# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Anti\nolo, Antonio' _publ_contact_author_email antonio.antinolo@uclm.es _publ_section_title ; LEWIS BASE CHARACTER OF THE PHOSPHORUS ATOM IN PHOSPHIDO-NIOBOCENE COMPLEXES. SYNTHESIS OF NEW EARLY-EARLY HOMO- AND HETEROBIMETALLIC ENTITIES. ; loop_ _publ_author_name A.Antinolo R.Reguillo S.Garcia-Yuste A.Otero I.Lopez-Solera # Attachment '- niobium 9 and 12.cif' data_9 _database_code_depnum_ccdc_archive 'CCDC 784737' #TrackingRef '- niobium 9 and 12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H37 Cl6 Nb O P Si2 Ta' _chemical_formula_weight 975.30 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' 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' Ta Ta -0.7052 6.5227 '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' 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' _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 10.515(3) _cell_length_b 12.939(3) _cell_length_c 13.888(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.035(6) _cell_angle_gamma 90.00 _cell_volume 1882.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prismatic _exptl_crystal_colour Red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 3.764 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.313282 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6395 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.1539 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 19.53 _reflns_number_total 3206 _reflns_number_gt 2131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 3206 _refine_ls_number_parameters 379 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1283 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 2.113 _refine_ls_shift/su_mean 0.113 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 Ta1 Ta 0.25216(12) 0.24973(9) 0.20332(10) 0.0631(5) Uani 1 1 d . . . Nb1 Nb -0.0156(3) 0.70655(19) 0.2863(2) 0.0552(9) Uani 1 1 d . . . Cl3 Cl 0.4636(7) 0.2239(8) 0.2654(6) 0.086(3) Uani 1 1 d . . . Cl6 Cl 0.0425(8) 0.2759(7) 0.1358(7) 0.086(3) Uani 1 1 d . . . Cl2 Cl 0.3203(12) 0.3769(9) 0.1025(9) 0.097(4) Uani 1 1 d . . . Cl4 Cl 0.2787(12) 0.1204(8) 0.0905(10) 0.103(5) Uani 1 1 d . . . Cl5 Cl 0.1807(14) 0.1301(9) 0.3085(9) 0.110(5) Uani 1 1 d . . . Cl1 Cl 0.2274(12) 0.3763(8) 0.3242(9) 0.092(4) Uani 1 1 d . . . P1 P 0.2156(9) 0.7018(7) 0.2418(7) 0.067(3) Uani 1 1 d . . . H1 H 0.27(2) 0.598(19) 0.240(19) 0.080 Uiso 1 1 d . . . C25 C -0.207(4) 0.662(2) 0.195(3) 0.074(12) Uani 1 1 d . . . H25 H -0.2810 0.6970 0.2054 0.088 Uiso 1 1 calc R . . C14 C -0.060(3) 0.791(2) 0.431(3) 0.053(10) Uani 1 1 d . . . H14 H -0.0765 0.7529 0.4854 0.063 Uiso 1 1 calc R . . C15 C -0.152(3) 0.826(2) 0.362(3) 0.059(10) Uani 1 1 d . . . H15 H -0.2387 0.8126 0.3601 0.071 Uiso 1 1 calc R . . C3 C -0.205(4) 1.097(2) 0.272(3) 0.110(18) Uani 1 1 d . . . H3A H -0.2603 1.1431 0.2345 0.132 Uiso 1 1 calc R . . H3B H -0.1234 1.1289 0.2872 0.132 Uiso 1 1 calc R . . H3C H -0.2420 1.0808 0.3315 0.132 Uiso 1 1 calc R . . C2 C -0.342(3) 0.915(2) 0.159(2) 0.089(14) Uani 1 1 d . . . H2A H -0.3685 0.9396 0.0948 0.107 Uiso 1 1 calc R . . H2B H -0.4042 0.9344 0.2019 0.107 Uiso 1 1 calc R . . H2C H -0.3355 0.8406 0.1572 0.107 Uiso 1 1 calc R . . C11 C -0.091(4) 0.888(2) 0.292(3) 0.061(11) Uani 1 1 d . . . C12 C 0.043(3) 0.880(2) 0.323(2) 0.048(9) Uani 1 1 d . . . H12 H 0.1083 0.9088 0.2910 0.057 Uiso 1 1 calc R . . Si1 Si -0.1840(10) 0.9713(9) 0.2007(8) 0.072(3) Uani 1 1 d . . . Si2 Si -0.2619(9) 0.4974(7) 0.3305(8) 0.065(3) Uani 1 1 d . . . C6 C -0.427(3) 0.509(2) 0.275(3) 0.095(13) Uani 1 1 d . . . H6A H -0.4846 0.4781 0.3164 0.114 Uiso 1 1 calc R . . H6B H -0.4344 0.4743 0.2135 0.114 Uiso 1 1 calc R . . H6C H -0.4482 0.5808 0.2655 0.114 Uiso 1 1 calc R . . O1 O 0.088(3) 0.551(2) 0.460(2) 0.114(11) Uani 1 1 d . . . C1 C 0.056(4) 0.605(3) 0.397(3) 0.069(12) Uani 1 1 d . . . C5 C -0.198(4) 0.365(2) 0.333(3) 0.087(14) Uani 1 1 d . . . H5A H -0.1099 0.3663 0.3566 0.105 Uiso 1 1 calc R . . H5B H -0.2071 0.3370 0.2688 0.105 Uiso 1 1 calc R . . H5C H -0.2452 0.3233 0.3747 0.105 Uiso 1 1 calc R . . C23 C -0.021(5) 0.612(4) 0.135(3) 0.099(17) Uani 1 1 d . . . H23 H 0.0466 0.6106 0.0965 0.119 Uiso 1 1 calc R . . C31 C 0.259(2) 0.741(3) 0.124(2) 0.060(8) Uani 1 1 d D . . C36 C 0.357(3) 0.686(2) 0.082(2) 0.060(10) Uani 1 1 d D . . H36 H 0.3965 0.6298 0.1137 0.072 Uiso 1 1 calc R . . C7 C -0.256(3) 0.552(2) 0.452(2) 0.063(9) Uani 1 1 d . . . H7A H -0.2577 0.6260 0.4476 0.076 Uiso 1 1 calc R . . H7B H -0.1795 0.5300 0.4884 0.076 Uiso 1 1 calc R . . H7C H -0.3291 0.5286 0.4829 0.076 Uiso 1 1 calc R . . C32 C 0.204(3) 0.826(2) 0.078(2) 0.083(12) Uani 1 1 d D . . H32 H 0.1401 0.8614 0.1058 0.099 Uiso 1 1 calc R . . C4 C -0.089(3) 0.996(2) 0.092(2) 0.084(13) Uani 1 1 d . . . H4A H -0.0984 0.9378 0.0492 0.101 Uiso 1 1 calc R . . H4B H -0.0005 1.0046 0.1141 0.101 Uiso 1 1 calc R . . H4C H -0.1204 1.0570 0.0594 0.101 Uiso 1 1 calc R . . C24 C -0.124(5) 0.688(3) 0.127(2) 0.094(14) Uani 1 1 d . . . H24 H -0.1326 0.7434 0.0844 0.113 Uiso 1 1 calc R . . C35 C 0.394(3) 0.720(3) -0.009(3) 0.074(12) Uani 1 1 d D . . H35 H 0.4543 0.6826 -0.0392 0.088 Uiso 1 1 calc R . . C34 C 0.339(4) 0.809(3) -0.053(4) 0.114(17) Uani 1 1 d D . . H34 H 0.3677 0.8324 -0.1102 0.137 Uiso 1 1 calc R . . C22 C -0.040(4) 0.542(3) 0.211(3) 0.083(13) Uani 1 1 d . . . H22 H 0.0135 0.4875 0.2326 0.099 Uiso 1 1 calc R . . C33 C 0.244(4) 0.862(3) -0.013(3) 0.098(15) Uani 1 1 d D . . H33 H 0.2056 0.9193 -0.0440 0.118 Uiso 1 1 calc R . . C21 C -0.160(4) 0.571(3) 0.246(3) 0.067(12) Uani 1 1 d . . . C13 C 0.060(4) 0.821(2) 0.409(2) 0.070(12) Uani 1 1 d . . . H13 H 0.1368 0.8061 0.4443 0.084 Uiso 1 1 calc R . . C45 C 0.463(6) 0.762(6) 0.470(5) 0.17(3) Uani 1 1 d D . . H45 H 0.4837 0.7292 0.5290 0.202 Uiso 1 1 calc R . . C41 C 0.336(3) 0.765(4) 0.323(3) 0.081(15) Uani 1 1 d D . . C42 C 0.380(3) 0.861(3) 0.314(3) 0.099(15) Uani 1 1 d D . . H42 H 0.3523 0.9004 0.2596 0.119 Uiso 1 1 calc R . . C46 C 0.376(5) 0.708(4) 0.406(4) 0.13(2) Uani 1 1 d D . . H46 H 0.3477 0.6409 0.4180 0.162 Uiso 1 1 calc R . . C43 C 0.469(3) 0.904(4) 0.384(4) 0.12(2) Uani 1 1 d D . . H43 H 0.4956 0.9726 0.3778 0.146 Uiso 1 1 calc R . . C44 C 0.519(5) 0.847(7) 0.463(4) 0.22(5) Uani 1 1 d D . . H44 H 0.5860 0.8690 0.5053 0.265 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 Ta1 0.0618(9) 0.0651(9) 0.0613(9) -0.0014(10) -0.0010(7) 0.0019(10) Nb1 0.063(2) 0.053(2) 0.052(2) -0.0028(15) 0.0129(17) -0.0035(16) Cl3 0.055(5) 0.124(10) 0.074(6) -0.018(7) -0.019(5) 0.025(6) Cl6 0.050(5) 0.102(9) 0.102(7) -0.016(7) -0.014(5) 0.004(6) Cl2 0.090(9) 0.115(9) 0.084(9) 0.028(7) -0.010(7) -0.018(7) Cl4 0.102(10) 0.095(8) 0.110(11) -0.041(8) 0.001(8) 0.019(7) Cl5 0.152(13) 0.092(9) 0.086(10) 0.031(7) 0.012(9) -0.024(8) Cl1 0.097(9) 0.089(8) 0.087(10) -0.035(7) -0.001(7) 0.025(7) P1 0.076(7) 0.070(6) 0.057(7) 0.003(5) 0.019(6) 0.007(6) C25 0.11(3) 0.07(3) 0.03(3) 0.02(2) -0.05(3) -0.01(2) C14 0.03(2) 0.05(2) 0.08(3) -0.007(17) 0.03(2) -0.013(17) C15 0.04(2) 0.07(2) 0.07(3) -0.04(2) -0.03(2) 0.00(2) C3 0.12(3) 0.04(2) 0.15(5) -0.04(2) -0.10(3) 0.02(2) C2 0.07(3) 0.12(3) 0.08(3) 0.08(2) 0.04(2) 0.04(2) C11 0.10(4) 0.03(2) 0.06(3) -0.002(18) 0.03(3) 0.01(2) C12 0.01(2) 0.06(2) 0.08(3) 0.00(2) 0.016(18) -0.009(15) Si1 0.051(7) 0.085(8) 0.081(9) 0.014(7) 0.009(7) 0.008(6) Si2 0.058(7) 0.066(7) 0.072(8) -0.002(5) 0.002(6) -0.007(5) C6 0.10(3) 0.04(2) 0.13(4) 0.00(2) -0.03(3) -0.01(2) O1 0.15(3) 0.09(2) 0.10(3) 0.016(18) 0.00(2) 0.025(19) C1 0.09(3) 0.06(3) 0.06(3) 0.00(2) 0.03(3) -0.01(2) C5 0.10(3) 0.06(2) 0.10(3) 0.02(2) -0.03(3) 0.02(2) C23 0.17(5) 0.08(3) 0.05(3) -0.04(3) 0.04(3) -0.05(4) C31 0.036(18) 0.08(3) 0.06(2) -0.02(3) -0.007(16) -0.01(2) C36 0.08(3) 0.05(2) 0.05(3) 0.00(2) 0.02(2) 0.04(2) C7 0.05(2) 0.07(2) 0.08(2) 0.030(18) 0.045(19) -0.002(17) C32 0.11(3) 0.07(3) 0.07(3) 0.03(2) 0.02(3) -0.01(2) C4 0.13(3) 0.06(2) 0.07(3) 0.006(19) 0.06(3) -0.01(2) C24 0.19(5) 0.09(3) 0.01(2) 0.00(2) -0.01(3) -0.01(3) C35 0.04(2) 0.10(4) 0.08(3) -0.01(2) 0.01(2) 0.01(2) C34 0.06(3) 0.11(4) 0.16(5) 0.03(4) -0.06(3) 0.00(3) C22 0.10(4) 0.05(2) 0.10(4) -0.02(3) 0.03(3) 0.01(2) C33 0.14(5) 0.06(3) 0.08(4) 0.03(2) -0.05(3) -0.03(3) C21 0.09(3) 0.05(3) 0.06(3) 0.01(2) 0.00(3) -0.02(2) C13 0.13(4) 0.05(2) 0.03(2) 0.006(18) 0.00(2) 0.00(2) C45 0.11(5) 0.30(9) 0.10(5) -0.05(6) 0.08(4) 0.07(6) C41 0.023(19) 0.14(4) 0.08(3) 0.05(4) 0.014(19) 0.03(3) C42 0.13(5) 0.11(3) 0.06(3) -0.06(3) 0.02(3) 0.00(3) C46 0.11(4) 0.13(4) 0.17(6) -0.05(5) 0.01(4) 0.05(3) C43 0.04(3) 0.22(6) 0.10(4) -0.13(5) 0.00(3) -0.03(3) C44 0.09(5) 0.49(13) 0.07(5) -0.03(6) -0.06(4) 0.13(7) _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 Ta1 Cl5 2.300(11) . ? Ta1 Cl2 2.314(11) . ? Ta1 Cl4 2.326(11) . ? Ta1 Cl3 2.337(7) . ? Ta1 Cl6 2.343(8) . ? Ta1 Cl1 2.376(11) . ? Nb1 C1 2.11(4) . ? Nb1 C13 2.35(3) . ? Nb1 C21 2.35(4) . ? Nb1 C25 2.35(3) . ? Nb1 C12 2.37(3) . ? Nb1 C14 2.37(3) . ? Nb1 C22 2.38(3) . ? Nb1 C15 2.41(3) . ? Nb1 C24 2.41(3) . ? Nb1 