# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p21n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H31 N Nb0.18 P Ta0.82' _chemical_formula_weight 481.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8981(2) _cell_length_b 14.3944(3) _cell_length_c 16.7428(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.847(2) _cell_angle_gamma 90.00 _cell_volume 2124.38(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6409 _cell_measurement_theta_min 2.7041 _cell_measurement_theta_max 32.5896 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 961 _exptl_absorpt_coefficient_mu 4.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.56437 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29002 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6190 _reflns_number_gt 4869 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0570P)^2^+8.7132P] 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 6190 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Ta1 Ta -0.27037(3) 0.423039(19) 0.65481(2) 0.01893(9) Uani 0.82 1 d P A 1 Nb1 Nb -0.2408(3) 0.41638(19) 0.62908(19) 0.0115(6) Uiso 0.18 1 d P A 2 P1 P -0.48731(19) 0.33510(11) 0.70037(10) 0.0307(3) Uani 1 1 d . . . N1 N -0.1386(6) 0.3358(4) 0.6983(3) 0.0297(11) Uani 1 1 d . . . C1 C -0.1174(8) 0.5616(5) 0.6523(5) 0.0383(15) Uani 1 1 d . . . H1A H -0.0359 0.5819 0.6959 0.046 Uiso 1 1 calc R A 1 C2 C -0.0955(7) 0.5081(5) 0.5838(4) 0.035 Uani 1 1 d . A . H2A H 0.0041 0.4845 0.5710 0.042 Uiso 1 1 calc R B 1 C3 C -0.2335(7) 0.5061(5) 0.5314(4) 0.037 Uani 1 1 d . . . H3A H -0.2484 0.4794 0.4758 0.044 Uiso 1 1 calc R A 1 C4 C -0.3419(7) 0.5613(4) 0.5665(4) 0.033 Uani 1 1 d . A . H4A H -0.4466 0.5773 0.5404 0.040 Uiso 1 1 calc R C 1 C5 C -0.2717(7) 0.5949(5) 0.6407(4) 0.031 Uani 1 1 d . A . H5A H -0.3167 0.6400 0.6763 0.037 Uiso 1 1 calc R D 1 C6 C -0.0311(5) 0.2727(4) 0.7342(3) 0.019 Uani 1 1 d . A . C7 C 0.0339(6) 0.2863(4) 0.8149(3) 0.021 Uani 1 1 d . . . C8 C 0.1406(6) 0.2214(4) 0.8503(4) 0.028 Uani 1 1 d . A . H8A H 0.1846 0.2295 0.9048 0.034 Uiso 1 1 calc R . . C9 C 0.1829(7) 0.1457(5) 0.8072(4) 0.033 Uani 1 1 d . . . H9A H 0.2577 0.1036 0.8316 0.039 Uiso 1 1 calc R A . C10 C 0.1156(6) 0.1314(4) 0.7281(4) 0.029 Uani 1 1 d . A . H10A H 0.1430 0.0784 0.6994 0.035 Uiso 1 1 calc R . . C11 C 0.0078(6) 0.1940(4) 0.6898(3) 0.024 Uani 1 1 d . . . C12 C -0.0085(6) 0.3703(4) 0.8618(4) 0.027 Uani 1 1 d . A . H12A H -0.1103 0.3921 0.8359 0.032 Uiso 1 1 calc R . . C13 C -0.0209(8) 0.3489(5) 0.9504(4) 0.040 Uani 1 1 d . . . H13A H -0.0936 0.2983 0.9534 0.060 Uiso 1 1 calc R A . H13B H -0.0556 0.4044 0.9764 0.060 Uiso 1 1 calc R . . H13C H 0.0787 0.3302 0.9782 0.060 Uiso 1 1 calc R . . C14 C 0.1043(7) 0.4496(5) 0.8555(4) 0.031 Uani 1 1 d . . . H14A H 0.1103 0.4627 0.7986 0.047 Uiso 1 1 calc R A . H14B H 0.2047 0.4313 0.8825 0.047 Uiso 1 1 calc R . . H14C H 0.0702 0.5053 0.8814 0.047 Uiso 1 1 calc R . . C15 C -0.0647(7) 0.1784(4) 0.6043(4) 0.029 Uani 1 1 d . A . H15A H -0.1667 0.2087 0.5988 0.035 Uiso 1 1 calc R . . C16 C -0.0916(9) 0.0766(5) 0.5830(5) 0.045 Uani 1 1 d . . . H16A H -0.1496 0.0477 0.6222 0.068 Uiso 1 1 calc R A . H16B H 0.0061 0.0448 0.5844 0.068 Uiso 1 1 calc R . . H16C H -0.1487 0.0715 0.5289 0.068 Uiso 1 1 calc R . . C17 C 0.0242(9) 0.2269(6) 0.5446(5) 0.047 Uani 1 1 d . . . H17A H 0.0398 0.2922 0.5601 0.070 Uiso 1 1 calc R A . H17B H -0.0328 0.2232 0.4903 0.070 Uiso 1 1 calc R . . H17C H 0.1228 0.1964 0.5451 0.070 Uiso 1 1 calc R . . C18 C -0.4767(8) 0.3219(5) 0.8089(4) 0.038 Uani 1 1 d . A . H18A H -0.5653 0.2872 0.8214 0.057 Uiso 1 1 calc R . . H18B H -0.4750 0.3834 0.8341 0.057 Uiso 1 1 calc R . . H18C H -0.3840 0.2881 0.8297 0.057 Uiso 1 1 calc R . . C19 C -0.5041(7) 0.2155(5) 0.6660(4) 0.035 Uani 1 1 d . A . H19A H -0.5908 0.1862 0.6864 0.053 Uiso 1 1 calc R . . H19B H -0.4111 0.1817 0.6862 0.053 Uiso 1 1 calc R . . H19C H -0.5196 0.2142 0.6069 0.053 Uiso 1 1 calc R . . C20 C -0.6767(7) 0.3807(5) 0.6720(4) 0.036 Uani 1 1 d . A . H20A H -0.7503 0.3404 0.6937 0.054 Uiso 1 1 calc R . . H20B H -0.6996 0.3828 0.6131 0.054 Uiso 1 1 calc R . . H20C H -0.6828 0.4435 0.6939 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.02042(14) 0.01846(14) 0.01834(16) 0.00242(11) 0.00419(11) 0.00325(10) P1 0.0368(8) 0.0274(8) 0.0277(8) -0.0003(6) 0.0032(6) 0.0041(6) N1 0.034(3) 0.026(3) 0.028(3) 0.000(2) -0.001(2) -0.001(2) C1 0.034(3) 0.033(3) 0.047(4) 0.001(3) 0.000(3) -0.008(3) C2 0.035 0.035 0.035 0.000 0.005 0.000 C3 0.037 0.037 0.037 0.000 0.005 0.000 C4 0.033 0.033 0.033 0.000 0.005 0.000 C5 0.031 0.031 0.031 0.000 0.004 0.000 C6 0.019 0.019 0.019 0.000 0.003 0.000 C7 0.021 0.021 0.021 0.000 0.003 0.000 C8 0.028 0.028 0.028 0.000 0.004 0.000 C9 0.033 0.033 0.033 0.000 0.004 0.000 C10 0.029 0.029 0.029 0.000 0.004 0.000 C11 0.024 0.024 0.024 0.000 0.003 0.000 C12 0.027 0.027 0.027 0.000 0.004 0.000 C13 0.040 0.040 0.040 0.000 0.006 0.000 C14 0.031 0.031 0.031 0.000 0.004 0.000 C15 0.029 0.029 0.029 0.000 0.004 0.000 C16 0.045 0.045 0.045 0.000 0.006 0.000 C17 0.047 0.047 0.047 0.000 0.006 0.000 C18 0.038 0.038 0.038 0.000 0.005 0.000 C19 0.035 0.035 0.035 0.000 0.005 0.000 C20 0.036 0.036 0.036 0.000 0.005 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N1 1.802(5) . ? Ta1 C2 2.416(7) . ? Ta1 C1 2.417(6) . ? Ta1 C3 2.448(7) . ? Ta1 C5 2.485(6) . ? Ta1 C4 2.510(7) . ? Ta1 P1 2.5125(18) . ? Nb1 N1 1.796(6) . ? Nb1 C2 2.063(7) . ? Nb1 C3 2.092(8) . ? Nb1 C1 2.368(7) . ? Nb1 C4 2.450(7) . ? Nb1 C5 2.595(7) . ? Nb1 P1 2.885(4) . ? P1 C20 1.810(7) . ? P1 C19 1.814(7) . ? P1 C18 1.816(7) . ? N1 C6 1.395(7) . ? C1 C2 1.417(10) . ? C1 C5 1.442(9) . ? C1 H1A 1.0000 . ? C2 C3 1.408(9) . ? C2 H2A 1.0000 . ? C3 C4 1.436(9) . ? C3 H3A 1.0000 . ? C4 C5 1.399(9) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 C7 1.409(7) . ? C6 C11 1.424(7) . ? C7 C8 1.403(8) . ? C7 C12 1.517(8) . ? C8 C9 1.388(9) . ? C8 H8A 0.9500 . ? C9 C10 1.392(9) . ? C9 H9A 0.9500 . ? C10 C11 1.405(8) . ? C10 H10A 0.9500 . ? C11 C15 1.506(8) . ? C12 C14 1.532(8) . ? C12 C13 1.535(9) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.519(9) . ? C15 C17 1.525(10) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 N1 Ta1 C2 97.2(2) . . ? N1 Ta1 C1 104.2(2) . . ? C2 Ta1 C1 34.1(2) . . ? N1 Ta1 C3 121.8(2) . . ? C2 Ta1 C3 33.6(2) . . ? C1 Ta1 C3 56.1(2) . . ? N1 Ta1 C5 136.6(2) . . ? C2 Ta1 C5 56.2(2) . . ? C1 Ta1 C5 34.2(2) . . ? C3 Ta1 C5 55.5(2) . . ? N1 Ta1 C4 