Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Simon J. Lancaster' 'David L. Hughes' _publ_contact_author_name 'Dr Simon J Lancaster' _publ_contact_author_address ; Wolfson Materials and Catalysis Centre School of Chemical Sciences & Pharmacy Univeristy of East Anglia Norfolk NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email S.LANCASTER@UEA.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The synthesis of half-sandwich bis(pentafluorophenyl)boryl-substituted cyclopentadienyl zirconium, niobium and tantalum complexes and the isolation and molecular structure of a zwitterionic niobocene ; data_simonl6a _database_code_CSD 201466 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 9' _chemical_melting_point ? _chemical_formula_moiety 'C25 H17 B Cl3 F10 Nb Si, 1.5(C7 H8)' _chemical_formula_structural [NbCl2{C5H4B(Cl)(C6F5)2}(C5H4SiMe3)].1.5(toluene) _chemical_formula_sum 'C35.5 H29 B Cl3 F10 Nb Si' _chemical_formula_weight 883.75 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.601(2) _cell_length_b 14.492(4) _cell_length_c 15.252(8) _cell_angle_alpha 116.58(3) _cell_angle_beta 99.60(2) _cell_angle_gamma 96.390(10) _cell_volume 1829.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'diamond-shaped plate' _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10730 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.46 _reflns_number_total 6318 _reflns_number_gt 5315 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _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^)+(0.0656P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6318 _refine_ls_number_parameters 465 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 Nb Nb 0.55031(3) 0.21951(2) 0.47414(2) 0.02857(11) Uani 1 1 d . . . B1 B 0.4554(4) 0.4449(3) 0.6855(3) 0.0301(7) Uani 1 1 d . . . C11 C 0.5792(3) 0.3835(2) 0.6375(2) 0.0301(7) Uani 1 1 d . . . C12 C 0.6443(3) 0.3095(3) 0.6585(2) 0.0330(7) Uani 1 1 d . . . H12 H 0.6126 0.2784 0.6952 0.040 Uiso 1 1 calc R . . C13 C 0.7634(4) 0.2907(3) 0.6154(2) 0.0379(8) Uani 1 1 d . . . H13 H 0.8265 0.2486 0.6218 0.045 Uiso 1 1 calc R . . C14 C 0.7700(4) 0.3474(3) 0.5604(3) 0.0375(8) Uani 1 1 d . . . H14 H 0.8362 0.3473 0.5223 0.045 Uiso 1 1 calc R . . C15 C 0.6568(3) 0.4045(2) 0.5739(2) 0.0327(7) Uani 1 1 d . . . H15 H 0.6368 0.4483 0.5459 0.039 Uiso 1 1 calc R . . Cl2 Cl 0.32855(8) 0.44800(6) 0.57501(5) 0.03211(19) Uani 1 1 d . . . C31 C 0.5232(4) 0.5699(3) 0.7688(2) 0.0319(7) Uani 1 1 d . . . C32 C 0.4313(4) 0.6359(3) 0.8095(2) 0.0369(8) Uani 1 1 d . . . C33 C 0.4760(5) 0.7412(3) 0.8797(3) 0.0477(10) Uani 1 1 d . . . C34 C 0.6214(5) 0.7857(3) 0.9145(3) 0.0522(11) Uani 1 1 d . . . C35 C 0.7191(4) 0.7244(3) 0.8789(3) 0.0479(10) Uani 1 1 d . . . C36 C 0.6686(4) 0.6203(3) 0.8085(2) 0.0396(8) Uani 1 1 d . . . F32 F 0.2868(2) 0.59787(17) 0.77939(15) 0.0490(5) Uani 1 1 d . . . F33 F 0.3794(3) 0.80073(19) 0.91508(18) 0.0700(8) Uani 1 1 d . . . F34 F 0.6673(3) 0.88854(17) 0.98494(17) 0.0746(9) Uani 1 1 d . . . F35 F 0.8613(3) 0.7664(2) 0.91495(18) 0.0760(9) Uani 1 1 d . . . F36 F 0.7728(2) 0.56398(19) 0.77923(17) 0.0582(7) Uani 1 1 d . . . C41 C 0.3743(3) 0.3905(2) 0.7423(2) 0.0293(7) Uani 1 1 d . . . C42 C 0.4550(3) 0.3981(2) 0.8309(2) 0.0303(7) Uani 1 1 d . . . C43 C 0.4029(4) 0.3573(3) 0.8888(2) 0.0331(7) Uani 1 1 d . . . C44 C 0.2619(4) 0.3033(3) 0.8569(3) 0.0401(8) Uani 1 1 d . . . C45 C 0.1772(4) 0.2926(3) 0.7701(3) 0.0430(9) Uani 1 1 d . . . C46 C 0.2319(4) 0.3372(3) 0.7159(2) 0.0366(8) Uani 1 1 d . . . F42 F 0.59676(19) 0.44744(15) 0.86558(13) 0.0360(4) Uani 1 1 d . . . F43 F 0.4887(2) 0.36949(15) 0.97419(13) 0.0409(5) Uani 1 1 d . . . F44 F 0.2083(2) 0.2604(2) 0.90982(17) 0.0576(6) Uani 1 1 d . . . F45 F 0.0381(2) 0.2394(2) 0.73765(19) 0.0675(8) Uani 1 1 d . . . F46 F 0.1358(2) 0.32469(18) 0.63325(15) 0.0471(5) Uani 1 1 d . . . Cl5 Cl 0.34234(9) 0.16966(6) 0.51667(6) 0.0371(2) Uani 1 1 d . . . Cl6 Cl 0.65135(10) 0.07093(7) 0.44917(6) 0.0430(2) Uani 1 1 d . . . C71 C 0.4378(3) 0.1103(2) 0.2915(2) 0.0301(7) Uani 1 1 d . . . C72 C 0.3635(4) 0.1933(3) 0.3305(2) 0.0329(7) Uani 1 1 d . . . H72 H 0.2664 0.1846 0.3314 0.039 Uiso 1 1 calc R . . C73 C 0.4587(4) 0.2909(3) 0.3677(2) 0.0344(7) Uani 1 1 d . . . H73 H 0.4364 0.3572 0.3988 0.041 Uiso 1 1 calc R . . C74 C 0.5943(4) 0.2700(3) 0.3493(2) 0.0343(7) Uani 1 1 d . . . H74 H 0.6767 0.3201 0.3648 0.041 Uiso 1 1 calc R . . C75 C 0.5821(4) 0.1602(3) 0.3036(2) 0.0314(7) Uani 1 1 d . . . H75 H 0.6562 0.1253 0.2843 0.038 Uiso 1 1 calc R . . Si7 Si 0.35606(10) -0.03706(7) 0.21773(7) 0.0345(2) Uani 1 1 d . . . C76 C 0.2630(4) -0.0822(3) 0.2938(3) 0.0470(9) Uani 1 1 d . . . H76A H 0.1880 -0.0441 0.3125 0.070 Uiso 1 1 calc R . . H76B H 0.3316 -0.0694 0.3536 0.070 Uiso 1 1 calc R . . H76C H 0.2216 -0.1564 0.2544 0.070 Uiso 1 1 calc R . . C77 C 0.5020(4) -0.1087(3) 0.1794(3) 0.0506(10) Uani 1 1 d . . . H77A H 0.5483 -0.0839 0.1404 0.076 Uiso 1 1 calc R . . H77B H 0.4616 -0.1829 0.1393 0.076 Uiso 1 1 calc R . . H77C H 0.5718 -0.0962 0.2385 0.076 Uiso 1 1 calc R . . C78 C 0.2226(4) -0.0536(3) 0.1045(3) 0.0480(9) Uani 1 1 d . . . H78A H 0.1479 -0.0162 0.1260 0.072 Uiso 1 1 calc R . . H78B H 0.1806 -0.1272 0.0612 0.072 Uiso 1 1 calc R . . H78C H 0.2708 -0.0260 0.0683 0.072 Uiso 1 1 calc R . . C81 C 0.9783(4) 0.2651(4) 0.3209(3) 0.0537(11) Uani 1 1 d . . . C82 C 0.9268(5) 0.2003(4) 0.2194(3) 0.0660(13) Uani 1 1 d . . . H82 H 0.9107 0.2292 0.1760 0.079 Uiso 1 1 calc R . . C83 C 0.8992(5) 0.0950(5) 0.1817(4) 0.0694(14) Uani 1 1 d . . . H83 H 0.8667 0.0527 0.1121 0.083 Uiso 1 1 calc R . . C84 C 0.9169(5) 0.0474(4) 0.2413(5) 0.0755(16) Uani 1 1 d . . . H84 H 0.8951 -0.0258 0.2131 0.091 Uiso 1 1 calc R . . C85 C 0.9697(4) 0.1125(4) 0.3480(4) 0.0685(13) Uani 1 1 d . . . H85 H 0.9830 0.0831 0.3910 0.082 Uiso 1 1 calc R . . C86 C 1.0004(4) 0.2212(4) 0.3856(3) 0.0511(10) Uani 1 1 d . . . H86 H 1.0362 0.2653 0.4547 0.061 Uiso 1 1 calc R . . C87 C 1.0108(5) 0.3857(4) 0.3632(5) 0.0809(16) Uani 1 1 d . . . H87A H 1.0719 0.4043 0.3272 0.121 Uiso 1 1 calc R . . H87B H 1.0588 0.4192 0.4337 0.121 Uiso 1 1 calc R . . H87C H 0.9219 0.4089 0.3551 0.121 Uiso 1 1 calc R . . C91 C 1.0396(18) 0.5350(11) -0.0115(8) 0.127(6) Uiso 0.481(4) 1 d PD . . C92 C 0.9480(11) 0.4549(8) -0.0824(6) 0.221(8) Uani 0.963(8) 1 d PD . . C93 C 0.882(2) 0.3763(11) -0.0622(10) 0.157(8) Uiso 0.481(4) 1 d PD . . C94 C 0.8720(8) 0.3877(9) 0.0300(10) 0.159(4) Uani 0.963(8) 1 d PD . . C95 C 0.959(2) 0.4817(13) 0.1070(10) 0.152(7) Uiso 0.481(4) 1 d PD . . 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 Nb 0.03645(18) 0.02688(17) 0.02595(17) 0.01483(13) 0.00866(12) 0.00849(12) B1 0.0329(18) 0.0286(19) 0.0279(17) 0.0137(15) 0.0047(15) 0.0065(14) C11 0.0370(16) 0.0246(16) 0.0232(14) 0.0093(12) 0.0018(13) 0.0036(13) C12 0.0380(17) 0.0352(18) 0.0252(15) 0.0144(14) 0.0053(13) 0.0095(14) C13 0.0351(17) 0.043(2) 0.0311(17) 0.0154(15) 0.0019(14) 0.0106(15) C14 0.0315(16) 0.0378(19) 0.0341(17) 0.0101(15) 0.0081(14) 0.0040(14) C15 0.0365(17) 0.0268(16) 0.0289(16) 0.0113(13) 0.0034(13) 0.0001(13) Cl2 0.0382(4) 0.0324(4) 0.0267(4) 0.0158(3) 0.0046(3) 0.0080(3) C31 0.0423(18) 0.0317(17) 0.0248(15) 0.0169(13) 0.0060(13) 0.0063(13) C32 0.049(2) 0.0334(18) 0.0286(16) 0.0155(14) 0.0049(15) 0.0123(15) C33 0.083(3) 0.034(2) 0.0281(17) 0.0152(15) 0.0115(18) 0.0217(19) C34 0.088(3) 0.031(2) 0.0261(17) 0.0113(15) 0.0072(19) -0.008(2) C35 0.059(2) 0.045(2) 0.0294(17) 0.0147(16) 0.0089(17) -0.0121(18) C36 0.046(2) 0.040(2) 0.0294(17) 0.0139(15) 0.0107(15) 0.0021(15) F32 0.0480(12) 0.0509(13) 0.0391(11) 0.0124(10) 0.0075(10) 0.0210(10) F33 0.103(2) 0.0477(14) 0.0473(13) 0.0092(11) 0.0128(13) 0.0394(14) F34 0.131(2) 0.0296(12) 0.0392(12) 0.0042(10) 0.0162(14) -0.0110(13) F35 0.0681(16) 0.0722(18) 0.0474(13) 0.0067(13) 0.0105(12) -0.0343(14) F36 0.0388(11) 0.0622(15) 0.0479(13) 0.0073(11) 0.0098(10) -0.0012(10) C41 0.0360(16) 0.0264(16) 0.0241(14) 0.0122(13) 0.0039(13) 0.0060(13) C42 0.0345(16) 0.0274(16) 0.0268(15) 0.0121(13) 0.0046(13) 0.0058(12) C43 0.0443(18) 0.0326(17) 0.0246(15) 0.0159(14) 0.0058(14) 0.0102(14) C44 0.046(2) 0.046(2) 0.0394(19) 0.0292(17) 0.0125(16) 0.0082(16) C45 0.0352(18) 0.054(2) 0.0414(19) 0.0281(18) 0.0051(16) -0.0004(16) C46 0.0385(18) 0.0408(19) 0.0318(17) 0.0212(15) 0.0030(15) 0.0045(15) F42 0.0337(9) 0.0395(11) 0.0318(9) 0.0179(8) 0.0012(8) 0.0024(8) F43 0.0538(12) 0.0430(12) 0.0274(9) 0.0199(9) 0.0036(9) 0.0111(9) F44 0.0580(13) 0.0785(17) 0.0559(13) 0.0505(13) 0.0155(11) 0.0035(12) F45 0.0405(12) 0.102(2) 0.0696(16) 0.0612(16) -0.0022(11) -0.0161(12) F46 0.0367(10) 0.0687(15) 0.0378(11) 0.0344(11) -0.0039(9) -0.0026(10) Cl5 0.0450(4) 0.0338(4) 0.0314(4) 0.0152(3) 0.0118(3) 0.0013(3) Cl6 0.0634(6) 0.0362(5) 0.0357(4) 0.0199(4) 0.0117(4) 0.0231(4) C71 0.0388(17) 0.0312(17) 0.0245(15) 0.0158(13) 0.0091(13) 0.0098(13) C72 0.0393(17) 0.0357(18) 0.0284(16) 0.0183(14) 0.0080(14) 0.0127(14) C73 0.052(2) 0.0298(17) 0.0273(16) 0.0178(14) 0.0084(15) 0.0150(14) C74 0.0471(19) 0.0330(17) 0.0268(15) 0.0186(14) 0.0096(14) 0.0028(14) C75 0.0390(17) 0.0344(17) 0.0239(15) 0.0152(13) 0.0100(13) 0.0097(13) Si7 0.0435(5) 0.0280(5) 0.0308(5) 0.0135(4) 0.0084(4) 0.0063(4) C76 0.059(2) 0.036(2) 0.045(2) 0.0211(17) 0.0107(18) -0.0007(17) C77 0.060(2) 0.038(2) 0.046(2) 0.0125(17) 0.0130(19) 0.0167(18) C78 0.055(2) 0.043(2) 0.039(2) 0.0171(17) 0.0055(17) 0.0050(17) C81 0.0292(18) 0.076(3) 0.053(2) 0.029(2) 0.0102(17) 0.0069(18) C82 0.048(2) 0.093(4) 0.051(3) 0.032(3) 0.008(2) 0.006(2) C83 0.049(2) 0.089(4) 0.052(3) 0.019(3) 0.009(2) 0.015(2) C84 0.038(2) 0.057(3) 0.104(4) 0.014(3) 0.019(3) 0.011(2) C85 0.045(2) 0.088(4) 0.097(4) 0.057(3) 0.029(3) 0.031(2) C86 0.0352(19) 0.077(3) 0.0354(19) 0.019(2) 0.0113(16) 0.0181(18) C87 0.053(3) 0.086(4) 0.106(4) 0.057(3) 0.007(3) -0.002(3) C92 0.132(9) 0.235(16) 0.41(2) 0.237(18) 0.092(12) 0.065(10) C94 0.091(5) 0.223(12) 0.223(12) 0.157(11) 0.027(7) 0.053(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 Nb Cl5 2.3367(9) . ? Nb Cl6 2.3615(11) . ? Nb C14 2.374(3) . ? Nb C73 2.389(3) . ? Nb C15 2.402(3) . ? Nb C74 2.405(3) . ? Nb C75 2.433(3) . ? Nb C72 2.440(3) . ? Nb C13 2.442(3) . ? Nb C12 2.455(3) . ? Nb C71 2.470(3) . ? Nb C11 2.501(3) . ? B1 C41 1.637(5) . ? B1 C11 1.638(5) . ? B1 C31 1.649(5) . ? B1 Cl2 1.929(4) . ? C11 C12 1.426(5) . ? C11 C15 1.429(4) . ? C12 C13 1.405(5) . ? C12 H12 0.9300 . ? C13 C14 1.416(5) . ? C13 H13 0.9300 . ? C14 C15 1.425(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C31 C32 1.385(5) . ? C31 C36 1.394(5) . ? C32 F32 1.353(4) . ? C32 C33 1.378(5) . ? C33 F33 1.350(5) . ? C33 C34 1.376(6) . ? C34 F34 1.353(4) . ? C34 C35 1.374(6) . ? C35 F35 1.342(4) . ? C35 C36 1.370(5) . ? C36 F36 1.369(4) . ? C41 C46 1.390(4) . ? C41 C42 1.392(4) . ? C42 F42 1.359(4) . ? C42 C43 1.389(4) . ? C43 F43 1.346(4) . ? C43 C44 1.373(5) . ? C44 F44 1.349(4) . ? C44 C45 1.365(5) . ? C45 F45 1.353(4) . ? C45 C46 1.387(5) . ? C46 F46 1.358(4) . ? C71 C72 1.414(5) . ? C71 C75 1.432(4) . ? C71 Si7 1.904(3) . ? C72 C73 1.407(5) . ? C72 H72 0.9300 . ? C73 C74 1.414(5) . ? C73 H73 0.9300 . ? C74 C75 1.404(5) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? Si7 C77 1.854(4) . ? Si7 C76 1.861(4) . ? Si7 C78 1.872(4) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C81 C82 1.366(6) . ? C81 C86 1.394(6) . ? C81 C87 1.540(7) . ? C82 C83 1.343(7) . ? C82 H82 0.9300 . ? C83 C84 1.366(8) . ? C83 H83 0.9300 . ? C84 C85 1.428(7) . ? C84 H84 0.9300 . ? C85 C86 1.389(7) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C91 C92 1.274(9) . ? C91 C93 1.300(16) 2_765 ? C91 C92 1.357(9) 2_765 ? C91 C95 1.368(16) 2_765 ? C91 C91 1.40(2) 2_765 ? C91 C94 1.485(12) 2_765 ? C92 C91 1.357(9) 2_765 ? C92 C95 1.419(10) 2_765 ? C92 C93 1.419(9) . ? C93 C91 1.300(16) 2_765 ? C93 C94 1.362(9) . ? C94 C95 1.387(9) . ? C94 C91 1.485(12) 2_765 ? C95 C91 1.368(16) 2_765 ? C95 C92 1.419(10) 2_765 ? 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 Nb Cl6 97.90(4) . . ? Cl5 Nb C14 136.40(9) . . ? Cl6 Nb C14 96.51(9) . . ? Cl5 Nb C73 101.94(9) . . ? Cl6 Nb C73 134.67(8) . . ? C14 Nb C73 96.43(13) . . ? Cl5 Nb C15 113.12(8) . . ? Cl6 Nb C15 130.23(9) . . ? C14 Nb C15 34.71(11) . . ? C73 Nb C15 76.99(12) . . ? Cl5 Nb C74 134.19(9) . . ? Cl6 Nb C74 108.42(9) . . ? C14 Nb C74 77.79(12) . . ? C73 Nb C74 34.30(12) . . ? C15 Nb C74 77.08(12) . . ? Cl5 Nb C75 125.90(8) . . ? Cl6 Nb C75 79.05(9) . . ? C14 Nb C75 97.18(12) . . ? C73 Nb C75 56.30(11) . . ? C15 Nb C75 108.67(11) . . ? C74 Nb C75 33.74(11) . . ? Cl5 Nb C72 79.15(9) . . ? Cl6 Nb C72 114.73(9) . . ? C14 Nb C72 129.79(12) . . ? C73 Nb C72 33.86(11) . . ? C15 Nb C72 108.85(12) . . ? C74 Nb C72 56.05(12) . . ? C75 Nb C72 55.45(11) . . ? Cl5 Nb C13 112.09(9) . . ? Cl6 Nb C13 76.40(9) . . ? C14 Nb C13 34.17(12) . . ? C73 Nb C13 129.92(12) . . ? C15 Nb C13 56.54(12) . . ? C74 Nb C13 110.19(12) . . ? C75 Nb C13 119.19(11) . . ? C72 Nb C13 163.75(12) . . ? Cl5 Nb C12 81.88(9) . . ? Cl6 Nb C12 93.91(9) . . ? C14 Nb C12 56.20(12) . . ? C73 Nb C12 128.86(11) . . ? C15 Nb C12 55.84(12) . . ? C74 Nb C12 130.96(12) . . ? C75 Nb C12 151.85(11) . . ? C72 Nb C12 147.40(11) . . ? C13 Nb C12 33.34(11) . . ? Cl5 Nb C71 91.96(8) . . ? Cl6 Nb C71 82.52(9) . . ? C14 Nb C71 130.70(11) . . ? C73 Nb C71 56.65(11) . . ? C15 Nb C71 131.28(11) . . ? C74 Nb C71 56.62(11) . . ? C75 Nb C71 33.94(10) . . ? C72 Nb C71 33.47(11) . . ? C13 Nb C71 149.73(11) . . ? C12 Nb C71 172.43(11) . . ? Cl5 Nb C11 82.03(8) . . ? Cl6 Nb C11 127.17(8) . . ? C14 Nb C11 56.80(11) . . ? C73 Nb C11 95.89(11) . . ? C15 Nb C11 33.81(11) . . ? C74 Nb C11 108.38(11) . . ? C75 Nb C11 141.66(11) . . ? C72 Nb C11 117.02(11) . . ? C13 Nb C11 55.93(11) . . ? C12 Nb C11 33.42(11) . . ? C71 Nb C11 150.19(11) . . ? C41 B1 C11 112.2(3) . . ? C41 B1 C31 107.3(2) . . ? C11 B1 C31 112.1(3) . . ? C41 B1 Cl2 114.4(2) . . ? C11 B1 Cl2 105.6(2) . . ? C31 B1 Cl2 105.1(2) . . ? C12 C11 C15 105.7(3) . . ? C12 C11 B1 128.5(3) . . ? C15 C11 B1 125.4(3) . . ? C12 C11 Nb 71.52(18) . . ? C15 C11 Nb 69.28(17) . . ? B1 C11 Nb 129.1(2) . . ? C13 C12 C11 110.0(3) . . ? C13 C12 Nb 72.81(18) . . ? C11 C12 Nb 75.06(18) . . ? C13 C12 H12 125.0 . . ? C11 C12 H12 125.0 . . ? Nb C12 H12 118.8 . . ? C12 C13 C14 107.6(3) . . ? C12 C13 Nb 73.85(18) . . ? C14 C13 Nb 70.27(19) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? Nb C13 H13 121.4 . . ? C13 C14 C15 107.7(3) . . ? C13 C14 Nb 75.56(19) . . ? C15 C14 Nb 73.72(18) . . ? C13 C14 H14 126.1 . . ? C15 C14 H14 126.1 . . ? Nb C14 H14 116.7 . . ? C14 C15 C11 108.9(3) . . ? C14 C15 Nb 71.57(18) . . ? C11 C15 Nb 76.91(18) . . ? C14 C15 H15 125.6 . . ? C11 C15 H15 125.6 . . ? Nb C15 H15 117.8 . . ? C32 C31 C36 112.8(3) . . ? C32 C31 B1 119.6(3) . . ? C36 C31 B1 127.5(3) . . ? F32 C32 C33 115.6(3) . . ? F32 C32 C31 119.8(3) . . ? C33 C32 C31 124.5(3) . . ? F33 C33 C34 119.8(3) . . ? F33 C33 C32 121.0(4) . . ? C34 C33 C32 119.2(4) . . ? F34 C34 C35 120.6(4) . . ? F34 C34 C33 120.0(4) . . ? C35 C34 C33 119.4(3) . . ? F35 C35 C36 121.3(4) . . ? F35 C35 C34 119.8(3) . . ? C36 C35 C34 118.9(3) . . ? F36 C36 C35 115.2(3) . . ? F36 C36 C31 119.7(3) . . ? C35 C36 C31 125.1(3) . . ? C46 C41 C42 113.1(3) . . ? C46 C41 B1 129.3(3) . . ? C42 C41 B1 117.6(3) . . ? F42 C42 C43 115.3(3) . . ? F42 C42 C41 119.7(3) . . ? C43 C42 C41 125.0(3) . . ? F43 C43 C44 120.4(3) . . ? F43 C43 C42 120.9(3) . . ? C44 C43 C42 118.8(3) . . ? F44 C44 C45 120.5(3) . . ? F44 C44 C43 120.5(3) . . ? C45 C44 C43 119.0(3) . . ? F45 C45 C44 119.7(3) . . ? F45 C45 C46 119.7(3) . . ? C44 C45 C46 120.6(3) . . ? F46 C46 C45 115.1(3) . . ? F46 C46 C41 121.4(3) . . ? C45 C46 C41 123.5(3) . . ? C72 C71 C75 105.6(3) . . ? C72 C71 Si7 127.1(2) . . ? C75 C71 Si7 126.5(2) . . ? C72 C71 Nb 72.10(17) . . ? C75 C71 Nb 71.60(17) . . ? Si7 C71 Nb 128.68(15) . . ? C73 C72 C71 109.7(3) . . ? C73 C72 Nb 71.10(19) . . ? C71 C72 Nb 74.44(19) . . ? C73 C72 H72 125.1 . . ? C71 C72 H72 125.1 . . ? Nb C72 H72 121.0 . . ? C72 C73 C74 107.6(3) . . ? C72 C73 Nb 75.05(19) . . ? C74 C73 Nb 73.45(19) . . ? C72 C73 H73 126.2 . . ? C74 C73 H73 126.2 . . ? Nb C73 H73 117.4 . . ? C75 C74 C73 107.7(3) . . ? C75 C74 Nb 74.22(18) . . ? C73 C74 Nb 72.25(18) . . ? C75 C74 H74 126.1 . . ? C73 C74 H74 126.1 . . ? Nb C74 H74 119.3 . . ? C74 C75 C71 109.3(3) . . ? C74 C75 Nb 72.04(18) . . ? C71 C75 Nb 74.46(17) . . ? C74 C75 H75 125.4 . . ? C71 C75 H75 125.4 . . ? Nb C75 H75 119.9 . . ? C77 Si7 C76 111.1(2) . . ? C77 Si7 C78 110.80(19) . . ? C76 Si7 C78 110.29(19) . . ? C77 Si7 C71 108.54(16) . . ? C76 Si7 C71 111.30(16) . . ? C78 Si7 C71 104.60(16) . . ? Si7 C76 H76A 109.5 . . ? Si7 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? Si7 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? Si7 C77 H77A 109.5 . . ? Si7 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? Si7 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? Si7 C78 H78A 109.5 . . ? Si7 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? Si7 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C82 C81 C86 119.5(5) . . ? C82 C81 C87 120.0(5) . . ? C86 C81 C87 120.5(4) . . ? C83 C82 C81 120.4(5) . . ? C83 C82 H82 119.8 . . ? C81 C82 H82 119.8 . . ? C82 C83 C84 122.8(5) . . ? C82 C83 H83 118.6 . . ? C84 C83 H83 118.6 . . ? C83 C84 C85 118.4(5) . . ? C83 C84 H84 120.8 . . ? C85 C84 H84 120.8 . . ? C86 C85 C84 118.0(5) . . ? C86 C85 H85 121.0 . . ? C84 C85 H85 121.0 . . ? C85 C86 C81 120.8(4) . . ? C85 C86 H86 119.6 . . ? C81 C86 H86 119.6 . . ? C81 C87 H87A 109.5 . . ? C81 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C81 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C92 C91 C93 172(2) . 2_765 ? C92 C91 C92 115.6(10) . 2_765 ? C93 C91 C92 64.5(7) 2_765 2_765 ? C92 C91 C95 64.9(7) . 2_765 ? C93 C91 C95 116.1(10) 2_765 2_765 ? C92 C91 C95 173(2) 2_765 2_765 ? C92 C91 C91 60.7(7) . 2_765 ? C93 C91 C91 118.9(11) 2_765 2_765 ? C92 C91 C91 54.9(7) 2_765 2_765 ? C95 C91 C91 125.0(11) 2_765 2_765 ? C92 C91 C94 122.4(10) . 2_765 ? C93 C91 C94 58.1(6) 2_765 2_765 ? C92 C91 C94 121.9(9) 2_765 2_765 ? C95 C91 C94 58.0(6) 2_765 2_765 ? C91 C91 C94 176.9(13) 2_765 2_765 ? C91 C92 C91 64.4(10) . 2_765 ? C91 C92 C95 60.8(7) . 2_765 ? C91 C92 C95 124.6(10) 2_765 2_765 ? C91 C92 C93 119.5(10) . . ? C91 C92 C93 55.8(7) 2_765 . ? C95 C92 C93 165.7(17) 2_765 . ? C91 C93 C94 67.8(7) 2_765 . ? C91 C93 C92 59.7(6) 2_765 . ? C94 C93 C92 126.7(10) . . ? C93 C94 C95 110.8(8) . . ? C93 C94 C91 54.1(7) . 2_765 ? C95 C94 C91 56.8(7) . 2_765 ? C91 C95 C94 65.2(7) 2_765 . ? C91 C95 C92 54.4(6) 2_765 2_765 ? C94 C95 C92 119.2(9) . 2_765 ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.600 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.074 #===END data_simonl3 _database_code_CSD 201467 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 10' _chemical_melting_point ? _chemical_formula_moiety 'C27 H14 B Cl2 F10 N Ti, 0.5(C7 H8)' _chemical_formula_structural [TiCl2(cp){C5H4B(py)(C6F5)2}].0.5tol _chemical_formula_sum 'C30.50 H18 B Cl2 F10 N Ti' _chemical_formula_weight 718.07 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 'I 2/a' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 12.545(1) _cell_length_b 13.546(1) _cell_length_c 34.000(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.04(1) _cell_angle_gamma 90.00 _cell_volume 5755.