Supplementary data for Dalton Trans. This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Roland Fischer' _publ_contact_author_email ROLAND.FISCHER@RUHR-UNI-BOCHUM.DE _publ_section_title ; Mixed Amido/Imido/Guanidinato Complexes of Niobium: Potential Precursors for MOCVD of Niobium Nitride Thin Films ; loop_ _publ_author_name 'Roland Fischer' 'Arne Baunemann' 'Daniela Bekermann' 'Christian Gemel' 'Harish Parala' 'Tobias B. Thiede' ; M.Winter ; # Attachment 'RAFISCHER_CIF.cif' # 1. SUBMISSION DETAILS data_cvd96 _database_code_depnum_ccdc_archive 'CCDC 637765' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H27 N4 Nb' _chemical_formula_weight 296.27 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 11.208(19) _cell_length_b 11.208(19) _cell_length_c 21.16(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2302(6) _cell_formula_units_Z 6 _cell_measurement_temperature 111(2) _cell_measurement_reflns_used 4600 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 27.499 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'Gaussian face-indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 111(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 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '887 images at 1.0 deg. in \w and 30 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10657 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1006 _reflns_number_gt 897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1006 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.0000 0.0000 0.17516(2) 0.03006(19) Uani 1 3 d S . . N1 N 0.0107(2) 0.1742(2) 0.14652(13) 0.0370(6) Uani 1 1 d . . . N2 N 0.0000 0.0000 0.25821(19) 0.0271(9) Uani 1 3 d S A . C1 C -0.0286(4) 0.1829(4) 0.08239(17) 0.0587(10) Uani 1 1 d . . . H1A H -0.1069 0.1990 0.0829 0.088 Uiso 1 1 calc R . . H1B H -0.0549 0.0964 0.0602 0.088 Uiso 1 1 calc R . . H1C H 0.0492 0.2592 0.0605 0.088 Uiso 1 1 calc R . . C2 C 0.0471(3) 0.2994(3) 0.18169(19) 0.0489(9) Uani 1 1 d . . . H2A H 0.1272 0.3775 0.1620 0.073 Uiso 1 1 calc R . . H2B H 0.0695 0.2890 0.2254 0.073 Uiso 1 1 calc R . . H2C H -0.0308 0.3160 0.1814 0.073 Uiso 1 1 calc R . . C3 C 0.0000 0.0000 0.3261(2) 0.0321(11) Uani 1 3 d S . . C41 C 0.1322(15) 0.1224(14) 0.3585(4) 0.070(6) Uani 0.410(17) 1 d P A 1 H4A H 0.2133 0.1149 0.3479 0.106 Uiso 0.410(17) 1 calc PR A 1 H4B H 0.1196 0.1173 0.4044 0.106 Uiso 0.410(17) 1 calc PR A 1 H4C H 0.1453 0.2106 0.3431 0.106 Uiso 0.410(17) 1 calc PR A 1 C4 C 0.0625(10) 0.1472(5) 0.3444(4) 0.044(3) Uani 0.590(17) 1 d P A 2 H4D H 0.1574 0.1984 0.3287 0.066 Uiso 0.590(17) 1 calc PR A 2 H4E H 0.0626 0.1546 0.3905 0.066 Uiso 0.590(17) 1 calc PR A 2 H4F H 0.0087 0.1857 0.3260 0.066 Uiso 0.590(17) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.01899(19) 0.01899(19) 0.0522(4) 0.000 0.000 0.00949(10) N1 0.0270(12) 0.0249(12) 0.0609(17) 0.0078(11) 0.0075(11) 0.0142(10) N2 0.0192(11) 0.0192(11) 0.043(3) 0.000 0.000 0.0096(6) C1 0.071(2) 0.045(2) 0.067(3) 0.0238(18) 0.024(2) 0.0344(19) C2 0.0345(16) 0.0229(14) 0.092(3) 0.0018(16) 0.0064(16) 0.0165(13) C3 0.0219(14) 0.0219(14) 0.053(3) 0.000 0.000 0.0109(7) C41 0.051(7) 0.072(7) 0.027(5) 0.009(4) -0.023(4) -0.016(6) C4 0.053(5) 0.031(3) 0.036(4) -0.010(2) 0.007(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N2 1.757(4) . ? Nb1 N1 1.990(4) 2 ? Nb1 N1 1.990(4) 3 ? Nb1 N1 1.990(4) . ? N1 C1 1.445(5) . ? N1 C2 1.454(4) . ? N2 C3 1.437(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.486(6) . ? C3 C4 1.486(6) 2 ? C3 C4 1.486(6) 3 ? C3 C41 1.585(9) . ? C3 C41 1.585(9) 3 ? C3 C41 1.585(9) 2 ? C41 H4A 0.9800 . ? C41 H4B 0.9800 . ? C41 H4C 0.9800 . ? C4 H4D 0.9800 . ? C4 H4E 0.9800 . ? C4 H4F 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 N2 Nb1 N1 107.73(8) . 2 ? N2 Nb1 N1 107.73(8) . 3 ? N1 Nb1 N1 111.16(8) 2 3 ? N2 Nb1 N1 107.73(8) . . ? N1 Nb1 N1 111.16(8) 2 . ? N1 Nb1 N1 111.16(8) 3 . ? C1 N1 C2 111.3(3) . . ? C1 N1 Nb1 118.8(2) . . ? C2 N1 Nb1 129.9(2) . . ? C3 N2 Nb1 180.0 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 105.1(4) . . ? N2 C3 C4 105.1(4) . 2 ? C4 C3 C4 113.5(3) . 2 ? N2 C3 C4 105.1(4) . 3 ? C4 C3 C4 113.5(3) . 3 ? C4 C3 C4 113.5(3) 2 3 ? N2 C3 C41 115.6(4) . . ? C4 C3 C41 37.7(6) . . ? C4 C3 C41 134.4(6) 2 . ? C4 C3 C41 75.8(7) 3 . ? N2 C3 C41 115.6(4) . 3 ? C4 C3 C41 134.4(6) . 3 ? C4 C3 C41 75.8(7) 2 3 ? C4 C3 C41 37.7(6) 3 3 ? C41 C3 C41 102.7(5) . 3 ? N2 C3 C41 115.6(4) . 2 ? C4 C3 C41 75.8(7) . 2 ? C4 C3 C41 37.7(6) 2 2 ? C4 C3 C41 134.4(6) 3 2 ? C41 C3 C41 102.7(5) . 2 ? C41 C3 C41 102.7(5) 3 2 ? C3 C41 H4A 109.5 . . ? C3 C41 H4B 109.5 . . ? C3 C41 H4C 109.5 . . ? C3 C4 H4D 109.5 . . ? C3 C4 H4E 109.5 . . ? H4D C4 H4E 109.5 . . ? C3 C4 H4F 109.5 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Nb1 N1 C1 -161.6(2) . . . . ? N1 Nb1 N1 C1 -43.8(2) 2 . . . ? N1 Nb1 N1 C1 80.6(2) 3 . . . ? N2 Nb1 N1 C2 14.9(3) . . . . ? N1 Nb1 N1 C2 132.7(3) 2 . . . ? N1 Nb1 N1 C2 -102.9(3) 3 . . . ? N1 Nb1 N2 C3 0(100) 2 . . . ? N1 Nb1 N2 C3 0(100) 3 . . . ? N1 Nb1 N2 C3 0(100) . . . . ? Nb1 N2 C3 C4 0(100) . . . . ? Nb1 N2 C3 C4 0(100) . . . 2 ? Nb1 N2 C3 C4 0(100) . . . 3 ? Nb1 N2 C3 C41 0(100) . . . . ? Nb1 N2 C3 C41 0(100) . . . 3 ? Nb1 N2 C3 C41 0(100) . . . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.634 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.075 #=================================END data_cvd105 _database_code_depnum_ccdc_archive 'CCDC 637766' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H55 N8 Nb' _chemical_formula_weight 548.67 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.7356(8) _cell_length_b 18.2221(4) _cell_length_c 18.3713(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.094(4) _cell_angle_gamma 90.00 _cell_volume 6077.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 108(2) _cell_measurement_reflns_used 16722 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.940 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 108(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 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '620 images at 1.0 deg. in \w and 30 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61092 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13926 _reflns_number_gt 10574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0372P)^2^+5.9016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13926 _refine_ls_number_parameters 629 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.119577(11) 0.622016(11) 0.223805(12) 0.01351(6) Uani 1 1 d . . . Nb2 Nb 0.624042(11) 0.654541(11) 0.269945(12) 0.01340(6) Uani 1 1 d . . . N1 N 0.17400(11) 0.72951(11) 0.25640(12) 0.0180(4) Uani 1 1 d . . . N2 N 0.23109(11) 0.63407(12) 0.32877(12) 0.0202(4) Uani 1 1 d . . . N3 N 0.06611(11) 0.63537(11) 0.32103(12) 0.0173(4) Uani 1 1 d . . . N4 N 0.08443(11) 0.52904(11) 0.27139(11) 0.0158(4) Uani 1 1 d . . . N5 N 0.02495(11) 0.65645(11) 0.13813(12) 0.0185(4) Uani 1 1 d . . . N6 N 0.15662(11) 0.58165(11) 0.15932(12) 0.0170(4) Uani 1 1 d . . . N7 N 0.03308(12) 0.52361(12) 0.36932(13) 0.0219(5) Uani 1 1 d . . . N8 N 0.29257(12) 0.75071(13) 0.36147(14) 0.0279(5) Uani 1 1 d . . . C1 C 0.23399(13) 0.70505(14) 0.31607(14) 0.0193(5) Uani 1 1 d . . . C2 C 0.06007(12) 0.56366(13) 0.32190(13) 0.0159(5) Uani 1 1 d . . . C3 C 0.36720(15) 0.73395(18) 0.3723(2) 0.0380(7) Uani 1 1 d . . . H3A H 0.3679 0.6890 0.3433 0.057 Uiso 1 1 calc R . . H3B H 0.3971 0.7268 0.4287 0.057 Uiso 1 1 calc R . . H3C H 0.3874 0.7746 0.3522 0.057 Uiso 1 1 calc R . . C4 C 0.28096(16) 0.82148(15) 0.39029(17) 0.0296(6) Uani 1 1 d . . . H4A H 0.2280 0.8299 0.3743 0.044 Uiso 1 1 calc R . . H4B H 0.3017 0.8600 0.3680 0.044 Uiso 1 1 calc R . . H4C H 0.3053 0.8225 0.4481 0.044 Uiso 1 1 calc R . . C5 C 0.28218(14) 0.59660(16) 0.39941(15) 0.0248(6) Uani 1 1 d . . . H5 H 