152.8(2) . . ? C2 Ta1 C4 55.7(2) . . ? C1 Ta1 C4 55.5(2) . . ? C3 Ta1 C4 33.7(2) . . ? C5 Ta1 C4 32.5(2) . . ? N1 Ta1 P1 90.62(17) . . ? C2 Ta1 P1 167.88(16) . . ? C1 Ta1 P1 151.44(18) . . ? C3 Ta1 P1 134.40(16) . . ? C5 Ta1 P1 122.44(15) . . ? C4 Ta1 P1 115.78(16) . . ? N1 Nb1 C2 111.3(3) . . ? N1 Nb1 C3 146.7(3) . . ? C2 Nb1 C3 39.6(3) . . ? N1 Nb1 C1 106.3(3) . . ? C2 Nb1 C1 36.5(3) . . ? C3 Nb1 C1 61.3(3) . . ? N1 Nb1 C4 161.7(3) . . ? C2 Nb1 C4 60.6(3) . . ? C3 Nb1 C4 35.8(2) . . ? C1 Nb1 C4 56.9(2) . . ? N1 Nb1 C5 129.8(3) . . ? C2 Nb1 C5 58.1(2) . . ? C3 Nb1 C5 57.5(2) . . ? C1 Nb1 C5 33.4(2) . . ? C4 Nb1 C5 32.0(2) . . ? N1 Nb1 P1 79.5(2) . . ? C2 Nb1 P1 164.1(2) . . ? C3 Nb1 P1 132.9(2) . . ? C1 Nb1 P1 130.7(2) . . ? C4 Nb1 P1 105.47(19) . . ? C5 Nb1 P1 106.03(18) . . ? C20 P1 C19 103.1(3) . . ? C20 P1 C18 102.7(3) . . ? C19 P1 C18 102.1(3) . . ? C20 P1 Ta1 117.7(2) . . ? C19 P1 Ta1 114.5(2) . . ? C18 P1 Ta1 114.8(2) . . ? C20 P1 Nb1 118.5(2) . . ? C19 P1 Nb1 106.7(2) . . ? C18 P1 Nb1 121.2(2) . . ? Ta1 P1 Nb1 8.43(6) . . ? C6 N1 Nb1 162.9(5) . . ? C6 N1 Ta1 176.5(4) . . ? Nb1 N1 Ta1 17.36(11) . . ? C2 C1 C5 107.8(6) . . ? C2 C1 Nb1 60.0(4) . . ? C5 C1 Nb1 82.0(4) . . ? C2 C1 Ta1 72.9(4) . . ? C5 C1 Ta1 75.5(4) . . ? Nb1 C1 Ta1 12.98(9) . . ? C2 C1 H1A 125.7 . . ? C5 C1 H1A 125.7 . . ? Nb1 C1 H1A 130.7 . . ? Ta1 C1 H1A 125.7 . . ? C3 C2 C1 108.1(6) . . ? C3 C2 Nb1 71.3(4) . . ? C1 C2 Nb1 83.5(4) . . ? C3 C2 Ta1 74.4(4) . . ? C1 C2 Ta1 73.0(4) . . ? Nb1 C2 Ta1 10.60(10) . . ? C3 C2 H2A 125.6 . . ? C1 C2 H2A 125.6 . . ? Nb1 C2 H2A 118.6 . . ? Ta1 C2 H2A 125.6 . . ? C2 C3 C4 108.1(6) . . ? C2 C3 Nb1 69.1(4) . . ? C4 C3 Nb1 85.9(4) . . ? C2 C3 Ta1 72.0(4) . . ? C4 C3 Ta1 75.5(4) . . ? Nb1 C3 Ta1 10.40(10) . . ? C2 C3 H3A 125.6 . . ? C4 C3 H3A 125.6 . . ? Nb1 C3 H3A 118.5 . . ? Ta1 C3 H3A 125.6 . . ? C5 C4 C3 108.1(6) . . ? C5 C4 Nb1 79.7(4) . . ? C3 C4 Nb1 58.4(4) . . ? C5 C4 Ta1 72.8(4) . . ? C3 C4 Ta1 70.8(4) . . ? Nb1 C4 Ta1 12.50(8) . . ? C5 C4 H4A 125.9 . . ? C3 C4 H4A 125.9 . . ? Nb1 C4 H4A 130.4 . . ? Ta1 C4 H4A 125.9 . . ? C4 C5 C1 107.8(6) . . ? C4 C5 Ta1 74.7(4) . . ? C1 C5 Ta1 70.3(4) . . ? C4 C5 Nb1 68.3(4) . . ? C1 C5 Nb1 64.6(4) . . ? Ta1 C5 Nb1 12.03(8) . . ? C4 C5 H5A 125.9 . . ? C1 C5 H5A 125.9 . . ? Ta1 C5 H5A 125.9 . . ? Nb1 C5 H5A 137.9 . . ? N1 C6 C7 119.4(5) . . ? N1 C6 C11 119.7(5) . . ? C7 C6 C11 120.9(5) . . ? C8 C7 C6 118.6(5) . . ? C8 C7 C12 120.9(5) . . ? C6 C7 C12 120.5(5) . . ? C9 C8 C7 121.3(6) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C8 C9 C10 119.9(6) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 C11 121.1(6) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C10 C11 C6 118.2(5) . . ? C10 C11 C15 121.0(5) . . ? C6 C11 C15 120.8(5) . . ? C7 C12 C14 110.3(5) . . ? C7 C12 C13 113.3(5) . . ? C14 C12 C13 110.5(5) . . ? C7 C12 H12A 107.5 . . ? C14 C12 H12A 107.5 . . ? C13 C12 H12A 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 113.5(5) . . ? C11 C15 C17 111.2(5) . . ? C16 C15 C17 111.6(6) . . ? C11 C15 H15A 106.7 . . ? C16 C15 H15A 106.7 . . ? C17 C15 H15A 106.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P1 C18 H18A 109.5 . . ? P1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P1 C19 H19A 109.5 . . ? P1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P1 C20 H20A 109.5 . . ? P1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.888 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.198 _database_code_depnum_ccdc_archive 'CCDC 960155' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_xx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H52 B2 N2 Nb2' _chemical_formula_sum 'C34 H52 B2 N2 Nb2' _chemical_formula_weight 696.22 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' 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6798(2) _cell_length_b 20.3557(5) _cell_length_c 15.7752(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.568(1) _cell_angle_gamma 90.00 _cell_volume 3406.9(1) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8094 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 30.39 _exptl_crystal_description red _exptl_crystal_colour block _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51133 _exptl_absorpt_correction_T_max 0.63503 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22730 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7437 _reflns_number_gt 6366 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0283P)^2^+4.7322P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7437 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.06175(2) 0.118306(11) 0.376298(14) 0.01853(7) Uani 1 1 d . . . Nb2 Nb -0.08827(2) 0.208152(11) 0.285737(14) 0.01722(7) Uani 1 1 d . . . N1 N 0.0943(2) 0.18856(11) 0.28946(13) 0.0193(4) Uani 1 1 d . . . N2 N -0.1272(2) 0.12206(10) 0.33678(14) 0.0191(4) Uani 1 1 d . . . B1 B 0.1467(4) 0.01460(17) 0.3319(2) 0.0320(7) Uani 1 1 d . . . B2 B -0.1228(3) 0.30115(15) 0.3832(2) 0.0222(6) Uani 1 1 d . . . C1 C 0.2017(3) 0.17199(18) 0.48365(19) 0.0363(7) Uani 1 1 d . . . C2 C 0.0752(3) 0.18264(16) 0.49991(18) 0.0323(7) Uani 1 1 d . . . C3 C 0.0267(3) 0.12092(16) 0.52413(18) 0.0307(6) Uani 1 1 d . . . C4 C 0.1225(3) 0.07414(16) 0.52213(18) 0.0320(7) Uani 1 1 d . . . C5 C 0.2299(3) 0.10584(18) 0.4970(2) 0.0346(7) Uani 1 1 d . . . C6 C -0.1536(3) 0.18224(14) 0.14190(17) 0.0244(6) Uani 1 1 d . . . C7 C -0.2676(3) 0.19428(15) 0.17793(18) 0.0267(6) Uani 1 1 d . . . C8 C -0.2690(3) 0.26111(15) 0.19909(18) 0.0269(6) Uani 1 1 d . . . C9 C -0.1587(3) 0.29108(14) 0.17426(18) 0.0257(6) Uani 1 1 d . . . C10 C -0.0877(3) 0.24254(15) 0.13830(18) 0.0267(6) Uani 1 1 d . . . C11 C -0.2338(2) 0.08007(13) 0.33919(17) 0.0208(5) Uani 1 1 d . . . C12 C -0.2541(3) 0.02617(13) 0.28243(18) 0.0240(5) Uani 1 1 d . . . C13 C -0.3597(3) -0.01388(15) 0.2871(2) 0.0302(6) Uani 1 1 d . . . C14 C -0.4437(3) -0.00302(16) 0.3460(2) 0.0340(7) Uani 1 1 d . . . C15 C -0.4238(3) 0.04962(16) 0.4007(2) 0.0318(6) Uani 1 1 d . . . C16 C -0.3221(3) 0.09259(13) 0.39824(18) 0.0244(6) Uani 1 1 d . . . C17 C -0.3170(3) 0.15445(14) 0.45304(18) 0.0241(6) Uani 1 1 d . . . C18 C -0.1692(3) 0.00926(14) 0.21427(19) 0.0288(6) Uani 1 1 d . . . C19 C -0.4117(3) 0.20477(16) 0.4104(2) 0.0309(6) Uani 1 1 d . . . C20 C -0.3440(3) 0.14298(17) 0.5450(2) 0.0318(6) Uani 1 1 d . . . C21 C -0.1138(4) -0.06048(16) 0.2274(2) 0.0370(7) Uani 1 1 d . . . C22 C -0.2397(4) 0.01497(18) 0.1237(2) 0.0384(8) Uani 1 1 d . . . C23 C 