data_(BDI)pyCl2Nb(NtBu) _publ_contact_author_name 'Prof. Robert G. Bergman' _publ_contact_author_address ;Department of Chemistry University of California at Berkeley Berkeley, CA 94720-1460 (USA) ; _publ_contact_author_email rbergman@berkeley.edu _publ_contact_author_phone (+1)510-642-2156 _publ_contact_author_fax (+1)510-642-7714 loop_ _publ_author_name _publ_author_address 'Bergman, Robert G.' ;Department of Chemistry University of California at Berkeley Berkeley, CA 94720-1460 (USA) ; 'Arnold, John' ;Department of Chemistry University of California at Berkeley Berkeley, CA 94720-1460 (USA) ; 'Tomson, Neil C.' ;Department of Chemistry University of California at Berkeley Berkeley, CA 94720-1460 (USA) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H55 Cl2 N4 Nb' _chemical_formula_sum 'C38 H55 Cl2 N4 Nb' _chemical_formula_weight 731.67 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8653(8) _cell_length_b 17.9863(17) _cell_length_c 24.392(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.7920(10) _cell_angle_gamma 90.00 _cell_volume 3832.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 136(2) _cell_measurement_reflns_used 5117 _cell_measurement_theta_min 6.615 _cell_measurement_theta_max 49.301 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.917772 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 136(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16890 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 24.70 _reflns_number_total 6495 _reflns_number_gt 5096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker-AXS XP v.6' _computing_publication_material 'Bruker-AXS XP v.6' _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^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6495 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.003 _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 0.17742(3) 0.193658(13) 0.098049(10) 0.02126(9) Uani 1 1 d . . . Cl1 Cl -0.08179(7) 0.15541(4) 0.06217(3) 0.02965(18) Uani 1 1 d . . . Cl2 Cl 0.42293(7) 0.20287(4) 0.15799(3) 0.02610(16) Uani 1 1 d . . . N1 N 0.2708(2) 0.17730(12) 0.04083(9) 0.0246(5) Uani 1 1 d . . . N2 N 0.1195(2) 0.30612(11) 0.08422(9) 0.0213(5) Uani 1 1 d . . . N3 N 0.0820(2) 0.20965(11) 0.18452(9) 0.0209(5) Uani 1 1 d . . . N4 N 0.2141(2) 0.06493(12) 0.11776(9) 0.0244(5) Uani 1 1 d . . . C1 C 0.3813(3) 0.15444(16) 0.00573(12) 0.0312(7) Uani 1 1 d . . . C2 C 0.4554(4) 0.22365(19) -0.01406(15) 0.0519(9) Uani 1 1 d . . . H2A H 0.3782 0.2541 -0.0356 0.078 Uiso 1 1 calc R . . H2B H 0.5293 0.2092 -0.0366 0.078 Uiso 1 1 calc R . . H2C H 0.5054 0.2513 0.0176 0.078 Uiso 1 1 calc R . . C3 C 0.2989(4) 0.10946(17) -0.04382(12) 0.0428(8) Uani 1 1 d . . . H3A H 0.2226 0.1400 -0.0657 0.064 Uiso 1 1 calc R . . H3B H 0.2506 0.0669 -0.0305 0.064 Uiso 1 1 calc R . . H3C H 0.3716 0.0933 -0.0663 0.064 Uiso 1 1 calc R . . C4 C 0.5031(4) 0.10521(19) 0.04001(13) 0.0443(8) Uani 1 1 d . . . H4A H 0.5558 0.1330 0.0711 0.066 Uiso 1 1 calc R . . H4B H 0.5750 0.0891 0.0171 0.066 Uiso 1 1 calc R . . H4C H 0.4549 0.0626 0.0533 0.066 Uiso 1 1 calc R . . C5 C 0.1850(3) 0.34558(14) 0.04115(11) 0.0230(6) Uani 1 1 d . . . C6 C 0.1055(3) 0.34757(15) -0.01388(11) 0.0286(6) Uani 1 1 d . . . C7 C 0.1754(3) 0.38352(16) -0.05336(12) 0.0368(7) Uani 1 1 d . . . H7A H 0.1266 0.3844 -0.0903 0.044 Uiso 1 1 calc R . . C8 C 0.3157(4) 0.41792(17) -0.03895(12) 0.0374(7) Uani 1 1 d . . . H8A H 0.3617 0.4407 -0.0661 0.045 Uiso 1 1 calc R . . C9 C 0.3880(3) 0.41846(16) 0.01606(12) 0.0327(7) Uani 1 1 d . . . H9A H 0.4812 0.4429 0.0257 0.039 Uiso 1 1 calc R . . C10 C 0.3231(3) 0.38297(14) 0.05730(11) 0.0239(6) Uani 1 1 d . . . C11 C -0.0518(3) 0.31400(16) -0.03148(12) 0.0355(7) Uani 1 1 d . . . H11A H -0.0888 0.2974 0.0021 0.043 Uiso 1 1 calc R . . C12 C -0.0490(4) 0.24730(18) -0.06918(14) 0.0503(9) Uani 1 1 d . . . H12A H 0.0222 0.2112 -0.0510 0.075 Uiso 1 1 calc R . . H12B H -0.0182 0.2628 -0.1033 0.075 Uiso 1 1 calc R . . H12C H -0.1494 0.2257 -0.0771 0.075 Uiso 1 1 calc R . . C13 C -0.1683(4) 0.37194(19) -0.06152(15) 0.0548(10) Uani 1 1 d . . . H13A H -0.1729 0.4139 -0.0376 0.082 Uiso 1 1 calc R . . H13B H -0.2677 0.3495 -0.0703 0.082 Uiso 1 1 calc R . . H13C H -0.1359 0.3880 -0.0952 0.082 Uiso 1 1 calc R . . C14 C 0.4003(3) 0.39014(15) 0.11755(11) 0.0261(6) Uani 1 1 d . . . H14A H 0.3514 0.3543 0.1392 0.031 Uiso 1 1 calc R . . C15 C 0.5706(3) 0.37105(16) 0.12605(13) 0.0356(7) Uani 1 1 d . . . H15A H 0.5836 0.3222 0.1116 0.053 Uiso 1 1 calc R . . H15B H 0.6121 0.3722 0.1650 0.053 Uiso 1 1 calc R . . H15C H 0.6230 0.4067 0.1068 0.053 Uiso 1 1 calc R . . C16 C 0.3762(3) 0.46740(16) 0.14063(12) 0.0368(7) Uani 1 1 d . . . H16A H 0.4264 0.4702 0.1787 0.055 Uiso 1 1 calc R . . H16B H 0.2686 0.4763 0.1386 0.055 Uiso 1 1 calc R . . H16C H 0.4184 0.5042 0.1191 0.055 Uiso 1 1 calc R . . C17 C -0.0335(3) 0.42267(16) 0.08507(13) 0.0342(7) Uani 1 1 d . . . H17A H 0.0521 0.4487 0.0748 0.051 Uiso 1 1 calc R . . H17B H -0.0743 0.4508 0.1126 0.051 Uiso 1 1 calc R . . H17C H -0.1112 0.4163 0.0528 0.051 Uiso 1 1 calc R . . C18 C 0.0187(3) 0.34675(15) 0.10880(11) 0.0253(6) Uani 1 1 d . . . C19 C -0.0457(3) 0.32448(16) 0.15342(12) 0.0294(7) Uani 1 1 d . . . H19A H -0.1237 0.3554 0.1609 0.035 Uiso 1 1 calc R . . C20 C -0.0156(3) 0.26310(15) 0.19033(11) 0.0262(6) Uani 1 1 d . . . C21 C -0.1092(3) 0.26357(17) 0.23673(13) 0.0395(8) Uani 1 1 d . . . H21A H -0.0665 0.2287 0.2650 0.059 Uiso 1 1 calc R . . H21B H -0.2129 0.2498 0.2221 0.059 Uiso 1 1 calc R . . H21C H -0.1077 0.3125 0.2525 0.059 Uiso 1 1 calc R . . C22 C 0.1206(3) 0.15664(15) 0.22946(10) 0.0230(6) Uani 1 1 d . . . C23 C 0.0326(3) 0.09154(15) 0.23067(11) 0.0267(6) Uani 1 1 d . . . C24 C 0.0892(3) 0.03737(17) 0.27027(12) 0.0351(7) Uani 1 1 d . . . H24A H 0.0349 -0.0067 0.2716 0.042 Uiso 1 1 calc R . . C25 C 0.2225(4) 0.04780(17) 0.30702(12) 0.0375(7) Uani 1 1 d . . . H25A H 0.2604 0.0099 0.3315 0.045 Uiso 1 1 calc R . . C26 C 0.3007(3) 0.11421(17) 0.30800(12) 0.0339(7) Uani 1 1 d . . . H26A H 0.3887 0.1215 0.3342 0.041 Uiso 1 1 calc R . . C27 C 0.2495(3) 0.17047(16) 0.27011(11) 0.0261(6) Uani 1 1 d . . . C28 C -0.1223(3) 0.07894(17) 0.19489(12) 0.0363(7) Uani 1 1 d . . . H28A H -0.1440 0.1214 0.1696 0.044 Uiso 1 1 calc R . . C29 C -0.1342(4) 0.00870(19) 0.16003(14) 0.0522(9) Uani 1 1 d . . . H29A H -0.0580 0.0096 0.1364 0.078 Uiso 1 1 calc R . . H29B H -0.2340 0.0059 0.1376 0.078 Uiso 1 1 calc R . . H29C H -0.1180 -0.0339 0.1841 0.078 Uiso 1 1 calc R . . C30 C -0.2480(4) 0.0762(2) 0.23192(15) 0.0501(9) Uani 1 1 d . . . H30A H -0.2434 0.1206 0.2539 0.075 Uiso 1 1 calc R . . H30B H -0.2317 0.0337 0.2560 0.075 Uiso 1 1 calc R . . H30C H -0.3468 0.0726 0.2088 0.075 Uiso 1 1 calc R . . C31 C 0.3287(3) 0.24588(16) 0.27627(12) 0.0318(7) Uani 1 1 d . . . H31A H 0.3080 0.2711 0.2401 0.038 Uiso 1 1 calc R . . C32 C 0.5031(3) 0.24103(19) 0.29433(13) 0.0442(8) Uani 1 1 d . . . H32A H 0.5461 0.2118 0.2679 0.066 Uiso 1 1 calc R . . H32B H 0.5261 0.2181 0.3303 0.066 Uiso 1 1 calc R . . H32C H 0.5461 0.2901 0.2961 0.066 Uiso 1 1 calc R . . C33 C 0.2634(4) 0.29378(19) 0.31851(15) 0.0516(9) Uani 1 1 d . . . H33A H 0.1545 0.2981 0.3075 0.077 Uiso 1 1 calc R . . H33B H 0.3089 0.3423 0.3200 0.077 Uiso 1 1 calc R . . H33C H 0.2858 0.2710 0.3546 0.077 Uiso 1 1 calc R . . C34 C 0.1649(3) 0.01654(16) 0.07574(12) 0.0317(7) Uani 1 1 d . . . H34A H 0.1020 0.0345 0.0441 0.038 Uiso 1 1 calc R . . C35 C 0.2030(4) -0.05713(16) 0.07753(13) 0.0396(8) Uani 1 1 d . . . H35A H 0.1678 -0.0881 0.0475 0.047 Uiso 1 1 calc R . . C36 C 0.2944(4) -0.08494(18) 0.12442(14) 0.0474(9) Uani 1 1 d . . . H36A H 0.3226 -0.1348 0.1266 0.057 Uiso 1 1 calc R . . C37 C 0.3431(4) -0.03707(17) 0.16810(13) 0.0426(8) Uani 1 1 d . . . H37A H 0.4034 -0.0543 0.2006 0.051 Uiso 1 1 calc R . . C38 C 0.3010(3) 0.03644(15) 0.16279(12) 0.0294(6) Uani 1 1 d . . . H38A H 0.3352 0.0682 0.1924 0.035 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 0.02149(15) 0.02051(15) 0.02122(15) 0.00021(10) 0.00202(9) -0.00036(10) Cl1 0.0254(4) 0.0313(4) 0.0303(4) 0.0035(3) -0.0008(3) -0.0057(3) Cl2 0.0223(4) 0.0280(4) 0.0270(4) -0.0008(3) 0.0013(3) -0.0006(3) N1 0.0280(13) 0.0236(12) 0.0218(12) 0.0028(10) 0.0033(9) -0.0010(10) N2 0.0198(12) 0.0208(12) 0.0231(12) 0.0025(9) 0.0029(9) -0.0007(9) N3 0.0174(11) 0.0219(12) 0.0232(12) 0.0027(9) 0.0026(9) -0.0003(9) N4 0.0265(13) 0.0229(13) 0.0234(12) 0.0025(10) 0.0030(9) -0.0025(9) C1 0.0361(17) 0.0322(17) 0.0274(17) -0.0037(13) 0.0117(13) -0.0009(13) C2 0.065(2) 0.044(2) 0.057(2) -0.0069(18) 0.0389(19) -0.0112(18) C3 0.057(2) 0.042(2) 0.0313(18) -0.0058(15) 0.0123(15) 0.0018(16) C4 0.0360(19) 0.058(2) 0.041(2) -0.0048(16) 0.0126(15) 0.0085(15) C5 0.0254(15) 0.0170(14) 0.0276(16) 0.0045(11) 0.0075(11) -0.0026(11) C6 0.0342(17) 0.0230(15) 0.0267(16) 0.0034(12) -0.0004(12) -0.0031(12) C7 0.050(2) 0.0313(17) 0.0268(17) 0.0062(13) 0.0003(14) -0.0095(15) C8 0.048(2) 0.0344(18) 0.0318(18) 0.0070(14) 0.0125(14) -0.0132(15) C9 0.0311(16) 0.0318(17) 0.0361(18) 0.0010(14) 0.0085(13) -0.0084(13) C10 0.0271(15) 0.0198(14) 0.0262(15) -0.0016(11) 0.0083(12) -0.0017(11) C11 0.0374(18) 0.0328(18) 0.0322(17) 0.0093(14) -0.0062(13) -0.0091(14) C12 0.061(2) 0.043(2) 0.041(2) 0.0029(16) -0.0092(17) -0.0169(17) C13 0.049(2) 0.049(2) 0.058(2) 0.0161(18) -0.0141(17) -0.0020(17) C14 0.0234(15) 0.0268(16) 0.0280(16) 0.0038(12) 0.0039(12) -0.0040(12) C15 0.0270(17) 0.0339(17) 0.0440(19) -0.0014(14) 0.0005(13) -0.0038(13) C16 0.0384(18) 0.0360(19) 0.0340(18) -0.0087(14) 0.0008(14) 0.0003(14) C17 0.0316(17) 0.0286(17) 0.0452(19) 0.0087(14) 0.0147(14) 0.0063(13) C18 0.0155(14) 0.0259(16) 0.0336(16) 0.0037(12) 0.0019(11) 0.0025(11) C19 0.0242(15) 0.0279(16) 0.0378(17) 0.0083(13) 0.0100(13) 0.0105(12) C20 0.0209(14) 0.0302(17) 0.0276(16) 0.0026(12) 0.0045(11) -0.0006(12) C21 0.0421(19) 0.0374(19) 0.044(2) 0.0119(15) 0.0210(15) 0.0151(15) C22 0.0268(15) 0.0246(15) 0.0188(14) 0.0014(11) 0.0073(11) 0.0058(12) C23 0.0294(16) 0.0272(16) 0.0253(15) 0.0037(12) 0.0095(12) 0.0019(12) C24 0.0418(19) 0.0278(17) 0.0378(18) 0.0068(14) 0.0124(14) 0.0031(14) C25 0.046(2) 0.0342(18) 0.0326(18) 0.0132(14) 0.0077(14) 0.0114(15) C26 0.0361(17) 0.0417(19) 0.0223(16) 0.0037(13) 0.0004(13) 0.0081(14) C27 0.0284(16) 0.0304(16) 0.0206(15) -0.0007(12) 0.0073(12) 0.0058(12) C28 0.0407(18) 0.0347(18) 0.0330(18) 0.0093(14) 0.0046(14) -0.0088(14) C29 0.055(2) 0.050(2) 0.052(2) -0.0058(17) 0.0115(17) -0.0272(17) C30 0.0372(19) 0.053(2) 0.062(2) 0.0128(18) 0.0129(16) -0.0049(16) C31 0.0345(17) 0.0337(17) 0.0265(16) -0.0058(13) 0.0034(13) 0.0020(13) C32 0.0400(19) 0.051(2) 0.0377(19) -0.0066(16) -0.0056(14) -0.0057(16) C33 0.060(2) 0.044(2) 0.052(2) -0.0203(17) 0.0142(18) -0.0001(17) C34 0.0362(17) 0.0305(17) 0.0269(16) 0.0024(13) 0.0014(13) -0.0054(13) C35 0.052(2) 0.0243(17) 0.0390(19) -0.0066(14) -0.0018(15) -0.0021(14) C36 0.065(2) 0.0210(17) 0.051(2) -0.0033(15) -0.0044(17) 0.0045(15) C37 0.051(2) 0.0312(18) 0.041(2) 0.0038(15) -0.0062(15) 0.0047(15) C38 0.0321(16) 0.0274(16) 0.0283(16) 0.0026(13) 0.0040(12) -0.0008(13) _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 1.765(2) . ? Nb1 N2 2.100(2) . ? Nb1 N4 2.376(2) . ? Nb1 Cl2 2.4125(7) . ? Nb1 Cl1 2.4157(7) . ? Nb1 N3 2.420(2) . ? N1 C1 1.465(3) . ? N2 C18 1.369(3) . ? N2 C5 1.467(3) . ? N3 C20 1.317(3) . ? N3 C22 1.449(3) . ? N4 C38 1.332(3) . ? N4 C34 1.359(3) . ? C1 C2 1.524(4) . ? C1 C4 1.530(4) . ? C1 C3 1.533(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.394(4) . ? C5 C6 1.406(4) . ? C6 C7 1.390(4) . ? C6 C11 1.513(4) . ? C7 C8 1.380(4) . ? C7 H7A 0.9300 . ? C8 C9 1.385(4) . ? C8 H8A 0.9300 . ? C9 C10 1.395(4) . ? C9 H9A 0.9300 . ? C10 C14 1.518(4) . ? C11 C12 1.514(4) . ? C11 C13 1.559(4) . ? C11 H11A 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.527(4) . ? C14 C16 1.528(4) . ? C14 H14A 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.524(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.372(4) . ? C19 C20 1.421(4) . ? C19 H19A 0.9300 . ? C20 C21 1.513(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C27 1.402(4) . ? C22 C23 1.410(4) . ? C23 C24 1.403(4) . ? C23 C28 