# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 440/122 data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51.50 H69 N4 Nb O2' _chemical_formula_weight 869.02 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' 'O' 'O' 0.0106 0.0060 '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 12.5569(10) _cell_length_b 13.0513(5) _cell_length_c 16.5008(5) _cell_angle_alpha 80.481(5) _cell_angle_beta 70.949(5) _cell_angle_gamma 82.328(5) _cell_volume 2511.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 10943 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 28.61 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8965 _exptl_absorpt_correction_T_max 0.9462 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14770 _diffrn_reflns_av_R_equivalents 0.1857 _diffrn_reflns_av_sigmaI/netI 0.4769 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.61 _reflns_number_total 10931 _reflns_number_gt 3301 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^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 10931 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2014 _refine_ls_R_factor_gt 0.0939 _refine_ls_wR_factor_ref 0.2295 _refine_ls_wR_factor_gt 0.2028 _refine_ls_goodness_of_fit_ref 0.759 _refine_ls_restrained_S_all 0.759 _refine_ls_shift/su_max 0.912 _refine_ls_shift/su_mean 0.017 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 0.23474(6) 0.34430(6) 0.20507(4) 0.0348(2) Uani 1 1 d . . . O1 O 0.0954(4) 0.2865(4) 0.2921(3) 0.0414(14) Uani 1 1 d . . . O2 O 0.2005(4) 0.2706(4) 0.1105(3) 0.0339(13) Uani 1 1 d . . . N1 N 0.3064(5) 0.1738(4) 0.2504(4) 0.0357(17) Uani 1 1 d . . . N2 N 0.4046(5) 0.3330(4) 0.1046(4) 0.0356(16) Uani 1 1 d . . . N3 N 0.1696(5) 0.4838(5) 0.1606(4) 0.0389(17) Uani 1 1 d . . . N4 N 0.2909(5) 0.3925(5) 0.2763(4) 0.0409(18) Uani 1 1 d . . . C1 C 0.0819(6) 0.2456(6) 0.3745(4) 0.0301(18) Uani 1 1 d . . . C2 C 0.1600(6) 0.1691(6) 0.3927(4) 0.0318(19) Uani 1 1 d . . . C3 C 0.1474(6) 0.1218(6) 0.4802(4) 0.043(2) Uani 1 1 d . . . H3A H 0.2037 0.0714 0.4929 0.052 Uiso 1 1 calc R . . C4 C 0.0528(6) 0.1509(6) 0.5451(4) 0.035(2) Uani 1 1 d . . . C5 C -0.0249(6) 0.2272(6) 0.5243(4) 0.038(2) Uani 1 1 d . . . H5A H -0.0873 0.2501 0.5703 0.046 Uiso 1 1 calc R . . C6 C -0.0180(6) 0.2728(6) 0.4408(4) 0.038(2) Uani 1 1 d . . . C7 C -0.1088(6) 0.3533(7) 0.4230(5) 0.051(2) Uani 1 1 d . . . C8 C -0.2070(7) 0.3681(8) 0.5036(5) 0.076(3) Uani 1 1 d . . . H8A H -0.1817 0.3982 0.5441 0.115 Uiso 1 1 calc R . . H8B H -0.2360 0.3005 0.5309 0.115 Uiso 1 1 calc R . . H8C H -0.2671 0.4152 0.4883 0.115 Uiso 1 1 calc R . . C9 C -0.1540(7) 0.3189(7) 0.3577(5) 0.061(3) Uani 1 1 d . . . H9A H -0.1835 0.2505 0.3801 0.091 Uiso 1 1 calc R . . H9B H -0.0929 0.3142 0.3031 0.091 Uiso 1 1 calc R . . H9C H -0.2148 0.3698 0.3479 0.091 Uiso 1 1 calc R . . C10 C -0.0597(7) 0.4615(6) 0.3872(5) 0.057(3) Uani 1 1 d . . . H10A H -0.0272 0.4816 0.4283 0.085 Uiso 1 1 calc R . . H10B H -0.1203 0.5140 0.3795 0.085 Uiso 1 1 calc R . . H10C H -0.0007 0.4568 0.3315 0.085 Uiso 1 1 calc R . . C11 C 0.0390(7) 0.1036(7) 0.6416(5) 0.053(3) Uani 1 1 d . . . C12 C -0.0792(10) 0.0877(14) 0.6887(7) 0.182(9) Uani 1 1 d . . . H12A H -0.0985 0.1086 0.7465 0.272 Uiso 1 1 calc R . . H12B H -0.0910 0.0138 0.6940 0.272 Uiso 1 1 calc R . . H12C H -0.1275 0.1299 0.6574 0.272 Uiso 1 1 calc R . . C13 C 0.0544(16) 0.1874(13) 0.6892(8) 0.204(9) Uani 1 1 d . . . H13A H 0.0133 0.2529 0.6736 0.306 Uiso 1 1 calc R . . H13B H 0.1350 0.1973 0.6733 0.306 Uiso 1 1 calc R . . H13C H 0.0249 0.1661 0.7517 0.306 Uiso 1 1 calc R . . C14 C 0.1102(15) 0.0194(15) 0.6511(7) 0.284(15) Uani 1 1 d . . . H14A H 0.0993 -0.0028 0.7127 0.426 Uiso 1 1 calc R . . H14B H 0.1884 0.0369 0.6222 0.426 Uiso 1 1 calc R . . H14C H 0.0950 -0.0372 0.6252 0.426 Uiso 1 1 calc R . . C15 C 0.2596(6) 0.1292(6) 0.3276(5) 0.046(2) Uani 1 1 d . . . H15A H 0.2939 0.0630 0.3439 0.055 Uiso 1 1 calc R . . C16 C 0.3925(6) 0.1107(6) 0.1955(4) 0.0312(18) Uani 1 1 d . . . C17 C 0.3589(6) 0.0178(6) 0.1810(4) 0.0346(19) Uani 1 1 d . . . H17A H 0.2830 0.0005 0.2075 0.042 Uiso 1 1 calc R . . C18 C 0.4378(6) -0.0486(6) 0.1274(4) 0.0348(19) Uani 1 1 d . . . H18A H 0.4165 -0.1122 0.1189 0.042 Uiso 1 1 calc R . . C19 C 0.5444(7) -0.0211(6) 0.0879(5) 0.041(2) Uani 1 1 d . . . H19A H 0.5975 -0.0658 0.0512 0.049 Uiso 1 1 calc R . . C20 C 0.5776(6) 0.0697(6) 0.0996(4) 0.0331(19) Uani 1 1 d . . . C21 C 0.6973(6) 0.0975(6) 0.0500(5) 0.049(2) Uani 1 1 d . . . H21A H 0.7512 0.0464 0.0697 0.073 Uiso 1 1 calc R . . H21B H 0.7067 0.1672 0.0602 0.073 Uiso 1 1 calc R . . H21C H 0.7113 0.0970 -0.0120 0.073 Uiso 1 1 calc R . . C22 C 0.5009(6) 0.1371(6) 0.1569(4) 0.0342(19) Uani 1 1 d . . . C23 C 0.5407(6) 0.2356(6) 0.1702(4) 0.0321(19) Uani 1 1 d . . . C24 C 0.6227(6) 0.2331(6) 0.2084(4) 0.037(2) Uani 1 1 d . . . C25 C 0.6661(7) 0.1328(7) 0.2535(5) 0.070(3) Uani 1 1 d . . . H25A H 0.6857 0.1484 0.3027 0.105 Uiso 1 1 calc R . . H25B H 0.7333 0.1015 0.2127 0.105 Uiso 1 1 calc R . . H25C H 0.6072 0.0839 0.2741 0.105 Uiso 1 1 calc R . . C26 C 0.6719(6) 0.3268(7) 0.2029(5) 0.046(2) Uani 1 1 d . . . H26A H 0.7312 0.3260 0.2270 0.056 Uiso 1 1 calc R . . C27 C 0.6343(7) 0.4184(6) 0.1631(5) 0.048(2) Uani 1 1 d . . . H27A H 0.6686 0.4806 0.1586 0.057 Uiso 1 1 calc R . . C28 C 0.5471(6) 0.4204(6) 0.1297(5) 0.043(2) Uani 1 1 d . . . H28A H 0.5209 0.4843 0.1025 0.052 Uiso 1 1 calc R . . C29 C 0.4977(6) 0.3316(6) 0.1351(4) 0.0298(18) Uani 1 1 d . . . C30 C 0.4276(6) 0.3168(5) 0.0230(4) 0.0288(18) Uani 1 1 d . . . H30A H 0.5047 0.3181 -0.0113 0.035 Uiso 1 1 calc R . . C31 C 0.3525(6) 0.2979(5) -0.0193(4) 0.0297(18) Uani 1 1 d . . . C32 C 0.3964(6) 0.2972(5) -0.1100(4) 0.0319(19) Uani 1 1 d . . . H32A H 0.4714 0.3158 -0.1391 0.038 Uiso 1 1 calc R . . C33 C 0.3351(6) 0.2709(5) -0.1570(4) 0.0315(18) Uani 1 1 d . . . C34 C 0.2257(6) 0.2379(5) -0.1085(4) 0.0342(19) Uani 1 1 d . . . H34A H 0.1819 0.2185 -0.1400 0.041 Uiso 1 1 calc R . . C35 C 0.1775(6) 0.2316(5) -0.0189(4) 0.0299(18) Uani 1 1 d . . . C36 C 0.2418(6) 0.2679(5) 0.0271(4) 0.0277(18) Uani 1 1 d . . . C37 C 0.3760(6) 0.2741(6) -0.2550(4) 0.0335(19) Uani 1 1 d . . . C38 C 0.3765(7) 0.1637(6) -0.2782(5) 0.053(2) Uani 1 1 d . . . H38A H 0.4333 0.1164 -0.2587 0.079 Uiso 1 1 calc R . . H38B H 0.3948 0.1669 -0.3410 0.079 Uiso 1 1 calc R . . H38C H 0.3017 0.1379 -0.2496 0.079 Uiso 1 1 calc R . . C39 C 0.4973(7) 0.3071(7) -0.2956(5) 0.062(3) Uani 1 1 d . . . H39A H 0.5485 0.2586 -0.2707 0.092 Uiso 1 1 calc R . . H39B H 0.4997 0.3777 -0.2838 0.092 Uiso 1 1 calc R . . H39C H 0.5210 0.3059 -0.3583 0.092 Uiso 1 1 calc R . . C40 C 0.2969(7) 0.3511(7) -0.2942(5) 0.057(3) Uani 1 1 d . . . H40A H 0.2197 0.3298 -0.2699 0.086 Uiso 1 1 calc R . . H40B H 0.3222 0.3517 -0.3571 0.086 Uiso 1 1 calc R . . H40C H 0.2984 0.4212 -0.2807 0.086 Uiso 1 1 calc R . . C41 C 0.0647(6) 0.1899(6) 0.0287(4) 0.039(2) Uani 1 1 d . . . C42 C 0.0772(6) 0.0941(6) 0.0957(5) 0.047(2) Uani 1 1 d . . . H42A H 0.1014 0.1160 0.1404 0.071 Uiso 1 1 calc R . . H42B H 0.1338 0.0416 0.0665 0.071 Uiso 1 1 calc R . . H42C H 0.0043 0.0640 0.1223 0.071 Uiso 1 1 calc R . . C43 C -0.0214(6) 0.2704(6) 0.0758(5) 0.048(2) Uani 1 1 d . . . H43A H 0.0027 0.2886 0.1221 0.072 Uiso 1 1 calc R . . H43B H -0.0951 0.2417 0.1007 0.072 Uiso 1 1 calc R . . H43C H -0.0274 0.3330 0.0350 0.072 Uiso 1 1 calc R . . C44 C 0.0127(6) 0.1517(7) -0.0339(5) 0.052(2) Uani 1 1 d . . . H44A H -0.0089 0.2118 -0.0712 0.078 Uiso 1 1 calc R . . H44B H -0.0544 0.1151 -0.0001 0.078 Uiso 1 1 calc R . . H44C H 0.0686 0.1042 -0.0697 0.078 Uiso 1 1 calc R . . C45 C -0.0152(7) 0.5231(6) 0.1358(5) 0.053(2) Uani 1 1 d . . . H45A H -0.0497 0.5489 0.0901 0.079 Uiso 1 1 calc R . . H45B H -0.0314 0.5752 0.1757 0.079 Uiso 1 1 calc R . . H45C H -0.0464 0.4579 0.1674 0.079 Uiso 1 1 calc R . . C46 C 0.1110(7) 0.5038(6) 0.0959(5) 0.047(2) Uani 1 1 d . . . H46A H 0.1274 0.4433 0.0634 0.056 Uiso 1 1 calc R . . H46B H 0.1399 0.5654 0.0544 0.056 Uiso 1 1 calc R . . C47 C 0.1753(7) 0.5834(6) 0.1938(5) 0.048(2) Uani 1 1 d . . . H47A H 0.1055 0.6296 0.1957 0.058 Uiso 1 1 calc R . . H47B H 0.1798 0.5669 0.2534 0.058 Uiso 1 1 calc R . . C48 C 0.2760(8) 0.6393(7) 0.1374(6) 0.083(3) Uani 1 1 d . . . H48A H 0.2753 0.7052 0.1587 0.125 Uiso 1 1 calc R . . H48B H 0.2732 0.6534 0.0779 0.125 Uiso 1 1 calc R . . H48C H 0.3455 0.5956 0.1387 0.125 Uiso 1 1 calc R . . C49 C 0.3480(8) 0.4191(8) 0.3309(6) 0.069(3) Uani 1 1 d . . . H49A H 0.3406 0.4959 0.3292 0.082 Uiso 1 1 calc R . . H49B H 0.4295 0.3964 0.3083 0.082 Uiso 1 1 calc R . . C50 C 0.3020(17) 0.3697(11) 0.4237(8) 0.224(11) Uani 1 1 d . . . H50A H 0.3561 0.3732 0.4544 0.336 Uiso 1 1 calc R . . H50B H 0.2904 0.2967 0.4248 0.336 Uiso 1 1 calc R . . H50C H 0.2298 0.4073 0.4519 0.336 Uiso 1 1 calc R . . C101 C 0.3906(16) -0.0932(15) 0.4839(12) 0.068(5) Uiso 0.50 1 d P . . C102 C 0.4554(19) -0.0010(19) 0.4822(15) 0.095(7) Uiso 0.50 1 d P . . C100 C 0.462(4) -0.141(3) 0.517(3) 0.220(17) Uiso 0.50 1 d P . . 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 0.0439(4) 0.0317(4) 0.0165(4) 0.0017(3) 0.0009(3) 0.0074(3) O1 0.051(3) 0.055(4) 0.008(3) 0.003(2) 0.001(2) -0.006(3) O2 0.050(3) 0.032(3) 0.011(3) -0.005(2) -0.001(2) 0.006(3) N1 0.034(4) 0.032(4) 0.022(3) 0.016(3) 0.006(3) 0.004(3) N2 0.043(4) 0.020(3) 0.038(4) 0.009(3) -0.010(3) -0.003(3) N3 0.029(3) 0.039(4) 0.033(4) 0.009(3) 0.003(3) 0.001(3) N4 0.056(4) 0.035(4) 0.016(4) 0.000(3) 0.005(3) 0.005(3) C1 0.047(5) 0.031(4) 0.015(4) -0.001(3) -0.016(3) -0.002(4) C2 0.030(4) 0.040(5) 0.020(4) 0.001(4) -0.003(3) -0.005(4) C3 0.045(5) 0.047(5) 0.022(4) 0.012(4) -0.001(4) 0.001(4) C4 0.038(4) 0.041(5) 0.017(4) 0.006(4) 0.000(3) -0.005(4) C5 0.038(4) 0.053(6) 0.016(4) -0.006(4) 0.004(3) -0.004(4) C6 0.041(4) 0.054(6) 0.011(4) -0.005(4) -0.005(3) 0.015(4) C7 0.042(5) 0.076(7) 0.019(5) -0.010(4) 0.008(4) 0.010(5) C8 0.052(6) 0.117(9) 0.035(6) -0.007(5) 0.004(4) 0.030(6) C9 0.054(5) 0.082(7) 0.037(6) -0.008(5) -0.009(4) 0.014(5) C10 0.057(6) 0.050(6) 0.053(6) -0.005(5) -0.015(5) 0.023(5) C11 0.068(6) 0.067(7) 0.008(4) 0.010(4) -0.004(4) 0.011(5) C12 0.092(10) 0.36(2) 0.057(8) 0.119(11) -0.023(7) -0.082(12) C13 0.38(3) 0.22(2) 0.041(9) 0.010(11) -0.088(13) -0.111(19) C14 0.32(2) 0.34(3) 0.026(7) 0.083(11) 0.032(10) 0.22(2) C15 0.059(5) 0.035(5) 0.024(4) 0.003(4) 0.000(4) 0.021(4) C16 0.040(4) 0.030(5) 0.012(4) 0.000(3) 0.003(3) 0.004(4) C17 0.031(4) 0.036(5) 0.026(4) 0.005(4) 0.001(3) -0.005(4) C18 0.053(5) 0.020(4) 0.026(4) -0.004(4) -0.005(4) -0.003(4) C19 0.049(5) 0.029(5) 0.029(5) 0.001(4) 0.000(4) 0.008(4) C20 0.035(4) 0.035(5) 0.021(4) 0.002(4) -0.003(3) 0.006(4) C21 0.045(5) 0.043(5) 0.044(5) -0.012(4) 