0.1986(2) 0.21068(14) 0.24769(16) 0.0216(5) Uani 1 1 d . . . C24 C 0.2392(3) 0.17426(15) 0.17937(17) 0.0260(6) Uani 1 1 d . . . C25 C 0.3414(3) 0.19873(18) 0.1402(2) 0.0351(7) Uani 1 1 d . . . C26 C 0.4028(3) 0.25574(19) 0.1669(2) 0.0377(8) Uani 1 1 d . . . C27 C 0.3623(3) 0.29099(18) 0.2334(2) 0.0344(7) Uani 1 1 d . . . C28 C 0.2602(3) 0.27006(15) 0.27439(17) 0.0256(6) Uani 1 1 d . . . C29 C 0.1799(3) 0.11098(15) 0.14390(19) 0.0300(6) Uani 1 1 d . . . C30 C 0.2159(3) 0.31458(15) 0.34246(19) 0.0267(6) Uani 1 1 d . . . C31 C 0.2754(4) 0.05481(19) 0.1476(3) 0.0451(9) Uani 1 1 d . . . C32 C 0.1179(3) 0.11874(16) 0.05094(19) 0.0307(6) Uani 1 1 d . . . C33 C 0.3222(3) 0.33735(19) 0.4095(2) 0.0365(7) Uani 1 1 d . . . C34 C 0.1491(3) 0.37530(17) 0.2990(2) 0.0369(7) Uani 1 1 d . . . H1A H 0.050(3) 0.0219(17) 0.365(2) 0.031(9) Uiso 1 1 d . . . H1B H 0.192(3) 0.0705(17) 0.326(2) 0.032(9) Uiso 1 1 d . . . H1C H 0.130(3) -0.0016(16) 0.269(2) 0.030(8) Uiso 1 1 d . . . H1D H 0.209(3) -0.0146(18) 0.377(2) 0.038(9) Uiso 1 1 d . . . H2A H -0.043(4) 0.2971(18) 0.335(2) 0.045(10) Uiso 1 1 d . . . H2B H -0.178(3) 0.2533(16) 0.3702(19) 0.025(8) Uiso 1 1 d . . . H2C H -0.173(3) 0.3427(18) 0.364(2) 0.036(9) Uiso 1 1 d . . . H2D H -0.079(3) 0.3034(16) 0.442(2) 0.032(9) Uiso 1 1 d . . . H1 H 0.240(3) 0.2060(16) 0.465(2) 0.025(8) Uiso 1 1 d . . . H2 H 0.034(3) 0.2218(19) 0.500(2) 0.037(10) Uiso 1 1 d . . . H3 H -0.056(4) 0.1126(18) 0.538(2) 0.040(10) Uiso 1 1 d . . . H4 H 0.119(3) 0.0283(19) 0.534(2) 0.038(9) Uiso 1 1 d . . . H5 H 0.305(4) 0.084(2) 0.487(3) 0.052(11) Uiso 1 1 d . . . H6 H -0.126(3) 0.1444(18) 0.121(2) 0.036(9) Uiso 1 1 d . . . H7 H -0.328(3) 0.1631(17) 0.186(2) 0.033(9) Uiso 1 1 d . . . H8 H -0.327(3) 0.2796(17) 0.225(2) 0.033(9) Uiso 1 1 d . . . H9 H -0.136(3) 0.3364(18) 0.182(2) 0.033(9) Uiso 1 1 d . . . H10 H -0.012(3) 0.2474(17) 0.117(2) 0.035(9) Uiso 1 1 d . . . H13 H -0.370(3) -0.0470(17) 0.251(2) 0.027(8) Uiso 1 1 d . . . H14 H -0.513(3) -0.0291(17) 0.349(2) 0.030(8) Uiso 1 1 d . . . H15 H -0.476(3) 0.0572(15) 0.441(2) 0.021(8) Uiso 1 1 d . . . H17 H -0.232(3) 0.1711(15) 0.4555(19) 0.024(8) Uiso 1 1 d . . . H18 H -0.104(2) 0.0399(13) 0.2190(16) 0.006(6) Uiso 1 1 d . . . H25 H 0.368(4) 0.177(2) 0.096(3) 0.049(11) Uiso 1 1 d . . . H26 H 0.478(4) 0.271(2) 0.140(3) 0.050(11) Uiso 1 1 d . . . H27 H 0.399(3) 0.3308(16) 0.252(2) 0.024(8) Uiso 1 1 d . . . H29 H 0.119(3) 0.0999(17) 0.179(2) 0.031(9) Uiso 1 1 d . . . H30 H 0.156(3) 0.2949(15) 0.374(2) 0.026(8) Uiso 1 1 d . . . H19A H -0.401(3) 0.2119(16) 0.351(2) 0.033(9) Uiso 1 1 d . . . H19B H -0.406(4) 0.248(2) 0.440(3) 0.048(11) Uiso 1 1 d . . . H19C H -0.496(4) 0.1891(18) 0.415(2) 0.038(9) Uiso 1 1 d . . . H20A H -0.432(3) 0.1297(17) 0.549(2) 0.035(9) Uiso 1 1 d . . . H20B H -0.336(3) 0.1831(19) 0.577(2) 0.038(10) Uiso 1 1 d . . . H20C H -0.289(4) 0.112(2) 0.572(3) 0.047(11) Uiso 1 1 d . . . H21A H -0.055(4) -0.0696(19) 0.184(3) 0.049(11) Uiso 1 1 d . . . H21B H -0.067(3) -0.0652(18) 0.284(2) 0.040(10) Uiso 1 1 d . . . H21C H -0.184(4) -0.094(2) 0.216(3) 0.054(12) Uiso 1 1 d . . . H22A H -0.301(4) -0.016(2) 0.114(2) 0.045(11) Uiso 1 1 d . . . H22B H -0.181(3) 0.0109(18) 0.080(2) 0.041(10) Uiso 1 1 d . . . H22C H -0.291(4) 0.058(2) 0.112(3) 0.053(11) Uiso 1 1 d . . . H31A H 0.232(3) 0.011(2) 0.129(2) 0.042(10) Uiso 1 1 d . . . H31B H 0.338(4) 0.0610(19) 0.108(3) 0.046(11) Uiso 1 1 d . . . H31C H 0.324(4) 0.049(2) 0.204(3) 0.057(12) Uiso 1 1 d . . . H32A H 0.062(3) 0.1546(15) 0.0453(18) 0.015(7) Uiso 1 1 d . . . H32B H 0.184(4) 0.1288(18) 0.016(2) 0.041(10) Uiso 1 1 d . . . H32C H 0.073(3) 0.0765(19) 0.032(2) 0.041(10) Uiso 1 1 d . . . H33A H 0.282(3) 0.3623(18) 0.454(2) 0.036(9) Uiso 1 1 d . . . H33B H 0.368(3) 0.3010(17) 0.438(2) 0.028(8) Uiso 1 1 d . . . H33C H 0.384(3) 0.3623(18) 0.384(2) 0.038(10) Uiso 1 1 d . . . H34A H 0.112(3) 0.3986(17) 0.340(2) 0.029(9) Uiso 1 1 d . . . H34B H 0.081(4) 0.3622(19) 0.256(2) 0.043(10) Uiso 1 1 d . . . H34C H 0.213(4) 0.403(2) 0.273(2) 0.047(11) Uiso 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 Nb1 0.01896(12) 0.01953(12) 0.01722(12) 0.00278(8) 0.00252(9) 0.00159(9) Nb2 0.01730(12) 0.01619(12) 0.01813(12) 0.00132(8) 0.00178(8) 0.00046(8) N1 0.0180(10) 0.0228(11) 0.0170(10) 0.0020(8) 0.0021(8) 0.0007(9) N2 0.0186(10) 0.0193(11) 0.0194(10) 0.0012(8) 0.0021(8) 0.0017(8) B1 0.0384(19) 0.0249(16) 0.0344(19) 0.0034(14) 0.0119(15) 0.0122(14) B2 0.0252(15) 0.0211(14) 0.0204(15) -0.0008(11) 0.0029(12) 0.0027(12) C1 0.0401(18) 0.0437(19) 0.0222(14) 0.0042(13) -0.0085(13) -0.0103(15) C2 0.0479(19) 0.0297(16) 0.0183(13) -0.0012(11) -0.0005(12) 0.0066(14) C3 0.0321(16) 0.0417(18) 0.0186(13) 0.0036(12) 0.0046(12) 0.0033(13) C4 0.0386(17) 0.0354(17) 0.0211(14) 0.0083(12) -0.0010(12) 0.0033(14) C5 0.0265(15) 0.050(2) 0.0249(15) 0.0074(14) -0.0053(12) 0.0053(14) C6 0.0288(14) 0.0243(14) 0.0191(13) 0.0008(11) -0.0006(11) 0.0005(11) C7 0.0240(14) 0.0309(15) 0.0229(14) 0.0034(11) -0.0065(11) -0.0020(12) C8 0.0250(14) 0.0296(15) 0.0245(14) 0.0018(11) -0.0039(11) 0.0092(12) C9 0.0309(15) 0.0223(14) 0.0223(13) 0.0042(11) -0.0037(11) 0.0012(11) C10 0.0298(15) 0.0297(15) 0.0201(13) 0.0050(11) -0.0003(11) -0.0015(12) C11 0.0204(12) 0.0187(12) 0.0228(13) 0.0057(10) -0.0002(10) 0.0007(10) C12 0.0252(13) 0.0190(13) 0.0267(14) 0.0019(11) -0.0014(11) -0.0027(11) C13 0.0331(16) 0.0214(14) 0.0343(16) 0.0022(12) -0.0033(12) -0.0051(12) C14 0.0286(15) 0.0293(16) 0.0439(18) 0.0058(13) 0.0026(13) -0.0103(13) C15 0.0270(15) 0.0321(16) 0.0373(17) 0.0026(13) 0.0084(13) -0.0045(12) C16 0.0231(13) 0.0214(13) 0.0286(14) 0.0064(11) 0.0022(11) 0.0019(11) C17 0.0223(13) 0.0224(13) 0.0289(14) 0.0022(11) 0.0084(11) 0.0013(11) C18 0.0349(16) 0.0223(14) 0.0298(15) -0.0051(11) 0.0060(12) -0.0063(12) C19 0.0251(15) 0.0305(16) 0.0378(18) 0.0039(13) 0.0065(13) 0.0054(12) C20 0.0308(16) 0.0349(17) 0.0306(16) 0.0033(13) 0.0082(13) 0.0013(14) C21 0.0461(19) 0.0248(15) 0.0398(19) -0.0073(13) 0.0037(16) 0.0029(14) C22 0.049(2) 0.0361(18) 0.0293(16) -0.0066(14) 0.0002(15) -0.0095(16) C23 0.0154(11) 0.0313(14) 0.0182(12) 0.0061(10) 0.0020(9) 0.0002(10) C24 0.0222(13) 0.0342(15) 0.0220(13) 0.0088(11) 0.0042(10) 0.0055(12) C25 0.0262(15) 0.055(2) 0.0248(15) 0.0109(14) 0.0080(12) 0.0110(14) C26 0.0201(14) 0.063(2) 0.0306(16) 0.0118(15) 0.0056(12) -0.0084(15) C27 0.0248(14) 0.048(2) 0.0295(16) 0.0114(14) -0.0025(12) -0.0136(14) C28 0.0205(13) 0.0337(15) 0.0217(13) 