data_global # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication in Organometallics ; _publ_contact_author ; M. Etienne ; _publ_contact_author_address ; Laboratoire de Chimie de Coordination 205 Route de Narbonne 31077 Toulouse Cedex 04 ; _publ_contact_author_email 'etienne@lcc-toulouse.fr' _publ_requested_journal ' Organometallics ' #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Elusive Niobium Alkyl Cations Related to Ethylene Polymerization ; loop_ _publ_author_name H. M. Pritchard, M. Etienne, L. Vendier, G. S. McGrady _publ_author_address ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex 04, France ; King's College London, Strand, London, UK WCR 2LS ; Department of Chemistry, University of New Brunswick, Fredericton, N. B., Canada E3B 6E2 #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Gottingen, Germany. Stoe, IPDS Manual. Version 2.75. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. DIFABS - N. Walker and D. Stuart, Acta Crystallogr., Sect A 1983, 39, 158-166. WINGX - 1.63 Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-Ray Diffraction Data. Farrugia, L. J. Appl. Crystallogr., 1999, 32, 837. ORTEP3 for Windows, Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565.; ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H55 B2 F24 N6 Nb1 O1' _chemical_formula_sum 'C56 H55 B2 F24 N6 Nb O' _chemical_formula_weight 1398.59 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7185(6) _cell_length_b 13.0870(7) _cell_length_c 18.5693(10) _cell_angle_alpha 91.249(4) _cell_angle_beta 94.824(4) _cell_angle_gamma 99.599(4) _cell_volume 3034.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6490 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 32.2 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.317 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 0.963 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_unetI/netI 0.0527 _diffrn_reflns_number 17779 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 23.21 _diffrn_reflns_theta_full 23.21 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 8700 _reflns_number_gt 6918 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1265P)^2^+8.5423P] 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_number_reflns 8700 _refine_ls_number_parameters 820 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2274 _refine_ls_wR_factor_gt 0.2155 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.905 _refine_ls_shift/su_mean 0.014 _refine_diff_density_max 1.482 _refine_diff_density_min -1.53 _refine_diff_density_rms 0.097 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 '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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.6672(6) 1.1511(6) 0.8485(4) 0.0521(17) Uani 1 1 d . A . C2 C 0.7243(6) 1.0723(6) 0.8559(4) 0.061(2) Uani 1 1 d . . . H2 H 0.7789 1.067 0.8931 0.073 Uiso 1 1 calc R . . C3 C 0.6882(6) 1.0012(5) 0.7995(4) 0.0544(18) Uani 1 1 d . . . C4 C 0.6822(7) 1.2504(7) 0.8932(4) 0.072(2) Uani 1 1 d . . . H4A H 0.7097 1.2383 0.9426 0.108 Uiso 1 1 calc R . . H4B H 0.6133 1.2744 0.8941 0.108 Uiso 1 1 calc R . . H4C H 0.7333 1.3031 0.8719 0.108 Uiso 1 1 calc R . . C5 C 0.7271(8) 0.9040(6) 0.7790(6) 0.093(3) Uani 1 1 d . . . H5A H 0.6719 0.844 0.7859 0.139 Uiso 1 1 calc R . . H5B H 0.7925 0.8985 0.8095 0.139 Uiso 1 1 calc R . . H5C H 0.7424 0.9056 0.7281 0.139 Uiso 1 1 calc R . . C6 C 0.5658(5) 1.2253(5) 0.5781(3) 0.0448(15) Uani 1 1 d . A . C7 C 0.6155(5) 1.1635(5) 0.5340(4) 0.0482(16) Uani 1 1 d . . . H7 H 0.6438 1.1816 0.4894 0.058 Uiso 1 1 calc R . . C8 C 0.6152(5) 1.0711(5) 0.5683(3) 0.0437(15) Uani 1 1 d . . . C9 C 0.5514(7) 1.3343(6) 0.5653(4) 