0.003(4) 0.008(4) C22 0.036(4) 0.026(4) 0.027(4) 0.010(4) -0.001(3) 0.002(4) C23 0.032(4) 0.034(5) 0.019(4) 0.000(4) 0.000(3) 0.009(4) C24 0.040(4) 0.041(5) 0.023(4) -0.004(4) -0.005(4) 0.010(4) C25 0.061(6) 0.085(8) 0.049(6) 0.010(5) -0.018(5) 0.026(5) C26 0.045(5) 0.062(6) 0.035(5) -0.018(5) -0.017(4) 0.012(5) C27 0.060(6) 0.032(5) 0.050(6) -0.015(4) -0.014(5) 0.003(4) C28 0.047(5) 0.031(5) 0.043(5) 0.006(4) -0.011(4) 0.004(4) C29 0.046(5) 0.030(5) 0.013(4) -0.011(3) -0.008(3) 0.007(4) C30 0.037(4) 0.028(4) 0.016(4) 0.000(3) 0.001(3) -0.007(4) C31 0.042(4) 0.028(4) 0.012(4) 0.000(3) -0.002(3) 0.001(4) C32 0.042(4) 0.026(4) 0.019(4) -0.001(3) 0.002(3) -0.002(4) C33 0.048(5) 0.024(4) 0.014(4) -0.006(3) 0.004(3) -0.009(4) C34 0.046(5) 0.028(4) 0.020(4) 0.003(3) -0.004(3) 0.001(4) C35 0.043(4) 0.030(4) 0.006(4) -0.001(3) 0.002(3) 0.007(4) C36 0.039(4) 0.025(4) 0.013(4) -0.003(3) -0.002(3) 0.001(3) C37 0.052(5) 0.033(5) 0.014(4) -0.008(4) -0.005(3) -0.008(4) C38 0.079(6) 0.046(6) 0.024(5) -0.005(4) -0.008(4) 0.005(5) C39 0.077(7) 0.074(7) 0.021(5) -0.003(4) 0.009(4) -0.031(6) C40 0.080(6) 0.066(7) 0.015(4) -0.002(4) -0.005(4) 0.001(5) C41 0.044(5) 0.043(5) 0.019(4) 0.007(4) -0.001(4) 0.000(4) C42 0.052(5) 0.029(5) 0.043(5) 0.003(4) 0.004(4) -0.003(4) C43 0.044(5) 0.048(6) 0.037(5) 0.003(4) 0.004(4) -0.004(4) C44 0.054(5) 0.071(7) 0.028(5) 0.001(4) -0.007(4) -0.020(5) C45 0.060(6) 0.045(6) 0.046(6) -0.003(4) -0.016(4) 0.012(5) C46 0.073(6) 0.036(5) 0.020(4) 0.000(4) -0.007(4) 0.014(4) C47 0.059(6) 0.026(5) 0.055(6) 0.000(4) -0.014(5) -0.006(4) C48 0.096(8) 0.051(7) 0.087(8) -0.007(6) 0.002(6) -0.029(6) C49 0.090(7) 0.075(8) 0.039(6) -0.030(6) -0.012(5) 0.004(6) C50 0.52(3) 0.144(14) 0.084(11) 0.048(10) -0.176(17) -0.147(18) _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 N4 1.783(7) . y Nb1 O1 2.011(5) . y Nb1 N3 2.019(6) . y Nb1 O2 2.142(5) . y Nb1 N2 2.238(6) . y Nb1 N1 2.382(5) . y O1 C1 1.341(7) . ? O2 C36 1.308(7) . ? N1 C15 1.291(8) . ? N1 C16 1.427(8) . ? N2 C30 1.329(8) . ? N2 C29 1.412(8) . ? N3 C46 1.456(9) . ? N3 C47 1.511(9) . ? N4 C49 1.428(10) . ? C1 C2 1.371(9) . ? C1 C6 1.418(9) . ? C2 C3 1.440(9) . ? C2 C15 1.457(10) . ? C3 C4 1.373(9) . ? C4 C5 1.381(9) . ? C4 C11 1.572(9) . ? C5 C6 1.388(9) . ? C6 C7 1.512(10) . ? C7 C8 1.510(10) . ? C7 C9 1.520(11) . ? C7 C10 1.563(11) . ? C11 C14 1.343(14) . ? C11 C12 1.458(12) . ? C11 C13 1.514(15) . ? C16 C22 1.366(9) . ? C16 C17 1.415(10) . ? C17 C18 1.402(10) . ? C18 C19 1.351(10) . ? C19 C20 1.369(10) . ? C20 C22 1.432(10) . ? C20 C21 1.518(10) . ? C22 C23 1.511(10) . ? C23 C24 1.367(9) . ? C23 C29 1.407(9) . ? C24 C26 1.418(11) . ? C24 C25 1.522(10) . ? C26 C27 1.370(10) . ? C27 C28 1.373(10) . ? C28 C29 1.363(10) . ? C30 C31 1.408(9) . ? C31 C32 1.417(9) . ? C31 C36 1.422(9) . ? C32 C33 1.364(9) . ? C33 C34 1.429(9) . ? C33 C37 1.524(9) . ? C34 C35 1.397(9) . ? C35 C36 1.440(9) . ? C35 C41 1.502(10) . ? C37 C40 1.534(10) . ? C37 C39 1.538(10) . ? C37 C38 1.550(10) . ? C41 C43 1.515(10) . ? C41 C42 1.554(9) . ? C41 C44 1.563(10) . ? C45 C46 1.508(10) . ? C47 C48 1.500(11) . ? C49 C50 1.513(14) . ? C101 C100 1.24(4) . ? C101 C102 1.53(3) . ? C102 C102 1.43(4) 2_656 ? C102 C100 1.82(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 N4 Nb1 O1 99.3(2) . . y N4 Nb1 N3 96.3(3) . . y O1 Nb1 N3 101.1(2) . . y N4 Nb1 O2 168.5(2) . . y O1 Nb1 O2 87.83(19) . . y N3 Nb1 O2 91.2(2) . . y N4 Nb1 N2 92.0(3) . . y O1 Nb1 N2 154.5(2) . . y N3 Nb1 N2 100.4(2) . . y O2 Nb1 N2 78.0(2) . . y N4 Nb1 N1 88.1(2) . . y O1 Nb1 N1 78.19(19) . . y N3 Nb1 N1 175.6(3) . . y O2 Nb1 N1 84.49(19) . . y N2 Nb1 N1 79.36(19) . . y C1 O1 Nb1 127.5(4) . . y C36 O2 Nb1 137.0(5) . . y C15 N1 C16 115.4(6) . . ? C15 N1 Nb1 119.5(5) . . y C16 N1 Nb1 124.8(4) . . y C30 N2 C29 117.0(6) . . ? C30 N2 Nb1 127.5(5) . . y C29 N2 Nb1 115.2(5) . . y C46 N3 C47 110.9(6) . . ? C46 N3 Nb1 126.8(5) . . y C47 N3 Nb1 122.2(5) . . y C49 N4 Nb1 171.9(6) . . y O1 C1 C2 119.1(6) . . ? O1 C1 C6 120.2(6) . . ? C2 C1 C6 120.3(6) . . ? C1 C2 C3 120.8(6) . . ? C1 C2 C15 124.1(6) . . ? C3 C2 C15 115.0(6) . . ? C4 C3 C2 118.9(7) . . ? C3 C4 C5 118.7(6) . . ? C3 C4 C11 120.0(6) . . ? C5 C4 C11 121.2(6) . . ? C4 C5 C6 124.4(7) . . ? C5 C6 C1 116.5(6) . . ? C5 C6 C7 121.3(6) . . ? C1 C6 C7 122.1(6) . . ? C8 C7 C6 112.1(6) . . ? C8 C7 C9 108.0(7) . . ? C6 C7 C9 109.6(7) . . ? C8 C7 C10 107.1(8) . . ? C6 C7 C10 110.1(6) . . ? C9 C7 C10 109.9(6) . . ? C14 C11 C12 113.5(12) . . ? C14 C11 C13 109.5(13) . . ? C12 C11 C13 98.9(11) . . ? C14 C11 C4 114.5(8) . . ? C12 C11 C4 110.5(7) . . ? C13 C11 C4 108.8(8) . . ? N1 C15 C2 127.2(7) . . ? C22 C16 C17 120.6(7) . . ? C22 C16 N1 123.4(7) . . ? C17 C16 N1 116.0(6) . . ? C18 C17 C16 119.9(7) . . ? C19 C18 C17 119.3(7) . . ? C18 C19 C20 121.6(7) . . ? C19 C20 C22 120.7(7) . . ? C19 C20 C21 118.5(7) . . ? C22 C20 C21 120.8(7) . . ? C16 C22 C20 117.8(7) . . ? C16 C22 C23 122.6(7) . . ? C20 C22 C23 119.6(6) . . ? C24 C23 C29 119.9(7) . . ? C24 C23 C22 122.0(6) . . ? C29 C23 C22 117.9(6) . . ? C23 C24 C26 118.7(7) . . ? C23 C24 C25 122.3(8) . . ? C26 C24 C25 119.0(7) . . ? C27 C26 C24 120.4(7) . . ? C26 C27 C28 120.1(8) . . ? C29 C28 C27 120.6(7) . . ? C28 C29 C23 120.0(7) . . ? C28 C29 N2 121.4(6) . . ? C23 C29 N2 118.6(7) . . ? N2 C30 C31 128.5(7) . . ? C30 C31 C32 