0.0079(11) -0.0016(10) -0.0039(11) C29 0.0356(16) 0.0311(15) 0.0248(14) 0.0046(12) 0.0102(12) 0.0090(13) C30 0.0229(13) 0.0284(15) 0.0282(14) 0.0021(11) 0.0003(11) -0.0091(12) C31 0.058(2) 0.0350(19) 0.045(2) 0.0057(16) 0.0202(19) 0.0210(18) C32 0.0362(16) 0.0322(16) 0.0244(15) -0.0041(12) 0.0062(13) 0.0030(14) C33 0.0326(16) 0.0429(19) 0.0321(17) 0.0031(15) -0.0044(14) -0.0104(15) C34 0.0385(18) 0.0308(17) 0.0404(19) 0.0064(14) 0.0001(15) -0.0061(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N1 2.037(2) . ? Nb1 N2 2.045(2) . ? Nb1 C2 2.340(3) . ? Nb1 C1 2.391(3) . ? Nb1 C3 2.404(3) . ? Nb1 B1 2.432(3) . ? Nb1 C5 2.476(3) . ? Nb1 C4 2.486(3) . ? Nb1 Nb2 2.7257(3) . ? Nb1 H1A 1.97(3) . ? Nb1 H1B 1.94(3) . ? Nb2 N1 1.984(2) . ? Nb2 N2 1.992(2) . ? Nb2 C6 2.356(3) . ? Nb2 C7 2.428(3) . ? Nb2 C10 2.430(3) . ? Nb2 C8 2.481(3) . ? Nb2 C9 2.491(3) . ? Nb2 B2 2.493(3) . ? Nb2 H2A 2.01(4) . ? Nb2 H2B 1.96(3) . ? N1 C23 1.430(3) . ? N2 C11 1.427(3) . ? B1 H1A 1.22(3) . ? B1 H1B 1.24(3) . ? B1 H1C 1.05(3) . ? B1 H1D 1.09(4) . ? B2 H2A 1.20(4) . ? B2 H2B 1.15(3) . ? B2 H2C 1.03(4) . ? B2 H2D 0.99(3) . ? C1 C5 1.391(5) . ? C1 C2 1.420(5) . ? C1 H1 0.87(3) . ? C2 C3 1.427(5) . ? C2 H2 0.91(4) . ? C3 C4 1.401(4) . ? C3 H3 0.95(4) . ? C4 C5 1.411(5) . ? C4 H4 0.95(4) . ? C5 H5 0.95(4) . ? C6 C10 1.419(4) . ? C6 C7 1.422(4) . ? C6 H6 0.90(4) . ? C7 C8 1.401(4) . ? C7 H7 0.93(4) . ? C8 C9 1.421(4) . ? C8 H8 0.86(4) . ? C9 C10 1.404(4) . ? C9 H9 0.96(4) . ? C10 H10 0.92(4) . ? C11 C12 1.417(4) . ? C11 C16 1.423(4) . ? C12 C13 1.400(4) . ? C12 C18 1.524(4) . ? C13 C14 1.381(5) . ? C13 H13 0.89(3) . ? C14 C15 1.377(5) . ? C14 H14 0.92(3) . ? C15 C16 1.399(4) . ? C15 H15 0.91(3) . ? C16 C17 1.525(4) . ? C17 C20 1.530(4) . ? C17 C19 1.539(4) . ? C17 H17 0.97(3) . ? C18 C22 1.542(4) . ? C18 C21 1.543(4) . ? C18 H18 0.93(3) . ? C19 H19A 0.97(4) . ? C19 H19B 0.99(4) . ? C19 H19C 0.97(4) . ? C20 H20A 0.99(4) . ? C20 H20B 0.96(4) . ? C20 H20C 0.93(4) . ? C21 H21A 1.00(4) . ? C21 H21B 0.98(4) . ? C21 H21C 1.01(4) . ? C22 H22A 0.92(4) . ? C22 H22B 0.99(4) . ? C22 H22C 1.03(4) . ? C23 C24 1.416(4) . ? C23 C28 1.417(4) . ? C24 C25 1.406(4) . ? C24 C29 1.514(4) . ? C25 C26 1.375(5) . ? C25 H25 0.91(4) . ? C26 C27 1.380(5) . ? C26 H26 1.01(4) . ? C27 C28 1.397(4) . ? C27 H27 0.93(3) . ? C28 C30 1.521(4) . ? C29 C31 1.529(4) . ? C29 C32 1.547(4) . ? C29 H29 0.93(3) . ? C30 C33 1.532(4) . ? C30 C34 1.547(4) . ? C30 H30 0.95(3) . ? C31 H31A 1.03(4) . ? C31 H31B 0.97(4) . ? C31 H31C 0.98(5) . ? C32 H32A 0.94(3) . ? C32 H32B 0.96(4) . ? C32 H32C 1.01(4) . ? C33 H33A 1.00(4) . ? C33 H33B 0.97(3) . ? C33 H33C 0.96(4) . ? C34 H34A 0.93(4) . ? C34 H34B 0.97(4) . ? C34 H34C 1.02(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Nb1 N2 90.41(9) . . ? N1 Nb1 C2 99.71(10) . . ? N2 Nb1 C2 101.39(10) . . ? N1 Nb1 C1 90.83(10) . . ? N2 Nb1 C1 135.57(11) . . ? C2 Nb1 C1 34.92(12) . . ? N1 Nb1 C3 133.95(10) . . ? N2 Nb1 C3 92.14(10) . . ? C2 Nb1 C3 34.98(11) . . ? C1 Nb1 C3 57.10(11) . . ? N1 Nb1 B1 108.51(10) . . ? N2 Nb1 B1 109.42(11) . . ? C2 Nb1 B1 137.44(12) . . ? C1 Nb1 B1 112.15(13) . . ? C3 Nb1 B1 113.78(12) . . ? N1 Nb1 C5 115.12(10) . . ? N2 Nb1 C5 147.35(10) . . ? C2 Nb1 C5 56.40(12) . . ? C1 Nb1 C5 33.15(12) . . ? C3 Nb1 C5 55.67(11) . . ? B1 Nb1 C5 82.58(13) . . ? N1 Nb1 C4 146.04(10) . . ? N2 Nb1 C4 116.09(10) . . ? C2 Nb1 C4 56.40(11) . . ? C1 Nb1 C4 55.53(11) . . ? C3 Nb1 C4 33.23(11) . . ? B1 Nb1 C4 83.46(12) . . ? C5 Nb1 C4 33.05(11) . . ? N1 Nb1 Nb2 46.52(6) . . ? N2 Nb1 Nb2 46.73(6) . . ? C2 Nb1 Nb2 92.16(8) . . ? C1 Nb1 Nb2 110.30(9) . . ? C3 Nb1 Nb2 110.26(8) . . ? B1 Nb1 Nb2 130.37(9) . . ? C5 Nb1 Nb2 143.41(9) . . ? C4 Nb1 Nb2 143.45(8) . . ? N1 Nb1 H1A 130.7(9) . . ? N2 Nb1 H1A 87.7(9) . . ? C2 Nb1 H1A 128.9(9) . . ? C1 Nb1 H1A 123.0(9) . . ? C3 Nb1 H1A 95.3(9) . . ? B1 Nb1 H1A 29.9(9) . . ? C5 Nb1 H1A 89.9(9) . . ? C4 Nb1 H1A 74.3(9) . . ? Nb2 Nb1 H1A 126.4(9) . . ? N1 Nb1 H1B 83.9(10) . . ? N2 Nb1 H1B 128.6(10) . . ? C2 Nb1 H1B 130.0(10) . . ? C1 Nb1 H1B 95.7(10) . . ? C3 Nb1 H1B 127.2(10) . . ? B1 Nb1 H1B 30.4(10) . . ? C5 Nb1 H1B 76.8(10) . . ? C4 Nb1 H1B 94.1(10) . . ? Nb2 Nb1 H1B 122.0(10) . . ? H1A Nb1 H1B 60.3(13) . . ? N1 Nb2 N2 93.51(9) . . ? N1 Nb2 C6 99.52(9) . . ? N2 Nb2 C6 98.03(9) . . ? N1 Nb2 C7 133.71(9) . . ? N2 Nb2 C7 89.79(10) . . ? C6 Nb2 C7 34.54(10) . . ? N1 Nb2 C10 88.65(9) . . ? N2 Nb2 C10 131.59(9) . . ? C6 Nb2 C10 34.46(10) . . ? C7 Nb2 C10 56.69(10) . . ? N1 Nb2 C8 143.48(10) . . ? N2 Nb2 C8 114.81(10) . . ? C6 Nb2 C8 55.97(10) . . ? C7 Nb2 C8 33.15(10) . . ? C10 Nb2 C8 55.54(10) . . ? N1 Nb2 C9 111.94(9) . . ? N2 Nb2 C9 145.20(9) . . ? C6 Nb2 C9 55.91(10) . . ? C7 Nb2 C9 55.52(10) . . ? C10 Nb2 C9 33.13(10) . . ? C8 Nb2 C9 33.20(10) . . ? N1 Nb2 B2 110.39(10) . . ? N2 Nb2 B2 111.47(10) . . ? C6 Nb2 B2 135.71(10) . . ? C7 Nb2 B2 111.11(10) . . ? C10 Nb2 B2 112.87(10) . . ? C8 Nb2 B2 81.34(10) . . ? C9 Nb2 B2 82.36(10) . . ? N1 Nb2 Nb1 48.16(6) . . ? N2 Nb2 Nb1 48.35(6) . . ? C6 Nb2 Nb1 116.50(7) . . ? C7 Nb2 Nb1 131.18(7) . . ? C10 Nb2 Nb1 129.01(7) . . ? C8 Nb2 Nb1 162.58(7) . . ? C9 Nb2 Nb1 159.51(7) . . ? B2 Nb2 Nb1 107.79(7) . . ? N1 Nb2 H2A 88.8(11) . . ? N2 Nb2 H2A 133.4(11) . . ? C6 Nb2 H2A 127.4(11) . . ? C7 Nb2 H2A 120.8(11) . . ? C10 Nb2 H2A 94.9(11) . . ? C8 Nb2 H2A 87.7(11) . . ? C9 Nb2 H2A 72.8(11) . . ? B2 Nb2 H2A 28.5(11) . . ? Nb1 Nb2 H2A 107.5(11) . . ? N1 Nb2 H2B 129.1(9) . . ? N2 Nb2 H2B 89.8(9) . . ? C6 Nb2 H2B 130.3(9) . . ? C7 Nb2 H2B 97.0(9) . . ? C10 Nb2 H2B 124.8(9) . . ? C8 Nb2 H2B 76.1(9) . . ? C9 Nb2 H2B 91.7(9) . . ? B2 Nb2 H2B 26.5(9) . . ? Nb1 Nb2 H2B 105.2(9) . . ? H2A Nb2 H2B 55.0(14) . . ? C23 N1 Nb2 137.51(17) . . ? C23 N1 Nb1 137.10(17) . . ? Nb2 N1 Nb1 85.32(8) . . ? C11 N2 Nb2 137.87(17) . . ? C11 N2 Nb1 137.04(17) . . ? Nb2 N2 Nb1 84.93(8) . . ? Nb1 B1 H1A 53.7(16) . . ? Nb1 B1 H1B 52.2(15) . . ? H1A B1 H1B 106(2) . . ? Nb1 B1 H1C 121.4(18) . . ? H1A B1 H1C 113(2) . . ? H1B B1 H1C 104(2) . . ? Nb1 B1 H1D 120.5(19) . . ? H1A B1 H1D 106(2) . . ? H1B B1 H1D 110(2) . . ? H1C B1 H1D 118(3) . . ? Nb2 B2 H2A 52.8(18) . . ? Nb2 B2 H2B 49.6(15) . . ? H2A B2 H2B 102(2) . . ? Nb2 B2 H2C 123.2(19) . . ? H2A B2 H2C 105(3) . . ? H2B B2 H2C 114(2) . . ? Nb2 B2 H2D 122(2) . . ? H2A B2 H2D 108(3) . . ? H2B B2 H2D 113(3) . . ? H2C B2 H2D 115(3) . . ? C5 C1 C2 108.3(3) . . ? C5 C1 Nb1 76.78(19) . . ? C2 C1 Nb1 70.57(17) . . ? C5 C1 H1 136(2) . . ? C2 C1 H1 