0.3139 0.6342 0.4371 0.030 Uiso 1 1 calc R . . C9 C 0.06379(15) 0.68219(14) 0.38480(15) 0.0235(6) Uani 1 1 d . . . H9 H 0.0610 0.6502 0.4278 0.028 Uiso 1 1 calc R . . C11 C 0.07351(15) 0.46160(15) 0.41589(16) 0.0262(6) Uani 1 1 d . . . H11A H 0.1132 0.4480 0.3990 0.039 Uiso 1 1 calc R . . H11B H 0.0400 0.4199 0.4080 0.039 Uiso 1 1 calc R . . H11C H 0.0946 0.4751 0.4720 0.039 Uiso 1 1 calc R . . C12 C -0.02794(15) 0.54855(15) 0.38763(17) 0.0274(6) Uani 1 1 d . . . H12A H -0.0092 0.5697 0.4409 0.041 Uiso 1 1 calc R . . H12B H -0.0602 0.5070 0.3852 0.041 Uiso 1 1 calc R . . H12C H -0.0558 0.5859 0.3491 0.041 Uiso 1 1 calc R . . C13 C 0.24079(16) 0.55404(18) 0.44015(17) 0.0353(7) Uani 1 1 d . . . H13A H 0.2092 0.5877 0.4543 0.053 Uiso 1 1 calc R . . H13B H 0.2761 0.5308 0.4882 0.053 Uiso 1 1 calc R . . H13C H 0.2104 0.5162 0.4043 0.053 Uiso 1 1 calc R . . C14 C 0.05665(14) 0.45641(13) 0.23880(15) 0.0191(5) Uani 1 1 d . . . H14 H 0.0317 0.4340 0.2714 0.023 Uiso 1 1 calc R . . C16 C 0.00535(15) 0.65115(16) 0.05314(15) 0.0263(6) Uani 1 1 d . . . H16A H -0.0380 0.6195 0.0295 0.040 Uiso 1 1 calc R . . H16B H 0.0467 0.6302 0.0433 0.040 Uiso 1 1 calc R . . H16C H -0.0058 0.7002 0.0295 0.040 Uiso 1 1 calc R . . C17 C -0.03687(15) 0.69057(17) 0.14998(17) 0.0308(6) Uani 1 1 d . . . H17A H -0.0476 0.7384 0.1234 0.046 Uiso 1 1 calc R . . H17B H -0.0242 0.6973 0.2067 0.046 Uiso 1 1 calc R . . H17C H -0.0803 0.6589 0.1278 0.046 Uiso 1 1 calc R . . C18 C 0.19151(14) 0.54858(14) 0.11049(15) 0.0208(5) Uani 1 1 d . . . C19 C 0.13256(17) 0.72959(16) 0.41911(17) 0.0337(7) Uani 1 1 d . . . H19A H 0.1763 0.6981 0.4389 0.051 Uiso 1 1 calc R . . H19B H 0.1304 0.7592 0.4627 0.051 Uiso 1 1 calc R . . H19C H 0.1353 0.7621 0.3778 0.051 Uiso 1 1 calc R . . C22 C 0.17020(14) 0.79916(14) 0.21520(15) 0.0225(5) Uani 1 1 d . . . H22 H 0.2167 0.8270 0.2442 0.027 Uiso 1 1 calc R . . C110 C 0.10588(18) 0.84442(16) 0.2159(2) 0.0391(7) Uani 1 1 d . . . H11D H 0.0597 0.8181 0.1872 0.059 Uiso 1 1 calc R . . H11E H 0.1049 0.8918 0.1903 0.059 Uiso 1 1 calc R . . H11F H 0.1115 0.8526 0.2707 0.059 Uiso 1 1 calc R . . C111 C -0.00362(18) 0.73273(16) 0.35525(18) 0.0345(7) Uani 1 1 d . . . H11G H 0.0000 0.7663 0.3153 0.052 Uiso 1 1 calc R . . H11H H -0.0055 0.7611 0.3997 0.052 Uiso 1 1 calc R . . H11I H -0.0484 0.7031 0.3318 0.052 Uiso 1 1 calc R . . C112 C 0.14169(16) 0.48858(16) 0.05755(17) 0.0313(6) Uani 1 1 d . . . H11J H 0.1341 0.4500 0.0907 0.047 Uiso 1 1 calc R . . H11K H 0.1651 0.4675 0.0241 0.047 Uiso 1 1 calc R . . H11L H 0.0941 0.5099 0.0240 0.047 Uiso 1 1 calc R . . C113 C 0.12171(15) 0.40769(15) 0.24482(17) 0.0276(6) Uani 1 1 d . . . H11M H 0.1499 0.4315 0.2178 0.041 Uiso 1 1 calc R . . H11N H 0.1034 0.3602 0.2198 0.041 Uiso 1 1 calc R . . H11O H 0.1536 0.4001 0.3006 0.041 Uiso 1 1 calc R . . C114 C 0.20522(17) 0.60694(16) 0.05863(18) 0.0313(6) Uani 1 1 d . . . H11V H 0.1582 0.6289 0.0242 0.047 Uiso 1 1 calc R . . H11W H 0.2288 0.5844 0.0261 0.047 Uiso 1 1 calc R . . H11Z H 0.2375 0.6451 0.0922 0.047 Uiso 1 1 calc R . . C115 C 0.26523(15) 0.51474(18) 0.16423(18) 0.0336(7) Uani 1 1 d . . . H11P H 0.2964 0.5526 0.1993 0.050 Uiso 1 1 calc R . . H11Q H 0.2899 0.4944 0.1317 0.050 Uiso 1 1 calc R . . H11R H 0.2565 0.4755 0.1961 0.050 Uiso 1 1 calc R . . C116 C 0.00067(15) 0.46315(15) 0.15385(16) 0.0259(6) Uani 1 1 d . . . H11S H -0.0409 0.4933 0.1526 0.039 Uiso 1 1 calc R . . H11T H -0.0172 0.4142 0.1329 0.039 Uiso 1 1 calc R . . H11U H 0.0240 0.4862 0.1214 0.039 Uiso 1 1 calc R . . C123 C 0.33155(17) 0.54340(18) 0.37905(19) 0.0394(8) Uani 1 1 d . . . H12D H 0.3013 0.5051 0.3437 0.059 Uiso 1 1 calc R . . H12E H 0.3665 0.5208 0.4277 0.059 Uiso 1 1 calc R . . H12F H 0.3587 0.5700 0.3526 0.059 Uiso 1 1 calc R . . C125 C 0.16379(19) 0.78637(17) 0.13121(17) 0.0373(7) Uani 1 1 d . . . H12G H 0.2080 0.7611 0.1323 0.056 Uiso 1 1 calc R . . H12H H 0.1588 0.8336 0.1041 0.056 Uiso 1 1 calc R . . H12I H 0.1204 0.7561 0.1029 0.056 Uiso 1 1 calc R . . N21 N 0.44485(12) 0.77414(12) 0.12497(14) 0.0283(5) Uani 1 1 d . . . N22 N 0.73250(12) 0.56179(12) 0.14304(13) 0.0237(5) Uani 1 1 d . . . N23 N 0.57154(11) 0.60075(12) 0.32793(12) 0.0200(4) Uani 1 1 d . . . N24 N 0.67115(11) 0.56076(11) 0.23219(12) 0.0164(4) Uani 1 1 d . . . N25 N 0.55855(11) 0.75260(11) 0.23765(12) 0.0175(4) Uani 1 1 d . . . N26 N 0.67208(11) 0.66657(11) 0.17454(12) 0.0172(4) Uani 1 1 d . . . N27 N 0.50965(11) 0.65978(11) 0.15352(12) 0.0173(4) Uani 1 1 d . . . N28 N 0.70312(11) 0.68276(11) 0.35270(11) 0.0169(4) Uani 1 1 d . . . C21 C 0.71280(17) 0.46200(16) 0.32940(18) 0.0356(7) Uani 1 1 d . . . H21A H 0.7630 0.4819 0.3503 0.053 Uiso 1 1 calc R . . H21B H 0.7148 0.4085 0.3356 0.053 Uiso 1 1 calc R . . H21C H 0.6852 0.4831 0.3585 0.053 Uiso 1 1 calc R . . C23 C 0.77398(13) 0.70210(14) 0.41334(15) 0.0209(5) Uani 1 1 d . . . C24 C 0.45707(17) 0.85067(16) 0.11131(19) 0.0357(7) Uani 1 1 d . . . H24A H 0.4398 0.8820 0.1438 0.054 Uiso 1 1 calc R . . H24B H 0.4299 0.8625 0.0553 0.054 Uiso 1 1 calc R . . H24C H 0.5098 0.8590 0.1256 0.054 Uiso 1 1 calc R . . C25 C 0.55211(17) 0.78207(18) 0.36544(17) 0.0357(7) Uani 1 1 d . . . H25A H 0.5164 0.7423 0.3570 0.054 Uiso 1 1 calc R . . H25B H 0.5416 0.8215 0.3957 0.054 Uiso 1 1 calc R . . H25C H 0.6020 0.7633 0.3949 0.054 Uiso 1 1 calc R . . C26 C 0.66448(19) 0.79521(16) 0.1381(2) 0.0378(7) Uani 1 1 d . . . H26A H 0.6116 0.7891 0.1072 0.057 Uiso 1 1 calc R . . H26B H 0.6839 0.8329 0.1134 0.057 Uiso 1 1 calc R . . H26C H 0.6727 0.8102 0.1921 0.057 Uiso 1 1 calc R . . C27 C 0.59785(16) 0.44727(15) 0.20680(18) 0.0296(6) Uani 1 1 d . . . H27A H 0.5679 0.4667 0.2342 0.044 Uiso 1 1 calc R . . H27B H 0.6019 0.3939 0.2133 0.044 Uiso 1 1 calc R . . H27C H 0.5745 0.4593 0.1504 0.044 Uiso 1 1 calc R . . C28 C 0.72258(17) 0.57953(16) 0.06294(17) 0.0324(7) Uani 1 1 d . . . H28A H 0.6726 0.5982 0.0342 0.049 Uiso 1 1 calc R . . H28B H 0.7300 0.5353 0.0366 0.049 Uiso 1 1 calc R . . H28C H 0.7584 0.6171 0.0637 0.049 Uiso 1 1 calc R . . C29 C 0.80332(16) 0.52856(17) 0.1900(2) 0.0351(7) Uani 1 1 d . . . H29A H 0.8430 0.5585 0.1860 0.053 Uiso 1 1 calc R . . H29B H 0.8054 0.4790 0.1701 0.053 Uiso 1 1 calc R . . H29C H 0.8093 0.5257 0.2454 0.053 Uiso 1 1 calc R . . C210 C 0.77549(15) 0.68457(19) 0.49552(16) 0.0333(7) Uani 1 1 d . . . H21D H 0.7354 0.7108 0.5031 0.050 Uiso 1 1 calc R . . H21E H 0.8228 0.7001 0.5361 0.050 Uiso 1 1 calc R . . H21F H 0.7693 0.6316 0.5000 0.050 Uiso 1 1 calc R . . C211 C 0.59755(16) 0.58914(18) 0.41304(16) 0.0330(7) Uani 1 1 d . . . H21G H 0.5644 0.6139 0.4333 0.050 Uiso 1 1 calc R . . H21H H 0.6473 0.6093 0.4391 0.050 Uiso 1 1 calc R . . H21I H 0.5984 0.5364 0.4240 0.050 Uiso 1 1 calc R . . C212 C 0.83304(14) 0.65598(16) 0.40017(16) 0.0251(6) Uani 1 1 d . . . H21V H 0.8237 0.6038 0.4053 0.038 Uiso 1 1 calc R . . H21W H 0.8817 0.6691 0.4398 0.038 Uiso 1 1 calc R . . H21Z H 0.8316 0.6655 0.3471 0.038 Uiso 1 1 calc R . . C213 C 0.42021(15) 0.56661(15) 0.07244(16) 0.0283(6) Uani 1 1 d . . . H21J H 0.4512 0.5259 0.1021 0.042 Uiso 1 1 calc R . . H21K H 0.3920 0.5512 0.0177 0.042 Uiso 1 1 calc R . . H21L H 0.3862 0.5807 0.0971 0.042 Uiso 1 1 calc R . . C214 C 0.78645(15) 0.73136(16) 0.18611(17) 0.0284(6) Uani 1 1 d . . . H21M H 0.7965 0.7476 0.2402 0.043 Uiso 1 1 calc R . . H21N H 0.8057 0.7677 0.1598 0.043 Uiso 1 1 calc R . . H21O H 0.8105 0.6840 0.1877 0.043 Uiso 1 1 calc R . . C215 C 0.49720(14) 0.57030(16) 0.29200(16) 0.0270(6) Uani 1 1 d . . . H21X H 0.4980 0.5188 0.3077 0.041 Uiso 1 1 calc R . . H21Y H 0.4796 0.5735 0.2343 0.041 Uiso 1 1 calc R . . H210 H 0.4642 0.5982 0.3100 0.041 Uiso 1 1 calc R . . C216 C 0.52152(16) 0.61082(16) 0.03492(15) 0.0287(6) Uani 1 1 d . . . H21P H 0.5519 0.6533 0.0346 0.043 Uiso 1 1 calc R . . H21Q H 0.4934 0.5946 -0.0195 0.043 Uiso 1 1 calc R . . H21R H 0.5534 0.5708 0.0650 0.043 Uiso 1 1 calc R . . C217 C 0.54649(14) 0.81159(15) 0.28610(16) 0.0258(6) Uani 1 1 d . . . H217 H 0.4955 0.8310 0.2575 0.031 Uiso 1 1 calc R . . C218 C 0.79008(16) 0.78373(16) 0.40860(18) 0.0332(7) Uani 1 1 d . . . H21S H 0.7842 0.7959 0.3545 0.050 Uiso 1 1 calc R . . H21T H 0.8407 0.7945 0.4452 0.050 Uiso 1 1 calc R . . H21U H 0.7556 0.8131 0.4231 0.050 Uiso 1 1 calc R . . C219 C 0.70357(14) 0.72324(14) 0.14043(15) 0.0211(5) Uani 1 1 d . . . H219 H 0.6944 0.7088 0.0848 0.025 Uiso 1 1 calc R . . C220 C 0.46880(14) 0.63210(14) 0.07313(14) 0.0212(5) Uani 1 1 d . . . H220 H 0.4363 0.6724 0.0411 0.025 Uiso 1 1 calc R . . C221 C 0.60028(16) 0.87474(15) 0.29717(19) 0.0339(7) Uani 1 1 d . . . H22A H 0.6509 0.8563 0.3216 0.051 Uiso 1 1 calc R . . H22B H 0.5925 0.9121 0.3315 0.051 Uiso 1 1 calc R . . H22C H 0.5921 0.8965 0.2456 0.051 Uiso 1 1 calc R . . C222 C 0.67457(14) 0.48141(13) 0.24193(16) 0.0215(5) Uani 1 1 d . . . H222 H 0.7043 0.4609 0.2134 0.026 Uiso 1 1 calc R . . C223 C 0.50340(13) 0.72858(14) 0.17161(15) 0.0191(5) Uani 1 1 d . . . C224 C 0.69294(13) 0.59704(14) 0.18178(14) 0.0168(5) Uani 1 1 d . . . C225 C 0.37019(15) 0.75461(17) 0.1121(2) 0.0378(7) Uani 1 1 d . . . H22D H 0.3678 0.7022 0.1227 0.057 Uiso 1 1 calc R . . H22E H 0.3377 0.7651 0.0571 0.057 Uiso 1 1 calc R . . H22F H 0.3543 0.7833 0.1477 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.01326(10) 0.01322(11) 0.01325(10) 0.00036(8) 0.00433(8) 0.00004(8) Nb2 0.01211(10) 0.01451(11) 0.01337(10) -0.00129(8) 0.00476(8) 0.00040(8) N1 0.0163(10) 0.0178(11) 0.0180(10) -0.0005(8) 0.0047(8) -0.0039(8) N2 0.0179(10) 0.0215(11) 0.0176(10) 0.0027(9) 0.0031(8) 0.0001(8) N3 0.0218(10) 0.0165(11) 0.0158(10) -0.0023(8) 0.0097(8) 0.0005(8) N4 0.0174(10) 0.0135(10) 0.0159(10) 0.0010(8) 0.0061(8) 0.0012(8) N5 0.0158(10) 0.0198(11) 0.0176(10) 0.0008(9) 0.0042(8) -0.0002(8) N6 0.0163(10) 0.0166(10) 0.0175(10) 0.0000(8) 0.0059(8) -0.0006(8) N7 0.0265(11) 0.0195(11) 0.0242(11) 0.0072(9) 0.0148(9) 0.0039(9) N8 0.0171(11) 0.0272(13) 0.0327(13) -0.0077(10) 0.0025(9) -0.0059(9) C1 0.0168(12) 0.0213(13) 0.0179(12) -0.0023(10) 0.0049(10) -0.0033(10) C2 0.0148(11) 0.0168(12) 0.0148(11) 0.0026(9) 0.0044(9) 0.0020(9) C3 0.0218(14) 0.0353(17) 0.051(2) 0.0002(15) 0.0085(13) -0.0077(12) C4 0.0316(15) 0.0249(14) 0.0254(14) -0.0028(12) 0.0039(12) -0.0103(12) C5 0.0164(12) 0.0313(15) 0.0191(13) 0.0062(11) -0.0013(10) 0.0004(11) C9 0.0337(15) 0.0209(13) 0.0208(13) -0.0041(11) 0.0160(11) -0.0024(11) C11 0.0278(14) 0.0257(14) 0.0269(14) 0.0117(11) 0.0126(12) 0.0025(11) C12 0.0278(14) 0.0277(15) 0.0337(15) -0.0005(12) 0.0195(12) -0.0017(11) C13 0.0264(15) 0.0457(19) 0.0279(15) 0.0189(14) 0.0043(12) 0.0054(13) C14 0.0226(12) 0.0122(12) 0.0239(13) -0.0008(10) 0.0107(10) -0.0024(9) C16 0.0229(13) 0.0332(15) 0.0183(13) 0.0022(11) 0.0032(10) 0.0029(11) C17 0.0243(14) 0.0400(17) 0.0251(14) 0.0019(13) 0.0065(11) 0.0110(12) C18 0.0232(13) 0.0216(13) 0.0203(12) -0.0002(10) 0.0115(10) 0.0016(10) C19 0.0471(18) 0.0304(16) 0.0288(15) -0.0142(13) 0.0204(14) -0.0107(13) C22 0.0244(13) 0.0157(12) 0.0230(13) 0.0005(10) 0.0045(11) -0.0079(10) C110 0.0386(17) 0.0197(15) 0.053(2) 0.0076(14) 0.0114(15) 0.0062(13) C111 0.0497(19) 0.0261(15) 0.0375(17) -0.0040(13) 0.0276(15) 0.0056(13) C112 0.0374(16) 0.0296(16) 0.0317(15) -0.0075(12) 0.0189(13) -0.0008(13) C113 0.0311(15) 0.0147(13) 0.0363(16) -0.0001(11) 0.0124(12) 0.0045(11) C114 0.0405(17) 0.0280(16) 0.0363(16) 0.0051(12) 0.0268(14) 0.0055(12) C115 0.0258(14) 0.0427(18) 0.0352(16) 0.0038(14) 0.0150(13) 0.0112(13) C116 0.0239(13) 0.0223(14) 0.0281(14) -0.0047(11) 0.0067(11) -0.0038(11) C123 0.0336(17) 0.046(2) 0.0371(17) 0.0178(15) 0.0117(14) 0.0181(14) C125 0.052(2) 0.0325(17) 0.0236(15) 0.0050(12) 0.0103(14) -0.0124(14) N21 0.0172(11) 0.0194(12) 0.0356(13) -0.0017(10) -0.0033(9) 0.0034(9) N22 0.0266(12) 0.0253(12) 0.0268(12) -0.0066(9) 0.0188(10) -0.0023(9) N23 0.0172(10) 0.0255(12) 0.0177(10) 0.0014(9) 0.0072(8) 0.0007(9) N24 0.0182(10) 0.0133(10) 0.0201(10) -0.0004(8) 0.0102(8) 0.0000(8) N25 0.0149(10) 0.0159(10) 0.0188(10) -0.0039(8) 0.0035(8) 0.0032(8) N26 0.0171(10) 0.0182(11) 0.0177(10) -0.0008(8) 0.0084(8) -0.0028(8) N27 0.0156(10) 0.0176(11) 0.0160(10) -0.0016(8) 0.0031(8) -0.0010(8) N28 0.0157(10) 0.0191(11) 0.0157(10) -0.0024(8) 0.0059(8) 0.0025(8) C21 0.0390(17) 0.0229(15) 0.0382(17) 0.0090(13) 0.0079(14) 0.0047(13) C23 0.0149(12) 0.0269(14) 0.0181(12) -0.0047(10) 0.0033(10) 0.0013(10) C24 0.0322(16) 0.0240(15) 0.0371(17) 0.0013(13) -0.0014(13) 0.0066(12) C25 0.0338(16) 0.0444(19) 0.0314(16) -0.0126(14) 0.0155(13) 0.0085(14) C26 0.051(2) 0.0226(15) 0.052(2) 0.0106(14) 0.0335(17) 0.0039(13) C27 0.0341(15) 0.0184(14) 0.0380(16) -0.0030(12) 0.0160(13) -0.0066(11) C28 0.0438(17) 0.0329(16) 0.0342(16) -0.0135(13) 0.0298(14) -0.0104(13) C29 0.0281(15) 0.0298(16) 0.057(2) -0.0042(14) 0.0275(15) 0.0023(12) C210 0.0216(14) 0.056(2) 0.0186(13) -0.0067(13) 0.0040(11) 0.0005(13) C211 0.0325(15) 0.0451(18) 0.0224(14) 0.0035(13) 0.0117(12) -0.0048(13) C212 0.0177(12) 0.0322(15) 0.0238(13) -0.0013(12) 0.0062(10) 0.0030(11) C213 0.0238(14) 0.0290(15) 0.0270(14) -0.0058(12) 0.0045(11) -0.0082(11) C214 0.0288(14) 0.0297(15) 0.0282(14) -0.0023(12) 0.0128(12) -0.0139(12) C215 0.0226(13) 0.0325(16) 0.0291(14) -0.0001(12) 0.0135(11) -0.0070(11) C216 0.0334(15) 0.0342(16) 0.0161(13) -0.0085(11) 0.0069(11) -0.0111(12) C217 0.0188(12) 0.0249(14) 0.0303(14) -0.0090(12) 0.0061(11) 0.0065(11) C218 0.0241(14) 0.0271(15) 0.0365(17) -0.0066(13) -0.0011(12) -0.0027(12) C219 0.0263(13) 0.0195(13) 0.0203(13) -0.0007(10) 0.0121(11) -0.0060(10) C220 0.0210(12) 0.0202(13) 0.0167(12) -0.0006(10) 0.0011(10) -0.0031(10) C221 0.0270(15) 0.0226(14) 0.0429(18) -0.0135(13) 0.0039(13) 0.0039(12) C222 0.0247(13) 0.0132(12) 0.0315(14) -0.0027(10) 0.0163(11) 0.0004(10) C223 0.0133(11) 0.0223(13) 0.0198(12) 0.0018(10) 0.0044(9) 0.0010(9) C224 0.0147(11) 0.0199(12) 0.0167(12) -0.0063(10) 0.0072(9) -0.0047(9) C225 0.0190(14) 0.0331(17) 0.0501(19) -0.0056(14) 0.0015(13) 0.0059(12) _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 N6 1.777(2) . ? Nb1 N5 2.013(2) . ? Nb1 N4 2.1427(19) . ? Nb1 N1 2.201(2) . ? Nb1 N2 2.298(2) . ? Nb1 N3 2.4170(19) . ? Nb1 C1 2.694(2) . ? Nb2 N28 1.775(2) . ? Nb2 N23 2.009(2) . ? Nb2 N25 2.148(2) . ? Nb2 N24 2.1843(19) . ? Nb2 N26 2.3069(19) . ? Nb2 N27 2.428(2) . ? N1 C1 1.336(3) . ? N1 C22 1.465(3) . ? N2 C1 1.319(3) . ? N2 C5 1.463(3) . ? N3 C2 1.313(3) . ? N3 C9 1.464(3) . ? N4 C2 1.357(3) . ? N4 C14 1.467(3) . ? N5 C16 1.457(3) . ? N5 C17 1.460(3) . ? N6 C18 1.458(3) . ? N7 C2 1.393(3) . ? N7 C12 1.445(3) . ? N7 C11 1.453(3) . ? N8 C1 1.403(3) . ? N8 C3 1.440(4) . ? N8 C4 1.446(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C13 1.519(4) . ? C5 C123 1.521(4) . ? C5 H5 1.0000 . ? C9 C19 1.521(4) . ? C9 C111 1.532(4) . ? C9 H9 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C116 1.523(4) . ? C14 C113 1.529(3) . ? C14 H14 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 C114 1.521(4) . ? C18 C115 1.531(4) . ? C18 C112 1.536(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C22 C125 1.516(4) . ? C22 C110 1.518(4) . ? C22 H22 1.0000 . ? C110 H11D 0.9800 . ? C110 H11E 0.9800 . ? C110 H11F 0.9800 . ? C111 H11G 0.9800 . ? C111 H11H 0.9800 . ? C111 H11I 0.9800 . ? C112 H11J 0.9800 . ? C112 H11K 0.9800 . ? C112 H11L 0.9800 . ? C113 H11M 0.9800 . ? C113 H11N 0.9800 . ? C113 H11O 0.9800 . ? C114 H11V 0.9800 . ? C114 H11W 0.9800 . ? C114 H11Z 0.9800 . ? C115 H11P 0.9800 . ? C115 H11Q 0.9800 . ? C115 H11R 0.9800 . ? C116 H11S 0.9800 . ? C116 H11T 0.9800 . ? C116 H11U 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C125 H12I 0.9800 . ? N21 C223 1.408(3) . ? N21 C225 1.442(4) . ? N21 C24 1.454(4) . ? N22 C224 1.402(3) . ? N22 