# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2247 data_structure1 _audit_creation_date 99-05-31 _audit_creation_method CRYSTALS_ver_07-07-97 # MartNb3 #============================================================================= ## -----------------REFERENCES ----------------------## _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refxyz #**************************************************************************** _cell_length_a 8.775(2) _cell_angle_alpha 90. _cell_length_b 12.804(2) _cell_angle_beta 103.61(2) _cell_length_c 12.648(2) _cell_angle_gamma 90. _cell_volume 1381.1 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Nb ' -2.1970 0.6210 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957 3.7559 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C13 H14 Cl2 N1 Nb1 ' _chemical_formula_moiety ' C13 H14 Cl2 N1 Nb1 ' _chemical_formula_weight 348.07 _cell_measurement_reflns_used 7157 _cell_measurement_theta_min 0 _cell_measurement_theta_max 26.45 _cell_measurement_temperature 180 _cell_formula_units_Z 4 _exptl_crystal_description ' box ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.02 _exptl_crystal_density_diffrn 1.67 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 688.18 _exptl_absorpt_coefficient_mu 1.20 _exptl_absorpt_correction_type multi-scan _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 180 _diffrn_reflns_number 7157 _reflns_number_total 2879 _diffrn_reflns_av_R_equivalents 0.032 _reflns_number_observed 2682 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.45 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _reflns_observed_criterion 3.00\s(I) _refine_diff_density_min -0.85 _refine_diff_density_max 1.96 _refine_ls_number_reflns 2682 _refine_ls_number_parameters 155 _refine_ls_R_factor_obs 0.0508 _refine_ls_wR_factor_obs 0.0533 _refine_ls_goodness_of_fit_obs 1.0881 _refine_ls_shift/su_max 0.000117 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 3.05 1.64 2.34 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Nb1 0.25566(3) -0.045993(17) 0.243929(18) 0.0293 1.0000 Uani N2 0.3900(3) 0.02683(19) 0.1898(2) 0.0367 1.0000 Uani C3 0.4792(3) 0.1031(2) 0.1570(2) 0.0343 1.0000 Uani C4 0.6081(3) 0.1448(2) 0.2315(2) 0.0373 1.0000 Uani C5 0.7006(4) 0.2173(2) 0.1959(3) 0.0434 1.0000 Uani C6 0.6665(3) 0.2492(2) 0.0888(3) 0.0459 1.0000 Uani C7 0.5387(4) 0.2087(2) 0.0167(3) 0.0456 1.0000 Uani C8 0.4424(3) 0.1355(2) 0.0482(2) 0.0390 1.0000 Uani C9 0.3055(4) 0.0898(3) -0.0308(3) 0.0538 1.0000 Uani C10 0.6488(4) 0.1088(3) 0.3474(3) 0.0523 1.0000 Uani Cl11 0.1232(1) -0.14705(6) 0.09761(7) 0.0481 1.0000 Uani Cl12 0.4200(1) -0.15778(6) 0.36692(7) 0.0517 1.0000 Uani C13 0.0968(4) -0.0320(3) 0.3821(3) 0.0492 1.0000 Uani C14 -0.0068(4) -0.0208(3) 0.2829(3) 0.0468 1.0000 Uani C15 0.0380(4) 0.0678(3) 0.2316(3) 0.0531 1.0000 Uani C16 0.1670(4) 0.1114(2) 0.3035(3) 0.0553 1.0000 Uani C17 0.2066(5) 0.0482(3) 0.3951(3) 0.0525 1.0000 Uani H51 0.7969 0.2475 0.2491 0.0456 1.0000 Uiso H61 0.7339 0.3035 0.0650 0.0495 1.0000 Uiso H71 0.5146 0.2333 -0.0611 0.0535 1.0000 Uiso H91 0.2949 0.1216 -0.1048 0.0540 1.0000 Uiso H92 0.3167 0.0124 -0.0360 0.0540 1.0000 Uiso H93 0.2055 0.1049 -0.0064 0.0540 1.0000 Uiso H101 0.7461 0.1448 0.3899 0.0541 1.0000 Uiso H102 0.6705 0.0305 0.3514 0.0541 1.0000 Uiso H103 0.5607 0.1227 0.3831 0.0541 1.0000 Uiso H131 0.0942 -0.0892 0.4368 0.0540 1.0000 Uiso H141 -0.0983 -0.0690 0.2510 0.0517 1.0000 Uiso H151 -0.0156 0.0936 0.1550 0.0603 1.0000 Uiso H161 0.2218 0.1787 0.2924 0.0551 1.0000 Uiso H171 0.2995 0.0587 0.4592 0.0648 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.03104(19) 0.02408(18) 0.03235(19) -0.00156(7) 0.00646(13) 0.00202(7) N2 0.0348(13) 0.0414(12) 0.0340(12) -0.0017(9) 0.0087(11) -0.0006(9) C3 0.0287(12) 0.0398(13) 0.0351(13) 0.000(1) 0.0088(11) 0.004(1) C4 0.0328(13) 0.0438(14) 0.0359(14) -0.001(1) 0.0090(11) 0.002(1) C5 0.0350(15) 0.0455(15) 0.0499(18) -0.0020(12) 0.0104(14) -0.0027(11) C6 0.0383(15) 0.0468(17) 0.0561(18) 0.0090(13) 0.0180(14) 0.0022(12) C7 0.0432(17) 0.0519(18) 0.0432(17) 0.0142(12) 0.0134(15) 0.0083(12) C8 0.0370(14) 0.0423(14) 0.0379(14) 0.0047(11) 0.0094(12) 0.0068(11) C9 0.0474(17) 0.070(2) 0.0383(16) 0.0083(15) -0.0022(14) -0.0016(15) C10 0.0450(17) 0.072(2) 0.0364(15) 0.0008(14) 0.0017(13) -0.0120(15) Cl11 0.0459(4) 0.0475(4) 0.0480(4) -0.0180(3) 0.0049(3) -0.0020(3) Cl12 0.0535(5) 0.0410(4) 0.0547(5) 0.0071(3) 0.0006(4) 0.0157(3) C13 0.055(2) 0.0509(17) 0.0476(18) 0.0021(13) 0.0229(17) 0.0068(13) C14 0.0355(16) 0.0525(17) 0.0541(19) -0.0096(14) 0.0141(15) 0.0033(13) C15 0.056(2) 0.0507(17) 0.054(2) 0.0107(15) 0.0166(17) 0.0287(16) C16 0.065(2) 0.0238(13) 0.084(3) -0.0113(14) 0.0328(19) 0.0029(13) C17 0.059(2) 0.0515(18) 0.0466(19) -0.0217(13) 0.0106(17) 0.0026(14) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nb1 . N2 . 1.763(2) yes Nb1 . Cl11 . 2.3319(7) yes Nb1 . Cl12 . 2.3433(7) yes Nb1 . C13 . 2.486(3) yes Nb1 . C14 . 2.487(3) yes Nb1 . C15 . 2.378(3) yes Nb1 . C16 . 2.347(3) yes Nb1 . C17 . 2.384(3) yes N2 . C3 . 1.375(4) yes C3 . C4 . 1.397(4) yes C3 . C8 . 1.400(4) yes C4 . C5 . 1.376(4) yes C4 . C10 . 1.498(4) yes C5 . C6 . 1.379(5) yes C5 . H51 . 1.024(3) no C6 . C7 . 1.370(5) yes C6 . H61 . 1.004(3) no C7 . C8 . 1.382(4) yes C7 . H71 . 1.007(3) no C8 . C9 . 1.489(5) yes C9 . H91 . 1.004(3) no C9 . H92 . 1.000(4) no C9 . H93 . 1.015(4) no C10 . H101 . 1.007(3) no C10 . H102 . 1.020(4) no C10 . H103 . 0.999(4) no C13 . C14 . 1.373(5) yes C13 . C17 . 1.392(5) yes C13 . H131 . 1.011(3) no C14 . C15 . 1.408(5) yes C14 . H141 . 1.018(3) no C15 . C16 . 1.391(5) yes C15 . H151 . 1.028(4) no C16 . C17 . 1.389(5) yes C16 . H161 . 1.012(3) no C17 . H171 . 1.014(4) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 . Nb1 . Cl11 . 103.85(8) yes N2 . Nb1 . Cl12 . 102.57(8) yes Cl11 . Nb1 . Cl12 . 107.57(3) yes N2 . Nb1 . C13 . 140.54(11) yes Cl11 . Nb1 . C13 . 