C23 2.42(3) . ? Nb1 C11 2.48(3) . ? Nb1 P1 2.562(9) . ? P1 C31 1.81(3) . ? P1 C41 1.81(4) . ? P1 H1 1.4(3) . ? C25 C24 1.37(4) . ? C25 C21 1.43(4) . ? C25 H25 0.9300 . ? C14 C15 1.38(4) . ? C14 C13 1.38(4) . ? C14 H14 0.9300 . ? C15 C11 1.44(4) . ? C15 H15 0.9300 . ? C3 Si1 1.93(3) . ? C3 H3A 0.9601 . ? C3 H3B 0.9601 . ? C3 H3C 0.9601 . ? C2 Si1 1.87(3) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C11 C12 1.44(4) . ? C11 Si1 1.87(4) . ? C12 C13 1.42(4) . ? C12 H12 0.9300 . ? Si1 C4 1.90(3) . ? Si2 C7 1.82(3) . ? Si2 C5 1.84(3) . ? Si2 C6 1.84(3) . ? Si2 C21 1.92(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? O1 C1 1.15(4) . ? C5 H5A 0.9601 . ? C5 H5B 0.9601 . ? C5 H5C 0.9601 . ? C23 C22 1.42(5) . ? C23 C24 1.46(5) . ? C23 H23 0.9300 . ? C31 C32 1.38(4) . ? C31 C36 1.41(4) . ? C36 C35 1.42(4) . ? C36 H36 0.9300 . ? C7 H7A 0.9601 . ? C7 H7B 0.9601 . ? C7 H7C 0.9601 . ? C32 C33 1.44(5) . ? C32 H32 0.9300 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C24 H24 0.9300 . ? C35 C34 1.41(5) . ? C35 H35 0.9300 . ? C34 C33 1.37(5) . ? C34 H34 0.9300 . ? C22 C21 1.45(5) . ? C22 H22 0.9300 . ? C33 H33 0.9300 . ? C13 H13 0.9300 . ? C45 C44 1.25(10) . ? C45 C46 1.41(7) . ? C45 H45 0.9300 . ? C41 C42 1.34(5) . ? C41 C46 1.41(6) . ? C42 C43 1.41(5) . ? C42 H42 0.9300 . ? C46 H46 0.9300 . ? C43 C44 1.38(8) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? 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 Cl5 Ta1 Cl2 177.0(5) . . ? Cl5 Ta1 Cl4 90.5(5) . . ? Cl2 Ta1 Cl4 92.4(3) . . ? Cl5 Ta1 Cl3 91.3(4) . . ? Cl2 Ta1 Cl3 89.4(4) . . ? Cl4 Ta1 Cl3 88.8(4) . . ? Cl5 Ta1 Cl6 90.2(4) . . ? Cl2 Ta1 Cl6 89.2(4) . . ? Cl4 Ta1 Cl6 89.9(4) . . ? Cl3 Ta1 Cl6 178.0(3) . . ? Cl5 Ta1 Cl1 87.3(3) . . ? Cl2 Ta1 Cl1 89.8(5) . . ? Cl4 Ta1 Cl1 177.4(5) . . ? Cl3 Ta1 Cl1 89.9(4) . . ? Cl6 Ta1 Cl1 91.5(4) . . ? C1 Nb1 C13 77.8(13) . . ? C1 Nb1 C21 83.7(14) . . ? C13 Nb1 C21 144.5(13) . . ? C1 Nb1 C25 118.2(14) . . ? C13 Nb1 C25 140.0(14) . . ? C21 Nb1 C25 35.5(11) . . ? C1 Nb1 C12 111.4(14) . . ? C13 Nb1 C12 34.9(10) . . ? C21 Nb1 C12 154.9(13) . . ? C25 Nb1 C12 122.8(11) . . ? C1 Nb1 C14 75.7(12) . . ? C13 Nb1 C14 33.9(10) . . ? C21 Nb1 C14 112.1(12) . . ? C25 Nb1 C14 110.6(13) . . ? C12 Nb1 C14 56.4(10) . . ? C1 Nb1 C22 77.4(15) . . ? C13 Nb1 C22 154.7(14) . . ? C21 Nb1 C22 35.5(11) . . ? C25 Nb1 C22 59.2(13) . . ? C12 Nb1 C22 163.4(13) . . ? C14 Nb1 C22 140.0(13) . . ? C1 Nb1 C15 105.7(13) . . ? C13 Nb1 C15 56.8(11) . . ? C21 Nb1 C15 100.8(13) . . ? C25 Nb1 C15 83.3(11) . . ? C12 Nb1 C15 56.7(9) . . ? C14 Nb1 C15 33.6(9) . . ? C22 Nb1 C15 136.3(13) . . ? C1 Nb1 C24 135.7(14) . . ? C13 Nb1 C24 146.4(12) . . ? C21 Nb1 C24 57.5(12) . . ? C25 Nb1 C24 33.5(11) . . ? C12 Nb1 C24 112.6(13) . . ? C14 Nb1 C24 135.4(16) . . ? C22 Nb1 C24 58.8(13) . . ? C15 Nb1 C24 102.2(15) . . ? C1 Nb1 C23 107.4(17) . . ? C13 Nb1 C23 158.3(14) . . ? C21 Nb1 C23 56.8(13) . . ? C25 Nb1 C23 56.8(14) . . ? C12 Nb1 C23 130.4(14) . . ? C14 Nb1 C23 167.2(14) . . ? C22 Nb1 C23 34.3(11) . . ? C15 Nb1 C23 136.8(16) . . ? C24 Nb1 C23 35.1(12) . . ? C1 Nb1 C11 131.3(13) . . ? C13 Nb1 C11 57.8(12) . . ? C21 Nb1 C11 120.6(14) . . ? C25 Nb1 C11 89.4(12) . . ? C12 Nb1 C11 34.5(10) . . ? C14 Nb1 C11 56.6(11) . . ? C22 Nb1 C11 147.0(14) . . ? C15 Nb1 C11 34.3(10) . . ? C24 Nb1 C11 89.7(14) . . ? C23 Nb1 C11 121.3(17) . . ? C1 Nb1 P1 83.0(10) . . ? C13 Nb1 P1 85.7(11) . . ? C21 Nb1 P1 122.0(11) . . ? C25 Nb1 P1 130.3(11) . . ? C12 Nb1 P1 80.9(7) . . ? C14 Nb1 P1 118.5(9) . . ? C22 Nb1 P1 86.5(11) . . ? C15 Nb1 P1 137.1(8) . . ? C24 Nb1 P1 99.2(13) . . ? C23 Nb1 P1 74.4(12) . . ? C11 Nb1 P1 110.1(10) . . ? C31 P1 C41 102.6(15) . . ? C31 P1 Nb1 122.3(10) . . ? C41 P1 Nb1 117.5(9) . . ? C31 P1 H1 97(10) . . ? C41 P1 H1 101(10) . . ? Nb1 P1 H1 113(10) . . ? C24 C25 C21 109(4) . . ? C24 C25 Nb1 76(2) . . ? C21 C25 Nb1 72(2) . . ? C24 C25 H25 125.2 . . ? C21 C25 H25 125.4 . . ? Nb1 C25 H25 118.7 . . ? C15 C14 C13 110(3) . . ? C15 C14 Nb1 75(2) . . ? C13 C14 Nb1 72.0(19) . . ? C15 C14 H14 124.9 . . ? C13 C14 H14 124.8 . . ? Nb1 C14 H14 120.4 . . ? C14 C15 C11 109(3) . . ? C14 C15 Nb1 71.8(19) . . ? C11 C15 Nb1 75.5(17) . . ? C14 C15 H15 125.1 . . ? C11 C15 H15 125.7 . . ? Nb1 C15 H15 119.0 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.4 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.4 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.4 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C15 C11 C12 104(3) . . ? C15 C11 Si1 123(3) . . ? C12 C11 Si1 133(3) . . ? C15 C11 Nb1 70.2(16) . . ? C12 C11 Nb1 68.5(16) . . ? Si1 C11 Nb1 132.4(17) . . ? C13 C12 C11 110(3) . . ? C13 C12 Nb1 71.7(17) . . ? C11 C12 Nb1 77.0(16) . . ? C13 C12 H12 125.3 . . ? C11 C12 H12 125.0 . . ? Nb1 C12 H12 118.2 . . ? C2 Si1 C11 112.5(16) . . ? C2 Si1 C4 109.4(15) . . ? C11 Si1 C4 110.6(16) . . ? C2 Si1 C3 110.7(16) . . ? C11 Si1 C3 102.3(16) . . ? C4 Si1 C3 111.1(18) . . ? C7 Si2 C5 111.2(16) . . ? C7 Si2 C6 108.0(16) . . ? C5 Si2 C6 114.3(15) . . ? C7 Si2 C21 113.5(15) . . ? C5 Si2 C21 104.8(18) . . ? C6 Si2 C21 105.1(17) . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.3 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.6 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C1 Nb1 176(4) . . ? Si2 C5 H5A 109.6 . . ? Si2 C5 H5B 109.4 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C22 C23 C24 110(4) . . ? C22 C23 Nb1 71(2) . . ? C24 C23 Nb1 71.9(19) . . ? C22 C23 H23 125.1 . . ? C24 C23 H23 125.0 . . ? Nb1 C23 H23 123.0 . . ? C32 C31 C36 120(3) . . ? C32 C31 P1 121(3) . . ? C36 C31 P1 119(3) . . ? C31 C36 C35 118(3) . . ? C31 C36 H36 121.0 . . ? C35 C36 H36 120.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.3 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.6 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C31 C32 C33 122(4) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.0 . . ? Si1 C4 H4A 109.4 . . ? Si1 C4 H4B 109.3 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.7 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C25 C24 C23 107(3) . . ? C25 C24 Nb1 71.0(18) . . ? C23 C24 Nb1 73(2) . . ? C25 C24 H24 126.6 . . ? C23 C24 H24 126.6 . . ? Nb1 C24 H24 121.4 . . ? C34 C35 C36 120(4) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 119.1 . . ? C33 C34 C35 122(5) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.0 . . ? C23 C22 C21 105(4) . . ? C23 C22 Nb1 74(2) . . ? C21 C22 Nb1 71(2) . . ? C23 C22 H22 127.6 . . ? C21 C22 H22 127.5 . . ? Nb1 C22 H22 119.5 . . ? C34 C33 C32 118(4) . . ? C34 C33 H33 121.5 . . ? C32 C33 H33 120.6 . . ? C25 C21 C22 109(3) . . ? C25 C21 Si2 122(4) . . ? C22 C21 Si2 129(3) . . ? C25 C21 Nb1 72.5(18) . . ? C22 C21 Nb1 74(2) . . ? Si2 C21 Nb1 127.6(18) . . ? C14 C13 C12 107(3) . . ? C14 C13 Nb1 74(2) . . ? C12 C13 Nb1 73.4(18) . . ? C14 C13 H13 126.7 . . ? C12 C13 H13 126.4 . . ? Nb1 C13 H13 117.7 . . ? C44 C45 C46 132(8) . . ? C44 C45 H45 115.7 . . ? C46 C45 H45 112.3 . . ? C42 C41 C46 119(5) . . ? C42 C41 P1 126(3) . . ? C46 C41 P1 114(5) . . ? C41 C42 C43 121(5) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.1 . . ? C45 C46 C41 112(6) . . ? C45 C46 H46 125.1 . . ? C41 C46 H46 122.4 . . ? C44 C43 C42 121(6) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 118.4 . . ? C45 C44 C43 113(7) . . ? C45 C44 H44 124.6 . . ? C43 C44 H44 122.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 19.53 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.787 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.121 #======================================================================= data_12 _database_code_depnum_ccdc_archive 'CCDC 784738' #TrackingRef '- niobium 9 and 12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H53 Cl5 N Nb2 O2 P Si2' _chemical_formula_weight 1042.06 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' O O 0.0106 0.0060 '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 12.0250(18) _cell_length_b 12.1588(18) _cell_length_c 15.964(2) _cell_angle_alpha 90.091(2) _cell_angle_beta 93.465(2) _cell_angle_gamma 90.778(3) _cell_volume 2329.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prismatic _exptl_crystal_colour Red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.746808 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10199 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 21.29 _reflns_number_total 5041 _reflns_number_gt 3899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.5549P] 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 5041 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2156 _refine_ls_wR_factor_gt 0.2044 _refine_ls_goodness_of_fit_ref 1.314 _refine_ls_restrained_S_all 1.314 _refine_ls_shift/su_max 0.029 _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 0.55447(8) 0.34388(8) 0.27953(6) 0.0362(4) Uani 1 1 d . . . Nb2 Nb 0.77825(9) 0.81337(10) 0.15043(7) 0.0544(4) Uani 1 1 d . . . Cl1 Cl 0.5052(4) 0.0433(4) 0.3476(3) 0.1186(16) Uani 1 1 d . . . Cl2 Cl 0.5938(3) 0.8541(4) 0.1864(2) 0.1039(16) Uani 1 1 d . . . Cl3 Cl 0.8446(3) 