0.065(2) Uani 1 1 d . . . H9A H 0.4846 1.3466 0.5839 0.097 Uiso 1 1 calc R . . H9B H 0.5484 1.3461 0.5132 0.097 Uiso 1 1 calc R . . H9C H 0.6118 1.382 0.5902 0.097 Uiso 1 1 calc R . . C10 C 0.6593(6) 0.9788(6) 0.5454(4) 0.063(2) Uani 1 1 d . . . H10A H 0.7166 0.9669 0.5813 0.095 Uiso 1 1 calc R . . H10B H 0.6882 0.9906 0.4984 0.095 Uiso 1 1 calc R . . H10C H 0.6024 0.918 0.5413 0.095 Uiso 1 1 calc R . . C11 C 0.2701(5) 1.0099(5) 0.7184(4) 0.0537(17) Uani 1 1 d . A . C12 C 0.2576(5) 0.9049(5) 0.7059(4) 0.0529(17) Uani 1 1 d . . . H12 H 0.193 0.8566 0.7063 0.063 Uiso 1 1 calc R . . C13 C 0.3559(5) 0.8825(5) 0.6926(3) 0.0415(15) Uani 1 1 d . . . C14 C 0.1839(6) 1.0734(7) 0.7331(6) 0.081(3) Uani 1 1 d . . . H14A H 0.2006 1.1078 0.7811 0.121 Uiso 1 1 calc R . . H14B H 0.1144 1.0275 0.7314 0.121 Uiso 1 1 calc R . . H14C H 0.1812 1.1257 0.6964 0.121 Uiso 1 1 calc R . . C15 C 0.3869(6) 0.7823(5) 0.6742(4) 0.0534(17) Uani 1 1 d . . . H15A H 0.4104 0.7837 0.6252 0.08 Uiso 1 1 calc R . . H15B H 0.3254 0.7266 0.6763 0.08 Uiso 1 1 calc R . . H15C H 0.4456 0.7697 0.7087 0.08 Uiso 1 1 calc R . . C16 C 0.3871(7) 1.1008(7) 0.8794(5) 0.072(2) Uani 1 1 d . A . H16A H 0.3094 1.0734 0.8761 0.087 Uiso 1 1 calc R . . H16B H 0.4222 1.0505 0.8537 0.087 Uiso 1 1 calc R . . C17 C 0.4277(9) 1.1090(9) 0.9535(5) 0.096(3) Uani 1 1 d . . . H17A H 0.5042 1.1381 0.9574 0.145 Uiso 1 1 calc R . . H17B H 0.4174 1.04 0.974 0.145 Uiso 1 1 calc R . . H17C H 0.3893 1.1544 0.9801 0.145 Uiso 1 1 calc R . . O1 O 0.4041(4) 1.1997(4) 0.8432(3) 0.0626(13) Uani 1 1 d D . . C18A C 0.3317(16) 1.2651(13) 0.8717(10) 0.094(4) Uani 0.61 1 d PD A 1 H18A H 0.2909 1.2282 0.9092 0.112 Uiso 0.61 1 calc PR A 1 H18B H 0.2802 1.2811 0.8323 0.112 Uiso 0.61 1 calc PR A 1 C19A C 0.3995(15) 1.3636(13) 0.9036(9) 0.094(4) Uani 0.61 1 d PD A 1 H19A H 0.4466 1.3474 0.9448 0.141 Uiso 0.61 1 calc PR A 1 H19B H 0.3531 1.4105 0.92 0.141 Uiso 0.61 1 calc PR A 1 H19C H 0.443 1.3972 0.8668 0.141 Uiso 0.61 1 calc PR A 1 C18B C 0.398(2) 1.299(2) 0.8812(19) 0.116(8) Uani 0.39 1 d PD A 2 H18C H 0.4312 1.3584 0.8542 0.139 Uiso 0.39 1 calc PR A 2 H18D H 0.4355 1.3021 0.9305 0.139 Uiso 0.39 1 calc PR A 2 C19B C 0.279(2) 1.298(2) 0.8844(18) 0.116(8) Uani 0.39 1 d PD A 2 H19D H 0.2445 1.2995 0.8353 0.174 Uiso 0.39 1 calc PR A 2 H19E H 0.2685 1.3599 0.9123 0.174 Uiso 0.39 1 calc PR A 2 H19F H 0.2469 1.2358 0.9078 0.174 Uiso 0.39 1 calc PR A 2 C20 C 0.3709(6) 1.3310(6) 0.7115(4) 0.0590(19) Uani 1 1 d . . . H20 H 0.3147 1.2969 0.7419 0.071 Uiso 1 1 calc R A . C21 C 0.3479(5) 1.2585(5) 0.6663(4) 0.0464(16) Uani 1 1 d . A . H21 H 0.2898 1.2227 0.6946 0.056 Uiso 1 1 calc R . . C22 C 0.3409(8) 1.4336(6) 0.7271(5) 0.076(2) Uani 1 1 d . A . H22A H 0.3796 1.4857 0.6975 0.114 Uiso 1 1 calc R . . H22B H 0.3596 1.4531 0.7784 0.114 Uiso 1 1 calc R . . H22C H 0.2637 1.4297 0.7157 0.114 Uiso 1 1 calc R . . C23 C 0.2786(7) 1.2303(7) 0.5935(5) 0.077(2) Uani 1 1 d . . . H23A H 0.2217 1.2725 0.5891 0.116 Uiso 1 1 calc R A . H23B H 0.2467 1.1567 0.592 0.116 Uiso 1 1 calc R . . H23C H 0.3238 1.244 0.5533 0.116 Uiso 1 1 calc R . . C30 C 1.0233(4) 0.6300(4) 0.6709(3) 0.0279(12) Uani 1 1 d . . . C31 C 1.0806(4) 0.5714(4) 0.6300(3) 0.0302(12) Uani 1 1 d . . . H31 H 1.0945 0.5068 0.6474 0.036 Uiso 1 1 calc R . . C32 C 1.1179(4) 0.6046(4) 0.5648(3) 0.0328(13) Uani 1 1 d . . . C33 C 1.1019(5) 0.6989(5) 0.5383(3) 0.0367(14) Uani 1 1 d . . . H33 H 1.1284 0.7219 0.4941 0.044 Uiso 1 1 calc R . . C34 C 1.0462(5) 0.7590(4) 0.5782(3) 0.0385(14) Uani 1 1 d . . . C35 C 1.0076(4) 0.7247(4) 0.6428(3) 0.0314(12) Uani 1 1 d . . . H35 H 0.9691 0.7673 0.6687 0.038 Uiso 1 1 calc R . . C36 C 1.1805(5) 0.5388(5) 0.5247(3) 