109.92(9) yes Cl12 . Nb1 . C13 . 86.35(9) yes N2 . Nb1 . C14 . 138.03(11) yes Cl11 . Nb1 . C14 . 85.26(8) yes Cl12 . Nb1 . C14 . 113.66(9) yes C13 . Nb1 . C14 . 32.05(12) yes N2 . Nb1 . C15 . 104.51(12) yes Cl11 . Nb1 . C15 . 92.6(1) yes Cl12 . Nb1 . C15 . 140.97(9) yes C13 . Nb1 . C15 . 55.06(12) yes C14 . Nb1 . C15 . 33.56(12) yes N2 . Nb1 . C16 . 88.44(11) yes Cl11 . Nb1 . C16 . 126.2(1) yes Cl12 . Nb1 . C16 . 120.7(1) yes C13 . Nb1 . C16 . 55.22(11) yes C14 . Nb1 . C16 . 55.44(11) yes N2 . Nb1 . C17 . 107.89(12) yes Cl11 . Nb1 . C17 . 140.1(1) yes Cl12 . Nb1 . C17 . 88.6(1) yes C13 . Nb1 . C17 . 33.13(12) yes C14 . Nb1 . C17 . 54.91(12) yes C15 . Nb1 . C16 . 34.22(13) yes C15 . Nb1 . C17 . 56.55(14) yes C16 . Nb1 . C17 . 34.14(13) yes Nb1 . N2 . C3 . 166.6(2) yes N2 . C3 . C4 . 119.7(2) yes N2 . C3 . C8 . 119.4(2) yes C4 . C3 . C8 . 120.8(3) yes C3 . C4 . C5 . 118.9(3) yes C3 . C4 . C10 . 120.8(3) yes C5 . C4 . C10 . 120.3(3) yes C4 . C5 . C6 . 120.9(3) yes C4 . C5 . H51 . 119.9(3) no C6 . C5 . H51 . 119.2(3) no C5 . C6 . C7 . 119.7(3) yes C5 . C6 . H61 . 119.5(3) no C7 . C6 . H61 . 120.7(3) no C6 . C7 . C8 . 121.7(3) yes C6 . C7 . H71 . 118.8(3) no C8 . C7 . H71 . 119.5(3) no C3 . C8 . C7 . 118.0(3) yes C3 . C8 . C9 . 120.4(3) yes C7 . C8 . C9 . 121.6(3) yes C8 . C9 . H91 . 110.4(3) no C8 . C9 . H92 . 110.9(3) no H91 . C9 . H92 . 109.2(3) no C8 . C9 . H93 . 109.9(3) no H91 . C9 . H93 . 108.0(3) no H92 . C9 . H93 . 108.3(3) no C4 . C10 . H101 . 111.0(3) no C4 . C10 . H102 . 110.4(3) no H101 . C10 . H102 . 107.4(3) no C4 . C10 . H103 . 110.9(3) no H101 . C10 . H103 . 109.1(3) no H102 . C10 . H103 . 108.0(3) no Nb1 . C13 . C14 . 74.04(19) yes Nb1 . C13 . C17 . 69.44(19) yes C14 . C13 . C17 . 108.8(3) yes Nb1 . C13 . H131 . 122.4(2) no C14 . C13 . H131 . 125.7(4) no C17 . C13 . H131 . 125.5(4) no Nb1 . C14 . C13 . 73.91(19) yes Nb1 . C14 . C15 . 68.95(18) yes C13 . C14 . C15 . 108.0(3) yes Nb1 . C14 . H141 . 121.6(2) no C13 . C14 . H141 . 126.2(4) no C15 . C14 . H141 . 125.8(4) no Nb1 . C15 . C14 . 77.49(17) yes Nb1 . C15 . C16 . 71.69(18) yes C14 . C15 . C16 . 107.2(3) yes Nb1 . C15 . H151 . 116.2(2) no C14 . C15 . H151 . 125.3(4) no C16 . C15 . H151 . 127.5(4) no Nb1 . C16 . C15 . 74.09(17) yes Nb1 . C16 . C17 . 74.40(17) yes C15 . C16 . C17 . 108.5(3) yes Nb1 . C16 . H161 . 118.8(2) no C15 . C16 . H161 . 126.3(4) no C17 . C16 . H161 . 125.2(4) no Nb1 . C17 . C13 . 77.42(18) yes Nb1 . C17 . C16 . 71.47(18) yes C13 . C17 . C16 . 107.5(3) yes Nb1 . C17 . H171 . 116.4(3) no C13 . C17 . H171 . 126.6(4) no C16 . C17 . H171 . 125.9(4) no #=END data_structure4 _audit_creation_method SHELXL _chemical_formula_moiety 'C58 H68 N6 Nb2' _chemical_formula_structural 'C58 H68 N6 NB2' _chemical_formula_analytical ? _chemical_formula_sum 'C58 H68 N6 Nb2' _chemical_formula_weight 1035.00 _chemical_compound_source 'synthesis as described' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.969(10) _cell_length_b 17.246(20) _cell_length_c 18.845(10) _cell_angle_alpha 76.26(6) _cell_angle_beta 89.60(3) _cell_angle_gamma 89.97(5) _cell_volume 2515.7(45) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 166 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method none _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7773 _exptl_absorpt_correction_T_max 0.9142 _exptl_special_details ? _diffrn_ambient_temperature 293(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 'Enraf-Nonius DIP2000' _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7909 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7909 _reflns_number_observed 7866 _reflns_observed_criterion 2sigma(I) _computing_data_collection 'DIP2000 Software XPRESS (Mac Science)' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO & SCALEPACK' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin & Pearce, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.9882P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7901 _refine_ls_number_parameters 644 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_obs 0.0667 _refine_ls_wR_factor_all 0.1551 _refine_ls_wR_factor_obs 0.1319 _refine_ls_goodness_of_fit_all 1.437 _refine_ls_goodness_of_fit_obs 1.430 _refine_ls_restrained_S_all 1.675 _refine_ls_restrained_S_obs 1.428 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nb1 Nb 0.59246(6) -0.00461(3) 0.24858(2) 0.02084(13) Uani 1 d . . Nb2 Nb 1.06709(6) 0.38235(3) 0.22754(3) 0.02611(14) Uani 1 d . . C11 C 0.8744(8) 0.0500(4) 0.2346(4) 0.0399(15) Uani 1 d . . H11 H 0.9518(8) 0.0246(4) 0.2108(4) 0.048 Uiso 1 calc R . C12 C 0.7761(8) 0.1145(4) 0.2019(3) 0.041(2) Uani 1 d . . H12 H 0.7770(8) 0.1399(4) 0.1525(3) 0.050 Uiso 1 calc R . C13 C 0.6765(8) 0.1346(3) 0.2548(3) 0.0389(15) Uani 1 d . . H13 H 0.5981(8) 0.1757(3) 0.2477(3) 0.047 Uiso 1 calc R . C14 C 0.7151(8) 0.0818(4) 0.3211(3) 0.0371(15) Uani 1 d . . H14 H 0.6665(8) 0.0816(4) 0.3662(3) 0.045 Uiso 1 calc R . C15 C 0.8388(8) 0.0297(3) 0.3084(3) 0.0379(14) Uani 1 d . . H15 H 0.8882(8) -0.0113(3) 0.3431(3) 0.045 Uiso 1 calc R . N21 N 0.5649(6) -0.0062(3) 0.1428(2) 0.0273(10) Uani 1 d . . H2 H 0.5329(6) -0.0522(3) 0.1376(2) 0.033 Uiso 1 calc R . C22 C 0.5851(8) 0.0490(3) 0.0755(3) 0.0330(13) Uani 1 d . . C23 C 0.7061(8) 0.0330(4) 0.0259(3) 0.0360(14) Uani 1 d . . C24 C 0.8072(8) -0.0409(4) 0.0435(3) 0.043(2) Uani 1 d . . H24A H 0.7339(8) -0.0864(4) 0.0536(24) 0.065 Uiso 1 calc R . H24B H 0.8746(42) -0.0414(13) 0.0856(15) 0.065 Uiso 1 calc R . H24C H 0.8787(41) -0.0428(13) 0.0028(10) 0.065 Uiso 1 calc R . C25 C 0.7241(9) 0.0876(4) -0.0401(3) 0.045(2) Uani 1 d . . H25 H 0.8014(9) 0.0774(4) -0.0740(3) 0.054 Uiso 1 calc R . C26 C 0.6327(9) 0.1558(4) -0.0573(3) 0.047(2) Uani 1 d . . H26 H 0.6494(9) 0.1921(4) -0.1019(3) 0.056 Uiso 1 calc R . C27 C 0.5164(9) 0.1710(4) -0.0091(4) 0.049(2) Uani 1 d . . H27 H 0.4544(9) 0.2180(4) -0.0211(4) 0.058 Uiso 1 calc R . C28 C 0.4887(9) 0.1175(4) 0.0579(3) 