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'bright red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16585 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5208 _reflns_number_gt 4083 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'XS (Sheldrick, 1997)' _computing_structure_refinement 'XL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'XL (Sheldrick, 1997)' _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^)+(0.0484P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5208 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.016 _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 Ti Ti 0.03414(3) 0.90778(3) 0.268143(11) 0.02637(11) Uani 1 1 d . . . C11 C 0.05470(16) 0.91796(14) 0.34319(6) 0.0253(4) Uani 1 1 d . . . C12 C 0.14219(17) 0.96419(15) 0.32561(6) 0.0301(5) Uani 1 1 d . . . H12 H 0.2130 0.9431 0.3285 0.036 Uiso 1 1 calc R . . C13 C 0.1039(2) 1.04619(17) 0.30333(7) 0.0391(6) Uani 1 1 d . . . H13 H 0.1455 1.0911 0.2907 0.047 Uiso 1 1 calc R . . C14 C -0.0084(2) 1.04861(17) 0.30342(7) 0.0402(6) Uani 1 1 d . . . H14 H -0.0547 1.0931 0.2899 0.048 Uiso 1 1 calc R . . C15 C -0.03698(17) 0.97034(15) 0.32799(6) 0.0303(5) Uani 1 1 d . . . H15 H -0.1066 0.9555 0.3334 0.036 Uiso 1 1 calc R . . B B 0.05853(18) 0.83845(17) 0.37950(7) 0.0249(5) Uani 1 1 d . . . N21 N -0.06143(13) 0.79124(12) 0.37779(5) 0.0234(4) Uani 1 1 d . . . C22 C -0.09983(17) 0.74093(15) 0.34527(6) 0.0279(5) Uani 1 1 d . . . H22 H -0.0544 0.7289 0.3256 0.034 Uiso 1 1 calc R . . C23 C -0.20344(16) 0.70676(16) 0.34000(7) 0.0319(5) Uani 1 1 d . . . H23 H -0.2273 0.6727 0.3171 0.038 Uiso 1 1 calc R . . C24 C -0.27151(17) 0.72373(16) 0.36915(7) 0.0323(5) Uani 1 1 d . . . H24 H -0.3417 0.7009 0.3664 0.039 Uiso 1 1 calc R . . C25 C -0.23346(17) 0.77490(17) 0.40227(7) 0.0374(5) Uani 1 1 d . . . H25 H -0.2779 0.7874 0.4222 0.045 Uiso 1 1 calc R . . C26 C -0.12935(17) 0.80763(16) 0.40584(7) 0.0322(5) Uani 1 1 d . . . H26 H -0.1047 0.8424 0.4284 0.039 Uiso 1 1 calc R . . C31 C 0.08012(15) 0.89204(15) 0.42345(6) 0.0254(4) Uani 1 1 d . . . C32 C 0.09061(17) 0.83292(16) 0.45720(6) 0.0304(5) Uani 1 1 d . . . F32 F 0.07441(11) 0.73441(9) 0.45362(4) 0.0411(3) Uani 1 1 d . . . C33 C 0.11311(17) 0.86706(17) 0.49531(6) 0.0331(5) Uani 1 1 d . . . F33 F 0.12211(12) 0.80538(11) 0.52638(4) 0.0492(4) Uani 1 1 d . . . C34 C 0.12540(16) 0.96708(18) 0.50114(7) 0.0333(5) Uani 1 1 d . . . F34 F 0.14584(10) 1.00351(11) 0.53806(4) 0.0439(3) Uani 1 1 d . . . C35 C 0.11521(17) 1.02941(16) 0.46926(7) 0.0323(5) Uani 1 1 d . . . F35 F 0.12637(11) 1.12776(10) 0.47527(4) 0.0468(4) Uani 1 1 d . . . C36 C 0.09338(16) 0.99207(15) 0.43144(6) 0.0278(5) Uani 1 1 d . . . F36 F 0.08440(11) 1.05911(9) 0.40209(4) 0.0401(3) Uani 1 1 d . . . C41 C 0.15374(16) 0.75413(15) 0.37919(6) 0.0251(4) Uani 1 1 d . . . C42 C 0.26012(17) 0.78399(16) 0.38431(6) 0.0287(5) Uani 1 1 d . . . F42 F 0.28431(9) 0.88156(9) 0.38848(4) 0.0360(3) Uani 1 1 d . . . C43 C 0.34708(18) 0.72071(18) 0.38626(7) 0.0359(5) Uani 1 1 d . . . F43 F 0.44800(10) 0.75706(11) 0.39068(4) 0.0503(4) Uani 1 1 d . . . C44 C 0.33022(19) 0.62094(18) 0.38430(7) 0.0390(6) Uani 1 1 d . . . F44 F 0.41291(12) 0.55798(12) 0.38649(5) 0.0583(4) Uani 1 1 d . . . C45 C 0.2272(2) 0.58691(16) 0.38031(7) 0.0376(5) Uani 1 1 d . . . F45 F 0.20812(13) 0.48864(10) 0.37851(5) 0.0581(4) Uani 1 1 d . . . C46 C 0.14245(18) 0.65243(16) 0.37788(6) 0.0312(5) Uani 1 1 d . . . F46 F 0.04369(11) 0.61033(9) 0.37552(4) 0.0429(3) Uani 1 1 d . . . Cl5 Cl 0.11110(4) 0.75103(4) 0.282017(15) 0.02940(13) Uani 1 1 d . . . C61 C -0.0207(2) 0.9642(2) 0.20279(7) 0.0521(7) Uani 1 1 d . . . H61 H -0.0917 0.9813 0.1958 0.063 Uiso 1 1 calc R . . C62 C 0.0582(2) 1.0274(2) 0.21873(8) 0.0487(7) Uani 1 1 d . . . H62 H 0.0497 1.0940 0.2243 0.058 Uiso 1 1 calc R . . C63 C 0.15476(19) 0.97212(19) 0.22509(7) 0.0400(6) Uani 1 1 d . . . H63 H 0.2203 0.9956 0.2361 0.048 Uiso 1 1 calc R . . C64 C 0.13291(18) 0.87656(18) 0.21178(7) 0.0361(5) Uani 1 1 d . . . H64 H 0.1824 0.8255 0.2115 0.043 Uiso 1 1 calc R . . C65 C 0.02381(19) 0.8701(2) 0.19890(7) 0.0428(6) Uani 1 1 d . . . H65 H -0.0124 0.8138 0.1895 0.051 Uiso 1 1 calc R . . Cl7 Cl -0.14444(4) 0.84840(5) 0.260210(17) 0.03999(16) Uani 1 1 d . . . C81 C 0.1764(6) 0.4163(5) 0.4851(2) 0.0536(17) Uiso 0.50 1 d P A -1 C82 C 0.2660(6) 0.3580(4) 0.4976(3) 0.0575(16) Uiso 0.50 1 d P A -1 H82 H 0.2623 0.2907 0.4922 0.069 Uiso 0.50 1 calc PR A -1 C83 C 0.3606(10) 0.3943(9) 0.5176(3) 0.107(4) Uiso 0.50 1 d P A -1 H83 H 0.4169 0.3523 0.5258 0.128 Uiso 0.50 1 calc PR A -1 C84 C 0.3672(8) 0.4963(7) 0.5248(3) 0.102(3) Uiso 0.50 1 d P A -1 H84 H 0.4297 0.5257 0.5360 0.122 Uiso 0.50 1 calc PR A -1 C85 C 0.2775(9) 0.5497(8) 0.5146(3) 0.116(4) Uiso 0.50 1 d P A -1 H85 H 0.2816 0.6153 0.5227 0.140 Uiso 0.50 1 calc PR A -1 C86 C 0.1828(9) 0.5247(7) 0.4947(3) 0.093(3) Uiso 0.50 1 d P A -1 H86 H 0.1281 0.5694 0.4877 0.112 Uiso 0.50 1 calc PR A -1 C87 C 0.0753(6) 0.3766(6) 0.4651(3) 0.090(2) Uiso 0.50 1 d P A -1 H87A H 0.0723 0.3911 0.4374 0.135 Uiso 0.50 1 calc PR A -1 H87B H 0.0154 0.4066 0.4761 0.135 Uiso 0.50 1 calc PR A -1 H87C H 0.0729 0.3064 0.4688 0.135 Uiso 0.50 1 calc PR A -1 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 Ti 0.02490(19) 0.0314(2) 0.0228(2) 0.00477(16) 0.00224(14) 0.00343(16) C11 0.0306(10) 0.0230(10) 0.0224(11) -0.0034(8) 0.0032(8) -0.0017(9) C12 0.0326(11) 0.0293(11) 0.0285(13) -0.0021(9) 0.0025(9) -0.0048(9) C13 0.0557(15) 0.0278(12) 0.0348(14) 0.0018(10) 0.0101(11) -0.0090(11) C14 0.0564(15) 0.0302(12) 0.0351(14) 0.0066(10) 0.0105(11) 0.0123(11) C15 0.0352(12) 0.0297(11) 0.0267(12) 0.0016(9) 0.0059(9) 0.0071(9) B 0.0273(12) 0.0225(11) 0.0247(13) -0.0031(9) 0.0015(9) -0.0018(10) N21 0.0262(8) 0.0213(8) 0.0228(10) -0.0007(7) 0.0024(7) -0.0010(7) C22 0.0318(11) 0.0281(11) 0.0237(12) -0.0019(9) 0.0021(8) -0.0032(9) C23 0.0317(11) 0.0332(12) 0.0298(13) -0.0042(9) -0.0023(9) -0.0065(10) C24 0.0264(10) 0.0307(12) 0.0396(14) 0.0001(10) 0.0023(9) -0.0024(9) C25 0.0305(11) 0.0423(13) 0.0405(14) -0.0085(11) 0.0098(10) -0.0015(10) C26 0.0327(11) 0.0346(12) 0.0297(13) -0.0100(10) 0.0053(9) -0.0025(10) C31 0.0255(10) 0.0267(11) 0.0241(12) -0.0036(9) 0.0025(8) -0.0006(9) C32 0.0355(11) 0.0290(12) 0.0267(12) -0.0036(9) 0.0024(9) 0.0025(9) F32 0.0682(9) 0.0268(7) 0.0280(7) 0.0012(5) 0.0035(6) 0.0006(6) C33 0.0332(12) 0.0423(13) 0.0237(12) -0.0032(10) 0.0015(9) 0.0047(10) F33 0.0665(9) 0.0579(9) 0.0223(8) 0.0016(6) -0.0007(6) 0.0100(7) C34 0.0205(10) 0.0519(14) 0.0276(13) -0.0165(11) 0.0025(8) -0.0005(10) F34 0.0347(7) 0.0661(9) 0.0307(8) -0.0243(7) 0.0021(5) -0.0032(7) C35 0.0266(10) 0.0322(12) 0.0392(14) -0.0152(10) 0.0087(9) -0.0075(9) F35 0.0572(9) 0.0356(7) 0.0497(9) -0.0213(6) 0.0167(7) -0.0164(7) C36 0.0267(10) 0.0289(11) 0.0282(12) -0.0029(9) 0.0049(8) -0.0020(9) F36 0.0592(9) 0.0240(6) 0.0377(8) -0.0032(6) 0.0073(6) -0.0062(6) C41 0.0320(11) 0.0265(11) 0.0163(10) -0.0017(8) -0.0008(8) 0.0016(9) C42 0.0329(11) 0.0278(11) 0.0253(12) -0.0037(9) 0.0030(9) 0.0037(9) F42 0.0292(6) 0.0334(7) 0.0445(8) -0.0028(6) -0.0015(5) -0.0038(5) C43 0.0317(12) 0.0488(14) 0.0269(13) -0.0006(10) 0.0019(9) 0.0078(11) F43 0.0284(7) 0.0676(10) 0.0547(10) -0.0006(8) 0.0023(6) 0.0096(7) C44 0.0448(14) 0.0440(14) 0.0285(13) -0.0016(11) 0.0041(10) 0.0248(12) F44 0.0601(10) 0.0604(10) 0.0549(10) 0.0014(8) 0.0073(7) 0.0379(8) C45 0.0577(15) 0.0245(12) 0.0300(13) -0.0042(10) 0.0004(10) 0.0110(11) F45 0.0798(11) 0.0256(7) 0.0677(11) -0.0055(7) -0.0004(8) 0.0137(7) C46 0.0393(12) 0.0278(11) 0.0258(12) -0.0017(9) -0.0006(9) 0.0012(10) F46 0.0455(8) 0.0246(7) 0.0570(10) -0.0027(6) -0.0041(6) -0.0040(6) Cl5 0.0327(3) 0.0303(3) 0.0254(3) -0.0003(2) 0.0033(2) 0.0048(2) C61 0.0405(14) 0.088(2) 0.0284(14) 0.0245(14) 0.0060(11) 0.0207(15) C62 0.0705(18) 0.0454(15) 0.0331(15) 0.0198(12) 0.0204(13) 0.0140(14) C63 0.0381(13) 0.0526(15) 0.0305(13) 0.0128(11) 0.0092(10) -0.0052(12) C64 0.0378(12) 0.0481(14) 0.0234(12) 0.0064(10) 0.0091(9) 0.0080(11) C65 0.0419(13) 0.0693(17) 0.0170(12) 0.0028(11) 0.0011(9) -0.0037(13) Cl7 0.0249(3) 0.0624(4) 0.0320(3) 0.0050(3) -0.0014(2) -0.0011(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 Ti C14 2.340(2) . ? Ti C13 2.351(2) . ? Ti C63 2.362(2) . ? Ti Cl5 2.3629(6) . ? Ti C62 2.372(2) . ? Ti Cl7 2.3733(7) . ? Ti C61 2.393(2) . ? Ti C65 2.401(2) . ? Ti C12 2.403(2) . ? Ti C64 2.409(2) . ? Ti C15 2.444(2) . ? Ti C11 2.546(2) . ? C11 C15 1.410(3) . ? C11 C12 1.439(3) . ? C11 B 1.636(3) . ? C12 C13 1.405(3) . ? C12 H12 0.9300 . ? C13 C14 1.409(3) . ? C13 H13 0.9300 . ? C14 C15 1.415(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? B N21 1.632(3) . ? B C41 1.653(3) . ? B C31 1.662(3) . ? N21 C22 1.351(3) . ? N21 C26 1.352(3) . ? C22 C23 1.377(3) . ? C22 H22 0.9300 . ? C23 C24 1.383(3) . ? C23 H23 0.9300 . ? C24 C25 1.372(3) . ? C24 H24 0.9300 . ? C25 C26 1.374(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C36 1.389(3) . ? C31 C32 1.396(3) . ? C32 F32 1.354(2) . ? C32 C33 1.381(3) . ? C33 F33 1.344(3) . ? C33 C34 1.376(3) . ? C34 F34 1.352(2) . ? C34 C35 1.371(3) . ? C35 F35 1.353(2) . ? C35 C36 1.387(3) . ? C36 F36 1.346(2) . ? C41 C46 1.385(3) . ? C41 C42 1.391(3) . ? C42 F42 1.361(2) . ? C42 C43 1.384(3) . ? C43 F43 1.354(3) . ? C43 C44 1.369(3) . ? C44 F44 1.340(3) . ? C44 C45 1.368(4) . ? C45 F45 1.353(3) . ? C45 C46 1.382(3) . ? C46 F46 1.360(3) . ? C61 C62 1.382(4) . ? C61 C65 1.403(4) . ? C61 H61 0.9300 . ? C62 C63 1.424(4) . ? C62 H62 0.9300 . ? C63 C64 1.391(4) . ? C63 H63 0.9300 . ? C64 C65 1.403(3) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C81 C82 1.408(10) . ? C81 C87 1.487(11) . ? C81 C86 1.504(12) . ? C82 C83 1.404(14) . ? C82 H82 0.9300 . ? C83 C84 1.404(14) . ? C83 H83 0.9300 . ? C84 C85 1.357(15) . ? C84 H84 0.9300 . ? C85 C86 1.358(12) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? 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 C14 Ti C13 34.96(9) . . ? C14 Ti C63 101.77(9) . . ? C13 Ti C63 77.94(9) . . ? C14 Ti Cl5 137.55(6) . . ? C13 Ti Cl5 119.18(6) . . ? C63 Ti Cl5 100.51(6) . . ? C14 Ti C62 81.67(9) . . ? C13 Ti C62 75.59(10) . . ? C63 Ti C62 35.02(9) . . ? Cl5 Ti C62 132.84(7) . . ? C14 Ti Cl7 94.55(7) . . ? C13 Ti Cl7 129.31(6) . . ? C63 Ti Cl7 134.77(7) . . ? Cl5 Ti Cl7 94.78(2) . . ? C62 Ti Cl7 109.17(8) . . ? C14 Ti C61 98.95(10) . . ? C13 Ti C61 106.36(10) . . ? C63 Ti C61 56.94(9) . . ? Cl5 Ti C61 123.48(8) . . ? C62 Ti C61 33.73(10) . . ? Cl7 Ti C61 79.11(7) . . ? C14 Ti C65 132.91(9) . . ? C13 Ti C65 130.84(9) . . ? C63 Ti C65 56.86(9) . . ? Cl5 Ti C65 89.46(7) . . ? C62 Ti C65 56.63(10) . . ? Cl7 Ti C65 81.23(6) . . ? C61 Ti C65 34.03(10) . . ? C14 Ti C12 57.42(8) . . ? C13 Ti C12 34.36(8) . . ? C63 Ti C12 92.30(8) . . ? Cl5 Ti C12 86.10(6) . . ? C62 Ti C12 105.13(9) . . ? Cl7 Ti C12 131.28(5) . . ? C61 Ti C12 138.52(10) . . ? C65 Ti C12 147.44(8) . . ? C14 Ti C64 135.00(8) . . ? C13 Ti C64 110.50(8) . . ? C63 Ti C64 33.87(8) . . ? Cl5 Ti C64 76.78(6) . . ? C62 Ti C64 56.65(8) . . ? Cl7 Ti C64 113.36(6) . . ? C61 Ti C64 56.19(8) . . ? C65 Ti C64 33.90(8) . . ? C12 Ti C64 114.19(8) . . ? C14 Ti C15 34.33(7) . . ? C13 Ti C15 56.40(8) . . ? C63 Ti C15 133.50(9) . . ? Cl5 Ti C15 108.55(5) . . ? C62 Ti C15 115.55(8) . . ? Cl7 Ti C15 78.59(6) . . ? C61 Ti C15 124.47(8) . . ? C65 Ti C15 153.86(8) . . ? C12 Ti C15 55.52(7) . . ? C64 Ti C15 166.90(8) . . ? C14 Ti C11 56.61(7) . . ? C13 Ti C11 56.38(7) . . ? C63 Ti C11 125.95(8) . . ? Cl5 Ti C11 81.08(5) . . ? C62 Ti C11 131.68(9) . . ? Cl7 Ti C11 98.27(5) . . ? C61 Ti C11 155.36(9) . . ? C65 Ti C11 170.46(8) . . ? C12 Ti C11 33.64(7) . . ? C64 Ti C11 142.46(7) . . ? C15 Ti C11 32.76(7) . . ? C15 C11 C12 104.83(18) . . ? C15 C11 B 125.23(18) . . ? C12 C11 B 128.85(19) . . ? C15 C11 Ti 69.65(12) . . ? C12 C11 Ti 67.72(11) . . ? B C11 Ti 135.59(13) . . ? C13 C12 C11 109.3(2) . . ? C13 C12 Ti 70.82(13) . . ? C11 C12 Ti 78.64(12) . . ? C13 C12 H12 125.3 . . ? C11 C12 H12 125.3 . . ? Ti C12 H12 117.0 . . ? C12 C13 C14 108.2(2) . . ? C12 C13 Ti 74.83(13) . . ? C14 C13 Ti 72.07(14) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? Ti C13 H13 119.0 . . ? C13 C14 C15 106.8(2) . . ? C13 C14 Ti 72.97(13) . . ? C15 C14 Ti 76.87(13) . . ? C13 C14 H14 126.6 . . ? C15 C14 H14 126.6 . . ? Ti C14 H14 115.9 . . ? C11 C15 C14 110.62(19) . . ? C11 C15 Ti 77.60(12) . . ? C14 C15 Ti 68.80(12) . . ? C11 C15 H15 124.7 . . ? C14 C15 H15 124.7 . . ? Ti C15 H15 120.4 . . ? N21 B C11 105.39(16) . . ? N21 B C41 113.17(16) . . ? C11 B C41 115.06(16) . . ? N21 B C31 106.27(15) . . ? C11 B C31 112.50(17) . . ? C41 B C31 104.28(16) . . ? C22 N21 C26 117.30(17) . . ? C22 N21 B 119.24(16) . . ? C26 N21 B 123.16(17) . . ? N21 C22 C23 122.76(19) . . ? N21 C22 H22 118.6 . . ? C23 C22 H22 118.6 . . ? C22 C23 C24 119.1(2) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 118.7(2) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 119.7(2) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N21 C26 C25 122.5(2) . . ? N21 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C36 C31 C32 113.44(19) . . ? C36 C31 B 127.52(18) . . ? C32 C31 B 118.99(18) . . ? F32 C32 C33 115.55(19) . . ? F32 C32 C31 119.27(18) . . ? C33 C32 C31 125.1(2) . . ? F33 C33 C34 119.9(2) . . ? F33 C33 C32 121.7(2) . . ? C34 C33 C32 118.4(2) . . ? F34 C34 C35 120.4(2) . . ? F34 C34 C33 120.2(2) . . ? C35 C34 C33 119.4(2) . . ? F35 C35 C34 119.1(2) . . ? F35 C35 C36 120.6(2) . . ? C34 C35 C36 120.4(2) . . ? F36 C36 C35 115.97(19) . . ? F36 C36 C31 120.81(18) . . ? C35 C36 C31 123.2(2) . . ? C46 C41 C42 112.80(19) . . ? C46 C41 B 127.98(19) . . ? C42 C41 B 118.95(18) . . ? F42 C42 C43 115.40(19) . . ? F42 C42 C41 119.89(18) . . ? C43 C42 C41 124.7(2) . . ? F43 C43 C44 120.2(2) . . ? F43 C43 C42 120.3(2) . . ? C44 C43 C42 119.4(2) . . ? F44 C44 C45 120.8(2) . . ? F44 C44 C43 120.7(2) . . ? C45 C44 C43 118.6(2) . . ? F45 C45 C44 119.9(2) . . ? F45 C45 C46 119.8(2) . . ? C44 C45 C46 120.3(2) . . ? F46 C46 C45 115.23(19) . . ? F46 C46 C41 120.60(19) . . ? C45 C46 C41 124.1(2) . . ? C62 C61 C65 108.8(2) . . ? C62 C61 Ti 72.30(14) . . ? C65 C61 Ti 73.31(14) . . ? C62 C61 H61 125.6 . . ? C65 C61 H61 125.6 . . ? Ti C61 H61 120.5 . . ? C61 C62 C63 107.7(2) . . ? C61 C62 Ti 73.97(14) . . ? C63 C62 Ti 72.12(13) . . ? C61 C62 H62 126.1 . . ? C63 C62 H62 126.1 . . ? Ti C62 H62 119.6 . . ? C64 C63 C62 107.4(2) . . ? C64 C63 Ti 74.91(13) . . ? C62 C63 Ti 72.86(13) . . ? C64 C63 H63 126.3 . . ? C62 C63 H63 126.3 . . ? Ti C63 H63 118.0 . . ? C63 C64 C65 108.6(2) . . ? C63 C64 Ti 71.22(13) . . ? C65 C64 Ti 72.74(12) . . ? C63 C64 H64 125.7 . . ? C65 C64 H64 125.7 . . ? Ti C64 H64 122.0 . . ? C64 C65 C61 107.4(2) . . ? C64 C65 Ti 73.36(13) . . ? C61 C65 Ti 72.67(14) . . ? C64 C65 H65 126.3 . . ? C61 C65 H65 126.3 . . ? Ti C65 H65 119.6 . . ? C82 C81 C87 124.2(6) . . ? C82 C81 C86 117.2(7) . . ? C87 C81 C86 118.6(7) . . ? C83 C82 C81 124.6(8) . . ? C83 C82 H82 117.7 . . ? C81 C82 H82 117.7 . . ? C82 C83 C84 117.6(11) . . ? C82 C83 H83 121.2 . . ? C84 C83 H83 121.2 . . ? C85 C84 C83 116.4(11) . . ? C85 C84 H84 121.8 . . ? C83 C84 H84 121.8 . . ? C84 C85 C86 131.6(12) . . ? C84 C85 H85 114.2 . . ? C86 C85 H85 114.2 . . ? C85 C86 C81 112.3(10) . . ? C85 C86 H86 123.9 . . ? C81 C86 H86 123.9 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.259 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.052 #===END data_simonl2 _database_code_CSD 201468 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 14' _chemical_melting_point ? _chemical_formula_structural [TiCl3{C5H4B(Py)(C6F5)2}].tol _chemical_formula_moiety 'C22 H9 B Cl3 F10 N Ti, C7 H8' _chemical_formula_sum 'C29 H17 B Cl3 F10 N Ti' _chemical_formula_weight 734.50 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Ti Ti 0.2776 0.4457 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.799(1) _cell_length_b 13.523(1) _cell_length_c 13.626(3) _cell_angle_alpha 107.44(1) _cell_angle_beta 92.97(1) _cell_angle_gamma 103.27(1) _cell_volume 1492.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'diamond-shaped prisms' _exptl_crystal_colour red-brown _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8342 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.45 _reflns_number_total 4926 _reflns_number_gt 4224 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'XS (Sheldrick, 1990)' _computing_structure_refinement 'XL (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'XL (Sheldrick, 1993)' _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^)+(0.0459P)^2^+0.2987P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4926 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 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 Ti Ti 0.11896(4) 0.77186(3) 0.34134(3) 0.02889(12) Uani 1 1 d . . . C11 C 0.3711(2) 0.81621(15) 0.28048(15) 0.0272(4) Uani 1 1 d . . . C12 C 0.2987(2) 0.90407(16) 0.29697(17) 0.0334(5) Uani 1 1 d . . . H12 H 0.2661 0.9300 0.2457 0.040 Uiso 1 1 calc R . . C13 C 0.2853(3) 0.94468(17) 0.40382(18) 0.0391(5) Uani 1 1 d . . . H13 H 0.2460 1.0031 0.4351 0.047 Uiso 1 1 calc R . . C14 C 0.3420(3) 0.88101(18) 0.45456(17) 0.0377(5) Uani 1 1 d . . . H14 H 0.3448 0.8888 0.5249 0.045 Uiso 1 1 calc R . . C15 C 0.3940(2) 0.80298(17) 0.37891(15) 0.0307(4) Uani 1 1 d . . . H15 H 0.4368 0.7507 0.3920 0.037 Uiso 1 1 calc R . . B B 0.4390(3) 0.75389(17) 0.17590(17) 0.0257(4) Uani 1 1 d . . . N21 N 0.45377(18) 0.64148(13) 0.19041(12) 0.0253(3) Uani 1 1 d . . . C22 C 0.3227(2) 0.56638(15) 0.19342(15) 0.0276(4) Uani 1 1 d . . . H22 H 0.2243 0.5783 0.1820 0.033 Uiso 1 1 calc R . . C23 C 0.3311(3) 0.47337(16) 0.21275(16) 0.0331(5) Uani 1 1 d . . . H23 H 0.2395 0.4232 0.2135 0.040 Uiso 1 1 calc R . . C24 C 0.4772(3) 0.45488(17) 0.23120(16) 0.0354(5) Uani 1 1 d . . . H24 H 0.4849 0.3918 0.2429 0.042 Uiso 1 1 calc R . . C25 C 0.6111(3) 0.53259(18) 0.23179(17) 0.0358(5) Uani 1 1 d . . . H25 H 0.7105 0.5234 0.2461 0.043 Uiso 1 1 calc R . . C26 C 0.5954(2) 0.62391(16) 0.21096(16) 0.0307(4) Uani 1 1 d . . . H26 H 0.6860 0.6754 0.2111 0.037 Uiso 1 1 calc R . . C31 C 0.6180(2) 0.82040(15) 0.16690(15) 0.0270(4) Uani 1 1 d . . . C32 C 0.6838(2) 0.78618(16) 0.07517(15) 0.0299(4) Uani 1 1 d . . . F32 F 0.60780(14) 0.69229(10) 0.00098(9) 0.0382(3) Uani 1 1 d . . . C33 C 0.8254(2) 0.83975(18) 0.05541(16) 0.0329(5) Uani 1 1 d . . . F33 F 0.88034(15) 0.80174(12) -0.03550(10) 0.0468(3) Uani 1 1 d . . . C34 C 0.9134(2) 0.93180(18) 0.12977(18) 0.0353(5) Uani 1 1 d . . . F34 F 1.05388(15) 0.98499(12) 0.11262(11) 0.0494(4) Uani 1 1 d . . . C35 C 0.8566(3) 0.96894(17) 0.22204(17) 0.0355(5) Uani 1 1 d . . . F35 F 0.94068(16) 1.05879(11) 0.29594(11) 0.0524(4) Uani 1 1 d . . . C36 C 0.7119(2) 0.91335(16) 0.23865(15) 0.0307(4) Uani 1 1 d . . . F36 F 0.66482(15) 0.95636(10) 0.33132(9) 0.0420(3) Uani 1 1 d . . . C41 C 0.3306(2) 0.74078(15) 0.06732(15) 0.0264(4) Uani 1 1 d . . . C42 C 0.3296(2) 0.83318(16) 0.04290(16) 0.0312(4) Uani 1 1 d . . . F42 F 0.41663(15) 0.93034(9) 0.10753(9) 0.0369(3) Uani 1 1 d . . . C43 C 0.2487(3) 0.83635(19) -0.04560(17) 0.0373(5) Uani 1 1 d . . . F43 F 0.25663(18) 0.93035(12) -0.06244(11) 0.0509(4) Uani 1 1 d . . . C44 C 0.1601(3) 0.7421(2) -0.11605(16) 0.0387(5) Uani 1 1 d . . . F44 F 0.07663(17) 0.74246(13) -0.20212(11) 0.0540(4) Uani 1 1 d . . . C45 C 0.1558(2) 0.64762(18) -0.09717(16) 0.0345(5) Uani 1 1 d . . . F45 F 0.06795(16) 0.55418(11) -0.16585(10) 0.0458(3) Uani 1 1 d . . . C46 C 0.2415(2) 0.64710(16) -0.00916(15) 0.0288(4) Uani 1 1 d . . . F46 F 0.23561(15) 0.54919(9) -0.00159(9) 0.0388(3) Uani 1 1 d . . . Cl5 Cl 0.00142(6) 0.70293(4) 0.17631(4) 0.03317(14) Uani 1 1 d . . . Cl6 Cl -0.06319(7) 0.84491(5) 0.42225(5) 0.04463(16) Uani 1 1 d . . . Cl7 Cl 0.09866(6) 0.62635(4) 0.39153(4) 0.03775(15) Uani 1 1 d . . . C81 C 0.6583(4) 0.6951(2) 0.6074(2) 0.0597(8) Uani 1 1 d . . . C82 C 0.4992(5) 0.6702(3) 0.5701(2) 0.0694(9) Uani 1 1 d . . . H82 H 0.4598 0.6168 0.5069 0.083 Uiso 1 1 calc R . . C83 C 0.3994(4) 0.7235(3) 0.6253(3) 0.0686(9) Uani 1 1 d . . . H83 H 0.2933 0.7056 0.5993 0.082 Uiso 1 1 calc R . . C84 C 0.4558(3) 0.8033(2) 0.7192(2) 0.0558(7) Uani 1 1 d . . . H84 H 0.3883 0.8397 0.7562 0.067 Uiso 1 1 calc R . . C85 C 0.6118(3) 0.8285(2) 0.7573(2) 0.0551(7) Uani 1 1 d . . . H85 H 0.6502 0.8816 0.8209 0.066 Uiso 1 1 calc R . . C86 C 0.7123(3) 0.7750(2) 0.7017(2) 0.0556(7) Uani 1 1 d . . . H86 H 0.8181 0.7932 0.7282 0.067 Uiso 1 1 calc R . . C87 C 0.7710(6) 0.6365(3) 0.5497(3) 0.1068(16) Uani 1 1 d . . . H87A H 0.7298 0.6051 0.4775 0.160 Uiso 1 1 calc R . . H87B H 0.7829 0.5812 0.5778 0.160 Uiso 1 1 calc R . . H87C H 0.8715 0.6862 0.5573 0.160 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 Ti 0.0238(2) 0.0334(2) 0.0292(2) 0.00883(15) 0.00693(15) 0.00755(15) C11 0.0184(9) 0.0296(10) 0.0285(10) 0.0047(7) 0.0026(8) 0.0027(7) C12 0.0299(11) 0.0301(11) 0.0390(12) 0.0094(8) 0.0109(9) 0.0064(8) C13 0.0353(12) 0.0299(11) 0.0456(13) 0.0032(9) 0.0146(10) 0.0055(9) C14 0.0316(12) 0.0425(12) 0.0283(10) 0.0013(9) 0.0051(9) 0.0016(9) C15 0.0224(10) 0.0377(11) 0.0287(10) 0.0081(8) 0.0022(8) 0.0049(8) B 0.0226(11) 0.0267(11) 0.0261(11) 0.0066(8) 0.0046(9) 0.0054(8) N21 0.0214(8) 0.0289(9) 0.0244(8) 0.0070(6) 0.0044(7) 0.0064(6) C22 0.0241(10) 0.0288(10) 0.0281(10) 0.0075(7) 0.0038(8) 0.0055(7) C23 0.0318(11) 0.0322(11) 0.0345(11) 0.0113(8) 0.0072(9) 0.0054(8) C24 0.0411(13) 0.0346(12) 0.0364(11) 0.0153(9) 0.0094(10) 0.0148(9) C25 0.0303(11) 0.0442(13) 0.0402(12) 0.0183(9) 0.0081(9) 0.0162(9) C26 0.0240(10) 0.0362(11) 0.0343(11) 0.0138(8) 0.0058(9) 0.0087(8) C31 0.0220(10) 0.0296(10) 0.0292(10) 0.0094(8) 0.0028(8) 0.0063(7) C32 0.0248(10) 0.0335(11) 0.0299(10) 0.0082(8) 0.0024(8) 0.0076(8) F32 0.0303(7) 0.0421(7) 0.0327(6) 0.0004(5) 0.0068(5) 0.0060(5) C33 0.0256(11) 0.0460(13) 0.0333(11) 0.0178(9) 0.0098(9) 0.0129(9) F33 0.0346(7) 0.0693(9) 0.0398(7) 0.0189(6) 0.0180(6) 0.0152(6) C34 0.0208(10) 0.0416(12) 0.0483(13) 0.0239(10) 0.0060(9) 0.0045(8) F34 0.0283(7) 0.0575(9) 0.0638(9) 0.0298(7) 0.0128(7) -0.0017(6) C35 0.0277(11) 0.0334(11) 0.0410(12) 0.0109(9) 0.0000(9) 0.0018(8) F35 0.0381(8) 0.0413(8) 0.0580(9) 0.0044(6) 0.0013(7) -0.0114(6) C36 0.0270(11) 0.0327(11) 0.0306(10) 0.0080(8) 0.0054(9) 0.0067(8) F36 0.0343(7) 0.0415(7) 0.0346(7) -0.0036(5) 0.0068(6) 0.0001(5) C41 0.0192(9) 0.0329(11) 0.0281(10) 0.0098(8) 0.0061(8) 0.0079(7) C42 0.0283(11) 0.0329(11) 0.0335(11) 0.0111(8) 0.0073(9) 0.0087(8) F42 0.0392(7) 0.0302(7) 0.0423(7) 0.0139(5) 0.0055(6) 0.0079(5) C43 0.0382(12) 0.0470(14) 0.0405(12) 0.0250(10) 0.0124(10) 0.0218(10) F43 0.0602(10) 0.0570(9) 0.0537(8) 0.0351(7) 0.0114(7) 0.0263(7) C44 0.0317(12) 0.0640(15) 0.0280(11) 0.0181(10) 0.0046(9) 0.0221(11) F44 0.0480(9) 0.0874(11) 0.0371(7) 0.0259(7) -0.0016(6) 0.0314(8) C45 0.0234(11) 0.0483(13) 0.0281(10) 0.0066(9) 0.0017(9) 0.0098(9) F45 0.0349(7) 0.0552(8) 0.0343(7) 0.0006(6) -0.0085(6) 0.0078(6) C46 0.0245(10) 0.0333(11) 0.0292(10) 0.0095(8) 0.0052(8) 0.0088(8) F46 0.0432(8) 0.0313(7) 0.0345(6) 0.0050(5) -0.0044(6) 0.0048(5) Cl5 0.0235(3) 0.0435(3) 0.0332(3) 0.0133(2) 0.0032(2) 0.0088(2) Cl6 0.0371(3) 0.0511(3) 0.0485(3) 0.0122(3) 0.0191(3) 0.0189(2) Cl7 0.0380(3) 0.0408(3) 0.0363(3) 0.0165(2) 0.0065(2) 0.0079(2) C81 0.076(2) 0.0626(18) 0.0615(17) 0.0409(14) 0.0337(16) 0.0250(15) C82 0.095(3) 0.075(2) 0.0372(14) 0.0246(13) -0.0050(16) 0.0125(18) C83 0.0487(17) 0.095(2) 0.072(2) 0.0474(19) -0.0082(16) 0.0128(16) C84 0.0529(17) 0.0681(19) 0.0652(18) 0.0394(15) 0.0177(14) 0.0254(14) C85 0.0544(17) 0.0411(14) 0.0677(18) 0.0182(12) 0.0040(14) 0.0078(11) C86 0.0395(15) 0.0458(15) 0.085(2) 0.0314(14) 0.0117(14) 0.0026(11) C87 0.153(4) 0.099(3) 0.116(3) 0.065(3) 0.097(3) 0.068(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 Ti Cl6 2.2399(7) . ? Ti Cl7 2.2426(7) . ? Ti Cl5 2.2483(8) . ? Ti C14 2.324(2) . ? Ti C13 2.332(2) . ? Ti C12 2.348(2) . ? Ti C15 2.360(2) . ? Ti C11 2.4182(19) . ? C11 C15 1.415(3) . ? C11 C12 1.439(3) . ? C11 B 1.642(3) . ? C12 C13 1.416(3) . ? C12 H12 0.9300 . ? C13 C14 1.409(3) . ? C13 H13 0.9300 . ? C14 C15 1.415(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? B N21 1.623(3) . ? B C31 1.656(3) . ? B C41 1.658(3) . ? N21 C26 1.352(3) . ? N21 C22 1.362(2) . ? C22 C23 1.377(3) . ? C22 H22 0.9300 . ? C23 C24 1.389(3) . ? C23 H23 0.9300 . ? C24 C25 1.385(3) . ? C24 H24 0.9300 . ? C25 C26 1.382(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C36 1.386(3) . ? C31 C32 1.401(3) . ? C32 F32 1.361(2) . ? C32 C33 1.373(3) . ? C33 F33 1.352(2) . ? C33 C34 1.377(3) . ? C34 F34 1.350(2) . ? C34 C35 1.373(3) . ? C35 F35 1.347(2) . ? C35 C36 1.389(3) . ? C36 F36 1.353(2) . ? C41 C42 1.388(3) . ? C41 C46 1.405(3) . ? C42 F42 1.365(2) . ? C42 C43 1.385(3) . ? C43 F43 1.345(3) . ? C43 C44 1.374(3) . ? C44 F44 1.353(3) . ? C44 C45 1.370(3) . ? C45 F45 1.356(2) . ? C45 C46 1.386(3) . ? C46 F46 1.348(2) . ? C81 C86 1.383(4) . ? C81 C82 1.393(5) . ? C81 C87 1.515(4) . ? C82 C83 1.375(5) . ? C82 H82 0.9300 . ? C83 C84 1.382(5) . ? C83 H83 0.9300 . ? C84 C85 1.370(4) . ? C84 H84 0.9300 . ? C85 C86 1.383(4) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? 