1.514(4) . ? C24 C25 1.369(4) . ? C24 H24A 0.9300 . ? C25 C26 1.379(4) . ? C25 H25A 0.9300 . ? C26 C27 1.393(4) . ? C26 H26A 0.9300 . ? C27 C31 1.523(4) . ? C28 C29 1.516(4) . ? C28 C30 1.550(4) . ? C28 H28A 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C33 1.531(4) . ? C31 C32 1.536(4) . ? C31 H31A 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.366(4) . ? C34 H34A 0.9300 . ? C35 C36 1.378(4) . ? C35 H35A 0.9300 . ? C36 C37 1.381(4) . ? C36 H36A 0.9300 . ? C37 C38 1.374(4) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Nb1 N2 99.69(9) . . ? N1 Nb1 N4 86.05(9) . . ? N2 Nb1 N4 172.98(7) . . ? N1 Nb1 Cl2 89.68(7) . . ? N2 Nb1 Cl2 101.65(6) . . ? N4 Nb1 Cl2 82.30(5) . . ? N1 Nb1 Cl1 102.21(7) . . ? N2 Nb1 Cl1 91.41(6) . . ? N4 Nb1 Cl1 83.38(5) . . ? Cl2 Nb1 Cl1 160.68(2) . . ? N1 Nb1 N3 171.92(8) . . ? N2 Nb1 N3 85.03(8) . . ? N4 Nb1 N3 89.74(7) . . ? Cl2 Nb1 N3 82.92(5) . . ? Cl1 Nb1 N3 84.12(5) . . ? C1 N1 Nb1 163.59(19) . . ? C18 N2 C5 115.0(2) . . ? C18 N2 Nb1 127.14(17) . . ? C5 N2 Nb1 117.73(16) . . ? C20 N3 C22 118.3(2) . . ? C20 N3 Nb1 120.94(17) . . ? C22 N3 Nb1 120.57(15) . . ? C38 N4 C34 116.2(2) . . ? C38 N4 Nb1 125.57(18) . . ? C34 N4 Nb1 117.15(18) . . ? N1 C1 C2 108.8(2) . . ? N1 C1 C4 108.8(2) . . ? C2 C1 C4 110.1(3) . . ? N1 C1 C3 109.4(2) . . ? C2 C1 C3 110.8(3) . . ? C4 C1 C3 108.9(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 122.1(2) . . ? C10 C5 N2 117.8(2) . . ? C6 C5 N2 120.0(2) . . ? C7 C6 C5 117.6(3) . . ? C7 C6 C11 119.1(2) . . ? C5 C6 C11 123.3(3) . . ? C8 C7 C6 121.4(3) . . ? C8 C7 H7A 119.3 . . ? C6 C7 H7A 119.3 . . ? C7 C8 C9 119.9(3) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C8 C9 C10 121.1(3) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C5 C10 C9 117.8(3) . . ? C5 C10 C14 123.0(2) . . ? C9 C10 C14 119.1(2) . . ? C6 C11 C12 112.3(3) . . ? C6 C11 C13 111.8(2) . . ? C12 C11 C13 108.8(3) . . ? C6 C11 H11A 107.9 . . ? C12 C11 H11A 107.9 . . ? C13 C11 H11A 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 C15 112.6(2) . . ? C10 C14 C16 111.4(2) . . ? C15 C14 C16 110.6(2) . . ? C10 C14 H14A 107.3 . . ? C15 C14 H14A 107.3 . . ? C16 C14 H14A 107.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C19 125.6(2) . . ? N2 C18 C17 119.4(2) . . ? C19 C18 C17 115.0(2) . . ? C18 C19 C20 132.2(3) . . ? C18 C19 H19A 113.9 . . ? C20 C19 H19A 113.9 . . ? N3 C20 C19 123.7(2) . . ? N3 C20 C21 122.6(2) . . ? C19 C20 C21 113.7(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 121.3(2) . . ? C27 C22 N3 118.5(2) . . ? C23 C22 N3 120.1(2) . . ? C24 C23 C22 117.2(3) . . ? C24 C23 C28 118.4(2) . . ? C22 C23 C28 124.3(2) . . ? C25 C24 C23 121.5(3) . . ? C25 C24 H24A 119.2 . . ? C23 C24 H24A 119.2 . . ? C24 C25 C26 120.4(3) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C27 120.7(3) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C26 C27 C22 118.3(3) . . ? C26 C27 C31 119.2(3) . . ? C22 C27 C31 122.3(2) . . ? C23 C28 C29 114.7(3) . . ? C23 C28 C30 109.9(2) . . ? C29 C28 C30 108.2(3) . . ? C23 C28 H28A 108.0 . . ? C29 C28 H28A 108.0 . . ? C30 C28 H28A 108.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 C33 110.3(2) . . ? C27 C31 C32 113.7(2) . . ? C33 C31 C32 108.5(2) . . ? C27 C31 H31A 108.1 . . ? C33 C31 H31A 108.1 . . ? C32 C31 H31A 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 C35 123.5(3) . . ? N4 C34 H34A 118.3 . . ? C35 C34 H34A 118.3 . . ? C34 C35 C36 119.1(3) . . ? C34 C35 H35A 120.5 . . ? C36 C35 H35A 120.5 . . ? C35 C36 C37 118.5(3) . . ? C35 C36 H36A 120.8 . . ? C37 C36 H36A 120.8 . . ? C38 C37 C36 118.9(3) . . ? C38 C37 H37A 120.6 . . ? C36 C37 H37A 120.6 . . ? N4 C38 C37 123.9(3) . . ? N4 C38 H38A 118.1 . . ? C37 C38 H38A 118.1 . . ? 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 131.5(7) . . . . ? N4 Nb1 N1 C1 -52.6(7) . . . . ? Cl2 Nb1 N1 C1 29.7(7) . . . . ? Cl1 Nb1 N1 C1 -134.9(7) . . . . ? N3 Nb1 N1 C1 6.2(11) . . . . ? N1 Nb1 N2 C18 166.1(2) . . . . ? N4 Nb1 N2 C18 21.5(8) . . . . ? Cl2 Nb1 N2 C18 -102.2(2) . . . . ? Cl1 Nb1 N2 C18 63.5(2) . . . . ? N3 Nb1 N2 C18 -20.5(2) . . . . ? N1 Nb1 N2 C5 -9.60(19) . . . . ? N4 Nb1 N2 C5 -154.2(6) . . . . ? Cl2 Nb1 N2 C5 82.09(17) . . . . ? Cl1 Nb1 N2 C5 -112.24(17) . . . . ? N3 Nb1 N2 C5 163.79(18) . . . . ? N1 Nb1 N3 C20 148.9(6) . . . . ? N2 Nb1 N3 C20 22.7(2) . . . . ? N4 Nb1 N3 C20 -152.6(2) . . . . ? Cl2 Nb1 N3 C20 125.12(19) . . . . ? Cl1 Nb1 N3 C20 -69.24(19) . . . . ? N1 Nb1 N3 C22 -36.6(7) . . . . ? N2 Nb1 N3 C22 -162.72(19) . . . . ? N4 Nb1 N3 C22 21.97(18) . . . . ? Cl2 Nb1 N3 C22 -60.31(18) . . . . ? Cl1 Nb1 N3 C22 105.34(18) . . . . ? N1 Nb1 N4 C38 115.1(2) . . . . ? N2 Nb1 N4 C38 -99.8(6) . . . . ? Cl2 Nb1 N4 C38 24.9(2) . . . . ? Cl1 Nb1 N4 C38 -142.1(2) . . . . ? N3 Nb1 N4 C38 -58.0(2) . . . . ? N1 Nb1 N4 C34 -52.6(2) . . . . ? N2 Nb1 N4 C34 92.5(7) . . . . ? Cl2 Nb1 N4 C34 -142.85(19) . . . . ? Cl1 Nb1 N4 C34 50.15(18) . . . . ? N3 Nb1 N4 C34 134.26(19) . . . . ? Nb1 N1 C1 C2 -109.7(7) . . . . ? Nb1 N1 C1 C4 10.3(8) . . . . ? Nb1 N1 C1 C3 129.1(6) . . . . ? C18 N2 C5 C10 92.1(3) . . . . ? Nb1 N2 C5 C10 -91.7(2) . . . . ? C18 N2 C5 C6 -85.2(3) . . . . ? Nb1 N2 C5 C6 91.1(3) . . . . ? C10 C5 C6 C7 5.1(4) . . . . ? N2 C5 C6 C7 -177.8(2) . . . . ? C10 C5 C6 C11 -173.8(3) . . . . ? N2 C5 C6 C11 3.4(4) . . . . ? C5 C6 C7 C8 -1.8(4) . . . . ? C11 C6 C7 C8 177.1(3) . . . . ? C6 C7 C8 C9 -1.5(5) . . . . ? C7 C8 C9 C10 1.7(5) . . . . ? C6 C5 C10 C9 -4.9(4) . . . . ? N2 C5 C10 C9 177.9(2) . . . . ? C6 C5 C10 C14 171.7(3) . . . . ? N2 C5 C10 C14 -5.5(4) . . . . ? C8 C9 C10 C5 1.4(4) . . . . ? C8 C9 C10 C14 -175.3(3) . . . . ? C7 C6 C11 C12 68.8(3) . . . . ? C5 C6 C11 C12 -112.3(3) . . . . ? C7 C6 C11 C13 -53.8(4) . . . . ? C5 C6 C11 C13 125.1(3) . . . . ? C5 C10 C14 C15 132.3(3) . . . . ? C9 C10 C14 C15 -51.2(3) . . . . ? C5 C10 C14 C16 -102.8(3) . . . . ? C9 C10 C14 C16 73.8(3) . . . . ? C5 N2 C18 C19 -173.5(3) . . . . ? Nb1 N2 C18 C19 10.7(4) . . . . ? C5 N2 C18 C17 8.4(3) . . . . ? Nb1 N2 C18 C17 -167.42(19) . . . . ? N2 C18 C19 C20 9.8(5) . . . . ? C17 C18 C19 C20 -172.0(3) . . . . ? C22 N3 C20 C19 170.4(3) . . . . ? Nb1 N3 C20 C19 -14.9(4) . . . . ? C22 N3 C20 C21 -11.1(4) . . . . ? Nb1 N3 C20 C21 163.6(2) . . . . ? C18 C19 C20 N3 -5.3(5) . . . . ? C18 C19 C20 C21 176.0(3) . . . . ? C20 N3 C22 C27 -92.9(3) . . . . ? Nb1 N3 C22 C27 92.4(2) . . . . ? C20 N3 C22 C23 89.3(3) . . . . ? Nb1 N3 C22 C23 -85.5(3) . . . . ? C27 C22 C23 C24 -7.2(4) . . . . ? N3 C22 C23 C24 170.6(2) . . . . ? C27 C22 C23 C28 168.6(3) . . . . ? N3 C22 C23 C28 -13.6(4) . . . . ? C22 C23 C24 C25 1.4(4) . . . . ? C28 C23 C24 C25 -174.7(3) . . . . ? C23 C24 C25 C26 3.6(5) . . . . ? C24 C25 C26 C27 -2.8(4) . . . . ? C25 C26 C27 C22 -2.8(4) . . . . ? C25 C26 C27 C31 173.6(3) . . . . ? C23 C22 C27 C26 8.0(4) . . . . ? N3 C22 C27 C26 -169.8(2) . . . . ? C23 C22 C27 C31 -168.3(2) . . . . ? N3 C22 C27 C31 13.9(4) . . . . ? C24 C23 C28 C29 -59.3(4) . . . . ? C22 C23 C28 C29 125.0(3) . . . . ? C24 C23 C28 C30 62.9(3) . . . . ? C22 C23 C28 C30 -112.9(3) . . . . ? C26 C27 C31 C33 -83.8(3) . . . . ? C22 C27 C31 C33 92.5(3) . . . . ? C26 C27 C31 C32 38.3(4) . . . . ? C22 C27 C31 C32 -145.4(3) . . . . ? C38 N4 C34 C35 -1.5(4) . . . . ? Nb1 N4 C34 C35 167.4(2) . . . . ? N4 C34 C35 C36 0.9(5) . . . . ? C34 C35 C36 C37 0.5(5) . . . . ? C35 C36 C37 C38 -1.1(5) . . . . ? C34 N4 C38 C37 0.8(4) . . . . ? Nb1 N4 C38 C37 -167.1(2) . . . . ? C36 C37 C38 N4 0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.014 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.067 #===END data_(BDI)Cl2Nb(NAr) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H58 Cl2 N3 Nb' _chemical_formula_sum 'C41 H58 Cl2 N3 Nb' _chemical_formula_weight 756.71 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P b c a' 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 17.840(5) _cell_length_b 21.065(6) _cell_length_c 21.778(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8184(4) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9056 _cell_measurement_theta_min 7.273 _cell_measurement_theta_max 52.551 _exptl_crystal_description 'block' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.900330 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37957 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 26.38 _reflns_number_total 8076 _reflns_number_gt 6046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker-AXS XP v.6' _computing_publication_material 'Bruker-AXS XP v.6' _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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8076 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.011 _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 0.568163(10) 0.136803(9) 0.727664(8) 0.01773(7) Uani 1 1 d . . . Cl1 Cl 0.45802(3) 0.08340(3) 0.76178(3) 0.02801(14) Uani 1 1 d . . . Cl2 Cl 0.49838(3) 0.23249(3) 0.72843(3) 0.02773(14) Uani 1 1 d . . . N1 N 0.57795(9) 0.11265(9) 0.65102(8) 0.0220(4) Uani 1 1 d . . . N2 N 0.63291(10) 0.06749(8) 0.77885(7) 0.0182(4) Uani 1 1 d . . . N3 N 0.66924(9) 0.19505(8) 0.73564(7) 0.0190(4) Uani 1 1 d . . . C1 C 0.57763(12) 0.09680(10) 0.58854(9) 0.0219(5) Uani 1 1 d . . . C2 C 0.51319(12) 0.11074(11) 0.55259(10) 0.0255(5) Uani 1 1 d . . . C3 C 0.51386(14) 0.09238(12) 0.49178(11) 0.0346(6) Uani 1 1 d . . . H3A H 0.4715 0.0995 0.4678 0.042 Uiso 1 1 calc R . . C4 C 0.57571(14) 0.06375(13) 0.46560(11) 0.0363(6) Uani 1 1 d . . . H4A H 0.5748 0.0521 0.4244 0.044 Uiso 1 1 calc R . . C5 C 0.63851(14) 0.05251(12) 0.50023(10) 0.0321(6) Uani 1 1 d . . . H5A H 0.6802 0.0340 0.4819 0.039 Uiso 1 1 calc R . . C6 C 0.64131(13) 0.06825(11) 0.56226(10) 0.0264(5) Uani 1 1 d . . . C7 C 0.44513(13) 0.14366(12) 0.58006(12) 0.0320(6) Uani 1 1 d . . . H7A H 0.4620 0.1671 0.6164 0.038 Uiso 1 1 calc R . . C8 C 0.38670(14) 0.09569(14) 0.60104(13) 0.0436(7) Uani 1 1 d . . . H8A H 0.4093 0.0661 0.6290 0.065 Uiso 1 1 calc R . . H8B H 0.3676 0.0732 0.5661 0.065 Uiso 1 1 calc R . . H8C H 0.3464 0.1175 0.6213 0.065 Uiso 1 1 calc R . . C9 C 0.40904(16) 0.19184(14) 0.53583(13) 0.0493(8) Uani 1 1 d . . . H9A H 0.4460 0.2222 0.5230 0.074 Uiso 1 1 calc R . . H9B H 0.3688 0.2134 0.5564 0.074 Uiso 1 1 calc R . . H9C H 0.3898 0.1699 0.5005 0.074 Uiso 1 1 calc R . . C10 C 0.71148(13) 0.05422(12) 0.59891(11) 0.0355(6) Uani 1 1 d . . . H10A H 0.7004 0.0632 0.6421 0.043 Uiso 1 1 calc R . . C11 C 0.73391(17) -0.01563(14) 0.59422(13) 0.0507(8) Uani 1 1 d . . . H11A H 0.6927 -0.0418 0.6071 0.076 Uiso 1 1 calc R . . H11B H 0.7764 -0.0235 0.6202 0.076 Uiso 1 1 calc R . . H11C H 0.7467 -0.0255 0.5525 0.076 Uiso 1 1 calc R . . C12 C 0.77686(15) 0.09620(16) 0.57996(15) 0.0554(8) Uani 1 1 d . . . H12A H 0.7626 0.1400 0.5836 0.083 Uiso 1 1 calc R . . H12B H 0.7902 0.0872 0.5381 0.083 Uiso 1 1 calc R . . H12C H 0.8190 0.0879 0.6061 0.083 Uiso 1 1 calc R . . C13 C 0.59471(12) 0.01857(10) 0.81446(10) 0.0217(5) Uani 1 1 d . . . C14 C 0.58235(12) -0.04134(11) 0.78824(10) 0.0241(5) Uani 1 1 d . . . C15 C 0.54857(14) -0.08754(12) 0.82445(11) 0.0340(6) Uani 1 1 d . . . H15A H 0.5402 -0.1277 0.8082 0.041 Uiso 1 1 calc R . . C16 C 0.52726(16) -0.07486(13) 0.88399(12) 0.0441(7) Uani 1 1 d . . . H16A H 0.5052 -0.1065 0.9077 0.053 Uiso 1 1 calc R . . C17 C 0.53866(16) -0.01533(13) 0.90822(11) 0.0420(7) Uani 1 1 d . . . H17A H 0.5241 -0.0073 0.9485 0.050 Uiso 1 1 calc R . . C18 C 0.57127(12) 0.03299(11) 0.87418(10) 0.0277(5) Uani 1 1 d . . . C19 C 0.60432(13) -0.05722(11) 0.72260(10) 0.0254(5) Uani 1 1 d . . . H19A H 0.6399 -0.0249 0.7085 0.031 Uiso 1 1 calc R . . C20 C 0.53592(14) -0.05546(12) 0.68015(11) 0.0349(6) Uani 1 1 d . . . H20A H 0.5123 -0.0146 0.6829 0.052 Uiso 1 1 calc R . . H20B H 0.5010 -0.0878 0.6923 0.052 Uiso 1 1 calc R . . H20C H 0.5516 -0.0629 0.6386 0.052 Uiso 1 1 calc R . . C21 C 0.64266(14) -0.12235(12) 0.71763(12) 0.0340(6) Uani 1 1 d . . . H21A H 0.6860 -0.1232 0.7438 0.051 Uiso 1 1 calc R . . H21B H 0.6577 -0.1296 0.6759 0.051 Uiso 1 1 calc R . . H21C H 0.6082 -0.1549 0.7301 0.051 Uiso 1 1 calc R . . C22 C 0.58067(13) 0.09867(12) 0.90199(11) 0.0320(6) Uani 1 1 d . . . H22A H 0.5901 0.1281 0.8680 0.038 Uiso 1 1 calc R . . C23 C 0.51016(16) 