0.0403(15) Uani 1 d . . C29 C 0.3501(11) 0.1308(5) 0.1070(4) 0.061(2) Uani 1 d . . H29A H 0.2763(40) 0.1714(24) 0.0806(9) 0.092 Uiso 1 calc R . H29B H 0.3962(11) 0.1476(32) 0.1479(16) 0.092 Uiso 1 calc R . H29C H 0.2886(44) 0.0821(10) 0.1242(24) 0.092 Uiso 1 calc R . N31 N 0.6189(5) -0.1083(2) 0.2866(2) 0.0226(9) Uani 1 d . . C32 C 0.6679(6) -0.1848(3) 0.3228(3) 0.0232(11) Uani 1 d . . C33 C 0.7356(7) -0.2369(3) 0.2830(3) 0.0302(12) Uani 1 d . . C34 C 0.7495(9) -0.2115(4) 0.2019(3) 0.044(2) Uani 1 d . . H34A H 0.8218(46) -0.1657(17) 0.1885(3) 0.066 Uiso 1 calc R . H34B H 0.6403(12) -0.1980(26) 0.1816(4) 0.066 Uiso 1 calc R . H34C H 0.7955(53) -0.2543(10) 0.1834(4) 0.066 Uiso 1 calc R . C35 C 0.7879(8) -0.3118(3) 0.3192(4) 0.0405(15) Uani 1 d . . H35 H 0.8317(8) -0.3466(3) 0.2929(4) 0.049 Uiso 1 calc R . C36 C 0.7758(9) -0.3354(3) 0.3936(4) 0.043(2) Uani 1 d . . H36 H 0.8133(9) -0.3857(3) 0.4179(4) 0.051 Uiso 1 calc R . C37 C 0.7087(8) -0.2851(3) 0.4325(3) 0.0353(13) Uani 1 d . . H37 H 0.7005(8) -0.3020(3) 0.4831(3) 0.042 Uiso 1 calc R . C38 C 0.6527(7) -0.2094(3) 0.3980(3) 0.0260(11) Uani 1 d . . C39 C 0.5781(8) -0.1551(4) 0.4404(3) 0.0368(14) Uani 1 d . . H39A H 0.5875(48) -0.1789(12) 0.4917(3) 0.055 Uiso 1 calc R . H39B H 0.4620(16) -0.1463(20) 0.4279(17) 0.055 Uiso 1 calc R . H39C H 0.6369(35) -0.1050(10) 0.4289(18) 0.055 Uiso 1 calc R . N41 N 0.3672(6) 0.0151(3) 0.2911(2) 0.0266(10) Uani 1 d . . H4 H 0.3332(6) 0.0637(3) 0.2782(2) 0.032 Uiso 1 calc R . C42 C 0.2566(7) -0.0367(3) 0.3379(3) 0.0246(11) Uani 1 d . . C43 C 0.1861(7) -0.1023(3) 0.3176(3) 0.0274(12) Uani 1 d . . C44 C 0.2130(8) -0.1159(4) 0.2430(3) 0.0365(14) Uani 1 d . . H44A H 0.3152(27) -0.1452(21) 0.2421(7) 0.055 Uiso 1 calc R . H44B H 0.2207(52) -0.0654(4) 0.2081(4) 0.055 Uiso 1 calc R . H44C H 0.1205(26) -0.1458(21) 0.2308(9) 0.055 Uiso 1 calc R . C45 C 0.0836(7) -0.1535(3) 0.3663(3) 0.0331(13) Uani 1 d . . H45 H 0.0378(7) -0.1976(3) 0.3531(3) 0.040 Uiso 1 calc R . C46 C 0.0480(7) -0.1406(4) 0.4337(3) 0.0373(14) Uani 1 d . . H46 H -0.0208(7) -0.1759(4) 0.4662(3) 0.045 Uiso 1 calc R . C47 C 0.1147(7) -0.0753(4) 0.4528(3) 0.0340(13) Uani 1 d . . H47 H 0.0898(7) -0.0667(4) 0.4986(3) 0.041 Uiso 1 calc R . C48 C 0.2178(7) -0.0218(3) 0.4060(3) 0.0308(13) Uani 1 d . . C49 C 0.2906(8) 0.0475(4) 0.4295(3) 0.042(2) Uani 1 d . . H49A H 0.2650(49) 0.0959(5) 0.3939(13) 0.063 Uiso 1 calc R . H49B H 0.4101(11) 0.0414(14) 0.4336(24) 0.063 Uiso 1 calc R . H49C H 0.2437(45) 0.0500(17) 0.4759(12) 0.063 Uiso 1 calc R . C52 C 1.2880(11) 0.2980(5) 0.1944(5) 0.057(2) Uani 1 d . . H52 H 1.3113(11) 0.3022(5) 0.1452(5) 0.069 Uiso 1 calc R 1 C51 C 1.1577(34) 0.2425(16) 0.2352(17) 0.054(9) Uani 0.57(3) d P 1 H51 H 1.0828(34) 0.2081(16) 0.2206(17) 0.065 Uiso 0.57(3) calc PR 1 C53 C 1.3597(17) 0.3363(10) 0.2292(12) 0.046(5) Uani 0.57(3) d P 1 H53 H 1.4411(17) 0.3747(10) 0.2112(12) 0.055 Uiso 0.57(3) calc PR 1 C54 C 1.3036(22) 0.3149(12) 0.3001(9) 0.042(6) Uani 0.57(3) d P 1 C54 H 1.3430(22) 0.3362(12) 0.3378(9) 0.051 Uiso 0.57(3) calc PR 1 C55 C 1.1882(38) 0.2609(18) 0.3073(15) 0.060(12) Uani 0.57(3) d P 1 H55 H 1.1329(38) 0.2373(18) 0.3507(15) 0.072 Uiso 0.57(3) calc PR 1 C51' C 1.1802(44) 0.2513(22) 0.2117(16) 0.030(6) Uani 0.43(3) d PU 2 H51' H 1.1365(44) 0.2257(22) 0.1776(16) 0.036 Uiso 0.43(3) calc PR 2 C53' C 1.3312(28) 0.3234(12) 0.2669(15) 0.032(6) Uani 0.43(3) d PU 2 H53' H 1.4164(28) 0.3570(12) 0.2750(15) 0.038 Uiso 0.43(3) calc PR 2 C54' C 1.2047(72) 0.2812(27) 0.3189(31) 0.068(15) Uani 0.43(3) d PU 2 H54' H 1.1873(72) 0.2856(27) 0.3666(31) 0.081 Uiso 0.43(3) calc PR 2 C55' C 1.1165(27) 0.2335(11) 0.2826(13) 0.031(5) Uani 0.43(3) d PU 2 H55' H 1.0321(27) 0.1971(11) 0.3016(13) 0.038 Uiso 0.43(3) calc PR 2 N61 N 1.0314(6) 0.4233(3) 0.1189(2) 0.0282(10) Uani 1 d . . H6 H 1.0115(6) 0.4735(3) 0.1041(2) 0.034 Uiso 1 calc R . C62 C 1.0352(7) 0.3797(3) 0.0645(3) 0.0273(12) Uani 1 d . . C63 C 0.9085(7) 0.3243(3) 0.0623(3) 0.0311(13) Uani 1 d . . C64 C 0.7530(7) 0.3203(4) 0.1075(3) 0.0364(14) Uani 1 d . . H64A H 0.7138(29) 0.3734(4) 0.1056(18) 0.055 Uiso 1 calc R . H64B H 0.7770(14) 0.2937(21) 0.1572(5) 0.055 Uiso 1 calc R . H64C H 0.6681(18) 0.2912(21) 0.0888(14) 0.055 Uiso 1 calc R . C65 C 0.9250(8) 0.2752(4) 0.0144(3) 0.0387(14) Uani 1 d . . H65 H 0.8440(8) 0.2364(4) 0.0144(3) 0.046 Uiso 1 calc R . C66 C 1.0577(9) 0.2825(4) -0.0328(3) 0.045(2) Uani 1 d . . H66 H 1.0694(9) 0.2476(4) -0.0633(3) 0.054 Uiso 1 calc R . C67 C 1.1740(9) 0.3418(4) -0.0349(3) 0.044(2) Uani 1 d . . H67 H 1.2603(9) 0.3489(4) -0.0693(3) 0.053 Uiso 1 calc R . C68 C 1.1652(7) 0.3911(3) 0.0132(3) 0.0320(13) Uani 1 d . . C69 C 1.2960(8) 0.4538(4) 0.0120(4) 0.046(2) Uani 1 d . . H69A H 1.3446(41) 0.4463(17) 0.0596(7) 0.070 Uiso 1 calc R . H69B H 1.2453(14) 0.5057(4) -0.0016(25) 0.070 Uiso 1 calc R . H69C H 1.3820(31) 0.4497(18) -0.0229(19) 0.070 Uiso 1 calc R . N71 N 0.8424(6) 0.3523(3) 0.2749(2) 0.0310(11) Uani 1 d . . H7 H 0.8014(6) 0.3092(3) 0.2668(2) 0.037 Uiso 1 calc R . C72 C 0.7391(7) 0.3881(3) 0.3188(3) 0.0277(12) Uani 1 d . . C73 C 0.6787(7) 0.4646(3) 0.2934(3) 0.0295(12) Uani 1 d . . C74 C 0.7043(8) 0.5111(4) 0.2165(3) 0.0389(14) Uani 1 d . . H74A H 0.6149(29) 0.5490(18) 0.2032(8) 0.058 Uiso 1 calc R . H74B H 0.7048(55) 0.4754(5) 0.1845(4) 0.058 Uiso 1 calc R . H74C H 0.8096(26) 0.5389(20) 0.2125(6) 0.058 Uiso 1 calc R . C75 C 0.5823(7) 0.4989(4) 0.3397(3) 0.0392(14) Uani 1 d . . H75 H 0.5398(7) 0.5501(4) 0.3227(3) 0.047 Uiso 1 calc R . C76 C 0.5492(8) 0.4578(5) 0.4101(4) 0.047(2) Uani 1 d . . H76 H 0.4872(8) 0.4814(5) 0.4413(4) 0.056 Uiso 1 calc R . C77 C 0.6081(8) 0.3820(5) 0.4340(3) 0.045(2) Uani 1 d . . H77 H 0.5843(8) 0.3544(5) 0.4817(3) 0.053 Uiso 1 calc R . C78 C 0.7017(8) 0.3448(4) 0.3900(3) 0.0364(14) Uani 1 d . . C79 C 0.7673(11) 0.2626(4) 0.4176(4) 0.062(2) Uani 1 d . . H79A H 0.8877(11) 0.2638(6) 0.4164(29) 0.094 Uiso 1 calc R . H79B H 0.7274(58) 