# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kawaguchi, Hiroyuki' _publ_contact_author_email hkawa@chem.titech.ac.jp _publ_section_title ; Synthesis and reactivity of niobium complexes having a tripodal triaryloxide ligand in bidentate, tridentate, and tetradentate coordination modes ; loop_ _publ_author_name F.Akagi Yu.Ishida T.Matsuo H.Kawaguchi #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #===END #============================================================================== data___[NEt3H][(anti-O3)NbCl3] _database_code_depnum_ccdc_archive 'CCDC 655244' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C56 H85 Cl3 N Nb O3 ' _chemical_formula_moiety 'C56 H85 Cl3 N Nb O3 ' _chemical_formula_weight 1019.56 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 47.957(11) _cell_length_b 13.286(3) _cell_length_c 19.889(5) _cell_angle_alpha 90.0000 _cell_angle_beta 116.905(3) _cell_angle_gamma 90.0000 _cell_volume 11300(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 13275 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4352.00 _exptl_absorpt_coefficient_mu 0.395 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 43895 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 62 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12900 _reflns_number_gt 10484 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2241 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 12900 _refine_ls_number_parameters 581 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1068P)^2^+66.2115P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.85 _refine_diff_density_min -3.36 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Nb Nb -2.073 0.621 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Nb(1) Nb 0.176610(8) 0.20825(3) 0.73183(2) 0.02723(13) Uani 1.00 1 d . . . Cl(1) Cl 0.22819(3) 0.19137(11) 0.73481(8) 0.0512(3) Uani 1.00 1 d . . . Cl(2) Cl 0.20358(3) 0.20428(9) 0.87065(6) 0.0457(3) Uani 1.00 1 d . . . Cl(3) Cl 0.18679(3) 0.38739(9) 0.74435(7) 0.0520(3) Uani 1.00 1 d . . . O(1) O 0.17345(6) 0.0669(2) 0.73198(16) 0.0272(6) Uani 1.00 1 d . . . O(2) O 0.13789(7) 0.2196(2) 0.73366(16) 0.0285(6) Uani 1.00 1 d . . . O(3) O 0.15696(6) 0.2180(2) 0.62596(16) 0.0261(5) Uani 1.00 1 d . . . N(1) N 0.27147(13) 0.3605(4) 0.8948(2) 0.0528(12) Uani 1.00 1 d . . . C(1) C 0.10764(8) 0.0643(2) 0.6044(2) 0.0179(6) Uani 1.00 1 d . . . C(2) C 0.12848(9) -0.0251(2) 0.6491(2) 0.0205(7) Uani 1.00 1 d . . . C(3) C 0.15855(9) -0.0234(2) 0.7102(2) 0.0217(7) Uani 1.00 1 d . . . C(4) C 0.17374(9) -0.1123(3) 0.7480(2) 0.0244(7) Uani 1.00 1 d . . . C(5) C 0.15890(10) -0.2029(3) 0.7185(2) 0.0279(8) Uani 1.00 1 d . . . C(6) C 0.12947(10) -0.2096(2) 0.6556(2) 0.0269(8) Uani 1.00 1 d . . . C(7) C 0.11494(9) -0.1200(3) 0.6239(2) 0.0245(7) Uani 1.00 1 d . . . C(8) C 0.09270(9) 0.1331(2) 0.6424(2) 0.0205(7) Uani 1.00 1 d . . . C(9) C 0.10671(9) 0.2019(2) 0.7027(2) 0.0230(7) Uani 1.00 1 d . . . C(10) C 0.08872(11) 0.2528(3) 0.7320(2) 0.0289(8) Uani 1.00 1 d . . . C(11) C 0.05671(11) 0.2386(3) 0.6972(2) 0.0324(9) Uani 1.00 1 d . . . C(12) C 0.04155(10) 0.1756(3) 0.6355(2) 0.0280(8) Uani 1.00 1 d . . . C(13) C 0.06019(9) 0.1238(3) 0.6103(2) 0.0232(7) Uani 1.00 1 d . . . C(14) C 0.11542(8) 0.1122(2) 0.5447(2) 0.0190(7) Uani 1.00 1 d . . . C(15) C 0.13718(9) 0.1888(2) 0.5546(2) 0.0201(7) Uani 1.00 1 d . . . C(16) C 0.13906(9) 0.2339(2) 0.4921(2) 0.0224(7) Uani 1.00 1 d . . . C(17) C 0.12037(10) 0.1935(3) 0.4216(2) 0.0253(8) Uani 1.00 1 d . . . C(18) C 0.09984(10) 0.1135(3) 0.4089(2) 0.0270(8) Uani 1.00 1 d . . . C(19) C 0.09733(9) 0.0765(3) 0.4707(2) 0.0233(7) Uani 1.00 1 d . . . C(20) C 0.20414(10) -0.1126(3) 0.8229(2) 0.0346(9) Uani 1.00 1 d . . . C(21) C 0.19595(12) -0.0638(4) 0.8822(2) 0.0444(12) Uani 1.00 1 d . . . C(22) C 0.21603(11) -0.2188(3) 0.8504(3) 0.0428(11) Uani 1.00 1 d . . . C(23) C 0.23093(12) -0.0564(4) 0.8180(3) 0.0575(16) Uani 1.00 1 d . . . C(24) C 0.11341(13) -0.3108(3) 0.6250(2) 0.0386(11) Uani 1.00 1 d . . . C(25) C 0.10122(17) -0.3152(4) 0.5393(3) 0.0574(16) Uani 1.00 1 d . . . C(26) C 0.08607(14) -0.3213(4) 0.6442(3) 0.0541(14) Uani 1.00 1 d . . . C(27) C 0.13528(14) -0.4006(3) 0.6594(3) 0.0516(13) Uani 1.00 1 d . . . C(28) C 0.10397(14) 0.3255(4) 0.8000(2) 0.0438(11) Uani 1.00 1 d . . . C(29) C 0.11730(19) 0.4160(4) 0.7768(4) 0.0685(19) Uani 1.00 1 d . . . C(30) C 0.12954(16) 0.2706(5) 0.8686(3) 0.0648(17) Uani 1.00 1 d . . . C(31) C 0.07998(17) 0.3647(5) 0.8253(3) 0.0636(17) Uani 1.00 1 d . . . C(32) C 0.00585(11) 0.1615(4) 0.5948(2) 0.0412(11) Uani 1.00 1 d . . . C(33) C -0.00671(13) 0.1969(5) 0.5128(3) 0.0608(17) Uani 1.00 1 d . . . C(34) C -0.00210(12) 0.0481(4) 0.5942(3) 0.0522(13) Uani 1.00 1 d . . . C(35) C -0.01041(14) 0.2167(5) 0.6341(4) 0.070(2) Uani 1.00 1 d . . . C(36) C 0.16022(10) 0.3250(3) 0.5002(2) 0.0298(8) Uani 1.00 1 d . . . C(37) C 0.15510(12) 0.3642(4) 0.4228(2) 0.0425(11) Uani 1.00 1 d . . . C(38) C 0.19491(11) 0.2934(4) 0.5431(3) 0.0467(12) Uani 1.00 1 d . . . C(39) C 0.15249(15) 0.4104(3) 0.5403(3) 0.0501(13) Uani 1.00 1 d . . . C(40) C 0.08044(12) 0.0725(3) 0.3286(2) 0.0383(10) Uani 1.00 1 d . . . C(41) C 0.06357(18) -0.0243(5) 0.3281(3) 0.0676(19) Uani 1.00 1 d . . . C(42) C 0.05755(19) 0.1517(6) 0.2804(3) 0.082(2) Uani 1.00 1 d . . . C(43) C 0.10206(19) 0.0466(6) 0.2931(4) 0.084(2) Uani 1.00 1 d . . . C(44) C 0.25530(17) 0.4163(5) 0.9323(4) 0.075(2) Uani 1.00 1 d . . . C(45) C 0.2437(2) 0.5198(6) 0.9002(5) 0.126(4) Uani 1.00 1 d . . . C(46) C 0.28404(15) 0.2639(5) 0.9351(4) 0.0654(17) Uani 1.00 1 d . . . C(47) C 0.30015(19) 0.2002(7) 0.9052(4) 0.098(3) Uani 1.00 1 d . . . C(48) C 0.2853(9) 0.432(2) 0.8709(18) 0.141(15) Uani 0.50 1 d P . . C(49) C 0.3130(8) 0.478(2) 0.934(2) 0.20(2) Uani 0.50 1 d P . . C(50) C 0.3018(3) 0.420(2) 0.8935(12) 0.072(6) Uani 0.50 1 d P . . C(51) C 0.3257(4) 0.442(2) 0.9749(10) 0.069(5) Uani 0.50 1 d P . . C(52) C 0.0442(6) 0.3922(19) 0.4702(15) 0.122(7) Uiso 0.50 1 d P . . C(53) C 0.0197(3) 0.4702(12) 0.4611(9) 0.156(5) Uiso 1.00 1 d . . . C(54) C -0.01140(18) 0.4792(5) 0.3769(4) 0.0225(14) Uiso 0.50 1 d P . . C(55) C -0.0194(3) 0.4433(12) 0.3216(9) 0.162(5) Uiso 1.00 1 d . . . C(56) C 0.0068(8) 0.352(2) 0.3496(19) 0.153(10) Uiso 0.50 1 d P . . C(57) C 0.0316(4) 0.3665(11) 0.4020(9) 0.148(4) Uiso 1.00 1 d . . . C(58) C 0.0694(2) 0.3760(6) 0.5362(5) 0.081(2) Uiso 1.00 1 d . . . C(59) C 0.0089(6) 0.438(2) 0.4018(16) 0.125(7) Uiso 0.50 1 d P . . C(60) C 0.05120(18) 0.4231(5) 0.5475(4) 0.0225(14) Uiso 0.50 1 d P . . C(61) C 0.0578(3) 0.3335(11) 0.4599(8) 0.068(3) Uiso 0.50 1 d P . . H(1) H 0.0896(8) 0.029(2) 0.571(2) 0.006(8) Uiso 1.00 1 c . . . H(2) H 0.1692 -0.2636 0.7420 0.033 Uiso 1.00 1 c R . . H(3) H 0.0946 -0.1227 0.5827 0.029 Uiso 1.00 1 c R . . H(4) H 0.0445 0.2734 0.7164 0.039 Uiso 1.00 1 c R . . H(5) H 0.0502 0.0794 0.5687 0.028 Uiso 1.00 1 c R . . H(6) H 0.1216 0.2222 0.3793 0.030 Uiso 1.00 1 c R . . H(7) H 0.0827 0.0243 0.4630 0.028 Uiso 1.00 1 c R . . H(8) H 0.1994 0.0090 0.8833 0.053 Uiso 1.00 1 c R . . H(9) H 0.2093 -0.0923 0.9320 0.053 Uiso 1.00 1 c R . . H(10) H 0.1740 -0.0771 0.8690 0.053 Uiso 1.00 1 c R . . H(11) H 0.2069 -0.2431 0.8825 0.051 Uiso 1.00 1 c R . . H(12) H 0.2389 -0.2177 0.8793 0.051 Uiso 1.00 1 c R . . H(13) H 0.2100 -0.2637 0.8069 0.051 Uiso 1.00 1 c R . . H(14) H 0.2428 -0.1032 0.8027 0.069 Uiso 1.00 1 c R . . H(15) H 0.2448 -0.0277 0.8674 0.069 Uiso 1.00 1 c R . . H(16) H 0.2224 -0.0022 0.7807 0.069 Uiso 1.00 1 c R . . H(17) H 0.0798 -0.2894 0.5144 0.069 Uiso 1.00 1 c R . . H(18) H 0.1015 -0.3851 0.5239 0.069 Uiso 1.00 1 c R . . H(19) H 0.1146 -0.2740 0.5249 0.069 Uiso 1.00 1 c R . . H(20) H 0.0933 -0.3539 0.6934 0.065 Uiso 1.00 1 c R . . H(21) H 0.0696 -0.3621 0.6056 0.065 Uiso 1.00 1 c R . . H(22) H 0.0778 -0.2544 0.6459 0.065 Uiso 1.00 1 c R . . H(23) H 0.1459 -0.4166 0.6287 0.062 Uiso 1.00 1 c R . . H(24) H 0.1231 -0.4590 0.6610 0.062 Uiso 1.00 1 c R . . H(25) H 0.1509 -0.3837 0.7108 0.062 Uiso 1.00 1 c R . . H(26) H 0.1390 0.4023 0.7878 0.082 Uiso 1.00 1 c R . . H(27) H 0.1166 0.4755 0.8051 0.082 Uiso 1.00 1 c R . . H(28) H 0.1049 0.4284 0.7227 0.082 Uiso 1.00 1 c R . . H(29) H 0.1202 0.2400 0.8985 0.078 Uiso 1.00 1 c R . . H(30) H 0.1456 0.3190 0.8998 0.078 Uiso 1.00 1 c R . . H(31) H 0.1390 0.2180 0.8511 0.078 Uiso 1.00 1 c R . . H(32) H 0.0705 0.4269 0.7980 0.076 Uiso 1.00 1 c R . . H(33) H 0.0905 0.3783 0.8796 0.076 Uiso 1.00 1 c R . . H(34) H 0.0637 0.3140 0.8143 0.076 Uiso 1.00 1 c R . . H(35) H -0.0120 0.2685 0.5095 0.073 Uiso 1.00 1 c R . . H(36) H -0.0255 0.1581 0.4807 0.073 Uiso 1.00 1 c R . . H(37) H 0.0093 0.1866 0.4957 0.073 Uiso 1.00 1 c R . . H(38) H -0.0029 0.0163 0.5488 0.063 Uiso 1.00 1 c R . . H(39) H -0.0224 0.0410 0.5942 0.063 Uiso 1.00 1 c R . . H(40) H 0.0141 0.0153 0.6390 0.063 Uiso 1.00 1 c R . . H(41) H -0.0120 0.1721 0.6715 0.084 Uiso 1.00 1 c R . . H(42) H -0.0314 0.2369 0.5968 0.084 Uiso 1.00 1 c R . . H(43) H 0.0017 0.2766 0.6594 0.084 Uiso 1.00 1 c R . . H(44) H 0.1694 0.3296 0.4076 0.051 Uiso 1.00 1 c R . . H(45) H 0.1592 0.4367 0.4259 0.051 Uiso 1.00 1 c R . . H(46) H 0.1335 0.3512 0.3855 0.051 Uiso 1.00 1 c R . . H(47) H 0.2023 0.3035 0.5973 0.056 Uiso 1.00 1 c R . . H(48) H 0.2074 0.3344 0.5259 0.056 Uiso 1.00 1 c R . . H(49) H 0.1970 0.2222 0.5332 0.056 Uiso 1.00 1 c R . . H(50) H 0.1362 0.4531 0.5029 0.060 Uiso 1.00 1 c R . . H(51) H 0.1713 0.4508 0.5689 0.060 Uiso 1.00 1 c R . . H(52) H 0.1451 0.3822 0.5748 0.060 Uiso 1.00 1 c R . . H(53) H 0.0770 -0.0819 0.3320 0.081 Uiso 1.00 1 c R . . H(54) H 0.0441 -0.0290 0.2809 0.081 Uiso 1.00 1 c R . . H(55) H 0.0587 -0.0246 0.3709 0.081 Uiso 1.00 1 c R . . H(56) H 0.0379 0.1445 0.2838 0.099 Uiso 1.00 1 c R . . H(57) H 0.0536 0.1433 0.2278 0.099 Uiso 1.00 1 c R . . H(58) H 0.0663 0.2187 0.2982 0.099 Uiso 1.00 1 c R . . H(59) H 0.1046 0.1059 0.2670 0.100 Uiso 1.00 1 c R . . H(60) H 0.0929 -0.0085 0.2570 0.100 Uiso 1.00 1 c R . . H(61) H 0.1225 0.0259 0.3327 0.100 Uiso 1.00 1 c R . . H(62) H 0.2699 0.4233 0.9866 0.090 Uiso 1.00 1 c R . . H(63) H 0.2373 0.3758 0.9282 0.090 Uiso 1.00 1 c R . . H(64) H 0.2602 0.5694 0.9262 0.151 Uiso 1.00 1 c R . . H(65) H 0.2253 0.5369 0.9072 0.151 Uiso 1.00 1 c R . . H(66) H 0.2380 0.5200 0.8462 0.151 Uiso 1.00 1 c R . . H(67) H 0.2986 0.2796 0.9882 0.078 Uiso 1.00 1 c R . . H(68) H 0.2664 0.2252 0.9353 0.078 Uiso 1.00 1 c R . . H(69) H 0.2852 0.1539 0.8680 0.118 Uiso 1.00 1 c R . . H(70) H 0.3163 0.1615 0.9463 0.118 Uiso 1.00 1 c R . . H(71) H 0.3099 0.2420 0.8810 0.118 Uiso 1.00 1 c R . . H(72) H 0.261(2) 0.344(7) 0.855(5) 0.11(3) Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb(1) 0.0228(2) 0.0260(2) 0.02138(19) -0.00727(14) -0.00015(14) 0.00199(14) Cl(1) 0.0217(5) 0.0666(8) 0.0549(7) -0.0034(5) 0.0083(5) 0.0277(6) Cl(2) 0.0469(6) 0.0436(6) 0.0230(5) -0.0095(5) -0.0051(4) 0.0001(4) Cl(3) 0.0631(8) 0.0283(6) 0.0391(6) -0.0188(5) 0.0007(5) -0.0018(4) O(1) 0.0196(13) 0.0255(14) 0.0286(14) -0.0007(10) 0.0040(11) 0.0053(11) O(2) 0.0288(14) 0.0276(15) 0.0231(13) -0.0027(11) 0.0065(11) -0.0037(11) O(3) 0.0234(13) 0.0254(14) 0.0219(13) -0.0043(11) 0.0036(10) 0.0015(10) N(1) 0.062(3) 0.054(2) 0.026(2) -0.017(2) 0.005(2) -0.0020(19) C(1) 0.0176(16) 0.0158(16) 0.0178(15) -0.0004(13) 0.0059(13) 0.0024(13) C(2) 0.0228(17) 0.0208(18) 0.0193(16) 0.0033(14) 0.0108(14) 0.0022(13) C(3) 0.0213(17) 0.0233(18) 0.0216(17) -0.0000(14) 0.0107(14) 0.0018(14) C(4) 0.0224(18) 0.029(2) 0.0257(18) 0.0071(15) 0.0138(15) 0.0067(15) C(5) 0.038(2) 0.0220(19) 0.0286(19) 0.0102(16) 0.0197(18) 0.0069(15) C(6) 0.038(2) 0.0197(19) 0.0250(18) 0.0019(16) 0.0157(17) 0.0014(15) C(7) 0.0287(19) 0.0235(19) 0.0208(17) 0.0012(15) 0.0107(15) 0.0010(14) C(8) 0.0232(17) 0.0192(17) 0.0161(15) 0.0025(14) 0.0062(13) 0.0027(13) C(9) 0.0270(18) 0.0194(18) 0.0169(16) -0.0006(14) 0.0050(14) 0.0017(13) C(10) 0.044(2) 0.0226(19) 0.0210(18) 0.0017(17) 0.0159(17) -0.0004(15) C(11) 0.041(2) 0.032(2) 0.029(2) 0.0103(18) 0.0198(19) 0.0011(17) C(12) 0.0250(19) 0.033(2) 0.0254(19) 0.0062(16) 0.0109(16) 0.0048(16) C(13) 0.0233(18) 0.0249(19) 0.0197(16) 0.0002(15) 0.0083(14) -0.0010(14) C(14) 0.0185(16) 0.0187(17) 0.0175(15) 0.0028(13) 0.0061(13) 0.0016(13) C(15) 0.0210(17) 0.0174(17) 0.0196(16) 0.0017(13) 0.0071(14) 0.0000(13) C(16) 0.0233(18) 0.0189(18) 0.0257(18) -0.0003(14) 0.0118(15) 0.0030(14) C(17) 0.0283(19) 0.028(2) 0.0221(18) 0.0001(15) 0.0138(15) 0.0036(15) C(18) 0.030(2) 0.030(2) 0.0213(17) -0.0040(16) 0.0125(15) -0.0031(15) C(19) 0.0269(18) 0.0236(19) 0.0209(17) -0.0044(15) 0.0120(15) -0.0034(14) C(20) 0.024(2) 0.037(2) 0.035(2) 0.0059(17) 0.0070(17) 0.0161(19) C(21) 0.047(2) 0.044(2) 0.024(2) 0.003(2) 0.0004(19) 0.0056(19) C(22) 0.030(2) 0.044(2) 0.048(2) 0.011(2) 0.012(2) 0.020(2) C(23) 0.025(2) 0.058(3) 0.075(4) 0.004(2) 0.010(2) 0.036(3) C(24) 0.056(3) 0.020(2) 0.034(2) 0.0030(19) 0.015(2) 0.0001(17) C(25) 0.091(4) 0.032(2) 0.037(2) -0.004(2) 0.018(2) -0.006(2) C(26) 0.060(3) 0.029(2) 0.070(3) -0.013(2) 0.027(3) -0.002(2) C(27) 0.067(3) 0.020(2) 0.059(3) 0.005(2) 0.021(2) -0.001(2) C(28) 0.060(3) 0.043(2) 0.030(2) -0.005(2) 0.022(2) -0.014(2) C(29) 0.102(5) 0.039(3) 0.077(4) -0.023(3) 0.053(4) -0.035(3) C(30) 0.063(3) 0.097(5) 0.025(2) -0.006(3) 0.011(2) -0.023(2) C(31) 0.081(4) 0.067(4) 0.047(3) 0.004(3) 0.032(3) -0.028(2) C(32) 0.025(2) 0.060(3) 0.039(2) 0.009(2) 0.0153(19) 0.002(2) C(33) 0.034(2) 0.088(4) 0.048(3) 0.014(2) 0.008(2) 0.017(3) C(34) 0.032(2) 0.075(4) 0.051(3) -0.009(2) 0.020(2) -0.008(2) C(35) 0.038(3) 0.098(5) 0.085(4) 0.004(3) 0.036(3) -0.025(4) C(36) 0.030(2) 0.028(2) 0.030(2) -0.0072(17) 0.0127(17) 0.0040(16) C(37) 0.045(2) 0.040(2) 0.040(2) -0.011(2) 0.017(2) 0.009(2) C(38) 0.029(2) 0.063(3) 0.042(2) -0.017(2) 0.011(2) 0.008(2) C(39) 0.077(3) 0.023(2) 0.054(3) -0.011(2) 0.033(2) -0.000(2) C(40) 0.045(2) 0.049(2) 0.0194(19) -0.017(2) 0.0133(18) -0.0062(18) C(41) 0.094(4) 0.073(4) 0.034(2) -0.046(3) 0.027(3) -0.023(2) C(42) 0.083(5) 0.086(5) 0.037(3) -0.008(4) -0.009(3) -0.002(3) C(43) 0.100(5) 0.115(6) 0.064(4) -0.057(4) 0.061(4) -0.054(4) C(44) 0.061(4) 0.060(4) 0.087(5) -0.031(3) 0.019(3) -0.018(3) C(45) 0.111(7) 0.066(5) 0.099(6) -0.005(4) -0.043(5) -0.012(4) C(46) 0.044(3) 0.082(4) 0.064(4) 0.001(3) 0.018(2) 0.015(3) C(47) 0.055(4) 0.137(8) 0.068(4) 0.013(4) -0.003(3) -0.036(5) C(48) 0.28(3) 0.100(18) 0.16(2) -0.11(2) 0.19(3) -0.072(19) C(49) 0.21(3) 0.17(3) 0.34(5) -0.17(3) 0.23(3) -0.17(3) C(50) 0.055(8) 0.113(16) 0.051(7) -0.038(9) 0.028(7) 0.007(8) C(51) 0.049(7) 0.096(13) 0.056(7) -0.032(7) 0.018(6) -0.008(7) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb(1) Cl(1) 2.4576(16) yes . . Nb(1) Cl(2) 2.4631(11) yes . . Nb(1) Cl(3) 2.4197(12) yes . . Nb(1) O(1) 1.884(2) yes . . Nb(1) O(2) 1.880(3) yes . . Nb(1) O(3) 1.882(2) yes . . O(1) C(3) 1.363(4) yes . . O(2) C(9) 1.356(4) yes . . O(3) C(15) 1.359(4) yes . . N(1) C(44) 1.494(11) yes . . N(1) C(46) 1.488(8) yes . . N(1) C(48) 1.36(4) yes . . N(1) C(50) 1.66(2) yes . . C(1) C(2) 1.548(4) yes . . C(1) C(8) 1.553(6) yes . . C(1) C(14) 1.534(6) yes . . C(2) C(3) 1.404(4) yes . . C(2) C(7) 1.403(5) yes . . C(3) C(4) 1.413(5) yes . . C(4) C(5) 1.386(5) yes . . C(4) C(20) 1.542(4) yes . . C(5) C(6) 1.402(5) yes . . C(6) C(7) 1.379(5) yes . . C(6) C(24) 1.532(5) yes . . C(8) C(9) 1.413(5) yes . . C(8) C(13) 1.397(5) yes . . C(9) C(10) 1.413(7) yes . . C(10) C(11) 1.382(6) yes . . C(10) C(28) 1.550(6) yes . . C(11) C(12) 1.388(5) yes . . C(12) C(13) 1.390(7) yes . . C(12) C(32) 1.539(6) yes . . C(14) C(15) 1.406(5) yes . . C(14) C(19) 1.411(4) yes . . C(15) C(16) 1.418(6) yes . . C(16) C(17) 1.387(5) yes . . C(16) C(36) 1.541(6) yes . . C(17) C(18) 1.392(6) yes . . C(18) C(19) 1.378(6) yes . . C(18) C(40) 1.538(5) yes . . C(20) C(21) 1.544(8) yes . . C(20) C(22) 1.527(6) yes . . C(20) C(23) 1.527(8) yes . . C(24) C(25) 1.532(7) yes . . C(24) C(26) 1.529(10) yes . . C(24) C(27) 1.530(6) yes . . C(28) C(29) 1.529(10) yes . . C(28) C(30) 1.544(7) yes . . C(28) C(31) 1.540(11) yes . . C(32) C(33) 1.535(8) yes . . C(32) C(34) 1.553(8) yes . . C(32) C(35) 1.520(11) yes . . C(36) C(37) 1.537(7) yes . . C(36) C(38) 1.545(6) yes . . C(36) C(39) 1.525(8) yes . . C(40) C(41) 1.517(9) yes . . C(40) C(42) 1.510(8) yes . . C(40) C(43) 1.535(12) yes . . C(44) C(45) 1.512(10) yes . . C(46) C(47) 1.444(13) yes . . C(48) C(49) 1.49(4) yes . . C(48) C(50) 0.73(4) yes . . C(49) C(50) 1.08(4) yes . . C(49) C(51) 0.90(4) yes . . C(50) C(51) 1.53(2) yes . . C(52) C(53) 1.52(3) yes . . C(52) C(57) 1.26(3) yes . . C(52) C(58) 1.34(2) yes . . C(52) C(59) 1.74(3) yes . . C(52) C(60) 1.48(3) yes . . C(52) C(61) 1.09(3) yes . . C(53) C(54) 1.668(15) yes . . C(53) C(59) 1.13(3) yes . . C(53) C(60) 1.811(15) yes . . C(54) C(55) 1.096(19) yes . . C(54) C(59) 1.02(2) yes . . C(55) C(56) 1.65(3) yes . . C(55) C(59) 1.56(2) yes . . C(56) C(57) 1.19(3) yes . . C(56) C(59) 1.52(4) yes . . C(57) C(59) 1.45(3) yes . . C(57) C(61) 1.339(19) yes . . C(58) C(60) 1.174(14) yes . . C(58) C(61) 1.472(18) yes . . N(1) H(72) 0.75(7) no . . C(1) H(1) 0.95(3) no . . C(5) H(2) 0.950 no . . C(7) H(3) 0.950 no . . C(11) H(4) 0.950 no . . C(13) H(5) 0.950 no . . C(17) H(6) 0.950 no . . C(19) H(7) 0.950 no . . C(21) H(8) 0.980 no . . C(21) H(9) 0.980 no . . C(21) H(10) 0.980 no . . C(22) H(11) 0.980 no . . C(22) H(12) 0.980 no . . C(22) H(13) 0.980 no . . C(23) H(14) 0.980 no . . C(23) H(15) 0.980 no . . C(23) H(16) 0.980 no . . C(25) H(17) 0.980 no . . C(25) H(18) 0.980 no . . C(25) H(19) 0.980 no . . C(26) H(20) 0.980 no . . C(26) H(21) 0.980 no . . C(26) H(22) 0.980 no . . C(27) H(23) 0.980 no . . C(27) H(24) 0.980 no . . C(27) H(25) 0.980 no . . C(29) H(26) 0.980 no . . C(29) H(27) 0.980 no . . C(29) H(28) 0.980 no . . C(30) H(29) 0.980 no . . C(30) H(30) 0.980 no . . C(30) H(31) 0.980 no . . C(31) H(32) 0.980 no . . C(31) H(33) 0.980 no . . C(31) H(34) 0.980 no . . C(33) H(35) 0.980 no . . C(33) H(36) 0.980 no . . C(33) H(37) 0.980 no . . C(34) H(38) 0.980 no . . C(34) H(39) 0.980 no . . C(34) H(40) 0.980 no . . C(35) H(41) 0.980 no . . C(35) H(42) 0.980 no . . C(35) H(43) 0.980 no . . C(37) H(44) 0.980 no . . C(37) H(45) 0.980 no . . C(37) H(46) 0.980 no . . C(38) H(47) 0.980 no . . C(38) H(48) 0.980 no . . C(38) H(49) 0.980 no . . C(39) H(50) 0.980 no . . C(39) H(51) 0.980 no . . C(39) H(52) 0.980 no . . C(41) H(53) 0.980 no . . C(41) H(54) 0.980 no . . C(41) H(55) 0.980 no . . C(42) H(56) 0.980 no . . C(42) H(57) 0.980 no . . C(42) H(58) 0.980 no . . C(43) H(59) 0.980 no . . C(43) H(60) 0.980 no . . C(43) H(61) 0.980 no . . C(44) H(62) 0.990 no . . C(44) H(63) 0.990 no . . C(45) H(64) 0.980 no . . C(45) H(65) 0.980 no . . C(45) H(66) 0.980 no . . C(46) H(67) 0.990 no . . C(46) H(68) 0.990 no . . C(47) H(69) 0.980 no . . C(47) H(70) 0.980 no . . C(47) H(71) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Nb(1) Cl(2) 87.64(4) yes . . . Cl(1) Nb(1) Cl(3) 86.17(5) yes . . . Cl(1) Nb(1) O(1) 89.42(10) yes . . . Cl(1) Nb(1) O(2) 177.69(9) yes . . . Cl(1) Nb(1) O(3) 91.27(10) yes . . . Cl(2) Nb(1) Cl(3) 85.79(4) yes . . . Cl(2) Nb(1) O(1) 88.78(9) yes . . . Cl(2) Nb(1) O(2) 90.13(9) yes . . . Cl(2) Nb(1) O(3) 176.95(9) yes . . . Cl(3) Nb(1) O(1) 173.14(7) yes . . . Cl(3) Nb(1) O(2) 94.25(9) yes . . . Cl(3) Nb(1) O(3) 91.30(9) yes . . . O(1) Nb(1) O(2) 89.95(13) yes . . . O(1) Nb(1) O(3) 94.06(12) yes . . . O(2) Nb(1) O(3) 90.99(13) yes . . . Nb(1) O(1) C(3) 155.2(2) yes . . . Nb(1) O(2) C(9) 150.9(2) yes . . . Nb(1) O(3) C(15) 155.2(2) yes . . . C(44) N(1) C(46) 109.5(5) yes . . . C(44) N(1) C(48) 105.8(17) yes . . . C(44) N(1) C(50) 115.3(11) yes . . . C(46) N(1) C(48) 130.4(16) yes . . . C(46) N(1) C(50) 105.8(10) yes . . . C(48) N(1) C(50) 25.5(16) yes . . . C(2) C(1) C(8) 119.5(3) yes . . . C(2) C(1) C(14) 116.3(3) yes . . . C(8) C(1) C(14) 117.3(3) yes . . . C(1) C(2) C(3) 128.9(3) yes . . . C(1) C(2) C(7) 114.2(2) yes . . . C(3) C(2) C(7) 116.9(3) yes . . . O(1) C(3) C(2) 118.4(3) yes . . . O(1) C(3) C(4) 119.8(2) yes . . . C(2) C(3) C(4) 121.8(3) yes . . . C(3) C(4) C(5) 117.3(3) yes . . . C(3) C(4) C(20) 123.4(3) yes . . . C(5) C(4) C(20) 119.2(3) yes . . . C(4) C(5) C(6) 123.4(3) yes . . . C(5) C(6) C(7) 116.7(3) yes . . . C(5) C(6) C(24) 122.2(3) yes . . . C(7) C(6) C(24) 121.1(3) yes . . . C(2) C(7) C(6) 123.8(3) yes . . . C(1) C(8) C(9) 130.4(3) yes . . . C(1) C(8) C(13) 113.0(3) yes . . . C(9) C(8) C(13) 116.7(4) yes . . . O(2) C(9) C(8) 120.1(4) yes . . . O(2) C(9) C(10) 118.9(3) yes . . . C(8) C(9) C(10) 121.0(3) yes . . . C(9) C(10) C(11) 118.4(3) yes . . . C(9) C(10) C(28) 121.5(4) yes . . . C(11) C(10) C(28) 120.1(5) yes . . . C(10) C(11) C(12) 123.0(5) yes . . . C(11) C(12) C(13) 116.9(4) yes . . . C(11) C(12) C(32) 123.5(4) yes . . . C(13) C(12) C(32) 119.6(3) yes . . . C(8) C(13) C(12) 123.9(3) yes . . . C(1) C(14) C(15) 128.1(3) yes . . . C(1) C(14) C(19) 114.7(3) yes . . . C(15) C(14) C(19) 117.1(3) yes . . . O(3) C(15) C(14) 118.5(3) yes . . . O(3) C(15) C(16) 120.2(3) yes . . . C(14) C(15) C(16) 121.4(3) yes . . . C(15) C(16) C(17) 117.0(3) yes . . . C(15) C(16) C(36) 122.7(3) yes . . . C(17) C(16) C(36) 120.2(4) yes . . . C(16) C(17) C(18) 124.0(4) yes . . . C(17) C(18) C(19) 116.8(3) yes . . . C(17) C(18) C(40) 120.3(4) yes . . . C(19) C(18) C(40) 122.9(4) yes . . . C(14) C(19) C(18) 123.4(3) yes . . . C(4) C(20) C(21) 106.3(3) yes . . . C(4) C(20) C(22) 112.6(3) yes . . . C(4) C(20) C(23) 113.1(4) yes . . . C(21) C(20) C(22) 107.3(4) yes . . . C(21) C(20) C(23) 110.8(4) yes . . . C(22) C(20) C(23) 106.6(4) yes . . . C(6) C(24) C(25) 110.3(4) yes . . . C(6) C(24) C(26) 108.3(4) yes . . . C(6) C(24) C(27) 112.7(3) yes . . . C(25) C(24) C(26) 109.6(4) yes . . . C(25) C(24) C(27) 107.9(4) yes . . . C(26) C(24) C(27) 108.0(4) yes . . . C(10) C(28) C(29) 108.9(4) yes . . . C(10) C(28) C(30) 110.5(4) yes . . . C(10) C(28) C(31) 111.6(4) yes . . . C(29) C(28) C(30) 111.4(5) yes . . . C(29) C(28) C(31) 107.9(5) yes . . . C(30) C(28) C(31) 106.5(5) yes . . . C(12) C(32) C(33) 109.3(4) yes . . . C(12) C(32) C(34) 109.5(3) yes . . . C(12) C(32) C(35) 112.2(4) yes . . . C(33) C(32) C(34) 108.2(4) yes . . . C(33) C(32) C(35) 110.7(4) yes . . . C(34) C(32) C(35) 106.9(5) yes . . . C(16) C(36) C(37) 111.2(3) yes . . . C(16) C(36) C(38) 109.7(3) yes . . . C(16) C(36) C(39) 109.6(4) yes . . . C(37) C(36) C(38) 106.8(4) yes . . . C(37) C(36) C(39) 107.8(4) yes . . . C(38) C(36) C(39) 111.7(3) yes . . . C(18) C(40) C(41) 112.2(4) yes . . . C(18) C(40) C(42) 109.7(4) yes . . . C(18) C(40) C(43) 109.9(4) yes . . . C(41) C(40) C(42) 110.8(5) yes . . . C(41) C(40) C(43) 106.0(5) yes . . . C(42) C(40) C(43) 108.2(5) yes . . . N(1) C(44) C(45) 114.5(8) yes . . . N(1) C(46) C(47) 116.4(7) yes . . . N(1) C(48) C(49) 112(3) yes . . . N(1) C(48) C(50) 101(3) yes . . . C(49) C(48) C(50) 43(3) yes . . . C(48) C(49) C(50) 27(2) yes . . . C(48) C(49) C(51) 122(3) yes . . . C(50) C(49) C(51) 102(3) yes . . . N(1) C(50) C(48) 54(3) yes . . . N(1) C(50) C(49) 118(3) yes . . . N(1) C(50) C(51) 108.6(18) yes . . . C(48) C(50) C(49) 110(4) yes . . . C(48) C(50) C(51) 134(4) yes . . . C(49) C(50) C(51) 35(2) yes . . . C(49) C(51) C(50) 43(2) yes . . . C(53) C(52) C(57) 95.0(17) yes . . . C(53) C(52) C(58) 122(2) yes . . . C(53) C(52) C(59) 40.1(13) yes . . . C(53) C(52) C(60) 74.5(16) yes . . . C(53) C(52) C(61) 164(2) yes . . . C(57) C(52) C(58) 143(2) yes . . . C(57) C(52) C(59) 55.1(16) yes . . . C(57) C(52) C(60) 166(2) yes . . . C(57) C(52) C(61) 69(2) yes . . . C(58) C(52) C(59) 162(2) yes . . . C(58) C(52) C(60) 49.0(10) yes . . . C(58) C(52) C(61) 73.7(16) yes . . . C(59) C(52) C(60) 113(2) yes . . . C(59) C(52) C(61) 124(2) yes . . . C(60) C(52) C(61) 121(2) yes . . . C(52) C(53) C(54) 117.5(15) yes . . . C(52) C(53) C(59) 80(2) yes . . . C(52) C(53) C(60) 51.7(12) yes . . . C(54) C(53) C(59) 37.1(15) yes . . . C(54) C(53) C(60) 163.9(11) yes . . . C(59) C(53) C(60) 130.6(19) yes . . . C(53) C(54) C(55) 136.4(13) yes . . . C(53) C(54) C(59) 41.8(18) yes . . . C(55) C(54) C(59) 95(2) yes . . . C(54) C(55) C(56) 96.6(15) yes . . . C(54) C(55) C(59) 40.9(13) yes . . . C(56) C(55) C(59) 56.5(16) yes . . . C(55) C(56) C(57) 119(2) yes . . . C(55) C(56) C(59) 58.6(16) yes . . . C(57) C(56) C(59) 63(2) yes . . . C(52) C(57) C(56) 142(3) yes . . . C(52) C(57) C(59) 79(2) yes . . . C(52) C(57) C(61) 49.7(15) yes . . . C(56) C(57) C(59) 70(2) yes . . . C(56) C(57) C(61) 151(2) yes . . . C(59) C(57) C(61) 129.1(19) yes . . . C(52) C(58) C(60) 71.6(15) yes . . . C(52) C(58) C(61) 45.5(15) yes . . . C(60) C(58) C(61) 115.9(9) yes . . . C(52) C(59) C(53) 59.5(17) yes . . . C(52) C(59) C(54) 161(3) yes . . . C(52) C(59) C(55) 155(2) yes . . . C(52) C(59) C(56) 90(2) yes . . . C(52) C(59) C(57) 45.4(14) yes . . . C(53) C(59) C(54) 101(2) yes . . . C(53) C(59) C(55) 146(2) yes . . . C(53) C(59) C(56) 148(2) yes . . . C(53) C(59) C(57) 105(2) yes . . . C(54) C(59) C(55) 44.5(13) yes . . . C(54) C(59) C(56) 108(2) yes . . . C(54) C(59) C(57) 154(2) yes . . . C(55) C(59) C(56) 64.9(16) yes . . . C(55) C(59) C(57) 110(2) yes . . . C(56) C(59) C(57) 47.2(16) yes . . . C(52) C(60) C(53) 53.8(12) yes . . . C(52) C(60) C(58) 59.4(11) yes . . . C(53) C(60) C(58) 112.1(9) yes . . . C(52) C(61) C(57) 61.3(16) yes . . . C(52) C(61) C(58) 60.8(15) yes . . . C(57) C(61) C(58) 122.0(15) yes . . . C(44) N(1) H(72) 114(9) no . . . C(46) N(1) H(72) 103(7) no . . . C(48) N(1) H(72) 93(9) no . . . C(50) N(1) H(72) 108(9) no . . . C(2) C(1) H(1) 100(2) no . . . C(8) C(1) H(1) 99(2) no . . . C(14) C(1) H(1) 97(2) no . . . C(4) C(5) H(2) 118.3 no . . . C(6) C(5) H(2) 118.3 no . . . C(2) C(7) H(3) 118.1 no . . . C(6) C(7) H(3) 118.1 no . . . C(10) C(11) H(4) 118.5 no . . . C(12) C(11) H(4) 118.5 no . . . C(8) C(13) H(5) 118.0 no . . . C(12) C(13) H(5) 118.0 no . . . C(16) C(17) H(6) 118.0 no . . . C(18) C(17) H(6) 118.0 no . . . C(14) C(19) H(7) 118.3 no . . . C(18) C(19) H(7) 118.3 no . . . C(20) C(21) H(8) 109.5 no . . . C(20) C(21) H(9) 109.5 no . . . C(20) C(21) H(10) 109.5 no . . . H(8) C(21) H(9) 109.5 no . . . H(8) C(21) H(10) 109.5 no . . . H(9) C(21) H(10) 109.5 no . . . C(20) C(22) H(11) 109.5 no . . . C(20) C(22) H(12) 109.5 no . . . C(20) C(22) H(13) 109.5 no . . . H(11) C(22) H(12) 109.5 no . . . H(11) C(22) H(13) 109.5 no . . . H(12) C(22) H(13) 109.5 no . . . C(20) C(23) H(14) 109.5 no . . . C(20) C(23) H(15) 109.5 no . . . C(20) C(23) H(16) 109.5 no . . . H(14) C(23) H(15) 109.5 no . . . H(14) C(23) H(16) 109.5 no . . . H(15) C(23) H(16) 109.5 no . . . C(24) C(25) H(17) 109.5 no . . . C(24) C(25) H(18) 109.5 no . . . C(24) C(25) H(19) 109.5 no . . . H(17) C(25) H(18) 109.5 no . . . H(17) C(25) H(19) 109.5 no . . . H(18) C(25) H(19) 109.5 no . . . C(24) C(26) H(20) 109.5 no . . . C(24) C(26) H(21) 109.5 no . . . C(24) C(26) H(22) 109.5 no . . . H(20) C(26) H(21) 109.5 no . . . H(20) C(26) H(22) 109.5 no . . . H(21) C(26) H(22) 109.5 no . . . C(24) C(27) H(23) 109.5 no . . . C(24) C(27) H(24) 109.5 no . . . C(24) C(27) H(25) 109.5 no . . . H(23) C(27) H(24) 109.5 no . . . H(23) C(27) H(25) 109.5 no . . . H(24) C(27) H(25) 109.5 no . . . C(28) C(29) H(26) 109.5 no . . . C(28) C(29) H(27) 109.5 no . . . C(28) C(29) H(28) 109.5 no . . . H(26) C(29) H(27) 109.5 no . . . H(26) C(29) H(28) 109.5 no . . . H(27) C(29) H(28) 109.5 no . . . C(28) C(30) H(29) 109.5 no . . . C(28) C(30) H(30) 109.5 no . . . C(28) C(30) H(31) 109.5 no . . . H(29) C(30) H(30) 109.5 no . . . H(29) C(30) H(31) 109.5 no . . . H(30) C(30) H(31) 109.5 no . . . C(28) C(31) H(32) 109.5 no . . . C(28) C(31) H(33) 109.5 no . . . C(28) C(31) H(34) 109.5 no . . . H(32) C(31) H(33) 109.5 no . . . H(32) C(31) H(34) 109.5 no . . . H(33) C(31) H(34) 109.5 no . . . C(32) C(33) H(35) 109.5 no . . . C(32) C(33) H(36) 109.5 no . . . C(32) C(33) H(37) 109.5 no . . . H(35) C(33) H(36) 109.5 no . . . H(35) C(33) H(37) 109.5 no . . . H(36) C(33) H(37) 109.5 no . . . C(32) C(34) H(38) 109.5 no . . . C(32) C(34) H(39) 109.5 no . . . C(32) C(34) H(40) 109.5 no . . . H(38) C(34) H(39) 109.5 no . . . H(38) C(34) H(40) 109.5 no . . . H(39) C(34) H(40) 109.5 no . . . C(32) C(35) H(41) 109.5 no . . . C(32) C(35) H(42) 109.5 no . . . C(32) C(35) H(43) 109.5 no . . . H(41) C(35) H(42) 109.5 no . . . H(41) C(35) H(43) 109.5 no . . . H(42) C(35) H(43) 109.5 no . . . C(36) C(37) H(44) 109.5 no . . . C(36) C(37) H(45) 109.5 no . . . C(36) C(37) H(46) 109.5 no . . . H(44) C(37) H(45) 109.5 no . . . H(44) C(37) H(46) 109.5 no . . . H(45) C(37) H(46) 109.5 no . . . C(36) C(38) H(47) 109.5 no . . . C(36) C(38) H(48) 109.5 no . . . C(36) C(38) H(49) 109.5 no . . . H(47) C(38) H(48) 109.5 no . . . H(47) C(38) H(49) 109.5 no . . . H(48) C(38) H(49) 109.5 no . . . C(36) C(39) H(50) 109.5 no . . . C(36) C(39) H(51) 109.5 no . . . C(36) C(39) H(52) 109.5 no . . . H(50) C(39) H(51) 109.5 no . . . H(50) C(39) H(52) 109.5 no . . . H(51) C(39) H(52) 109.5 no . . . C(40) C(41) H(53) 109.5 no . . . C(40) C(41) H(54) 109.5 no . . . C(40) C(41) H(55) 109.5 no . . . H(53) C(41) H(54) 109.5 no . . . H(53) C(41) H(55) 109.5 no . . . H(54) C(41) H(55) 109.5 no . . . C(40) C(42) H(56) 109.5 no . . . C(40) C(42) H(57) 109.5 no . . . C(40) C(42) H(58) 109.5 no . . . H(56) C(42) H(57) 109.5 no . . . H(56) C(42) H(58) 109.5 no . . . H(57) C(42) H(58) 109.5 no . . . C(40) C(43) H(59) 109.5 no . . . C(40) C(43) H(60) 109.5 no . . . C(40) C(43) H(61) 109.5 no . . . H(59) C(43) H(60) 109.5 no . . . H(59) C(43) H(61) 109.5 no . . . H(60) C(43) H(61) 109.5 no . . . N(1) C(44) H(62) 108.6 no . . . N(1) C(44) H(63) 108.6 no . . . C(45) C(44) H(62) 108.6 no . . . C(45) C(44) H(63) 108.6 no . . . H(62) C(44) H(63) 107.6 no . . . C(44) C(45) H(64) 109.5 no . . . C(44) C(45) H(65) 109.5 no . . . C(44) C(45) H(66) 109.5 no . . . H(64) C(45) H(65) 109.5 no . . . H(64) C(45) H(66) 109.5 no . . . H(65) C(45) H(66) 109.5 no . . . N(1) C(46) H(67) 108.2 no . . . N(1) C(46) H(68) 108.2 no . . . C(47) C(46) H(67) 108.2 no . . . C(47) C(46) H(68) 108.2 no . . . H(67) C(46) H(68) 107.3 no . . . C(46) C(47) H(69) 109.5 no . . . C(46) C(47) H(70) 109.5 no . . . C(46) C(47) H(71) 109.5 no . . . H(69) C(47) H(70) 109.5 no . . . H(69) C(47) H(71) 109.5 no . . . H(70) C(47) H(71) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Nb(1) O(1) C(3) -138.5(7) ? . . . . Cl(1) Nb(1) O(2) C(9) -134(2) ? . . . . Cl(1) Nb(1) O(3) C(15) 118.2(6) ? . . . . Cl(2) Nb(1) O(1) C(3) 133.8(7) ? . . . . Cl(2) Nb(1) O(2) C(9) -148.5(5) ? . . . . Cl(2) Nb(1) O(3) C(15) -172.8(15) ? . . . . Cl(3) Nb(1) O(1) C(3) 171.5(7) ? . . . . Cl(3) Nb(1) O(2) C(9) 125.7(5) ? . . . . Cl(3) Nb(1) O(3) C(15) -155.6(6) ? . . . . O(1) Nb(1) O(2) C(9) -59.7(5) ? . . . . O(2) Nb(1) O(1) C(3) 43.7(7) ? . . . . O(1) Nb(1) O(3) C(15) 28.7(6) ? . . . . O(3) Nb(1) O(1) C(3) -47.3(7) ? . . . . O(2) Nb(1) O(3) C(15) -61.3(6) ? . . . . O(3) Nb(1) O(2) C(9) 34.3(5) ? . . . . Nb(1) O(1) C(3) C(2) 9.0(10) ? . . . . Nb(1) O(1) C(3) C(4) -172.3(5) ? . . . . Nb(1) O(2) C(9) C(8) 11.9(7) ? . . . . Nb(1) O(2) C(9) C(10) -168.2(3) ? . . . . Nb(1) O(3) C(15) C(14) 10.9(9) ? . . . . Nb(1) O(3) C(15) C(16) -168.1(5) ? . . . . C(44) N(1) C(46) C(47) 179.4(5) ? . . . . C(46) N(1) C(44) C(45) 175.4(5) ? . . . . C(44) N(1) C(48) C(49) 73(3) ? . . . . C(44) N(1) C(48) C(50) 116(3) ? . . . . C(48) N(1) C(44) C(45) 30.9(14) ? . . . . C(44) N(1) C(50) C(48) -73(4) ? . . . . C(44) N(1) C(50) C(49) 21(3) ? . . . . C(44) N(1) C(50) C(51) 58(2) ? . . . . C(50) N(1) C(44) C(45) 56.2(10) ? . . . . C(46) N(1) C(48) C(49) -61(3) ? . . . . C(46) N(1) C(48) C(50) -18(5) ? . . . . C(48) N(1) C(46) C(47) -48(2) ? . . . . C(46) N(1) C(50) C(48) 166(4) ? . . . . C(46) N(1) C(50) C(49) -100(3) ? . . . . C(46) N(1) C(50) C(51) -63(2) ? . . . . C(50) N(1) C(46) C(47) -55.8(11) ? . . . . C(48) N(1) C(50) C(49) 94(5) ? . . . . C(48) N(1) C(50) C(51) 131(5) ? . . . . C(50) N(1) C(48) C(49) -43(3) ? . . . . C(2) C(1) C(8) C(9) 68.2(5) ? . . . . C(2) C(1) C(8) C(13) -111.9(3) ? . . . . C(8) C(1) C(2) C(3) -71.0(6) ? . . . . C(8) C(1) C(2) C(7) 109.2(4) ? . . . . C(2) C(1) C(14) C(15) -86.4(4) ? . . . . C(2) C(1) C(14) C(19) 96.3(3) ? . . . . C(14) C(1) C(2) C(3) 79.3(5) ? . . . . C(14) C(1) C(2) C(7) -100.6(4) ? . . . . C(8) C(1) C(14) C(15) 64.5(4) ? . . . . C(8) C(1) C(14) C(19) -112.8(3) ? . . . . C(14) C(1) C(8) C(9) -81.8(4) ? . . . . C(14) C(1) C(8) C(13) 98.1(3) ? . . . . C(1) C(2) C(3) O(1) -5.3(7) ? . . . . C(1) C(2) C(3) C(4) 176.0(4) ? . . . . C(1) C(2) C(7) C(6) 179.8(4) ? . . . . C(3) C(2) C(7) C(6) -0.1(6) ? . . . . C(7) C(2) C(3) O(1) 174.5(4) ? . . . . C(7) C(2) C(3) C(4) -4.1(7) ? . . . . O(1) C(3) C(4) C(5) -173.2(4) ? . . . . O(1) C(3) C(4) C(20) 11.9(7) ? . . . . C(2) C(3) C(4) C(5) 5.4(7) ? . . . . C(2) C(3) C(4) C(20) -169.5(4) ? . . . . C(3) C(4) C(5) C(6) -2.6(8) ? . . . . C(3) C(4) C(20) C(21) 64.3(6) ? . . . . C(3) C(4) C(20) C(22) -178.4(5) ? . . . . C(3) C(4) C(20) C(23) -57.5(6) ? . . . . C(5) C(4) C(20) C(21) -110.5(5) ? . . . . C(5) C(4) C(20) C(22) 6.8(7) ? . . . . C(5) C(4) C(20) C(23) 127.7(5) ? . . . . C(20) C(4) C(5) C(6) 172.6(5) ? . . . . C(4) C(5) C(6) C(7) -1.3(8) ? . . . . C(4) C(5) C(6) C(24) -179.0(5) ? . . . . C(5) C(6) C(7) C(2) 2.7(8) ? . . . . C(5) C(6) C(24) C(25) -132.2(5) ? . . . . C(5) C(6) C(24) C(26) 107.9(5) ? . . . . C(5) C(6) C(24) C(27) -11.5(8) ? . . . . C(7) C(6) C(24) C(25) 50.3(7) ? . . . . C(7) C(6) C(24) C(26) -69.6(6) ? . . . . C(7) C(6) C(24) C(27) 170.9(5) ? . . . . C(24) C(6) C(7) C(2) -179.6(5) ? . . . . C(1) C(8) C(9) O(2) 4.0(6) ? . . . . C(1) C(8) C(9) C(10) -175.9(3) ? . . . . C(1) C(8) C(13) C(12) 178.4(3) ? . . . . C(9) C(8) C(13) C(12) -1.7(6) ? . . . . C(13) C(8) C(9) O(2) -175.9(3) ? . . . . C(13) C(8) C(9) C(10) 4.2(5) ? . . . . O(2) C(9) C(10) C(11) 176.3(3) ? . . . . O(2) C(9) C(10) C(28) -2.1(6) ? . . . . C(8) C(9) C(10) C(11) -3.8(6) ? . . . . C(8) C(9) C(10) C(28) 177.8(4) ? . . . . C(9) C(10) C(11) C(12) 0.8(6) ? . . . . C(9) C(10) C(28) C(29) 65.6(6) ? . . . . C(9) C(10) C(28) C(30) -57.0(7) ? . . . . C(9) C(10) C(28) C(31) -175.3(4) ? . . . . C(11) C(10) C(28) C(29) -112.7(6) ? . . . . C(11) C(10) C(28) C(30) 124.6(5) ? . . . . C(11) C(10) C(28) C(31) 6.3(6) ? . . . . C(28) C(10) C(11) C(12) 179.2(4) ? . . . . C(10) C(11) C(12) C(13) 1.7(6) ? . . . . C(10) C(11) C(12) C(32) -178.1(4) ? . . . . C(11) C(12) C(13) C(8) -1.2(6) ? . . . . C(11) C(12) C(32) C(33) 118.0(5) ? . . . . C(11) C(12) C(32) C(34) -123.7(5) ? . . . . C(11) C(12) C(32) C(35) -5.2(7) ? . . . . C(13) C(12) C(32) C(33) -61.8(6) ? . . . . C(13) C(12) C(32) C(34) 56.5(6) ? . . . . C(13) C(12) C(32) C(35) 175.1(4) ? . . . . C(32) C(12) C(13) C(8) 178.6(4) ? . . . . C(1) C(14) C(15) O(3) 8.8(6) ? . . . . C(1) C(14) C(15) C(16) -172.2(3) ? . . . . C(1) C(14) C(19) C(18) 177.0(3) ? . . . . C(15) C(14) C(19) C(18) -0.6(6) ? . . . . C(19) C(14) C(15) O(3) -173.9(3) ? . . . . C(19) C(14) C(15) C(16) 5.1(5) ? . . . . O(3) C(15) C(16) C(17) 173.7(3) ? . . . . O(3) C(15) C(16) C(36) -7.4(6) ? . . . . C(14) C(15) C(16) C(17) -5.3(6) ? . . . . C(14) C(15) C(16) C(36) 173.6(3) ? . . . . C(15) C(16) C(17) C(18) 1.1(6) ? . . . . C(15) C(16) C(36) C(37) -174.4(4) ? . . . . C(15) C(16) C(36) C(38) 67.6(5) ? . . . . C(15) C(16) C(36) C(39) -55.4(5) ? . . . . C(17) C(16) C(36) C(37) 4.4(6) ? . . . . C(17) C(16) C(36) C(38) -113.5(4) ? . . . . C(17) C(16) C(36) C(39) 123.5(4) ? . . . . C(36) C(16) C(17) C(18) -177.8(4) ? . . . . C(16) C(17) C(18) C(19) 3.0(6) ? . . . . C(16) C(17) C(18) C(40) -178.9(4) ? . . . . C(17) C(18) C(19) C(14) -3.3(6) ? . . . . C(17) C(18) C(40) C(41) 170.9(5) ? . . . . C(17) C(18) C(40) C(42) -65.6(7) ? . . . . C(17) C(18) C(40) C(43) 53.2(6) ? . . . . C(19) C(18) C(40) C(41) -11.3(7) ? . . . . C(19) C(18) C(40) C(42) 112.3(6) ? . . . . C(19) C(18) C(40) C(43) -128.9(5) ? . . . . C(40) C(18) C(19) C(14) 178.8(4) ? . . . . N(1) C(48) C(49) C(50) 82(4) ? . . . . N(1) C(48) C(49) C(51) 35(7) ? . . . . N(1) C(48) C(50) C(49) -111(4) ? . . . . N(1) C(48) C(50) C(51) -81(5) ? . . . . C(49) C(48) C(50) N(1) 111(4) ? . . . . C(49) C(48) C(50) C(51) 30(4) ? . . . . C(50) C(48) C(49) C(51) -47(6) ? . . . . C(48) C(49) C(50) N(1) -59(4) ? . . . . C(48) C(49) C(50) C(51) -141(5) ? . . . . C(48) C(49) C(51) C(50) 20(3) ? . . . . C(51) C(49) C(50) N(1) 82(4) ? . . . . C(51) C(49) C(50) C(48) 141(5) ? . . . . N(1) C(50) C(51) C(49) -113(5) ? . . . . C(48) C(50) C(51) C(49) -56(8) ? . . . . C(53) C(52) C(57) C(56) -39(4) ? . . . . C(53) C(52) C(57) C(59) -3.2(19) ? . . . . C(53) C(52) C(57) C(61) 180(2) ? . . . . C(57) C(52) C(53) C(54) 5(2) ? . . . . C(57) C(52) C(53) C(59) 4(2) ? . . . . C(57) C(52) C(53) C(60) 171(2) ? . . . . C(53) C(52) C(58) C(60) 15(2) ? . . . . C(53) C(52) C(58) C(61) -179(2) ? . . . . C(58) C(52) C(53) C(54) -177.1(19) ? . . . . C(58) C(52) C(53) C(59) -178(3) ? . . . . C(58) C(52) C(53) C(60) -11.5(17) ? . . . . C(53) C(52) C(59) C(54) -5(8) ? . . . . C(53) C(52) C(59) C(55) -178(6) ? . . . . C(53) C(52) C(59) C(56) -169(3) ? . . . . C(53) C(52) C(59) C(57) 175(3) ? . . . . C(59) C(52) C(53) C(54) 1.1(19) ? . . . . C(59) C(52) C(53) C(60) 167(2) ? . . . . C(53) C(52) C(60) C(58) -167.1(17) ? . . . . C(60) C(52) C(53) C(54) -165.7(14) ? . . . . C(60) C(52) C(53) C(59) -167(2) ? . . . . C(53) C(52) C(61) C(57) -1(7) ? . . . . C(53) C(52) C(61) C(58) 177(6) ? . . . . C(61) C(52) C(53) C(54) 6(10) ? . . . . C(61) C(52) C(53) C(59) 5(8) ? . . . . C(61) C(52) C(53) C(60) 172(11) ? . . . . C(57) C(52) C(58) C(60) -169(4) ? . . . . C(57) C(52) C(58) C(61) -3(3) ? . . . . C(58) C(52) C(57) C(56) 145(4) ? . . . . C(58) C(52) C(57) C(59) -180(4) ? . . . . C(58) C(52) C(57) C(61) 3(3) ? . . . . C(57) C(52) C(59) C(53) -175(3) ? . . . . C(57) C(52) C(59) C(54) -180(9) ? . . . . C(57) C(52) C(59) C(55) 7(5) ? . . . . C(57) C(52) C(59) C(56) 16(2) ? . . . . C(59) C(52) C(57) C(56) -35(3) ? . . . . C(59) C(52) C(57) C(61) -177(2) ? . . . . C(57) C(52) C(60) C(53) -41(9) ? . . . . C(57) C(52) C(60) C(58) 151(10) ? . . . . C(60) C(52) C(57) C(56) 1(11) ? . . . . C(60) C(52) C(57) C(59) 36(9) ? . . . . C(60) C(52) C(57) C(61) -140(10) ? . . . . C(57) C(52) C(61) C(58) 178(2) ? . . . . C(61) C(52) C(57) C(56) 142(3) ? . . . . C(61) C(52) C(57) C(59) 177(2) ? . . . . C(58) C(52) C(59) C(53) 5(8) ? . . . . C(58) C(52) C(59) C(54) 0(15) ? . . . . C(58) C(52) C(59) C(55) -173(6) ? . . . . C(58) C(52) C(59) C(56) -164(8) ? . . . . C(58) C(52) C(59) C(57) 180(9) ? . . . . C(59) C(52) C(58) C(60) 11(8) ? . . . . C(59) C(52) C(58) C(61) 177(8) ? . . . . C(58) C(52) C(60) C(53) 167.1(17) ? . . . . C(60) C(52) C(58) C(61) 166(2) ? . . . . C(58) C(52) C(61) C(57) -178(2) ? . . . . C(61) C(52) C(58) C(60) -166(2) ? . . . . C(59) C(52) C(60) C(53) -9.3(15) ? . . . . C(59) C(52) C(60) C(58) -176(2) ? . . . . C(60) C(52) C(59) C(53) 14(2) ? . . . . C(60) C(52) C(59) C(54) 9(10) ? . . . . C(60) C(52) C(59) C(55) -164(5) ? . . . . C(60) C(52) C(59) C(56) -155(2) ? . . . . C(60) C(52) C(59) C(57) -171(2) ? . . . . C(59) C(52) C(61) C(57) 3(2) ? . . . . C(59) C(52) C(61) C(58) -179(3) ? . . . . C(61) C(52) C(59) C(53) -178(2) ? . . . . C(61) C(52) C(59) C(54) 177(7) ? . . . . C(61) C(52) C(59) C(55) 3(8) ? . . . . C(61) C(52) C(59) C(56) 13(3) ? . . . . C(61) C(52) C(59) C(57) -3(2) ? . . . . C(60) C(52) C(61) C(57) 170(3) ? . . . . C(60) C(52) C(61) C(58) -12.2(17) ? . . . . C(61) C(52) C(60) C(53) -177(3) ? . . . . C(61) C(52) C(60) C(58) 16(2) ? . . . . C(52) C(53) C(54) C(55) -2(3) ? . . . . C(52) C(53) C(54) C(59) -2(3) ? . . . . C(52) C(53) C(59) C(54) 178(2) ? . . . . C(52) C(53) C(59) C(55) 179(4) ? . . . . C(52) C(53) C(59) C(56) 21(6) ? . . . . C(52) C(53) C(59) C(57) -4(2) ? . . . . C(52) C(53) C(60) C(58) 11.9(16) ? . . . . C(54) C(53) C(59) C(52) -178(2) ? . . . . C(54) C(53) C(59) C(55) 0(2) ? . . . . C(54) C(53) C(59) C(56) -157(8) ? . . . . C(54) C(53) C(59) C(57) 178(3) ? . . . . C(59) C(53) C(54) C(55) -0(2) ? . . . . C(54) C(53) C(60) C(52) 52(5) ? . . . . C(54) C(53) C(60) C(58) 64(5) ? . . . . C(60) C(53) C(54) C(55) -47(6) ? . . . . C(60) C(53) C(54) C(59) -46(5) ? . . . . C(59) C(53) C(60) C(52) 17(3) ? . . . . C(59) C(53) C(60) C(58) 29(3) ? . . . . C(60) C(53) C(59) C(52) -14(2) ? . . . . C(60) C(53) C(59) C(54) 164.7(18) ? . . . . C(60) C(53) C(59) C(55) 165(3) ? . . . . C(60) C(53) C(59) C(56) 8(8) ? . . . . C(60) C(53) C(59) C(57) -17(3) ? . . . . C(53) C(54) C(55) C(56) 12(2) ? . . . . C(53) C(54) C(55) C(59) 0.3(17) ? . . . . C(53) C(54) C(59) C(52) 4(7) ? . . . . C(53) C(54) C(59) C(55) -179.7(18) ? . . . . C(53) C(54) C(59) C(56) 168(4) ? . . . . C(53) C(54) C(59) C(57) -175(7) ? . . . . C(55) C(54) C(59) C(52) -176(8) ? . . . . C(55) C(54) C(59) C(53) 179.7(18) ? . . . . C(55) C(54) C(59) C(56) -13(3) ? . . . . C(55) C(54) C(59) C(57) 4(7) ? . . . . C(59) C(54) C(55) C(56) 11(2) ? . . . . C(54) C(55) C(56) C(57) -29(4) ? . . . . C(54) C(55) C(56) C(59) -9(2) ? . . . . C(54) C(55) C(59) C(52) 177(6) ? . . . . C(54) C(55) C(59) C(53) -1(3) ? . . . . C(54) C(55) C(59) C(56) 167(3) ? . . . . C(54) C(55) C(59) C(57) -178(3) ? . . . . C(56) C(55) C(59) C(52) 10(5) ? . . . . C(56) C(55) C(59) C(53) -167(6) ? . . . . C(56) C(55) C(59) C(54) -167(3) ? . . . . C(56) C(55) C(59) C(57) 15(2) ? . . . . C(59) C(55) C(56) C(57) -20(3) ? . . . . C(55) C(56) C(57) C(52) 57(5) ? . . . . C(55) C(56) C(57) C(59) 19(3) ? . . . . C(55) C(56) C(57) C(61) 156(4) ? . . . . C(55) C(56) C(59) C(52) -176(2) ? . . . . C(55) C(56) C(59) C(53) 166(7) ? . . . . C(55) C(56) C(59) C(54) 10(2) ? . . . . C(55) C(56) C(59) C(57) -160(2) ? . . . . C(57) C(56) C(59) C(52) -16(2) ? . . . . C(57) C(56) C(59) C(53) -34(6) ? . . . . C(57) C(56) C(59) C(54) 170(3) ? . . . . C(57) C(56) C(59) C(55) 160(2) ? . . . . C(59) C(56) C(57) C(52) 37(4) ? . . . . C(59) C(56) C(57) C(61) 137(6) ? . . . . C(52) C(57) C(59) C(53) 4(2) ? . . . . C(52) C(57) C(59) C(54) 180(6) ? . . . . C(52) C(57) C(59) C(55) -177(2) ? . . . . C(52) C(57) C(59) C(56) -158(3) ? . . . . C(52) C(57) C(61) C(58) -2(2) ? . . . . C(56) C(57) C(59) C(52) 158(3) ? . . . . C(56) C(57) C(59) C(53) 162(3) ? . . . . C(56) C(57) C(59) C(54) -22(6) ? . . . . C(56) C(57) C(59) C(55) -19(2) ? . . . . C(56) C(57) C(61) C(52) -128(6) ? . . . . C(56) C(57) C(61) C(58) -130(6) ? . . . . C(59) C(57) C(61) C(52) -4(3) ? . . . . C(59) C(57) C(61) C(58) -6(3) ? . . . . C(61) C(57) C(59) C(52) 3(2) ? . . . . C(61) C(57) C(59) C(53) 7(3) ? . . . . C(61) C(57) C(59) C(54) -177(5) ? . . . . C(61) C(57) C(59) C(55) -174(2) ? . . . . C(61) C(57) C(59) C(56) -155(3) ? . . . . C(52) C(58) C(60) C(53) -11.2(15) ? . . . . C(52) C(58) C(61) C(57) 2(2) ? . . . . C(60) C(58) C(61) C(52) 15(2) ? . . . . C(60) C(58) C(61) C(57) 17(2) ? . . . . C(61) C(58) C(60) C(52) -10.9(15) ? . . . . C(61) C(58) C(60) C(53) -22.1(14) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) C(47) 3.581(7) ? . . Cl(2) C(44) 3.583(7) ? . . Cl(2) C(46) 3.561(7) ? . . Cl(3) C(45) 3.534(8) ? . . C(3) C(50) 3.46(2) ? . 6_546 C(4) C(50) 3.53(2) ? . 6_546 C(23) C(48) 3.48(3) ? . 6_546 C(44) Cl(2) 3.583(7) ? . . C(45) Cl(3) 3.534(8) ? . . C(46) Cl(2) 3.561(7) ? . . C(47) Cl(1) 3.581(7) ? . . C(48) C(23) 3.48(3) ? . 6_556 C(50) C(3) 3.46(2) ? . 6_556 C(50) C(4) 3.53(2) ? . 6_556 C(52) C(54) 2.72(2) ? . . C(52) C(55) 3.22(2) ? . . C(52) C(56) 2.32(3) ? . . C(53) C(53) 3.04(3) ? . 3_566 C(53) C(54) 3.49(2) ? . 3_566 C(53) C(55) 2.57(2) ? . . C(53) C(56) 2.56(3) ? . . C(53) C(57) 2.05(2) ? . . C(53) C(58) 2.501(17) ? . . C(53) C(61) 2.59(2) ? . . C(54) C(52) 2.72(2) ? . . C(54) C(53) 3.49(2) ? . 3_566 C(54) C(56) 2.09(3) ? . . C(54) C(57) 2.410(19) ? . . C(54) C(60) 3.444(9) ? . . C(54) C(60) 3.192(14) ? . 3_566 C(54) C(61) 3.541(17) ? . . C(55) C(52) 3.22(2) ? . . C(55) C(53) 2.57(2) ? . . C(55) C(57) 2.46(2) ? . . C(56) C(52) 2.32(3) ? . . C(56) C(53) 2.56(3) ? . . C(56) C(54) 2.09(3) ? . . C(56) C(58) 3.58(2) ? . . C(56) C(61) 2.45(3) ? . . C(57) C(53) 2.05(2) ? . . C(57) C(54) 2.410(19) ? . . C(57) C(55) 2.46(2) ? . . C(57) C(58) 2.460(17) ? . . C(57) C(60) 2.71(2) ? . . C(58) C(53) 2.501(17) ? . . C(58) C(56) 3.58(2) ? . . C(58) C(57) 2.460(17) ? . . C(58) C(59) 3.04(2) ? . . C(59) C(58) 3.04(2) ? . . C(59) C(60) 2.69(2) ? . . C(59) C(61) 2.52(3) ? . . C(60) C(54) 3.444(9) ? . . C(60) C(54) 3.192(14) ? . 3_566 C(60) C(57) 2.71(2) ? . . C(60) C(59) 2.69(2) ? . . C(60) C(61) 2.25(2) ? . . C(61) C(53) 2.59(2) ? . . C(61) C(54) 3.541(17) ? . . C(61) C(56) 2.45(3) ? . . C(61) C(59) 2.52(3) ? . . C(61) C(60) 2.25(2) ? . . Cl(1) H(12) 3.515 ? . 6_556 Cl(1) H(13) 3.473 ? . 6_556 Cl(1) H(14) 3.298 ? . 6_556 Cl(1) H(66) 3.573 ? . 6_546 Cl(1) H(68) 3.583 ? . . Cl(1) H(69) 2.860 ? . . Cl(1) H(72) 2.98(9) ? . . Cl(2) H(62) 3.047 ? . 7_557 Cl(2) H(63) 2.727 ? . . Cl(2) H(67) 2.864 ? . 7_557 Cl(2) H(68) 2.704 ? . . Cl(2) H(68) 3.581 ? . 7_557 Cl(2) H(72) 3.44(11) ? . . Cl(3) H(23) 3.441 ? . 1_565 Cl(3) H(24) 3.415 ? . 1_565 Cl(3) H(25) 3.409 ? . 1_565 Cl(3) H(63) 3.353 ? . . Cl(3) H(65) 3.526 ? . . Cl(3) H(66) 2.957 ? . . Cl(3) H(72) 3.27(8) ? . . C(1) H(60) 3.493 ? . 4_555 C(2) H(59) 3.225 ? . 4_555 C(2) H(60) 3.320 ? . 4_555 C(3) H(59) 3.439 ? . 4_555 C(3) H(61) 3.567 ? . 4_555 C(4) H(59) 3.506 ? . 4_555 C(4) H(71) 3.574 ? . 6_546 C(5) H(59) 3.415 ? . 4_555 C(5) H(71) 3.061 ? . 6_546 C(6) H(59) 3.261 ? . 4_555 C(6) H(71) 3.364 ? . 6_546 C(7) H(59) 3.109 ? . 4_555 C(8) H(60) 2.813 ? . 4_555 C(9) H(60) 2.974 ? . 4_555 C(10) H(53) 3.231 ? . 4_555 C(10) H(60) 3.276 ? . 4_555 C(11) H(53) 3.178 ? . 4_555 C(11) H(54) 3.435 ? . 4_555 C(11) H(60) 3.450 ? . 4_555 C(12) H(54) 3.442 ? . 4_555 C(12) H(60) 3.383 ? . 4_555 C(13) H(60) 3.029 ? . 4_555 C(17) H(10) 3.539 ? . 4_554 C(19) H(39) 3.579 ? . 3_556 C(21) H(61) 3.237 ? . 4_555 C(21) H(62) 3.018 ? . 7_557 C(21) H(64) 3.420 ? . 7_557 C(22) H(44) 3.281 ? . 4_555 C(22) H(47) 3.580 ? . 6_546 C(22) H(48) 3.442 ? . 6_546 C(22) H(64) 3.434 ? . 1_545 C(22) H(65) 3.399 ? . 1_545 C(23) H(47) 3.416 ? . 6_546 C(23) H(48) 3.489 ? . 6_546 C(25) H(29) 3.461 ? . 4_554 C(25) H(33) 3.096 ? . 4_554 C(25) H(42) 3.379 ? . 3_556 C(26) H(35) 3.553 ? . 3_556 C(26) H(36) 3.576 ? . 3_556 C(27) H(28) 3.246 ? . 1_545 C(27) H(51) 3.597 ? . 1_545 C(27) H(52) 3.478 ? . 1_545 C(29) H(20) 3.418 ? . 1_565 C(29) H(24) 2.953 ? . 1_565 C(29) H(45) 3.355 ? . 4_565 C(30) H(19) 3.492 ? . 4_555 C(30) H(53) 3.392 ? . 4_555 C(30) H(67) 3.398 ? . 7_557 C(30) H(70) 3.530 ? . 7_557 C(33) H(17) 3.516 ? . 3_556 C(33) H(22) 3.525 ? . 3_556 C(33) H(38) 3.202 ? . 3_556 C(34) H(5) 3.453 ? . 3_556 C(34) H(37) 3.532 ? . 3_556 C(34) H(38) 3.082 ? . 3_556 C(34) H(54) 3.365 ? . 4_555 C(34) H(55) 3.107 ? . 3_556 C(35) H(17) 3.440 ? . 3_556 C(35) H(34) 3.408 ? . 2_556 C(35) H(41) 3.562 ? . 2_556 C(35) H(55) 3.416 ? . 3_556 C(37) H(11) 3.345 ? . 4_554 C(37) H(27) 3.084 ? . 4_564 C(38) H(11) 3.554 ? . 4_554 C(38) H(12) 2.838 ? . 6_556 C(38) H(14) 3.452 ? . 6_556 C(38) H(15) 3.540 ? . 6_556 C(38) H(64) 3.559 ? . 6_546 C(39) H(18) 3.569 ? . 1_565 C(39) H(23) 2.996 ? . 1_565 C(41) H(39) 3.015 ? . 3_556 C(41) H(40) 3.421 ? . 4_554 C(41) H(41) 3.160 ? . 3_556 C(42) H(22) 3.508 ? . 4_554 C(42) H(40) 3.445 ? . 4_554 C(43) H(10) 3.102 ? . 4_554 C(44) H(8) 3.456 ? . 7_557 C(44) H(9) 3.389 ? . 7_557 C(45) H(9) 3.216 ? . 7_557 C(45) H(11) 3.550 ? . 1_565 C(45) H(12) 3.508 ? . 1_565 C(45) H(13) 3.409 ? . 1_565 C(47) H(23) 3.337 ? . 6_556 C(47) H(30) 3.569 ? . 7_557 C(47) H(51) 3.533 ? . 6_546 C(48) H(14) 3.122 ? . 6_556 C(48) H(16) 2.996 ? . 6_556 C(49) H(49) 3.382 ? . 6_556 C(50) H(14) 3.514 ? . 6_556 C(50) H(16) 3.285 ? . 6_556 C(51) H(8) 3.591 ? . 7_557 C(51) H(10) 3.578 ? . 7_557 C(52) H(35) 3.534 ? . . C(52) H(37) 3.361 ? . . C(53) H(21) 3.567 ? . 1_565 C(53) H(35) 3.426 ? . . C(53) H(35) 3.567 ? . 3_566 C(54) H(21) 3.348 ? . 3_556 C(54) H(32) 3.573 ? . 3_566 C(54) H(43) 3.401 ? . 3_566 C(55) H(21) 3.493 ? . 3_556 C(55) H(32) 3.060 ? . 3_566 C(56) H(37) 3.599 ? . . C(57) H(37) 3.484 ? . . C(58) H(18) 3.585 ? . 1_565 C(58) H(24) 3.438 ? . 1_565 C(58) H(28) 3.380 ? . . C(58) H(52) 3.354 ? . . C(59) H(35) 3.555 ? . . C(60) H(21) 3.055 ? . 1_565 C(60) H(24) 3.520 ? . 1_565 C(60) H(28) 3.264 ? . . C(60) H(35) 3.450 ? . . C(61) H(37) 3.352 ? . . H(1) H(39) 3.528 ? . 3_556 H(2) H(44) 3.404 ? . 4_555 H(2) H(71) 3.035 ? . 6_546 H(3) H(36) 3.004 ? . 3_556 H(3) H(59) 3.484 ? . 4_555 H(4) H(41) 3.516 ? . 2_556 H(4) H(53) 3.308 ? . 4_555 H(4) H(54) 3.495 ? . 4_555 H(5) C(34) 3.453 ? . 3_556 H(5) H(36) 3.358 ? . 3_556 H(5) H(38) 2.725 ? . 3_556 H(5) H(39) 3.307 ? . 3_556 H(5) H(60) 3.486 ? . 4_555 H(6) H(10) 3.243 ? . 4_554 H(7) H(39) 2.723 ? . 3_556 H(8) C(44) 3.456 ? . 7_557 H(8) C(51) 3.591 ? . 7_557 H(8) H(61) 3.384 ? . 4_555 H(8) H(62) 2.496 ? . 7_557 H(8) H(64) 3.544 ? . 7_557 H(9) C(44) 3.389 ? . 7_557 H(9) C(45) 3.216 ? . 7_557 H(9) H(49) 2.909 ? . 4_555 H(9) H(62) 2.683 ? . 7_557 H(9) H(64) 2.541 ? . 7_557 H(9) H(65) 3.395 ? . 7_557 H(10) C(17) 3.539 ? . 4_555 H(10) C(43) 3.102 ? . 4_555 H(10) C(51) 3.578 ? . 7_557 H(10) H(6) 3.243 ? . 4_555 H(10) H(44) 3.470 ? . 4_555 H(10) H(49) 3.514 ? . 4_555 H(10) H(59) 3.038 ? . 4_555 H(10) H(61) 2.336 ? . 4_555 H(10) H(62) 3.560 ? . 7_557 H(11) C(37) 3.345 ? . 4_555 H(11) C(38) 3.554 ? . 4_555 H(11) C(45) 3.550 ? . 1_545 H(11) H(44) 2.368 ? . 4_555 H(11) H(48) 3.088 ? . 4_555 H(11) H(49) 3.252 ? . 4_555 H(11) H(64) 3.391 ? . 1_545 H(11) H(65) 3.028 ? . 1_545 H(12) Cl(1) 3.515 ? . 6_546 H(12) C(38) 2.838 ? . 6_546 H(12) C(45) 3.508 ? . 1_545 H(12) H(47) 2.658 ? . 6_546 H(12) H(48) 2.504 ? . 6_546 H(12) H(49) 2.878 ? . 6_546 H(12) H(64) 3.009 ? . 1_545 H(12) H(65) 3.419 ? . 1_545 H(12) H(66) 3.544 ? . 1_545 H(13) Cl(1) 3.473 ? . 6_546 H(13) C(45) 3.409 ? . 1_545 H(13) H(44) 3.477 ? . 4_555 H(13) H(64) 3.344 ? . 1_545 H(13) H(65) 3.196 ? . 1_545 H(13) H(66) 3.119 ? . 1_545 H(13) H(71) 3.414 ? . 6_546 H(14) Cl(1) 3.298 ? . 6_546 H(14) C(38) 3.452 ? . 6_546 H(14) C(48) 3.122 ? . 6_546 H(14) C(50) 3.514 ? . 6_546 H(14) H(47) 2.771 ? . 6_546 H(14) H(48) 3.261 ? . 6_546 H(14) H(72) 3.146 ? . 6_546 H(15) C(38) 3.540 ? . 6_546 H(15) H(47) 3.218 ? . 6_546 H(15) H(48) 2.952 ? . 6_546 H(15) H(62) 3.564 ? . 7_557 H(15) H(68) 3.594 ? . . H(15) H(69) 3.092 ? . . H(16) C(48) 2.996 ? . 6_546 H(16) C(50) 3.285 ? . 6_546 H(16) H(69) 3.413 ? . . H(17) C(33) 3.516 ? . 3_556 H(17) C(35) 3.440 ? . 3_556 H(17) H(33) 3.179 ? . 4_554 H(17) H(35) 3.076 ? . 3_556 H(17) H(36) 3.172 ? . 3_556 H(17) H(42) 2.473 ? . 3_556 H(18) C(39) 3.569 ? . 1_545 H(18) C(58) 3.585 ? . 1_545 H(18) H(29) 3.572 ? . 4_554 H(18) H(33) 2.674 ? . 4_554 H(18) H(50) 2.861 ? . 1_545 H(19) C(30) 3.492 ? . 4_554 H(19) H(29) 2.685 ? . 4_554 H(19) H(30) 3.480 ? . 4_554 H(19) H(33) 2.931 ? . 4_554 H(19) H(70) 3.212 ? . 6_546 H(19) H(71) 3.245 ? . 6_546 H(20) C(29) 3.418 ? . 1_545 H(20) H(27) 3.011 ? . 1_545 H(20) H(28) 2.952 ? . 1_545 H(20) H(46) 3.412 ? . 4_555 H(20) H(58) 3.418 ? . 4_555 H(20) H(59) 3.547 ? . 4_555 H(21) C(53) 3.567 ? . 1_545 H(21) C(54) 3.348 ? . 3_556 H(21) C(55) 3.493 ? . 3_556 H(21) C(60) 3.055 ? . 1_545 H(21) H(28) 3.531 ? . 1_545 H(21) H(35) 2.948 ? . 3_556 H(21) H(36) 3.389 ? . 3_556 H(22) C(33) 3.525 ? . 3_556 H(22) C(42) 3.508 ? . 4_555 H(22) H(35) 3.273 ? . 3_556 H(22) H(36) 2.925 ? . 3_556 H(22) H(57) 2.811 ? . 4_555 H(22) H(58) 3.347 ? . 4_555 H(22) H(59) 2.923 ? . 4_555 H(23) Cl(3) 3.441 ? . 1_545 H(23) C(39) 2.996 ? . 1_545 H(23) C(47) 3.337 ? . 6_546 H(23) H(50) 2.901 ? . 1_545 H(23) H(51) 2.704 ? . 1_545 H(23) H(52) 2.873 ? . 1_545 H(23) H(69) 3.408 ? . 6_546 H(23) H(70) 3.004 ? . 6_546 H(23) H(71) 3.057 ? . 6_546 H(24) Cl(3) 3.415 ? . 1_545 H(24) C(29) 2.953 ? . 1_545 H(24) C(58) 3.438 ? . 1_545 H(24) C(60) 3.520 ? . 1_545 H(24) H(26) 2.932 ? . 1_545 H(24) H(27) 3.144 ? . 1_545 H(24) H(28) 2.341 ? . 1_545 H(24) H(52) 3.183 ? . 1_545 H(25) Cl(3) 3.409 ? . 1_545 H(25) H(26) 3.398 ? . 1_545 H(25) H(27) 3.538 ? . 1_545 H(25) H(28) 3.410 ? . 1_545 H(25) H(71) 3.573 ? . 6_546 H(26) H(24) 2.932 ? . 1_565 H(26) H(25) 3.398 ? . 1_565 H(26) H(45) 3.263 ? . 4_565 H(27) C(37) 3.084 ? . 4_565 H(27) H(20) 3.011 ? . 1_565 H(27) H(24) 3.144 ? . 1_565 H(27) H(25) 3.538 ? . 1_565 H(27) H(44) 3.550 ? . 4_565 H(27) H(45) 2.619 ? . 4_565 H(27) H(46) 2.709 ? . 4_565 H(28) C(27) 3.246 ? . 1_565 H(28) C(58) 3.380 ? . . H(28) C(60) 3.264 ? . . H(28) H(20) 2.952 ? . 1_565 H(28) H(21) 3.531 ? . 1_565 H(28) H(24) 2.341 ? . 1_565 H(28) H(25) 3.410 ? . 1_565 H(29) C(25) 3.461 ? . 4_555 H(29) H(18) 3.572 ? . 4_555 H(29) H(19) 2.685 ? . 4_555 H(29) H(53) 2.823 ? . 4_555 H(29) H(67) 3.516 ? . 7_557 H(29) H(70) 3.465 ? . 7_557 H(30) C(47) 3.569 ? . 7_557 H(30) H(19) 3.480 ? . 4_555 H(30) H(45) 3.304 ? . 4_565 H(30) H(67) 2.904 ? . 7_557 H(30) H(70) 2.777 ? . 7_557 H(31) H(53) 3.353 ? . 4_555 H(31) H(60) 3.521 ? . 4_555 H(31) H(61) 3.317 ? . 4_555 H(31) H(67) 3.241 ? . 7_557 H(32) C(54) 3.573 ? . 3_566 H(32) C(55) 3.060 ? . 3_566 H(33) C(25) 3.096 ? . 4_555 H(33) H(17) 3.179 ? . 4_555 H(33) H(18) 2.674 ? . 4_555 H(33) H(19) 2.931 ? . 4_555 H(33) H(50) 3.312 ? . 4_565 H(34) C(35) 3.408 ? . 2_556 H(34) H(41) 3.225 ? . 2_556 H(34) H(42) 3.007 ? . 2_556 H(34) H(43) 3.440 ? . 2_556 H(34) H(53) 3.136 ? . 4_555 H(35) C(26) 3.553 ? . 3_556 H(35) C(52) 3.534 ? . . H(35) C(53) 3.426 ? . . H(35) C(53) 3.567 ? . 3_566 H(35) C(59) 3.555 ? . . H(35) C(60) 3.450 ? . . H(35) H(17) 3.076 ? . 3_556 H(35) H(21) 2.948 ? . 3_556 H(35) H(22) 3.273 ? . 3_556 H(36) C(26) 3.576 ? . 3_556 H(36) H(3) 3.004 ? . 3_556 H(36) H(5) 3.358 ? . 3_556 H(36) H(17) 3.172 ? . 3_556 H(36) H(21) 3.389 ? . 3_556 H(36) H(22) 2.925 ? . 3_556 H(36) H(38) 2.880 ? . 3_556 H(36) H(40) 3.530 ? . 3_556 H(37) C(34) 3.532 ? . 3_556 H(37) C(52) 3.361 ? . . H(37) C(56) 3.599 ? . . H(37) C(57) 3.484 ? . . H(37) C(61) 3.352 ? . . H(37) H(38) 2.810 ? . 3_556 H(37) H(40) 3.593 ? . 3_556 H(38) C(33) 3.202 ? . 3_556 H(38) C(34) 3.082 ? . 3_556 H(38) H(5) 2.725 ? . 3_556 H(38) H(36) 2.880 ? . 3_556 H(38) H(37) 2.810 ? . 3_556 H(38) H(38) 2.129 ? . 3_556 H(38) H(40) 3.552 ? . 3_556 H(39) C(19) 3.579 ? . 3_556 H(39) C(41) 3.015 ? . 3_556 H(39) H(1) 3.528 ? . 3_556 H(39) H(5) 3.307 ? . 3_556 H(39) H(7) 2.723 ? . 3_556 H(39) H(53) 3.573 ? . 3_556 H(39) H(54) 3.100 ? . 3_556 H(39) H(55) 2.155 ? . 3_556 H(40) C(41) 3.421 ? . 4_555 H(40) C(42) 3.445 ? . 4_555 H(40) H(36) 3.530 ? . 3_556 H(40) H(37) 3.593 ? . 3_556 H(40) H(38) 3.552 ? . 3_556 H(40) H(54) 2.528 ? . 4_555 H(40) H(55) 3.406 ? . 3_556 H(40) H(56) 3.336 ? . 4_555 H(40) H(57) 2.849 ? . 4_555 H(40) H(60) 3.432 ? . 4_555 H(41) C(35) 3.562 ? . 2_556 H(41) C(41) 3.160 ? . 3_556 H(41) H(4) 3.516 ? . 2_556 H(41) H(34) 3.225 ? . 2_556 H(41) H(41) 2.797 ? . 2_556 H(41) H(43) 3.461 ? . 2_556 H(41) H(53) 3.309 ? . 3_556 H(41) H(54) 2.865 ? . 3_556 H(41) H(54) 3.210 ? . 4_555 H(41) H(55) 2.802 ? . 3_556 H(42) C(25) 3.379 ? . 3_556 H(42) H(17) 2.473 ? . 3_556 H(42) H(34) 3.007 ? . 2_556 H(42) H(55) 3.292 ? . 3_556 H(43) C(54) 3.401 ? . 3_566 H(43) H(34) 3.440 ? . 2_556 H(43) H(41) 3.461 ? . 2_556 H(44) C(22) 3.281 ? . 4_554 H(44) H(2) 3.404 ? . 4_554 H(44) H(10) 3.470 ? . 4_554 H(44) H(11) 2.368 ? . 4_554 H(44) H(13) 3.477 ? . 4_554 H(44) H(27) 3.550 ? . 4_564 H(44) H(65) 3.218 ? . 4_564 H(45) C(29) 3.355 ? . 4_564 H(45) H(26) 3.263 ? . 4_564 H(45) H(27) 2.619 ? . 4_564 H(45) H(30) 3.304 ? . 4_564 H(45) H(65) 3.374 ? . 4_564 H(46) H(20) 3.412 ? . 4_554 H(46) H(27) 2.709 ? . 4_564 H(47) C(22) 3.580 ? . 6_556 H(47) C(23) 3.416 ? . 6_556 H(47) H(12) 2.658 ? . 6_556 H(47) H(14) 2.771 ? . 6_556 H(47) H(15) 3.218 ? . 6_556 H(48) C(22) 3.442 ? . 6_556 H(48) C(23) 3.489 ? . 6_556 H(48) H(11) 3.088 ? . 4_554 H(48) H(12) 2.504 ? . 6_556 H(48) H(14) 3.261 ? . 6_556 H(48) H(15) 2.952 ? . 6_556 H(48) H(65) 3.326 ? . 4_564 H(49) C(49) 3.382 ? . 6_546 H(49) H(9) 2.909 ? . 4_554 H(49) H(10) 3.514 ? . 4_554 H(49) H(11) 3.252 ? . 4_554 H(49) H(12) 2.878 ? . 6_556 H(49) H(64) 2.736 ? . 6_546 H(50) H(18) 2.861 ? . 1_565 H(50) H(23) 2.901 ? . 1_565 H(50) H(33) 3.312 ? . 4_564 H(50) H(70) 3.435 ? . 6_556 H(51) C(27) 3.597 ? . 1_565 H(51) C(47) 3.533 ? . 6_556 H(51) H(23) 2.704 ? . 1_565 H(51) H(69) 3.293 ? . 6_556 H(51) H(70) 2.906 ? . 6_556 H(52) C(27) 3.478 ? . 1_565 H(52) C(58) 3.354 ? . . H(52) H(23) 2.873 ? . 1_565 H(52) H(24) 3.183 ? . 1_565 H(53) C(10) 3.231 ? . 4_554 H(53) C(11) 3.178 ? . 4_554 H(53) C(30) 3.392 ? . 4_554 H(53) H(4) 3.308 ? . 4_554 H(53) H(29) 2.823 ? . 4_554 H(53) H(31) 3.353 ? . 4_554 H(53) H(34) 3.136 ? . 4_554 H(53) H(39) 3.573 ? . 3_556 H(53) H(41) 3.309 ? . 3_556 H(54) C(11) 3.435 ? . 4_554 H(54) C(12) 3.442 ? . 4_554 H(54) C(34) 3.365 ? . 4_554 H(54) H(4) 3.495 ? . 4_554 H(54) H(39) 3.100 ? . 3_556 H(54) H(40) 2.528 ? . 4_554 H(54) H(41) 2.865 ? . 3_556 H(54) H(41) 3.210 ? . 4_554 H(55) C(34) 3.107 ? . 3_556 H(55) C(35) 3.416 ? . 3_556 H(55) H(39) 2.155 ? . 3_556 H(55) H(40) 3.406 ? . 3_556 H(55) H(41) 2.802 ? . 3_556 H(55) H(42) 3.292 ? . 3_556 H(56) H(40) 3.336 ? . 4_554 H(56) H(56) 3.255 ? . 2_555 H(57) H(22) 2.811 ? . 4_554 H(57) H(40) 2.849 ? . 4_554 H(58) H(20) 3.418 ? . 4_554 H(58) H(22) 3.347 ? . 4_554 H(59) C(2) 3.225 ? . 4_554 H(59) C(3) 3.439 ? . 4_554 H(59) C(4) 3.506 ? . 4_554 H(59) C(5) 3.415 ? . 4_554 H(59) C(6) 3.261 ? . 4_554 H(59) C(7) 3.109 ? . 4_554 H(59) H(3) 3.484 ? . 4_554 H(59) H(10) 3.038 ? . 4_554 H(59) H(20) 3.547 ? . 4_554 H(59) H(22) 2.923 ? . 4_554 H(60) C(1) 3.493 ? . 4_554 H(60) C(2) 3.320 ? . 4_554 H(60) C(8) 2.813 ? . 4_554 H(60) C(9) 2.974 ? . 4_554 H(60) C(10) 3.276 ? . 4_554 H(60) C(11) 3.450 ? . 4_554 H(60) C(12) 3.383 ? . 4_554 H(60) C(13) 3.029 ? . 4_554 H(60) H(5) 3.486 ? . 4_554 H(60) H(31) 3.521 ? . 4_554 H(60) H(40) 3.432 ? . 4_554 H(61) C(3) 3.567 ? . 4_554 H(61) C(21) 3.237 ? . 4_554 H(61) H(8) 3.384 ? . 4_554 H(61) H(10) 2.336 ? . 4_554 H(61) H(31) 3.317 ? . 4_554 H(62) Cl(2) 3.047 ? . 7_557 H(62) C(21) 3.018 ? . 7_557 H(62) H(8) 2.496 ? . 7_557 H(62) H(9) 2.683 ? . 7_557 H(62) H(10) 3.560 ? . 7_557 H(62) H(15) 3.564 ? . 7_557 H(62) H(68) 3.435 ? . 7_557 H(63) Cl(2) 2.727 ? . . H(63) Cl(3) 3.353 ? . . H(63) H(67) 3.546 ? . 7_557 H(63) H(68) 3.105 ? . 7_557 H(64) C(21) 3.420 ? . 7_557 H(64) C(22) 3.434 ? . 1_565 H(64) C(38) 3.559 ? . 6_556 H(64) H(8) 3.544 ? . 7_557 H(64) H(9) 2.541 ? . 7_557 H(64) H(11) 3.391 ? . 1_565 H(64) H(12) 3.009 ? . 1_565 H(64) H(13) 3.344 ? . 1_565 H(64) H(49) 2.736 ? . 6_556 H(65) Cl(3) 3.526 ? . . H(65) C(22) 3.399 ? . 1_565 H(65) H(9) 3.395 ? . 7_557 H(65) H(11) 3.028 ? . 1_565 H(65) H(12) 3.419 ? . 1_565 H(65) H(13) 3.196 ? . 1_565 H(65) H(44) 3.218 ? . 4_565 H(65) H(45) 3.374 ? . 4_565 H(65) H(48) 3.326 ? . 4_565 H(66) Cl(1) 3.573 ? . 6_556 H(66) Cl(3) 2.957 ? . . H(66) H(12) 3.544 ? . 1_565 H(66) H(13) 3.119 ? . 1_565 H(67) Cl(2) 2.864 ? . 7_557 H(67) C(30) 3.398 ? . 7_557 H(67) H(29) 3.516 ? . 7_557 H(67) H(30) 2.904 ? . 7_557 H(67) H(31) 3.241 ? . 7_557 H(67) H(63) 3.546 ? . 7_557 H(68) Cl(1) 3.583 ? . . H(68) Cl(2) 2.704 ? . . H(68) Cl(2) 3.581 ? . 7_557 H(68) H(15) 3.594 ? . . H(68) H(62) 3.435 ? . 7_557 H(68) H(63) 3.105 ? . 7_557 H(69) Cl(1) 2.860 ? . . H(69) H(15) 3.092 ? . . H(69) H(16) 3.413 ? . . H(69) H(23) 3.408 ? . 6_556 H(69) H(51) 3.293 ? . 6_546 H(70) C(30) 3.530 ? . 7_557 H(70) H(19) 3.212 ? . 6_556 H(70) H(23) 3.004 ? . 6_556 H(70) H(29) 3.465 ? . 7_557 H(70) H(30) 2.777 ? . 7_557 H(70) H(50) 3.435 ? . 6_546 H(70) H(51) 2.906 ? . 6_546 H(71) C(4) 3.574 ? . 6_556 H(71) C(5) 3.061 ? . 6_556 H(71) C(6) 3.364 ? . 6_556 H(71) H(2) 3.035 ? . 6_556 H(71) H(13) 3.414 ? . 6_556 H(71) H(19) 3.245 ? . 6_556 H(71) H(23) 3.057 ? . 6_556 H(71) H(25) 3.573 ? . 6_556 H(72) Cl(1) 2.98(9) ? . . H(72) Cl(2) 3.44(11) ? . . H(72) Cl(3) 3.27(8) ? . . H(72) H(14) 3.146 ? . 6_556 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- Kawaguchi_CIF_rivised.cif' #============================================================================== data__O2OHNbCl3-AN-Complex-1 _database_code_depnum_ccdc_archive 'CCDC 789692' #TrackingRef '- Kawaguchi_CIF_rivised.cif' _audit_creation_date 2010-11-16 _audit_creation_method 'by CrystalStructure 4.