0.12154(14) 0.93483(13) 0.0473(7) Uani 1 1 d . . . H23A H 0.4685 0.1201 0.9070 0.071 Uiso 1 1 calc R . . H23B H 0.5174 0.1643 0.9487 0.071 Uiso 1 1 calc R . . H23C H 0.5002 0.0946 0.9694 0.071 Uiso 1 1 calc R . . C24 C 0.64839(17) 0.10179(17) 0.94436(15) 0.0686(11) Uani 1 1 d . . . H24A H 0.6921 0.0875 0.9227 0.103 Uiso 1 1 calc R . . H24B H 0.6400 0.0751 0.9794 0.103 Uiso 1 1 calc R . . H24C H 0.6558 0.1448 0.9577 0.103 Uiso 1 1 calc R . . C25 C 0.74610(13) 0.00682(11) 0.80766(11) 0.0284(5) Uani 1 1 d . . . H25A H 0.7308 0.0038 0.8498 0.043 Uiso 1 1 calc R . . H25B H 0.7994 0.0127 0.8057 0.043 Uiso 1 1 calc R . . H25C H 0.7327 -0.0315 0.7864 0.043 Uiso 1 1 calc R . . C26 C 0.70735(12) 0.06275(10) 0.77782(9) 0.0202(5) Uani 1 1 d . . . C27 C 0.75496(12) 0.10811(10) 0.75252(10) 0.0227(5) Uani 1 1 d . . . H27A H 0.8037 0.0949 0.7446 0.027 Uiso 1 1 calc R . . C28 C 0.73847(12) 0.17097(10) 0.73758(9) 0.0213(5) Uani 1 1 d . . . C29 C 0.80559(13) 0.21358(12) 0.72859(11) 0.0316(6) Uani 1 1 d . . . H29A H 0.7971 0.2409 0.6940 0.047 Uiso 1 1 calc R . . H29B H 0.8493 0.1881 0.7213 0.047 Uiso 1 1 calc R . . H29C H 0.8130 0.2389 0.7647 0.047 Uiso 1 1 calc R . . C30 C 0.66366(11) 0.26398(10) 0.73173(9) 0.0201(5) Uani 1 1 d . . . C31 C 0.66054(12) 0.29365(10) 0.67381(10) 0.0231(5) Uani 1 1 d . . . C32 C 0.64904(12) 0.35870(10) 0.67235(11) 0.0266(5) Uani 1 1 d . . . H32A H 0.6464 0.3791 0.6346 0.032 Uiso 1 1 calc R . . C33 C 0.64144(13) 0.39397(11) 0.72515(11) 0.0281(5) Uani 1 1 d . . . H33A H 0.6318 0.4373 0.7230 0.034 Uiso 1 1 calc R . . C34 C 0.64826(13) 0.36433(11) 0.78148(11) 0.0271(5) Uani 1 1 d . . . H34A H 0.6453 0.3885 0.8171 0.032 Uiso 1 1 calc R . . C35 C 0.65940(12) 0.29939(11) 0.78594(10) 0.0239(5) Uani 1 1 d . . . C36 C 0.66836(13) 0.25773(11) 0.61376(10) 0.0279(5) Uani 1 1 d . . . H36A H 0.6763 0.2128 0.6235 0.034 Uiso 1 1 calc R . . C37 C 0.59714(14) 0.26297(12) 0.57519(11) 0.0347(6) Uani 1 1 d . . . H37A H 0.5550 0.2488 0.5989 0.052 Uiso 1 1 calc R . . H37B H 0.6020 0.2370 0.5392 0.052 Uiso 1 1 calc R . . H37C H 0.5897 0.3064 0.5632 0.052 Uiso 1 1 calc R . . C38 C 0.73599(14) 0.28099(13) 0.57642(11) 0.0386(6) Uani 1 1 d . . . H38A H 0.7806 0.2776 0.6009 0.058 Uiso 1 1 calc R . . H38B H 0.7284 0.3245 0.5648 0.058 Uiso 1 1 calc R . . H38C H 0.7412 0.2554 0.5402 0.058 Uiso 1 1 calc R . . C39 C 0.66565(14) 0.26922(12) 0.84905(10) 0.0328(6) Uani 1 1 d . . . H39A H 0.6760 0.2239 0.8435 0.039 Uiso 1 1 calc R . . C40 C 0.59192(16) 0.27576(14) 0.88403(12) 0.0467(7) Uani 1 1 d . . . H40A H 0.5521 0.2572 0.8604 0.070 Uiso 1 1 calc R . . H40B H 0.5814 0.3199 0.8909 0.070 Uiso 1 1 calc R . . H40C H 0.5959 0.2543 0.9228 0.070 Uiso 1 1 calc R . . C41 C 0.72998(16) 0.29804(15) 0.88628(13) 0.0544(8) Uani 1 1 d . . . H41A H 0.7761 0.2931 0.8641 0.082 Uiso 1 1 calc R . . H41B H 0.7337 0.2767 0.9251 0.082 Uiso 1 1 calc R . . H41C H 0.7204 0.3423 0.8930 0.082 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 0.01556(11) 0.01883(12) 0.01879(11) -0.00021(8) -0.00083(7) 0.00091(8) Cl1 0.0188(3) 0.0267(3) 0.0385(3) 0.0046(3) 0.0014(2) -0.0010(2) Cl2 0.0202(3) 0.0225(3) 0.0405(3) 0.0003(3) 0.0017(2) 0.0034(2) N1 0.0220(10) 0.0203(10) 0.0236(10) 0.0031(8) -0.0033(7) 0.0020(8) N2 0.0194(9) 0.0155(9) 0.0197(9) -0.0006(7) -0.0011(7) 0.0003(7) N3 0.0170(9) 0.0179(9) 0.0220(9) 0.0005(7) -0.0003(7) 0.0002(7) C1 0.0280(12) 0.0177(11) 0.0200(11) 0.0016(9) -0.0010(9) -0.0034(9) C2 0.0258(12) 0.0233(12) 0.0276(12) 0.0013(10) -0.0031(9) -0.0048(10) C3 0.0384(15) 0.0395(15) 0.0259(13) 0.0001(11) -0.0084(11) -0.0025(12) C4 0.0492(16) 0.0394(15) 0.0203(12) -0.0034(11) 0.0000(11) -0.0006(13) C5 0.0384(14) 0.0319(14) 0.0260(13) -0.0024(11) 0.0071(11) 0.0021(11) C6 0.0300(13) 0.0236(12) 0.0257(12) 0.0024(10) 0.0003(10) -0.0025(10) C7 0.0275(13) 0.0383(15) 0.0304(13) -0.0046(11) -0.0066(10) -0.0004(11) C8 0.0319(15) 0.0482(18) 0.0508(17) -0.0060(14) 0.0038(12) -0.0006(13) C9 0.0443(17) 0.0548(19) 0.0489(17) 0.0043(15) -0.0111(13) 0.0155(15) C10 0.0343(14) 0.0417(16) 0.0305(13) -0.0063(12) -0.0009(10) 0.0128(12) C11 0.0594(19) 0.0479(18) 0.0447(16) 0.0073(14) 0.0044(14) 0.0284(16) C12 0.0340(16) 0.061(2) 0.072(2) -0.0161(17) -0.0036(14) 0.0041(15) C13 0.0173(11) 0.0233(12) 0.0244(11) 0.0041(10) -0.0030(9) -0.0009(9) C14 0.0234(12) 0.0222(12) 0.0267(12) 0.0024(10) -0.0046(9) -0.0003(10) C15 0.0398(15) 0.0248(13) 0.0373(14) 0.0006(11) -0.0042(11) -0.0101(11) C16 0.0614(19) 0.0364(16) 0.0345(15) 0.0097(12) 0.0021(13) -0.0168(14) C17 0.0599(18) 0.0419(16) 0.0244(13) 0.0022(12) 0.0077(12) -0.0154(14) C18 0.0305(13) 0.0292(13) 0.0234(12) 0.0012(10) -0.0011(9) -0.0049(11) C19 0.0238(12) 0.0226(12) 0.0299(13) -0.0026(10) -0.0006(9) -0.0025(10) C20 0.0345(14) 0.0411(16) 0.0291(13) -0.0093(12) -0.0027(11) 0.0018(12) C21 0.0304(14) 0.0244(13) 0.0471(16) -0.0057(11) -0.0003(11) -0.0015(11) C22 0.0403(15) 0.0343(14) 0.0213(12) -0.0037(11) 0.0043(10) -0.0088(12) C23 0.0531(18) 0.0444(17) 0.0444(16) -0.0089(14) 0.0140(14) -0.0053(14) C24 0.058(2) 0.069(2) 0.078(2) -0.043(2) -0.0207(17) 0.0046(18) C25 0.0233(12) 0.0235(13) 0.0383(14) 0.0021(11) -0.0065(10) 0.0009(10) C26 0.0210(12) 0.0202(12) 0.0195(11) -0.0043(9) -0.0026(8) -0.0003(9) C27 0.0170(11) 0.0233(13) 0.0277(11) -0.0006(10) 0.0013(9) 0.0007(9) C28 0.0190(12) 0.0214(12) 0.0235(12) -0.0015(9) 0.0010(9) -0.0025(9) C29 0.0201(12) 0.0263(13) 0.0484(15) 0.0046(11) -0.0005(10) -0.0029(10) C30 0.0158(11) 0.0188(11) 0.0258(11) 0.0017(9) -0.0001(9) -0.0002(9) C31 0.0178(11) 0.0246(12) 0.0269(12) -0.0001(10) -0.0006(9) -0.0026(9) C32 0.0264(13) 0.0236(12) 0.0298(13) 0.0069(10) -0.0035(10) -0.0042(10) C33 0.0258(13) 0.0166(12) 0.0420(15) 0.0043(11) -0.0037(10) -0.0010(10) C34 0.0253(13) 0.0229(12) 0.0330(13) -0.0064(10) 0.0008(9) -0.0026(10) C35 0.0198(12) 0.0230(12) 0.0287(12) -0.0005(10) -0.0001(9) -0.0011(10) C36 0.0373(14) 0.0243(13) 0.0223(12) 0.0041(10) 0.0015(10) -0.0010(11) C37 0.0447(15) 0.0327(15) 0.0268(13) 0.0026(11) -0.0028(11) -0.0080(12) C38 0.0427(16) 0.0427(16) 0.0303(13) 0.0023(12) 0.0078(11) -0.0018(13) C39 0.0480(16) 0.0254(13) 0.0248(12) -0.0027(10) -0.0021(11) 0.0011(12) C40 0.0663(19) 0.0431(17) 0.0308(15) 0.0018(13) 0.0119(13) -0.0048(15) C41 0.063(2) 0.062(2) 0.0382(16) 0.0057(15) -0.0193(14) -0.0022(17) _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 1.7538(18) . ? Nb1 N2 2.1699(17) . ? Nb1 N3 2.1879(18) . ? Nb1 Cl2 2.3693(8) . ? Nb1 Cl1 2.3829(8) . ? N1 C1 1.401(3) . ? N2 C26 1.332(3) . ? N2 C13 1.459(3) . ? N3 C28 1.336(3) . ? N3 C30 1.458(3) . ? C1 C6 1.407(3) . ? C1 C2 1.422(3) . ? C2 C3 1.380(3) . ? C2 C7 1.521(3) . ? C3 C4 1.381(3) . ? C3 H3A 0.9300 . ? C4 C5 1.371(3) . ? C4 H4A 0.9300 . ? C5 C6 1.392(3) . ? C5 H5A 0.9300 . ? C6 C10 1.514(3) . ? C7 C8 1.522(3) . ? C7 C9 1.540(4) . ? C7 H7A 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.521(4) . ? C10 C11 1.528(4) . ? C10 H10A 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.399(3) . ? C13 C14 1.403(3) . ? C14 C15 1.390(3) . ? C14 C19 1.519(3) . ? C15 C16 1.377(3) . ? C15 H15A 0.9300 . ? C16 C17 1.376(4) . ? C16 H16A 0.9300 . ? C17 C18 1.387(3) . ? C17 H17A 0.9300 . ? C18 C22 1.519(3) . ? C19 C20 1.531(3) . ? C19 C21 1.537(3) . ? C19 H19A 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C24 1.522(4) . ? C22 C23 1.525(3) . ? C22 H22A 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.513(3) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.392(3) . ? C27 C28 1.395(3) . ? C27 H27A 0.9300 . ? C28 C29 1.509(3) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C35 1.399(3) . ? C30 C31 1.409(3) . ? C31 C32 1.386(3) . ? C31 C36 1.517(3) . ? C32 C33 1.376(3) . ? C32 H32A 0.9300 . ? C33 C34 1.382(3) . ? C33 H33A 0.9300 . ? C34 C35 1.386(3) . ? C34 H34A 0.9300 . ? C35 C39 1.518(3) . ? C36 C37 1.527(3) . ? C36 C38 1.535(3) . ? C36 H36A 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.526(3) . ? C39 C41 1.531(3) . ? C39 H39A 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Nb1 N2 103.93(7) . . ? N1 Nb1 N3 98.99(7) . . ? N2 Nb1 N3 84.14(7) . . ? N1 Nb1 Cl2 107.81(6) . . ? N2 Nb1 Cl2 148.05(5) . . ? N3 Nb1 Cl2 87.45(5) . . ? N1 Nb1 Cl1 104.00(6) . . ? N2 Nb1 Cl1 87.77(5) . . ? N3 Nb1 Cl1 156.86(5) . . ? Cl2 Nb1 Cl1 88.06(3) . . ? C1 N1 Nb1 173.27(16) . . ? C26 N2 C13 114.94(17) . . ? C26 N2 Nb1 124.93(14) . . ? C13 N2 Nb1 119.99(13) . . ? C28 N3 C30 116.30(18) . . ? C28 N3 Nb1 123.48(15) . . ? C30 N3 Nb1 119.84(13) . . ? N1 C1 C6 119.6(2) . . ? N1 C1 C2 119.3(2) . . ? C6 C1 C2 121.1(2) . . ? C3 C2 C1 117.6(2) . . ? C3 C2 C7 120.8(2) . . ? C1 C2 C7 121.5(2) . . ? C2 C3 C4 121.7(2) . . ? C2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? C5 C4 C3 120.1(2) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 121.5(2) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C1 117.9(2) . . ? C5 C6 C10 119.7(2) . . ? C1 C6 C10 122.5(2) . . ? C2 C7 C8 111.2(2) . . ? C2 C7 C9 112.8(2) . . ? C8 C7 C9 109.8(2) . . ? C2 C7 H7A 107.6 . . ? C8 C7 H7A 107.6 . . ? C9 C7 H7A 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 112.2(2) . . ? C6 C10 C11 111.7(2) . . ? C12 C10 C11 109.9(2) . . ? C6 C10 H10A 107.6 . . ? C12 C10 H10A 107.6 . . ? C11 C10 H10A 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 121.8(2) . . ? C18 C13 N2 118.70(19) . . ? C14 C13 N2 119.51(19) . . ? C15 C14 C13 117.8(2) . . ? C15 C14 C19 119.4(2) . . ? C13 C14 C19 122.7(2) . . ? C16 C15 C14 121.2(2) . . ? C16 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C17 C16 C15 119.8(2) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 121.7(2) . . ? C16 C17 H17A 119.1 . . ? C18 C17 H17A 119.1 . . ? C17 C18 C13 117.6(2) . . ? C17 C18 C22 120.1(2) . . ? C13 C18 C22 122.3(2) . . ? C14 C19 C20 110.92(19) . . ? C14 C19 C21 112.19(19) . . ? C20 C19 C21 109.49(19) . . ? C14 C19 H19A 108.0 . . ? C20 C19 H19A 108.0 . . ? C21 C19 H19A 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C24 111.6(2) . . ? C18 C22 C23 112.5(2) . . ? C24 C22 C23 110.9(2) . . ? C18 C22 H22A 107.1 . . ? C24 C22 H22A 107.1 . . ? C23 C22 H22A 107.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 C27 124.3(2) . . ? N2 C26 C25 120.45(19) . . ? C27 C26 C25 115.20(19) . . ? C26 C27 C28 128.0(2) . . ? C26 C27 H27A 116.0 . . ? C28 C27 H27A 116.0 . . ? N3 C28 C27 124.2(2) . . ? N3 C28 C29 120.2(2) . . ? C27 C28 C29 115.31(19) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 121.1(2) . . ? C35 C30 N3 119.05(18) . . ? C31 C30 N3 119.79(18) . . ? C32 C31 C30 117.7(2) . . ? C32 C31 C36 119.1(2) . . ? C30 C31 C36 123.15(19) . . ? C33 C32 C31 122.0(2) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 119.3(2) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? C33 C34 C35 121.4(2) . . ? C33 C34 H34A 119.3 . . ? C35 C34 H34A 119.3 . . ? C34 C35 C30 118.4(2) . . ? C34 C35 C39 119.2(2) . . ? C30 C35 C39 122.5(2) . . ? C31 C36 C37 111.20(19) . . ? C31 C36 C38 111.69(19) . . ? C37 C36 C38 109.84(19) . . ? C31 C36 H36A 108.0 . . ? C37 C36 H36A 108.0 . . ? C38 C36 H36A 108.