0.0419(15) Uani 1 1 d . . . C37 C 1.0249(6) 0.8615(5) 0.5503(4) 0.0506(17) Uani 1 1 d . . . C40 C 0.9848(4) 0.4807(4) 0.7734(3) 0.0287(12) Uani 1 1 d . . . C41 C 1.0136(5) 0.4577(5) 0.8458(3) 0.0364(13) Uani 1 1 d . . . H41 H 1.039 0.5129 0.8802 0.044 Uiso 1 1 calc R . . C42 C 1.0054(5) 0.3556(5) 0.8675(3) 0.0449(15) Uani 1 1 d . B . C43 C 0.9719(5) 0.2731(5) 0.8185(4) 0.0459(16) Uani 1 1 d . . . H43 H 0.9678 0.2036 0.8332 0.055 Uiso 1 1 calc R . . C44 C 0.9445(5) 0.2946(5) 0.7473(3) 0.0377(14) Uani 1 1 d . . . C45 C 0.9500(4) 0.3961(4) 0.7264(3) 0.0311(12) Uani 1 1 d . . . H45 H 0.9289 0.4083 0.6775 0.037 Uiso 1 1 calc R . . C46 C 0.9083(6) 0.2079(5) 0.6932(4) 0.0504(17) Uani 1 1 d . . . C50 C 1.0597(4) 0.6840(4) 0.8068(3) 0.0278(12) Uani 1 1 d . . . C51 C 1.0297(5) 0.7711(4) 0.8377(3) 0.0340(13) Uani 1 1 d . . . H51 H 0.9581 0.7826 0.8284 0.041 Uiso 1 1 calc R . . C52 C 1.1017(5) 0.8420(4) 0.8818(3) 0.0371(14) Uani 1 1 d . C . C53 C 1.2067(5) 0.8285(5) 0.8963(3) 0.0399(14) Uani 1 1 d . . . H53 H 1.2555 0.8763 0.9273 0.048 Uiso 1 1 calc R . . C54 C 1.2392(5) 0.7441(5) 0.8649(3) 0.0375(14) Uani 1 1 d . . . C55 C 1.1671(4) 0.6728(4) 0.8215(3) 0.0325(13) Uani 1 1 d . . . H55 H 1.1912 0.6146 0.801 0.039 Uiso 1 1 calc R . . C57 C 1.3525(5) 0.7261(6) 0.8797(4) 0.0518(17) Uani 1 1 d . . . C60 C 0.8549(4) 0.6115(4) 0.7523(3) 0.0294(12) Uani 1 1 d . . . C61 C 0.7862(4) 0.6170(4) 0.6906(3) 0.0303(12) Uani 1 1 d . . . H61 H 0.814 0.6167 0.6447 0.036 Uiso 1 1 calc R . . C62 C 0.6790(4) 0.6229(4) 0.6935(3) 0.0349(13) Uani 1 1 d . . . C63 C 0.6352(5) 0.6220(4) 0.7594(3) 0.0386(14) Uani 1 1 d . . . H63 H 0.5619 0.6268 0.7619 0.046 Uiso 1 1 calc R . . C64 C 0.7013(5) 0.6139(5) 0.8217(3) 0.0380(14) Uani 1 1 d . D . C65 C 0.8080(4) 0.6087(4) 0.8175(3) 0.0344(13) Uani 1 1 d . . . H65 H 0.8513 0.6029 0.861 0.041 Uiso 1 1 calc R . . C67 C 0.6113(5) 0.6328(5) 0.6245(4) 0.0456(15) Uani 1 1 d . . . C24 C 0.5979(6) 1.3458(5) 0.7419(4) 0.0587(19) Uani 1 1 d . . . H24A H 0.583 1.3959 0.7056 0.088 Uiso 1 1 calc R A . H24B H 0.6637 1.3201 0.7324 0.088 Uiso 1 1 calc R . . H24C H 0.6069 1.3796 0.7902 0.088 Uiso 1 1 calc R . . B1 B 0.5462(5) 0.9954(5) 0.6878(4) 0.0366(15) Uani 1 1 d . . . H1 H 0.5703 0.9302 0.672 0.044 Uiso 1 1 calc R . . B2 B 0.9814(5) 0.6006(5) 0.7503(3) 0.0277(13) Uani 1 1 d . . . N1 N 0.5944(4) 1.1309(4) 0.7895(3) 0.0417(12) Uani 1 1 d . . . N2 N 0.6091(4) 1.0377(4) 0.7594(3) 0.0408(12) Uani 1 1 d . A . N3 N 0.5657(4) 1.0770(4) 0.6302(2) 0.0345(11) Uani 1 1 d . A . N4 N 0.5353(4) 1.1731(4) 0.6364(3) 0.0376(11) Uani 1 1 d . . . N5 N 0.4270(4) 0.9730(3) 0.6988(3) 0.0347(11) Uani 1 1 d . A . N6 N 0.3749(4) 1.0521(4) 0.7146(3) 0.0465(13) Uani 1 1 d . . . F1 F 1.1848(4) 0.5614(4) 0.45508(19) 0.0667(12) Uani 1 1 d . . . F2 F 1.2805(3) 0.5463(4) 0.5523(2) 0.0608(11) Uani 1 1 d . . . F3 F 1.1381(4) 0.4374(3) 0.5245(3) 0.0700(12) Uani 1 1 d . . . F4 F 1.1043(5) 0.9081(4) 0.5156(4) 0.120(2) Uani 1 1 d . . . F5 F 0.9439(5) 0.8521(4) 0.5018(3) 0.114(2) Uani 1 1 d . . . F6 F 1.0114(6) 0.9262(4) 0.6009(3) 0.105(2) Uani 1 1 d . . . F7 F 0.9718(6) 0.2134(4) 0.6395(3) 0.113(2) Uani 1 1 d . . . F8 F 0.9149(5) 0.1153(3) 0.7176(3) 0.0964(18) Uani 1 1 d . . . F9 F 0.8158(5) 0.2071(5) 0.6630(5) 0.160(4) Uani 1 1 d . . . C47 C 1.0292(7) 0.3359(5) 0.9455(5) 0.076(3) Uani 1 1 d D . . F10A F 1.0994(9) 0.2661(8) 0.9502(5) 0.1024(19) Uani 0.61 1 d PD B 1 F11A F 1.0746(10) 0.4136(9) 0.9888(5) 0.1024(19) Uani 0.61 1 d PD B 1 F12A F 0.9486(9) 0.2989(8) 0.9805(5) 0.1024(19) Uani 0.61 1 d PD B 1 F10B F 1.0434(15) 0.2429(11) 0.9645(8) 0.1024(19) Uani 0.39 1 d PD B 2 F11B F 1.1100(14) 0.4107(14) 0.9735(8) 0.1024(19) Uani 0.39 1 d PD B 2 F12B F 0.9429(13) 