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 Cl6 Ti Cl7 102.32(3) . . ? Cl6 Ti Cl5 101.51(3) . . ? Cl7 Ti Cl5 103.11(3) . . ? Cl6 Ti C14 99.03(6) . . ? Cl7 Ti C14 97.73(7) . . ? Cl5 Ti C14 146.70(6) . . ? Cl6 Ti C13 85.69(6) . . ? Cl7 Ti C13 132.63(7) . . ? Cl5 Ti C13 121.13(6) . . ? C14 Ti C13 35.24(9) . . ? Cl6 Ti C12 108.73(5) . . ? Cl7 Ti C12 143.10(6) . . ? Cl5 Ti C12 89.92(6) . . ? C14 Ti C12 58.58(8) . . ? C13 Ti C12 35.21(7) . . ? Cl6 Ti C15 134.09(5) . . ? Cl7 Ti C15 86.38(6) . . ? Cl5 Ti C15 120.49(5) . . ? C14 Ti C15 35.16(7) . . ? C13 Ti C15 58.07(8) . . ? C12 Ti C15 57.71(8) . . ? Cl6 Ti C11 142.70(5) . . ? Cl7 Ti C11 109.55(5) . . ? Cl5 Ti C11 89.85(5) . . ? C14 Ti C11 58.52(7) . . ? C13 Ti C11 58.53(7) . . ? C12 Ti C11 35.10(7) . . ? C15 Ti C11 34.44(7) . . ? C15 C11 C12 105.49(17) . . ? C15 C11 B 125.24(18) . . ? C12 C11 B 128.71(18) . . ? C15 C11 Ti 70.53(11) . . ? C12 C11 Ti 69.78(11) . . ? B C11 Ti 130.59(13) . . ? C13 C12 C11 108.9(2) . . ? C13 C12 Ti 71.76(12) . . ? C11 C12 Ti 75.12(11) . . ? C13 C12 H12 125.5 . . ? C11 C12 H12 125.5 . . ? Ti C12 H12 119.4 . . ? C14 C13 C12 108.02(18) . . ? C14 C13 Ti 72.09(12) . . ? C12 C13 Ti 73.02(12) . . ? C14 C13 H13 126.0 . . ? C12 C13 H13 126.0 . . ? Ti C13 H13 120.7 . . ? C13 C14 C15 107.44(19) . . ? C13 C14 Ti 72.66(13) . . ? C15 C14 Ti 73.80(12) . . ? C13 C14 H14 126.3 . . ? C15 C14 H14 126.3 . . ? Ti C14 H14 119.2 . . ? C14 C15 C11 110.0(2) . . ? C14 C15 Ti 71.04(12) . . ? C11 C15 Ti 75.03(11) . . ? C14 C15 H15 125.0 . . ? C11 C15 H15 125.0 . . ? Ti C15 H15 120.6 . . ? N21 B C11 105.56(15) . . ? N21 B C31 107.05(15) . . ? C11 B C31 111.85(15) . . ? N21 B C41 114.56(15) . . ? C11 B C41 112.78(16) . . ? C31 B C41 105.03(15) . . ? C26 N21 C22 117.66(17) . . ? C26 N21 B 121.54(16) . . ? C22 N21 B 120.42(16) . . ? N21 C22 C23 122.12(19) . . ? N21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C22 C23 C24 119.7(2) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 118.5(2) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C26 C25 C24 119.3(2) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? N21 C26 C25 122.72(19) . . ? N21 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C36 C31 C32 113.47(17) . . ? C36 C31 B 127.45(16) . . ? C32 C31 B 118.95(17) . . ? F32 C32 C33 116.49(17) . . ? F32 C32 C31 119.28(17) . . ? C33 C32 C31 124.19(19) . . ? F33 C33 C32 120.6(2) . . ? F33 C33 C34 119.79(18) . . ? C32 C33 C34 119.62(18) . . ? F34 C34 C35 120.2(2) . . ? F34 C34 C33 120.67(19) . . ? C35 C34 C33 119.11(19) . . ? F35 C35 C34 120.15(19) . . ? F35 C35 C36 120.25(19) . . ? C34 C35 C36 119.6(2) . . ? F36 C36 C31 120.55(17) . . ? F36 C36 C35 115.47(18) . . ? C31 C36 C35 123.98(18) . . ? C42 C41 C46 112.85(18) . . ? C42 C41 B 117.75(17) . . ? C46 C41 B 129.33(17) . . ? F42 C42 C43 115.02(18) . . ? F42 C42 C41 119.76(18) . . ? C43 C42 C41 125.2(2) . . ? F43 C43 C44 120.4(2) . . ? F43 C43 C42 120.5(2) . . ? C44 C43 C42 119.1(2) . . ? F44 C44 C45 120.4(2) . . ? F44 C44 C43 120.7(2) . . ? C45 C44 C43 118.9(2) . . ? F45 C45 C44 119.44(19) . . ? F45 C45 C46 120.1(2) . . ? C44 C45 C46 120.5(2) . . ? F46 C46 C45 115.30(18) . . ? F46 C46 C41 121.30(18) . . ? C45 C46 C41 123.39(19) . . ? C86 C81 C82 117.8(3) . . ? C86 C81 C87 119.8(3) . . ? C82 C81 C87 122.4(3) . . ? C83 C82 C81 121.0(3) . . ? C83 C82 H82 119.5 . . ? C81 C82 H82 119.5 . . ? C82 C83 C84 120.3(3) . . ? C82 C83 H83 119.8 . . ? C84 C83 H83 119.8 . . ? C85 C84 C83 119.5(3) . . ? C85 C84 H84 120.3 . . ? C83 C84 H84 120.3 . . ? C84 C85 C86 120.2(3) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C85 C86 C81 121.3(3) . . ? C85 C86 H86 119.4 . . ? C81 C86 H86 119.4 . . ? C81 C87 H87A 109.5 . . ? C81 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C81 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.252 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.050 #===END data_simonl4 _database_code_CSD 201469 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 15' _chemical_melting_point ? _chemical_formula_moiety 'C32 H19 B Cl3 F10 N3 Zr, 1.5(C D Cl3)' _chemical_formula_structural [Zr(py)2Cl3{C5H4B(py)(C6F5)2}].1.5(CDCl3) _chemical_formula_sum 'C33.50 H19/D1.5 B Cl7.50 F10 N3 Zr' _chemical_formula_weight 1024.4 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.201(1) _cell_length_b 18.241(1) _cell_length_c 21.174(3) _cell_angle_alpha 67.46(1) _cell_angle_beta 76.82(1) _cell_angle_gamma 84.93(1) _cell_volume 3890.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour 'clear, colourless' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2020 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22856 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.42 _reflns_number_total 13163 _reflns_number_gt 11449 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'XS (Sheldrick, 1997)' _computing_structure_refinement 'XL, SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _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^)+(0.0456P)^2^+2.2116P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13163 _refine_ls_number_parameters 1023 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _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 Zr1A Zr 0.83459(2) 0.232471(13) 0.847228(12) 0.01945(7) Uani 1 1 d . . . B1A B 0.4812(2) 0.26420(16) 0.83144(14) 0.0210(5) Uani 1 1 d . . . C11A C 0.6291(2) 0.26186(14) 0.79967(12) 0.0219(5) Uani 1 1 d . . . C12A C 0.7035(2) 0.33152(15) 0.76940(13) 0.0243(5) Uani 1 1 d . . . H12A H 0.6835 0.3782 0.7775 0.029 Uiso 1 1 calc R . . C13A C 0.8122(2) 0.31885(16) 0.72527(13) 0.0293(6) Uani 1 1 d . . . H13A H 0.8734 0.3560 0.6979 0.035 Uiso 1 1 calc R . . C14A C 0.8108(2) 0.24048(17) 0.73035(13) 0.0279(6) Uani 1 1 d . . . H14A H 0.8716 0.2157 0.7075 0.034 Uiso 1 1 calc R . . C15A C 0.7005(2) 0.20522(15) 0.77643(13) 0.0244(5) Uani 1 1 d . . . H15A H 0.6781 0.1527 0.7895 0.029 Uiso 1 1 calc R . . N21A N 0.41775(19) 0.17764(12) 0.85702(10) 0.0220(4) Uani 1 1 d . . . C22A C 0.4765(2) 0.10966(15) 0.88716(13) 0.0255(5) Uani 1 1 d . . . H22A H 0.5563 0.1123 0.8920 0.031 Uiso 1 1 calc R . . C23A C 0.4219(2) 0.03600(16) 0.91118(14) 0.0309(6) Uani 1 1 d . . . H23A H 0.4647 -0.0099 0.9317 0.037 Uiso 1 1 calc R . . C24A C 0.3032(3) 0.03129(16) 0.90439(14) 0.0322(6) Uani 1 1 d . . . H24A H 0.2657 -0.0177 0.9194 0.039 Uiso 1 1 calc R . . C25A C 0.2415(2) 0.10073(16) 0.87484(14) 0.0313(6) Uani 1 1 d . . . H25A H 0.1612 0.0991 0.8704 0.038 Uiso 1 1 calc R . . C26A C 0.3004(2) 0.17259(16) 0.85198(13) 0.0267(5) Uani 1 1 d . . . H26A H 0.2581 0.2191 0.8325 0.032 Uiso 1 1 calc R . . C31A C 0.4168(2) 0.32269(14) 0.76526(13) 0.0230(5) Uani 1 1 d . . . C32A C 0.3154(2) 0.37163(14) 0.77188(13) 0.0232(5) Uani 1 1 d . . . F32A F 0.25724(13) 0.37025(9) 0.83597(7) 0.0280(3) Uani 1 1 d . . . C33A C 0.2643(2) 0.42219(14) 0.71637(14) 0.0265(5) Uani 1 1 d . . . F33A F 0.16522(14) 0.46615(9) 0.72773(8) 0.0324(3) Uani 1 1 d . . . C34A C 0.3136(3) 0.42519(15) 0.64976(14) 0.0298(6) Uani 1 1 d . . . F34A F 0.26682(16) 0.47402(10) 0.59487(9) 0.0416(4) Uani 1 1 d . . . C35A C 0.4115(2) 0.37671(16) 0.63945(14) 0.0296(6) Uani 1 1 d . . . F35A F 0.45974(16) 0.37761(11) 0.57486(8) 0.0428(4) Uani 1 1 d . . . C36A C 0.4588(2) 0.32646(15) 0.69630(13) 0.0255(5) Uani 1 1 d . . . F36A F 0.55071(14) 0.27870(10) 0.68097(8) 0.0356(4) Uani 1 1 d . . . C41A C 0.4513(2) 0.29506(15) 0.89767(13) 0.0233(5) Uani 1 1 d . . . C42A C 0.4687(2) 0.37393(15) 0.88750(13) 0.0252(5) Uani 1 1 d . . . F42A F 0.50610(14) 0.42845(8) 0.82126(8) 0.0306(3) Uani 1 1 d . . . C43A C 0.4488(3) 0.40468(16) 0.93948(15) 0.0319(6) Uani 1 1 d . . . F43A F 0.46958(17) 0.48156(10) 0.92407(9) 0.0420(4) Uani 1 1 d . . . C44A C 0.4073(3) 0.35441(18) 1.00860(15) 0.0352(6) Uani 1 1 d . . . F44A F 0.38756(19) 0.38268(12) 1.05989(9) 0.0523(5) Uani 1 1 d . . . C45A C 0.3866(3) 0.27640(17) 1.02216(14) 0.0321(6) Uani 1 1 d . . . F45A F 0.34338(17) 0.22640(11) 1.08879(8) 0.0453(4) Uani 1 1 d . . . C46A C 0.4087(2) 0.24830(15) 0.96827(13) 0.0253(5) Uani 1 1 d . . . F46A F 0.38385(14) 0.17013(9) 0.98907(8) 0.0303(3) Uani 1 1 d . . . N51A N 0.80404(19) 0.34310(12) 0.88496(11) 0.0250(4) Uani 1 1 d . . . C52A C 0.7498(2) 0.33560(17) 0.95094(14) 0.0310(6) Uani 1 1 d . . . H52A H 0.7139 0.2872 0.9815 0.037 Uiso 1 1 calc R . . C53A C 0.7449(3) 0.39616(19) 0.97533(16) 0.0422(7) Uani 1 1 d . . . H53A H 0.7061 0.3886 1.0212 0.051 Uiso 1 1 calc R . . C54A C 0.7986(3) 0.46848(19) 0.93055(17) 0.0446(8) Uani 1 1 d . . . H54A H 0.7972 0.5101 0.9458 0.054 Uiso 1 1 calc R . . C55A C 0.8544(3) 0.47738(17) 0.86263(16) 0.0406(7) Uani 1 1 d . . . H55A H 0.8909 0.5253 0.8314 0.049 Uiso 1 1 calc R . . C56A C 0.8552(3) 0.41420(15) 0.84165(14) 0.0314(6) Uani 1 1 d . . . H56A H 0.8926 0.4209 0.7958 0.038 Uiso 1 1 calc R . . Cl6A Cl 1.04367(5) 0.29026(4) 0.78579(3) 0.02653(13) Uani 1 1 d . . . Cl7A Cl 0.92137(6) 0.10164(4) 0.84667(4) 0.03075(15) Uani 1 1 d . . . Cl8A Cl 0.68260(5) 0.16224(4) 0.95598(3) 0.02744(14) Uani 1 1 d . . . N91A N 0.95287(19) 0.19928(13) 0.94111(11) 0.0256(5) Uani 1 1 d . . . C92A C 0.9536(2) 0.12472(16) 0.98902(14) 0.0307(6) Uani 1 1 d . . . H92A H 0.9078 0.0862 0.9866 0.037 Uiso 1 1 calc R . . C93A C 1.0194(3) 0.10259(19) 1.04188(15) 0.0416(7) Uani 1 1 d . . . H93A H 1.0180 0.0503 1.0735 0.050 Uiso 1 1 calc R . . C94A C 1.0868(3) 0.1594(2) 1.04677(16) 0.0448(8) Uani 1 1 d . . . H94A H 1.1309 0.1462 1.0819 0.054 Uiso 1 1 calc R . . C95A C 1.0875(3) 0.23640(19) 0.99832(15) 0.0378(7) Uani 1 1 d . . . H95A H 1.1321 0.2758 1.0004 0.045 Uiso 1 1 calc R . . C96A C 1.0202(2) 0.25383(17) 0.94650(14) 0.0292(6) Uani 1 1 d . . . H96A H 1.0217 0.3056 0.9139 0.035 Uiso 1 1 calc R . . Zr2B Zr 0.35995(2) 0.230343(13) 0.348211(12) 0.02061(7) Uani 1 1 d . . . B1B B 0.0095(3) 0.26507(16) 0.32776(14) 0.0213(5) Uani 1 1 d . . . C11B C 0.1573(2) 0.25849(15) 0.29827(13) 0.0231(5) Uani 1 1 d . . . C12B C 0.2350(2) 0.32692(16) 0.26478(13) 0.0261(5) Uani 1 1 d . . . H12B H 0.2165 0.3757 0.2691 0.031 Uiso 1 1 calc R . . C13B C 0.3441(2) 0.30914(18) 0.22418(13) 0.0328(6) Uani 1 1 d . . . H13B H 0.4074 0.3443 0.1959 0.039 Uiso 1 1 calc R . . C14B C 0.3393(2) 0.22909(19) 0.23428(14) 0.0340(6) Uani 1 1 d . . . H14B H 0.3997 0.2012 0.2145 0.041 Uiso 1 1 calc R . . C15B C 0.2264(2) 0.19788(17) 0.27998(14) 0.0285(6) Uani 1 1 d . . . H15B H 0.2014 0.1455 0.2957 0.034 Uiso 1 1 calc R . . N21B N -0.05776(18) 0.17871(12) 0.35862(10) 0.0214(4) Uani 1 1 d . . . C22B C -0.0023(2) 0.11091(15) 0.39238(14) 0.0266(5) Uani 1 1 d . . . H22B H 0.0780 0.1130 0.3966 0.032 Uiso 1 1 calc R . . C23B C -0.0612(3) 0.03801(16) 0.42107(14) 0.0303(6) Uani 1 1 d . . . H23B H -0.0198 -0.0079 0.4431 0.036 Uiso 1 1 calc R . . C24B C -0.1812(3) 0.03386(16) 0.41678(14) 0.0310(6) Uani 1 1 d . . . H24B H -0.2220 -0.0145 0.4359 0.037 Uiso 1 1 calc R . . C25B C -0.2398(2) 0.10374(16) 0.38311(14) 0.0310(6) Uani 1 1 d . . . H25B H -0.3209 0.1028 0.3798 0.037 Uiso 1 1 calc R . . C26B C -0.1764(2) 0.17459(15) 0.35463(14) 0.0266(5) Uani 1 1 d . . . H26B H -0.2161 0.2210 0.3320 0.032 Uiso 1 1 calc R . . C31B C -0.0521(2) 0.32117(14) 0.25907(13) 0.0225(5) Uani 1 1 d . . . C32B C -0.1568(2) 0.36814(14) 0.26493(13) 0.0233(5) Uani 1 1 d . . . F32B F -0.21898(13) 0.36552(9) 0.32872(7) 0.0278(3) Uani 1 1 d . . . C33B C -0.2067(2) 0.41797(15) 0.20886(14) 0.0271(5) Uani 1 1 d . . . F33B F -0.30954(14) 0.45986(9) 0.21965(8) 0.0334(4) Uani 1 1 d . . . C34B C -0.1521(3) 0.42330(16) 0.14224(14) 0.0325(6) Uani 1 1 d . . . F34B F -0.19862(17) 0.47155(10) 0.08699(9) 0.0450(4) Uani 1 1 d . . . C35B C -0.0506(3) 0.37702(17) 0.13260(14) 0.0325(6) Uani 1 1 d . . . F35B F 0.00236(17) 0.38002(11) 0.06787(8) 0.0479(5) Uani 1 1 d . . . C36B C -0.0052(2) 0.32695(15) 0.19015(14) 0.0273(5) Uani 1 1 d . . . F36B F 0.09103(15) 0.28147(10) 0.17507(8) 0.0380(4) Uani 1 1 d . . . C41B C -0.0213(2) 0.30371(15) 0.38883(13) 0.0233(5) Uani 1 1 d . . . C42B C -0.0014(2) 0.38423(15) 0.37229(13) 0.0259(5) Uani 1 1 d . . . F42B F 0.04213(14) 0.43268(8) 0.30447(8) 0.0309(3) Uani 1 1 d . . . C43B C -0.0259(2) 0.42198(16) 0.41917(15) 0.0300(6) Uani 1 1 d . . . F43B F -0.00246(16) 0.49970(10) 0.39785(10) 0.0415(4) Uani 1 1 d . . . C44B C -0.0752(3) 0.37883(18) 0.48875(15) 0.0337(6) Uani 1 1 d . . . F44B F -0.10158(17) 0.41406(12) 0.53564(10) 0.0495(5) Uani 1 1 d . . . C45B C -0.0978(2) 0.29934(18) 0.50843(14) 0.0316(6) Uani 1 1 d . . . F45B F -0.14898(16) 0.25627(11) 0.57601(8) 0.0441(4) Uani 1 1 d . . . C46B C -0.0704(2) 0.26367(15) 0.45982(13) 0.0248(5) Uani 1 1 d . . . F46B F -0.09768(14) 0.18529(9) 0.48598(8) 0.0309(3) Uani 1 1 d . . . N51B N 0.33984(19) 0.35123(12) 0.37141(11) 0.0232(4) Uani 1 1 d . . . C52B C 0.2735(2) 0.35615(16) 0.43138(14) 0.0285(6) Uani 1 1 d . . . H52B H 0.2279 0.3122 0.4639 0.034 Uiso 1 1 calc R . . C53B C 0.2701(3) 0.42395(17) 0.44671(15) 0.0358(6) Uani 1 1 d . . . H53B H 0.2226 0.4252 0.4885 0.043 Uiso 1 1 calc R . . C54B C 0.3379(3) 0.48939(16) 0.39951(15) 0.0349(6) Uani 1 1 d . . . H54B H 0.3367 0.5354 0.4088 0.042 Uiso 1 1 calc R . . C55B C 0.4076(2) 0.48521(15) 0.33810(14) 0.0300(6) Uani 1 1 d . . . H55B H 0.4557 0.5280 0.3058 0.036 Uiso 1 1 calc R . . C56B C 0.4050(2) 0.41639(14) 0.32533(13) 0.0261(5) Uani 1 1 d . . . H56B H 0.4502 0.4148 0.2832 0.031 Uiso 1 1 calc R . . Cl6B Cl 0.57538(5) 0.27623(4) 0.28305(3) 0.02644(14) Uani 1 1 d . . . Cl7B Cl 0.43253(6) 0.09297(4) 0.36281(4) 0.03431(16) Uani 1 1 d . . . Cl8B Cl 0.20219(5) 0.17468(4) 0.45776(3) 0.02622(13) Uani 1 1 d . . . N91B N 0.47644(19) 0.20626(13) 0.44165(11) 0.0262(5) Uani 1 1 d . . . C92B C 0.4713(2) 0.13582(16) 0.49573(14) 0.0317(6) Uani 1 1 d . . . H92B H 0.4258 0.0951 0.4966 0.038 Uiso 1 1 calc R . . C93B C 0.5311(3) 0.12127(18) 0.55043(16) 0.0405(7) Uani 1 1 d . . . H93B H 0.5257 0.0717 0.5865 0.049 Uiso 1 1 calc R . . C94B C 0.5977(3) 0.18058(19) 0.55055(16) 0.0417(7) Uani 1 1 d . . . H94B H 0.6369 0.1723 0.5870 0.050 Uiso 1 1 calc R . . C95B C 0.6056(3) 0.25320(18) 0.49524(15) 0.0346(6) Uani 1 1 d . . . H95B H 0.6507 0.2945 0.4937 0.042 Uiso 1 1 calc R . . C96B C 0.5447(2) 0.26325(16) 0.44198(14) 0.0276(5) Uani 1 1 d . . . H96B H 0.5516 0.3119 0.4047 0.033 Uiso 1 1 calc R . . C1C C 0.8183(3) 1.0082(2) 0.75232(19) 0.0377(8) Uani 0.8171(16) 1 d P A 1 H1C H 0.8421 1.0533 0.7610 0.045 Uiso 0.8171(16) 1 calc PR A 1 Cl1C Cl 0.93829(8) 0.93829(5) 0.76316(5) 0.0396(2) Uani 0.8171(16) 1 d P A 1 Cl2C Cl 0.79494(9) 1.04347(6) 0.66687(5) 0.0603(2) Uani 1 1 d . . . Cl3C Cl 0.68593(10) 0.96649(6) 0.81448(7) 0.0785(3) Uani 1 1 d . . . Cl4C Cl 0.5411(4) 1.0635(3) 0.7349(2) 0.0405(11) Uani 0.1829(16) 1 d P A 2 C1C' C 0.6664(15) 0.9983(10) 0.7395(8) 0.036(4) Uiso 0.1829(16) 1 d P A 2 C1D C 0.3109(3) 0.86180(19) 0.79799(17) 0.0421(7) Uani 1 1 d . . . H1D H 0.3666 0.8458 0.7625 0.050 Uiso 1 1 calc R . . Cl1D Cl 0.38494(9) 0.84545(6) 0.86770(5) 0.0560(2) Uani 1 1 d . . . Cl2D Cl 0.27730(11) 0.96311(6) 0.75986(6) 0.0730(3) Uani 1 1 d . . . Cl3D Cl 0.17714(10) 0.80518(7) 0.82724(7) 0.0790(3) Uani 1 1 d . . . C1E C 0.1524(3) 0.19586(18) 0.67250(16) 0.0406(7) Uani 1 1 d . . . H1E H 0.1095 0.1915 0.7196 0.049 Uiso 1 1 calc R . . Cl1E Cl 0.09188(9) 0.12432(6) 0.65185(5) 0.0579(2) Uani 1 1 d . . . Cl2E Cl 0.12614(9) 0.29209(5) 0.61322(4) 0.0530(2) Uani 1 1 d . . . Cl3E Cl 0.30941(9) 0.17986(7) 0.67220(7) 0.0698(3) Uani 1 1 d . . . 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 Zr1A 0.01992(13) 0.01757(12) 0.02071(13) -0.00603(10) -0.00623(9) 0.00069(9) B1A 0.0222(14) 0.0177(13) 0.0224(13) -0.0064(11) -0.0060(11) 0.0011(11) C11A 0.0227(12) 0.0230(12) 0.0206(12) -0.0070(10) -0.0086(9) 0.0017(10) C12A 0.0255(13) 0.0207(12) 0.0255(13) -0.0045(10) -0.0110(10) 0.0007(10) C13A 0.0250(13) 0.0352(15) 0.0202(12) 0.0002(11) -0.0080(10) -0.0035(11) C14A 0.0219(13) 0.0419(15) 0.0226(13) -0.0143(12) -0.0073(10) 0.0035(11) C15A 0.0267(13) 0.0262(13) 0.0256(13) -0.0127(11) -0.0118(10) 0.0036(10) N21A 0.0228(11) 0.0214(10) 0.0223(10) -0.0089(9) -0.0045(8) 0.0010(8) C22A 0.0245(13) 0.0214(12) 0.0301(13) -0.0089(11) -0.0068(10) 0.0018(10) C23A 0.0322(15) 0.0215(13) 0.0354(15) -0.0077(11) -0.0061(11) 0.0017(11) C24A 0.0345(15) 0.0249(14) 0.0339(15) -0.0101(12) -0.0001(11) -0.0059(11) C25A 0.0264(14) 0.0303(14) 0.0365(15) -0.0111(12) -0.0064(11) -0.0042(11) C26A 0.0248(13) 0.0266(13) 0.0279(13) -0.0087(11) -0.0076(10) 0.0023(11) C31A 0.0241(13) 0.0193(12) 0.0272(13) -0.0079(10) -0.0092(10) -0.0008(10) C32A 0.0244(13) 0.0194(12) 0.0268(13) -0.0084(10) -0.0076(10) -0.0012(10) F32A 0.0267(8) 0.0301(8) 0.0280(8) -0.0120(6) -0.0067(6) 0.0050(6) C33A 0.0262(13) 0.0178(12) 0.0379(15) -0.0100(11) -0.0138(11) 0.0037(10) F33A 0.0290(8) 0.0257(8) 0.0459(9) -0.0143(7) -0.0166(7) 0.0090(6) C34A 0.0367(15) 0.0235(13) 0.0299(14) -0.0048(11) -0.0189(12) 0.0035(11) F34A 0.0512(10) 0.0375(9) 0.0353(9) -0.0056(8) -0.0263(8) 0.0113(8) C35A 0.0333(15) 0.0339(15) 0.0250(13) -0.0123(12) -0.0114(11) 0.0021(12) F35A 0.0484(10) 0.0564(11) 0.0258(8) -0.0168(8) -0.0136(7) 0.0104(9) C36A 0.0261(13) 0.0238(13) 0.0293(13) -0.0110(11) -0.0109(10) 0.0036(10) F36A 0.0365(9) 0.0448(10) 0.0338(9) -0.0233(8) -0.0147(7) 0.0175(8) C41A 0.0207(12) 0.0248(13) 0.0273(13) -0.0115(11) -0.0089(10) 0.0033(10) C42A 0.0257(13) 0.0255(13) 0.0261(13) -0.0102(11) -0.0091(10) 0.0042(10) F42A 0.0389(9) 0.0220(7) 0.0307(8) -0.0090(6) -0.0079(7) -0.0011(6) C43A 0.0336(15) 0.0297(14) 0.0402(16) -0.0188(13) -0.0156(12) 0.0069(12) F43A 0.0562(11) 0.0299(9) 0.0519(11) -0.0257(8) -0.0174(9) 0.0035(8) C44A 0.0410(16) 0.0420(17) 0.0323(15) -0.0232(13) -0.0144(12) 0.0117(13) F44A 0.0746(13) 0.0568(12) 0.0395(10) -0.0334(9) -0.0160(9) 0.0102(10) C45A 0.0319(15) 0.0387(16) 0.0243(13) -0.0107(12) -0.0069(11) 0.0044(12) F45A 0.0578(11) 0.0514(11) 0.0231(8) -0.0120(8) -0.0051(7) 0.0008(9) C46A 0.0210(13) 0.0266(13) 0.0282(13) -0.0096(11) -0.0070(10) 0.0021(10) F46A 0.0331(8) 0.0273(8) 0.0262(8) -0.0063(6) -0.0037(6) -0.0015(6) N51A 0.0281(12) 0.0219(11) 0.0276(11) -0.0106(9) -0.0108(9) 0.0056(9) C52A 0.0299(14) 0.0340(15) 0.0321(14) -0.0156(12) -0.0070(11) 0.0009(12) C53A 0.0461(18) 0.0507(19) 0.0403(17) -0.0290(15) -0.0104(14) 0.0052(15) C54A 0.058(2) 0.0376(17) 0.056(2) -0.0319(16) -0.0247(16) 0.0108(15) C55A 0.061(2) 0.0236(14) 0.0413(17) -0.0089(13) -0.0257(15) 0.0026(13) C56A 0.0451(17) 0.0202(13) 0.0294(14) -0.0056(11) -0.0158(12) 0.0004(11) Cl6A 0.0227(3) 0.0296(3) 0.0268(3) -0.0093(3) -0.0048(2) -0.0040(2) Cl7A 0.0353(4) 0.0211(3) 0.0400(4) -0.0134(3) -0.0147(3) 0.0058(3) Cl8A 0.0245(3) 0.0282(3) 0.0240(3) -0.0028(3) -0.0056(2) -0.0025(2) N91A 0.0239(11) 0.0263(11) 0.0251(11) -0.0069(9) -0.0082(9) 0.0026(9) C92A 0.0283(14) 0.0291(14) 0.0282(14) -0.0050(11) -0.0049(11) 0.0032(11) C93A 0.0360(16) 0.0446(18) 0.0310(15) 0.0002(13) -0.0107(12) 0.0096(14) C94A 0.0359(17) 0.065(2) 0.0316(16) -0.0122(15) -0.0178(13) 0.0086(16) C95A 0.0289(15) 0.0539(19) 0.0347(15) -0.0187(14) -0.0117(12) 0.0022(13) C96A 0.0262(14) 0.0327(14) 0.0298(14) -0.0117(12) -0.0089(11) 0.0021(11) Zr2B 0.01955(13) 0.01948(13) 0.02433(13) -0.00919(10) -0.00624(9) 0.00101(9) B1B 0.0231(14) 0.0178(13) 0.0235(14) -0.0071(11) -0.0066(11) -0.0005(11) C11B 0.0239(13) 0.0260(13) 0.0223(12) -0.0108(10) -0.0080(10) 0.0015(10) C12B 0.0259(13) 0.0269(13) 0.0241(13) -0.0058(11) -0.0093(10) 0.0001(11) C13B 0.0279(14) 0.0474(17) 0.0195(13) -0.0063(12) -0.0075(10) -0.0034(12) C14B 0.0211(13) 0.0577(19) 0.0332(15) -0.0282(14) -0.0073(11) 0.0046(13) C15B 0.0265(14) 0.0354(15) 0.0341(14) -0.0219(12) -0.0122(11) 0.0044(11) N21B 0.0231(11) 0.0216(10) 0.0224(10) -0.0107(9) -0.0064(8) 0.0016(8) C22B 0.0269(13) 0.0235(13) 0.0325(14) -0.0115(11) -0.0118(11) 0.0041(10) C23B 0.0375(15) 0.0215(13) 0.0324(14) -0.0079(11) -0.0134(12) 0.0037(11) C24B 0.0346(15) 0.0236(13) 0.0331(15) -0.0086(11) -0.0053(11) -0.0053(11) C25B 0.0252(14) 0.0295(14) 0.0378(15) -0.0105(12) -0.0078(11) -0.0044(11) C26B 0.0245(13) 0.0253(13) 0.0318(14) -0.0107(11) -0.0105(10) 0.0029(10) C31B 0.0249(13) 0.0186(12) 0.0255(13) -0.0080(10) -0.0086(10) -0.0007(10) C32B 0.0230(13) 0.0213(12) 0.0271(13) -0.0096(10) -0.0063(10) -0.0022(10) F32B 0.0251(8) 0.0299(8) 0.0282(8) -0.0112(6) -0.0062(6) 0.0048(6) C33B 0.0289(14) 0.0210(12) 0.0343(14) -0.0107(11) -0.0128(11) 0.0029(11) F33B 0.0313(8) 0.0271(8) 0.0460(9) -0.0141(7) -0.0185(7) 0.0086(7) C34B 0.0438(17) 0.0254(13) 0.0315(15) -0.0064(12) -0.0225(13) 0.0023(12) F34B 0.0617(12) 0.0411(10) 0.0342(9) -0.0082(8) -0.0289(8) 0.0122(9) C35B 0.0421(16) 0.0356(15) 0.0239(13) -0.0131(12) -0.0113(12) -0.0005(13) F35B 0.0608(12) 0.0607(12) 