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 C40 110.5(2) . . ? C35 C39 C41 111.6(2) . . ? C40 C39 C41 110.2(2) . . ? C35 C39 H39A 108.1 . . ? C40 C39 H39A 108.1 . . ? C41 C39 H39A 108.1 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 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 153.2(14) . . . . ? N3 Nb1 N1 C1 -120.6(14) . . . . ? Cl2 Nb1 N1 C1 -30.4(14) . . . . ? Cl1 Nb1 N1 C1 62.1(14) . . . . ? N1 Nb1 N2 C26 69.79(18) . . . . ? N3 Nb1 N2 C26 -28.04(16) . . . . ? Cl2 Nb1 N2 C26 -103.60(17) . . . . ? Cl1 Nb1 N2 C26 173.66(16) . . . . ? N1 Nb1 N2 C13 -105.68(15) . . . . ? N3 Nb1 N2 C13 156.48(15) . . . . ? Cl2 Nb1 N2 C13 80.92(17) . . . . ? Cl1 Nb1 N2 C13 -1.81(14) . . . . ? N1 Nb1 N3 C28 -71.73(17) . . . . ? N2 Nb1 N3 C28 31.49(16) . . . . ? Cl2 Nb1 N3 C28 -179.37(16) . . . . ? Cl1 Nb1 N3 C28 101.62(18) . . . . ? N1 Nb1 N3 C30 100.93(15) . . . . ? N2 Nb1 N3 C30 -155.84(15) . . . . ? Cl2 Nb1 N3 C30 -6.70(14) . . . . ? Cl1 Nb1 N3 C30 -85.71(18) . . . . ? Nb1 N1 C1 C6 173.5(13) . . . . ? Nb1 N1 C1 C2 -5.6(15) . . . . ? N1 C1 C2 C3 -177.7(2) . . . . ? C6 C1 C2 C3 3.2(3) . . . . ? N1 C1 C2 C7 1.2(3) . . . . ? C6 C1 C2 C7 -177.8(2) . . . . ? C1 C2 C3 C4 -2.5(4) . . . . ? C7 C2 C3 C4 178.5(2) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? C3 C4 C5 C6 1.3(4) . . . . ? C4 C5 C6 C1 -0.6(4) . . . . ? C4 C5 C6 C10 179.2(2) . . . . ? N1 C1 C6 C5 179.2(2) . . . . ? C2 C1 C6 C5 -1.7(3) . . . . ? N1 C1 C6 C10 -0.6(3) . . . . ? C2 C1 C6 C10 178.5(2) . . . . ? C3 C2 C7 C8 84.4(3) . . . . ? C1 C2 C7 C8 -94.5(3) . . . . ? C3 C2 C7 C9 -39.5(3) . . . . ? C1 C2 C7 C9 141.6(2) . . . . ? C5 C6 C10 C12 69.3(3) . . . . ? C1 C6 C10 C12 -110.9(3) . . . . ? C5 C6 C10 C11 -54.6(3) . . . . ? C1 C6 C10 C11 125.2(2) . . . . ? C26 N2 C13 C18 99.2(2) . . . . ? Nb1 N2 C13 C18 -84.9(2) . . . . ? C26 N2 C13 C14 -80.9(2) . . . . ? Nb1 N2 C13 C14 95.0(2) . . . . ? C18 C13 C14 C15 -2.7(3) . . . . ? N2 C13 C14 C15 177.4(2) . . . . ? C18 C13 C14 C19 177.3(2) . . . . ? N2 C13 C14 C19 -2.6(3) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? C19 C14 C15 C16 -179.5(2) . . . . ? C14 C15 C16 C17 0.7(4) . . . . ? C15 C16 C17 C18 0.1(5) . . . . ? C16 C17 C18 C13 -2.1(4) . . . . ? C16 C17 C18 C22 178.1(3) . . . . ? C14 C13 C18 C17 3.4(3) . . . . ? N2 C13 C18 C17 -176.7(2) . . . . ? C14 C13 C18 C22 -176.8(2) . . . . ? N2 C13 C18 C22 3.1(3) . . . . ? C15 C14 C19 C20 78.5(3) . . . . ? C13 C14 C19 C20 -101.5(3) . . . . ? C15 C14 C19 C21 -44.2(3) . . . . ? C13 C14 C19 C21 135.7(2) . . . . ? C17 C18 C22 C24 79.7(3) . . . . ? C13 C18 C22 C24 -100.1(3) . . . . ? C17 C18 C22 C23 -45.8(3) . . . . ? C13 C18 C22 C23 134.4(2) . . . . ? C13 N2 C26 C27 -172.5(2) . . . . ? Nb1 N2 C26 C27 11.8(3) . . . . ? C13 N2 C26 C25 4.8(3) . . . . ? Nb1 N2 C26 C25 -170.88(14) . . . . ? N2 C26 C27 C28 16.6(4) . . . . ? C25 C26 C27 C28 -160.9(2) . . . . ? C30 N3 C28 C27 167.72(19) . . . . ? Nb1 N3 C28 C27 -19.4(3) . . . . ? C30 N3 C28 C29 -6.9(3) . . . . ? Nb1 N3 C28 C29 166.02(15) . . . . ? C26 C27 C28 N3 -12.1(4) . . . . ? C26 C27 C28 C29 162.7(2) . . . . ? C28 N3 C30 C35 -90.8(2) . . . . ? Nb1 N3 C30 C35 96.0(2) . . . . ? C28 N3 C30 C31 91.0(2) . . . . ? Nb1 N3 C30 C31 -82.2(2) . . . . ? C35 C30 C31 C32 -3.4(3) . . . . ? N3 C30 C31 C32 174.78(19) . . . . ? C35 C30 C31 C36 177.2(2) . . . . ? N3 C30 C31 C36 -4.6(3) . . . . ? C30 C31 C32 C33 0.5(3) . . . . ? C36 C31 C32 C33 179.9(2) . . . . ? C31 C32 C33 C34 2.5(4) . . . . ? C32 C33 C34 C35 -2.8(4) . . . . ? C33 C34 C35 C30 0.0(3) . . . . ? C33 C34 C35 C39 -179.3(2) . . . . ? C31 C30 C35 C34 3.2(3) . . . . ? N3 C30 C35 C34 -175.1(2) . . . . ? C31 C30 C35 C39 -177.5(2) . . . . ? N3 C30 C35 C39 4.2(3) . . . . ? C32 C31 C36 C37 -61.9(3) . . . . ? C30 C31 C36 C37 117.4(2) . . . . ? C32 C31 C36 C38 61.2(3) . . . . ? C30 C31 C36 C38 -119.5(2) . . . . ? C34 C35 C39 C40 64.8(3) . . . . ? C30 C35 C39 C40 -114.5(2) . . . . ? C34 C35 C39 C41 -58.3(3) . . . . ? C30 C35 C39 C41 122.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.882 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.065 #===END data_(BDI)Cl(ptol)Nb(NtBu) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H57 Cl N3 Nb' _chemical_formula_sum 'C40 H57 Cl N3 Nb' _chemical_formula_weight 708.25 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P 2(1) 2(1) 2(1)' 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' _cell_length_a 13.757(2) _cell_length_b 16.524(3) _cell_length_c 17.039(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3873.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 122(2) _cell_measurement_reflns_used 3462 _cell_measurement_theta_min 6.848 _cell_measurement_theta_max 44.787 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.870265 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17262 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.1235 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 24.70 _reflns_number_total 6488 _reflns_number_gt 5497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker-AXS XP v.6' _computing_publication_material 'Bruker-AXS XP v.6' _refine_special_details ; The crystal was found to be racemically twinned, and the data were successfully refined with a BASF parameter of 0.53382. 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.53(5) _refine_ls_number_reflns 6488 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.003 _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 0.66492(3) 0.89493(2) 0.20581(2) 0.02253(13) Uani 1 1 d . . . Cl1 Cl 0.60690(8) 0.99224(6) 0.30081(8) 0.0322(3) Uani 1 1 d . . . N1 N 0.7754(3) 0.9482(2) 0.1993(3) 0.0285(9) Uani 1 1 d . . . N2 N 0.7186(3) 0.7845(2) 0.1606(2) 0.0240(9) Uani 1 1 d . . . N3 N 0.5591(3) 0.8089(2) 0.2727(2) 0.0266(9) Uani 1 1 d . . . C1 C 0.8571(3) 1.0020(3) 0.2160(3) 0.0356(12) Uani 1 1 d . . . C2 C 0.8258(4) 1.0880(3) 0.1953(4) 0.0532(15) Uani 1 1 d . . . H2A H 0.8122 1.0914 0.1390 0.080 Uiso 1 1 calc R . . H2B H 0.8781 1.1259 0.2088 0.080 Uiso 1 1 calc R . . H2C H 0.7671 1.1020 0.2249 0.080 Uiso 1 1 calc R . . C3 C 0.8790(4) 0.9967(4) 0.3047(4) 0.0538(16) Uani 1 1 d . . . H3A H 0.8993 0.9415 0.3179 0.081 Uiso 1 1 calc R . . H3B H 0.8204 1.0106 0.3345 0.081 Uiso 1 1 calc R . . H3C H 0.9312 1.0347 0.3180 0.081 Uiso 1 1 calc R . . C4 C 0.9447(4) 0.9759(4) 0.1676(4) 0.0584(18) Uani 1 1 d . . . H4A H 0.9290 0.9797 0.1117 0.088 Uiso 1 1 calc R . . H4B H 0.9617 0.9199 0.1807 0.088 Uiso 1 1 calc R . . H4C H 1.0000 1.0114 0.1795 0.088 Uiso 1 1 calc R . . C5 C 0.5890(3) 0.9400(3) 0.1049(3) 0.0258(11) Uani 1 1 d . . . C6 C 0.5957(3) 1.0178(3) 0.0745(3) 0.0282(11) Uani 1 1 d . . . H6A H 0.6429 1.0539 0.0952 0.034 Uiso 1 1 calc R . . C7 C 0.5349(3) 1.0442(3) 0.0143(3) 0.0313(11) Uani 1 1 d . . . H7A H 0.5417 1.0976 -0.0056 0.038 Uiso 1 1 calc R . . C8 C 0.4645(3) 0.9935(3) -0.0169(3) 0.0301(11) Uani 1 1 d . . . C9 C 0.4565(4) 0.9163(3) 0.0132(3) 0.0387(13) Uani 1 1 d . . . H9A H 0.4088 0.8806 -0.0074 0.046 Uiso 1 1 calc R . . C10 C 0.5170(3) 0.8901(3) 0.0730(3) 0.0326(11) Uani 1 1 d . . . H10A H 0.5093 0.8368 0.0929 0.039 Uiso 1 1 calc R . . C11 C 0.3959(4) 1.0231(3) -0.0794(4) 0.0438(14) Uani 1 1 d . . . H11A H 0.4121 1.0791 -0.0931 0.066 Uiso 1 1 calc R . . H11B H 0.3290 1.0207 -0.0596 0.066 Uiso 1 1 calc R . . H11C H 0.4019 0.9887 -0.1260 0.066 Uiso 1 1 calc R . . C12 C 0.8209(3) 0.7806(3) 0.1354(3) 0.0260(10) Uani 1 1 d . . . C13 C 0.8478(3) 0.8018(3) 0.0591(3) 0.0281(11) Uani 1 1 d . . . C14 C 0.9465(4) 0.7966(3) 0.0390(3) 0.0360(12) Uani 1 1 d . . . H14A H 0.9667 0.8120 -0.0122 0.043 Uiso 1 1 calc R . . C15 C 1.0144(4) 0.7696(3) 0.0919(4) 0.0436(14) Uani 1 1 d . . . H15A H 1.0806 0.7651 0.0768 0.052 Uiso 1 1 calc R . . C16 C 0.9863(4) 0.7491(4) 0.1673(3) 0.0424(14) Uani 1 1 d . . . H16A H 1.0339 0.7306 0.2035 0.051 Uiso 1 1 calc R . . C17 C 0.8896(3) 0.7549(3) 0.1914(3) 0.0343(12) Uani 1 1 d . . . C18 C 0.7776(3) 0.8351(3) -0.0026(3) 0.0310(12) Uani 1 1 d . . . H18A H 0.7100 0.8263 0.0172 0.037 Uiso 1 1 calc R . . C19 C 0.7922(4) 0.9264(3) -0.0135(3) 0.0435(14) Uani 1 1 d . . . H19A H 0.7859 0.9536 0.0374 0.065 Uiso 1 1 calc R . . H19B H 0.7428 0.9473 -0.0497 0.065 Uiso 1 1 calc R . . H19C H 0.8570 0.9366 -0.0351 0.065 Uiso 1 1 calc R . . C20 C 0.7870(4) 0.7903(4) -0.0824(3) 0.0448(14) Uani 1 1 d . . . H20A H 0.7774 0.7321 -0.0744 0.067 Uiso 1 1 calc R . . H20B H 0.8519 0.7998 -0.1043 0.067 Uiso 1 1 calc R . . H20C H 0.7378 0.8108 -0.1189 0.067 Uiso 1 1 calc R . . C21 C 0.8620(4) 0.7343(4) 0.2742(3) 0.0454(15) Uani 1 1 d . . . H21A H 0.8046 0.7683 0.2885 0.054 Uiso 1 1 calc R . . C22 C 0.9420(5) 0.7524(4) 0.3328(3) 0.0562(17) Uani 1 1 d . . . H22A H 0.9622 0.8090 0.3275 0.084 Uiso 1 1 calc R . . H22B H 0.9977 0.7169 0.3227 0.084 Uiso 1 1 calc R . . H22C H 0.9178 0.7430 0.3861 0.084 Uiso 1 1 calc R . . C23 C 0.8325(5) 0.6468(4) 0.2832(4) 0.072(2) Uani 1 1 d . . . H23A H 0.7806 0.6342 0.2457 0.108 Uiso 1 1 calc R . . H23B H 0.8090 0.6375 0.3367 0.108 Uiso 1 1 calc R . . H23C H 0.8886 0.6119 0.2729 0.108 Uiso 1 1 calc R . . C24 C 0.7022(4) 0.6540(3) 0.0878(3) 0.0378(13) Uani 1 1 d . . . H24A H 0.6558 0.6091 0.0839 0.057 Uiso 1 1 calc R . . H24B H 0.7651 0.6333 0.1058 0.057 Uiso 1 1 calc R . . H24C H 0.7100 0.6794 0.0363 0.057 Uiso 1 1 calc R . . C25 C 0.6645(4) 0.7160(3) 0.1460(3) 0.0266(10) Uani 1 1 d . . . C26 C 0.5789(3) 0.6983(3) 0.1825(3) 0.0266(11) Uani 1 1 d . . . H26A H 0.5434 0.6546 0.1605 0.032 Uiso 1 1 calc R . . C27 C 0.5358(3) 0.7354(3) 0.2478(3) 0.0261(11) Uani 1 1 d . . . C28 C 0.4614(4) 0.6855(3) 0.2908(4) 0.0403(12) Uani 1 1 d . . . H28A H 0.4357 0.7167 0.3351 0.060 Uiso 1 1 calc R . . H28B H 0.4919 0.6358 0.3102 0.060 Uiso 1 1 calc R . . H28C H 0.4082 0.6716 0.2550 0.060 Uiso 1 1 calc R . . C29 C 0.5093(3) 0.8368(3) 0.3430(3) 0.0289(11) Uani 1 1 d . . . C30 C 0.4171(4) 0.8727(3) 0.3364(3) 0.0363(13) Uani 1 1 d . . . C31 C 0.3759(4) 0.9035(4) 0.4050(3) 0.0464(14) Uani 1 1 d . . . H31A H 0.3129 0.9270 0.4023 0.056 Uiso 1 1 calc R . . C32 C 0.4225(4) 0.9012(4) 0.4760(3) 0.0506(15) Uani 1 1 d . . . H32A H 0.3936 0.9248 0.5211 0.061 Uiso 1 1 calc R . . C33 C 0.5124(4) 0.8639(3) 0.4810(3) 0.0451(14) Uani 1 1 d . . . H33A H 0.5438 0.8603 0.5305 0.054 Uiso 1 1 calc R . . C34 C 0.5579(4) 0.8313(3) 0.4148(3) 0.0307(11) Uani 1 1 d . . . C35 C 0.3627(4) 0.8790(3) 0.2592(3) 0.0441(15) Uani 1 1 d . . . H35A H 0.4009 0.8492 0.2185 0.053 Uiso 1 1 calc R . . C36 C 0.3516(5) 0.9661(4) 0.2321(4) 0.0645(19) Uani 1 1 d . . . H36A H 0.4158 0.9916 0.2288 0.097 Uiso 1 1 calc R . . H36B H 0.3112 0.9959 0.2697 0.097 Uiso 1 1 calc R . . H36C H 0.3207 0.9671 0.1803 0.097 Uiso 1 1 calc R . . C37 C 0.2595(4) 0.8387(4) 0.2646(4) 0.0616(18) Uani 1 1 d . . . H37A H 0.2264 0.8438 0.2139 0.092 Uiso 1 1 calc R . . H37B H 0.2212 0.8659 0.3052 0.092 Uiso 1 1 calc R . . H37C H 0.2666 0.7813 0.2779 0.092 Uiso 1 1 calc R . . C38 C 0.6578(4) 0.7915(3) 0.4221(3) 0.0353(11) Uani 1 1 d . . . H38A H 0.6801 0.7770 0.3680 0.042 Uiso 1 1 calc R . . C39 C 0.7311(5) 0.8490(4) 0.4564(5) 0.068(2) Uani 1 1 d . . . H39A H 0.7943 0.8219 0.4603 0.102 Uiso 1 1 calc R . . H39B H 0.7097 0.8659 0.5087 0.102 Uiso 1 1 calc R . . H39C H 0.7369 0.8966 0.4224 0.102 Uiso 1 1 calc R . . C40 C 0.6546(6) 0.7142(5) 0.4702(7) 0.118(4) Uani 1 1 d . . . H40A H 0.7200 0.6909 0.4732 0.177 Uiso 1 1 calc R . . H40B H 0.6106 0.6754 0.4451 0.177 Uiso 1 1 calc R . . H40C H 0.6312 0.7264 0.5232 0.177 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 0.0236(2) 0.0217(2) 0.0223(2) -0.00016(18) 0.00011(18) 0.00010(16) Cl1 0.0420(6) 0.0241(6) 0.0304(7) -0.0040(6) 0.0060(6) -0.0011(5) N1 0.033(2) 0.026(2) 0.026(2) 0.0017(19) -0.001(2) 0.0013(16) N2 0.023(2) 0.023(2) 0.026(2) 0.0012(17) 0.0008(17) 0.0020(16) N3 0.025(2) 0.025(2) 0.030(2) -0.0050(17) 0.0072(17) -0.0026(15) C1 0.027(3) 0.039(3) 0.040(3) -0.003(3) -0.003(2) -0.010(2) C2 0.051(3) 0.039(3) 0.069(4) 0.008(3) -0.013(3) -0.014(3) C3 0.046(3) 0.074(4) 0.041(4) 0.001(3) -0.014(3) -0.016(3) C4 0.036(3) 0.071(4) 0.068(5) -0.019(4) 0.017(3) -0.017(3) C5 0.024(2) 0.030(3) 0.023(3) -0.003(2) 0.001(2) 0.0065(19) C6 0.027(3) 0.026(3) 0.031(3) 0.002(2) -0.001(2) -0.004(2) C7 0.034(3) 0.027(3) 0.033(3) 0.005(2) -0.001(2) 0.003(2) C8 0.029(3) 0.026(3) 0.036(3) -0.001(2) -0.005(2) 0.007(2) C9 0.032(3) 0.043(3) 0.042(3) -0.007(3) -0.013(2) 0.002(2) C10 0.039(3) 0.028(3) 0.032(3) -0.004(2) -0.001(2) -0.002(2) C11 0.040(3) 0.046(3) 0.045(4) 0.007(3) -0.013(3) 0.000(3) C12 0.022(2) 0.023(2) 0.032(3) -0.001(2) 0.003(2) 0.0021(19) C13 0.027(3) 0.027(2) 0.031(3) -0.007(2) 0.001(2) 0.000(2) C14 0.030(3) 0.044(3) 0.034(3) -0.007(2) 0.007(2) -0.001(2) C15 0.026(3) 0.050(3) 0.054(4) -0.007(3) 0.003(3) 0.008(2) C16 0.028(3) 0.058(4) 0.042(3) 0.002(3) -0.004(2) 0.014(3) C17 0.026(3) 0.037(3) 0.040(4) 0.004(2) 0.000(2) 0.011(2) C18 0.022(3) 0.043(3) 0.029(3) -0.005(2) 0.000(2) 0.002(2) C19 0.051(3) 0.048(3) 0.031(3) 0.008(3) 0.004(3) 0.005(3) C20 0.037(3) 0.068(4) 0.029(3) -0.003(3) 0.003(3) -0.003(3) C21 0.036(3) 0.062(4) 0.038(4) 0.011(3) 0.001(2) 0.019(3) C22 0.074(4) 0.063(4) 0.032(3) 0.005(3) -0.005(3) 0.031(3) C23 0.075(4) 0.076(4) 0.065(5) 0.039(4) -0.012(4) -0.009(4) C24 0.043(3) 0.027(3) 0.043(3) -0.007(2) 0.010(3) -0.001(2) C25 0.030(2) 0.026(2) 0.023(3) 0.0004(19) 0.002(2) 0.008(2) C26 0.027(2) 0.023(2) 0.029(3) 0.0012(19) 0.001(2) -0.0014(19) C27 0.025(3) 0.021(2) 0.032(3) 0.000(2) 0.001(2) -0.0019(19) C28 0.040(3) 0.037(3) 0.044(3) -0.004(3) 0.015(3) -0.008(2) C29 0.030(3) 0.026(2) 0.030(3) -0.004(2) 0.010(2) -0.003(2) C30 0.029(3) 0.039(3) 0.041(3) -0.004(2) 0.006(2) 0.000(2) C31 0.034(3) 0.053(4) 0.052(4) -0.014(3) 0.011(3) 0.003(3) C32 0.048(3) 0.064(4) 0.040(3) -0.017(3) 0.018(3) -0.002(3) C33 0.056(4) 0.045(3) 0.034(3) -0.005(3) 0.006(3) -0.004(3) C34 0.037(3) 0.028(3) 0.027(3) -0.001(2) 0.014(2) -0.007(2) C35 0.034(3) 0.052(4) 0.046(3) -0.016(3) 0.004(2) 0.007(2) C36 0.063(4) 0.064(4) 0.067(5) 0.000(3) -0.017(4) 0.025(3) C37 0.034(3) 0.083(5) 0.068(5) -0.023(4) 0.002(3) -0.004(3) C38 0.046(3) 0.038(3) 0.023(3) 0.005(2) -0.006(3) 0.001(3) C39 0.041(4) 0.065(4) 0.099(6) -0.021(4) -0.013(4) 0.004(3) C40 0.073(5) 0.060(5) 0.221(12) 0.069(6) -0.018(7) -0.006(4) _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 1.759(4) . ? Nb1 N2 2.114(4) . ? Nb1 C5 2.145(5) . ? Nb1 N3 2.332(4) . ? Nb1 Cl1 2.4172(13) . ? N1 C1 1.462(6) . ? N2 C25 1.378(6) . ? N2 C12 1.472(6) . ? N3 C27 1.326(6) . ? N3 C29 1.454(6) . ? C1 C4 1.522(7) . ? C1 C2 1.526(7) . ? C1 C3 1.544(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? 