# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[(ArO)2NbCl2](THF)2 _database_code_depnum_ccdc_archive 'CCDC 902913' #TrackingRef '14202_web_deposit_cif_file_0_HiroyukiKawaguchi_1348537764.CIF-kawaguchi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H70 Cl2 Nb O2, 2(C4 H8 O)' _chemical_formula_sum 'C62 H86 Cl2 Nb O4' _chemical_formula_weight 1059.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nb Nb -2.0727 0.6215 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, -y, z' _cell_length_a 21.571(8) _cell_length_b 10.906(4) _cell_length_c 24.181(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.853(3) _cell_angle_gamma 90.00 _cell_volume 5316(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8536 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Platelet _exptl_crystal_colour Green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9564 _exptl_absorpt_correction_T_max 0.9925 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Mercury375R CCD (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 13.6612 _diffrn_reflns_number 52911 _diffrn_reflns_av_R_equivalents 0.1129 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12181 _reflns_number_gt 7665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2009)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2009)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+0.9222P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12181 _refine_ls_number_parameters 598 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1244 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.2170 _refine_ls_wR_factor_gt 0.1792 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.91476(2) 0.66588(4) 0.265102(18) 0.02414(14) Uani 1 1 d . . . Cl1 Cl 1.01071(6) 0.64036(12) 0.34890(5) 0.0344(3) Uani 1 1 d . . . Cl2 Cl 0.94405(6) 0.85985(11) 0.23998(6) 0.0336(3) Uani 1 1 d . . . O1 O 0.93522(15) 0.5581(3) 0.21406(13) 0.0253(7) Uani 1 1 d . . . C1 C 0.9394(2) 0.4483(4) 0.1864(2) 0.0247(10) Uani 1 1 d . . . C2 C 0.9153(2) 0.3395(4) 0.2021(2) 0.0270(10) Uani 1 1 d . . . C3 C 0.9223(2) 0.2321(5) 0.1732(2) 0.0309(11) Uani 1 1 d . . . H1 H 0.9064 0.1573 0.1832 0.037 Uiso 1 1 calc R . . C4 C 0.9514(3) 0.2298(5) 0.1307(2) 0.0342(12) Uani 1 1 d . . . C5 C 0.9758(2) 0.3391(4) 0.1176(2) 0.0292(11) Uani 1 1 d . . . H2 H 0.9960 0.3388 0.0885 0.035 Uiso 1 1 calc R . . C6 C 0.9722(2) 0.4502(4) 0.1454(2) 0.0272(10) Uani 1 1 d . . . C7 C 0.8798(2) 0.3194(4) 0.2475(2) 0.0249(10) Uani 1 1 d . . . C8 C 0.8649(2) 0.4357(4) 0.2774(2) 0.0261(10) Uani 1 1 d . . . H3 H 0.9070 0.4793 0.2986 0.031 Uiso 1 1 calc R . . H4 H 0.8361 0.4914 0.2466 0.031 Uiso 1 1 calc R . . C9 C 0.9243(2) 0.2347(5) 0.2975(2) 0.0308(11) Uani 1 1 d . . . H5 H 0.9342 0.1585 0.2800 0.037 Uiso 1 1 calc R . . H6 H 0.9668 0.2765 0.3189 0.037 Uiso 1 1 calc R . . C10 C 0.8120(2) 0.2559(5) 0.2165(2) 0.0290(11) Uani 1 1 d . . . H7 H 0.7827 0.3117 0.1861 0.035 Uiso 1 1 calc R . . H8 H 0.8187 0.1810 0.1962 0.035 Uiso 1 1 calc R . . C11 C 0.8305(2) 0.4029(4) 0.3213(2) 0.0277(10) Uani 1 1 d . . . H9 H 0.8217 0.4796 0.3399 0.033 Uiso 1 1 calc R . . C12 C 0.8764(3) 0.3188(5) 0.3694(2) 0.0332(12) Uani 1 1 d . . . H10 H 0.9187 0.3615 0.3906 0.040 Uiso 1 1 calc R . . H11 H 0.8553 0.2979 0.3984 0.040 Uiso 1 1 calc R . . C13 C 0.8898(2) 0.2025(5) 0.3411(2) 0.0306(11) Uani 1 1 d . . . H12 H 0.9190 0.1469 0.3725 0.037 Uiso 1 1 calc R . . C14 C 0.8244(3) 0.1382(4) 0.3081(2) 0.0326(11) Uani 1 1 d . . . H13 H 0.8025 0.1154 0.3364 0.039 Uiso 1 1 calc R . . H14 H 0.8331 0.0619 0.2898 0.039 Uiso 1 1 calc R . . C15 C 0.7782(3) 0.2214(5) 0.2599(2) 0.0315(11) Uani 1 1 d . . . H15 H 0.7356 0.1779 0.2386 0.038 Uiso 1 1 calc R . . C16 C 0.7647(2) 0.3378(4) 0.2885(2) 0.0318(11) Uani 1 1 d . . . H16 H 0.7424 0.3169 0.3167 0.038 Uiso 1 1 calc R . . H17 H 0.7351 0.3926 0.2578 0.038 Uiso 1 1 calc R . . C17 C 1.0050(2) 0.5661(4) 0.1300(2) 0.0260(10) Uani 1 1 d . . . C18 C 1.0597(2) 0.6164(4) 0.1848(2) 0.0291(11) Uani 1 1 d . . . H18 H 1.0405 0.6397 0.2149 0.035 Uiso 1 1 calc R . . H19 H 1.0932 0.5516 0.2020 0.035 Uiso 1 1 calc R . . C19 C 0.9533(2) 0.6680(4) 0.1035(2) 0.0302(11) Uani 1 1 d . . . H20 H 0.9180 0.6370 0.0675 0.036 Uiso 1 1 calc R . . H21 H 0.9325 0.6916 0.1324 0.036 Uiso 1 1 calc R . . C20 C 1.0366(3) 0.5349(4) 0.0835(2) 0.0299(11) Uani 1 1 d . . . H22 H 1.0694 0.4682 0.0989 0.036 Uiso 1 1 calc R . . H23 H 1.0017 0.5050 0.0470 0.036 Uiso 1 1 calc R . . C21 C 1.0931(3) 0.7273(5) 0.1696(2) 0.0365(12) Uani 1 1 d . . . H24 H 1.1282 0.7586 0.2063 0.044 Uiso 1 1 calc R . . C22 C 1.0409(3) 0.8279(5) 0.1435(2) 0.0345(12) Uani 1 1 d . . . H25 H 1.0212 0.8525 0.1731 0.041 Uiso 1 1 calc R . . H26 H 1.0623 0.9009 0.1337 0.041 Uiso 1 1 calc R . . C23 C 0.9866(3) 0.7804(5) 0.0878(2) 0.0321(11) Uani 1 1 d . . . H27 H 0.9527 0.8461 0.0711 0.039 Uiso 1 1 calc R . . C24 C 1.0190(3) 0.7468(5) 0.0423(2) 0.0368(12) Uani 1 1 d . . . H28 H 0.9849 0.7167 0.0054 0.044 Uiso 1 1 calc R . . H29 H 1.0403 0.8201 0.0327 0.044 Uiso 1 1 calc R . . C25 C 1.0711(3) 0.6469(5) 0.0688(2) 0.0360(12) Uani 1 1 d . . . H30 H 1.0916 0.6230 0.0392 0.043 Uiso 1 1 calc R . . C26 C 1.1244(3) 0.6935(5) 0.1243(2) 0.0379(13) Uani 1 1 d . . . H31 H 1.1462 0.7663 0.1149 0.045 Uiso 1 1 calc R . . H32 H 1.1585 0.6293 0.1406 0.045 Uiso 1 1 calc R . . C27 C 0.9555(3) 0.1126(5) 0.0992(3) 0.0469(15) Uani 1 1 d . . . H33 H 0.9211 0.1126 0.0596 0.070 Uiso 1 1 calc R . . H34 H 0.9487 0.0425 0.1218 0.070 Uiso 1 1 calc R . . H35 H 0.9993 0.1065 0.0957 0.070 Uiso 1 1 calc R . . C28 C 0.7862(2) 0.7140(4) 0.2967(2) 0.0235(10) Uani 1 1 d . . . C29 C 0.7293(2) 0.7123(4) 0.2451(2) 0.0279(10) Uani 1 1 d . . . C30 C 0.6695(2) 0.6781(4) 0.2519(2) 0.0302(11) Uani 1 1 d . . . H36 H 0.6304 0.6721 0.2177 0.036 Uiso 1 1 calc R . . C31 C 0.6660(2) 0.6529(5) 0.3068(2) 0.0314(11) Uani 1 1 d . . . C32 C 0.7210(2) 0.6730(4) 0.3564(2) 0.0300(11) Uani 1 1 d . . . H37 H 0.7171 0.6632 0.3940 0.036 Uiso 1 1 calc R . . C33 C 0.7830(2) 0.7074(4) 0.3542(2) 0.0264(10) Uani 1 1 d . . . C34 C 0.7288(2) 0.7569(4) 0.1838(2) 0.0260(10) Uani 1 1 d . . . C35 C 0.7657(2) 0.6704(4) 0.1556(2) 0.0282(10) Uani 1 1 d . . . H38 H 0.7454 0.5878 0.1510 0.034 Uiso 1 1 calc R . . H39 H 0.8126 0.6630 0.1822 0.034 Uiso 1 1 calc R . . C36 C 0.7588(3) 0.8867(4) 0.1892(2) 0.0284(11) Uani 1 1 d . . . H40 H 0.7335 0.9435 0.2052 0.034 Uiso 1 1 calc R . . H41 H 0.8053 0.8852 0.2171 0.034 Uiso 1 1 calc R . . C37 C 0.6567(2) 0.7680(5) 0.1392(2) 0.0348(12) Uani 1 1 d . . . H42 H 0.6352 0.6866 0.1340 0.042 Uiso 1 1 calc R . . H43 H 0.6315 0.8243 0.1555 0.042 Uiso 1 1 calc R . . C38 C 0.7631(3) 0.7174(5) 0.0944(2) 0.0287(11) Uani 1 1 d . . . H44 H 0.7880 0.6603 0.0774 0.034 Uiso 1 1 calc R . . C39 C 0.7946(3) 0.8454(4) 0.1028(2) 0.0315(11) Uani 1 1 d . . . H45 H 0.8414 0.8402 0.1298 0.038 Uiso 1 1 calc R . . H46 H 0.7940 0.8770 0.0642 0.038 Uiso 1 1 calc R . . C40 C 0.7566(3) 0.9328(5) 0.1284(2) 0.0323(11) Uani 1 1 d . . . H47 H 0.7778 1.0156 0.1333 0.039 Uiso 1 1 calc R . . C41 C 0.6854(3) 0.9428(5) 0.0861(2) 0.0371(12) Uani 1 1 d . . . H48 H 0.6843 0.9740 0.0473 0.045 Uiso 1 1 calc R . . H49 H 0.6606 1.0007 0.1020 0.045 Uiso 1 1 calc R . . C42 C 0.6538(3) 0.8159(5) 0.0788(2) 0.0371(13) Uani 1 1 d . . . H50 H 0.6065 0.8213 0.0516 0.044 Uiso 1 1 calc R . . C43 C 0.6908(3) 0.7256(5) 0.0535(2) 0.0364(12) Uani 1 1 d . . . H51 H 0.6699 0.6437 0.0493 0.044 Uiso 1 1 calc R . . H52 H 0.6883 0.7533 0.0137 0.044 Uiso 1 1 calc R . . O2 O 0.84803(15) 0.7215(3) 0.29200(13) 0.0239(7) Uani 1 1 d . . . C44 C 0.8408(2) 0.7381(4) 0.4115(2) 0.0260(10) Uani 1 1 d . . . C45 C 0.8723(3) 0.8618(4) 0.4039(2) 0.0300(11) Uani 1 1 d . . . H53 H 0.8887 0.8555 0.3706 0.036 Uiso 1 1 calc R . . H54 H 0.8383 0.9272 0.3944 0.036 Uiso 1 1 calc R . . C46 C 0.8951(2) 0.6368(4) 0.4295(2) 0.0283(11) Uani 1 1 d . . . H55 H 0.8757 0.5590 0.4368 0.034 Uiso 1 1 calc R . . H56 H 0.9118 0.6231 0.3968 0.034 Uiso 1 1 calc R . . C47 C 0.8160(2) 0.7523(5) 0.4639(2) 0.0340(12) Uani 1 1 d . . . H57 H 0.7965 0.6739 0.4703 0.041 Uiso 1 1 calc R . . H58 H 0.7811 0.8160 0.4543 0.041 Uiso 1 1 calc R . . C48 C 0.9300(2) 0.8950(5) 0.4607(2) 0.0300(11) Uani 1 1 d . . . H59 H 0.9500 0.9743 0.4546 0.036 Uiso 1 1 calc R . . C49 C 0.9825(2) 0.7964(5) 0.4758(2) 0.0321(11) Uani 1 1 d . . . H60 H 1.0198 0.8192 0.5121 0.039 Uiso 1 1 calc R . . H61 H 0.9998 0.7878 0.4432 0.039 Uiso 1 1 calc R . . C50 C 0.9526(3) 0.6747(4) 0.4854(2) 0.0317(11) Uani 1 1 d . . . H62 H 0.9876 0.6099 0.4953 0.038 Uiso 1 1 calc R . . C51 C 0.9276(3) 0.6884(5) 0.5372(2) 0.0389(13) Uani 1 1 d . . . H63 H 0.9087 0.6098 0.5443 0.047 Uiso 1 1 calc R . . H64 H 0.9647 0.7113 0.5737 0.047 Uiso 1 1 calc R . . C52 C 0.8741(3) 0.7887(5) 0.5211(2) 0.0372(13) Uani 1 1 d . . . H65 H 0.8568 0.7980 0.5542 0.045 Uiso 1 1 calc R . . C53 C 0.9040(3) 0.9098(5) 0.5119(2) 0.0374(12) Uani 1 1 d . . . H66 H 0.9408 0.9333 0.5485 0.045 Uiso 1 1 calc R . . H67 H 0.8699 0.9751 0.5023 0.045 Uiso 1 1 calc R . . C54 C 0.6007(3) 0.6107(6) 0.3114(3) 0.0454(15) Uani 1 1 d . . . H68 H 0.6025 0.5221 0.3186 0.068 Uiso 1 1 calc R . . H69 H 0.5643 0.6293 0.2744 0.068 Uiso 1 1 calc R . . H70 H 0.5935 0.6535 0.3442 0.068 Uiso 1 1 calc R . . O3 O 0.6731(3) 0.1052(6) 0.3125(3) 0.104(2) Uani 1 1 d . . . C55 C 0.6534(5) -0.0116(7) 0.2926(5) 0.099(3) Uani 1 1 d . . . H71 H 0.6913 -0.0693 0.3061 0.118 Uiso 1 1 calc R . . H72 H 0.6339 -0.0137 0.2488 0.118 Uiso 1 1 calc R . . C56 C 0.5969(5) -0.0461(7) 0.3222(6) 0.125(4) Uani 1 1 d . . . H73 H 0.5513 -0.0485 0.2926 0.150 Uiso 1 1 calc R . . H74 H 0.6069 -0.1236 0.3450 0.150 Uiso 1 1 calc R . . C57 C 0.6090(5) 0.0610(9) 0.3596(4) 0.099(3) Uani 1 1 d . . . H75 H 0.6454 0.0444 0.3977 0.119 Uiso 1 1 calc R . . H76 H 0.5686 0.0819 0.3682 0.119 Uiso 1 1 calc R . . C58 C 0.6270(5) 0.1626(10) 0.3294(4) 0.094(3) Uani 1 1 d . . . H77 H 0.5888 0.1915 0.2951 0.112 Uiso 1 1 calc R . . H78 H 0.6461 0.2320 0.3565 0.112 Uiso 1 1 calc R . . O4 O 0.7500 0.4553(8) 0.0000 0.091(2) Uiso 1 2 d S . . C59 C 0.7346(9) 0.3802(12) -0.0509(6) 0.055(4) Uiso 0.55(3) 1 d P A 1 H79 H 0.7622 0.4040 -0.0743 0.066 Uiso 0.55(3) 1 calc PR A 1 H80 H 0.6874 0.3907 -0.0762 0.066 Uiso 0.55(3) 1 calc PR A 1 C60 C 0.7476(9) 0.2514(11) -0.0319(6) 0.057(4) Uiso 0.55(3) 1 d P . 1 H81 H 0.7895 0.2225 -0.0355 0.068 Uiso 0.55(3) 1 calc PR A 1 H82 H 0.7109 0.1978 -0.0562 0.068 Uiso 0.55(3) 1 calc PR A 1 C61 C 0.7044(11) 0.3847(15) -0.0451(7) 0.056(5) Uiso 0.45(3) 1 d P A 2 H83 H 0.7127 0.3938 -0.0827 0.067 Uiso 0.45(3) 1 calc PR A 2 H84 H 0.6584 0.4107 -0.0517 0.067 Uiso 0.45(3) 1 calc PR A 2 C62 C 0.7152(12) 0.2554(16) -0.0240(8) 0.067(6) Uiso 0.45(3) 1 d P . 