117.0(7) . . ? C30 C31 C36 122.0(6) . . ? C32 C31 C36 120.5(7) . . ? C33 C32 C31 122.5(7) . . ? C32 C33 C34 115.9(6) . . ? C32 C33 C37 124.6(7) . . ? C34 C33 C37 119.6(7) . . ? C35 C34 C33 125.6(7) . . ? C34 C35 C36 116.4(7) . . ? C34 C35 C41 122.9(7) . . ? C36 C35 C41 120.7(6) . . ? O2 C36 C31 120.5(7) . . ? O2 C36 C35 120.6(6) . . ? C31 C36 C35 118.9(6) . . ? C33 C37 C40 109.6(6) . . ? C33 C37 C39 112.2(6) . . ? C40 C37 C39 108.8(6) . . ? C33 C37 C38 109.2(6) . . ? C40 C37 C38 109.7(6) . . ? C39 C37 C38 107.2(7) . . ? C35 C41 C43 112.7(7) . . ? C35 C41 C42 110.5(6) . . ? C43 C41 C42 108.3(6) . . ? C35 C41 C44 111.7(6) . . ? C43 C41 C44 106.8(6) . . ? C42 C41 C44 106.5(7) . . ? N3 C46 C45 112.2(6) . . ? C48 C47 N3 111.3(7) . . ? N4 C49 C50 112.7(9) . . ? C100 C101 C102 82(2) . . ? C102 C102 C101 129(3) 2_656 . ? C102 C102 C100 87(2) 2_656 . ? C101 C102 C100 42.3(14) . . ? C101 C100 C102 56(2) . . ? 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 N4 Nb1 O1 C1 -31.3(6) . . . . y N3 Nb1 O1 C1 -129.7(6) . . . . y O2 Nb1 O1 C1 139.6(6) . . . . y N2 Nb1 O1 C1 83.7(8) . . . . y N1 Nb1 O1 C1 54.8(6) . . . . y N4 Nb1 O2 C36 -57.4(14) . . . . y O1 Nb1 O2 C36 174.2(6) . . . . y N3 Nb1 O2 C36 73.1(6) . . . . y N2 Nb1 O2 C36 -27.2(6) . . . . y N1 Nb1 O2 C36 -107.5(6) . . . . y N4 Nb1 N1 C15 70.7(7) . . . . y O1 Nb1 N1 C15 -29.2(6) . . . . y N3 Nb1 N1 C15 -110(3) . . . . y O2 Nb1 N1 C15 -118.1(7) . . . . y N2 Nb1 N1 C15 163.0(7) . . . . y N4 Nb1 N1 C16 -115.6(6) . . . . y O1 Nb1 N1 C16 144.5(6) . . . . y N3 Nb1 N1 C16 64(3) . . . . y O2 Nb1 N1 C16 55.6(6) . . . . y N2 Nb1 N1 C16 -23.3(6) . . . . y N4 Nb1 N2 C30 -168.2(6) . . . . y O1 Nb1 N2 C30 75.3(7) . . . . y N3 Nb1 N2 C30 -71.5(6) . . . . y O2 Nb1 N2 C30 17.5(5) . . . . y N1 Nb1 N2 C30 104.1(5) . . . . y N4 Nb1 N2 C29 19.2(5) . . . . y O1 Nb1 N2 C29 -97.2(7) . . . . y N3 Nb1 N2 C29 116.0(5) . . . . y O2 Nb1 N2 C29 -155.0(5) . . . . y N1 Nb1 N2 C29 -68.4(5) . . . . y N4 Nb1 N3 C46 178.4(6) . . . . y O1 Nb1 N3 C46 -80.8(6) . . . . y O2 Nb1 N3 C46 7.2(6) . . . . y N2 Nb1 N3 C46 85.3(6) . . . . y N1 Nb1 N3 C46 -1(3) . . . . y N4 Nb1 N3 C47 -2.6(5) . . . . y O1 Nb1 N3 C47 98.2(5) . . . . y O2 Nb1 N3 C47 -173.8(5) . . . . y N2 Nb1 N3 C47 -95.7(5) . . . . y N1 Nb1 N3 C47 178(3) . . . . y O1 Nb1 N4 C49 108(4) . . . . y N3 Nb1 N4 C49 -149(4) . . . . y O2 Nb1 N4 C49 -19(5) . . . . y N2 Nb1 N4 C49 -49(4) . . . . y N1 Nb1 N4 C49 31(4) . . . . y Nb1 O1 C1 C2 -51.1(9) . . . . y Nb1 O1 C1 C6 135.8(6) . . . . y O1 C1 C2 C3 -178.8(7) . . . . ? C6 C1 C2 C3 -5.8(11) . . . . ? O1 C1 C2 C15 1.0(12) . . . . ? C6 C1 C2 C15 174.0(8) . . . . ? C1 C2 C3 C4 3.2(12) . . . . ? C15 C2 C3 C4 -176.6(7) . . . . ? C2 C3 C4 C5 -2.3(12) . . . . ? C2 C3 C4 C11 -177.8(7) . . . . ? C3 C4 C5 C6 4.3(12) . . . . ? C11 C4 C5 C6 179.7(8) . . . . ? C4 C5 C6 C1 -6.6(12) . . . . ? C4 C5 C6 C7 177.8(8) . . . . ? O1 C1 C6 C5 -179.8(7) . . . . ? C2 C1 C6 C5 7.2(12) . . . . ? O1 C1 C6 C7 -4.3(12) . . . . ? C2 C1 C6 C7 -177.3(8) . . . . ? C5 C6 C7 C8 -5.0(12) . . . . ? C1 C6 C7 C8 179.6(8) . . . . ? C5 C6 C7 C9 -124.9(8) . . . . ? C1 C6 C7 C9 59.8(10) . . . . ? C5 C6 C7 C10 114.1(8) . . . . ? C1 C6 C7 C10 -61.2(10) . . . . ? C3 C4 C11 C14 -14.5(17) . . . . ? C5 C4 C11 C14 170.1(14) . . . . ? C3 C4 C11 C12 -144.2(11) . . . . ? C5 C4 C11 C12 40.4(13) . . . . ? C3 C4 C11 C13 108.3(11) . . . . ? C5 C4 C11 C13 -67.1(12) . . . . ? C16 N1 C15 C2 -170.7(8) . . . . ? Nb1 N1 C15 C2 3.6(12) . . . . ? C1 C2 C15 N1 19.5(14) . . . . ? C3 C2 C15 N1 -160.7(8) . . . . ? C15 N1 C16 C22 -122.1(8) . . . . ? Nb1 N1 C16 C22 64.0(8) . . . . ? C15 N1 C16 C17 59.3(9) . . . . ? Nb1 N1 C16 C17 -114.7(6) . . . . ? C22 C16 C17 C18 0.8(10) . . . . ? N1 C16 C17 C18 179.5(6) . . . . ? C16 C17 C18 C19 -2.2(10) . . . . ? C17 C18 C19 C20 0.6(10) . . . . ? C18 C19 C20 C22 2.3(10) . . . . ? C18 C19 C20 C21 -177.4(6) . . . . ? C17 C16 C22 C20 2.0(10) . . . . ? N1 C16 C22 C20 -176.6(6) . . . . ? C17 C16 C22 C23 179.7(6) . . . . ? N1 C16 C22 C23 1.2(10) . . . . ? C19 C20 C22 C16 -3.6(10) . . . . ? C21 C20 C22 C16 176.1(6) . . . . ? C19 C20 C22 C23 178.6(6) . . . . ? C21 C20 C22 C23 -1.7(10) . . . . ? C16 C22 C23 C24 117.0(8) . . . . ? C20 C22 C23 C24 -65.3(9) . . . . ? C16 C22 C23 C29 -68.5(9) . . . . ? C20 C22 C23 C29 109.3(7) . . . . ? C29 C23 C24 C26 -7.2(11) . . . . ? C22 C23 C24 C26 167.3(6) . . . . ? C29 C23 C24 C25 175.2(6) . . . . ? C22 C23 C24 C25 -10.3(11) . . . . ? C23 C24 C26 C27 2.6(11) . . . . ? C25 C24 C26 C27 -179.7(7) . . . . ? C24 C26 C27 C28 1.3(12) . . . . ? C26 C27 C28 C29 -0.5(13) . . . . ? C27 C28 C29 C23 -4.1(12) . . . . ? C27 C28 C29 N2 177.1(7) . . . . ? C24 C23 C29 C28 8.0(11) . . . . ? C22 C23 C29 C28 -166.6(7) . . . . ? C24 C23 C29 N2 -173.2(7) . . . . ? C22 C23 C29 N2 12.1(9) . . . . ? C30 N2 C29 C28 91.1(9) . . . . ? Nb1 N2 C29 C28 -95.6(7) . . . . ? C30 N2 C29 C23 -87.7(8) . . . . ? Nb1 N2 C29 C23 85.7(7) . . . . ? C29 N2 C30 C31 169.1(7) . . . . ? Nb1 N2 C30 C31 -3.3(10) . . . . ? N2 C30 C31 C32 171.7(6) . . . . ? N2 C30 C31 C36 -16.1(11) . . . . ? C30 C31 C32 C33 174.1(7) . . . . ? C36 C31 C32 C33 1.7(10) . . . . ? C31 C32 C33 C34 -3.5(10) . . . . ? C31 C32 C33 C37 176.8(6) . . . . ? C32 C33 C34 C35 0.6(11) . . . . ? C37 C33 C34 C35 -179.7(6) . . . . ? C33 C34 C35 C36 4.1(10) . . . . ? C33 C34 C35 C41 -176.1(7) . . . . ? Nb1 