0.2291(9) 0.3872(19) 0.094 Uiso 1 calc R . H79C H 0.7291(59) 0.2419(13) 0.4669(11) 0.094 Uiso 1 calc R . N81 N 1.1091(6) 0.4727(3) 0.2524(2) 0.0282(10) Uani 1 d . . C82 C 1.1681(7) 0.5377(3) 0.2771(3) 0.0278(12) Uani 1 d . . C83 C 1.1517(7) 0.5381(4) 0.3508(3) 0.0332(13) Uani 1 d . . C84 C 1.0746(8) 0.4689(4) 0.4037(3) 0.044(2) Uani 1 d . . H84A H 1.1294(38) 0.4206(5) 0.3996(17) 0.065 Uiso 1 calc R . H84B H 0.9574(14) 0.4658(16) 0.3931(16) 0.065 Uiso 1 calc R . H84C H 1.0872(50) 0.4757(14) 0.4525(4) 0.065 Uiso 1 calc R . C85 C 1.2116(8) 0.6035(4) 0.3737(4) 0.042(2) Uani 1 d . . H85 H 1.2015(8) 0.6045(4) 0.4226(4) 0.051 Uiso 1 calc R . C86 C 1.2852(9) 0.6665(4) 0.3258(4) 0.049(2) Uani 1 d . . H86 H 1.3238(9) 0.7100(4) 0.3422(4) 0.058 Uiso 1 calc R . C87 C 1.3018(9) 0.6653(4) 0.2536(4) 0.047(2) Uani 1 d . . H87 H 1.3528(9) 0.7081(4) 0.2213(4) 0.057 Uiso 1 calc R . C88 C 1.2440(8) 0.6015(3) 0.2280(3) 0.0369(14) Uani 1 d . . C89 C 1.2621(10) 0.5991(4) 0.1496(3) 0.047(2) Uani 1 d . . H89A H 1.3218(55) 0.6456(15) 0.1236(7) 0.071 Uiso 1 calc R . H89B H 1.1529(10) 0.5979(29) 0.1287(8) 0.071 Uiso 1 calc R . H89C H 1.3232(53) 0.5521(16) 0.1463(4) 0.071 Uiso 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 0.0219(3) 0.0195(2) 0.0211(2) -0.0047(2) -0.0008(2) 0.0003(2) Nb2 0.0274(3) 0.0236(3) 0.0279(3) -0.0071(2) -0.0027(2) 0.0037(2) C11 0.030(3) 0.042(4) 0.052(4) -0.020(3) 0.005(3) -0.009(3) C12 0.047(4) 0.035(3) 0.035(3) 0.004(3) -0.003(3) -0.019(3) C13 0.045(4) 0.022(3) 0.050(4) -0.008(3) -0.008(3) -0.008(3) C14 0.041(4) 0.043(3) 0.032(3) -0.019(3) 0.001(3) -0.021(3) C15 0.033(4) 0.031(3) 0.048(4) -0.006(3) -0.013(3) -0.006(3) N21 0.034(3) 0.024(2) 0.025(2) -0.008(2) -0.004(2) -0.003(2) C22 0.039(4) 0.034(3) 0.027(3) -0.008(2) -0.006(3) -0.010(3) C23 0.040(4) 0.043(3) 0.027(3) -0.011(3) 0.001(3) -0.015(3) C24 0.044(4) 0.051(4) 0.038(3) -0.016(3) 0.015(3) -0.012(3) C25 0.047(4) 0.061(4) 0.026(3) -0.008(3) 0.001(3) -0.022(4) C26 0.050(4) 0.052(4) 0.032(3) 0.002(3) -0.011(3) -0.016(3) C27 0.055(5) 0.040(4) 0.046(4) -0.002(3) -0.029(3) 0.001(3) C28 0.048(4) 0.039(3) 0.033(3) -0.006(3) -0.015(3) 0.003(3) C29 0.074(6) 0.059(5) 0.051(4) -0.015(4) -0.021(4) 0.032(4) N31 0.019(2) 0.027(2) 0.021(2) -0.005(2) -0.001(2) -0.001(2) C32 0.020(3) 0.019(2) 0.029(3) -0.004(2) -0.004(2) -0.005(2) C33 0.030(3) 0.025(3) 0.037(3) -0.010(2) -0.002(3) 0.000(2) C34 0.055(4) 0.041(4) 0.039(4) -0.015(3) 0.002(3) 0.013(3) C35 0.047(4) 0.028(3) 0.049(4) -0.013(3) -0.006(3) 0.009(3) C36 0.051(4) 0.021(3) 0.051(4) 0.000(3) -0.006(3) 0.006(3) C37 0.033(3) 0.030(3) 0.038(3) 0.003(3) -0.003(3) -0.003(3) C38 0.024(3) 0.024(3) 0.029(3) -0.005(2) -0.003(2) -0.003(2) C39 0.041(4) 0.040(3) 0.028(3) -0.005(3) 0.001(3) 0.003(3) N41 0.028(3) 0.022(2) 0.031(2) -0.007(2) 0.001(2) 0.003(2) C42 0.019(3) 0.027(3) 0.027(3) -0.006(2) -0.003(2) 0.005(2) C43 0.017(3) 0.031(3) 0.034(3) -0.008(2) -0.007(2) 0.011(2) C44 0.038(4) 0.037(3) 0.041(3) -0.022(3) -0.004(3) -0.003(3) C45 0.023(3) 0.031(3) 0.044(3) -0.005(3) -0.008(3) -0.001(2) C46 0.022(3) 0.048(4) 0.035(3) 0.005(3) -0.004(3) 0.004(3) C47 0.024(3) 0.052(4) 0.025(3) -0.009(3) -0.002(2) 0.010(3) C48 0.022(3) 0.044(3) 0.030(3) -0.014(3) -0.005(2) 0.008(3) C49 0.043(4) 0.052(4) 0.038(3) -0.024(3) 0.003(3) 0.005(3) C52 0.048(5) 0.059(5) 0.063(5) -0.012(4) 0.013(4) 0.021(4) C51 0.039(11) 0.020(8) 0.100(26) -0.007(15) 0.018(15) -0.006(6) C53 0.032(7) 0.060(9) 0.051(11) -0.022(9) 0.007(7) 0.007(6) C54 0.035(9) 0.075(12) 0.021(8) -0.021(8) -0.013(7) 0.038(8) C55 0.061(19) 0.057(19) 0.042(14) 0.027(16) 0.019(13) 0.045(16) C51' 0.028(10) 0.029(10) 0.036(9) -0.012(8) 0.006(7) 0.006(8) C53' 0.028(8) 0.036(7) 0.030(10) -0.004(8) -0.009(8) -0.002(6) C54' 0.069(17) 0.065(17) 0.070(16) -0.018(9) 0.000(9) 0.003(9) C55' 0.034(8) 0.022(7) 0.036(8) -0.003(6) 0.002(7) 0.007(6) N61 0.032(3) 0.021(2) 0.030(2) -0.004(2) 0.000(2) -0.003(2) C62 0.029(3) 0.030(3) 0.021(3) -0.003(2) -0.004(2) 0.004(2) C63 0.032(3) 0.034(3) 0.026(3) -0.004(2) -0.008(2) 0.001(3) C64 0.028(3) 0.040(3) 0.041(3) -0.011(3) 0.001(3) -0.008(3) C65 0.047(4) 0.041(3) 0.029(3) -0.008(3) -0.010(3) -0.002(3) C66 0.057(4) 0.049(4) 0.034(3) -0.022(3) -0.004(3) 0.007(3) C67 0.045(4) 0.063(4) 0.024(3) -0.008(3) 0.007(3) 0.008(3) C68 0.028(3) 0.037(3) 0.029(3) -0.003(2) -0.001(2) 0.002(2) C69 0.036(4) 0.052(4) 0.045(4) -0.001(3) 0.009(3) -0.006(3) N71 0.038(3) 0.024(2) 0.031(2) -0.005(2) 0.001(2) -0.002(2) C72 0.024(3) 0.032(3) 0.025(3) -0.003(2) 0.001(2) -0.008(2) C73 0.022(3) 0.034(3) 0.031(3) -0.003(2) -0.004(2) 0.000(2) C74 0.038(4) 0.035(3) 0.037(3) 0.005(3) -0.002(3) 0.012(3) C75 0.025(3) 0.050(4) 0.045(4) -0.017(3) -0.002(3) 0.009(3) C76 0.027(3) 0.081(5) 0.038(4) -0.027(4) 0.006(3) 0.002(3) C77 0.030(4) 0.077(5) 0.024(3) -0.007(3) -0.002(3) -0.006(3) C78 0.030(3) 0.047(4) 0.027(3) 0.001(3) -0.004(3) -0.008(3) C79 0.072(6) 0.055(4) 0.044(4) 0.020(3) 0.011(4) 0.006(4) N81 0.022(2) 0.033(2) 0.030(2) -0.007(2) -0.002(2) 0.003(2) C82 0.026(3) 0.026(3) 0.034(3) -0.009(2) -0.005(2) 0.005(2) C83 0.021(3) 0.043(3) 0.040(3) -0.017(3) -0.009(2) 0.006(3) C84 0.042(4) 0.058(4) 0.036(3) -0.022(3) 0.001(3) -0.001(3) C85 0.037(4) 0.048(4) 0.050(4) -0.028(3) -0.007(3) 0.007(3) C86 0.049(4) 0.037(4) 0.070(5) -0.031(3) -0.013(4) 0.006(3) C87 0.049(4) 0.025(3) 0.065(5) -0.005(3) -0.011(3) -0.001(3) C88 0.041(4) 0.024(3) 0.045(4) -0.006(3) -0.014(3) 0.008(3) C89 0.062(5) 0.037(3) 0.040(4) -0.001(3) -0.009(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N31 1.775(5) . ? Nb1 N21 2.014(4) . ? Nb1 N41 2.022(5) . ? Nb1 C15 2.413(6) . ? Nb1 C11 2.425(6) . ? Nb1 C14 2.457(5) . ? Nb1 C12 2.502(6) . ? Nb1 C13 2.523(6) . ? Nb2 N81 1.763(5) . ? Nb2 N71 2.008(5) . ? Nb2 N61 2.023(5) . ? Nb2 C53' 2.38(2) . ? Nb2 C54' 2.41(5) . ? Nb2 C52 2.454(7) . ? Nb2 C54 2.461(14) . ? Nb2 C53 2.461(14) . ? Nb2 C55 2.47(2) . ? Nb2 C51 2.49(3) . ? Nb2 C51' 2.52(4) . ? Nb2 C55' 2.56(2) . ? C11 C15 1.377(9) . ? C11 C12 1.381(9) . ? C11 H11 0.93 . ? C12 C13 1.378(9) . ? C12 H12 0.93 . ? C13 C14 1.396(9) . ? C13 H13 0.93 . ? C14 C15 1.392(9) . ? C14 H14 0.93 . ? C15 H15 0.93 . ? N21 C22 1.402(7) . ? N21 H2 0.86 . ? C22 C28 1.384(9) . ? C22 C23 1.410(8) . ? C23 C25 1.377(9) . ? C23 C24 1.478(9) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 C26 1.357(10) . ? C25 H25 0.93 . ? C26 C27 1.362(10) . ? C26 H26 0.93 . ? C27 C28 1.391(9) . ? C27 H27 0.93 . ? C28 C29 1.488(10) . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? N31 C32 1.391(7) . ? C32 C38 1.385(7) . ? C32 C33 1.404(7) . ? C33 C35 1.375(8) . ? C33 C34 1.490(8) . ? C34 H34A 0.96 . ? C34 H34B 0.96 . ? C34 H34C 0.96 . ? C35 C36 1.367(9) . ? C35 H35 0.93 . ? C36 C37 1.368(9) . ? C36 H36 0.93 . ? C37 C38 1.388(8) . ? C37 H37 0.93 . ? C38 C39 1.489(8) . ? C39 H39A 0.96 . ? C39 H39B 0.96 . ? C39 H39C 0.96 . ? N41 C42 1.402(7) . ? N41 H4 0.86 . ? C42 C43 1.397(7) . ? C42 C48 1.400(7) . ? C43 C45 1.376(8) . ? C43 C44 1.494(8) . ? C44 H44A 0.96 . ? C44 H44B 0.96 . ? C44 H44C 0.96 . ? C45 C46 1.367(8) . ? C45 H45 0.93 . ? C46 C47 1.371(9) . ? C46 H46 0.93 . ? C47 C48 1.381(8) . ? C47 H47 0.93 . ? C48 C49 1.489(8) . ? C49 H49A 0.96 . ? C49 H49B 0.96 . ? C49 H49C 0.96 . ? C52 C51' 1.17(4) . ? C52 C53 1.18(2) . ? C52 C51 1.49(3) . ? C52 C53' 1.57(2) . ? C52 H52 0.93 . ? C51 C55 1.49(4) . ? C51 H51 0.93 . ? C53 C54 1.37(2) . ? C53 H53 0.93 . ? C54 C55 1.29(4) . ? C54 H54 0.93 . ? C55 H55 0.93 . ? C51' C55' 1.39(3) . ? C51' H51' 0.93 . ? C53' C54' 1.47(6) . ? C53' H53' 0.93 . ? C54' C55' 1.38(6) . ? C54' H54' 0.93 . ? C55' H55' 0.93 . ? N61 C62 1.407(7) . ? N61 H6 0.86 . ? C62 C68 1.394(8) . ? C62 C63 1.398(8) . ? C63 C65 1.383(8) . ? C63 C64 1.490(8) . ? C64 H64A 0.96 . ? C64 H64B 0.96 . ? C64 H64C 0.96 . ? C65 C66 1.363(9) . ? C65 H65 0.93 . ? C66 C67 1.373(9) . ? C66 H66 0.93 . ? C67 C68 1.384(8) . ? C67 H67 0.93 . ? C68 C69 1.499(8) . ? C69 H69A 0.96 . ? C69 H69B 0.96 . ? C69 H69C 0.96 . ? N71 C72 1.405(7) . ? N71 H7 0.86 . ? C72 C73 1.380(8) . ? C72 C78 1.403(8) . ? C73 C75 1.392(8) . ? C73 C74 1.492(8) . ? C74 H74A 0.96 . ? C74 H74B 0.96 . ? C74 H74C 0.96 . ? C75 C76 1.372(9) . ? C75 H75 0.93 . ? C76 C77 1.361(10) . ? C76 H76 0.93 . ? C77 C78 1.377(9) . ? C77 H77 0.93 . ? C78 C79 1.485(9) . ? C79 H79A 0.96 . ? C79 H79B 0.96 . ? C79 H79C 0.96 . ? N81 C82 1.395(7) . ? C82 C88 1.392(8) . ? C82 C83 1.397(8) . ? C83 C85 1.385(8) . ? C83 C84 1.490(9) . ? C84 H84A 0.96 . ? C84 H84B 0.96 . ? C84 H84C 0.96 . ? C85 C86 1.366(10) . ? C85 H85 0.93 . ? C86 C87 1.371(10) . ? C86 H86 0.93 . ? C87 C88 1.383(8) . ? C87 H87 0.93 . ? C88 C89 1.494(9) . ? C89 H89A 0.96 . ? C89 H89B 0.96 . ? C89 H89C 0.96 . ? 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 N31 Nb1 N21 99.4(2) . . ? N31 Nb1 N41 101.3(2) . . ? N21 Nb1 N41 109.4(2) . . ? N31 Nb1 C15 92.7(2) . . ? N21 Nb1 C15 128.3(2) . . ? N41 Nb1 C15 117.1(2) . . ? N31 Nb1 C11 105.1(2) . . ? N21 Nb1 C11 95.5(2) . . ? N41 Nb1 C11 139.9(2) . . ? C15 Nb1 C11 33.1(2) . . ? N31 Nb1 C14 114.4(2) . . ? N21 Nb1 C14 138.6(2) . . ? N41 Nb1 C14 87.4(2) . . ? C15 Nb1 C14 33.2(2) . . ? C11 Nb1 C14 54.3(2) . . ? N31 Nb1 C12 137.4(2) . . ? N21 Nb1 C12 85.6(2) . . ? N41 Nb1 C12 117.0(2) . . ? C15 Nb1 C12 54.3(2) . . ? C11 Nb1 C12 32.5(2) . . ? C14 Nb1 C12 53.5(2) . . ? N31 Nb1 C13 145.9(2) . . ? N21 Nb1 C13 108.3(2) . . ? N41 Nb1 C13 88.0(2) . . ? C15 Nb1 C13 54.5(2) . . ? C11 Nb1 C13 53.8(2) . . ? C14 Nb1 C13 32.5(2) . . ? C12 Nb1 C13 31.8(2) . . ? N81 Nb2 N71 101.7(2) . . ? N81 Nb2 N61 100.3(2) . . ? N71 Nb2 N61 108.1(2) . . ? N81 Nb2 C53' 94.9(5) . . ? N71 Nb2 C53' 127.0(6) . . ? N61 Nb2 C53' 117.8(7) . . ? N81 Nb2 C54' 104.9(13) . . ? N71 Nb2 C54' 91.4(14) . . ? N61 Nb2 C54' 144.1(13) . . ? C53' Nb2 C54' 35.6(14) . . ? N81 Nb2 C52 123.0(3) . . ? N71 Nb2 C52 130.0(3) . . ? N61 Nb2 C52 86.2(2) . . ? C53' Nb2 C52 37.9(6) . . ? C54' Nb2 C52 58.7(14) . . ? N81 Nb2 C54 92.0(5) . . ? N71 Nb2 C54 113.5(5) . . ? N61 Nb2 C54 133.0(4) . . ? C52 Nb2 C54 50.2(4) . . ? N81 Nb2 C53 96.8(4) . . ? N71 Nb2 C53 142.0(5) . . ? N61 Nb2 C53 100.7(5) . . ? C52 Nb2 C53 27.9(4) . . ? C54 Nb2 C53 32.4(5) . . ? N81 Nb2 C55 116.0(10) . . ? N71 Nb2 C55 89.3(7) . . ? N61 Nb2 C55 135.7(8) . . ? C52 Nb2 C55 53.4(7) . . ? C54 Nb2 C55 30.4(9) . . ? C53 Nb2 C55 52.7(8) . . ? N81 Nb2 C51 146.5(7) . . ? N71 Nb2 C51 95.0(6) . . ? N61 Nb2 C51 101.7(7) . . ? C52 Nb2 C51 35.1(6) . . ? C54 Nb2 C51 54.6(8) . . ? C53 Nb2 C51 54.5(7) . . ? C55 Nb2 C51 34.9(10) . . ? N81 Nb2 C51' 147.0(9) . . ? N71 Nb2 C51' 103.1(8) . . ? N61 Nb2 C51' 92.3(7) . . ? C53' Nb2 C51' 52.5(10) . . ? C54' Nb2 C51' 53.3(14) . . ? C52 Nb2 C51' 27.2(8) . . ? N81 Nb2 C55' 136.6(5) . . ? N71 Nb2 C55' 80.3(5) . . ? N61 Nb2 C55' 120.5(5) . . ? C53' Nb2 C55' 54.8(7) . . ? C54' Nb2 C55' 32.1(13) . . ? C52 Nb2 C55' 52.7(5) . . ? C51' Nb2 C55' 31.8(7) . . ? C15 C11 C12 108.8(6) . . ? C15 C11 Nb1 73.0(3) . . ? C12 C11 Nb1 76.8(4) . . ? C15 C11 H11 125.6(4) . . ? C12 C11 H11 125.6(4) . . ? Nb1 C11 H11 116.6(2) . . ? C13 C12 C11 108.5(6) . . ? C13 C12 Nb1 74.9(3) . . ? C11 C12 Nb1 70.7(3) . . ? C13 C12 H12 125.8(4) . . ? C11 C12 H12 125.8(4) . . ? Nb1 C12 H12 120.36(15) . . ? C12 C13 C14 107.2(6) . . ? C12 C13 Nb1 73.2(3) . . ? C14 C13 Nb1 71.1(3) . . ? C12 C13 H13 126.4(4) . . ? C14 C13 H13 126.4(4) . . ? Nb1 C13 H13 121.0(2) . . ? C15 C14 C13 108.4(6) . . ? C15 C14 Nb1 71.7(3) . . ? C13 C14 Nb1 76.3(3) . . ? C15 C14 H14 125.8(4) . . ? C13 C14 H14 125.8(4) . . ? Nb1 C14 H14 118.12(15) . . ? C11 C15 C14 107.1(6) . . ? C11 C15 Nb1 73.9(3) . . ? C14 C15 Nb1 75.1(3) . . ? C11 C15 H15 126.4(4) . . ? C14 C15 H15 126.4(4) . . ? Nb1 C15 H15 116.7(2) . . ? C22 N21 Nb1 135.8(4) . . ? C22 N21 H2 112.1(3) . . ? Nb1 N21 H2 112.10(13) . . ? C28 C22 N21 121.0(6) . . ? C28 C22 C23 120.6(6) . . ? N21 C22 C23 118.4(6) . . ? C25 C23 C22 117.7(6) . . ? C25 C23 C24 121.2(6) . . ? C22 C23 C24 121.0(5) . . ? C23 C24 H24A 109.5(3) . . ? C23 C24 H24B 109.5(3) . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5(3) . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C23 122.1(7) . . ? C26 C25 H25 118.9(4) . . ? C23 C25 H25 118.9(4) . . ? C25 C26 C27 119.8(6) . . ? C25 C26 H26 120.1(4) . . ? C27 C26 H26 120.1(4) . . ? C26 C27 C28 121.1(7) . . ? C26 C27 H27 119.4(4) . . ? C28 C27 H27 119.4(4) . . ? C22 C28 C27 118.5(6) . . ? C22 C28 C29 120.7(6) . . ? C27 C28 C29 120.6(6) . . ? C28 C29 H29A 109.5(4) . . ? C28 C29 H29B 109.5(4) . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5(4) . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 N31 Nb1 168.5(4) . . ? C38 C32 N31 120.2(5) . . ? C38 C32 C33 119.9(5) . . ? N31 C32 C33 119.9(5) . . ? C35 C33 C32 119.7(5) . . ? C35 C33 C34 120.1(5) . . ? C32 C33 C34 120.2(5) . . ? C33 C34 H34A 109.5(3) . . ? C33 C34 H34B 109.5(4) . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5(3) . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C33 120.3(6) . . ? C36 C35 H35 119.8(4) . . ? C33 C35 H35 119.8(4) . . ? C35 C36 C37 120.1(6) . . ? C35 C36 H36 119.9(4) . . ? C37 C36 H36 119.9(4) . . ? C36 C37 C38 121.4(6) . . ? C36 C37 H37 119.3(4) . . ? C38 C37 H37 119.3(3) . . ? C32 C38 C37 118.6(5) . . ? C32 C38 C39 120.2(5) . . ? C37 C38 C39 121.3(5) . . ? C38 C39 H39A 109.5(3) . . ? C38 C39 H39B 109.5(3) . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5(3) . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 N41 Nb1 131.3(3) . . ? C42 N41 H4 114.4(3) . . ? Nb1 N41 H4 114.36(13) . . ? C43 C42 C48 120.0(5) . . ? C43 C42 N41 121.1(5) . . ? C48 C42 N41 118.8(5) . . ? C45 C43 C42 119.3(5) . . ? C45 C43 C44 119.3(5) . . ? C42 C43 C44 121.4(5) . . ? C43 C44 H44A 109.5(3) . . ? C43 C44 H44B 109.5(3) . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5(3) . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C43 121.2(5) . . ? C46 C45 H45 119.4(4) . . ? C43 C45 H45 119.4(3) . . ? C45 C46 C47 119.4(5) . . ? C45 C46 H46 120.3(4) . . ? C47 C46 H46 120.3(3) . . ? C46 C47 C48 121.9(5) . . ? C46 C47 H47 119.0(3) . . ? C48 C47 H47 119.0(3) . . ? C47 C48 C42 118.2(5) . . ? C47 C48 C49 120.2(5) . . ? C42 C48 C49 121.5(5) . . ? C48 C49 H49A 109.5(4) . . ? C48 C49 H49B 109.5(3) . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5(3) . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C53 C52 C51 115.2(15) . . ? C51' C52 C53' 103.8(18) . . ? C51' C52 Nb2 79.4(18) . . ? C53 C52 Nb2 76.4(7) . . ? C51 C52 Nb2 73.7(11) . . ? C53' C52 Nb2 68.6(8) . . ? C53 C52 H52 122.4(11) . . ? C51 C52 H52 122.4(13) . . ? Nb2 C52 H52 118.7(2) . . ? C55 C51 C52 95.9(20) . . ? C55 C51 Nb2 71.8(13) . . ? C52 C51 Nb2 71.1(10) . . ? C55 C51 H51 132.1(17) . . ? C52 C51 H51 132.1(13) . . ? Nb2 C51 H51 118.3(7) . . ? C52 C53 C54 109.1(16) . . ? C52 C53 Nb2 75.7(8) . . ? C54 C53 Nb2 73.8(8) . . ? C52 C53 H53 125.5(11) . . ? C54 C53 H53 125.5(12) . . ? Nb2 C53 H53 117.0(4) . . ? C55 C54 C53 110.4(19) . . ? C55 C54 Nb2 75.2(11) . . ? C53 C54 Nb2 73.8(9) . . ? C55 C54 H54 124.8(16) . . ? C53 C54 H54 124.8(12) . . ? Nb2 C54 H54 117.9(4) . . ? C54 C55 C51 109.3(19) . . ? C54 C55 Nb2 74.4(11) . . ? C51 C55 Nb2 73.2(13) . . ? C54 C55 H55 125.4(16) . . ? C51 C55 H55 125.4(17) . . ? Nb2 C55 H55 118.8(6) . . ? C52 C51' C55' 120.7(32) . . ? C52 C51' Nb2 73.5(18) . . ? C55' C51' Nb2 75.9(18) . . ? C52 C51' H51' 119.6(16) . . ? C55' C51' H51' 119.6(20) . . ? Nb2 C51' H51' 122.2(8) . . ? C54' C53' C52 103.3(24) . . ? C54' C53' Nb2 73.2(21) . . ? C52 C53' Nb2 73.5(8) . . ? C54' C53' H53' 128.3(24) . . ? C52 C53' H53' 128.3(10) . . ? Nb2 C53' H53' 117.5(5) . . ? C55' C54' C53' 106.1(41) . . ? C55' C54' Nb2 80.0(24) . . ? C53' C54' Nb2 71.2(20) . . ? C55' C54' H54' 126.9(28) . . ? C53' C54' H54' 126.9(24) . . ? Nb2 C54' H54' 114.4(13) . . ? C54' C55' C51' 105.7(33) . . ? C54' C55' Nb2 67.9(22) . . ? C51' C55' Nb2 72.3(19) . . ? C54' C55' H55' 127.1(28) . . ? C51' C55' H55' 127.2(20) . . ? Nb2 C55' H55' 124.3(5) . . ? C62 N61 Nb2 128.0(3) . . ? C62 N61 H6 116.0(3) . . ? Nb2 N61 H6 116.00(14) . . ? C68 C62 C63 119.9(5) . . ? C68 C62 N61 120.3(5) . . ? C63 C62 N61 119.8(5) . . ? C65 C63 C62 118.9(6) . . ? C65 C63 C64 119.7(5) . . ? C62 C63 C64 121.3(5) . . ? C63 C64 H64A 109.5(3) . . ? C63 C64 H64B 109.5(3) . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5(3) . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 C63 121.3(6) . . ? C66 C65 H65 119.4(4) . . ? C63 C65 H65 119.4(4) . . ? C65 C66 C67 119.5(6) . . ? C65 C66 H66 120.2(4) . . ? C67 C66 H66 120.2(4) . . ? C66 C67 C68 121.3(6) . . ? C66 C67 H67 119.4(4) . . ? C68 C67 H67 119.4(4) . . ? C67 C68 C62 118.7(5) . . ? C67 C68 C69 120.8(6) . . ? C62 C68 C69 120.4(5) . . ? C68 C69 H69A 109.5(3) . . ? C68 C69 H69B 109.5(4) . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5(3) . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C72 N71 Nb2 132.5(4) . . ? C72 N71 H7 113.7(3) . . ? Nb2 N71 H7 113.75(14) . . ? C73 C72 C78 120.5(5) . . ? C73 C72 N71 121.2(5) . . ? C78 C72 N71 118.3(5) . . ? C72 C73 C75 119.2(5) . . ? C72 C73 C74 122.7(5) . . ? C75 C73 C74 118.0(5) . . ? C73 C74 H74A 109.5(3) . . ? C73 C74 H74B 109.5(3) . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5(3) . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 C73 120.7(6) . . ? C76 C75 H75 119.7(4) . . ? C73 C75 H75 119.7(4) . . ? C77 C76 C75 119.3(6) . . ? C77 C76 H76 120.3(4) . . ? C75 C76 H76 120.3(4) . . ? C76 C77 C78 122.4(6) . . ? C76 C77 H77 118.8(4) . . ? C78 C77 H77 118.8(4) . . ? C77 C78 C72 117.9(6) . . ? C77 C78 C79 121.5(6) . . ? C72 C78 C79 120.6(6) . . ? C78 C79 H79A 109.5(4) . . ? C78 C79 H79B 109.5(4) . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5(4) . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C82 N81 Nb2 170.0(4) . . ? C88 C82 N81 119.7(5) . . ? C88 C82 C83 120.5(5) . . ? N81 C82 C83 119.7(5) . . ? C85 C83 C82 118.4(6) . . ? C85 C83 C84 121.0(6) . . ? C82 C83 C84 120.6(5) . . ? C83 C84 H84A 109.5(3) . . ? C83 C84 H84B 109.5(3) . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5(3) . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C85 C83 121.4(6) . . ? C86 C85 H85 119.3(4) . . ? C83 C85 H85 119.3(4) . . ? C85 C86 C87 119.8(6) . . ? C85 C86 H86 120.1(4) . . ? C87 C86 H86 120.1(4) . . ? C86 C87 C88 121.1(6) . . ? C86 C87 H87 119.5(4) . . ? C88 C87 H87 119.5(4) . . ? C87 C88 C82 118.8(6) . . ? C87 C88 C89 121.7(6) . . ? C82 C88 C89 119.4(5) . . ? C88 C89 H89A 109.5(3) . . ? C88 C89 H89B 109.5(4) . . ? H89A C89 H89B 109.5 . . ? C88 C89 H89C 109.5(3) . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? _refine_diff_density_max 0.392 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.073 #=END data_structure7 _audit_creation_method SHELXL _chemical_formula_sum 'C22 H27 N2 Nb' _chemical_formula_weight 412.37 _chemical_melting_point ? _chemical_compound_source ? 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 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.490(2) _cell_length_b 24.276(5) _cell_length_c 10.274(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.29(3) _cell_angle_gamma 90.00 _cell_volume 2010.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.38 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7154 _exptl_absorpt_correction_T_max 0.9513 _diffrn_ambient_temperature 150(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 'Enraf-Nonius DIP2000' _diffrn_measurement_method \w _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18234 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.38 _reflns_number_total 4150 _reflns_number_observed 2444 _reflns_observed_criterion 2sigma(I) _computing_data_collection 'DIP2000 Software XPRESS (Mac Science)' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO & SCALEPACK' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin & Pearce, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.1972P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 2444 _refine_ls_number_parameters 232 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_obs 0.0553 _refine_ls_wR_factor_all 0.1178 _refine_ls_wR_factor_obs 0.1178 _refine_ls_goodness_of_fit_all 1.392 _refine_ls_goodness_of_fit_obs 1.392 _refine_ls_restrained_S_all 1.392 _refine_ls_restrained_S_obs 1.392 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nb1 Nb 0.27625(8) -0.12937(3) 0.41916(7) 0.0358(2) Uani 1 d . . N1 N 0.3715(7) -0.0555(2) 0.4076(6) 0.0384(14) Uani 1 d D . H1 H 0.4360(22) -0.0423(5) 0.4935(28) 0.046 Uiso 1 calc RD . N2 N 0.1519(7) -0.1413(2) 0.2478(6) 0.0375(14) Uani 1 d . . C1 C 0.0842(11) -0.1157(4) 0.5177(9) 0.067(3) Uani 1 d . . H1A H 0.1347(15) -0.1019(25) 0.6088(26) 0.101 Uiso 1 calc R . H1B H 0.0291(54) -0.1499(7) 0.5220(60) 0.101 Uiso 1 calc R . H1C H 0.0049(46) -0.0895(21) 0.4654(38) 0.101 Uiso 1 calc R . C11 C 0.3653(8) -0.0180(3) 0.3010(7) 0.034(2) Uani 1 d . . C12 C 0.5120(8) -0.0073(3) 0.2684(8) 0.043(2) Uani 1 d . . C13 C 0.6697(9) -0.0372(4) 0.3442(9) 0.055(2) Uani 1 d . . H13A H 0.6526(23) -0.0762(4) 0.3317(49) 0.082 Uiso 1 calc R . H13B H 0.7000(40) -0.0286(19) 0.4401(13) 0.082 Uiso 1 calc R . H13C H 0.7569(20) -0.0259(18) 0.3091(41) 0.082 Uiso 1 calc R . C14 C 0.5056(10) 0.0283(3) 0.1628(9) 0.053(2) Uani 1 d . . H14 H 0.6020(10) 0.0356(3) 0.1411(9) 0.064 Uiso 1 calc R . C15 C 0.3601(11) 0.0532(3) 0.0886(9) 0.056(2) Uani 1 d . . H15 H 0.3580(11) 0.0769(3) 0.0170(9) 0.067 Uiso 1 calc R . C16 C 0.2189(10) 0.0430(3) 0.1204(8) 0.045(2) Uani 1 d . . H16 H 0.1211(10) 0.0604(3) 0.0702(8) 0.054 Uiso 1 calc R . C17 C 0.2167(8) 0.0076(3) 0.2249(7) 0.034(2) Uani 1 d . . C18 C 0.0581(9) -0.0021(3) 0.2567(8) 0.049(2) Uani 1 d . . H18A H 0.0808(13) -0.0035(22) 0.3543(8) 0.074 Uiso 1 calc R . H18B H 0.0100(35) -0.0363(11) 0.2168(46) 0.074 Uiso 1 calc R . H18C H -0.0179(26) 0.0275(12) 0.2194(47) 0.074 Uiso 1 calc R . C21 C 0.0735(9) -0.1576(3) 0.1127(7) 0.037(2) Uani 1 d . . C22 C -0.0904(9) -0.1769(3) 0.0755(9) 0.049(2) Uani 1 d . . C23 C -0.1798(10) -0.1798(4) 0.1779(11) 0.070(3) Uani 1 d . . H23A H -0.2794(42) -0.2010(23) 0.1415(28) 0.106 Uiso 1 calc R . H23B H -0.2079(71) -0.1433(4) 0.1988(50) 0.106 Uiso 1 calc R . H23C H -0.1102(32) -0.1970(24) 0.2600(26) 0.106 Uiso 1 calc R . C24 C -0.1637(12) -0.1922(4) -0.0624(11) 0.069(3) Uani 1 d . . H24 H -0.2712(12) -0.2060(4) -0.0900(11) 0.083 Uiso 1 calc R . C25 C -0.0819(14) -0.1874(4) -0.1567(10) 0.074(3) Uani 1 d . . H25 H -0.1337(14) -0.1979(4) -0.2471(10) 0.089 Uiso 1 calc R . C26 C 0.0764(12) -0.1671(3) -0.1185(9) 0.060(2) Uani 1 d . . H26 H 0.1303(12) -0.1634(3) -0.1840(9) 0.072 Uiso 1 calc R . C27 C 0.1578(10) -0.1520(3) 0.0151(8) 0.045(2) Uani 1 d . . C28 C 0.3329(11) -0.1312(4) 0.0567(9) 0.065(2) Uani 1 d . . H28A H 0.4023(18) -0.1548(16) 0.1263(48) 0.097 Uiso 1 calc R . H28B H 0.3367(17) -0.0944(11) 0.0918(62) 0.097 Uiso 1 calc R . H28C H 0.3719(29) -0.1311(25) -0.0215(17) 0.097 Uiso 1 calc R . C31 C 0.4316(14) -0.1720(4) 0.6444(10) 0.073(3) Uani 1 d . . H31 H 0.4182(14) -0.1587(4) 0.7251(10) 0.088 Uiso 1 calc R . C32 C 0.5467(12) -0.1545(4) 0.5895(14) 0.085(4) Uani 1 d . . H32 H 0.6273(12) -0.1280(4) 0.6266(14) 0.102 Uiso 1 calc R . C33 C 0.5236(15) -0.1837(5) 0.4640(14) 0.091(4) Uani 1 d . . H33 H 0.5820(15) -0.1790(5) 0.4019(14) 0.109 Uiso 1 calc R . C34 C 0.3945(15) -0.2205(4) 0.4547(11) 0.077(3) Uani 1 d . . H34 H 0.3536(15) -0.2465(4) 0.3857(11) 0.093 Uiso 1 calc R . C35 C 0.3376(13) -0.2121(4) 0.5647(11) 0.072(3) Uani 1 d . . H35 H 0.2501(13) -0.2307(4) 0.5816(11) 0.086 Uiso 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 0.0340(3) 0.0399(3) 0.0299(3) 0.0029(4) 0.0049(2) 0.0025(4) N1 0.037(3) 0.041(3) 0.031(3) -0.010(3) 0.001(3) 0.001(3) N2 0.035(3) 0.037(4) 0.036(3) 0.001(3) 0.005(3) -0.004(3) C1 0.070(6) 0.084(7) 0.055(6) 0.016(5) 0.029(5) 0.017(5) C11 0.036(4) 