2 0.01810(19) 0.0171(2) 0.0323(2) 0.00058(17) 0.00731(16) -0.00128(15) Cl1 0.0277(5) 0.0354(7) 0.0316(6) -0.0018(5) 0.0037(5) -0.0055(5) Cl2 0.0475(7) 0.0185(6) 0.0449(7) -0.0020(5) 0.0242(6) -0.0061(5) Cl3 0.0342(6) 0.0286(7) 0.0389(6) 0.0022(5) 0.0016(5) 0.0047(5) Cl4 0.0679(9) 0.0372(8) 0.0364(7) 0.0071(6) 0.0282(6) 0.0091(7) Cl5 0.0290(6) 0.0353(8) 0.0833(10) -0.0066(7) 0.0246(7) -0.0015(5) Cl6 0.0471(7) 0.0430(8) 0.0280(6) -0.0074(5) 0.0084(5) -0.0065(6) Cl7 0.0276(6) 0.0401(8) 0.0508(7) 0.0048(6) 0.0156(5) 0.0066(5) Cl8 0.0418(7) 0.0331(7) 0.0636(9) 0.0058(6) 0.0327(6) -0.0047(6) Cl9 0.0254(6) 0.0322(7) 0.0711(9) -0.0023(6) -0.0109(6) 0.0009(5) Cl10 0.0606(8) 0.0193(6) 0.0454(7) 0.0052(5) 0.0005(6) -0.0066(6) Cl11 0.0373(7) 0.0424(8) 0.0601(8) -0.0121(7) 0.0187(6) 0.0092(6) P1 0.0240(5) 0.0209(6) 0.0263(6) -0.0009(5) 0.0092(5) -0.0014(5) P2 0.0284(6) 0.0203(6) 0.0366(7) 0.0008(5) 0.0172(5) -0.0009(5) P3 0.0267(6) 0.0182(6) 0.0311(6) 0.0003(5) 0.0061(5) 0.0011(5) Si1 0.0419(8) 0.0251(7) 0.0369(7) 0.0003(6) 0.0216(6) -0.0083(6) Si2 0.0369(7) 0.0204(7) 0.0350(7) -0.0019(6) 0.0159(6) 0.0009(6) Si3 0.0251(6) 0.0250(7) 0.0346(7) 0.0016(6) 0.0004(5) -0.0006(5) Si4 0.0427(8) 0.0263(8) 0.0337(7) -0.0011(6) -0.0002(6) -0.0098(6) N1 0.032(2) 0.022(2) 0.031(2) -0.0011(16) 0.0166(17) 0.0001(16) N2 0.035(2) 0.0171(19) 0.0266(19) -0.0053(15) 0.0136(16) -0.0042(16) N3 0.0241(18) 0.022(2) 0.031(2) -0.0016(16) 0.0117(16) -0.0019(15) N4 0.0220(17) 0.0186(19) 0.0244(18) -0.0024(15) 0.0054(15) 0.0007(15) N5 0.0214(17) 0.018(2) 0.0283(19) -0.0021(15) 0.0038(15) -0.0024(15) N6 0.0263(19) 0.019(2) 0.034(2) -0.0006(17) 0.0051(16) -0.0007(16) C1 0.099(5) 0.024(3) 0.097(5) -0.006(3) 0.075(4) 0.002(3) C2 0.041(3) 0.036(3) 0.054(3) -0.005(3) 0.002(3) 0.009(2) C3 0.050(3) 0.038(3) 0.049(3) -0.014(3) 0.001(3) 0.005(3) C4 0.098(5) 0.044(4) 0.072(4) -0.007(3) 0.064(4) -0.019(4) C5 0.064(4) 0.043(4) 0.040(3) 0.013(3) 0.006(3) -0.018(3) C6 0.032(3) 0.032(3) 0.061(3) 0.004(3) 0.015(3) -0.005(2) C7 0.071(4) 0.041(4) 0.063(4) 0.011(3) -0.029(3) -0.002(3) C8 0.027(3) 0.069(4) 0.054(3) -0.021(3) 0.001(2) -0.004(3) C9 0.040(3) 0.043(3) 0.028(2) 0.001(2) 0.001(2) -0.005(2) C10 0.059(4) 0.038(3) 0.064(4) -0.008(3) 0.003(3) -0.022(3) C11 0.086(5) 0.046(4) 0.041(3) 0.007(3) -0.016(3) -0.022(3) C12 