0.0265(9) -0.0201(8) -0.0150(8) 0.0118(10) C36B 0.0278(14) 0.0272(13) 0.0324(14) -0.0154(11) -0.0107(11) 0.0043(11) F36B 0.0387(9) 0.0496(10) 0.0347(9) -0.0256(8) -0.0139(7) 0.0161(8) C41B 0.0205(12) 0.0259(13) 0.0272(13) -0.0123(11) -0.0090(10) 0.0031(10) C42B 0.0240(13) 0.0265(13) 0.0305(14) -0.0123(11) -0.0106(10) 0.0037(10) F42B 0.0374(9) 0.0226(7) 0.0327(8) -0.0101(6) -0.0068(7) -0.0034(6) C43B 0.0288(14) 0.0274(14) 0.0429(16) -0.0209(12) -0.0132(12) 0.0042(11) F43B 0.0467(10) 0.0312(9) 0.0601(11) -0.0287(8) -0.0178(8) 0.0026(7) C44B 0.0316(15) 0.0441(17) 0.0402(16) -0.0300(14) -0.0135(12) 0.0068(13) F44B 0.0552(11) 0.0626(12) 0.0508(11) -0.0440(10) -0.0119(9) 0.0055(9) C45B 0.0281(14) 0.0443(17) 0.0264(14) -0.0178(13) -0.0064(11) 0.0027(12) F45B 0.0484(11) 0.0600(12) 0.0257(8) -0.0200(8) -0.0026(7) -0.0055(9) C46B 0.0229(13) 0.0260(13) 0.0266(13) -0.0094(11) -0.0087(10) 0.0019(10) F46B 0.0355(9) 0.0292(8) 0.0262(8) -0.0089(6) -0.0046(6) -0.0021(7) N51B 0.0261(11) 0.0197(10) 0.0249(11) -0.0080(9) -0.0097(9) 0.0040(8) C52B 0.0300(14) 0.0279(13) 0.0282(14) -0.0118(11) -0.0041(11) -0.0020(11) C53B 0.0405(17) 0.0348(15) 0.0349(15) -0.0200(13) -0.0004(12) -0.0023(13) C54B 0.0432(17) 0.0266(14) 0.0403(16) -0.0172(13) -0.0104(13) -0.0010(12) C55B 0.0355(15) 0.0220(13) 0.0307(14) -0.0059(11) -0.0098(11) -0.0017(11) C56B 0.0323(14) 0.0201(12) 0.0241(13) -0.0055(10) -0.0081(10) 0.0025(10) Cl6B 0.0207(3) 0.0275(3) 0.0323(3) -0.0126(3) -0.0050(2) -0.0008(2) Cl7B 0.0336(4) 0.0217(3) 0.0522(4) -0.0175(3) -0.0127(3) 0.0040(3) Cl8B 0.0239(3) 0.0253(3) 0.0265(3) -0.0059(2) -0.0059(2) -0.0018(2) N91B 0.0234(11) 0.0246(11) 0.0297(12) -0.0076(9) -0.0091(9) 0.0028(9) C92B 0.0293(14) 0.0249(13) 0.0360(15) -0.0051(12) -0.0098(11) 0.0036(11) C93B 0.0422(17) 0.0361(16) 0.0353(16) -0.0030(13) -0.0144(13) 0.0083(13) C94B 0.0393(17) 0.0500(19) 0.0380(16) -0.0138(15) -0.0206(13) 0.0085(14) C95B 0.0305(15) 0.0405(16) 0.0376(16) -0.0163(13) -0.0139(12) 0.0019(12) C96B 0.0247(13) 0.0263(13) 0.0317(14) -0.0089(11) -0.0100(11) 0.0011(11) C1C 0.042(2) 0.0319(19) 0.044(2) -0.0183(16) -0.0091(16) -0.0008(16) Cl1C 0.0444(5) 0.0385(5) 0.0379(5) -0.0132(4) -0.0166(4) 0.0055(4) Cl2C 0.0584(5) 0.0601(6) 0.0647(6) -0.0207(5) -0.0282(4) 0.0158(4) Cl3C 0.0595(6) 0.0605(6) 0.0962(8) -0.0276(6) 0.0195(5) -0.0051(5) Cl4C 0.038(2) 0.049(2) 0.043(2) -0.0264(19) -0.0131(17) 0.0101(18) C1D 0.0398(17) 0.0456(18) 0.0478(18) -0.0270(15) -0.0073(14) 0.0039(14) Cl1D 0.0614(5) 0.0654(6) 0.0504(5) -0.0301(4) -0.0199(4) 0.0153(4) Cl2D 0.1082(9) 0.0510(6) 0.0728(7) -0.0306(5) -0.0412(6) 0.0260(5) Cl3D 0.0481(6) 0.0911(8) 0.1123(9) -0.0615(7) 0.0032(6) -0.0180(5) C1E 0.0428(18) 0.0421(17) 0.0392(17) -0.0210(14) -0.0013(13) -0.0042(14) Cl1E 0.0600(6) 0.0599(5) 0.0640(6) -0.0378(5) -0.0001(4) -0.0177(4) Cl2E 0.0687(6) 0.0478(5) 0.0348(4) -0.0080(4) -0.0070(4) -0.0067(4) Cl3E 0.0424(5) 0.0705(6) 0.1088(9) -0.0482(6) -0.0158(5) 0.0052(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1A N51A 2.412(2) . ? Zr1A Cl8A 2.4855(7) . ? Zr1A N91A 2.492(2) . ? Zr1A C14A 2.497(2) . ? Zr1A Cl7A 2.4994(7) . ? Zr1A Cl6A 2.5067(7) . ? Zr1A C13A 2.514(2) . ? Zr1A C15A 2.546(2) . ? Zr1A C12A 2.547(2) . ? Zr1A C11A 2.651(2) . ? B1A N21A 1.631(3) . ? B1A C11A 1.643(4) . ? B1A C41A 1.659(4) . ? B1A C31A 1.674(3) . ? C11A C15A 1.419(3) . ? C11A C12A 1.428(3) . ? C12A C13A 1.417(4) . ? C12A H12A 0.9300 . ? C13A C14A 1.393(4) . ? C13A H13A 0.9300 . ? C14A C15A 1.415(4) . ? C14A H14A 0.9300 . ? C15A H15A 0.9300 . ? N21A C22A 1.349(3) . ? N21A C26A 1.357(3) . ? C22A C23A 1.385(4) . ? C22A H22A 0.9300 . ? C23A C24A 1.383(4) . ? C23A H23A 0.9300 . ? C24A C25A 1.382(4) . ? C24A H24A 0.9300 . ? C25A C26A 1.381(4) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C31A C32A 1.396(3) . ? C31A C36A 1.405(4) . ? C32A F32A 1.357(3) . ? C32A C33A 1.394(3) . ? C33A F33A 1.342(3) . ? C33A C34A 1.374(4) . ? C34A F34A 1.349(3) . ? C34A C35A 1.378(4) . ? C35A F35A 1.345(3) . ? C35A C36A 1.389(4) . ? C36A F36A 1.353(3) . ? C41A C42A 1.395(3) . ? C41A C46A 1.400(4) . ? C42A F42A 1.367(3) . ? C42A C43A 1.384(4) . ? C43A F43A 1.341(3) . ? C43A C44A 1.391(4) . ? C44A F44A 1.339(3) . ? C44A C45A 1.369(4) . ? C45A F45A 1.355(3) . ? C45A C46A 1.387(4) . ? C46A F46A 1.356(3) . ? N51A C52A 1.349(3) . ? N51A C56A 1.353(3) . ? C52A C53A 1.380(4) . ? C52A H52A 0.9300 . ? C53A C54A 1.387(5) . ? C53A H53A 0.9300 . ? C54A C55A 1.384(4) . ? C54A H54A 0.9300 . ? C55A C56A 1.384(4) . ? C55A H55A 0.9300 . ? C56A H56A 0.9300 . ? N91A C92A 1.350(3) . ? N91A C96A 1.353(3) . ? C92A C93A 1.391(4) . ? C92A H92A 0.9300 . ? C93A C94A 1.383(5) . ? C93A H93A 0.9300 . ? C94A C95A 1.385(5) . ? C94A H94A 0.9300 . ? C95A C96A 1.393(4) . ? C95A H95A 0.9300 . ? C96A H96A 0.9300 . ? Zr2B N51B 2.418(2) . ? Zr2B C14B 2.484(3) . ? Zr2B Cl8B 2.4852(8) . ? Zr2B Cl7B 2.4893(7) . ? Zr2B N91B 2.494(2) . ? Zr2B C13B 2.504(3) . ? Zr2B Cl6B 2.5260(7) . ? Zr2B C15B 2.544(2) . ? Zr2B C12B 2.547(2) . ? Zr2B C11B 2.647(2) . ? B1B N21B 1.635(3) . ? B1B C11B 1.642(4) . ? B1B C41B 1.655(4) . ? B1B C31B 1.682(3) . ? C11B C15B 1.419(4) . ? C11B C12B 1.432(4) . ? C12B C13B 1.415(4) . ? C12B H12B 0.9300 . ? C13B C14B 1.396(4) . ? C13B H13B 0.9300 . ? C14B C15B 1.417(4) . ? C14B H14B 0.9300 . ? C15B H15B 0.9300 . ? N21B C22B 1.347(3) . ? N21B C26B 1.361(3) . ? C22B C23B 1.387(4) . ? C22B H22B 0.9300 . ? C23B C24B 1.379(4) . ? C23B H23B 0.9300 . ? C24B C25B 1.390(4) . ? C24B H24B 0.9300 . ? C25B C26B 1.381(4) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? C31B C36B 1.399(4) . ? C31B C32B 1.401(3) . ? C32B F32B 1.356(3) . ? C32B C33B 1.391(3) . ? C33B F33B 1.349(3) . ? C33B C34B 1.373(4) . ? C34B F34B 1.350(3) . ? C34B C35B 1.379(4) . ? C35B F35B 1.346(3) . ? C35B C36B 1.388(4) . ? C36B F36B 1.356(3) . ? C41B C46B 1.396(4) . ? C41B C42B 1.399(3) . ? C42B F42B 1.366(3) . ? C42B C43B 1.379(4) . ? C43B F43B 1.343(3) . ? C43B C44B 1.383(4) . ? C44B F44B 1.345(3) . ? C44B C45B 1.376(4) . ? C45B F45B 1.356(3) . ? C45B C46B 1.382(4) . ? C46B F46B 1.355(3) . ? N51B C52B 1.348(3) . ? N51B C56B 1.356(3) . ? C52B C53B 1.389(4) . ? C52B H52B 0.9300 . ? C53B C54B 1.378(4) . ? C53B H53B 0.9300 . ? C54B C55B 1.382(4) . ? C54B H54B 0.9300 . ? C55B C56B 1.386(3) . ? C55B H55B 0.9300 . ? C56B H56B 0.9300 . ? N91B C96B 1.347(3) . ? N91B C92B 1.349(3) . ? C92B C93B 1.395(4) . ? C92B H92B 0.9300 . ? C93B C94B 1.369(4) . ? C93B H93B 0.9300 . ? C94B C95B 1.385(4) . ? C94B H94B 0.9300 . ? C95B C96B 1.393(4) . ? C95B H95B 0.9300 . ? C96B H96B 0.9300 . ? C1C Cl2C 1.746(4) . ? C1C Cl3C 1.747(4) . ? C1C Cl1C 1.760(4) . ? C1C H1C 0.9800 . ? Cl2C C1C' 1.829(16) . ? Cl3C C1C' 1.527(16) . ? Cl4C C1C' 1.753(16) . ? C1D Cl3D 1.747(3) . ? C1D Cl2D 1.755(3) . ? C1D Cl1D 1.770(3) . ? C1D H1D 0.9800 . ? C1E Cl1E 1.756(3) . ? C1E Cl3E 1.756(3) . ? C1E Cl2E 1.769(3) . ? C1E H1E 0.9800 . ? 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 N51A Zr1A Cl8A 85.49(5) . . ? N51A Zr1A N91A 74.50(7) . . ? Cl8A Zr1A N91A 76.44(5) . . ? N51A Zr1A C14A 124.01(8) . . ? Cl8A Zr1A C14A 121.68(6) . . ? N91A Zr1A C14A 152.37(8) . . ? N51A Zr1A Cl7A 155.26(5) . . ? Cl8A Zr1A Cl7A 89.64(3) . . ? N91A Zr1A Cl7A 80.77(5) . . ? C14A Zr1A Cl7A 78.86(7) . . ? N51A Zr1A Cl6A 85.09(5) . . ? Cl8A Zr1A Cl6A 151.06(2) . . ? N91A Zr1A Cl6A 74.68(5) . . ? C14A Zr1A Cl6A 85.97(6) . . ? Cl7A Zr1A Cl6A 87.59(2) . . ? N51A Zr1A C13A 92.36(8) . . ? Cl8A Zr1A C13A 132.45(6) . . ? N91A Zr1A C13A 148.04(8) . . ? C14A Zr1A C13A 32.28(9) . . ? Cl7A Zr1A C13A 108.58(7) . . ? Cl6A Zr1A C13A 75.26(6) . . ? N51A Zr1A C15A 123.71(7) . . ? Cl8A Zr1A C15A 89.29(6) . . ? N91A Zr1A C15A 156.36(8) . . ? C14A Zr1A C15A 32.58(8) . . ? Cl7A Zr1A C15A 80.38(6) . . ? Cl6A Zr1A C15A 118.53(6) . . ? C13A Zr1A C15A 53.32(9) . . ? N51A Zr1A C12A 74.37(8) . . ? Cl8A Zr1A C12A 103.16(6) . . ? N91A Zr1A C12A 148.80(8) . . ? C14A Zr1A C12A 53.37(8) . . ? Cl7A Zr1A C12A 130.29(6) . . ? Cl6A Zr1A C12A 100.52(6) . . ? C13A Zr1A C12A 32.51(8) . . ? C15A Zr1A C12A 52.53(8) . . ? N51A Zr1A C11A 92.84(7) . . ? Cl8A Zr1A C11A 79.12(6) . . ? N91A Zr1A C11A 153.20(7) . . ? C14A Zr1A C11A 53.50(8) . . ? Cl7A Zr1A C11A 110.05(6) . . ? Cl6A Zr1A C11A 128.64(6) . . ? C13A Zr1A C11A 53.51(8) . . ? C15A Zr1A C11A 31.61(8) . . ? C12A Zr1A C11A 31.81(7) . . ? N21A B1A C11A 111.71(19) . . ? N21A B1A C41A 108.99(19) . . ? C11A B1A C41A 112.10(19) . . ? N21A B1A C31A 104.62(18) . . ? C11A B1A C31A 107.13(19) . . ? C41A B1A C31A 112.06(19) . . ? C15A C11A C12A 104.7(2) . . ? C15A C11A B1A 130.4(2) . . ? C12A C11A B1A 122.3(2) . . ? C15A C11A Zr1A 70.11(13) . . ? C12A C11A Zr1A 70.10(13) . . ? B1A C11A Zr1A 137.68(15) . . ? C13A C12A C11A 109.8(2) . . ? C13A C12A Zr1A 72.44(14) . . ? C11A C12A Zr1A 78.09(13) . . ? C13A C12A H12A 125.1 . . ? C11A C12A H12A 125.1 . . ? Zr1A C12A H12A 116.2 . . ? C14A C13A C12A 107.5(2) . . ? C14A C13A Zr1A 73.18(14) . . ? C12A C13A Zr1A 75.05(14) . . ? C14A C13A H13A 126.3 . . ? C12A C13A H13A 126.3 . . ? Zr1A C13A H13A 117.6 . . ? C13A C14A C15A 107.9(2) . . ? C13A C14A Zr1A 74.54(14) . . ? C15A C14A Zr1A 75.62(14) . . ? C13A C14A H14A 126.0 . . ? C15A C14A H14A 126.0 . . ? Zr1A C14A H14A 115.9 . . ? C14A C15A C11A 110.0(2) . . ? C14A C15A Zr1A 71.80(13) . . ? C11A C15A Zr1A 78.28(13) . . ? C14A C15A H15A 125.0 . . ? C11A C15A H15A 125.0 . . ? Zr1A C15A H15A 116.7 . . ? C22A N21A C26A 118.0(2) . . ? C22A N21A B1A 121.7(2) . . ? C26A N21A B1A 120.2(2) . . ? N21A C22A C23A 122.1(2) . . ? N21A C22A H22A 118.9 . . ? C23A C22A H22A 118.9 . . ? C24A C23A C22A 119.4(2) . . ? C24A C23A H23A 120.3 . . ? C22A C23A H23A 120.3 . . ? C25A C24A C23A 118.8(2) . . ? C25A C24A H24A 120.6 . . ? C23A C24A H24A 120.6 . . ? C26A C25A C24A 119.3(2) . . ? C26A C25A H25A 120.3 . . ? C24A C25A H25A 120.3 . . ? N21A C26A C25A 122.3(2) . . ? N21A C26A H26A 118.9 . . ? C25A C26A H26A 118.9 . . ? C32A C31A C36A 112.5(2) . . ? C32A C31A B1A 124.7(2) . . ? C36A C31A B1A 122.8(2) . . ? F32A C32A C33A 115.3(2) . . ? F32A C32A C31A 120.1(2) . . ? C33A C32A C31A 124.6(2) . . ? F33A C33A C34A 119.8(2) . . ? F33A C33A C32A 120.6(2) . . ? C34A C33A C32A 119.6(2) . . ? F34A C34A C33A 121.0(2) . . ? F34A C34A C35A 119.9(2) . . ? C33A C34A C35A 119.1(2) . . ? F35A C35A C34A 120.1(2) . . ? F35A C35A C36A 120.4(2) . . ? C34A C35A C36A 119.5(2) . . ? F36A C36A C35A 114.7(2) . . ? F36A C36A C31A 120.7(2) . . ? C35A C36A C31A 124.6(2) . . ? C42A C41A C46A 112.0(2) . . ? C42A C41A B1A 121.7(2) . . ? C46A C41A B1A 126.3(2) . . ? F42A C42A C43A 114.5(2) . . ? F42A C42A C41A 119.8(2) . . ? C43A C42A C41A 125.8(2) . . ? F43A C43A C42A 121.0(3) . . ? F43A C43A C44A 120.0(2) . . ? C42A C43A C44A 118.9(3) . . ? F44A C44A C45A 121.6(3) . . ? F44A C44A C43A 120.1(3) . . ? C45A C44A C43A 118.3(2) . . ? F45A C45A C44A 119.7(2) . . ? F45A C45A C46A 119.8(3) . . ? C44A C45A C46A 120.6(3) . . ? F46A C46A C45A 114.4(2) . . ? F46A C46A C41A 121.3(2) . . ? C45A C46A C41A 124.4(2) . . ? C52A N51A C56A 117.1(2) . . ? C52A N51A Zr1A 122.80(18) . . ? C56A N51A Zr1A 119.67(17) . . ? N51A C52A C53A 123.2(3) . . ? N51A C52A H52A 118.4 . . ? C53A C52A H52A 118.4 . . ? C52A C53A C54A 119.1(3) . . ? C52A C53A H53A 120.5 . . ? C54A C53A H53A 120.5 . . ? C55A C54A C53A 118.5(3) . . ? C55A C54A H54A 120.7 . . ? C53A C54A H54A 120.7 . . ? C56A C55A C54A 119.2(3) . . ? C56A C55A H55A 120.4 . . ? C54A C55A H55A 120.4 . . ? N51A C56A C55A 122.8(3) . . ? N51A C56A H56A 118.6 . . ? C55A C56A H56A 118.6 . . ? C92A N91A C96A 116.6(2) . . ? C92A N91A Zr1A 120.93(18) . . ? C96A N91A Zr1A 122.43(17) . . ? N91A C92A C93A 123.4(3) . . ? N91A C92A H92A 118.3 . . ? C93A C92A H92A 118.3 . . ? C94A C93A C92A 119.0(3) . . ? C94A C93A H93A 120.5 . . ? C92A C93A H93A 120.5 . . ? C93A C94A C95A 118.8(3) . . ? C93A C94A H94A 120.6 . . ? C95A C94A H94A 120.6 . . ? C94A C95A C96A 118.9(3) . . ? C94A C95A H95A 120.6 . . ? C96A C95A H95A 120.6 . . ? N91A C96A C95A 123.3(3) . . ? N91A C96A H96A 118.3 . . ? C95A C96A H96A 118.3 . . ? N51B Zr2B C14B 121.89(9) . . ? N51B Zr2B Cl8B 85.92(5) . . ? C14B Zr2B Cl8B 123.11(7) . . ? N51B Zr2B Cl7B 155.66(5) . . ? C14B Zr2B Cl7B 80.46(7) . . ? Cl8B Zr2B Cl7B 89.07(3) . . ? N51B Zr2B N91B 74.55(7) . . ? C14B Zr2B N91B 152.41(8) . . ? Cl8B Zr2B N91B 76.82(5) . . ? Cl7B Zr2B N91B 81.11(5) . . ? N51B Zr2B C13B 89.80(8) . . ? C14B Zr2B C13B 32.51(10) . . ? Cl8B Zr2B C13B 132.23(7) . . ? Cl7B Zr2B C13B 110.88(7) . . ? N91B Zr2B C13B 146.65(8) . . ? N51B Zr2B Cl6B 86.15(5) . . ? C14B Zr2B Cl6B 83.47(6) . . ? Cl8B Zr2B Cl6B 152.10(2) . . ? Cl7B Zr2B Cl6B 87.24(2) . . ? N91B Zr2B Cl6B 75.29(5) . . ? C13B Zr2B Cl6B 74.41(7) . . ? N51B Zr2B C15B 123.38(8) . . ? C14B Zr2B C15B 32.70(9) . . ? Cl8B Zr2B C15B 90.49(7) . . ? Cl7B Zr2B C15B 80.42(6) . . ? N91B Zr2B C15B 157.70(8) . . ? C13B Zr2B C15B 53.57(9) . . ? Cl6B Zr2B C15B 116.06(6) . . ? N51B Zr2B C12B 73.04(8) . . ? C14B Zr2B C12B 53.54(9) . . ? Cl8B Zr2B C12B 102.19(6) . . ? Cl7B Zr2B C12B 131.27(6) . . ? N91B Zr2B C12B 147.56(8) . . ? C13B Zr2B C12B 32.53(8) . . ? Cl6B Zr2B C12B 100.96(6) . . ? C15B Zr2B C12B 52.65(9) . . ? N51B Zr2B C11B 92.91(7) . . ? C14B Zr2B C11B 53.67(8) . . ? Cl8B Zr2B C11B 79.01(6) . . ? Cl7B Zr2B C11B 109.49(6) . . ? N91B Zr2B C11B 153.41(7) . . ? C13B Zr2B C11B 53.70(8) . . ? Cl6B Zr2B C11B 128.10(6) . . ? C15B Zr2B C11B 31.64(8) . . ? C12B Zr2B C11B 31.93(8) . . ? N21B B1B C11B 111.58(19) . . ? N21B B1B C41B 109.03(19) . . ? C11B B1B C41B 112.65(19) . . ? N21B B1B C31B 105.48(18) . . ? C11B B1B C31B 107.44(19) . . ? C41B B1B C31B 110.41(19) . . ? C15B C11B C12B 104.7(2) . . ? C15B C11B B1B 130.5(2) . . ? C12B C11B B1B 122.1(2) . . ? C15B C11B Zr2B 70.16(13) . . ? C12B C11B Zr2B 70.18(13) . . ? B1B C11B Zr2B 137.62(16) . . ? C13B C12B C11B 109.8(2) . . ? C13B C12B Zr2B 72.03(14) . . ? C11B C12B Zr2B 77.89(14) . . ? C13B C12B H12B 125.1 . . ? C11B C12B H12B 125.1 . . ? Zr2B C12B H12B 116.8 . . ? C14B C13B C12B 107.5(2) . . ? C14B C13B Zr2B 72.97(15) . . ? C12B C13B Zr2B 75.44(14) . . ? C14B C13B H13B 126.3 . . ? C12B C13B H13B 126.3 . . ? Zr2B C13B H13B 117.4 . . ? C13B C14B C15B 108.0(2) . . ? C13B C14B Zr2B 74.51(15) . . ? C15B C14B Zr2B 75.98(15) . . ? C13B C14B H14B 126.0 . . ? C15B C14B H14B 126.0 . . ? Zr2B C14B H14B 115.7 . . ? C14B C15B C11B 109.9(2) . . ? C14B C15B Zr2B 71.32(14) . . ? C11B C15B Zr2B 78.20(14) . . ? C14B C15B H15B 125.1 . . ? C11B C15B H15B 125.1 . . ? Zr2B C15B H15B 117.2 . . ? C22B N21B C26B 118.0(2) . . ? C22B N21B B1B 122.15(19) . . ? C26B N21B B1B 119.7(2) . . ? N21B C22B C23B 122.2(2) . . ? N21B C22B H22B 118.9 . . ? C23B C22B H22B 118.9 . . ? C24B C23B C22B 119.8(2) . . ? C24B C23B H23B 120.1 . . ? C22B C23B H23B 120.1 . . ? C23B C24B C25B 118.4(2) . . ? C23B C24B H24B 120.8 . . ? C25B C24B H24B 120.8 . . ? C26B C25B C24B 119.5(2) . . ? C26B C25B H25B 120.3 . . ? C24B C25B H25B 120.3 . . ? N21B C26B C25B 122.2(2) . . ? N21B C26B H26B 118.9 . . ? C25B C26B H26B 118.9 . . ? C36B C31B C32B 112.4(2) . . ? C36B C31B B1B 124.5(2) . . ? C32B C31B B1B 123.1(2) . . ? F32B C32B C33B 115.2(2) . . ? F32B C32B C31B 120.2(2) . . ? C33B C32B C31B 124.6(2) . . ? F33B C33B C34B 119.9(2) . . ? F33B C33B C32B 120.5(2) . . ? C34B C33B C32B 119.6(2) . . ? F34B C34B C33B 120.7(3) . . ? F34B C34B C35B 120.3(3) . . ? C33B C34B C35B 119.1(2) . . ? F35B C35B C34B 119.9(2) . . ? F35B C35B C36B 120.7(2) . . ? C34B C35B C36B 119.4(2) . . ? F36B C36B C35B 114.5(2) . . ? F36B C36B C31B 120.8(2) . . ? C35B C36B C31B 124.8(2) . . ? C46B C41B C42B 112.4(2) . . ? C46B C41B B1B 126.4(2) . . ? C42B C41B B1B 121.2(2) . . ? F42B C42B C43B 114.6(2) . . ? F42B C42B C41B 119.9(2) . . ? C43B C42B C41B 125.5(2) . . ? F43B C43B C42B 120.7(3) . . ? F43B C43B C44B 120.1(2) . . ? C42B C43B C44B 119.2(2) . . ? F44B C44B C45B 121.1(3) . . ? F44B C44B C43B 120.7(3) . . ? C45B C44B C43B 118.3(2) . . ? F45B C45B C44B 119.3(2) . . ? F45B C45B C46B 120.0(3) . . ? C44B C45B C46B 120.6(3) . . ? F46B C46B C45B 114.7(2) . . ? F46B C46B C41B 121.2(2) . . ? C45B C46B C41B 124.1(2) . . ? C52B N51B C56B 116.9(2) . . ? C52B N51B Zr2B 123.18(17) . . ? C56B N51B Zr2B 119.75(16) . . ? N51B C52B C53B 122.9(3) . . ? N51B C52B H52B 118.6 . . ? C53B C52B H52B 118.6 . . ? C54B C53B C52B 119.5(3) . . ? C54B C53B H53B 120.3 . . ? C52B C53B H53B 120.3 . . ? C53B C54B C55B 118.6(3) . . ? C53B C54B H54B 120.7 . . ? C55B C54B H54B 120.7 . . ? C54B C55B C56B 119.1(3) . . ? C54B C55B H55B 120.4 . . ? C56B C55B H55B 120.4 . . ? N51B C56B C55B 123.1(2) . . ? N51B C56B H56B 118.5 . . ? C55B C56B H56B 118.5 . . ? C96B N91B C92B 116.5(2) . . ? C96B N91B Zr2B 121.99(16) . . ? C92B N91B Zr2B 121.47(18) . . ? N91B C92B C93B 123.1(3) . . ? N91B C92B H92B 118.5 . . ? C93B C92B H92B 118.5 . . ? C94B C93B C92B 119.5(3) . . ? C94B C93B H93B 120.3 . . ? C92B C93B H93B 120.3 . . ? C93B C94B C95B 118.6(3) . . ? C93B C94B H94B 120.7 . . ? C95B C94B H94B 120.7 . . ? C94B C95B C96B 118.8(3) . . ? C94B C95B H95B 120.6 . . ? C96B C95B H95B 120.6 . . ? N91B C96B C95B 123.5(3) . . ? N91B C96B H96B 118.2 . . ? C95B C96B H96B 118.2 . . ? Cl2C C1C Cl3C 112.4(2) . . ? Cl2C C1C Cl1C 111.2(2) . . ? Cl3C C1C Cl1C 109.6(2) . . ? Cl2C C1C H1C 107.8 . . ? Cl3C C1C H1C 107.8 . . ? Cl1C C1C H1C 107.8 . . ? C1C Cl2C C1C' 61.0(5) . . ? C1C' Cl3C C1C 67.0(6) . . ? Cl3C C1C' Cl4C 108.0(9) . . ? Cl3C C1C' Cl2C 119.5(10) . . ? Cl4C C1C' Cl2C 110.3(9) . . ? Cl3D C1D Cl2D 110.53(18) . . ? Cl3D C1D Cl1D 110.81(18) . . ? Cl2D C1D Cl1D 109.76(17) . . ? Cl3D C1D H1D 108.6 . . ? Cl2D C1D H1D 108.6 . . ? Cl1D C1D H1D 108.6 . . ? Cl1E C1E Cl3E 111.22(17) . . ? Cl1E C1E Cl2E 109.88(17) . . ? Cl3E C1E Cl2E 110.89(17) . . ? Cl1E C1E H1E 108.3 . . ? Cl3E C1E H1E 108.3 . . ? Cl2E C1E H1E 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21A B1A C11A C15A 16.8(3) . . . . ? C41A B1A C11A C15A 139.5(2) . . . . ? C31A B1A C11A C15A -97.2(3) . . . . ? N21A B1A C11A C12A 175.6(2) . . . . ? C41A B1A C11A C12A -61.8(3) . . . . ? C31A B1A C11A C12A 61.5(3) . . . . ? N21A B1A C11A Zr1A -88.9(3) . . . . ? C41A B1A C11A Zr1A 33.7(3) . . . . ? C31A B1A C11A Zr1A 157.05(18) . . . . ? N51A Zr1A C11A C15A 168.38(15) . . . . ? Cl8A Zr1A C11A C15A -106.76(14) . . . . ? N91A Zr1A C11A C15A -131.28(18) . . . . ? C14A Zr1A C11A C15A 37.09(15) . . . . ? Cl7A Zr1A C11A C15A -21.17(15) . . . . ? Cl6A Zr1A C11A C15A 82.39(15) . . . . ? C13A Zr1A C11A C15A 77.56(16) . . . . ? C12A Zr1A C11A C15A 114.7(2) . . . . ? N51A Zr1A C11A C12A 53.71(15) . . . . ? Cl8A Zr1A C11A C12A 138.57(15) . . . . ? N91A Zr1A C11A C12A 114.05(19) . . . . ? C14A Zr1A C11A C12A -77.58(16) . . . . ? Cl7A Zr1A C11A C12A -135.84(13) . . . . ? Cl6A Zr1A C11A C12A -32.28(17) . . . . ? C13A Zr1A C11A C12A -37.11(15) . . . . ? C15A Zr1A C11A C12A -114.7(2) . . . . ? N51A Zr1A C11A B1A -62.8(2) . . . . ? Cl8A Zr1A C11A B1A 22.1(2) . . . . ? N91A Zr1A C11A B1A -2.5(3) . . . . ? C14A Zr1A C11A B1A 165.9(3) . . . . ? Cl7A Zr1A C11A B1A 107.7(2) . . . . ? Cl6A Zr1A C11A B1A -148.8(2) . . . . ? C13A Zr1A C11A B1A -153.6(3) . . . . ? C15A Zr1A C11A B1A 128.8(3) . . . . ? C12A Zr1A C11A B1A -116.5(3) . . . . ? C15A C11A C12A C13A 4.1(3) . . . . ? B1A C11A C12A C13A -159.3(2) . . . . ? Zr1A C11A C12A C13A 66.19(17) . . . . ? C15A C11A C12A Zr1A -62.04(16) . . . . ? B1A C11A C12A Zr1A 134.5(2) . . . . ? N51A Zr1A C12A C13A 121.23(16) . . . . ? Cl8A Zr1A C12A C13A -157.36(14) . . . . ? N91A Zr1A C12A C13A 117.15(18) . . . . ? C14A Zr1A C12A C13A -37.47(16) . . . . ? Cl7A Zr1A C12A C13A -56.41(17) . . . . ? Cl6A Zr1A C12A C13A 39.41(16) . . . . ? C15A Zr1A C12A C13A -78.61(17) . . . . ? C11A Zr1A C12A C13A -115.5(2) . . . . ? N51A Zr1A C12A C11A -123.28(15) . . . . ? Cl8A Zr1A C12A C11A -41.87(15) . . . . ? N91A Zr1A C12A C11A -127.36(16) . . . . ? C14A Zr1A C12A C11A 78.02(16) . . . . ? Cl7A Zr1A C12A C11A 59.08(16) . . . . ? Cl6A Zr1A C12A C11A 154.90(13) . . . . ? C13A Zr1A C12A C11A 115.5(2) . . . . ? C15A Zr1A C12A C11A 36.88(14) . . . . ? C11A C12A C13A C14A -3.3(3) . . . . ? Zr1A C12A C13A C14A 66.54(17) . . . . ? C11A C12A C13A Zr1A -69.87(17) . . . . ? N51A Zr1A C13A C14A -169.42(16) . . . . ? Cl8A Zr1A C13A C14A -83.38(17) . . . . ? N91A Zr1A C13A C14A 126.63(17) . . . . ? Cl7A Zr1A C13A C14A 23.99(16) . . . . ? Cl6A Zr1A C13A C14A 106.28(15) . . . . ? C15A Zr1A C13A C14A -37.97(15) . . . . ? C12A Zr1A C13A C14A -113.9(2) . . . . ? C11A Zr1A C13A C14A -77.63(16) . . . . ? N51A Zr1A C13A C12A -55.51(16) . . . . ? Cl8A Zr1A C13A C12A 30.54(19) . . . . ? N91A Zr1A C13A C12A -119.45(17) . . . . ? C14A Zr1A C13A C12A 113.9(2) . . . . ? Cl7A Zr1A C13A C12A 137.91(14) . . . . ? Cl6A Zr1A C13A C12A -139.81(16) . . . . ? C15A Zr1A C13A C12A 75.95(16) . . . . ? C11A Zr1A C13A C12A 36.29(14) . . . . ? C12A C13A C14A C15A 1.1(3) . . . . ? Zr1A C13A C14A C15A 68.89(17) . . . . ? C12A C13A C14A Zr1A -67.81(17) . . . . ? N51A Zr1A C14A C13A 12.78(19) . . . . ? Cl8A Zr1A C14A C13A 120.54(15) . . . . ? N91A Zr1A C14A C13A -113.7(2) . . . . ? Cl7A Zr1A C14A C13A -156.87(16) . . . . ? Cl6A Zr1A C14A C13A -68.54(15) . . . . ? C15A Zr1A C14A C13A 113.6(2) . . . . ? C12A Zr1A C14A C13A 37.74(15) . . . . ? C11A Zr1A C14A C13A 77.64(16) . . . . ? N51A Zr1A C14A C15A -100.81(16) . . . . ? Cl8A Zr1A C14A C15A 6.95(17) . . . . ? N91A Zr1A C14A C15A 132.75(17) . . . . ? Cl7A Zr1A C14A C15A 89.53(15) . . . . ? Cl6A Zr1A C14A C15A 177.87(15) . . . . ? C13A Zr1A C14A C15A -113.6(2) . . . . ? C12A Zr1A C14A C15A -75.85(16) . . . . ? C11A Zr1A C14A C15A -35.95(14) . . . . ? C13A C14A C15A C11A 1.5(3) . . . . ? Zr1A C14A C15A C11A 69.71(17) . . . . ? C13A C14A C15A Zr1A -68.16(17) . . . . ? C12A C11A C15A C14A -3.5(3) . . . . ? B1A C11A C15A C14A 158.1(2) . . . . ? Zr1A