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C45 H65 Cl3 N Nb O3' _chemical_formula_moiety 'C45 H65 Cl3 N Nb O3' _chemical_formula_weight 867.28 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.485(5) _cell_length_b 20.674(8) _cell_length_c 20.252(8) _cell_angle_alpha 90.0000 _cell_angle_beta 116.921(5) _cell_angle_gamma 90.0000 _cell_volume 4661(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6422 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 173 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832.00 _exptl_absorpt_coefficient_mu 0.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.911 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 173 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 34400 _diffrn_reflns_av_R_equivalents 0.0983 _diffrn_reflns_theta_max 26.50 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9473 _reflns_number_gt 6502 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.1322 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 9471 _refine_ls_number_parameters 482 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0404P)^2^+3.1693P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.370 _refine_diff_density_min -0.410 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Nb(1) Nb 0.72927(4) 0.88402(2) 0.04967(2) 0.02206(12) Uani 1.0 4 d . . . Cl(1) Cl 0.63421(13) 0.92124(6) 0.12107(7) 0.0432(4) Uani 1.0 4 d . . . Cl(2) Cl 0.53854(11) 0.87928(8) -0.05300(7) 0.0469(4) Uani 1.0 4 d . . . Cl(3) Cl 0.91625(11) 0.91973(6) 0.14900(6) 0.0321(3) Uani 1.0 4 d . . . O(1) O 0.7308(3) 0.79938(14) 0.08007(15) 0.0216(7) Uani 1.0 4 d . . . O(2) O 1.1353(3) 0.84824(15) 0.12991(17) 0.0309(8) Uani 1.0 4 d . . . O(3) O 0.8055(3) 0.86786(13) -0.01007(14) 0.0208(7) Uani 1.0 4 d . . . N(1) N 0.7234(4) 0.9892(2) 0.0164(2) 0.0367(11) Uani 1.0 4 d . . . C(1) C 0.9378(4) 0.7607(2) 0.0692(3) 0.0174(10) Uani 1.0 4 d . . . C(2) C 0.8364(4) 0.7140(2) 0.0564(2) 0.0186(10) Uani 1.0 4 d . . . C(3) C 0.7418(4) 0.7338(2) 0.0707(2) 0.0189(10) Uani 1.0 4 d . . . C(4) C 0.6566(4) 0.6895(3) 0.0738(3) 0.0230(11) Uani 1.0 4 d . . . C(5) C 0.6630(4) 0.6271(2) 0.0513(3) 0.0254(11) Uani 1.0 4 d . . . C(6) C 0.7467(4) 0.6064(3) 0.0277(3) 0.0246(11) Uani 1.0 4 d . . . C(7) C 0.8330(4) 0.6506(2) 0.0313(3) 0.0218(10) Uani 1.0 4 d . . . C(8) C 1.0639(4) 0.7381(2) 0.1264(2) 0.0192(10) Uani 1.0 4 d . . . C(9) C 1.1545(4) 0.7853(3) 0.1567(3) 0.0224(10) Uani 1.0 4 d . . . C(10) C 1.2676(4) 0.7708(3) 0.2163(3) 0.0267(11) Uani 1.0 4 d . . . C(11) C 1.2855(4) 0.7063(3) 0.2394(3) 0.0293(12) Uani 1.0 4 d . . . C(12) C 1.1992(4) 0.6579(3) 0.2104(3) 0.0234(11) Uani 1.0 4 d . . . C(13) C 1.0884(4) 0.6759(2) 0.1548(3) 0.0209(10) Uani 1.0 4 d . . . C(14) C 0.5668(4) 0.7086(3) 0.1025(3) 0.0292(12) Uani 1.0 4 d . . . C(15) C 0.4717(5) 0.7559(3) 0.0485(3) 0.0390(13) Uani 1.0 4 d . . . C(16) C 0.4990(5) 0.6499(3) 0.1101(3) 0.0432(14) Uani 1.0 4 d . . . C(17) C 0.6330(5) 0.7403(3) 0.1791(3) 0.0373(13) Uani 1.0 4 d . . . C(18) C 0.7408(5) 0.5366(3) 0.0005(3) 0.0303(12) Uani 1.0 4 d . . . C(19) C 0.6217(5) 0.5265(3) -0.0697(3) 0.0507(16) Uani 1.0 4 d . . . C(20) C 0.7460(6) 0.4893(3) 0.0603(3) 0.0500(16) Uani 1.0 4 d . . . C(21) C 0.8444(5) 0.5205(3) -0.0167(4) 0.0495(16) Uani 1.0 4 d . . . C(22) C 1.3638(5) 0.8232(3) 0.2555(3) 0.0310(12) Uani 1.0 4 d . . . C(23) C 1.4793(5) 0.7941(3) 0.3179(3) 0.0471(16) Uani 1.0 4 d . . . C(24) C 1.4005(5) 0.8580(3) 0.2018(3) 0.0381(13) Uani 1.0 4 d . . . C(25) C 1.3169(5) 0.8741(3) 0.2904(3) 0.0439(15) Uani 1.0 4 d . . . C(26) C 1.2236(5) 0.5897(3) 0.2428(3) 0.0279(12) Uani 1.0 4 d . . . C(27) C 1.2297(5) 0.5932(3) 0.3205(3) 0.0352(13) Uani 1.0 4 d . . . C(28) C 1.3433(5) 0.5644(3) 0.2500(3) 0.0388(14) Uani 1.0 4 d . . . C(29) C 1.1257(5) 0.5419(3) 0.1970(3) 0.0440(15) Uani 1.0 4 d . . . C(30) C 0.6784(5) 0.9244(3) -0.1702(3) 0.0357(13) Uani 1.0 4 d . . . C(31) C 0.8331(5) 0.9344(3) -0.2148(3) 0.0377(13) Uani 1.0 4 d . . . C(32) C 0.8137(4) 0.9214(3) -0.1457(3) 0.0242(11) Uani 1.0 4 d . . . C(33) C 0.8781(5) 0.9766(3) -0.0900(3) 0.0342(13) Uani 1.0 4 d . . . C(34) C 0.8667(4) 0.8570(2) -0.1084(3) 0.0190(10) Uani 1.0 4 d . . . C(35) C 0.9218(4) 0.8152(3) -0.1385(3) 0.0217(10) Uani 1.0 4 d . . . C(36) C 0.9797(4) 0.7576(2) -0.1057(3) 0.0222(10) Uani 1.0 4 d . . . C(37) C 0.9884(4) 0.7434(2) -0.0363(3) 0.0223(10) Uani 1.0 4 d . . . C(38) C 0.9334(4) 0.7806(2) -0.0043(3) 0.0188(10) Uani 1.0 4 d . . . C(39) C 0.8684(4) 0.8359(2) -0.0416(3) 0.0196(10) Uani 1.0 4 d . . . C(40) C 1.0315(5) 0.7107(3) -0.1423(3) 0.0273(11) Uani 1.0 4 d . . . C(41) C 1.0123(5) 0.7333(3) -0.2185(3) 0.0393(14) Uani 1.0 4 d . . . C(42) C 1.1662(5) 0.7043(4) -0.0926(3) 0.0590(19) Uani 1.0 4 d . . . C(43) C 0.9720(7) 0.6450(3) -0.1507(4) 0.0597(19) Uani 1.0 4 d . . . C(44) C 0.7303(6) 1.0431(3) 0.0077(3) 0.0398(14) Uani 1.0 4 d . . . C(45) C 0.7478(7) 1.1125(3) -0.0008(4) 0.075(3) Uani 1.0 4 d . . . H(1) H 0.9262 0.7979 0.0888 0.0300 Uiso 1.0 4 calc R . . H(2) H 1.0665 0.8604 0.1223 0.0371 Uiso 1.0 4 calc R . . H(5) H 0.6070 0.5962 0.0519 0.0305 Uiso 1.0 4 calc R . . H(7) H 0.8915 0.6373 0.0164 0.0261 Uiso 1.0 4 calc R . . H(11) H 1.3621 0.6946 0.2776 0.0352 Uiso 1.0 4 calc R . . H(13) H 1.0267 0.6443 0.1351 0.0250 Uiso 1.0 4 calc R . . H(15A) H 0.4086 0.7625 0.0639 0.0467 Uiso 1.0 4 calc R . . H(15B) H 0.4363 0.7377 -0.0017 0.0467 Uiso 1.0 4 calc R . . H(15C) H 0.5099 0.7974 0.0488 0.0467 Uiso 1.0 4 calc R . . H(16A) H 0.5563 0.6156 0.1370 0.0518 Uiso 1.0 4 calc R . . H(16B) H 0.4428 0.6343 0.0607 0.0518 Uiso 1.0 4 calc R . . H(16C) H 0.4542 0.6622 0.1374 0.0518 Uiso 1.0 4 calc R . . H(17A) H 0.7007 0.7129 0.2113 0.0447 Uiso 1.0 4 calc R . . H(17B) H 0.5776 0.7453 0.2009 0.0447 Uiso 1.0 4 calc R . . H(17C) H 0.6630 0.7829 0.1740 0.0447 Uiso 1.0 4 calc R . . H(19A) H 0.6237 0.5502 -0.1110 0.0609 Uiso 1.0 4 calc R . . H(19B) H 0.5552 0.5425 -0.0612 0.0609 Uiso 1.0 4 calc R . . H(19C) H 0.6103 0.4803 -0.0817 0.0609 Uiso 1.0 4 calc R . . H(20A) H 0.7352 0.4450 0.0411 0.0601 Uiso 1.0 4 calc R . . H(20B) H 0.6820 0.4997 0.0739 0.0601 Uiso 1.0 4 calc R . . H(20C) H 0.8241 0.4930 0.1041 0.0601 Uiso 1.0 4 calc R . . H(21A) H 0.9207 0.5279 0.0276 0.0594 Uiso 1.0 4 calc R . . H(21B) H 0.8403 0.5482 -0.0570 0.0594 Uiso 1.0 4 calc R . . H(21C) H 0.8390 0.4751 -0.0316 0.0594 Uiso 1.0 4 calc R . . H(23A) H 1.4601 0.7732 0.3546 0.0565 Uiso 1.0 4 calc R . . H(23B) H 1.5381 0.8286 0.3417 0.0565 Uiso 1.0 4 calc R . . H(23C) H 1.5130 0.7621 0.2968 0.0565 Uiso 1.0 4 calc R . . H(24A) H 1.3323 0.8832 0.1660 0.0457 Uiso 1.0 4 calc R . . H(24B) H 1.4245 0.8260 0.1753 0.0457 Uiso 1.0 4 calc R . . H(24C) H 1.4681 0.8871 0.2297 0.0457 Uiso 1.0 4 calc R . . H(25A) H 1.3723 0.9109 0.3069 0.0527 Uiso 1.0 4 calc R . . H(25B) H 1.3107 0.8553 0.3330 0.0527 Uiso 1.0 4 calc R . . H(25C) H 1.2374 0.8888 0.2538 0.0527 Uiso 1.0 4 calc R . . H(27A) H 1.1539 0.6105 0.3165 0.0423 Uiso 1.0 4 calc R . . H(27B) H 1.2960 0.6216 0.3522 0.0423 Uiso 1.0 4 calc R . . H(27C) H 1.2431 0.5497 0.3421 0.0423 Uiso 1.0 4 calc R . . H(28A) H 1.3575 0.5208 0.2712 0.0465 Uiso 1.0 4 calc R . . H(28B) H 1.4083 0.5931 0.2825 0.0465 Uiso 1.0 4 calc R . . H(28C) H 1.3409 0.5631 0.2010 0.0465 Uiso 1.0 4 calc R . . H(29A) H 1.1190 0.5395 0.1470 0.0528 Uiso 1.0 4 calc R . . H(29B) H 1.0490 0.5563 0.1943 0.0528 Uiso 1.0 4 calc R . . H(29C) H 1.1460 0.4991 0.2203 0.0528 Uiso 1.0 4 calc R . . H(30A) H 0.6465 0.9657 -0.1951 0.0428 Uiso 1.0 4 calc R . . H(30B) H 0.6638 0.9207 -0.1267 0.0428 Uiso 1.0 4 calc R . . H(30C) H 0.6384 0.8887 -0.2043 0.0428 Uiso 1.0 4 calc R . . H(31A) H 0.7946 0.9001 -0.2514 0.0452 Uiso 1.0 4 calc R . . H(31B) H 0.9194 0.9351 -0.2004 0.0452 Uiso 1.0 4 calc R . . H(31C) H 0.7976 0.9762 -0.2365 0.0452 Uiso 1.0 4 calc R . . H(33A) H 0.8344 1.0173 -0.1089 0.0411 Uiso 1.0 4 calc R . . H(33B) H 0.9603 0.9812 -0.0838 0.0411 Uiso 1.0 4 calc R . . H(33C) H 0.8805 0.9664 -0.0422 0.0411 Uiso 1.0 4 calc R . . H(35) H 0.9196 0.8271 -0.1844 0.0261 Uiso 1.0 4 calc R . . H(37) H 1.0338 0.7068 -0.0103 0.0267 Uiso 1.0 4 calc R . . H(41A) H 0.9264 0.7402 -0.2503 0.0471 Uiso 1.0 4 calc R . . H(41B) H 1.0425 0.7003 -0.2406 0.0471 Uiso 1.0 4 calc R . . H(41C) H 1.0557 0.7739 -0.2136 0.0471 Uiso 1.0 4 calc R . . H(42A) H 1.1999 0.6722 -0.1136 0.0708 Uiso 1.0 4 calc R . . H(42B) H 1.1802 0.6905 -0.0430 0.0708 Uiso 1.0 4 calc R . . H(42C) H 1.2051 0.7462 -0.0891 0.0708 Uiso 1.0 4 calc R . . H(43A) H 0.8848 0.6496 -0.1797 0.0716 Uiso 1.0 4 calc R . . H(43B) H 0.9907 0.6277 -0.1016 0.0716 Uiso 1.0 4 calc R . . H(43C) H 1.0022 0.6153 -0.1762 0.0716 Uiso 1.0 4 calc R . . H(45A) H 0.7827 1.1180 -0.0352 0.0900 Uiso 1.0 4 calc R . . H(45B) H 0.8022 1.1309 0.0475 0.0900 Uiso 1.0 4 calc R . . H(45C) H 0.6702 1.1348 -0.0204 0.0900 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb(1) 0.0278(3) 0.0160(2) 0.0234(3) 0.0045(2) 0.01256(18) -0.00047(19) Cl(1) 0.0614(9) 0.0288(8) 0.0599(9) 0.0004(7) 0.0454(8) -0.0094(7) Cl(2) 0.0290(7) 0.0674(11) 0.0363(8) 0.0078(8) 0.0078(6) 0.0116(8) Cl(3) 0.0387(8) 0.0250(7) 0.0287(7) -0.0041(6) 0.0119(6) -0.0038(5) O(1) 0.0223(17) 0.0158(17) 0.0287(17) 0.0014(13) 0.0132(14) -0.0033(13) O(2) 0.0289(19) 0.0184(18) 0.043(2) 0.0006(14) 0.0146(16) 0.0088(15) O(3) 0.0250(17) 0.0169(17) 0.0189(16) 0.0068(13) 0.0084(14) 0.0014(12) N(1) 0.052(3) 0.026(3) 0.035(3) 0.012(3) 0.022(3) 0.002(2) C(1) 0.018(3) 0.017(3) 0.019(3) 0.0022(19) 0.010(2) 0.0014(19) C(2) 0.021(3) 0.016(3) 0.015(3) 0.0034(19) 0.0047(19) 0.0038(17) C(3) 0.023(3) 0.014(3) 0.018(3) 0.0013(19) 0.007(2) -0.0023(17) C(4) 0.021(3) 0.019(3) 0.027(3) 0.004(2) 0.010(2) -0.0013(19) C(5) 0.023(3) 0.019(3) 0.035(3) 0.000(2) 0.013(3) 0.006(2) C(6) 0.024(3) 0.019(3) 0.028(3) 0.000(2) 0.010(2) -0.002(2) C(7) 0.027(3) 0.020(3) 0.020(3) 0.006(2) 0.012(2) -0.0004(19) C(8) 0.024(3) 0.022(3) 0.014(3) 0.004(2) 0.012(2) 0.0024(18) C(9) 0.025(3) 0.021(3) 0.024(3) 0.002(2) 0.013(3) 0.0041(19) C(10) 0.024(3) 0.032(3) 0.026(3) -0.001(3) 0.013(3) -0.000(2) C(11) 0.022(3) 0.040(4) 0.021(3) 0.003(3) 0.004(2) 0.005(3) C(12) 0.026(3) 0.024(3) 0.021(3) 0.004(2) 0.011(3) 0.003(2) C(13) 0.024(3) 0.020(3) 0.018(3) -0.000(2) 0.010(2) -0.0028(19) C(14) 0.024(3) 0.028(3) 0.042(3) 0.001(2) 0.021(3) 0.001(3) C(15) 0.026(3) 0.039(4) 0.053(4) 0.007(3) 0.019(3) 0.002(3) C(16) 0.043(4) 0.038(4) 0.065(4) -0.002(3) 0.038(3) 0.002(3) C(17) 0.038(3) 0.040(4) 0.040(3) 0.000(3) 0.023(3) -0.002(3) C(18) 0.033(3) 0.018(3) 0.039(3) 0.000(2) 0.016(3) -0.008(2) C(19) 0.050(4) 0.030(4) 0.059(4) -0.003(3) 0.013(3) -0.018(3) C(20) 0.069(5) 0.019(3) 0.068(4) 0.008(3) 0.036(4) -0.001(3) C(21) 0.055(4) 0.021(3) 0.075(4) -0.007(3) 0.032(4) -0.025(3) C(22) 0.028(3) 0.034(3) 0.032(3) -0.006(3) 0.015(3) -0.002(3) C(23) 0.038(4) 0.051(4) 0.039(4) -0.014(3) 0.006(3) 0.005(3) C(24) 0.030(3) 0.041(4) 0.052(4) -0.002(3) 0.025(3) -0.000(3) C(25) 0.043(4) 0.051(4) 0.044(4) -0.018(3) 0.025(3) -0.019(3) C(26) 0.027(3) 0.029(3) 0.024(3) 0.008(3) 0.008(3) 0.007(2) C(27) 0.037(3) 0.036(3) 0.035(3) 0.007(3) 0.018(3) 0.012(3) C(28) 0.050(4) 0.036(4) 0.033(3) 0.014(3) 0.022(3) 0.007(3) C(29) 0.055(4) 0.022(3) 0.038(3) 0.007(3) 0.006(3) 0.009(3) C(30) 0.036(3) 0.038(4) 0.031(3) 0.014(3) 0.014(3) 0.010(3) C(31) 0.052(4) 0.028(3) 0.036(3) 0.005(3) 0.022(3) 0.011(3) C(32) 0.026(3) 0.026(3) 0.017(3) 0.003(2) 0.007(2) 0.006(2) C(33) 0.046(4) 0.019(3) 0.036(3) -0.006(3) 0.018(3) 0.000(3) C(34) 0.018(3) 0.018(3) 0.019(3) -0.0039(18) 0.006(2) -0.0006(18) C(35) 0.026(3) 0.026(3) 0.017(3) -0.002(2) 0.012(2) 0.0004(19) C(36) 0.023(3) 0.021(3) 0.025(3) -0.000(2) 0.013(2) -0.0026(19) C(37) 0.025(3) 0.018(3) 0.025(3) 0.0049(19) 0.013(2) 0.0045(19) C(38) 0.022(3) 0.017(3) 0.018(3) -0.0013(19) 0.010(2) 0.0031(18) C(39) 0.020(3) 0.017(3) 0.020(3) 0.0007(19) 0.009(2) -0.0009(18) C(40) 0.036(3) 0.024(3) 0.028(3) 0.001(3) 0.021(3) -0.002(2) C(41) 0.054(4) 0.041(4) 0.033(3) 0.003(3) 0.029(3) -0.001(3) C(42) 0.055(4) 0.076(5) 0.051(4) 0.034(4) 0.029(4) -0.000(4) C(43) 0.111(6) 0.029(4) 0.062(4) -0.009(4) 0.060(4) -0.011(3) C(44) 0.069(4) 0.029(4) 0.034(3) 0.016(3) 0.034(3) 0.008(3) C(45) 0.159(8) 0.021(3) 0.058(4) 0.015(5) 0.060(5) 0.012(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb(1) Cl(1) 2.376(2) yes . . Nb(1) Cl(2) 2.3495(13) yes . . Nb(1) Cl(3) 2.4061(13) yes . . Nb(1) O(1) 1.852(3) yes . . Nb(1) O(3) 1.877(4) yes . . Nb(1) N(1) 2.268(5) yes . . O(1) C(3) 1.385(6) yes . . O(2) C(9) 1.388(6) yes . . O(3) C(39) 1.384(7) yes . . N(1) C(44) 1.136(7) yes . . C(1) C(2) 1.519(7) yes . . C(1) C(8) 1.545(6) yes . . C(1) C(38) 1.521(7) yes . . C(2) C(3) 1.398(8) yes . . C(2) C(7) 1.400(6) yes . . C(3) C(4) 1.427(7) yes . . C(4) C(5) 1.384(7) yes . . C(4) C(14) 1.531(9) yes . . C(5) C(6) 1.397(8) yes . . C(6) C(7) 1.388(7) yes . . C(6) C(18) 1.535(7) yes . . C(8) C(9) 1.406(6) yes . . C(8) C(13) 1.386(6) yes . . C(9) C(10) 1.414(6) yes . . C(10) C(11) 1.396(7) yes . . C(10) C(22) 1.544(7) yes . . C(11) C(12) 1.390(7) yes . . C(12) C(13) 1.382(6) yes . . C(12) C(26) 1.526(7) yes . . C(14) C(15) 1.544(7) yes . . C(14) C(16) 1.527(8) yes . . C(14) C(17) 1.535(7) yes . . C(18) C(19) 1.536(6) yes . . C(18) C(20) 1.536(9) yes . . C(18) C(21) 1.521(10) yes . . C(22) C(23) 1.545(6) yes . . C(22) C(24) 1.538(9) yes . . C(22) C(25) 1.525(9) yes . . C(26) C(27) 1.541(8) yes . . C(26) C(28) 1.527(8) yes . . C(26) C(29) 1.518(7) yes . . C(30) C(32) 1.531(7) yes . . C(31) C(32) 1.548(9) yes . . C(32) C(33) 1.549(6) yes . . C(32) C(34) 1.527(6) yes . . C(34) C(35) 1.404(8) yes . . C(34) C(39) 1.411(7) yes . . C(35) C(36) 1.395(6) yes . . C(36) C(37) 1.391(7) yes . . C(36) C(40) 1.530(8) yes . . C(37) C(38) 1.374(8) yes . . C(38) C(39) 1.408(6) yes . . C(40) C(41) 1.523(8) yes . . C(40) C(42) 1.526(7) yes . . C(40) C(43) 1.521(8) yes . . C(44) C(45) 1.474(9) yes . . O(2) H(2) 0.840 no . . C(1) H(1) 0.908 no . . C(5) H(5) 0.950 no . . C(7) H(7) 0.950 no . . C(11) H(11) 0.950 no . . C(13) H(13) 0.950 no . . C(15) H(15A) 0.980 no . . C(15) H(15B) 0.980 no . . C(15) H(15C) 0.980 no . . C(16) H(16A) 0.980 no . . C(16) H(16B) 0.980 no . . C(16) H(16C) 0.980 no . . C(17) H(17A) 0.980 no . . C(17) H(17B) 0.980 no . . C(17) H(17C) 0.980 no . . C(19) H(19A) 0.980 no . . C(19) H(19B) 0.980 no . . C(19) H(19C) 0.980 no . . C(20) H(20A) 0.980 no . . C(20) H(20B) 0.980 no . . C(20) H(20C) 0.980 no . . C(21) H(21A) 0.980 no . . C(21) H(21B) 0.980 no . . C(21) H(21C) 0.980 no . . C(23) H(23A) 0.980 no . . C(23) H(23B) 0.980 no . . C(23) H(23C) 0.980 no . . C(24) H(24A) 0.980 no . . C(24) H(24B) 0.980 no . . C(24) H(24C) 0.980 no . . C(25) H(25A) 0.980 no . . C(25) H(25B) 0.980 no . . C(25) H(25C) 0.980 no . . C(27) H(27A) 0.980 no . . C(27) H(27B) 0.980 no . . C(27) H(27C) 0.980 no . . C(28) H(28A) 0.980 no . . C(28) H(28B) 0.980 no . . C(28) H(28C) 0.980 no . . C(29) H(29A) 0.980 no . . C(29) H(29B) 0.980 no . . C(29) H(29C) 0.980 no . . C(30) H(30A) 0.980 no . . C(30) H(30B) 0.980 no . . C(30) H(30C) 0.980 no . . C(31) H(31A) 0.980 no . . C(31) H(31B) 0.980 no . . C(31) H(31C) 0.980 no . . C(33) H(33A) 0.980 no . . C(33) H(33B) 0.980 no . . C(33) H(33C) 0.980 no . . C(35) H(35) 0.950 no . . C(37) H(37) 0.950 no . . C(41) H(41A) 0.980 no . . C(41) H(41B) 0.980 no . . C(41) H(41C) 0.980 no . . C(42) H(42A) 0.980 no . . C(42) H(42B) 0.980 no . . C(42) H(42C) 0.980 no . . C(43) H(43A) 0.980 no . . C(43) H(43B) 0.980 no . . C(43) H(43C) 0.980 no . . C(45) H(45A) 0.980 no . . C(45) H(45B) 0.980 no . . C(45) H(45C) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Nb(1) Cl(2) 88.09(7) yes . . . Cl(1) Nb(1) Cl(3) 87.41(6) yes . . . Cl(1) Nb(1) O(1) 92.09(12) yes . . . Cl(1) Nb(1) O(3) 171.33(10) yes . . . Cl(1) Nb(1) N(1) 84.95(15) yes . . . Cl(2) Nb(1) Cl(3) 164.51(6) yes . . . Cl(2) Nb(1) O(1) 96.23(9) yes . . . Cl(2) Nb(1) O(3) 91.65(9) yes . . . Cl(2) Nb(1) N(1) 83.89(10) yes . . . Cl(3) Nb(1) O(1) 98.74(8) yes . . . Cl(3) Nb(1) O(3) 90.59(9) yes . . . Cl(3) Nb(1) N(1) 80.95(10) yes . . . O(1) Nb(1) O(3) 96.56(14) yes . . . O(1) Nb(1) N(1) 177.03(18) yes . . . O(3) Nb(1) N(1) 86.40(16) yes . . . Nb(1) O(1) C(3) 150.0(4) yes . . . Nb(1) O(3) C(39) 160.4(3) yes . . . Nb(1) N(1) C(44) 172.2(4) yes . . . C(2) C(1) C(8) 115.1(4) yes . . . C(2) C(1) C(38) 110.3(3) yes . . . C(8) C(1) C(38) 113.0(5) yes . . . C(1) C(2) C(3) 119.8(4) yes . . . C(1) C(2) C(7) 122.9(5) yes . . . C(3) C(2) C(7) 117.4(5) yes . . . O(1) C(3) C(2) 117.4(4) yes . . . O(1) C(3) C(4) 120.0(5) yes . . . C(2) C(3) C(4) 122.5(4) yes . . . C(3) C(4) C(5) 115.4(5) yes . . . C(3) C(4) C(14) 122.7(4) yes . . . C(5) C(4) C(14) 121.9(5) yes . . . C(4) C(5) C(6) 124.2(5) yes . . . C(5) C(6) C(7) 117.6(5) yes . . . C(5) C(6) C(18) 119.2(5) yes . . . C(7) C(6) C(18) 123.2(5) yes . . . C(2) C(7) C(6) 122.0(5) yes . . . C(1) C(8) C(9) 117.6(4) yes . . . C(1) C(8) C(13) 123.4(4) yes . . . C(9) C(8) C(13) 118.7(4) yes . . . O(2) C(9) C(8) 121.2(4) yes . . . O(2) C(9) C(10) 117.5(4) yes . . . C(8) C(9) C(10) 121.3(4) yes . . . C(9) C(10) C(11) 115.8(4) yes . . . C(9) C(10) C(22) 122.2(4) yes . . . C(11) C(10) C(22) 122.0(4) yes . . . C(10) C(11) C(12) 124.7(4) yes . . . C(11) C(12) C(13) 116.7(4) yes . . . C(11) C(12) C(26) 121.1(4) yes . . . C(13) C(12) C(26) 122.0(4) yes . . . C(8) C(13) C(12) 122.6(4) yes . . . C(4) C(14) C(15) 110.7(5) yes . . . C(4) C(14) C(16) 111.6(5) yes . . . C(4) C(14) C(17) 110.0(4) yes . . . C(15) C(14) C(16) 106.9(4) yes . . . C(15) C(14) C(17) 109.6(4) yes . . . C(16) C(14) C(17) 107.9(5) yes . . . C(6) C(18) C(19) 109.2(4) yes . . . C(6) C(18) C(20) 109.8(5) yes . . . C(6) C(18) C(21) 112.3(5) yes . . . C(19) C(18) C(20) 108.7(5) yes . . . C(19) C(18) C(21) 109.1(5) yes . . . C(20) C(18) C(21) 107.7(5) yes . . . C(10) C(22) C(23) 111.6(4) yes . . . C(10) C(22) C(24) 112.1(4) yes . . . C(10) C(22) C(25) 110.5(5) yes . . . C(23) C(22) C(24) 107.1(5) yes . . . C(23) C(22) C(25) 107.6(4) yes . . . C(24) C(22) C(25) 107.8(5) yes . . . C(12) C(26) C(27) 107.7(4) yes . . . C(12) C(26) C(28) 110.7(5) yes . . . C(12) C(26) C(29) 112.9(4) yes . . . C(27) C(26) C(28) 109.0(4) yes . . . C(27) C(26) C(29) 107.9(5) yes . . . C(28) C(26) C(29) 108.5(5) yes . . . C(30) C(32) C(31) 107.6(4) yes . . . C(30) C(32) C(33) 109.8(5) yes . . . C(30) C(32) C(34) 111.2(4) yes . . . C(31) C(32) C(33) 106.8(5) yes . . . C(31) C(32) C(34) 112.9(5) yes . . . C(33) C(32) C(34) 108.5(3) yes . . . C(32) C(34) C(35) 120.6(5) yes . . . C(32) C(34) C(39) 123.9(5) yes . . . C(35) C(34) C(39) 115.4(4) yes . . . C(34) C(35) C(36) 124.7(5) yes . . . C(35) C(36) C(37) 116.6(5) yes . . . C(35) C(36) C(40) 123.5(5) yes . . . C(37) C(36) C(40) 119.9(4) yes . . . C(36) C(37) C(38) 122.1(4) yes . . . C(1) C(38) C(37) 120.4(4) yes . . . C(1) C(38) C(39) 120.1(5) yes . . . C(37) C(38) C(39) 119.5(5) yes . . . O(3) C(39) C(34) 122.0(4) yes . . . O(3) C(39) C(38) 116.7(5) yes . . . C(34) C(39) C(38) 121.3(5) yes . . . C(36) C(40) C(41) 112.9(4) yes . . . C(36) C(40) C(42) 108.4(4) yes . . . C(36) C(40) C(43) 109.1(6) yes . . . C(41) C(40) C(42) 108.4(5) yes . . . C(41) C(40) C(43) 108.4(4) yes . . . C(42) C(40) C(43) 109.4(5) yes . . . N(1) C(44) C(45) 176.3(7) yes . . . C(9) O(2) H(2) 109.466 no . . . C(2) C(1) H(1) 109.101 no . . . C(8) C(1) H(1) 103.727 no . . . C(38) C(1) H(1) 104.865 no . . . C(4) C(5) H(5) 117.923 no . . . C(6) C(5) H(5) 117.925 no . . . C(2) C(7) H(7) 118.985 no . . . C(6) C(7) H(7) 118.986 no . . . C(10) C(11) H(11) 117.624 no . . . C(12) C(11) H(11) 117.628 no . . . C(8) C(13) H(13) 118.683 no . . . C(12) C(13) H(13) 118.684 no . . . C(14) C(15) H(15A) 109.473 no . . . C(14) C(15) H(15B) 109.467 no . . . C(14) C(15) H(15C) 109.472 no . . . H(15A) C(15) H(15B) 109.471 no . . . H(15A) C(15) H(15C) 109.468 no . . . H(15B) C(15) H(15C) 109.476 no . . . C(14) C(16) H(16A) 109.473 no . . . C(14) C(16) H(16B) 109.466 no . . . C(14) C(16) H(16C) 109.468 no . . . H(16A) C(16) H(16B) 109.477 no . . . H(16A) C(16) H(16C) 109.471 no . . . H(16B) C(16) H(16C) 109.473 no . . . C(14) C(17) H(17A) 109.472 no . . . C(14) C(17) H(17B) 109.473 no . . . C(14) C(17) H(17C) 109.475 no . . . H(17A) C(17) H(17B) 109.474 no . . . H(17A) C(17) H(17C) 109.472 no . . . H(17B) C(17) H(17C) 109.462 no . . . C(18) C(19) H(19A) 109.472 no . . . C(18) C(19) H(19B) 109.472 no . . . C(18) C(19) H(19C) 109.471 no . . . H(19A) C(19) H(19B) 109.466 no . . . H(19A) C(19) H(19C) 109.473 no . . . H(19B) C(19) H(19C) 109.473 no . . . C(18) C(20) H(20A) 109.472 no . . . C(18) C(20) H(20B) 109.473 no . . . C(18) C(20) H(20C) 109.464 no . . . H(20A) C(20) H(20B) 109.472 no . . . H(20A) C(20) H(20C) 109.476 no . . . H(20B) C(20) H(20C) 109.470 no . . . C(18) C(21) H(21A) 109.466 no . . . C(18) C(21) H(21B) 109.471 no . . . C(18) C(21) H(21C) 109.471 no . . . H(21A) C(21) H(21B) 109.474 no . . . H(21A) C(21) H(21C) 109.470 no . . . H(21B) C(21) H(21C) 109.476 no . . . C(22) C(23) H(23A) 109.472 no . . . C(22) C(23) H(23B) 109.471 no . . . C(22) C(23) H(23C) 109.469 no . . . H(23A) C(23) H(23B) 109.475 no . . . H(23A) C(23) H(23C) 109.474 no . . . H(23B) C(23) H(23C) 109.466 no . . . C(22) C(24) H(24A) 109.467 no . . . C(22) C(24) H(24B) 109.465 no . . . C(22) C(24) H(24C) 109.473 no . . . H(24A) C(24) H(24B) 109.475 no . . . H(24A) C(24) H(24C) 109.470 no . . . H(24B) C(24) H(24C) 109.478 no . . . C(22) C(25) H(25A) 109.468 no . . . C(22) C(25) H(25B) 109.475 no . . . C(22) C(25) H(25C) 109.475 no . . . H(25A) C(25) H(25B) 109.472 no . . . H(25A) C(25) H(25C) 109.473 no . . . H(25B) C(25) H(25C) 109.465 no . . . C(26) C(27) H(27A) 109.467 no . . . C(26) C(27) H(27B) 109.470 no . . . C(26) C(27) H(27C) 109.463 no . . . H(27A) C(27) H(27B) 109.472 no . . . H(27A) C(27) H(27C) 109.481 no . . . H(27B) C(27) H(27C) 109.474 no . . . C(26) C(28) H(28A) 109.469 no . . . C(26) C(28) H(28B) 109.468 no . . . C(26) C(28) H(28C) 109.468 no . . . H(28A) C(28) H(28B) 109.469 no . . . H(28A) C(28) H(28C) 109.480 no . . . H(28B) C(28) H(28C) 109.473 no . . . C(26) C(29) H(29A) 109.472 no . . . C(26) C(29) H(29B) 109.470 no . . . C(26) C(29) H(29C) 109.472 no . . . H(29A) C(29) H(29B) 109.480 no . . . H(29A) C(29) H(29C) 109.465 no . . . H(29B) C(29) H(29C) 109.469 no . . . C(32) C(30) H(30A) 109.467 no . . . C(32) C(30) H(30B) 109.471 no . . . C(32) C(30) H(30C) 109.468 no . . . H(30A) C(30) H(30B) 109.477 no . . . H(30A) C(30) H(30C) 109.477 no . . . H(30B) C(30) H(30C) 109.467 no . . . C(32) C(31) H(31A) 109.474 no . . . C(32) C(31) H(31B) 109.468 no . . . C(32) C(31) H(31C) 109.470 no . . . H(31A) C(31) H(31B) 109.480 no . . . H(31A) C(31) H(31C) 109.470 no . . . H(31B) C(31) H(31C) 109.465 no . . . C(32) C(33) H(33A) 109.471 no . . . C(32) C(33) H(33B) 109.475 no . . . C(32) C(33) H(33C) 109.473 no . . . H(33A) C(33) H(33B) 109.469 no . . . H(33A) C(33) H(33C) 109.471 no . . . H(33B) C(33) H(33C) 109.469 no . . . C(34) C(35) H(35) 117.671 no . . . C(36) C(35) H(35) 117.678 no . . . C(36) C(37) H(37) 118.958 no . . . C(38) C(37) H(37) 118.959 no . . . C(40) C(41) H(41A) 109.469 no . . . C(40) C(41) H(41B) 109.467 no . . . C(40) C(41) H(41C) 109.468 no . . . H(41A) C(41) H(41B) 109.472 no . . . H(41A) C(41) H(41C) 109.474 no . . . H(41B) C(41) H(41C) 109.476 no . . . C(40) C(42) H(42A) 109.471 no . . . C(40) C(42) H(42B) 109.469 no . . . C(40) C(42) H(42C) 109.474 no . . . H(42A) C(42) H(42B) 109.475 no . . . H(42A) C(42) H(42C) 109.464 no . . . H(42B) C(42) H(42C) 109.474 no . . . C(40) C(43) H(43A) 109.466 no . . . C(40) C(43) H(43B) 109.466 no . . . C(40) C(43) H(43C) 109.472 no . . . H(43A) C(43) H(43B) 109.474 no . . . H(43A) C(43) H(43C) 109.472 no . . . H(43B) C(43) H(43C) 109.478 no . . . C(44) C(45) H(45A) 109.465 no . . . C(44) C(45) H(45B) 109.468 no . . . C(44) C(45) H(45C) 109.473 no . . . H(45A) C(45) H(45B) 109.480 no . . . H(45A) C(45) H(45C) 109.478 no . . . H(45B) C(45) H(45C) 109.463 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Nb(1) O(1) C(3) 162.8(4) no . . . . Cl(2) Nb(1) O(1) C(3) 74.5(4) no . . . . Cl(3) Nb(1) O(1) C(3) -109.5(4) no . . . . O(3) Nb(1) O(1) C(3) -17.9(4) no . . . . Nb(1) O(1) C(3) C(2) 45.9(6) no . . . . Nb(1) O(1) C(3) C(4) -132.5(5) no . . . . C(2) C(1) C(8) C(9) -161.9(4) no . . . . C(2) C(1) C(8) C(13) 11.3(7) no . . . . C(8) C(1) C(2) C(3) 119.9(4) no . . . . C(8) C(1) C(2) C(7) -59.4(6) no . . . . C(2) C(1) C(38) C(37) -86.1(5) no . . . . C(2) C(1) C(38) C(39) 91.2(5) no . . . . C(38) C(1) C(2) C(3) -110.9(4) no . . . . C(38) C(1) C(2) C(7) 69.8(5) no . . . . C(8) C(1) C(38) C(37) 44.3(5) no . . . . C(8) C(1) C(38) C(39) -138.4(4) no . . . . C(38) C(1) C(8) C(9) 70.2(5) no . . . . C(38) C(1) C(8) C(13) -116.7(5) no . . . . C(1) C(2) C(3) O(1) 14.0(5) no . . . . C(1) C(2) C(3) C(4) -167.5(3) no . . . . C(1) C(2) C(7) C(6) 172.8(3) no . . . . C(3) C(2) C(7) C(6) -6.5(6) no . . . . C(7) C(2) C(3) O(1) -166.6(3) no . . . . C(7) C(2) C(3) C(4) 11.8(5) no . . . . O(1) C(3) C(4) C(5) 169.4(3) no . . . . O(1) C(3) C(4) C(14) -12.7(5) no . . . . C(2) C(3) C(4) C(5) -9.0(5) no . . . . C(2) C(3) C(4) C(14) 168.9(3) no . . . . C(3) C(4) C(5) C(6) 0.9(6) no . . . . C(3) C(4) C(14) C(15) 69.2(5) no . . . . C(3) C(4) C(14) C(16) -171.9(3) no . . . . C(3) C(4) C(14) C(17) -52.2(5) no . . . . C(5) C(4) C(14) C(15) -113.0(4) no . . . . C(5) C(4) C(14) C(16) 6.0(5) no . . . . C(5) C(4) C(14) C(17) 125.7(4) no . . . . C(14) C(4) C(5) C(6) -177.1(3) no . . . . C(4) C(5) C(6) C(7) 4.0(6) no . . . . C(4) C(5) C(6) C(18) -177.1(4) no . . . . C(5) C(6) C(7) C(2) -1.0(6) no . . . . C(5) C(6) C(18) C(19) 63.9(6) no . . . . C(5) C(6) C(18) C(20) -55.2(5) no . . . . C(5) C(6) C(18) C(21) -175.0(3) no . . . . C(7) C(6) C(18) C(19) -117.2(5) no . . . . C(7) C(6) C(18) C(20) 123.7(5) no . . . . C(7) C(6) C(18) C(21) 3.9(6) no . . . . C(18) C(6) C(7) C(2) -180.0(4) no . . . . C(1) C(8) C(9) O(2) -7.3(8) no . . . . C(1) C(8) C(9) C(10) 171.5(5) no . . . . C(1) C(8) C(13) C(12) -174.5(5) no . . . . C(9) C(8) C(13) C(12) -1.5(8) no . . . . C(13) C(8) C(9) O(2) 179.3(5) no . . . . C(13) C(8) C(9) C(10) -1.9(8) no . . . . O(2) C(9) C(10) C(11) -177.1(5) no . . . . O(2) C(9) C(10) C(22) 5.1(8) no . . . . C(8) C(9) C(10) C(11) 4.1(8) no . . . . C(8) C(9) C(10) C(22) -173.7(5) no . . . . C(9) C(10) C(11) C(12) -3.2(9) no . . . . C(9) C(10) C(22) C(23) -179.2(5) no . . . . C(9) C(10) C(22) C(24) -59.1(7) no . . . . C(9) C(10) C(22) C(25) 61.1(7) no . . . . C(11) C(10) C(22) C(23) 3.1(8) no . . . . C(11) C(10) C(22) C(24) 123.2(6) no . . . . C(11) C(10) C(22) C(25) -116.5(6) no . . . . C(22) C(10) C(11) C(12) 174.6(5) no . . . . C(10) C(11) C(12) C(13) 0.1(9) no . . . . C(10) C(11) C(12) C(26) -175.5(5) no . . . . C(11) C(12) C(13) C(8) 2.4(8) no . . . . C(11) C(12) C(26) C(27) 69.0(7) no . . . . C(11) C(12) C(26) C(28) -50.0(7) no . . . . C(11) C(12) C(26) C(29) -171.9(5) no . . . . C(13) C(12) C(26) C(27) -106.3(5) no . . . . C(13) C(12) C(26) C(28) 134.7(5) no . . . . C(13) C(12) C(26) C(29) 12.7(8) no . . . . C(26) C(12) C(13) C(8) 177.9(5) no . . . . C(30) C(32) C(34) C(35) 118.8(5) no . . . . C(30) C(32) C(34) C(39) -63.6(5) no . . . . C(31) C(32) C(34) C(35) -2.2(5) no . . . . C(31) C(32) C(34) C(39) 175.4(4) no . . . . C(33) C(32) C(34) C(35) -120.3(5) no . . . . C(33) C(32) C(34) C(39) 57.3(6) no . . . . C(32) C(34) C(35) C(36) 175.5(4) no . . . . C(32) C(34) C(39) O(3) 10.1(6) no . . . . C(32) C(34) C(39) C(38) -170.8(4) no . . . . C(35) C(34) C(39) O(3) -172.2(4) no . . . . C(35) C(34) C(39) C(38) 7.0(6) no . . . . C(39) C(34) C(35) C(36) -2.4(6) no . . . . C(34) C(35) C(36) C(37) -4.0(6) no . . . . C(34) C(35) C(36) C(40) 175.6(4) no . . . . C(35) C(36) C(37) C(38) 6.0(6) no . . . . C(35) C(36) C(40) C(41) -0.5(6) no . . . . C(35) C(36) C(40) C(42) 119.7(4) no . . . . C(35) C(36) C(40) C(43) -121.2(5) no . . . . C(37) C(36) C(40) C(41) 179.1(4) no . . . . C(37) C(36) C(40) C(42) -60.7(6) no . . . . C(37) C(36) C(40) C(43) 58.4(5) no . . . . C(40) C(36) C(37) C(38) -173.6(4) no . . . . C(36) C(37) C(38) C(1) 175.7(4) no . . . . C(36) C(37) C(38) C(39) -1.7(6) no . . . . C(1) C(38) C(39) O(3) -3.4(6) no . . . . C(1) C(38) C(39) C(34) 177.4(3) no . . . . C(37) C(38) C(39) O(3) 174.0(4) no . . . . C(37) C(38) C(39) C(34) -5.2(6) no . . . . #===END #============================================================================== data__O3NbCl3-syn-Complex-3-syn _database_code_depnum_ccdc_archive 'CCDC 789693' #TrackingRef '- Kawaguchi_CIF_rivised.