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 C6 1.390(6) . ? C5 C10 1.398(7) . ? C6 C7 1.393(7) . ? C6 H6A 0.9500 . ? C7 C8 1.386(7) . ? C7 H7A 0.9500 . ? C8 C9 1.378(7) . ? C8 C11 1.505(7) . ? C9 C10 1.386(7) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.397(7) . ? C12 C17 1.408(7) . ? C13 C14 1.404(7) . ? C13 C18 1.529(7) . ? C14 C15 1.372(7) . ? C14 H14A 0.9500 . ? C15 C16 1.384(8) . ? C15 H15A 0.9500 . ? C16 C17 1.396(7) . ? C16 H16A 0.9500 . ? C17 C21 1.501(8) . ? C18 C19 1.534(7) . ? C18 C20 1.554(7) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.509(9) . ? C21 C22 1.516(8) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.517(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.363(7) . ? C26 C27 1.402(6) . ? C26 H26A 0.9500 . ? C27 C28 1.504(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.398(7) . ? C29 C30 1.405(7) . ? C30 C31 1.395(7) . ? C30 C35 1.517(8) . ? C31 C32 1.370(8) . ? C31 H31A 0.9500 . ? C32 C33 1.384(8) . ? C32 H32A 0.9500 . ? C33 C34 1.397(7) . ? C33 H33A 0.9500 . ? C34 C38 1.529(7) . ? C35 C36 1.520(9) . ? C35 C37 1.569(7) . ? C35 H35A 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.503(8) . ? C38 C40 1.518(9) . ? C38 H38A 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 Nb1 N2 96.12(15) . . ? N1 Nb1 C5 101.31(19) . . ? N2 Nb1 C5 100.23(16) . . ? N1 Nb1 N3 151.03(17) . . ? N2 Nb1 N3 82.56(13) . . ? C5 Nb1 N3 107.42(16) . . ? N1 Nb1 Cl1 89.71(13) . . ? N2 Nb1 Cl1 159.03(11) . . ? C5 Nb1 Cl1 98.34(13) . . ? N3 Nb1 Cl1 82.64(9) . . ? C1 N1 Nb1 163.0(4) . . ? C25 N2 C12 115.4(4) . . ? C25 N2 Nb1 125.9(3) . . ? C12 N2 Nb1 118.5(3) . . ? C27 N3 C29 116.1(4) . . ? C27 N3 Nb1 123.5(3) . . ? C29 N3 Nb1 120.2(3) . . ? N1 C1 C4 109.3(4) . . ? N1 C1 C2 107.8(4) . . ? C4 C1 C2 111.3(5) . . ? N1 C1 C3 107.8(4) . . ? C4 C1 C3 111.0(5) . . ? C2 C1 C3 109.5(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C10 116.5(4) . . ? C6 C5 Nb1 126.0(4) . . ? C10 C5 Nb1 116.9(3) . . ? C5 C6 C7 121.7(4) . . ? C5 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C8 C7 C6 120.7(4) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C9 C8 C7 118.2(4) . . ? C9 C8 C11 120.9(5) . . ? C7 C8 C11 120.8(4) . . ? C8 C9 C10 121.0(5) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C9 C10 C5 121.8(5) . . ? C9 C10 H10A 119.1 . . ? C5 C10 H10A 119.1 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 121.9(4) . . ? C13 C12 N2 120.9(4) . . ? C17 C12 N2 117.2(4) . . ? C12 C13 C14 117.9(5) . . ? C12 C13 C18 124.3(4) . . ? C14 C13 C18 117.7(4) . . ? C15 C14 C13 121.2(5) . . ? C15 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? C14 C15 C16 120.0(5) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C17 121.4(5) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C16 C17 C12 117.6(5) . . ? C16 C17 C21 120.1(5) . . ? C12 C17 C21 122.4(4) . . ? C13 C18 C19 110.8(4) . . ? C13 C18 C20 112.2(4) . . ? C19 C18 C20 110.6(4) . . ? C13 C18 H18A 107.7 . . ? C19 C18 H18A 107.7 . . ? C20 C18 H18A 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 C23 112.4(5) . . ? C17 C21 C22 113.0(5) . . ? C23 C21 C22 108.5(5) . . ? C17 C21 H21A 107.5 . . ? C23 C21 H21A 107.5 . . ? C22 C21 H21A 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N2 124.1(4) . . ? C26 C25 C24 116.7(4) . . ? N2 C25 C24 119.2(4) . . ? C25 C26 C27 129.4(4) . . ? C25 C26 H26A 115.3 . . ? C27 C26 H26A 115.3 . . ? N3 C27 C26 123.5(4) . . ? N3 C27 C28 120.7(4) . . ? C26 C27 C28 115.8(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 121.9(5) . . ? C34 C29 N3 118.4(4) . . ? C30 C29 N3 119.6(5) . . ? C31 C30 C29 117.0(5) . . ? C31 C30 C35 120.0(5) . . ? C29 C30 C35 122.9(5) . . ? C32 C31 C30 122.6(5) . . ? C32 C31 H31A 118.7 . . ? C30 C31 H31A 118.7 . . ? C31 C32 C33 119.0(5) . . ? C31 C32 H32A 120.5 . . ? C33 C32 H32A 120.5 . . ? C32 C33 C34 121.5(6) . . ? C32 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C33 C34 C29 117.9(5) . . ? C33 C34 C38 120.3(5) . . ? C29 C34 C38 121.9(4) . . ? C30 C35 C36 112.2(5) . . ? C30 C35 C37 111.6(5) . . ? C36 C35 C37 109.2(5) . . ? C30 C35 H35A 107.9 . . ? C36 C35 H35A 107.9 . . ? C37 C35 H35A 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C40 110.0(6) . . ? C39 C38 C34 111.2(4) . . ? C40 C38 C34 112.4(5) . . ? C39 C38 H38A 107.7 . . ? C40 C38 H38A 107.7 . . ? C34 C38 H38A 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 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 -140.9(11) . . . . ? C5 Nb1 N1 C1 117.4(11) . . . . ? N3 Nb1 N1 C1 -55.2(12) . . . . ? Cl1 Nb1 N1 C1 18.9(11) . . . . ? N1 Nb1 N2 C25 -176.2(4) . . . . ? C5 Nb1 N2 C25 -73.5(4) . . . . ? N3 Nb1 N2 C25 33.0(4) . . . . ? Cl1 Nb1 N2 C25 78.4(5) . . . . ? N1 Nb1 N2 C12 -1.9(3) . . . . ? C5 Nb1 N2 C12 100.8(3) . . . . ? N3 Nb1 N2 C12 -152.7(3) . . . . ? Cl1 Nb1 N2 C12 -107.3(4) . . . . ? N1 Nb1 N3 C27 -113.9(4) . . . . ? N2 Nb1 N3 C27 -24.7(4) . . . . ? C5 Nb1 N3 C27 73.7(4) . . . . ? Cl1 Nb1 N3 C27 170.2(4) . . . . ? N1 Nb1 N3 C29 70.5(5) . . . . ? N2 Nb1 N3 C29 159.7(3) . . . . ? C5 Nb1 N3 C29 -101.9(3) . . . . ? Cl1 Nb1 N3 C29 -5.4(3) . . . . ? Nb1 N1 C1 C4 160.3(10) . . . . ? Nb1 N1 C1 C2 -78.6(12) . . . . ? Nb1 N1 C1 C3 39.5(13) . . . . ? N1 Nb1 C5 C6 -33.8(4) . . . . ? N2 Nb1 C5 C6 -132.2(4) . . . . ? N3 Nb1 C5 C6 142.4(4) . . . . ? Cl1 Nb1 C5 C6 57.6(4) . . . . ? N1 Nb1 C5 C10 155.1(3) . . . . ? N2 Nb1 C5 C10 56.6(4) . . . . ? N3 Nb1 C5 C10 -28.7(4) . . . . ? Cl1 Nb1 C5 C10 -113.6(3) . . . . ? C10 C5 C6 C7 -1.1(7) . . . . ? Nb1 C5 C6 C7 -172.3(4) . . . . ? C5 C6 C7 C8 0.6(7) . . . . ? C6 C7 C8 C9 -0.1(7) . . . . ? C6 C7 C8 C11 177.3(5) . . . . ? C7 C8 C9 C10 0.1(8) . . . . ? C11 C8 C9 C10 -177.3(5) . . . . ? C8 C9 C10 C5 -0.6(8) . . . . ? C6 C5 C10 C9 1.1(7) . . . . ? Nb1 C5 C10 C9 173.1(4) . . . . ? C25 N2 C12 C13 87.2(5) . . . . ? Nb1 N2 C12 C13 -87.7(5) . . . . ? C25 N2 C12 C17 -92.9(5) . . . . ? Nb1 N2 C12 C17 92.1(4) . . . . ? C17 C12 C13 C14 0.2(7) . . . . ? N2 C12 C13 C14 -179.9(4) . . . . ? C17 C12 C13 C18 -176.0(4) . . . . ? N2 C12 C13 C18 3.8(7) . . . . ? C12 C13 C14 C15 1.6(7) . . . . ? C18 C13 C14 C15 178.1(5) . . . . ? C13 C14 C15 C16 -1.8(8) . . . . ? C14 C15 C16 C17 0.1(9) . . . . ? C15 C16 C17 C12 1.6(8) . . . . ? C15 C16 C17 C21 -178.4(5) . . . . ? C13 C12 C17 C16 -1.8(7) . . . . ? N2 C12 C17 C16 178.4(5) . . . . ? C13 C12 C17 C21 178.2(5) . . . . ? N2 C12 C17 C21 -1.7(7) . . . . ? C12 C13 C18 C19 104.6(5) . . . . ? C14 C13 C18 C19 -71.7(6) . . . . ? C12 C13 C18 C20 -131.3(5) . . . . ? C14 C13 C18 C20 52.4(6) . . . . ? C16 C17 C21 C23 -92.0(6) . . . . ? C12 C17 C21 C23 88.0(6) . . . . ? C16 C17 C21 C22 31.2(7) . . . . ? C12 C17 C21 C22 -148.7(5) . . . . ? C12 N2 C25 C26 161.3(4) . . . . ? Nb1 N2 C25 C26 -24.2(6) . . . . ? C12 N2 C25 C24 -16.7(6) . . . . ? Nb1 N2 C25 C24 157.8(3) . . . . ? N2 C25 C26 C27 -10.8(8) . . . . ? C24 C25 C26 C27 167.2(5) . . . . ? C29 N3 C27 C26 -178.0(4) . . . . ? Nb1 N3 C27 C26 6.2(6) . . . . ? C29 N3 C27 C28 0.3(6) . . . . ? Nb1 N3 C27 C28 -175.5(3) . . . . ? C25 C26 C27 N3 19.1(8) . . . . ? C25 C26 C27 C28 -159.2(5) . . . . ? C27 N3 C29 C34 99.3(5) . . . . ? Nb1 N3 C29 C34 -84.7(5) . . . . ? C27 N3 C29 C30 -84.5(5) . . . . ? Nb1 N3 C29 C30 91.4(5) . . . . ? C34 C29 C30 C31 0.4(7) . . . . ? N3 C29 C30 C31 -175.6(4) . . . . ? C34 C29 C30 C35 -179.6(5) . . . . ? N3 C29 C30 C35 4.4(7) . . . . ? C29 C30 C31 C32 1.4(8) . . . . ? C35 C30 C31 C32 -178.5(6) . . . . ? C30 C31 C32 C33 -2.8(9) . . . . ? C31 C32 C33 C34 2.4(9) . . . . ? C32 C33 C34 C29 -0.6(8) . . . . ? C32 C33 C34 C38 179.2(5) . . . . ? C30 C29 C34 C33 -0.8(7) . . . . ? N3 C29 C34 C33 175.3(4) . . . . ? C30 C29 C34 C38 179.4(4) . . . . ? N3 C29 C34 C38 -4.6(7) . . . . ? C31 C30 C35 C36 66.5(7) . . . . ? C29 C30 C35 C36 -113.5(6) . . . . ? C31 C30 C35 C37 -56.4(7) . . . . ? C29 C30 C35 C37 123.7(5) . . . . ? C33 C34 C38 C39 -57.1(7) . . . . ? C29 C34 C38 C39 122.8(6) . . . . ? C33 C34 C38 C40 66.7(7) . . . . ? C29 C34 C38 C40 -113.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.261 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.071 #===END data_(BDI)pyNb(NtBu)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H64 N5 Nb' _chemical_formula_sum 'C42 H64 N5 Nb' _chemical_formula_weight 731.89 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 'P b c a' 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 19.6487(12) _cell_length_b 18.8868(12) _cell_length_c 22.3644(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8299.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 457(2) _cell_measurement_reflns_used 4710 _cell_measurement_theta_min 4.674 _cell_measurement_theta_max 42.741 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.887106 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature -120(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 APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33520 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 22.73 _reflns_number_total 5593 _reflns_number_gt 4337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.631' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker-AXS XP v.6' _computing_publication_material 'Bruker-AXS XP v.6' _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^)+(0.0340P)^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 5593 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.382 _refine_ls_restrained_S_all 1.382 _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 0.169581(12) 0.622412(13) 0.387077(11) 0.02031(11) Uani 1 1 d . . . N1 N 0.11461(12) 0.68000(12) 0.42928(11) 0.0281(6) Uani 1 1 d . . . N2 N 0.12356(12) 0.55732(12) 0.34362(11) 0.0270(6) Uani 1 1 d . . . N3 N 0.20266(11) 0.68696(11) 0.31047(10) 0.0212(6) Uani 1 1 d . . . N4 N 0.27916(11) 0.64664(12) 0.42304(10) 0.0228(6) Uani 1 1 d . . . N5 N 0.17895(12) 0.53144(12) 0.45524(11) 0.0255(6) Uani 1 1 d . . . C1 C 0.05645(16) 0.71603(16) 0.45664(15) 0.0345(8) Uani 1 1 d . . . C2 C -0.00939(17) 0.6770(2) 0.44198(19) 0.0636(12) Uani 1 1 d . . . H2A H -0.0155 0.6756 0.3994 0.095 Uiso 1 1 calc R . . H2B H -0.0471 0.7013 0.4600 0.095 Uiso 1 1 calc R . . H2C H -0.0070 0.6296 0.4573 0.095 Uiso 1 1 calc R . . C3 C 0.0540(2) 0.79197(17) 0.43403(18) 0.0611(12) Uani 1 1 d . . . H3A H 0.0483 0.7919 0.3914 0.092 Uiso 1 1 calc R . . H3B H 0.0956 0.8157 0.4442 0.092 Uiso 1 1 calc R . . H3C H 0.0164 0.8162 0.4523 0.092 Uiso 1 1 calc R . . C4 C 0.06541(19) 0.7178(2) 0.52452(16) 0.0545(11) Uani 1 1 d . . . H4A H 0.1068 0.7423 0.5343 0.082 Uiso 1 1 calc R . . H4B H 0.0676 0.6703 0.5396 0.082 Uiso 1 1 calc R . . H4C H 0.0275 0.7420 0.5423 0.082 Uiso 1 1 calc R . . C5 C 0.07827(15) 0.50243(15) 0.32173(15) 0.0307(8) Uani 1 1 d . . . C6 C 0.10735(19) 0.42991(16) 0.3364(2) 0.0653(13) Uani 1 1 d . . . H6A H 0.1121 0.4252 0.3790 0.098 Uiso 1 1 calc R . . H6B H 0.1511 0.4248 0.3178 0.098 Uiso 1 1 calc R . . H6C H 0.0772 0.3939 0.3217 0.098 Uiso 1 1 calc R . . C7 C 0.00898(19) 0.5093(2) 0.3511(2) 0.0765(15) Uani 1 1 d . . . H7A H -0.0099 0.5550 0.3421 