C28 1.443(3) . ? N22 C29 1.455(4) . ? N23 C211 1.457(3) . ? N23 C215 1.462(3) . ? N24 C224 1.339(3) . ? N24 C222 1.455(3) . ? N25 C223 1.346(3) . ? N25 C217 1.473(3) . ? N26 C224 1.323(3) . ? N26 C219 1.467(3) . ? N27 C223 1.315(3) . ? N27 C220 1.467(3) . ? N28 C23 1.449(3) . ? C21 C222 1.525(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C218 1.531(4) . ? C23 C212 1.531(3) . ? C23 C210 1.532(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C217 1.516(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C219 1.514(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C222 1.526(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C210 H21D 0.9800 . ? C210 H21E 0.9800 . ? C210 H21F 0.9800 . ? C211 H21G 0.9800 . ? C211 H21H 0.9800 . ? C211 H21I 0.9800 . ? C212 H21V 0.9800 . ? C212 H21W 0.9800 . ? C212 H21Z 0.9800 . ? C213 C220 1.528(4) . ? C213 H21J 0.9800 . ? C213 H21K 0.9800 . ? C213 H21L 0.9800 . ? C214 C219 1.525(4) . ? C214 H21M 0.9800 . ? C214 H21N 0.9800 . ? C214 H21O 0.9800 . ? C215 H21X 0.9800 . ? C215 H21Y 0.9800 . ? C215 H210 0.9800 . ? C216 C220 1.516(4) . ? C216 H21P 0.9800 . ? C216 H21Q 0.9800 . ? C216 H21R 0.9800 . ? C217 C221 1.524(4) . ? C217 H217 1.0000 . ? C218 H21S 0.9800 . ? C218 H21T 0.9800 . ? C218 H21U 0.9800 . ? C219 H219 1.0000 . ? C220 H220 1.0000 . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C222 H222 1.0000 . ? C225 H22D 0.9800 . ? C225 H22E 0.9800 . ? C225 H22F 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 N6 Nb1 N5 96.08(9) . . ? N6 Nb1 N4 103.20(8) . . ? N5 Nb1 N4 102.47(8) . . ? N6 Nb1 N1 105.38(8) . . ? N5 Nb1 N1 98.01(8) . . ? N4 Nb1 N1 142.57(7) . . ? N6 Nb1 N2 95.16(8) . . ? N5 Nb1 N2 156.30(8) . . ? N4 Nb1 N2 95.17(7) . . ? N1 Nb1 N2 58.81(7) . . ? N6 Nb1 N3 161.32(8) . . ? N5 Nb1 N3 90.36(8) . . ? N4 Nb1 N3 58.20(7) . . ? N1 Nb1 N3 90.98(7) . . ? N2 Nb1 N3 85.55(7) . . ? N6 Nb1 C1 100.92(8) . . ? N5 Nb1 C1 127.47(8) . . ? N4 Nb1 C1 120.86(7) . . ? N1 Nb1 C1 29.53(7) . . ? N2 Nb1 C1 29.30(7) . . ? N3 Nb1 C1 88.83(7) . . ? N28 Nb2 N23 98.64(9) . . ? N28 Nb2 N25 103.14(8) . . ? N23 Nb2 N25 99.94(8) . . ? N28 Nb2 N24 99.09(8) . . ? N23 Nb2 N24 99.15(8) . . ? N25 Nb2 N24 148.00(8) . . ? N28 Nb2 N26 97.93(8) . . ? N23 Nb2 N26 154.21(8) . . ? N25 Nb2 N26 95.35(8) . . ? N24 Nb2 N26 58.68(7) . . ? N28 Nb2 N27 160.87(8) . . ? N23 Nb2 N27 89.52(8) . . ? N25 Nb2 N27 58.20(7) . . ? N24 Nb2 N27 96.63(7) . . ? N26 Nb2 N27 81.03(7) . . ? C1 N1 C22 124.2(2) . . ? C1 N1 Nb1 96.15(15) . . ? C22 N1 Nb1 135.23(16) . . ? C1 N2 C5 123.5(2) . . ? C1 N2 Nb1 92.23(14) . . ? C5 N2 Nb1 143.09(17) . . ? C2 N3 C9 122.6(2) . . ? C2 N3 Nb1 88.67(14) . . ? C9 N3 Nb1 144.06(16) . . ? C2 N4 C14 121.5(2) . . ? C2 N4 Nb1 99.77(14) . . ? C14 N4 Nb1 132.51(15) . . ? C16 N5 C17 107.6(2) . . ? C16 N5 Nb1 126.30(16) . . ? C17 N5 Nb1 126.12(17) . . ? C18 N6 Nb1 176.43(17) . . ? C2 N7 C12 122.6(2) . . ? C2 N7 C11 121.3(2) . . ? C12 N7 C11 115.0(2) . . ? C1 N8 C3 121.1(2) . . ? C1 N8 C4 122.3(2) . . ? C3 N8 C4 116.0(2) . . ? N2 C1 N1 112.7(2) . . ? N2 C1 N8 124.0(2) . . ? N1 C1 N8 123.3(2) . . ? N2 C1 Nb1 58.47(12) . . ? N1 C1 Nb1 54.32(12) . . ? N8 C1 Nb1 177.44(19) . . ? N3 C2 N4 113.3(2) . . ? N3 C2 N7 126.0(2) . . ? N4 C2 N7 120.6(2) . . ? N8 C3 H3A 109.5 . . ? N8 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N8 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N8 C4 H4A 109.5 . . ? N8 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N8 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C13 111.0(2) . . ? N2 C5 C123 111.4(2) . . ? C13 C5 C123 108.4(2) . . ? N2 C5 H5 108.7 . . ? C13 C5 H5 108.7 . . ? C123 C5 H5 108.7 . . ? N3 C9 C19 111.1(2) . . ? N3 C9 C111 111.2(2) . . ? C19 C9 C111 108.4(2) . . ? N3 C9 H9 108.7 . . ? C19 C9 H9 108.7 . . ? C111 C9 H9 108.7 . . ? N7 C11 H11A 109.5 . . ? N7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 H12A 109.5 . . ? N7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C116 110.5(2) . . ? N4 C14 C113 109.0(2) . . ? C116 C14 C113 111.8(2) . . ? N4 C14 H14 108.5 . . ? C116 C14 H14 108.5 . . ? C113 C14 H14 108.5 . . ? N5 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N6 C18 C114 109.8(2) . . ? N6 C18 C115 109.2(2) . . ? C114 C18 C115 109.1(2) . . ? N6 C18 C112 110.1(2) . . ? C114 C18 C112 109.1(2) . . ? C115 C18 C112 109.4(2) . . ? C9 C19 H19A 109.5 . . ? C9 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C22 C125 111.1(2) . . ? N1 C22 C110 109.9(2) . . ? C125 C22 C110 110.9(2) . . ? N1 C22 H22 108.3 . . ? C125 C22 H22 108.3 . . ? C110 C22 H22 108.3 . . ? C22 C110 H11D 109.5 . . ? C22 C110 H11E 109.5 . . ? H11D C110 H11E 109.5 . . ? C22 C110 H11F 109.5 . . ? H11D C110 H11F 109.5 . . ? H11E C110 H11F 109.5 . . ? C9 C111 H11G 109.5 . . ? C9 C111 H11H 109.5 . . ? H11G C111 H11H 109.5 . . ? C9 C111 H11I 109.5 . . ? H11G C111 H11I 109.5 . . ? H11H C111 H11I 109.5 . . ? C18 C112 H11J 109.5 . . ? C18 C112 H11K 109.5 . . ? H11J C112 H11K 109.5 . . ? C18 C112 H11L 109.5 . . ? H11J C112 H11L 109.5 . . ? H11K C112 H11L 109.5 . . ? C14 C113 H11M 109.5 . . ? C14 C113 H11N 109.5 . . ? H11M C113 H11N 109.5 . . ? C14 C113 H11O 109.5 . . ? H11M C113 H11O 109.5 . . ? H11N C113 H11O 109.5 . . ? C18 C114 H11V 109.5 . . ? C18 C114 H11W 109.5 . . ? H11V C114 H11W 109.5 . . ? C18 C114 H11Z 109.5 . . ? H11V C114 H11Z 109.5 . . ? H11W C114 H11Z 109.5 . . ? C18 C115 H11P 109.5 . . ? C18 C115 H11Q 109.5 . . ? H11P C115 H11Q 109.5 . . ? C18 C115 H11R 109.5 . . ? H11P C115 H11R 109.5 . . ? H11Q C115 H11R 109.5 . . ? C14 C116 H11S 109.5 . . ? C14 C116 H11T 109.5 . . ? H11S C116 H11T 109.5 . . ? C14 C116 H11U 109.5 . . ? H11S C116 H11U 109.5 . . ? H11T C116 H11U 109.5 . . ? C5 C123 H12D 109.5 . . ? C5 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C5 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C22 C125 H12G 109.5 . . ? C22 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C22 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C223 N21 C225 119.8(2) . . ? C223 N21 C24 121.2(2) . . ? C225 N21 C24 115.9(2) . . ? C224 N22 C28 122.4(2) . . ? C224 N22 C29 119.1(2) . . ? C28 N22 C29 114.3(2) . . ? C211 N23 C215 107.4(2) . . ? C211 N23 Nb2 127.01(17) . . ? C215 N23 Nb2 125.51(16) . . ? C224 N24 C222 124.3(2) . . ? C224 N24 Nb2 97.22(15) . . ? C222 N24 Nb2 138.01(15) . . ? C223 N25 C217 121.1(2) . . ? C223 N25 Nb2 99.48(15) . . ? C217 N25 Nb2 131.49(16) . . ? C224 N26 C219 123.4(2) . . ? C224 N26 Nb2 92.13(14) . . ? C219 N26 Nb2 139.53(16) . . ? C223 N27 C220 120.9(2) . . ? C223 N27 Nb2 87.81(14) . . ? C220 N27 Nb2 145.85(16) . . ? C23 N28 Nb2 171.26(17) . . ? C222 C21 H21A 109.5 . . ? C222 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C222 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N28 C23 C218 110.6(2) . . ? N28 C23 C212 108.1(2) . . ? C218 C23 C212 109.7(2) . . ? N28 C23 C210 110.3(2) . . ? C218 C23 C210 109.5(2) . . ? C212 C23 C210 108.6(2) . . ? N21 C24 H24A 109.5 . . ? N21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C217 C25 H25A 109.5 . . ? C217 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C217 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C219 C26 H26A 109.5 . . ? C219 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C219 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C222 C27 H27A 109.5 . . ? C222 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C222 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N22 C28 H28A 109.5 . . ? N22 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N22 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N22 C29 H29A 109.5 . . ? N22 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N22 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 C210 H21D 109.5 . . ? C23 C210 H21E 109.5 . . ? H21D C210 H21E 109.5 . . ? C23 C210 H21F 109.5 . . ? H21D C210 