2 H85 H 0.7133 0.1991 -0.0567 0.081 Uiso 0.45(3) 1 calc PR A 2 H86 H 0.6814 0.2300 -0.0074 0.081 Uiso 0.45(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0235(2) 0.0260(2) 0.0245(2) -0.00423(17) 0.01051(18) -0.00137(17) Cl1 0.0245(6) 0.0445(7) 0.0313(6) -0.0058(5) 0.0065(5) 0.0011(5) Cl2 0.0330(7) 0.0304(7) 0.0423(7) -0.0021(5) 0.0192(6) -0.0034(5) O1 0.0301(18) 0.0249(17) 0.0227(16) -0.0037(13) 0.0118(15) 0.0008(14) C1 0.027(2) 0.018(2) 0.028(2) -0.0017(18) 0.010(2) 0.0031(18) C2 0.026(2) 0.029(3) 0.024(2) -0.0014(19) 0.007(2) 0.005(2) C3 0.037(3) 0.027(3) 0.034(3) -0.006(2) 0.018(2) 0.001(2) C4 0.040(3) 0.027(3) 0.033(3) -0.004(2) 0.011(2) 0.006(2) C5 0.035(3) 0.031(3) 0.025(2) -0.002(2) 0.015(2) 0.004(2) C6 0.025(2) 0.030(3) 0.024(2) -0.001(2) 0.005(2) 0.007(2) C7 0.023(2) 0.027(2) 0.023(2) -0.0017(19) 0.006(2) -0.0007(19) C8 0.032(3) 0.022(2) 0.023(2) -0.0002(18) 0.008(2) -0.0013(19) C9 0.026(3) 0.031(3) 0.030(3) 0.000(2) 0.003(2) 0.005(2) C10 0.032(3) 0.029(3) 0.023(2) -0.001(2) 0.006(2) -0.001(2) C11 0.038(3) 0.017(2) 0.031(3) -0.0039(19) 0.017(2) -0.002(2) C12 0.038(3) 0.037(3) 0.021(2) 0.001(2) 0.007(2) -0.004(2) C13 0.034(3) 0.030(3) 0.022(2) 0.004(2) 0.004(2) 0.002(2) C14 0.042(3) 0.023(2) 0.031(3) 0.004(2) 0.010(2) -0.001(2) C15 0.034(3) 0.028(3) 0.032(3) -0.003(2) 0.011(2) -0.005(2) C16 0.032(3) 0.032(3) 0.034(3) 0.003(2) 0.015(2) -0.001(2) C17 0.024(2) 0.030(3) 0.022(2) 0.0002(19) 0.005(2) 0.0046(19) C18 0.028(3) 0.031(3) 0.029(3) 0.000(2) 0.010(2) 0.001(2) C19 0.029(3) 0.034(3) 0.029(3) 0.000(2) 0.013(2) 0.008(2) C20 0.038(3) 0.030(3) 0.023(2) -0.003(2) 0.012(2) 0.005(2) C21 0.039(3) 0.042(3) 0.034(3) -0.002(2) 0.020(3) -0.008(2) C22 0.044(3) 0.029(3) 0.038(3) 0.000(2) 0.023(3) 0.001(2) C23 0.038(3) 0.031(3) 0.029(3) 0.002(2) 0.014(2) 0.008(2) C24 0.046(3) 0.040(3) 0.029(3) 0.003(2) 0.019(3) 0.003(2) C25 0.040(3) 0.044(3) 0.028(3) 0.001(2) 0.018(2) 0.005(2) C26 0.029(3) 0.051(3) 0.040(3) 0.000(3) 0.020(3) 0.003(2) C27 0.071(4) 0.024(3) 0.060(4) -0.007(3) 0.041(3) 0.004(3) C28 0.022(2) 0.026(2) 0.027(2) -0.0028(19) 0.013(2) -0.0006(18) C29 0.026(2) 0.026(2) 0.031(3) -0.006(2) 0.009(2) -0.004(2) C30 0.029(3) 0.036(3) 0.022(2) -0.001(2) 0.005(2) -0.010(2) C31 0.025(3) 0.039(3) 0.030(3) -0.006(2) 0.011(2) -0.008(2) C32 0.032(3) 0.036(3) 0.026(2) -0.002(2) 0.014(2) -0.004(2) C33 0.029(3) 0.025(2) 0.029(2) -0.001(2) 0.014(2) -0.0030(19) C34 0.029(2) 0.025(2) 0.021(2) -0.0006(18) 0.005(2) -0.0007(19) C35 0.032(3) 0.028(3) 0.025(2) -0.004(2) 0.011(2) -0.004(2) C36 0.034(3) 0.027(3) 0.025(2) -0.003(2) 0.011(2) -0.001(2) C37 0.028(3) 0.046(3) 0.028(3) 0.004(2) 0.008(2) -0.005(2) C38 0.038(3) 0.029(3) 0.018(2) -0.0011(19) 0.008(2) -0.004(2) C39 0.040(3) 0.033(3) 0.021(2) 0.004(2) 0.011(2) -0.004(2) C40 0.037(3) 0.027(3) 0.032(3) 0.000(2) 0.013(2) -0.004(2) C41 0.044(3) 0.040(3) 0.025(3) 0.005(2) 0.010(2) 0.011(2) C42 0.031(3) 0.053(3) 0.022(2) 0.000(2) 0.002(2) -0.003(2) C43 0.038(3) 0.043(3) 0.020(2) -0.001(2) 0.001(2) -0.009(2) O2 0.0216(16) 0.0302(18) 0.0215(16) -0.0017(13) 0.0096(14) -0.0011(13) C44 0.025(2) 0.033(3) 0.021(2) -0.0037(19) 0.010(2) -0.002(2) C45 0.035(3) 0.026(3) 0.025(3) 0.001(2) 0.006(2) 0.000(2) C46 0.031(3) 0.026(2) 0.026(2) 0.0022(19) 0.008(2) -0.004(2) C47 0.035(3) 0.048(3) 0.021(2) -0.007(2) 0.011(2) -0.007(2) C48 0.033(3) 0.031(3) 0.026(3) -0.004(2) 0.012(2) -0.009(2) C49 0.028(3) 0.041(3) 0.021(2) -0.008(2) 0.001(2) -0.005(2) C50 0.035(3) 0.032(3) 0.025(2) -0.002(2) 0.007(2) 0.004(2) C51 0.045(3) 0.042(3) 0.022(3) 0.005(2) 0.002(2) -0.014(2) C52 0.041(3) 0.050(3) 0.024(3) -0.011(2) 0.016(2) -0.011(3) C53 0.040(3) 0.041(3) 0.030(3) -0.011(2) 0.010(2) 0.000(2) C54 0.038(3) 0.065(4) 0.039(3) -0.009(3) 0.021(3) -0.019(3) O3 0.094(5) 0.082(5) 0.150(6) 0.006(4) 0.062(5) 0.019(4) C55 0.118(7) 0.046(5) 0.177(10) 0.007(5) 0.107(8) 0.010(5) C56 0.110(8) 0.030(4) 0.232(13) 0.012(6) 0.059(9) 0.024(5) C57 0.120(8) 0.108(8) 0.076(6) 0.055(6) 0.044(6) 0.005(6) C58 0.074(6) 0.127(9) 0.086(6) -0.007(6) 0.035(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.868(3) . ? Nb1 O2 1.879(3) . ? Nb1 Cl1 2.3412(14) . ? Nb1 Cl2 2.3488(15) . ? O1 C1 1.390(5) . ? C1 C2 1.401(6) . ? C1 C6 1.409(6) . ? C2 C3 1.400(6) . ? C2 C7 1.562(7) . ? C3 C4 1.381(7) . ? C3 H1 0.9500 . ? C4 C5 1.385(7) . ? C4 C27 1.505(7) . ? C5 C6 1.400(6) . ? C5 H2 0.9500 . ? C6 C17 1.557(7) . ? C7 C8 1.548(6) . ? C7 C10 1.549(6) . ? C7 C9 1.553(6) . ? C8 C11 1.540(6) . ? C8 H3 0.9900 . ? C8 H4 0.9900 . ? C9 C13 1.530(7) . ? C9 H5 0.9900 . ? C9 H6 0.9900 . ? C10 C15 1.523(7) . ? C10 H7 0.9900 . ? C10 H8 0.9900 . ? C11 C16 1.531(7) . ? C11 C12 1.536(7) . ? C11 H9 1.0000 . ? C12 C13 1.517(7) . ? C12 H10 0.9900 . ? C12 H11 0.9900 . ? C13 C14 1.523(7) . ? C13 H12 1.0000 . ? C14 C15 1.532(7) . ? C14 H13 0.9900 . ? C14 H14 0.9900 . ? C15 C16 1.522(7) . ? C15 H15 1.0000 . ? C16 H16 0.9900 . ? C16 H17 0.9900 . ? C17 C18 1.528(6) . ? C17 C19 1.543(6) . ? C17 C20 1.546(6) . ? C18 C21 1.519(7) . ? C18 H18 0.9900 . ? C18 H19 0.9900 . ? C19 C23 1.535(7) . ? C19 H20 0.9900 . ? C19 H21 0.9900 . ? C20 C25 1.537(7) . ? C20 H22 0.9900 . ? C20 H23 0.9900 . ? C21 C26 1.523(7) . ? C21 C22 1.538(7) . ? C21 H24 1.0000 . ? C22 C23 1.527(7) . ? C22 H25 0.9900 . ? C22 H26 0.9900 . ? C23 C24 1.543(7) . ? C23 H27 1.0000 . ? C24 C25 1.531(7) . ? C24 H28 0.9900 . ? C24 H29 0.9900 . ? C25 C26 1.511(7) . ? C25 H30 1.0000 . ? C26 H31 0.9900 . ? C26 H32 0.9900 . ? C27 H33 0.9800 . ? C27 H34 0.9800 . ? C27 H35 0.9800 . ? C28 O2 1.381(5) . ? C28 C29 1.404(6) . ? C28 C33 1.419(6) . ? C29 C30 1.406(7) . ? C29 C34 1.557(7) . ? C30 C31 1.386(7) . ? C30 H36 0.9500 . ? C31 C32 1.370(7) . ? C31 C54 1.521(7) . ? C32 C33 1.408(6) . ? C32 H37 0.9500 . ? C33 C44 1.535(7) . ? C34 C35 1.542(6) . ? C34 C36 1.542(7) . ? C34 C37 1.550(7) . ? C35 C38 1.548(6) . ? C35 H38 0.9900 . ? C35 H39 0.9900 . ? C36 C40 1.538(7) . ? C36 H40 0.9900 . ? C36 H41 0.9900 . ? C37 C42 1.531(7) . ? C37 H42 0.9900 . ? C37 H43 0.9900 . ? C38 C43 1.523(7) . ? C38 C39 1.534(7) . ? C38 H44 1.0000 . ? C39 C40 1.525(7) . ? C39 H45 0.9900 . ? C39 H46 0.9900 . ? C40 C41 1.517(7) . ? C40 H47 1.0000 . ? C41 C42 1.526(7) . ? C41 H48 0.9900 . ? C41 H49 0.9900 . ? C42 C43 1.526(7) . ? C42 H50 1.0000 . ? C43 H51 0.9900 . ? C43 H52 0.9900 . ? C44 C47 1.548(6) . ? C44 C45 1.550(7) . ? C44 C46 1.555(7) . ? C45 C48 1.533(7) . ? C45 H53 0.9900 . ? C45 H54 0.9900 . ? C46 C50 1.529(7) . ? C46 H55 0.9900 . ? C46 H56 0.9900 . ? C47 C52 1.551(7) . ? C47 H57 0.9900 . ? C47 H58 0.9900 . ? C48 C49 1.509(7) . ? C48 C53 1.539(7) . ? C48 H59 1.0000 . ? C49 C50 1.528(7) . ? C49 H60 0.9900 . ? C49 H61 0.9900 . ? C50 C51 1.539(7) . ? C50 H62 1.0000 . ? C51 C52 1.537(8) . ? C51 H63 0.9900 . ? C51 H64 0.9900 . ? C52 C53 1.520(8) . ? C52 H65 1.0000 . ? C53 H66 0.9900 . ? C53 H67 0.9900 . ? C54 H68 0.9800 . ? C54 H69 0.9800 . ? C54 H70 0.9800 . ? O3 C58 1.357(10) . ? O3 C55 1.375(10) . ? C55 C56 1.663(13) . ? C55 H71 0.9900 . ? C55 H72 0.9900 . ? C56 C57 1.444(13) . ? C56 H73 0.9900 . ? C56 H74 0.9900 . ? C57 C58 1.453(11) . ? C57 H75 0.9900 . ? C57 H76 0.9900 . ? C58 H77 0.9900 . ? C58 H78 0.9900 . ? O4 C61 1.409(16) . ? O4 C61 1.409(16) 2_655 ? O4 C59 1.417(13) . ? O4 C59 1.417(13) 2_655 ? C59 C60 1.474(17) . ? C59 H79 0.9900 . ? C59 H80 0.9900 . ? C60 C60 1.51(3) 2_655 ? C60 H81 0.9900 . ? C60 H82 0.9900 . ? C61 C62 1.49(2) . ? C61 H83 0.9900 . ? C61 H84 0.9900 . ? C62 C62 1.54(4) 2_655 ? C62 H85 0.9900 . ? C62 H86 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nb1 O2 145.34(14) . . ? O1 Nb1 Cl1 98.80(10) . . ? O2 Nb1 Cl1 106.80(10) . . ? O1 Nb1 Cl2 104.33(10) . . ? O2 Nb1 Cl2 96.22(10) . . ? Cl1 Nb1 Cl2 95.43(5) . . ? C1 O1 Nb1 158.7(3) . . ? O1 C1 C2 120.3(4) . . ? O1 C1 C6 117.5(4) . . ? C2 C1 C6 122.1(4) . . ? C3 C2 C1 117.1(4) . . ? C3 C2 C7 113.6(4) . . ? C1 C2 C7 129.2(4) . . ? C4 C3 C2 123.1(5) . . ? C4 C3 H1 118.5 . . ? C2 C3 H1 118.5 . . ? C3 C4 C5 117.6(5) . . ? C3 C4 C27 121.0(5) . . ? C5 C4 C27 121.3(5) . . ? C4 C5 C6 123.0(5) . . ? C4 C5 H2 118.5 . . ? C6 C5 H2 118.5 . . ? C5 C6 C1 116.9(4) . . ? C5 C6 C17 118.7(4) . . ? C1 C6 C17 124.4(4) . . ? C8 C7 C10 106.0(4) . . ? C8 C7 C9 107.3(4) . . ? C10 C7 C9 109.1(4) . . ? C8 C7 C2 116.6(4) . . ? C10 C7 C2 109.7(4) . . ? C9 C7 C2 108.0(4) . . ? C11 C8 C7 111.3(4) . . ? C11 C8 H3 109.4 . . ? C7 C8 H3 109.4 . . ? C11 C8 H4 109.4 . . ? C7 C8 H4 109.4 . . ? H3 C8 H4 108.0 . . ? C13 C9 C7 110.8(4) . . ? C13 C9 H5 109.5 . . ? C7 C9 H5 109.5 . . ? C13 C9 H6 109.5 . . ? C7 C9 H6 109.5 . . ? H5 C9 H6 108.1 . . ? C15 C10 C7 112.2(4) . . ? C15 C10 H7 109.2 . . ? C7 C10 H7 109.2 . . ? C15 C10 H8 109.2 . . ? C7 C10 H8 109.2 . . ? H7 C10 H8 107.9 . . ? C16 C11 C12 110.1(4) . . ? C16 C11 C8 109.7(4) . . ? C12 C11 C8 108.7(4) . . ? C16 C11 H9 109.4 . . ? C12 C11 H9 109.4 . . ? C8 C11 H9 109.4 . . ? C13 C12 C11 109.4(4) . . ? C13 C12 H10 109.8 . . ? C11 C12 H10 109.8 . . ? C13 C12 H11 109.8 . . ? C11 C12 H11 109.8 . . ? H10 C12 H11 108.2 . . ? C12 C13 C14 109.4(4) . . ? C12 C13 C9 109.7(4) . . ? C14 C13 C9 109.4(4) . . ? C12 C13 H12 109.5 . . ? C14 C13 H12 109.5 . . ? C9 C13 H12 109.5 . . ? C13 C14 C15 110.8(4) . . ? C13 C14 H13 109.5 . . ? C15 C14 H13 109.5 . . ? C13 C14 H14 109.5 . . ? C15 C14 H14 109.5 . . ? H13 C14 H14 108.1 . . ? C16 C15 C10 108.9(4) . . ? C16 C15 C14 109.1(4) . . ? C10 C15 C14 109.3(4) . . ? C16 C15 H15 109.9 . . ? C10 C15 H15 109.9 . . ? C14 C15 H15 109.9 . . ? C15 C16 C11 109.3(4) . . ? C15 C16 H16 109.8 . . ? C11 C16 H16 109.8 . . ? C15 C16 H17 109.8 . . ? C11 C16 H17 109.8 . . ? H16 C16 H17 108.3 . . ? C18 C17 C19 108.9(4) . . ? C18 C17 C20 107.7(4) . . ? C19 C17 C20 107.3(4) . . ? C18 C17 C6 111.2(4) . . ? C19 C17 C6 111.2(4) . . ? C20 C17 C6 110.5(4) . . ? C21 C18 C17 111.2(4) . . ? C21 C18 H18 109.4 . . ? C17 C18 H18 109.4 . . ? C21 C18 H19 109.4 . . ? C17 C18 H19 109.4 . . ? H18 C18 H19 108.0 . . ? C23 C19 C17 110.2(4) . . ? C23 C19 H20 109.6 . . ? C17 C19 H20 109.6 . . ? C23 C19 H21 109.6 . . ? C17 C19 H21 109.6 . . ? H20 C19 H21 108.1 . . ? C25 C20 C17 111.6(4) . . ? C25 C20 H22 109.3 . . ? C17 C20 H22 109.3 . . ? C25 C20 H23 109.3 . . ? C17 C20 H23 109.3 . . ? H22 C20 H23 108.0 . . ? C18 C21 C26 110.6(4) . . ? C18 C21 C22 109.1(4) . . ? C26 C21 C22 109.0(4) . . ? C18 C21 H24 109.4 . . ? C26 C21 H24 109.4 . . ? C22 C21 H24 109.4 . . ? C23 C22 C21 109.8(4) . . ? C23 C22 H25 109.7 . . ? C21 C22 H25 109.7 . . ? C23 C22 H26 109.7 . . ? C21 C22 H26 109.7 . . ? H25 C22 H26 108.2 . . ? C22 C23 C19 109.4(4) . . ? C22 C23 C24 108.0(4) . . ? C19 C23 C24 110.9(4) . . ? C22 C23 H27 109.5 . . ? C19 C23 H27 109.5 . . ? C24 C23 H27 109.5 . . ? C25 C24 C23 108.8(4) . . ? C25 C24 H28 109.9 . . ? C23 C24 H28 109.9 . . ? C25 C24 H29 109.9 . . ? C23 C24 H29 109.9 . . ? H28 C24 H29 108.3 . . ? C26 C25 C24 110.2(4) . . ? C26 C25 C20 109.8(4) . . ? C24 C25 C20 108.6(4) . . ? C26 C25 H30 109.4 . . ? C24 C25 H30 109.4 . . ? C20 C25 H30 109.4 . . ? C25 C26 C21 109.2(4) . . ? C25 C26 H31 109.8 . . ? C21 C26 H31 109.8 . . ? C25 C26 H32 109.8 . . ? C21 C26 H32 109.8 . . ? H31 C26 H32 108.3 . . ? C4 C27 H33 109.5 . . ? C4 C27 H34 109.5 . . ? H33 C27 H34 109.5 . . ? C4 C27 H35 109.5 . . ? H33 C27 H35 109.5 . . ? H34 C27 H35 109.5 . . ? O2 C28 C29 119.5(4) . . ? O2 C28 C33 118.0(4) . . ? C29 C28 C33 122.5(4) . . ? C28 C29 C30 116.7(4) . . ? C28 C29 C34 123.3(4) . . ? C30 C29 C34 119.8(4) . . ? C31 C30 C29 122.0(5) . . ? C31 C30 H36 119.0 . . ? C29 C30 H36 119.0 . . ? C32 C31 C30 118.7(5) . . ? C32 C31 C54 121.4(5) . . ? C30 C31 C54 119.9(5) . . ? C31 C32 C33 123.3(5) . . ? C31 C32 H37 118.4 . . ? C33 C32 H37 118.4 . . ? C32 C33 C28 115.3(4) . . ? C32 C33 C44 120.2(4) . . ? C28 C33 C44 124.5(4) . . ? C35 C34 C36 109.4(4) . . ? C35 C34 C37 106.7(4) . . ? C36 C34 C37 105.9(4) . . ? C35 C34 C29 113.6(4) . . ? C36 C34 C29 110.2(4) . . ? C37 C34 C29 110.7(4) . . ? C34 C35 C38 111.8(4) . . ? C34 C35 H38 109.2 . . ? C38 C35 H38 109.2 . . ? C34 C35 H39 109.2 . . ? C38 C35 H39 109.2 . . ? H38 C35 H39 107.9 . . ? C40 C36 C34 110.5(4) . . ? C40 C36 H40 109.6 . . ? C34 C36 H40 109.6 . . ? C40 C36 H41 109.6 . . ? C34 C36 H41 109.6 . . ? H40 C36 H41 108.1 . . ? C42 C37 C34 112.4(4) . . ? C42 C37 H42 109.1 . . ? C34 C37 H42 109.1 . . ? C42 C37 H43 109.1 . . ? C34 C37 H43 109.1 . . ? H42 C37 H43 107.9 . . ? C43 C38 C39 109.6(4) . . ? C43 C38 C35 108.7(4) . . ? C39 C38 C35 108.1(4) . . ? C43 C38 H44 110.1 . . ? C39 C38 H44 110.1 . . ? C35 C38 H44 110.1 . . ? C40 C39 C38 110.2(4) . . ? C40 C39 H45 109.6 . . ? C38 C39 H45 109.6 . . ? C40 C39 H46 109.6 . . ? C38 C39 H46 109.6 . . ? H45 C39 H46 108.1 . . ? C41 C40 C39 109.4(4) . . ? C41 C40 C36 110.3(4) . . ? C39 C40 C36 110.3(4) . . ? C41 C40 H47 108.9 . . ? C39 C40 H47 108.9 . . ? C36 C40 