O2 C36 C31 19.0(10) . . . . ? Nb1 O2 C36 C35 -162.9(5) . . . . ? C30 C31 C36 O2 9.4(10) . . . . ? C32 C31 C36 O2 -178.6(6) . . . . ? C30 C31 C36 C35 -168.7(6) . . . . ? C32 C31 C36 C35 3.2(10) . . . . ? C34 C35 C36 O2 176.0(6) . . . . ? C41 C35 C36 O2 -3.8(10) . . . . ? C34 C35 C36 C31 -5.8(9) . . . . ? C41 C35 C36 C31 174.4(6) . . . . ? C32 C33 C37 C40 -119.0(8) . . . . ? C34 C33 C37 C40 61.4(9) . . . . ? C32 C33 C37 C39 2.0(10) . . . . ? C34 C33 C37 C39 -177.6(7) . . . . ? C32 C33 C37 C38 120.8(8) . . . . ? C34 C33 C37 C38 -58.9(8) . . . . ? C34 C35 C41 C43 -118.1(7) . . . . ? C36 C35 C41 C43 61.7(8) . . . . ? C34 C35 C41 C42 120.5(7) . . . . ? C36 C35 C41 C42 -59.7(9) . . . . ? C34 C35 C41 C44 2.2(10) . . . . ? C36 C35 C41 C44 -178.1(6) . . . . ? C47 N3 C46 C45 -75.2(8) . . . . ? Nb1 N3 C46 C45 103.9(7) . . . . ? C46 N3 C47 C48 -86.2(8) . . . . ? Nb1 N3 C47 C48 94.6(7) . . . . ? Nb1 N4 C49 C50 -92(4) . . . . ? C100 C101 C102 C102 -6(4) . . . 2_656 ? C102 C102 C100 C101 175(3) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 28.61 _diffrn_measured_fraction_theta_full 0.851 _refine_diff_density_max 1.188 _refine_diff_density_min -1.761 _refine_diff_density_rms 0.130 data_dec1596 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H84 N5 Nb O2' _chemical_formula_weight 952.19 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 13.670(2) _cell_length_b 20.289(14) _cell_length_c 19.765(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.26(3) _cell_angle_gamma 90.00 _cell_volume 5477.6(49) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method ? _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type psiscans _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _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 CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10018 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.98 _reflns_number_total 9597 _reflns_number_observed 6753 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 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^)+(0.0780P)^2^+7.3706P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9592 _refine_ls_number_parameters 611 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_obs 0.0479 _refine_ls_wR_factor_all 0.1477 _refine_ls_wR_factor_obs 0.1165 _refine_ls_goodness_of_fit_all 0.886 _refine_ls_goodness_of_fit_obs 0.846 _refine_ls_restrained_S_all 0.890 _refine_ls_restrained_S_obs 0.846 _refine_ls_shift/esd_max 0.002 _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 Nb Nb 0.35846(2) 0.19022(2) 0.17890(2) 0.03275(12) Uani 1 d . . O1 O 0.4312(2) 0.13309(12) 0.24464(13) 0.0349(6) Uani 1 d . . O2 O 0.3018(2) 0.23390(13) 0.09378(13) 0.0384(6) Uani 1 d . . N1 N 0.4922(2) 0.22614(14) 0.15681(14) 0.0310(7) Uani 1 d . . N2 N 0.3967(2) 0.11730(15) 0.0924(2) 0.0353(7) Uani 1 d . . N3 N 0.3280(2) 0.2633(2) 0.2414(2) 0.0397(8) Uani 1 d . . N4 N 0.2351(2) 0.1364(2) 0.1890(2) 0.0446(8) Uani 1 d . . N5 N 0.7188(3) 0.2753(2) 0.1707(2) 0.0462(9) Uani 1 d . . H5N H 0.7011(34) 0.2505(23) 0.1381(23) 0.055(15) Uiso 1 d . . C1 C 0.5248(3) 0.1258(2) 0.2683(2) 0.0335(8) Uani 1 d . . C2 C 0.5515(3) 0.0736(2) 0.3133(2) 0.0373(9) Uani 1 d . . C3 C 0.6499(3) 0.0680(2) 0.3324(2) 0.0445(10) Uani 1 d . . H3 H 0.6683(3) 0.0336(2) 0.3612(2) 0.053 Uiso 1 calc R . C4 C 0.7228(3) 0.1103(2) 0.3114(2) 0.0433(10) Uani 1 d . . C5 C 0.6934(3) 0.1629(2) 0.2710(2) 0.0396(9) Uani 1 d . . H5 H 0.7399(3) 0.1931(2) 0.2573(2) 0.047 Uiso 1 calc R . C6 C 0.5957(3) 0.1717(2) 0.2502(2) 0.0332(8) Uani 1 d . . C7 C 0.5596(3) 0.2361(2) 0.2174(2) 0.0331(8) Uani 1 d . . H7 H 0.5158(3) 0.2537(2) 0.2511(2) 0.040 Uiso 1 calc R . C8 C 0.5328(3) 0.2327(2) 0.0918(2) 0.0344(8) Uani 1 d . . C9 C 0.5280(3) 0.2933(2) 0.0596(2) 0.0415(9) Uani 1 d . . H9 H 0.4984(3) 0.3287(2) 0.0806(2) 0.050 Uiso 1 calc R . C10 C 0.5665(3) 0.3017(2) -0.0031(2) 0.0507(11) Uani 1 d . . H10 H 0.5655(3) 0.3430(2) -0.0235(2) 0.061 Uiso 1 calc R . C11 C 0.6065(3) 0.2489(2) -0.0354(2) 0.0534(11) Uani 1 d . . H11 H 0.6331(3) 0.2552(2) -0.0775(2) 0.064 Uiso 1 calc R . C12 C 0.6083(3) 0.1863(2) -0.0068(2) 0.0449(10) Uani 1 d . . C13 C 0.5737(3) 0.1785(2) 0.0589(2) 0.0348(8) Uani 1 d . . C14 C 0.5743(3) 0.1116(2) 0.0906(2) 0.0341(8) Uani 1 d . . C15 C 0.6617(3) 0.0776(2) 0.1064(2) 0.0399(9) Uani 1 d . . C16 C 0.6564(3) 0.0129(2) 0.1280(2) 0.0474(11) Uani 1 d . . H16 H 0.7139(3) -0.0098(2) 0.1391(2) 0.057 Uiso 1 calc R . C17 C 0.5688(3) -0.0182(2) 0.1334(2) 0.0530(11) Uani 1 d . . H17 H 0.5674(3) -0.0623(2) 0.1462(2) 0.064 Uiso 1 calc R . C18 C 0.4820(3) 0.0149(2) 0.1202(2) 0.0453(10) Uani 1 d . . H18 H 0.4222(3) -0.0061(2) 0.1246(2) 0.054 Uiso 1 calc R . C19 C 0.4860(3) 0.0800(2) 0.1003(2) 0.0352(9) Uani 1 d . . C20 C 0.3415(3) 0.1079(2) 0.0391(2) 0.0398(9) Uani 1 d . . H20 H 0.3575(3) 0.0730(2) 0.0111(2) 0.048 Uiso 1 calc R . C21 C 0.2570(3) 0.1466(2) 0.0188(2) 0.0407(9) Uani 1 d . . C22 C 0.1911(3) 0.1207(2) -0.0302(2) 0.0487(11) Uani 1 d . . H22 H 0.2003(3) 0.0780(2) -0.0456(2) 0.058 Uiso 1 calc R . C23 C 0.1136(3) 0.1564(3) -0.0560(2) 0.0541(12) Uani 1 d . . C24 C 0.1105(3) 0.2230(2) -0.0370(2) 0.0530(11) Uani 1 d . . H24 H 0.0612(3) 0.2490(2) -0.0567(2) 0.064 Uiso 1 calc R . C25 C 0.1753(3) 0.2527(2) 0.0089(2) 0.0451(10) Uani 1 d . . C26 C 0.2462(3) 0.2118(2) 0.0426(2) 0.0396(9) Uani 1 d . . C27 C 