0.115 Uiso 1 1 calc R . . H7B H 0.0137 0.5043 0.3936 0.115 Uiso 1 1 calc R . . H7C H -0.0207 0.4731 0.3361 0.115 Uiso 1 1 calc R . . C8 C 0.0710(2) 0.5094(2) 0.25439(17) 0.0709(14) Uani 1 1 d . . . H8A H 0.0526 0.5552 0.2449 0.106 Uiso 1 1 calc R . . H8B H 0.0409 0.4733 0.2398 0.106 Uiso 1 1 calc R . . H8C H 0.1148 0.5042 0.2359 0.106 Uiso 1 1 calc R . . C9 C 0.17772(15) 0.67105(15) 0.25055(13) 0.0257(7) Uani 1 1 d . . . C10 C 0.21520(16) 0.62351(16) 0.21493(14) 0.0318(8) Uani 1 1 d . . . C11 C 0.19178(18) 0.60919(17) 0.15744(15) 0.0402(9) Uani 1 1 d . . . H11A H 0.2158 0.5776 0.1335 0.048 Uiso 1 1 calc R . . C12 C 0.13407(19) 0.64064(17) 0.13516(15) 0.0414(9) Uani 1 1 d . . . H12A H 0.1196 0.6310 0.0964 0.050 Uiso 1 1 calc R . . C13 C 0.09823(17) 0.68634(16) 0.17060(15) 0.0380(9) Uani 1 1 d . . . H13A H 0.0591 0.7073 0.1553 0.046 Uiso 1 1 calc R . . C14 C 0.11828(16) 0.70273(15) 0.22881(14) 0.0297(8) Uani 1 1 d . . . C15 C 0.28071(17) 0.59001(18) 0.23716(16) 0.0446(9) Uani 1 1 d . . . H15A H 0.2838 0.5989 0.2802 0.054 Uiso 1 1 calc R . . C16 C 0.2816(2) 0.5109(2) 0.2281(3) 0.0984(19) Uani 1 1 d . . . H16A H 0.3237 0.4920 0.2427 0.148 Uiso 1 1 calc R . . H16B H 0.2772 0.5005 0.1863 0.148 Uiso 1 1 calc R . . H16C H 0.2444 0.4899 0.2495 0.148 Uiso 1 1 calc R . . C17 C 0.3421(2) 0.6232(3) 0.2082(3) 0.108(2) Uani 1 1 d . . . H17A H 0.3826 0.6010 0.2231 0.162 Uiso 1 1 calc R . . H17B H 0.3432 0.6729 0.2174 0.162 Uiso 1 1 calc R . . H17C H 0.3396 0.6170 0.1657 0.162 Uiso 1 1 calc R . . C18 C 0.07464(16) 0.75207(16) 0.26536(15) 0.0374(9) Uani 1 1 d . . . H18A H 0.0960 0.7576 0.3047 0.045 Uiso 1 1 calc R . . C19 C 0.0679(2) 0.82599(18) 0.2372(2) 0.0709(13) Uani 1 1 d . . . H19A H 0.1124 0.8457 0.2310 0.106 Uiso 1 1 calc R . . H19B H 0.0424 0.8562 0.2634 0.106 Uiso 1 1 calc R . . H19C H 0.0448 0.8222 0.1995 0.106 Uiso 1 1 calc R . . C20 C 0.00405(18) 0.72202(19) 0.27467(19) 0.0594(11) Uani 1 1 d . . . H20A H 0.0075 0.6758 0.2923 0.089 Uiso 1 1 calc R . . H20B H -0.0188 0.7186 0.2369 0.089 Uiso 1 1 calc R . . H20C H -0.0213 0.7526 0.3008 0.089 Uiso 1 1 calc R . . C21 C 0.2517(2) 0.79461(18) 0.26467(16) 0.0530(11) Uani 1 1 d . . . H21A H 0.2217 0.7816 0.2326 0.080 Uiso 1 1 calc R . . H21B H 0.2978 0.7942 0.2506 0.080 Uiso 1 1 calc R . . H21C H 0.2403 0.8412 0.2785 0.080 Uiso 1 1 calc R . . C22 C 0.24403(15) 0.74240(15) 0.31539(14) 0.0276(8) Uani 1 1 d . . . C23 C 0.28505(15) 0.75531(15) 0.36516(13) 0.0287(8) Uani 1 1 d . . . H23A H 0.3001 0.8018 0.3690 0.034 Uiso 1 1 calc R . . C24 C 0.30704(15) 0.70929(15) 0.41022(14) 0.0262(7) Uani 1 1 d . . . C25 C 0.37139(16) 0.73452(16) 0.44182(16) 0.0406(9) Uani 1 1 d . . . H25A H 0.3839 0.7009 0.4721 0.061 Uiso 1 1 calc R . . H25B H 0.3631 0.7798 0.4600 0.061 Uiso 1 1 calc R . . H25C H 0.4077 0.7387 0.4133 0.061 Uiso 1 1 calc R . . C26 C 0.31576(14) 0.60447(15) 0.46663(14) 0.0262(8) Uani 1 1 d . . . C27 C 0.36582(16) 0.55675(16) 0.44705(15) 0.0338(8) Uani 1 1 d . . . C28 C 0.40273(17) 0.51915(18) 0.48978(19) 0.0467(10) Uani 1 1 d . . . H28A H 0.4363 0.4878 0.4774 0.056 Uiso 1 1 calc R . . C29 C 0.39051(19) 0.52746(19) 0.54977(19) 0.0520(11) Uani 1 1 d . . . H29A H 0.4163 0.5028 0.5777 0.062 Uiso 1 1 calc R . . C30 C 0.33975(18) 0.57251(17) 0.56820(16) 0.0452(10) Uani 1 1 d . . . H30A H 0.3312 0.5772 0.6089 0.054 Uiso 1 1 calc R . . C31 C 0.30076(17) 0.61134(15) 0.52800(15) 0.0335(8) Uani 1 1 d . . . C32 C 0.38052(18) 0.54529(19) 0.38088(17) 0.0479(10) Uani 1 1 d . . . H32A H 0.3401 0.5600 0.3584 0.057 Uiso 1 1 calc R . . C33 C 0.3947(2) 0.4676(2) 0.3655(2) 0.0719(13) Uani 1 1 d . . . H33A H 0.4036 0.4634 0.3234 0.108 Uiso 1 1 calc R . . H33B H 0.3558 0.4394 0.3757 0.108 Uiso 1 1 calc R . . H33C H 0.4335 0.4514 0.3876 0.108 Uiso 1 1 calc R . . C34 C 0.4400(2) 0.5898(2) 0.3593(2) 0.0928(17) Uani 1 1 d . . . H34A H 0.4317 0.6387 0.3687 0.139 Uiso 1 1 calc R . . H34B H 0.4448 0.5846 0.3168 0.139 Uiso 1 1 calc R . . H34C H 0.4809 0.5745 0.3788 0.139 Uiso 1 1 calc R . . C35 C 0.24520(19) 0.65945(18) 0.55100(16) 0.0442(10) Uani 1 1 d . . . H35A H 0.2105 0.6623 0.5196 0.053 Uiso 1 1 calc R . . C36 C 0.2102(2) 0.63230(19) 0.60683(14) 0.0545(11) Uani 1 1 d . . . H36A H 0.1757 0.6653 0.6189 0.082 Uiso 1 1 calc R . . H36B H 0.2431 0.6272 0.6383 0.082 Uiso 1 1 calc R . . H36C H 0.1898 0.5872 0.5986 0.082 Uiso 1 1 calc R . . C37 C 0.2691(2) 0.73380(19) 0.5630(2) 0.0799(15) Uani 1 1 d . . . H37A H 0.2915 0.7521 0.5281 0.120 Uiso 1 1 calc R . . H37B H 0.3004 0.7336 0.5960 0.120 Uiso 1 1 calc R . . H37C H 0.2307 0.7632 0.5726 0.120 Uiso 1 1 calc R . . C38 C 0.22190(16) 0.47800(15) 0.44510(15) 0.0326(8) Uani 1 1 d . . . H38A H 0.2513 0.4814 0.4126 0.039 Uiso 1 1 calc R . . C39 C 0.22496(18) 0.41820(17) 0.48014(16) 0.0419(9) Uani 1 1 d . . . H39A H 0.2559 0.3823 0.4717 0.050 Uiso 1 1 calc R . . C40 C 0.18136(19) 0.41274(18) 0.52787(17) 0.0476(10) Uani 1 1 d . . . H40A H 0.1826 0.3733 0.5527 0.057 Uiso 1 1 calc R . . C41 C 0.1360(2) 0.46635(18) 0.53836(16) 0.0474(10) Uani 1 1 d . . . H41A H 0.1054 0.4632 0.5700 0.057 Uiso 1 1 calc R . . C42 C 0.13609(16) 0.52505(16) 0.50160(15) 0.0341(8) Uani 1 1 d . . . H42A H 0.1054 0.5614 0.5092 0.041 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 0.01957(17) 0.01858(16) 0.02279(17) -0.00022(13) 0.00031(12) -0.00046(11) N1 0.0263(15) 0.0271(14) 0.0310(16) -0.0016(13) 0.0036(12) 0.0033(11) N2 0.0300(15) 0.0226(13) 0.0285(15) 0.0038(13) -0.0043(13) -0.0060(11) N3 0.0216(13) 0.0215(13) 0.0205(14) -0.0016(12) -0.0014(11) -0.0015(11) N4 0.0242(14) 0.0203(13) 0.0239(14) 0.0020(12) -0.0034(12) -0.0020(11) N5 0.0259(15) 0.0226(13) 0.0280(15) 0.0024(12) 0.0001(12) -0.0039(12) C1 0.0314(19) 0.0349(18) 0.037(2) -0.0067(17) 0.0047(17) 0.0060(15) C2 0.030(2) 0.082(3) 0.079(3) -0.035(3) 0.010(2) 0.002(2) C3 0.077(3) 0.044(2) 0.063(3) -0.010(2) 0.011(2) 0.028(2) C4 0.052(2) 0.064(3) 0.047(2) -0.018(2) 0.009(2) 0.013(2) C5 0.0275(19) 0.0227(17) 0.042(2) -0.0027(16) -0.0082(16) -0.0055(14) C6 0.062(3) 0.030(2) 0.104(4) -0.012(2) -0.030(3) -0.0042(18) C7 0.040(3) 0.063(3) 0.127(4) -0.037(3) 0.005(3) -0.017(2) C8 0.092(4) 0.062(3) 0.058(3) -0.001(2) -0.032(3) -0.035(2) C9 0.0309(19) 0.0240(16) 0.0223(17) 0.0009(15) -0.0014(15) -0.0119(14) C10 0.039(2) 0.0315(18) 0.0248(18) -0.0017(16) 0.0042(16) -0.0083(16) C11 0.053(2) 0.040(2) 0.028(2) -0.0089(18) 0.0069(18) -0.0077(17) C12 0.059(3) 0.041(2) 0.0243(19) -0.0020(17) -0.0108(19) -0.0142(19) C13 0.046(2) 0.0340(19) 0.034(2) 0.0049(18) -0.0139(18) -0.0096(16) C14 0.037(2) 0.0262(17) 0.0260(19) 0.0010(16) -0.0062(16) -0.0075(15) C15 0.042(2) 0.057(2) 0.035(2) -0.0160(19) 0.0003(18) 0.0080(18) C16 0.078(4) 0.058(3) 0.159(6) -0.020(3) -0.032(4) 0.031(3) C17 0.040(3) 0.141(5) 0.141(5) 0.018(4) -0.004(3) -0.006(3) C18 0.040(2) 0.0382(19) 0.034(2) -0.0009(17) -0.0130(17) 0.0030(16) C19 0.086(3) 0.037(2) 0.090(4) -0.002(2) -0.001(3) 0.010(2) C20 0.046(2) 0.059(2) 0.073(3) -0.012(2) 0.003(2) 0.003(2) C21 0.066(3) 0.050(2) 0.043(2) 0.018(2) -0.016(2) -0.0286(19) C22 0.0324(19) 0.0218(17) 0.028(2) 0.0069(16) 0.0018(15) -0.0015(14) C23 0.037(2) 0.0191(16) 0.0299(19) 0.0021(15) -0.0086(16) -0.0110(14) C24 0.0238(17) 0.0277(17) 0.0271(18) -0.0042(15) -0.0007(14) -0.0030(14) C25 0.036(2) 0.0373(19) 0.048(2) 0.0077(18) -0.0154(18) -0.0148(16) C26 0.0237(18) 0.0216(16) 0.033(2) 0.0042(15) -0.0062(15) -0.0048(13) C27 0.0253(18) 0.0333(18) 0.043(2) 0.0057(18) -0.0032(17) -0.0014(15) C28 0.033(2) 0.039(2) 0.068(3) 0.014(2) -0.009(2) 0.0075(17) C29 0.052(3) 0.046(2) 0.058(3) 0.015(2) -0.022(2) 0.008(2) C30 0.059(3) 0.042(2) 0.035(2) 0.0112(19) -0.0130(19) -0.0013(19) C31 0.039(2) 0.0272(18) 0.034(2) 0.0041(16) -0.0059(17) -0.0031(15) C32 0.037(2) 0.057(2) 0.050(3) 0.008(2) 0.0054(19) 0.0244(18) C33 0.070(3) 0.069(3) 0.077(3) -0.015(3) 0.013(3) 0.017(2) C34 0.108(4) 0.069(3) 0.102(4) 0.017(3) 0.069(3) 0.008(3) C35 0.062(3) 0.040(2) 0.030(2) 0.0030(18) 0.0005(18) 0.0098(18) C36 0.072(3) 0.063(3) 0.028(2) -0.001(2) 0.002(2) 0.000(2) C37 0.109(4) 0.042(2) 0.088(4) -0.011(2) 0.033(3) -0.001(2) C38 0.032(2) 0.0291(18) 0.037(2) 0.0022(17) -0.0021(16) -0.0030(15) C39 0.046(2) 0.028(2) 0.052(2) 0.0037(19) -0.007(2) 0.0024(16) C40 0.068(3) 0.032(2) 0.042(2) 0.0134(19) -0.006(2) -0.0038(19) C41 0.062(3) 0.043(2) 0.037(2) 0.0087(19) 0.0125(19) -0.013(2) C42 0.036(2) 0.0315(19) 0.035(2) 0.0001(17) 0.0065(18) -0.0036(16) _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 1.800(2) . ? Nb1 N2 1.809(2) . ? Nb1 N3 2.201(2) . ? Nb1 N5 2.304(2) . ? Nb1 N4 2.344(2) . ? N1 C1 1.464(4) . ? N2 C5 1.451(3) . ? N3 C22 1.330(3) . ? N3 C9 1.458(4) . ? N4 C24 1.335(4) . ? N4 C26 1.450(4) . ? N5 C38 1.335(4) . ? N5 C42 1.341(4) . ? C1 C3 1.522(4) . ? C1 C2 1.524(5) . ? C1 C4 1.529(5) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C7 1.517(5) . ? C5 C8 1.519(5) . ? C5 C6 1.520(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C14 1.399(4) . ? C9 C10 1.408(4) . ? C10 C11 1.392(4) . ? C10 C15 1.518(5) . ? C11 C12 1.374(5) . ? C11 H11A 0.9300 . ? C12 C13 1.367(5) . ? C12 H12A 0.9300 . ? C13 C14 1.395(4) . ? C13 H13A 0.9300 . ? C14 C18 1.507(4) . ? C15 C17 1.506(5) . ? C15 C16 1.508(5) . ? C15 H15A 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.513(5) . ? C18 C19 1.537(5) . ? C18 H18A 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.510(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.396(4) . ? C23 C24 1.399(4) . ? C23 H23A 0.9300 . ? C24 C25 1.525(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.404(4) . ? C26 C31 1.410(4) . ? C27 C28 1.394(4) . ? C27 C32 1.523(5) . ? C28 C29 1.372(5) . ? C28 H28A 0.9300 . ? C29 C30 1.374(5) . ? C29 H29A 0.9300 . ? C30 C31 1.390(4) . ? C30 H30A 0.9300 . ? C31 C35 1.511(5) . ? C32 C34 1.518(5) . ? C32 C33 1.532(5) . ? C32 H32A 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C37 1.505(5) . ? C35 C36 1.515(5) . ? C35 H35A 0.9800 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.376(4) . ? C38 H38A 0.9300 . ? C39 C40 1.373(5) . ? C39 H39A 0.9300 . ? C40 C41 1.369(5) . ? C40 H40A 0.9300 . ? C41 C42 1.380(4) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Nb1 N2 113.10(11) . . ? N1 Nb1 N3 104.52(10) . . ? N2 Nb1 N3 96.08(10) . . ? N1 Nb1 N5 98.71(10) . . ? N2 Nb1 N5 83.60(9) . . ? N3 Nb1 N5 154.75(9) . . ? N1 Nb1 N4 104.67(9) . . ? N2 Nb1 N4 140.91(9) . . ? N3 Nb1 N4 83.55(8) . . ? N5 Nb1 N4 81.09(8) . . ? C1 N1 Nb1 165.5(2) . . ? C5 N2 Nb1 166.7(2) . . ? C22 N3 C9 116.3(2) . . ? C22 N3 Nb1 123.5(2) . . ? C9 N3 Nb1 120.14(17) . . ? C24 N4 C26 115.3(2) . . ? C24 N4 Nb1 118.44(19) . . ? C26 N4 Nb1 125.40(17) . . ? C38 N5 C42 117.4(3) . . ? C38 N5 Nb1 120.1(2) . . ? C42 N5 Nb1 121.9(2) . . ? N1 C1 C3 108.9(3) . . ? N1 C1 C2 110.4(3) . . ? C3 C1 C2 110.9(3) . . ? N1 C1 C4 109.6(3) . . ? C3 C1 C4 108.2(3) . . ? C2 C1 C4 108.8(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C7 110.1(3) . . ? N2 C5 C8 109.3(3) . . ? C7 C5 C8 109.7(3) . . ? N2 C5 C6 109.9(2) . . ? C7 C5 C6 108.8(3) . . ? C8 C5 C6 109.2(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 120.8(3) . . ? C14 C9 N3 120.8(3) . . ? C10 C9 N3 118.4(3) . . ? C11 C10 C9 118.3(3) . . ? C11 C10 C15 120.1(3) . . ? C9 C10 C15 121.6(3) . . ? C12 C11 C10 121.6(3) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C13 C12 C11 119.2(3) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C12 C13 C14 122.4(3) . . ? C12 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? C13 C14 C9 117.7(3) . . ? C13 C14 C18 118.9(3) . . ? C9 C14 C18 123.4(3) . . ? C17 C15 C16 110.3(4) . . ? C17 C15 C10 111.4(3) . . ? C16 C15 C10 112.2(3) . . ? C17 C15 H15A 107.6 . . ? C16 C15 H15A 107.6 . . ? C10 C15 H15A 107.6 . . ? 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 . . ? C14 C18 C20 111.4(3) . . ? C14 C18 C19 112.8(3) . . ? C20 C18 C19 108.6(3) . . ? C14 C18 H18A 108.0 . . ? C20 C18 H18A 108.0 . . ? C19 C18 H18A 108.