0.3542(13) 0.9828(7) 0.1024(19) Uani 0.39 1 d PD B 2 C56 C 1.0648(5) 0.9298(5) 0.9151(4) 0.0500(17) Uani 1 1 d D . . F13A F 1.1390(6) 0.9990(6) 0.9519(5) 0.0962(16) Uani 0.69 1 d PD C 1 F14A F 1.0199(7) 0.9895(6) 0.8650(5) 0.0962(16) Uani 0.69 1 d PD C 1 F15A F 0.9746(7) 0.9065(7) 0.9454(5) 0.0962(16) Uani 0.69 1 d PD C 1 F13B F 1.1023(17) 1.0228(10) 0.8904(11) 0.0962(16) Uani 0.31 1 d PD C 2 F14B F 0.9583(12) 0.9276(16) 0.9126(12) 0.0962(16) Uani 0.31 1 d PD C 2 F15B F 1.0725(16) 0.9228(13) 0.9887(7) 0.0962(16) Uani 0.31 1 d PD C 2 F16 F 1.3838(3) 0.6685(4) 0.8303(2) 0.0739(14) Uani 1 1 d . . . F17 F 1.4218(4) 0.8148(5) 0.8819(4) 0.118(2) Uani 1 1 d . . . F18 F 1.3694(4) 0.6838(6) 0.9418(3) 0.103(2) Uani 1 1 d . . . C66 C 0.6577(5) 0.6115(5) 0.8927(4) 0.0547(18) Uani 1 1 d D . . F19A F 0.6873(11) 0.5303(8) 0.9302(5) 0.0766(14) Uani 0.51 1 d PD D 1 F20A F 0.7083(8) 0.6956(8) 0.9369(4) 0.0766(14) Uani 0.51 1 d PD D 1 F21A F 0.5554(7) 0.6128(10) 0.8959(5) 0.0766(14) Uani 0.51 1 d PD D 1 F19B F 0.7020(11) 0.5642(10) 0.9460(5) 0.0766(14) Uani 0.49 1 d PD D 2 F20B F 0.6275(9) 0.6979(8) 0.9128(5) 0.0766(14) Uani 0.49 1 d PD D 2 F21B F 0.5537(7) 0.5504(9) 0.8860(5) 0.0766(14) Uani 0.49 1 d PD D 2 F22 F 0.6428(3) 0.5859(3) 0.5679(2) 0.0644(11) Uani 1 1 d . . . F23 F 0.5088(3) 0.5927(3) 0.6283(2) 0.0647(11) Uani 1 1 d . . . F24 F 0.6152(3) 0.7318(3) 0.6075(2) 0.0624(11) Uani 1 1 d . . . Nb1 Nb 0.46469(5) 1.21630(4) 0.73655(3) 0.0443(2) Uani 1 1 d . A . 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 C1 0.051(4) 0.065(5) 0.036(4) -0.004(3) -0.002(3) -0.001(4) C2 0.058(4) 0.066(5) 0.052(4) 0.010(4) -0.018(4) 0.002(4) C3 0.051(4) 0.047(4) 0.062(5) 0.011(3) -0.015(4) 0.007(3) C4 0.067(5) 0.094(6) 0.048(4) -0.024(4) -0.011(4) 0.006(5) C5 0.093(7) 0.048(5) 0.130(8) -0.002(5) -0.059(6) 0.028(5) C6 0.043(4) 0.048(4) 0.042(4) 0.010(3) 0.002(3) 0.005(3) C7 0.041(4) 0.061(4) 0.040(4) 0.010(3) 0.005(3) -0.002(3) C8 0.034(3) 0.051(4) 0.042(4) -0.011(3) 0.004(3) -0.005(3) C9 0.074(5) 0.059(5) 0.066(5) 0.027(4) 0.014(4) 0.017(4) C10 0.059(5) 0.060(5) 0.071(5) -0.015(4) 0.028(4) 0.002(4) C11 0.043(4) 0.052(4) 0.067(5) 0.006(3) 0.011(3) 0.007(3) C12 0.039(4) 0.058(4) 0.057(4) 0.007(3) 0.001(3) -0.006(3) C13 0.043(4) 0.040(3) 0.039(3) 0.007(3) -0.003(3) 0.001(3) C14 0.046(4) 0.072(6) 0.125(8) 0.000(5) 0.027(5) 0.007(4) C15 0.062(4) 0.040(4) 0.053(4) 0.000(3) -0.007(3) -0.002(3) C16 0.075(6) 0.072(5) 0.070(6) 0.021(4) 0.016(4) 0.007(4) C17 0.112(8) 0.100(7) 0.073(6) 0.003(5) 0.008(6) 0.003(6) O1 0.082(4) 0.064(3) 0.048(3) 0.005(2) 0.023(3) 0.021(3) C18A 0.138(12) 0.078(8) 0.078(8) -0.002(6) 0.025(8) 0.048(8) C19A 0.138(12) 0.078(8) 0.078(8) -0.002(6) 0.025(8) 0.048(8) C18B 0.120(17) 0.081(14) 0.13(2) -0.016(13) -0.051(16) 0.008(14) C19B 0.120(17) 0.081(14) 0.13(2) -0.016(13) -0.051(16) 0.008(14) C20 0.055(4) 0.072(5) 0.050(4) 0.009(4) 0.016(4) 0.005(4) C21 0.039(3) 0.039(4) 0.064(4) 0.010(3) 0.017(3) 0.007(3) C22 0.098(7) 0.065(5) 0.074(6) 0.013(4) 0.012(5) 0.039(5) C23 0.069(5) 0.085(6) 0.076(6) -0.013(5) -0.009(4) 0.018(5) C30 0.022(3) 0.035(3) 0.024(3) -0.001(2) -0.005(2) 0.003(2) C31 0.028(3) 0.031(3) 0.030(3) 0.003(2) 0.001(2) 0.002(2) C32 0.025(3) 0.044(3) 0.027(3) -0.002(2) 0.001(2) 0.000(2) C33 0.034(3) 0.050(4) 0.023(3) 0.005(3) 0.005(2) -0.002(3) C34 0.042(3) 0.036(3) 0.033(3) 0.009(3) -0.005(3) -0.001(3) C35 0.035(3) 0.033(3) 0.027(3) 0.001(2) -0.001(2) 0.008(2) C36 0.037(4) 0.058(4) 0.029(3) 0.001(3) 0.003(3) 0.005(3) C37 0.066(5) 0.043(4) 0.041(4) 0.011(3) 0.002(3) 0.005(3) C40 0.026(3) 0.037(3) 0.025(3) 0.004(2) 0.002(2) 0.008(2) C41 0.036(3) 0.044(3) 0.028(3) 0.004(3) -0.003(2) 0.008(3) C42 0.051(4) 0.045(4) 