H47 108.9 . . ? C40 C41 C42 108.4(4) . . ? C40 C41 H48 110.0 . . ? C42 C41 H48 110.0 . . ? C40 C41 H49 110.0 . . ? C42 C41 H49 110.0 . . ? H48 C41 H49 108.4 . . ? C41 C42 C43 110.8(4) . . ? C41 C42 C37 109.5(4) . . ? C43 C42 C37 108.3(4) . . ? C41 C42 H50 109.4 . . ? C43 C42 H50 109.4 . . ? C37 C42 H50 109.4 . . ? C38 C43 C42 109.8(4) . . ? C38 C43 H51 109.7 . . ? C42 C43 H51 109.7 . . ? C38 C43 H52 109.7 . . ? C42 C43 H52 109.7 . . ? H51 C43 H52 108.2 . . ? C28 O2 Nb1 153.0(3) . . ? C33 C44 C47 110.7(4) . . ? C33 C44 C45 109.4(4) . . ? C47 C44 C45 107.7(4) . . ? C33 C44 C46 112.7(4) . . ? C47 C44 C46 106.7(4) . . ? C45 C44 C46 109.5(4) . . ? C48 C45 C44 110.5(4) . . ? C48 C45 H53 109.6 . . ? C44 C45 H53 109.6 . . ? C48 C45 H54 109.6 . . ? C44 C45 H54 109.6 . . ? H53 C45 H54 108.1 . . ? C50 C46 C44 110.4(4) . . ? C50 C46 H55 109.6 . . ? C44 C46 H55 109.6 . . ? C50 C46 H56 109.6 . . ? C44 C46 H56 109.6 . . ? H55 C46 H56 108.1 . . ? C44 C47 C52 110.6(4) . . ? C44 C47 H57 109.5 . . ? C52 C47 H57 109.5 . . ? C44 C47 H58 109.5 . . ? C52 C47 H58 109.5 . . ? H57 C47 H58 108.1 . . ? C49 C48 C45 110.3(4) . . ? C49 C48 C53 109.7(4) . . ? C45 C48 C53 109.5(4) . . ? C49 C48 H59 109.1 . . ? C45 C48 H59 109.1 . . ? C53 C48 H59 109.1 . . ? C48 C49 C50 109.6(4) . . ? C48 C49 H60 109.8 . . ? C50 C49 H60 109.8 . . ? C48 C49 H61 109.8 . . ? C50 C49 H61 109.8 . . ? H60 C49 H61 108.2 . . ? C49 C50 C46 110.7(4) . . ? C49 C50 C51 109.2(4) . . ? C46 C50 C51 109.7(4) . . ? C49 C50 H62 109.1 . . ? C46 C50 H62 109.1 . . ? C51 C50 H62 109.1 . . ? C52 C51 C50 108.2(4) . . ? C52 C51 H63 110.1 . . ? C50 C51 H63 110.1 . . ? C52 C51 H64 110.1 . . ? C50 C51 H64 110.1 . . ? H63 C51 H64 108.4 . . ? C53 C52 C51 109.6(4) . . ? C53 C52 C47 110.0(4) . . ? C51 C52 C47 109.8(4) . . ? C53 C52 H65 109.2 . . ? C51 C52 H65 109.2 . . ? C47 C52 H65 109.2 . . ? C52 C53 C48 108.8(4) . . ? C52 C53 H66 109.9 . . ? C48 C53 H66 109.9 . . ? C52 C53 H67 109.9 . . ? C48 C53 H67 109.9 . . ? H66 C53 H67 108.3 . . ? C31 C54 H68 109.5 . . ? C31 C54 H69 109.5 . . ? H68 C54 H69 109.5 . . ? C31 C54 H70 109.5 . . ? H68 C54 H70 109.5 . . ? H69 C54 H70 109.5 . . ? C58 O3 C55 111.4(7) . . ? O3 C55 C56 104.0(7) . . ? O3 C55 H71 111.0 . . ? C56 C55 H71 111.0 . . ? O3 C55 H72 111.0 . . ? C56 C55 H72 111.0 . . ? H71 C55 H72 109.0 . . ? C57 C56 C55 95.2(7) . . ? C57 C56 H73 112.7 . . ? C55 C56 H73 112.7 . . ? C57 C56 H74 112.7 . . ? C55 C56 H74 112.7 . . ? H73 C56 H74 110.2 . . ? C56 C57 C58 108.8(8) . . ? C56 C57 H75 109.9 . . ? C58 C57 H75 109.9 . . ? C56 C57 H76 109.9 . . ? C58 C57 H76 109.9 . . ? H75 C57 H76 108.3 . . ? O3 C58 C57 99.0(8) . . ? O3 C58 H77 112.0 . . ? C57 C58 H77 112.0 . . ? O3 C58 H78 112.0 . . ? C57 C58 H78 112.0 . . ? H77 C58 H78 109.7 . . ? C61 O4 C61 113.8(15) . 2_655 ? C61 O4 C59 103.9(9) 2_655 . ? C61 O4 C59 103.9(9) . 2_655 ? C59 O4 C59 109.4(12) . 2_655 ? O4 C59 C60 108.7(10) . . ? O4 C59 H79 110.0 . . ? C60 C59 H79 110.0 . . ? O4 C59 H80 110.0 . . ? C60 C59 H80 110.0 . . ? H79 C59 H80 108.3 . . ? C59 C60 C60 104.8(8) . 2_655 ? C59 C60 H81 110.8 . . ? C60 C60 H81 110.8 2_655 . ? C59 C60 H82 110.8 . . ? C60 C60 H82 110.8 2_655 . ? H81 C60 H82 108.9 . . ? O4 C61 C62 105.7(12) . . ? O4 C61 H83 110.6 . . ? C62 C61 H83 110.6 . . ? O4 C61 H84 110.6 . . ? C62 C61 H84 110.6 . . ? H83 C61 H84 108.7 . . ? C61 C62 C62 104.5(10) . 2_655 ? C61 C62 H85 110.8 . . ? C62 C62 H85 110.8 2_655 . ? C61 C62 H86 110.8 . . ? C62 C62 H86 110.8 2_655 . ? H85 C62 H86 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Nb1 O1 C1 -50.3(9) . . . . ? Cl1 Nb1 O1 C1 87.2(8) . . . . ? Cl2 Nb1 O1 C1 -174.8(8) . . . . ? Nb1 O1 C1 C2 -0.9(11) . . . . ? Nb1 O1 C1 C6 -177.0(6) . . . . ? O1 C1 C2 C3 -178.8(4) . . . . ? C6 C1 C2 C3 -2.9(7) . . . . ? O1 C1 C2 C7 2.2(7) . . . . ? C6 C1 C2 C7 178.2(4) . . . . ? C1 C2 C3 C4 -0.1(7) . . . . ? C7 C2 C3 C4 179.0(4) . . . . ? C2 C3 C4 C5 1.6(8) . . . . ? C2 C3 C4 C27 -177.7(5) . . . . ? C3 C4 C5 C6 -0.1(8) . . . . ? C27 C4 C5 C6 179.2(5) . . . . ? C4 C5 C6 C1 -2.6(7) . . . . ? C4 C5 C6 C17 176.4(4) . . . . ? O1 C1 C6 C5 -179.8(4) . . . . ? C2 C1 C6 C5 4.2(7) . . . . ? O1 C1 C6 C17 1.2(7) . . . . ? C2 C1 C6 C17 -174.8(4) . . . . ? C3 C2 C7 C8 -175.0(4) . . . . ? C1 C2 C7 C8 3.9(7) . . . . ? C3 C2 C7 C10 -54.6(5) . . . . ? C1 C2 C7 C10 124.4(5) . . . . ? C3 C2 C7 C9 64.2(5) . . . . ? C1 C2 C7 C9 -116.9(5) . . . . ? C10 C7 C8 C11 58.0(5) . . . . ? C9 C7 C8 C11 -58.4(5) . . . . ? C2 C7 C8 C11 -179.6(4) . . . . ? C8 C7 C9 C13 58.2(5) . . . . ? C10 C7 C9 C13 -56.2(5) . . . . ? C2 C7 C9 C13 -175.4(4) . . . . ? C8 C7 C10 C15 -59.5(5) . . . . ? C9 C7 C10 C15 55.7(5) . . . . ? C2 C7 C10 C15 173.9(4) . . . . ? C7 C8 C11 C16 -60.2(5) . . . . ? C7 C8 C11 C12 60.3(5) . . . . ? C16 C11 C12 C13 59.8(5) . . . . ? C8 C11 C12 C13 -60.4(5) . . . . ? C11 C12 C13 C14 -58.9(5) . . . . ? C11 C12 C13 C9 61.1(5) . . . . ? C7 C9 C13 C12 -60.8(5) . . . . ? C7 C9 C13 C14 59.1(5) . . . . ? C12 C13 C14 C15 59.6(5) . . . . ? C9 C13 C14 C15 -60.6(5) . . . . ? C7 C10 C15 C16 61.8(5) . . . . ? C7 C10 C15 C14 -57.2(5) . . . . ? C13 C14 C15 C16 -59.6(5) . . . . ? C13 C14 C15 C10 59.3(5) . . . . ? C10 C15 C16 C11 -60.0(5) . . . . ? C14 C15 C16 C11 59.1(5) . . . . ? C12 C11 C16 C15 -59.9(5) . . . . ? C8 C11 C16 C15 59.7(5) . . . . ? C5 C6 C17 C18 -118.8(5) . . . . ? C1 C6 C17 C18 60.2(6) . . . . ? C5 C6 C17 C19 119.7(5) . . . . ? C1 C6 C17 C19 -61.3(6) . . . . ? C5 C6 C17 C20 0.8(6) . . . . ? C1 C6 C17 C20 179.8(4) . . . . ? C19 C17 C18 C21 -58.8(5) . . . . ? C20 C17 C18 C21 57.2(5) . . . . ? C6 C17 C18 C21 178.3(4) . . . . ? C18 C17 C19 C23 58.1(5) . . . . ? C20 C17 C19 C23 -58.2(5) . . . . ? C6 C17 C19 C23 -179.1(4) . . . . ? C18 C17 C20 C25 -56.8(5) . . . . ? C19 C17 C20 C25 60.2(5) . . . . ? C6 C17 C20 C25 -178.4(4) . . . . ? C17 C18 C21 C26 -60.1(5) . . . . ? C17 C18 C21 C22 59.7(5) . . . . ? C18 C21 C22 C23 -59.7(5) . . . . ? C26 C21 C22 C23 61.1(5) . . . . ? C21 C22 C23 C19 59.9(5) . . . . ? C21 C22 C23 C24 -61.0(5) . . . . ? C17 C19 C23 C22 -59.3(5) . . . . ? C17 C19 C23 C24 59.7(5) . . . . ? C22 C23 C24 C25 60.4(5) . . . . ? C19 C23 C24 C25 -59.5(6) . . . . ? C23 C24 C25 C26 -61.1(6) . . . . ? C23 C24 C25 C20 59.2(5) . . . . ? C17 C20 C25 C26 58.9(5) . . . . ? C17 C20 C25 C24 -61.7(5) . . . . ? C24 C25 C26 C21 60.9(6) . . . . ? C20 C25 C26 C21 -58.7(6) . . . . ? C18 C21 C26 C25 59.8(6) . . . . ? C22 C21 C26 C25 -60.1(6) . . . . ? O2 C28 C29 C30 166.6(4) . . . . ? C33 C28 C29 C30 -12.9(7) . . . . ? O2 C28 C29 C34 -19.0(7) . . . . ? C33 C28 C29 C34 161.5(4) . . . . ? C28 C29 C30 C31 3.0(7) . . . . ? C34 C29 C30 C31 -171.6(4) . . . . ? C29 C30 C31 C32 6.1(8) . . . . ? C29 C30 C31 C54 -177.2(5) . . . . ? C30 C31 C32 C33 -6.0(8) . . . . ? C54 C31 C32 C33 177.4(5) . . . . ? C31 C32 C33 C28 -3.2(7) . . . . ? C31 C32 C33 C44 175.1(5) . . . . ? O2 C28 C33 C32 -166.6(4) . . . . ? C29 C28 C33 C32 12.9(7) . . . . ? O2 C28 C33 C44 15.2(7) . . . . ? C29 C28 C33 C44 -165.3(4) . . . . ? C28 C29 C34 C35 71.4(6) . . . . ? C30 C29 C34 C35 -114.4(5) . . . . ? C28 C29 C34 C36 -51.8(6) . . . . ? C30 C29 C34 C36 122.4(5) . . . . ? C28 C29 C34 C37 -168.6(4) . . . . ? C30 C29 C34 C37 5.6(6) . . . . ? C36 C34 C35 C38 -57.1(5) . . . . ? C37 C34 C35 C38 57.0(5) . . . . ? C29 C34 C35 C38 179.2(4) . . . . ? C35 C34 C36 C40 55.9(5) . . . . ? C37 C34 C36 C40 -58.7(5) . . . . ? C29 C34 C36 C40 -178.4(4) . . . . ? C35 C34 C37 C42 -57.8(5) . . . . ? C36 C34 C37 C42 58.6(5) . . . . ? C29 C34 C37 C42 178.1(4) . . . . ? C34 C35 C38 C43 -60.1(5) . . . . ? C34 C35 C38 C39 58.8(5) . . . . ? C43 C38 C39 C40 58.5(5) . . . . ? C35 C38 C39 C40 -59.9(5) . . . . ? C38 C39 C40 C41 -60.7(5) . . . . ? C38 C39 C40 C36 60.8(5) . . . . ? C34 C36 C40 C41 62.5(5) . . . . ? C34 C36 C40 C39 -58.5(5) . . . . ? C39 C40 C41 C42 60.8(5) . . . . ? C36 C40 C41 C42 -60.7(5) . . . . ? C40 C41 C42 C43 -60.5(5) . . . . ? C40 C41 C42 C37 58.9(5) . . . . ? C34 C37 C42 C41 -60.2(6) . . . . ? C34 C37 C42 C43 60.8(6) . . . . ? C39 C38 C43 C42 -57.0(5) . . . . ? C35 C38 C43 C42 61.0(5) . . . . ? C41 C42 C43 C38 58.9(5) . . . . ? C37 C42 C43 C38 -61.2(5) . . . . ? C29 C28 O2 Nb1 -57.0(8) . . . . ? C33 C28 O2 Nb1 122.5(6) . . . . ? O1 Nb1 O2 C28 11.3(8) . . . . ? Cl1 Nb1 O2 C28 -124.5(6) . . . . ? Cl2 Nb1 O2 C28 137.9(6) . . . . ? C32 C33 C44 C47 -12.1(6) . . . . ? C28 C33 C44 C47 166.0(5) . . . . ? C32 C33 C44 C45 -130.7(5) . . . . ? C28 C33 C44 C45 47.5(6) . . . . ? C32 C33 C44 C46 107.3(5) . . . . ? C28 C33 C44 C46 -74.6(6) . . . . ? C33 C44 C45 C48 179.7(4) . . . . ? C47 C44 C45 C48 59.2(5) . . . . ? C46 C44 C45 C48 -56.4(5) . . . . ? C33 C44 C46 C50 177.8(4) . . . . ? C47 C44 C46 C50 -60.5(5) . . . . ? C45 C44 C46 C50 55.7(5) . . . . ? C33 C44 C47 C52 -177.6(4) . . . . ? C45 C44 C47 C52 -58.0(5) . . . . ? C46 C44 C47 C52 59.4(5) . . . . ? C44 C45 C48 C49 59.4(5) . . . . ? C44 C45 C48 C53 -61.5(5) . . . . ? C45 C48 C49 C50 -60.3(5) . . . . ? C53 C48 C49 C50 60.4(5) . . . . ? C48 C49 C50 C46 59.9(5) . . . . ? C48 C49 C50 C51 -60.9(5) . . . . ? C44 C46 C50 C49 -57.9(5) . . . . ? C44 C46 C50 C51 62.6(5) . . . . ? C49 C50 C51 C52 60.6(5) . . . . ? C46 C50 C51 C52 -60.8(5) . . . . ? C50 C51 C52 C53 -61.2(5) . . . . ? C50 C51 C52 C47 59.7(5) . . . . ? C44 C47 C52 C53 59.9(6) . . . . ? C44 C47 C52 C51 -60.8(6) . . . . ? C51 C52 C53 C48 60.8(5) . . . . ? C47 C52 C53 C48 -60.0(6) . . . . ? C49 C48 C53 C52 -60.2(5) . . . . ? C45 C48 C53 C52 61.0(5) . . . . ? C58 O3 C55 C56 -21.1(11) . . . . ? O3 C55 C56 C57 -8.5(10) . . . . ? C55 C56 C57 C58 33.5(10) . . . . ? C55 O3 C58 C57 41.3(10) . . . . ? C56 C57 C58 O3 -48.1(10) . . . . ? C61 O4 C59 C60 -90(2) . . . . ? C61 O4 C59 C60 23.7(12) 2_655 . . . ? C59 O4 C59 C60 -6.4(7) 2_655 . . . ? O4 C59 C60 C60 16.1(18) . . . 2_655 ? C61 O4 C61 C62 7.9(10) 2_655 . . . ? C59 O4 C61 C62 83(2) . . . . ? C59 O4 C61 C62 -21.4(13) 2_655 . . . ? O4 C61 C62 C62 -20(2) . . . 2_655 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 -0.296 0.500 190 26 ' ' 2 0.750 0.296 0.500 190 26 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.386 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.109 data_[{(ArO)2Nb}2(H)4](benzene)(pentane) _database_code_depnum_ccdc_archive 'CCDC 902914' #TrackingRef '14202_web_deposit_cif_file_0_HiroyukiKawaguchi_1348537764.CIF-kawaguchi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H144 Nb2 O4, C6 H6, C5 H12' _chemical_formula_sum 'C119 H162 Nb2 O4' _chemical_formula_weight 1842.