0.6436(4) 0.1288(3) -0.0470(2) 0.0679(14) Uani 1 d . . H27A H 0.6264(24) 0.0885(3) -0.0250(10) 0.102 Uiso 1 calc R . H27B H 0.7134(5) 0.1312(10) -0.0500(16) 0.102 Uiso 1 calc R . H27C H 0.6135(21) 0.1299(10) -0.0917(6) 0.102 Uiso 1 calc R . C28 C 0.7604(3) 0.1097(2) 0.1035(3) 0.0575(12) Uani 1 d . . H28A H 0.7812(11) 0.1243(15) 0.1480(4) 0.086 Uiso 1 calc R . H28B H 0.7563(6) 0.1468(10) 0.0734(13) 0.086 Uiso 1 calc R . H28C H 0.8068(6) 0.0785(5) 0.0873(16) 0.086 Uiso 1 calc R . C29 C 0.4760(3) 0.0272(2) 0.3434(2) 0.0429(10) Uani 1 d . . C30 C 0.4311(4) -0.0178(2) 0.2882(2) 0.0554(12) Uani 1 d . . H30A H 0.4020(4) 0.0086(2) 0.2525(2) 0.083 Uiso 1 calc R . H30B H 0.3818(4) -0.0451(2) 0.3072(2) 0.083 Uiso 1 calc R . H30C H 0.4813(4) -0.0451(2) 0.2704(2) 0.083 Uiso 1 calc R . C31 C 0.3956(3) 0.0678(2) 0.3760(2) 0.0569(12) Uani 1 d . . H31A H 0.3654(3) 0.0965(2) 0.3428(2) 0.085 Uiso 1 calc R . H31B H 0.4239(3) 0.0936(2) 0.4125(2) 0.085 Uiso 1 calc R . H31C H 0.3472(3) 0.0386(2) 0.3932(2) 0.085 Uiso 1 calc R . C32 C 0.5211(4) -0.0173(3) 0.3987(3) 0.0671(14) Uani 1 d . . H32A H 0.5500(4) 0.0093(3) 0.4343(3) 0.101 Uiso 1 calc R . H32B H 0.5704(4) -0.0446(3) 0.3798(3) 0.101 Uiso 1 calc R . H32C H 0.4710(4) -0.0446(3) 0.4167(3) 0.101 Uiso 1 calc R . C33 C 0.8294(3) 0.1008(3) 0.3351(3) 0.0598(13) Uani 1 d . . C37 C 0.1682(3) 0.3265(2) 0.0257(3) 0.0544(12) Uani 1 d . . C38 C 0.2671(4) 0.3596(3) 0.0214(3) 0.075(2) Uani 1 d . . H38A H 0.3137(4) 0.3376(3) 0.0512(3) 0.113 Uiso 1 calc R . H38B H 0.2618(4) 0.4049(3) 0.0346(3) 0.113 Uiso 1 calc R . H38C H 0.2884(4) 0.3572(3) -0.0242(3) 0.113 Uiso 1 calc R . C39 C 0.1320(4) 0.3343(3) 0.0977(3) 0.077(2) Uani 1 d . . H39A H 0.0693(4) 0.3134(3) 0.1007(3) 0.115 Uiso 1 calc R . H39B H 0.1261(4) 0.3803(3) 0.1082(3) 0.115 Uiso 1 calc R . H39C H 0.1779(4) 0.3140(3) 0.1293(3) 0.115 Uiso 1 calc R . C40 C 0.0957(5) 0.3622(3) -0.0219(4) 0.105(2) Uani 1 d . . H40A H 0.0325(5) 0.3418(3) -0.0198(4) 0.157 Uiso 1 calc R . H40B H 0.1177(5) 0.3597(3) -0.0674(4) 0.157 Uiso 1 calc R . H40C H 0.0912(5) 0.4075(3) -0.0085(4) 0.157 Uiso 1 calc R . C41 C 0.0304(3) 0.1268(3) -0.1014(3) 0.069(2) Uani 1 d . . C42 C 0.0524(5) 0.0581(4) -0.1234(4) 0.113(3) Uani 1 d . . H42A H 0.1127(5) 0.0578(4) -0.1467(4) 0.170 Uiso 1 calc R . H42B H 0.0003(5) 0.0425(4) -0.1532(4) 0.170 Uiso 1 calc R . H42C H 0.0583(5) 0.0300(4) -0.0844(4) 0.170 Uiso 1 calc R . C43 C 0.0175(5) 0.1683(4) -0.1677(3) 0.106(2) Uani 1 d . . H43A H 0.0032(5) 0.2132(4) -0.1564(3) 0.160 Uiso 1 calc R . H43B H -0.0354(5) 0.1505(4) -0.1954(3) 0.160 Uiso 1 calc R . H43C H 0.0768(5) 0.1667(4) -0.1921(3) 0.160 Uiso 1 calc R . C44 C -0.0633(4) 0.1310(5) -0.0645(4) 0.138(4) Uani 1 d . . H44A H -0.0744(4) 0.1758(5) -0.0513(4) 0.208 Uiso 1 calc R . H44B H -0.0586(4) 0.1037(5) -0.0248(4) 0.208 Uiso 1 calc R . H44C H -0.1167(4) 0.1162(5) -0.0936(4) 0.208 Uiso 1 calc R . C45 C 0.6330(3) 0.2928(2) 0.2090(2) 0.0399(9) Uani 1 d . . H45 H 0.5983(3) 0.3276(2) 0.1834(2) 0.048 Uiso 1 calc R . C46 C 0.7670(4) 0.3327(3) 0.1415(3) 0.076(2) Uani 1 d . . H46A H 0.7984(4) 0.3586(3) 0.1774(3) 0.091 Uiso 1 calc R . H46B H 0.7185(4) 0.3602(3) 0.1181(3) 0.091 Uiso 1 calc R . C47 C 0.8415(5) 0.3112(4) 0.0931(4) 0.122(3) Uani 1 d . . H47A H 0.8724(5) 0.3492(4) 0.0745(4) 0.183 Uiso 1 calc R . H47B H 0.8102(5) 0.2861(4) 0.0572(4) 0.183 Uiso 1 calc R . H47C H 0.8899(5) 0.2844(4) 0.1164(4) 0.183 Uiso 1 calc R . C48 C 0.6649(4) 0.3222(2) 0.2773(2) 0.0538(12) Uani 1 d . . H48A H 0.7105(4) 0.3573(2) 0.2706(2) 0.081 Uiso 1 calc R . H48B H 0.6956(4) 0.2887(2) 0.3050(2) 0.081 Uiso 1 calc R . H48C H 0.6087(4) 0.3390(2) 0.2992(2) 0.081 Uiso 1 calc R . C49 C 0.2961(3) 0.2497(2) 0.3105(2) 0.0520(11) Uani 1 d . . H49A H 0.2740(3) 0.2044(2) 0.3128(2) 0.062 Uiso 1 calc R . H49B H 0.2410(3) 0.2779(2) 0.3197(2) 0.062 Uiso 1 calc R . C50 C 0.3762(4) 0.2607(3) 0.3648(2) 0.0709(15) Uani 1 d . . H50A H 0.3512(4) 0.2511(3) 0.4085(2) 0.106 Uiso 1 calc R . H50B H 0.3974(4) 0.3058(3) 0.3637(2) 0.106 Uiso 1 calc R . H50C H 0.4305(4) 0.2322(3) 0.3567(2) 0.106 Uiso 1 calc R . C51 C 0.3534(3) 0.3322(2) 0.2291(2) 0.0488(11) Uani 1 d . . H51A H 0.3646(3) 0.3375(2) 0.1812(2) 0.059 Uiso 1 calc R . H51B H 0.4146(3) 0.3418(2) 0.2536(2) 0.059 Uiso 1 calc R . C52 C 0.2790(4) 0.3820(2) 0.2488(3) 0.0639(13) Uani 1 d . . H52A H 0.3022(4) 0.4255(2) 0.2388(3) 0.096 Uiso 1 calc R . H52B H 0.2686(4) 0.3785(2) 0.2964(3) 0.096 Uiso 1 calc R . H52C H 0.2185(4) 0.3741(2) 0.2238(3) 0.096 Uiso 1 calc R . C53 C 0.1393(3) 0.1688(2) 0.1950(3) 0.0596(13) Uani 1 d . . H53A H 0.1491(3) 0.2160(2) 0.1928(3) 0.072 Uiso 1 calc R . H53B H 0.1153(3) 0.1588(2) 0.2394(3) 0.072 Uiso 1 calc R . C54 C 0.0607(3) 0.1501(3) 0.1425(3) 0.075(2) Uani 1 d . . H54A H 0.0017(3) 0.1738(3) 0.1509(3) 0.113 Uiso 1 calc R . H54B H 0.0484(3) 0.1036(3) 0.1449(3) 0.113 Uiso 1 calc R . H54C H 0.0822(3) 0.1610(3) 0.0982(3) 0.113 Uiso 1 calc R . C55 C 0.2269(3) 0.0646(2) 0.1858(3) 0.0607(13) Uani 1 d . . H55A H 0.2922(3) 0.0462(2) 0.1837(3) 0.073 Uiso 1 calc R . H55B H 0.1913(3) 0.0529(2) 0.1441(3) 0.073 Uiso 1 calc R . C56 C 0.1768(4) 0.0328(3) 0.2441(3) 0.091(2) Uani 1 d . . H56A H 0.1749(4) -0.0141(3) 0.2377(3) 0.136 Uiso 1 calc R . H56B H 0.1113(4) 0.0495(3) 0.2461(3) 0.136 Uiso 1 calc R . H56C H 0.2124(4) 0.0428(3) 0.2857(3) 0.136 Uiso 1 calc R . C34 C 0.8397(11) 