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C23 123.8(3) . . ? N3 C22 C21 120.8(3) . . ? C23 C22 C21 115.3(3) . . ? C22 C23 C24 130.1(3) . . ? C22 C23 H23A 114.9 . . ? C24 C23 H23A 114.9 . . ? N4 C24 C23 125.4(3) . . ? N4 C24 C25 121.2(3) . . ? C23 C24 C25 113.3(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 120.6(3) . . ? C27 C26 N4 119.4(3) . . ? C31 C26 N4 120.0(3) . . ? C28 C27 C26 118.5(3) . . ? C28 C27 C32 119.7(3) . . ? C26 C27 C32 121.8(3) . . ? C29 C28 C27 121.4(3) . . ? C29 C28 H28A 119.3 . . ? C27 C28 H28A 119.3 . . ? C28 C29 C30 119.4(3) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? C29 C30 C31 122.2(4) . . ? C29 C30 H30A 118.9 . . ? C31 C30 H30A 118.9 . . ? C30 C31 C26 117.8(3) . . ? C30 C31 C35 119.7(3) . . ? C26 C31 C35 122.5(3) . . ? C34 C32 C27 112.1(3) . . ? C34 C32 C33 108.6(3) . . ? C27 C32 C33 112.9(3) . . ? C34 C32 H32A 107.7 . . ? C27 C32 H32A 107.7 . . ? C33 C32 H32A 107.7 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C31 113.4(3) . . ? C37 C35 C36 108.1(3) . . ? C31 C35 C36 113.9(3) . . ? C37 C35 H35A 107.0 . . ? C31 C35 H35A 107.0 . . ? C36 C35 H35A 107.0 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C38 C39 123.5(3) . . ? N5 C38 H38A 118.3 . . ? C39 C38 H38A 118.3 . . ? C40 C39 C38 118.5(3) . . ? C40 C39 H39A 120.7 . . ? C38 C39 H39A 120.7 . . ? C41 C40 C39 118.9(3) . . ? C41 C40 H40A 120.5 . . ? C39 C40 H40A 120.5 . . ? C40 C41 C42 119.4(3) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? N5 C42 C41 122.2(3) . . ? N5 C42 H42A 118.9 . . ? C41 C42 H42A 118.9 . . ? 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 0.0(9) . . . . ? N3 Nb1 N1 C1 103.3(9) . . . . ? N5 Nb1 N1 C1 -86.7(9) . . . . ? N4 Nb1 N1 C1 -169.7(8) . . . . ? N1 Nb1 N2 C5 -48.3(9) . . . . ? N3 Nb1 N2 C5 -156.9(9) . . . . ? N5 Nb1 N2 C5 48.5(9) . . . . ? N4 Nb1 N2 C5 115.8(8) . . . . ? N1 Nb1 N3 C22 68.9(2) . . . . ? N2 Nb1 N3 C22 -175.3(2) . . . . ? N5 Nb1 N3 C22 -87.4(3) . . . . ? N4 Nb1 N3 C22 -34.6(2) . . . . ? N1 Nb1 N3 C9 -109.5(2) . . . . ? N2 Nb1 N3 C9 6.3(2) . . . . ? N5 Nb1 N3 C9 94.2(3) . . . . ? N4 Nb1 N3 C9 147.0(2) . . . . ? N1 Nb1 N4 C24 -69.5(2) . . . . ? N2 Nb1 N4 C24 125.5(2) . . . . ? N3 Nb1 N4 C24 33.8(2) . . . . ? N5 Nb1 N4 C24 -166.3(2) . . . . ? N1 Nb1 N4 C26 99.5(2) . . . . ? N2 Nb1 N4 C26 -65.4(3) . . . . ? N3 Nb1 N4 C26 -157.1(2) . . . . ? N5 Nb1 N4 C26 2.8(2) . . . . ? N1 Nb1 N5 C38 -173.3(2) . . . . ? N2 Nb1 N5 C38 74.3(2) . . . . ? N3 Nb1 N5 C38 -16.4(3) . . . . ? N4 Nb1 N5 C38 -69.6(2) . . . . ? N1 Nb1 N5 C42 15.7(2) . . . . ? N2 Nb1 N5 C42 -96.8(2) . . . . ? N3 Nb1 N5 C42 172.6(2) . . . . ? N4 Nb1 N5 C42 119.3(2) . . . . ? Nb1 N1 C1 C3 -115.2(8) . . . . ? Nb1 N1 C1 C2 6.8(10) . . . . ? Nb1 N1 C1 C4 126.6(8) . . . . ? Nb1 N2 C5 C7 35.8(10) . . . . ? Nb1 N2 C5 C8 156.3(8) . . . . ? Nb1 N2 C5 C6 -84.0(9) . . . . ? C22 N3 C9 C14 -88.2(3) . . . . ? Nb1 N3 C9 C14 90.3(3) . . . . ? C22 N3 C9 C10 91.3(3) . . . . ? Nb1 N3 C9 C10 -90.2(3) . . . . ? C14 C9 C10 C11 0.4(4) . . . . ? N3 C9 C10 C11 -179.1(3) . . . . ? C14 C9 C10 C15 178.5(3) . . . . ? N3 C9 C10 C15 -1.0(4) . . . . ? C9 C10 C11 C12 0.6(5) . . . . ? C15 C10 C11 C12 -177.6(3) . . . . ? C10 C11 C12 C13 -0.9(5) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C12 C13 C14 C9 0.6(5) . . . . ? C12 C13 C14 C18 -178.3(3) . . . . ? C10 C9 C14 C13 -0.9(4) . . . . ? N3 C9 C14 C13 178.6(3) . . . . ? C10 C9 C14 C18 177.9(3) . . . . ? N3 C9 C14 C18 -2.7(4) . . . . ? C11 C10 C15 C17 73.1(4) . . . . ? C9 C10 C15 C17 -105.0(4) . . . . ? C11 C10 C15 C16 -51.1(5) . . . . ? C9 C10 C15 C16 130.8(4) . . . . ? C13 C14 C18 C20 61.5(4) . . . . ? C9 C14 C18 C20 -117.3(3) . . . . ? C13 C14 C18 C19 -60.9(4) . . . . ? C9 C14 C18 C19 120.3(3) . . . . ? C9 N3 C22 C23 -164.1(3) . . . . ? Nb1 N3 C22 C23 17.5(4) . . . . ? C9 N3 C22 C21 13.1(4) . . . . ? Nb1 N3 C22 C21 -165.3(2) . . . . ? N3 C22 C23 C24 19.5(5) . . . . ? C21 C22 C23 C24 -157.8(3) . . . . ? C26 N4 C24 C23 172.7(3) . . . . ? Nb1 N4 C24 C23 -17.2(4) . . . . ? C26 N4 C24 C25 -2.3(4) . . . . ? Nb1 N4 C24 C25 167.8(2) . . . . ? C22 C23 C24 N4 -18.1(5) . . . . ? C22 C23 C24 C25 157.3(3) . . . . ? C24 N4 C26 C27 -90.3(3) . . . . ? Nb1 N4 C26 C27 100.3(3) . . . . ? C24 N4 C26 C31 90.0(3) . . . . ? Nb1 N4 C26 C31 -79.4(3) . . . . ? C31 C26 C27 C28 -3.3(4) . . . . ? N4 C26 C27 C28 177.0(3) . . . . ? C31 C26 C27 C32 176.7(3) . . . . ? N4 C26 C27 C32 -3.0(4) . . . . ? C26 C27 C28 C29 0.7(5) . . . . ? C32 C27 C28 C29 -179.3(3) . . . . ? C27 C28 C29 C30 1.6(6) . . . . ? C28 C29 C30 C31 -1.2(5) . . . . ? C29 C30 C31 C26 -1.4(5) . . . . ? C29 C30 C31 C35 179.4(3) . . . . ? C27 C26 C31 C30 3.6(4) . . . . ? N4 C26 C31 C30 -176.7(3) . . . . ? C27 C26 C31 C35 -177.1(3) . . . . ? N4 C26 C31 C35 2.6(4) . . . . ? C28 C27 C32 C34 -83.9(4) . . . . ? C26 C27 C32 C34 96.1(4) . . . . ? C28 C27 C32 C33 39.2(4) . . . . ? C26 C27 C32 C33 -140.8(3) . . . . ? C30 C31 C35 C37 90.6(4) . . . . ? C26 C31 C35 C37 -88.6(4) . . . . ? C30 C31 C35 C36 -33.5(5) . . . . ? C26 C31 C35 C36 147.3(3) . . . . ? C42 N5 C38 C39 -1.2(4) . . . . ? Nb1 N5 C38 C39 -172.6(2) . . . . ? N5 C38 C39 C40 0.4(5) . . . . ? C38 C39 C40 C41 0.9(5) . . . . ? C39 C40 C41 C42 -1.3(5) . . . . ? C38 N5 C42 C41 0.7(5) . . . . ? Nb1 N5 C42 C41 171.9(2) . . . . ? C40 C41 C42 N5 0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.417 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.055 #===END data_(BDI)(dmap)Nb(NtBu)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H69 N6 Nb' _chemical_formula_sum 'C44 H69 N6 Nb' _chemical_formula_weight 774.96 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 'P 2(1)/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 15.530(3) _cell_length_b 12.284(2) _cell_length_c 23.724(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.887(3) _cell_angle_gamma 90.00 _cell_volume 4307.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 3108 _cell_measurement_theta_min 6.875 _cell_measurement_theta_max 44.343 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.315 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.921823 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17130 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 23.54 _reflns_number_total 6328 _reflns_number_gt 4105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v 7.07' _computing_data_reduction 'Bruker SAINT v 7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker-AXS XP v.6' _computing_publication_material 'Bruker-AXS XP v.6' _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^)+(0.0500P)^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 6328 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.003 _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 0.88893(2) 0.75341(3) 0.118367(14) 0.02103(11) Uani 1 1 d . . . N1 N 0.87398(19) 0.6107(2) 0.12924(13) 0.0285(8) Uani 1 1 d . . . N2 N 0.8754(2) 0.7870(2) 0.04248(13) 0.0299(8) Uani 1 1 d . . . N3 N 0.76000(19) 0.8271(2) 0.12059(13) 0.0239(7) Uani 1 1 d . . . N4 N 0.94192(19) 0.8278(2) 0.21355(12) 0.0223(7) Uani 1 1 d . . . N5 N 1.04047(17) 0.7457(3) 0.12641(12) 0.0234(6) Uani 1 1 d . . . N6 N 1.3035(2) 0.7326(3) 0.11292(15) 0.0408(9) Uani 1 1 d . . . C1 C 0.8575(3) 0.4945(3) 0.12177(18) 0.0359(10) Uani 1 1 d . . . C2 C 0.7705(3) 0.4675(3) 0.1356(2) 0.0642(15) Uani 1 1 d . . . H2A H 0.7760 0.4904 0.1762 0.096 Uiso 1 1 calc R . . H2B H 0.7597 0.3888 0.1319 0.096 Uiso 1 1 calc R . . H2C H 0.7197 0.5059 0.1078 0.096 Uiso 1 1 calc R . . C3 C 0.9356(3) 0.4330(3) 0.1653(2) 0.0511(13) Uani 1 1 d . . . H3A H 0.9407 0.4553 0.2059 0.077 Uiso 1 1 calc R . . H3B H 0.9921 0.4497 0.1570 0.077 Uiso 1 1 calc R . . H3C H 0.9239 0.3545 0.1611 0.077 Uiso 1 1 calc R . . C4 C 0.8499(3) 0.4592(3) 0.05886(19) 0.0559(13) Uani 1 1 d . . . H4A H 0.8000 0.4985 0.0308 0.084 Uiso 1 1 calc R . . H4B H 0.8382 0.3808 0.0548 0.084 Uiso 1 1 calc R . . H4C H 0.9065 0.4757 0.0506 0.084 Uiso 1 1 calc R . . C5 C 0.8816(3) 0.7962(3) -0.01720(17) 0.0310(10) Uani 1 1 d . . . C6 C 0.8744(3) 0.6858(3) -0.04650(19) 0.0518(13) Uani 1 1 d . . . H6A H 0.9232 0.6387 -0.0230 0.078 Uiso 1 1 calc R . . H6B H 0.8795 0.6942 -0.0864 0.078 Uiso 1 1 calc R . . H6C H 0.8158 0.6529 -0.0490 0.078 Uiso 1 1 calc R . . C7 C 0.8065(3) 0.8701(4) -0.05322(18) 0.0501(12) Uani 1 1 d . . . H7A H 0.7477 0.8386 -0.0551 0.075 Uiso 1 1 calc R . . H7B H 0.8108 0.8776 -0.0934 0.075 Uiso 1 1 calc R . . H7C H 0.8125 0.9419 -0.0344 0.075 Uiso 1 1 calc R . . C8 C 0.9736(3) 0.8440(4) -0.01390(19) 0.0542(13) Uani 1 1 d . . . H8A H 1.0215 0.7956 0.0094 0.081 Uiso 1 1 calc R . . H8B H 0.9801 0.9157 0.0050 0.081 Uiso 1 1 calc R . . H8C H 0.9782 0.8514 -0.0540 0.081 Uiso 1 1 calc R . . C9 C 0.6973(2) 0.8708(3) 0.06689(16) 0.0233(8) Uani 1 1 d . . . C10 C 0.6972(2) 0.9834(3) 0.05694(16) 0.0270(9) Uani 1 1 d . . . C11 C 0.6346(2) 1.0260(3) 0.00676(17) 0.0337(10) Uani 1 1 d . . . H11A H 0.6336 1.1023 -0.0002 0.040 Uiso 1 1 calc R . . C12 C 0.5742(3) 0.9605(3) -0.03295(18) 0.0377(11) Uani 1 1 d . . . H12A H 0.5312 0.9912 -0.0668 0.045 Uiso 1 1 calc R . . C13 C 0.5762(2) 0.8505(3) -0.02365(17) 0.0326(10) Uani 1 1 d . . . H13A H 0.5352 0.8051 -0.0518 0.039 Uiso 1 1 calc R . . C14 C 0.6368(2) 0.8041(3) 0.02599(17) 0.0275(9) Uani 1 1 d . . . C15 C 0.7622(3) 1.0596(3) 0.09931(17) 0.0328(10) Uani 1 1 d . . . H15A H 0.8003 1.0157 0.1333 0.039 Uiso 1 1 calc R . . C16 C 0.8242(3) 1.1142(4) 0.0695(2) 0.0558(13) Uani 1 1 d . . . H16A H 0.8559 1.0585 0.0539 0.084 Uiso 1 1 calc R . . H16B H 0.8685 1.1593 0.0984 0.084 Uiso 1 1 calc R . . H16C H 0.7883 1.1601 0.0369 0.084 Uiso 1 1 calc R . . C17 C 0.7123(3) 1.1464(4) 0.1239(2) 0.0632(14) Uani 1 1 d . . . H17A H 0.6722 1.1108 0.1431 0.095 Uiso 1 1 calc R . . H17B H 0.6763 1.1923 0.0914 0.095 Uiso 1 1 calc R . . H17C H 0.7564 1.1915 0.1529 0.095 Uiso 1 1 calc R . . C18 C 0.6358(3) 0.6812(3) 0.03379(17) 0.0326(10) Uani 1 1 d . . . H18A H 0.6955 0.6599 0.0622 0.039 Uiso 1 1 calc R . . C19 C 0.6240(3) 0.6184(3) -0.02279(19) 0.0559(13) Uani 1 1 d . . . H19A H 0.6706 0.6406 -0.0404 0.084 Uiso 1 1 calc R . . H19B H 0.5640 0.6335 -0.0507 0.084 Uiso 1 1 calc R . . H19C H 0.6297 0.5403 -0.0140 0.084 Uiso 1 1 calc R . . C20 C 0.5628(4) 0.6452(4) 0.0604(2) 0.0736(16) Uani 1 1 d . . . H20A H 0.5642 0.5658 0.0644 0.110 Uiso 1 1 calc R . . H20B H 0.5034 0.6679 0.0343 0.110 Uiso 1 1 calc R . . H20C H 0.5738 0.6788 0.0994 0.110 Uiso 1 1 calc R . . C21 C 0.6384(2) 0.8648(3) 0.16545(18) 0.0389(11) Uani 1 1 d . . . H21A H 0.5984 0.8506 0.1253 0.058 Uiso 1 1 calc R . . H21B H 0.6359 0.9424 0.1746 0.058 Uiso 1 1 calc R . . H21C H 0.6185 0.8215 0.1939 0.058 Uiso 1 1 calc R . . C22 C 0.7348(2) 0.8339(3) 0.16946(16) 0.0250(9) Uani 1 1 d . . . C23 C 0.7926(2) 0.8201(3) 0.22622(17) 0.0294(9) Uani 1 1 d . . . H23A H 0.7642 0.8018 0.2552 0.035 Uiso 1 1 calc R . . C24 C 0.8872(3) 0.8291(3) 0.24735(16) 0.0276(9) Uani 1 1 d . . . C25 C 0.9241(3) 0.8506(3) 0.31341(15) 0.0339(10) Uani 1 1 d . . . H25A H 0.9874 0.8273 0.3280 0.051 Uiso 1 1 calc R . . H25B H 0.8885 0.8097 0.3340 0.051 Uiso 1 1 calc R . . H25C H 0.9201 0.9286 0.3210 0.051 Uiso 1 1 calc R . . C26 C 1.0355(2) 0.8527(3) 0.24448(15) 0.0247(9) Uani 1 1 d . . . C27 C 1.0644(2) 0.9616(3) 0.24815(16) 0.0277(9) Uani 1 1 d . . . C28 C 1.1537(3) 0.9846(3) 0.28059(17) 0.0375(10) Uani 1 1 d . . . H28A H 1.1744 1.0578 0.2841 0.045 Uiso 1 1 calc R . . C29 C 1.2126(3) 0.9028(3) 0.30767(18) 0.0422(11) Uani 1 1 d . . . H29A H 1.2731 0.9197 0.3302 0.051 Uiso 1 1 calc R . . C30 C 1.1833(3) 0.7969(3) 0.30189(17) 0.0374(11) Uani 1 1 d . . . H30A H 1.2247 0.7413 0.3206 0.045 Uiso 1 1 calc R . . C31 C 1.0962(2) 0.7679(3) 0.26998(16) 0.0285(9) Uani 1 1 d . . . C32 C 1.0033(3) 1.0528(3) 0.21452(18) 0.0353(10) Uani 1 1 d . . . H32A H 0.9573 1.0192 0.1797 0.042 Uiso 1 1 calc R . . C33 C 1.0566(3) 1.1365(3) 0.19052(19) 0.0508(12) Uani 1 1 d . . . H33A H 1.0156 1.1939 0.1692 0.076 Uiso 1 1 calc R . . H33B H 1.0841 1.1004 0.1634 0.076 Uiso 1 1 calc R . . H33C H 1.1042 1.1687 0.2236 0.076 Uiso 1 1 calc R . . C34 C 0.9531(3) 1.1095(4) 0.2507(2) 0.0627(14) Uani 1 1 d . . . H34A H 0.9191 1.0559 0.2659 0.094 Uiso 1 1 calc R . . H34B H 0.9111 1.1625 0.2259 0.094 Uiso 1 1 calc R . . H34C H 0.9962 1.1472 0.2839 0.094 Uiso 1 1 calc R . . C35 C 1.0686(3) 0.6491(3) 0.26261(17) 0.0314(10) Uani 1 1 d . . . H35A H 1.0184 0.6420 0.2245 0.038 Uiso 1 1 calc R . . C36 C 1.1462(3) 0.5765(3) 0.25848(18) 0.0422(11) Uani 1 1 d . . . H36A H 1.1690 0.6031 0.2268 0.063 