0.039(4) 0.013(3) -0.005(3) 0.011(3) C43 0.045(4) 0.039(3) 0.053(4) 0.014(3) -0.004(3) 0.008(3) C44 0.035(3) 0.040(3) 0.039(3) 0.002(3) 0.002(3) 0.008(3) C45 0.025(3) 0.043(3) 0.026(3) 0.006(2) 0.000(2) 0.009(2) C46 0.059(4) 0.039(4) 0.051(4) 0.000(3) -0.002(4) 0.005(3) C50 0.032(3) 0.031(3) 0.022(3) 0.004(2) 0.005(2) 0.009(2) C51 0.033(3) 0.038(3) 0.033(3) 0.004(2) 0.011(2) 0.009(3) C52 0.045(4) 0.036(3) 0.030(3) -0.001(2) 0.007(3) 0.005(3) C53 0.044(4) 0.043(3) 0.030(3) -0.005(3) 0.001(3) -0.001(3) C54 0.032(3) 0.048(4) 0.030(3) -0.002(3) -0.001(2) 0.002(3) C55 0.035(3) 0.035(3) 0.027(3) -0.003(2) 0.003(2) 0.007(2) C57 0.039(4) 0.067(5) 0.048(4) -0.010(3) -0.006(3) 0.013(3) C60 0.029(3) 0.031(3) 0.028(3) 0.001(2) -0.001(2) 0.007(2) C61 0.034(3) 0.032(3) 0.025(3) 0.000(2) -0.002(2) 0.008(2) C62 0.032(3) 0.032(3) 0.040(3) 0.003(2) -0.007(3) 0.010(2) C63 0.027(3) 0.040(3) 0.051(4) 0.001(3) 0.002(3) 0.014(3) C64 0.034(3) 0.045(3) 0.038(3) 0.004(3) 0.006(3) 0.012(3) C65 0.030(3) 0.043(3) 0.031(3) 0.005(2) 0.000(2) 0.010(3) C67 0.037(4) 0.051(4) 0.050(4) 0.001(3) -0.003(3) 0.014(3) C24 0.065(5) 0.042(4) 0.064(5) -0.010(3) 0.008(4) -0.005(3) B1 0.037(4) 0.035(4) 0.036(4) 0.000(3) -0.003(3) 0.005(3) B2 0.025(3) 0.035(3) 0.024(3) 0.000(3) -0.001(3) 0.008(3) N1 0.044(3) 0.046(3) 0.034(3) 0.000(2) 0.002(2) 0.003(2) N2 0.040(3) 0.037(3) 0.044(3) 0.005(2) -0.005(2) 0.005(2) N3 0.035(3) 0.034(3) 0.033(3) 0.000(2) 0.001(2) 0.004(2) N4 0.037(3) 0.040(3) 0.035(3) 0.005(2) 0.004(2) 0.004(2) N5 0.034(3) 0.029(2) 0.038(3) 0.002(2) -0.001(2) 0.002(2) N6 0.038(3) 0.040(3) 0.060(4) 0.003(2) 0.007(3) 0.002(2) F1 0.074(3) 0.108(3) 0.028(2) 0.001(2) 0.0124(19) 0.040(3) F2 0.036(2) 0.103(3) 0.046(2) -0.011(2) 0.0007(17) 0.021(2) F3 0.071(3) 0.056(3) 0.086(3) -0.017(2) 0.033(2) 0.007(2) F4 0.134(5) 0.073(3) 0.167(6) 0.073(4) 0.069(5) 0.023(3) F5 0.146(5) 0.067(3) 0.120(5) 0.016(3) -0.074(4) 0.031(3) F6 0.210(7) 0.052(3) 0.066(3) 0.012(2) 0.014(4) 0.056(3) F7 0.178(6) 0.077(3) 0.073(3) -0.029(3) 0.037(4) -0.014(4) F8 0.164(6) 0.040(2) 0.080(3) 0.000(2) -0.001(3) 0.008(3) F9 0.103(5) 0.122(5) 0.239(9) -0.122(6) -0.108(5) 0.052(4) C47 0.095(7) 0.046(4) 0.076(6) 0.030(4) -0.038(5) -0.003(4) F10A 0.135(5) 0.119(4) 0.050(2) 0.044(3) -0.014(3) 0.019(4) F11A 0.135(5) 0.119(4) 0.050(2) 0.044(3) -0.014(3) 0.019(4) F12A 0.135(5) 0.119(4) 0.050(2) 0.044(3) -0.014(3) 0.019(4) F10B 0.135(5) 0.119(4) 0.050(2) 0.044(3) -0.014(3) 0.019(4) F11B 0.135(5) 0.119(4) 0.050(2) 0.044(3) -0.014(3) 0.019(4) F12B 0.135(5) 0.119(4) 0.050(2) 0.044(3) -0.014(3) 0.019(4) C56 0.059(4) 0.038(4) 0.054(4) -0.010(3) 0.020(4) 0.004(3) F13A 0.107(3) 0.071(3) 0.117(4) -0.039(3) 0.020(3) 0.035(2) F14A 0.107(3) 0.071(3) 0.117(4) -0.039(3) 0.020(3) 0.035(2) F15A 0.107(3) 0.071(3) 0.117(4) -0.039(3) 0.020(3) 0.035(2) F13B 0.107(3) 0.071(3) 0.117(4) -0.039(3) 0.020(3) 0.035(2) F14B 0.107(3) 0.071(3) 0.117(4) -0.039(3) 0.020(3) 0.035(2) F15B 0.107(3) 0.071(3) 0.117(4) -0.039(3) 0.020(3) 0.035(2) F16 0.042(2) 0.128(4) 0.056(3) -0.026(3) -0.0034(19) 0.035(2) F17 0.040(3) 0.091(4) 0.212(7) -0.031(4) -0.023(3) 0.000(3) F18 0.073(3) 0.205(7) 0.051(3) 0.027(3) 0.004(2) 0.076(4) C66 0.033(3) 0.086(5) 0.052(4) 0.009(4) 0.009(3) 0.028(4) F19A 0.075(3) 0.118(4) 0.046(2) 0.000(3) 0.022(2) 0.034(3) F20A 0.075(3) 0.118(4) 0.046(2) 0.000(3) 0.022(2) 0.034(3) F21A 0.075(3) 0.118(4) 0.046(2) 0.000(3) 0.022(2) 0.034(3) F19B 0.075(3) 0.118(4) 0.046(2) 0.000(3) 0.022(2) 0.034(3) F20B 0.075(3) 0.118(4) 0.046(2) 0.000(3) 0.022(2) 0.034(3) F21B 0.075(3) 0.118(4) 0.046(2) 0.000(3) 0.022(2) 0.034(3) F22 0.069(3) 0.081(3) 0.046(2) -0.016(2) -0.020(2) 0.035(2) F23 0.041(2) 0.079(3) 0.069(3) 