0.0894(13) 0.4104(8) 0.154(11) Uani 0.67(2) d P 1 H34A H 0.7979(11) 0.0538(13) 0.4228(8) 0.231 Uiso 0.67(2) calc PR 1 H34B H 0.8214(11) 0.1287(13) 0.4338(8) 0.231 Uiso 0.67(2) calc PR 1 H34C H 0.9065(11) 0.0785(13) 0.4226(8) 0.231 Uiso 0.67(2) calc PR 1 C35 C 0.8948(7) 0.1561(6) 0.3172(9) 0.095(6) Uani 0.67(2) d P 1 H35A H 0.8889(7) 0.1640(6) 0.2694(9) 0.142 Uiso 0.67(2) calc PR 1 H35B H 0.9613(7) 0.1449(6) 0.3297(9) 0.142 Uiso 0.67(2) calc PR 1 H35C H 0.8764(7) 0.1951(6) 0.3411(9) 0.142 Uiso 0.67(2) calc PR 1 C36 C 0.8701(9) 0.0386(7) 0.3009(11) 0.134(8) Uani 0.67(2) d P 1 H36A H 0.8300(9) 0.0013(7) 0.3111(11) 0.201 Uiso 0.67(2) calc PR 1 H36B H 0.9360(9) 0.0308(7) 0.3177(11) 0.201 Uiso 0.67(2) calc PR 1 H36C H 0.8697(9) 0.0451(7) 0.2528(11) 0.201 Uiso 0.67(2) calc PR 1 C34A C 0.8476(21) 0.1676(12) 0.3824(19) 0.120(14) Uani 0.33(2) d P 2 H34D H 0.8050(21) 0.1665(12) 0.4198(19) 0.180 Uiso 0.33(2) calc PR 2 H34E H 0.8340(21) 0.2062(12) 0.3556(19) 0.180 Uiso 0.33(2) calc PR 2 H34F H 0.9145(21) 0.1687(12) 0.3992(19) 0.180 Uiso 0.33(2) calc PR 2 C36A C 0.8375(21) 0.0500(15) 0.3883(19) 0.128(18) Uani 0.33(2) d P 2 H36D H 0.7916(21) 0.0593(15) 0.4226(19) 0.192 Uiso 0.33(2) calc PR 2 H36E H 0.9027(21) 0.0500(15) 0.4082(19) 0.192 Uiso 0.33(2) calc PR 2 H36F H 0.8234(21) 0.0075(15) 0.3688(19) 0.192 Uiso 0.33(2) calc PR 2 C35A C 0.8879(21) 0.0982(32) 0.2804(17) 0.212(35) Uani 0.33(2) d P 2 H35D H 0.8732(21) 0.1349(32) 0.2510(17) 0.318 Uiso 0.33(2) calc PR 2 H35E H 0.8760(21) 0.0578(32) 0.2561(17) 0.318 Uiso 0.33(2) calc PR 2 H35F H 0.9554(21) 0.1002(32) 0.2957(17) 0.318 Uiso 0.33(2) calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb 0.0310(2) 0.0314(2) 0.0359(2) -0.0046(2) 0.00138(13) 0.0008(2) O1 0.0310(13) 0.0332(14) 0.0407(15) 0.0002(11) 0.0029(11) -0.0010(11) O2 0.0376(14) 0.0360(15) 0.0408(15) -0.0047(12) -0.0079(12) 0.0027(12) N1 0.033(2) 0.029(2) 0.031(2) -0.0034(13) 0.0011(13) -0.0011(13) N2 0.032(2) 0.032(2) 0.042(2) -0.0055(14) -0.0015(14) 0.0013(13) N3 0.042(2) 0.034(2) 0.044(2) -0.0059(15) 0.0082(15) -0.0006(15) N4 0.037(2) 0.039(2) 0.058(2) -0.003(2) 0.005(2) -0.003(2) N5 0.042(2) 0.049(2) 0.047(2) 0.004(2) 0.001(2) -0.009(2) C1 0.037(2) 0.030(2) 0.033(2) -0.006(2) 0.000(2) -0.001(2) C2 0.046(2) 0.031(2) 0.035(2) 0.000(2) -0.001(2) -0.001(2) C3 0.051(2) 0.039(2) 0.043(2) 0.009(2) -0.009(2) 0.003(2) C4 0.044(2) 0.043(2) 0.042(2) 0.001(2) -0.007(2) -0.004(2) C5 0.042(2) 0.038(2) 0.038(2) 0.004(2) -0.003(2) -0.004(2) C6 0.038(2) 0.034(2) 0.028(2) -0.003(2) 0.000(2) 0.000(2) C7 0.038(2) 0.032(2) 0.029(2) -0.002(2) 0.001(2) -0.002(2) C8 0.033(2) 0.039(2) 0.031(2) 0.001(2) -0.003(2) 0.000(2) C9 0.044(2) 0.039(2) 0.041(2) 0.005(2) -0.003(2) 0.004(2) C10 0.066(3) 0.041(2) 0.044(2) 0.011(2) -0.004(2) 0.001(2) C11 0.066(3) 0.059(3) 0.035(2) 0.008(2) 0.008(2) 0.000(2) C12 0.051(2) 0.052(3) 0.032(2) -0.003(2) 0.002(2) 0.000(2) C13 0.032(2) 0.041(2) 0.031(2) -0.001(2) 0.000(2) 0.003(2) C14 0.040(2) 0.036(2) 0.027(2) -0.005(2) 0.000(2) 0.005(2) C15 0.041(2) 0.045(2) 0.034(2) -0.007(2) 0.001(2) 0.008(2) C16 0.049(3) 0.047(3) 0.046(2) -0.002(2) 0.002(2) 0.019(2) C17 0.062(3) 0.035(2) 0.063(3) 0.004(2) 0.007(2) 0.014(2) C18 0.048(2) 0.036(2) 0.052(3) -0.004(2) 0.007(2) 0.000(2) C19 0.040(2) 0.035(2) 0.031(2) -0.008(2) -0.002(2) 0.007(2) C20 0.041(2) 0.035(2) 0.043(2) -0.011(2) -0.001(2) 0.000(2) C21 0.037(2) 0.043(2) 0.041(2) -0.006(2) -0.006(2) 0.002(2) C22 0.041(2) 0.055(3) 0.050(3) -0.016(2) -0.007(2) 0.003(2) C23 0.037(2) 0.069(3) 0.056(3) -0.013(2) -0.008(2) 0.000(2) C24 0.042(2) 0.059(3) 0.057(3) -0.004(2) -0.012(2) 0.011(2) C25 0.039(2) 0.050(3) 0.047(2) 0.001(2) -0.004(2) 0.009(2) C26 0.031(2) 0.046(2) 0.041(2) -0.002(2) -0.003(2) 0.003(2) C27 0.092(4) 0.069(3) 0.045(3) -0.009(2) 0.021(3) 0.007(3) C28 0.041(2) 0.067(3) 0.064(3) -0.001(2) 0.002(2) 0.009(2) C29 0.051(2) 0.033(2) 0.045(2) 0.005(2) 0.004(2) -0.002(2) C30 0.063(3) 0.042(2) 0.062(3) -0.002(2) 0.004(2) -0.014(2) C31 0.064(3) 0.049(3) 0.060(3) -0.001(2) 0.021(2) -0.009(2) C32 0.075(3) 0.058(3) 0.069(3) 0.024(3) 0.007(3) -0.007(3) C33 0.042(3) 0.064(3) 0.072(3) 0.016(3) -0.017(2) -0.001(2) C37 0.049(3) 0.048(3) 0.065(3) -0.002(2) -0.014(2) 0.010(2) C38 0.071(4) 0.053(3) 0.102(4) 0.017(3) 0.005(3) -0.003(3) C39 0.073(4) 0.062(3) 0.094(4) -0.021(3) 0.008(3) 0.011(3) C40 0.113(5) 0.060(4) 0.135(6) -0.005(4) -0.066(5) 0.028(4) C41 0.042(3) 0.085(4) 0.077(4) -0.026(3) -0.021(2) 0.008(3) C42 0.083(4) 0.106(5) 0.146(6) -0.057(5) -0.055(4) -0.001(4) C43 0.089(5) 0.130(6) 0.096(5) -0.027(4) -0.049(4) 0.014(4) C44 0.050(4) 0.217(10) 0.149(7) -0.078(7) 0.007(4) -0.035(5) C45 0.047(2) 0.036(2) 0.036(2) 0.001(2) -0.004(2) -0.007(2) C46 0.063(3) 0.077(4) 0.089(4) 0.022(3) 0.017(3) -0.019(3) C47 0.080(4) 0.142(7) 0.149(7) 0.047(6) 0.059(5) -0.006(4) C48 0.066(3) 0.045(3) 0.049(3) -0.007(2) -0.012(2) -0.013(2) C49 0.059(3) 0.048(3) 0.050(3) -0.009(2) 0.018(2) 0.000(2) C50 0.101(4) 0.070(3) 0.041(3) -0.005(2) 0.006(3) -0.005(3) C51 0.063(3) 0.033(2) 0.051(3) -0.005(2) 0.010(2) 0.001(2) C52 0.071(3) 0.046(3) 0.074(3) -0.013(2) -0.003(3) 0.010(2) C53 0.041(2) 0.055(3) 0.084(4) -0.004(3) 0.012(2) -0.003(2) C54 0.042(3) 0.086(4) 0.098(4) 0.003(3) 0.000(3) -0.002(3) C55 0.047(3) 0.045(3) 0.089(4) 0.001(3) 0.001(3) -0.009(2) C56 0.068(4) 0.077(4) 0.128(6) 0.031(4) 