0.9619(3) 0.23867(18) 0.0634(9) Uani 1 1 d . . . Cl4 Cl 0.9531(3) 0.8098(3) 0.0900(2) 0.0637(9) Uani 1 1 d . . . Cl5 Cl 0.7020(3) 0.6965(3) 0.0382(2) 0.0903(13) Uani 1 1 d . . . Si1 Si 0.3405(3) 0.5745(3) 0.18305(19) 0.0428(8) Uani 1 1 d . . . Si2 Si 0.8611(3) 0.3571(3) 0.2177(3) 0.0636(11) Uani 1 1 d . . . P1 P 0.4274(2) 0.1889(2) 0.32541(17) 0.0426(8) Uani 1 1 d . . . O1 O 0.8019(9) 0.7132(8) 0.2224(6) 0.091(3) Uani 1 1 d . . . O2 O 0.7454(6) 0.9590(6) 0.0518(4) 0.0463(19) Uani 1 1 d . . . N1 N 0.7286(8) 0.2654(8) 0.4345(6) 0.047(2) Uani 1 1 d . . . C1 C 0.6667(10) 0.2885(8) 0.3782(8) 0.045(3) Uani 1 1 d . . . C2 C 0.2079(10) 0.4927(12) 0.1712(10) 0.088(5) Uani 1 1 d . . . H2A H 0.2190 0.4286 0.1376 0.131 Uiso 1 1 calc R . . H2B H 0.1506 0.5368 0.1443 0.131 Uiso 1 1 calc R . . H2C H 0.1859 0.4705 0.2255 0.131 Uiso 1 1 calc R . . C3 C 0.3125(12) 0.7119(11) 0.2317(8) 0.072(4) Uani 1 1 d . . . H3A H 0.2774 0.7008 0.2835 0.108 Uiso 1 1 calc R . . H3B H 0.2643 0.7535 0.1940 0.108 Uiso 1 1 calc R . . H3C H 0.3816 0.7514 0.2425 0.108 Uiso 1 1 calc R . . C4 C 0.4055(11) 0.5905(11) 0.0824(7) 0.065(4) Uani 1 1 d . . . H4A H 0.4807 0.6169 0.0924 0.098 Uiso 1 1 calc R . . H4B H 0.3640 0.6422 0.0480 0.098 Uiso 1 1 calc R . . H4C H 0.4057 0.5207 0.0542 0.098 Uiso 1 1 calc R . . C5 C 0.8783(13) 0.4840(13) 0.2834(15) 0.149(9) Uani 1 1 d . . . H5A H 0.8356 0.5423 0.2573 0.223 Uiso 1 1 calc R . . H5B H 0.9555 0.5054 0.2885 0.223 Uiso 1 1 calc R . . H5C H 0.8524 0.4697 0.3381 0.223 Uiso 1 1 calc R . . C6 C 0.9124(14) 0.375(2) 0.1147(11) 0.160(11) Uani 1 1 d . . . H6A H 0.9380 0.3063 0.0946 0.240 Uiso 1 1 calc R . . H6B H 0.9730 0.4278 0.1176 0.240 Uiso 1 1 calc R . . H6C H 0.8536 0.4018 0.0770 0.240 Uiso 1 1 calc R . . C7 C 0.9373(11) 0.2482(12) 0.2758(10) 0.088(5) Uani 1 1 d . . . H7A H 0.9100 0.2415 0.3309 0.132 Uiso 1 1 calc R . . H7B H 1.0154 0.2666 0.2805 0.132 Uiso 1 1 calc R . . H7C H 0.9264 0.1796 0.2464 0.132 Uiso 1 1 calc R . . C11 C 0.4390(8) 0.5083(8) 0.2642(6) 0.034(3) Uani 1 1 d . . . C12 C 0.4060(9) 0.4474(9) 0.3336(6) 0.040(3) Uani 1 1 d . . . H12 H 0.3306 0.4196 0.3416 0.048 Uiso 1 1 calc R . . C13 C 0.4982(11) 0.4428(9) 0.3937(7) 0.051(3) Uani 1 1 d . . . H13 H 0.4949 0.4138 0.4508 0.061 Uiso 1 1 calc R . . C14 C 0.5887(11) 0.4994(9) 0.3636(8) 0.055(3) Uani 1 1 d . . . H14 H 0.6586 0.5183 0.3954 0.066 Uiso 1 1 calc R . . C15 C 0.5527(9) 0.5399(9) 0.2823(7) 0.046(3) Uani 1 1 d . . . H15 H 0.5965 0.5883 0.2475 0.055 Uiso 1 1 calc R . . C21 C 0.7105(9) 0.3175(9) 0.1991(7) 0.041(3) Uani 1 1 d . . . C22 C 0.6286(9) 0.3743(9) 0.1498(7) 0.044(3) Uani 1 1 d . . . H22 H 0.6401 0.4472 0.1255 0.053 Uiso 1 1 calc R . . C23 C 0.5340(9) 0.3070(9) 0.1314(6) 0.043(3) Uani 1 1 d . . . H23 H 0.4696 0.3251 0.0936 0.051 Uiso 1 1 calc R . . C24 C 0.5551(9) 0.2066(10) 0.1684(7) 0.047(3) Uani 1 1 d . . . H24 H 0.5063 0.1414 0.1632 0.056 Uiso 1 1 calc R . . C25 C 0.6597(9) 0.2110(9) 0.2098(6) 0.042(3) Uani 1 1 d . . . H25 H 0.6969 0.1483 0.2373 0.051 Uiso 1 1 calc R . . C31 C 0.8086(8) 0.2392(9) 0.4978(6) 0.039(3) Uani 1 1 d . . . C32 C 0.8384(9) 0.1324(10) 0.5074(7) 0.049(3) Uani 1 1 d . . . C33 C 0.9196(10) 0.1085(11) 0.5710(8) 0.059(3) Uani 1 1 d . . . H33 H 0.9416 0.0361 0.5798 0.071 Uiso 1 1 calc R . . C34 C 0.9661(10) 0.1893(12) 0.6195(8) 0.065(4) Uani 1 1 d . . . H34 H 1.0220 0.1720 0.6599 0.078 Uiso 1 1 calc R . . C35 C 0.9325(11) 0.2991(12) 0.6107(8) 0.066(4) Uani 1 1 d . . . H35 H 0.9633 0.3536 0.6461 0.080 Uiso 1 1 calc R . . C36 C 0.8530(10) 0.3239(11) 0.5485(7) 0.053(3) Uani 1 1 d . . . C37 C 0.7868(11) 0.0426(10) 0.4531(7) 0.064(4) Uani 1 1 d . . . H37A H 0.7073 0.0436 0.4558 0.096 Uiso 1 1 calc R . . H37B H 0.8144 -0.0272 0.4725 0.096 Uiso 1 1 calc R . . H37C H 0.8057 0.0538 0.3961 0.096 Uiso 1 1 calc R . . C38 C 0.8132(14) 0.4398(11) 0.5366(9) 0.092(5) Uani 1 1 d . . . H38A H 0.8346 0.4670 0.4834 0.138 Uiso 1 1 calc R . . H38B H 0.8461 0.4856 0.5807 0.138 Uiso 1 1 calc R . . H38C H 0.7335 0.4410 0.5381 0.138 Uiso 1 1 calc R . . C41 C 0.3684(12) 0.2068(10) 0.4282(7) 0.055(4) Uani 1 1 d . . . C42 C 0.2606(13) 0.2395(9) 0.4345(9) 0.067(4) Uani 1 1 d . . . H42 H 0.2161 0.2474 0.3852 0.080 Uiso 1 1 calc R . . C43 C 0.2142(17) 0.2613(10) 0.5099(11) 0.091(6) Uani 1 1 d . . . H43 H 0.1416 0.2857 0.5130 0.109 Uiso 1 1 calc R . . C44 C 0.284(2) 0.2442(14) 0.5799(12) 0.115(9) Uani 1 1 d . . . H44 H 0.2545 0.2564 0.6316 0.138 Uiso 1 1 calc R . . C45 C 0.390(2) 0.2116(15) 0.5810(11) 0.100(7) Uani 1 1 d . . . H45 H 0.4316 0.2010 