0.004(2) -0.0182(19) 0.006(2) F24 0.075(3) 0.048(2) 0.063(3) 0.0117(19) -0.020(2) 0.019(2) Nb1 0.0456(4) 0.0374(4) 0.0507(4) -0.0004(3) 0.0119(3) 0.0059(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.359(11) . ? C1 N1 1.366(8) . ? C1 C4 1.502(10) . ? C2 C3 1.381(10) . ? C2 H2 0.95 . ? C3 N2 1.357(8) . ? C3 C5 1.494(11) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 N4 1.343(8) . ? C6 C7 1.397(10) . ? C6 C9 1.491(9) . ? C7 C8 1.379(9) . ? C7 H7 0.95 . ? C8 N3 1.362(8) . ? C8 C10 1.483(10) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 N6 1.364(8) . ? C11 C12 1.370(10) . ? C11 C14 1.519(10) . ? C12 C13 1.371(10) . ? C12 H12 0.95 . ? C13 N5 1.361(8) . ? C13 C15 1.474(9) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17 1.424(12) . ? C16 O1 1.464(9) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? O1 C18A 1.478(15) . ? O1 C18B 1.48(2) . ? O1 Nb1 2.186(5) . ? C18A C19A 1.51(2) . ? C18A H18A 0.99 . ? C18A H18B 0.99 . ? C19A H19A 0.98 . ? C19A H19B 0.98 . ? C19A H19C 0.98 . ? C18B C19B 1.52(2) . ? C18B H18C 0.99 . ? C18B H18D 0.99 . ? C19B H19D 0.98 . ? C19B H19E 0.98 . ? C19B H19F 0.98 . ? C20 C21 1.234(10) . ? C20 C22 1.484(11) . ? C20 Nb1 2.104(8) . ? C20 H20 1 . ? C21 C23 1.553(11) . ? C21 Nb1 2.047(7) . ? C21 H21 1 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.9802 . ? C23 H23B 0.9802 . ? C23 H23C 0.9802 . ? C30 C35 1.394(8) . ? C30 C31 1.395(8) . ? C30 B2 1.642(8) . ? C31 C32 1.390(8) . ? C31 H31 0.95 . ? C32 C33 1.378(8) . ? C32 C36 1.493(8) . ? C33 C34 1.386(9) . ? C33 H33 0.95 . ? C34 C35 1.389(8) . ? C34 C37 1.506(9) . ? C35 H35 0.95 . ? C36 F2 1.318(7) . ? C36 F1 1.336(7) . ? C36 F3 1.346(8) . ? C37 F6 1.293(8) . ? C37 F5 1.298(8) . ? C37 F4 1.315(9) . ? C40 C45 1.383(8) . ? C40 C41 1.414(8) . ? C40 B2 1.644(8) . ? C41 C42 1.394(9) . ? C41 H41 0.95 . ? C42 C43 1.383(9) . ? C42 C47 1.492(10) . ? C43 C44 1.385(9) . ? C43 H43 0.95 . ? C44 C45 1.384(8) . ? C44 C46 1.486(9) . ? C45 H45 0.95 . ? C46 F9 1.258(9) . ? C46 F8 1.316(8) . ? C46 F7 1.331(9) . ? C50 C51 1.389(8) . ? C50 C55 1.403(8) . ? C50 B2 1.642(8) . ? C51 C52 1.388(8) . ? C51 H51 0.95 . ? C52 C53 1.382(9) . ? C52 C56 1.456(9) . ? C53 C54 1.376(9) . ? C53 H53 0.95 . ? C54 C55 1.386(8) . ? C54 C57 1.502(9) . ? C55 H55 0.95 . ? C57 F16 1.305(8) . ? C57 F18 1.307(8) . ? C57 F17 1.333(9) . ? C60 C61 1.391(8) . ? C60 C65 1.394(8) . ? C60 B2 1.642(8) . ? C61 C62 1.384(8) . ? C61 H61 0.95 . ? C62 C63 1.387(9) . ? C62 C67 1.503(9) . ? C63 C64 1.388(9) . ? C63 H63 0.95 . ? C64 C65 1.379(8) . ? C64 C66 1.470(9) . ? C65 H65 0.95 . ? C67 F23 1.331(8) . ? C67 F22 1.330(8) . ? C67 F24 1.334(7) . ? C24 Nb1 2.182(7) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? B1 N5 1.527(8) . ? B1 N3 1.533(8) . ? B1 N2 1.535(8) . ? B1 H1 1 . ? N1 N2 1.379(7) . ? N1 Nb1 2.307(5) . ? N3 N4 1.381(7) . ? N4 Nb1 2.233(5) . ? N5 N6 1.358(7) . ? N6 Nb1 2.270(5) . ? C47 F12A 1.293(11) . ? C47 F11A 1.306(11) . ? C47 F10B 1.312(12) . ? C47 F11B 1.354(14) . ? C47 F10A 1.379(11) . ? C47 F12B 1.396(13) . ? C56 F15A 1.313(9) . ? C56 F13A 1.325(9) . ? C56 F13B 1.337(13) . ? C56 F14B 1.347(14) . ? C56 F15B 1.368(13) . ? C56 F14A 1.376(9) . ? C66 F20B 1.310(10) . ? C66 F21A 1.310(10) . ? C66 F19B 1.315(11) . ? C66 F19A 1.371(11) . ? C66 F20A 1.392(10) . ? C66 F21B 1.422(10) . ? 