Uiso 1 1 calc R . . H36B H 1.1244 0.5017 0.2497 0.063 Uiso 1 1 calc R . . H36C H 1.1950 0.5782 0.2962 0.063 Uiso 1 1 calc R . . C37 C 1.0335(3) 0.6072(3) 0.31223(18) 0.0457(12) Uani 1 1 d . . . H37A H 0.9839 0.6537 0.3152 0.069 Uiso 1 1 calc R . . H37B H 1.0826 0.6086 0.3499 0.069 Uiso 1 1 calc R . . H37C H 1.0116 0.5324 0.3034 0.069 Uiso 1 1 calc R . . C38 C 1.0952(3) 0.8331(3) 0.13450(16) 0.0291(10) Uani 1 1 d . . . H38A H 1.0720 0.9004 0.1434 0.035 Uiso 1 1 calc R . . C39 C 1.1811(3) 0.8328(3) 0.13102(16) 0.0326(10) Uani 1 1 d . . . H39A H 1.2163 0.8975 0.1392 0.039 Uiso 1 1 calc R . . C40 C 1.2178(2) 0.7372(3) 0.11537(16) 0.0302(9) Uani 1 1 d . . . C41 C 1.1597(3) 0.6471(3) 0.10354(17) 0.0328(10) Uani 1 1 d . . . H41A H 1.1787 0.5806 0.0907 0.039 Uiso 1 1 calc R . . C42 C 1.0751(2) 0.6545(3) 0.11042(16) 0.0287(9) Uani 1 1 d . . . H42A H 1.0386 0.5908 0.1034 0.034 Uiso 1 1 calc R . . C43 C 1.3625(3) 0.8263(4) 0.1294(2) 0.0492(12) Uani 1 1 d . . . H43A H 1.3660 0.8494 0.1696 0.074 Uiso 1 1 calc R . . H43B H 1.3384 0.8860 0.1016 0.074 Uiso 1 1 calc R . . H43C H 1.4231 0.8070 0.1281 0.074 Uiso 1 1 calc R . . C44 C 1.3355(3) 0.6407(3) 0.08673(19) 0.0465(12) Uani 1 1 d . . . H44A H 1.3227 0.5731 0.1046 0.070 Uiso 1 1 calc R . . H44B H 1.4008 0.6475 0.0938 0.070 Uiso 1 1 calc R . . H44C H 1.3044 0.6394 0.0440 0.070 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 0.02054(18) 0.02039(18) 0.02360(19) 0.00039(17) 0.00888(13) 0.00060(16) N1 0.0231(18) 0.0261(18) 0.0347(19) 0.0007(14) 0.0063(15) 0.0011(13) N2 0.0239(18) 0.0388(19) 0.0287(19) 0.0023(14) 0.0105(15) 0.0046(13) N3 0.0211(17) 0.0243(17) 0.0258(19) 0.0005(14) 0.0065(15) 0.0004(13) N4 0.0191(17) 0.0251(17) 0.0243(18) 0.0025(14) 0.0090(14) -0.0005(13) N5 0.0218(15) 0.0272(16) 0.0223(16) -0.0010(16) 0.0082(12) 0.0010(16) N6 0.026(2) 0.050(2) 0.052(2) -0.0118(18) 0.0201(16) -0.0074(16) C1 0.040(2) 0.018(2) 0.049(3) 0.0030(19) 0.012(2) -0.0007(18) C2 0.053(3) 0.039(3) 0.105(4) 0.023(3) 0.029(3) -0.006(2) C3 0.057(3) 0.021(2) 0.066(3) 0.008(2) 0.006(3) 0.001(2) C4 0.073(3) 0.030(2) 0.058(3) -0.012(2) 0.008(3) -0.007(2) C5 0.029(2) 0.041(2) 0.025(2) 0.0028(19) 0.0101(19) -0.0005(18) C6 0.058(3) 0.057(3) 0.040(3) 0.002(2) 0.015(2) 0.006(2) C7 0.055(3) 0.064(3) 0.033(3) 0.011(2) 0.015(2) 0.014(2) C8 0.049(3) 0.082(4) 0.035(3) 0.007(2) 0.018(2) -0.015(3) C9 0.017(2) 0.030(2) 0.027(2) -0.0024(17) 0.0116(17) 0.0016(16) C10 0.026(2) 0.030(2) 0.028(2) -0.0029(18) 0.0131(18) 0.0017(17) C11 0.031(2) 0.034(2) 0.036(3) 0.005(2) 0.011(2) 0.0099(19) C12 0.032(2) 0.049(3) 0.030(2) 0.007(2) 0.008(2) 0.014(2) C13 0.026(2) 0.044(3) 0.027(2) -0.005(2) 0.0085(19) 0.0007(19) C14 0.019(2) 0.036(2) 0.031(2) -0.0021(19) 0.0137(19) 0.0010(18) C15 0.036(2) 0.019(2) 0.039(2) 0.0031(18) 0.005(2) 0.0028(17) C16 0.052(3) 0.052(3) 0.063(3) -0.002(2) 0.016(3) -0.017(2) C17 0.069(4) 0.056(3) 0.068(4) -0.026(3) 0.025(3) -0.007(3) C18 0.024(2) 0.034(3) 0.039(3) -0.006(2) 0.009(2) -0.0101(18) C19 0.075(4) 0.038(3) 0.056(3) -0.013(2) 0.021(3) -0.003(2) C20 0.083(4) 0.048(3) 0.112(5) -0.003(3) 0.062(4) -0.014(3) C21 0.028(2) 0.051(3) 0.042(3) 0.003(2) 0.015(2) 0.0064(19) C22 0.028(2) 0.022(2) 0.028(2) 0.0004(17) 0.0131(19) 0.0013(16) C23 0.030(2) 0.034(2) 0.028(2) 0.0031(18) 0.0159(19) -0.0014(17) C24 0.029(2) 0.025(2) 0.030(2) 0.0034(17) 0.0105(19) 0.0036(17) C25 0.034(2) 0.045(3) 0.025(2) -0.0010(19) 0.0137(19) -0.0016(19) C26 0.029(2) 0.029(2) 0.019(2) 0.0022(17) 0.0128(18) 0.0010(17) C27 0.032(2) 0.028(2) 0.025(2) 0.0022(17) 0.0111(18) -0.0001(17) C28 0.039(3) 0.037(2) 0.033(3) 0.002(2) 0.006(2) -0.009(2) C29 0.028(2) 0.049(3) 0.040(3) 0.004(2) -0.004(2) -0.008(2) C30 0.027(2) 0.045(3) 0.036(3) 0.008(2) 0.003(2) 0.0026(19) C31 0.025(2) 0.039(3) 0.023(2) 0.0032(18) 0.0088(17) 0.0000(18) C32 0.032(2) 0.028(2) 0.040(3) -0.0005(19) 0.003(2) -0.0009(18) C33 0.057(3) 0.044(3) 0.052(3) 0.012(2) 0.019(2) 0.006(2) C34 0.067(4) 0.057(3) 0.078(4) 0.020(3) 0.043(3) 0.023(3) C35 0.031(2) 0.031(2) 0.030(2) 0.0066(18) 0.0071(19) 0.0034(18) C36 0.042(3) 0.041(3) 0.042(3) 0.000(2) 0.010(2) 0.009(2) C37 0.060(3) 0.034(2) 0.051(3) 0.011(2) 0.027(2) -0.001(2) C38 0.039(3) 0.020(2) 0.032(2) -0.0064(17) 0.016(2) -0.0007(18) C39 0.031(2) 0.036(2) 0.035(3) -0.0096(19) 0.015(2) -0.0146(18) C40 0.026(2) 0.038(3) 0.027(2) -0.0028(19) 0.0080(17) -0.001(2) C41 0.033(2) 0.027(2) 0.044(3) -0.0011(19) 0.021(2) 0.0079(18) C42 0.026(2) 0.024(2) 0.037(2) -0.0021(18) 0.0108(19) -0.0010(17) C43 0.032(3) 0.061(3) 0.061(3) -0.011(2) 0.024(2) -0.011(2) C44 0.028(2) 0.060(3) 0.058(3) -0.011(2) 0.023(2) 0.002(2) _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 1.795(3) . ? Nb1 N1 1.797(3) . ? Nb1 N3 2.213(3) . ? Nb1 N5 2.304(3) . ? Nb1 N4 2.339(3) . ? N1 C1 1.452(4) . ? N2 C5 1.453(5) . ? N3 C22 1.335(4) . ? N3 C9 1.448(4) . ? N4 C24 1.336(4) . ? N4 C26 1.445(4) . ? N5 C38 1.346(4) . ? N5 C42 1.347(4) . ? N6 C40 1.352(5) . ? N6 C44 1.447(5) . ? N6 C43 1.448(5) . ? C1 C2 1.522(6) . ? C1 C4 1.523(6) . ? C1 C3 1.530(5) . ? C5 C6 1.513(5) . ? C5 C7 1.517(5) . ? C5 C8 1.524(5) . ? C9 C14 1.391(5) . ? C9 C10 1.403(5) . ? C10 C11 1.388(5) . ? C10 C15 1.511(5) . ? C11 C12 1.368(5) . ? C12 C13 1.368(5) . ? C13 C14 1.384(5) . ? C14 C18 1.522(5) . ? C15 C16 1.516(5) . ? C15 C17 1.534(5) . ? C18 C19 1.510(5) . ? C18 C20 1.522(6) . ? C21 C22 1.520(5) . ? C22 C23 1.380(5) . ? C23 C24 1.403(5) . ? C24 C25 1.517(5) . ? C26 C27 1.406(5) . ? C26 C31 1.410(5) . ? C27 C28 1.393(5) . ? C27 C32 1.526(5) . ? C28 C29 1.377(5) . ? C29 C30 1.371(5) . ? C30 C31 1.379(5) . ? C31 C35 1.516(5) . ? C32 C34 1.496(6) . ? C32 C33 1.535(5) . ? C35 C36 1.526(5) . ? C35 C37 1.531(5) . ? C38 C39 1.362(5) . ? C39 C40 1.405(5) . ? C40 C41 1.401(5) . ? C41 C42 1.375(5) . ? 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 112.80(13) . . ? N2 Nb1 N3 95.85(12) . . ? N1 Nb1 N3 103.75(12) . . ? N2 Nb1 N5 83.94(11) . . ? N1 Nb1 N5 96.98(12) . . ? N3 Nb1 N5 157.48(10) . . ? N2 Nb1 N4 140.94(12) . . ? N1 Nb1 N4 105.38(11) . . ? N3 Nb1 N4 82.52(10) . . ? N5 Nb1 N4 83.60(10) . . ? C1 N1 Nb1 165.3(3) . . ? C5 N2 Nb1 166.7(3) . . ? C22 N3 C9 116.3(3) . . ? C22 N3 Nb1 123.7(2) . . ? C9 N3 Nb1 119.9(2) . . ? C24 N4 C26 114.7(3) . . ? C24 N4 Nb1 119.0(2) . . ? C26 N4 Nb1 125.0(2) . . ? C38 N5 C42 114.5(3) . . ? C38 N5 Nb1 124.2(2) . . ? C42 N5 Nb1 119.8(2) . . ? C40 N6 C44 121.5(3) . . ? C40 N6 C43 120.3(3) . . ? C44 N6 C43 117.6(3) . . ? N1 C1 C2 108.9(3) . . ? N1 C1 C4 110.9(3) . . ? C2 C1 C4 110.0(4) . . ? N1 C1 C3 109.3(3) . . ? C2 C1 C3 108.6(3) . . ? C4 C1 C3 109.2(4) . . ? N2 C5 C6 111.1(3) . . ? N2 C5 C7 109.1(3) . . ? C6 C5 C7 110.0(3) . . ? N2 C5 C8 108.7(3) . . ? C6 C5 C8 107.7(4) . . ? C7 C5 C8 110.2(3) . . ? C14 C9 C10 119.8(3) . . ? C14 C9 N3 121.6(3) . . ? C10 C9 N3 118.7(3) . . ? C11 C10 C9 118.8(3) . . ? C11 C10 C15 119.0(3) . . ? C9 C10 C15 122.2(3) . . ? C12 C11 C10 121.3(4) . . ? C11 C12 C13 119.6(4) . . ? C12 C13 C14 121.3(4) . . ? C13 C14 C9 119.2(4) . . ? C13 C14 C18 118.8(3) . . ? C9 C14 C18 121.9(4) . . ? C10 C15 C16 110.7(3) . . ? C10 C15 C17 111.8(3) . . ? C16 C15 C17 109.7(3) . . ? C19 C18 C20 108.5(3) . . ? C19 C18 C14 113.7(3) . . ? C20 C18 C14 112.0(3) . . ? N3 C22 C23 124.3(3) . . ? N3 C22 C21 120.5(3) . . ? C23 C22 C21 115.1(3) . . ? C22 C23 C24 129.4(4) . . ? N4 C24 C23 125.0(3) . . ? N4 C24 C25 120.9(3) . . ? C23 C24 C25 113.8(3) . . ? C27 C26 C31 121.1(3) . . ? C27 C26 N4 119.0(3) . . ? C31 C26 N4 119.8(3) . . ? C28 C27 C26 118.2(3) . . ? C28 C27 C32 119.6(3) . . ? C26 C27 C32 122.0(3) . . ? C29 C28 C27 121.0(4) . . ? C30 C29 C28 119.5(4) . . ? C29 C30 C31 122.6(4) . . ? C30 C31 C26 117.3(3) . . ? C30 C31 C35 120.4(3) . . ? C26 C31 C35 122.2(3) . . ? C34 C32 C27 113.1(3) . . ? C34 C32 C33 109.6(3) . . ? C27 C32 C33 111.5(3) . . ? C31 C35 C36 111.7(3) . . ? C31 C35 C37 112.9(3) . . ? C36 C35 C37 109.1(3) . . ? N5 C38 C39 125.2(3) . . ? C38 C39 C40 120.2(3) . . ? N6 C40 C41 122.8(4) . . ? N6 C40 C39 122.1(3) . . ? C41 C40 C39 115.2(3) . . ? C42 C41 C40 120.3(3) . . ? N5 C42 C41 124.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Nb1 N1 C1 -1.3(10) . . . . ? N3 Nb1 N1 C1 101.2(10) . . . . ? N5 Nb1 N1 C1 -87.6(10) . . . . ? N4 Nb1 N1 C1 -172.9(10) . . . . ? N1 Nb1 N2 C5 -58.6(12) . . . . ? N3 Nb1 N2 C5 -166.2(11) . . . . ? N5 Nb1 N2 C5 36.4(11) . . . . ? N4 Nb1 N2 C5 108.5(11) . . . . ? N2 Nb1 N3 C22 -175.1(3) . . . . ? N1 Nb1 N3 C22 69.7(3) . . . . ? N5 Nb1 N3 C22 -86.8(4) . . . . ? N4 Nb1 N3 C22 -34.4(3) . . . . ? N2 Nb1 N3 C9 5.2(2) . . . . ? N1 Nb1 N3 C9 -110.0(2) . . . . ? N5 Nb1 N3 C9 93.5(3) . . . . ? N4 Nb1 N3 C9 145.9(2) . . . . ? N2 Nb1 N4 C24 125.9(3) . . . . ? N1 Nb1 N4 C24 -66.5(3) . . . . ? N3 Nb1 N4 C24 35.8(2) . . . . ? N5 Nb1 N4 C24 -162.0(3) . . . . ? N2 Nb1 N4 C26 -67.8(3) . . . . ? N1 Nb1 N4 C26 99.9(3) . . . . ? N3 Nb1 N4 C26 -157.9(3) . . . . ? N5 Nb1 N4 C26 4.4(3) . . . . ? N2 Nb1 N5 C38 82.6(3) . . . . ? N1 Nb1 N5 C38 -165.1(3) . . . . ? N3 Nb1 N5 C38 -8.1(4) . . . . ? N4 Nb1 N5 C38 -60.4(3) . . . . ? N2 Nb1 N5 C42 -83.0(3) . . . . ? N1 Nb1 N5 C42 29.3(3) . . . . ? N3 Nb1 N5 C42 -173.7(3) . . . . ? N4 Nb1 N5 C42 134.1(3) . . . . ? Nb1 N1 C1 C2 -112.9(10) . . . . ? Nb1 N1 C1 C4 8.3(12) . . . . ? Nb1 N1 C1 C3 128.7(9) . . . . ? Nb1 N2 C5 C6 54.1(12) . . . . ? Nb1 N2 C5 C7 175.5(10) . . . . ? Nb1 N2 C5 C8 -64.3(12) . . . . ? C22 N3 C9 C14 -97.1(4) . . . . ? Nb1 N3 C9 C14 82.6(4) . . . . ? C22 N3 C9 C10 81.6(4) . . . . ? Nb1 N3 C9 C10 -98.7(3) . . . . ? C14 C9 C10 C11 1.5(5) . . . . ? N3 C9 C10 C11 -177.3(3) . . . . ? C14 C9 C10 C15 -179.2(3) . . . . ? N3 C9 C10 C15 2.1(5) . . . . ? C9 C10 C11 C12 -0.6(6) . . . . ? C15 C10 C11 C12 -179.9(4) . . . . ? C10 C11 C12 C13 -1.0(6) . . . . ? C11 C12 C13 C14 1.5(6) . . . . ? C12 C13 C14 C9 -0.6(6) . . . . ? C12 C13 C14 C18 -179.9(4) . . . . ? C10 C9 C14 C13 -1.0(5) . . . . ? N3 C9 C14 C13 177.8(3) . . . . ? C10 C9 C14 C18 178.3(3) . . . . ? N3 C9 C14 C18 -2.9(6) . . . . ? C11 C10 C15 C16 -63.8(5) . . . . ? C9 C10 C15 C16 116.9(4) . . . . ? C11 C10 C15 C17 58.9(5) . . . . ? C9 C10 C15 C17 -120.4(4) . . . . ? C13 C14 C18 C19 41.1(5) . . . . ? C9 C14 C18 C19 -138.2(4) . . . . ? C13 C14 C18 C20 -82.4(5) . . . . ? C9 C14 C18 C20 98.3(5) . . . . ? C9 N3 C22 C23 -164.6(3) . . . . ? Nb1 N3 C22 C23 15.7(5) . . . . ? C9 N3 C22 C21 11.8(5) . . . . ? Nb1 N3 C22 C21 -167.9(2) . . . . ? N3 C22 C23 C24 21.1(6) . . . . ? C21 C22 C23 C24 -155.5(4) . . . . ? C26 N4 C24 C23 172.2(3) . . . . ? Nb1 N4 C24 C23 -20.1(5) . . . . ? C26 N4 C24 C25 -2.5(5) . . . . ? Nb1 N4 C24 C25 165.2(2) . . . . ? C22 C23 C24 N4 -17.0(6) . . . . ? C22 C23 C24 C25 158.1(4) . . . . ? C24 N4 C26 C27 -89.9(4) . . . . ? Nb1 N4 C26 C27 103.3(3) . . . . ? C24 N4 C26 C31 90.6(4) . . . . ? Nb1 N4 C26 C31 -76.2(4) . . . . ? C31 C26 C27 C28 -3.6(5) . . . . ? N4 C26 C27 C28 176.9(3) . . . . ? C31 C26 C27 C32 172.2(3) . . . . ? N4 C26 C27 C32 -7.3(5) . . . . ? C26 C27 C28 C29 0.9(6) . . . . ? C32 C27 C28 C29 -175.0(4) . . . . ? C27 C28 C29 C30 1.0(6) . . . . ? C28 C29 C30 C31 -0.3(7) . . . . ? C29 C30 C31 C26 -2.2(6) . . . . ? C29 C30 C31 C35 177.1(4) . . . . ? C27 C26 C31 C30 4.2(5) . . . . ? N4 C26 C31 C30 -176.3(3) . . . . ? C27 C26 C31 C35 -175.1(3) . . . . ? N4 C26 C31 C35 4.4(5) . . . . ? C28 C27 C32 C34 -90.1(5) . . . . ? C26 C27 C32 C34 94.2(4) . . . . ? C28 C27 C32 C33 34.0(5) . . . . ? C26 C27 C32 C33 -141.7(4) . . . . ? C30 C31 C35 C36 -34.3(5) . . . . ? C26 C31 C35 C36 145.0(4) . . . . ? C30 C31 C35 C37 89.2(4) . . . . ? C26 C31 C35 C37 -91.6(4) . . . . ? C42 N5 C38 C39 -3.9(5) . . . . ? Nb1 N5 C38 C39 -170.2(3) . . . . ? N5 C38 C39 C40 3.0(6) . . . . ? C44 N6 C40 C41 12.4(6) . . . . ? C43 N6 C40 C41 -175.9(4) . . . . ? C44 N6 C40 C39 -168.7(4) . . . . ? C43 N6 C40 C39 3.0(6) . . . . ? C38 C39 C40 N6 -178.2(4) . . . . ? C38 C39 C40 C41 0.8(5) . . . . ? N6 C40 C41 C42 175.8(4) . . . . ? C39 C40 C41 C42 -3.2(5) . . . . ? C38 N5 C42 C41 1.2(5) . . . . ? Nb1 N5 C42 C41 168.1(3) . . . . ? C40 C41 C42 N5 2.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.54 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.717 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.064