0.074(4) 0.040(4) 0.040(3) -0.013(3) 0.010(3) -0.003(3) _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 Nb1 N3 2.180(4) . ? Nb1 N4 2.197(4) . ? Nb1 N2 2.223(3) . ? Nb1 N1 2.227(3) . ? Nb1 Cl3 2.3497(14) . ? Nb1 Cl1 2.3666(14) . ? Nb1 Cl2 2.3847(12) . ? Nb1 P1 2.8146(12) . ? Nb1 P2 2.8277(13) . ? Nb2 N4 1.979(4) . ? Nb2 N3 1.987(4) . ? Nb2 N5 2.153(4) . ? Nb2 N6 2.219(4) . ? Nb2 Cl9 2.3245(14) . ? Nb2 Cl8 2.3771(13) . ? Nb2 P3 2.7690(12) . ? Cl4 P2 1.9946(18) . ? Cl5 P2 1.9880(17) . ? Cl6 P1 1.9967(17) . ? Cl7 P1 1.9951(16) . ? Cl10 P3 2.0132(17) . ? Cl11 P3 2.0095(17) . ? P1 N2 1.565(4) . ? P1 N4 1.590(4) . ? P2 N1 1.571(4) . ? P2 N3 1.594(4) . ? P3 N6 1.568(4) . ? P3 N5 1.580(4) . ? Si1 N2 1.786(4) . ? Si1 C6 1.835(5) . ? Si1 C4 1.861(6) . ? Si1 C5 1.865(6) . ? Si2 N1 1.793(4) . ? Si2 C2 1.846(5) . ? Si2 C3 1.854(5) . ? Si2 C1 1.873(5) . ? Si3 N5 1.785(4) . ? Si3 C7 1.849(6) . ? Si3 C8 1.850(5) . ? Si3 C9 1.855(5) . ? Si4 N6 1.786(4) . ? Si4 C11 1.842(6) . ? Si4 C10 1.854(6) . ? Si4 C12 1.870(6) . ? 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 N3 Nb1 N4 67.76(13) . . ? N3 Nb1 N2 135.43(13) . . ? N4 Nb1 N2 67.91(13) . . ? N3 Nb1 N1 67.64(14) . . ? N4 Nb1 N1 135.15(13) . . ? N2 Nb1 N1 156.91(14) . . ? N3 Nb1 Cl3 93.63(10) . . ? N4 Nb1 Cl3 89.30(9) . . ? N2 Nb1 Cl3 90.23(10) . . ? N1 Nb1 Cl3 89.01(10) . . ? N3 Nb1 Cl1 88.83(10) . . ? N4 Nb1 Cl1 90.68(9) . . ? N2 Nb1 Cl1 87.29(10) . . ? N1 Nb1 Cl1 92.89(10) . . ? Cl3 Nb1 Cl1 177.33(4) . . ? N3 Nb1 Cl2 145.37(10) . . ? N4 Nb1 Cl2 146.81(9) . . ? N2 Nb1 Cl2 78.92(10) . . ? N1 Nb1 Cl2 78.00(10) . . ? Cl3 Nb1 Cl2 89.90(5) . . ? Cl1 Nb1 Cl2 88.67(5) . . ? N3 Nb1 P1 101.86(10) . . ? N4 Nb1 P1 34.25(9) . . ? N2 Nb1 P1 33.66(10) . . ? N1 Nb1 P1 169.39(10) . . ? Cl3 Nb1 P1 90.23(4) . . ? Cl1 Nb1 P1 88.25(4) . . ? Cl2 Nb1 P1 112.58(4) . . ? N3 Nb1 P2 34.11(10) . . ? N4 Nb1 P2 101.56(9) . . ? N2 Nb1 P2 169.47(10) . . ? N1 Nb1 P2 33.62(10) . . ? Cl3 Nb1 P2 89.68(4) . . ? Cl1 Nb1 P2 92.94(4) . . ? Cl2 Nb1 P2 111.61(4) . . ? P1 Nb1 P2 135.81(4) . . ? N4 Nb2 N3 75.95(14) . . ? N4 Nb2 N5 93.89(14) . . ? N3 Nb2 N5 111.22(14) . . ? N4 Nb2 N6 98.02(14) . . ? N3 Nb2 N6 173.96(14) . . ? N5 Nb2 N6 69.03(13) . . ? N4 Nb2 Cl9 95.46(11) . . ? N3 Nb2 Cl9 96.68(11) . . ? N5 Nb2 Cl9 151.97(10) . . ? N6 Nb2 Cl9 