0.009(4) -0.015(3) C34 0.084(9) 0.293(32) 0.081(9) 0.062(14) -0.055(7) -0.080(14) C35 0.032(5) 0.086(8) 0.163(17) 0.047(8) -0.036(7) -0.011(5) C36 0.063(7) 0.109(10) 0.226(23) -0.047(11) -0.060(10) 0.036(7) C34A 0.086(17) 0.106(18) 0.162(32) -0.024(18) -0.070(20) -0.003(14) C36A 0.078(15) 0.111(20) 0.187(40) 0.087(24) -0.113(21) -0.028(16) C35A 0.071(21) 0.436(100) 0.130(27) 0.088(44) 0.035(18) 0.136(43) _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 Nb O1 1.979(3) . ? Nb N3 1.984(3) . ? Nb N4 2.025(3) . ? Nb O2 2.028(3) . ? Nb N1 2.032(3) . ? Nb N2 2.336(3) . ? O1 C1 1.354(4) . ? O2 C26 1.320(5) . ? N1 C8 1.425(5) . ? N1 C7 1.495(4) . ? N2 C20 1.286(5) . ? N2 C19 1.439(5) . ? N3 C51 1.463(5) . ? N3 C49 1.476(5) . ? N4 C55 1.462(6) . ? N4 C53 1.474(5) . ? N5 C45 1.465(5) . ? N5 C46 1.468(6) . ? C1 C6 1.400(5) . ? C1 C2 1.421(5) . ? C2 C3 1.387(5) . ? C2 C29 1.534(5) . ? C3 C4 1.392(6) . ? C4 C5 1.384(6) . ? C4 C33 1.525(6) . ? C5 C6 1.393(5) . ? C6 C7 1.530(5) . ? C7 C45 1.540(5) . ? C8 C9 1.386(5) . ? C8 C13 1.405(5) . ? C9 C10 1.377(6) . ? C10 C11 1.372(6) . ? C11 C12 1.389(6) . ? C12 C13 1.410(5) . ? C12 C27 1.502(6) . ? C13 C14 1.494(5) . ? C14 C19 1.387(5) . ? C14 C15 1.404(5) . ? C15 C16 1.383(6) . ? C15 C28 1.501(6) . ? C16 C17 1.363(6) . ? C17 C18 1.379(6) . ? C18 C19 1.380(6) . ? C20 C21 1.439(5) . ? C21 C22 1.399(5) . ? C21 C26 1.414(6) . ? C22 C23 1.365(6) . ? C23 C24 1.403(7) . ? C23 C41 1.542(6) . ? C24 C25 1.382(6) . ? C25 C26 1.422(5) . ? C25 C37 1.538(6) . ? C29 C32 1.529(6) . ? C29 C30 1.532(6) . ? C29 C31 1.535(6) . ? C33 C35A 1.37(3) . ? C33 C36A 1.47(3) . ? C33 C35 1.486(10) . ? C33 C34 1.51(2) . ? C33 C36 1.545(13) . ? C33 C34A 1.66(2) . ? C37 C38 1.515(7) . ? C37 C40 1.521(7) . ? C37 C39 1.534(7) . ? C41 C42 1.492(8) . ? C41 C44 1.502(8) . ? C41 C43 1.562(9) . ? C45 C48 1.523(6) . ? C46 C47 1.489(8) . ? C49 C50 1.519(7) . ? C51 C52 1.496(6) . ? C53 C54 1.512(7) . ? C55 C56 1.508(7) . ? 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 O1 Nb N3 98.12(13) . . ? O1 Nb N4 91.02(13) . . ? N3 Nb N4 98.38(14) . . ? O1 Nb O2 164.99(10) . . ? N3 Nb O2 96.16(13) . . ? N4 Nb O2 91.47(13) . . ? O1 Nb N1 85.31(11) . . ? N3 Nb N1 94.49(13) . . ? N4 Nb N1 167.00(12) . . ? O2 Nb N1 88.98(11) . . ? O1 Nb N2 89.35(11) . . ? N3 Nb N2 170.87(12) . . ? N4 Nb N2 86.68(13) . . ? O2 Nb N2 76.02(11) . . ? N1 Nb N2 80.83(11) . . ? C1 O1 Nb 137.2(2) . . ? C26 O2 Nb 132.6(3) . . ? C8 N1 C7 117.4(3) . . ? C8 N1 Nb 127.8(2) . . ? C7 N1 Nb 114.0(2) . . ? C20 N2 C19 118.7(3) . . ? C20 N2 Nb 123.5(3) . . ? C19 N2 Nb 117.8(2) . . ? C51 N3 C49 114.4(3) . . ? C51 N3 Nb 123.6(3) . . ? C49 N3 Nb 120.9(3) . . ? C55 N4 C53 112.3(3) . . ? C55 N4 Nb 126.6(3) . . ? C53 N4 Nb 120.9(3) . . ? C45 N5 C46 113.1(4) . . ? O1 C1 C6 119.6(3) . . ? O1 C1 C2 120.9(3) . . ? C6 C1 C2 119.5(3) . . ? C3 C2 C1 117.0(4) . . ? C3 C2 C29 120.3(3) . . ? C1 C2 C29 122.7(3) . . ? C2 C3 C4 124.6(4) . . ? C5 C4 C3 116.9(4) . . ? C5 C4 C33 121.9(4) . . ? C3 C4 C33 121.2(4) . . ? C4 C5 C6 121.5(4) . . ? C5 C6 C1 120.3(3) . . ? C5 C6 C7 121.6(3) . . ? C1 C6 C7 117.5(3) . . ? N1 C7 C6 113.7(3) . . ? N1 C7 C45 113.4(3) . . ? C6 C7 C45 118.9(3) . . ? C9 C8 C13 119.7(3) . . ? C9 C8 N1 118.9(3) . . ? C13 C8 N1 121.4(3) . . ? C10 C9 C8 120.7(4) . . ? C11 C10 C9 119.7(4) . . ? C10 C11 C12 121.7(4) . . ? C11 C12 C13 118.5(4) . . ? C11 C12 C27 119.8(4) . . ? C13 C12 C27 121.7(4) . . ? C8 C13 C12 119.5(4) . . ? C8 C13 C14 120.8(3) . . ? C12 C13 C14 119.6(3) . . ? C19 C14 C15 118.7(4) . . ? C19 C14 C13 119.2(3) . . ? C15 C14 C13 122.0(3) . . ? C16 C15 C14 118.7(4) . . ? C16 C15 C28 118.7(4) . . ? C14 C15 C28 122.5(4) . . ? C17 C16 C15 121.4(4) . . ? C16 C17 C18 120.7(4) . . ? C17 C18 C19 118.5(4) . . ? C18 C19 C14 121.7(4) . . ? C18 C19 N2 119.5(4) . . ? C14 C19 N2 118.7(3) . . ? N2 C20 C21 125.8(4) . . ? C22 C21 C26 120.5(4) . . ? C22 C21 C20 118.4(4) . . ? C26 C21 C20 120.7(3) . . ? C23 C22 C21 122.0(4) . . ? C22 C23 C24 116.2(4) . . ? C22 C23 C41 123.7(4) . . ? C24 C23 C41 120.1(4) . . ? C25 C24 C23 124.8(4) . . ? C24 C25 C26 117.4(4) . . ? C24 C25 C37 121.5(4) . . ? C26 C25 C37 121.0(4) . . ? O2 C26 C21 120.6(3) . . ? O2 C26 C25 121.5(4) . . ? C21 C26 C25 118.0(4) . . ? C32 C29 C30 107.2(4) . . ? C32 C29 C2 112.4(4) . . ? C30 C29 C2 110.3(3) . . ? C32 C29 C31 106.9(4) . . ? C30 C29 C31 110.2(4) . . ? C2 C29 C31 109.7(3) . . ? C35A C33 C36A 120.5(23) . . ? C35 C33 C34 108.5(9) . . ? C35A C33 C4 110.0(13) . . ? C36A C33 C4 110.6(11) . . ? C35 C33 C4 114.0(5) . . ? C34 C33 C4 112.0(8) . . ? C35 C33 C36 106.4(9) . . ? C34 C33 C36 106.6(11) . . ? C4 C33 C36 109.0(6) . . ? C35A C33 C34A 113.3(26) . . ? C36A C33 C34A 99.5(17) . . ? C4 C33 C34A 100.9(9) . . ? C38 C37 C40 108.4(5) . . ? C38 C37 C39 109.1(4) . . ? C40 C37 C39 107.4(5) . . ? C38 C37 C25 110.8(4) . . ? C40 C37 C25 112.1(4) . . ? C39 C37 C25 109.0(4) . . ? C42 C41 C44 112.3(6) . . ? C42 C41 C23 112.4(4) . . ? C44 C41 C23 108.5(5) . . ? C42 C41 C43 106.1(5) . . ? C44 C41 C43 107.9(6) . . ? C23 C41 C43 109.5(5) . . ? N5 C45 C48 110.2(4) . . ? N5 C45 C7 114.4(3) . . ? C48 C45 C7 111.2(3) . . ? N5 C46 C47 110.4(5) . . ? N3 C49 C50 113.3(4) . . ? N3 C51 C52 115.7(4) . . ? N4 C53 C54 116.3(4) . . ? N4 C55 C56 115.4(5) . . ? _refine_diff_density_max 0.457 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.060