C11A C15A C14A -65.50(17) . . . . ? C12A C11A C15A Zr1A 62.03(16) . . . . ? B1A C11A C15A Zr1A -136.4(2) . . . . ? N51A Zr1A C15A C14A 101.80(16) . . . . ? Cl8A Zr1A C15A C14A -174.09(15) . . . . ? N91A Zr1A C15A C14A -121.9(2) . . . . ? Cl7A Zr1A C15A C14A -84.33(15) . . . . ? Cl6A Zr1A C15A C14A -2.42(17) . . . . ? C13A Zr1A C15A C14A 37.61(15) . . . . ? C12A Zr1A C15A C14A 78.67(17) . . . . ? C11A Zr1A C15A C14A 115.8(2) . . . . ? N51A Zr1A C15A C11A -13.99(18) . . . . ? Cl8A Zr1A C15A C11A 70.11(14) . . . . ? N91A Zr1A C15A C11A 122.33(19) . . . . ? C14A Zr1A C15A C11A -115.8(2) . . . . ? Cl7A Zr1A C15A C11A 159.87(15) . . . . ? Cl6A Zr1A C15A C11A -118.21(13) . . . . ? C13A Zr1A C15A C11A -78.18(16) . . . . ? C12A Zr1A C15A C11A -37.12(14) . . . . ? C11A B1A N21A C22A 36.4(3) . . . . ? C41A B1A N21A C22A -88.0(3) . . . . ? C31A B1A N21A C22A 151.9(2) . . . . ? C11A B1A N21A C26A -147.4(2) . . . . ? C41A B1A N21A C26A 88.2(3) . . . . ? C31A B1A N21A C26A -31.9(3) . . . . ? C26A N21A C22A C23A 1.5(4) . . . . ? B1A N21A C22A C23A 177.8(2) . . . . ? N21A C22A C23A C24A -0.1(4) . . . . ? C22A C23A C24A C25A -1.2(4) . . . . ? C23A C24A C25A C26A 1.0(4) . . . . ? C22A N21A C26A C25A -1.7(4) . . . . ? B1A N21A C26A C25A -178.1(2) . . . . ? C24A C25A C26A N21A 0.5(4) . . . . ? N21A B1A C31A C32A 95.1(3) . . . . ? C11A B1A C31A C32A -146.2(2) . . . . ? C41A B1A C31A C32A -22.9(3) . . . . ? N21A B1A C31A C36A -83.8(3) . . . . ? C11A B1A C31A C36A 34.9(3) . . . . ? C41A B1A C31A C36A 158.3(2) . . . . ? C36A C31A C32A F32A 174.7(2) . . . . ? B1A C31A C32A F32A -4.3(4) . . . . ? C36A C31A C32A C33A -3.2(4) . . . . ? B1A C31A C32A C33A 177.9(2) . . . . ? F32A C32A C33A F33A 0.8(3) . . . . ? C31A C32A C33A F33A 178.8(2) . . . . ? F32A C32A C33A C34A -177.3(2) . . . . ? C31A C32A C33A C34A 0.7(4) . . . . ? F33A C33A C34A F34A 2.5(4) . . . . ? C32A C33A C34A F34A -179.4(2) . . . . ? F33A C33A C34A C35A -176.7(2) . . . . ? C32A C33A C34A C35A 1.4(4) . . . . ? F34A C34A C35A F35A -0.5(4) . . . . ? C33A C34A C35A F35A 178.7(2) . . . . ? F34A C34A C35A C36A -179.8(2) . . . . ? C33A C34A C35A C36A -0.6(4) . . . . ? F35A C35A C36A F36A -2.4(4) . . . . ? C34A C35A C36A F36A 176.9(2) . . . . ? F35A C35A C36A C31A 178.3(2) . . . . ? C34A C35A C36A C31A -2.4(4) . . . . ? C32A C31A C36A F36A -175.2(2) . . . . ? B1A C31A C36A F36A 3.8(4) . . . . ? C32A C31A C36A C35A 4.0(4) . . . . ? B1A C31A C36A C35A -177.0(2) . . . . ? N21A B1A C41A C42A -164.8(2) . . . . ? C11A B1A C41A C42A 71.0(3) . . . . ? C31A B1A C41A C42A -49.5(3) . . . . ? N21A B1A C41A C46A 15.9(3) . . . . ? C11A B1A C41A C46A -108.3(3) . . . . ? C31A B1A C41A C46A 131.2(2) . . . . ? C46A C41A C42A F42A -177.8(2) . . . . ? B1A C41A C42A F42A 2.9(4) . . . . ? C46A C41A C42A C43A 0.8(4) . . . . ? B1A C41A C42A C43A -178.6(2) . . . . ? F42A C42A C43A F43A -2.1(4) . . . . ? C41A C42A C43A F43A 179.3(2) . . . . ? F42A C42A C43A C44A 178.3(2) . . . . ? C41A C42A C43A C44A -0.4(4) . . . . ? F43A C43A C44A F44A 0.2(4) . . . . ? C42A C43A C44A F44A 179.9(2) . . . . ? F43A C43A C44A C45A 179.7(2) . . . . ? C42A C43A C44A C45A -0.6(4) . . . . ? F44A C44A C45A F45A 1.0(4) . . . . ? C43A C44A C45A F45A -178.5(2) . . . . ? F44A C44A C45A C46A -179.4(2) . . . . ? C43A C44A C45A C46A 1.1(4) . . . . ? F45A C45A C46A F46A -0.2(3) . . . . ? C44A C45A C46A F46A -179.7(2) . . . . ? F45A C45A C46A C41A 178.9(2) . . . . ? C44A C45A C46A C41A -0.6(4) . . . . ? C42A C41A C46A F46A 178.8(2) . . . . ? B1A C41A C46A F46A -1.9(4) . . . . ? C42A C41A C46A C45A -0.3(4) . . . . ? B1A C41A C46A C45A 179.0(2) . . . . ? Cl8A Zr1A N51A C52A 15.72(19) . . . . ? N91A Zr1A N51A C52A -61.44(19) . . . . ? C14A Zr1A N51A C52A 141.34(19) . . . . ? Cl7A Zr1A N51A C52A -63.6(3) . . . . ? Cl6A Zr1A N51A C52A -136.88(19) . . . . ? C13A Zr1A N51A C52A 148.1(2) . . . . ? C15A Zr1A N51A C52A 101.9(2) . . . . ? C12A Zr1A N51A C52A 120.7(2) . . . . ? C11A Zr1A N51A C52A 94.6(2) . . . . ? Cl8A Zr1A N51A C56A -172.33(18) . . . . ? N91A Zr1A N51A C56A 110.50(19) . . . . ? C14A Zr1A N51A C56A -46.7(2) . . . . ? Cl7A Zr1A N51A C56A 108.4(2) . . . . ? Cl6A Zr1A N51A C56A 35.06(18) . . . . ? C13A Zr1A N51A C56A -39.93(19) . . . . ? C15A Zr1A N51A C56A -86.2(2) . . . . ? C12A Zr1A N51A C56A -67.31(19) . . . . ? C11A Zr1A N51A C56A -93.49(19) . . . . ? C56A N51A C52A C53A -0.2(4) . . . . ? Zr1A N51A C52A C53A 172.0(2) . . . . ? N51A C52A C53A C54A -0.4(4) . . . . ? C52A C53A C54A C55A 0.6(5) . . . . ? C53A C54A C55A C56A -0.2(5) . . . . ? C52A N51A C56A C55A 0.5(4) . . . . ? Zr1A N51A C56A C55A -171.9(2) . . . . ? C54A C55A C56A N51A -0.3(4) . . . . ? N51A Zr1A N91A C92A 139.6(2) . . . . ? Cl8A Zr1A N91A C92A 50.62(19) . . . . ? C14A Zr1A N91A C92A -84.1(3) . . . . ? Cl7A Zr1A N91A C92A -41.26(19) . . . . ? Cl6A Zr1A N91A C92A -131.3(2) . . . . ? C13A Zr1A N91A C92A -151.7(2) . . . . ? C15A Zr1A N91A C92A -3.8(3) . . . . ? C12A Zr1A N91A C92A 143.71(19) . . . . ? C11A Zr1A N91A C92A 75.4(3) . . . . ? N51A Zr1A N91A C96A -41.14(19) . . . . ? Cl8A Zr1A N91A C96A -130.2(2) . . . . ? C14A Zr1A N91A C96A 95.1(2) . . . . ? Cl7A Zr1A N91A C96A 137.96(19) . . . . ? Cl6A Zr1A N91A C96A 47.94(18) . . . . ? C13A Zr1A N91A C96A 27.5(3) . . . . ? C15A Zr1A N91A C96A 175.45(19) . . . . ? C12A Zr1A N91A C96A -37.1(3) . . . . ? C11A Zr1A N91A C96A -105.4(2) . . . . ? C96A N91A C92A C93A -0.2(4) . . . . ? Zr1A N91A C92A C93A 179.0(2) . . . . ? N91A C92A C93A C94A 0.8(4) . . . . ? C92A C93A C94A C95A -0.6(4) . . . . ? C93A C94A C95A C96A 0.0(4) . . . . ? C92A N91A C96A C95A -0.4(4) . . . . ? Zr1A N91A C96A C95A -179.6(2) . . . . ? C94A C95A C96A N91A 0.5(4) . . . . ? N21B B1B C11B C15B 17.5(4) . . . . ? C41B B1B C11B C15B 140.5(3) . . . . ? C31B B1B C11B C15B -97.7(3) . . . . ? N21B B1B C11B C12B 176.2(2) . . . . ? C41B B1B C11B C12B -60.8(3) . . . . ? C31B B1B C11B C12B 61.0(3) . . . . ? N21B B1B C11B Zr2B -88.4(3) . . . . ? C41B B1B C11B Zr2B 34.6(3) . . . . ? C31B B1B C11B Zr2B 156.40(18) . . . . ? N51B Zr2B C11B C15B 165.35(16) . . . . ? C14B Zr2B C11B C15B 37.09(16) . . . . ? Cl8B Zr2B C11B C15B -109.38(15) . . . . ? Cl7B Zr2B C11B C15B -24.33(16) . . . . ? N91B Zr2B C11B C15B -134.27(18) . . . . ? C13B Zr2B C11B C15B 77.75(17) . . . . ? Cl6B Zr2B C11B C15B 77.96(16) . . . . ? C12B Zr2B C11B C15B 114.7(2) . . . . ? N51B Zr2B C11B C12B 50.66(15) . . . . ? C14B Zr2B C11B C12B -77.61(17) . . . . ? Cl8B Zr2B C11B C12B 135.93(15) . . . . ? Cl7B Zr2B C11B C12B -139.02(13) . . . . ? N91B Zr2B C11B C12B 111.04(19) . . . . ? C13B Zr2B C11B C12B -36.94(15) . . . . ? Cl6B Zr2B C11B C12B -36.73(17) . . . . ? C15B Zr2B C11B C12B -114.7(2) . . . . ? N51B Zr2B C11B B1B -65.7(2) . . . . ? C14B Zr2B C11B B1B 166.1(3) . . . . ? Cl8B Zr2B C11B B1B 19.6(2) . . . . ? Cl7B Zr2B C11B B1B 104.7(2) . . . . ? N91B Zr2B C11B B1B -5.3(3) . . . . ? C13B Zr2B C11B B1B -153.3(3) . . . . ? Cl6B Zr2B C11B B1B -153.0(2) . . . . ? C15B Zr2B C11B B1B 129.0(3) . . . . ? C12B Zr2B C11B B1B -116.3(3) . . . . ? C15B C11B C12B C13B 3.5(3) . . . . ? B1B C11B C12B C13B -159.9(2) . . . . ? Zr2B C11B C12B C13B 65.62(17) . . . . ? C15B C11B C12B Zr2B -62.10(16) . . . . ? B1B C11B C12B Zr2B 134.5(2) . . . . ? N51B Zr2B C12B C13B 118.11(17) . . . . ? C14B Zr2B C12B C13B -37.69(16) . . . . ? Cl8B Zr2B C12B C13B -160.05(15) . . . . ? Cl7B Zr2B C12B C13B -60.40(18) . . . . ? N91B Zr2B C12B C13B 115.41(19) . . . . ? Cl6B Zr2B C12B C13B 35.62(16) . . . . ? C15B Zr2B C12B C13B -78.90(18) . . . . ? C11B Zr2B C12B C13B -115.7(2) . . . . ? N51B Zr2B C12B C11B -126.15(16) . . . . ? C14B Zr2B C12B C11B 78.05(16) . . . . ? Cl8B Zr2B C12B C11B -44.31(15) . . . . ? Cl7B Zr2B C12B C11B 55.34(17) . . . . ? N91B Zr2B C12B C11B -128.85(16) . . . . ? C13B Zr2B C12B C11B 115.7(2) . . . . ? Cl6B Zr2B C12B C11B 151.36(13) . . . . ? C15B Zr2B C12B C11B 36.84(14) . . . . ? C11B C12B C13B C14B -2.9(3) . . . . ? Zr2B C12B C13B C14B 66.49(18) . . . . ? C11B C12B C13B Zr2B -69.42(17) . . . . ? N51B Zr2B C13B C14B -171.34(16) . . . . ? Cl8B Zr2B C13B C14B -87.04(17) . . . . ? Cl7B Zr2B C13B C14B 21.80(17) . . . . ? N91B Zr2B C13B C14B 127.99(17) . . . . ? Cl6B Zr2B C13B C14B 102.60(16) . . . . ? C15B Zr2B C13B C14B -38.00(15) . . . . ? C12B Zr2B C13B C14B -113.8(2) . . . . ? C11B Zr2B C13B C14B -77.58(17) . . . . ? N51B Zr2B C13B C12B -57.53(16) . . . . ? C14B Zr2B C13B C12B 113.8(2) . . . . ? Cl8B Zr2B C13B C12B 26.8(2) . . . . ? Cl7B Zr2B C13B C12B 135.61(14) . . . . ? N91B Zr2B C13B C12B -118.19(17) . . . . ? Cl6B Zr2B C13B C12B -143.59(17) . . . . ? C15B Zr2B C13B C12B 75.81(17) . . . . ? C11B Zr2B C13B C12B 36.24(14) . . . . ? C12B C13B C14B C15B 1.1(3) . . . . ? Zr2B C13B C14B C15B 69.26(18) . . . . ? C12B C13B C14B Zr2B -68.16(17) . . . . ? N51B Zr2B C14B C13B 10.21(19) . . . . ? Cl8B Zr2B C14B C13B 118.02(15) . . . . ? Cl7B Zr2B C14B C13B -159.40(16) . . . . ? N91B Zr2B C14B C13B -110.7(2) . . . . ? Cl6B Zr2B C14B C13B -71.11(16) . . . . ? C15B Zr2B C14B C13B 113.5(2) . . . . ? C12B Zr2B C14B C13B 37.71(15) . . . . ? C11B Zr2B C14B C13B 77.67(17) . . . . ? N51B Zr2B C14B C15B -103.30(17) . . . . ? Cl8B Zr2B C14B C15B 4.51(19) . . . . ? Cl7B Zr2B C14B C15B 87.09(16) . . . . ? N91B Zr2B C14B C15B 135.81(18) . . . . ? C13B Zr2B C14B C15B -113.5(2) . . . . ? Cl6B Zr2B C14B C15B 175.38(16) . . . . ? C12B Zr2B C14B C15B -75.80(17) . . . . ? C11B Zr2B C14B C15B -35.84(15) . . . . ? C13B C14B C15B C11B 1.1(3) . . . . ? Zr2B C14B C15B C11B 69.40(18) . . . . ? C13B C14B C15B Zr2B -68.27(18) . . . . ? C12B C11B C15B C14B -2.8(3) . . . . ? B1B C11B C15B C14B 158.6(2) . . . . ? Zr2B C11B C15B C14B -64.95(18) . . . . ? C12B C11B C15B Zr2B 62.12(16) . . . . ? B1B C11B C15B Zr2B -136.4(2) . . . . ? N51B Zr2B C15B C14B 98.34(17) . . . . ? Cl8B Zr2B C15B C14B -176.22(16) . . . . ? Cl7B Zr2B C15B C14B -87.25(16) . . . . ? N91B Zr2B C15B C14B -121.7(2) . . . . ? C13B Zr2B C15B C14B 37.77(17) . . . . ? Cl6B Zr2B C15B C14B -5.11(18) . . . . ? C12B Zr2B C15B C14B 78.76(18) . . . . ? C11B Zr2B C15B C14B 115.9(2) . . . . ? N51B Zr2B C15B C11B -17.61(19) . . . . ? C14B Zr2B C15B C11B -115.9(2) . . . . ? Cl8B Zr2B C15B C11B 67.83(15) . . . . ? Cl7B Zr2B C15B C11B 156.81(15) . . . . ? N91B Zr2B C15B C11B 122.4(2) . . . . ? C13B Zr2B C15B C11B -78.17(17) . . . . ? Cl6B Zr2B C15B C11B -121.06(14) . . . . ? C12B Zr2B C15B C11B -37.19(14) . . . . ? C11B B1B N21B C22B 35.4(3) . . . . ? C41B B1B N21B C22B -89.7(3) . . . . ? C31B B1B N21B C22B 151.7(2) . . . . ? C11B B1B N21B C26B -149.1(2) . . . . ? C41B B1B N21B C26B 85.8(3) . . . . ? C31B B1B N21B C26B -32.7(3) . . . . ? C26B N21B C22B C23B 1.7(4) . . . . ? B1B N21B C22B C23B 177.3(2) . . . . ? N21B C22B C23B C24B -1.5(4) . . . . ? C22B C23B C24B C25B 0.3(4) . . . . ? C23B C24B C25B C26B 0.6(4) . . . . ? C22B N21B C26B C25B -0.8(4) . . . . ? B1B N21B C26B C25B -176.5(2) . . . . ? C24B C25B C26B N21B -0.4(4) . . . . ? N21B B1B C31B C36B -90.4(3) . . . . ? C11B B1B C31B C36B 28.7(3) . . . . ? C41B B1B C31B C36B 151.9(2) . . . . ? N21B B1B C31B C32B 90.0(3) . . . . ? C11B B1B C31B C32B -150.8(2) . . . . ? C41B B1B C31B C32B -27.6(3) . . . . ? C36B C31B C32B F32B 175.6(2) . . . . ? B1B C31B C32B F32B -4.9(4) . . . . ? C36B C31B C32B C33B -2.7(4) . . . . ? B1B C31B C32B C33B 176.9(2) . . . . ? F32B C32B C33B F33B 0.3(3) . . . . ? C31B C32B C33B F33B 178.6(2) . . . . ? F32B C32B C33B C34B -178.5(2) . . . . ? C31B C32B C33B C34B -0.1(4) . . . . ? F33B C33B C34B F34B 1.5(4) . . . . ? C32B C33B C34B F34B -179.7(2) . . . . ? F33B C33B C34B C35B -176.8(2) . . . . ? C32B C33B C34B C35B 2.0(4) . . . . ? F34B C34B C35B F35B 0.1(4) . . . . ? C33B C34B C35B F35B 178.4(2) . . . . ? F34B C34B C35B C36B -179.1(2) . . . . ? C33B C34B C35B C36B -0.8(4) . . . . ? F35B C35B C36B F36B -2.2(4) . . . . ? C34B C35B C36B F36B 177.0(2) . . . . ? F35B C35B C36B C31B 178.4(2) . . . . ? C34B C35B C36B C31B -2.5(4) . . . . ? C32B C31B C36B F36B -175.4(2) . . . . ? B1B C31B C36B F36B 5.0(4) . . . . ? C32B C31B C36B C35B 4.0(4) . . . . ? B1B C31B C36B C35B -175.6(2) . . . . ? N21B B1B C41B C46B 14.2(3) . . . . ? C11B B1B C41B C46B -110.2(3) . . . . ? C31B B1B C41B C46B 129.7(2) . . . . ? N21B B1B C41B C42B -164.3(2) . . . . ? C11B B1B C41B C42B 71.2(3) . . . . ? C31B B1B C41B C42B -48.9(3) . . . . ? C46B C41B C42B F42B -177.6(2) . . . . ? B1B C41B C42B F42B 1.2(3) . . . . ? C46B C41B C42B C43B 0.2(4) . . . . ? B1B C41B C42B C43B 179.0(2) . . . . ? F42B C42B C43B F43B -2.6(3) . . . . ? C41B C42B C43B F43B 179.5(2) . . . . ? F42B C42B C43B C44B 177.3(2) . . . . ? C41B C42B C43B C44B -0.6(4) . . . . ? F43B C43B C44B F44B 0.7(4) . . . . ? C42B C43B C44B F44B -179.2(2) . . . . ? F43B C43B C44B C45B -180.0(2) . . . . ? C42B C43B C44B C45B 0.1(4) . . . . ? F44B C44B C45B F45B 1.0(4) . . . . ? C43B C44B C45B F45B -178.4(2) . . . . ? F44B C44B C45B C46B 179.9(2) . . . . ? C43B C44B C45B C46B 0.6(4) . . . . ? F45B C45B C46B F46B -0.7(3) . . . . ? C44B C45B C46B F46B -179.7(2) . . . . ? F45B C45B C46B C41B 177.9(2) . . . . ? C44B C45B C46B C41B -1.1(4) . . . . ? C42B C41B C46B F46B 179.2(2) . . . . ? B1B C41B C46B F46B 0.5(4) . . . . ? C42B C41B C46B C45B 0.6(4) . . . . ? B1B C41B C46B C45B -178.0(2) . . . . ? C14B Zr2B N51B C52B 134.81(19) . . . . ? Cl8B Zr2B N51B C52B 7.90(19) . . . . ? Cl7B Zr2B N51B C52B -70.7(2) . . . . ? N91B Zr2B N51B C52B -69.54(19) . . . . ? C13B Zr2B N51B C52B 140.3(2) . . . . ? Cl6B Zr2B N51B C52B -145.34(19) . . . . ? C15B Zr2B N51B C52B 95.8(2) . . . . ? C12B Zr2B N51B C52B 112.0(2) . . . . ? C11B Zr2B N51B C52B 86.6(2) . . . . ? C14B Zr2B N51B C56B -50.6(2) . . . . ? Cl8B Zr2B N51B C56B -177.55(17) . . . . ? Cl7B Zr2B N51B C56B 103.80(19) . . . . ? N91B Zr2B N51B C56B 105.01(18) . . . . ? C13B Zr2B N51B C56B -45.17(18) . . . . ? Cl6B Zr2B N51B C56B 29.21(17) . . . . ? C15B Zr2B N51B C56B -89.66(19) . . . . ? C12B Zr2B N51B C56B -73.48(18) . . . . ? C11B Zr2B N51B C56B -98.80(18) . . . . ? C56B N51B C52B C53B 0.0(4) . . . . ? Zr2B N51B C52B C53B 174.7(2) . . . . ? N51B C52B C53B C54B -0.6(4) . . . . ? C52B C53B C54B C55B -0.2(4) . . . . ? C53B C54B C55B C56B 1.4(4) . . . . ? C52B N51B C56B C55B 1.3(4) . . . . ? Zr2B N51B C56B C55B -173.56(19) . . . . ? C54B C55B C56B N51B -2.1(4) . . . . ? N51B Zr2B N91B C96B -38.66(19) . . . . ? C14B Zr2B N91B C96B 92.2(3) . . . . ? Cl8B Zr2B N91B C96B -128.02(19) . . . . ? Cl7B Zr2B N91B C96B 140.84(19) . . . . ? C13B Zr2B N91B C96B 26.1(3) . . . . ? Cl6B Zr2B N91B C96B 51.37(18) . . . . ? C15B Zr2B N91B C96B 175.2(2) . . . . ? C12B Zr2B N91B C96B -36.0(3) . . . . ? C11B Zr2B N91B C96B -102.9(2) . . . . ? N51B Zr2B N91B C92B 139.4(2) . . . . ? C14B Zr2B N91B C92B -89.7(3) . . . . ? Cl8B Zr2B N91B C92B 50.02(19) . . . . ? Cl7B Zr2B N91B C92B -41.12(19) . . . . ? C13B Zr2B N91B C92B -155.9(2) . . . . ? Cl6B Zr2B N91B C92B -130.6(2) . . . . ? C15B Zr2B N91B C92B -6.7(3) . . . . ? C12B Zr2B N91B C92B 142.1(2) . . . . ? C11B Zr2B N91B C92B 75.1(3) . . . . ? C96B N91B C92B C93B 0.9(4) . . . . ? Zr2B N91B C92B C93B -177.3(2) . . . . ? N91B C92B C93B C94B 0.6(5) . . . . ? C92B C93B C94B C95B -1.2(5) . . . . ? C93B C94B C95B C96B 0.5(4) . . . . ? C92B N91B C96B C95B -1.7(4) . . . . ? Zr2B N91B C96B C95B 176.4(2) . . . . ? C94B C95B C96B N91B 1.0(4) . . . . ? Cl3C C1C Cl2C C1C' 0.5(6) . . . . ? Cl1C C1C Cl2C C1C' 123.7(6) . . . . ? Cl2C C1C Cl3C C1C' -0.5(6) . . . . ? Cl1C C1C Cl3C C1C' -124.7(7) . . . . ? C1C Cl3C C1C' Cl4C -126.5(10) . . . . ? C1C Cl3C C1C' Cl2C 0.5(7) . . . . ? C1C Cl2C C1C' Cl3C -0.6(7) . . . . ? C1C Cl2C C1C' Cl4C 125.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.42 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.724 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.067 #===END data_simonl5 _database_code_CSD 201470 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 16' _chemical_melting_point ? _chemical_formula_moiety 'C27 H14 B Cl4 F10 N2 Nb' _chemical_formula_structural [Nb(py)Cl4{C5H4B(py)(C6F5)2}] _chemical_formula_sum 'C27 H14 B Cl4 F10 N2 Nb' _chemical_formula_weight 801.92 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.553(2) _cell_length_b 15.695(1) _cell_length_c 21.135(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.14(1) _cell_angle_gamma 90.00 _cell_volume 5700.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour 'bright red' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30927 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.33 _reflns_number_total 9754 _reflns_number_gt 5979 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'XS (Sheldrick, 1997)' _computing_structure_refinement 'XL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1045P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9754 _refine_ls_number_parameters 1199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1699 _refine_ls_wR_factor_gt 0.1510 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.008 _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 Nb3X Nb 0.15153(13) 0.88424(17) 0.44243(12) 0.0323(6) Uani 0.15 1 d P A 1 C11X C 0.0965(18) 1.034(2) 0.3904(17) 0.045(7) Uiso 0.15 1 d P A 1 C12X C 0.0901(15) 1.0211(18) 0.4530(14) 0.031(6) Uiso 0.15 1 d P A 1 C13X C 0.1674(18) 1.015(2) 0.5076(17) 0.048(8) Uiso 0.15 1 d P A 1 C14X C 0.2165(16) 1.0212(19) 0.4720(15) 0.038(6) Uiso 0.15 1 d P A 1 C15X C 0.1728(18) 1.029(2) 0.4033(18) 0.048(8) Uiso 0.15 1 d P A 1 B1X B 0.0177(17) 1.060(2) 0.3224(17) 0.034(7) Uiso 0.15 1 d P A 1 N21X N 0.0479(14) 1.0901(17) 0.2592(13) 0.043(6) Uiso 0.15 1 d P A 1 C22X C 0.0960(14) 1.0428(18) 0.2441(13) 0.030(6) Uiso 0.15 1 d P A 1 C23X C 0.1120(19) 1.060(2) 0.1884(18) 0.051(8) Uiso 0.15 1 d P A 1 C24X C 0.087(2) 1.143(3) 0.154(2) 0.052(9) Uiso 0.15 1 d P A 1 C25X C 0.039(2) 1.184(3) 0.177(2) 0.043(9) Uiso 0.15 1 d P A 1 C26X C 0.0187(19) 1.167(2) 0.2258(18) 0.051(8) Uiso 0.15 1 d P A 1 C31X C -0.0233(19) 1.149(2) 0.3434(17) 0.031(9) Uiso 0.15 1 d P A 1 C32X C -0.094(2) 1.170(2) 0.3200(16) 0.028(6) Uiso 0.15 1 d P A 1 F32X F -0.1497(10) 1.1228(12) 0.2679(10) 0.050(4) Uiso 0.15 1 d P A 1 C33X C -0.129(2) 1.236(3) 0.335(2) 0.063(10) Uiso 0.15 1 d P A 1 F33X F -0.2017(16) 1.2605(18) 0.3083(15) 0.095(8) Uiso 0.15 1 d P A 1 C34X C -0.072(3) 1.296(3) 0.384(3) 0.086(13) Uiso 0.15 1 d P A 1 F34X F -0.1087(15) 1.3701(18) 0.3993(14) 0.094(8) Uiso 0.15 1 d P A 1 C35X C -0.001(2) 1.279(2) 0.4089(18) 0.054(8) Uiso 0.15 1 d P A 1 F35X F 0.050(2) 1.330(3) 0.457(2) 0.125(16) Uiso 0.15 1 d P A 1 C36X C 0.0257(19) 1.205(2) 0.3897(17) 0.049(8) Uiso 0.15 1 d P A 1 F36X F 0.1078(12) 1.1940(14) 0.4211(11) 0.053(5) Uiso 0.15 1 d P A 1 C41X C -0.0508(15) 0.9842(18) 0.2932(14) 0.032(6) Uiso 0.15 1 d P A 1 C42X C -0.0985(15) 0.9593(19) 0.3286(15) 0.037(6) Uiso 0.15 1 d P A 1 F42X F -0.0899(10) 1.0038(12) 0.3853(9) 0.049(4) Uiso 0.15 1 d P A 1 C43X C -0.153(2) 0.898(2) 0.309(2) 0.057(9) Uiso 0.15 1 d P A 1 F43X F -0.1901(12) 0.8775(14) 0.3528(11) 0.065(5) Uiso 0.15 1 d P A 1 C44X C -0.1627(16) 0.8481(19) 0.2538(15) 0.038(6) Uiso 0.15 1 d P A 1 F44X F -0.212(2) 0.786(2) 0.2320(18) 0.114(11) Uiso 0.15 1 d P A 1 C45X C -0.1239(18) 0.873(2) 0.2136(17) 0.046(7) Uiso 0.15 1 d P A 1 F45X F -0.1283(13) 0.8200(16) 0.1560(12) 0.067(6) Uiso 0.15 1 d P A 1 C46X C -0.0671(17) 0.936(2) 0.2319(16) 0.044(7) Uiso 0.15 1 d P A 1 F46X F -0.0293(10) 0.9488(12) 0.1890(9) 0.050(4) Uiso 0.15 1 d P A 1 Cl6X Cl 0.2183(6) 0.8489(7) 0.5621(6) 0.041(3) Uani 0.15 1 d P A 1 Cl7X Cl 0.2734(5) 0.8616(7) 0.4309(5) 0.040(2) Uani 0.15 1 d P A 1 Cl8X Cl 0.0923(5) 0.8501(6) 0.3225(4) 0.0389(17) Uani 0.15 1 d P A 1 N91X N 0.1566(15) 0.7320(19) 0.4396(14) 0.048(6) Uiso 0.15 1 d P A 1 C92X C 0.1787(18) 0.689(2) 0.3972(18) 0.050(8) Uiso 0.15 1 d P A 1 C93X C 0.178(2) 0.600(3) 0.390(2) 0.065(10) Uiso 0.15 1 d P A 1 C94X C 0.152(3) 0.553(3) 0.432(2) 0.070(11) Uiso 0.15 1 d P A 1 C95X C 0.1312(17) 0.595(2) 0.4789(16) 0.046(7) Uiso 0.15 1 d P A 1 C96X C 0.133(2) 0.684(2) 0.484(2) 0.058(9) Uiso 0.15 1 d P A 1 Nb4Y Nb 0.35573(14) 0.13203(17) 0.05508(13) 0.0336(6) Uani 0.15 1 d P B 1 C11Y C 0.4068(19) 0.278(2) 0.1086(18) 0.049(8) Uiso 0.15 1 d P B 1 C12Y C 0.4174(15) 0.2709(18) 0.0466(14) 0.032(6) Uiso 0.15 1 d P B 1 C13Y C 0.3414(17) 0.267(2) -0.0035(16) 0.044(7) Uiso 0.15 1 d P B 1 C14Y C 0.2896(17) 0.265(2) 0.0230(17) 0.045(7) Uiso 0.15 1 d P B 1 C15Y C 0.331(2) 0.275(2) 0.094(2) 0.051(9) Uiso 0.15 1 d P B 1 B1Y B 0.4830(18) 0.308(2) 0.1782(17) 0.034(7) Uiso 0.15 1 d P B 1 N21Y N 0.4514(13) 0.3333(16) 0.2387(13) 0.041(6) Uiso 0.15 1 d P B 1 C22Y C 0.3991(19) 0.287(2) 0.2525(18) 0.051(8) Uiso 0.15 1 d P B 1 C23Y C 0.3748(19) 0.310(2) 0.3037(18) 0.052(8) Uiso 0.15 1 d P B 1 C24Y C 0.404(2) 0.388(3) 0.343(2) 0.046(9) Uiso 0.15 1 d P B 1 C25Y C 0.452(3) 0.428(3) 0.327(2) 0.041(9) Uiso 0.15 1 d P B 1 C26Y C 0.4771(19) 0.410(2) 0.2772(18) 0.050(8) Uiso 0.15 1 d P B 1 C31Y C 0.5251(19) 0.399(2) 0.1613(18) 0.030(9) Uiso 0.15 1 d P B 1 C32Y C 0.597(2) 0.421(2) 0.1924(19) 0.046(8) Uiso 0.15 1 d P B 1 F32Y F 0.6496(10) 0.3727(12) 0.2468(10) 0.050(4) Uiso 0.15 1 d P B 1 C33Y C 0.6323(19) 0.494(2) 0.1799(18) 0.051(8) Uiso 0.15 1 d P B 1 F33Y F 0.7041(14) 0.5176(17) 0.2130(14) 0.075(7) Uiso 0.15 1 d P B 1 C34Y C 0.585(2) 0.543(3) 0.134(2) 0.070(10) Uiso 0.15 1 d P B 1 F34Y F 0.6136(12) 0.6256(14) 0.1230(12) 0.067(6) Uiso 0.15 1 d P B 1 C35Y C 0.497(2) 0.536(3) 0.092(2) 0.070(11) Uiso 0.15 1 d P B 1 C36Y C 0.4781(17) 0.457(2) 0.1157(16) 0.042(7) Uiso 0.15 1 d P B 1 F36Y F 0.3994(12) 0.4411(14) 0.0823(11) 0.062(5) Uiso 0.15 1 d P B 1 C41Y C 0.5529(17) 0.231(2) 0.2117(16) 0.043(7) Uiso 0.15 1 d P B 1 C42Y C 0.6018(18) 0.208(2) 0.1717(17) 0.049(8) Uiso 0.15 1 d P B 1 F42Y F 0.5926(9) 0.2575(11) 0.1200(9) 