116(2) . . ? Nb1 C1 H1 114(2) . . ? C1 C2 C3 107.2(3) . . ? C1 C2 Nb1 74.51(18) . . ? C3 C2 Nb1 74.98(17) . . ? C1 C2 H2 127(2) . . ? C3 C2 H2 125(2) . . ? Nb1 C2 H2 121(2) . . ? C4 C3 C2 107.7(3) . . ? C4 C3 Nb1 76.59(17) . . ? C2 C3 Nb1 70.03(16) . . ? C4 C3 H3 126(2) . . ? C2 C3 H3 127(2) . . ? Nb1 C3 H3 118(2) . . ? C3 C4 C5 108.3(3) . . ? C3 C4 Nb1 70.18(16) . . ? C5 C4 Nb1 73.08(17) . . ? C3 C4 H4 128(2) . . ? C5 C4 H4 124(2) . . ? Nb1 C4 H4 122(2) . . ? C1 C5 C4 108.5(3) . . ? C1 C5 Nb1 70.07(17) . . ? C4 C5 Nb1 73.87(17) . . ? C1 C5 H5 127(3) . . ? C4 C5 H5 124(3) . . ? Nb1 C5 H5 118(2) . . ? C10 C6 C7 108.5(3) . . ? C10 C6 Nb2 75.60(16) . . ? C7 C6 Nb2 75.48(16) . . ? C10 C6 H6 123(2) . . ? C7 C6 H6 129(2) . . ? Nb2 C6 H6 118(2) . . ? C8 C7 C6 107.2(3) . . ? C8 C7 Nb2 75.49(16) . . ? C6 C7 Nb2 69.98(15) . . ? C8 C7 H7 127(2) . . ? C6 C7 H7 126(2) . . ? Nb2 C7 H7 119(2) . . ? C7 C8 C9 108.6(3) . . ? C7 C8 Nb2 71.35(16) . . ? C9 C8 Nb2 73.81(16) . . ? C7 C8 H8 124(2) . . ? C9 C8 H8 127(2) . . ? Nb2 C8 H8 119(2) . . ? C10 C9 C8 108.2(3) . . ? C10 C9 Nb2 71.02(15) . . ? C8 C9 Nb2 72.98(16) . . ? C10 C9 H9 126(2) . . ? C8 C9 H9 126(2) . . ? Nb2 C9 H9 121(2) . . ? C9 C10 C6 107.4(3) . . ? C9 C10 Nb2 75.85(16) . . ? C6 C10 Nb2 69.94(15) . . ? C9 C10 H10 128(2) . . ? C6 C10 H10 125(2) . . ? Nb2 C10 H10 119(2) . . ? C12 C11 C16 119.2(2) . . ? C12 C11 N2 120.8(2) . . ? C16 C11 N2 120.0(2) . . ? C13 C12 C11 118.9(3) . . ? C13 C12 C18 117.0(3) . . ? C11 C12 C18 124.1(2) . . ? C14 C13 C12 122.1(3) . . ? C14 C13 H13 121(2) . . ? C12 C13 H13 117(2) . . ? C15 C14 C13 118.8(3) . . ? C15 C14 H14 119(2) . . ? C13 C14 H14 122(2) . . ? C14 C15 C16 122.2(3) . . ? C14 C15 H15 121(2) . . ? C16 C15 H15 117(2) . . ? C15 C16 C11 118.8(3) . . ? C15 C16 C17 118.5(3) . . ? C11 C16 C17 122.4(2) . . ? C16 C17 C20 114.4(2) . . ? C16 C17 C19 108.8(2) . . ? C20 C17 C19 109.3(2) . . ? C16 C17 H17 106.5(19) . . ? C20 C17 H17 107.1(18) . . ? C19 C17 H17 110.6(19) . . ? C12 C18 C22 111.7(3) . . ? C12 C18 C21 111.3(3) . . ? C22 C18 C21 109.5(3) . . ? C12 C18 H18 107.0(16) . . ? C22 C18 H18 107.8(16) . . ? C21 C18 H18 109.4(16) . . ? C17 C19 H19A 112(2) . . ? C17 C19 H19B 112(2) . . ? H19A C19 H19B 108(3) . . ? C17 C19 H19C 109(2) . . ? H19A C19 H19C 110(3) . . ? H19B C19 H19C 105(3) . . ? C17 C20 H20A 113(2) . . ? C17 C20 H20B 110(2) . . ? H20A C20 H20B 103(3) . . ? C17 C20 H20C 111(2) . . ? H20A C20 H20C 110(3) . . ? H20B C20 H20C 109(3) . . ? C18 C21 H21A 110(2) . . ? C18 C21 H21B 111(2) . . ? H21A C21 H21B 108(3) . . ? C18 C21 H21C 109(2) . . ? H21A C21 H21C 106(3) . . ? H21B C21 H21C 112(3) . . ? C18 C22 H22A 112(2) . . ? C18 C22 H22B 111(2) . . ? H22A C22 H22B 109(3) . . ? C18 C22 H22C 115(2) . . ? H22A C22 H22C 102(3) . . ? H22B C22 H22C 108(3) . . ? C24 C23 C28 120.0(2) . . ? C24 C23 N1 120.6(2) . . ? C28 C23 N1 119.4(2) . . ? C25 C24 C23 118.0(3) . . ? C25 C24 C29 116.9(3) . . ? C23 C24 C29 125.1(2) . . ? C26 C25 C24 122.1(3) . . ? C26 C25 H25 118(3) . . ? C24 C25 H25 120(3) . . ? C25 C26 C27 119.5(3) . . ? C25 C26 H26 121(2) . . ? C27 C26 H26 120(2) . . ? C26 C27 C28 121.5(3) . . ? C26 C27 H27 122.4(19) . . ? C28 C27 H27 116.1(19) . . ? C27 C28 C23 118.9(3) . . ? C27 C28 C30 117.9(3) . . ? C23 C28 C30 123.2(2) . . ? C24 C29 C31 111.9(3) . . ? C24 C29 C32 112.3(2) . . ? C31 C29 C32 108.9(3) . . ? C24 C29 H29 106(2) . . ? C31 C29 H29 108(2) . . ? C32 C29 H29 110(2) . . ? C28 C30 C33 113.7(3) . . ? C28 C30 C34 109.1(3) . . ? C33 C30 C34 109.4(3) . . ? C28 C30 H30 113.9(19) . . ? C33 C30 H30 105(2) . . ? C34 C30 H30 105(2) . . ? C29 C31 H31A 111(2) . . ? C29 C31 H31B 113(2) . . ? H31A C31 H31B 104(3) . . ? C29 C31 H31C 114(2) . . ? H31A C31 H31C 109(3) . . ? H31B C31 H31C 105(3) . . ? C29 C32 H32A 111.6(17) . . ? C29 C32 H32B 108(2) . . ? H32A C32 H32B 106(3) . . ? C29 C32 H32C 109(2) . . ? H32A C32 H32C 111(3) . . ? H32B C32 H32C 111(3) . . ? C30 C33 H33A 107(2) . . ? C30 C33 H33B 113(2) . . ? H33A C33 H33B 107(3) . . ? C30 C33 H33C 111(2) . . ? H33A C33 H33C 114(3) . . ? H33B C33 H33C 105(3) . . ? C30 C34 H34A 108(2) . . ? C30 C34 H34B 111(2) . . ? H34A C34 H34B 106(3) . . ? C30 C34 H34C 109(2) . . ? H34A C34 H34C 111(3) . . ? H34B C34 H34C 111(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.950 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 960156' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_7 _chemical_name_systematic ; [CpTa(u-NAr)(BH4)]2 ; _chemical_melting_point ? _cell_length_a 10.6770(2) _cell_length_b 20.3428(2) _cell_length_c 15.7568(2) _cell_angle_alpha 90 _cell_angle_beta 96.4877(5) _cell_angle_gamma 90 _cell_volume 3400.46(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ta -1.2580 6.5230 29.2024 1.7733 15.2293 9.3705 14.5135 0.2960 4.7649 63.3644 9.2435 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C34 H52 B2 N2 Ta2' _chemical_formula_moiety 'C34 H52 B2 N2 Ta2' _chemical_compound_source ? _chemical_formula_weight 872.32 _cell_measurement_reflns_used 55248 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour darkred _exptl_crystal_size_min 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 6.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 0.38 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 55248 _reflns_number_total 7965 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_min 5.128 _diffrn_reflns_theta_max 27.482 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.482 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.54 _refine_diff_density_max 1.40 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 5841 _refine_ls_number_restraints 8 _refine_ls_number_parameters 393 _oxford_refine_ls_R_factor_ref 0.0256 _refine_ls_wR_factor_ref 0.0291 _refine_ls_goodness_of_fit_ref 1.0738 _refine_ls_shift/su_max 0.0030621 _refine_ls_shift/su_mean 0.0000344 _oxford_reflns_number_all 7740 _refine_ls_R_factor_all 0.0407 _refine_ls_wR_factor_all 0.0502 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6198 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_gt 0.0291 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.279 0.129 0.872E-01 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ta1 Ta 0.561951(15) 0.618891(8) 0.377086(10) 0.0150 1.0000 Uani . . . . . . Ta2 Ta 0.411923(15) 0.708087(8) 0.284949(10) 0.0139 1.0000 Uani . . . . . . B1 B 0.6462(6) 0.5170(3) 0.3325(4) 0.0318 1.0000 Uani . U . . . . B2 B 0.3774(5) 0.7993(2) 0.3815(3) 0.0194 1.0000 Uani . U . . . . N1 N 0.3740(3) 0.62224(17) 0.3362(2) 0.0162 1.0000 Uani . . . . . . N2 N 0.5941(3) 0.68842(17) 0.2890(2) 0.0150 1.0000 Uani . . . . . . C1 C 0.2676(4) 0.5803(2) 0.3384(3) 0.0198 1.0000 Uani . . . . . . C2 C 0.1788(4) 0.5929(2) 0.3976(3) 0.0202 1.0000 Uani . . . . . . C3 C 0.0778(5) 0.5493(3) 0.4005(3) 0.0314 1.0000 Uani . . . . . . C4 C 0.0582(5) 0.4970(3) 0.3452(4) 0.0354 1.0000 Uani . . . . . . C5 C 0.1428(5) 0.4861(2) 0.2862(3) 0.0311 1.0000 Uani . . . . . . C6 C 0.2476(4) 0.5261(2) 0.2814(3) 0.0239 1.0000 Uani . . . . . . C7 C 0.1842(4) 0.6537(2) 0.4523(3) 0.0219 1.0000 Uani . . . . . . C8 C 0.0892(5) 0.7037(3) 0.4105(3) 0.0308 1.0000 Uani . . . . . . C9 C 0.1585(5) 0.6420(3) 0.5449(3) 0.0303 1.0000 Uani . . . . . . C10 C 0.3325(5) 0.5097(2) 0.2134(3) 0.0279 1.0000 Uani . . . . . . C11 C 0.2622(6) 0.5146(3) 0.1230(4) 0.0416 1.0000 Uani . . . . . . C12 C 0.3873(6) 0.4398(3) 0.2266(4) 0.0393 1.0000 Uani . . . . . . C13 C 0.6989(4) 0.7103(2) 0.2476(3) 0.0193 1.0000 Uani . . . . . . C14 C 0.7601(4) 0.7696(2) 0.2743(3) 0.0224 1.0000 Uani . . . . . . C15 C 0.8620(5) 0.7900(3) 0.2333(3) 0.0354 1.0000 Uani . . . . . . C16 C 0.9036(5) 0.7546(3) 0.1673(3) 0.0381 1.0000 Uani . . . . . . C17 C 0.8420(5) 0.6976(3) 0.1399(3) 0.0334 1.0000 Uani . . . . . . C18 C 0.7395(4) 0.6739(2) 0.1795(3) 0.0233 1.0000 Uani . . . . . . C19 C 0.7155(4) 0.8137(2) 0.3419(3) 0.0247 1.0000 Uani . . . . . . C20 C 0.6495(5) 0.8744(2) 0.2990(4) 0.0331 1.0000 Uani . . . . . . C21 C 0.8225(5) 0.8371(3) 0.4088(3) 0.0350 1.0000 Uani . . . . . . C22 C 0.6790(5) 0.6106(2) 0.1437(3) 0.0298 1.0000 Uani . . . . . . C23 C 0.6190(5) 0.6191(2) 0.0512(3) 0.0274 1.0000 Uani . . . . . . C24 C 0.7752(7) 0.5542(3) 0.1473(4) 0.0463 1.0000 Uani . . . . . . C25 C 0.5743(5) 0.6829(3) 0.4993(3) 0.0319 1.0000 Uani . . . . . . C26 C 0.7005(5) 0.6725(3) 0.4828(3) 0.0344 1.0000 Uani . . . . . . C27 C 0.7286(5) 0.6063(3) 0.4963(3) 0.0325 1.0000 Uani . . . . . . C28 C 0.6214(5) 0.5748(3) 0.5215(3) 0.0300 1.0000 Uani . . . . . . C29 C 0.5266(5) 0.6213(3) 0.5234(3) 0.0278 1.0000 Uani . . . . . . C30 C 0.3479(4) 0.6820(2) 0.1421(3) 0.0232 1.0000 Uani . . . . . . C31 C 0.4137(4) 0.7426(2) 0.1387(3) 0.0244 1.0000 Uani . . . . . . C32 C 0.3417(5) 0.7910(2) 0.1741(3) 0.0273 1.0000 Uani . . . . . . C33 C 0.2323(5) 0.7610(2) 0.1993(3) 0.0280 1.0000 Uani . . . . . . C34 C 0.2339(4) 0.6939(3) 0.1783(3) 0.0269 1.0000 Uani . . . . . . H1 H 0.688(5) 0.578(3) 0.333(4) 0.036(9) 1.0000 Uiso . U . . . . H2 H 0.551(4) 0.529(2) 0.362(3) 0.017(8) 1.0000 Uiso . U . . . . H3 H 0.701(6) 0.487(3) 0.380(4) 0.039(9) 1.0000 Uiso . U . . . . H4 H 0.632(6) 0.501(3) 0.267(4) 0.040(9) 1.0000 Uiso . U . . . . H5 H 0.453(5) 0.794(3) 0.336(3) 0.026(8) 1.0000 Uiso . U . . . . H6 H 0.317(5) 0.751(3) 0.370(3) 0.029(8) 1.0000 Uiso . U . . . . H7 H 0.414(5) 0.799(3) 0.440(4) 0.027(8) 1.0000 Uiso . U . . . . H8 H 0.326(5) 0.836(3) 0.360(3) 0.020(8) 1.0000 Uiso . U . . . . H31 H 0.0181 0.5564 0.4442 0.0384 1.0000 Uiso . . . . . . H41 H -0.0160 0.4673 0.3475 0.0422 1.0000 Uiso . . . . . . H51 H 0.1282 0.4483 0.2457 0.0371 1.0000 Uiso . . . . . . H71 H 0.2729 0.6703 0.4557 0.0269 1.0000 Uiso . . . . . . H81 H 0.0918 0.7444 0.4462 0.0374 1.0000 Uiso . . . . . . H82 H 0.1111 0.7149 0.3522 0.0374 1.0000 Uiso . . . . . . H83 H 0.0025 0.6843 0.4059 0.0374 1.0000 Uiso . . . . . . H91 H 0.1640 0.6847 0.5766 0.0372 1.0000 Uiso . . . . . . H92 H 0.2225 0.6107 0.5730 0.0372 1.0000 Uiso . . . . . . H93 H 0.0723 0.6229 0.5455 0.0372 1.0000 Uiso . . . . . . H101 H 0.4024 0.5427 0.2191 0.0338 1.0000 Uiso . . . . . . H111 H 0.3211 0.5035 0.0801 0.0501 1.0000 Uiso . . . . . . H112 H 0.2300 0.5604 0.1128 0.0501 1.0000 Uiso . . . . . . H113 H 0.1898 0.4832 0.1173 0.0501 1.0000 Uiso . . . . . . H121 H 0.4429 0.4301 0.1811 0.0474 1.0000 Uiso . . . . . . H122 H 0.4377 0.4370 0.2839 0.0474 1.0000 Uiso . . . . . . H123 H 0.3169 0.4072 0.2232 0.0474 1.0000 Uiso . . . . . . H151 H 0.9065 0.8316 0.2523 0.0420 1.0000 Uiso . . . . . . H161 H 0.9779 0.7702 0.1395 0.0463 1.0000 Uiso . . . . . . H171 H 0.8707 0.6726 0.0910 0.0409 1.0000 Uiso . . . . . . H191 H 0.6563 0.7869 0.3727 0.0295 1.0000 Uiso . . . . . . H201 H 0.6199 0.9036 0.3437 0.0393 1.0000 Uiso . . . . . . H202 H 0.7101 0.8990 0.2668 0.0393 1.0000 Uiso . . . . . . H203 H 0.5756 0.8600 0.2586 0.0393 1.0000 Uiso . . . . . . H211 H 0.7869 0.8659 0.4515 0.0411 1.0000 Uiso . . . . . . H212 H 0.8857 0.8624 0.3798 0.0411 1.0000 Uiso . . . . . . H213 H 0.8643 0.7981 0.4385 0.0411 1.0000 Uiso . . . . . . H221 H 0.6114 0.5995 0.1804 0.0366 1.0000 Uiso . . . . . . H231 H 0.5803 0.5765 0.0299 0.0330 1.0000 Uiso . . . . . . H232 H 0.6853 0.6324 0.0145 0.0330 1.0000 Uiso . . . . . . H233 H 0.5524 0.6538 0.0488 0.0330 1.0000 Uiso . . . . . . H241 H 0.7327 0.5134 0.1234 0.0573 1.0000 Uiso . . . . . . H242 H 0.8450 0.5663 0.1130 0.0573 1.0000 Uiso . . . . . . H243 H 0.8105 0.5463 0.2080 0.0573 1.0000 Uiso . . . . . . H251 H 0.5275 0.7256 0.4947 0.0377 1.0000 Uiso . . . . . . H261 H 0.7591 0.7067 0.4646 0.0401 1.0000 Uiso . . . . . . H271 H 0.8110 0.5848 0.4893 0.0386 1.0000 Uiso . . . . . . H281 H 0.6148 0.5271 0.5357 0.0357 1.0000 Uiso . . . . . . H291 H 0.4398 0.6129 0.5391 0.0336 1.0000 Uiso . . . . . . H301 H 0.3769 0.6384 0.1223 0.0274 1.0000 Uiso . . . . . . H311 H 0.4961 0.7494 0.1154 0.0287 1.0000 Uiso . . . . . . H321 H 0.3640 0.8387 0.1804 0.0319 1.0000 Uiso . . . . . . H331 H 0.1649 0.7837 0.2273 0.0330 1.0000 Uiso . . . . . . H341 H 0.1675 0.6607 0.1872 0.0315 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.01516(9) 0.01603(9) 0.01428(9) 0.00319(6) 0.00363(6) 0.00184(6) Ta2 0.01374(8) 0.01370(8) 0.01462(8) 0.00170(6) 0.00256(6) 0.00047(6) B1 0.038(3) 0.027(3) 0.032(3) 0.003(2) 0.012(2) 0.009(2) B2 0.020(2) 0.018(2) 0.021(2) 0.0035(18) 0.0050(19) 0.0072(19) N1 0.0181(17) 0.0148(17) 0.0163(17) 0.0000(13) 0.0046(13) -0.0008(13) N2 0.0162(17) 0.0165(17) 0.0131(16) 0.0024(12) 0.0048(13) 0.0005(13) C1 0.018(2) 0.018(2) 0.023(2) 0.0035(16) 0.0006(17) -0.0031(16) C2 0.018(2) 0.019(2) 0.024(2) 0.0053(17) 0.0041(17) -0.0004(17) C3 0.024(2) 0.031(3) 0.042(3) 0.004(2) 0.012(2) -0.006(2) C4 0.025(3) 0.033(3) 0.047(3) 0.002(2) 0.001(2) -0.013(2) C5 0.032(3) 0.024(2) 0.036(3) -0.001(2) 0.002(2) -0.009(2) C6 0.023(2) 0.018(2) 0.029(2) 0.0032(18) -0.0021(18) -0.0003(18) C7 0.019(2) 0.024(2) 0.024(2) 0.0032(17) 0.0083(17) 0.0028(18) C8 0.028(2) 0.028(3) 0.037(3) 0.006(2) 