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nb Nb -2.0727 0.6215 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 21.761(3) _cell_length_b 18.617(3) _cell_length_c 23.707(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.768(3) _cell_angle_gamma 90.00 _cell_volume 9584(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 21826 _cell_measurement_theta_min 3.0100 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3960 _exptl_absorpt_coefficient_mu 0.295 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9655 _exptl_absorpt_correction_T_max 0.9883 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Saturn CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 79045 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 21925 _reflns_number_gt 16228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1009P)^2^+18.1898P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21925 _refine_ls_number_parameters 1067 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1874 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.312426(15) 0.947047(18) 0.292090(14) 0.02140(10) Uani 1 1 d . . . Nb2 Nb 0.233654(15) 1.045278(17) 0.248563(14) 0.02120(10) Uani 1 1 d . . . O1 O 0.35632(12) 0.88483(15) 0.24474(11) 0.0263(6) Uani 1 1 d . . . O2 O 0.32988(13) 0.93832(15) 0.37201(12) 0.0276(6) Uani 1 1 d . . . O3 O 0.14855(12) 1.02472(15) 0.23210(12) 0.0271(6) Uani 1 1 d . . . O4 O 0.26023(14) 1.14034(15) 0.23397(12) 0.0310(6) Uani 1 1 d . . . H1 H 0.270(2) 0.988(3) 0.213(2) 0.057(16) Uiso 1 1 d . . . H2 H 0.237(2) 0.930(3) 0.279(2) 0.048(15) Uiso 1 1 d . . . H3 H 0.252(2) 1.033(2) 0.3141(19) 0.033(12) Uiso 1 1 d . . . H4 H 0.3235(19) 1.026(2) 0.2741(17) 0.023(10) Uiso 1 1 d . . . C1 C 0.3842(2) 0.8666(2) 0.19610(17) 0.0272(8) Uani 1 1 d . . . C2 C 0.3489(2) 0.8410(2) 0.14800(18) 0.0321(9) Uani 1 1 d . . . C3 C 0.3785(2) 0.8426(3) 0.09735(19) 0.0423(12) Uani 1 1 d . . . H5 H 0.3549 0.8314 0.0634 0.051 Uiso 1 1 calc R . . C4 C 0.4402(3) 0.8596(3) 0.0936(2) 0.0434(12) Uani 1 1 d . . . C5 C 0.4748(2) 0.8714(2) 0.14339(19) 0.0354(10) Uani 1 1 d . . . H6 H 0.5181 0.8772 0.1420 0.042 Uiso 1 1 calc R . . C6 C 0.44938(19) 0.8754(2) 0.19585(17) 0.0284(8) Uani 1 1 d . . . C7 C 0.2842(2) 0.8080(2) 0.14494(17) 0.0293(9) Uani 1 1 d . . . C8 C 0.2581(2) 0.7908(3) 0.2018(2) 0.0443(12) Uani 1 1 d . . . H7 H 0.2538 0.8359 0.2233 0.053 Uiso 1 1 calc R . . H8 H 0.2873 0.7593 0.2240 0.053 Uiso 1 1 calc R . . C9 C 0.2868(3) 0.7367(3) 0.1120(3) 0.0520(14) Uani 1 1 d . . . H9 H 0.3155 0.7033 0.1328 0.062 Uiso 1 1 calc R . . H10 H 0.3027 0.7460 0.0745 0.062 Uiso 1 1 calc R . . C10 C 0.2375(2) 0.8571(3) 0.1127(2) 0.0443(11) Uani 1 1 d . . . H11 H 0.2524 0.8689 0.0752 0.053 Uiso 1 1 calc R . . H12 H 0.2336 0.9026 0.1339 0.053 Uiso 1 1 calc R . . C11 C 0.1948(2) 0.7531(3) 0.1943(2) 0.0407(11) Uani 1 1 d . . . H13 H 0.1795 0.7424 0.2323 0.049 Uiso 1 1 calc R . . C12 C 0.1991(2) 0.6838(3) 0.1611(3) 0.0536(14) Uani 1 1 d . . . H14 H 0.2277 0.6501 0.1817 0.064 Uiso 1 1 calc R . . H15 H 0.1581 0.6608 0.1562 0.064 Uiso 1 1 calc R . . C13 C 0.2224(3) 0.7014(3) 0.1040(3) 0.0638(19) Uani 1 1 d . . . H16 H 0.2257 0.6560 0.0819 0.077 Uiso 1 1 calc R . . C14 C 0.1795(3) 0.7518(4) 0.0718(2) 0.0674(19) Uani 1 1 d . . . H17 H 0.1384 0.7293 0.0654 0.081 Uiso 1 1 calc R . . H18 H 0.1954 0.7625 0.0346 0.081 Uiso 1 1 calc R . . C15 C 0.1740(3) 0.8204(3) 0.1049(2) 0.0559(15) Uani 1 1 d . . . H19 H 0.1444 0.8534 0.0838 0.067 Uiso 1 1 calc R . . C16 C 0.1503(2) 0.8038(3) 0.1625(2) 0.0493(13) Uani 1 1 d . . . H20 H 0.1466 0.8488 0.1843 0.059 Uiso 1 1 calc R . . H21 H 0.1091 0.7813 0.1577 0.059 Uiso 1 1 calc R . . C17 C 0.4690(3) 0.8624(4) 0.0378(2) 0.0664(19) Uani 1 1 d . . . H22 H 0.4876 0.9098 0.0329 0.100 Uiso 1 1 calc R . . H23 H 0.4374 0.8539 0.0071 0.100 Uiso 1 1 calc R . . H24 H 0.5009 0.8253 0.0368 0.100 Uiso 1 1 calc R . . C18 C 0.49256(18) 0.8861(2) 0.24915(17) 0.0268(8) Uani 1 1 d . . . C19 C 0.4806(2) 0.8272(3) 0.2934(2) 0.0400(11) Uani 1 1 d . . . H25 H 0.4373 0.8299 0.3035 0.048 Uiso 1 1 calc R . . H26 H 0.4872 0.7793 0.2767 0.048 Uiso 1 1 calc R . . C20 C 0.4859(2) 0.9602(2) 0.2753(2) 0.0384(10) Uani 1 1 d . . . H27 H 0.4428 0.9674 0.2850 0.046 Uiso 1 1 calc R . . H28 H 0.4958 0.9975 0.2475 0.046 Uiso 1 1 calc R . . C21 C 0.5614(2) 0.8777(3) 0.2367(2) 0.0466(12) Uani 1 1 d . . . H29 H 0.5675 0.8297 0.2200 0.056 Uiso 1 1 calc R . . H30 H 0.5717 0.9141 0.2083 0.056 Uiso 1 1 calc R . . C22 C 0.5237(2) 0.8360(3) 0.3473(2) 0.0464(12) Uani 1 1 d . . . H31 H 0.5143 0.7988 0.3760 0.056 Uiso 1 1 calc R . . C23 C 0.5130(2) 0.9099(3) 0.3697(2) 0.0401(11) Uani 1 1 d . . . H32 H 0.5371 0.9156 0.4064 0.048 Uiso 1 1 calc R . . H33 H 0.4689 0.9150 0.3768 0.048 Uiso 1 1 calc R . . C24 C 0.5305(2) 0.9687(3) 0.3305(2) 0.0428(11) Uani 1 1 d . . . H34 H 0.5251 1.0169 0.3482 0.051 Uiso 1 1 calc R . . C25 C 0.5949(2) 0.9596(3) 0.3132(3) 0.0497(14) Uani 1 1 d . . . H35 H 0.6240 0.9681 0.3464 0.060 Uiso 1 1 calc R . . H36 H 0.6031 0.9962 0.2843 0.060 Uiso 1 1 calc R . . C26 C 0.6063(2) 0.8862(3) 0.2897(2) 0.0468(12) Uani 1 1 d . . . H37 H 0.6500 0.8811 0.2797 0.056 Uiso 1 1 calc R . . C27 C 0.5895(2) 0.8283(3) 0.3305(3) 0.0573(16) Uani 1 1 d . . . H38 H 0.6179 0.8307 0.3649 0.069 Uiso 1 1 calc R . . H39 H 0.5947 0.7806 0.3129 0.069 Uiso 1 1 calc R . . C28 C 0.31585(18) 0.9381(2) 0.42797(16) 0.0236(8) Uani 1 1 d . . . C29 C 0.32037(18) 1.0019(2) 0.46022(17) 0.0267(8) Uani 1 1 d . A . C30 C 0.29135(19) 1.0006(2) 0.51115(17) 0.0294(9) Uani 1 1 d . . . H40 H 0.2916 1.0434 0.5330 0.035 Uiso 1 1 calc R . . C31 C 0.2623(2) 0.9408(2) 0.53158(18) 0.0303(9) Uani 1 1 d . . . C32 C 0.26865(19) 0.8769(2) 0.50284(17) 0.0294(9) Uani 1 1 d . . . H41 H 0.2536 0.8340 0.5188 0.035 Uiso 1 1 calc R . . C33 C 0.29609(18) 0.8728(2) 0.45165(16) 0.0256(8) Uani 1 1 d . . . C34 C 0.35759(18) 1.0699(2) 0.44700(17) 0.0258(8) Uani 1 1 d . . . C35 C 0.4225(3) 1.0491(3) 0.4356(3) 0.0300(15) Uiso 0.622(6) 1 d P A 1 H42 H 0.4215 1.0153 0.4033 0.036 Uiso 0.622(6) 1 calc PR A 1 H43 H 0.4419 1.0243 0.4691 0.036 Uiso 0.622(6) 1 calc PR A 1 C36 C 0.3622(3) 1.1233(4) 0.4993(3) 0.0291(15) Uiso 0.622(6) 1 d P A 1 H44 H 0.3204 1.1400 0.5070 0.035 Uiso 0.622(6) 1 calc PR A 1 H45 H 0.3795 1.0974 0.5332 0.035 Uiso 0.622(6) 1 calc PR A 1 C37 C 0.3274(3) 1.1140(4) 0.3986(3) 0.0319(16) Uiso 0.622(6) 1 d P A 1 H46 H 0.2860 1.1298 0.4086 0.038 Uiso 0.622(6) 1 calc PR A 1 H47 H 0.3222 1.0838 0.3642 0.038 Uiso 0.622(6) 1 calc PR A 1 C38 C 0.4615(4) 1.1154(4) 0.4219(3) 0.0354(17) Uiso 0.622(6) 1 d P A 1 H48 H 0.5034 1.0995 0.4121 0.042 Uiso 0.622(6) 1 calc PR A 1 C39 C 0.4674(4) 1.1650(4) 0.4738(3) 0.0338(16) Uiso 0.622(6) 1 d P A 1 H49 H 0.4878 1.1391 0.5063 0.041 Uiso 0.622(6) 1 calc PR A 1 H50 H 0.4928 1.2074 0.4656 0.041 Uiso 0.622(6) 1 calc PR A 1 C40 C 0.4034(4) 1.1895(4) 0.4884(3) 0.0306(17) Uiso 0.622(6) 1 d P A 1 H51 H 0.4064 1.2215 0.5224 0.037 Uiso 0.622(6) 1 calc PR A 1 C41 C 0.3719(4) 1.2296(5) 0.4371(3) 0.0392(18) Uiso 0.622(6) 1 d P A 1 H52 H 0.3304 1.2457 0.4462 0.047 Uiso 0.622(6) 1 calc PR A 1 H53 H 0.3964 1.2726 0.4285 0.047 Uiso 0.622(6) 1 calc PR A 1 C42 C 0.3668(4) 1.1806(4) 0.3861(3) 0.0333(16) Uiso 0.622(6) 1 d P A 1 H54 H 0.3471 1.2072 0.3530 0.040 Uiso 0.622(6) 1 calc PR A 1 C43 C 0.4302(3) 1.1551(4) 0.3721(3) 0.0304(16) Uiso 0.622(6) 1 d P A 1 H55 H 0.4264 1.1229 0.3388 0.036 Uiso 0.622(6) 1 calc PR A 1 H56 H 0.4556 1.1969 0.3624 0.036 Uiso 0.622(6) 1 calc PR A 1 C44 C 0.3987(6) 1.0614(6) 0.3919(5) 0.035(3) Uiso 0.378(6) 1 d P A 2 H57 H 0.4254 1.0186 0.3965 0.042 Uiso 0.378(6) 1 calc PR A 2 H58 H 0.3711 1.0549 0.3574 0.042 Uiso 0.378(6) 1 calc PR A 2 C45 C 0.4041(6) 1.0804(8) 0.4959(6) 0.046(3) Uiso 0.378(6) 1 d P A 2 H59 H 0.4330 1.0393 0.4978 0.056 Uiso 0.378(6) 1 calc PR A 2 H60 H 0.3827 1.0814 0.5315 0.056 Uiso 0.378(6) 1 calc PR A 2 C46 C 0.3162(5) 1.1324(6) 0.4345(5) 0.034(3) Uiso 0.378(6) 1 d P A 2 H61 H 0.2888 1.1388 0.4658 0.041 Uiso 0.378(6) 1 calc PR A 2 H62 H 0.2902 1.1229 0.3995 0.041 Uiso 0.378(6) 1 calc PR A 2 C47 C 0.4396(6) 1.1309(7) 0.3857(5) 0.029(3) Uiso 0.378(6) 1 d P A 2 H63 H 0.4653 1.1266 0.3525 0.035 Uiso 0.378(6) 1 calc PR A 2 C48 C 0.4800(7) 1.1414(8) 0.4403(6) 0.045(3) Uiso 0.378(6) 1 d P A 2 H64 H 0.5064 1.0985 0.4472 0.054 Uiso 0.378(6) 1 calc PR A 2 H65 H 0.5072 1.1834 0.4362 0.054 Uiso 0.378(6) 1 calc PR A 2 C49 C 0.4417(7) 1.1529(7) 0.4900(6) 0.042(3) Uiso 0.378(6) 1 d P A 2 H66 H 0.4682 1.1631 0.5251 0.050 Uiso 0.378(6) 1 calc PR A 2 C50 C 0.3926(7) 1.2124(9) 0.4790(6) 0.041(3) Uiso 0.378(6) 1 d P A 2 H67 H 0.3659 1.2138 0.5112 0.049 Uiso 0.378(6) 1 calc PR A 2 H68 H 0.4138 1.2594 0.4775 0.049 Uiso 0.378(6) 1 calc PR A 2 C51 C 0.3541(7) 1.2027(9) 0.4271(6) 0.045(3) Uiso 0.378(6) 1 d P A 2 H69 H 0.3262 1.2448 0.4199 0.054 Uiso 0.378(6) 1 calc PR A 2 C52 C 0.3950(6) 1.1916(7) 0.3781(5) 0.035(3) Uiso 0.378(6) 1 d P A 2 H70 H 0.3684 1.1830 0.3432 0.041 Uiso 0.378(6) 1 calc PR A 2 H71 H 0.4183 1.2364 0.3724 0.041 Uiso 0.378(6) 1 calc PR A 2 C53 C 0.2248(2) 0.9462(3) 0.5826(2) 0.0400(11) Uani 1 1 d . . . H72 H 0.2020 0.9013 0.5870 0.060 Uiso 1 1 calc R . . H73 H 0.1957 0.9862 0.5776 0.060 Uiso 1 1 calc R . . H74 H 0.2523 0.9545 0.6164 0.060 Uiso 1 1 calc R . . C54 C 0.30647(18) 0.7985(2) 0.42467(17) 0.0262(8) Uani 1 1 d . . . C55 C 0.37515(18) 0.7906(2) 0.41187(18) 0.0285(8) Uani 1 1 d . . . H75 H 0.3862 0.8291 0.3855 0.034 Uiso 1 1 calc R . . H76 H 0.4013 0.7963 0.4473 0.034 Uiso 1 1 calc R . . C56 C 0.26565(19) 0.7844(2) 0.37041(18) 0.0286(8) Uani 1 1 d . . . H77 H 0.2218 0.7872 0.3790 0.034 Uiso 1 1 calc R . . H78 H 0.2733 0.8222 0.3423 0.034 Uiso 1 1 calc R . . C57 C 0.29289(19) 0.7371(2) 0.46609(17) 0.0277(8) Uani 1 1 d . . . H79 H 0.3183 0.7440 0.5019 0.033 Uiso 1 1 calc R . . H80 H 0.2491 0.7393 0.4748 0.033 Uiso 1 1 calc R . . C58 C 0.3878(2) 0.7165(2) 0.3855(2) 0.0335(9) Uani 1 1 d . . . H81 H 0.4320 0.7135 0.3765 0.040 Uiso 1 1 calc R . . C59 C 0.3467(2) 0.7067(2) 0.33170(19) 0.0351(10) Uani 1 1 d . . . H82 H 0.3553 0.6596 0.3145 0.042 Uiso 1 1 calc R . . H83 H 0.3556 0.7447 0.3042 0.042 Uiso 1 1 calc R . . C60 C 0.2785(2) 0.7104(2) 0.34510(18) 0.0319(9) Uani 1 1 d . . . H84 H 0.2518 0.7034 0.3096 0.038 Uiso 1 1 calc R . . C61 C 0.2653(2) 0.6514(2) 0.38753(18) 0.0310(9) Uani 1 1 d . . . H85 H 0.2735 0.6037 0.3711 0.037 Uiso 1 1 calc R . . H86 H 0.2215 0.6532 0.3963 0.037 Uiso 1 1 calc R . . C62 C 0.30661(19) 0.6626(2) 0.44159(18) 0.0298(9) Uani 1 1 d . . . H87 H 0.2976 0.6246 0.4697 0.036 Uiso 1 1 calc R . . C63 C 0.37376(19) 0.6579(2) 0.4283(2) 0.0343(10) Uani 1 1 d . . . H88 H 0.3824 0.6101 0.4125 0.041 Uiso 1 1 calc R . . H89 H 0.4004 0.6644 0.4634 0.041 Uiso 1 1 calc R . . C64 C 0.09722(18) 0.9837(2) 0.21631(18) 0.0278(8) Uani 1 1 d . . . C65 C 0.07574(19) 0.9844(2) 0.15895(19) 0.0306(9) Uani 1 1 d . . . C66 C 0.0321(2) 0.9327(2) 0.1419(2) 0.0389(11) Uani 1 1 d . . . H90 H 0.0184 0.9305 0.1030 0.047 Uiso 1 1 calc R . . C67 C 0.0080(2) 0.8845(2) 0.1788(2) 0.0392(11) Uani 1 1 d . . . C68 C 0.0248(2) 0.8920(2) 0.2357(2) 0.0340(9) Uani 1 1 d . . . H91 H 0.0060 0.8614 0.2617 0.041 Uiso 1 1 calc R . . C69 C 0.06800(18) 0.9425(2) 0.25708(19) 0.0301(9) Uani 1 1 d . . . C70 C 0.0940(2) 1.0420(2) 0.1165(2) 0.0344(10) Uani 1 1 d . . . C71 C 0.0783(2) 1.1169(2) 0.1391(2) 0.0386(10) Uani 1 1 d . . . H92 H 0.0339 1.1189 0.1454 0.046 Uiso 1 1 calc R . . H93 H 0.1016 1.1248 0.1759 0.046 Uiso 1 1 calc R . . C72 C 0.0565(3) 1.0338(3) 0.0584(2) 0.0464(12) Uani 1 1 d . . . H94 H 0.0659 0.9866 0.0418 0.056 Uiso 1 1 calc R . . H95 H 0.0120 1.0350 0.0645 0.056 Uiso 1 1 calc R . . C73 C 0.1624(2) 1.0405(2) 0.10248(19) 0.0362(10) Uani 1 1 d . . . H96 H 0.1888 1.0457 0.1379 0.043 Uiso 1 1 calc R . . H97 H 0.1718 0.9935 0.0856 0.043 Uiso 1 1 calc R . . C74 C 0.0941(3) 1.1768(3) 0.0979(2) 0.0457(12) Uani 1 1 d . . . H98 H 0.0844 1.2246 0.1143 0.055 Uiso 1 1 calc R . . C75 C 0.0558(3) 1.1659(3) 0.0415(2) 0.0583(16) Uani 1 1 d . . . H99 H 0.0113 1.1678 0.0480 0.070 Uiso 1 1 calc R . . H100 H 0.0649 1.2047 0.0147 0.070 Uiso 1 1 calc R . . C76 C 0.0716(3) 1.0934(3) 0.0168(2) 0.0550(15) Uani 1 1 d . . . H101 H 0.0464 1.0861 -0.0196 0.066 Uiso 1 1 calc R . . C77 C 0.1397(3) 1.0901(3) 0.0056(2) 0.0532(14) Uani 1 1 d . . . H102 H 0.1496 1.1281 -0.0215 0.064 Uiso 1 1 calc R . . H103 H 0.1494 1.0430 -0.0109 0.064 Uiso 1 1 calc R . . C78 C 0.1778(2) 1.1008(3) 0.06126(19) 0.0413(11) Uani 1 1 d . . . H104 H 0.2227 1.0993 0.0544 0.050 Uiso 1 1 calc R . . C79 C 0.1620(2) 1.1731(3) 0.0873(2) 0.0437(12) Uani 1 1 d . . . H105 H 0.1868 1.1797 0.1234 0.052 Uiso 1 1 calc R . . H106 H 0.1723 1.2124 0.0614 0.052 Uiso 1 1 calc R . . C80 C -0.0368(3) 0.8267(3) 0.1575(3) 0.0538(14) Uani 1 1 d . . . H107 H -0.0647 0.8463 0.1272 0.081 Uiso 1 1 calc R . . H108 H -0.0608 0.8102 0.1886 0.081 Uiso 1 1 calc R . . H109 H -0.0139 0.7861 0.1429 0.081 Uiso 1 1 calc R . . C81 C 0.07462(19) 0.9501(2) 0.32237(19) 0.0291(9) Uani 1 1 d . . . C82 C 