0.044(4) Uiso 0.15 1 d P B 1 C43Y C 0.654(2) 0.148(3) 0.190(2) 0.066(10) Uiso 0.15 1 d P B 1 F43Y F 0.6931(12) 0.1280(14) 0.1511(11) 0.067(6) Uiso 0.15 1 d P B 1 C44Y C 0.663(2) 0.097(3) 0.244(2) 0.075(11) Uiso 0.15 1 d P B 1 F44Y F 0.7110(13) 0.0296(15) 0.2615(12) 0.074(6) Uiso 0.15 1 d P B 1 C45Y C 0.6215(18) 0.117(2) 0.2867(17) 0.046(7) Uiso 0.15 1 d P B 1 F45Y F 0.6259(13) 0.0658(17) 0.3413(12) 0.069(6) Uiso 0.15 1 d P B 1 C46Y C 0.571(2) 0.177(3) 0.268(2) 0.065(10) Uiso 0.15 1 d P B 1 F46Y F 0.5278(13) 0.1910(16) 0.3107(12) 0.080(6) Uiso 0.15 1 d P B 1 Cl6Y Cl 0.2979(6) 0.0972(7) -0.0654(4) 0.054(2) Uani 0.15 1 d P B 1 Cl7Y Cl 0.2311(4) 0.1047(6) 0.0630(4) 0.048(2) Uani 0.15 1 d P B 1 Cl8Y Cl 0.4100(5) 0.0957(5) 0.1735(4) 0.0379(17) Uani 0.15 1 d P B 1 N91Y N 0.3547(15) -0.017(2) 0.0565(14) 0.046(7) Uiso 0.15 1 d P B 1 C92Y C 0.3302(16) -0.0652(19) 0.0964(15) 0.037(6) Uiso 0.15 1 d P B 1 C93Y C 0.3333(19) -0.150(2) 0.1029(18) 0.052(8) Uiso 0.15 1 d P B 1 C94Y C 0.362(2) -0.201(3) 0.062(2) 0.064(10) Uiso 0.15 1 d P B 1 C95Y C 0.381(2) -0.154(3) 0.014(2) 0.073(11) Uiso 0.15 1 d P B 1 C96Y C 0.3827(19) -0.063(2) 0.0154(19) 0.054(8) Uiso 0.15 1 d P B 1 Nb1A Nb 0.35024(2) 0.63330(3) 0.05628(2) 0.03589(16) Uani 0.85 1 d P C 2 C11A C 0.4093(3) 0.7771(3) 0.1097(3) 0.0383(12) Uani 0.85 1 d P C 2 C12A C 0.4135(3) 0.7689(3) 0.0441(3) 0.0405(12) Uani 0.85 1 d P C 2 H12A H 0.4593 0.7662 0.0361 0.049 Uiso 0.85 1 calc PR C 2 C13A C 0.3382(3) 0.7653(4) -0.0067(3) 0.0456(13) Uani 0.85 1 d P C 2 H13A H 0.3258 0.7617 -0.0535 0.055 Uiso 0.85 1 calc PR C 2 C14A C 0.2858(3) 0.7681(4) 0.0260(3) 0.0472(14) Uani 0.85 1 d P C 2 H14A H 0.2319 0.7669 0.0046 0.057 Uiso 0.85 1 calc PR C 2 C15A C 0.3280(3) 0.7731(4) 0.0968(3) 0.0435(13) Uani 0.85 1 d P C 2 H15A H 0.3064 0.7738 0.1300 0.052 Uiso 0.85 1 calc PR C 2 B1A B 0.4847(3) 0.8078(4) 0.1785(3) 0.0384(14) Uani 0.85 1 d P C 2 N21A N 0.4550(2) 0.8372(3) 0.2381(2) 0.0390(10) Uani 0.85 1 d P C 2 C22A C 0.4051(3) 0.7885(4) 0.2559(3) 0.0480(14) Uani 0.85 1 d P C 2 H22A H 0.3847 0.7393 0.2311 0.058 Uiso 0.85 1 calc PR C 2 C23A C 0.3840(3) 0.8099(4) 0.3094(3) 0.0532(16) Uani 0.85 1 d P C 2 H23A H 0.3503 0.7749 0.3207 0.064 Uiso 0.85 1 calc PR C 2 C24A C 0.4124(3) 0.8827(4) 0.3465(3) 0.0533(16) Uani 0.85 1 d P C 2 H24A H 0.3989 0.8972 0.3832 0.064 Uiso 0.85 1 calc PR C 2 C25A C 0.4617(4) 0.9340(5) 0.3278(4) 0.0494(17) Uani 0.85 1 d P C 2 H25A H 0.4808 0.9846 0.3511 0.059 Uiso 0.85 1 calc PR C 2 C26A C 0.4824(3) 0.9096(3) 0.2743(3) 0.0417(13) Uani 0.85 1 d P C 2 H26A H 0.5164 0.9439 0.2627 0.050 Uiso 0.85 1 calc PR C 2 C31A C 0.5198(3) 0.8954(4) 0.1553(3) 0.0410(13) Uani 0.85 1 d P C 2 C32A C 0.5981(4) 0.9199(4) 0.1835(4) 0.0459(15) Uani 0.85 1 d P C 2 F32A F 0.65062(17) 0.8724(2) 0.23266(19) 0.0566(9) Uani 0.85 1 d P C 2 C33A C 0.6262(3) 0.9916(4) 0.1631(4) 0.0622(18) Uani 0.85 1 d P C 2 F33A F 0.7029(2) 1.0111(3) 0.1929(3) 0.0872(14) Uani 0.85 1 d P C 2 C34A C 0.5767(4) 1.0451(4) 0.1163(4) 0.072(2) Uani 0.85 1 d P C 2 F34A F 0.6049(3) 1.1174(3) 0.0980(3) 0.1092(18) Uani 0.85 1 d P C 2 C35A C 0.4980(4) 1.0281(4) 0.0879(4) 0.0635(18) Uani 0.85 1 d P C 2 F35A F 0.4589(3) 1.0857(2) 0.04371(18) 0.0932(13) Uani 1 1 d . C 2 C36A C 0.4729(3) 0.9553(4) 0.1090(3) 0.0494(14) Uani 0.85 1 d P C 2 F36A F 0.39487(18) 0.9426(2) 0.08041(19) 0.0565(9) Uani 0.85 1 d P C 2 C41A C 0.5522(3) 0.7333(3) 0.2078(3) 0.0374(12) Uani 0.85 1 d P C 2 C42A C 0.5963(3) 0.7090(4) 0.1700(3) 0.0439(13) Uani 0.85 1 d P C 2 F42A F 0.58862(17) 0.7540(2) 0.11243(16) 0.0480(8) Uani 0.85 1 d P C 2 C43A C 0.6502(3) 0.6450(4) 0.1867(3) 0.0472(14) Uani 0.85 1 d P C 2 F43A F 0.68802(19) 0.6251(2) 0.14603(19) 0.0613(10) Uani 0.85 1 d P C 2 C44A C 0.6626(3) 0.5973(4) 0.2448(3) 0.0502(14) Uani 0.85 1 d P C 2 F44A F 0.71180(19) 0.5303(2) 0.2613(2) 0.0657(10) Uani 0.85 1 d P C 2 C45A C 0.6225(3) 0.6182(4) 0.2852(3) 0.0480(14) Uani 0.85 1 d P C 2 F45A F 0.6315(2) 0.5703(3) 0.3417(2) 0.0647(11) Uani 0.85 1 d P C 2 C46A C 0.5696(3) 0.6846(4) 0.2664(3) 0.0439(13) Uani 0.85 1 d P C 2 F46A F 0.53245(18) 0.6986(2) 0.31061(16) 0.0519(8) Uani 0.85 1 d P C 2 Cl5A Cl 0.47133(7) 0.59444(9) 0.04615(7) 0.0401(3) Uani 0.85 1 d P C 2 Cl6A Cl 0.28568(11) 0.59553(13) -0.06283(10) 0.0472(5) Uani 0.85 1 d P C 2 Cl7A Cl 0.22626(11) 0.60894(13) 0.06715(11) 0.0472(5) Uani 0.85 1 d P C 2 Cl8A Cl 0.40902(8) 0.59893(9) 0.17664(7) 0.0412(3) Uani 0.85 1 d P C 2 N91A N 0.3450(2) 0.4812(3) 0.0588(2) 0.0388(10) Uani 0.85 1 d P C 2 C92A C 0.3200(3) 0.4384(4) 0.1023(3) 0.0422(13) Uani 0.85 1 d P C 2 H92A H 0.3027 0.4697 0.1311 0.051 Uiso 0.85 1 calc PR C 2 C93A C 0.3189(3) 0.3517(4) 0.1059(3) 0.0482(14) Uani 0.85 1 d P C 2 H93A H 0.3007 0.3254 0.1364 0.058 Uiso 0.85 1 calc PR C 2 C94A C 0.3448(4) 0.3031(4) 0.0644(3) 0.0525(15) Uani 0.85 1 d P C 2 H94A H 0.3451 0.2439 0.0667 0.063 Uiso 0.85 1 calc PR C 2 C95A C 0.3698(3) 0.3444(4) 0.0202(3) 0.0513(14) Uani 0.85 1 d P C 2 H95A H 0.3870 0.3134 -0.0088 0.062 Uiso 0.85 1 calc PR C 2 C96A C 0.3698(3) 0.4326(4) 0.0180(3) 0.0456(13) Uani 0.85 1 d P C 2 H96A H 0.3875 0.4595 -0.0126 0.055 Uiso 0.85 1 calc PR C 2 Nb2B Nb 0.14487(2) 0.38286(3) 0.44499(2) 0.03718(16) Uani 0.85 1 d P D 2 C11B C 0.0887(3) 0.5270(3) 0.3883(3) 0.0368(12) Uani 0.85 1 d P D 2 C12B C 0.0830(3) 0.5210(3) 0.4536(3) 0.0413(13) Uani 0.85 1 d P D 2 H12B H 0.0364 0.5198 0.4606 0.050 Uiso 0.85 1 calc PR D 2 C13B C 0.1573(3) 0.5174(4) 0.5060(3) 0.0471(14) Uani 0.85 1 d P D 2 H13B H 0.1681 0.5159 0.5527 0.056 Uiso 0.85 1 calc PR D 2 C14B C 0.2117(3) 0.5165(3) 0.4754(3) 0.0436(13) Uani 0.85 1 d P D 2 H14B H 0.2655 0.5136 0.4977 0.052 Uiso 0.85 1 calc PR D 2 C15B C 0.1701(3) 0.5209(4) 0.4036(3) 0.0423(13) Uani 0.85 1 d P D 2 H15B H 0.1929 0.5200 0.3712 0.051 Uiso 0.85 1 calc PR D 2 B1B B 0.0156(3) 0.5572(4) 0.3189(3) 0.0387(14) Uani 0.85 1 d P D 2 N21B N 0.0487(2) 0.5852(3) 0.2598(2) 0.0382(10) Uani 0.85 1 d P D 2 C22B C 0.1005(3) 0.5365(4) 0.2460(3) 0.0406(12) Uani 0.85 1 d P D 2 H22B H 0.1190 0.4871 0.2712 0.049 Uiso 0.85 1 calc PR D 2 C23B C 0.1270(3) 0.5580(4) 0.1955(3) 0.0529(15) Uani 0.85 1 d P D 2 H23B H 0.1627 0.5234 0.1866 0.063 Uiso 0.85 1 calc PR D 2 C24B C 0.0998(4) 0.6316(5) 0.1579(3) 0.0510(15) Uani 0.85 1 d P D 2 H24B H 0.1169 0.6474 0.1235 0.061 Uiso 0.85 1 calc PR D 2 C25B C 0.0466(4) 0.6808(5) 0.1730(3) 0.0462(15) Uani 0.85 1 d P D 2 H25B H 0.0275 0.7307 0.1488 0.055 Uiso 0.85 1 calc PR D 2 C26B C 0.0223(3) 0.6563(4) 0.2233(3) 0.0414(13) Uani 0.85 1 d P D 2 H26B H -0.0138 0.6899 0.2327 0.050 Uiso 0.85 1 calc PR D 2 C31B C -0.0210(3) 0.6450(4) 0.3384(3) 0.0396(13) Uani 0.85 1 d P D 2 C32B C -0.0987(3) 0.6701(4) 0.3045(3) 0.0443(14) Uani 0.85 1 d P D 2 F32B F -0.14885(17) 0.6208(2) 0.25565(18) 0.0534(8) Uani 0.85 1 d P D 2 C33B C -0.1289(3) 0.7452(4) 0.3166(3) 0.0529(15) Uani 0.85 1 d P D 2 F33B F -0.2043(2) 0.7661(3) 0.2799(3) 0.0746(12) Uani 0.85 1 d P D 2 C34B C -0.0823(4) 0.8014(4) 0.3627(4) 0.0593(17) Uani 0.85 1 d P D 2 F34B F -0.1113(3) 0.8776(2) 0.3725(2) 0.0788(12) Uani 0.85 1 d P D 2 C35B C -0.0058(4) 0.7816(4) 0.3984(3) 0.0551(15) Uani 0.85 1 d P D 2 F35B F 0.03756(17) 0.83857(18) 0.44786(16) 0.0618(8) Uani 1 1 d . D 2 C36B C 0.0233(3) 0.7050(4) 0.3849(3) 0.0463(14) Uani 0.85 1 d P D 2 F36B F 0.10046(18) 0.6919(2) 0.41992(19) 0.0570(9) Uani 0.85 1 d P D 2 C41B C -0.0516(3) 0.4823(3) 0.2890(3) 0.0393(12) Uani 0.85 1 d P D 2 C42B C -0.0984(3) 0.4606(4) 0.3253(3) 0.0447(13) Uani 0.85 1 d P D 2 F42B F -0.09270(17) 0.5069(2) 0.38058(17) 0.0508(8) Uani 0.85 1 d P D 2 C43B C -0.1514(3) 0.3952(4) 0.3080(3) 0.0536(16) Uani 0.85 1 d P D 2 F43B F -0.19271(19) 0.3781(2) 0.3474(2) 0.0655(10) Uani 0.85 1 d P D 2 C44B C -0.1616(3) 0.3466(4) 0.2518(4) 0.0540(16) Uani 0.85 1 d P D 2 F44B F -0.21072(18) 0.2795(2) 0.2350(2) 0.0722(11) Uani 0.85 1 d P D 2 C45B C -0.1191(3) 0.3658(4) 0.2126(3) 0.0522(15) Uani 0.85 1 d P D 2 F45B F -0.1268(2) 0.3158(3) 0.1575(2) 0.0649(12) Uani 0.85 1 d P D 2 C46B C -0.0663(3) 0.4324(4) 0.2311(3) 0.0441(13) Uani 0.85 1 d P D 2 F46B F -0.02784(17) 0.4437(2) 0.18861(16) 0.0498(8) Uani 0.85 1 d P D 2 Cl5B Cl 0.01992(10) 0.34808(10) 0.45183(8) 0.0448(4) Uani 0.85 1 d P D 2 Cl6B Cl 0.20331(10) 0.34693(11) 0.56486(7) 0.0502(4) Uani 0.85 1 d P D 2 Cl7B Cl 0.26930(8) 0.35515(11) 0.43700(8) 0.0463(4) Uani 0.85 1 d P D 2 Cl8B Cl 0.08849(8) 0.34628(9) 0.32465(7) 0.0395(3) Uani 0.85 1 d P D 2 N91B N 0.1469(3) 0.2307(3) 0.4447(2) 0.0431(11) Uani 0.85 1 d P D 2 C92B C 0.1719(3) 0.1842(4) 0.4028(3) 0.0437(13) Uani 0.85 1 d P D 2 H92B H 0.1910 0.2135 0.3741 0.052 Uiso 0.85 1 calc PR D 2 C93B C 0.1709(3) 0.0977(4) 0.3998(3) 0.0464(13) Uani 0.85 1 d P D 2 H93B H 0.1901 0.0696 0.3707 0.056 Uiso 0.85 1 calc PR D 2 C94B C 0.1411(3) 0.0514(4) 0.4406(3) 0.0486(14) Uani 0.85 1 d P D 2 H94B H 0.1391 -0.0078 0.4389 0.058 Uiso 0.85 1 calc PR D 2 C95B C 0.1151(4) 0.0961(4) 0.4831(3) 0.0526(14) Uani 0.85 1 d P D 2 H95B H 0.0946 0.0675 0.5110 0.063 Uiso 0.85 1 calc PR D 2 C96B C 0.1191(3) 0.1834(4) 0.4846(3) 0.0499(14) Uani 0.85 1 d P D 2 H96B H 0.1019 0.2121 0.5147 0.060 Uiso 0.85 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb3X 0.0357(13) 0.0288(16) 0.0274(14) 0.0001(11) 0.0062(11) 0.0016(10) Cl6X 0.045(5) 0.040(7) 0.027(4) -0.006(5) 0.002(3) 0.009(5) Cl7X 0.033(4) 0.054(7) 0.034(5) -0.002(5) 0.013(3) -0.011(5) Cl8X 0.053(5) 0.031(5) 0.027(4) 0.000(3) 0.008(4) -0.002(4) Nb4Y 0.0380(13) 0.0275(16) 0.0308(15) -0.0025(11) 0.0077(12) -0.0010(10) Cl6Y 0.067(6) 0.044(6) 0.042(5) -0.003(4) 0.009(4) -0.006(5) Cl7Y 0.037(4) 0.047(6) 0.046(5) -0.003(4) 0.000(4) 0.004(4) Cl8Y 0.042(4) 0.036(5) 0.032(4) -0.002(3) 0.009(4) 0.003(3) Nb1A 0.0377(3) 0.0332(3) 0.0345(3) -0.0009(2) 0.0109(2) -0.00124(18) C11A 0.040(3) 0.027(3) 0.044(3) 0.003(2) 0.011(3) 0.004(2) C12A 0.049(3) 0.029(3) 0.044(3) 0.000(2) 0.020(3) -0.003(2) C13A 0.051(3) 0.036(3) 0.045(3) 0.003(3) 0.012(3) -0.001(2) C14A 0.039(3) 0.035(3) 0.055(4) 0.000(3) 0.004(3) 0.003(2) C15A 0.036(3) 0.041(4) 0.052(4) -0.006(3) 0.015(3) 0.002(2) B1A 0.036(3) 0.039(4) 0.041(4) -0.006(3) 0.015(3) -0.003(2) N21A 0.039(2) 0.035(3) 0.041(3) -0.002(2) 0.012(2) -0.0018(18) C22A 0.048(3) 0.041(4) 0.059(4) -0.004(3) 0.025(3) -0.006(2) C23A 0.048(3) 0.061(4) 0.059(4) -0.003(3) 0.030(3) -0.002(3) C24A 0.054(3) 0.060(4) 0.052(4) -0.008(3) 0.026(3) 0.000(3) C25A 0.054(4) 0.040(5) 0.054(4) -0.006(3) 0.019(3) 0.002(3) C26A 0.043(3) 0.037(3) 0.041(3) -0.005(2) 0.011(2) 0.000(2) C31A 0.041(3) 0.034(4) 0.045(3) -0.006(3) 0.013(3) -0.003(3) C32A 0.040(3) 0.045(4) 0.052(4) -0.003(3) 0.016(3) -0.005(3) F32A 0.0420(16) 0.051(2) 0.066(2) 0.0037(18) 0.0078(17) -0.0052(15) C33A 0.047(3) 0.057(4) 0.079(5) -0.002(4) 0.020(3) -0.015(3) F33A 0.053(2) 0.072(3) 0.130(4) 0.006(3) 0.028(2) -0.0243(19) C34A 0.075(4) 0.045(4) 0.090(6) 0.018(4) 0.025(4) -0.014(3) F34A 0.103(3) 0.073(3) 0.144(5) 0.044(3) 0.037(3) -0.028(3) C35A 0.073(4) 0.046(4) 0.064(5) 0.011(3) 0.018(4) -0.005(3) F35A 0.154(3) 0.053(2) 0.060(2) 0.0277(18) 0.026(2) 0.051(2) C36A 0.043(3) 0.042(4) 0.058(4) -0.002(3) 0.014(3) -0.001(2) F36A 0.0459(18) 0.041(2) 0.068(3) -0.0021(17) 0.0053(17) 0.0045(15) C41A 0.031(2) 0.036(3) 0.043(3) -0.005(2) 0.012(2) -0.003(2) C42A 0.036(3) 0.047(4) 0.048(4) 0.000(3) 0.016(3) 0.001(2) F42A 0.0459(17) 0.052(2) 0.050(2) 0.0054(16) 0.0226(15) 0.0059(14) C43A 0.036(3) 0.049(4) 0.054(4) -0.005(3) 0.015(3) -0.003(2) F43A 0.0527(19) 0.065(2) 0.074(3) -0.0049(19) 0.0326(19) 0.0134(16) C44A 0.041(3) 0.041(4) 0.061(4) -0.003(3) 0.011(3) 0.004(2) F44A 0.0456(18) 0.052(2) 0.089(3) 0.011(2) 0.013(2) 0.0146(15) C45A 0.045(3) 0.042(4) 0.048(4) 0.005(3) 0.007(3) -0.002(2) F45A 0.053(2) 0.066(3) 0.062(3) 0.026(2) 0.006(2) 0.008(2) C46A 0.037(3) 0.048(4) 0.043(3) -0.003(3) 0.010(2) -0.004(2) F46A 0.0553(18) 0.054(2) 0.047(2) 0.0029(16) 0.0203(16) 0.0011(15) Cl5A 0.0421(6) 0.0359(8) 0.0421(8) 0.0019(6) 0.0156(6) 0.0033(5) Cl6A 0.0520(10) 0.0448(13) 0.0386(9) -0.0025(9) 0.0101(8) 0.0003(9) Cl7A 0.0419(8) 0.0476(14) 0.0523(11) -0.0023(11) 0.0178(7) -0.0028(10) Cl8A 0.0459(7) 0.0365(8) 0.0364(8) -0.0012(6) 0.0100(6) -0.0042(6) N91A 0.040(2) 0.035(3) 0.038(3) -0.0035(19) 0.010(2) -0.0024(18) C92A 0.041(3) 0.043(4) 0.037(3) 0.001(2) 0.009(2) -0.005(2) C93A 0.056(3) 0.041(4) 0.038(3) -0.001(3) 0.006(3) -0.008(3) C94A 0.065(4) 0.041(4) 0.039(4) 0.003(3) 0.006(3) -0.006(3) C95A 0.059(3) 0.038(4) 0.050(4) -0.010(3) 0.013(3) 0.000(3) C96A 0.049(3) 0.047(4) 0.037(3) -0.003(3) 0.013(3) 0.002(2) Nb2B 0.0395(3) 0.0343(3) 0.0351(3) 0.0013(2) 0.0111(2) 0.00002(19) C11B 0.039(3) 0.030(3) 0.042(3) 0.000(2) 0.016(2) 0.001(2) C12B 0.050(3) 0.029(3) 0.046(3) -0.002(2) 0.019(3) -0.002(2) C13B 0.062(3) 0.039(3) 0.037(3) -0.005(2) 0.015(3) -0.007(3) C14B 0.042(3) 0.035(3) 0.046(3) 0.000(2) 0.008(3) -0.002(2) C15B 0.040(3) 0.038(3) 0.045(3) 0.006(3) 0.011(3) -0.002(2) B1B 0.039(3) 0.040(4) 0.039(4) 0.002(3) 0.016(3) -0.003(2) N21B 0.036(2) 0.037(3) 0.040(3) 0.000(2) 0.013(2) 0.0000(18) C22B 0.040(3) 0.037(3) 0.045(3) 0.003(2) 0.016(2) 0.004(2) C23B 0.053(3) 0.056(4) 0.055(4) 0.000(3) 0.026(3) 0.006(3) C24B 0.057(4) 0.051(4) 0.054(4) 0.002(3) 0.031(3) 0.000(3) C25B 0.046(4) 0.043(4) 0.052(4) 0.010(3) 0.021(3) 0.003(3) C26B 0.039(3) 0.038(3) 0.046(3) 0.001(2) 0.015(3) 0.002(2) C31B 0.045(3) 0.035(4) 0.039(3) 0.005(3) 0.015(3) 0.002(3) C32B 0.042(3) 0.038(3) 0.056(4) 0.004(3) 0.021(3) 0.000(2) F32B 0.0432(16) 0.045(2) 0.063(2) -0.0015(17) 0.0086(16) 0.0067(14) C33B 0.052(3) 0.044(4) 0.066(4) 0.003(3) 0.026(3) 0.009(3) F33B 0.052(2) 0.058(3) 0.114(4) 0.000(2) 0.031(2) 0.0159(17) C34B 0.074(4) 0.033(4) 0.080(5) 0.000(3) 0.040(4) 0.010(3) F34B 0.099(3) 0.045(2) 0.099(3) -0.008(2) 0.045(3) 0.012(2) C35B 0.065(4) 0.038(4) 0.062(4) -0.007(3) 0.024(3) -0.003(3) F35B 0.0713(18) 0.0343(18) 0.062(2) -0.0017(14) 0.0053(16) -0.0142(14) C36B 0.046(3) 0.039(4) 0.053(4) 0.003(3) 0.018(3) 0.003(2) F36B 0.0481(18) 0.041(2) 0.067(3) 0.0008(17) 0.0047(17) -0.0065(15) C41B 0.035(3) 0.035(3) 0.048(3) 0.005(2) 0.015(2) 0.002(2) C42B 0.038(3) 0.035(3) 0.060(4) -0.001(3) 0.017(3) 0.001(2) F42B 0.0525(18) 0.046(2) 0.061(2) -0.0061(16) 0.0298(17) -0.0054(14) C43B 0.038(3) 0.049(4) 0.076(5) 0.001(3) 0.024(3) -0.003(3) F43B 0.055(2) 0.056(2) 0.092(3) 0.004(2) 0.035(2) -0.0117(16) C44B 0.040(3) 0.035(3) 0.080(5) -0.003(3) 0.014(3) -0.005(2) F44B 0.0442(18) 0.051(2) 0.107(3) -0.011(2) 0.013(2) -0.0104(16) C45B 0.044(3) 0.046(4) 0.057(4) -0.013(3) 0.007(3) 0.002(3) F45B 0.053(2) 0.054(3) 0.070(3) -0.024(2) 0.004(2) -0.0048(19) C46B 0.037(3) 0.040(3) 0.047(4) 0.004(3) 0.007(3) 0.005(2) F46B 0.0516(17) 0.051(2) 0.0436(19) -0.0034(15) 0.0147(15) 0.0047(14) Cl5B 0.0496(8) 0.0380(9) 0.0497(9) -0.0031(6) 0.0220(7) -0.0046(6) Cl6B 0.0623(9) 0.0442(10) 0.0366(8) 0.0020(7) 0.0102(7) -0.0014(8) Cl7B 0.0396(7) 0.0461(11) 0.0512(9) 0.0007(7) 0.0147(7) 0.0020(6) Cl8B 0.0442(7) 0.0342(8) 0.0361(8) 0.0014(6) 0.0106(6) 0.0029(6) N91B 0.044(3) 0.040(3) 0.040(3) 0.002(2) 0.010(2) 0.000(2) C92B 0.041(3) 0.048(4) 0.036(3) 0.005(2) 0.008(2) 0.005(2) C93B 0.048(3) 0.038(4) 0.047(4) -0.001(3) 0.010(3) 0.004(2) C94B 0.053(3) 0.041(4) 0.040(4) 0.002(3) 0.004(3) 0.000(2) C95B 0.067(4) 0.041(4) 0.044(4) 0.008(3) 0.013(3) -0.003(3) C96B 0.060(3) 0.044(4) 0.045(4) 0.007(3) 0.018(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 Nb3X Cl7X 2.391(9) . ? Nb3X N91X 2.39(3) . ? Nb3X Cl8X 2.412(9) . ? Nb3X Cl6X 2.425(11) . ? Nb3X C14X 2.43(3) . ? Nb3X C13X 2.43(3) . ? Nb3X C12X 2.48(3) . ? Nb3X C15X 2.50(4) . ? Nb3X C11X 2.63(3) . ? C11X C15X 1.34(4) . ? C11X C12X 1.39(4) . ? C11X B1X 1.67(5) . ? C12X C13X 1.47(4) . ? C13X C14X 1.39(4) . ? C14X C15X 1.38(4) . ? B1X C41X 1.68(4) . ? B1X N21X 1.70(4) . ? B1X C31X 1.72(4) . ? N21X C22X 1.29(3) . ? N21X C26X 1.40(4) . ? C22X C23X 1.34(4) . ? C23X C24X 1.48(5) . ? C24X C25X 1.33(5) . ? C25X C26X 1.25(5) . ? C31X C32X 1.27(4) . ? C31X C36X 1.38(5) . ? C32X C33X 1.31(5) . ? C32X F32X 1.40(4) . ? C33X F33X 1.31(4) . ? C33X C34X 1.50(6) . ? C34X C35X 1.25(5) . ? C34X F34X 1.44(5) . ? C35X F35X 1.36(5) . ? C35X C36X 1.39(5) . ? C36X F36X 1.42(4) . ? C41X C42X 1.41(4) . ? C41X C46X 1.43(4) . ? C42X C43X 1.34(5) . ? C42X F42X 1.34(3) . ? C43X C44X 1.36(5) . ? C43X F43X 1.39(4) . ? C44X F44X 1.30(4) . ? C44X C45X 1.36(4) . ? C45X C46X 1.39(4) . ? C45X F45X 1.45(4) . ? C46X F46X 1.36(3) . ? N91X C92X 1.30(4) . ? N91X C96X 1.39(4) . ? C92X C93X 1.40(5) . ? C93X C94X 1.37(6) . ? C94X C95X 1.37(6) . ? C95X C96X 1.39(5) . ? Nb4Y N91Y 2.34(3) . ? Nb4Y C14Y 2.38(3) . ? Nb4Y Cl8Y 2.388(8) . ? Nb4Y C13Y 2.41(3) . ? Nb4Y Cl7Y 2.419(8) . ? Nb4Y Cl6Y 2.423(9) . ? Nb4Y C15Y 2.49(4) . ? Nb4Y C12Y 2.50(3) . ? Nb4Y C11Y 2.57(3) . ? C11Y C15Y 1.32(5) . ? C11Y C12Y 1.40(4) . ? C11Y B1Y 1.68(5) . ? C12Y C13Y 1.41(4) . ? C13Y C14Y 1.28(4) . ? C14Y C15Y 1.41(5) . ? B1Y N21Y 1.64(4) . ? B1Y C41Y 1.72(4) . ? B1Y C31Y 1.73(4) . ? N21Y C22Y 1.33(4) . ? N21Y C26Y 1.43(4) . ? C22Y C23Y 1.37(4) . ? C23Y C24Y 1.47(5) . ? C24Y C25Y 1.25(5) . ? C25Y C26Y 1.33(5) . ? C31Y C32Y 1.29(5) . ? C31Y C36Y 1.37(5) . ? C32Y C33Y 1.39(5) . ? C32Y F32Y 1.41(4) . ? C33Y C34Y 1.30(5) . ? C33Y F33Y 1.30(4) . ? C34Y F34Y 1.45(5) . ? C34Y C35Y 1.53(5) . ? C35Y C36Y 1.42(5) . ? C36Y F36Y 1.38(4) . ? C41Y C46Y 1.39(5) . ? C41Y C42Y 1.50(4) . ? C42Y F42Y 1.30(4) . ? C42Y C43Y 1.30(5) . ? C43Y F43Y 1.32(4) . ? C43Y C44Y 1.36(6) . ? C44Y F44Y 1.34(5) . ? C44Y C45Y 1.42(5) . ? C45Y C46Y 1.28(5) . ? C45Y F45Y 1.39(4) . ? C46Y F46Y 1.42(4) . ? N91Y C92Y 1.34(4) . ? N91Y C96Y 1.37(4) . ? C92Y C93Y 1.34(5) . ? C93Y C94Y 1.42(5) . ? C94Y C95Y 1.40(6) . ? C95Y C96Y 1.43(6) . ? Nb1A N91A 2.391(5) . ? Nb1A C14A 2.396(6) . ? Nb1A Cl5A 2.4140(12) . ? Nb1A Cl6A 2.419(2) . ? Nb1A Cl8A 2.4209(15) . ? Nb1A Cl7A 2.427(2) . ? Nb1A C13A 2.427(5) . ? Nb1A C15A 2.447(5) . ? Nb1A C12A 2.489(5) . ? Nb1A C11A 2.576(5) . ? C11A C12A 1.423(7) . ? C11A C15A 1.429(7) . ? C11A B1A 1.665(8) . ? C12A C13A 1.406(8) . ? C12A H12A 0.9300 . ? C13A C14A 1.389(8) . ? C13A H13A 0.9300 . ? C14A C15A 1.406(8) . ? C14A H14A 0.9300 . ? C15A H15A 0.9300 . ? B1A N21A 1.620(7) . ? B1A C41A 1.653(8) . ? B1A C31A 1.671(8) . ? N21A C26A 1.357(7) . ? N21A C22A 1.359(6) . ? C22A C23A 1.371(8) . ? C22A H22A 0.9300 . ? C23A C24A 1.373(9) . ? C23A H23A 0.9300 . ? C24A C25A 1.383(9) . ? C24A H24A 0.9300 . ? C25A C26A 1.378(8) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C31A C36A 1.399(8) . ? C31A C32A 1.401(8) . ? C32A F32A 1.350(7) . ? C32A C33A 1.376(9) . ? C33A F33A 1.356(7) . ? C33A C34A 1.357(10) . ? C34A F34A 1.364(7) . ? C34A C35A 1.380(9) . ? C35A F35A 1.306(7) . ? C35A C36A 1.370(8) . ? C36A F36A 1.357(6) . ? C41A C46A 1.386(8) . ? C41A C42A 1.395(7) . ? C42A C43A 1.366(8) . ? C42A F42A 1.368(6) . ? C43A F43A 1.335(6) . ? C43A C44A 1.382(8) . ? C44A F44A 1.349(6) . ? C44A C45A 1.366(8) . ? C45A F45A 1.367(7) . ? C45A C46A 1.382(8) . ? C46A F46A 1.371(6) . ? N91A C92A 1.352(6) . ? N91A C96A 1.355(7) . ? C92A C93A 1.364(8) . ? C92A H92A 0.9300 . ? C93A C94A 1.377(9) . ? C93A H93A 0.9300 . ? C94A C95A 1.355(9) . ? C94A H94A 0.9300 . ? C95A C96A 1.385(8) . ? C95A H95A 0.9300 . ? C96A H96A 0.9300 . ? Nb2B N91B 2.388(5) . ? Nb2B C14B 2.398(5) . ? Nb2B Cl7B 2.4168(14) . ? Nb2B Cl6B 2.4169(15) . ? Nb2B Cl8B 2.4263(14) . ? Nb2B Cl5B 2.4384(16) . ? Nb2B C13B 2.440(6) . ? Nb2B C15B 2.448(5) . ? Nb2B C12B 2.493(5) . ? Nb2B C11B 2.588(5) . ? C11B C15B 1.424(7) . ? C11B C12B 1.427(7) . ? C11B B1B 1.648(8) . ? C12B C13B 1.408(8) . ? C12B H12B 0.9300 . ? C13B C14B 1.390(8) . ? C13B H13B 0.9300 . ? C14B C15B 1.421(8) . ? C14B H14B 0.9300 . ? C15B H15B 0.9300 . ? B1B N21B 1.644(7) . ? B1B C41B 1.656(8) . ? B1B C31B 1.657(9) . ? N21B C26B 1.341(7) . ? N21B C22B 1.344(6) . ? C22B C23B 1.373(7) . ? C22B H22B 0.9300 . ? C23B C24B 1.385(9) . ? C23B H23B 0.9300 . ? C24B C25B 1.383(8) . ? C24B H24B 0.9300 . ? C25B C26B 1.356(8) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? C31B C36B 1.385(8) . ? C31B C32B 1.402(8) . ? C32B F32B 1.344(7) . ? C32B C33B 1.369(8) . ? C33B C34B 1.356(9) . ? C33B F33B 1.360(7) . ? C34B F34B 1.360(7) . ? C34B C35B 1.368(9) . ? C35B F35B 1.381(7) . ? C35B C36B 1.390(8) . ? C36B F36B 1.357(6) . ? C41B C46B 1.392(8) . ? C41B C42B 1.401(7) . ? C42B F42B 1.346(6) . ? C42B C43B 1.371(8) . ? C43B F43B 1.354(7) . ? C43B C44B 1.363(9) . ? C44B F44B 1.350(6) . ? C44B C45B 1.377(9) . ? C45B F45B 1.365(7) . ? C45B C46B 1.384(8) . ? C46B F46B 1.352(6) . ? N91B C92B 1.357(7) . ? N91B C96B 1.362(7) . ? C92B C93B 1.358(8) . ? C92B H92B 0.9300 . ? C93B C94B 1.390(8) . ? C93B H93B 0.9300 . ? C94B C95B 1.364(8) . ? C94B H94B 0.9300 . ? C95B C96B 1.372(8) . ? C95B H95B 0.9300 . ? C96B H96B 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 Cl7X Nb3X N91X 78.6(7) . . ? Cl7X Nb3X Cl8X 86.2(3) . . ? N91X Nb3X Cl8X 76.0(7) . . ? Cl7X Nb3X Cl6X 86.7(4) . . ? N91X Nb3X Cl6X 77.7(7) . . ? Cl8X Nb3X Cl6X 153.7(4) . . ? Cl7X Nb3X C14X 76.1(7) . . ? N91X Nb3X C14X 150.4(9) . . ? Cl8X Nb3X C14X 116.9(7) . . ? Cl6X Nb3X C14X 85.7(8) . . ? Cl7X Nb3X C13X 105.5(8) . . ? N91X Nb3X C13X 149.5(10) . . ? Cl8X Nb3X C13X 133.9(8) . . ? Cl6X Nb3X C13X 72.4(8) . . ? C14X Nb3X C13X 33.2(10) . . ? Cl7X Nb3X C12X 128.5(7) . . ? N91X Nb3X C12X 152.9(8) . . ? Cl8X Nb3X C12X 104.1(7) . . ? Cl6X Nb3X C12X 100.1(7) . . ? C14X Nb3X C12X 53.9(9) . . ? C13X Nb3X C12X 34.7(10) . . ? Cl7X Nb3X C15X 80.1(8) . . ? N91X Nb3X C15X 152.5(10) . . ? Cl8X Nb3X C15X 85.5(8) . . ? Cl6X Nb3X C15X 118.1(8) . . ? C14X Nb3X C15X 32.4(10) . . ? C13X Nb3X C15X 54.4(11) . . ? C12X Nb3X C15X 51.5(9) . . ? Cl7X Nb3X C11X 108.8(7) . . ? N91X Nb3X C11X 153.4(10) . . ? Cl8X Nb3X C11X 78.9(8) . . ? Cl6X Nb3X C11X 127.3(8) . . ? C14X Nb3X C11X 52.7(10) . . ? C13X Nb3X C11X 55.0(11) . . ? C12X Nb3X C11X 