0.6310 0.120 Uiso 1 1 calc R . . C46 C 0.4348(14) 0.1939(11) 0.5011(8) 0.078(5) Uani 1 1 d . . . H46 H 0.5088 0.1737 0.4983 0.093 Uiso 1 1 calc R . . C51 C 0.3095(9) 0.1395(9) 0.2607(7) 0.042(3) Uani 1 1 d . . . C52 C 0.2700(9) 0.1989(9) 0.1922(7) 0.044(3) Uani 1 1 d . . . H52 H 0.3063 0.2638 0.1781 0.053 Uiso 1 1 calc R . . C53 C 0.1761(9) 0.1628(11) 0.1434(7) 0.057(4) Uani 1 1 d . . . H53 H 0.1506 0.2023 0.0965 0.068 Uiso 1 1 calc R . . C54 C 0.1227(10) 0.0695(12) 0.1655(9) 0.062(4) Uani 1 1 d . . . H54 H 0.0595 0.0465 0.1333 0.074 Uiso 1 1 calc R . . C55 C 0.1572(10) 0.0090(12) 0.2317(8) 0.062(4) Uani 1 1 d . . . H55 H 0.1185 -0.0548 0.2448 0.075 Uiso 1 1 calc R . . C56 C 0.2503(10) 0.0418(10) 0.2803(7) 0.059(3) Uani 1 1 d . . . H56 H 0.2746 -0.0003 0.3263 0.070 Uiso 1 1 calc R . . C61 C 0.8223(9) 1.0517(9) 0.0373(7) 0.050(3) Uani 1 1 d . . . H61A H 0.8839 1.0274 0.0057 0.060 Uiso 1 1 calc R . . H61B H 0.8520 1.0823 0.0904 0.060 Uiso 1 1 calc R . . C62 C 0.7562(10) 1.1353(11) -0.0109(8) 0.066(4) Uani 1 1 d . . . H62A H 0.8004 1.1705 -0.0524 0.079 Uiso 1 1 calc R . . H62B H 0.7298 1.1913 0.0261 0.079 Uiso 1 1 calc R . . C63 C 0.6610(11) 1.0718(12) -0.0522(8) 0.071(4) Uani 1 1 d . . . H63A H 0.5963 1.1180 -0.0613 0.085 Uiso 1 1 calc R . . H63B H 0.6808 1.0426 -0.1058 0.085 Uiso 1 1 calc R . . C64 C 0.6383(9) 0.9816(10) 0.0068(7) 0.050(3) Uani 1 1 d . . . H64A H 0.5838 1.0039 0.0456 0.061 Uiso 1 1 calc R . . H64B H 0.6102 0.9168 -0.0234 0.061 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 0.0405(6) 0.0333(6) 0.0340(6) -0.0038(4) -0.0062(5) 0.0019(5) Nb2 0.0545(8) 0.0660(9) 0.0412(7) 0.0160(6) -0.0059(5) -0.0126(6) Cl1 0.118(4) 0.093(3) 0.143(4) -0.008(3) -0.002(3) 0.000(3) Cl2 0.050(2) 0.203(5) 0.059(2) 0.046(3) 0.0073(18) -0.012(3) Cl3 0.075(2) 0.073(2) 0.0417(18) -0.0030(16) -0.0102(16) 0.0211(18) Cl4 0.056(2) 0.065(2) 0.070(2) -0.0072(17) -0.0024(17) 0.0048(17) Cl5 0.109(3) 0.089(3) 0.069(2) 0.004(2) -0.016(2) -0.050(2) Si1 0.0430(19) 0.041(2) 0.0445(19) 0.0082(15) 0.0006(15) -0.0012(15) Si2 0.042(2) 0.061(3) 0.087(3) -0.012(2) 0.0006(19) -0.0081(18) P1 0.0532(19) 0.0409(19) 0.0329(17) -0.0003(13) -0.0026(14) -0.0032(15) O1 0.118(8) 0.077(7) 0.075(7) 0.027(5) -0.009(6) -0.006(6) O2 0.041(4) 0.061(5) 0.035(4) 0.014(4) -0.006(4) -0.005(4) N1 0.057(6) 0.045(6) 0.037(6) -0.001(5) -0.010(6) 0.015(5) C1 0.064(8) 0.020(6) 0.051(8) -0.010(6) 0.014(7) 0.001(6) C2 0.045(8) 0.067(10) 0.147(15) 0.029(10) -0.017(9) 0.001(7) C3 0.087(10) 0.063(9) 0.065(9) 0.018(7) -0.008(8) 0.022(8) C4 0.082(9) 0.071(9) 0.044(8) 0.011(7) 0.003(7) 0.016(8) C5 0.069(11) 0.066(12) 0.31(3) -0.084(15) -0.017(14) -0.014(9) C6 0.060(11) 0.31(3) 0.110(15) 0.064(17) -0.007(10) -0.071(15) C7 0.059(9) 0.077(11) 0.126(14) 0.002(9) -0.005(9) 0.006(8) C11 0.043(7) 0.019(6) 0.041(7) 0.001(5) 0.005(5) -0.003(5) C12 0.046(7) 0.042(7) 0.034(6) 0.006(5) 0.014(6) 0.015(5) C13 0.073(9) 0.037(7) 0.041(7) -0.001(5) -0.009(7) 0.017(7) C14 0.064(9) 0.033(7) 0.064(9) -0.012(6) -0.028(7) 0.006(6) C15 0.042(7) 0.036(7) 0.058(8) 0.003(6) -0.004(6) 0.000(5) C21 0.037(7) 0.046(8) 0.041(7) -0.003(5) 0.004(5) 0.015(6) C22 0.048(7) 0.043(7) 0.041(7) -0.009(6) 0.009(6) -0.007(6) C23 0.044(7) 0.055(8) 0.029(6) -0.009(6) 0.001(5) 0.001(6) C24 0.053(8) 0.042(8) 0.045(7) -0.006(6) 0.004(6) -0.001(6) C25 0.038(7) 0.043(8) 0.045(7) 0.001(5) -0.001(6) 0.005(6) C31 0.040(7) 0.048(8) 0.027(6) -0.010(5) -0.007(5) 0.008(6) C32 0.044(7) 0.050(9) 0.054(8) 0.021(6) 0.003(6) 0.011(6) C33 0.064(9) 0.050(8) 0.064(9) 0.023(7) 0.002(7) 0.003(7) C34 0.059(8) 0.076(11) 0.056(9) 0.032(8) -0.019(7) 0.000(8) C35 0.066(9) 0.072(11) 0.057(9) 0.002(7) -0.020(7) -0.016(8) C36 0.048(7) 0.066(9) 0.043(7) -0.002(6) -0.009(6) 0.004(7) C37 0.092(10) 0.046(8) 0.054(8) -0.003(6) 0.002(7) 0.012(7) C38 0.139(14) 0.044(9) 0.089(11) -0.018(8) -0.035(10) 0.019(9) C41 0.085(10) 0.047(8) 0.033(7) 0.003(6) 0.011(7) -0.030(7) C42 0.101(12) 0.032(8) 0.070(10) 0.000(6) 0.033(9) -0.024(8) C43 0.161(17) 0.040(9) 0.080(12) -0.002(8) 0.079(13) -0.002(9) C44 0.25(3) 0.045(11) 0.056(13) -0.017(9) 0.069(18) -0.061(15) C45 0.18(2) 0.077(13) 0.042(11) -0.006(8) -0.009(13) -0.047(14) C46 0.126(13) 0.055(9) 0.049(9) 0.000(7) -0.021(9) -0.028(9) C51 0.050(7) 0.038(7) 0.038(7) -0.002(6) 0.010(6) -0.009(6) C52 0.045(7) 0.044(7) 0.046(7) 0.008(6) 0.014(6) 0.001(6) C53 0.037(7) 0.088(10) 0.045(7) -0.024(7) -0.007(6) -0.013(7) C54 0.034(7) 0.088(11) 0.062(9) -0.029(8) 0.002(7) -0.024(8) C55 0.059(9) 0.080(10) 