83.52(10) . . ? N4 Nb2 Cl8 163.33(11) . . ? N3 Nb2 Cl8 88.32(11) . . ? N5 Nb2 Cl8 86.59(10) . . ? N6 Nb2 Cl8 97.71(10) . . ? Cl9 Nb2 Cl8 91.78(5) . . ? N4 Nb2 P3 99.26(10) . . ? N3 Nb2 P3 145.82(11) . . ? N5 Nb2 P3 34.68(10) . . ? N6 Nb2 P3 34.46(10) . . ? Cl9 Nb2 P3 117.49(4) . . ? Cl8 Nb2 P3 90.62(4) . . ? N2 P1 N4 103.01(19) . . ? N2 P1 Cl7 115.09(15) . . ? N4 P1 Cl7 110.91(14) . . ? N2 P1 Cl6 115.07(16) . . ? N4 P1 Cl6 110.87(14) . . ? Cl7 P1 Cl6 102.13(8) . . ? N2 P1 Nb1 51.95(13) . . ? N4 P1 Nb1 51.07(13) . . ? Cl7 P1 Nb1 127.88(7) . . ? Cl6 P1 Nb1 129.72(6) . . ? N1 P2 N3 101.65(19) . . ? N1 P2 Cl5 115.12(16) . . ? N3 P2 Cl5 111.11(15) . . ? N1 P2 Cl4 114.86(16) . . ? N3 P2 Cl4 111.79(15) . . ? Cl5 P2 Cl4 102.64(8) . . ? N1 P2 Nb1 51.72(13) . . ? N3 P2 Nb1 50.10(13) . . ? Cl5 P2 Nb1 124.89(7) . . ? Cl4 P2 Nb1 132.22(7) . . ? N6 P3 N5 103.8(2) . . ? N6 P3 Cl11 115.00(15) . . ? N5 P3 Cl11 112.72(14) . . ? N6 P3 Cl10 112.12(15) . . ? N5 P3 Cl10 113.22(15) . . ? Cl11 P3 Cl10 100.40(8) . . ? N6 P3 Nb2 53.18(14) . . ? N5 P3 Nb2 50.80(13) . . ? Cl11 P3 Nb2 134.65(7) . . ? Cl10 P3 Nb2 124.90(7) . . ? N2 Si1 C6 109.2(2) . . ? N2 Si1 C4 107.8(2) . . ? C6 Si1 C4 106.4(3) . . ? N2 Si1 C5 108.4(2) . . ? C6 Si1 C5 116.4(3) . . ? C4 Si1 C5 108.4(3) . . ? N1 Si2 C2 110.4(2) . . ? N1 Si2 C3 109.2(2) . . ? C2 Si2 C3 113.9(3) . . ? N1 Si2 C1 108.4(2) . . ? C2 Si2 C1 108.1(3) . . ? C3 Si2 C1 106.6(3) . . ? N5 Si3 C7 109.8(2) . . ? N5 Si3 C8 106.8(2) . . ? C7 Si3 C8 110.1(3) . . ? N5 Si3 C9 107.9(2) . . ? C7 Si3 C9 109.0(3) . . ? C8 Si3 C9 113.2(3) . . ? N6 Si4 C11 109.0(2) . . ? N6 Si4 C10 107.7(2) . . ? C11 Si4 C10 113.8(3) . . ? N6 Si4 C12 109.9(2) . . ? C11 Si4 C12 107.4(3) . . ? C10 Si4 C12 109.0(3) . . ? P2 N1 Si2 127.3(2) . . ? P2 N1 Nb1 94.67(18) . . ? Si2 N1 Nb1 137.8(2) . . ? P1 N2 Si1 129.5(2) . . ? P1 N2 Nb1 94.39(17) . . ? Si1 N2 Nb1 135.92(19) . . ? P2 N3 Nb2 152.0(2) . . ? P2 N3 Nb1 95.79(18) . . ? Nb2 N3 Nb1 107.90(15) . . ? P1 N4 Nb2 157.7(2) . . ? P1 N4 Nb1 94.67(17) . . ? Nb2 N4 Nb1 107.56(15) . . ? P3 N5 Si3 129.7(2) . . ? P3 N5 Nb2 94.52(16) . . ? Si3 N5 Nb2 135.1(2) . . ? P3 N6 Si4 128.9(2) . . ? P3 N6 Nb2 92.36(17) . . ? Si4 N6 Nb2 136.4(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.661 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.123