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C59.50 H87.50 Cl3 N Nb O3' _chemical_formula_moiety 'C59.50 H87.50 Cl3 N Nb O3' _chemical_formula_weight 1064.12 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 13.987(6) _cell_length_b 20.447(8) _cell_length_c 21.538(9) _cell_angle_alpha 94.951(6) _cell_angle_beta 99.947(5) _cell_angle_gamma 97.388(7) _cell_volume 5980(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14703 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 173 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2270.00 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.928 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 173 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 45362 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_max 0.941 _diffrn_measured_fraction_theta_full 0.941 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 24591 _reflns_number_gt 18783 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1520 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 24585 _refine_ls_number_parameters 1201 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0518P)^2^+11.7241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.740 _refine_diff_density_min -0.420 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Nb(1) Nb 0.17791(2) 0.203036(15) 0.267278(16) 0.01916(8) Uani 1.0 2 d . . . Nb(2) Nb 0.37431(2) 0.793246(16) 0.110382(15) 0.01938(8) Uani 1.0 2 d . . . Cl(1) Cl 0.29186(7) 0.12718(5) 0.24577(5) 0.0293(2) Uani 1.0 2 d . . . Cl(2) Cl 0.05017(7) 0.10848(5) 0.22525(6) 0.0329(3) Uani 1.0 2 d . . . Cl(3) Cl 0.19177(9) 0.16289(5) 0.37053(5) 0.0373(3) Uani 1.0 2 d . . . Cl(4) Cl 0.47560(8) 0.81611(5) 0.03291(5) 0.0317(3) Uani 1.0 2 d . . . Cl(5) Cl 0.31059(7) 0.68701(5) 0.04685(5) 0.0280(2) Uani 1.0 2 d . . . Cl(6) Cl 0.24103(7) 0.83713(5) 0.04281(5) 0.0299(2) Uani 1.0 2 d . . . O(1) O 0.07526(19) 0.24951(12) 0.29198(12) 0.0215(6) Uani 1.0 2 d . . . O(2) O 0.28528(18) 0.27273(12) 0.29922(12) 0.0219(6) Uani 1.0 2 d . . . O(3) O 0.16237(18) 0.22603(11) 0.18098(12) 0.0205(6) Uani 1.0 2 d . . . O(4) O 0.28042(18) 0.77045(12) 0.16490(12) 0.0224(6) Uani 1.0 2 d . . . O(5) O 0.41894(19) 0.88217(12) 0.15128(12) 0.0231(6) Uani 1.0 2 d . . . O(6) O 0.47436(18) 0.75222(12) 0.15770(12) 0.0219(6) Uani 1.0 2 d . . . N(1) N -0.2112(3) 0.25487(17) 0.09452(17) 0.0318(8) Uani 1.0 2 d . . . N(2) N 0.1586(3) 0.97247(18) 0.2511(3) 0.0460(11) Uani 1.0 2 d . . . C(1) C 0.1636(3) 0.35016(17) 0.23833(17) 0.0182(7) Uani 1.0 2 d . . . C(2) C 0.0679(3) 0.35840(17) 0.25917(17) 0.0180(7) Uani 1.0 2 d . . . C(3) C 0.0281(3) 0.30412(17) 0.28828(17) 0.0184(7) Uani 1.0 2 d . . . C(4) C -0.0574(3) 0.30737(18) 0.31411(17) 0.0204(8) Uani 1.0 2 d . . . C(5) C -0.1031(3) 0.36365(18) 0.30603(19) 0.0243(8) Uani 1.0 2 d . . . C(6) C -0.0671(3) 0.41692(18) 0.27574(18) 0.0233(8) Uani 1.0 2 d . . . C(7) C 0.0194(3) 0.41248(18) 0.25301(18) 0.0226(8) Uani 1.0 2 d . . . C(8) C 0.2579(3) 0.38311(17) 0.28013(17) 0.0196(8) Uani 1.0 2 d . . . C(9) C 0.3191(3) 0.33998(17) 0.30824(17) 0.0178(7) Uani 1.0 2 d . . . C(10) C 0.4128(3) 0.36467(18) 0.34387(18) 0.0223(8) Uani 1.0 2 d . . . C(11) C 0.4385(3) 0.43357(19) 0.35236(19) 0.0253(9) Uani 1.0 2 d . . . C(12) C 0.3786(3) 0.47777(18) 0.32682(19) 0.0238(8) Uani 1.0 2 d . . . C(13) C 0.2879(3) 0.45110(18) 0.29010(18) 0.0213(8) Uani 1.0 2 d . . . C(14) C 0.1655(3) 0.34161(17) 0.16824(17) 0.0168(7) Uani 1.0 2 d . . . C(15) C 0.1645(3) 0.27565(17) 0.14162(18) 0.0195(8) Uani 1.0 2 d . . . C(16) C 0.1660(3) 0.26227(18) 0.07649(18) 0.0218(8) Uani 1.0 2 d . . . C(17) C 0.1749(3) 0.31716(19) 0.04229(18) 0.0237(8) Uani 1.0 2 d . . . C(18) C 0.1809(3) 0.38257(18) 0.06826(18) 0.0212(8) Uani 1.0 2 d . . . C(19) C 0.1746(3) 0.39368(17) 0.13150(18) 0.0194(8) Uani 1.0 2 d . . . C(20) C -0.0951(3) 0.2532(2) 0.3536(2) 0.0275(9) Uani 1.0 2 d . . . C(21) C -0.1887(4) 0.2683(3) 0.3771(3) 0.0360(11) Uani 1.0 2 d . . . C(22) C -0.1204(4) 0.1850(2) 0.3145(3) 0.0378(11) Uani 1.0 2 d . . . C(23) C -0.0159(4) 0.2504(3) 0.4116(2) 0.0397(11) Uani 1.0 2 d . . . C(24) C -0.1172(3) 0.4790(2) 0.2694(3) 0.0318(10) Uani 1.0 2 d . . . C(25) C -0.2184(4) 0.4704(3) 0.2889(3) 0.0561(16) Uani 1.0 2 d . . . C(26) C -0.0520(4) 0.5368(3) 0.3127(3) 0.0477(13) Uani 1.0 2 d . . . C(27) C -0.1310(4) 0.4955(3) 0.2008(3) 0.0468(13) Uani 1.0 2 d . . . C(28) C 0.4833(3) 0.3182(2) 0.3708(2) 0.0304(9) Uani 1.0 2 d . . . C(29) C 0.5039(4) 0.2714(3) 0.3165(3) 0.0416(12) Uani 1.0 2 d . . . C(30) C 0.4401(4) 0.2783(3) 0.4193(3) 0.0425(12) Uani 1.0 2 d . . . C(31) C 0.5823(4) 0.3568(3) 0.4055(3) 0.0440(12) Uani 1.0 2 d . . . C(32) C 0.4145(4) 0.5530(2) 0.3383(3) 0.0340(10) Uani 1.0 2 d . . . C(33) C 0.4325(5) 0.5755(3) 0.4093(3) 0.0574(15) Uani 1.0 2 d . . . C(34) C 0.5117(5) 0.5675(3) 0.3143(4) 0.0656(18) Uani 1.0 2 d . . . C(35) C 0.3416(5) 0.5928(3) 0.3043(4) 0.069(2) Uani 1.0 2 d . . . C(36) C 0.1578(3) 0.19063(19) 0.04448(19) 0.0285(9) Uani 1.0 2 d . . . C(37) C 0.2431(4) 0.1570(3) 0.0744(3) 0.0407(11) Uani 1.0 2 d . . . C(38) C 0.1603(5) 0.1887(3) -0.0263(2) 0.0445(13) Uani 1.0 2 d . . . C(39) C 0.0598(4) 0.1511(3) 0.0518(3) 0.0435(12) Uani 1.0 2 d . . . C(40) C 0.1967(4) 0.4417(2) 0.0293(2) 0.0302(9) Uani 1.0 2 d . . . C(41) C 0.3081(6) 0.4535(4) 0.0249(4) 0.0422(19) Uiso 0.6000 2 d . . . C(42) C 0.1368(6) 0.4226(4) -0.0403(4) 0.0384(18) Uiso 0.6000 2 d . . . C(43) C 0.1683(7) 0.5049(4) 0.0591(4) 0.0404(18) Uiso 0.6000 2 d . . . C(44) C 0.4325(3) 0.82285(17) 0.25998(18) 0.0208(8) Uani 1.0 2 d . . . C(45) C 0.3364(3) 0.79417(17) 0.27688(18) 0.0201(8) Uani 1.0 2 d . . . C(46) C 0.2617(3) 0.76725(17) 0.22483(17) 0.0194(8) Uani 1.0 2 d . . . C(47) C 0.1700(3) 0.73685(18) 0.23492(19) 0.0230(8) Uani 1.0 2 d . . . C(48) C 0.1581(3) 0.73587(19) 0.2977(2) 0.0265(9) Uani 1.0 2 d . . . C(49) C 0.2301(3) 0.76131(18) 0.35005(19) 0.0265(9) Uani 1.0 2 d . . . C(50) C 0.3199(3) 0.79049(18) 0.33846(18) 0.0248(8) Uani 1.0 2 d . . . C(51) C 0.4514(3) 0.92446(18) 0.20616(18) 0.0219(8) Uani 1.0 2 d . . . C(52) C 0.4595(3) 0.89718(18) 0.26481(18) 0.0209(8) Uani 1.0 2 d . . . C(53) C 0.4936(3) 0.93822(19) 0.32079(19) 0.0263(9) Uani 1.0 2 d . . . C(54) C 0.5208(3) 1.0061(2) 0.3213(2) 0.0290(9) Uani 1.0 2 d . . . C(55) C 0.5100(3) 1.03122(19) 0.2633(2) 0.0291(9) Uani 1.0 2 d . . . C(56) C 0.4778(3) 0.99333(18) 0.20454(19) 0.0240(8) Uani 1.0 2 d . . . C(57) C 0.5165(3) 0.78301(18) 0.27021(18) 0.0215(8) Uani 1.0 2 d . . . C(58) C 0.5318(3) 0.74657(18) 0.21501(18) 0.0213(8) Uani 1.0 2 d . . . C(59) C 0.6067(3) 0.70683(19) 0.21817(19) 0.0249(9) Uani 1.0 2 d . . . C(60) C 0.6686(3) 0.7092(2) 0.2766(2) 0.0318(10) Uani 1.0 2 d . . . C(61) C 0.6586(3) 0.7469(2) 0.3311(3) 0.0332(10) Uani 1.0 2 d . . . C(62) C 0.5800(3) 0.7824(2) 0.32717(19) 0.0274(9) Uani 1.0 2 d . . . C(63) C 0.0889(3) 0.7015(2) 0.1801(2) 0.0297(9) Uani 1.0 2 d . . . C(64) C 0.1259(4) 0.6387(3) 0.1542(3) 0.0445(12) Uani 1.0 2 d . . . C(65) C -0.0068(4) 0.6804(3) 0.2027(3) 0.0447(12) Uani 1.0 2 d . . . C(66) C 0.0659(4) 0.7453(3) 0.1272(3) 0.0423(12) Uani 1.0 2 d . . . C(67) C 0.2114(4) 0.7566(2) 0.4185(2) 0.0328(10) Uani 1.0 2 d . . . C(68) C 0.1196(10) 0.7039(7) 0.4214(7) 0.065(4) Uiso 0.5000 2 d . . . C(69) C 0.1904(9) 0.8267(6) 0.4453(6) 0.050(3) Uiso 0.5000 2 d . . . C(70) C 0.2988(10) 0.7371(7) 0.4600(7) 0.064(4) Uiso 0.5000 2 d . . . C(71) C 0.4752(3) 1.02451(19) 0.1420(2) 0.0291(9) Uani 1.0 2 d . . . C(72) C 0.5063(4) 1.1008(2) 0.1533(3) 0.0425(12) Uani 1.0 2 d . . . C(73) C 0.5486(4) 0.9960(3) 0.1051(3) 0.0403(11) Uani 1.0 2 d . . . C(74) C 0.3721(4) 1.0116(3) 0.1014(3) 0.0377(11) Uani 1.0 2 d . . . C(75) C 0.5617(4) 1.0517(2) 0.3840(2) 0.0370(11) Uani 1.0 2 d . . . C(76) C 0.6292(11) 1.1140(7) 0.3714(7) 0.065(4) Uiso 0.5000 2 d . . . C(77) C 0.4698(11) 1.0771(8) 0.4092(8) 0.070(4) Uiso 0.5000 2 d . . . C(78) C 0.6216(9) 1.0147(6) 0.4325(6) 0.048(3) Uiso 0.5000 2 d . . . C(79) C 0.6221(3) 0.6637(2) 0.1591(2) 0.0308(9) Uani 1.0 2 d . . . C(80) C 0.6559(4) 0.7092(3) 0.1114(3) 0.0435(12) Uani 1.0 2 d . . . C(81) C 0.5264(4) 0.6179(2) 0.1281(3) 0.0388(11) Uani 1.0 2 d . . . C(82) C 0.7003(4) 0.6184(3) 0.1761(3) 0.0440(12) Uani 1.0 2 d . . . C(83) C 0.7336(4) 0.7504(3) 0.3936(3) 0.0507(14) Uani 1.0 2 d . . . C(84) C 0.8052(15) 0.8152(10) 0.4037(10) 0.114(7) Uiso 0.5000 2 d . . . C(85) C 0.6781(12) 0.7413(8) 0.4497(8) 0.084(5) Uiso 0.5000 2 d . . . C(86) C 0.7957(12) 0.6902(8) 0.3927(8) 0.079(4) Uiso 0.5000 2 d . . . C(87) C 0.8380(9) 0.7799(6) 0.3796(6) 0.057(3) Uiso 0.5000 2 d . . . C(88) C 0.7101(9) 0.7970(6) 0.4481(6) 0.059(3) Uiso 0.5000 2 d . . . C(89) C 0.7357(11) 0.6800(7) 0.4157(7) 0.075(4) Uiso 0.5000 2 d . . . C(90) C -0.3135(3) 0.2477(3) 0.1097(2) 0.0370(11) Uani 1.0 2 d . . . C(91) C -0.3174(4) 0.2709(3) 0.1777(3) 0.0546(14) Uani 1.0 2 d . . . C(92) C -0.1658(4) 0.3269(3) 0.1010(3) 0.0425(12) Uani 1.0 2 d . . . C(93) C -0.0836(4) 0.3371(3) 0.0644(3) 0.0595(16) Uani 1.0 2 d . . . C(94) C -0.1435(4) 0.2146(3) 0.1317(3) 0.0444(12) Uani 1.0 2 d . . . C(95) C -0.1837(5) 0.1417(3) 0.1247(3) 0.0590(15) Uani 1.0 2 d . . . C(96) C 0.0563(4) 0.9553(3) 0.2638(4) 0.0534(15) Uani 1.0 2 d . . . C(97) C 0.0283(5) 0.8825(3) 0.2710(4) 0.074(2) Uani 1.0 2 d . . . C(98) C 0.1733(5) 0.9418(3) 0.1881(4) 0.0613(17) Uani 1.0 2 d . . . C(99) C 0.1073(6) 0.9594(4) 0.1328(4) 0.078(2) Uani 1.0 2 d . . . C(100) C 0.2374(5) 0.9576(3) 0.3022(4) 0.0610(17) Uani 1.0 2 d . . . C(101) C 0.2285(6) 0.9856(3) 0.3679(4) 0.085(3) Uani 1.0 2 d . . . C(102) C -0.1752(5) 1.0041(3) 0.2300(5) 0.069(2) Uani 1.0 2 d . . . C(103) C -0.2131(6) 0.9820(4) 0.2769(5) 0.090(3) Uani 1.0 2 d . . . C(104) C -0.2662(7) 0.9233(5) 0.2716(5) 0.106(4) Uani 1.0 2 d . . . C(105) C -0.2815(6) 0.8847(4) 0.2186(6) 0.115(4) Uani 1.0 2 d . . . C(106) C -0.2475(6) 0.9045(5) 0.1664(5) 0.107(4) Uani 1.0 2 d . . . C(107) C -0.1892(6) 0.9685(4) 0.1737(5) 0.084(3) Uani 1.0 2 d . . . C(108) C -0.4605(5) 0.4343(3) 0.1597(4) 0.0610(16) Uani 1.0 2 d . . . C(109) C -0.5299(4) 0.3902(3) 0.1778(3) 0.0514(14) Uani 1.0 2 d . . . C(110) C -0.5718(4) 0.3349(3) 0.1391(3) 0.0565(15) Uani 1.0 2 d . . . C(111) C -0.5465(5) 0.3226(4) 0.0817(3) 0.0637(17) Uani 1.0 2 d . . . C(112) C -0.4776(5) 0.3656(4) 0.0621(3) 0.071(2) Uani 1.0 2 d . . . C(113) C -0.4338(5) 0.4219(4) 0.1010(4) 0.070(2) Uani 1.0 2 d . . . C(114) C 0.1220(7) 0.5025(5) 0.4698(5) 0.122(4) Uani 1.0 2 d . . . C(115) C 0.2018(7) 0.5229(4) 0.5172(4) 0.092(3) Uani 1.0 2 d . . . C(116) C 0.2729(7) 0.4858(4) 0.5228(5) 0.110(4) Uani 1.0 2 d . . . C(117) C 0.2716(7) 0.4312(5) 0.4846(5) 0.096(3) Uani 1.0 2 d . . . C(118) C 0.1993(9) 0.4136(5) 0.4376(4) 0.104(3) Uani 1.0 2 d . . . C(119) C 0.1231(8) 0.4452(5) 0.4288(5) 0.121(4) Uani 1.0 2 d . . . C(120) C 0.1023(15) 1.0105(11) 0.5047(11) 0.103(6) Uiso 0.5000 2 d . . . C(121) C 0.0305(18) 1.0590(10) 0.4757(11) 0.089(6) Uiso 0.5000 2 d . . . C(122) C -0.0657(13) 1.0374(8) 0.4649(8) 0.082(5) Uiso 0.5000 2 d . . . C(123) C 0.1128(11) 0.4858(7) 0.0357(7) 0.050(4) Uiso 0.4000 2 d . . . C(124) C 0.2936(12) 0.4918(8) 0.0685(8) 0.065(4) Uiso 0.4000 2 d . . . C(125) C 0.2077(13) 0.4244(8) -0.0372(8) 0.066(4) Uiso 0.4000 2 d . . . C(126) C 0.1424(9) 0.8042(6) 0.4335(6) 0.050(3) Uiso 0.5000 2 d . . . C(127) C 0.1727(8) 0.6834(5) 0.4258(5) 0.044(3) Uiso 0.5000 2 d . . . C(128) C 0.3130(8) 0.7737(6) 0.4682(5) 0.040(3) Uiso 0.5000 2 d . . . C(129) C 0.6626(8) 1.0933(6) 0.3768(6) 0.042(3) Uiso 0.5000 2 d . . . C(130) C 0.5790(9) 1.0118(6) 0.4422(6) 0.045(3) Uiso 0.5000 2 d . . . C(131) C 0.4891(8) 1.0990(6) 0.3944(6) 0.041(3) Uiso 0.5000 2 d . . . C(132) C -0.0108(16) 1.0351(10) 0.4452(10) 0.095(6) Uiso 0.5000 2 d . . . C(133) C 0.0754(17) 1.0440(12) 0.4857(11) 0.095(6) Uiso 0.5000 2 d . . . C(134) C 0.076(3) 1.0217(16) 0.5482(16) 0.173(11) Uiso 0.5000 2 d . . . H(1A) H -0.2179 0.2388 0.0520 0.0381 Uiso 1.0 2 calc R . . H(1) H 0.1673 0.3033 0.2475 0.0219 Uiso 1.0 2 calc R . . H(2A) H 0.1688 1.0182 0.2500 0.0552 Uiso 1.0 2 calc R . . H(5) H -0.1620 0.3659 0.3220 0.0292 Uiso 1.0 2 calc R . . H(7) H 0.0458 0.4481 0.2325 0.0272 Uiso 1.0 2 calc R . . H(10A) H 0.3021 0.9760 0.2934 0.0732 Uiso 1.0 2 calc R . . H(10B) H 0.2348 0.9088 0.3010 0.0732 Uiso 1.0 2 calc R . . H(10C) H 0.1652 0.9667 0.3773 0.1015 Uiso 1.0 2 calc R . . H(10D) H 0.2325 1.0340 0.3698 0.1015 Uiso 1.0 2 calc R . . H(10E) H 0.2818 0.9743 0.3991 0.1015 Uiso 1.0 2 calc R . . H(11) H 0.5009 0.4515 0.3771 0.0303 Uiso 1.0 2 calc R . . H(13) H 0.2459 0.4799 0.2715 0.0255 Uiso 1.0 2 calc R . . H(17) H 0.1771 0.3093 -0.0015 0.0285 Uiso 1.0 2 calc R . . H(19) H 0.1765 0.4378 0.1501 0.0233 Uiso 1.0 2 calc R . . H(21A) H -0.1749 0.3111 0.4035 0.0432 Uiso 1.0 2 calc R . . H(21B) H -0.2102 0.2333 0.4021 0.0432 Uiso 1.0 2 calc R . . H(21C) H -0.2405 0.2701 0.3405 0.0432 Uiso 1.0 2 calc R . . H(22A) H -0.0614 0.1723 0.3010 0.0453 Uiso 1.0 2 calc R . . H(22B) H -0.1705 0.1870 0.2770 0.0453 Uiso 1.0 2 calc R . . H(22C) H -0.1456 0.1521 0.3404 0.0453 Uiso 1.0 2 calc R . . H(23A) H -0.0023 0.2933 0.4378 0.0476 Uiso 1.0 2 calc R . . H(23B) H 0.0442 0.2403 0.3976 0.0476 Uiso 1.0 2 calc R . . H(23C) H -0.0389 0.2157 0.4365 0.0476 Uiso 1.0 2 calc R . . H(25A) H -0.2110 0.4610 0.3332 0.0673 Uiso 1.0 2 calc R . . H(25B) H -0.2612 0.4334 0.2616 0.0673 Uiso 1.0 2 calc R . . H(25C) H -0.2475 0.5112 0.2843 0.0673 Uiso 1.0 2 calc R . . H(26A) H -0.0814 0.5775 0.3076 0.0572 Uiso 1.0 2 calc R . . H(26B) H 0.0132 0.5426 0.3013 0.0572 Uiso 1.0 2 calc R . . H(26C) H -0.0462 0.5273 0.3569 0.0572 Uiso 1.0 2 calc R . . H(27A) H -0.1613 0.5360 0.1976 0.0561 Uiso 1.0 2 calc R . . H(27B) H -0.1736 0.4586 0.1732 0.0561 Uiso 1.0 2 calc R . . H(27C) H -0.0671 0.5023 0.1877 0.0561 Uiso 1.0 2 calc R . . H(29A) H 0.4429 0.2429 0.2959 0.0499 Uiso 1.0 2 calc R . . H(29B) H 0.5522 0.2438 0.3335 0.0499 Uiso 1.0 2 calc R . . H(29C) H 0.5295 0.2976 0.2854 0.0499 Uiso 1.0 2 calc R . . H(30A) H 0.3753 0.2543 0.3994 0.0510 Uiso 1.0 2 calc R . . H(30B) H 0.4338 0.3086 0.4557 0.0510 Uiso 1.0 2 calc R . . H(30C) H 0.4836 0.2465 0.4336 0.0510 Uiso 1.0 2 calc R . . H(31A) H 0.5718 0.3867 0.4411 0.0528 Uiso 1.0 2 calc R . . H(31B) H 0.6127 0.3829 0.3761 0.0528 Uiso 1.0 2 calc R . . H(31C) H 0.6256 0.3256 0.4216 0.0528 Uiso 1.0 2 calc R . . H(33A) H 0.3707 0.5676 0.4249 0.0689 Uiso 1.0 2 calc R . . H(33B) H 0.4582 0.6230 0.4169 0.0689 Uiso 1.0 2 calc R . . H(33C) H 0.4802 0.5505 0.4318 0.0689 Uiso 1.0 2 calc R . . H(34A) H 0.5361 0.6151 0.3228 0.0787 Uiso 1.0 2 calc R . . H(34B) H 0.5007 0.5540 0.2686 0.0787 Uiso 1.0 2 calc R . . H(34C) H 0.5602 0.5427 0.3363 0.0787 Uiso 1.0 2 calc R . . H(35A) H 0.3682 0.6401 0.3124 0.0831 Uiso 1.0 2 calc R . . H(35B) H 0.2798 0.5852 0.3199 0.0831 Uiso 1.0 2 calc R . . H(35C) H 0.3298 0.5789 0.2586 0.0831 Uiso 1.0 2 calc R . . H(37A) H 0.3051 0.1814 0.0680 0.0489 Uiso 1.0 2 calc R . . H(37B) H 0.2354 0.1112 0.0544 0.0489 Uiso 1.0 2 calc R . . H(37C) H 0.2435 0.1567 0.1199 0.0489 Uiso 1.0 2 calc R . . H(38A) H 0.1536 0.1425 -0.0449 0.0533 Uiso 1.0 2 calc R . . H(38B) H 0.2227 0.2128 -0.0321 0.0533 Uiso 1.0 2 calc R . . H(38C) H 0.1060 0.2095 -0.0474 0.0533 Uiso 1.0 2 calc R . . H(39A) H 0.0053 0.1707 0.0293 0.0522 Uiso 1.0 2 calc R . . H(39B) H 0.0559 0.1526 0.0969 0.0522 Uiso 1.0 2 calc R . . H(39C) H 0.0558 0.1049 0.0339 0.0522 Uiso 1.0 2 calc R . . H(44) H 0.4139 0.8136 0.2128 0.0249 Uiso 1.0 2 calc R . . H(48) H 0.0963 0.7164 0.3053 0.0318 Uiso 1.0 2 calc R . . H(50) H 0.3709 0.8082 0.3732 0.0297 Uiso 1.0 2 calc R . . H(53) H 0.4986 0.9196 0.3599 0.0315 Uiso 1.0 2 calc R . . H(55) H 0.5258 1.0779 0.2635 0.0349 Uiso 1.0 2 calc R . . H(60) H 0.7207 0.6834 0.2793 0.0382 Uiso 1.0 2 calc R . . H(62) H 0.5694 0.8068 0.3643 0.0329 Uiso 1.0 2 calc R . . H(64A) H 0.1859 0.6515 0.1377 0.0534 Uiso 1.0 2 calc R . . H(64B) H 0.0755 0.6140 0.1200 0.0534 Uiso 1.0 2 calc R . . H(64C) H 0.1400 0.6107 0.1883 0.0534 Uiso 1.0 2 calc R . . H(65A) H -0.0551 0.6559 0.1673 0.0536 Uiso 1.0 2 calc R . . H(65B) H -0.0319 0.7199 0.2187 0.0536 Uiso 1.0 2 calc R . . H(65C) H 0.0053 0.6520 0.2367 0.0536 Uiso 1.0 2 calc R . . H(66A) H 0.0401 0.7842 0.1437 0.0508 Uiso 1.0 2 calc R . . H(66B) H 0.0168 0.7200 0.0925 0.0508 Uiso 1.0 2 calc R . . H(66C) H 0.1259 0.7597 0.1114 0.0508 Uiso 1.0 2 calc R . . H(72A) H 0.4961 1.1195 0.1127 0.0510 Uiso 1.0 2 calc R . . H(72B) H 0.5759 1.1108 0.1732 0.0510 Uiso 1.0 2 calc R . . H(72C) H 0.4667 1.1204 0.1813 0.0510 Uiso 1.0 2 calc R . . H(73A) H 0.5279 0.9482 0.0934 0.0484 Uiso 1.0 2 calc R . . H(73B) H 0.6141 1.0035 0.1319 0.0484 Uiso 1.0 2 calc R . . H(73C) H 0.5505 1.0180 0.0667 0.0484 Uiso 1.0 2 calc R . . H(74A) H 0.3263 1.0306 0.1249 0.0452 Uiso 1.0 2 calc R . . H(74B) H 0.3513 0.9636 0.0914 0.0452 Uiso 1.0 2 calc R . . H(74C) H 0.3726 1.0321 0.0620 0.0452 Uiso 1.0 2 calc R . . H(80A) H 0.7176 0.7373 0.1312 0.0521 Uiso 1.0 2 calc R . . H(80B) H 0.6056 0.7371 0.0986 0.0521 Uiso 1.0 2 calc R . . H(80C) H 0.6660 0.6820 0.0740 0.0521 Uiso 1.0 2 calc R . . H(81A) H 0.5389 0.5883 0.0930 0.0466 Uiso 1.0 2 calc R . . H(81B) H 0.4765 0.6448 0.1119 0.0466 Uiso 1.0 2 calc R . . H(81C) H 0.5030 0.5913 0.1597 0.0466 Uiso 1.0 2 calc R . . H(82A) H 0.7631 0.6457 0.1952 0.0528 Uiso 1.0 2 calc R . . H(82B) H 0.7078 0.5919 0.1376 0.0528 Uiso 1.0 2 calc R . . H(82C) H 0.6798 0.5889 0.2063 0.0528 Uiso 1.0 2 calc R . . H(90A) H -0.3541 0.2733 0.0814 0.0444 Uiso 1.0 2 calc R . . H(90B) H -0.3431 0.2004 0.1004 0.0444 Uiso 1.0 2 calc R . . H(91A) H -0.2894 0.3179 0.1873 0.0655 Uiso 1.0 2 calc R . . H(91B) H -0.2796 0.2447 0.2062 0.0655 Uiso 1.0 2 calc R . . H(91C) H -0.3858 0.2651 0.1836 0.0655 Uiso 1.0 2 calc R . . H(92A) H -0.2168 0.3539 0.0854 0.0509 Uiso 1.0 2 calc R . . H(92B) H -0.1401 0.3424 0.1464 0.0509 Uiso 1.0 2 calc R . . H(93A) H -0.1090 0.3229 0.0193 0.0714 Uiso 1.0 2 calc R . . H(93B) H -0.0324 0.3108 0.0801 0.0714 Uiso 1.0 2 calc R . . H(93C) H -0.0558 0.3842 0.0700 0.0714 Uiso 1.0 2 calc R . . H(94A) H -0.1315 0.2321 0.1771 0.0533 Uiso 1.0 2 calc R . . H(94B) H -0.0798 0.2200 0.1173 0.0533 Uiso 1.0 2 calc R . . H(95A) H -0.1944 0.1238 0.0800 0.0708 Uiso 1.0 2 calc R . . H(95B) H -0.2461 0.1359 0.1399 0.0708 Uiso 1.0 2 calc R . . H(95C) H -0.1367 0.1181 0.1498 0.0708 Uiso 1.0 2 calc R . . H(96A) H 0.0091 0.9676 0.2285 0.0641 Uiso 1.0 2 calc R . . H(96B) H 0.0505 0.9821 0.3031 0.0641 Uiso 1.0 2 calc R . . H(97A) H 0.0731 0.8701 0.3069 0.0888 Uiso 1.0 2 calc R . . H(97B) H 0.0328 0.8554 0.2321 0.0888 Uiso 1.0 2 calc R . . H(97C) H -0.0391 0.8750 0.2787 0.0888 Uiso 1.0 2 calc R . . H(98A) H 0.2420 0.9558 0.1837 0.0735 Uiso 1.0 2 calc R . . H(98B) H 0.1636 0.8930 0.1877 0.0735 Uiso 1.0 2 calc R . . H(99A) H 0.1178 1.0076 0.1317 0.0931 Uiso 1.0 2 calc R . . H(99B) H 0.0390 0.9449 0.1361 0.0931 Uiso 1.0 2 calc R . . H(99C) H 0.1212 0.9373 0.0938 0.0931 Uiso 1.0 2 calc R . . H(102) H -0.1367 1.0468 0.2363 0.0825 Uiso 1.0 2 calc R . . H(103) H -0.2019 1.0093 0.3162 0.1082 Uiso 1.0 2 calc R . . H(104) H -0.2934 0.9091 0.3065 0.1276 Uiso 1.0 2 calc R . . H(105) H -0.3173 0.8415 0.2160 0.1376 Uiso 1.0 2 calc R . . H(106) H -0.2620 0.8771 0.1270 0.1281 Uiso 1.0 2 calc R . . H(107) H -0.1615 0.9848 0.1398 0.1008 Uiso 1.0 2 calc R . . H(108) H -0.4306 0.4731 0.1872 0.0732 Uiso 1.0 2 calc R . . H(109) H -0.5487 0.3987 0.2177 0.0616 Uiso 1.0 2 calc R . . H(110) H -0.6194 0.3043 0.1521 0.0678 Uiso 1.0 2 calc R . . H(111) H -0.5770 0.2835 0.0548 0.0765 Uiso 1.0 2 calc R . . H(112) H -0.4603 0.3565 0.0218 0.0853 Uiso 1.0 2 calc R . . H(113) H -0.3856 0.4521 0.0880 0.0838 Uiso 1.0 2 calc R . . H(114) H 0.0676 0.5263 0.4647 0.1462 Uiso 1.0 2 calc R . . H(115) H 0.2059 0.5623 0.5451 0.1103 Uiso 1.0 2 calc R . . H(116) H 0.3281 0.4991 0.5560 0.1325 Uiso 1.0 2 calc R . . H(117) H 0.3233 0.4053 0.4918 0.1149 Uiso 1.0 2 calc R . . H(118) H 0.2014 0.3765 0.4084 0.1252 Uiso 1.0 2 calc R . . H(119) H 0.0693 0.4296 0.3951 0.1457 Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb(1) 0.02087(17) 0.01477(16) 0.02292(18) 0.00384(12) 0.00479(13) 0.00481(13) Nb(2) 0.02174(17) 0.02141(17) 0.01479(16) 0.00491(13) 0.00192(13) 0.00126(12) Cl(1) 0.0284(5) 0.0243(5) 0.0377(6) 0.0113(4) 0.0071(4) 0.0050(4) Cl(2) 0.0282(5) 0.0184(5) 0.0505(7) -0.0025(4) 0.0094(5) -0.0002(5) Cl(3) 0.0477(7) 0.0384(6) 0.0331(6) 0.0155(5) 0.0130(5) 0.0204(5) Cl(4) 0.0372(6) 0.0369(6) 0.0234(5) 0.0045(5) 0.0120(5) 0.0041(4) Cl(5) 0.0306(5) 0.0267(5) 0.0239(5) 0.0040(4) 0.0015(4) -0.0053(4) Cl(6) 0.0333(5) 0.0333(6) 0.0226(5) 0.0128(4) -0.0030(4) 0.0049(4) O(1) 0.0253(14) 0.0164(13) 0.0253(14) 0.0043(10) 0.0090(11) 0.0049(11) O(2) 0.0211(13) 0.0192(13) 0.0252(14) 0.0034(10) 0.0025(11) 0.0036(11) O(3) 0.0235(13) 0.0156(13) 0.0224(14) 0.0024(10) 0.0032(11) 0.0053(10) O(4) 0.0226(14) 0.0243(14) 0.0194(13) 0.0029(11) 0.0029(11) 0.0014(11) O(5) 0.0277(14) 0.0225(14) 0.0191(13) 0.0022(11) 0.0047(11) 0.0034(11) O(6) 0.0223(13) 0.0237(14) 0.0196(13) 0.0051(11) 0.0018(11) 0.0034(11) N(1) 0.0314(19) 0.037(2) 0.0240(18) 0.0049(16) -0.0013(15) -0.0015(15) N(2) 0.040(3) 0.0205(19) 0.083(4) 0.0102(16) 0.018(3) 0.013(2) C(1) 0.0184(17) 0.0176(18) 0.0187(18) 0.0023(14) 0.0033(14) 0.0026(14) C(2) 0.0189(17) 0.0182(18) 0.0166(17) 0.0028(14) 0.0013(14) 0.0035(14) C(3) 0.0208(18) 0.0160(18) 0.0172(18) 0.0023(14) 0.0011(14) 0.0006(14) C(4) 0.0225(18) 0.0215(19) 0.0170(18) 0.0008(15) 0.0053(15) 0.0005(15) C(5) 0.0211(19) 0.027(2) 0.026(2) 0.0043(16) 0.0062(16) 0.0007(16) C(6) 0.0240(19) 0.0219(19) 0.024(2) 0.0067(15) 0.0007(16) 0.0033(16) C(7) 0.0238(19) 0.0196(19) 0.024(2) 0.0016(15) 0.0032(16) 0.0052(15) C(8) 0.0206(18) 0.0211(19) 0.0175(18) 0.0006(14) 0.0066(15) 0.0018(14) C(9) 0.0221(18) 0.0155(17) 0.0169(17) 0.0039(14) 0.0043(14) 0.0041(14) C(10) 0.0227(19) 0.025(2) 0.0187(18) 0.0034(15) 0.0037(15) 0.0015(15) C(11) 0.0193(18) 0.027(2) 0.026(2) -0.0004(15) -0.0001(16) -0.0013(16) C(12) 0.025(2) 0.0202(19) 0.026(2) 0.0014(15) 0.0076(16) 0.0005(16) C(13) 0.0242(19) 0.0185(18) 0.0216(19) 0.0044(15) 0.0045(15) 0.0025(15) C(14) 0.0139(16) 0.0166(17) 0.0186(18) 0.0015(13) -0.0004(13) 0.0022(14) C(15) 0.0175(17) 0.0180(18) 0.0229(19) 0.0029(14) 0.0018(15) 0.0041(15) C(16) 0.0223(19) 0.0230(19) 0.0201(19) 0.0060(15) 0.0022(15) 0.0018(15) C(17) 0.027(2) 0.029(2) 0.0167(18) 0.0069(16) 0.0031(15) 0.0037(15) C(18) 0.0200(18) 0.0193(19) 0.025(2) 0.0027(14) 0.0036(15) 0.0070(15) C(19) 0.0183(17) 0.0154(18) 0.0243(19) 0.0031(14) 0.0029(15) 0.0026(14) C(20) 0.027(2) 0.031(3) 0.028(3) 0.0035(17) 0.0134(17) 0.0084(17) C(21) 0.040(3) 0.035(3) 0.041(3) 0.007(2) 0.024(3) 0.012(2) C(22) 0.041(3) 0.030(3) 0.047(3) -0.0010(19) 0.024(3) 0.007(2) C(23) 0.046(3) 0.052(3) 0.029(3) 0.014(3) 0.015(2) 0.018(2) C(24) 0.030(3) 0.028(3) 0.043(3) 0.0158(18) 0.0128(19) 0.0080(19) C(25) 0.051(4) 0.051(4) 0.084(5) 0.035(3) 0.033(3) 0.029(3) C(26) 0.064(4) 0.028(3) 0.053(4) 0.022(3) 0.008(3) -0.001(3) C(27) 0.050(3) 0.045(3) 0.051(4) 0.027(3) 0.007(3) 0.014(3) C(28) 0.021(2) 0.031(3) 0.036(3) 0.0073(17) -0.0040(17) 0.0039(18) C(29) 0.030(3) 0.043(3) 0.051(3) 0.018(2) 0.002(2) -0.002(3) C(30) 0.045(3) 0.041(3) 0.039(3) 0.009(3) -0.005(3) 0.015(3) C(31) 0.028(3) 0.042(3) 0.056(4) 0.007(2) -0.013(3) 0.006(3) C(32) 0.037(3) 0.020(2) 0.039(3) -0.0037(17) -0.002(2) -0.0006(18) C(33) 0.074(4) 0.033(3) 0.058(4) -0.001(3) 0.007(3) -0.013(3) C(34) 0.069(4) 0.040(3) 0.086(5) -0.021(3) 0.032(4) 0.006(3) C(35) 0.075(5) 0.020(3) 0.097(6) -0.001(3) -0.021(4) 0.008(3) C(36) 0.039(3) 0.021(2) 0.024(2) 0.0069(17) 0.0016(18) -0.0011(16) C(37) 0.056(3) 0.033(3) 0.037(3) 0.024(3) 0.007(3) 0.002(2) C(38) 0.079(4) 0.028(3) 0.028(3) 0.017(3) 0.012(3) -0.0020(19) C(39) 0.049(3) 0.029(3) 0.046(3) -0.004(2) 0.006(3) -0.011(2) C(40) 0.036(3) 0.028(3) 0.028(3) 0.0040(18) 0.0076(18) 0.0095(18) C(44) 0.0228(19) 0.0197(19) 0.0187(18) 0.0005(15) 0.0027(15) 0.0016(15) C(45) 0.0248(19) 0.0137(17) 0.0221(19) 0.0039(14) 0.0037(15) 0.0032(14) C(46) 0.0236(19) 0.0178(18) 0.0175(18) 0.0047(14) 0.0048(15) 0.0019(14) C(47) 0.0201(18) 0.0188(19) 0.030(2) 0.0026(15) 0.0046(16) 0.0018(16) C(48) 0.026(2) 0.023(2) 0.033(3) 0.0029(16) 0.0095(17) 0.0068(17) C(49) 0.038(3) 0.021(2) 0.022(2) 0.0042(17) 0.0114(17) 0.0014(16) C(50) 0.031(2) 0.0215(19) 0.0197(19) -0.0002(16) 0.0021(16) 0.0017(15) C(51) 0.0214(18) 0.0226(19) 0.0215(19) 0.0040(15) 0.0032(15) 0.0013(15) C(52) 0.0202(18) 0.0189(19) 0.0229(19) 0.0002(14) 0.0045(15) 0.0012(15) C(53) 0.029(2) 0.026(2) 0.022(2) 0.0006(16) 0.0034(16) 0.0002(16) C(54) 0.029(2) 0.027(2) 0.029(3) -0.0009(17) 0.0035(17) -0.0023(17) C(55) 0.028(2) 0.0181(19) 0.040(3) -0.0008(16) 0.0078(18) 0.0006(17) C(56) 0.0225(19) 0.022(2) 0.028(2) 0.0031(15) 0.0052(16) 0.0034(16) C(57) 0.0206(18) 0.0187(18) 0.024(2) -0.0023(14) 0.0031(15) 0.0072(15) C(58) 0.0197(18) 0.0228(19) 0.0208(19) 0.0001(15) 0.0017(15) 0.0081(15) C(59) 0.0219(19) 0.023(2) 0.031(3) 0.0002(15) 0.0057(16) 0.0105(16) C(60) 0.021(2) 0.033(3) 0.041(3) 0.0028(17) -0.0009(18) 0.0159(19) C(61) 0.022(2) 0.036(3) 0.038(3) -0.0043(17) -0.0048(18) 0.015(2) C(62) 0.029(2) 0.029(2) 0.021(2) -0.0055(17) -0.0007(16) 0.0052(16) C(63) 0.023(2) 0.033(3) 0.030(3) -0.0029(17) 0.0015(17) 0.0038(18) C(64) 0.041(3) 0.035(3) 0.050(3) 0.001(2) -0.000(3) -0.015(3) C(65) 0.026(3) 0.057(3) 0.044(3) -0.010(2) 0.002(2) 0.002(3) C(66) 0.029(3) 0.057(3) 0.034(3) -0.003(2) -0.008(2) 0.009(3) C(67) 0.048(3) 0.030(3) 0.024(2) 0.0037(19) 0.0150(19) 0.0071(17) C(71) 0.033(3) 0.024(2) 0.033(3) 0.0036(17) 0.0100(18) 0.0095(17) C(72) 0.055(3) 0.029(3) 0.046(3) 0.002(3) 0.015(3) 0.014(2) C(73) 0.044(3) 0.042(3) 0.041(3) 0.007(3) 0.022(3) 0.012(3) C(74) 0.042(3) 0.035(3) 0.037(3) 0.009(2) 0.003(2) 0.014(2) C(75) 0.049(3) 0.024(3) 0.032(3) -0.0052(19) 0.002(2) -0.0052(18) C(79) 0.030(3) 0.030(3) 0.038(3) 0.0106(17) 0.0111(19) 0.0117(19) C(80) 0.050(3) 0.045(3) 0.048(3) 0.022(3) 0.026(3) 0.018(3) C(81) 0.043(3) 0.029(3) 0.046(3) 0.015(2) 0.006(3) -0.000(2) C(82) 0.035(3) 0.045(3) 0.059(4) 0.020(3) 0.013(3) 0.014(3) C(83) 0.037(3) 0.065(4) 0.042(3) -0.000(3) -0.017(3) 0.021(3) C(90) 0.027(3) 0.052(3) 0.033(3) 0.009(2) 0.0022(19) 0.007(2) C(91) 0.047(3) 0.082(4) 0.040(3) 0.019(3) 0.017(3) 0.004(3) C(92) 0.043(3) 0.042(3) 0.034(3) -0.007(3) -0.004(2) -0.002(2) C(93) 0.038(3) 0.070(4) 0.062(4) -0.012(3) -0.002(3) 0.016(3) C(94) 0.038(3) 0.068(4) 0.032(3) 0.020(3) 0.006(2) 0.013(3) C(95) 0.078(5) 0.057(4) 0.047(4) 0.023(3) 0.007(3) 0.025(3) C(96) 0.042(3) 0.035(3) 0.095(5) 0.017(3) 0.031(3) 0.023(3) C(97) 0.054(4) 0.044(4) 0.134(7) 0.007(3) 0.037(4) 0.031(4) C(98) 0.054(4) 0.040(3) 0.100(6) 0.016(3) 0.033(4) 0.009(3) C(99) 0.090(6) 0.062(4) 0.086(6) 0.029(4) 0.024(5) -0.005(4) C(100) 0.047(4) 0.038(3) 0.100(6) 0.014(3) 0.008(4) 0.017(3) C(101) 0.096(6) 0.048(4) 0.103(7) 0.012(4) -0.002(5) 0.015(4) C(102) 0.044(4) 0.037(3) 0.125(7) -0.005(3) 0.022(4) 0.013(4) C(103) 0.084(6) 0.082(6) 0.104(7) 0.003(5) 0.026(5) 0.007(5) C(104) 0.130(8) 0.075(6) 0.148(10) 0.037(6) 0.089(8) 0.046(6) C(105) 0.079(6) 0.042(4) 0.233(13) -0.021(4) 0.091(7) -0.004(6) C(106) 0.081(6) 0.094(6) 0.139(9) 0.014(5) 0.032(6) -0.047(6) C(107) 0.066(5) 0.098(6) 0.114(7) 0.039(5) 0.048(5) 0.056(6) C(108) 0.065(4) 0.043(3) 0.070(5) 0.011(3) -0.004(4) 0.003(3) C(109) 0.056(4) 0.067(4) 0.039(3) 0.027(3) 0.013(3) 0.010(3) C(110) 0.034(3) 0.067(4) 0.068(4) 0.004(3) 0.014(3) 0.002(3) C(111) 0.051(4) 0.075(4) 0.057(4) 0.021(3) -0.010(3) -0.019(4) C(112) 0.064(4) 0.124(6) 0.044(4) 0.057(5) 0.024(3) 0.021(4) C(113) 0.051(4) 0.079(5) 0.093(6) 0.015(4) 0.027(4) 0.049(5) C(114) 0.100(7) 0.119(8) 0.132(9) 0.052(6) -0.042(6) 0.004(7) C(115) 0.120(7) 0.060(5) 0.077(6) 0.020(5) -0.028(5) -0.011(4) C(116) 0.093(6) 0.052(5) 0.148(9) -0.015(4) -0.066(6) 0.010(5) C(117) 0.074(6) 0.086(6) 0.136(9) 0.013(5) 0.033(6) 0.038(6) C(118) 0.163(10) 0.120(7) 0.042(4) 0.055(7) 0.023(6) 0.012(5) C(119) 0.129(8) 0.118(8) 0.082(6) 0.025(7) -0.060(6) -0.037(6) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb(1) Cl(1) 2.4346(13) yes . . Nb(1) Cl(2) 2.4496(12) yes . . Nb(1) Cl(3) 2.4215(14) yes . . Nb(1) O(1) 1.943(3) yes . . Nb(1) O(2) 1.919(3) yes . . Nb(1) O(3) 1.939(3) yes . . Nb(2) Cl(4) 2.4064(14) yes . . Nb(2) Cl(5) 2.4399(12) yes . . Nb(2) Cl(6) 2.4732(13) yes . . Nb(2) O(4) 1.947(3) yes . . Nb(2) O(5) 1.927(3) yes . . Nb(2) O(6) 1.912(3) yes . . O(1) C(3) 1.369(5) yes . . O(2) C(9) 1.381(5) yes . . O(3) C(15) 1.378(5) yes . . O(4) C(46) 1.366(5) yes . . O(5) C(51) 1.374(5) yes . . O(6) C(58) 1.374(5) yes . . N(1) C(90) 1.514(6) yes . . N(1) C(92) 1.512(6) yes . . N(1) C(94) 1.505(7) yes . . N(2) C(96) 1.506(7) yes . . N(2) C(98) 1.504(9) yes . . N(2) C(100) 1.497(8) yes . . C(1) C(2) 1.508(6) yes . . C(1) C(8) 1.503(5) yes . . C(1) C(14) 1.510(6) yes . . C(2) C(3) 1.420(6) yes . . C(2) C(7) 1.374(6) yes . . C(3) C(4) 1.410(6) yes . . C(4) C(5) 1.396(6) yes . . C(4) C(20) 1.548(6) yes . . C(5) C(6) 1.400(6) yes . . C(6) C(7) 1.392(6) yes . . C(6) C(24) 1.532(6) yes . . C(8) C(9) 1.408(6) yes . . C(8) C(13) 1.387(5) yes . . C(9) C(10) 1.406(5) yes . . C(10) C(11) 1.397(6) yes . . C(10) C(28) 1.534(6) yes . . C(11) C(12) 1.394(6) yes . . C(12) C(13) 1.390(5) yes . . C(12) C(32) 1.540(6) yes . . C(14) C(15) 1.417(5) yes . . C(14) C(19) 1.386(6) yes . . C(15) C(16) 1.410(6) yes . . C(16) C(17) 1.399(6) yes . . C(16) C(36) 1.546(6) yes . . C(17) C(18) 1.391(6) yes . . C(18) C(19) 1.381(6) yes . . C(18) C(40) 1.545(6) yes . . C(20) C(21) 1.538(7) yes . . C(20) C(22) 1.533(6) yes . . C(20) C(23) 1.530(6) yes . . C(24) C(25) 1.539(8) yes . . C(24) C(26) 1.527(6) yes . . C(24) C(27) 1.529(8) yes . . C(28) C(29) 1.536(7) yes . . C(28) C(30) 1.536(7) yes . . C(28) C(31) 1.537(6) yes . . C(32) C(33) 1.527(8) yes . . C(32) C(34) 1.540(9) yes . . C(32) C(35) 1.516(8) yes . . C(36) C(37) 1.528(7) yes . . C(36) C(38) 1.529(7) yes . . C(36) C(39) 1.539(7) yes . . C(40) C(41) 1.566(10) yes . . C(40) C(42) 1.576(9) yes . . C(40) C(43) 1.522(10) yes . . C(40) C(123) 1.586(17) yes . . C(40) C(124) 1.642(15) yes . . C(40) C(125) 1.484(19) yes . . C(41) C(124) 1.232(19) yes . . C(41) C(125) 1.765(17) yes . . C(43) C(124) 1.79(2) yes . . C(44) C(45) 1.512(6) yes . . C(44) C(52) 1.508(5) yes . . C(44) C(57) 1.511(6) yes . . C(45) C(46) 1.411(5) yes . . C(45) C(50) 1.391(6) yes . . C(46) C(47) 1.412(6) yes . . C(47) C(48) 1.392(7) yes . . C(47) C(63) 1.543(5) yes . . C(48) C(49) 1.389(6) yes . . C(49) C(50) 1.392(6) yes . . C(49) C(67) 1.551(7) yes . . C(51) C(52) 1.417(6) yes . . C(51) C(56) 1.414(6) yes . . C(52) C(53) 1.382(5) yes . . C(53) C(54) 1.389(6) yes . . C(54) C(55) 1.383(7) yes . . C(54) C(75) 1.550(6) yes . . C(55) C(56) 1.396(6) yes . . C(56) C(71) 1.536(6) yes . . C(57) C(58) 1.411(6) yes . . C(57) C(62) 1.386(6) yes . . C(58) C(59) 1.403(6) yes . . C(59) C(60) 1.392(6) yes . . C(59) C(79) 1.546(6) yes . . C(60) C(61) 1.386(7) yes . . C(61) C(62) 1.388(7) yes . . C(61) C(83) 1.547(7) yes . . C(63) C(64) 1.541(7) yes . . C(63) C(65) 1.525(7) yes . . C(63) C(66) 1.526(7) yes . . C(67) C(68) 1.581(14) yes . . C(67) C(69) 1.581(13) yes . . C(67) C(70) 1.502(15) yes . . C(67) C(126) 1.510(14) yes . . C(67) C(127) 1.556(11) yes . . C(67) C(128) 1.602(10) yes . . C(71) C(72) 1.551(6) yes . . C(71) C(73) 1.544(7) yes . . C(71) C(74) 1.529(6) yes . . C(75) C(76) 1.557(15) yes . . C(75) C(77) 1.606(18) yes . . C(75) C(78) 1.538(13) yes . . C(75) C(129) 1.591(12) yes . . C(75) C(130) 1.557(13) yes . . C(75) C(131) 1.519(13) yes . . C(79) C(80) 1.537(7) yes . . C(79) C(81) 1.542(6) yes . . C(79) C(82) 1.539(7) yes . . C(83) C(84) 1.53(2) yes . . C(83) C(85) 1.557(19) yes . . C(83) C(86) 1.597(17) yes . . C(83) C(87) 1.596(14) yes . . C(83) C(88) 1.553(14) yes . . C(83) C(89) 1.556(16) yes . . C(84) C(88) 1.79(3) yes . . C(85) C(88) 1.18(2) yes . . C(85) C(89) 1.75(3) yes . . C(86) C(87) 1.91(2) yes . . C(90) C(91) 1.511(8) yes . . C(92) C(93) 1.506(9) yes . . C(94) C(95) 1.510(8) yes . . C(96) C(97) 1.516(8) yes . . C(98) C(99) 1.477(10) yes . . C(100) C(101) 1.512(11) yes . . C(102) C(103) 1.309(13) yes . . C(102) C(107) 1.330(12) yes . . C(103) C(104) 1.311(12) yes . . C(104) C(105) 1.301(15) yes . . C(105) C(106) 1.367(17) yes . . C(106) C(107) 1.430(12) yes . . C(108) C(109) 1.367(9) yes . . C(108) C(113) 1.392(11) yes . . C(109) C(110) 1.348(8) yes . . C(110) C(111) 1.355(10) yes . . C(111) C(112) 1.366(10) yes . . C(112) C(113) 1.370(10) yes . . C(114) C(115) 1.369(12) yes . . C(114) C(119) 1.410(14) yes . . C(115) C(116) 1.323(13) yes . . C(116) C(117) 1.323(13) yes . . C(117) C(118) 1.292(13) yes . . C(118) C(119) 1.310(17) yes . . C(120) C(121) 1.59(4) yes . . C(120) C(122) 1.32(3) yes . 