0.1125(2) 1.0151(3) 0.3457(2) 0.0404(11) Uani 1 1 d . . . H110 H 0.1550 1.0112 0.3334 0.048 Uiso 1 1 calc R . . H111 H 0.0943 1.0597 0.3292 0.048 Uiso 1 1 calc R . . C83 C 0.1038(3) 0.8828(3) 0.3502(2) 0.0470(12) Uani 1 1 d . . . H112 H 0.1465 0.8774 0.3386 0.056 Uiso 1 1 calc R . . H113 H 0.0801 0.8398 0.3371 0.056 Uiso 1 1 calc R . . C84 C 0.0097(2) 0.9608(3) 0.3443(2) 0.0450(12) Uani 1 1 d . . . H114 H -0.0168 0.9199 0.3317 0.054 Uiso 1 1 calc R . . H115 H -0.0087 1.0051 0.3276 0.054 Uiso 1 1 calc R . . C85 C 0.1152(2) 1.0208(3) 0.4103(2) 0.0419(11) Uani 1 1 d . . . H116 H 0.1412 1.0628 0.4232 0.050 Uiso 1 1 calc R . . C86 C 0.1427(2) 0.9527(3) 0.4338(2) 0.0503(14) Uani 1 1 d . . . H117 H 0.1464 0.9557 0.4756 0.060 Uiso 1 1 calc R . . H118 H 0.1847 0.9470 0.4206 0.060 Uiso 1 1 calc R . . C87 C 0.1047(2) 0.8878(3) 0.4162(2) 0.0491(13) Uani 1 1 d . . . H119 H 0.1232 0.8434 0.4338 0.059 Uiso 1 1 calc R . . C88 C 0.0395(2) 0.8972(3) 0.4329(3) 0.0502(13) Uani 1 1 d . . . H120 H 0.0392 0.8970 0.4746 0.060 Uiso 1 1 calc R . . H121 H 0.0142 0.8562 0.4183 0.060 Uiso 1 1 calc R . . C89 C 0.0113(2) 0.9663(3) 0.4103(2) 0.0479(13) Uani 1 1 d . . . H122 H -0.0315 0.9717 0.4228 0.057 Uiso 1 1 calc R . . C90 C 0.0495(2) 1.0302(3) 0.4287(3) 0.0506(13) Uani 1 1 d . . . H123 H 0.0503 1.0352 0.4703 0.061 Uiso 1 1 calc R . . H124 H 0.0311 1.0744 0.4115 0.061 Uiso 1 1 calc R . . C91 C 0.29243(18) 1.2037(2) 0.24268(17) 0.0265(8) Uani 1 1 d . . . C92 C 0.26679(19) 1.2575(2) 0.27629(17) 0.0280(8) Uani 1 1 d . B . C93 C 0.30534(19) 1.3151(2) 0.29308(18) 0.0306(9) Uani 1 1 d . . . H125 H 0.2893 1.3518 0.3158 0.037 Uiso 1 1 calc R . . C94 C 0.3653(2) 1.3212(2) 0.2782(2) 0.0351(10) Uani 1 1 d . . . C95 C 0.3853(2) 1.2720(2) 0.23971(19) 0.0341(9) Uani 1 1 d . . . H126 H 0.4252 1.2782 0.2264 0.041 Uiso 1 1 calc R . . C96 C 0.35009(19) 1.2139(2) 0.21941(18) 0.0291(9) Uani 1 1 d . C . C97 C 0.19924(18) 1.2605(2) 0.29198(18) 0.0284(8) Uani 1 1 d . . . C98 C 0.1562(3) 1.2577(4) 0.2377(3) 0.0314(15) Uiso 0.636(6) 1 d P B 1 H127 H 0.1633 1.2123 0.2174 0.038 Uiso 0.636(6) 1 calc PR B 1 H128 H 0.1664 1.2980 0.2126 0.038 Uiso 0.636(6) 1 calc PR B 1 C99 C 0.1840(3) 1.3350(4) 0.3207(3) 0.0329(16) Uiso 0.636(6) 1 d P B 1 H129 H 0.2099 1.3399 0.3565 0.039 Uiso 0.636(6) 1 calc PR B 1 H130 H 0.1951 1.3746 0.2954 0.039 Uiso 0.636(6) 1 calc PR B 1 C100 C 0.1812(3) 1.2035(4) 0.3341(3) 0.0306(15) Uiso 0.636(6) 1 d P B 1 H131 H 0.2072 1.2091 0.3697 0.037 Uiso 0.636(6) 1 calc PR B 1 H132 H 0.1892 1.1553 0.3186 0.037 Uiso 0.636(6) 1 calc PR B 1 C101 C 0.0876(4) 1.2626(5) 0.2505(4) 0.040(2) Uiso 0.636(6) 1 d P B 1 H133 H 0.0609 1.2582 0.2147 0.048 Uiso 0.636(6) 1 calc PR B 1 C102 C 0.0762(4) 1.3339(4) 0.2784(4) 0.0416(19) Uiso 0.636(6) 1 d P B 1 H134 H 0.0322 1.3375 0.2861 0.050 Uiso 0.636(6) 1 calc PR B 1 H135 H 0.0856 1.3732 0.2523 0.050 Uiso 0.636(6) 1 calc PR B 1 C103 C 0.1154(6) 1.3430(7) 0.3336(5) 0.038(3) Uiso 0.636(6) 1 d P B 1 H136 H 0.1076 1.3907 0.3512 0.046 Uiso 0.636(6) 1 calc PR B 1 C104 C 0.1017(4) 1.2810(4) 0.3741(3) 0.0408(18) Uiso 0.636(6) 1 d P B 1 H137 H 0.1284 1.2856 0.4094 0.049 Uiso 0.636(6) 1 calc PR B 1 H138 H 0.0583 1.2839 0.3841 0.049 Uiso 0.636(6) 1 calc PR B 1 C105 C 0.1129(4) 1.2091(5) 0.3469(4) 0.038(2) Uiso 0.636(6) 1 d P B 1 H139 H 0.1022 1.1695 0.3730 0.045 Uiso 0.636(6) 1 calc PR B 1 C106 C 0.0740(5) 1.2021(6) 0.2902(5) 0.045(3) Uiso 0.636(6) 1 d P B 1 H140 H 0.0832 1.1556 0.2723 0.054 Uiso 0.636(6) 1 calc PR B 1 H141 H 0.0297 1.2027 0.2974 0.054 Uiso 0.636(6) 1 calc PR B 1 C107 C 0.1601(5) 1.1916(6) 0.2768(5) 0.028(2) Uiso 0.364(6) 1 d P B 2 H142 H 0.1783 1.1495 0.2973 0.034 Uiso 0.364(6) 1 calc PR B 2 H143 H 0.1599 1.1819 0.2357 0.034 Uiso 0.364(6) 1 calc PR B 2 C108 C 0.1708(5) 1.3219(6) 0.2604(5) 0.027(2) Uiso 0.364(6) 1 d P B 2 H144 H 0.1702 1.3119 0.2194 0.033 Uiso 0.364(6) 1 calc PR B 2 H145 H 0.1961 1.3654 0.2682 0.033 Uiso 0.364(6) 1 calc PR B 2 C109 C 0.1991(5) 1.2691(6) 0.3564(5) 0.028(2) Uiso 0.364(6) 1 d P B 2 H146 H 0.2253 1.3104 0.3689 0.033 Uiso 0.364(6) 1 calc PR B 2 H147 H 0.2160 1.2253 0.3754 0.033 Uiso 0.364(6) 1 calc PR B 2 C110 C 0.0911(8) 1.2039(9) 0.2944(7) 0.035(4) Uiso 0.364(6) 1 d P B 2 H148 H 0.0651 1.1609 0.2843 0.042 Uiso 0.364(6) 1 calc PR B 2 C111 C 0.0665(7) 1.2694(7) 0.2617(6) 0.036(3) Uiso 0.364(6) 1 d P B 2 H149 H 0.0674 1.2602 0.2207 0.043 Uiso 0.364(6) 1 calc PR B 2 H150 H 0.0231 1.2777 0.2702 0.043 Uiso 0.364(6) 1 calc PR B 2 C112 C 0.1042(7) 1.3362(8) 0.2771(6) 0.041(3) Uiso 0.364(6) 1 d P B 2 H151 H 0.0863 1.3797 0.2574 0.050 Uiso 0.364(6) 1 calc PR B 2 C113 C 0.1060(11) 1.3447(12) 0.3405(9) 0.041(6) Uiso 0.364(6) 1 d P B 2 H152 H 0.1312 1.3875 0.3513 0.049 Uiso 0.364(6) 1 calc PR B 2 H153 H 0.0637 1.3537 0.3517 0.049 Uiso 0.364(6) 1 calc PR B 2 C114 C 0.1316(6) 1.2819(6) 0.3724(5) 0.031(3) Uiso 0.364(6) 1 d P B 2 H154 H 0.1307 1.2906 0.4139 0.037 Uiso 0.364(6) 1 calc PR B 2 C115 C 0.0932(8) 1.2169(8) 0.3557(6) 0.041(4) Uiso 0.364(6) 1 d P B 2 H155 H 0.1107 1.1742 0.3758 0.050 Uiso 0.364(6) 1 calc PR B 2 H156 H 0.0508 1.2240 0.3674 0.050 Uiso 0.364(6) 1 calc PR B 2 C116 C 0.4067(2) 1.3804(3) 0.3016(2) 0.0476(12) Uani 1 1 d . . . H157 H 0.4298 1.3635 0.3360 0.071 Uiso 1 1 calc R . . H158 H 0.3816 1.4220 0.3107 0.071 Uiso 1 1 calc R . . H159 H 0.4355 1.3941 0.2735 0.071 Uiso 1 1 calc R . . C117 C 0.37487(19) 1.1707(2) 0.17054(18) 0.0300(9) Uani 1 1 d . . . C118 C 0.3293(4) 1.1131(4) 0.1425(3) 0.0324(19) Uiso 0.526(6) 1 d P C 1 H160 H 0.3202 1.0762 0.1709 0.039 Uiso 0.526(6) 1 calc PR C 1 H161 H 0.2901 1.1367 0.1298 0.039 Uiso 0.526(6) 1 calc PR C 1 C119 C 0.4318(4) 1.1266(5) 0.1936(4) 0.034(2) Uiso 0.526(6) 1 d P C 1 H162 H 0.4625 1.1590 0.2130 0.041 Uiso 0.526(6) 1 calc PR C 1 H163 H 0.4191 1.0907 0.2213 0.041 Uiso 0.526(6) 1 calc PR C 1 C120 C 0.3902(4) 1.2224(5) 0.1257(4) 0.038(2) Uiso 0.526(6) 1 d P C 1 H164 H 0.4183 1.2595 0.1425 0.046 Uiso 0.526(6) 1 calc PR C 1 H165 H 0.3519 1.2467 0.1110 0.046 Uiso 0.526(6) 1 calc PR C 1 C121 C 0.3569(5) 1.0770(7) 0.0921(5) 0.044(3) Uiso 0.526(6) 1 d P C 1 H166 H 0.3264 1.0426 0.0739 0.052 Uiso 0.526(6) 1 calc PR C 1 C122 C 0.4112(5) 1.0373(6) 0.1153(5) 0.046(3) Uiso 0.526(6) 1 d P C 1 H167 H 0.4296 1.0106 0.0844 0.055 Uiso 0.526(6) 1 calc PR C 1 H168 H 0.3984 1.0019 0.1434 0.055 Uiso 0.526(6) 1 calc PR C 1 C123 C 0.4607(5) 1.0884(6) 0.1440(5) 0.049(3) Uiso 0.526(6) 1 d P C 1 H169 H 0.4980 1.0605 0.1579 0.059 Uiso 0.526(6) 1 calc PR C 1 C124 C 0.4776(5) 1.1443(6) 0.1006(4) 0.046(2) Uiso 0.526(6) 1 d P C 1 H170 H 0.4977 1.1201 0.0695 0.055 Uiso 0.526(6) 1 calc PR C 1 H171 H 0.5076 1.1786 0.1188 0.055 Uiso 0.526(6) 1 calc PR C 1 C125 C 0.4207(5) 1.1861(5) 0.0760(4) 0.043(2) Uiso 0.526(6) 1 d P C 1 H172 H 0.4327 1.2226 0.0478 0.052 Uiso 0.526(6) 1 calc PR C 1 C126 C 0.3755(5) 1.1318(5) 0.0487(4) 0.043(2) Uiso 0.526(6) 1 d P C 1 H173 H 0.3384 1.1572 0.0326 0.051 Uiso 0.526(6) 1 calc PR C 1 H174 H 0.3947 1.1069 0.0175 0.051 Uiso 0.526(6) 1 calc PR C 1 C127 C 0.3260(4) 1.1720(5) 0.1196(4) 0.034(2) Uiso 0.474(6) 1 d P C 2 H175 H 0.2872 1.1506 0.1314 0.041 Uiso 0.474(6) 1 calc PR C 2 H176 H 0.3174 1.2225 0.1086 0.041 Uiso 0.474(6) 1 calc PR C 2 C128 C 0.3927(5) 1.0949(6) 0.1842(4) 0.041(2) Uiso 0.474(6) 1 d P C 2 H177 H 0.3563 1.0692 0.1970 0.050 Uiso 0.474(6) 1 calc PR C 2 H178 H 0.4246 1.0951 0.2160 0.050 Uiso 0.474(6) 1 calc PR C 2 C129 C 0.4336(5) 1.2070(5) 0.1456(4) 0.039(2) Uiso 0.474(6) 1 d P C 2 H179 H 0.4233 1.2570 0.1343 0.047 Uiso 0.474(6) 1 calc PR C 2 H180 H 0.4675 1.2089 0.1755 0.047 Uiso 0.474(6) 1 calc PR C 2 C130 C 0.3473(5) 1.1307(6) 0.0684(5) 0.040(2) Uiso 0.474(6) 1 d P C 2 H181 H 0.3141 1.1298 0.0372 0.047 Uiso 0.474(6) 1 calc PR C 2 C131 C 0.3633(6) 1.0543(7) 0.0883(6) 0.043(3) Uiso 0.474(6) 1 d P C 2 H182 H 0.3736 1.0249 0.0554 0.052 Uiso 0.474(6) 1 calc PR C 2 H183 H 0.3269 1.0325 0.1045 0.052 Uiso 0.474(6) 1 calc PR C 2 C132 C 0.4182(6) 1.0525(7) 0.1332(6) 0.049(3) Uiso 0.474(6) 1 d P C 2 H184 H 0.4285 1.0019 0.1444 0.059 Uiso 0.474(6) 1 calc PR C 2 C133 C 0.4709(6) 1.0879(7) 0.1125(6) 0.053(3) Uiso 0.474(6) 1 d P C 2 H185 H 0.4849 1.0610 0.0797 0.064 Uiso 0.474(6) 1 calc PR C 2 H186 H 0.5049 1.0878 0.1424 0.064 Uiso 0.474(6) 1 calc PR C 2 C134 C 0.4558(5) 1.1668(6) 0.0945(4) 0.035(2) Uiso 0.474(6) 1 d P C 2 H187 H 0.4932 1.1906 0.0808 0.042 Uiso 0.474(6) 1 calc PR C 2 C135 C 0.4053(5) 1.1647(6) 0.0485(5) 0.039(2) Uiso 0.474(6) 1 d P C 2 H188 H 0.4194 1.1371 0.0160 0.046 Uiso 0.474(6) 1 calc PR C 2 H189 H 0.3960 1.2143 0.0354 0.046 Uiso 0.474(6) 1 calc PR C 2 C136 C 0.1436(6) 0.4226(7) 0.1237(6) 0.141(4) Uiso 1 1 d . . . H190 H 0.1247 0.4109 0.1575 0.169 Uiso 1 1 calc R . . C137 C 0.1350(5) 0.4875(7) 0.1011(5) 0.130(4) Uiso 1 1 d . . . H191 H 0.1055 0.5200 0.1143 0.156 Uiso 1 1 calc R . . C138 C 0.1686(6) 0.5038(8) 0.0605(6) 0.151(4) Uiso 1 1 d . . . H192 H 0.1681 0.5520 0.0473 0.181 Uiso 1 1 calc R . . C139 C 0.2054(7) 0.4545(8) 0.0349(7) 0.169(5) Uiso 1 1 d . . . H193 H 0.2287 0.4682 0.0042 0.202 Uiso 1 1 calc R . . C140 C 0.2076(6) 0.3855(8) 0.0551(6) 0.148(4) Uiso 1 1 d . . . H194 H 0.2293 0.3486 0.0373 0.178 Uiso 1 1 calc R . . C141 C 0.1783(5) 0.3737(7) 0.0997(5) 0.129(4) Uiso 1 1 d . . . H195 H 0.1816 0.3274 0.1164 0.155 Uiso 1 1 calc R . . C142 C 0.2813(6) 0.5170(7) 0.2407(5) 0.150(4) Uiso 1 1 d . . . H196 H 0.2840 0.5454 0.2756 0.225 Uiso 1 1 calc R . . H197 H 0.2812 0.4658 0.2501 0.225 Uiso 1 1 calc R . . H198 H 0.2432 0.5292 0.2184 0.225 Uiso 1 1 calc R . . C143 C 0.3402(5) 0.5348(6) 0.2042(5) 0.129(4) Uiso 1 1 d . . . H199 H 0.3399 0.5877 0.2000 0.155 Uiso 1 1 calc R . . H200 H 0.3766 0.5235 0.2298 0.155 Uiso 1 1 calc R . . C144 C 0.3554(9) 0.5072(12) 0.1486(8) 0.237(8) Uiso 1 1 d . . . H206 H 0.3167 0.5101 0.1243 0.284 Uiso 1 1 calc R . . H207 H 0.3837 0.5430 0.1335 0.284 Uiso 1 1 calc R . . C145 C 0.3790(8) 0.4447(9) 0.1381(7) 0.174(6) Uiso 1 1 d . . . H208 H 0.3606 0.4101 0.1638 0.209 Uiso 1 1 calc R . . H209 H 0.4233 0.4477 0.1502 0.209 Uiso 1 1 calc R . . C146 C 0.3754(7) 0.4114(9) 0.0825(7) 0.196(6) Uiso 1 1 d . . . H203 H 0.3965 0.3648 0.0846 0.294 Uiso 1 1 calc R . . H204 H 0.3952 0.4426 0.0557 0.294 Uiso 1 1 calc R . . H205 H 0.3321 0.4042 0.0696 0.294 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.02255(18) 0.02180(18) 0.01982(18) 0.00032(12) 0.00130(13) 0.00134(13) Nb2 0.02057(18) 0.01938(17) 0.02342(18) 0.00003(12) -0.00020(13) -0.00163(12) O1 0.0274(14) 0.0264(14) 0.0253(14) 0.0029(11) 0.0036(11) 0.0016(11) O2 0.0299(15) 0.0300(14) 0.0233(14) 0.0056(11) 0.0044(12) -0.0020(12) O3 0.0229(13) 0.0271(14) 0.0309(15) -0.0001(11) -0.0024(11) -0.0034(11) O4 0.0391(16) 0.0246(14) 0.0287(15) 0.0016(11) -0.0028(13) -0.0061(12) C1 0.036(2) 0.0222(19) 0.0239(19) -0.0011(14) 0.0083(17) 0.0019(16) C2 0.039(2) 0.031(2) 0.026(2) 0.0005(16) 0.0041(18) -0.0032(18) C3 0.058(3) 0.046(3) 0.023(2) -0.0052(19) 0.008(2) -0.019(2) C4 0.059(3) 0.043(3) 0.031(2) -0.007(2) 0.018(2) -0.013(2) C5 0.037(2) 0.033(2) 0.038(2) -0.0038(18) 0.015(2) -0.0030(19) C6 0.032(2) 0.0246(19) 0.029(2) -0.0005(15) 0.0060(17) 0.0022(16) C7 0.036(2) 0.027(2) 0.025(2) -0.0025(15) 0.0017(17) -0.0052(17) C8 0.036(2) 0.059(3) 0.037(3) 0.005(2) 0.000(2) -0.013(2) C9 0.051(3) 0.035(3) 0.073(4) -0.018(2) 0.024(3) -0.012(2) C10 0.046(3) 0.041(3) 0.046(3) 0.008(2) -0.001(2) -0.001(2) C11 0.034(2) 0.049(3) 0.039(3) 0.005(2) 0.002(2) -0.015(2) C12 0.040(3) 0.034(3) 0.087(4) -0.001(3) 0.013(3) -0.008(2) C13 0.067(4) 0.048(3) 0.081(4) -0.041(3) 0.035(3) -0.024(3) C14 0.068(4) 0.095(5) 0.040(3) -0.014(3) 0.002(3) -0.044(4) C15 0.045(3) 0.063(4) 0.058(3) 0.018(3) -0.012(3) -0.008(3) C16 0.046(3) 0.043(3) 0.060(3) -0.012(2) 0.005(3) -0.003(2) C17 0.087(5) 0.078(4) 