H21F 109.5 . . ? H21E C210 H21F 109.5 . . ? N23 C211 H21G 109.5 . . ? N23 C211 H21H 109.5 . . ? H21G C211 H21H 109.5 . . ? N23 C211 H21I 109.5 . . ? H21G C211 H21I 109.5 . . ? H21H C211 H21I 109.5 . . ? C23 C212 H21V 109.5 . . ? C23 C212 H21W 109.5 . . ? H21V C212 H21W 109.5 . . ? C23 C212 H21Z 109.5 . . ? H21V C212 H21Z 109.5 . . ? H21W C212 H21Z 109.5 . . ? C220 C213 H21J 109.5 . . ? C220 C213 H21K 109.5 . . ? H21J C213 H21K 109.5 . . ? C220 C213 H21L 109.5 . . ? H21J C213 H21L 109.5 . . ? H21K C213 H21L 109.5 . . ? C219 C214 H21M 109.5 . . ? C219 C214 H21N 109.5 . . ? H21M C214 H21N 109.5 . . ? C219 C214 H21O 109.5 . . ? H21M C214 H21O 109.5 . . ? H21N C214 H21O 109.5 . . ? N23 C215 H21X 109.5 . . ? N23 C215 H21Y 109.5 . . ? H21X C215 H21Y 109.5 . . ? N23 C215 H210 109.5 . . ? H21X C215 H210 109.5 . . ? H21Y C215 H210 109.5 . . ? C220 C216 H21P 109.5 . . ? C220 C216 H21Q 109.5 . . ? H21P C216 H21Q 109.5 . . ? C220 C216 H21R 109.5 . . ? H21P C216 H21R 109.5 . . ? H21Q C216 H21R 109.5 . . ? N25 C217 C25 110.7(2) . . ? N25 C217 C221 111.3(2) . . ? C25 C217 C221 110.8(2) . . ? N25 C217 H217 108.0 . . ? C25 C217 H217 108.0 . . ? C221 C217 H217 108.0 . . ? C23 C218 H21S 109.5 . . ? C23 C218 H21T 109.5 . . ? H21S C218 H21T 109.5 . . ? C23 C218 H21U 109.5 . . ? H21S C218 H21U 109.5 . . ? H21T C218 H21U 109.5 . . ? N26 C219 C26 109.0(2) . . ? N26 C219 C214 112.1(2) . . ? C26 C219 C214 110.9(2) . . ? N26 C219 H219 108.3 . . ? C26 C219 H219 108.3 . . ? C214 C219 H219 108.3 . . ? N27 C220 C216 110.4(2) . . ? N27 C220 C213 111.9(2) . . ? C216 C220 C213 109.8(2) . . ? N27 C220 H220 108.2 . . ? C216 C220 H220 108.2 . . ? C213 C220 H220 108.2 . . ? C217 C221 H22A 109.5 . . ? C217 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C217 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? N24 C222 C21 109.9(2) . . ? N24 C222 C27 111.3(2) . . ? C21 C222 C27 110.5(2) . . ? N24 C222 H222 108.4 . . ? C21 C222 H222 108.4 . . ? C27 C222 H222 108.4 . . ? N27 C223 N25 114.5(2) . . ? N27 C223 N21 123.0(2) . . ? N25 C223 N21 122.5(2) . . ? N26 C224 N24 111.8(2) . . ? N26 C224 N22 127.0(2) . . ? N24 C224 N22 121.3(2) . . ? N21 C225 H22D 109.5 . . ? N21 C225 H22E 109.5 . . ? H22D C225 H22E 109.5 . . ? N21 C225 H22F 109.5 . . ? H22D C225 H22F 109.5 . . ? H22E C225 H22F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Nb1 N1 C1 -85.00(16) . . . . ? N5 Nb1 N1 C1 176.39(15) . . . . ? N4 Nb1 N1 C1 53.5(2) . . . . ? N2 Nb1 N1 C1 1.70(14) . . . . ? N3 Nb1 N1 C1 85.89(15) . . . . ? N6 Nb1 N1 C22 70.8(2) . . . . ? N5 Nb1 N1 C22 -27.8(2) . . . . ? N4 Nb1 N1 C22 -150.7(2) . . . . ? N2 Nb1 N1 C22 157.5(3) . . . . ? N3 Nb1 N1 C22 -118.3(2) . . . . ? C1 Nb1 N1 C22 155.8(3) . . . . ? N6 Nb1 N2 C1 103.17(15) . . . . ? N5 Nb1 N2 C1 -14.9(3) . . . . ? N4 Nb1 N2 C1 -153.04(15) . . . . ? N1 Nb1 N2 C1 -1.71(14) . . . . ? N3 Nb1 N2 C1 -95.57(15) . . . . ? N6 Nb1 N2 C5 -90.5(3) . . . . ? N5 Nb1 N2 C5 151.4(3) . . . . ? N4 Nb1 N2 C5 13.2(3) . . . . ? N1 Nb1 N2 C5 164.6(3) . . . . ? N3 Nb1 N2 C5 70.7(3) . . . . ? C1 Nb1 N2 C5 166.3(4) . . . . ? N6 Nb1 N3 C2 -5.4(3) . . . . ? N5 Nb1 N3 C2 105.03(14) . . . . ? N4 Nb1 N3 C2 0.54(13) . . . . ? N1 Nb1 N3 C2 -156.95(14) . . . . ? N2 Nb1 N3 C2 -98.35(14) . . . . ? C1 Nb1 N3 C2 -127.50(14) . . . . ? N6 Nb1 N3 C9 146.9(3) . . . . ? N5 Nb1 N3 C9 -102.6(3) . . . . ? N4 Nb1 N3 C9 152.9(3) . . . . ? N1 Nb1 N3 C9 -4.6(3) . . . . ? N2 Nb1 N3 C9 54.0(3) . . . . ? C1 Nb1 N3 C9 24.9(3) . . . . ? N6 Nb1 N4 C2 177.51(14) . . . . ? N5 Nb1 N4 C2 -83.10(15) . . . . ? N1 Nb1 N4 C2 38.5(2) . . . . ? N2 Nb1 N4 C2 80.97(14) . . . . ? N3 Nb1 N4 C2 -0.53(13) . . . . ? C1 Nb1 N4 C2 65.99(16) . . . . ? N6 Nb1 N4 C14 -31.2(2) . . . . ? N5 Nb1 N4 C14 68.2(2) . . . . ? N1 Nb1 N4 C14 -170.20(18) . . . . ? N2 Nb1 N4 C14 -127.7(2) . . . . ? N3 Nb1 N4 C14 150.8(2) . . . . ? C1 Nb1 N4 C14 -142.71(19) . . . . ? N6 Nb1 N5 C16 -4.7(2) . . . . ? N4 Nb1 N5 C16 -109.6(2) . . . . ? N1 Nb1 N5 C16 101.9(2) . . . . ? N2 Nb1 N5 C16 113.2(2) . . . . ? N3 Nb1 N5 C16 -167.1(2) . . . . ? C1 Nb1 N5 C16 104.1(2) . . . . ? N6 Nb1 N5 C17 174.6(2) . . . . ? N4 Nb1 N5 C17 69.6(2) . . . . ? N1 Nb1 N5 C17 -78.9(2) . . . . ? N2 Nb1 N5 C17 -67.5(3) . . . . ? N3 Nb1 N5 C17 12.2(2) . . . . ? C1 Nb1 N5 C17 -76.6(2) . . . . ? N5 Nb1 N6 C18 163(3) . . . . ? N4 Nb1 N6 C18 -93(3) . . . . ? N1 Nb1 N6 C18 63(3) . . . . ? N2 Nb1 N6 C18 4(3) . . . . ? N3 Nb1 N6 C18 -88(3) . . . . ? C1 Nb1 N6 C18 33(3) . . . . ? C5 N2 C1 N1 -167.6(2) . . . . ? Nb1 N2 C1 N1 2.6(2) . . . . ? C5 N2 C1 N8 10.7(4) . . . . ? Nb1 N2 C1 N8 -179.1(2) . . . . ? C5 N2 C1 Nb1 -170.2(3) . . . . ? C22 N1 C1 N2 -162.3(2) . . . . ? Nb1 N1 C1 N2 -2.7(2) . . . . ? C22 N1 C1 N8 19.4(4) . . . . ? Nb1 N1 C1 N8 179.0(2) . . . . ? C22 N1 C1 Nb1 -159.6(3) . . . . ? C3 N8 C1 N2 54.9(4) . . . . ? C4 N8 C1 N2 -134.0(3) . . . . ? C3 N8 C1 N1 -127.0(3) . . . . ? C4 N8 C1 N1 44.1(4) . . . . ? C3 N8 C1 Nb1 -108(4) . . . . ? C4 N8 C1 Nb1 63(4) . . . . ? N6 Nb1 C1 N2 -80.98(16) . . . . ? N5 Nb1 C1 N2 172.53(14) . . . . ? N4 Nb1 C1 N2 31.73(17) . . . . ? N1 Nb1 C1 N2 177.0(2) . . . . ? N3 Nb1 C1 N2 82.97(15) . . . . ? N6 Nb1 C1 N1 101.98(15) . . . . ? N5 Nb1 C1 N1 -4.50(18) . . . . ? N4 Nb1 C1 N1 -145.30(14) . . . . ? N2 Nb1 C1 N1 -177.0(2) . . . . ? N3 Nb1 C1 N1 -94.06(15) . . . . ? N6 Nb1 C1 N8 82(4) . . . . ? N5 Nb1 C1 N8 -24(4) . . . . ? N4 Nb1 C1 N8 -165(4) . . . . ? N1 Nb1 C1 N8 -20(4) . . . . ? N2 Nb1 C1 N8 163(4) . . . . ? N3 Nb1 C1 N8 -114(4) . . . . ? C9 N3 C2 N4 -161.9(2) . . . . ? Nb1 N3 C2 N4 -0.80(19) . . . . ? C9 N3 C2 N7 17.0(4) . . . . ? Nb1 N3 C2 N7 178.2(2) . . . . ? C14 N4 C2 N3 -154.6(2) . . . . ? Nb1 N4 C2 N3 0.9(2) . . . . ? C14 N4 C2 N7 26.4(3) . . . . ? Nb1 N4 C2 N7 -178.12(18) . . . . ? C12 N7 C2 N3 37.7(4) . . . . ? C11 N7 C2 N3 -130.0(3) . . . . ? C12 N7 C2 N4 -143.4(2) . . . . ? C11 N7 C2 N4 48.9(3) . . . . ? C1 N2 C5 C13 126.1(3) . . . . ? Nb1 N2 C5 C13 -37.4(4) . . . . ? C1 N2 C5 C123 -113.0(3) . . . . ? Nb1 N2 C5 C123 83.5(3) . . . . ? C2 N3 C9 C19 123.8(3) . . . . ? Nb1 N3 C9 C19 -22.8(4) . . . . ? C2 N3 C9 C111 -115.4(3) . . . . ? Nb1 N3 C9 C111 98.0(3) . . . . ? C2 N4 C14 C116 102.4(3) . . . . ? Nb1 N4 C14 C116 -43.9(3) . . . . ? C2 N4 C14 C113 -134.3(2) . . . . ? Nb1 N4 C14 C113 79.4(3) . . . . ? Nb1 N6 C18 C114 -100(3) . . . . ? Nb1 N6 C18 C115 20(3) . . . . ? Nb1 N6 C18 C112 140(3) . . . . ? C1 N1 C22 C125 110.9(3) . . . . ? Nb1 N1 C22 C125 -39.6(3) . . . . ? C1 N1 C22 C110 -126.1(3) . . . . ? Nb1 N1 C22 C110 83.4(3) . . . . ? N28 Nb2 N23 C211 -2.2(2) . . . . ? N25 Nb2 N23 C211 -107.3(2) . . . . ? N24 Nb2 N23 C211 98.5(2) . . . . ? N26 Nb2 N23 C211 127.2(2) . . . . ? N27 Nb2 N23 C211 -164.8(2) . . . . ? N28 Nb2 N23 C215 173.3(2) . . . . ? N25 Nb2 N23 C215 68.2(2) . . . . ? N24 Nb2 N23 C215 -86.0(2) . . . . ? N26 Nb2 N23 C215 -57.3(3) . . . . ? N27 Nb2 N23 C215 10.6(2) . . . . ? N28 Nb2 N24 C224 -90.96(15) . . . . ? N23 Nb2 N24 C224 168.68(14) . . . . ? N25 Nb2 N24 C224 42.7(2) . . . . ? N26 Nb2 N24 C224 2.84(13) . . . . ? N27 Nb2 N24 C224 78.10(15) . . . . ? N28 Nb2 N24 C222 97.2(2) . . . . ? N23 Nb2 N24 C222 -3.2(3) . . . . ? N25 Nb2 N24 C222 -129.2(2) . . . . ? N26 Nb2 N24 C222 -169.0(3) . . . . ? N27 Nb2 N24 C222 -93.8(2) . . . . ? N28 Nb2 N25 C223 175.23(15) . . . . ? N23 Nb2 N25 C223 -83.38(16) . . . . ? N24 Nb2 N25 C223 42.4(2) . . . . ? N26 Nb2 N25 C223 75.77(15) . . . . ? N27 Nb2 N25 C223 -0.20(13) . . . . ? N28 Nb2 N25 C217 -36.9(2) . . . . ? N23 Nb2 N25 C217 64.5(2) . . . . ? N24 Nb2 N25 C217 -169.70(19) . . . . ? N26 Nb2 N25 C217 -136.3(2) . . . . ? N27 Nb2 N25 C217 147.7(2) . . . . ? N28 Nb2 N26 C224 93.00(15) . . . . ? N23 Nb2 N26 C224 -36.6(2) . . . . ? N25 Nb2 N26 C224 -162.91(14) . . . . ? N24 Nb2 N26 C224 -2.85(13) . . . . ? N27 Nb2 N26 C224 -106.32(14) . . . . ? N28 Nb2 N26 C219 -60.1(3) . . . . ? N23 Nb2 N26 C219 170.3(2) . . . . ? N25 Nb2 N26 C219 44.0(2) . . . . ? N24 Nb2 N26 C219 -155.9(3) . . . . ? N27 Nb2 N26 C219 100.6(2) . . . . ? N28 Nb2 N27 C223 -13.5(3) . . . . ? N23 Nb2 N27 C223 102.24(15) . . . . ? N25 Nb2 N27 C223 0.21(14) . . . . ? N24 Nb2 N27 C223 -158.61(14) . . . . ? N26 Nb2 N27 C223 -101.85(15) . . . . ? N28 Nb2 N27 C220 135.7(3) . . . . ? N23 Nb2 N27 C220 -108.6(3) . . . . ? N25 Nb2 N27 C220 149.4(3) . . . . ? N24 Nb2 N27 C220 -9.4(3) . . . . ? N26 Nb2 N27 C220 47.3(3) . . . . ? N23 Nb2 N28 C23 134.7(12) . . . . ? N25 Nb2 N28 C23 -122.9(12) . . . . ? N24 Nb2 N28 C23 34.0(12) . . . . ? N26 Nb2 N28 C23 -25.4(12) . . . . ? N27 Nb2 N28 C23 -110.9(12) . . . . ? Nb2 N28 C23 C218 97.0(12) . . . . ? Nb2 N28 C23 C212 -23.1(13) . . . . ? Nb2 N28 C23 C210 -141.7(11) . . . . ? C223 N25 C217 C25 111.7(3) . . . . ? Nb2 N25 C217 C25 -30.5(3) . . . . ? C223 N25 C217 C221 -124.6(3) . . . . ? Nb2 N25 C217 C221 93.2(3) . . . . ? C224 N26 C219 C26 177.5(2) . . . . ? Nb2 N26 C219 C26 -35.3(3) . . . . ? C224 N26 C219 C214 -59.4(3) . . . . ? Nb2 N26 C219 C214 87.8(3) . . . . ? C223 N27 C220 C216 114.3(3) . . . . ? Nb2 N27 C220 C216 -29.0(4) . . . . ? C223 N27 C220 C213 -123.1(2) . . . . ? Nb2 N27 C220 C213 93.6(3) . . . . ? C224 N24 C222 C21 129.2(3) . . . . ? Nb2 N24 C222 C21 -60.5(3) . . . . ? C224 N24 C222 C27 -108.1(3) . . . . ? Nb2 N24 C222 C27 62.1(3) . . . . ? C220 N27 C223 N25 -160.7(2) . . . . ? Nb2 N27 C223 N25 -0.3(2) . . . . ? C220 N27 C223 N21 17.9(4) . . . . ? Nb2 N27 C223 N21 178.3(2) . . . . ? C217 N25 C223 N27 -151.9(2) . . . . ? Nb2 N25 C223 N27 0.4(2) . . . . ? C217 N25 C223 N21 29.5(4) . . . . ? Nb2 N25 C223 N21 -178.3(2) . . . . ? C225 N21 C223 N27 60.8(4) . . . . ? C24 N21 C223 N27 -140.1(3) . . . . ? C225 N21 C223 N25 -120.8(3) . . . . ? C24 N21 C223 N25 38.4(4) . . . . ? C219 N26 C224 N24 163.7(2) . . . . ? Nb2 N26 C224 N24 4.3(2) . . . . ? C219 N26 C224 N22 -16.8(4) . . . . ? Nb2 N26 C224 N22 -176.2(2) . . . . ? C222 N24 C224 N26 168.9(2) . . . . ? Nb2 N24 C224 N26 -4.6(2) . . . . ? C222 N24 C224 N22 -10.7(4) . . . . ? Nb2 N24 C224 N22 175.88(19) . . . . ? C28 N22 C224 N26 -35.2(4) . . . . ? C29 N22 C224 N26 120.5(3) . . . . ? C28 N22 C224 N24 144.3(2) . . . . ? C29 N22 C224 N24 -60.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.966 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.083 #=================================END data_cvd81 _database_code_depnum_ccdc_archive 'CCDC 637767' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H67 N8 Nb' _chemical_formula_weight 632.83 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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.4815(9) _cell_length_b 18.2528(18) _cell_length_c 34.814(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7295.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 108(2) _cell_measurement_reflns_used 3342 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.931 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details 'Gaussian face-indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 108(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 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 35 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56871 _diffrn_reflns_av_R_equivalents 0.1846 _diffrn_reflns_av_sigmaI/netI 0.1508 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6417 _reflns_number_gt 4000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6417 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1845 _refine_ls_R_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _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 0.02353(5) 0.17453(3) 0.122858(17) 0.02311(19) Uani 1 1 d . . . N5 N 0.1167(5) 0.2639(3) 0.13697(15) 0.0261(16) Uani 1 1 d . . . N6 N -0.0998(5) 0.2233(3) 0.10681(15) 0.0276(15) Uani 1 1 d . . . N3 N -0.0698(5) 0.0641(3) 0.12914(15) 0.0288(15) Uani 1 1 d . . . C13 C -0.1517(7) 0.2157(5) 0.2177(2) 0.051(3) Uani 1 1 d . . . H11A H -0.2215 0.1913 0.2077 0.076 Uiso 1 1 calc R . . H11B H -0.1320 0.2573 0.2011 0.076 Uiso 1 1 calc R . . H11C H -0.1667 0.2333 0.2438 0.076 Uiso 1 1 calc R . . N4 N -0.0261(5) 0.1327(3) 0.17980(14) 0.0253(14) Uani 1 1 d . . . C8 C -0.0081(9) -0.0359(5) 0.0871(3) 0.076(4) Uani 1 1 d . . . H12A H 0.0564 -0.0468 0.1046 0.114 Uiso 1 1 calc R . . H12B H 0.0182 -0.0014 0.0674 0.114 Uiso 1 1 calc R . . H12C H -0.0345 -0.0813 0.0748 0.114 Uiso 1 1 calc R . . C12 C -0.0775(7) -0.0156(4) 0.2208(2) 0.043(2) Uani 1 1 d . . . H13A H -0.1175 -0.0071 0.2456 0.052 Uiso 1 1 calc R . . H13B H 0.0016 0.0056 0.2229 0.052 Uiso 1 1 calc R . . N7 N -0.1402(6) 0.0232(3) 0.19104(16) 0.0300(16) Uani 1 1 d . . . C2 C -0.0799(6) 0.0720(4) 0.1673(2) 0.0229(18) Uani 1 1 d . . . C9 C -0.1074(7) -0.0025(4) 0.1094(2) 0.037(2) Uani 1 1 d . . . H15A H -0.1344 -0.0386 0.1291 0.045 Uiso 1 1 calc R . . C14 C -0.0507(6) 0.1617(4) 0.21826(18) 0.0263(19) Uani 1 1 d . . . H16A H -0.0720 0.1199 0.2354 0.032 Uiso 1 1 calc R . . N8 N 0.2782(5) 0.0669(3) 0.06144(15) 0.0243(15) Uani 1 1 d . . . C23 C 0.1313(7) 0.2541(4) 0.0339(2) 0.038(2) Uani 1 1 d . . . H21A H 0.2045 0.2635 0.0476 0.056 Uiso 1 1 calc R . . H21B H 0.0668 0.2772 0.0478 0.056 Uiso 1 1 calc R . . H21C H 0.1360 0.2745 0.0079 0.056 Uiso 1 1 calc R . . N1 N 0.1061(5) 0.1402(3) 0.07034(14) 0.0206(14) Uani 1 1 d . . . C6 C 0.3705(8) 0.0892(5) 0.1677(2) 0.062(3) Uani 1 1 d . . . H22A H 0.4193 0.1172 0.1499 0.092 Uiso 1 1 calc R . . H22B H 0.4182 0.0523 0.1808 0.092 Uiso 1 1 calc R . . H22C H 0.3365 0.1225 0.1867 0.092 Uiso 1 1 calc R . . N2 N 0.2009(5) 0.1039(3) 0.12327(16) 0.0290(15) Uani 1 1 d . . . C24 C -0.0001(6) 0.1541(4) 0.01016(19) 0.034(2) Uani 1 1 d . . . H24B H -0.0105 0.1008 0.0092 0.051 Uiso 1 1 calc R . . H24C H 0.0049 0.1734 -0.0160 0.051 Uiso 1 1 calc R . . H24D H -0.0665 0.1764 0.0234 0.051 Uiso 1 1 calc R . . C5 C 0.2720(7) 0.0508(4) 0.1451(2) 0.035(2) Uani 1 1 d . . . H24A H 0.3083 0.0159 0.1265 0.043 Uiso 1 1 calc R . . C26 C 0.2709(7) -0.0585(4) 0.0337(2) 0.039(2) Uani 1 1 d . . . H25A H 0.2417 -0.0862 0.0115 0.058 Uiso 1 1 calc R . . H25B H 0.2361 -0.0779 0.0573 0.058 Uiso 1 1 calc R . . H25C H 0.3558 -0.0631 0.0350 0.058 Uiso 1 1 calc R . . C4 C 0.4020(7) 0.0731(5) 0.0673(2) 0.041(2) Uani 1 1 d . . . H26A H 0.4343 0.0239 0.0727 0.050 Uiso 1 1 calc R . . H26B H 0.4166 0.1043 0.0901 0.050 Uiso 1 1 calc R . . C1 C 0.1986(6) 0.1027(4) 0.0850(2) 0.0219(17) Uani 1 1 d . . . C22 C 0.1106(6) 0.1719(4) 0.03157(18) 0.0277(18) Uani 1 1 d . . . H28A H 0.1775 0.1492 0.0175 0.033 Uiso 1 1 calc R . . C3 C 0.2380(6) 0.0225(4) 0.0292(2) 0.0291(19) Uani 1 1 d . . . H29A H 0.2725 0.0416 0.0051 0.035 Uiso 1 1 calc R . . H29B H 0.1523 0.0267 0.0271 0.035 Uiso 1 1 calc R . . C29 C 0.0352(7) 0.3798(4) 0.1647(2) 0.045(2) Uani 1 1 d . . . H31A H 0.0140 0.4300 0.1577 0.067 Uiso 1 1 calc R . . H31B H 0.0949 0.3810 0.1849 0.067 Uiso 1 1 calc R . . H31C H -0.0338 0.3540 0.1743 0.067 Uiso 1 1 calc R . . C30 C 0.3327(7) 0.2745(5) 0.1286(3) 0.057(3) Uani 1 1 d . . . H32A H 0.4060 0.2717 0.1429 0.085 Uiso 1 1 calc R . . H32B H 0.3255 0.3231 0.1168 0.085 Uiso 1 1 calc R . . H32C H 0.3321 0.2370 0.1084 0.085 Uiso 1 1 calc R . . C16 C 0.2299(7) 0.2617(4) 0.1560(2) 0.040(2) Uani 1 1 d . . . H33A H 0.2395 0.2134 0.1686 0.048 Uiso 1 1 calc R . . H33B H 0.2316 0.2995 0.1764 0.048 Uiso 1 1 calc R . . C17 C 0.0828(7) 0.3402(4) 0.1297(2) 0.038(2) Uani 1 1 d . . . H17D H 0.0228 0.3409 0.1093 0.046 Uiso 1 1 calc R . . H17E H 0.1514 0.3673 0.1200 0.046 Uiso 1 1 calc R . . C21 C -0.2569(7) 0.3063(5) 0.1264(2) 0.062(3) Uani 1 1 d . . . H41A H -0.2711 0.2759 0.1492 0.093 Uiso 1 1 calc R . . H41B H -0.3302 0.3287 0.1181 0.093 Uiso 1 1 calc R . . H41C H -0.2006 0.3448 0.1328 0.093 Uiso 1 1 calc R . . C18 C -0.2083(7) 0.2586(5) 0.0941(2) 