2_576 C(120) C(134) 1.09(5) yes . . C(121) C(122) 1.33(3) yes . . C(121) C(134) 1.85(4) yes . . C(122) C(134) 1.20(4) yes . 2_576 C(132) C(133) 1.34(3) yes . . C(132) C(134) 1.41(4) yes . 2_576 C(133) C(134) 1.46(5) yes . . N(1) H(1A) 0.930 no . . N(2) H(2A) 0.930 no . . C(1) H(1) 1.000 no . . C(5) H(5) 0.950 no . . C(7) H(7) 0.950 no . . C(11) H(11) 0.950 no . . C(13) H(13) 0.950 no . . C(17) H(17) 0.950 no . . C(19) H(19) 0.950 no . . C(21) H(21A) 0.980 no . . C(21) H(21B) 0.980 no . . C(21) H(21C) 0.980 no . . C(22) H(22A) 0.980 no . . C(22) H(22B) 0.980 no . . C(22) H(22C) 0.980 no . . C(23) H(23A) 0.980 no . . C(23) H(23B) 0.980 no . . C(23) H(23C) 0.980 no . . C(25) H(25A) 0.980 no . . C(25) H(25B) 0.980 no . . C(25) H(25C) 0.980 no . . C(26) H(26A) 0.980 no . . C(26) H(26B) 0.980 no . . C(26) H(26C) 0.980 no . . C(27) H(27A) 0.980 no . . C(27) H(27B) 0.980 no . . C(27) H(27C) 0.980 no . . C(29) H(29A) 0.980 no . . C(29) H(29B) 0.980 no . . C(29) H(29C) 0.980 no . . C(30) H(30A) 0.980 no . . C(30) H(30B) 0.980 no . . C(30) H(30C) 0.980 no . . C(31) H(31A) 0.980 no . . C(31) H(31B) 0.980 no . . C(31) H(31C) 0.980 no . . C(33) H(33A) 0.980 no . . C(33) H(33B) 0.980 no . . C(33) H(33C) 0.980 no . . C(34) H(34A) 0.980 no . . C(34) H(34B) 0.980 no . . C(34) H(34C) 0.980 no . . C(35) H(35A) 0.980 no . . C(35) H(35B) 0.980 no . . C(35) H(35C) 0.980 no . . C(37) H(37A) 0.980 no . . C(37) H(37B) 0.980 no . . C(37) H(37C) 0.980 no . . C(38) H(38A) 0.980 no . . C(38) H(38B) 0.980 no . . C(38) H(38C) 0.980 no . . C(39) H(39A) 0.980 no . . C(39) H(39B) 0.980 no . . C(39) H(39C) 0.980 no . . C(44) H(44) 1.000 no . . C(48) H(48) 0.950 no . . C(50) H(50) 0.950 no . . C(53) H(53) 0.950 no . . C(55) H(55) 0.950 no . . C(60) H(60) 0.950 no . . C(62) H(62) 0.950 no . . C(64) H(64A) 0.980 no . . C(64) H(64B) 0.980 no . . C(64) H(64C) 0.980 no . . C(65) H(65A) 0.980 no . . C(65) H(65B) 0.980 no . . C(65) H(65C) 0.980 no . . C(66) H(66A) 0.980 no . . C(66) H(66B) 0.980 no . . C(66) H(66C) 0.980 no . . C(72) H(72A) 0.980 no . . C(72) H(72B) 0.980 no . . C(72) H(72C) 0.980 no . . C(73) H(73A) 0.980 no . . C(73) H(73B) 0.980 no . . C(73) H(73C) 0.980 no . . C(74) H(74A) 0.980 no . . C(74) H(74B) 0.980 no . . C(74) H(74C) 0.980 no . . C(80) H(80A) 0.980 no . . C(80) H(80B) 0.980 no . . C(80) H(80C) 0.980 no . . C(81) H(81A) 0.980 no . . C(81) H(81B) 0.980 no . . C(81) H(81C) 0.980 no . . C(82) H(82A) 0.980 no . . C(82) H(82B) 0.980 no . . C(82) H(82C) 0.980 no . . C(90) H(90A) 0.990 no . . C(90) H(90B) 0.990 no . . C(91) H(91A) 0.980 no . . C(91) H(91B) 0.980 no . . C(91) H(91C) 0.980 no . . C(92) H(92A) 0.990 no . . C(92) H(92B) 0.990 no . . C(93) H(93A) 0.980 no . . C(93) H(93B) 0.980 no . . C(93) H(93C) 0.980 no . . C(94) H(94A) 0.990 no . . C(94) H(94B) 0.990 no . . C(95) H(95A) 0.980 no . . C(95) H(95B) 0.980 no . . C(95) H(95C) 0.980 no . . C(96) H(96A) 0.990 no . . C(96) H(96B) 0.990 no . . C(97) H(97A) 0.980 no . . C(97) H(97B) 0.980 no . . C(97) H(97C) 0.980 no . . C(98) H(98A) 0.990 no . . C(98) H(98B) 0.990 no . . C(99) H(99A) 0.980 no . . C(99) H(99B) 0.980 no . . C(99) H(99C) 0.980 no . . C(100) H(10A) 0.990 no . . C(100) H(10B) 0.990 no . . C(101) H(10C) 0.980 no . . C(101) H(10D) 0.980 no . . C(101) H(10E) 0.980 no . . C(102) H(102) 0.950 no . . C(103) H(103) 0.950 no . . C(104) H(104) 0.950 no . . C(105) H(105) 0.950 no . . C(106) H(106) 0.950 no . . C(107) H(107) 0.950 no . . C(108) H(108) 0.950 no . . C(109) H(109) 0.950 no . . C(110) H(110) 0.950 no . . C(111) H(111) 0.950 no . . C(112) H(112) 0.950 no . . C(113) H(113) 0.950 no . . C(114) H(114) 0.950 no . . C(115) H(115) 0.950 no . . C(116) H(116) 0.950 no . . C(117) H(117) 0.950 no . . C(118) H(118) 0.950 no . . C(119) H(119) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Nb(1) Cl(2) 85.02(5) yes . . . Cl(1) Nb(1) Cl(3) 85.85(5) yes . . . Cl(1) Nb(1) O(1) 168.91(9) yes . . . Cl(1) Nb(1) O(2) 90.59(9) yes . . . Cl(1) Nb(1) O(3) 91.09(9) yes . . . Cl(2) Nb(1) Cl(3) 88.93(5) yes . . . Cl(2) Nb(1) O(1) 87.46(8) yes . . . Cl(2) Nb(1) O(2) 175.60(9) yes . . . Cl(2) Nb(1) O(3) 85.96(8) yes . . . Cl(3) Nb(1) O(1) 85.87(9) yes . . . Cl(3) Nb(1) O(2) 90.62(9) yes . . . Cl(3) Nb(1) O(3) 174.25(7) yes . . . O(1) Nb(1) O(2) 96.86(11) yes . . . O(1) Nb(1) O(3) 96.50(11) yes . . . O(2) Nb(1) O(3) 94.27(11) yes . . . Cl(4) Nb(2) Cl(5) 87.32(4) yes . . . Cl(4) Nb(2) Cl(6) 88.44(5) yes . . . Cl(4) Nb(2) O(4) 173.42(7) yes . . . Cl(4) Nb(2) O(5) 88.93(9) yes . . . Cl(4) Nb(2) O(6) 90.61(9) yes . . . Cl(5) Nb(2) Cl(6) 85.68(4) yes . . . Cl(5) Nb(2) O(4) 87.69(8) yes . . . Cl(5) Nb(2) O(5) 172.90(9) yes . . . Cl(5) Nb(2) O(6) 89.33(8) yes . . . Cl(6) Nb(2) O(4) 86.91(9) yes . . . Cl(6) Nb(2) O(5) 88.19(9) yes . . . Cl(6) Nb(2) O(6) 174.96(8) yes . . . O(4) Nb(2) O(5) 95.57(11) yes . . . O(4) Nb(2) O(6) 93.61(12) yes . . . O(5) Nb(2) O(6) 96.75(11) yes . . . Nb(1) O(1) C(3) 147.7(3) yes . . . Nb(1) O(2) C(9) 147.6(3) yes . . . Nb(1) O(3) C(15) 147.3(2) yes . . . Nb(2) O(4) C(46) 148.5(2) yes . . . Nb(2) O(5) C(51) 149.2(3) yes . . . Nb(2) O(6) C(58) 148.7(3) yes . . . C(90) N(1) C(92) 111.5(4) yes . . . C(90) N(1) C(94) 114.0(4) yes . . . C(92) N(1) C(94) 110.9(4) yes . . . C(96) N(2) C(98) 114.1(4) yes . . . C(96) N(2) C(100) 113.9(5) yes . . . C(98) N(2) C(100) 109.1(5) yes . . . C(2) C(1) C(8) 118.8(3) yes . . . C(2) C(1) C(14) 118.7(3) yes . . . C(8) C(1) C(14) 115.4(3) yes . . . C(1) C(2) C(3) 114.3(4) yes . . . C(1) C(2) C(7) 126.1(4) yes . . . C(3) C(2) C(7) 119.5(4) yes . . . O(1) C(3) C(2) 119.0(4) yes . . . O(1) C(3) C(4) 120.8(4) yes . . . C(2) C(3) C(4) 120.2(4) yes . . . C(3) C(4) C(5) 117.2(4) yes . . . C(3) C(4) C(20) 121.5(4) yes . . . C(5) C(4) C(20) 121.2(4) yes . . . C(4) C(5) C(6) 123.7(4) yes . . . C(5) C(6) C(7) 117.1(4) yes . . . C(5) C(6) C(24) 122.5(4) yes . . . C(7) C(6) C(24) 120.4(4) yes . . . C(2) C(7) C(6) 122.3(4) yes . . . C(1) C(8) C(9) 115.7(3) yes . . . C(1) C(8) C(13) 124.4(4) yes . . . C(9) C(8) C(13) 119.9(3) yes . . . O(2) C(9) C(8) 118.4(3) yes . . . O(2) C(9) C(10) 120.8(4) yes . . . C(8) C(9) C(10) 120.8(4) yes . . . C(9) C(10) C(11) 116.4(4) yes . . . C(9) C(10) C(28) 121.6(4) yes . . . C(11) C(10) C(28) 122.0(3) yes . . . C(10) C(11) C(12) 124.2(4) yes . . . C(11) C(12) C(13) 117.5(4) yes . . . C(11) C(12) C(32) 120.1(4) yes . . . C(13) C(12) C(32) 122.4(4) yes . . . C(8) C(13) C(12) 121.1(4) yes . . . C(1) C(14) C(15) 115.5(4) yes . . . C(1) C(14) C(19) 124.1(4) yes . . . C(15) C(14) C(19) 120.2(4) yes . . . O(3) C(15) C(14) 118.2(4) yes . . . O(3) C(15) C(16) 121.8(3) yes . . . C(14) C(15) C(16) 120.0(4) yes . . . C(15) C(16) C(17) 116.6(4) yes . . . C(15) C(16) C(36) 121.7(4) yes . . . C(17) C(16) C(36) 121.7(4) yes . . . C(16) C(17) C(18) 124.3(4) yes . . . C(17) C(18) C(19) 117.7(4) yes . . . C(17) C(18) C(40) 122.2(4) yes . . . C(19) C(18) C(40) 120.1(4) yes . . . C(14) C(19) C(18) 121.1(4) yes . . . C(4) C(20) C(21) 111.6(4) yes . . . C(4) C(20) C(22) 111.4(4) yes . . . C(4) C(20) C(23) 109.0(4) yes . . . C(21) C(20) C(22) 107.0(4) yes . . . C(21) C(20) C(23) 108.2(4) yes . . . C(22) C(20) C(23) 109.5(4) yes . . . C(6) C(24) C(25) 112.3(4) yes . . . C(6) C(24) C(26) 108.4(4) yes . . . C(6) C(24) C(27) 110.2(4) yes . . . C(25) C(24) C(26) 108.3(5) yes . . . C(25) C(24) C(27) 108.1(4) yes . . . C(26) C(24) C(27) 109.5(4) yes . . . C(10) C(28) C(29) 109.7(4) yes . . . C(10) C(28) C(30) 110.5(4) yes . . . C(10) C(28) C(31) 111.7(4) yes . . . C(29) C(28) C(30) 110.5(4) yes . . . C(29) C(28) C(31) 107.5(4) yes . . . C(30) C(28) C(31) 106.8(4) yes . . . C(12) C(32) C(33) 109.3(4) yes . . . C(12) C(32) C(34) 109.0(4) yes . . . C(12) C(32) C(35) 112.6(4) yes . . . C(33) C(32) C(34) 108.8(5) yes . . . C(33) C(32) C(35) 108.8(5) yes . . . C(34) C(32) C(35) 108.3(5) yes . . . C(16) C(36) C(37) 110.8(3) yes . . . C(16) C(36) C(38) 112.1(4) yes . . . C(16) C(36) C(39) 109.0(4) yes . . . C(37) C(36) C(38) 107.0(4) yes . . . C(37) C(36) C(39) 109.9(4) yes . . . C(38) C(36) C(39) 108.0(4) yes . . . C(18) C(40) C(41) 107.4(5) yes . . . C(18) C(40) C(42) 109.3(4) yes . . . C(18) C(40) C(43) 112.6(5) yes . . . C(18) C(40) C(123) 107.7(7) yes . . . C(18) C(40) C(124) 107.0(7) yes . . . C(18) C(40) C(125) 115.7(7) yes . . . C(41) C(40) C(42) 107.4(6) yes . . . C(41) C(40) C(43) 109.6(5) yes . . . C(41) C(40) C(123) 137.2(7) yes . . . C(41) C(40) C(124) 45.1(7) yes . . . C(41) C(40) C(125) 70.7(8) yes . . . C(42) C(40) C(43) 110.4(5) yes . . . C(42) C(40) C(123) 83.1(7) yes . . . C(42) C(40) C(124) 140.3(8) yes . . . C(42) C(40) C(125) 37.2(8) yes . . . C(43) C(40) C(123) 32.5(6) yes . . . C(43) C(40) C(124) 68.6(7) yes . . . C(43) C(40) C(125) 128.9(8) yes . . . C(123) C(40) C(124) 100.9(8) yes . . . C(123) C(40) C(125) 113.8(9) yes . . . C(124) C(40) C(125) 110.6(10) yes . . . C(40) C(41) C(124) 70.7(9) yes . . . C(40) C(41) C(125) 52.5(7) yes . . . C(124) C(41) C(125) 117.1(12) yes . . . C(40) C(43) C(124) 58.9(6) yes . . . C(45) C(44) C(52) 119.2(4) yes . . . C(45) C(44) C(57) 117.7(4) yes . . . C(52) C(44) C(57) 116.5(3) yes . . . C(44) C(45) C(46) 115.3(4) yes . . . C(44) C(45) C(50) 124.7(3) yes . . . C(46) C(45) C(50) 120.0(4) yes . . . O(4) C(46) C(45) 118.8(4) yes . . . O(4) C(46) C(47) 120.9(3) yes . . . C(45) C(46) C(47) 120.3(4) yes . . . C(46) C(47) C(48) 116.7(4) yes . . . C(46) C(47) C(63) 122.5(4) yes . . . C(48) C(47) C(63) 120.7(4) yes . . . C(47) C(48) C(49) 124.6(4) yes . . . C(48) C(49) C(50) 117.3(4) yes . . . C(48) C(49) C(67) 121.2(4) yes . . . C(50) C(49) C(67) 121.5(4) yes . . . C(45) C(50) C(49) 121.2(4) yes . . . O(5) C(51) C(52) 118.3(4) yes . . . O(5) C(51) C(56) 121.2(4) yes . . . C(52) C(51) C(56) 120.5(4) yes . . . C(44) C(52) C(51) 115.3(3) yes . . . C(44) C(52) C(53) 125.0(4) yes . . . C(51) C(52) C(53) 119.7(4) yes . . . C(52) C(53) C(54) 121.6(4) yes . . . C(53) C(54) C(55) 117.2(4) yes . . . C(53) C(54) C(75) 121.6(4) yes . . . C(55) C(54) C(75) 121.3(4) yes . . . C(54) C(55) C(56) 125.0(4) yes . . . C(51) C(56) C(55) 116.0(4) yes . . . C(51) C(56) C(71) 122.2(4) yes . . . C(55) C(56) C(71) 121.7(4) yes . . . C(44) C(57) C(58) 114.8(4) yes . . . C(44) C(57) C(62) 125.7(4) yes . . . C(58) C(57) C(62) 119.4(4) yes . . . O(6) C(58) C(57) 119.1(4) yes . . . O(6) C(58) C(59) 120.3(4) yes . . . C(57) C(58) C(59) 120.5(4) yes . . . C(58) C(59) C(60) 117.0(4) yes . . . C(58) C(59) C(79) 121.7(4) yes . . . C(60) C(59) C(79) 121.2(4) yes . . . C(59) C(60) C(61) 123.9(4) yes . . . C(60) C(61) C(62) 117.5(4) yes . . . C(60) C(61) C(83) 121.1(5) yes . . . C(62) C(61) C(83) 121.3(5) yes . . . C(57) C(62) C(61) 121.5(4) yes . . . C(47) C(63) C(64) 106.9(4) yes . . . C(47) C(63) C(65) 111.9(4) yes . . . C(47) C(63) C(66) 112.3(4) yes . . . C(64) C(63) C(65) 108.5(4) yes . . . C(64) C(63) C(66) 110.0(4) yes . . . C(65) C(63) C(66) 107.2(4) yes . . . C(49) C(67) C(68) 112.7(6) yes . . . C(49) C(67) C(69) 108.0(6) yes . . . C(49) C(67) C(70) 110.7(7) yes . . . C(49) C(67) C(126) 109.8(6) yes . . . C(49) C(67) C(127) 109.3(5) yes . . . C(49) C(67) C(128) 110.1(6) yes . . . C(68) C(67) C(69) 107.7(8) yes . . . C(68) C(67) C(70) 107.5(8) yes . . . C(68) C(67) C(126) 81.6(8) yes . . . C(68) C(67) C(127) 33.2(7) yes . . . C(68) C(67) C(128) 128.1(7) yes . . . C(69) C(67) C(70) 110.3(7) yes . . . C(69) C(67) C(126) 28.2(6) yes . . . C(69) C(67) C(127) 134.9(7) yes . . . C(69) C(67) C(128) 85.1(6) yes . . . C(70) C(67) C(126) 130.2(8) yes . . . C(70) C(67) C(127) 78.8(7) yes . . . C(70) C(67) C(128) 27.6(7) yes . . . C(126) C(67) C(127) 113.0(7) yes . . . C(126) C(67) C(128) 109.9(6) yes . . . C(127) C(67) C(128) 104.7(6) yes . . . C(56) C(71) C(72) 112.0(4) yes . . . C(56) C(71) C(73) 109.2(4) yes . . . C(56) C(71) C(74) 111.3(4) yes . . . C(72) C(71) C(73) 106.9(4) yes . . . C(72) C(71) C(74) 107.2(4) yes . . . C(73) C(71) C(74) 110.1(4) yes . . . C(54) C(75) C(76) 110.3(6) yes . . . C(54) C(75) C(77) 107.3(6) yes . . . C(54) C(75) C(78) 110.7(5) yes . . . C(54) C(75) C(129) 108.0(6) yes . . . C(54) C(75) C(130) 112.3(5) yes . . . C(54) C(75) C(131) 108.8(5) yes . . . C(76) C(75) C(77) 107.5(9) yes . . . C(76) C(75) C(78) 108.6(8) yes . . . C(76) C(75) C(129) 24.6(7) yes . . . C(76) C(75) C(130) 126.5(7) yes . . . C(76) C(75) C(131) 85.8(8) yes . . . C(77) C(75) C(78) 112.4(8) yes . . . C(77) C(75) C(129) 129.1(7) yes . . . C(77) C(75) C(130) 89.2(8) yes . . . C(77) C(75) C(131) 23.1(8) yes . . . C(78) C(75) C(129) 87.6(7) yes . . . C(78) C(75) C(130) 24.7(7) yes . . . C(78) C(75) C(131) 129.1(8) yes . . . C(129) C(75) C(130) 109.5(7) yes . . . C(129) C(75) C(131) 109.2(7) yes . . . C(130) C(75) C(131) 109.0(7) yes . . . C(59) C(79) C(80) 109.3(4) yes . . . C(59) C(79) C(81) 110.6(4) yes . . . C(59) C(79) C(82) 111.9(4) yes . . . C(80) C(79) C(81) 110.1(4) yes . . . C(80) C(79) C(82) 108.3(4) yes . . . C(81) C(79) C(82) 106.7(4) yes . . . C(61) C(83) C(84) 110.3(9) yes . . . C(61) C(83) C(85) 109.6(7) yes . . . C(61) C(83) C(86) 111.4(7) yes . . . C(61) C(83) C(87) 106.9(6) yes . . . C(61) C(83) C(88) 112.6(6) yes . . . C(61) C(83) C(89) 110.3(6) yes . . . C(84) C(83) C(85) 112.8(11) yes . . . C(84) C(83) C(86) 108.1(11) yes . . . C(84) C(83) C(87) 39.2(10) yes . . . C(84) C(83) C(88) 70.9(10) yes . . . C(84) C(83) C(89) 135.7(10) yes . . . C(85) C(83) C(86) 104.6(10) yes . . . C(85) C(83) C(87) 141.0(8) yes . . . C(85) C(83) C(88) 44.4(8) yes . . . C(85) C(83) C(89) 68.4(9) yes . . . C(86) C(83) C(87) 73.7(8) yes . . . C(86) C(83) C(88) 133.0(8) yes . . . C(86) C(83) C(89) 39.0(9) yes . . . C(87) C(83) C(88) 107.9(7) yes . . . C(87) C(83) C(89) 110.8(9) yes . . . C(88) C(83) C(89) 108.3(9) yes . . . C(83) C(84) C(88) 55.2(9) yes . . . C(83) C(85) C(88) 67.7(11) yes . . . C(83) C(85) C(89) 55.8(8) yes . . . C(88) C(85) C(89) 117.7(15) yes . . . C(83) C(86) C(87) 53.1(7) yes . . . C(83) C(87) C(86) 53.2(7) yes . . . C(83) C(88) C(84) 53.9(8) yes . . . C(83) C(88) C(85) 67.9(11) yes . . . C(84) C(88) C(85) 118.8(15) yes . . . C(83) C(89) C(85) 55.8(8) yes . . . N(1) C(90) C(91) 114.4(4) yes . . . N(1) C(92) C(93) 111.9(5) yes . . . N(1) C(94) C(95) 113.1(4) yes . . . N(2) C(96) C(97) 114.1(5) yes . . . N(2) C(98) C(99) 114.5(6) yes . . . N(2) C(100) C(101) 113.3(6) yes . . . C(103) C(102) C(107) 121.6(7) yes . . . C(102) C(103) C(104) 122.2(9) yes . . . C(103) C(104) C(105) 120.0(11) yes . . . C(104) C(105) C(106) 121.8(8) yes . . . C(105) C(106) C(107) 116.9(9) yes . . . C(102) C(107) C(106) 117.3(9) yes . . . C(109) C(108) C(113) 119.7(6) yes . . . C(108) C(109) C(110) 120.2(6) yes . . . C(109) C(110) C(111) 120.5(6) yes . . . C(110) C(111) C(112) 120.8(6) yes . . . C(111) C(112) C(113) 119.5(7) yes . . . C(108) C(113) C(112) 119.3(7) yes . . . C(115) C(114) C(119) 117.9(9) yes . . . C(114) C(115) C(116) 117.5(8) yes . . . C(115) C(116) C(117) 123.7(8) yes . . . C(116) C(117) C(118) 119.3(10) yes . . . C(117) C(118) C(119) 122.3(9) yes . . . C(114) C(119) C(118) 119.1(9) yes . . . C(121) C(120) C(122) 117.7(19) yes . . 2_576 C(121) C(120) C(134) 85(3) yes . . . C(122) C(120) C(134) 59(3) yes 2_576 . . C(120) C(121) C(122) 117.6(17) yes . . . C(120) C(121) C(134) 35.9(15) yes . . . C(122) C(121) C(134) 102.6(18) yes . . . C(120) C(122) C(121) 121.0(19) yes 2_576 . . C(120) C(122) C(134) 51(2) yes 2_576 . 2_576 C(121) C(122) C(134) 107(3) yes . . 2_576 C(40) C(124) C(41) 64.2(8) yes . . . C(40) C(124) C(43) 52.5(6) yes . . . C(41) C(124) C(43) 112.2(11) yes . . . C(40) C(125) C(41) 56.9(7) yes . . . C(133) C(132) C(134) 115(3) yes . . 2_576 C(132) C(133) C(134) 117(3) yes . . . C(120) C(134) C(121) 59(2) yes . . . C(120) C(134) C(122) 70(3) yes . . 2_576 C(120) C(134) C(132) 106(3) yes . . 2_576 C(120) C(134) C(133) 39(2) yes . . . C(121) C(134) C(122) 108(3) yes . . 2_576 C(121) C(134) C(132) 111(2) yes . . 2_576 C(121) C(134) C(133) 22.2(14) yes . . . C(122) C(134) C(132) 41.4(17) yes 2_576 . 2_576 C(122) C(134) C(133) 101(3) yes 2_576 . . C(132) C(134) C(133) 120(3) yes 2_576 . . C(90) N(1) H(1A) 106.651 no . . . C(92) N(1) H(1A) 106.657 no . . . C(94) N(1) H(1A) 106.651 no . . . C(96) N(2) H(2A) 106.404 no . . . C(98) N(2) H(2A) 106.403 no . . . C(100) N(2) H(2A) 106.413 no . . . C(2) C(1) H(1) 98.873 no . . . C(8) C(1) H(1) 98.876 no . . . C(14) C(1) H(1) 98.873 no . . . C(4) C(5) H(5) 118.158 no . . . C(6) C(5) H(5) 118.173 no . . . C(2) C(7) H(7) 118.883 no . . . C(6) C(7) H(7) 118.864 no . . . C(10) C(11) H(11) 117.912 no . . . C(12) C(11) H(11) 117.896 no . . . C(8) C(13) H(13) 119.451 no . . . C(12) C(13) H(13) 119.447 no . . . C(16) C(17) H(17) 117.866 no . . . C(18) C(17) H(17) 117.870 no . . . C(14) C(19) H(19) 119.424 no . . . C(18) C(19) H(19) 119.428 no . . . C(20) C(21) H(21A) 109.479 no . . . C(20) C(21) H(21B) 109.464 no . . . C(20) C(21) H(21C) 109.482 no . . . H(21A) C(21) H(21B) 109.458 no . . . H(21A) C(21) H(21C) 109.474 no . . . H(21B) C(21) H(21C) 109.471 no . . . C(20) C(22) H(22A) 109.469 no . . . C(20) C(22) H(22B) 109.480 no . . . C(20) C(22) H(22C) 109.468 no . . . H(22A) C(22) H(22B) 109.488 no . . . H(22A) C(22) H(22C) 109.459 no . . . H(22B) C(22) H(22C) 109.463 no . . . C(20) C(23) H(23A) 109.470 no . . . C(20) C(23) H(23B) 109.471 no . . . C(20) C(23) H(23C) 109.469 no . . . H(23A) C(23) H(23B) 109.468 no . . . H(23A) C(23) H(23C) 109.467 no . . . H(23B) C(23) H(23C) 109.483 no . . . C(24) C(25) H(25A) 109.469 no . . . C(24) C(25) H(25B) 109.468 no . . . C(24) C(25) H(25C) 109.471 no . . . H(25A) C(25) H(25B) 109.476 no . . . H(25A) C(25) H(25C) 109.472 no . . . H(25B) C(25) H(25C) 109.472 no . . . C(24) C(26) H(26A) 109.474 no . . . C(24) C(26) H(26B) 109.472 no . . . C(24) C(26) H(26C) 109.471 no . . . H(26A) C(26) H(26B) 109.479 no . . . H(26A) C(26) H(26C) 109.465 no . . . H(26B) C(26) H(26C) 109.466 no . . . C(24) C(27) H(27A) 109.485 no . . . C(24) C(27) H(27B) 109.468 no . . . C(24) C(27) H(27C) 109.478 no . . . H(27A) C(27) H(27B) 109.464 no . . . H(27A) C(27) H(27C) 109.473 no . . . H(27B) C(27) H(27C) 109.459 no . . . C(28) C(29) H(29A) 109.472 no . . . C(28) C(29) H(29B) 109.474 no . . . C(28) C(29) H(29C) 109.465 no . . . H(29A) C(29) H(29B) 109.482 no . . . H(29A) C(29) H(29C) 109.464 no . . . H(29B) C(29) H(29C) 109.471 no . . . C(28) C(30) H(30A) 109.464 no . . . C(28) C(30) H(30B) 109.468 no . . . C(28) C(30) H(30C) 109.479 no . . . H(30A) C(30) H(30B) 109.470 no . . . H(30A) C(30) H(30C) 109.475 no . . . H(30B) C(30) H(30C) 109.472 no . . . C(28) C(31) H(31A) 109.470 no . . . C(28) C(31) H(31B) 109.476 no . . . C(28) C(31) H(31C) 109.468 no . . . H(31A) C(31) H(31B) 109.469 no . . . H(31A) C(31) H(31C) 109.473 no . . . H(31B) C(31) H(31C) 109.471 no . . . C(32) C(33) H(33A) 109.471 no . . . C(32) C(33) H(33B) 109.482 no . . . C(32) C(33) H(33C) 109.474 no . . . H(33A) C(33) H(33B) 109.466 no . . . H(33A) C(33) H(33C) 109.462 no . . . H(33B) C(33) H(33C) 109.472 no . . . C(32) C(34) H(34A) 109.471 no . . . C(32) C(34) H(34B) 109.466 no . . . C(32) C(34) H(34C) 109.464 no . . . H(34A) C(34) H(34B) 109.471 no . . . H(34A) C(34) H(34C) 109.471 no . . . H(34B) C(34) H(34C) 109.485 no . . . C(32) C(35) H(35A) 109.469 no . . . C(32) C(35) H(35B) 109.475 no . . . C(32) C(35) H(35C) 109.468 no . . . H(35A) C(35) H(35B) 109.479 no . . . H(35A) C(35) H(35C) 109.471 no . . . H(35B) C(35) H(35C) 109.465 no . . . C(36) C(37) H(37A) 109.472 no . . . C(36) C(37) H(37B) 109.476 no . . . C(36) C(37) H(37C) 109.469 no . . . H(37A) C(37) H(37B) 109.467 no . . . H(37A) C(37) H(37C) 109.464 no . . . H(37B) C(37) H(37C) 109.480 no . . . C(36) C(38) H(38A) 109.486 no . . . C(36) C(38) H(38B) 109.472 no . . . C(36) C(38) H(38C) 109.476 no . . . H(38A) C(38) H(38B) 109.469 no . . . H(38A) C(38) H(38C) 109.464 no . . . H(38B) C(38) H(38C) 109.460 no . . . C(36) C(39) H(39A) 109.472 no . . . C(36) C(39) H(39B) 109.465 no . . . C(36) C(39) H(39C) 109.477 no . . . H(39A) C(39) H(39B) 109.468 no . . . H(39A) C(39) H(39C) 109.473 no . . . H(39B) C(39) H(39C) 109.471 no . . . C(45) C(44) H(44) 98.616 no . . . C(52) C(44) H(44) 98.607 no . . . C(57) C(44) H(44) 98.608 no . . . C(47) C(48) H(48) 117.713 no . . . C(49) C(48) H(48) 117.692 no . . . C(45) C(50) H(50) 119.418 no . . . C(49) C(50) H(50) 119.412 no . . . C(52) C(53) H(53) 119.187 no . . . C(54) C(53) H(53) 119.178 no . . . C(54) C(55) H(55) 117.508 no . . . C(56) C(55) H(55) 117.517 no . . . C(59) C(60) H(60) 118.071 no . . . C(61) C(60) H(60) 118.065 no . . . C(57) C(62) H(62) 119.261 no . . . C(61) C(62) H(62) 119.254 no . . . C(63) C(64) H(64A) 109.473 no . . . C(63) C(64) H(64B) 109.481 no . . . C(63) C(64) H(64C) 109.470 no . . . H(64A) C(64) H(64B) 109.473 no . . . H(64A) C(64) H(64C) 109.468 no . . . H(64B) C(64) H(64C) 109.462 no . . . C(63) C(65) H(65A) 109.468 no . . . C(63) C(65) H(65B) 109.477 no . . . C(63) C(65) H(65C) 109.471 no . . . H(65A) C(65) H(65B) 109.478 no . . . H(65A) C(65) H(65C) 109.469 no . . . H(65B) C(65) H(65C) 109.465 no . . . C(63) C(66) H(66A) 109.467 no . . . C(63) C(66) H(66B) 109.465 no . . . C(63) C(66) H(66C) 109.476 no . . . H(66A) C(66) H(66B) 109.468 no . . . H(66A) C(66) H(66C) 109.477 no . . . H(66B) C(66) H(66C) 109.474 no . . . C(71) C(72) H(72A) 109.478 no . . . C(71) C(72) H(72B) 109.478 no . . . C(71) C(72) H(72C) 109.474 no . . . H(72A) C(72) H(72B) 109.461 no . . . H(72A) C(72) H(72C) 109.466 no . . . H(72B) C(72) H(72C) 109.470 no . . . C(71) C(73) H(73A) 109.473 no . . . C(71) C(73) H(73B) 109.462 no . . . C(71) C(73) H(73C) 109.460 no . . . H(73A) C(73) H(73B) 109.472 no . . . H(73A) C(73) H(73C) 109.485 no . . . H(73B) C(73) H(73C) 109.476 no . . . C(71) C(74) H(74A) 109.470 no . . . C(71) C(74) H(74B) 109.482 no . . . C(71) C(74) H(74C) 109.471 no . . . H(74A) C(74) H(74B) 109.468 no . . . H(74A) C(74) H(74C) 109.467 no . . . H(74B) C(74) H(74C) 109.469 no . . . C(79) C(80) H(80A) 109.476 no . . . C(79) C(80) H(80B) 109.471 no . . . C(79) C(80) H(80C) 109.464 no . . . H(80A) C(80) H(80B) 109.480 no . . . H(80A) C(80) H(80C) 109.460 no . . . H(80B) C(80) H(80C) 109.476 no . . . C(79) C(81) H(81A) 109.474 no . . . C(79) C(81) H(81B) 109.476 no . . . C(79) C(81) H(81C) 109.477 no . . . H(81A) C(81) H(81B) 109.471 no . . . H(81A) C(81) H(81C) 109.464 no . . . H(81B) C(81) H(81C) 109.466 no . . . C(79) C(82) H(82A) 109.467 no . . . C(79) C(82) H(82B) 109.475 no . . . C(79) C(82) H(82C) 109.463 no . . . H(82A) C(82) H(82B) 109.477 no . . . H(82A) C(82) H(82C) 109.476 no . . . H(82B) C(82) H(82C) 109.470 no . . . N(1) C(90) H(90A) 108.663 no . . . N(1) C(90) H(90B) 108.669 no . . . C(91) C(90) H(90A) 108.657 no . . . C(91) C(90) H(90B) 108.676 no . . . H(90A) C(90) H(90B) 107.609 no . . . C(90) C(91) H(91A) 109.477 no . . . C(90) C(91) H(91B) 109.469 no . . . C(90) C(91) H(91C) 109.463 no . . . H(91A) C(91) H(91B) 109.471 no . . . H(91A) C(91) H(91C) 109.478 no . . . H(91B) C(91) H(91C) 109.469 no . . . N(1) C(92) H(92A) 109.230 no . . . N(1) C(92) H(92B) 109.250 no . . . C(93) C(92) H(92A) 109.236 no . . . C(93) C(92) H(92B) 109.238 no . . . H(92A) C(92) H(92B) 107.921 no . . . C(92) C(93) H(93A) 109.476 no . . . C(92) C(93) H(93B) 109.468 no . . . C(92) C(93) H(93C) 109.465 no . . . H(93A) C(93) H(93B) 109.481 no . . . H(93A) C(93) H(93C) 109.478 no . . . H(93B) C(93) H(93C) 109.460 no . . . N(1) C(94) H(94A) 108.958 no . . . N(1) C(94) H(94B) 108.962 no . . . C(95) C(94) H(94A) 108.959 no . . . C(95) C(94) H(94B) 108.959 no . . . H(94A) C(94) H(94B) 107.760 no . . . C(94) C(95) H(95A) 109.473 no . . . C(94) C(95) H(95B) 109.478 no . . . C(94) C(95) H(95C) 109.468 no . . . H(95A) C(95) H(95B) 109.473 no . . . H(95A) C(95) H(95C) 109.471 no . . . H(95B) C(95) H(95C) 109.464 no . . . N(2) C(96) H(96A) 108.727 no . . . N(2) C(96) H(96B) 108.726 no . . . C(97) C(96) H(96A) 108.740 no . . . C(97) C(96) H(96B) 108.742 no . . . H(96A) C(96) H(96B) 107.631 no . . . C(96) C(97) H(97A) 109.463 no . . . C(96) C(97) H(97B) 109.475 no . . . C(96) C(97) H(97C) 109.466 no . . . H(97A) C(97) H(97B) 109.472 no . . . H(97A) C(97) H(97C) 109.478 no . . . H(97B) C(97) H(97C) 109.473 no . . . N(2) C(98) H(98A) 108.621 no . . . N(2) C(98) H(98B) 108.631 no . . . C(99) C(98) H(98A) 108.629 no . . . C(99) C(98) H(98B) 108.627 no . . . H(98A) C(98) H(98B) 107.570 no . . . C(98) C(99) H(99A) 109.476 no . . . C(98) C(99) H(99B) 109.479 no . . . C(98) C(99) H(99C) 109.476 no . . . H(99A) C(99) H(99B) 109.469 no . . . H(99A) C(99) H(99C) 109.464 no . . . H(99B) C(99) H(99C) 109.463 no . . . N(2) C(100) H(10A) 108.918 no . . . N(2) C(100) H(10B) 108.927 no . . . C(101) C(100) H(10A) 108.913 no . . . C(101) C(100) H(10B) 108.925 no . . . H(10A) C(100) H(10B) 107.749 no . . . C(100) C(101) H(10C) 109.464 no . . . C(100) C(101) H(10D) 109.480 no . . . C(100) C(101) H(10E) 109.466 no . . . H(10C) C(101) H(10D) 109.481 no . . . H(10C) C(101) H(10E) 109.468 no . . . H(10D) C(101) H(10E) 109.467 no . . . C(103) C(102) H(102) 119.187 no . . . C(107) C(102) H(102) 119.174 no . . . C(102) C(103) H(103) 118.883 no . . . C(104) C(103) H(103) 118.894 no . . . C(103) C(104) H(104) 119.988 no . . . C(105) C(104) H(104) 119.975 no . . . C(104) C(105) H(105) 119.108 no . . . C(106) C(105) H(105) 119.124 no . . . C(105) C(106) H(106) 121.548 no . . . C(107) C(106) H(106) 121.541 no . . . C(102) C(107) H(107) 121.325 no . . . C(106) C(107) H(107) 121.340 no . . . C(109) C(108) H(108) 120.158 no . . . C(113) C(108) H(108) 120.176 no . . . C(108) C(109) H(109) 119.900 no . . . C(110) C(109) H(109) 119.905 no . . . C(109) C(110) H(110) 119.744 no . . . C(111) C(110) H(110) 119.747 no . . . C(110) C(111) H(111) 119.585 no . . . C(112) C(111) H(111) 119.580 no . . . C(111) C(112) H(112) 120.249 no . . . C(113) C(112) H(112) 120.273 no . . . C(108) C(113) H(113) 120.348 no . . . C(112) C(113) H(113) 120.338 no . . . C(115) C(114) H(114) 121.032 no . . . C(119) C(114) H(114) 121.041 no . . . C(114) C(115) H(115) 121.264 no . . . C(116) C(115) H(115) 121.247 no . . . C(115) C(116) H(116) 118.163 no . . . C(117) C(116) H(116) 118.173 no . . . C(116) C(117) H(117) 120.348 no . . . C(118) C(117) H(117) 120.339 no . . . C(117) C(118) H(118) 118.872 no . . . C(119) C(118) H(118) 118.867 no . . . C(114) C(119) H(119) 120.424 no . . . C(118) C(119) H(119) 120.427 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Nb(1) O(2) C(9) 150.3(4) no . . . . Cl(1) Nb(1) O(3) C(15) -128.1(4) no . . . . Cl(2) Nb(1) O(1) C(3) -123.8(3) no . . . . Cl(2) Nb(1) O(3) C(15) 147.0(4) no . . . . Cl(3) Nb(1) O(1) C(3) 147.1(3) no . . . . Cl(3) Nb(1) O(2) C(9) -123.9(4) no . . . . O(1) Nb(1) O(2) C(9) -37.9(4) no . . . . O(2) Nb(1) O(1) C(3) 57.0(3) no . . . . O(1) Nb(1) O(3) C(15) 60.0(4) no . . . . O(3) Nb(1) O(1) C(3) -38.1(3) no . . . . O(2) Nb(1) O(3) C(15) -37.4(4) no . . . . O(3) Nb(1) O(2) C(9) 59.2(4) no . . . . Cl(4) Nb(2) O(5) C(51) -137.2(4) no . . . . Cl(4) Nb(2) O(6) C(58) 130.3(4) no . . . . Cl(5) Nb(2) O(4) C(46) 134.3(4) no . . . . Cl(5) Nb(2) O(6) C(58) -142.4(4) no . . . . Cl(6) Nb(2) O(4) C(46) -139.9(4) no . . . . Cl(6) Nb(2) O(5) C(51) 134.3(4) no . . . . O(4) Nb(2) O(5) C(51) 47.6(4) no . . . . O(5) Nb(2) O(4) C(46) -52.0(4) no . . . . O(4) Nb(2) O(6) C(58) -54.8(4) no . . . . O(6) Nb(2) O(4) C(46) 45.1(4) no . . . . O(5) Nb(2) O(6) C(58) 41.3(4) no . . . . O(6) Nb(2) O(5) C(51) -46.7(4) no . . . . Nb(1) O(1) C(3) C(2) -8.7(6) no . . . . Nb(1) O(1) C(3) C(4) 172.7(3) no . . . . Nb(1) O(2) C(9) C(8) -7.6(7) no . . . . Nb(1) O(2) C(9) C(10) 173.2(3) no . . . . Nb(1) O(3) C(15) C(14) -13.6(6) no . . . . Nb(1) O(3) C(15) C(16) 166.2(3) no . . . . Nb(2) O(4) C(46) C(45) 5.7(7) no . . . . Nb(2) O(4) C(46) C(47) -173.5(3) no . . . . Nb(2) O(5) C(51) C(52) -0.5(7) no . . . . Nb(2) O(5) C(51) C(56) 178.4(3) no . . . . Nb(2) O(6) C(58) C(57) 4.2(7) no . . . . Nb(2) O(6) C(58) C(59) -173.6(3) no . . . . C(90) N(1) C(92) C(93) -159.0(3) no . . . . C(92) N(1) C(90) C(91) -64.5(5) no . . . . C(90) N(1) C(94) C(95) 55.5(5) no . . . . C(94) N(1) C(90) C(91) 62.0(5) no . . . . C(92) N(1) C(94) C(95) -177.7(4) no . . . . C(94) N(1) C(92) C(93) 72.8(5) no . . . . C(96) N(2) C(98) C(99) 58.2(6) no . . . . C(98) N(2) C(96) C(97) 66.3(6) no . . . . C(96) N(2) C(100) C(101) -50.6(5) no . . . . C(100) N(2) C(96) C(97) -59.8(6) no . . . . C(98) N(2) C(100) C(101) -179.3(4) no . . . . C(100) N(2) C(98) C(99) -173.2(4) no . . . . C(2) C(1) C(8) C(9) 112.8(4) no . . . . C(2) C(1) C(8) C(13) -69.6(5) no . . . . C(8) C(1) C(2) C(3) -98.9(4) no . . . . C(8) C(1) C(2) C(7) 80.3(5) no . . . . C(2) C(1) C(14) C(15) -101.1(4) no . . . . C(2) C(1) C(14) C(19) 83.3(4) no . . . . C(14) C(1) C(2) C(3) 111.7(4) no . . . . C(14) C(1) C(2) C(7) -69.1(4) no . . . . C(8) C(1) C(14) C(15) 108.5(4) no . . . . C(8) C(1) C(14) C(19) -67.1(5) no . . . . C(14) C(1) C(8) C(9) -96.8(4) no . . . . C(14) C(1) C(8) C(13) 80.8(5) no . . . . C(1) C(2) C(3) O(1) -3.2(5) no . . . . C(1) C(2) C(3) C(4) 175.4(3) no . . . . C(1) C(2) C(7) C(6) -177.6(3) no . . . . C(3) C(2) C(7) C(6) 1.5(5) no . . . . C(7) C(2) C(3) O(1) 177.6(3) no . . . . C(7) C(2) C(3) C(4) -3.8(5) no . . . . O(1) C(3) C(4) C(5) -177.5(3) no . . . . O(1) C(3) C(4) C(20) 6.6(5) no . . . . C(2) C(3) C(4) C(5) 3.9(5) no . . . . C(2) C(3) C(4) C(20) -172.0(3) no . . . . C(3) C(4) C(5) C(6) -2.0(5) no . . . . C(3) C(4) C(20) C(21) 179.4(3) no . . . . C(3) C(4) C(20) C(22) -61.1(4) no . . . . C(3) C(4) C(20) C(23) 59.9(4) no . . . . C(5) C(4) C(20) C(21) 3.6(5) no . . . . C(5) C(4) C(20) C(22) 123.1(4) no . . . . C(5) C(4) C(20) C(23) -115.9(4) no . . . . C(20) C(4) C(5) C(6) 174.0(3) no . . . . C(4) C(5) C(6) C(7) -0.2(5) no . . . . C(4) C(5) C(6) C(24) -178.0(3) no . . . . C(5) C(6) C(7) C(2) 0.5(5) no . . . . C(5) C(6) C(24) C(25) -10.2(5) no . . . . C(5) C(6) C(24) C(26) 109.5(4) no . . . . C(5) C(6) C(24) C(27) -130.7(4) no . . . . C(7) C(6) C(24) C(25) 172.1(3) no . . . . C(7) C(6) C(24) C(26) -68.2(5) no . . . . C(7) C(6) C(24) C(27) 51.6(4) no . . . . C(24) C(6) C(7) C(2) 178.3(3) no . . . . C(1) C(8) C(9) O(2) -4.6(5) no . . . . C(1) C(8) C(9) C(10) 174.5(3) no . . . . C(1) C(8) C(13) C(12) -176.6(4) no . . . . C(9) C(8) C(13) C(12) 1.0(6) no . . . . C(13) C(8) C(9) O(2) 177.7(4) no . . . . C(13) C(8) C(9) C(10) -3.2(6) no . . . . O(2) C(9) C(10) C(11) -177.5(3) no . . . . O(2) C(9) C(10) C(28) 3.6(6) no . . . . C(8) C(9) C(10) C(11) 3.4(6) no . . . . C(8) C(9) C(10) C(28) -175.5(4) no . . . . C(9) C(10) C(11) C(12) -1.5(6) no . . . . C(9) C(10) C(28) C(29) 58.6(5) no . . . . C(9) C(10) C(28) C(30) -63.5(5) no . . . . C(9) C(10) C(28) C(31) 177.7(4) no . . . . C(11) C(10) C(28) C(29) -120.2(4) no . . . . C(11) C(10) C(28) C(30) 117.7(4) no . . . . C(11) C(10) C(28) C(31) -1.1(6) no . . . . C(28) C(10) C(11) C(12) 177.4(4) no . . . . C(10) C(11) C(12) C(13) -0.7(7) no . . . . C(10) C(11) C(12) C(32) -179.2(4) no . . . . C(11) C(12) C(13) C(8) 0.9(6) no . . . . C(11) C(12) C(32) C(33) -61.8(5) no . . . . C(11) C(12) C(32) C(34) 57.0(5) no . . . . C(11) C(12) C(32) C(35) 177.2(4) no . . . . C(13) C(12) C(32) C(33) 119.8(4) no . . . . C(13) C(12) C(32) C(34) -121.5(4) no . . . . C(13) C(12) C(32) C(35) -1.3(6) no . . . . C(32) C(12) C(13) C(8) 179.5(4) no . . . . C(1) C(14) C(15) O(3) -0.3(5) no . . . . C(1) C(14) C(15) C(16) 179.9(3) no . . . . C(1) C(14) C(19) C(18) 176.6(3) no . . . . C(15) C(14) C(19) C(18) 1.2(5) no . . . . C(19) C(14) C(15) O(3) 175.5(3) no . . . . C(19) C(14) C(15) C(16) -4.3(5) no . . . . O(3) C(15) C(16) C(17) -175.7(3) no . . . . O(3) C(15) C(16) C(36) 4.5(5) no . . . . C(14) C(15) C(16) C(17) 4.1(5) no . . . . C(14) C(15) C(16) C(36) -175.7(3) no . . . . C(15) C(16) C(17) C(18) -0.9(6) no . . . . C(15) C(16) C(36) C(37) -61.1(5) no . . . . C(15) C(16) C(36) C(38) 179.5(3) no . . . . C(15) C(16) C(36) C(39) 60.0(5) no . . . . C(17) C(16) C(36) C(37) 119.2(4) no . . . . C(17) C(16) C(36) C(38) -0.3(5) no . . . . C(17) C(16) C(36) C(39) -119.8(4) no . . . . C(36) C(16) C(17) C(18) 178.8(4) no . . . . C(16) C(17) C(18) C(19) -2.0(6) no . . . . C(16) C(17) C(18) C(40) 176.4(3) no . . . . C(17) C(18) C(19) C(14) 1.9(5) no . . . . C(17) C(18) C(40) C(41) -77.9(4) no . . . . C(17) C(18) C(40) C(42) 38.3(5) no . . . . C(17) C(18) C(40) C(43) 161.4(3) no . . . . C(17) C(18) C(40) C(123) 127.1(4) no . . . . C(17) C(18) C(40) C(124) -125.2(4) no . . . . C(17) C(18) C(40) C(125) -1.5(6) no . . . . C(19) C(18) C(40) C(41) 100.5(4) no . . . . C(19) C(18) C(40) C(42) -143.3(4) no . . . . C(19) C(18) C(40) C(43) -20.2(5) no . . . . C(19) C(18) C(40) C(123) -54.5(4) no . . . . C(19) C(18) C(40) C(124) 53.2(5) no . . . . C(19) C(18) C(40) C(125) 176.9(3) no . . . . C(40) C(18) C(19) C(14) -176.6(3) no . . . . C(18) C(40) C(41) C(124) -96.9(4) no . . . . C(18) C(40) C(41) C(125) 111.9(4) no . . . . C(18) C(40) C(43) C(124) 100.2(4) no . . . . C(18) C(40) C(124) C(41) 97.8(7) no . . . . C(18) C(40) C(124) C(43) -108.2(5) no . . . . C(18) C(40) C(125) C(41) -100.5(5) no . . . . C(42) C(40) C(41) C(124) 145.7(5) no . . . . C(42) C(40) C(41) C(125) -5.6(4) no . . . . C(41) C(40) C(43) C(124) -19.2(5) no . . . . C(43) C(40) C(41) C(124) 25.7(6) no . . . . C(43) C(40) C(41) C(125) -125.6(5) no . . . . C(123) C(40) C(41) C(124) 46.8(11) no . . . . C(123) C(40) C(41) C(125) -104.5(10) no . . . . C(41) C(40) C(124) C(43) 154.0(10) no . . . . C(124) C(40) C(41) C(125) -151.2(10) no . . . . C(125) C(40) C(41) C(124) 151.2(9) no . . . . C(42) C(40) C(43) C(124) -137.3(5) no . . . . C(42) C(40) C(124) C(41) -57.4(14) no . . . . C(42) C(40) C(124) C(43) 96.6(11) no . . . . C(42) C(40) C(125) C(41) 171.2(12) no . . . . C(123) C(40) C(43) C(124) -172.2(13) no . . . . C(43) C(40) C(124) C(41) -154.0(9) no . . . . C(43) C(40) C(125) C(41) 100.0(8) no . . . . C(125) C(40) C(43) C(124) -99.7(10) no . . . . C(123) C(40) C(124) C(41) -149.7(8) no . . . . C(123) C(40) C(124) C(43) 4.3(7) no . . . . C(123) C(40) C(125) C(41) 134.0(7) no . . . . C(124) C(40) C(125) C(41) 21.3(8) no . . . . C(125) C(40) C(124) C(41) -29.0(11) no . . . . C(125) C(40) C(124) C(43) 125.0(9) no . . . . C(40) C(41) C(124) C(43) -22.1(8) no . . . . C(124) C(41) C(125) C(40) -30.7(12) no . . . . C(125) C(41) C(124) C(40) 25.4(10) no . . . . C(125) C(41) C(124) C(43) 3.3(16) no . . . . C(40) C(43) C(124) C(41) 25.2(9) no . . . . C(45) C(44) C(52) C(51) -106.1(4) no . . . . C(45) C(44) C(52) C(53) 76.3(5) no . . . . C(52) C(44) C(45) C(46) 104.8(4) no . . . . C(52) C(44) C(45) C(50) -78.1(5) no . . . . C(45) C(44) C(57) C(58) 100.3(4) no . . . . C(45) C(44) C(57) C(62) -82.9(4) no . . . . C(57) C(44) C(45) C(46) -104.6(4) no . . . . C(57) C(44) C(45) C(50) 72.5(5) no . . . . C(52) C(44) C(57) C(58) -108.4(4) no . . . . C(52) C(44) C(57) C(62) 68.4(5) no . . . . C(57) C(44) C(52) C(51) 103.1(4) no . . . . C(57) C(44) C(52) C(53) -74.6(5) no . . . . C(44) C(45) C(46) O(4) -1.5(5) no . . . . C(44) C(45) C(46) C(47) 177.6(3) no . . . . C(44) C(45) C(50) C(49) -177.8(3) no . . . . C(46) C(45) C(50) C(49) -0.9(6) no . . . . C(50) C(45) C(46) O(4) -178.8(4) no . . . . C(50) C(45) C(46) C(47) 0.4(6) no . . . . O(4) C(46) C(47) C(48) 179.8(3) no . . . . O(4) C(46) C(47) C(63) 4.4(6) no . . . . C(45) C(46) C(47) C(48) 0.7(6) no . . . . C(45) C(46) C(47) C(63) -174.7(3) no . . . . C(46) C(47) C(48) C(49) -1.3(6) no . . . . C(46) C(47) C(63) C(64) 68.4(5) no . . . . C(46) C(47) C(63) C(65) -173.0(4) no . . . . C(46) C(47) C(63) C(66) -52.4(5) no . . . . C(48) C(47) C(63) C(64) -106.9(4) no . . . . C(48) C(47) C(63) C(65) 11.7(5) no . . . . C(48) C(47) C(63) C(66) 132.4(4) no . . . . C(63) C(47) C(48) C(49) 174.2(4) no . . . . C(47) C(48) C(49) C(50) 0.9(6) no . . . . C(47) C(48) C(49) C(67) -178.5(4) no . . . . C(48) C(49) C(50) C(45) 0.3(6) no . . . . C(48) C(49) C(67) C(68) 16.7(6) no . . . . C(48) C(49) C(67) C(69) -102.1(4) no . . . . C(48) C(49) C(67) C(70) 137.1(4) no . . . . C(48) C(49) C(67) C(126) -72.3(5) no . . . . C(48) C(49) C(67) C(127) 52.1(5) no . . . . C(48) C(49) C(67) C(128) 166.6(4) no . . . . C(50) C(49) C(67) C(68) -162.6(4) no . . . . C(50) C(49) C(67) C(69) 78.6(5) no . . . . C(50) C(49) C(67) C(70) -42.2(5) no . . . . C(50) C(49) C(67) C(126) 108.4(4) no . . . . C(50) C(49) C(67) C(127) -127.2(4) no . . . . C(50) C(49) C(67) C(128) -12.7(5) no . . . . C(67) C(49) C(50) C(45) 179.6(4) no . . . . O(5) C(51) C(52) C(44) 1.1(5) no . . . . O(5) C(51) C(52) C(53) 178.8(3) no . . . . O(5) C(51) C(56) C(55) -179.8(3) no . . . . O(5) C(51) C(56) C(71) -2.0(6) no . . . . C(52) C(51) C(56) C(55) -0.9(6) no . . . . C(52) C(51) C(56) C(71) 176.9(3) no . . . . C(56) C(51) C(52) C(44) -177.9(3) no . . . . C(56) C(51) C(52) C(53) -0.1(6) no . . . . C(44) C(52) C(53) C(54) 177.4(4) no . . . . C(51) C(52) C(53) C(54) -0.2(6) no . . . . C(52) C(53) C(54) C(55) 1.5(6) no . . . . C(52) C(53) C(54) C(75) -178.3(4) no . . . . C(53) C(54) C(55) C(56) -2.7(7) no . . . . C(53) C(54) C(75) C(76) 153.4(4) no . . . . C(53) C(54) C(75) C(77) -89.8(5) no . . . . C(53) C(54) C(75) C(78) 33.2(6) no . . . . C(53) C(54) C(75) C(129) 127.5(4) no . . . . C(53) C(54) C(75) C(130) 6.7(6) no . . . . C(53) C(54) C(75) C(131) -114.1(5) no . . . . C(55) C(54) C(75) C(76) -26.4(6) no . . . . C(55) C(54) C(75) C(77) 90.4(5) no . . . . C(55) C(54) C(75) C(78) -146.6(4) no . . . . C(55) C(54) C(75) C(129) -52.3(6) no . . . . C(55) C(54) C(75) C(130) -173.1(4) no . . . . C(55) C(54) C(75) C(131) 66.1(5) no . . . . C(75) C(54) C(55) C(56) 177.1(4) no . . . . C(54) C(55) C(56) C(51) 2.4(6) no . . . . C(54) C(55) C(56) C(71) -175.4(4) no . . . . C(51) C(56) C(71) C(72) 179.3(4) no . . . . C(51) C(56) C(71) C(73) -62.5(5) no . . . . C(51) C(56) C(71) C(74) 59.3(5) no . . . . C(55) C(56) C(71) C(72) -3.0(6) no . . . . C(55) C(56) C(71) C(73) 115.1(4) no . . . . C(55) C(56) C(71) C(74) -123.0(4) no . . . . C(44) C(57) C(58) O(6) 3.0(5) no . . . . C(44) C(57) C(58) C(59) -179.2(3) no . . . . C(44) C(57) C(62) C(61) -176.3(4) no . . . . C(58) C(57) C(62) C(61) 0.3(6) no . . . . C(62) C(57) C(58) O(6) -174.0(4) no . . . . C(62) C(57) C(58) C(59) 3.8(6) no . . . . O(6) C(58) C(59) C(60) 173.2(3) no . . . . O(6) C(58) C(59) C(79) -5.1(6) no . . . . C(57) C(58) C(59) C(60) -4.6(6) no . . . . C(57) C(58) C(59) C(79) 177.0(3) no . . . . C(58) C(59) C(60) C(61) 1.5(6) no . . . . C(58) C(59) C(79) C(80) 67.0(5) no . . . . C(58) C(59) C(79) C(81) -54.3(5) no . . . . C(58) C(59) C(79) C(82) -173.1(4) no . . . . C(60) C(59) C(79) C(80) -111.3(4) no . . . . C(60) C(59) C(79) C(81) 127.4(4) no . . . . C(60) C(59) C(79) C(82) 8.6(5) no . . . . C(79) C(59) C(60) C(61) 179.8(4) no . . . . C(59) C(60) C(61) C(62) 2.4(7) no . . . . C(59) C(60) C(61) C(83) -176.4(4) no . . . . C(60) C(61) C(62) C(57) -3.3(6) no . . . . C(60) C(61) C(83) C(84) 101.4(5) no . . . . C(60) C(61) C(83) C(85) -133.9(5) no . . . . C(60) C(61) C(83) C(86) -18.7(6) no . . . . C(60) C(61) C(83) C(87) 60.0(6) no . . . . C(60) C(61) C(83) C(88) 178.4(4) no . . . . C(60) C(61) C(83) C(89) -60.5(6) no . . . . C(62) C(61) C(83) C(84) -77.4(6) no . . . . C(62) C(61) C(83) C(85) 47.3(6) no . . . . C(62) C(61) C(83) C(86) 162.5(4) no . . . . C(62) C(61) C(83) C(87) -118.8(5) no . . . . C(62) C(61) C(83) C(88) -0.4(6) no . . . . C(62) C(61) C(83) C(89) 120.7(5) no . . . . C(83) C(61) C(62) C(57) 175.5(4) no . . . . C(61) C(83) C(84) C(88) 107.8(6) no . . . . C(61) C(83) C(85) C(88) -102.7(7) no . . . . C(61) C(83) C(85) C(89) 104.7(5) no . . . . C(61) C(83) C(86) C(87) 102.2(5) no . . . . C(61) C(83) C(87) C(86) -107.9(5) no . . . . C(61) C(83) C(88) C(84) -104.7(5) no . . . . C(61) C(83) C(88) C(85) 95.4(6) no . . . . C(61) C(83) C(89) C(85) -103.8(5) no . . . . C(84) C(83) C(85) C(88) 20.6(13) no . . . . C(84) C(83) C(85) C(89) -132.0(10) no . . . . C(85) C(83) C(84) C(88) -15.1(9) no . . . . C(84) C(83) C(86) C(87) -19.1(10) no . . . . C(86) C(83) C(84) C(88) -130.3(8) no . . . . C(84) C(83) C(87) C(86) 150.6(14) no . . . . C(87) C(83) C(84) C(88) -160.0(14) no . . . . C(84) C(83) C(88) C(85) -159.9(11) no . . . . C(84) C(83) C(89) C(85) 100.9(15) no . . . . C(89) C(83) C(84) C(88) -96.9(14) no . . . . C(85) C(83) C(86) C(87) -139.5(7) no . . . . C(86) C(83) C(85) C(88) 137.8(8) no . . . . C(86) C(83) C(85) C(89) -14.7(7) no . . . . C(85) C(83) C(87) C(86) 93.3(13) no . . . . C(87) C(83) C(85) C(88) 55.8(16) no . . . . C(87) C(83) C(85) C(89) -96.8(12) no . . . . C(85) C(83) C(88) C(84) 159.9(11) no . . . . C(88) C(83) C(85) C(89) -152.6(11) no . . . . C(89) C(83) C(85) C(88) 152.6(10) no . . . . C(86) C(83) C(88) C(84) 97.2(10) no . . . . C(86) C(83) C(88) C(85) -62.7(11) no . . . . C(88) C(83) C(86) C(87) -99.5(10) no . . . . C(86) C(83) C(89) C(85) 157.0(12) no . . . . C(89) C(83) C(86) C(87) -161.5(12) no . . . . C(87) C(83) C(88) C(84) 13.1(6) no . . . . C(87) C(83) C(88) C(85) -146.8(7) no . . . . C(88) C(83) C(87) C(86) 130.7(7) no . . . . C(87) C(83) C(89) C(85) 138.0(6) no . . . . C(89) C(83) C(87) C(86) 12.3(7) no . . . . C(88) C(83) C(89) C(85) 19.9(6) no . . . . C(89) C(83) C(88) C(84) 133.1(7) no . . . . C(89) C(83) C(88) C(85) -26.8(9) no . . . . C(83) C(84) C(88) C(85) 21.3(11) no . . . . C(83) C(85) C(88) C(84) -18.5(9) no . . . . C(88) C(85) C(89) C(83) -28.8(12) no . . . . C(89) C(85) C(88) C(83) 25.5(11) no . . . . C(89) C(85) C(88) C(84) 7.1(18) no . . . . C(103) C(102) C(107) C(106) -0.1(11) no . . . . C(107) C(102) C(103) C(104) 0.7(12) no . . . . C(102) C(103) C(104) C(105) 0.9(14) no . . . . C(103) C(104) C(105) C(106) -3.1(14) no . . . . C(104) C(105) C(106) C(107) 3.6(13) no . . . . C(105) C(106) C(107) C(102) -2.0(12) no . . . . C(109) C(108) C(113) C(112) -0.0(10) no . . . . C(113) C(108) C(109) C(110) 0.5(9) no . . . . C(108) C(109) C(110) C(111) -0.7(9) no . . . . C(109) C(110) C(111) C(112) 0.5(10) no . . . . C(110) C(111) C(112) C(113) -0.0(11) no . . . . C(111) C(112) C(113) C(108) -0.2(11) no . . . . C(115) C(114) C(119) C(118) 0.4(15) no . . . . C(119) C(114) C(115) C(116) -2.6(14) no . . . . C(114) C(115) C(116) C(117) 1.1(14) no . . . . C(115) C(116) C(117) C(118) 2.7(16) no . . . . C(116) C(117) C(118) C(119) -5.1(16) no . . . . C(117) C(118) C(119) C(114) 3.6(16) no . . . . C(121) C(120) C(122) C(121) 22(3) no . . 2_576 2_576 C(121) C(120) C(122) C(134) -64.5(17) no . . 2_576 . C(122) C(120) C(121) C(122) -22(3) no 2_576 . . . C(122) C(120) C(121) C(134) 50.8(16) no 2_576 . . . C(121) C(120) C(134) C(122) 126.6(16) no . . . 2_576 C(121) C(120) C(134) C(132) 105(2) no . . . 2_576 C(121) C(120) C(134) C(133) -12.2(10) no . . . . C(134) C(120) C(121) C(122) -72(3) no . . . . C(122) C(120) C(134) C(121) -126.6(16) no 2_576 . . . C(122) C(120) C(134) C(132) -21.4(15) no 2_576 . . 2_576 C(122) C(120) C(134) C(133) -139(2) no 2_576 . . . C(134) C(120) C(122) C(121) 87(3) no . . 2_576 2_576 C(120) C(121) C(122) C(120) 22(3) no . . . 2_576 C(120) C(121) C(122) C(134) -32(3) no . . . 2_576 C(120) C(121) C(134) C(122) -53(3) no . . . 2_576 C(120) C(121) C(134) C(132) -97(3) no . . . 2_576 C(120) C(121) C(134) C(133) 20.6(17) no . . . . C(122) C(121) C(134) C(120) 120.1(19) no . . . . C(122) C(121) C(134) C(122) 67(3) no . . . 2_576 C(122) C(121) C(134) C(132) 23(3) no . . . 2_576 C(122) C(121) C(134) C(133) 141(3) no . . . . C(134) C(121) C(122) C(120) -13(3) no . . . 2_576 C(134) C(121) C(122) C(134) -66.5(19) no . . . 2_576 C(120) C(122) C(134) C(121) -46.4(18) no 2_576 . 2_576 2_576 C(120) C(122) C(134) C(132) -148(2) no 2_576 . 2_576 . C(120) C(122) C(134) C(133) -24.8(15) no 2_576 . 2_576 2_576 C(121) C(122) C(134) C(120) 116.7(19) no . . 2_576 2_576 C(121) C(122) C(134) C(121) 70(3) no . . 2_576 2_576 C(121) C(122) C(134) C(132) -31.3(14) no . . 2_576 . C(121) C(122) C(134) C(133) 92(3) no . . 2_576 2_576 C(133) C(132) C(134) C(120) 73(4) no . . 2_576 2_576 C(133) C(132) C(134) C(121) 10(4) no . . 2_576 2_576 C(133) C(132) C(134) C(122) 104(3) no . . 2_576 . C(133) C(132) C(134) C(133) 33(4) no . . 2_576 2_576 C(134) C(132) C(133) C(134) -32(3) no 2_576 . . . C(132) C(133) C(134) C(120) 112(3) no . . . . C(132) C(133) C(134) C(121) -38.9(17) no . . . . C(132) C(133) C(134) C(122) 73(3) no . . . 2_576 C(132) C(133) C(134) C(132) 34(4) no . . . 2_576 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag N(1) H(1A) Cl(6) . . 2_565 3.297(4) 0.930 2.405 160.8 no #===END #============================================================================== data__O2OHNbBn3-Complex-4 _database_code_depnum_ccdc_archive 'CCDC 789694' #TrackingRef '- Kawaguchi_CIF_rivised.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C71 H91 Nb O3' _chemical_formula_moiety 'C71 H91 Nb O3' _chemical_formula_weight 1085.40 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 22.812(7) _cell_length_b 14.173(4) _cell_length_c 20.084(6) _cell_angle_alpha 90.0000 _cell_angle_beta 106.140(4) _cell_angle_gamma 90.0000 _cell_volume 6238(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15816 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 173 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328.0 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.954 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 173 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 48519 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measured_fraction_theta_full 0.983 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 14088 _reflns_number_gt 11992 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1521 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 14088 _refine_ls_number_parameters 672 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0689P)^2^+6.9955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.870 _refine_diff_density_min -0.450 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' 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' #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Nb(1) Nb 0.201516(10) 0.583694(16) 0.540210(12) 0.02373(8) Uani 1.0 4 d . . . O(1) O 0.14868(8) 0.58011(12) 0.59942(9) 0.0247(4) Uani 1.0 4 d . . . O(2) O 0.26675(8) 0.61266(13) 0.62321(9) 0.0263(4) Uani 1.0 4 d . . . O(3) O 0.32875(13) 0.3259(2) 0.62608(15) 0.0336(7) Uiso 0.7000 4 d . . . O(4) O 0.1223(3) 0.3071(4) 0.6409(3) 0.0226(12) Uiso 0.3000 4 d . . . C(1) C 0.23062(11) 0.43046(16) 0.65983(13) 0.0199(5) Uani 1.0 4 d . . . C(2) C 0.18217(11) 0.46975(17) 0.69168(13) 0.0219(5) Uani 1.0 4 d . . . C(3) C 0.14511(11) 0.54599(17) 0.66168(13) 0.0217(5) Uani 1.0 4 d . . . C(4) C 0.10583(11) 0.58930(17) 0.69563(14) 0.0244(5) Uani 1.0 4 d . . . C(5) C 0.10282(12) 0.54885(19) 0.75771(14) 0.0275(6) Uani 1.0 4 d . . . C(6) C 0.13759(12) 0.47160(19) 0.78839(14) 0.0263(6) Uani 1.0 4 d . . . C(7) C 0.17852(12) 0.43470(17) 0.75537(14) 0.0245(6) Uani 1.0 4 d . . . C(8) C 0.07190(12) 0.68211(19) 0.66903(15) 0.0292(6) Uani 1.0 4 d . . . C(9) C 0.03151(14) 0.6759(3) 0.59405(17) 0.0410(8) Uani 1.0 4 d . . . C(10) C 0.11934(15) 0.7606(2) 0.67347(17) 0.0391(7) Uani 1.0 4 d . . . C(11) C 0.03054(16) 0.7122(3) 0.71402(19) 0.0473(9) Uani 1.0 4 d . . . C(12) C 0.13362(14) 0.4299(3) 0.85794(15) 0.0346(7) Uani 1.0 4 d . . . C(13) C 0.0777(3) 0.4663(4) 0.8773(3) 0.0744(15) Uani 1.0 4 d . . . C(14) C 0.1921(2) 0.4540(4) 0.91449(18) 0.0611(11) Uani 1.0 4 d . . . C(15) C 0.12804(18) 0.3221(3) 0.85187(19) 0.0494(9) Uani 1.0 4 d . . . C(16) C 0.29125(11) 0.47681(17) 0.69834(13) 0.0224(5) Uani 1.0 4 d . . . C(17) C 0.30481(11) 0.56893(18) 0.67963(13) 0.0229(5) Uani 1.0 4 d . . . C(18) C 0.35710(12) 0.61615(19) 0.72045(14) 0.0267(6) Uani 1.0 4 d . . . C(19) C 0.39508(12) 0.56707(19) 0.77600(14) 0.0280(6) Uani 1.0 4 d . . . C(20) C 0.38381(12) 0.4755(2) 0.79425(14) 0.0265(6) Uani 1.0 4 d . . . C(21) C 0.33043(12) 0.43272(18) 0.75550(13) 0.0239(5) Uani 1.0 4 d . . . C(22) C 0.37125(14) 0.7192(2) 0.70517(16) 0.0356(7) Uani 1.0 4 d . . . C(23) C 0.31738(17) 0.7831(2) 0.70522(19) 0.0458(8) Uani 1.0 4 d . . . C(24) C 0.38622(15) 0.7239(3) 0.63527(17) 0.0411(8) Uani 1.0 4 d . . . C(25) C 0.42724(18) 0.7576(3) 0.76076(19) 0.0565(11) Uani 1.0 4 d . . . C(26) C 0.42798(13) 0.4239(3) 0.85568(15) 0.0343(7) Uani 1.0 4 d . . . C(27) C 0.4372(3) 0.3179(5) 0.8330(4) 0.0555(16) Uiso 0.6000 4 d . . . C(28) C 0.4013(4) 0.4166(6) 0.9154(4) 0.0611(17) Uiso 0.6000 4 d . . . C(29) C 0.4941(4) 0.4628(6) 0.8738(4) 0.0573(16) Uiso 0.6000 4 d . . . C(30) C 0.23053(11) 0.32283(17) 0.65174(13) 0.0221(5) Uani 1.0 4 d . . . C(31) C 0.28074(12) 0.27632(19) 0.63895(15) 0.0293(6) Uani 1.0 4 d . . . C(32) C 0.28016(13) 0.17927(19) 0.62723(15) 0.0296(6) Uani 1.0 4 d . . . C(33) C 0.22625(14) 0.13064(19) 0.62362(15) 0.0312(6) Uani 1.0 4 d . . . C(34) C 0.17448(13) 0.17368(19) 0.63223(15) 0.0296(6) Uani 1.0 4 d . . . C(35) C 0.17756(12) 0.27041(18) 0.64674(14) 0.0267(6) Uani 1.0 4 d . . . C(36) C 0.33761(15) 0.1280(3) 0.61984(19) 0.0429(8) Uani 1.0 4 d . . . C(37) C 0.3492(2) 0.1547(4) 0.5497(3) 0.0710(13) Uani 1.0 4 d . . . C(38) C 0.3268(3) 0.0211(3) 0.6134(4) 0.108(3) Uani 1.0 4 d . . . C(39) C 0.3912(3) 0.1509(5) 0.6786(3) 0.102(3) Uani 1.0 4 d . . . C(40) C 0.11485(15) 0.1191(3) 0.62603(19) 0.0447(8) Uani 1.0 4 d . . . C(41) C 0.06444(17) 0.1567(3) 0.5633(3) 0.0592(11) Uani 1.0 4 d . . . C(42) C 0.1219(2) 0.0140(3) 0.6128(4) 0.0861(18) Uani 1.0 4 d . . . C(43) C 0.0953(2) 0.1311(5) 0.6923(3) 0.0829(16) Uani 1.0 4 d . . . C(44) C 0.15461(12) 0.4521(2) 0.49277(15) 0.0297(6) Uani 1.0 4 d . . . C(45) C 0.10858(12) 0.50383(19) 0.43923(14) 0.0284(6) Uani 1.0 4 d . . . C(46) C 0.11570(14) 0.5213(3) 0.37341(16) 0.0379(7) Uani 1.0 4 d . . . C(47) C 0.07270(16) 0.5740(3) 0.32504(17) 0.0447(8) Uani 1.0 4 d . . . C(48) C 0.02213(16) 0.6102(3) 0.34116(19) 0.0462(8) Uani 1.0 4 d . . . C(49) C 0.01418(14) 0.5931(3) 0.40630(18) 0.0406(8) Uani 1.0 4 d . . . C(50) C 0.05674(12) 0.5412(2) 0.45470(15) 0.0310(6) Uani 1.0 4 d . . . C(51) C 0.17234(14) 0.7194(2) 0.48935(16) 0.0347(7) Uani 1.0 4 d . . . C(52) C 0.21396(13) 0.76486(19) 0.45311(15) 0.0310(6) Uani 1.0 4 d . . . C(53) C 0.26812(15) 0.8069(3) 0.49058(17) 0.0401(7) Uani 1.0 4 d . . . C(54) C 0.30783(16) 0.8466(3) 0.45737(19) 0.0499(9) Uani 1.0 4 d . . . C(55) C 0.29366(17) 0.8474(3) 0.38604(19) 0.0492(9) Uani 1.0 4 d . . . C(56) C 0.23934(17) 0.8083(3) 0.34761(18) 0.0464(8) Uani 1.0 4 d . . . C(57) C 0.20020(15) 0.7659(3) 0.38084(16) 0.0386(7) Uani 1.0 4 d . . . C(58) C 0.27979(13) 0.5270(3) 0.50764(16) 0.0370(7) Uani 1.0 4 d . . . C(59) C 0.27695(13) 0.4766(3) 0.44190(17) 0.0385(7) Uani 1.0 4 d . . . C(60) C 0.27070(16) 0.5259(3) 0.38018(19) 0.0510(9) Uani 1.0 4 d . . . C(61) C 0.26696(18) 0.4773(5) 0.3183(2) 0.0694(14) Uani 1.0 4 d . . . C(62) C 0.26975(19) 0.3800(5) 0.3177(3) 0.0713(14) Uani 1.0 4 d . . . C(63) C 0.27713(19) 0.3319(4) 0.3780(3) 0.0643(12) Uani 1.0 4 d . . . C(64) C 0.28053(17) 0.3786(3) 0.4397(2) 0.0491(9) Uani 1.0 4 d . . . C(65) C 0.4018(6) 0.3309(9) 0.8729(7) 0.073(3) Uiso 0.4000 4 d . . . C(66) C 0.4263(5) 0.4824(8) 0.9243(6) 0.062(3) Uiso 0.4000 4 d . . . C(67) C 0.4888(7) 0.4155(11) 0.8417(8) 0.086(4) Uiso 0.4000 4 d . . . C(68) C 0.5163(3) 0.3907(4) 0.5634(3) 0.0851(16) Uani 1.0 4 d . . . C(69) C 0.5619(3) 0.4475(5) 0.5904(4) 0.0966(18) Uani 1.0 4 d . . . C(70) C 0.5594(4) 0.5135(7) 0.6380(5) 0.146(4) Uani 1.0 4 d . . . C(71) C 0.5095(3) 0.5193(5) 0.6622(4) 0.108(3) Uani 1.0 4 d . . . C(72) C 0.4624(3) 0.4663(5) 0.6369(3) 0.0873(16) Uani 1.0 4 d . . . C(73) C 0.4645(3) 0.3992(5) 0.5876(4) 0.102(2) Uani 1.0 4 d . . . C(74) C 0.5205(6) 0.3175(8) 0.5125(5) 0.218(6) Uani 1.0 4 d . . . H(1) H 0.2203 0.4563 0.6116 0.0239 Uiso 1.0 4 calc R . . H(5) H 0.0754 0.5755 0.7805 0.0330 Uiso 1.0 4 calc R . . H(7) H 0.2046 0.3845 0.7766 0.0294 Uiso 1.0 4 calc R . . H(9A) H 0.0016 0.6252 0.5903 0.0492 Uiso 1.0 4 calc R . . H(9B) H 0.0570 0.6625 0.5631 0.0492 Uiso 1.0 4 calc R . . H(9C) H 0.0102 0.7360 0.5808 0.0492 Uiso 1.0 4 calc R . . H(10A) H 0.1494 0.7402 0.6498 0.0469 Uiso 1.0 4 calc R . . H(10B) H 0.1401 0.7739 0.7222 0.0469 Uiso 1.0 4 calc R . . H(10C) H 0.0988 0.8179 0.6512 0.0469 Uiso 1.0 4 calc R . . H(11A) H 0.0554 0.7224 0.7618 0.0567 Uiso 1.0 4 calc R . . H(11B) H 0.0004 0.6626 0.7132 0.0567 Uiso 1.0 4 calc R . . H(11C) H 0.0094 0.7709 0.6957 0.0567 Uiso 1.0 4 calc R . . H(13A) H 0.0871 0.5276 0.9004 0.0893 Uiso 1.0 4 calc R . . H(13B) H 0.0664 0.4213 0.9087 0.0893 Uiso 1.0 4 calc R . . H(13C) H 0.0437 0.4733 0.8353 0.0893 Uiso 1.0 4 calc R . . H(14A) H 0.1913 0.4231 0.9579 0.0733 Uiso 1.0 4 calc R . . H(14B) H 0.1948 0.5225 0.9214 0.0733 Uiso 1.0 4 calc R . . H(14C) H 0.2275 0.4318 0.9004 0.0733 Uiso 1.0 4 calc R . . H(15A) H 0.1645 0.2962 0.8420 0.0593 Uiso 1.0 4 calc R . . H(15B) H 0.0919 0.3055 0.8142 0.0593 Uiso 1.0 4 calc R . . H(15C) H 0.1241 0.2958 0.8956 0.0593 Uiso 1.0 4 calc R . . H(19) H 0.4308 0.5979 0.8030 0.0336 Uiso 1.0 4 calc R . . H(21) H 0.3204 0.3716 0.7684 0.0286 Uiso 1.0 4 calc R . . H(23A) H 0.2812 0.7621 0.6693 0.0549 Uiso 1.0 4 calc R . . H(23B) H 0.3271 0.8482 0.6958 0.0549 Uiso 1.0 4 calc R . . H(23C) H 0.3093 0.7800 0.7506 0.0549 Uiso 1.0 4 calc R . . H(24A) H 0.3518 0.6989 0.5987 0.0493 Uiso 1.0 4 calc R . . H(24B) H 0.4227 0.6861 0.6377 0.0493 Uiso 1.0 4 calc R . . H(24C) H 0.3937 0.7896 0.6248 0.0493 Uiso 1.0 4 calc R . . H(25A) H 0.4215 0.7479 0.8068 0.0678 Uiso 1.0 4 calc R . . H(25B) H 0.4318 0.8251 0.7531 0.0678 Uiso 1.0 4 calc R . . H(25C) H 0.4639 0.7240 0.7577 0.0678 Uiso 1.0 4 calc R . . H(33) H 0.2250 0.0647 0.6148 0.0375 Uiso 1.0 4 calc R . . H(37A) H 0.3593 0.2219 0.5499 0.0851 Uiso 1.0 4 calc R . . H(37B) H 0.3124 0.1418 0.5119 0.0851 Uiso 1.0 4 calc R . . H(37C) H 0.3832 0.1172 0.5431 0.0851 Uiso 1.0 4 calc R . . H(38A) H 0.3645 -0.0106 0.6115 0.1299 Uiso 1.0 4 calc R . . H(38B) H 0.2944 0.0074 0.5709 0.1299 Uiso 1.0 4 calc R . . H(38C) H 0.3146 -0.0018 0.6536 0.1299 Uiso 1.0 4 calc R . . H(39A) H 0.3832 0.1319 0.7222 0.1219 Uiso 1.0 4 calc R . . H(39B) H 0.3989 0.2190 0.6794 0.1219 Uiso 1.0 4 calc R . . H(39C) H 0.4271 0.1170 0.6732 0.1219 Uiso 1.0 4 calc R . . H(41A) H 0.0549 0.2222 0.5718 0.0711 Uiso 1.0 4 calc R . . H(41B) H 0.0277 0.1179 0.5565 0.0711 Uiso 1.0 4 calc R . . H(41C) H 0.0787 0.1537 0.5216 0.0711 Uiso 1.0 4 calc R . . H(42A) H 0.1437 0.0063 0.5774 0.1033 Uiso 1.0 4 calc R . . H(42B) H 0.0815 -0.0152 0.5966 0.1033 Uiso 1.0 4 calc R . . H(42C) H 0.1451 -0.0166 0.6559 0.1033 Uiso 1.0 4 calc R . . H(43A) H 0.0576 0.0958 0.6882 0.0994 Uiso 1.0 4 calc R . . H(43B) H 0.0883 0.1982 0.6994 0.0994 Uiso 1.0 4 calc R . . H(43C) H 0.1275 0.1072 0.7318 0.0994 Uiso 1.0 4 calc R . . H(44A) H 0.1808 0.4109 0.4733 0.0357 Uiso 1.0 4 calc R . . H(44B) H 0.1368 0.4159 0.5246 0.0357 Uiso 1.0 4 calc R . . H(46) H 0.1503 0.4969 0.3616 0.0454 Uiso 1.0 4 calc R . . H(47) H 0.0782 0.5852 0.2805 0.0536 Uiso 1.0 4 calc R . . H(48) H -0.0070 0.6465 0.3080 0.0554 Uiso 1.0 4 calc R . . H(49) H -0.0207 0.6174 0.4175 0.0488 Uiso 1.0 4 calc R . . H(50) H 0.0509 0.5305 0.4991 0.0371 Uiso 1.0 4 calc R . . H(51A) H 0.1321 0.7102 0.4551 0.0416 Uiso 1.0 4 calc R . . H(51B) H 0.1663 0.7640 0.5248 0.0416 Uiso 1.0 4 calc R . . H(53) H 0.2781 0.8084 0.5397 0.0481 Uiso 1.0 4 calc R . . H(54) H 0.3452 0.8734 0.4840 0.0598 Uiso 1.0 4 calc R . . H(55) H 0.3211 0.8747 0.3635 0.0591 Uiso 1.0 4 calc R . . H(56) H 0.2287 0.8104 0.2984 0.0556 Uiso 1.0 4 calc R . . H(57) H 0.1636 0.7372 0.3540 0.0464 Uiso 1.0 4 calc R . . H(58A) H 0.3075 0.5812 0.5092 0.0444 Uiso 1.0 4 calc R . . H(58B) H 0.3014 0.4838 0.5452 0.0444 Uiso 1.0 4 calc R . . H(60) H 0.2690 0.5929 0.3801 0.0612 Uiso 1.0 4 calc R . . H(61) H 0.2625 0.5116 0.2765 0.0833 Uiso 1.0 4 calc R . . H(62) H 0.2665 0.3471 0.2757 0.0856 Uiso 1.0 4 calc R . . H(63) H 0.2800 0.2650 0.3779 0.0771 Uiso 1.0 4 calc R . . H(64) H 0.2854 0.3433 0.4811 0.0589 Uiso 1.0 4 calc R . . H(69) H 0.5981 0.4421 0.5760 0.1159 Uiso 1.0 4 calc R . . H(70) H 0.5925 0.5560 0.6546 0.1753 Uiso 1.0 4 calc R . . H(71) H 0.5092 0.5627 0.6981 0.1298 Uiso 1.0 4 calc R . . H(72) H 0.4267 0.4734 0.6521 0.1047 Uiso 1.0 4 calc R . . H(73) H 0.4306 0.3586 0.5700 0.1220 Uiso 1.0 4 calc R . . H(74A) H 0.5397 0.2608 0.5371 0.2614 Uiso 1.0 4 calc R . . H(74B) H 0.5452 0.3412 0.4832 0.2614 Uiso 1.0 4 calc R . . H(74C) H 0.4795 0.3019 0.4835 0.2614 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb(1) 0.02486(12) 0.02415(13) 0.02364(13) -0.00039(9) 0.00914(9) 0.00416(9) O(1) 0.0258(9) 0.0234(9) 0.0266(10) 0.0025(7) 0.0103(8) 0.0045(8) O(2) 0.0286(10) 0.0222(9) 0.0279(10) -0.0038(7) 0.0078(8) 0.0014(8) C(1) 0.0200(11) 0.0177(11) 0.0230(12) -0.0007(9) 0.0077(10) 0.0019(9) C(2) 0.0202(12) 0.0179(11) 0.0289(13) -0.0013(9) 0.0089(10) -0.0015(10) C(3) 0.0223(12) 0.0190(11) 0.0249(13) -0.0028(9) 0.0084(10) 0.0005(10) C(4) 0.0226(12) 0.0209(12) 0.0306(14) 0.0004(10) 0.0087(10) -0.0010(11) C(5) 0.0253(13) 0.0284(13) 0.0323(15) 0.0010(11) 0.0139(11) -0.0022(11) C(6) 0.0285(13) 0.0278(13) 0.0250(13) -0.0029(11) 0.0113(11) 0.0015(11) C(7) 0.0258(13) 0.0203(12) 0.0287(14) -0.0000(10) 0.0096(11) 0.0041(10) C(8) 0.0280(14) 0.0255(13) 0.0347(15) 0.0066(11) 0.0096(12) -0.0007(11) C(9) 0.0343(16) 0.0347(16) 0.0460(18) 0.0110(13) -0.0022(14) -0.0018(14) C(10) 0.0458(18) 0.0209(14) 0.0472(18) 0.0008(12) 0.0075(14) 0.0000(13) C(11) 0.049(2) 0.0419(18) 0.056(2) 0.0221(16) 0.0231(17) 0.0024(16) C(12) 0.0400(16) 0.0399(17) 0.0282(15) 0.0020(13) 0.0168(13) 0.0066(13) C(13) 0.090(4) 0.093(4) 0.063(3) 0.041(3) 0.060(3) 0.037(3) C(14) 0.075(3) 0.070(3) 0.0320(19) -0.019(3) 0.0048(18) 0.0032(18) C(15) 0.059(3) 0.047(2) 0.049(2) -0.0107(17) 0.0261(17) 0.0144(16) C(16) 0.0207(12) 0.0230(12) 0.0256(13) -0.0022(10) 0.0100(10) -0.0028(10) C(17) 0.0238(12) 0.0245(13) 0.0229(13) -0.0019(10) 0.0104(10) -0.0012(10) C(18) 0.0279(13) 0.0260(13) 0.0289(14) -0.0078(11) 0.0124(11) -0.0032(11) C(19) 0.0243(13) 0.0342(15) 0.0258(14) -0.0078(11) 0.0076(11) -0.0053(11) C(20) 0.0220(12) 0.0331(14) 0.0248(13) 0.0006(11) 0.0070(10) -0.0022(11) C(21) 0.0245(12) 0.0232(12) 0.0254(13) -0.0014(10) 0.0095(10) -0.0007(10) C(22) 0.0397(16) 0.0288(14) 0.0365(16) -0.0162(12) 0.0077(13) -0.0023(12) C(23) 0.065(3) 0.0236(14) 0.052(2) -0.0080(15) 0.0234(18) -0.0021(14) C(24) 0.0381(17) 0.0425(18) 0.0437(18) -0.0137(14) 0.0129(14) 0.0082(14) C(25) 0.066(3) 0.043(2) 0.052(2) -0.0334(18) 0.0019(18) -0.0010(17) C(26) 0.0273(14) 0.0440(17) 0.0282(15) 0.0013(12) 0.0018(11) 0.0047(13) C(30) 0.0254(12) 0.0170(11) 0.0241(13) -0.0008(9) 0.0075(10) 0.0006(10) C(31) 0.0272(13) 0.0226(13) 0.0415(16) 0.0001(10) 0.0151(12) -0.0013(12) C(32) 0.0351(15) 0.0240(13) 0.0331(15) 0.0038(11) 0.0151(12) 0.0009(11) C(33) 0.0434(16) 0.0194(13) 0.0322(15) -0.0027(11) 0.0126(13) -0.0015(11) C(34) 0.0331(14) 0.0235(13) 0.0319(15) -0.0067(11) 0.0082(12) 0.0027(11) C(35) 0.0264(13) 0.0239(13) 0.0311(14) -0.0010(10) 0.0099(11) 0.0035(11) C(36) 0.0439(18) 0.0292(16) 0.064(3) 0.0108(13) 0.0283(17) -0.0004(15) C(37) 0.068(3) 0.081(4) 0.075(3) 0.013(3) 0.039(3) -0.014(3) C(38) 0.089(4) 0.043(3) 0.212(8) 0.027(3) 0.073(5) -0.008(4) C(39) 0.058(3) 0.140(6) 0.089(4) 0.060(4) -0.009(3) -0.032(4) C(40) 0.0375(17) 0.0344(16) 0.059(3) -0.0126(14) 0.0078(15) 0.0070(15) C(41) 0.0396(19) 0.054(3) 