0.008(2) 0.005(2) C9 0.032(3) 0.033(3) 0.028(3) 0.005(2) 0.013(2) 0.001(2) C10 0.037(3) 0.019(2) 0.029(2) -0.0044(18) 0.006(2) -0.004(2) C11 0.058(4) 0.037(3) 0.030(3) -0.007(2) 0.007(3) -0.012(3) C12 0.050(3) 0.023(3) 0.045(3) -0.006(2) 0.008(3) 0.000(2) C13 0.0108(18) 0.030(2) 0.017(2) 0.0091(17) 0.0021(15) 0.0031(16) C14 0.017(2) 0.030(2) 0.020(2) 0.0082(18) 0.0003(16) -0.0046(18) C15 0.021(2) 0.053(3) 0.031(3) 0.013(2) -0.003(2) -0.016(2) C16 0.019(2) 0.071(4) 0.026(3) 0.018(3) 0.0093(19) -0.001(2) C17 0.021(2) 0.055(3) 0.026(2) 0.013(2) 0.0116(19) 0.006(2) C18 0.020(2) 0.034(3) 0.016(2) 0.0070(18) 0.0051(17) 0.0082(19) C19 0.025(2) 0.024(2) 0.025(2) 0.0045(18) 0.0018(18) -0.0068(18) C20 0.035(3) 0.025(3) 0.038(3) 0.006(2) -0.001(2) -0.007(2) C21 0.035(3) 0.033(3) 0.034(3) -0.002(2) -0.006(2) -0.013(2) C22 0.040(3) 0.024(2) 0.027(2) 0.0017(19) 0.012(2) 0.011(2) C23 0.035(3) 0.029(2) 0.018(2) -0.0038(18) 0.0052(19) 0.000(2) C24 0.065(4) 0.036(3) 0.043(3) 0.003(2) 0.025(3) 0.023(3) C25 0.048(3) 0.030(3) 0.016(2) -0.0010(18) -0.003(2) 0.006(2) C26 0.035(3) 0.043(3) 0.021(2) 0.002(2) -0.010(2) -0.010(2) C27 0.023(2) 0.049(3) 0.025(2) 0.006(2) -0.0025(19) 0.008(2) C28 0.033(3) 0.035(3) 0.021(2) 0.0108(19) 0.000(2) 0.004(2) C29 0.028(2) 0.041(3) 0.015(2) 0.0055(19) 0.0046(18) 0.005(2) C30 0.028(2) 0.025(2) 0.015(2) 0.0007(16) -0.0029(17) -0.0005(18) C31 0.029(2) 0.027(2) 0.016(2) 0.0052(17) -0.0035(18) 0.0000(19) C32 0.034(3) 0.021(2) 0.024(2) 0.0056(18) -0.006(2) 0.0015(19) C33 0.025(2) 0.030(3) 0.027(2) 0.0044(19) -0.0038(19) 0.006(2) C34 0.020(2) 0.037(3) 0.023(2) 0.0038(19) -0.0069(18) -0.0016(19) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.08465(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ta1 . Ta2 . 2.7277(2) yes Ta1 . B1 . 2.396(6) yes Ta1 . N1 . 2.039(4) yes Ta1 . N2 . 2.038(3) yes Ta1 . C25 . 2.316(5) yes Ta1 . C26 . 2.365(5) yes Ta1 . C27 . 2.451(5) yes Ta1 . C28 . 2.462(5) yes Ta1 . C29 . 2.379(4) yes Ta1 . H1 . 1.79(6) no Ta1 . H2 . 1.84(5) no Ta2 . B2 . 2.454(5) yes Ta2 . N1 . 1.985(3) yes Ta2 . N2 . 1.980(3) yes Ta2 . C30 . 2.339(4) yes Ta2 . C31 . 2.411(4) yes Ta2 . C32 . 2.483(4) yes Ta2 . C33 . 2.465(5) yes Ta2 . C34 . 2.407(4) yes Ta2 . H5 . 1.95(5) no Ta2 . H6 . 1.97(5) no B1 . H1 . 1.31(6) no B1 . H2 . 1.19(5) no B1 . H3 . 1.08(6) no B1 . H4 . 1.07(6) no B2 . H5 . 1.14(5) no B2 . H6 . 1.18(6) no B2 . H7 . 0.95(6) no B2 . H8 . 0.96(5) no N1 . C1 . 1.424(5) yes N2 . C13 . 1.428(5) yes C1 . C2 . 1.427(6) yes C1 . C6 . 1.423(6) yes C2 . C3 . 1.400(6) yes C2 . C7 . 1.505(6) yes C3 . C4 . 1.377(8) yes C3 . H31 . 1.000 no C4 . C5 . 1.386(8) yes C4 . H41 . 1.000 no C5 . C6 . 1.392(7) yes C5 . H51 . 1.000 no C6 . C10 . 1.517(7) yes C7 . C8 . 1.531(7) yes C7 . C9 . 1.534(6) yes C7 . H71 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no C8 . H81 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C9 . H91 . 1.000 no C10 . C11 . 1.536(7) yes C10 . C12 . 1.542(7) yes C10 . H101 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C11 . H111 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C12 . H121 . 1.000 no C13 . C14 . 1.413(6) yes C13 . C18 . 1.411(6) yes C14 . C15 . 1.390(6) yes C14 . C19 . 1.511(7) yes C15 . C16 . 1.379(8) yes C15 . H151 . 1.000 no C16 . C17 . 1.378(9) yes C16 . H161 . 1.000 no C17 . C18 . 1.405(6) yes C17 . H171 . 1.000 no C18 . C22 . 1.520(7) yes C19 . C20 . 1.540(7) yes C19 . C21 . 1.539(7) yes C19 . H191 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no C20 . H201 . 1.000 no C21 . H212 . 1.000 no C21 . H213 . 1.000 no C21 . H211 . 1.000 no C22 . C23 . 1.534(7) yes C22 . C24 . 1.537(7) yes C22 . H221 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C23 . H231 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no C24 . H241 . 1.000 no C25 . C26 . 1.417(8) yes C25 . C29 . 1.421(7) yes C25 . H251 . 1.000 no C26 . C27 . 1.389(8) yes C26 . H261 . 1.000 no C27 . C28 . 1.408(7) yes C27 . H271 . 1.000 no C28 . C29 . 1.388(7) yes C28 . H281 . 1.000 no C29 . H291 . 1.000 no C30 . C31 . 1.423(7) yes C30 . C34 . 1.422(7) yes C30 . H301 . 1.000 no C31 . C32 . 1.403(7) yes C31 . H311 . 1.000 no C32 . C33 . 1.415(7) yes C32 . H321 . 1.000 no C33 . C34 . 1.405(7) yes C33 . H331 . 1.000 no C34 . H341 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Ta2 . Ta1 . B1 . 129.56(15) yes Ta2 . Ta1 . N1 . 46.49(10) yes B1 . Ta1 . N1 . 108.97(19) yes Ta2 . Ta1 . N2 . 46.36(10) yes B1 . Ta1 . N2 . 107.64(17) yes N1 . Ta1 . N2 . 89.83(14) yes Ta2 . Ta1 . C25 . 92.48(12) yes B1 . Ta1 . C25 . 137.9(2) yes N1 . Ta1 . C25 . 101.86(17) yes N2 . Ta1 . C25 . 100.26(16) yes Ta2 . Ta1 . C26 . 110.57(14) yes B1 . Ta1 . C26 . 112.3(2) yes N1 . Ta1 . C26 . 136.25(17) yes N2 . Ta1 . C26 . 91.14(16) yes C25 . Ta1 . C26 . 35.2(2) yes Ta2 . Ta1 . C27 . 144.02(14) yes B1 . Ta1 . C27 . 82.5(2) yes N1 . Ta1 . C27 . 148.17(15) yes N2 . Ta1 . C27 . 115.52(16) yes C25 . Ta1 . C27 . 56.85(18) yes Ta2 . Ta1 . C28 . 143.99(12) yes B1 . Ta1 . C28 . 83.66(19) yes N1 . Ta1 . C28 . 116.52(15) yes N2 . Ta1 . C28 . 146.80(16) yes C25 . Ta1 . C28 . 56.74(18) yes Ta2 . Ta1 . C29 . 110.74(12) yes B1 . Ta1 . C29 . 114.06(19) yes N1 . Ta1 . C29 . 92.71(15) yes N2 . Ta1 . C29 . 134.71(16) yes C25 . Ta1 . C29 . 35.20(18) yes Ta2 . Ta1 . H1 . 121.8(18) no B1 . Ta1 . H1 . 32.6(19) no N1 . Ta1 . H1 . 130.4(18) no N2 . Ta1 . H1 . 82.5(19) no C25 . Ta1 . H1 . 127.7(18) no Ta2 . Ta1 . H2 . 124.3(14) no B1 . Ta1 . H2 . 28.9(15) no N1 . Ta1 . H2 . 86.9(14) no N2 . Ta1 . H2 . 127.6(14) no C25 . Ta1 . H2 . 131.6(14) no C26 . Ta1 . C27 . 33.48(19) yes C26 . Ta1 . C28 . 56.02(18) yes C27 . Ta1 . C28 . 33.30(17) yes C26 . Ta1 . C29 . 57.52(18) yes C27 . Ta1 . C29 . 55.96(17) yes C28 . Ta1 . C29 . 33.28(17) yes C26 . Ta1 . H1 . 93.0(18) no C27 . Ta1 . H1 . 74.7(18) no C28 . Ta1 . H1 . 93.5(18) no C29 . Ta1 . H1 . 126.5(18) no C26 . Ta1 . H2 . 125.1(14) no C27 . Ta1 . H2 . 91.6(14) no C28 . Ta1 . H2 . 76.6(14) no C29 . Ta1 . H2 . 97.7(14) no H1 . Ta1 . H2 . 61(2) no Ta1 . Ta2 . B2 . 107.08(12) yes Ta1 . Ta2 . N1 . 48.16(10) yes B2 . Ta2 . N1 . 111.20(15) yes Ta1 . Ta2 . N2 . 48.15(10) yes B2 . Ta2 . N2 . 110.43(15) yes N1 . Ta2 . N2 . 93.12(14) yes Ta1 . Ta2 . C30 . 116.84(12) yes B2 . Ta2 . C30 . 136.07(16) yes N1 . Ta2 . C30 . 98.10(15) yes N2 . Ta2 . C30 . 99.44(15) yes Ta1 . Ta2 . C31 . 129.41(12) yes B2 . Ta2 . C31 . 112.94(16) yes N1 . Ta2 . C31 . 131.99(15) yes N2 . Ta2 . C31 . 