31.3(9) . . ? C15X Nb3X C11X 30.1(10) . . ? C15X C11X C12X 105(3) . . ? C15X C11X B1X 135(3) . . ? C12X C11X B1X 120(2) . . ? C15X C11X Nb3X 70(2) . . ? C12X C11X Nb3X 68.4(17) . . ? B1X C11X Nb3X 131(2) . . ? C11X C12X C13X 110(2) . . ? C11X C12X Nb3X 80.3(18) . . ? C13X C12X Nb3X 70.8(17) . . ? C14X C13X C12X 103(3) . . ? C14X C13X Nb3X 73.3(19) . . ? C12X C13X Nb3X 74.5(17) . . ? C15X C14X C13X 109(3) . . ? C15X C14X Nb3X 77(2) . . ? C13X C14X Nb3X 73.6(19) . . ? C11X C15X C14X 112(3) . . ? C11X C15X Nb3X 80(2) . . ? C14X C15X Nb3X 70.9(19) . . ? C11X B1X C41X 116(2) . . ? C11X B1X N21X 108(2) . . ? C41X B1X N21X 110(2) . . ? C11X B1X C31X 108(2) . . ? C41X B1X C31X 109(2) . . ? N21X B1X C31X 107(2) . . ? C22X N21X C26X 123(3) . . ? C22X N21X B1X 120(2) . . ? C26X N21X B1X 117(2) . . ? N21X C22X C23X 120(3) . . ? C22X C23X C24X 119(3) . . ? C25X C24X C23X 111(3) . . ? C26X C25X C24X 131(4) . . ? C25X C26X N21X 115(3) . . ? C32X C31X C36X 115(3) . . ? C32X C31X B1X 128(3) . . ? C36X C31X B1X 118(3) . . ? C31X C32X C33X 130(4) . . ? C31X C32X F32X 121(3) . . ? C33X C32X F32X 109(3) . . ? C32X C33X F33X 130(4) . . ? C32X C33X C34X 113(4) . . ? F33X C33X C34X 117(4) . . ? C35X C34X F34X 126(4) . . ? C35X C34X C33X 121(4) . . ? F34X C34X C33X 113(4) . . ? C34X C35X F35X 122(4) . . ? C34X C35X C36X 120(4) . . ? F35X C35X C36X 118(3) . . ? C31X C36X C35X 122(3) . . ? C31X C36X F36X 124(3) . . ? C35X C36X F36X 114(3) . . ? C42X C41X C46X 112(3) . . ? C42X C41X B1X 123(2) . . ? C46X C41X B1X 126(2) . . ? C43X C42X F42X 118(3) . . ? C43X C42X C41X 126(3) . . ? F42X C42X C41X 116(3) . . ? C42X C43X C44X 122(3) . . ? C42X C43X F43X 118(3) . . ? C44X C43X F43X 120(3) . . ? F44X C44X C45X 118(3) . . ? F44X C44X C43X 126(3) . . ? C45X C44X C43X 116(3) . . ? C44X C45X C46X 124(3) . . ? C44X C45X F45X 119(3) . . ? C46X C45X F45X 116(3) . . ? F46X C46X C45X 117(3) . . ? F46X C46X C41X 122(3) . . ? C45X C46X C41X 121(3) . . ? C92X N91X C96X 116(3) . . ? C92X N91X Nb3X 124(2) . . ? C96X N91X Nb3X 120(2) . . ? N91X C92X C93X 126(3) . . ? C94X C93X C92X 118(4) . . ? C93X C94X C95X 117(4) . . ? C94X C95X C96X 123(3) . . ? C95X C96X N91X 119(3) . . ? N91Y Nb4Y C14Y 150.7(10) . . ? N91Y Nb4Y Cl8Y 75.5(7) . . ? C14Y Nb4Y Cl8Y 118.4(8) . . ? N91Y Nb4Y C13Y 152.0(10) . . ? C14Y Nb4Y C13Y 31.0(10) . . ? Cl8Y Nb4Y C13Y 131.9(8) . . ? N91Y Nb4Y Cl7Y 79.0(6) . . ? C14Y Nb4Y Cl7Y 76.8(7) . . ? Cl8Y Nb4Y Cl7Y 85.5(3) . . ? C13Y Nb4Y Cl7Y 105.5(7) . . ? N91Y Nb4Y Cl6Y 77.6(7) . . ? C14Y Nb4Y Cl6Y 85.5(8) . . ? Cl8Y Nb4Y Cl6Y 153.1(4) . . ? C13Y Nb4Y Cl6Y 74.9(8) . . ? Cl7Y Nb4Y Cl6Y 88.6(3) . . ? N91Y Nb4Y C15Y 153.5(10) . . ? C14Y Nb4Y C15Y 33.5(12) . . ? Cl8Y Nb4Y C15Y 86.0(9) . . ? C13Y Nb4Y C15Y 51.6(12) . . ? Cl7Y Nb4Y C15Y 80.9(9) . . ? Cl6Y Nb4Y C15Y 119.0(9) . . ? N91Y Nb4Y C12Y 151.5(8) . . ? C14Y Nb4Y C12Y 54.4(9) . . ? Cl8Y Nb4Y C12Y 105.0(7) . . ? C13Y Nb4Y C12Y 33.3(10) . . ? Cl7Y Nb4Y C12Y 129.4(6) . . ? Cl6Y Nb4Y C12Y 98.9(7) . . ? C15Y Nb4Y C12Y 51.8(10) . . ? N91Y Nb4Y C11Y 152.6(10) . . ? C14Y Nb4Y C11Y 54.0(11) . . ? Cl8Y Nb4Y C11Y 79.1(8) . . ? C13Y Nb4Y C11Y 52.9(11) . . ? Cl7Y Nb4Y C11Y 109.4(7) . . ? Cl6Y Nb4Y C11Y 127.4(8) . . ? C15Y Nb4Y C11Y 30.1(11) . . ? C12Y Nb4Y C11Y 32.0(9) . . ? C15Y C11Y C12Y 107(3) . . ? C15Y C11Y B1Y 133(3) . . ? C12Y C11Y B1Y 118(3) . . ? C15Y C11Y Nb4Y 72(2) . . ? C12Y C11Y Nb4Y 71.3(18) . . ? B1Y C11Y Nb4Y 134(2) . . ? C11Y C12Y C13Y 105(2) . . ? C11Y C12Y Nb4Y 76.7(18) . . ? C13Y C12Y Nb4Y 70.0(17) . . ? C14Y C13Y C12Y 112(3) . . ? C14Y C13Y Nb4Y 73(2) . . ? C12Y C13Y Nb4Y 76.7(18) . . ? C13Y C14Y C15Y 105(3) . . ? C13Y C14Y Nb4Y 76(2) . . ? C15Y C14Y Nb4Y 77(2) . . ? C11Y C15Y C14Y 112(3) . . ? C11Y C15Y Nb4Y 78(2) . . ? C14Y C15Y Nb4Y 69(2) . . ? N21Y B1Y C11Y 109(2) . . ? N21Y B1Y C41Y 106(2) . . ? C11Y B1Y C41Y 114(3) . . ? N21Y B1Y C31Y 107(2) . . ? C11Y B1Y C31Y 111(2) . . ? C41Y B1Y C31Y 110(2) . . ? C22Y N21Y C26Y 117(3) . . ? C22Y N21Y B1Y 123(3) . . ? C26Y N21Y B1Y 120(2) . . ? N21Y C22Y C23Y 121(3) . . ? C22Y C23Y C24Y 121(3) . . ? C25Y C24Y C23Y 114(3) . . ? C24Y C25Y C26Y 128(4) . . ? C25Y C26Y N21Y 120(3) . . ? C32Y C31Y C36Y 116(3) . . ? C32Y C31Y B1Y 125(3) . . ? C36Y C31Y B1Y 118(3) . . ? C31Y C32Y C33Y 126(4) . . ? C31Y C32Y F32Y 122(3) . . ? C33Y C32Y F32Y 111(3) . . ? C34Y C33Y F33Y 120(4) . . ? C34Y C33Y C32Y 114(3) . . ? F33Y C33Y C32Y 126(3) . . ? C33Y C34Y F34Y 118(3) . . ? C33Y C34Y C35Y 131(4) . . ? F34Y C34Y C35Y 111(3) . . ? C36Y C35Y C34Y 102(3) . . ? C31Y C36Y F36Y 120(3) . . ? C31Y C36Y C35Y 130(3) . . ? F36Y C36Y C35Y 109(3) . . ? C46Y C41Y C42Y 110(3) . . ? C46Y C41Y B1Y 133(3) . . ? C42Y C41Y B1Y 117(3) . . ? F42Y C42Y C43Y 121(3) . . ? F42Y C42Y C41Y 115(3) . . ? C43Y C42Y C41Y 123(3) . . ? C42Y C43Y F43Y 121(4) . . ? C42Y C43Y C44Y 121(4) . . ? F43Y C43Y C44Y 117(4) . . ? F44Y C44Y C43Y 124(4) . . ? F44Y C44Y C45Y 118(4) . . ? C43Y C44Y C45Y 119(4) . . ? C46Y C45Y F45Y 119(3) . . ? C46Y C45Y C44Y 119(4) . . ? F45Y C45Y C44Y 121(3) . . ? C45Y C46Y C41Y 128(4) . . ? C45Y C46Y F46Y 116(4) . . ? C41Y C46Y F46Y 116(3) . . ? C92Y N91Y C96Y 114(3) . . ? C92Y N91Y Nb4Y 126(2) . . ? C96Y N91Y Nb4Y 121(2) . . ? N91Y C92Y C93Y 128(3) . . ? C92Y C93Y C94Y 120(3) . . ? C95Y C94Y C93Y 114(4) . . ? C94Y C95Y C96Y 121(4) . . ? N91Y C96Y C95Y 122(3) . . ? N91A Nb1A C14A 150.19(17) . . ? N91A Nb1A Cl5A 78.26(10) . . ? C14A Nb1A Cl5A 125.92(14) . . ? N91A Nb1A Cl6A 76.73(11) . . ? C14A Nb1A Cl6A 86.37(15) . . ? Cl5A Nb1A Cl6A 87.60(6) . . ? N91A Nb1A Cl8A 76.10(11) . . ? C14A Nb1A Cl8A 117.36(15) . . ? Cl5A Nb1A Cl8A 88.35(5) . . ? Cl6A Nb1A Cl8A 152.78(7) . . ? N91A Nb1A Cl7A 78.03(11) . . ? C14A Nb1A Cl7A 76.66(14) . . ? Cl5A Nb1A Cl7A 156.29(6) . . ? Cl6A Nb1A Cl7A 86.82(7) . . ? Cl8A Nb1A Cl7A 86.16(6) . . ? N91A Nb1A C13A 150.32(17) . . ? C14A Nb1A C13A 33.46(19) . . ? Cl5A Nb1A C13A 93.64(13) . . ? Cl6A Nb1A C13A 74.42(15) . . ? Cl8A Nb1A C13A 132.72(15) . . ? Cl7A Nb1A C13A 106.96(14) . . ? N91A Nb1A C15A 150.95(17) . . ? C14A Nb1A C15A 33.74(19) . . ? Cl5A Nb1A C15A 122.89(12) . . ? Cl6A Nb1A C15A 120.10(14) . . ? Cl8A Nb1A C15A 84.30(14) . . ? Cl7A Nb1A C15A 79.47(13) . . ? C13A Nb1A C15A 55.5(2) . . ? N91A Nb1A C12A 151.71(16) . . ? C14A Nb1A C12A 54.86(18) . . ? Cl5A Nb1A C12A 73.53(13) . . ? Cl6A Nb1A C12A 99.79(13) . . ? Cl8A Nb1A C12A 104.81(13) . . ? Cl7A Nb1A C12A 130.15(13) . . ? C13A Nb1A C12A 33.21(18) . . ? C15A Nb1A C12A 54.37(18) . . ? N91A Nb1A C11A 151.52(16) . . ? C14A Nb1A C11A 55.27(18) . . ? Cl5A Nb1A C11A 90.24(11) . . ? Cl6A Nb1A C11A 129.28(13) . . ? Cl8A Nb1A C11A 77.62(13) . . ? Cl7A Nb1A C11A 110.98(12) . . ? C13A Nb1A C11A 55.16(18) . . ? C15A Nb1A C11A 32.93(16) . . ? C12A Nb1A C11A 32.58(16) . . ? C12A C11A C15A 104.5(5) . . ? C12A C11A B1A 122.7(4) . . ? C15A C11A B1A 131.2(5) . . ? C12A C11A Nb1A 70.3(3) . . ? C15A C11A Nb1A 68.6(3) . . ? B1A C11A Nb1A 135.7(4) . . ? C13A C12A C11A 110.2(5) . . ? C13A C12A Nb1A 71.0(3) . . ? C11A C12A Nb1A 77.1(3) . . ? C13A C12A H12A 124.9 . . ? C11A C12A H12A 124.9 . . ? Nb1A C12A H12A 118.7 . . ? C14A C13A C12A 107.4(5) . . ? C14A C13A Nb1A 72.1(3) . . ? C12A C13A Nb1A 75.8(3) . . ? C14A C13A H13A 126.3 . . ? C12A C13A H13A 126.3 . . ? Nb1A C13A H13A 117.8 . . ? C13A C14A C15A 108.5(5) . . ? C13A C14A Nb1A 74.5(3) . . ? C15A C14A Nb1A 75.1(3) . . ? C13A C14A H14A 125.7 . . ? C15A C14A H14A 125.7 . . ? Nb1A C14A H14A 116.7 . . ? C14A C15A C11A 109.3(5) . . ? C14A C15A Nb1A 71.1(3) . . ? C11A C15A Nb1A 78.5(3) . . ? C14A C15A H15A 125.4 . . ? C11A C15A H15A 125.4 . . ? Nb1A C15A H15A 116.8 . . ? N21A B1A C41A 110.0(4) . . ? N21A B1A C11A 109.9(4) . . ? C41A B1A C11A 113.0(4) . . ? N21A B1A C31A 106.1(4) . . ? C41A B1A C31A 111.6(4) . . ? C11A B1A C31A 105.9(5) . . ? C26A N21A C22A 117.6(4) . . ? C26A N21A B1A 120.8(4) . . ? C22A N21A B1A 121.5(4) . . ? N21A C22A C23A 121.8(6) . . ? N21A C22A H22A 119.1 . . ? C23A C22A H22A 119.1 . . ? C22A C23A C24A 120.5(5) . . ? C22A C23A H23A 119.8 . . ? C24A C23A H23A 119.8 . . ? C23A C24A C25A 118.4(6) . . ? C23A C24A H24A 120.8 . . ? C25A C24A H24A 120.8 . . ? C26A C25A C24A 119.4(6) . . ? C26A C25A H25A 120.3 . . ? C24A C25A H25A 120.3 . . ? N21A C26A C25A 122.3(5) . . ? N21A C26A H26A 118.8 . . ? C25A C26A H26A 118.8 . . ? C36A C31A C32A 112.6(6) . . ? C36A C31A B1A 123.4(5) . . ? C32A C31A B1A 123.9(5) . . ? F32A C32A C33A 116.4(5) . . ? F32A C32A C31A 120.5(5) . . ? C33A C32A C31A 123.1(6) . . ? F33A C33A C34A 120.1(6) . . ? F33A C33A C32A 119.6(6) . . ? C34A C33A C32A 120.2(6) . . ? C33A C34A F34A 119.6(6) . . ? C33A C34A C35A 120.7(6) . . ? F34A C34A C35A 119.6(6) . . ? F35A C35A C36A 130.2(6) . . ? F35A C35A C34A 112.8(6) . . ? C36A C35A C34A 117.0(6) . . ? F36A C36A C35A 114.4(6) . . ? F36A C36A C31A 119.4(5) . . ? C35A C36A C31A 126.2(6) . . ? C46A C41A C42A 111.8(5) . . ? C46A C41A B1A 127.8(5) . . ? C42A C41A B1A 120.3(5) . . ? C43A C42A F42A 115.5(5) . . ? C43A C42A C41A 125.7(5) . . ? F42A C42A C41A 118.8(5) . . ? F43A C43A C42A 121.1(5) . . ? F43A C43A C44A 119.6(5) . . ? C42A C43A C44A 119.2(5) . . ? F44A C44A C45A 120.0(6) . . ? F44A C44A C43A 121.4(5) . . ? C45A C44A C43A 118.5(5) . . ? C44A C45A F45A 119.7(6) . . ? C44A C45A C46A 119.8(6) . . ? F45A C45A C46A 120.4(5) . . ? F46A C46A C45A 114.2(5) . . ? F46A C46A C41A 120.9(5) . . ? C45A C46A C41A 124.9(5) . . ? C92A N91A C96A 116.0(5) . . ? C92A N91A Nb1A 122.6(4) . . ? C96A N91A Nb1A 121.4(4) . . ? N91A C92A C93A 123.3(5) . . ? N91A C92A H92A 118.3 . . ? C93A C92A H92A 118.3 . . ? C92A C93A C94A 120.1(6) . . ? C92A C93A H93A 120.0 . . ? C94A C93A H93A 120.0 . . ? C95A C94A C93A 117.7(6) . . ? C95A C94A H94A 121.1 . . ? C93A C94A H94A 121.1 . . ? C94A C95A C96A 120.4(6) . . ? C94A C95A H95A 119.8 . . ? C96A C95A H95A 119.8 . . ? N91A C96A C95A 122.4(5) . . ? N91A C96A H96A 118.8 . . ? C95A C96A H96A 118.8 . . ? N91B Nb2B C14B 150.26(17) . . ? N91B Nb2B Cl7B 78.66(11) . . ? C14B Nb2B Cl7B 76.39(14) . . ? N91B Nb2B Cl6B 76.61(12) . . ? C14B Nb2B Cl6B 86.63(14) . . ? Cl7B Nb2B Cl6B 88.18(5) . . ? N91B Nb2B Cl8B 76.19(12) . . ? C14B Nb2B Cl8B 117.56(14) . . ? Cl7B Nb2B Cl8B 85.98(5) . . ? Cl6B Nb2B Cl8B 152.80(6) . . ? N91B Nb2B Cl5B 78.03(11) . . ? C14B Nb2B Cl5B 125.98(13) . . ? Cl7B Nb2B Cl5B 156.69(6) . . ? Cl6B Nb2B Cl5B 86.94(6) . . ? Cl8B Nb2B Cl5B 88.01(5) . . ? N91B Nb2B C13B 150.28(17) . . ? C14B Nb2B C13B 33.39(18) . . ? Cl7B Nb2B C13B 106.86(14) . . ? Cl6B Nb2B C13B 74.45(14) . . ? Cl8B Nb2B C13B 132.58(14) . . ? Cl5B Nb2B C13B 93.74(14) . . ? N91B Nb2B C15B 151.50(18) . . ? C14B Nb2B C15B 34.08(19) . . ? Cl7B Nb2B C15B 79.49(14) . . ? Cl6B Nb2B C15B 120.70(15) . . ? Cl8B Nb2B C15B 84.25(14) . . ? Cl5B Nb2B C15B 122.27(13) . . ? C13B Nb2B C15B 55.3(2) . . ? N91B Nb2B C12B 151.45(16) . . ? C14B Nb2B C12B 54.93(18) . . ? Cl7B Nb2B C12B 129.80(13) . . ? Cl6B Nb2B C12B 99.42(13) . . ? Cl8B Nb2B C12B 104.71(13) . . ? Cl5B Nb2B C12B 73.51(13) . . ? C13B Nb2B C12B 33.16(18) . . ? C15B Nb2B C12B 53.93(18) . . ? N91B Nb2B C11B 151.22(16) . . ? C14B Nb2B C11B 55.73(18) . . ? Cl7B Nb2B C11B 110.70(11) . . ? Cl6B Nb2B C11B 129.25(12) . . ? Cl8B Nb2B C11B 77.41(12) . . ? Cl5B Nb2B C11B 89.84(11) . . ? C13B Nb2B C11B 55.24(18) . . ? C15B Nb2B C11B 32.71(17) . . ? C12B Nb2B C11B 32.55(16) . . ? C15B C11B C12B 103.6(5) . . ? C15B C11B B1B 131.9(5) . . ? C12B C11B B1B 122.9(4) . . ? C15B C11B Nb2B 68.2(3) . . ? C12B C11B Nb2B 70.0(3) . . ? B1B C11B Nb2B 135.8(4) . . ? C13B C12B C11B 110.9(5) . . ? C13B C12B Nb2B 71.4(3) . . ? C11B C12B Nb2B 77.4(3) . . ? C13B C12B H12B 124.6 . . ? C11B C12B H12B 124.6 . . ? Nb2B C12B H12B 118.3 . . ? C14B C13B C12B 107.5(5) . . ? C14B C13B Nb2B 71.7(3) . . ? C12B C13B Nb2B 75.5(3) . . ? C14B C13B H13B 126.2 . . ? C12B C13B H13B 126.2 . . ? Nb2B C13B H13B 118.6 . . ? C13B C14B C15B 107.4(5) . . ? C13B C14B Nb2B 74.9(3) . . ? C15B C14B Nb2B 74.9(3) . . ? C13B C14B H14B 126.3 . . ? C15B C14B H14B 126.3 . . ? Nb2B C14B H14B 116.1 . . ? C14B C15B C11B 110.4(5) . . ? C14B C15B Nb2B 71.1(3) . . ? C11B C15B Nb2B 79.1(3) . . ? C14B C15B H15B 124.8 . . ? C11B C15B H15B 124.8 . . ? Nb2B C15B H15B 116.8 . . ? N21B B1B C11B 109.6(4) . . ? N21B B1B C41B 110.0(4) . . ? C11B B1B C41B 112.6(4) . . ? N21B B1B C31B 105.8(4) . . ? C11B B1B C31B 107.1(4) . . ? C41B B1B C31B 111.3(4) . . ? C26B N21B C22B 119.0(4) . . ? C26B N21B B1B 120.0(4) . . ? C22B N21B B1B 121.0(4) . . ? N21B C22B C23B 121.6(5) . . ? N21B C22B H22B 119.2 . . ? C23B C22B H22B 119.2 . . ? C22B C23B C24B 119.4(5) . . ? C22B C23B H23B 120.3 . . ? C24B C23B H23B 120.3 . . ? C25B C24B C23B 118.1(5) . . ? C25B C24B H24B 121.0 . . ? C23B C24B H24B 121.0 . . ? C26B C25B C24B 120.0(6) . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? N21B C26B C25B 121.9(5) . . ? N21B C26B H26B 119.0 . . ? C25B C26B H26B 119.0 . . ? C36B C31B C32B 113.1(6) . . ? C36B C31B B1B 123.5(5) . . ? C32B C31B B1B 123.0(5) . . ? F32B C32B C33B 115.2(5) . . ? F32B C32B C31B 120.8(5) . . ? C33B C32B C31B 124.0(6) . . ? C34B C33B F33B 119.5(5) . . ? C34B C33B C32B 120.0(6) . . ? F33B C33B C32B 120.4(6) . . ? C33B C34B F34B 120.0(6) . . ? C33B C34B C35B 119.7(6) . . ? F34B C34B C35B 120.2(6) . . ? C34B C35B F35B 117.2(5) . . ? C34B C35B C36B 119.1(6) . . ? F35B C35B C36B 123.7(6) . . ? F36B C36B C31B 120.4(5) . . ? F36B C36B C35B 115.6(5) . . ? C31B C36B C35B 124.1(6) . . ? C46B C41B C42B 112.9(5) . . ? C46B C41B B1B 127.2(5) . . ? C42B C41B B1B 119.8(5) . . ? F42B C42B C43B 116.7(5) . . ? F42B C42B C41B 118.8(5) . . ? C43B C42B C41B 124.5(6) . . ? F43B C43B C44B 120.0(5) . . ? F43B C43B C42B 120.0(6) . . ? C44B C43B C42B 120.1(6) . . ? F44B C44B C43B 121.7(6) . . ? F44B C44B C45B 119.7(6) . . ? C43B C44B C45B 118.6(5) . . ? F45B C45B C44B 119.2(6) . . ? F45B C45B C46B 120.7(6) . . ? C44B C45B C46B 120.1(6) . . ? F46B C46B C45B 114.0(5) . . ? F46B C46B C41B 122.2(5) . . ? C45B C46B C41B 123.8(6) . . ? C92B N91B C96B 114.4(5) . . ? C92B N91B Nb2B 123.3(4) . . ? C96B N91B Nb2B 122.2(4) . . ? N91B C92B C93B 124.4(5) . . ? N91B C92B H92B 117.8 . . ? C93B C92B H92B 117.8 . . ? C92B C93B C94B 119.7(5) . . ? C92B C93B H93B 120.1 . . ? C94B C93B H93B 120.1 . . ? C95B C94B C93B 117.4(6) . . ? C95B C94B H94B 121.3 . . ? C93B C94B H94B 121.3 . . ? C94B C95B C96B 120.0(6) . . ? C94B C95B H95B 120.0 . . ? C96B C95B H95B 120.0 . . ? N91B C96B C95B 124.0(6) . . ? N91B C96B H96B 118.0 . . ? C95B C96B H96B 118.0 . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.659 _refine_diff_density_min -2.094 _refine_diff_density_rms 0.126 data_simonl7 _database_code_CSD 205215 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 9a, ref. 27' _chemical_melting_point ? _chemical_formula_moiety 'C25 H17 B Cl3 F10 Nb Si, C7 H8' _chemical_formula_structural '[Nb Cl2 (C5H4SiMe3) {C5H4B(Cl)(C6F5)2}].tol' _chemical_formula_sum 'C32 H25 B Cl3 F10 Nb Si' _chemical_formula_weight 837.68 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.801(1) _cell_length_b 15.892(1) _cell_length_c 15.892(1) _cell_angle_alpha 90.00 _cell_angle_beta 110.45(1) _cell_angle_gamma 90.00 _cell_volume 3265.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelipiped _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18703 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.43 _reflns_number_total 5959 _reflns_number_gt 5347 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _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^)+(0.0600P)^2^+0.264P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5959 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Nb Nb 0.072468(13) 0.214675(11) 0.131154(12) 0.02321(8) Uani 1 1 d . . . B B -0.17716(17) 0.09673(14) 0.07089(15) 0.0245(5) Uani 1 1 d . . . C11 C -0.10572(14) 0.16509(13) 0.04223(13) 0.0240(4) Uani 1 1 d . . . C12 C -0.10851(15) 0.25479(13) 0.04792(14) 0.0275(4) Uani 1 1 d . . . H12 H -0.1455 0.2848 0.0769 0.033 Uiso 1 1 calc R . . C13 C -0.04682(17) 0.29087(14) 0.00296(15) 0.0333(5) Uani 1 1 d . . . H13 H -0.0388 0.3481 -0.0049 0.040 Uiso 1 1 calc R . . C14 C 0.00055(17) 0.22487(15) -0.02795(15) 0.0335(5) Uani 1 1 d . . . H14 H 0.0469 0.2305 -0.0583 0.040 Uiso 1 1 calc R . . C15 C -0.03604(16) 0.14780(14) -0.00382(13) 0.0285(4) Uani 1 1 d . . . H15 H -0.0172 0.0943 -0.0163 0.034 Uiso 1 1 calc R . . Cl2 Cl -0.09084(4) -0.00041(3) 0.11639(3) 0.03005(13) Uani 1 1 d . . . C31 C -0.27226(15) 0.05898(12) -0.01633(13) 0.0246(4) Uani 1 1 d . . . C32 C -0.33908(16) -0.00051(12) -0.00107(13) 0.0261(4) Uani 1 1 d . . . F32 F -0.32625(10) -0.02440(8) 0.08415(8) 0.0339(3) Uani 1 1 d . . . C33 C -0.41955(16) -0.03822(13) -0.06775(15) 0.0299(4) Uani 1 1 d . . . F33 F -0.47990(10) -0.09582(8) -0.04695(9) 0.0394(3) Uani 1 1 d . . . C34 C -0.43842(16) -0.01677(14) -0.15621(14) 0.0308(5) Uani 1 1 d . . . F34 F -0.51758(10) -0.05212(9) -0.22230(9) 0.0431(3) Uani 1 1 d . . . C35 C -0.37641(16) 0.04230(14) -0.17555(14) 0.0299(4) Uani 1 1 d . . . F35 F -0.39531(11) 0.06489(9) -0.26170(8) 0.0433(3) Uani 1 1 d . . . C36 C -0.29562(15) 0.07846(12) -0.10670(14) 0.0260(4) Uani 1 1 d . . . F36 F -0.23809(10) 0.13564(8) -0.13233(8) 0.0351(3) Uani 1 1 d . . . C41 C -0.22964(15) 0.13597(13) 0.14047(13) 0.0248(4) Uani 1 1 d . . . C42 C -0.30776(16) 0.19511(13) 0.10786(14) 0.0265(4) Uani 1 1 d . . . F42 F -0.33489(10) 0.22153(7) 0.02104(8) 0.0324(3) Uani 1 1 d . . . C43 C -0.36348(17) 0.23010(14) 0.15675(16) 0.0317(5) Uani 1 1 d . . . F43 F -0.44166(11) 0.28460(8) 0.11839(10) 0.0435(4) Uani 1 1 d . . . C44 C -0.34092(18) 0.20628(14) 0.24518(16) 0.0345(5) Uani 1 1 d . . . F44 F -0.39517(12) 0.23786(10) 0.29349(10) 0.0489(4) Uani 1 1 d . . . C45 C -0.26400(17) 0.14835(15) 0.28155(14) 0.0342(5) Uani 1 1 d . . . F45 F -0.24189(12) 0.12350(10) 0.36752(9) 0.0477(4) Uani 1 1 d . . . C46 C -0.21082(16) 0.11401(13) 0.23004(14) 0.0293(4) Uani 1 1 d . . . F46 F -0.13911(10) 0.05586(9) 0.27184(8) 0.0403(3) Uani 1 1 d . . . Cl5 Cl 0.01041(4) 0.20534(4) 0.25086(4) 0.03385(14) Uani 1 1 d . . . Cl6 Cl 0.13274(4) 0.35460(3) 0.15616(4) 0.03770(14) Uani 1 1 d . . . C71 C 0.25281(15) 0.18565(13) 0.22929(14) 0.0259(4) Uani 1 1 d . . . C72 C 0.19280(15) 0.11257(13) 0.22823(15) 0.0292(4) Uani 1 1 d . . . H72 H 0.1818 0.0897 0.2780 0.035 Uiso 1 1 calc R . . C73 C 0.15269(16) 0.08019(13) 0.14071(15) 0.0324(5) Uani 1 1 d . . . H73 H 0.1090 0.0340 0.1223 0.039 Uiso 1 1 calc R . . C74 C 0.19084(16) 0.13077(14) 0.08511(15) 0.0323(5) Uani 1 1 d . . . H74 H 0.1784 0.1226 0.0243 0.039 Uiso 1 1 calc R . . C75 C 0.25068(15) 0.19528(14) 0.13895(14) 0.0279(4) Uani 1 1 d . . . H75 H 0.2838 0.2377 0.1191 0.033 Uiso 1 1 calc R . . Si7 Si 0.33943(4) 0.24173(4) 0.33384(4) 0.02798(14) Uani 1 1 d . . . C76 C 0.26390(19) 0.26943(16) 0.40703(16) 0.0377(5) Uani 1 1 d . . . H76A H 0.2347 0.2193 0.4220 0.057 Uiso 1 1 calc R . . H76B H 0.2094 0.3076 0.3757 0.057 Uiso 1 1 calc R . . H76C H 0.3088 0.2956 0.4610 0.057 Uiso 1 1 calc R . . C77 C 0.39844(18) 0.33602(14) 0.30149(16) 0.0365(5) Uani 1 1 d . . . H77A H 0.4366 0.3191 0.2641 0.055 Uiso 1 1 calc R . . H77B H 0.4443 0.3629 0.3546 0.055 Uiso 1 1 calc R . . H77C H 0.3449 0.3746 0.2691 0.055 Uiso 1 1 calc R . . C78 C 0.43961(18) 0.16093(16) 0.38907(16) 0.0396(5) Uani 1 1 d . . . H78A H 0.4073 0.1130 0.4050 0.059 Uiso 1 1 calc R . . H78B H 0.4896 0.1844 0.4422 0.059 Uiso 1 1 calc R . . H78C H 0.4735 0.1438 0.3484 0.059 Uiso 1 1 calc R . . C81 C 0.27478(19) 0.49674(16) -0.01967(16) 0.0400(5) Uani 1 1 d . . . C82 C 0.29405(19) 0.55061(15) -0.08030(17) 0.0397(5) Uani 1 1 d . . . H82 H 0.3617 0.5669 -0.0713 0.048 Uiso 1 1 calc R . . C83 C 0.2139(2) 0.58081(15) -0.15447(18) 0.0454(6) Uani 1 1 d . . . H83 H 0.2279 0.6165 -0.1951 0.054 Uiso 1 1 calc R . . C84 C 0.1123(2) 0.55721(18) -0.16753(18) 0.0521(7) Uani 1 1 d . . . H84 H 0.0581 0.5776 -0.2167 0.062 Uiso 1 1 calc R . . C85 C 0.0926(2) 0.50388(18) -0.1076(2) 0.0536(7) Uani 1 1 d . . . H85 H 0.0250 0.4881 -0.1161 0.064 Uiso 1 1 calc R . . C86 C 0.1730(2) 0.47338(17) -0.03455(19) 0.0483(6) Uani 1 1 d . . . H86 H 0.1587 0.4367 0.0052 0.058 Uiso 1 1 calc R . . C87 C 0.3616(2) 0.4645(2) 0.06165(18) 0.0588(8) Uani 1 1 d . . . H87A H 0.3694 0.4050 0.0558 0.088 Uiso 1 1 calc R . . H87B H 0.3457 0.4755 0.1148 0.088 Uiso 1 1 calc R . . H87C H 0.4248 0.4925 0.0660 0.088 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 Nb 0.02026(12) 0.02502(13) 0.02469(12) -0.00262(6) 0.00828(8) -0.00093(6) B 0.0222(11) 0.0251(11) 0.0240(11) -0.0002(9) 0.0054(9) 0.0019(8) C11 0.0182(9) 0.0305(10) 0.0202(9) -0.0032(8) 0.0027(8) -0.0003(7) C12 0.0214(10) 0.0298(11) 0.0283(11) -0.0001(8) 0.0047(8) 0.0018(8) C13 0.0276(11) 0.0342(12) 0.0318(12) 0.0095(9) 0.0026(9) -0.0007(8) C14 0.0263(11) 0.0504(14) 0.0239(11) 0.0038(9) 0.0089(9) -0.0042(9) C15 0.0238(10) 0.0369(11) 0.0222(10) -0.0062(8) 0.0047(8) -0.0021(8) Cl2 0.0254(3) 0.0289(3) 0.0326(3) 0.0008(2) 0.0061(2) 0.00329(19) C31 0.0218(10) 0.0253(10) 0.0265(10) -0.0024(8) 0.0082(8) 0.0015(7) C32 0.0244(10) 0.0287(10) 0.0248(10) -0.0002(8) 0.0081(8) 0.0008(8) F32 0.0343(7) 0.0372(7) 0.0283(6) 0.0032(5) 0.0087(5) -0.0084(5) C33 0.0252(10) 0.0280(11) 0.0367(12) -0.0011(9) 0.0110(9) -0.0026(8) F33 0.0330(7) 0.0398(7) 0.0432(8) -0.0016(6) 0.0107(6) -0.0139(5) C34 0.0232(10) 0.0327(11) 0.0318(11) -0.0079(9) 0.0036(9) -0.0005(8) F34 0.0324(7) 0.0529(8) 0.0353(7) -0.0121(6) 0.0009(6) -0.0125(6) C35 0.0278(11) 0.0363(12) 0.0236(10) -0.0010(8) 0.0065(8) 0.0024(8) F35 0.0418(8) 0.0608(9) 0.0230(6) -0.0003(6) 0.0059(6) -0.0095(6) C36 0.0239(10) 0.0262(10) 0.0285(10) -0.0003(8) 0.0098(8) 0.0010(8) F36 0.0317(7) 0.0445(7) 0.0273(6) 0.0035(5) 0.0081(5) -0.0097(5) C41 0.0219(10) 0.0273(10) 0.0243(10) -0.0017(8) 0.0069(8) -0.0037(7) C42 0.0253(10) 0.0292(10) 