0.046(8) -0.015(7) -0.002(7) -0.032(8) C56 0.072(9) 0.059(9) 0.045(8) 0.001(6) 0.003(7) 0.006(7) C61 0.048(7) 0.054(8) 0.047(7) 0.017(6) -0.006(6) -0.013(6) C62 0.059(8) 0.072(10) 0.065(9) 0.007(7) -0.003(7) 0.003(8) C63 0.058(9) 0.102(12) 0.053(8) 0.026(8) 0.002(7) 0.014(8) C64 0.035(7) 0.063(9) 0.051(8) 0.000(6) -0.011(6) 0.004(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 Nb1 C1 2.127(14) . ? Nb1 C13 2.322(11) . ? Nb1 C22 2.332(10) . ? Nb1 C14 2.334(10) . ? Nb1 C21 2.361(10) . ? Nb1 C25 2.381(10) . ? Nb1 C15 2.384(11) . ? Nb1 C12 2.399(10) . ? Nb1 C23 2.404(10) . ? Nb1 C24 2.434(10) . ? Nb1 C11 2.454(10) . ? Nb1 P1 2.547(3) . ? Nb2 O1 1.691(9) . ? Nb2 Cl4 2.367(3) . ? Nb2 Cl2 2.383(4) . ? Nb2 Cl3 2.387(3) . ? Nb2 O2 2.392(7) . ? Nb2 Cl5 2.414(4) . ? Cl1 P1 2.036(6) . ? Si1 C4 1.838(12) . ? Si1 C2 1.868(12) . ? Si1 C3 1.884(13) . ? Si1 C11 1.889(11) . ? Si2 C6 1.805(17) . ? Si2 C7 1.841(15) . ? Si2 C5 1.866(15) . ? Si2 C21 1.874(11) . ? P1 C51 1.798(11) . ? P1 C41 1.840(12) . ? O2 C64 1.466(12) . ? O2 C61 1.475(12) . ? N1 C1 1.169(14) . ? N1 C31 1.393(14) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C11 C12 1.408(13) . ? C11 C15 1.428(14) . ? C12 C13 1.423(15) . ? C12 H12 0.9800 . ? C13 C14 1.390(16) . ? C13 H13 0.9800 . ? C14 C15 1.433(15) . ? C14 H14 0.9800 . ? C15 H15 0.9800 . ? C21 C22 1.411(15) . ? C21 C25 1.439(15) . ? C22 C23 1.409(14) . ? C22 H22 0.9800 . ? C23 C24 1.377(15) . ? C23 H23 0.9800 . ? C24 C25 1.386(14) . ? C24 H24 0.9800 . ? C25 H25 0.9800 . ? C31 C32 1.358(15) . ? C31 C36 1.390(15) . ? C32 C33 1.400(16) . ? C32 C37 1.497(16) . ? C33 C34 1.344(17) . ? C33 H33 0.9300 . ? C34 C35 1.405(18) . ? C34 H34 0.9300 . ? C35 C36 1.373(17) . ? C35 H35 0.9300 . ? C36 C38 1.503(18) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C41 C42 1.370(18) . ? C41 C46 1.381(18) . ? C42 C43 1.385(17) . ? C42 H42 0.9300 . ? C43 C44 1.37(3) . ? C43 H43 0.9300 . ? C44 C45 1.34(3) . ? C44 H44 0.9300 . ? C45 C46 1.43(2) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C52 1.376(15) . ? C51 C56 1.422(15) . ? C52 C53 1.398(14) . ? C52 H52 0.9300 . ? C53 C54 1.354(17) . ? C53 H53 0.9300 . ? C54 C55 1.337(18) . ? C54 H54 0.9300 . ? C55 C56 1.377(16) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C62 1.487(16) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.491(17) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.481(16) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? 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 C1 Nb1 C13 77.9(4) . . ? C1 Nb1 C22 116.7(4) . . ? C13 Nb1 C22 139.6(4) . . ? C1 Nb1 C14 75.8(4) . . ? C13 Nb1 C14 34.7(4) . . ? C22 Nb1 C14 108.8(4) . . ? C1 Nb1 C21 82.3(4) . . ? C13 Nb1 C21 141.4(4) . . ? C22 Nb1 C21 35.0(4) . . ? C14 Nb1 C21 108.2(4) . . ? C1 Nb1 C25 78.0(4) . . ? C13 Nb1 C25 155.8(4) . . ? C22 Nb1 C25 56.5(4) . . ? C14 Nb1 C25 137.8(4) . . ? C21 Nb1 C25 35.3(3) . . ? C1 Nb1 C15 108.6(4) . . ? C13 Nb1 C15 57.4(4) . . ? C22 Nb1 C15 82.3(4) . . ? C14 Nb1 C15 35.4(4) . . ? C21 Nb1 C15 99.4(4) . . ? C25 Nb1 C15 134.3(4) . . ? C1 Nb1 C12 111.1(4) . . ? C13 Nb1 C12 35.0(4) . . ? C22 Nb1 C12 124.7(4) . . ? C14 Nb1 C12 58.1(4) . . ? C21 Nb1 C12 154.9(4) . . ? C25 Nb1 C12 164.1(4) . . ? C15 Nb1 C12 56.8(4) . . ? C1 Nb1 C23 133.7(4) . . ? C13 Nb1 C23 148.3(4) . . ? C22 Nb1 C23 34.6(3) . . ? C14 Nb1 C23 135.9(4) . . ? C21 Nb1 C23 58.4(4) . . ? C25 Nb1 C23 55.9(4) . . ? C15 Nb1 C23 101.6(4) . . ? C12 Nb1 C23 114.7(4) . . ? C1 Nb1 C24 106.7(4) . . ? C13 Nb1 C24 160.5(4) . . ? C22 Nb1 C24 56.0(4) . . ? C14 Nb1 C24 164.4(4) . . ? C21 Nb1 C24 57.8(4) . . ? C25 Nb1 C24 33.4(3) . . ? C15 Nb1 C24 134.3(4) . . ? C12 Nb1 C24 131.5(4) . . ? C23 Nb1 C24 33.1(4) . . ? C1 Nb1 C11 132.2(3) . . ? C13 Nb1 C11 57.3(4) . . ? C22 Nb1 C11 91.6(4) . . ? C14 Nb1 C11 58.2(4) . . ? C21 Nb1 C11 121.9(4) . . ? C25 Nb1 C11 146.1(4) . . ? C15 Nb1 C11 34.3(3) . . ? C12 Nb1 C11 33.7(3) . . ? C23 Nb1 C11 91.7(4) . . ? C24 Nb1 C11 121.1(4) . . ? C1 Nb1 P1 85.0(3) . . ? C13 Nb1 P1 87.0(3) . . ? C22 Nb1 P1 129.6(3) . . ? C14 Nb1 P1 120.9(3) . . ? C21 Nb1 P1 124.1(3) . . ? C25 Nb1 P1 88.7(3) . . ? C15 Nb1 P1 136.1(3) . . ? C12 Nb1 P1 79.4(3) . . ? C23 Nb1 P1 97.0(3) . . ? C24 Nb1 P1 74.7(3) . . ? C11 Nb1 P1 106.6(2) . . ? O1 Nb2 Cl4 98.0(4) . . ? O1 Nb2 Cl2 96.7(4) . . ? Cl4 Nb2 Cl2 165.33(14) . . ? O1 Nb2 Cl3 96.1(3) . . ? Cl4 Nb2 Cl3 89.38(11) . . ? Cl2 Nb2 Cl3 88.60(15) . . ? O1 Nb2 O2 178.3(4) . . ? Cl4 Nb2 O2 82.47(19) . . ? Cl2 Nb2 O2 82.9(2) . . ? Cl3 Nb2 O2 82.28(19) . . ? O1 Nb2 Cl5 97.1(3) . . ? Cl4 