0.039(3) -0.016(3) 0.034(3) -0.036(4) C18 0.028(2) 0.0212(18) 0.032(2) 0.0006(15) 0.0098(17) -0.0012(15) C19 0.038(2) 0.033(2) 0.049(3) 0.003(2) 0.003(2) 0.001(2) C20 0.033(2) 0.035(2) 0.047(3) 0.000(2) -0.001(2) 0.0016(19) C21 0.041(3) 0.044(3) 0.057(3) -0.002(2) 0.014(2) 0.001(2) C22 0.054(3) 0.031(2) 0.055(3) 0.009(2) 0.007(3) 0.003(2) C23 0.029(2) 0.038(3) 0.052(3) 0.001(2) -0.003(2) 0.0003(19) C24 0.044(3) 0.032(2) 0.054(3) 0.000(2) 0.013(2) 0.005(2) C25 0.031(2) 0.034(3) 0.086(4) -0.005(2) 0.017(3) -0.006(2) C26 0.042(3) 0.039(3) 0.060(3) 0.003(2) 0.009(2) 0.012(2) C27 0.031(2) 0.036(3) 0.104(5) -0.001(3) -0.002(3) 0.001(2) C28 0.0229(18) 0.0283(19) 0.0196(18) 0.0026(14) 0.0017(15) 0.0021(15) C29 0.0268(19) 0.0239(19) 0.029(2) 0.0039(15) -0.0019(16) 0.0022(16) C30 0.036(2) 0.0248(19) 0.028(2) -0.0001(16) 0.0042(17) 0.0032(17) C31 0.036(2) 0.030(2) 0.026(2) 0.0032(16) 0.0053(17) 0.0021(17) C32 0.034(2) 0.026(2) 0.029(2) 0.0071(16) 0.0026(17) -0.0024(17) C33 0.0276(19) 0.0258(19) 0.0231(19) -0.0003(15) -0.0010(16) -0.0014(16) C34 0.028(2) 0.0246(19) 0.0246(19) 0.0025(15) -0.0010(16) -0.0018(16) C53 0.049(3) 0.037(2) 0.035(2) 0.0047(19) 0.015(2) 0.004(2) C54 0.0246(19) 0.0258(19) 0.028(2) 0.0019(15) 0.0035(16) -0.0009(15) C55 0.0229(19) 0.028(2) 0.034(2) 0.0042(16) 0.0007(16) -0.0027(16) C56 0.030(2) 0.0239(19) 0.032(2) 0.0016(16) 0.0022(17) -0.0017(16) C57 0.029(2) 0.028(2) 0.026(2) 0.0044(15) 0.0035(16) -0.0008(16) C58 0.028(2) 0.031(2) 0.043(3) 0.0040(18) 0.0089(19) 0.0053(17) C59 0.043(3) 0.029(2) 0.034(2) -0.0013(17) 0.009(2) 0.0020(19) C60 0.038(2) 0.026(2) 0.031(2) 0.0014(16) -0.0009(18) -0.0008(18) C61 0.034(2) 0.0227(19) 0.036(2) -0.0003(16) 0.0019(18) -0.0020(17) C62 0.032(2) 0.025(2) 0.033(2) 0.0058(16) 0.0044(17) 0.0019(16) C63 0.030(2) 0.030(2) 0.042(3) 0.0079(18) 0.0014(19) 0.0040(17) C64 0.027(2) 0.0170(17) 0.038(2) 0.0016(15) -0.0057(17) -0.0035(15) C65 0.027(2) 0.025(2) 0.038(2) 0.0023(17) -0.0113(17) -0.0046(16) C66 0.038(2) 0.033(2) 0.044(3) 0.0057(19) -0.017(2) -0.0088(19) C67 0.036(2) 0.030(2) 0.050(3) -0.0010(19) -0.011(2) -0.0090(19) C68 0.031(2) 0.029(2) 0.042(2) 0.0058(18) -0.0003(19) -0.0039(18) C69 0.0213(19) 0.025(2) 0.043(2) 0.0043(17) -0.0031(17) 0.0005(15) C70 0.042(2) 0.022(2) 0.037(2) 0.0004(17) -0.009(2) -0.0052(18) C71 0.040(2) 0.027(2) 0.047(3) 0.0037(19) -0.009(2) 0.0040(19) C72 0.058(3) 0.035(2) 0.044(3) 0.003(2) -0.017(2) -0.011(2) C73 0.043(3) 0.035(2) 0.030(2) 0.0031(18) -0.0066(19) -0.0011(19) C74 0.060(3) 0.026(2) 0.049(3) 0.005(2) -0.014(2) -0.002(2) C75 0.066(4) 0.045(3) 0.061(4) 0.020(3) -0.025(3) -0.008(3) C76 0.072(4) 0.046(3) 0.043(3) 0.012(2) -0.027(3) -0.013(3) C77 0.083(4) 0.046(3) 0.027(2) 0.006(2) -0.017(3) -0.016(3) C78 0.050(3) 0.042(3) 0.030(2) 0.0071(19) -0.010(2) -0.010(2) C79 0.058(3) 0.034(2) 0.037(3) 0.0063(19) -0.009(2) -0.008(2) C80 0.058(3) 0.037(3) 0.063(4) 0.002(2) -0.014(3) -0.018(2) C81 0.0219(19) 0.029(2) 0.036(2) 0.0054(16) 0.0028(17) -0.0029(16) C82 0.046(3) 0.034(2) 0.042(3) 0.000(2) 0.008(2) -0.010(2) C83 0.050(3) 0.040(3) 0.050(3) 0.003(2) -0.001(2) 0.010(2) C84 0.032(2) 0.043(3) 0.059(3) 0.002(2) 0.000(2) 0.002(2) C85 0.047(3) 0.040(3) 0.040(3) -0.006(2) 0.012(2) -0.010(2) C86 0.025(2) 0.073(4) 0.053(3) 0.008(3) 0.006(2) -0.002(2) C87 0.046(3) 0.043(3) 0.057(3) 0.012(2) -0.002(2) 0.010(2) C88 0.049(3) 0.044(3) 0.059(3) 0.001(2) 0.019(3) -0.013(2) C89 0.028(2) 0.061(3) 0.056(3) 0.013(3) 0.011(2) 0.004(2) C90 0.046(3) 0.049(3) 0.057(3) -0.008(3) 0.000(3) 0.007(2) C91 0.029(2) 0.0231(19) 0.027(2) -0.0001(15) -0.0045(16) -0.0053(16) C92 0.030(2) 0.0251(19) 0.028(2) 0.0020(15) -0.0048(16) -0.0025(16) C93 0.031(2) 0.0232(19) 0.037(2) -0.0018(16) -0.0017(18) -0.0020(16) C94 0.035(2) 0.029(2) 0.040(2) -0.0020(18) -0.0046(19) -0.0058(18) C95 0.029(2) 0.036(2) 0.038(2) -0.0011(18) -0.0005(18) -0.0071(18) C96 0.029(2) 0.027(2) 0.031(2) 0.0028(16) -0.0032(17) 0.0013(16) C97 0.0254(19) 0.028(2) 0.031(2) 0.0000(16) -0.0009(16) -0.0030(16) C116 0.045(3) 0.039(3) 0.058(3) -0.010(2) -0.005(2) -0.017(2) C117 0.028(2) 0.031(2) 0.030(2) 0.0028(16) 0.0028(17) -0.0017(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.912(3) . ? Nb1 O2 1.915(3) . ? Nb1 Nb2 2.6674(5) . ? Nb1 H1 2.17(6) . ? Nb1 H2 1.68(5) . ? Nb1 H3 2.16(4) . ? Nb1 H4 1.55(4) . ? Nb2 O4 1.901(3) . ? Nb2 O3 1.906(3) . ? Nb2 H1 1.60(5) . ? Nb2 H3 1.60(5) . ? Nb2 H4 2.04(4) . ? O1 C1 1.380(5) . ? O2 C28 1.381(5) . ? O3 C64 1.384(5) . ? O4 C91 1.381(5) . ? C1 C2 1.415(6) . ? C1 C6 1.429(6) . ? C2 C3 1.400(6) . ? C2 C7 1.533(6) . ? C3 C4 1.387(7) . ? C3 H5 0.9500 . ? C4 C5 1.375(7) . ? C4 C17 1.504(7) . ? C5 C6 1.396(6) . ? C5 H6 0.9500 . ? C6 C18 1.537(6) . ? C7 C8 1.530(6) . ? C7 C10 1.535(6) . ? C7 C9 1.542(6) . ? C8 C11 1.547(6) . ? C8 H7 0.9900 . ? C8 H8 0.9900 . ? C9 C13 1.549(7) . ? C9 H9 0.9900 . ? C9 H10 0.9900 . ? C10 C15 1.543(7) . ? C10 H11 0.9900 . ? C10 H12 0.9900 . ? C11 C16 1.515(7) . ? C11 C12 1.517(7) . ? C11 H13 1.0000 . ? C12 C13 1.510(8) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 C14 1.498(10) . ? C13 H16 1.0000 . ? C14 C15 1.507(9) . ? C14 H17 0.9900 . ? C14 H18 0.9900 . ? C15 C16 1.522(8) . ? C15 H19 1.0000 . ? C16 H20 0.9900 . ? C16 H21 0.9900 . ? C17 H22 0.9800 . ? C17 H23 0.9800 . ? C17 H24 0.9800 . ? C18 C20 1.524(6) . ? C18 C19 1.552(6) . ? C18 C21 1.554(6) . ? C19 C22 1.542(7) . ? C19 H25 0.9900 . ? C19 H26 0.9900 . ? C20 C24 1.585(7) . ? C20 H27 0.9900 . ? C20 H28 0.9900 . ? C21 C26 1.548(8) . ? C21 H29 0.9900 . ? C21 H30 0.9900 . ? C22 C23 1.500(7) . ? C22 C27 1.518(7) . ? C22 H31 1.0000 . ? C23 C24 1.501(7) . ? C23 H32 0.9900 . ? C23 H33 0.9900 . ? C24 C25 1.495(7) . ? C24 H34 1.0000 . ? C25 C26 1.503(7) . ? C25 H35 0.9900 . ? C25 H36 0.9900 . ? C26 C27 1.510(8) . ? C26 H37 1.0000 . ? C27 H38 0.9900 . ? C27 H39 0.9900 . ? C28 C29 1.412(5) . ? C28 C33 1.419(5) . ? C29 C30 1.399(6) . ? C29 C34 1.546(5) . ? C30 C31 1.384(6) . ? C30 H40 0.9500 . ? C31 C32 1.383(6) . ? C31 C53 1.506(6) . ? C32 C33 1.389(6) . ? C32 H41 0.9500 . ? C33 C54 1.547(5) . ? C34 C46 1.489(12) . ? C34 C45 1.500(14) . ? C34 C35 1.505(8) . ? C34 C37 1.526(8) . ? C34 C36 1.587(8) . ? C34 C44 1.637(13) . ? C35 C38 1.545(10) . ? C35 H42 0.9900 . ? C35 H43 0.9900 . ? C36 C40 1.554(10) . ? C36 H44 0.9900 . ? C36 H45 0.9900 . ? C37 C42 1.547(10) . ? C37 H46 0.9900 . ? C37 H47 0.9900 . ? C38 C43 1.516(10) . ? C38 C39 1.538(10) . ? C38 H48 1.0000 . ? C39 C40 1.526(11) . ? C39 H49 0.9900 . ? C39 H50 0.9900 . ? C40 C41 1.549(11) . ? C40 H51 1.0000 . ? C41 C42 1.513(11) . ? C41 H52 0.9900 . ? C41 H53 0.9900 . ? C42 C43 1.517(10) . ? C42 H54 1.0000 . ? C43 H55 0.9900 . ? C43 H56 0.9900 . ? C44 C47 1.582(17) . ? C44 H57 0.9900 . ? C44 H58 0.9900 . ? C45 C49 1.590(19) . ? C45 H59 0.9900 . ? C45 H60 0.9900 . ? C46 C51 1.563(19) . ? C46 H61 0.9900 . ? C46 H62 0.9900 . ? C47 C52 1.494(17) . ? C47 C48 1.529(18) . ? C47 H63 1.0000 . ? C48 C49 1.50(2) . ? C48 H64 0.9900 . ? C48 H65 0.9900 . ? C49 C50 1.55(2) . ? C49 H66 1.0000 . ? C50 C51 1.45(2) . ? C50 H67 0.9900 . ? C50 H68 0.9900 . ? C51 C52 1.523(19) . ? C51 H69 1.0000 . ? C52 H70 0.9900 . ? C52 H71 0.9900 . ? C53 H72 0.9800 . ? C53 H73 0.9800 . ? C53 H74 0.9800 . ? C54 C56 1.537(6) . ? C54 C57 1.548(5) . ? C54 C55 1.552(5) . ? C55 C58 1.547(6) . ? C55 H75 0.9900 . ? C55 H76 0.9900 . ? C56 C60 1.536(6) . ? C56 H77 0.9900 . ? C56 H78 0.9900 . ? C57 C62 1.541(6) . ? C57 H79 0.9900 . ? C57 H80 0.9900 . ? C58 C59 1.519(6) . ? C58 C63 1.535(6) . ? C58 H81 1.0000 . ? C59 C60 1.540(6) . ? C59 H82 0.9900 . ? C59 H83 0.9900 . ? C60 C61 1.529(6) . ? C60 H84 1.0000 . ? C61 C62 1.530(6) . ? C61 H85 0.9900 . ? C61 H86 0.9900 . ? C62 C63 1.517(6) . ? C62 H87 1.0000 . ? C63 H88 0.9900 . ? C63 H89 0.9900 . ? C64 C65 1.409(6) . ? C64 C69 1.417(6) . ? C65 C66 1.393(6) . ? C65 C70 1.541(6) . ? C66 C67 1.381(7) . ? C66 H90 0.9500 . ? C67 C68 1.381(6) . ? C67 C80 1.517(6) . ? C68 C69 1.401(6) . ? C68 H91 0.9500 . ? C69 C81 1.552(6) . ? C70 C71 1.540(6) . ? C70 C73 1.546(7) . ? C70 C72 1.561(6) . ? C71 C74 1.537(6) . ? C71 H92 0.9900 . ? C71 H93 0.9900 . ? C72 C76 1.534(7) . ? C72 H94 0.9900 . ? C72 H95 0.9900 . ? C73 C78 1.539(6) . ? C73 H96 0.9900 . ? C73 H97 0.9900 . ? C74 C79 1.515(7) . ? C74 C75 1.542(7) . ? C74 H98 1.0000 . ? C75 C76 1.521(8) . ? C75 H99 0.9900 . ? C75 H100 0.9900 . ? C76 C77 1.524(9) . ? C76 H101 1.0000 . ? C77 C78 1.524(6) . ? C77 H102 0.9900 . ? C77 H103 0.9900 . ? C78 C79 1.530(7) . ? C78 H104 1.0000 . ? C79 H105 0.9900 . ? C79 H106 0.9900 . ? C80 H107 0.9800 . ? C80 H108 0.9800 . ? C80 H109 0.9800 . ? C81 C83 1.535(6) . ? C81 C82 1.546(6) . ? C81 C84 1.550(6) . ? C82 C85 1.533(7) . ? C82 H110 0.9900 . ? C82 H111 0.9900 . ? C83 C87 1.567(7) . ? C83 H112 0.9900 . ? C83 H113 0.9900 . ? C84 C89 1.565(8) . ? C84 H114 0.9900 . ? C84 H115 0.9900 . ? C85 C86 1.495(7) . ? C85 C90 1.531(7) . ? C85 H116 1.0000 . ? C86 C87 1.508(8) . ? C86 H117 0.9900 . ? C86 H118 0.9900 . ? C87 C88 1.508(7) . ? C87 H119 1.0000 . ? C88 C89 1.510(7) . ? C88 H120 0.9900 . ? C88 H121 0.9900 . ? C89 C90 1.499(8) . ? C89 H122 1.0000 . ? C90 H123 0.9900 . ? C90 H124 0.9900 . ? C91 C96 1.416(6) . ? C91 C92 1.417(6) . ? C92 C93 1.403(5) . ? C92 C97 1.541(6) . ? C93 C94 1.378(6) . ? C93 H125 0.9500 . ? C94 C95 1.383(6) . ? C94 C116 1.506(6) . ? C95 C96 1.394(6) . ? C95 H126 0.9500 . ? C96 C117 1.537(6) . ? C97 C108 1.479(11) . ? C97 C100 1.526(8) . ? C97 C109 1.536(11) . ? C97 C98 1.542(7) . ? C97 C107 1.569(12) . ? C97 C99 1.590(8) . ? C98 C101 1.547(11) . ? C98 H127 0.9900 . ? C98 H128 0.9900 . ? C99 C103 1.551(14) . ? C99 H129 0.9900 . ? C99 H130 0.9900 . ? C100 C105 1.540(11) . ? C100 H131 0.9900 . ? C100 H132 0.9900 . ? C101 C106 1.509(13) . ? C101 C102 1.510(12) . ? C101 H133 1.0000 . ? C102 C103 1.522(15) . ? C102 H134 0.9900 . ? C102 H135 0.9900 . ? C103 C104 1.544(15) . ? C103 H136 1.0000 . ? C104 C105 1.511(12) . ? C104 H137 0.9900 . ? C104 H138 0.9900 . ? C105 C106 1.547(13) . ? C105 H139 1.0000 . ? C106 H140 0.9900 . ? C106 H141 0.9900 . ? C107 C110 1.60(2) . ? C107 H142 0.9900 . ? C107 H143 0.9900 . ? C108 C112 1.550(19) . ? C108 H144 0.9900 . ? C108 H145 0.9900 . ? C109 C114 1.560(17) . ? C109 H146 0.9900 . ? C109 H147 0.9900 . ? C110 C115 1.47(2) . ? C110 C111 1.52(2) . ? C110 H148 1.0000 . ? C111 C112 1.52(2) . ? C111 H149 0.9900 . ? C111 H150 0.9900 . ? C112 C113 1.51(3) . ? C112 H151 1.0000 . ? C113 C114 1.48(3) . ? C113 H152 0.9900 . ? C113 H153 0.9900 . ? C114 C115 1.51(2) . ? C114 H154 1.0000 . ? C115 H155 0.9900 . ? C115 H156 0.9900 . ? C116 H157 0.9800 . ? C116 H158 0.9800 . ? C116 H159 0.9800 . ? C117 C120 1.488(10) . ? C117 C128 1.493(11) . ? C117 C119 1.555(9) . ? C117 C127 1.555(10) . ? C117 C118 1.577(9) . ? C117 C129 1.595(11) . ? C118 C121 1.528(14) . ? C118 H160 0.9900 . ? C118 H161 0.9900 . ? C119 C123 1.543(14) . ? C119 H162 0.9900 . ? C119 H163 0.9900 . ? C120 C125 1.545(13) . ? C120 H164 0.9900 . ? C120 H165 0.9900 . ? C121 C122 1.469(16) . ? C121 C126 1.523(15) . ? C121 H166 1.0000 . ? C122 C123 1.559(16) . ? C122 H167 0.9900 . ? C122 H168 0.9900 . ? C123 C124 1.525(15) . ? C123 H169 1.0000 . ? C124 C125 1.546(14) . ? C124 H170 0.9900 . ? C124 H171 0.9900 . ? C125 C126 1.524(14) . ? C125 H172 1.0000 . ? C126 H173 0.9900 . ? C126 H174 0.9900 . ? C127 C130 1.535(14) . ? C127 H175 0.9900 . ? C127 H176 0.9900 . ? C128 C132 1.574(17) . ? C128 H177 0.9900 . ? C128 H178 0.9900 . ? C129 C134 1.528(14) . ? C129 H179 0.9900 . ? C129 H180 0.9900 . ? C130 C135 1.516(15) . ? C130 C131 1.531(16) . ? C130 H181 1.0000 . ? C131 C132 1.546(18) . ? C131 H182 0.9900 . ? C131 H183 0.9900 . ? C132 C133 1.437(18) . ? C132 H184 1.0000 . ? C133 C134 1.558(16) . ? C133 H185 