88.60(15) yes C30 . Ta2 . C31 . 34.82(16) yes Ta1 . Ta2 . C32 . 159.87(12) yes B2 . Ta2 . C32 . 82.38(16) yes N1 . Ta2 . C32 . 145.57(15) yes N2 . Ta2 . C32 . 112.15(16) yes C30 . Ta2 . C32 . 56.27(16) yes Ta1 . Ta2 . C33 . 162.90(12) yes B2 . Ta2 . C33 . 81.20(17) yes N1 . Ta2 . C33 . 115.13(16) yes N2 . Ta2 . C33 . 143.78(15) yes C30 . Ta2 . C33 . 56.43(17) yes Ta1 . Ta2 . C34 . 131.40(12) yes B2 . Ta2 . C34 . 111.17(17) yes N1 . Ta2 . C34 . 89.81(16) yes N2 . Ta2 . C34 . 133.89(16) yes C30 . Ta2 . C34 . 34.84(17) yes Ta1 . Ta2 . H5 . 106.8(15) no B2 . Ta2 . H5 . 27.1(16) no N1 . Ta2 . H5 . 131.9(15) no N2 . Ta2 . H5 . 89.8(16) no C30 . Ta2 . H5 . 128.7(15) no Ta1 . Ta2 . H6 . 104.4(16) no B2 . Ta2 . H6 . 28.3(16) no N1 . Ta2 . H6 . 88.2(16) no N2 . Ta2 . H6 . 130.2(16) no C30 . Ta2 . H6 . 129.7(16) no C31 . Ta2 . C32 . 33.27(17) yes C31 . Ta2 . C33 . 55.87(16) yes C32 . Ta2 . C33 . 33.24(17) yes C31 . Ta2 . C34 . 57.24(16) yes C32 . Ta2 . C34 . 55.87(16) yes C33 . Ta2 . C34 . 33.49(17) yes C31 . Ta2 . H5 . 96.0(15) no C32 . Ta2 . H5 . 73.4(15) no C33 . Ta2 . H5 . 87.5(15) no C34 . Ta2 . H5 . 121.0(15) no C31 . Ta2 . H6 . 125.5(16) no C32 . Ta2 . H6 . 92.3(16) no C33 . Ta2 . H6 . 75.6(16) no C34 . Ta2 . H6 . 95.9(16) no H5 . Ta2 . H6 . 55(2) no Ta1 . B1 . H1 . 47(2) no Ta1 . B1 . H2 . 49(2) no H1 . B1 . H2 . 96(3) no Ta1 . B1 . H3 . 118(3) no H1 . B1 . H3 . 111(4) no H2 . B1 . H3 . 106(4) no Ta1 . B1 . H4 . 122(3) no H1 . B1 . H4 . 107(4) no H2 . B1 . H4 . 113(4) no H3 . B1 . H4 . 120(4) no Ta2 . B2 . H5 . 51(3) no Ta2 . B2 . H6 . 53(3) no H5 . B2 . H6 . 104(4) no Ta2 . B2 . H7 . 121(3) no H5 . B2 . H7 . 111(4) no H6 . B2 . H7 . 107(4) no Ta2 . B2 . H8 . 120(3) no H5 . B2 . H8 . 106(4) no H6 . B2 . H8 . 108(4) no H7 . B2 . H8 . 120(4) no Ta1 . N1 . Ta2 . 85.35(13) yes Ta1 . N1 . C1 . 137.0(3) yes Ta2 . N1 . C1 . 137.5(3) yes Ta1 . N2 . Ta2 . 85.49(13) yes Ta1 . N2 . C13 . 136.7(3) yes Ta2 . N2 . C13 . 137.7(3) yes N1 . C1 . C2 . 119.9(4) yes N1 . C1 . C6 . 120.8(4) yes C2 . C1 . C6 . 119.3(4) yes C1 . C2 . C3 . 118.6(4) yes C1 . C2 . C7 . 122.4(4) yes C3 . C2 . C7 . 118.8(4) yes C2 . C3 . C4 . 122.1(5) yes C2 . C3 . H31 . 119.0 no C4 . C3 . H31 . 119.0 no C3 . C4 . C5 . 119.0(5) yes C3 . C4 . H41 . 120.5 no C5 . C4 . H41 . 120.5 no C4 . C5 . C6 . 122.1(5) yes C4 . C5 . H51 . 118.9 no C6 . C5 . H51 . 118.9 no C1 . C6 . C5 . 118.9(4) yes C1 . C6 . C10 . 123.9(4) yes C5 . C6 . C10 . 117.3(4) yes C2 . C7 . C8 . 108.6(4) yes C2 . C7 . C9 . 114.7(4) yes C8 . C7 . C9 . 109.3(4) yes C2 . C7 . H71 . 106.5 no C8 . C7 . H71 . 112.1 no C9 . C7 . H71 . 105.7 no C7 . C8 . H82 . 109.5 no C7 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no C7 . C8 . H81 . 109.5 no C7 . C9 . H92 . 109.5 no C7 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C7 . C9 . H91 . 109.5 no C6 . C10 . C11 . 111.8(4) yes C6 . C10 . C12 . 110.8(4) yes C11 . C10 . C12 . 108.9(4) yes C6 . C10 . H101 . 106.7 no C11 . C10 . H101 . 108.7 no C12 . C10 . H101 . 109.8 no C10 . C11 . H112 . 109.5 no C10 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no C10 . C11 . H111 . 109.5 no C10 . C12 . H122 . 109.5 no C10 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C10 . C12 . H121 . 109.5 no N2 . C13 . C14 . 119.4(4) yes N2 . C13 . C18 . 120.4(4) yes C14 . C13 . C18 . 120.2(4) yes C13 . C14 . C15 . 118.5(5) yes C13 . C14 . C19 . 123.0(4) yes C15 . C14 . C19 . 118.5(4) yes C14 . C15 . C16 . 122.1(5) yes C14 . C15 . H151 . 119.0 no C16 . C15 . H151 . 119.0 no C15 . C16 . C17 . 119.4(4) yes C15 . C16 . H161 . 120.3 no C17 . C16 . H161 . 120.3 no C16 . C17 . C18 . 121.2(5) yes C16 . C17 . H171 . 119.4 no C18 . C17 . H171 . 119.4 no C13 . C18 . C17 . 118.6(5) yes C13 . C18 . C22 . 125.0(4) yes C17 . C18 . C22 . 116.5(4) yes C14 . C19 . C20 . 109.4(4) yes C14 . C19 . C21 . 113.4(4) yes C20 . C19 . C21 . 108.7(4) yes C14 . C19 . H191 . 106.6 no C20 . C19 . H191 . 111.5 no C21 . C19 . H191 . 107.3 no C19 . C20 . H202 . 109.5 no C19 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C19 . C20 . H201 . 109.5 no C19 . C21 . H212 . 109.5 no C19 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C19 . C21 . H211 . 109.5 no C18 . C22 . C23 . 111.8(4) yes C18 . C22 . C24 . 111.3(5) yes C23 . C22 . C24 . 108.9(4) yes C18 . C22 . H221 . 106.3 no C23 . C22 . H221 . 108.9 no C24 . C22 . H221 . 109.4 no C22 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C23 . H231 . 109.5 no C22 . C24 . H242 . 109.5 no C22 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C22 . C24 . H241 . 109.5 no Ta1 . C25 . C26 . 74.3(3) yes Ta1 . C25 . C29 . 74.8(3) yes C26 . C25 . C29 . 107.1(5) yes Ta1 . C25 . H251 . 116.6 no C26 . C25 . H251 . 126.5 no C29 . C25 . H251 . 126.5 no Ta1 . C26 . C25 . 70.5(3) yes Ta1 . C26 . C27 . 76.7(3) yes C25 . C26 . C27 . 108.1(5) yes Ta1 . C26 . H261 . 118.8 no C25 . C26 . H261 . 125.9 no C27 . C26 . H261 . 125.9 no C26 . C27 . Ta1 . 69.9(3) yes C26 . C27 . C28 . 108.4(5) yes Ta1 . C27 . C28 . 73.8(3) yes C26 . C27 . H271 . 125.8 no Ta1 . C27 . H271 . 122.2 no C28 . C27 . H271 . 125.8 no C27 . C28 . Ta1 . 72.9(3) yes C27 . C28 . C29 . 108.3(5) yes Ta1 . C28 . C29 . 70.1(3) yes C27 . C28 . H281 . 125.8 no Ta1 . C28 . H281 . 122.8 no C29 . C28 . H281 . 125.8 no Ta1 . C29 . C25 . 70.0(3) yes Ta1 . C29 . C28 . 76.6(3) yes C25 . C29 . C28 . 108.1(4) yes Ta1 . C29 . H291 . 119.2 no C25 . C29 . H291 . 126.0 no C28 . C29 . H291 . 126.0 no Ta2 . C30 . C31 . 75.4(3) yes Ta2 . C30 . C34 . 75.2(3) yes C31 . C30 . C34 . 108.4(4) yes Ta2 . C30 . H301 . 115.7 no C31 . C30 . H301 . 125.8 no C34 . C30 . H301 . 125.8 no C30 . C31 . Ta2 . 69.8(2) yes C30 . C31 . C32 . 107.4(4) yes Ta2 . C31 . C32 . 76.2(3) yes C30 . C31 . H311 . 126.3 no Ta2 . C31 . H311 . 119.6 no C32 . C31 . H311 . 126.3 no C31 . C32 . Ta2 . 70.6(3) yes C31 . C32 . C33 . 108.3(4) yes Ta2 . C32 . C33 . 72.7(3) yes C31 . C32 . H321 . 125.8 no Ta2 . C32 . H321 . 122.6 no C33 . C32 . H321 . 125.8 no C32 . C33 . Ta2 . 74.1(3) yes C32 . C33 . C34 . 108.7(4) yes Ta2 . C33 . C34 . 71.0(3) yes C32 . C33 . H331 . 125.6 no Ta2 . C33 . H331 . 120.9 no C34 . C33 . H331 . 125.6 no Ta2 . C34 . C30 . 69.9(2) yes Ta2 . C34 . C33 . 75.5(3) yes C30 . C34 . C33 . 107.1(4) yes Ta2 . C34 . H341 . 120.0 no C30 . C34 . H341 . 126.5 no C33 . C34 . H341 . 126.5 no Ta1 . H1 . B1 . 100(3) no Ta1 . H2 . B1 . 102(3) no B2 . H5 . Ta2 . 102(3) no B2 . H6 . Ta2 . 99(3) no _database_code_depnum_ccdc_archive 'CCDC 960157'