0.075(3) -0.0141(17) 0.0014(18) 0.002(2) C(42) 0.060(3) 0.033(2) 0.149(5) -0.0226(19) 0.001(3) 0.012(3) C(43) 0.062(3) 0.117(5) 0.076(3) -0.048(3) 0.031(3) 0.011(3) C(44) 0.0275(14) 0.0307(14) 0.0302(15) -0.0020(11) 0.0067(11) -0.0014(12) C(45) 0.0258(13) 0.0292(14) 0.0287(14) -0.0066(11) 0.0052(11) -0.0034(11) C(46) 0.0340(15) 0.0490(18) 0.0311(16) -0.0027(14) 0.0099(13) -0.0027(14) C(47) 0.0450(19) 0.055(2) 0.0326(17) -0.0055(16) 0.0078(14) 0.0075(15) C(48) 0.0391(18) 0.0472(19) 0.047(2) 0.0008(15) 0.0027(15) 0.0141(16) C(49) 0.0285(15) 0.0413(18) 0.052(2) -0.0001(13) 0.0113(14) 0.0050(15) C(50) 0.0280(14) 0.0326(15) 0.0333(15) -0.0059(11) 0.0103(12) -0.0011(12) C(51) 0.0359(15) 0.0312(15) 0.0382(16) -0.0004(12) 0.0121(13) 0.0102(13) C(52) 0.0338(14) 0.0263(14) 0.0319(15) -0.0004(11) 0.0078(12) 0.0074(12) C(53) 0.0449(18) 0.0382(17) 0.0348(16) -0.0086(14) 0.0072(14) 0.0055(13) C(54) 0.0401(18) 0.052(2) 0.053(3) -0.0151(16) 0.0059(16) 0.0072(17) C(55) 0.049(2) 0.052(2) 0.054(3) -0.0091(16) 0.0269(17) 0.0125(17) C(56) 0.058(3) 0.050(2) 0.0339(17) -0.0065(17) 0.0170(16) 0.0058(15) C(57) 0.0391(17) 0.0403(17) 0.0347(16) -0.0079(13) 0.0072(13) 0.0051(13) C(58) 0.0301(15) 0.0457(18) 0.0383(17) -0.0022(13) 0.0146(13) -0.0039(14) C(59) 0.0254(14) 0.054(2) 0.0380(17) 0.0041(13) 0.0113(12) -0.0021(15) C(60) 0.0375(18) 0.074(3) 0.046(2) 0.0034(17) 0.0190(15) 0.0082(19) C(61) 0.045(3) 0.127(5) 0.040(3) 0.004(3) 0.0175(17) 0.014(3) C(62) 0.052(3) 0.122(5) 0.044(3) -0.004(3) 0.0196(19) -0.028(3) C(63) 0.061(3) 0.071(3) 0.068(3) -0.003(2) 0.030(3) -0.030(3) C(64) 0.048(2) 0.055(3) 0.047(2) 0.0079(17) 0.0166(16) -0.0078(17) C(68) 0.117(5) 0.082(4) 0.053(3) 0.004(4) 0.019(3) -0.006(3) C(69) 0.069(4) 0.116(5) 0.109(5) -0.011(4) 0.031(4) -0.006(4) C(70) 0.083(5) 0.140(7) 0.202(9) -0.035(5) 0.018(6) -0.063(7) C(71) 0.068(4) 0.111(5) 0.129(6) 0.014(4) 0.000(4) -0.041(5) C(72) 0.071(4) 0.117(5) 0.078(4) 0.003(4) 0.027(3) -0.015(4) C(73) 0.091(5) 0.108(5) 0.103(5) -0.042(4) 0.023(4) -0.010(4) C(74) 0.340(17) 0.185(10) 0.136(8) 0.013(11) 0.079(10) -0.088(8) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb(1) O(1) 1.915(2) yes . . Nb(1) O(2) 1.9449(17) yes . . Nb(1) C(44) 2.229(3) yes . . Nb(1) C(51) 2.193(3) yes . . Nb(1) C(58) 2.216(4) yes . . O(1) C(3) 1.364(4) yes . . O(2) C(17) 1.369(3) yes . . O(3) C(31) 1.385(5) yes . . O(4) C(35) 1.339(7) yes . . C(1) C(2) 1.528(4) yes . . C(1) C(16) 1.532(4) yes . . C(1) C(30) 1.534(4) yes . . C(2) C(3) 1.401(4) yes . . C(2) C(7) 1.396(4) yes . . C(3) C(4) 1.409(4) yes . . C(4) C(5) 1.391(4) yes . . C(4) C(8) 1.544(4) yes . . C(5) C(6) 1.391(4) yes . . C(6) C(7) 1.389(5) yes . . C(6) C(12) 1.543(5) yes . . C(8) C(9) 1.534(4) yes . . C(8) C(10) 1.537(5) yes . . C(8) C(11) 1.537(6) yes . . C(12) C(13) 1.523(7) yes . . C(12) C(14) 1.530(5) yes . . C(12) C(15) 1.535(5) yes . . C(16) C(17) 1.416(4) yes . . C(16) C(21) 1.392(4) yes . . C(17) C(18) 1.414(4) yes . . C(18) C(19) 1.394(4) yes . . C(18) C(22) 1.546(5) yes . . C(19) C(20) 1.391(4) yes . . C(20) C(21) 1.389(4) yes . . C(20) C(26) 1.544(4) yes . . C(22) C(23) 1.526(5) yes . . C(22) C(24) 1.536(5) yes . . C(22) C(25) 1.543(5) yes . . C(26) C(27) 1.600(8) yes . . C(26) C(28) 1.492(10) yes . . C(26) C(29) 1.552(8) yes . . C(26) C(65) 1.525(14) yes . . C(26) C(66) 1.618(13) yes . . C(26) C(67) 1.495(18) yes . . C(27) C(65) 1.300(17) yes . . C(27) C(67) 1.792(17) yes . . C(28) C(65) 1.486(15) yes . . C(30) C(31) 1.406(4) yes . . C(30) C(35) 1.398(4) yes . . C(31) C(32) 1.395(4) yes . . C(32) C(33) 1.394(5) yes . . C(32) C(36) 1.542(5) yes . . C(33) C(34) 1.382(5) yes . . C(34) C(35) 1.399(4) yes . . C(34) C(40) 1.539(5) yes . . C(36) C(37) 1.549(7) yes . . C(36) C(38) 1.534(6) yes . . C(36) C(39) 1.481(6) yes . . C(40) C(41) 1.546(5) yes . . C(40) C(42) 1.531(6) yes . . C(40) C(43) 1.526(7) yes . . C(44) C(45) 1.473(4) yes . . C(45) C(46) 1.398(5) yes . . C(45) C(50) 1.407(5) yes . . C(46) C(47) 1.391(5) yes . . C(47) C(48) 1.381(6) yes . . C(48) C(49) 1.391(6) yes . . C(49) C(50) 1.380(4) yes . . C(51) C(52) 1.493(5) yes . . C(52) C(53) 1.389(4) yes . . C(52) C(57) 1.397(5) yes . . C(53) C(54) 1.385(6) yes . . C(54) C(55) 1.378(6) yes . . C(55) C(56) 1.381(5) yes . . C(56) C(57) 1.391(6) yes . . C(58) C(59) 1.486(5) yes . . C(59) C(60) 1.395(6) yes . . C(59) C(64) 1.393(6) yes . . C(60) C(61) 1.403(7) yes . . C(61) C(62) 1.381(9) yes . . C(62) C(63) 1.358(7) yes . . C(63) C(64) 1.389(7) yes . . C(68) C(69) 1.308(9) yes . . C(68) C(73) 1.402(11) yes . . C(68) C(74) 1.478(13) yes . . C(69) C(70) 1.350(12) yes . . C(70) C(71) 1.357(12) yes . . C(71) C(72) 1.294(9) yes . . C(72) C(73) 1.384(10) yes . . C(1) H(1) 1.000 no . . C(5) H(5) 0.950 no . . C(7) H(7) 0.950 no . . C(9) H(9A) 0.980 no . . C(9) H(9B) 0.980 no . . C(9) H(9C) 0.980 no . . C(10) H(10A) 0.980 no . . C(10) H(10B) 0.980 no . . C(10) H(10C) 0.980 no . . C(11) H(11A) 0.980 no . . C(11) H(11B) 0.980 no . . C(11) H(11C) 0.980 no . . C(13) H(13A) 0.980 no . . C(13) H(13B) 0.980 no . . C(13) H(13C) 0.980 no . . C(14) H(14A) 0.980 no . . C(14) H(14B) 0.980 no . . C(14) H(14C) 0.980 no . . C(15) H(15A) 0.980 no . . C(15) H(15B) 0.980 no . . C(15) H(15C) 0.980 no . . C(19) H(19) 0.950 no . . C(21) H(21) 0.950 no . . C(23) H(23A) 0.980 no . . C(23) H(23B) 0.980 no . . C(23) H(23C) 0.980 no . . C(24) H(24A) 0.980 no . . C(24) H(24B) 0.980 no . . C(24) H(24C) 0.980 no . . C(25) H(25A) 0.980 no . . C(25) H(25B) 0.980 no . . C(25) H(25C) 0.980 no . . C(33) H(33) 0.950 no . . C(37) H(37A) 0.980 no . . C(37) H(37B) 0.980 no . . C(37) H(37C) 0.980 no . . C(38) H(38A) 0.980 no . . C(38) H(38B) 0.980 no . . C(38) H(38C) 0.980 no . . C(39) H(39A) 0.980 no . . C(39) H(39B) 0.980 no . . C(39) H(39C) 0.980 no . . C(41) H(41A) 0.980 no . . C(41) H(41B) 0.980 no . . C(41) H(41C) 0.980 no . . C(42) H(42A) 0.980 no . . C(42) H(42B) 0.980 no . . C(42) H(42C) 0.980 no . . C(43) H(43A) 0.980 no . . C(43) H(43B) 0.980 no . . C(43) H(43C) 0.980 no . . C(44) H(44A) 0.990 no . . C(44) H(44B) 0.990 no . . C(46) H(46) 0.950 no . . C(47) H(47) 0.950 no . . C(48) H(48) 0.950 no . . C(49) H(49) 0.950 no . . C(50) H(50) 0.950 no . . C(51) H(51A) 0.990 no . . C(51) H(51B) 0.990 no . . C(53) H(53) 0.950 no . . C(54) H(54) 0.950 no . . C(55) H(55) 0.950 no . . C(56) H(56) 0.950 no . . C(57) H(57) 0.950 no . . C(58) H(58A) 0.990 no . . C(58) H(58B) 0.990 no . . C(60) H(60) 0.950 no . . C(61) H(61) 0.950 no . . C(62) H(62) 0.950 no . . C(63) H(63) 0.950 no . . C(64) H(64) 0.950 no . . C(69) H(69) 0.950 no . . C(70) H(70) 0.950 no . . C(71) H(71) 0.950 no . . C(72) H(72) 0.950 no . . C(73) H(73) 0.950 no . . C(74) H(74A) 0.980 no . . C(74) H(74B) 0.980 no . . C(74) H(74C) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Nb(1) O(2) 86.39(8) yes . . . O(1) Nb(1) C(44) 86.16(10) yes . . . O(1) Nb(1) C(51) 98.66(11) yes . . . O(1) Nb(1) C(58) 150.65(10) yes . . . O(2) Nb(1) C(44) 134.85(9) yes . . . O(2) Nb(1) C(51) 105.95(10) yes . . . O(2) Nb(1) C(58) 80.92(10) yes . . . C(44) Nb(1) C(51) 119.19(10) yes . . . C(44) Nb(1) C(58) 84.31(12) yes . . . C(51) Nb(1) C(58) 110.22(13) yes . . . Nb(1) O(1) C(3) 141.91(16) yes . . . Nb(1) O(2) C(17) 140.51(17) yes . . . C(2) C(1) C(16) 106.8(2) yes . . . C(2) C(1) C(30) 115.3(3) yes . . . C(16) C(1) C(30) 117.0(2) yes . . . C(1) C(2) C(3) 121.4(3) yes . . . C(1) C(2) C(7) 119.2(2) yes . . . C(3) C(2) C(7) 119.1(3) yes . . . O(1) C(3) C(2) 119.0(3) yes . . . O(1) C(3) C(4) 119.8(2) yes . . . C(2) C(3) C(4) 121.1(3) yes . . . C(3) C(4) C(5) 116.8(3) yes . . . C(3) C(4) C(8) 121.9(3) yes . . . C(5) C(4) C(8) 121.1(3) yes . . . C(4) C(5) C(6) 123.9(3) yes . . . C(5) C(6) C(7) 117.4(3) yes . . . C(5) C(6) C(12) 122.2(3) yes . . . C(7) C(6) C(12) 120.3(3) yes . . . C(2) C(7) C(6) 121.5(3) yes . . . C(4) C(8) C(9) 113.4(3) yes . . . C(4) C(8) C(10) 108.6(3) yes . . . C(4) C(8) C(11) 111.3(3) yes . . . C(9) C(8) C(10) 108.6(3) yes . . . C(9) C(8) C(11) 107.1(3) yes . . . C(10) C(8) C(11) 107.6(3) yes . . . C(6) C(12) C(13) 111.4(3) yes . . . C(6) C(12) C(14) 109.2(3) yes . . . C(6) C(12) C(15) 109.5(3) yes . . . C(13) C(12) C(14) 110.7(3) yes . . . C(13) C(12) C(15) 107.5(4) yes . . . C(14) C(12) C(15) 108.5(3) yes . . . C(1) C(16) C(17) 119.6(2) yes . . . C(1) C(16) C(21) 120.4(3) yes . . . C(17) C(16) C(21) 119.7(2) yes . . . O(2) C(17) C(16) 120.1(2) yes . . . O(2) C(17) C(18) 120.3(3) yes . . . C(16) C(17) C(18) 119.6(3) yes . . . C(17) C(18) C(19) 117.7(3) yes . . . C(17) C(18) C(22) 121.4(3) yes . . . C(19) C(18) C(22) 120.9(3) yes . . . C(18) C(19) C(20) 123.9(3) yes . . . C(19) C(20) C(21) 117.2(3) yes . . . C(19) C(20) C(26) 121.7(3) yes . . . C(21) C(20) C(26) 121.1(3) yes . . . C(16) C(21) C(20) 121.9(3) yes . . . C(18) C(22) C(23) 110.4(3) yes . . . C(18) C(22) C(24) 109.5(3) yes . . . C(18) C(22) C(25) 111.5(3) yes . . . C(23) C(22) C(24) 111.0(3) yes . . . C(23) C(22) C(25) 107.2(3) yes . . . C(24) C(22) C(25) 107.3(3) yes . . . C(20) C(26) C(27) 109.0(3) yes . . . C(20) C(26) C(28) 110.7(4) yes . . . C(20) C(26) C(29) 113.3(4) yes . . . C(20) C(26) C(65) 112.4(5) yes . . . C(20) C(26) C(66) 105.8(5) yes . . . C(20) C(26) C(67) 108.7(6) yes . . . C(27) C(26) C(28) 106.2(5) yes . . . C(27) C(26) C(29) 101.8(5) yes . . . C(27) C(26) C(65) 49.1(7) yes . . . C(27) C(26) C(66) 139.5(5) yes . . . C(27) C(26) C(67) 70.7(7) yes . . . C(28) C(26) C(29) 115.0(5) yes . . . C(28) C(26) C(65) 59.0(6) yes . . . C(28) C(26) C(66) 40.5(6) yes . . . C(28) C(26) C(67) 138.9(7) yes . . . C(29) C(26) C(65) 132.1(6) yes . . . C(29) C(26) C(66) 82.5(6) yes . . . C(29) C(26) C(67) 34.9(7) yes . . . C(65) C(26) C(66) 98.4(7) yes . . . C(65) C(26) C(67) 114.6(8) yes . . . C(66) C(26) C(67) 116.4(7) yes . . . C(26) C(27) C(65) 62.5(7) yes . . . C(26) C(27) C(67) 51.9(6) yes . . . C(65) C(27) C(67) 109.6(9) yes . . . C(26) C(28) C(65) 61.6(7) yes . . . C(1) C(30) C(31) 120.6(3) yes . . . C(1) C(30) C(35) 120.8(3) yes . . . C(31) C(30) C(35) 118.0(3) yes . . . O(3) C(31) C(30) 121.5(3) yes . . . O(3) C(31) C(32) 116.1(3) yes . . . C(30) C(31) C(32) 121.6(3) yes . . . C(31) C(32) C(33) 117.6(3) yes . . . C(31) C(32) C(36) 120.9(3) yes . . . C(33) C(32) C(36) 121.5(3) yes . . . C(32) C(33) C(34) 123.2(3) yes . . . C(33) C(34) C(35) 117.6(3) yes . . . C(33) C(34) C(40) 122.3(3) yes . . . C(35) C(34) C(40) 120.1(3) yes . . . O(4) C(35) C(30) 125.1(4) yes . . . O(4) C(35) C(34) 111.7(4) yes . . . C(30) C(35) C(34) 121.9(3) yes . . . C(32) C(36) C(37) 109.6(3) yes . . . C(32) C(36) C(38) 110.6(4) yes . . . C(32) C(36) C(39) 110.8(4) yes . . . C(37) C(36) C(38) 103.2(5) yes . . . C(37) C(36) C(39) 111.0(4) yes . . . C(38) C(36) C(39) 111.2(4) yes . . . C(34) C(40) C(41) 109.5(3) yes . . . C(34) C(40) C(42) 111.7(4) yes . . . C(34) C(40) C(43) 109.8(3) yes . . . C(41) C(40) C(42) 106.5(4) yes . . . C(41) C(40) C(43) 110.0(4) yes . . . C(42) C(40) C(43) 109.3(4) yes . . . Nb(1) C(44) C(45) 93.17(17) yes . . . C(44) C(45) C(46) 122.1(3) yes . . . C(44) C(45) C(50) 119.9(3) yes . . . C(46) C(45) C(50) 117.9(3) yes . . . C(45) C(46) C(47) 120.7(4) yes . . . C(46) C(47) C(48) 120.6(4) yes . . . C(47) C(48) C(49) 119.4(3) yes . . . C(48) C(49) C(50) 120.3(4) yes . . . C(45) C(50) C(49) 121.0(3) yes . . . Nb(1) C(51) C(52) 117.0(2) yes . . . C(51) C(52) C(53) 120.7(3) yes . . . C(51) C(52) C(57) 121.4(3) yes . . . C(53) C(52) C(57) 117.9(3) yes . . . C(52) C(53) C(54) 121.0(3) yes . . . C(53) C(54) C(55) 120.6(4) yes . . . C(54) C(55) C(56) 119.5(4) yes . . . C(55) C(56) C(57) 120.1(4) yes . . . C(52) C(57) C(56) 120.9(3) yes . . . Nb(1) C(58) C(59) 126.62(19) yes . . . C(58) C(59) C(60) 121.1(4) yes . . . C(58) C(59) C(64) 121.2(4) yes . . . C(60) C(59) C(64) 117.6(4) yes . . . C(59) C(60) C(61) 120.5(5) yes . . . C(60) C(61) C(62) 120.4(5) yes . . . C(61) C(62) C(63) 119.3(5) yes . . . C(62) C(63) C(64) 121.2(5) yes . . . C(59) C(64) C(63) 121.0(4) yes . . . C(26) C(65) C(27) 68.5(8) yes . . . C(26) C(65) C(28) 59.4(6) yes . . . C(27) C(65) C(28) 125.1(11) yes . . . C(26) C(67) C(27) 57.4(6) yes . . . C(69) C(68) C(73) 116.9(6) yes . . . C(69) C(68) C(74) 121.5(8) yes . . . C(73) C(68) C(74) 121.5(8) yes . . . C(68) C(69) C(70) 122.3(7) yes . . . C(69) C(70) C(71) 120.0(7) yes . . . C(70) C(71) C(72) 120.9(8) yes . . . C(71) C(72) C(73) 119.2(7) yes . . . C(68) C(73) C(72) 120.6(6) yes . . . C(2) C(1) H(1) 105.586 no . . . C(16) C(1) H(1) 105.571 no . . . C(30) C(1) H(1) 105.576 no . . . C(4) C(5) H(5) 118.064 no . . . C(6) C(5) H(5) 118.082 no . . . C(2) C(7) H(7) 119.250 no . . . C(6) C(7) H(7) 119.238 no . . . C(8) C(9) H(9A) 109.466 no . . . C(8) C(9) H(9B) 109.476 no . . . C(8) C(9) H(9C) 109.475 no . . . H(9A) C(9) H(9B) 109.466 no . . . H(9A) C(9) H(9C) 109.468 no . . . H(9B) C(9) H(9C) 109.475 no . . . C(8) C(10) H(10A) 109.481 no . . . C(8) C(10) H(10B) 109.471 no . . . C(8) C(10) H(10C) 109.473 no . . . H(10A) C(10) H(10B) 109.471 no . . . H(10A) C(10) H(10C) 109.467 no . . . H(10B) C(10) H(10C) 109.465 no . . . C(8) C(11) H(11A) 109.472 no . . . C(8) C(11) H(11B) 109.468 no . . . C(8) C(11) H(11C) 109.470 no . . . H(11A) C(11) H(11B) 109.473 no . . . H(11A) C(11) H(11C) 109.474 no . . . H(11B) C(11) H(11C) 109.470 no . . . C(12) C(13) H(13A) 109.474 no . . . C(12) C(13) H(13B) 109.469 no . . . C(12) C(13) H(13C) 109.472 no . . . H(13A) C(13) H(13B) 109.477 no . . . H(13A) C(13) H(13C) 109.460 no . . . H(13B) C(13) H(13C) 109.476 no . . . C(12) C(14) H(14A) 109.466 no . . . C(12) C(14) H(14B) 109.478 no . . . C(12) C(14) H(14C) 109.462 no . . . H(14A) C(14) H(14B) 109.483 no . . . H(14A) C(14) H(14C) 109.468 no . . . H(14B) C(14) H(14C) 109.470 no . . . C(12) C(15) H(15A) 109.468 no . . . C(12) C(15) H(15B) 109.473 no . . . C(12) C(15) H(15C) 109.471 no . . . H(15A) C(15) H(15B) 109.467 no . . . H(15A) C(15) H(15C) 109.476 no . . . H(15B) C(15) H(15C) 109.473 no . . . C(18) C(19) H(19) 118.076 no . . . C(20) C(19) H(19) 118.070 no . . . C(16) C(21) H(21) 119.074 no . . . C(20) C(21) H(21) 119.068 no . . . C(22) C(23) H(23A) 109.465 no . . . C(22) C(23) H(23B) 109.482 no . . . C(22) C(23) H(23C) 109.475 no . . . H(23A) C(23) H(23B) 109.467 no . . . H(23A) C(23) H(23C) 109.468 no . . . H(23B) C(23) H(23C) 109.469 no . . . C(22) C(24) H(24A) 109.461 no . . . C(22) C(24) H(24B) 109.472 no . . . C(22) C(24) H(24C) 109.474 no . . . H(24A) C(24) H(24B) 109.458 no . . . H(24A) C(24) H(24C) 109.470 no . . . H(24B) C(24) H(24C) 109.492 no . . . C(22) C(25) H(25A) 109.461 no . . . C(22) C(25) H(25B) 109.469 no . . . C(22) C(25) H(25C) 109.472 no . . . H(25A) C(25) H(25B) 109.466 no . . . H(25A) C(25) H(25C) 109.478 no . . . H(25B) C(25) H(25C) 109.480 no . . . C(32) C(33) H(33) 118.400 no . . . C(34) C(33) H(33) 118.410 no . . . C(36) C(37) H(37A) 109.480 no . . . C(36) C(37) H(37B) 109.485 no . . . C(36) C(37) H(37C) 109.474 no . . . H(37A) C(37) H(37B) 109.465 no . . . H(37A) C(37) H(37C) 109.466 no . . . H(37B) C(37) H(37C) 109.457 no . . . C(36) C(38) H(38A) 109.476 no . . . C(36) C(38) H(38B) 109.468 no . . . C(36) C(38) H(38C) 109.474 no . . . H(38A) C(38) H(38B) 109.475 no . . . H(38A) C(38) H(38C) 109.477 no . . . H(38B) C(38) H(38C) 109.458 no . . . C(36) C(39) H(39A) 109.473 no . . . C(36) C(39) H(39B) 109.481 no . . . C(36) C(39) H(39C) 109.474 no . . . H(39A) C(39) H(39B) 109.478 no . . . H(39A) C(39) H(39C) 109.457 no . . . H(39B) C(39) H(39C) 109.464 no . . . C(40) C(41) H(41A) 109.473 no . . . C(40) C(41) H(41B) 109.476 no . . . C(40) C(41) H(41C) 109.473 no . . . H(41A) C(41) H(41B) 109.470 no . . . H(41A) C(41) H(41C) 109.464 no . . . H(41B) C(41) H(41C) 109.470 no . . . C(40) C(42) H(42A) 109.474 no . . . C(40) C(42) H(42B) 109.467 no . . . C(40) C(42) H(42C) 109.474 no . . . H(42A) C(42) H(42B) 109.466 no . . . H(42A) C(42) H(42C) 109.488 no . . . H(42B) C(42) H(42C) 109.459 no . . . C(40) C(43) H(43A) 109.475 no . . . C(40) C(43) H(43B) 109.470 no . . . C(40) C(43) H(43C) 109.471 no . . . H(43A) C(43) H(43B) 109.466 no . . . H(43A) C(43) H(43C) 109.470 no . . . H(43B) C(43) H(43C) 109.474 no . . . Nb(1) C(44) H(44A) 113.066 no . . . Nb(1) C(44) H(44B) 113.073 no . . . C(45) C(44) H(44A) 113.078 no . . . C(45) C(44) H(44B) 113.079 no . . . H(44A) C(44) H(44B) 110.464 no . . . C(45) C(46) H(46) 119.639 no . . . C(47) C(46) H(46) 119.644 no . . . C(46) C(47) H(47) 119.700 no . . . C(48) C(47) H(47) 119.708 no . . . C(47) C(48) H(48) 120.280 no . . . C(49) C(48) H(48) 120.271 no . . . C(48) C(49) H(49) 119.832 no . . . C(50) C(49) H(49) 119.833 no . . . C(45) C(50) H(50) 119.505 no . . . C(49) C(50) H(50) 119.494 no . . . Nb(1) C(51) H(51A) 108.063 no . . . Nb(1) C(51) H(51B) 108.064 no . . . C(52) C(51) H(51A) 108.048 no . . . C(52) C(51) H(51B) 108.054 no . . . H(51A) C(51) H(51B) 107.267 no . . . C(52) C(53) H(53) 119.480 no . . . C(54) C(53) H(53) 119.493 no . . . C(53) C(54) H(54) 119.724 no . . . C(55) C(54) H(54) 119.722 no . . . C(54) C(55) H(55) 120.251 no . . . C(56) C(55) H(55) 120.254 no . . . C(55) C(56) H(56) 119.967 no . . . C(57) C(56) H(56) 119.956 no . . . C(52) C(57) H(57) 119.534 no . . . C(56) C(57) H(57) 119.533 no . . . Nb(1) C(58) H(58A) 105.659 no . . . Nb(1) C(58) H(58B) 105.653 no . . . C(59) C(58) H(58A) 105.653 no . . . C(59) C(58) H(58B) 105.662 no . . . H(58A) C(58) H(58B) 106.132 no . . . C(59) C(60) H(60) 119.758 no . . . C(61) C(60) H(60) 119.743 no . . . C(60) C(61) H(61) 119.812 no . . . C(62) C(61) H(61) 119.807 no . . . C(61) C(62) H(62) 120.365 no . . . C(63) C(62) H(62) 120.358 no . . . C(62) C(63) H(63) 119.386 no . . . C(64) C(63) H(63) 119.405 no . . . C(59) C(64) H(64) 119.520 no . . . C(63) C(64) H(64) 119.514 no . . . C(68) C(69) H(69) 118.865 no . . . C(70) C(69) H(69) 118.873 no . . . C(69) C(70) H(70) 119.985 no . . . C(71) C(70) H(70) 119.992 no . . . C(70) C(71) H(71) 119.573 no . . . C(72) C(71) H(71) 119.556 no . . . C(71) C(72) H(72) 120.408 no . . . C(73) C(72) H(72) 120.404 no . . . C(68) C(73) H(73) 119.714 no . . . C(72) C(73) H(73) 119.722 no . . . C(68) C(74) H(74A) 109.471 no . . . C(68) C(74) H(74B) 109.473 no . . . C(68) C(74) H(74C) 109.477 no . . . H(74A) C(74) H(74B) 109.465 no . . . H(74A) C(74) H(74C) 109.462 no . . . H(74B) C(74) H(74C) 109.480 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Nb(1) O(2) C(17) 79.7(3) no . . . . O(2) Nb(1) O(1) C(3) -45.06(19) no . . . . O(1) Nb(1) C(44) C(45) 91.51(15) no . . . . C(44) Nb(1) O(1) C(3) 90.37(19) no . . . . O(1) Nb(1) C(51) C(52) 162.68(16) no . . . . C(51) Nb(1) O(1) C(3) -150.67(19) no . . . . O(1) Nb(1) C(58) C(59) 110.8(3) no . . . . C(58) Nb(1) O(1) C(3) 19.2(3) no . . . . O(2) Nb(1) C(44) C(45) 172.55(10) no . . . . C(44) Nb(1) O(2) C(17) -1.3(3) no . . . . O(2) Nb(1) C(51) C(52) 73.98(19) no . . . . C(51) Nb(1) O(2) C(17) 177.7(3) no . . . . O(2) Nb(1) C(58) C(59) 176.3(3) no . . . . C(58) Nb(1) O(2) C(17) -73.8(3) no . . . . C(44) Nb(1) C(51) C(52) -106.89(18) no . . . . C(51) Nb(1) C(44) C(45) -6.3(2) no . . . . C(44) Nb(1) C(58) C(59) 39.1(3) no . . . . C(58) Nb(1) C(44) C(45) -116.29(16) no . . . . C(51) Nb(1) C(58) C(59) -80.0(3) no . . . . C(58) Nb(1) C(51) C(52) -12.0(2) no . . . . Nb(1) O(1) C(3) C(2) -21.2(4) no . . . . Nb(1) O(1) C(3) C(4) 156.97(16) no . . . . Nb(1) O(2) C(17) C(16) -17.0(5) no . . . . Nb(1) O(2) C(17) C(18) 164.40(17) no . . . . C(2) C(1) C(16) C(17) -80.9(3) no . . . . C(2) C(1) C(16) C(21) 93.2(3) no . . . . C(16) C(1) C(2) C(3) 96.2(3) no . . . . C(16) C(1) C(2) C(7) -77.9(3) no . . . . C(2) C(1) C(30) C(31) -164.80(18) no . . . . C(2) C(1) C(30) C(35) 24.6(3) no . . . . C(30) C(1) C(2) C(3) -132.0(2) no . . . . C(30) C(1) C(2) C(7) 54.0(3) no . . . . C(16) C(1) C(30) C(31) -38.0(4) no . . . . C(16) C(1) C(30) C(35) 151.5(3) no . . . . C(30) C(1) C(16) C(17) 148.2(3) no . . . . C(30) C(1) C(16) C(21) -37.7(4) no . . . . C(1) C(2) C(3) O(1) 6.0(4) no . . . . C(1) C(2) C(3) C(4) -172.13(18) no . . . . C(1) C(2) C(7) C(6) 176.39(19) no . . . . C(3) C(2) C(7) C(6) 2.2(4) no . . . . C(7) C(2) C(3) O(1) -179.94(19) no . . . . C(7) C(2) C(3) C(4) 1.9(4) no . . . . O(1) C(3) C(4) C(5) 177.79(18) no . . . . O(1) C(3) C(4) C(8) -7.4(4) no . . . . C(2) C(3) C(4) C(5) -4.1(4) no . . . . C(2) C(3) C(4) C(8) 170.71(19) no . . . . C(3) C(4) C(5) C(6) 2.4(4) no . . . . C(3) C(4) C(8) C(9) 57.3(3) no . . . . C(3) C(4) C(8) C(10) -63.6(3) no . . . . C(3) C(4) C(8) C(11) 178.11(19) no . . . . C(5) C(4) C(8) C(9) -128.1(3) no . . . . C(5) C(4) C(8) C(10) 111.0(3) no . . . . C(5) C(4) C(8) C(11) -7.3(3) no . . . . C(8) C(4) C(5) C(6) -172.5(2) no . . . . C(4) C(5) C(6) C(7) 1.5(4) no . . . . C(4) C(5) C(6) C(12) 179.0(2) no . . . . C(5) C(6) C(7) C(2) -3.8(4) no . . . . C(5) C(6) C(12) C(13) 14.4(4) no . . . . C(5) C(6) C(12) C(14) -108.2(3) no . . . . C(5) C(6) C(12) C(15) 133.2(3) no . . . . C(7) C(6) C(12) C(13) -168.2(2) no . . . . C(7) C(6) C(12) C(14) 69.2(3) no . . . . C(7) C(6) C(12) C(15) -49.4(3) no . . . . C(12) C(6) C(7) C(2) 178.6(2) no . . . . C(1) C(16) C(17) O(2) -6.3(4) no . . . . C(1) C(16) C(17) C(18) 172.3(3) no . . . . C(1) C(16) C(21) C(20) -175.8(3) no . . . . C(17) C(16) C(21) C(20) -1.7(5) no . . . . C(21) C(16) C(17) O(2) 179.6(3) no . . . . C(21) C(16) C(17) C(18) -1.8(4) no . . . . O(2) C(17) C(18) C(19) -178.2(3) no . . . . O(2) C(17) C(18) C(22) 3.0(4) no . . . . C(16) C(17) C(18) C(19) 3.3(4) no . . . . C(16) C(17) C(18) C(22) -175.6(3) no . . . . C(17) C(18) C(19) C(20) -1.4(5) no . . . . C(17) C(18) C(22) C(23) 55.8(4) no . . . . C(17) C(18) C(22) C(24) -66.7(4) no . . . . C(17) C(18) C(22) C(25) 174.7(3) no . . . . C(19) C(18) C(22) C(23) -123.0(3) no . . . . C(19) C(18) C(22) C(24) 114.5(3) no . . . . C(19) C(18) C(22) C(25) -4.0(4) no . . . . C(22) C(18) C(19) C(20) 177.5(3) no . . . . C(18) C(19) C(20) C(21) -2.0(5) no . . . . C(18) C(19) C(20) C(26) 179.0(3) no . . . . C(19) C(20) C(21) C(16) 3.5(5) no . . . . C(19) C(20) C(26) C(27) -136.1(3) no . . . . C(19) C(20) C(26) C(28) 107.3(3) no . . . . C(19) C(20) C(26) C(29) -23.6(4) no . . . . C(19) C(20) C(26) C(65) 171.3(3) no . . . . C(19) C(20) C(26) C(66) 64.9(4) no . . . . C(19) C(20) C(26) C(67) -60.8(4) no . . . . C(21) C(20) C(26) C(27) 44.9(4) no . . . . C(21) C(20) C(26) C(28) -71.6(4) no . . . . C(21) C(20) C(26) C(29) 157.5(3) no . . . . C(21) C(20) C(26) C(65) -7.7(4) no . . . . C(21) C(20) C(26) C(66) -114.0(3) no . . . . C(21) C(20) C(26) C(67) 120.2(3) no . . . . C(26) C(20) C(21) C(16) -177.5(3) no . . . . C(20) C(26) C(27) C(65) -103.6(3) no . . . . C(20) C(26) C(27) C(67) 103.8(3) no . . . . C(20) C(26) C(28) C(65) 104.4(3) no . . . . C(20) C(26) C(65) C(27) 96.2(5) no . . . . C(20) C(26) C(65) C(28) -101.5(4) no . . . . C(20) C(26) C(67) C(27) -104.2(4) no . . . . C(27) C(26) C(28) C(65) -13.9(4) no . . . . C(28) C(26) C(27) C(65) 15.8(4) no . . . . C(28) C(26) C(27) C(67) -136.8(4) no . . . . C(29) C(26) C(27) C(65) 136.5(4) no . . . . C(29) C(26) C(27) C(67) -16.1(4) no . . . . C(27) C(26) C(65) C(28) 162.3(7) no . . . . C(65) C(26) C(27) C(67) -152.6(7) no . . . . C(66) C(26) C(27) C(65) 44.3(8) no . . . . C(66) C(26) C(27) C(67) -108.3(8) no . . . . C(67) C(26) C(27) C(65) 152.6(7) no . . . . C(29) C(26) C(28) C(65) -125.6(4) no . . . . C(28) C(26) C(65) C(27) -162.3(7) no . . . . C(66) C(26) C(28) C(65) -165.3(8) no . . . . C(28) C(26) C(67) C(27) 92.8(9) no . . . . C(67) C(26) C(28) C(65) -92.8(10) no . . . . C(29) C(26) C(65) C(27) -65.2(9) no . . . . C(29) C(26) C(65) C(28) 97.0(8) no . . . . C(29) C(26) C(67) C(27) 151.7(11) no . . . . C(66) C(26) C(65) C(27) -152.7(5) no . . . . C(66) C(26) C(65) C(28) 9.6(5) no . . . . C(65) C(26) C(67) C(27) 22.5(7) no . . . . C(67) C(26) C(65) C(27) -28.5(9) no . . . . C(67) C(26) C(65) C(28) 133.8(7) no . . . . C(66) C(26) C(67) C(27) 136.5(6) no . . . . C(26) C(27) C(65) C(28) -18.7(8) no . . . . C(65) C(27) C(67) C(26) -25.7(8) no . . . . C(67) C(27) C(65) C(26) 22.6(7) no . . . . C(67) C(27) C(65) C(28) 3.9(13) no . . . . C(26) C(28) C(65) C(27) 20.2(8) no . . . . C(1) C(30) C(31) O(3) -6.8(4) no . . . . C(1) C(30) C(31) C(32) -176.0(2) no . . . . C(1) C(30) C(35) O(4) 7.6(4) no . . . . C(1) C(30) C(35) C(34) 173.3(2) no . . . . C(31) C(30) C(35) O(4) -163.2(3) no . . . . C(31) C(30) C(35) C(34) 2.5(4) no . . . . C(35) C(30) C(31) O(3) 164.0(3) no . . . . C(35) C(30) C(31) C(32) -5.2(4) no . . . . O(3) C(31) C(32) C(33) -165.2(3) no . . . . O(3) C(31) C(32) C(36) 15.8(4) no . . . . C(30) C(31) C(32) C(33) 4.5(4) no . . . . C(30) C(31) C(32) C(36) -174.4(3) no . . . . C(31) C(32) C(33) C(34) -1.1(4) no . . . . C(31) C(32) C(36) C(37) -71.5(4) no . . . . C(31) C(32) C(36) C(38) 175.3(3) no . . . . C(31) C(32) C(36) C(39) 51.4(4) no . . . . C(33) C(32) C(36) C(37) 109.5(3) no . . . . C(33) C(32) C(36) C(38) -3.7(4) no . . . . C(33) C(32) C(36) C(39) -127.6(3) no . . . . C(36) C(32) C(33) C(34) 177.8(3) no . . . . C(32) C(33) C(34) C(35) -1.4(5) no . . . . C(32) C(33) C(34) C(40) 178.3(3) no . . . . C(33) C(34) C(35) O(4) 168.2(3) no . . . . C(33) C(34) C(35) C(30) 0.7(4) no . . . . C(33) C(34) C(40) C(41) -115.2(3) no . . . . C(33) C(34) C(40) C(42) 2.5(4) no . . . . C(33) C(34) C(40) C(43) 123.9(3) no . . . . C(35) C(34) C(40) C(41) 64.5(4) no . . . . C(35) C(34) C(40) C(42) -177.8(3) no . . . . C(35) C(34) C(40) C(43) -56.4(4) no . . . . C(40) C(34) C(35) O(4) -11.5(4) no . . . . C(40) C(34) C(35) C(30) -179.0(3) no . . . . Nb(1) C(44) C(45) C(46) 94.0(3) no . . . . Nb(1) C(44) C(45) C(50) -83.1(3) no . . . . C(44) C(45) C(46) C(47) -177.1(3) no . . . . C(44) C(45) C(50) C(49) 177.4(3) no . . . . C(46) C(45) C(50) C(49) 0.2(4) no . . . . C(50) C(45) C(46) C(47) 0.0(4) no . . . . C(45) C(46) C(47) C(48) 0.1(5) no . . . . C(46) C(47) C(48) C(49) -0.4(5) no . . . . C(47) C(48) C(49) C(50) 0.6(5) no . . . . C(48) C(49) C(50) C(45) -0.5(5) no . . . . Nb(1) C(51) C(52) C(53) -73.6(3) no . . . . Nb(1) C(51) C(52) C(57) 105.9(3) no . . . . C(51) C(52) C(53) C(54) 178.0(3) no . . . . C(51) C(52) C(57) C(56) -179.9(3) no . . . . C(53) C(52) C(57) C(56) -0.5(5) no . . . . C(57) C(52) C(53) C(54) -1.5(5) no . . . . C(52) C(53) C(54) C(55) 1.7(5) no . . . . C(53) C(54) C(55) C(56) 0.1(6) no . . . . C(54) C(55) C(56) C(57) -2.0(6) no . . . . C(55) C(56) C(57) C(52) 2.2(5) no . . . . Nb(1) C(58) C(59) C(60) 80.0(4) no . . . . Nb(1) C(58) C(59) C(64) -100.1(3) no . . . . C(58) C(59) C(60) C(61) -178.8(3) no . . . . C(58) C(59) C(64) C(63) 179.2(3) no . . . . C(60) C(59) C(64) C(63) -0.9(5) no . . . . C(64) C(59) C(60) C(61) 1.3(5) no . . . . C(59) C(60) C(61) C(62) -0.3(6) no . . . . C(60) C(61) C(62) C(63) -1.0(6) no . . . . C(61) C(62) C(63) C(64) 1.5(7) no . . . . C(62) C(63) C(64) C(59) -0.5(6) no . . . . C(69) C(68) C(73) C(72) 1.1(9) no . . . . C(73) C(68) C(69) C(70) -1.9(9) no . . . . C(74) C(68) C(69) C(70) -178.6(6) no . . . . C(74) C(68) C(73) C(72) 177.9(6) no . . . . C(68) C(69) C(70) C(71) 3.6(12) no . . . . C(69) C(70) C(71) C(72) -4.6(12) no . . . . C(70) C(71) C(72) C(73) 3.9(10) no . . . . C(71) C(72) C(73) C(68) -2.2(9) no . . . . #===END #============================================================================== data__O3CNbBn-Complex-5 _database_code_depnum_ccdc_archive 'CCDC 789695' #TrackingRef '- Kawaguchi_CIF_rivised.