0.029(3) 0.034(4) -0.004(3) 0.008(3) -0.002(3) C12 0.031(4) 0.040(4) 0.056(5) -0.012(4) 0.010(3) -0.004(3) C13 0.036(4) 0.066(5) 0.063(6) -0.017(5) 0.017(4) 0.003(4) C14 0.047(5) 0.049(5) 0.066(6) -0.001(4) 0.022(4) -0.004(4) C15 0.066(6) 0.043(5) 0.059(6) 0.005(4) 0.021(5) -0.006(4) C16 0.049(5) 0.042(4) 0.042(5) 0.004(3) 0.012(4) 0.006(4) C17 0.032(4) 0.034(4) 0.034(4) -0.005(3) 0.008(3) 0.003(3) C18 0.034(4) 0.057(5) 0.052(5) 0.005(4) 0.007(4) 0.010(4) C21 0.042(4) 0.021(3) 0.037(4) 0.003(3) -0.003(3) 0.003(3) C22 0.040(4) 0.033(4) 0.058(6) 0.006(4) -0.004(4) 0.002(3) C23 0.041(5) 0.061(6) 0.097(8) 0.021(5) 0.004(5) -0.008(4) C24 0.053(5) 0.048(5) 0.076(8) -0.004(5) -0.023(5) -0.003(4) C25 0.091(8) 0.054(6) 0.049(6) -0.009(5) -0.021(6) 0.017(5) C26 0.082(7) 0.045(5) 0.044(5) -0.004(4) 0.005(5) 0.013(5) C27 0.058(5) 0.039(4) 0.032(4) -0.003(3) 0.004(4) 0.006(4) C28 0.076(6) 0.069(6) 0.059(6) -0.015(5) 0.037(5) -0.012(6) C31 0.090(8) 0.072(7) 0.042(6) 0.018(5) -0.003(5) 0.017(6) C32 0.048(6) 0.066(6) 0.109(10) 0.027(7) -0.021(6) 0.001(5) C33 0.076(8) 0.099(9) 0.110(11) 0.065(8) 0.048(7) 0.060(7) C34 0.101(9) 0.058(6) 0.055(7) -0.003(5) -0.001(6) 0.032(6) C35 0.078(7) 0.050(6) 0.078(8) 0.019(5) 0.010(6) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N2 1.770(6) . ? Nb1 N1 1.987(6) . ? Nb1 C1 2.197(8) . ? Nb1 C33 2.398(9) . ? Nb1 C34 2.410(9) . ? Nb1 C35 2.461(9) . ? Nb1 C32 2.487(9) . ? Nb1 C31 2.500(9) . ? N1 C11 1.412(9) . ? N1 H1 0.94(3) . ? N2 C21 1.395(9) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C11 C17 1.404(9) . ? C11 C12 1.411(10) . ? C12 C14 1.374(11) . ? C12 C13 1.508(10) . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C14 C15 1.371(11) . ? C14 H14 0.93 . ? C15 C16 1.360(11) . ? C15 H15 0.93 . ? C16 C17 1.379(10) . ? C16 H16 0.93 . ? C17 C18 1.500(10) . ? C18 H18A 0.96 . ? C18 H18B 0.96 . ? C18 H18C 0.96 . ? C21 C22 1.403(10) . ? C21 C27 1.410(11) . ? C22 C24 1.407(12) . ? C22 C23 1.480(12) . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 C25 1.362(14) . ? C24 H24 0.93 . ? C25 C26 1.368(14) . ? C25 H25 0.93 . ? C26 C27 1.378(11) . ? C26 H26 0.93 . ? C27 C28 1.500(11) . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C31 C32 1.341(15) . ? C31 C35 1.358(13) . ? C31 H31 0.93 . ? C32 C33 1.43(2) . ? C32 H32 0.93 . ? C33 C34 1.40(2) . ? C33 H33 0.93 . ? C34 C35 1.376(14) . ? C34 H34 0.93 . ? C35 H35 0.93 . ? 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 102.4(2) . . ? N2 Nb1 C1 100.7(3) . . ? N1 Nb1 C1 105.4(3) . . ? N2 Nb1 C33 108.3(4) . . ? N1 Nb1 C33 99.2(4) . . ? C1 Nb1 C33 136.5(4) . . ? N2 Nb1 C34 95.2(3) . . ? N1 Nb1 C34 132.9(4) . . ? C1 Nb1 C34 113.7(4) . . ? C33 Nb1 C34 33.7(4) . . ? N2 Nb1 C35 114.7(3) . . ? N1 Nb1 C35 139.5(3) . . ? C1 Nb1 C35 83.6(4) . . ? C33 Nb1 C35 55.2(4) . . ? C34 Nb1 C35 32.8(3) . . ? N2 Nb1 C32 142.3(4) . . ? N1 Nb1 C32 87.7(3) . . ? C1 Nb1 C32 111.5(4) . . ? C33 Nb1 C32 34.0(4) . . ? C34 Nb1 C32 54.5(4) . . ? C35 Nb1 C32 53.1(3) . . ? N2 Nb1 C31 146.1(3) . . ? N1 Nb1 C31 108.8(3) . . ? C1 Nb1 C31 83.6(4) . . ? C33 Nb1 C31 54.5(4) . . ? C34 Nb1 C31 53.5(3) . . ? C35 Nb1 C31 31.8(3) . . ? C32 Nb1 C31 31.2(4) . . ? C11 N1 Nb1 135.3(5) . . ? C11 N1 H1 112.3(4) . . ? Nb1 N1 H1 112.3(2) . . ? C21 N2 Nb1 170.3(5) . . ? Nb1 C1 H1A 109.5(3) . . ? Nb1 C1 H1B 109.5(3) . . ? H1A C1 H1B 109.5 . . ? Nb1 C1 H1C 109.5(2) . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C17 C11 C12 119.5(7) . . ? C17 C11 N1 121.7(6) . . ? C12 C11 N1 118.8(6) . . ? C14 C12 C11 119.0(7) . . ? C14 C12 C13 121.3(7) . . ? C11 C12 C13 119.7(7) . . ? C12 C13 H13A 109.5(4) . . ? C12 C13 H13B 109.5(4) . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5(5) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C12 121.4(8) . . ? C15 C14 H14 119.3(5) . . ? C12 C14 H14 119.3(5) . . ? C16 C15 C14 119.7(8) . . ? C16 C15 H15 120.2(5) . . ? C14 C15 H15 120.2(5) . . ? C15 C16 C17 121.9(7) . . ? C15 C16 H16 119.0(5) . . ? C17 C16 H16 119.0(4) . . ? C16 C17 C11 118.6(7) . . ? C16 C17 C18 120.0(6) . . ? C11 C17 C18 121.4(6) . . ? C17 C18 H18A 109.5(4) . . ? C17 C18 H18B 109.5(4) . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5(4) . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C21 C22 119.3(7) . . ? N2 C21 C27 119.3(6) . . ? C22 C21 C27 121.3(7) . . ? C21 C22 C24 116.8(9) . . ? C21 C22 C23 120.5(8) . . ? C24 C22 C23 122.7(8) . . ? C22 C23 H23A 109.5(5) . . ? C22 C23 H23B 109.5(5) . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5(5) . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C22 122.0(9) . . ? C25 C24 H24 119.0(6) . . ? C22 C24 H24 119.0(6) . . ? C24 C25 C26 120.0(9) . . ? C24 C25 H25 120.0(6) . . ? C26 C25 H25 120.0(6) . . ? C25 C26 C27 121.5(10) . . ? C25 C26 H26 119.3(6) . . ? C27 C26 H26 119.3(6) . . ? C26 C27 C21 118.4(8) . . ? C26 C27 C28 121.0(8) . . ? C21 C27 C28 120.6(7) . . ? C27 C28 H28A 109.5(5) . . ? C27 C28 H28B 109.5(5) . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5(4) . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C31 C35 110.0(11) . . ? C32 C31 Nb1 73.8(6) . . ? C35 C31 Nb1 72.5(5) . . ? C32 C31 H31 125.0(8) . . ? C35 C31 H31 125.0(7) . . ? Nb1 C31 H31 120.3(3) . . ? C31 C32 C33 108.0(10) . . ? C31 C32 Nb1 75.0(5) . . ? C33 C32 Nb1 69.6(5) . . ? C31 C32 H32 126.0(8) . . ? C33 C32 H32 126.0(8) . . ? Nb1 C32 H32 121.2(3) . . ? C34 C33 C32 105.2(10) . . ? C34 C33 Nb1 73.6(6) . . ? C32 C33 Nb1 76.4(6) . . ? C34 C33 H33 127.4(8) . . ? C32 C33 H33 127.4(8) . . ? Nb1 C33 H33 115.2(3) . . ? C35 C34 C33 108.6(10) . . ? C35 C34 Nb1 75.6(6) . . ? C33 C34 Nb1 72.7(5) . . ? C35 C34 H34 125.7(7) . . ? C33 C34 H34 125.7(8) . . ? Nb1 C34 H34 117.9(3) . . ? C31 C35 C34 108.1(10) . . ? C31 C35 Nb1 75.7(5) . . ? C34 C35 Nb1 71.6(5) . . ? C31 C35 H35 126.0(7) . . ? C34 C35 H35 126.0(7) . . ? Nb1 C35 H35 118.6(3) . . ? _refine_diff_density_max 0.424 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.086