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 C2 C1 N1 109.7(6) . . ? C2 C1 C4 127.7(7) . . ? N1 C1 C4 122.5(7) . . ? C1 C2 C3 107.5(6) . . ? C1 C2 H2 126.3 . . ? C3 C2 H2 126.3 . . ? N2 C3 C2 107.3(6) . . ? N2 C3 C5 122.6(6) . . ? C2 C3 C5 130.0(7) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 C7 109.8(6) . . ? N4 C6 C9 124.0(6) . . ? C7 C6 C9 126.1(6) . . ? C8 C7 C6 106.2(6) . . ? C8 C7 H7 126.9 . . ? C6 C7 H7 126.9 . . ? N3 C8 C7 107.9(6) . . ? N3 C8 C10 123.5(6) . . ? C7 C8 C10 128.6(6) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 C12 109.0(6) . . ? N6 C11 C14 123.6(6) . . ? C12 C11 C14 127.5(7) . . ? C11 C12 C13 107.1(6) . . ? C11 C12 H12 126.5 . . ? C13 C12 H12 126.5 . . ? N5 C13 C12 107.7(6) . . ? N5 C13 C15 122.6(6) . . ? C12 C13 C15 129.7(6) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 O1 113.3(8) . . ? C17 C16 H16A 108.9 . . ? O1 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? O1 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 O1 C18A 107.6(9) . . ? C16 O1 C18B 121.7(16) . . ? C18A O1 C18B 35.0(13) . . ? C16 O1 Nb1 123.0(5) . . ? C18A O1 Nb1 123.9(8) . . ? C18B O1 Nb1 114.6(15) . . ? O1 C18A C19A 107.8(13) . . ? O1 C18A H18A 110.2 . . ? C19A C18A H18A 110.2 . . ? O1 C18A H18B 110.1 . . ? C19A C18A H18B 110.1 . . ? H18A C18A H18B 108.5 . . ? O1 C18B C19B 104.6(17) . . ? O1 C18B H18C 110.9 . . ? C19B C18B H18C 110.8 . . ? O1 C18B H18D 110.8 . . ? C19B C18B H18D 110.8 . . ? H18C C18B H18D 108.9 . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21 C20 C22 139.3(8) . . ? C21 C20 Nb1 70.2(5) . . ? C22 C20 Nb1 150.5(6) . . ? C21 C20 H20 90.4 . . ? C22 C20 H20 90.4 . . ? Nb1 C20 H20 90.4 . . ? C20 C21 C23 139.4(7) . . ? C20 C21 Nb1 75.3(5) . . ? C23 C21 Nb1 144.9(5) . . ? C20 C21 H21 92 . . ? C23 C21 H21 92 . . ? Nb1 C21 H21 92 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C35 C30 C31 115.8(5) . . ? C35 C30 B2 118.3(5) . . ? C31 C30 B2 125.8(5) . . ? C32 C31 C30 122.1(5) . . ? C32 C31 H31 118.9 . . ? C30 C31 H31 118.9 . . ? C33 C32 C31 121.0(5) . . ? C33 C32 C36 119.7(5) . . ? C31 C32 C36 119.2(5) . . ? C32 C33 C34 118.0(5) . . ? C32 C33 H33 121 . . ? C34 C33 H33 121 . . ? C33 C34 C35 120.7(5) . . ? C33 C34 C37 119.6(5) . . ? C35 C34 C37 119.7(6) . . ? C34 C35 C30 122.4(5) . . ? C34 C35 H35 118.8 . . ? C30 C35 H35 118.8 . . ? F2 C36 F1 106.2(5) . . ? F2 C36 F3 106.0(5) . . ? F1 C36 F3 105.2(5) . . ? F2 C36 C32 113.1(5) . . ? F1 C36 C32 113.4(5) . . ? F3 C36 C32 112.3(5) . . ? F6 C37 F5 108.9(7) . . ? F6 C37 F4 106.3(7) . . ? F5 C37 F4 102.9(7) . . ? F6 C37 C34 113.2(6) . . ? F5 C37 C34 113.0(6) . . ? F4 C37 C34 111.8(6) . . ? C45 C40 C41 115.9(5) . . ? C45 C40 B2 122.9(5) . . ? C41 C40 B2 120.9(5) . . ? C42 C41 C40 121.3(6) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C43 C42 C41 121.1(6) . . ? C43 C42 C47 119.9(6) . . ? C41 C42 C47 118.9(6) . . ? C42 C43 C44 118.2(6) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C45 C44 C43 120.6(6) . . ? C45 C44 C46 119.8(5) . . ? C43 C44 C46 119.6(6) . . ? C40 C45 C44 123.0(5) . . ? C40 C45 H45 118.5 . . ? C44 C45 H45 118.5 . . ? F9 C46 F8 109.1(7) . . ? F9 C46 F7 105.2(8) . . ? F8 C46 F7 101.8(6) . . ? F9 C46 C44 113.9(6) . . ? F8 C46 C44 114.5(6) . . ? F7 C46 C44 111.2(6) . . ? C51 C50 C55 116.3(5) . . ? C51 C50 B2 124.5(5) . . ? C55 C50 B2 119.0(5) . . ? C52 C51 C50 121.8(5) . . ? C52 C51 H51 119.1 . . ? C50 C51 H51 119.1 . . ? C53 C52 C51 120.9(5) . . ? C53 C52 C56 119.7(6) . . ? C51 C52 C56 119.4(6) . . ? C54 C53 C52 118.6(5) . . ? C54 C53 H53 120.7 . . ? C52 C53 H53 120.7 . . ? C53 C54 C55 120.5(6) . . ? C53 C54 C57 120.2(5) . . ? C55 C54 C57 119.2(5) . . ? C54 C55 C50 121.9(5) . . ? C54 C55 H55 119 . . ? C50 C55 H55 119 . . ? F16 C57 F18 107.3(6) . . ? F16 C57 F17 104.6(6) . . ? F18 C57 F17 106.0(6) . . ? F16 C57 C54 114.0(5) . . ? F18 C57 C54 112.9(6) . . ? F17 C57 C54 111.4(6) . . ? C61 C60 C65 115.7(5) . . ? C61 C60 B2 123.6(5) . . ? C65 C60 B2 120.6(5) . . ? C62 C61 C60 122.5(5) . . ? C62 C61 H61 118.7 . . ? C60 C61 H61 118.7 . . ? C61 C62 C63 120.4(5) . . ? C61 