0.0252(10) -0.0028(8) 0.0090(8) -0.0043(8) F42 0.0318(7) 0.0372(7) 0.0265(6) 0.0030(5) 0.0080(5) 0.0082(5) C43 0.0249(11) 0.0339(11) 0.0370(12) -0.0046(9) 0.0115(9) -0.0004(8) F43 0.0372(8) 0.0432(9) 0.0529(9) -0.0025(6) 0.0194(7) 0.0121(6) C44 0.0317(12) 0.0402(13) 0.0384(13) -0.0114(9) 0.0209(10) -0.0087(9) F44 0.0493(9) 0.0603(9) 0.0511(9) -0.0142(7) 0.0351(7) -0.0044(7) C45 0.0318(12) 0.0468(13) 0.0251(11) -0.0030(9) 0.0112(9) -0.0125(9) F45 0.0528(9) 0.0675(10) 0.0269(7) 0.0019(6) 0.0191(6) -0.0088(7) C46 0.0230(10) 0.0351(11) 0.0270(11) 0.0004(9) 0.0053(8) -0.0032(8) F46 0.0365(7) 0.0498(8) 0.0309(7) 0.0104(6) 0.0072(6) 0.0074(6) Cl5 0.0253(3) 0.0511(3) 0.0267(3) -0.0059(2) 0.0110(2) -0.0043(2) Cl6 0.0299(3) 0.0264(3) 0.0524(3) -0.0032(2) 0.0089(2) -0.0031(2) C71 0.0201(10) 0.0280(10) 0.0295(11) -0.0007(8) 0.0086(8) 0.0032(8) C72 0.0236(10) 0.0248(10) 0.0367(12) 0.0036(9) 0.0075(9) 0.0027(8) C73 0.0232(10) 0.0254(11) 0.0437(13) -0.0074(9) 0.0057(9) 0.0032(8) C74 0.0231(10) 0.0415(12) 0.0320(11) -0.0105(9) 0.0091(9) 0.0050(9) C75 0.0183(10) 0.0368(11) 0.0313(11) -0.0027(9) 0.0120(8) 0.0015(8) Si7 0.0245(3) 0.0339(3) 0.0258(3) -0.0046(2) 0.0092(2) -0.0046(2) C76 0.0375(13) 0.0455(13) 0.0336(12) -0.0091(10) 0.0166(10) -0.0082(10) C77 0.0333(12) 0.0390(13) 0.0390(13) -0.0079(10) 0.0148(10) -0.0071(9) C78 0.0318(12) 0.0476(14) 0.0350(12) 0.0003(10) 0.0062(10) -0.0037(10) C81 0.0367(13) 0.0463(14) 0.0353(12) -0.0089(10) 0.0103(10) 0.0015(10) C82 0.0344(12) 0.0406(13) 0.0449(14) -0.0117(11) 0.0149(11) -0.0057(10) C83 0.0621(17) 0.0329(13) 0.0417(14) -0.0041(10) 0.0189(12) 0.0077(11) C84 0.0462(15) 0.0503(15) 0.0447(15) -0.0207(12) -0.0029(12) 0.0152(12) C85 0.0316(14) 0.0565(17) 0.0693(19) -0.0228(15) 0.0134(13) -0.0052(12) C86 0.0469(15) 0.0487(15) 0.0544(16) -0.0060(12) 0.0240(13) -0.0077(12) C87 0.0552(18) 0.071(2) 0.0415(15) -0.0006(14) 0.0061(13) 0.0088(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 Nb Cl5 2.3479(6) . ? Nb Cl6 2.3588(5) . ? Nb C14 2.377(2) . ? Nb C73 2.387(2) . ? Nb C15 2.393(2) . ? Nb C74 2.412(2) . ? Nb C75 2.4386(19) . ? Nb C72 2.445(2) . ? Nb C13 2.446(2) . ? Nb C12 2.467(2) . ? Nb C71 2.4753(19) . ? Nb C11 2.4974(19) . ? B C11 1.635(3) . ? B C41 1.642(3) . ? B C31 1.653(3) . ? B Cl2 1.930(2) . ? C11 C15 1.424(3) . ? C11 C12 1.430(3) . ? C12 C13 1.410(3) . ? C12 H12 0.9300 . ? C13 C14 1.412(3) . ? C13 H13 0.9300 . ? C14 C15 1.427(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C31 C36 1.392(3) . ? C31 C32 1.400(3) . ? C32 F32 1.357(2) . ? C32 C33 1.376(3) . ? C33 F33 1.354(2) . ? C33 C34 1.380(3) . ? C34 F34 1.345(2) . ? C34 C35 1.376(3) . ? C35 F35 1.350(2) . ? C35 C36 1.385(3) . ? C36 F36 1.359(2) . ? C41 C42 1.387(3) . ? C41 C46 1.399(3) . ? C42 F42 1.364(2) . ? C42 C43 1.386(3) . ? C43 F43 1.351(3) . ? C43 C44 1.382(3) . ? C44 F44 1.343(3) . ? C44 C45 1.371(3) . ? C45 F45 1.351(3) . ? C45 C46 1.388(3) . ? C46 F46 1.347(2) . ? C71 C72 1.423(3) . ? C71 C75 1.434(3) . ? C71 Si7 1.896(2) . ? C72 C73 1.403(3) . ? C72 H72 0.9300 . ? C73 C74 1.424(3) . ? C73 H73 0.9300 . ? C74 C75 1.404(3) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? Si7 C77 1.862(2) . ? Si7 C76 1.866(2) . ? Si7 C78 1.866(2) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C81 C82 1.382(4) . ? C81 C86 1.391(4) . ? C81 C87 1.512(3) . ? C82 C83 1.390(4) . ? C82 H82 0.9300 . ? C83 C84 1.395(4) . ? C83 H83 0.9300 . ? C84 C85 1.371(4) . ? C84 H84 0.9300 . ? C85 C86 1.383(4) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? 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 Nb Cl6 97.47(2) . . ? Cl5 Nb C14 136.98(6) . . ? Cl6 Nb C14 96.12(6) . . ? Cl5 Nb C73 100.62(6) . . ? Cl6 Nb C73 134.82(5) . . ? C14 Nb C73 98.09(8) . . ? Cl5 Nb C15 114.01(5) . . ? Cl6 Nb C15 130.02(6) . . ? C14 Nb C15 34.82(7) . . ? C73 Nb C15 77.91(7) . . ? Cl5 Nb C74 133.50(6) . . ? Cl6 Nb C74 109.63(6) . . ? C14 Nb C74 77.90(8) . . ? C73 Nb C74 34.53(8) . . ? C15 Nb C74 76.15(7) . . ? Cl5 Nb C75 126.71(5) . . ? Cl6 Nb C75 79.66(5) . . ? C14 Nb C75 95.83(8) . . ? C73 Nb C75 56.39(7) . . ? C15 Nb C75 107.07(7) . . ? C74 Nb C75 33.65(7) . . ? Cl5 Nb C72 78.84(6) . . ? Cl6 Nb C72 113.42(5) . . ? C14 Nb C72 130.95(8) . . ? C73 Nb C72 33.72(7) . . ? C15 Nb C72 110.19(7) . . ? C74 Nb C72 56.08(8) . . ? C75 Nb C72 55.50(7) . . ? Cl5 Nb C13 112.10(6) . . ? Cl6 Nb C13 76.63(5) . . ? C14 Nb C13 34.00(8) . . ? C73 Nb C13 131.18(8) . . ? C15 Nb C13 56.30(8) . . ? C74 Nb C13 110.55(8) . . ? C75 Nb C13 118.57(8) . . ? C72 Nb C13 164.79(8) . . ? Cl5 Nb C12 82.14(5) . . ? Cl6 Nb C12 94.48(5) . . ? C14 Nb C12 56.21(8) . . ? C73 Nb C12 128.73(7) . . ? C15 Nb C12 55.60(7) . . ? C74 Nb C12 130.27(7) . . ? C75 Nb C12 150.94(7) . . ? C72 Nb C12 147.87(7) . . ? C13 Nb C12 33.36(7) . . ? Cl5 Nb C71 92.80(5) . . ? Cl6 Nb C71 81.48(5) . . ? C14 Nb C71 129.58(7) . . ? C73 Nb C71 56.71(7) . . ? C15 Nb C71 131.18(7) . . ? C74 Nb C71 56.61(7) . . ? C75 Nb C71 33.92(7) . . ? C72 Nb C71 33.61(7) . . ? C13 Nb C71 148.54(7) . . ? C12 Nb C71 173.09(7) . . ? Cl5 Nb C11 82.69(5) . . ? Cl6 Nb C11 127.76(5) . . ? C14 Nb C11 57.11(7) . . ? C73 Nb C11 95.55(7) . . ? C15 Nb C11 33.77(7) . . ? C74 Nb C11 106.94(7) . . ? C75 Nb C11 139.92(7) . . ? C72 Nb C11 117.71(7) . . ? C13 Nb C11 56.07(7) . . ? C12 Nb C11 33.47(7) . . ? C71 Nb C11 150.72(7) . . ? C11 B C41 112.71(16) . . ? C11 B C31 112.76(16) . . ? C41 B C31 107.14(16) . . ? C11 B Cl2 106.42(14) . . ? C41 B Cl2 114.29(14) . . ? C31 B Cl2 103.25(13) . . ? C15 C11 C12 105.24(18) . . ? C15 C11 B 126.59(18) . . ? C12 C11 B 127.79(18) . . ? C15 C11 Nb 69.11(11) . . ? C12 C11 Nb 72.09(10) . . ? B C11 Nb 128.49(13) . . ? C13 C12 C11 109.82(19) . . ? C13 C12 Nb 72.51(12) . . ? C11 C12 Nb 74.44(11) . . ? C13 C12 H12 125.1 . . ? C11 C12 H12 125.1 . . ? Nb C12 H12 119.7 . . ? C12 C13 C14 108.00(19) . . ? C12 C13 Nb 74.13(12) . . ? C14 C13 Nb 70.33(12) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Nb C13 H13 121.3 . . ? C13 C14 C15 107.1(2) . . ? C13 C14 Nb 75.67(13) . . ? C15 C14 Nb 73.22(12) . . ? C13 C14 H14 126.5 . . ? C15 C14 H14 126.5 . . ? Nb C14 H14 116.8 . . ? C11 C15 C14 109.77(19) . . ? C11 C15 Nb 77.12(11) . . ? C14 C15 Nb 71.97(12) . . ? C11 C15 H15 125.1 . . ? C14 C15 H15 125.1 . . ? Nb C15 H15 117.6 . . ? C36 C31 C32 113.56(18) . . ? C36 C31 B 127.89(18) . . ? C32 C31 B 118.55(18) . . ? F32 C32 C33 115.81(18) . . ? F32 C32 C31 119.85(17) . . ? C33 C32 C31 124.34(19) . . ? F33 C33 C32 120.42(19) . . ? F33 C33 C34 120.16(18) . . ? C32 C33 C34 119.42(19) . . ? F34 C34 C35 120.6(2) . . ? F34 C34 C33 120.3(2) . . ? C35 C34 C33 119.04(19) . . ? F35 C35 C34 119.56(18) . . ? F35 C35 C36 120.53(19) . . ? C34 C35 C36 119.92(19) . . ? F36 C36 C35 115.72(18) . . ? F36 C36 C31 120.57(17) . . ? C35 C36 C31 123.71(19) . . ? C42 C41 C46 113.13(19) . . ? C42 C41 B 118.29(17) . . ? C46 C41 B 128.44(18) . . ? F42 C42 C43 115.71(19) . . ? F42 C42 C41 119.30(18) . . ? C43 C42 C41 125.0(2) . . ? F43 C43 C44 119.7(2) . . ? F43 C43 C42 121.1(2) . . ? C44 C43 C42 119.2(2) . . ? F44 C44 C45 120.9(2) . . ? F44 C44 C43 120.4(2) . . ? C45 C44 C43 118.6(2) . . ? F45 C45 C44 119.4(2) . . ? F45 C45 C46 120.2(2) . . ? C44 C45 C46 120.4(2) . . ? F46 C46 C45 115.31(19) . . ? F46 C46 C41 121.06(19) . . ? C45 C46 C41 123.6(2) . . ? C72 C71 C75 105.49(18) . . ? C72 C71 Si7 125.46(16) . . ? C75 C71 Si7 127.82(16) . . ? C72 C71 Nb 72.05(11) . . ? C75 C71 Nb 71.64(11) . . ? Si7 C71 Nb 130.67(10) . . ? C73 C72 C71 109.73(19) . . ? C73 C72 Nb 70.86(11) . . ? C71 C72 Nb 74.34(11) . . ? C73 C72 H72 125.1 . . ? C71 C72 H72 125.1 . . ? Nb C72 H72 121.3 . . ? C72 C73 C74 107.74(19) . . ? C72 C73 Nb 75.42(11) . . ? C74 C73 Nb 73.69(12) . . ? C72 C73 H73 126.1 . . ? C74 C73 H73 126.1 . . ? Nb C73 H73 116.9 . . ? C75 C74 C73 107.46(19) . . ? C75 C74 Nb 74.21(12) . . ? C73 C74 Nb 71.79(12) . . ? C75 C74 H74 126.3 . . ? C73 C74 H74 126.3 . . ? Nb C74 H74 119.6 . . ? C74 C75 C71 109.5(2) . . ? C74 C75 Nb 72.14(11) . . ? C71 C75 Nb 74.44(11) . . ? C74 C75 H75 125.2 . . ? C71 C75 H75 125.2 . . ? Nb C75 H75 119.9 . . ? C77 Si7 C76 112.08(11) . . ? C77 Si7 C78 111.10(11) . . ? C76 Si7 C78 110.65(12) . . ? C77 Si7 C71 109.82(10) . . ? C76 Si7 C71 109.79(10) . . ? C78 Si7 C71 103.02(10) . . ? Si7 C76 H76A 109.5 . . ? Si7 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? Si7 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? Si7 C77 H77A 109.5 . . ? Si7 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? Si7 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? Si7 C78 H78A 109.5 . . ? Si7 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? Si7 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C82 C81 C86 118.4(2) . . ? C82 C81 C87 121.2(2) . . ? C86 C81 C87 120.4(3) . . ? C81 C82 C83 121.0(2) . . ? C81 C82 H82 119.5 . . ? C83 C82 H82 119.5 . . ? C82 C83 C84 119.6(3) . . ? C82 C83 H83 120.2 . . ? C84 C83 H83 120.2 . . ? C85 C84 C83 119.7(2) . . ? C85 C84 H84 120.2 . . ? C83 C84 H84 120.2 . . ? C84 C85 C86 120.3(3) . . ? C84 C85 H85 119.8 . . ? C86 C85 H85 119.8 . . ? C85 C86 C81 121.0(3) . . ? C85 C86 H86 119.5 . . ? C81 C86 H86 119.5 . . ? C81 C87 H87A 109.5 . . ? C81 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C81 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C41 B C11 C15 168.33(18) . . . . ? C31 B C11 C15 -70.2(2) . . . . ? Cl2 B C11 C15 42.3(2) . . . . ? C41 B C11 C12 -19.8(3) . . . . ? C31 B C11 C12 101.6(2) . . . . ? Cl2 B C11 C12 -145.88(17) . . . . ? C41 B C11 Nb 77.0(2) . . . . ? C31 B C11 Nb -161.52(13) . . . . ? Cl2 B C11 Nb -49.0(2) . . . . ? Cl5 Nb C11 C15 -158.44(12) . . . . ? Cl6 Nb C11 C15 107.75(12) . . . . ? C14 Nb C11 C15 37.65(13) . . . . ? C73 Nb C11 C15 -58.41(13) . . . . ? C74 Nb C11 C15 -25.10(14) . . . . ? C75 Nb C11 C15 -16.86(18) . . . . ? C72 Nb C11 C15 -85.17(14) . . . . ? C13 Nb C11 C15 78.64(14) . . . . ? C12 Nb C11 C15 114.77(18) . . . . ? C71 Nb C11 C15 -75.81(18) . . . . ? Cl5 Nb C11 C12 86.79(11) . . . . ? Cl6 Nb C11 C12 -7.02(14) . . . . ? C14 Nb C11 C12 -77.12(13) . . . . ? C73 Nb C11 C12 -173.18(12) . . . . ? C15 Nb C11 C12 -114.77(18) . . . . ? C74 Nb C11 C12 -139.87(12) . . . . ? C75 Nb C11 C12 -131.63(13) . . . . ? C72 Nb C11 C12 160.07(12) . . . . ? C13 Nb C11 C12 -36.13(12) . . . . ? C71 Nb C11 C12 169.42(14) . . . . ? Cl5 Nb C11 B -37.67(16) . . . . ? Cl6 Nb C11 B -131.48(15) . . . . ? C14 Nb C11 B 158.4(2) . . . . ? C73 Nb C11 B 62.36(18) . . . . ? C15 Nb C11 B 120.8(2) . . . . ? C74 Nb C11 B 95.68(17) . . . . ? C75 Nb C11 B 103.92(18) . . . . ? C72 Nb C11 B 35.61(19) . . . . ? C13 Nb C11 B -160.6(2) . . . . ? C12 Nb C11 B -124.5(2) . . . . ? C71 Nb C11 B 45.0(2) . . . . ? C15 C11 C12 C13 2.9(2) . . . . ? B C11 C12 C13 -170.35(18) . . . . ? Nb C11 C12 C13 64.40(14) . . . . ? C15 C11 C12 Nb -61.55(13) . . . . ? B C11 C12 Nb 125.25(19) . . . . ? Cl5 Nb C12 C13 154.20(13) . . . . ? Cl6 Nb C12 C13 57.26(13) . . . . ? C14 Nb C12 C13 -37.11(13) . . . . ? C73 Nb C12 C13 -108.46(14) . . . . ? C15 Nb C12 C13 -79.46(14) . . . . ? C74 Nb C12 C13 -63.26(16) . . . . ? C75 Nb C12 C13 -19.5(2) . . . . ? C72 Nb C12 C13 -151.76(15) . . . . ? C71 Nb C12 C13 111.1(6) . . . . ? C11 Nb C12 C13 -117.18(18) . . . . ? Cl5 Nb C12 C11 -88.62(11) . . . . ? Cl6 Nb C12 C11 174.44(11) . . . . ? C14 Nb C12 C11 80.07(13) . . . . ? C73 Nb C12 C11 8.72(16) . . . . ? C15 Nb C12 C11 37.72(12) . . . . ? C74 Nb C12 C11 53.91(15) . . . . ? C75 Nb C12 C11 97.72(17) . . . . ? C72 Nb C12 C11 -34.58(19) . . . . ? C13 Nb C12 C11 117.18(18) . . . . ? C71 Nb C12 C11 -131.7(5) . . . . ? C11 C12 C13 C14 -3.0(2) . . . . ? Nb C12 C13 C14 62.59(15) . . . . ? C11 C12 C13 Nb -65.63(14) . . . . ? Cl5 Nb C13 C12 -27.73(14) . . . . ? Cl6 Nb C13 C12 -120.46(13) . . . . ? C14 Nb C13 C12 116.29(19) . . . . ? C73 Nb C13 C12 100.54(15) . . . . ? C15 Nb C13 C12 77.17(13) . . . . ? C74 Nb C13 C12 133.30(13) . . . . ? C75 Nb C13 C12 169.38(12) . . . . ? C72 Nb C13 C12 106.5(3) . . . . ? C71 Nb C13 C12 -167.59(13) . . . . ? C11 Nb C13 C12 36.25(12) . . . . ? Cl5 Nb C13 C14 -144.02(12) . . . . ? Cl6 Nb C13 C14 123.25(13) . . . . ? C73 Nb C13 C14 -15.74(18) . . . . ? C15 Nb C13 C14 -39.12(13) . . . . ? C74 Nb C13 C14 17.01(15) . . . . ? C75 Nb C13 C14 53.09(15) . . . . ? C72 Nb C13 C14 -9.8(3) . . . . ? C12 Nb C13 C14 -116.29(19) . . . . ? C71 Nb C13 C14 76.12(19) . . . . ? C11 Nb C13 C14 -80.04(14) . . . . ? C12 C13 C14 C15 2.0(2) . . . . ? Nb C13 C14 C15 67.03(14) . . . . ? C12 C13 C14 Nb -65.07(15) . . . . ? Cl5 Nb C14 C13 52.94(16) . . . . ? Cl6 Nb C14 C13 -54.92(13) . . . . ? C73 Nb C14 C13 168.09(13) . . . . ? C15 Nb C14 C13 113.19(19) . . . . ? C74 Nb C14 C13 -163.73(14) . . . . ? C75 Nb C14 C13 -135.10(13) . . . . ? C72 Nb C14 C13 176.61(12) . . . . ? C12 Nb C14 C13 36.39(12) . . . . ? C71 Nb C14 C13 -138.90(13) . . . . ? C11 Nb C14 C13 76.70(13) . . . . ? Cl5 Nb C14 C15 -60.25(16) . . . . ? Cl6 Nb C14 C15 -168.10(12) . . . . ? C73 Nb C14 C15 54.91(14) . . . . ? C74 Nb C14 C15 83.08(14) . . . . ? C75 Nb C14 C15 111.72(13) . . . . ? C72 Nb C14 C15 63.42(16) . . . . ? C13 Nb C14 C15 -113.19(19) . . . . ? C12 Nb C14 C15 -76.79(13) . . . . ? C71 Nb C14 C15 107.91(14) . . . . ? C11 Nb C14 C15 -36.49(12) . . . . ? C12 C11 C15 C14 -1.6(2) . . . . ? B C11 C15 C14 171.70(18) . . . . ? Nb C11 C15 C14 -65.19(14) . . . . ? C12 C11 C15 Nb 63.57(13) . . . . ? B C11 C15 Nb -123.12(18) . . . . ? C13 C14 C15 C11 -0.2(2) . . . . ? Nb C14 C15 C11 68.52(14) . . . . ? C13 C14 C15 Nb -68.71(15) . . . . ? Cl5 Nb C15 C11 23.51(13) . . . . ? Cl6 Nb C15 C11 -100.54(12) . . . . ? C14 Nb C15 C11 -116.06(19) . . . . ? C73 Nb C15 C11 119.88(13) . . . . ? C74 Nb C15 C11 155.30(14) . . . . ? C75 Nb C15 C11 168.74(12) . . . . ? C72 Nb C15 C11 109.97(12) . . . . ? C13 Nb C15 C11 -77.90(13) . . . . ? C12 Nb C15 C11 -37.37(12) . . . . ? C71 Nb C15 C11 140.95(12) . . . . ? Cl5 Nb C15 C14 139.58(12) . . . . ? Cl6 Nb C15 C14 15.53(15) . . . . ? C73 Nb C15 C14 -124.06(14) . . . . ? C74 Nb C15 C14 -88.64(14) . . . . ? C75 Nb C15 C14 -75.20(14) . . . . ? C72 Nb C15 C14 -133.97(13) . . . . ? C13 Nb C15 C14 38.16(13) . . . . ? C12 Nb C15 C14 78.70(14) . . . . ? C71 Nb C15 C14 -102.99(14) . . . . ? C11 Nb C15 C14 116.06(19) . . . . ? C11 B C31 C36 0.3(3) . . . . ? C41 B C31 C36 124.9(2) . . . . ? Cl2 B C31 C36 -114.1(2) . . . . ? C11 B C31 C32 179.75(17) . . . . ? C41 B C31 C32 -55.7(2) . . . . ? Cl2 B C31 C32 65.3(2) . . . . ? C36 C31 C32 F32 -178.98(17) . . . . ? B C31 C32 F32 1.5(3) . . . . ? C36 C31 C32 C33 1.1(3) . . . . ? B C31 C32 C33 -178.41(19) . . . . ? F32 C32 C33 F33 -0.5(3) . . . . ? C31 C32 C33 F33 179.39(18) . . . . ? F32 C32 C33 C34 179.39(18) . . . . ? C31 C32 C33 C34 -0.7(3) . . . . ? F33 C33 C34 F34 0.8(3) . . . . ? C32 C33 C34 F34 -179.12(19) . . . . ? F33 C33 C34 C35 179.60(19) . . . . ? C32 C33 C34 C35 -0.3(3) . . . . ? F34 C34 C35 F35 0.0(3) . . . . ? C33 C34 C35 F35 -178.80(19) . . . . ? F34 C34 C35 C36 179.61(19) . . . . ? C33 C34 C35 C36 0.8(3) . . . . ? F35 C35 C36 F36 -0.9(3) . . . . ? C34 C35 C36 F36 179.48(18) . . . . ? F35 C35 C36 C31 179.27(18) . . . . ? C34 C35 C36 C31 -0.4(3) . . . . ? C32 C31 C36 F36 179.60(18) . . . . ? B C31 C36 F36 -0.9(3) . . . . ? C32 C31 C36 C35 -0.6(3) . . . . ? B C31 C36 C35 178.9(2) . . . . ? C11 B C41 C42 70.5(2) . . . . ? C31 B C41 C42 -54.2(2) . . . . ? Cl2 B C41 C42 -167.88(15) . . . . ? C11 B C41 C46 -114.0(2) . . . . ? C31 B C41 C46 121.4(2) . . . . ? Cl2 B C41 C46 7.7(3) . . . . ? C46 C41 C42 F42 -179.30(17) . . . . ? B C41 C42 F42 -3.1(3) . . . . ? C46 C41 C42 C43 -0.2(3) . . . . ? B C41 C42 C43 176.00(19) . . . . ? F42 C42 C43 F43 2.1(3) . . . . ? C41 C42 C43 F43 -176.96(19) . . . . ? F42 C42 C43 C44 179.74(18) . . . . ? C41 C42 C43 C44 0.6(3) . . . . ? F43 C43 C44 F44 -1.0(3) . . . . ? C42 C43 C44 F44 -178.59(19) . . . . ? F43 C43 C44 C45 177.42(19) . . . . ? C42 C43 C44 C45 -0.2(3) . . . . ? F44 C44 C45 F45 -0.7(3) . . . . ? C43 C44 C45 F45 -179.10(19) . . . . ? F44 C44 C45 C46 177.81(19) . . . . ? C43 C44 C45 C46 -0.6(3) . . . . ? F45 C45 C46 F46 0.5(3) . . . . ? C44 C45 C46 F46 -178.04(19) . . . . ? F45 C45 C46 C41 179.54(19) . . . . ? C44 C45 C46 C41 1.0(3) . . . . ? C42 C41 C46 F46 178.41(18) . . . . ? B C41 C46 F46 2.6(3) . . . . ? C42 C41 C46 C45 -0.6(3) . . . . ? B C41 C46 C45 -176.36(19) . . . . ? Cl5 Nb C71 C72 64.94(12) . . . . ? Cl6 Nb C71 C72 162.09(12) . . . . ? C14 Nb C71 C72 -107.00(14) . . . . ? C73 Nb C71 C72 -35.93(13) . . . . ? C15 Nb C71 C72 -60.80(15) . . . . ? C74 Nb C71 C72 -77.54(14) . . . . ? C75 Nb C71 C72 -113.79(18) . . . . ? C13 Nb C71 C72 -151.78(15) . . . . ? C12 Nb C71 C72 107.6(6) . . . . ? C11 Nb C71 C72 -15.1(2) . . . . ? Cl5 Nb C71 C75 178.73(12) . . . . ? Cl6 Nb C71 C75 -84.13(12) . . . . ? C14 Nb C71 C75 6.79(16) . . . . ? C73 Nb C71 C75 77.86(14) . . . . ? C15 Nb C71 C75 52.99(16) . . . . ? C74 Nb C71 C75 36.25(13) . . . . ? C72 Nb C71 C75 113.79(18) . . . . ? C13 Nb C71 C75 -38.0(2) . . . . ? C12 Nb C71 C75 -138.6(5) . . . . ? C11 Nb C71 C75 98.72(16) . . . . ? Cl5 Nb C71 Si7 -56.76(13) . . . . ? Cl6 Nb C71 Si7 40.38(12) . . . . ? C14 Nb C71 Si7 131.30(13) . . . . ? C73 Nb C71 Si7 -157.63(17) . . . . ? C15 Nb C71 Si7 177.50(11) . . . . ? C74 Nb C71 Si7 160.75(17) . . . . ? C75 Nb C71 Si7 124.5(2) . . . . ? C72 Nb C71 Si7 -121.7(2) . . . . ? C13 Nb C71 Si7 86.52(19) . . . . ? C12 Nb C71 Si7 -14.1(7) . . . . ? C11 Nb C71 Si7 -136.77(13) . . . . ? C75 C71 C72 C73 -1.8(2) . . . . ? Si7 C71 C72 C73 -169.92(15) . . . . ? Nb C71 C72 C73 62.47(14) . . . . ? C75 C71 C72 Nb -64.31(13) . . . . ? Si7 C71 C72 Nb 127.61(15) . . . . ? Cl5 Nb C72 C73 129.33(13) . . . . ? Cl6 Nb C72 C73 -137.28(12) . . . . ? C14 Nb C72 C73 -15.30(17) . . . . ? C15 Nb C72 C73 17.65(15) . . . . ? C74 Nb C72 C73 -38.66(13) . . . . ? C75 Nb C72 C73 -79.63(14) . . . . ? C13 Nb C72 C73 -8.1(3) . . . . ? C12 Nb C72 C73 74.52(19) . . . . ? C71 Nb C72 C73 -117.92(19) . . . . ? C11 Nb C72 C73 53.82(15) . . . . ? Cl5 Nb C72 C71 -112.74(12) . . . . ? Cl6 Nb C72 C71 -19.36(13) . . . . ? C14 Nb C72 C71 102.62(14) . . . . ? C73 Nb C72 C71 117.92(19) . . . . ? C15 Nb C72 C71 135.58(12) . . . . ? C74 Nb C72 C71 79.26(13) . . . . ? C75 Nb C72 C71 38.29(12) . . . . ? C13 Nb C72 C71 109.9(3) . . . . ? C12 Nb C72 C71 -167.55(13) . . . . ? C11 Nb C72 C71 171.74(11) . . . . ? C71 C72 C73 C74 2.5(2) . . . . ? Nb C72 C73 C74 67.17(14) . . . . ? C71 C72 C73 Nb -64.67(14) . . . . ? Cl5 Nb C73 C72 -50.54(13) . . . . ? Cl6 Nb C73 C72 61.35(16) . . . . ? C14 Nb C73 C72 168.38(13) . . . . ? C15 Nb C73 C72 -163.08(14) . . . . ? C74 Nb C73 C72 113.85(18) . . . . ? C75 Nb C73 C72 76.73(13) . . . . ? C13 Nb C73 C72 177.20(12) . . . . ? C12 Nb C73 C72 -138.93(12) . . . . ? C71 Nb C73 C72 35.81(12) . . . . ? C11 Nb C73 C72 -134.11(13) . . . . ? Cl5 Nb C73 C74 -164.39(11) . . . . ? Cl6 Nb C73 C74 -52.50(15) . . . . ? C14 Nb C73 C74 54.54(13) . . . . ? C15 Nb C73 C74 83.08(13) . . . . ? C75 Nb C73 C74 -37.11(12) . . . . ? C72 Nb C73 C74 -113.85(18) . . . . ? C13 Nb C73 C74 63.35(15) . . . . ? C12 Nb C73 C74 107.22(13) . . . . ? C71 Nb C73 C74 -78.04(13) . . . . ? C11 Nb C73 C74 112.04(12) . . . . ? C72 C73 C74 C75 -2.2(2) . . . . ? Nb C73 C74 C75 66.19(14) . . . . ? C72 C73 C74 Nb -68.34(14) . . . . ? Cl5 Nb C74 C75 -93.53(14) . . . . ? Cl6 Nb C74 C75 28.39(14) . . . . ? C14 Nb C74 C75 120.64(15) . . . . ? C73 Nb C74 C75 -114.92(19) . . . . ? C15 Nb C74 C75 156.36(15) . . . . ? C72 Nb C74 C75 -77.19(14) . . . . ? C13 Nb C74 C75 111.01(14) . . . . ? C12 Nb C74 C75 142.65(13) . . . . ? C71 Nb C74 C75 -36.55(13) . . . . ? C11 Nb C74 C75 170.41(13) . . . . ? Cl5 Nb C74 C73 21.39(15) . . . . ? Cl6 Nb C74 C73 143.31(11) . . . . ? C14 Nb C74 C73 -124.44(13) . . . . ? C15 Nb C74 C73 -88.72(13) . . . . ? C75 Nb C74 C73 114.92(19) . . . . ? C72 Nb C74 C73 37.73(12) . . . . ? C13 Nb C74 C73 -134.07(12) . . . . ? C12 Nb C74 C73 -102.43(14) . . . . ? C71 Nb C74 C73 78.37(13) . . . . ? C11 Nb C74 C73 -74.67(13) . . . . ? C73 C74 C75 C71 1.0(2) . . . . ? Nb C74 C75 C71 65.59(14) . . . . ? C73 C74 C75 Nb -64.57(14) . . . . ? C72 C71 C75 C74 0.5(2) . . . . ? Si7 C71 C75 C74 168.17(15) . . . . ? Nb C71 C75 C74 -64.12(14) . . . . ? C72 C71 C75 Nb 64.59(13) . . . . ? Si7 C71 C75 Nb -127.71(16) . . . . ? Cl5 Nb C75 C74 115.43(13) . . . . ? Cl6 Nb C75 C74 -152.92(14) . . . . ? C14 Nb C75 C74 -57.74(14) . . . . ? C73 Nb C75 C74 38.11(13) . . . . ? C15 Nb C75 C74 -24.04(15) . . . . ? C72 Nb C75 C74 79.08(15) . . . . ? C13 Nb C75 C74 -84.45(15) . . . . ? C12 Nb C75 C74 -72.4(2) . . . . ? C71 Nb C75 C74 117.01(19) . . . . ? C11 Nb C75 C74 -14.33(19) . . . . ? Cl5 Nb C75 C71 -1.58(15) . . . . ? Cl6 Nb C75 C71 90.07(12) . . . . ? C14 Nb C75 C71 -174.75(13) . . . . ? C73 Nb C75 C71 -78.90(13) . . . . ? C15 Nb C75 C71 -141.04(12) . . . . ? C74 Nb C75 C71 -117.01(19) . . . . ? C72 Nb C75 C71 -37.93(12) . . . . ? C13 Nb C75 C71 158.54(12) . . . . ? C12 Nb C75 C71 170.58(13) . . . . ? C11 Nb C75 C71 -131.34(13) . . . . ? C72 C71 Si7 C77 -178.07(17) . . . . ? C75 C71 Si7 C77 16.5(2) . . . . ? Nb C71 Si7 C77 -81.59(15) . . . . ? C72 C71 Si7 C76 -54.4(2) . . . . ? C75 C71 Si7 C76 140.19(19) . . . . ? Nb C71 Si7 C76 42.08(17) . . . . ? C72 C71 Si7 C78 63.49(19) . . . . ? C75 C71 Si7 C78 -101.9(2) . . . . ? Nb C71 Si7 C78 159.98(13) . . . . ? C86 C81 C82 C83 0.0(4) . . . . ? C87 C81 C82 C83 -179.3(2) . . . . ? C81 C82 C83 C84 0.7(4) . . . . ? C82 C83 C84 C85 -0.6(4) . . . . ? C83 C84 C85 C86 -0.1(4) . . . . ? C84 C85 C86 C81 0.8(4) . . . . ? C82 C81 C86 C85 -0.7(4) . . . . ? C87 C81 C86 C85 178.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.392 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.072