0.040(2) Uani 1 1 d . . . C15 C 0.0561(6) 0.1979(4) 0.2341(2) 0.038(2) Uani 1 1 d . . . H11D H 0.1203 0.1625 0.2347 0.057 Uiso 1 1 calc R . . H11E H 0.0404 0.2152 0.2602 0.057 Uiso 1 1 calc R . . H11F H 0.0775 0.2395 0.2178 0.057 Uiso 1 1 calc R . . C7 C 0.1984(8) 0.0078(5) 0.1725(2) 0.068(3) Uani 1 1 d . . . H21D H 0.1366 -0.0173 0.1582 0.102 Uiso 1 1 calc R . . H21E H 0.1636 0.0410 0.1914 0.102 Uiso 1 1 calc R . . H21F H 0.2469 -0.0285 0.1857 0.102 Uiso 1 1 calc R . . C25 C 0.4642(8) 0.1051(6) 0.0335(2) 0.078(3) Uani 1 1 d . . . H21G H 0.5476 0.1084 0.0391 0.117 Uiso 1 1 calc R . . H21H H 0.4335 0.1542 0.0282 0.117 Uiso 1 1 calc R . . H21I H 0.4521 0.0737 0.0110 0.117 Uiso 1 1 calc R . . C20 C -0.1864(8) 0.3078(5) 0.0586(2) 0.072(3) Uani 1 1 d . . . H44A H -0.1577 0.2776 0.0373 0.107 Uiso 1 1 calc R . . H44B H -0.1283 0.3452 0.0650 0.107 Uiso 1 1 calc R . . H44C H -0.2593 0.3316 0.0510 0.107 Uiso 1 1 calc R . . C10 C -0.2054(10) 0.0121(5) 0.0820(3) 0.080(4) Uani 1 1 d . . . H12D H -0.2718 0.0325 0.0961 0.121 Uiso 1 1 calc R . . H12E H -0.2288 -0.0338 0.0697 0.121 Uiso 1 1 calc R . . H12F H -0.1799 0.0471 0.0624 0.121 Uiso 1 1 calc R . . C11 C -0.2601(9) 0.0067(7) 0.1847(3) 0.090(4) Uani 1 1 d . . . H19A H -0.2912 0.0425 0.1659 0.108 Uiso 1 1 calc R . . H19B H -0.2652 -0.0424 0.1727 0.108 Uiso 1 1 calc R . . C19 C -0.2958(8) 0.2014(5) 0.0831(3) 0.081(4) Uani 1 1 d . . . H43A H -0.2652 0.1721 0.0618 0.122 Uiso 1 1 calc R . . H43B H -0.3684 0.2253 0.0751 0.122 Uiso 1 1 calc R . . H43C H -0.3112 0.1696 0.1052 0.122 Uiso 1 1 calc R . . C27 C -0.0662(10) -0.0973(5) 0.2147(3) 0.079(4) Uani 1 1 d . . . H18A H -0.0236 -0.1190 0.2362 0.119 Uiso 1 1 calc R . . H18B H -0.0238 -0.1066 0.1907 0.119 Uiso 1 1 calc R . . H18C H -0.1440 -0.1193 0.2130 0.119 Uiso 1 1 calc R . . C28 C -0.3330(9) 0.0074(7) 0.2174(3) 0.097(4) Uani 1 1 d . . . H17A H -0.4124 -0.0062 0.2099 0.146 Uiso 1 1 calc R . . H17B H -0.3335 0.0566 0.2287 0.146 Uiso 1 1 calc R . . H17C H -0.3036 -0.0277 0.2364 0.146 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0322(4) 0.0187(3) 0.0184(3) -0.0016(4) -0.0004(4) 0.0004(4) N5 0.025(4) 0.021(4) 0.032(4) -0.003(3) -0.001(3) 0.000(3) N6 0.027(4) 0.030(4) 0.025(4) -0.005(3) 0.006(3) 0.004(3) N3 0.049(4) 0.026(4) 0.012(3) -0.006(3) 0.007(3) -0.006(3) C13 0.042(6) 0.074(7) 0.036(5) -0.011(5) 0.018(4) 0.004(5) N4 0.038(4) 0.023(4) 0.014(3) -0.004(3) -0.005(3) -0.013(3) C8 0.106(9) 0.044(6) 0.078(7) -0.042(5) 0.056(7) -0.029(6) C12 0.057(6) 0.041(6) 0.031(5) 0.002(4) 0.005(4) -0.008(5) N7 0.039(4) 0.031(4) 0.020(4) 0.004(3) 0.002(3) -0.014(3) C2 0.021(4) 0.019(4) 0.029(5) 0.008(4) 0.000(4) -0.002(3) C9 0.068(6) 0.018(5) 0.025(5) -0.001(4) 0.014(4) -0.006(4) C14 0.033(5) 0.025(5) 0.021(4) -0.006(3) 0.006(3) -0.010(4) N8 0.024(4) 0.029(4) 0.021(3) -0.003(3) -0.004(3) 0.005(3) C23 0.053(6) 0.034(6) 0.026(5) 0.007(4) 0.004(4) -0.005(4) N1 0.033(4) 0.016(3) 0.012(3) 0.002(3) 0.003(3) -0.004(3) C6 0.082(8) 0.054(7) 0.048(6) -0.007(5) -0.034(5) 0.034(6) N2 0.045(4) 0.030(4) 0.012(3) 0.000(3) -0.003(3) 0.006(3) C24 0.039(6) 0.037(5) 0.026(4) 0.003(3) -0.007(4) -0.002(4) C5 0.044(6) 0.039(6) 0.023(5) 0.003(4) 0.003(4) 0.021(4) C26 0.041(6) 0.030(5) 0.045(5) -0.009(4) 0.001(4) 0.007(4) C4 0.038(6) 0.040(6) 0.046(6) -0.012(4) 0.002(5) -0.004(4) C1 0.027(5) 0.014(4) 0.025(5) -0.001(3) 0.002(4) -0.004(3) C22 0.034(5) 0.032(5) 0.017(4) 0.009(4) 0.004(3) -0.003(4) C3 0.028(5) 0.040(5) 0.019(4) -0.003(4) -0.001(4) -0.004(4) C29 0.055(6) 0.025(5) 0.054(5) -0.011(4) 0.005(5) -0.006(4) C30 0.046(6) 0.056(6) 0.068(7) 0.007(6) -0.005(6) -0.016(5) C16 0.056(7) 0.020(5) 0.044(6) -0.010(4) -0.006(5) -0.003(4) C17 0.049(5) 0.015(5) 0.050(6) -0.002(4) 0.013(4) -0.008(4) C21 0.063(6) 0.070(8) 0.052(6) -0.009(6) -0.006(5) 0.039(5) C18 0.032(6) 0.041(6) 0.046(6) -0.006(4) -0.003(4) 0.008(4) C15 0.035(5) 0.043(6) 0.035(5) -0.009(4) -0.007(4) 0.002(4) C7 0.086(8) 0.075(8) 0.044(6) 0.029(6) 0.028(6) 0.044(6) C25 0.055(7) 0.128(10) 0.051(6) 0.005(6) 0.008(6) -0.043(7) C20 0.082(8) 0.086(9) 0.047(6) 0.021(6) -0.008(5) 0.042(6) C10 0.144(11) 0.036(7) 0.061(7) -0.016(5) -0.047(7) -0.003(7) C11 0.065(8) 0.141(13) 0.063(8) 0.018(7) 0.024(6) -0.045(8) C19 0.057(7) 0.055(8) 0.132(10) -0.023(7) -0.044(7) 0.016(6) C27 0.137(11) 0.042(7) 0.058(7) 0.007(5) -0.004(6) -0.007(7) C28 0.076(9) 0.153(13) 0.063(8) -0.024(8) 0.005(7) 0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N6 1.764(6) . ? Nb1 N5 2.012(6) . ? Nb1 N1 2.153(5) . ? Nb1 N4 2.199(5) . ? Nb1 N3 2.293(6) . ? Nb1 N2 2.411(6) . ? N5 C16 1.460(9) . ? N5 C17 1.468(8) . ? N6 C18 1.471(9) . ? N3 C2 1.340(8) . ? N3 C9 1.460(9) . ? C13 C14 1.522(10) . ? C13 H11A 0.9800 . ? C13 H11B 0.9800 . ? C13 H11C 0.9800 . ? N4 C2 1.342(8) . ? N4 C14 1.467(8) . ? C8 C9 1.508(10) . ? C8 H12A 0.9800 . ? C8 H12B 0.9800 . ? C8 H12C 0.9800 . ? C12 N7 1.446(9) . ? C12 C27 1.513(11) . ? C12 H13A 0.9900 . ? C12 H13B 0.9900 . ? N7 C2 1.399(8) . ? N7 C11 1.427(10) . ? C9 C10 1.499(11) . ? C9 H15A 1.0000 . ? C14 C15 1.498(9) . ? C14 H16A 1.0000 . ? N8 C1 1.390(8) . ? N8 C4 1.440(8) . ? N8 C3 1.460(8) . ? C23 C22 1.522(10) . ? C23 H21A 0.9800 . ? C23 H21B 0.9800 . ? C23 H21C 0.9800 . ? N1 C1 1.363(8) . ? N1 C22 1.469(8) . ? C6 C5 1.545(11) . ? C6 H22A 0.9800 . ? C6 H22B 0.9800 . ? C6 H22C 0.9800 . ? N2 C1 1.334(8) . ? N2 C5 1.478(8) . ? C24 C22 1.509(9) . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C5 C7 1.494(11) . ? C5 H24A 1.0000 . ? C26 C3 1.533(10) . ? C26 H25A 0.9800 . ? C26 H25B 0.9800 . ? C26 H25C 0.9800 . ? C4 C25 1.495(10) . ? C4 H26A 0.9900 . ? C4 H26B 0.9900 . ? C22 H28A 1.0000 . ? C3 H29A 0.9900 . ? C3 H29B 0.9900 . ? C29 C17 1.519(9) . ? C29 H31A 0.9800 . ? C29 H31B 0.9800 . ? C29 H31C 0.9800 . ? C30 C16 1.537(10) . ? C30 H32A 0.9800 . ? C30 H32B 0.9800 . ? C30 H32C 0.9800 . ? C16 H33A 0.9900 . ? C16 H33B 0.9900 . ? C17 H17D 0.9900 . ? C17 H17E 0.9900 . ? C21 C18 1.527(10) . ? C21 H41A 0.9800 . ? C21 H41B 0.9800 . ? C21 H41C 0.9800 . ? C18 C19 1.499(11) . ? C18 C20 1.547(11) . ? C15 H11D 0.9800 . ? C15 H11E 0.9800 . ? C15 H11F 0.9800 . ? C7 H21D 0.9800 . ? C7 H21E 0.9800 . ? C7 H21F 0.9800 . ? C25 H21G 0.9800 . ? C25 H21H 0.9800 . ? C25 H21I 0.9800 . ? C20 H44A 0.9800 . ? C20 H44B 0.9800 . ? C20 H44C 0.9800 . ? C10 H12D 0.9800 . ? C10 H12E 0.9800 . ? C10 H12F 0.9800 . ? C11 C28 1.415(12) . ? C11 H19A 0.9900 . ? C11 H19B 0.9900 . ? C19 H43A 0.9800 . ? C19 H43B 0.9800 . ? C19 H43C 0.9800 . ? C27 H18A 0.9800 . ? C27 H18B 0.9800 . ? C27 H18C 0.9800 . ? C28 H17A 0.9800 . ? C28 H17B 0.9800 . ? C28 H17C 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 N6 Nb1 N5 95.4(3) . . ? N6 Nb1 N1 103.4(2) . . ? N5 Nb1 N1 102.1(2) . . ? N6 Nb1 N4 104.6(2) . . ? N5 Nb1 N4 101.5(2) . . ? N1 Nb1 N4 141.2(2) . . ? N6 Nb1 N3 95.7(2) . . ? N5 Nb1 N3 159.7(2) . . ? N1 Nb1 N3 91.8(2) . . ? N4 Nb1 N3 59.20(19) . . ? N6 Nb1 N2 161.9(2) . . ? N5 Nb1 N2 89.0(2) . . ? N1 Nb1 N2 58.5(2) . . ? N4 Nb1 N2 91.6(2) . . ? N3 Nb1 N2 85.6(2) . . ? C16 N5 C17 109.9(6) . . ? C16 N5 Nb1 124.2(5) . . ? C17 N5 Nb1 125.8(5) . . ? C18 N6 Nb1 175.3(6) . . ? C2 N3 C9 121.9(6) . . ? C2 N3 Nb1 92.3(4) . . ? C9 N3 Nb1 145.5(4) . . ? C14 C13 H11A 109.5 . . ? C14 C13 H11B 109.5 . . ? H11A C13 H11B 109.5 . . ? C14 C13 H11C 109.5 . . ? H11A C13 H11C 109.5 . . ? H11B C13 H11C 109.5 . . ? C2 N4 C14 120.4(6) . . ? C2 N4 Nb1 96.5(4) . . ? C14 N4 Nb1 138.3(4) . . ? C9 C8 H12A 109.5 . . ? C9 C8 H12B 109.5 . . ? H12A C8 H12B 109.5 . . ? C9 C8 H12C 109.5 . . ? H12A C8 H12C 109.5 . . ? H12B C8 H12C 109.5 . . ? N7 C12 C27 115.0(7) . . ? N7 C12 H13A 108.5 . . ? C27 C12 H13A 108.5 . . ? N7 C12 H13B 108.5 . . ? C27 C12 H13B 108.5 . . ? H13A C12 H13B 107.5 . . ? C2 N7 C11 121.3(7) . . ? C2 N7 C12 119.3(6) . . ? C11 N7 C12 119.3(7) . . ? N3 C2 N4 111.8(6) . . ? N3 C2 N7 124.1(6) . . ? N4 C2 N7 124.2(6) . . ? N3 C9 C10 111.9(7) . . ? N3 C9 C8 110.9(7) . . ? C10 C9 C8 108.2(7) . . ? N3 C9 H15A 108.6 . . ? C10 C9 H15A 108.6 . . ? C8 C9 H15A 108.6 . . ? N4 C14 C15 109.7(5) . . ? N4 C14 C13 111.6(6) . . ? C15 C14 C13 110.1(6) . . ? N4 C14 H16A 108.5 . . ? C15 C14 H16A 108.5 . . ? C13 C14 H16A 108.5 . . ? C1 N8 C4 121.9(6) . . ? C1 N8 C3 120.4(6) . . ? C4 N8 C3 117.7(6) . . ? C22 C23 H21A 109.5 . . ? C22 C23 H21B 109.5 . . ? H21A C23 H21B 109.5 . . ? C22 C23 H21C 109.5 . . ? H21A C23 H21C 109.5 . . ? H21B C23 H21C 109.5 . . ? C1 N1 C22 120.9(6) . . ? C1 N1 Nb1 99.9(4) . . ? C22 N1 Nb1 133.0(5) . . ? C5 C6 H22A 109.5 . . ? C5 C6 H22B 109.5 . . ? H22A C6 H22B 109.5 . . ? C5 C6 H22C 109.5 . . ? H22A C6 H22C 109.5 . . ? H22B C6 H22C 109.5 . . ? C1 N2 C5 121.0(6) . . ? C1 N2 Nb1 89.2(4) . . ? C5 N2 Nb1 145.1(4) . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C24 H24D 109.5 . . ? H24B C24 H24D 109.5 . . ? H24C C24 H24D 109.5 . . ? N2 C5 C7 111.1(6) . . ? N2 C5 C6 111.6(6) . . ? C7 C5 C6 109.2(7) . . ? N2 C5 H24A 108.3 . . ? C7 C5 H24A 108.3 . . ? C6 C5 H24A 108.3 . . ? C3 C26 H25A 109.5 . . ? C3 C26 H25B 109.5 . . ? H25A C26 H25B 109.5 . . ? C3 C26 H25C 109.5 . . ? H25A C26 H25C 109.5 . . ? H25B C26 H25C 109.5 . . ? N8 C4 C25 113.0(7) . . ? N8 C4 H26A 109.0 . . ? C25 C4 H26A 109.0 . . ? N8 C4 H26B 109.0 . . ? C25 C4 H26B 109.0 . . ? H26A C4 H26B 107.8 . . ? N2 C1 N1 112.4(6) . . ? N2 C1 N8 125.7(7) . . ? N1 C1 N8 121.9(6) . . ? N1 C22 C24 109.8(6) . . ? N1 C22 C23 110.1(6) . . ? C24 C22 C23 111.7(6) . . ? N1 C22 H28A 108.4 . . ? C24 C22 H28A 108.4 . . ? C23 C22 H28A 108.4 . . ? N8 C3 C26 112.3(6) . . ? N8 C3 H29A 109.1 . . ? C26 C3 H29A 109.1 . . ? N8 C3 H29B 109.1 . . ? C26 C3 H29B 109.1 . . ? H29A C3 H29B 107.9 . . ? C17 C29 H31A 109.5 . . ? C17 C29 H31B 109.5 . . ? H31A C29 H31B 109.5 . . ? C17 C29 H31C 109.5 . . ? H31A C29 H31C 109.5 . . ? H31B C29 H31C 109.5 . . ? C16 C30 H32A 109.5 . . ? C16 C30 H32B 109.5 . . ? H32A C30 H32B 109.5 . . ? C16 C30 H32C 109.5 . . ? H32A C30 H32C 109.5 . . ? H32B C30 H32C 109.5 . . ? N5 C16 C30 113.3(7) . . ? N5 C16 H33A 108.9 . . ? C30 C16 H33A 108.9 . . ? N5 C16 H33B 108.9 . . ? C30 C16 H33B 108.9 . . ? H33A C16 H33B 107.7 . . ? N5 C17 C29 114.1(6) . . ? N5 C17 H17D 108.7 . . ? C29 C17 H17D 108.7 . . ? N5 C17 H17E 108.7 . . ? C29 C17 H17E 108.7 . . ? H17D C17 H17E 107.6 . . ? C18 C21 H41A 109.5 . . ? C18 C21 H41B 109.5 . . ? H41A C21 H41B 109.5 . . ? C18 C21 H41C 109.5 . . ? H41A C21 H41C 109.5 . . ? H41B C21 H41C 109.5 . . ? N6 C18 C19 109.8(7) . . ? N6 C18 C21 109.7(6) . . ? C19 C18 C21 109.9(7) . . ? N6 C18 C20 110.9(7) . . ? C19 C18 C20 108.0(8) . . ? C21 C18 C20 108.5(7) . . ? C14 C15 H11D 109.5 . . ? C14 C15 H11E 109.5 . . ? H11D C15 H11E 109.5 . . ? C14 C15 H11F 109.5 . . ? H11D C15 H11F 109.5 . . ? H11E C15 H11F 109.5 . . ? C5 C7 H21D 109.5 . . ? C5 C7 H21E 109.5 . . ? H21D C7 H21E 109.5 . . ? C5 C7 H21F 109.5 . . ? H21D C7 H21F 109.5 . . ? H21E C7 H21F 109.5 . . ? C4 C25 H21G 109.5 . . ? C4 C25 H21H 109.5 . . ? H21G C25 H21H 109.5 . . ? C4 C25 H21I 109.5 . . ? H21G C25 H21I 109.5 . . ? H21H C25 H21I 109.5 . . ? C18 C20 H44A 109.5 . . ? C18 C20 H44B 109.5 . . ? H44A C20 H44B 109.5 . . ? C18 C20 H44C 109.5 . . ? H44A C20 H44C 109.5 . . ? H44B C20 H44C 109.5 . . ? C9 C10 H12D 109.5 . . ? C9 C10 H12E 109.5 . . ? H12D C10 H12E 109.5 . . ? C9 C10 H12F 109.5 . . ? H12D C10 H12F 109.5 . . ? H12E C10 H12F 109.5 . . ? C28 C11 N7 116.3(9) . . ? C28 C11 H19A 108.2 . . ? N7 C11 H19A 108.2 . . ? C28 C11 H19B 108.2 . . ? N7 C11 H19B 108.2 . . ? H19A C11 H19B 107.4 . . ? C18 C19 H43A 109.5 . . ? C18 C19 H43B 109.5 . . ? H43A C19 H43B 109.5 . . ? C18 C19 H43C 109.5 . . ? H43A C19 H43C 109.5 . . ? H43B C19 H43C 109.5 . . ? C12 C27 H18A 109.5 . . ? C12 C27 H18B 109.5 . . ? H18A C27 H18B 109.5 . . ? C12 C27 H18C 109.5 . . ? H18A C27 H18C 109.5 . . ? H18B C27 H18C 109.5 . . ? C11 C28 H17A 109.5 . . ? C11 C28 H17B 109.5 . . ? H17A C28 H17B 109.5 . . ? C11 C28 H17C 109.5 . . ? H17A C28 H17C 109.5 . . ? H17B C28 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Nb1 N5 C16 174.4(5) . . . . ? N1 Nb1 N5 C16 -80.7(6) . . . . ? N4 Nb1 N5 C16 68.2(6) . . . . ? N3 Nb1 N5 C16 51.4(9) . . . . ? N2 Nb1 N5 C16 -23.2(6) . . . . ? N6 Nb1 N5 C17 -6.0(6) . . . . ? N1 Nb1 N5 C17 99.0(5) . . . . ? N4 Nb1 N5 C17 -112.1(5) . . . . ? N3 Nb1 N5 C17 -128.9(7) . . . . ? N2 Nb1 N5 C17 156.4(5) . . . . ? N5 Nb1 N6 C18 -156(6) . . . . ? N1 Nb1 N6 C18 100(6) . . . . ? N4 Nb1 N6 C18 -52(6) . . . . ? N3 Nb1 N6 C18 7(6) . . . . ? N2 Nb1 N6 C18 101(6) . . . . ? N6 Nb1 N3 C2 -100.8(4) . . . . ? N5 Nb1 N3 C2 22.1(8) . . . . ? N1 Nb1 N3 C2 155.5(4) . . . . ? N4 Nb1 N3 C2 2.9(4) . . . . ? N2 Nb1 N3 C2 97.3(4) . . . . ? N6 Nb1 N3 C9 85.2(9) . . . . ? N5 Nb1 N3 C9 -151.8(8) . . . . ? N1 Nb1 N3 C9 -18.4(9) . . . . ? N4 Nb1 N3 C9 -171.1(9) . . . . ? N2 Nb1 N3 C9 -76.6(9) . . . . ? N6 Nb1 N4 C2 85.0(5) . . . . ? N5 Nb1 N4 C2 -176.2(4) . . . . ? N1 Nb1 N4 C2 -49.9(6) . . . . ? N3 Nb1 N4 C2 -2.9(4) . . . . ? N2 Nb1 N4 C2 -86.9(4) . . . . ? N6 Nb1 N4 C14 -68.4(7) . . . . ? N5 Nb1 N4 C14 30.4(7) . . . . ? N1 Nb1 N4 C14 156.7(6) . . . . ? N3 Nb1 N4 C14 -156.3(8) . . . . ? N2 Nb1 N4 C14 119.8(7) . . . . ? C27 C12 N7 C2 -111.9(9) . . . . ? C27 C12 N7 C11 63.4(11) . . . . ? C9 N3 C2 N4 171.6(6) . . . . ? Nb1 N3 C2 N4 -4.3(6) . . . . ? C9 N3 C2 N7 -9.0(11) . . . . ? Nb1 N3 C2 N7 175.0(6) . . . . ? C14 N4 C2 N3 164.4(6) . . . . ? Nb1 N4 C2 N3 4.6(6) . . . . ? C14 N4 C2 N7 -15.0(10) . . . . ? Nb1 N4 C2 N7 -174.8(6) . . . . ? C11 N7 C2 N3 -57.1(11) . . . . ? C12 N7 C2 N3 118.1(8) . . . . ? C11 N7 C2 N4 122.2(9) . . . . ? C12 N7 C2 N4 -62.6(10) . . . . ? C2 N3 C9 C10 116.3(8) . . . . ? Nb1 N3 C9 C10 -70.8(11) . . . . ? C2 N3 C9 C8 -122.8(8) . . . . ? Nb1 N3 C9 C8 50.0(12) . . . . ? C2 N4 C14 C15 148.2(7) . . . . ? Nb1 N4 C14 C15 -62.9(9) . . . . ? C2 N4 C14 C13 -89.5(8) . . . . ? Nb1 N4 C14 C13 59.4(9) . . . . ? N6 Nb1 N1 C1 -179.4(4) . . . . ? N5 Nb1 N1 C1 82.0(4) . . . . ? N4 Nb1 N1 C1 -44.2(6) . . . . ? N3 Nb1 N1 C1 -83.1(4) . . . . ? N2 Nb1 N1 C1 0.7(4) . . . . ? N6 Nb1 N1 C22 29.6(6) . . . . ? N5 Nb1 N1 C22 -69.0(6) . . . . ? N4 Nb1 N1 C22 164.8(5) . . . . ? N3 Nb1 N1 C22 125.9(6) . . . . ? N2 Nb1 N1 C22 -150.3(6) . . . . ? N6 Nb1 N2 C1 -0.8(10) . . . . ? N5 Nb1 N2 C1 -105.5(4) . . . . ? N1 Nb1 N2 C1 -0.7(4) . . . . ? N4 Nb1 N2 C1 153.0(4) . . . . ? N3 Nb1 N2 C1 94.1(4) . . . . ? N6 Nb1 N2 C5 -152.6(9) . . . . ? N5 Nb1 N2 C5 102.7(8) . . . . ? N1 Nb1 N2 C5 -152.5(9) . . . . ? N4 Nb1 N2 C5 1.2(8) . . . . ? N3 Nb1 N2 C5 -57.7(8) . . . . ? C1 N2 C5 C7 -122.7(8) . . . . ? Nb1 N2 C5 C7 23.9(12) . . . . ? C1 N2 C5 C6 115.2(7) . . . . ? Nb1 N2 C5 C6 -98.2(9) . . . . ? C1 N8 C4 C25 -119.8(8) . . . . ? C3 N8 C4 C25 59.1(9) . . . . ? C5 N2 C1 N1 162.6(6) . . . . ? Nb1 N2 C1 N1 1.0(6) . . . . ? C5 N2 C1 N8 -16.2(11) . . . . ? Nb1 N2 C1 N8 -177.8(6) . . . . ? C22 N1 C1 N2 154.5(6) . . . . ? Nb1 N1 C1 N2 -1.1(6) . . . . ? C22 N1 C1 N8 -26.7(10) . . . . ? Nb1 N1 C1 N8 177.7(5) . . . . ? C4 N8 C1 N2 -47.0(10) . . . . ? C3 N8 C1 N2 134.2(7) . . . . ? C4 N8 C1 N1 134.3(7) . . . . ? C3 N8 C1 N1 -44.5(10) . . . . ? C1 N1 C22 C24 133.8(6) . . . . ? Nb1 N1 C22 C24 -80.0(8) . . . . ? C1 N1 C22 C23 -102.7(8) . . . . ? Nb1 N1 C22 C23 43.5(8) . . . . ? C1 N8 C3 C26 -117.0(7) . . . . ? C4 N8 C3 C26 64.1(8) . . . . ? C17 N5 C16 C30 -77.8(8) . . . . ? Nb1 N5 C16 C30 101.9(7) . . . . ? C16 N5 C17 C29 -78.4(8) . . . . ? Nb1 N5 C17 C29 101.8(7) . . . . ? Nb1 N6 C18 C19 -22(7) . . . . ? Nb1 N6 C18 C21 98(6) . . . . ? Nb1 N6 C18 C20 -142(6) . . . . ? C2 N7 C11 C28 -134.2(10) . . . . ? C12 N7 C11 C28 50.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.519 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.077 #=================================END