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C50 H67 Nb O3' _chemical_formula_moiety 'C50 H67 Nb O3' _chemical_formula_weight 808.98 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 14.679(5) _cell_length_b 11.916(4) _cell_length_c 27.664(9) _cell_angle_alpha 90.0000 _cell_angle_beta 110.455(5) _cell_angle_gamma 90.0000 _cell_volume 4534(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11763 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 173 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728.00 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.941 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 173 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 35050 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 10347 _reflns_number_gt 8895 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1779 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 10347 _refine_ls_number_parameters 481 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0894P)^2^+5.7055P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.130 _refine_diff_density_min -0.580 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' 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' #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Nb(1) Nb 0.81056(2) 0.81326(2) 0.787006(11) 0.02435(11) Uani 1.0 4 d . . . O(1) O 0.75025(17) 0.7191(2) 0.72809(9) 0.0274(5) Uani 1.0 4 d . . . O(2) O 0.94563(17) 0.7668(2) 0.81478(9) 0.0307(6) Uani 1.0 4 d . . . O(3) O 0.79261(18) 0.8626(2) 0.84831(9) 0.0298(5) Uani 1.0 4 d . . . C(1) C 0.7742(3) 0.6557(3) 0.82077(12) 0.0243(7) Uani 1.0 4 d . . . C(2) C 0.7135(3) 0.5803(3) 0.77753(12) 0.0247(7) Uani 1.0 4 d . . . C(3) C 0.7030(3) 0.6194(3) 0.72814(13) 0.0252(7) Uani 1.0 4 d . . . C(4) C 0.6490(3) 0.5626(3) 0.68286(13) 0.0298(7) Uani 1.0 4 d . . . C(5) C 0.6059(3) 0.4617(3) 0.68966(14) 0.0315(8) Uani 1.0 4 d . . . C(6) C 0.6142(3) 0.4188(3) 0.73779(14) 0.0304(7) Uani 1.0 4 d . . . C(7) C 0.6694(3) 0.4788(3) 0.78170(13) 0.0293(7) Uani 1.0 4 d . . . C(8) C 0.8798(3) 0.6119(3) 0.84786(12) 0.0243(7) Uani 1.0 4 d . . . C(9) C 0.9601(3) 0.6729(3) 0.84652(13) 0.0269(7) Uani 1.0 4 d . . . C(10) C 1.0552(3) 0.6422(3) 0.87719(14) 0.0316(8) Uani 1.0 4 d . . . C(11) C 1.0665(3) 0.5427(3) 0.90405(15) 0.0352(8) Uani 1.0 4 d . . . C(12) C 0.9885(3) 0.4739(3) 0.90374(14) 0.0313(8) Uani 1.0 4 d . . . C(13) C 0.8957(3) 0.5127(3) 0.87629(13) 0.0285(7) Uani 1.0 4 d . . . C(14) C 0.7327(3) 0.6893(3) 0.86167(12) 0.0236(6) Uani 1.0 4 d . . . C(15) C 0.7502(3) 0.8010(3) 0.87709(13) 0.0254(7) Uani 1.0 4 d . . . C(16) C 0.7263(3) 0.8481(3) 0.91754(13) 0.0283(7) Uani 1.0 4 d . . . C(17) C 0.6769(3) 0.7779(4) 0.93977(14) 0.0325(8) Uani 1.0 4 d . . . C(18) C 0.6526(3) 0.6674(4) 0.92427(14) 0.0345(8) Uani 1.0 4 d . . . C(19) C 0.6834(3) 0.6228(3) 0.88596(14) 0.0309(8) Uani 1.0 4 d . . . C(20) C 0.7477(3) 0.9677(3) 0.74252(16) 0.0378(9) Uani 1.0 4 d . . . C(21) C 0.8489(3) 0.9901(3) 0.74831(15) 0.0349(8) Uani 1.0 4 d . . . C(22) C 0.8919(3) 0.9362(4) 0.71625(15) 0.0417(9) Uani 1.0 4 d . . . C(23) C 0.9907(4) 0.9472(5) 0.72545(18) 0.0522(11) Uani 1.0 4 d . . . C(24) C 1.0490(4) 1.0079(5) 0.7669(2) 0.0540(12) Uani 1.0 4 d . . . C(25) C 1.0090(4) 1.0587(4) 0.7999(2) 0.0563(12) Uani 1.0 4 d . . . C(26) C 0.9112(4) 1.0483(4) 0.79155(17) 0.0451(10) Uani 1.0 4 d . . . C(27) C 0.6353(3) 0.6100(4) 0.62925(14) 0.0362(8) Uani 1.0 4 d . . . C(28) C 0.5788(4) 0.7210(4) 0.62240(16) 0.0483(11) Uani 1.0 4 d . . . C(29) C 0.7345(3) 0.6321(4) 0.62351(15) 0.0409(9) Uani 1.0 4 d . . . C(30) C 0.5786(4) 0.5298(5) 0.58579(15) 0.0526(12) Uani 1.0 4 d . . . C(31) C 0.5601(3) 0.3116(3) 0.74327(15) 0.0365(9) Uani 1.0 4 d . . . C(32) C 0.5470(4) 0.2301(4) 0.6985(2) 0.0601(13) Uani 1.0 4 d . . . C(33) C 0.6145(5) 0.2489(5) 0.7935(2) 0.0742(19) Uani 1.0 4 d . . . C(34) C 0.4595(4) 0.3460(5) 0.7432(3) 0.0599(14) Uani 1.0 4 d . . . C(35) C 1.1424(3) 0.7212(4) 0.88222(18) 0.0435(10) Uani 1.0 4 d . . . C(36) C 1.1559(4) 0.7369(4) 0.8302(2) 0.0538(12) Uani 1.0 4 d . . . C(37) C 1.1225(4) 0.8349(4) 0.90230(18) 0.0506(11) Uani 1.0 4 d . . . C(38) C 1.2367(4) 0.6767(5) 0.9215(3) 0.079(2) Uani 1.0 4 d . . . C(39) C 1.0058(3) 0.3598(4) 0.93217(17) 0.0434(10) Uani 1.0 4 d . . . C(40) C 1.1025(19) 0.357(3) 0.9798(10) 0.114(8) Uiso 0.4000 4 d . . . C(41) C 1.0720(6) 0.3742(7) 0.9901(3) 0.0437(17) Uiso 0.6000 4 d . . . C(42) C 0.9146(10) 0.3370(12) 0.9549(6) 0.057(3) Uiso 0.4000 4 d . . . C(43) C 0.9137(8) 0.3014(10) 0.9289(5) 0.076(3) Uiso 0.6000 4 d . . . C(44) C 0.9950(15) 0.2671(17) 0.8954(8) 0.091(5) Uiso 0.4000 4 d . . . C(45) C 1.0648(7) 0.2835(8) 0.9064(4) 0.059(2) Uiso 0.6000 4 d . . . C(46) C 0.7547(3) 0.9686(4) 0.93594(14) 0.0349(8) Uani 1.0 4 d . . . C(47) C 0.7059(4) 1.0516(4) 0.89196(16) 0.0465(10) Uani 1.0 4 d . . . C(48) C 0.7228(4) 0.9995(4) 0.98102(16) 0.0482(11) Uani 1.0 4 d . . . C(49) C 0.8662(4) 0.9801(4) 0.95392(18) 0.0477(10) Uani 1.0 4 d . . . C(50) C 0.5943(4) 0.5957(5) 0.94954(18) 0.0513(12) Uani 1.0 4 d . . . C(51) C 0.5741(9) 0.4843(11) 0.9294(5) 0.084(3) Uiso 0.6000 4 d . . . C(52) C 0.6391(11) 0.4613(12) 0.9536(6) 0.062(4) Uiso 0.4000 4 d . . . C(53) C 0.6516(6) 0.5961(7) 1.0104(3) 0.0456(16) Uiso 0.6000 4 d . . . C(54) C 0.588(2) 0.632(3) 0.9953(11) 0.139(9) Uiso 0.4000 4 d . . . C(55) C 0.4994(7) 0.6672(8) 0.9467(4) 0.061(2) Uiso 0.6000 4 d . . . C(56) C 0.4967(12) 0.5556(15) 0.9070(7) 0.079(5) Uiso 0.4000 4 d . . . H(5) H 0.5691 0.4204 0.6598 0.0378 Uiso 1.0 4 calc R . . H(7) H 0.6770 0.4500 0.8149 0.0351 Uiso 1.0 4 calc R . . H(11) H 1.1306 0.5194 0.9239 0.0423 Uiso 1.0 4 calc R . . H(13) H 0.8412 0.4703 0.8769 0.0342 Uiso 1.0 4 calc R . . H(17) H 0.6586 0.8066 0.9671 0.0389 Uiso 1.0 4 calc R . . H(19) H 0.6706 0.5463 0.8763 0.0371 Uiso 1.0 4 calc R . . H(20A) H 0.7038 0.9542 0.7066 0.0453 Uiso 1.0 4 calc R . . H(20B) H 0.7193 1.0212 0.7607 0.0453 Uiso 1.0 4 calc R . . H(22) H 0.8529 0.8920 0.6881 0.0501 Uiso 1.0 4 calc R . . H(23) H 1.0182 0.9123 0.7029 0.0627 Uiso 1.0 4 calc R . . H(24) H 1.1165 1.0152 0.7729 0.0648 Uiso 1.0 4 calc R . . H(25) H 1.0492 1.1009 0.8286 0.0676 Uiso 1.0 4 calc R . . H(26) H 0.8854 1.0809 0.8153 0.0542 Uiso 1.0 4 calc R . . H(28A) H 0.5141 0.7067 0.6239 0.0580 Uiso 1.0 4 calc R . . H(28B) H 0.5724 0.7542 0.5889 0.0580 Uiso 1.0 4 calc R . . H(28C) H 0.6141 0.7731 0.6501 0.0580 Uiso 1.0 4 calc R . . H(29A) H 0.7711 0.6869 0.6494 0.0490 Uiso 1.0 4 calc R . . H(29B) H 0.7243 0.6617 0.5889 0.0490 Uiso 1.0 4 calc R . . H(29C) H 0.7713 0.5618 0.6285 0.0490 Uiso 1.0 4 calc R . . H(30A) H 0.5686 0.5652 0.5523 0.0631 Uiso 1.0 4 calc R . . H(30B) H 0.5154 0.5128 0.5888 0.0631 Uiso 1.0 4 calc R . . H(30C) H 0.6156 0.4602 0.5885 0.0631 Uiso 1.0 4 calc R . . H(32A) H 0.5208 0.1588 0.7056 0.0721 Uiso 1.0 4 calc R . . H(32B) H 0.6100 0.2168 0.6946 0.0721 Uiso 1.0 4 calc R . . H(32C) H 0.5018 0.2625 0.6665 0.0721 Uiso 1.0 4 calc R . . H(33A) H 0.5748 0.1859 0.7975 0.0891 Uiso 1.0 4 calc R . . H(33B) H 0.6271 0.3002 0.8228 0.0891 Uiso 1.0 4 calc R . . H(33C) H 0.6764 0.2206 0.7923 0.0891 Uiso 1.0 4 calc R . . H(34A) H 0.4665 0.3868 0.7751 0.0719 Uiso 1.0 4 calc R . . H(34B) H 0.4198 0.2787 0.7411 0.0719 Uiso 1.0 4 calc R . . H(34C) H 0.4277 0.3944 0.7134 0.0719 Uiso 1.0 4 calc R . . H(36A) H 1.2007 0.7994 0.8326 0.0646 Uiso 1.0 4 calc R . . H(36B) H 1.0929 0.7534 0.8035 0.0646 Uiso 1.0 4 calc R . . H(36C) H 1.1827 0.6680 0.8211 0.0646 Uiso 1.0 4 calc R . . H(37A) H 1.1169 0.8251 0.9363 0.0608 Uiso 1.0 4 calc R . . H(37B) H 1.0616 0.8659 0.8783 0.0608 Uiso 1.0 4 calc R . . H(37C) H 1.1761 0.8865 0.9051 0.0608 Uiso 1.0 4 calc R . . H(38A) H 1.2540 0.6055 0.9092 0.0948 Uiso 1.0 4 calc R . . H(38B) H 1.2279 0.6647 0.9546 0.0948 Uiso 1.0 4 calc R . . H(38C) H 1.2889 0.7314 0.9259 0.0948 Uiso 1.0 4 calc R . . H(47A) H 0.7224 1.0314 0.8617 0.0558 Uiso 1.0 4 calc R . . H(47B) H 0.7291 1.1278 0.9030 0.0558 Uiso 1.0 4 calc R . . H(47C) H 0.6352 1.0486 0.8831 0.0558 Uiso 1.0 4 calc R . . H(48A) H 0.7543 0.9493 1.0101 0.0578 Uiso 1.0 4 calc R . . H(48B) H 0.6520 0.9919 0.9706 0.0578 Uiso 1.0 4 calc R . . H(48C) H 0.7415 1.0772 0.9914 0.0578 Uiso 1.0 4 calc R . . H(49A) H 0.8886 0.9581 0.9258 0.0572 Uiso 1.0 4 calc R . . H(49B) H 0.8962 0.9312 0.9838 0.0572 Uiso 1.0 4 calc R . . H(49C) H 0.8846 1.0582 0.9636 0.0572 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb(1) 0.02546(17) 0.02299(16) 0.02606(17) -0.00132(11) 0.01085(12) 0.00508(11) O(1) 0.0280(12) 0.0300(12) 0.0258(12) -0.0032(10) 0.0114(10) 0.0036(10) O(2) 0.0266(12) 0.0318(13) 0.0340(13) -0.0031(10) 0.0110(10) 0.0087(11) O(3) 0.0358(13) 0.0248(12) 0.0333(13) -0.0020(10) 0.0177(11) 0.0040(10) C(1) 0.0251(15) 0.0232(15) 0.0249(15) -0.0033(12) 0.0092(13) 0.0027(12) C(2) 0.0193(14) 0.0265(16) 0.0271(16) 0.0002(12) 0.0065(13) 0.0009(13) C(3) 0.0235(15) 0.0238(15) 0.0296(16) 0.0016(13) 0.0108(13) 0.0014(13) C(4) 0.0273(16) 0.0350(18) 0.0276(17) 0.0042(14) 0.0100(14) 0.0022(14) C(5) 0.0278(17) 0.0324(18) 0.0291(17) -0.0017(14) 0.0035(14) -0.0036(14) C(6) 0.0249(16) 0.0273(17) 0.0352(18) 0.0005(14) 0.0059(14) 0.0013(14) C(7) 0.0285(17) 0.0286(17) 0.0291(17) -0.0016(14) 0.0081(14) 0.0022(14) C(8) 0.0246(15) 0.0257(16) 0.0227(15) 0.0000(13) 0.0085(13) -0.0007(12) C(9) 0.0275(16) 0.0243(16) 0.0283(16) 0.0001(13) 0.0091(14) 0.0004(13) C(10) 0.0270(17) 0.0305(17) 0.0350(18) -0.0022(14) 0.0079(15) -0.0003(15) C(11) 0.0292(18) 0.0305(18) 0.041(2) 0.0023(15) 0.0058(16) 0.0042(16) C(12) 0.0340(18) 0.0255(17) 0.0308(17) 0.0032(14) 0.0067(15) 0.0031(14) C(13) 0.0300(17) 0.0253(16) 0.0294(17) -0.0024(14) 0.0092(14) 0.0013(13) C(14) 0.0221(15) 0.0251(15) 0.0236(15) -0.0003(13) 0.0080(12) 0.0047(13) C(15) 0.0235(15) 0.0273(16) 0.0261(16) -0.0012(13) 0.0096(13) 0.0039(13) C(16) 0.0285(17) 0.0322(17) 0.0230(16) 0.0037(14) 0.0077(14) 0.0021(13) C(17) 0.0308(17) 0.043(2) 0.0264(17) 0.0016(15) 0.0131(14) 0.0022(15) C(18) 0.0307(18) 0.045(2) 0.0321(18) -0.0043(16) 0.0158(15) 0.0083(16) C(19) 0.0301(17) 0.0301(18) 0.0343(18) -0.0059(14) 0.0134(15) 0.0041(15) C(20) 0.039(2) 0.0276(18) 0.046(3) 0.0021(15) 0.0145(17) 0.0127(16) C(21) 0.043(2) 0.0266(17) 0.0368(19) -0.0043(15) 0.0160(17) 0.0112(15) C(22) 0.051(3) 0.043(3) 0.035(2) -0.0093(19) 0.0202(18) 0.0046(17) C(23) 0.057(3) 0.060(3) 0.050(3) -0.006(3) 0.032(3) 0.003(3) C(24) 0.045(3) 0.058(3) 0.064(3) -0.017(3) 0.026(3) 0.004(3) C(25) 0.053(3) 0.049(3) 0.065(3) -0.014(3) 0.018(3) -0.010(3) C(26) 0.048(3) 0.039(3) 0.052(3) -0.0059(19) 0.022(2) -0.0039(19) C(27) 0.0346(19) 0.048(3) 0.0264(17) 0.0018(17) 0.0107(15) 0.0018(16) C(28) 0.048(3) 0.063(3) 0.032(2) 0.018(3) 0.0118(18) 0.016(2) C(29) 0.040(2) 0.055(3) 0.0317(19) -0.0011(19) 0.0176(17) -0.0029(18) C(30) 0.053(3) 0.074(4) 0.028(2) -0.015(3) 0.0110(19) -0.005(2) C(31) 0.0354(19) 0.0281(18) 0.038(2) -0.0094(15) 0.0029(16) 0.0028(15) C(32) 0.069(4) 0.039(3) 0.068(4) -0.018(3) 0.019(3) -0.014(3) C(33) 0.085(4) 0.043(3) 0.065(4) -0.028(3) -0.011(3) 0.019(3) C(34) 0.050(3) 0.049(3) 0.090(4) -0.017(3) 0.037(3) -0.003(3) C(35) 0.0262(18) 0.038(2) 0.058(3) -0.0051(16) 0.0040(18) 0.0048(19) C(36) 0.044(3) 0.045(3) 0.085(4) -0.009(2) 0.038(3) -0.009(3) C(37) 0.052(3) 0.047(3) 0.045(3) -0.018(2) 0.007(2) -0.006(2) C(38) 0.029(3) 0.065(4) 0.118(6) -0.014(3) -0.006(3) 0.031(4) C(39) 0.046(3) 0.0283(19) 0.049(3) 0.0043(17) 0.0078(19) 0.0095(17) C(46) 0.041(2) 0.037(2) 0.0279(17) -0.0002(16) 0.0130(16) -0.0019(15) C(47) 0.064(3) 0.033(2) 0.043(3) 0.011(2) 0.019(2) 0.0002(18) C(48) 0.061(3) 0.049(3) 0.037(2) -0.003(2) 0.020(2) -0.0116(19) C(49) 0.048(3) 0.042(3) 0.050(3) -0.0109(19) 0.013(2) -0.0096(19) C(50) 0.053(3) 0.064(3) 0.047(3) -0.015(3) 0.032(3) 0.009(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb(1) O(1) 1.921(3) yes . . Nb(1) O(2) 1.940(3) yes . . Nb(1) O(3) 1.898(3) yes . . Nb(1) C(1) 2.243(4) yes . . Nb(1) C(20) 2.227(4) yes . . O(1) C(3) 1.376(5) yes . . O(2) C(9) 1.392(5) yes . . O(3) C(15) 1.381(5) yes . . C(1) C(2) 1.513(5) yes . . C(1) C(8) 1.557(5) yes . . C(1) C(14) 1.515(6) yes . . C(2) C(3) 1.400(5) yes . . C(2) C(7) 1.395(5) yes . . C(3) C(4) 1.400(5) yes . . C(4) C(5) 1.402(6) yes . . C(4) C(27) 1.533(6) yes . . C(5) C(6) 1.391(6) yes . . C(6) C(7) 1.398(5) yes . . C(6) C(31) 1.541(6) yes . . C(8) C(9) 1.397(5) yes . . C(8) C(13) 1.394(5) yes . . C(9) C(10) 1.405(5) yes . . C(10) C(11) 1.378(6) yes . . C(10) C(35) 1.555(6) yes . . C(11) C(12) 1.406(6) yes . . C(12) C(13) 1.387(5) yes . . C(12) C(39) 1.547(6) yes . . C(14) C(15) 1.394(5) yes . . C(14) C(19) 1.393(6) yes . . C(15) C(16) 1.402(6) yes . . C(16) C(17) 1.384(6) yes . . C(16) C(46) 1.532(6) yes . . C(17) C(18) 1.392(6) yes . . C(18) C(19) 1.394(6) yes . . C(18) C(50) 1.539(7) yes . . C(20) C(21) 1.463(6) yes . . C(21) C(22) 1.410(7) yes . . C(21) C(26) 1.408(6) yes . . C(22) C(23) 1.387(7) yes . . C(23) C(24) 1.374(7) yes . . C(24) C(25) 1.386(9) yes . . C(25) C(26) 1.376(8) yes . . C(27) C(28) 1.537(7) yes . . C(27) C(29) 1.542(7) yes . . C(27) C(30) 1.534(6) yes . . C(31) C(32) 1.533(7) yes . . C(31) C(33) 1.533(7) yes . . C(31) C(34) 1.532(7) yes . . C(35) C(36) 1.532(9) yes . . C(35) C(37) 1.531(7) yes . . C(35) C(38) 1.525(6) yes . . C(39) C(40) 1.56(3) yes . . C(39) C(41) 1.567(9) yes . . C(39) C(42) 1.686(18) yes . . C(39) C(43) 1.495(13) yes . . C(39) C(44) 1.47(2) yes . . C(39) C(45) 1.586(12) yes . . C(43) C(44) 1.80(3) yes . . C(46) C(47) 1.537(6) yes . . C(46) C(48) 1.523(7) yes . . C(46) C(49) 1.541(6) yes . . C(50) C(51) 1.430(13) yes . . C(50) C(52) 1.719(15) yes . . C(50) C(53) 1.597(9) yes . . C(50) C(54) 1.37(4) yes . . C(50) C(55) 1.612(12) yes . . C(50) C(56) 1.577(16) yes . . C(51) C(56) 1.38(2) yes . . C(54) C(55) 1.57(3) yes . . C(55) C(56) 1.72(2) yes . . C(5) H(5) 0.950 no . . C(7) H(7) 0.950 no . . C(11) H(11) 0.950 no . . C(13) H(13) 0.950 no . . C(17) H(17) 0.950 no . . C(19) H(19) 0.950 no . . C(20) H(20A) 0.990 no . . C(20) H(20B) 0.990 no . . C(22) H(22) 0.950 no . . C(23) H(23) 0.950 no . . C(24) H(24) 0.950 no . . C(25) H(25) 0.950 no . . C(26) H(26) 0.950 no . . C(28) H(28A) 0.980 no . . C(28) H(28B) 0.980 no . . C(28) H(28C) 0.980 no . . C(29) H(29A) 0.980 no . . C(29) H(29B) 0.980 no . . C(29) H(29C) 0.980 no . . C(30) H(30A) 0.980 no . . C(30) H(30B) 0.980 no . . C(30) H(30C) 0.980 no . . C(32) H(32A) 0.980 no . . C(32) H(32B) 0.980 no . . C(32) H(32C) 0.980 no . . C(33) H(33A) 0.980 no . . C(33) H(33B) 0.980 no . . C(33) H(33C) 0.980 no . . C(34) H(34A) 0.980 no . . C(34) H(34B) 0.980 no . . C(34) H(34C) 0.980 no . . C(36) H(36A) 0.980 no . . C(36) H(36B) 0.980 no . . C(36) H(36C) 0.980 no . . C(37) H(37A) 0.980 no . . C(37) H(37B) 0.980 no . . C(37) H(37C) 0.980 no . . C(38) H(38A) 0.980 no . . C(38) H(38B) 0.980 no . . C(38) H(38C) 0.980 no . . C(47) H(47A) 0.980 no . . C(47) H(47B) 0.980 no . . C(47) H(47C) 0.980 no . . C(48) H(48A) 0.980 no . . C(48) H(48B) 0.980 no . . C(48) H(48C) 0.980 no . . C(49) H(49A) 0.980 no . . C(49) H(49B) 0.980 no . . C(49) H(49C) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Nb(1) O(2) 105.88(11) yes . . . O(1) Nb(1) O(3) 140.56(12) yes . . . O(1) Nb(1) C(1) 76.01(12) yes . . . O(1) Nb(1) C(20) 91.99(13) yes . . . O(2) Nb(1) O(3) 100.16(11) yes . . . O(2) Nb(1) C(1) 87.42(12) yes . . . O(2) Nb(1) C(20) 128.57(14) yes . . . O(3) Nb(1) C(1) 76.12(12) yes . . . O(3) Nb(1) C(20) 94.44(15) yes . . . C(1) Nb(1) C(20) 144.01(14) yes . . . Nb(1) O(1) C(3) 125.9(3) yes . . . Nb(1) O(2) C(9) 112.9(3) yes . . . Nb(1) O(3) C(15) 125.5(2) yes . . . Nb(1) C(1) C(2) 109.2(3) yes . . . Nb(1) C(1) C(8) 98.0(3) yes . . . Nb(1) C(1) C(14) 107.8(2) yes . . . C(2) C(1) C(8) 113.2(3) yes . . . C(2) C(1) C(14) 117.9(3) yes . . . C(8) C(1) C(14) 108.8(3) yes . . . C(1) C(2) C(3) 114.0(3) yes . . . C(1) C(2) C(7) 127.7(3) yes . . . C(3) C(2) C(7) 118.3(3) yes . . . O(1) C(3) C(2) 113.9(3) yes . . . O(1) C(3) C(4) 123.0(4) yes . . . C(2) C(3) C(4) 123.1(4) yes . . . C(3) C(4) C(5) 115.8(4) yes . . . C(3) C(4) C(27) 121.9(4) yes . . . C(5) C(4) C(27) 122.2(3) yes . . . C(4) C(5) C(6) 123.4(3) yes . . . C(5) C(6) C(7) 118.3(4) yes . . . C(5) C(6) C(31) 121.5(3) yes . . . C(7) C(6) C(31) 120.0(4) yes . . . C(2) C(7) C(6) 121.0(4) yes . . . C(1) C(8) C(9) 121.3(3) yes . . . C(1) C(8) C(13) 119.9(3) yes . . . C(9) C(8) C(13) 118.7(3) yes . . . O(2) C(9) C(8) 119.4(3) yes . . . O(2) C(9) C(10) 119.4(4) yes . . . C(8) C(9) C(10) 121.2(3) yes . . . C(9) C(10) C(11) 117.2(4) yes . . . C(9) C(10) C(35) 120.6(4) yes . . . C(11) C(10) C(35) 122.2(3) yes . . . C(10) C(11) C(12) 123.7(4) yes . . . C(11) C(12) C(13) 116.8(4) yes . . . C(11) C(12) C(39) 121.4(4) yes . . . C(13) C(12) C(39) 121.7(4) yes . . . C(8) C(13) C(12) 122.0(4) yes . . . C(1) C(14) C(15) 113.7(4) yes . . . C(1) C(14) C(19) 128.5(3) yes . . . C(15) C(14) C(19) 117.8(4) yes . . . O(3) C(15) C(14) 113.8(4) yes . . . O(3) C(15) C(16) 122.4(3) yes . . . C(14) C(15) C(16) 123.8(4) yes . . . C(15) C(16) C(17) 115.3(4) yes . . . C(15) C(16) C(46) 121.7(4) yes . . . C(17) C(16) C(46) 122.9(4) yes . . . C(16) C(17) C(18) 123.6(4) yes . . . C(17) C(18) C(19) 118.6(4) yes . . . C(17) C(18) C(50) 120.5(4) yes . . . C(19) C(18) C(50) 120.9(4) yes . . . C(14) C(19) C(18) 120.7(4) yes . . . Nb(1) C(20) C(21) 83.2(3) yes . . . C(20) C(21) C(22) 120.6(4) yes . . . C(20) C(21) C(26) 121.1(5) yes . . . C(22) C(21) C(26) 117.3(4) yes . . . C(21) C(22) C(23) 120.7(4) yes . . . C(22) C(23) C(24) 120.6(5) yes . . . C(23) C(24) C(25) 119.7(5) yes . . . C(24) C(25) C(26) 120.5(5) yes . . . C(21) C(26) C(25) 121.1(5) yes . . . C(4) C(27) C(28) 108.6(4) yes . . . C(4) C(27) C(29) 110.7(3) yes . . . C(4) C(27) C(30) 112.3(4) yes . . . C(28) C(27) C(29) 109.2(4) yes . . . C(28) C(27) C(30) 108.5(3) yes . . . C(29) C(27) C(30) 107.4(4) yes . . . C(6) C(31) C(32) 111.7(4) yes . . . C(6) C(31) C(33) 111.7(4) yes . . . C(6) C(31) C(34) 108.0(4) yes . . . C(32) C(31) C(33) 107.6(4) yes . . . C(32) C(31) C(34) 108.7(4) yes . . . C(33) C(31) C(34) 109.2(5) yes . . . C(10) C(35) C(36) 111.2(4) yes . . . C(10) C(35) C(37) 108.2(4) yes . . . C(10) C(35) C(38) 111.6(4) yes . . . C(36) C(35) C(37) 109.7(4) yes . . . C(36) C(35) C(38) 109.2(5) yes . . . C(37) C(35) C(38) 106.9(4) yes . . . C(12) C(39) C(40) 112.7(11) yes . . . C(12) C(39) C(41) 110.9(4) yes . . . C(12) C(39) C(42) 108.7(6) yes . . . C(12) C(39) C(43) 113.3(5) yes . . . C(12) C(39) C(44) 110.5(9) yes . . . C(12) C(39) C(45) 107.1(5) yes . . . C(40) C(39) C(41) 23.7(12) yes . . . C(40) C(39) C(42) 106.7(13) yes . . . C(40) C(39) C(43) 125.2(12) yes . . . C(40) C(39) C(44) 114.3(13) yes . . . C(40) C(39) C(45) 83.5(12) yes . . . C(41) C(39) C(42) 85.8(6) yes . . . C(41) C(39) C(43) 109.7(7) yes . . . C(41) C(39) C(44) 131.9(8) yes . . . C(41) C(39) C(45) 106.3(5) yes . . . C(42) C(39) C(43) 29.4(7) yes . . . C(42) C(39) C(44) 103.2(11) yes . . . C(42) C(39) C(45) 134.7(7) yes . . . C(43) C(39) C(44) 74.5(11) yes . . . C(43) C(39) C(45) 109.3(7) yes . . . C(44) C(39) C(45) 37.2(9) yes . . . C(39) C(43) C(44) 52.2(8) yes . . . C(39) C(44) C(43) 53.3(9) yes . . . C(16) C(46) C(47) 110.0(3) yes . . . C(16) C(46) C(48) 111.9(4) yes . . . C(16) C(46) C(49) 109.0(4) yes . . . C(47) C(46) C(48) 107.6(4) yes . . . C(47) C(46) C(49) 110.3(4) yes . . . C(48) C(46) C(49) 108.1(4) yes . . . C(18) C(50) C(51) 114.3(8) yes . . . C(18) C(50) C(52) 106.6(7) yes . . . C(18) C(50) C(53) 107.8(5) yes . . . C(18) C(50) C(54) 118.2(14) yes . . . C(18) C(50) C(55) 107.1(5) yes . . . C(18) C(50) C(56) 109.5(8) yes . . . C(51) C(50) C(52) 35.3(7) yes . . . C(51) C(50) C(53) 112.0(7) yes . . . C(51) C(50) C(54) 125.4(15) yes . . . C(51) C(50) C(55) 114.4(7) yes . . . C(51) C(50) C(56) 54.4(8) yes . . . C(52) C(50) C(53) 83.4(6) yes . . . C(52) C(50) C(54) 112.3(14) yes . . . C(52) C(50) C(55) 143.1(8) yes . . . C(52) C(50) C(56) 89.7(8) yes . . . C(53) C(50) C(54) 37.4(12) yes . . . C(53) C(50) C(55) 100.2(6) yes . . . C(53) C(50) C(56) 142.5(9) yes . . . C(54) C(50) C(55) 62.8(12) yes . . . C(54) C(50) C(56) 116.6(15) yes . . . C(55) C(50) C(56) 65.1(8) yes . . . C(50) C(51) C(56) 68.3(9) yes . . . C(50) C(54) C(55) 66.1(13) yes . . . C(50) C(55) C(54) 51.0(13) yes . . . C(50) C(55) C(56) 56.5(7) yes . . . C(54) C(55) C(56) 99.6(14) yes . . . C(50) C(56) C(51) 57.4(8) yes . . . C(50) C(56) C(55) 58.4(7) yes . . . C(51) C(56) C(55) 111.0(11) yes . . . C(4) C(5) H(5) 118.287 no . . . C(6) C(5) H(5) 118.308 no . . . C(2) C(7) H(7) 119.481 no . . . C(6) C(7) H(7) 119.474 no . . . C(10) C(11) H(11) 118.160 no . . . C(12) C(11) H(11) 118.172 no . . . C(8) C(13) H(13) 119.011 no . . . C(12) C(13) H(13) 119.017 no . . . C(16) C(17) H(17) 118.219 no . . . C(18) C(17) H(17) 118.228 no . . . C(14) C(19) H(19) 119.625 no . . . C(18) C(19) H(19) 119.638 no . . . Nb(1) C(20) H(20A) 114.770 no . . . Nb(1) C(20) H(20B) 114.764 no . . . C(21) C(20) H(20A) 114.770 no . . . C(21) C(20) H(20B) 114.772 no . . . H(20A) C(20) H(20B) 111.853 no . . . C(21) C(22) H(22) 119.656 no . . . C(23) C(22) H(22) 119.660 no . . . C(22) C(23) H(23) 119.693 no . . . C(24) C(23) H(23) 119.695 no . . . C(23) C(24) H(24) 120.140 no . . . C(25) C(24) H(24) 120.126 no . . . C(24) C(25) H(25) 119.772 no . . . C(26) C(25) H(25) 119.762 no . . . C(21) C(26) H(26) 119.447 no . . . C(25) C(26) H(26) 119.452 no . . . C(27) C(28) H(28A) 109.473 no . . . C(27) C(28) H(28B) 109.476 no . . . C(27) C(28) H(28C) 109.470 no . . . H(28A) C(28) H(28B) 109.483 no . . . H(28A) C(28) H(28C) 109.455 no . . . H(28B) C(28) H(28C) 109.469 no . . . C(27) C(29) H(29A) 109.484 no . . . C(27) C(29) H(29B) 109.469 no . . . C(27) C(29) H(29C) 109.473 no . . . H(29A) C(29) H(29B) 109.468 no . . . H(29A) C(29) H(29C) 109.469 no . . . H(29B) C(29) H(29C) 109.464 no . . . C(27) C(30) H(30A) 109.468 no . . . C(27) C(30) H(30B) 109.474 no . . . C(27) C(30) H(30C) 109.462 no . . . H(30A) C(30) H(30B) 109.476 no . . . H(30A) C(30) H(30C) 109.473 no . . . H(30B) C(30) H(30C) 109.476 no . . . C(31) C(32) H(32A) 109.477 no . . . C(31) C(32) H(32B) 109.480 no . . . C(31) C(32) H(32C) 109.477 no . . . H(32A) C(32) H(32B) 109.467 no . . . H(32A) C(32) H(32C) 109.461 no . . . H(32B) C(32) H(32C) 109.466 no . . . C(31) C(33) H(33A) 109.474 no . . . C(31) C(33) H(33B) 109.468 no . . . C(31) C(33) H(33C) 109.469 no . . . H(33A) C(33) H(33B) 109.478 no . . . H(33A) C(33) H(33C) 109.475 no . . . H(33B) C(33) H(33C) 109.463 no . . . C(31) C(34) H(34A) 109.477 no . . . C(31) C(34) H(34B) 109.466 no . . . C(31) C(34) H(34C) 109.475 no . . . H(34A) C(34) H(34B) 109.478 no . . . H(34A) C(34) H(34C) 109.471 no . . . H(34B) C(34) H(34C) 109.460 no . . . C(35) C(36) H(36A) 109.463 no . . . C(35) C(36) H(36B) 109.475 no . . . C(35) C(36) H(36C) 109.477 no . . . H(36A) C(36) H(36B) 109.473 no . . . H(36A) C(36) H(36C) 109.468 no . . . H(36B) C(36) H(36C) 109.471 no . . . C(35) C(37) H(37A) 109.477 no . . . C(35) C(37) H(37B) 109.468 no . . . C(35) C(37) H(37C) 109.473 no . . . H(37A) C(37) H(37B) 109.464 no . . . H(37A) C(37) H(37C) 109.473 no . . . H(37B) C(37) H(37C) 109.472 no . . . C(35) C(38) H(38A) 109.469 no . . . C(35) C(38) H(38B) 109.472 no . . . C(35) C(38) H(38C) 109.474 no . . . H(38A) C(38) H(38B) 109.471 no . . . H(38A) C(38) H(38C) 109.471 no . . . H(38B) C(38) H(38C) 109.470 no . . . C(46) C(47) H(47A) 109.469 no . . . C(46) C(47) H(47B) 109.481 no . . . C(46) C(47) H(47C) 109.482 no . . . H(47A) C(47) H(47B) 109.462 no . . . H(47A) C(47) H(47C) 109.457 no . . . H(47B) C(47) H(47C) 109.476 no . . . C(46) C(48) H(48A) 109.472 no . . . C(46) C(48) H(48B) 109.468 no . . . C(46) C(48) H(48C) 109.476 no . . . H(48A) C(48) H(48B) 109.468 no . . . H(48A) C(48) H(48C) 109.466 no . . . H(48B) C(48) H(48C) 109.477 no . . . C(46) C(49) H(49A) 109.463 no . . . C(46) C(49) H(49B) 109.468 no . . . C(46) C(49) H(49C) 109.472 no . . . H(49A) C(49) H(49B) 109.473 no . . . H(49A) C(49) H(49C) 109.465 no . . . H(49B) C(49) H(49C) 109.486 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Nb(1) O(2) C(9) -82.41(18) no . . . . O(2) Nb(1) O(1) C(3) 92.8(2) no . . . . O(1) Nb(1) O(3) C(15) 32.2(3) no . . . . O(3) Nb(1) O(1) C(3) -36.6(3) no . . . . O(1) Nb(1) C(1) C(2) -7.82(17) no . . . . O(1) Nb(1) C(1) C(8) 110.25(18) no . . . . O(1) Nb(1) C(1) C(14) -136.99(17) no . . . . C(1) Nb(1) O(1) C(3) 9.64(19) no . . . . O(1) Nb(1) C(20) C(21) -110.84(18) no . . . . C(20) Nb(1) O(1) C(3) -136.0(3) no . . . . O(2) Nb(1) O(3) C(15) -98.73(19) no . . . . O(3) Nb(1) O(2) C(9) 67.66(17) no . . . . O(2) Nb(1) C(1) C(2) -114.9(2) no . . . . O(2) Nb(1) C(1) C(8) 3.18(16) no . . . . O(2) Nb(1) C(1) C(14) 115.94(16) no . . . . C(1) Nb(1) O(2) C(9) -7.75(17) no . . . . O(2) Nb(1) C(20) C(21) 1.4(3) no . . . . C(20) Nb(1) O(2) C(9) 171.75(17) no . . . . O(3) Nb(1) C(1) C(2) 144.0(2) no . . . . O(3) Nb(1) C(1) C(8) -97.95(16) no . . . . O(3) Nb(1) C(1) C(14) 14.81(14) no . . . . C(1) Nb(1) O(3) C(15) -13.98(17) no . . . . O(3) Nb(1) C(20) C(21) 108.10(18) no . . . . C(20) Nb(1) O(3) C(15) 130.79(19) no . . . . C(1) Nb(1) C(20) C(21) -179.50(15) no . . . . C(20) Nb(1) C(1) C(2) 65.8(4) no . . . . C(20) Nb(1) C(1) C(8) -176.2(2) no . . . . C(20) Nb(1) C(1) C(14) -63.4(3) no . . . . Nb(1) O(1) C(3) C(2) -8.8(4) no . . . . Nb(1) O(1) C(3) C(4) 170.8(2) no . . . . Nb(1) O(2) C(9) C(8) 11.2(4) no . . . . Nb(1) O(2) C(9) C(10) -167.9(2) no . . . . Nb(1) O(3) C(15) C(14) 8.8(4) no . . . . Nb(1) O(3) C(15) C(16) -170.38(16) no . . . . Nb(1) C(1) C(2) C(3) 6.2(4) no . . . . Nb(1) C(1) C(2) C(7) -174.6(3) no . . . . Nb(1) C(1) C(8) C(9) 1.8(4) no . . . . Nb(1) C(1) C(8) C(13) 178.6(3) no . . . . Nb(1) C(1) C(14) C(15) -15.5(3) no . . . . Nb(1) C(1) C(14) C(19) 166.7(2) no . . . . C(2) C(1) C(8) C(9) 116.8(4) no . . . . C(2) C(1) C(8) C(13) -66.5(4) no . . . . C(8) C(1) C(2) C(3) -101.8(3) no . . . . C(8) C(1) C(2) C(7) 77.4(5) no . . . . C(2) C(1) C(14) C(15) -139.6(3) no . . . . C(2) C(1) C(14) C(19) 42.6(4) no . . . . C(14) C(1) C(2) C(3) 129.6(3) no . . . . C(14) C(1) C(2) C(7) -51.2(5) no . . . . C(8) C(1) C(14) C(15) 89.8(3) no . . . . C(8) C(1) C(14) C(19) -88.0(4) no . . . . C(14) C(1) C(8) C(9) -110.1(4) no . . . . C(14) C(1) C(8) C(13) 66.6(4) no . . . . C(1) C(2) C(3) O(1) 0.2(5) no . . . . C(1) C(2) C(3) C(4) -179.5(3) no . . . . C(1) C(2) C(7) C(6) 179.3(3) no . . . . C(3) C(2) C(7) C(6) -1.5(5) no . . . . C(7) C(2) C(3) O(1) -179.1(3) no . . . . C(7) C(2) C(3) C(4) 1.3(5) no . . . . O(1) C(3) C(4) C(5) 179.6(3) no . . . . O(1) C(3) C(4) C(27) -2.2(6) no . . . . C(2) C(3) C(4) C(5) -0.8(5) no . . . . C(2) C(3) C(4) C(27) 177.4(3) no . . . . C(3) C(4) C(5) C(6) 0.5(6) no . . . . C(3) C(4) C(27) C(28) -63.3(5) no . . . . C(3) C(4) C(27) C(29) 56.6(5) no . . . . C(3) C(4) C(27) C(30) 176.6(3) no . . . . C(5) C(4) C(27) C(28) 114.7(4) no . . . . C(5) C(4) C(27) C(29) -125.4(4) no . . . . C(5) C(4) C(27) C(30) -5.3(5) no . . . . C(27) C(4) C(5) C(6) -177.6(4) no . . . . C(4) C(5) C(6) C(7) -0.8(6) no . . . . C(4) C(5) C(6) C(31) 175.9(3) no . . . . C(5) C(6) C(7) C(2) 1.3(6) no . . . . C(5) C(6) C(31) C(32) 31.1(5) no . . . . C(5) C(6) C(31) C(33) 151.6(4) no . . . . C(5) C(6) C(31) C(34) -88.4(5) no . . . . C(7) C(6) C(31) C(32) -152.3(3) no . . . . C(7) C(6) C(31) C(33) -31.8(5) no . . . . C(7) C(6) C(31) C(34) 88.3(4) no . . . . C(31) C(6) C(7) C(2) -175.5(3) no . . . . C(1) C(8) C(9) O(2) -8.8(5) no . . . . C(1) C(8) C(9) C(10) 170.3(3) no . . . . C(1) C(8) C(13) C(12) -175.9(3) no . . . . C(9) C(8) C(13) C(12) 0.9(6) no . . . . C(13) C(8) C(9) O(2) 174.5(3) no . . . . C(13) C(8) C(9) C(10) -6.4(5) no . . . . O(2) C(9) C(10) C(11) -173.8(3) no . . . . O(2) C(9) C(10) C(35) 9.1(6) no . . . . C(8) C(9) C(10) C(11) 7.1(6) no . . . . C(8) C(9) C(10) C(35) -170.0(3) no . . . . C(9) C(10) C(11) C(12) -2.4(6) no . . . . C(9) C(10) C(35) C(36) -63.6(5) no . . . . C(9) C(10) C(35) C(37) 56.9(5) no . . . . C(9) C(10) C(35) C(38) 174.2(4) no . . . . C(11) C(10) C(35) C(36) 119.5(4) no . . . . C(11) C(10) C(35) C(37) -120.0(4) no . . . . C(11) C(10) C(35) C(38) -2.7(6) no . . . . C(35) C(10) C(11) C(12) 174.6(4) no . . . . C(10) C(11) C(12) C(13) -2.8(6) no . . . . C(10) C(11) C(12) C(39) 176.5(4) no . . . . C(11) C(12) C(13) C(8) 3.5(6) no . . . . C(11) C(12) C(39) C(40) 28.4(6) no . . . . C(11) C(12) C(39) C(41) 53.9(6) no . . . . C(11) C(12) C(39) C(42) 146.6(4) no . . . . C(11) C(12) C(39) C(43) 177.8(4) no . . . . C(11) C(12) C(39) C(44) -100.8(4) no . . . . C(11) C(12) C(39) C(45) -61.6(5) no . . . . C(13) C(12) C(39) C(40) -152.3(4) no . . . . C(13) C(12) C(39) C(41) -126.8(4) no . . . . C(13) C(12) C(39) C(42) -34.2(5) no . . . . C(13) C(12) C(39) C(43) -2.9(6) no . . . . C(13) C(12) C(39) C(44) 78.4(5) no . . . . C(13) C(12) C(39) C(45) 117.6(4) no . . . . C(39) C(12) C(13) C(8) -175.8(4) no . . . . C(1) C(14) C(15) O(3) 6.7(4) no . . . . C(1) C(14) C(15) C(16) -174.1(3) no . . . . C(1) C(14) C(19) C(18) 177.9(3) no . . . . C(15) C(14) C(19) C(18) 0.2(4) no . . . . C(19) C(14) C(15) O(3) -175.3(3) no . . . . C(19) C(14) C(15) C(16) 3.9(4) no . . . . O(3) C(15) C(16) C(17) 174.8(3) no . . . . O(3) C(15) C(16) C(46) -6.1(5) no . . . . C(14) C(15) C(16) C(17) -4.3(5) no . . . . C(14) C(15) C(16) C(46) 174.8(3) no . . . . C(15) C(16) C(17) C(18) 0.7(5) no . . . . C(15) C(16) C(46) C(47) 61.9(4) no . . . . C(15) C(16) C(46) C(48) -178.7(3) no . . . . C(15) C(16) C(46) C(49) -59.2(4) no . . . . C(17) C(16) C(46) C(47) -119.1(4) no . . . . C(17) C(16) C(46) C(48) 0.4(5) no . . . . C(17) C(16) C(46) C(49) 119.9(4) no . . . . C(46) C(16) C(17) C(18) -178.4(3) no . . . . C(16) C(17) C(18) C(19) 3.1(5) no . . . . C(16) C(17) C(18) C(50) -177.8(3) no . . . . C(17) C(18) C(19) C(14) -3.5(5) no . . . . C(17) C(18) C(50) C(51) 179.5(3) no . . . . C(17) C(18) C(50) C(52) -143.6(3) no . . . . C(17) C(18) C(50) C(53) -55.3(5) no . . . . C(17) C(18) C(50) C(54) -16.1(6) no . . . . C(17) C(18) C(50) C(55) 51.7(4) no . . . . C(17) C(18) C(50) C(56) 120.7(4) no . . . . C(19) C(18) C(50) C(51) -1.4(5) no . . . . C(19) C(18) C(50) C(52) 35.5(4) no . . . . C(19) C(18) C(50) C(53) 123.8(4) no . . . . C(19) C(18) C(50) C(54) 163.0(3) no . . . . C(19) C(18) C(50) C(55) -129.1(4) no . . . . C(19) C(18) C(50) C(56) -60.2(5) no . . . . C(50) C(18) C(19) C(14) 177.3(3) no . . . . Nb(1) C(20) C(21) C(22) 79.3(3) no . . . . Nb(1) C(20) C(21) C(26) -88.5(3) no . . . . C(20) C(21) C(22) C(23) -172.5(4) no . . . . C(20) C(21) C(26) C(25) 172.7(4) no . . . . C(22) C(21) C(26) C(25) 4.5(6) no . . . . C(26) C(21) C(22) C(23) -4.2(6) no . . . . C(21) C(22) C(23) C(24) 2.0(7) no . . . . C(22) C(23) C(24) C(25) 0.1(8) no . . . . C(23) C(24) C(25) C(26) 0.2(8) no . . . . C(24) C(25) C(26) C(21) -2.6(7) no . . . . C(12) C(39) C(43) C(44) 106.0(5) no . . . . C(12) C(39) C(44) C(43) -109.5(5) no . . . . C(40) C(39) C(43) C(44) -109.1(14) no . . . . C(40) C(39) C(44) C(43) 122.1(13) no . . . . C(41) C(39) C(43) C(44) -129.5(5) no . . . . C(41) C(39) C(44) C(43) 102.8(11) no . . . . C(42) C(39) C(43) C(44) -166.9(13) no . . . . C(42) C(39) C(44) C(43) 6.6(6) no . . . . C(45) C(39) C(43) C(44) -13.3(5) no . . . . C(45) C(39) C(44) C(43) 158.9(14) no . . . . C(18) C(50) C(51) C(56) -97.3(6) no . . . . C(18) C(50) C(54) C(55) 95.7(10) no . . . . C(18) C(50) C(55) C(54) -113.5(4) no . . . . C(18) C(50) C(55) C(56) 104.0(4) no . . . . C(18) C(50) C(56) C(51) 106.5(6) no . . . . C(18) C(50) C(56) C(55) -100.3(6) no . . . . C(52) C(50) C(51) C(56) 178.2(16) no . . . . C(53) C(50) C(51) C(56) 139.8(6) no . . . . C(51) C(50) C(54) C(55) -101.8(12) no . . . . C(54) C(50) C(51) C(56) 99.6(16) no . . . . C(51) C(50) C(55) C(54) 118.8(8) no . . . . C(51) C(50) C(55) C(56) -23.7(7) no . . . . C(55) C(50) C(51) C(56) 26.7(8) no . . . . C(51) C(50) C(56) C(55) 153.2(12) no . . . . C(52) C(50) C(54) C(55) -139.5(8) no . . . . C(52) C(50) C(55) C(54) 91.5(11) no . . . . C(52) C(50) C(55) C(56) -51.0(11) no . . . . C(52) C(50) C(56) C(51) -1.1(8) no . . . . C(52) C(50) C(56) C(55) 152.2(8) no . . . . C(53) C(50) C(54) C(55) 178(3) no . . . . C(53) C(50) C(55) C(54) -1.1(4) no . . . . C(53) C(50) C(55) C(56) -143.6(5) no . . . . C(53) C(50) C(56) C(51) -79.7(14) no . . . . C(53) C(50) C(56) C(55) 73.5(12) no . . . . C(54) C(50) C(55) C(56) -142.5(16) no . . . . C(54) C(50) C(56) C(51) -116.0(16) no . . . . C(54) C(50) C(56) C(55) 37.3(16) no . . . . C(56) C(50) C(54) C(55) -38.1(15) no . . . . C(55) C(50) C(56) C(51) -153.2(10) no . . . . C(56) C(50) C(55) C(54) 142.5(9) no . . . . C(50) C(51) C(56) C(55) -24.3(10) no . . . . C(50) C(54) C(55) C(56) 31.0(12) no . . . . C(50) C(55) C(56) C(51) 24.0(9) no . . . . C(54) C(55) C(56) C(50) -28.7(14) no . . . . C(54) C(55) C(56) C(51) -4.7(19) no . . . . #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================