Nb2 Cl5 89.26(13) . . ? Cl2 Nb2 Cl5 89.39(16) . . ? Cl3 Nb2 Cl5 166.79(13) . . ? O2 Nb2 Cl5 84.5(2) . . ? C4 Si1 C2 111.7(7) . . ? C4 Si1 C3 111.5(6) . . ? C2 Si1 C3 109.4(7) . . ? C4 Si1 C11 111.2(5) . . ? C2 Si1 C11 109.8(5) . . ? C3 Si1 C11 103.0(5) . . ? C6 Si2 C7 111.1(9) . . ? C6 Si2 C5 112.4(11) . . ? C7 Si2 C5 106.4(8) . . ? C6 Si2 C21 105.4(6) . . ? C7 Si2 C21 110.5(6) . . ? C5 Si2 C21 111.2(6) . . ? C51 P1 C41 102.6(5) . . ? C51 P1 Cl1 99.0(4) . . ? C41 P1 Cl1 98.6(5) . . ? C51 P1 Nb1 122.5(4) . . ? C41 P1 Nb1 115.9(3) . . ? Cl1 P1 Nb1 114.46(19) . . ? C64 O2 C61 108.2(8) . . ? C64 O2 Nb2 125.2(6) . . ? C61 O2 Nb2 125.8(6) . . ? C1 N1 C31 175.9(12) . . ? N1 C1 Nb1 175.4(9) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 C11 C15 106.6(9) . . ? C12 C11 Si1 125.0(8) . . ? C15 C11 Si1 125.5(8) . . ? C12 C11 Nb1 71.0(6) . . ? C15 C11 Nb1 70.2(6) . . ? Si1 C11 Nb1 138.9(5) . . ? C11 C12 C13 108.2(10) . . ? C11 C12 Nb1 75.3(6) . . ? C13 C12 Nb1 69.5(6) . . ? C11 C12 H12 125.7 . . ? C13 C12 H12 125.7 . . ? Nb1 C12 H12 125.7 . . ? C14 C13 C12 109.6(11) . . ? C14 C13 Nb1 73.1(7) . . ? C12 C13 Nb1 75.5(6) . . ? C14 C13 H13 124.9 . . ? C12 C13 H13 124.9 . . ? Nb1 C13 H13 124.9 . . ? C13 C14 C15 106.4(10) . . ? C13 C14 Nb1 72.1(6) . . ? C15 C14 Nb1 74.2(6) . . ? C13 C14 H14 126.4 . . ? C15 C14 H14 126.4 . . ? Nb1 C14 H14 126.4 . . ? C11 C15 C14 109.1(10) . . ? C11 C15 Nb1 75.6(6) . . ? C14 C15 Nb1 70.4(6) . . ? C11 C15 H15 125.3 . . ? C14 C15 H15 125.3 . . ? Nb1 C15 H15 125.3 . . ? C22 C21 C25 103.1(9) . . ? C22 C21 Si2 127.0(9) . . ? C25 C21 Si2 127.7(9) . . ? C22 C21 Nb1 71.4(6) . . ? C25 C21 Nb1 73.1(6) . . ? Si2 C21 Nb1 132.1(5) . . ? C23 C22 C21 111.0(10) . . ? C23 C22 Nb1 75.5(6) . . ? C21 C22 Nb1 73.7(6) . . ? C23 C22 H22 124.3 . . ? C21 C22 H22 124.3 . . ? Nb1 C22 H22 124.3 . . ? C24 C23 C22 107.0(10) . . ? C24 C23 Nb1 74.7(6) . . ? C22 C23 Nb1 69.9(5) . . ? C24 C23 H23 126.3 . . ? C22 C23 H23 126.3 . . ? Nb1 C23 H23 126.3 . . ? C23 C24 C25 108.7(10) . . ? C23 C24 Nb1 72.3(6) . . ? C25 C24 Nb1 71.2(6) . . ? C23 C24 H24 125.6 . . ? C25 C24 H24 125.6 . . ? Nb1 C24 H24 125.6 . . ? C24 C25 C21 110.2(10) . . ? C24 C25 Nb1 75.4(6) . . ? C21 C25 Nb1 71.6(6) . . ? C24 C25 H25 124.7 . . ? C21 C25 H25 124.7 . . ? Nb1 C25 H25 124.7 . . ? C32 C31 C36 123.4(10) . . ? C32 C31 N1 118.5(10) . . ? C36 C31 N1 118.1(10) . . ? C31 C32 C33 117.3(11) . . ? C31 C32 C37 122.1(10) . . ? C33 C32 C37 120.6(11) . . ? C34 C33 C32 120.5(12) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 121.8(12) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C36 C35 C34 118.4(12) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C35 C36 C31 118.5(12) . . ? C35 C36 C38 120.7(12) . . ? C31 C36 C38 120.7(11) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C42 C41 C46 118.5(13) . . ? C42 C41 P1 121.3(10) . . ? C46 C41 P1 120.1(12) . . ? C41 C42 C43 123.7(16) . . ? C41 C42 H42 118.1 . . ? C43 C42 H42 118.1 . . ? C44 C43 C42 114.7(18) . . ? C44 C43 H43 122.6 . . ? C42 C43 H43 122.6 . . ? C45 C44 C43 126.4(19) . . ? C45 C44 H44 116.8 . . ? C43 C44 H44 116.8 . . ? C44 C45 C46 116.6(18) . . ? C44 C45 H45 121.7 . . ? C46 C45 H45 121.7 . . ? C41 C46 C45 119.9(16) . . ? C41 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C52 C51 C56 117.5(10) . . ? C52 C51 P1 120.5(8) . . ? C56 C51 P1 121.9(9) . . ? C51 C52 C53 120.7(11) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C54 C53 C52 119.1(12) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C55 C54 C53 122.6(11) . . ? C55 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? C54 C55 C56 119.6(12) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C55 C56 C51 120.5(12) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? O2 C61 C62 106.5(9) . . ? O2 C61 H61A 110.4 . . ? C62 C61 H61A 110.4 . . ? O2 C61 H61B 110.4 . . ? C62 C61 H61B 110.4 . . ? H61A C61 H61B 108.6 . . ? C61 C62 C63 104.5(11) . . ? C61 C62 H62A 110.9 . . ? C63 C62 H62A 110.9 . . ? C61 C62 H62B 110.9 . . ? C63 C62 H62B 110.9 . . ? H62A C62 H62B 108.9 . . ? C64 C63 C62 105.0(10) . . ? C64 C63 H63A 110.7 . . ? C62 C63 H63A 110.7 . . ? C64 C63 H63B 110.7 . . ? C62 C63 H63B 110.7 . . ? H63A C63 H63B 108.8 . . ? O2 C64 C63 105.6(9) . . ? O2 C64 H64A 110.6 . . ? C63 C64 H64A 110.6 . . ? O2 C64 H64B 110.6 . . ? C63 C64 H64B 110.6 . . ? H64A C64 H64B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 21.29 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.972 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.116