C62 C67 119.2(5) . . ? C63 C62 C67 120.4(5) . . ? C62 C63 C64 118.2(5) . . ? C62 C63 H63 120.9 . . ? C64 C63 H63 120.9 . . ? C65 C64 C63 120.4(5) . . ? C65 C64 C66 119.6(5) . . ? C63 C64 C66 120.0(5) . . ? C64 C65 C60 122.7(5) . . ? C64 C65 H65 118.6 . . ? C60 C65 H65 118.6 . . ? F23 C67 F22 106.5(5) . . ? F23 C67 F24 107.1(5) . . ? F22 C67 F24 105.8(5) . . ? F23 C67 C62 112.5(5) . . ? F22 C67 C62 112.9(5) . . ? F24 C67 C62 111.5(5) . . ? Nb1 C24 H24A 109.5 . . ? Nb1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Nb1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 B1 N3 109.4(5) . . ? N5 B1 N2 109.0(5) . . ? N3 B1 N2 109.2(5) . . ? N5 B1 H1 109.8 . . ? N3 B1 H1 109.7 . . ? N2 B1 H1 109.8 . . ? C60 B2 C50 111.9(4) . . ? C60 B2 C30 111.0(4) . . ? C50 B2 C30 104.1(4) . . ? C60 B2 C40 103.8(4) . . ? C50 B2 C40 111.3(4) . . ? C30 B2 C40 115.1(4) . . ? C1 N1 N2 106.1(5) . . ? C1 N1 Nb1 134.4(5) . . ? N2 N1 Nb1 119.6(4) . . ? C3 N2 N1 109.5(5) . . ? C3 N2 B1 130.2(6) . . ? N1 N2 B1 120.2(5) . . ? C8 N3 N4 109.3(5) . . ? C8 N3 B1 128.5(5) . . ? N4 N3 B1 122.2(5) . . ? C6 N4 N3 106.8(5) . . ? C6 N4 Nb1 133.5(4) . . ? N3 N4 Nb1 119.4(3) . . ? N6 N5 C13 109.3(5) . . ? N6 N5 B1 119.9(5) . . ? C13 N5 B1 130.7(5) . . ? N5 N6 C11 107.0(5) . . ? N5 N6 Nb1 121.3(4) . . ? C11 N6 Nb1 131.6(4) . . ? F12A C47 F11A 100.5(10) . . ? F12A C47 F10B 73.5(10) . . ? F11A C47 F10B 117.0(12) . . ? F12A C47 F11B 123.2(12) . . ? F11A C47 F11B 24.1(11) . . ? F10B C47 F11B 112.4(12) . . ? F12A C47 F10A 107.2(8) . . ? F11A C47 F10A 104.7(9) . . ? F10B C47 F10A 34.3(8) . . ? F11B C47 F10A 88.8(11) . . ? F12A C47 F12B 31.6(8) . . ? F11A C47 F12B 78.9(10) . . ? F10B C47 F12B 103.8(12) . . ? F11B C47 F12B 103.0(13) . . ? F10A C47 F12B 135.4(9) . . ? F12A C47 C42 116.6(7) . . ? F11A C47 C42 118.7(7) . . ? F10B C47 C42 119.3(9) . . ? F11B C47 C42 108.5(9) . . ? F10A C47 C42 108.0(8) . . ? F12B C47 C42 108.5(8) . . ? F15A C56 F13A 115.1(7) . . ? F15A C56 F13B 124.9(10) . . ? F13A C56 F13B 56.6(10) . . ? F15A C56 F14B 30.6(10) . . ? F13A C56 F14B 125.9(10) . . ? F13B C56 F14B 103.9(13) . . ? F15A C56 F15B 63.2(9) . . ? F13A C56 F15B 63.7(9) . . ? F13B C56 F15B 115.7(12) . . ? F14B C56 F15B 91.8(13) . . ? F15A C56 F14A 92.0(7) . . ? F13A C56 F14A 102.4(7) . . ? F13B C56 F14A 49.0(10) . . ? F14B C56 F14A 62.4(11) . . ? F15B C56 F14A 136.8(9) . . ? F15A C56 C52 114.8(6) . . ? F13A C56 C52 116.4(6) . . ? F13B C56 C52 115.8(8) . . ? F14B C56 C52 117.3(10) . . ? F15B C56 C52 110.0(8) . . ? F14A C56 C52 112.5(6) . . ? F20B C66 F21A 61.1(7) . . ? F20B C66 F19B 113.8(8) . . ? F21A C66 F19B 114.5(10) . . ? F20B C66 F19A 132.8(8) . . ? F21A C66 F19A 110.2(8) . . ? F19B C66 F19A 22.3(8) . . ? F20B C66 F20A 47.5(6) . . ? F21A C66 F20A 104.2(8) . . ? F19B C66 F20A 78.9(8) . . ? F19A C66 F20A 101.2(8) . . ? F20B C66 F21B 96.1(7) . . ? F21A C66 F21B 35.0(6) . . ? F19B C66 F21B 99.3(9) . . ? F19A C66 F21B 84.9(8) . . ? F20A C66 F21B 134.6(7) . . ? F20B C66 C64 114.6(6) . . ? F21A C66 C64 119.2(6) . . ? F19B C66 C64 119.8(7) . . ? F19A C66 C64 109.4(7) . . ? F20A C66 C64 111.0(6) . . ? F21B C66 C64 108.9(6) . . ? C21 Nb1 C20 34.5(3) . . ? C21 Nb1 C24 105.6(3) . . ? C20 Nb1 C24 84.0(3) . . ? C21 Nb1 O1 108.3(2) . . ? C20 Nb1 O1 90.9(2) . . ? C24 Nb1 O1 108.9(2) . . ? C21 Nb1 N4 84.6(2) . . ? C20 Nb1 N4 108.5(2) . . ? C24 Nb1 N4 82.8(2) . . ? O1 Nb1 N4 158.55(19) . . ? C21 Nb1 N6 85.3(2) . . ? C20 Nb1 N6 113.6(3) . . ? C24 Nb1 N6 158.3(2) . . ? O1 Nb1 N6 84.5(2) . . ? N4 Nb1 N6 79.53(19) . . ? C21 Nb1 N1 163.0(2) . . ? C20 Nb1 N1 162.0(3) . . ? C24 Nb1 N1 82.5(3) . . ? O1 Nb1 N1 82.31(19) . . ? N4 Nb1 N1 81.51(18) . . ? N6 Nb1 N1 82.50(19) . . ?