0.9900 . ? C133 H186 0.9900 . ? C134 C135 1.498(14) . ? C134 H187 1.0000 . ? C135 H188 0.9900 . ? C135 H189 0.9900 . ? C136 C137 1.330(15) . ? C136 C141 1.335(14) . ? C136 H190 0.9500 . ? C137 C138 1.284(15) . ? C137 H191 0.9500 . ? C138 C139 1.383(17) . ? C138 H192 0.9500 . ? C139 C140 1.371(16) . ? C139 H193 0.9500 . ? C140 C141 1.287(14) . ? C140 H194 0.9500 . ? C141 H195 0.9500 . ? C142 C143 1.627(15) . ? C142 H196 0.9800 . ? C142 H197 0.9800 . ? C142 H198 0.9800 . ? C143 C144 1.473(19) . ? C143 H199 0.9900 . ? C143 H200 0.9900 . ? C144 C145 1.30(2) . ? C144 H206 0.9900 . ? C144 H207 0.9900 . ? C145 C146 1.454(18) . ? C145 H208 0.9900 . ? C145 H209 0.9900 . ? C146 H203 0.9800 . ? C146 H204 0.9800 . ? C146 H205 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nb1 O2 117.09(12) . . ? O1 Nb1 Nb2 121.43(8) . . ? O2 Nb1 Nb2 121.44(9) . . ? O1 Nb1 H1 84.7(14) . . ? O2 Nb1 H1 158.2(14) . . ? Nb2 Nb1 H1 36.8(14) . . ? O1 Nb1 H2 107.5(18) . . ? O2 Nb1 H2 106.8(18) . . ? Nb2 Nb1 H2 57.6(18) . . ? H1 Nb1 H2 64(2) . . ? O1 Nb1 H3 158.0(12) . . ? O2 Nb1 H3 84.7(12) . . ? Nb2 Nb1 H3 36.7(12) . . ? H1 Nb1 H3 73.5(19) . . ? H2 Nb1 H3 65(2) . . ? O1 Nb1 H4 108.5(15) . . ? O2 Nb1 H4 109.2(15) . . ? Nb2 Nb1 H4 49.7(15) . . ? H1 Nb1 H4 60(2) . . ? H2 Nb1 H4 107(2) . . ? H3 Nb1 H4 58.0(19) . . ? O4 Nb2 O3 116.92(12) . . ? O4 Nb2 Nb1 120.88(9) . . ? O3 Nb2 Nb1 122.18(9) . . ? O4 Nb2 H1 111(2) . . ? O3 Nb2 H1 106(2) . . ? Nb1 Nb2 H1 54(2) . . ? O4 Nb2 H3 104.2(16) . . ? O3 Nb2 H3 110.7(16) . . ? Nb1 Nb2 H3 54.1(16) . . ? H1 Nb2 H3 109(3) . . ? O4 Nb2 H4 85.6(12) . . ? O3 Nb2 H4 157.5(12) . . ? Nb1 Nb2 H4 35.3(12) . . ? H1 Nb2 H4 63(2) . . ? H3 Nb2 H4 61(2) . . ? C1 O1 Nb1 154.6(2) . . ? C28 O2 Nb1 155.4(3) . . ? C64 O3 Nb2 157.2(3) . . ? C91 O4 Nb2 157.8(3) . . ? O1 C1 C2 120.8(4) . . ? O1 C1 C6 117.8(4) . . ? C2 C1 C6 121.4(4) . . ? C3 C2 C1 115.4(4) . . ? C3 C2 C7 116.2(4) . . ? C1 C2 C7 128.4(4) . . ? C4 C3 C2 124.1(4) . . ? C4 C3 H5 117.9 . . ? C2 C3 H5 117.9 . . ? C5 C4 C3 117.4(4) . . ? C5 C4 C17 120.8(5) . . ? C3 C4 C17 121.7(5) . . ? C4 C5 C6 123.0(4) . . ? C4 C5 H6 118.5 . . ? C6 C5 H6 118.5 . . ? C5 C6 C1 116.7(4) . . ? C5 C6 C18 118.8(4) . . ? C1 C6 C18 124.4(4) . . ? C8 C7 C2 115.8(4) . . ? C8 C7 C10 106.9(4) . . ? C2 C7 C10 111.1(4) . . ? C8 C7 C9 107.1(4) . . ? C2 C7 C9 107.8(4) . . ? C10 C7 C9 107.8(4) . . ? C7 C8 C11 111.9(4) . . ? C7 C8 H7 109.2 . . ? C11 C8 H7 109.2 . . ? C7 C8 H8 109.2 . . ? C11 C8 H8 109.2 . . ? H7 C8 H8 107.9 . . ? C7 C9 C13 111.4(4) . . ? C7 C9 H9 109.3 . . ? C13 C9 H9 109.3 . . ? C7 C9 H10 109.3 . . ? C13 C9 H10 109.3 . . ? H9 C9 H10 108.0 . . ? C7 C10 C15 110.8(4) . . ? C7 C10 H11 109.5 . . ? C15 C10 H11 109.5 . . ? C7 C10 H12 109.5 . . ? C15 C10 H12 109.5 . . ? H11 C10 H12 108.1 . . ? C16 C11 C12 109.3(4) . . ? C16 C11 C8 108.0(4) . . ? C12 C11 C8 111.1(4) . . ? C16 C11 H13 109.5 . . ? C12 C11 H13 109.5 . . ? C8 C11 H13 109.5 . . ? C13 C12 C11 108.5(4) . . ? C13 C12 H14 110.0 . . ? C11 C12 H14 110.0 . . ? C13 C12 H15 110.0 . . ? C11 C12 H15 110.0 . . ? H14 C12 H15 108.4 . . ? C14 C13 C12 111.0(5) . . ? C14 C13 C9 108.9(5) . . ? C12 C13 C9 109.7(5) . . ? C14 C13 H16 109.1 . . ? C12 C13 H16 109.1 . . ? C9 C13 H16 109.1 . . ? C13 C14 C15 109.5(4) . . ? C13 C14 H17 109.8 . . ? C15 C14 H17 109.8 . . ? C13 C14 H18 109.8 . . ? C15 C14 H18 109.8 . . ? H17 C14 H18 108.2 . . ? C14 C15 C16 109.7(5) . . ? C14 C15 C10 109.7(5) . . ? C16 C15 C10 109.6(5) . . ? C14 C15 H19 109.3 . . ? C16 C15 H19 109.3 . . ? C10 C15 H19 109.3 . . ? C11 C16 C15 109.3(4) . . ? C11 C16 H20 109.8 . . ? C15 C16 H20 109.8 . . ? C11 C16 H21 109.8 . . ? C15 C16 H21 109.8 . . ? H20 C16 H21 108.3 . . ? C4 C17 H22 109.5 . . ? C4 C17 H23 109.5 . . ? H22 C17 H23 109.5 . . ? C4 C17 H24 109.5 . . ? H22 C17 H24 109.5 . . ? H23 C17 H24 109.5 . . ? C20 C18 C6 112.5(3) . . ? C20 C18 C19 109.9(4) . . ? C6 C18 C19 110.1(3) . . ? C20 C18 C21 106.7(4) . . ? C6 C18 C21 112.1(4) . . ? C19 C18 C21 105.3(4) . . ? C22 C19 C18 111.4(4) . . ? C22 C19 H25 109.3 . . ? C18 C19 H25 109.3 . . ? C22 C19 H26 109.3 . . ? C18 C19 H26 109.3 . . ? H25 C19 H26 108.0 . . ? C18 C20 C24 110.9(4) . . ? C18 C20 H27 109.5 . . ? C24 C20 H27 109.5 . . ? C18 C20 H28 109.5 . . ? C24 C20 H28 109.5 . . ? H27 C20 H28 108.0 . . ? C26 C21 C18 113.6(4) . . ? C26 C21 H29 108.8 . . ? C18 C21 H29 108.8 . . ? C26 C21 H30 108.8 . . ? C18 C21 H30 108.8 . . ? H29 C21 H30 107.7 . . ? C23 C22 C27 110.5(4) . . ? C23 C22 C19 106.9(4) . . ? C27 C22 C19 107.8(5) . . ? C23 C22 H31 110.5 . . ? C27 C22 H31 110.5 . . ? C19 C22 H31 110.5 . . ? C22 C23 C24 113.4(4) . . ? C22 C23 H32 108.9 . . ? C24 C23 H32 108.9 . . ? C22 C23 H33 108.9 . . ? C24 C23 H33 108.9 . . ? H32 C23 H33 107.7 . . ? C25 C24 C23 111.6(4) . . ? C25 C24 C20 107.2(4) . . ? C23 C24 C20 105.8(4) . . ? C25 C24 H34 110.7 . . ? C23 C24 H34 110.7 . . ? C20 C24 H34 110.7 . . ? C24 C25 C26 112.6(4) . . ? C24 C25 H35 109.1 . . ? C26 C25 H35 109.1 . . ? C24 C25 H36 109.1 . . ? C26 C25 H36 109.1 . . ? H35 C25 H36 107.8 . . ? C25 C26 C27 111.0(5) . . ? C25 C26 C21 106.5(4) . . ? C27 C26 C21 106.3(5) . . ? C25 C26 H37 110.9 . . ? C27 C26 H37 110.9 . . ? C21 C26 H37 110.9 . . ? C26 C27 C22 111.8(4) . . ? C26 C27 H38 109.3 . . ? C22 C27 H38 109.3 . . ? C26 C27 H39 109.3 . . ? C22 C27 H39 109.3 . . ? H38 C27 H39 107.9 . . ? O2 C28 C29 120.4(3) . . ? O2 C28 C33 118.3(3) . . ? C29 C28 C33 121.3(4) . . ? C30 C29 C28 115.7(4) . . ? C30 C29 C34 117.5(4) . . ? C28 C29 C34 126.7(4) . . ? C31 C30 C29 124.0(4) . . ? C31 C30 H40 118.0 . . ? C29 C30 H40 118.0 . . ? C32 C31 C30 117.2(4) . . ? C32 C31 C53 122.0(4) . . ? C30 C31 C53 120.8(4) . . ? C31 C32 C33 122.7(4) . . ? C31 C32 H41 118.6 . . ? C33 C32 H41 118.6 . . ? C32 C33 C28 117.2(4) . . ? C32 C33 C54 119.5(3) . . ? C28 C33 C54 123.2(3) . . ? C46 C34 C45 114.8(8) . . ? C46 C34 C35 136.6(6) . . ? C45 C34 C35 65.1(6) . . ? C45 C34 C37 138.3(7) . . ? C35 C34 C37 111.5(5) . . ? C46 C34 C29 111.2(5) . . ? C45 C34 C29 106.6(6) . . ? C35 C34 C29 109.7(4) . . ? C37 C34 C29 112.8(4) . . ? C46 C34 C36 70.8(6) . . ? C45 C34 C36 46.4(6) . . ? C35 C34 C36 106.8(4) . . ? C37 C34 C36 104.6(4) . . ? C29 C34 C36 111.2(4) . . ? C46 C34 C44 105.7(7) . . ? C45 C34 C44 104.6(7) . . ? C37 C34 C44 71.5(5) . . ? C29 C34 C44 113.8(5) . . ? C36 C34 C44 132.3(6) . . ? C34 C35 C38 111.6(5) . . ? C34 C35 H42 109.3 . . ? C38 C35 H42 109.3 . . ? C34 C35 H43 109.3 . . ? C38 C35 H43 109.3 . . ? H42 C35 H43 108.0 . . ? C40 C36 C34 112.0(5) . . ? C40 C36 H44 109.2 . . ? C34 C36 H44 109.2 . . ? C40 C36 H45 109.2 . . ? C34 C36 H45 109.2 . . ? H44 C36 H45 107.9 . . ? C34 C37 C42 111.0(5) . . ? C34 C37 H46 109.4 . . ? C42 C37 H46 109.4 . . ? C34 C37 H47 109.4 . . ? C42 C37 H47 109.4 . . ? H46 C37 H47 108.0 . . ? C43 C38 C39 109.9(6) . . ? C43 C38 C35 109.1(6) . . ? C39 C38 C35 109.2(6) . . ? C43 C38 H48 109.5 . . ? C39 C38 H48 109.5 . . ? C35 C38 H48 109.5 . . ? C40 C39 C38 109.4(6) . . ? C40 C39 H49 109.8 . . ? C38 C39 H49 109.8 . . ? C40 C39 H50 109.8 . . ? C38 C39 H50 109.8 . . ? H49 C39 H50 108.2 . . ? C39 C40 C41 109.2(6) . . ? C39 C40 C36 110.2(7) . . ? C41 C40 C36 106.4(6) . . ? C39 C40 H51 110.3 . . ? C41 C40 H51 110.3 . . ? C36 C40 H51 110.3 . . ? C42 C41 C40 110.0(7) . . ? C42 C41 H52 109.7 . . ? C40 C41 H52 109.7 . . ? C42 C41 H53 109.7 . . ? C40 C41 H53 109.7 . . ? H52 C41 H53 108.2 . . ? C41 C42 C43 110.1(6) . . ? C41 C42 C37 110.1(7) . . ? C43 C42 C37 108.4(6) . . ? C41 C42 H54 109.4 . . ? C43 C42 H54 109.4 . . ? C37 C42 H54 109.4 . . ? C38 C43 C42 110.5(6) . . ? C38 C43 H55 109.5 . . ? C42 C43 H55 109.5 . . ? C38 C43 H56 109.5 . . ? C42 C43 H56 109.5 . . ? H55 C43 H56 108.1 . . ? C47 C44 C34 109.6(8) . . ? C47 C44 H57 109.7 . . ? C34 C44 H57 109.7 . . ? C47 C44 H58 109.7 . . ? C34 C44 H58 109.7 . . ? H57 C44 H58 108.2 . . ? C34 C45 C49 111.6(10) . . ? C34 C45 H59 109.3 . . ? C49 C45 H59 109.3 . . ? C34 C45 H60 109.3 . . ? C49 C45 H60 109.3 . . ? H59 C45 H60 108.0 . . ? C34 C46 C51 111.1(9) . . ? C34 C46 H61 109.4 . . ? C51 C46 H61 109.4 . . ? C34 C46 H62 109.4 . . ? C51 C46 H62 109.4 . . ? H61 C46 H62 108.0 . . ? C52 C47 C48 109.8(10) . . ? C52 C47 C44 105.4(10) . . ? C48 C47 C44 108.8(11) . . ? C52 C47 H63 110.9 . . ? C48 C47 H63 110.9 . . ? C44 C47 H63 110.9 . . ? C49 C48 C47 111.3(12) . . ? C49 C48 H64 109.4 . . ? C47 C48 H64 109.4 . . ? C49 C48 H65 109.4 . . ? C47 C48 H65 109.4 . . ? H64 C48 H65 108.0 . . ? C48 C49 C50 112.5(12) . . ? C48 C49 C45 105.2(11) . . ? C50 C49 C45 105.6(12) . . ? C48 C49 H66 111.1 . . ? C50 C49 H66 111.1 . . ? C45 C49 H66 111.1 . . ? C51 C50 C49 114.0(12) . . ? C51 C50 H67 108.8 . . ? C49 C50 H67 108.8 . . ? C51 C50 H68 108.8 . . ? C49 C50 H68 108.8 . . ? H67 C50 H68 107.6 . . ? C50 C51 C52 109.3(12) . . ? C50 C51 C46 106.7(12) . . ? C52 C51 C46 108.2(12) . . ? C50 C51 H69 110.9 . . ? C52 C51 H69 110.9 . . ? C46 C51 H69 110.9 . . ? C47 C52 C51 114.6(11) . . ? C47 C52 H70 108.6 . . ? C51 C52 H70 108.6 . . ? C47 C52 H71 108.6 . . ? C51 C52 H71 108.6 . . ? H70 C52 H71 107.6 . . ? C31 C53 H72 109.5 . . ? C31 C53 H73 109.5 . . ? H72 C53 H73 109.5 . . ? C31 C53 H74 109.5 . . ? H72 C53 H74 109.5 . . ? H73 C53 H74 109.5 . . ? C56 C54 C33 114.0(3) . . ? C56 C54 C57 106.4(3) . . ? C33 C54 C57 111.0(3) . . ? C56 C54 C55 109.4(3) . . ? C33 C54 C55 109.5(3) . . ? C57 C54 C55 106.3(3) . . ? C58 C55 C54 111.3(3) . . ? C58 C55 H75 109.4 . . ? C54 C55 H75 109.4 . . ? C58 C55 H76 109.4 . . ? C54 C55 H76 109.4 . . ? H75 C55 H76 108.0 . . ? C60 C56 C54 111.7(3) . . ? C60 C56 H77 109.3 . . ? C54 C56 H77 109.3 . . ? C60 C56 H78 109.3 . . ? C54 C56 H78 109.3 . . ? H77 C56 H78 107.9 . . ? C62 C57 C54 112.1(3) . . ? C62 C57 H79 109.2 . . ? C54 C57 H79 109.2 . . ? C62 C57 H80 109.2 . . ? C54 C57 H80 109.2 . . ? H79 C57 H80 107.9 . . ? C59 C58 C63 109.7(4) . . ? C59 C58 C55 109.7(3) . . ? C63 C58 C55 108.5(4) . . ? C59 C58 H81 109.6 . . ? C63 C58 H81 109.6 . . ? C55 C58 H81 109.6 . . ? C58 C59 C60 110.1(4) . . ? C58 C59 H82 109.6 . . ? C60 C59 H82 109.6 . . ? C58 C59 H83 109.6 . . ? C60 C59 H83 109.6 . . ? H82 C59 H83 108.2 . . ? C61 C60 C56 109.9(3) . . ? C61 C60 C59 109.2(4) . . ? C56 C60 C59 108.9(3) . . ? C61 C60 H84 109.6 . . ? C56 C60 H84 109.6 . . ? C59 C60 H84 109.6 . . ? C60 C61 C62 109.2(3) . . ? C60 C61 H85 109.8 . . ? C62 C61 H85 109.8 . . ? C60 C61 H86 109.8 . . ? C62 C61 H86 109.8 . . ? H85 C61 H86 108.3 . . ? C63 C62 C61 109.8(4) . . ? C63 C62 C57 110.0(3) . . ? C61 C62 C57 108.7(3) . . ? C63 C62 H87 109.4 . . ? C61 C62 H87 109.4 . . ? C57 C62 H87 109.4 . . ? C62 C63 C58 109.5(3) . . ? C62 C63 H88 109.8 . . ? C58 C63 H88 109.8 . . ? C62 C63 H89 109.8 . . ? C58 C63 H89 109.8 . . ? H88 C63 H89 108.2 . . ? O3 C64 C65 117.8(4) . . ? O3 C64 C69 120.3(4) . . ? C65 C64 C69 121.9(4) . . ? C66 C65 C64 116.8(4) . . ? C66 C65 C70 119.4(4) . . ? C64 C65 C70 123.6(3) . . ? C67 C66 C65 123.0(4) . . ? C67 C66 H90 118.5 . . ? C65 C66 H90 118.5 . . ? C66 C67 C68 117.8(4) . . ? C66 C67 C80 120.9(4) . . ? C68 C67 C80 121.4(4) . . ? C67 C68 C69 123.3(4) . . ? C67 C68 H91 118.3 . . ? C69 C68 H91 118.3 . . ? C68 C69 C64 115.9(4) . . ? C68 C69 C81 116.0(4) . . ? C64 C69 C81 127.9(4) . . ? C71 C70 C65 109.2(4) . . ? C71 C70 C73 109.2(4) . . ? C65 C70 C73 114.9(4) . . ? C71 C70 C72 106.3(4) . . ? C65 C70 C72 111.5(4) . . ? C73 C70 C72 105.3(4) . . ? C74 C71 C70 111.8(4) . . ? C74 C71 H92 109.3 . . ? C70 C71 H92 109.3 . . ? C74 C71 H93 109.3 . . ? C70 C71 H93 109.3 . . ? H92 C71 H93 107.9 . . ? C76 C72 C70 112.0(4) . . ? C76 C72 H94 109.2 . . ? C70 C72 H94 109.2 . . ? C76 C72 H95 109.2 . . ? C70 C72 H95 109.2 . . ? H94 C72 H95 107.9 . . ? C78 C73 C70 112.1(4) . . ? C78 C73 H96 109.2 . . ? C70 C73 H96 109.2 . . ? C78 C73 H97 109.2 . . ? C70 C73 H97 109.2 . . ? H96 C73 H97 107.9 . . ? C79 C74 C71 109.5(4) . . ? C79 C74 C75 109.2(5) . . ? C71 C74 C75 109.0(4) . . ? C79 C74 H98 109.7 . . ? C71 C74 H98 109.7 . . ? C75 C74 H98 109.7 . . ? C76 C75 C74 109.1(4) . . ? C76 C75 H99 109.9 . . ? C74 C75 H99 109.9 . . ? C76 C75 H100 109.9 . . ? C74 C75 H100 109.9 . . ? H99 C75 H100 108.3 . . ? C75 C76 C77 110.5(5) . . ? C75 C76 C72 109.4(5) . . ? C77 C76 C72 109.5(4) . . ? C75 C76 H101 109.2 . . ? C77 C76 H101 109.2 . . ? C72 C76 H101 109.2 . . ? C76 C77 C78 109.0(4) . . ? C76 C77 H102 109.9 . . ? C78 C77 H102 109.9 . . ? C76 C77 H103 109.9 . . ? C78 C77 H103 109.9 . . ? H102 C77 H103 108.3 . . ? C77 C78 C79 109.8(4) . . ? C77 C78 C73 109.0(4) . . ? C79 C78 C73 108.7(4) . . ? C77 C78 H104 109.8 . . ? C79 C78 H104 109.8 . . ? C73 C78 H104 109.8 . . ? C74 C79 C78 110.8(4) . . ? C74 C79 H105 109.5 . . ? C78 C79 H105 109.5 . . ? C74 C79 H106 109.5 . . ? C78 C79 H106 109.5 . . ? H105 C79 H106 108.1 . . ? C67 C80 H107 109.5 . . ? C67 C80 H108 109.5 . . ? H107 C80 H108 109.5 . . ? C67 C80 H109 109.5 . . ? H107 C80 H109 109.5 . . ? H108 C80 H109 109.5 . . ? C83 C81 C82 106.9(4) . . ? C83 C81 C84 108.7(4) . . ? C82 C81 C84 104.9(4) . . ? C83 C81 C69 111.2(4) . . ? C82 C81 C69 116.1(3) . . ? C84 C81 C69 108.6(4) . . ? C85 C82 C81 113.3(4) . . ? C85 C82 H110 108.9 . . ? C81 C82 H110 108.9 . . ? C85 C82 H111 108.9 . . ? C81 C82 H111 108.9 . . ? H110 C82 H111 107.7 . . ? C81 C83 C87 111.0(4) . . ? C81 C83 H112 109.4 . . ? C87 C83 H112 109.4 . . ? C81 C83 H113 109.4 . . ? C87 C83 H113 109.4 . . ? H112 C83 H113 108.0 . . ? C81 C84 C89 112.5(4) . . ? C81 C84 H114 109.1 . . ? C89 C84 H114 109.1 . . ? C81 C84 H115 109.1 . . ? C89 C84 H115 109.1 . . ? H114 C84 H115 107.8 . . ? C86 C85 C90 110.5(4) . . ? C86 C85 C82 107.6(4) . . ? C90 C85 C82 108.6(4) . . ? C86 C85 H116 110.1 . . ? C90 C85 H116 110.1 . . ? C82 C85 H116 110.1 . . ? C85 C86 C87 112.1(4) . . ? C85 C86 H117 109.2 . . ? C87 C86 H117 109.2 . . ? C85 C86 H118 109.2 . . ? C87 C86 H118 109.2 . . ? H117 C86 H118 107.9 . . ? C88 C87 C86 110.1(5) . . ? C88 C87 C83 108.6(5) . . ? C86 C87 C83 107.1(4) . . ? C88 C87 H119 110.3 . . ? C86 C87 H119 110.3 . . ? C83 C87 H119 110.3 . . ? C87 C88 C89 111.9(4) . . ? C87 C88 H120 109.2 . . ? C89 C88 H120 109.2 . . ? C87 C88 H121 109.2 . . ? C89 C88 H121 109.2 . . ? H120 C88 H121 107.9 . . ? C90 C89 C88 111.6(5) . . ? C90 C89 C84 108.6(4) . . ? C88 C89 C84 106.3(5) . . ? C90 C89 H122 110.1 . . ? C88 C89 H122 110.1 . . ? C84 C89 H122 110.1 . . ? C89 C90 C85 109.7(4) . . ? C89 C90 H123 109.7 . . ? C85 C90 H123 109.7 . . ? C89 C90 H124 109.7 . . ? C85 C90 H124 109.7 . . ? H123 C90 H124 108.2 . . ? O4 C91 C96 120.6(4) . . ? O4 C91 C92 118.3(4) . . ? C96 C91 C92 121.1(4) . . ? C93 C92 C91 116.7(4) . . ? C93 C92 C97 117.8(4) . . ? C91 C92 C97 125.3(3) . . ? C94 C93 C92 123.3(4) . . ? C94 C93 H125 118.4 . . ? C92 C93 H125 118.4 . . ? C93 C94 C95 117.3(4) . . ? C93 C94 C116 121.2(4) . . ? C95 C94 C116 121.4(4) . . ? C94 C95 C96 123.5(4) . . ? C94 C95 H126 118.3 . . ? C96 C95 H126 118.3 . . ? C95 C96 C91 116.8(4) . . ? C95 C96 C117 117.0(4) . . ? C91 C96 C117 126.0(4) . . ? C108 C97 C100 138.7(6) . . ? C108 C97 C109 113.2(7) . . ? C100 C97 C109 53.4(5) . . ? C108 C97 C92 106.2(5) . . ? C100 C97 C92 115.1(4) . . ? C109 C97 C92 107.9(5) . . ? C108 C97 C98 52.6(5) . . ? C100 C97 C98 110.8(4) . . ? C109 C97 C98 142.5(6) . . ? C92 C97 C98 109.5(4) . . ? C108 C97 C107 108.3(7) . . ? C100 C97 C107 54.7(5) . . ? C109 C97 C107 106.1(6) . . ? C92 C97 C107 115.3(5) . . ? C98 C97 C107 59.4(5) . . ? C108 C97 C99 56.6(5) . . ? C100 C97 C99 104.8(4) . . ? C109 C97 C99 57.9(5) . . ? C92 C97 C99 111.3(4) . . ? C98 C97 C99 104.8(4) . . ? C107 C97 C99 133.3(5) . . ? C97 C98 C101 112.0(5) . . ? C97 C98 H127 109.2 . . ? C101 C98 H127 109.2 . . ? C97 C98 H128 109.2 . . ? C101 C98 H128 109.2 . . ? H127 C98 H128 107.9 . . ? C103 C99 C97 113.5(6) . . ? C103 C99 H129 108.9 . . ? C97 C99 H129 108.9 . . ? C103 C99 H130 108.9 . . ? C97 C99 H130 108.9 . . ? H129 C99 H130 107.7 . . ? C97 C100 C105 112.0(5) . . ? C97 C100 H131 109.2 . . ? C105 C100 H131 109.2 . . ? C97 C100 H132 109.2 . . ? C105 C100 H132 109.2 . . ? H131 C100 H132 107.9 . . ? C106 C101 C102 109.7(8) . . ? C106 C101 C98 108.0(8) . . ? C102 C101 C98 109.0(7) . . ? C106 C101 H133 110.0 . . ? C102 C101 H133 110.0 . . ? C98 C101 H133 110.0 . . ? C101 C102 C103 112.1(8) . . ? C101 C102 H134 109.2 . . ? C103 C102 H134 109.2 . . ? C101 C102 H135 109.2 . . ? C103 C102 H135 109.2 . . ? H134 C102 H135 107.9 . . ? C102 C103 C104 109.3(9) . . ? C102 C103 C99 108.2(9) . . ? C104 C103 C99 106.1(9) . . ? C102 C103 H136 111.0 . . ? C104 C103 H136 111.0 . . ? C99 C103 H136 111.0 . . ? C105 C104 C103 110.7(8) . . ? C105 C104 H137 109.5 . . ? C103 C104 H137 109.5 . . ? C105 C104 H138 109.5 . . ? C103 C104 H138 109.5 . . ? H137 C104 H138 108.1 . . ? C104 C105 C100 109.2(7) . . ? C104 C105 C106 110.6(7) . . ? C100 C105 C106 107.6(8) . . ? C104 C105 H139 109.8 . . ? C100 C105 H139 109.8 . . ? C106 C105 H139 109.8 . . ? C101 C106 C105 111.2(8) . . ? C101 C106 H140 109.4 . . ? C105 C106 H140 109.4 . . ? C101 C106 H141 109.4 . . ? C105 C106 H141 109.4 . . ? H140 C106 H141 108.0 . . ? C97 C107 C110 109.1(9) . . ? C97 C107 H142 109.9 . . ? C110 C107 H142 109.9 . . ? C97 C107 H143 109.9 . . ? C110 C107 H143 109.9 . . ? H142 C107 H143 108.3 . . ? C97 C108 C112 111.8(9) . . ? C97 C108 H144 109.3 . . ? C112 C108 H144 109.3 . . ? C97 C108 H145 109.3 . . ? C112 C108 H145 109.3 . . ? H144 C108 H145 107.9 . . ? C97 C109 C114 108.7(8) . . ? C97 C109 H146 110.0 . . ? C114 C109 H146 110.0 . . ? C97 C109 H147 110.0 . . ? C114 C109 H147 110.0 . . ? H146 C109 H147 108.3 . . ? C115 C110 C111 110.9(13) . . ? C115 C110 C107 108.1(14) . . ? C111 C110 C107 106.7(13) . . ? C115 C110 H148 110.3 . . ? C111 C110 H148 110.3 . . ? C107 C110 H148 110.3 . . ? C112 C111 C110 111.6(13) . . ? C112 C111 H149 109.3 . . ? C110 C111 H149 109.3 . . ? C112 C111 H150 109.3 . . ? C110 C111 H150 109.3 . . ? H149 C111 H150 108.0 . . ? C113 C112 C111 107.6(14) . . ? C113 C112 C108 107.9(14) . . ? C111 C112 C108 107.3(12) . . ? C113 C112 H151 111.3 . . ? C111 C112 H151 111.3 . . ? C108 C112 H151 111.3 . . ? C114 C113 C112 114.2(16) . . ? C114 C113 H152 108.7 . . ? C112 C113 H152 108.7 . . ? C114 C113 H153 108.7 . . ? C112 C113 H153 108.7 . . ? H152 C113 H153 107.6 . . ? C113 C114 C115 108.5(14) . . ? C113 C114 C109 108.9(13) . . ? C115 C114 C109 109.2(11) . . ? C113 C114 H154 110.1 . . ? C115 C114 H154 110.1 . . ? C109 C114 H154 110.1 . . ? C110 C115 C114 111.9(13) . . ? C110 C115 H155 109.2 . . ? C114 C115 H155 109.2 . . ? C110 C115 H156 109.2 . . ? C114 C115 H156 109.2 . . ? H155 C115 H156 107.9 . . ? C94 C116 H157 109.5 . . ? C94 C116 H158 109.5 . . ? H157 C116 H158 109.5 . . ? C94 C116 H159 109.5 . . ? H157 C116 H159 109.5 . . ? H158 C116 H159 109.5 . . ? C120 C117 C128 134.4(6) . . ? C120 C117 C96 107.8(5) . . ? C128 C117 C96 115.4(5) . . ? C120 C117 C119 112.4(5) . . ? C96 C117 C119 108.8(4) . . ? C120 C117 C127 66.9(5) . . ? C128 C117 C127 109.8(6) . . ? C96 C117 C127 108.7(5) . . ? C119 C117 C127 140.3(6) . . ? C120 C117 C118 107.6(5) . . ? C128 C117 C118 66.2(5) . . ? C96 C117 C118 115.5(4) . . ? C119 C117 C118 104.7(5) . . ? C127 C117 C118 46.0(5) . . ? C128 C117 C129 106.2(6) . . ? C96 C117 C129 112.8(5) . . ? C119 C117 C129 73.4(5) . . ? C127 C117 C129 103.2(6) . . ? C118 C117 C129 129.0(5) . . ? C121 C118 C117 111.1(7) . . ? C121 C118 H160 109.4 . . ? C117 C118 H160 109.4 . . ? C121 C118 H161 109.4 . . ? C117 C118 H161 109.4 . . ? H160 C118 H161 108.0 . . ? C123 C119 C117 109.3(7) . . ? C123 C119 H162 109.8 . . ? C117 C119 H162 109.8 . . ? C123 C119 H163 109.8 . . ? C117 C119 H163 109.8 . . ? H162 C119 H163 108.3 . . ? C117 C120 C125 113.0(7) . . ? C117 C120 H164 109.0 . . ? C125 C120 H164 109.0 . . ? C117 C120 H165 109.0 . . ? C125 C120 H165 109.0 . . ? H164 C120 H165 107.8 . . ? C122 C121 C126 110.3(10) . . ? C122 C121 C118 106.1(9) . . ? C126 C121 C118 111.6(10) . . ? C122 C121 H166 109.6 . . ? C126 C121 H166 109.6 . . ? C118 C121 H166 109.6 . . ? C121 C122 C123 111.8(10) . . ? C121 C122 H167 109.3 . . ? C123 C122 H167 109.3 . . ? C121 C122 H168 109.3 . . ? C123 C122 H168 109.3 . . ? H167 C122 H168 107.9 . . ? C124 C123 C119 109.1(9) . . ? C124 C123 C122 108.2(9) . . ? C119 C123 C122 108.1(9) . . ? C124 C123 H169 110.5 . . ? C119 C123 H169 110.5 . . ? C122 C123 H169 110.5 . . ? C123 C124 C125 112.1(9) . . ? C123 C124 H170 109.2 . . ? C125 C124 H170 109.2 . . ? C123 C124 H171 109.2 . . ? C125 C124 H171 109.2 . . ? H170 C124 H171 107.9 . . ? C126 C125 C120 108.4(8) . . ? C126 C125 C124 107.8(8) . . ? C120 C125 C124 107.8(8) . . ? C126 C125 H172 110.9 . . ? C120 C125 H172 110.9 . . ? C124 C125 H172 110.9 . . ? C121 C126 C125 110.5(9) . . ? C121 C126 H173 109.5 . . ? C125 C126 H173 109.5 . . ? C121 C126 H174 109.5 . . ? C125 C126 H174 109.5 . . ? H173 C126 H174 108.1 . . ? C130 C127 C117 112.3(7) . . ? C130 C127 H175 109.2 . . ? C117 C127 H175 109.2 . . ? C130 C127 H176 109.2 . . ? C117 C127 H176 109.2 . . ? H175 C127 H176 107.9 . . ? C117 C128 C132 113.9(8) . . ? C117 C128 H177 108.8 . . ? C132 C128 H177 108.8 . . ? C117 C128 H178 108.8 . . ? C132 C128 H178 108.8 . . ? H177 C128 H178 107.7 . . ? C134 C129 C117 112.9(7) . . ? C134 C129 H179 109.0 . . ? C117 C129 H179 109.0 . . ? C134 C129 H180 109.0 . . ? C117 C129 H180 109.0 . . ? H179 C129 H180 107.8 . . ? C135 C130 C131 107.9(9) . . ? C135 C130 C127 109.7(8) . . ? C131 C130 C127 107.2(9) . . ? C135 C130 H181 110.6 . . ? C131 C130 H181 110.6 . . ? C127 C130 H181 110.6 . . ? C130 C131 C132 112.4(10) . . ? C130 C131 H182 109.1 . . ? C132 C131 H182 109.1 . . ? C130 C131 H183 109.1 . . ? C132 C131 H183 109.1 . . ? H182 C131 H183 107.9 . . ? C133 C132 C131 110.6(11) . . ? C133 C132 C128 111.2(12) . . ? C131 C132 C128 102.9(10) . . ? C133 C132 H184 110.6 . . ? C131 C132 H184 110.6 . . ? C128 C132 H184 110.6 . . ? C132 C133 C134 111.5(10) . . ? C132 C133 H185 109.3 . . ? C134 C133 H185 109.3 . . ? C132 C133 H186 109.3 . . ? C134 C133 H186 109.3 . . ? H185 C133 H186 108.0 . . ? C135 C134 C129 109.5(10) . . ? C135 C134 C133 107.9(9) . . ? C129 C134 C133 108.5(9) . . ? C135 C134 H187 110.3 . . ? C129 C134 H187 110.3 . . ? C133 C134 H187 110.3 . . ? C134 C135 C130 111.7(9) . . ? C134 C135 H188 109.3 . . ? C130 C135 H188 109.3 . . ? C134 C135 H189 109.3 . . ? C130 C135 H189 109.3 . . ? H188 C135 H189 107.9 . . ? C137 C136 C141 121.1(13) . . ? C137 C136 H190 119.4 . . ? C141 C136 H190 119.4 . . ? C138 C137 C136 116.4(14) . . ? C138 C137 H191 121.8 . . ? C136 C137 H191 121.8 . . ? C137 C138 C139 123.2(15) . . ? C137 C138 H192 118.4 . . ? C139 C138 H192 118.4 . . ? C140 C139 C138 118.4(16) . . ? C140 C139 H193 120.8 . . ? C138 C139 H193 120.8 . . ? C141 C140 C139 116.0(15) . . ? C141 C140 H194 122.0 . . ? C139 C140 H194 122.0 . . ? C140 C141 C136 123.9(14) . . ? C140 C141 H195 118.1 . . ? C136 C141 H195 118.1 . . ? C143 C142 H196 109.5 . . ? C143 C142 H197 109.5 . . ? H196 C142 H197 109.5 . . ? C143 C142 H198 109.5 . . ? H196 C142 H198 109.5 . . ? H197 C142 H198 109.5 . . ? C144 C143 C142 129.5(13) . . ? C144 C143 H199 104.9 . . ? C142 C143 H199 104.9 . . ? C144 C143 H200 104.9 . . ? C142 C143 H200 104.9 . . ? H199 C143 H200 105.8 . . ? C145 C144 C143 126.8(19) . . ? C145 C144 H206 105.6 . . ? C143 C144 H206 105.6 . . ? C145 C144 H207 105.6 . . ? C143 C144 H207 105.6 . . ? H206 C144 H207 106.1 . . ? C144 C145 C146 123.8(18) . . ? C144 C145 H208 106.4 . . ? C146 C145 H208 106.4 . . ? C144 C145 H209 106.4 . . ? C146 C145 H209 106.4 . . ? H208 C145 H209 106.5 . . ? C145 C146 H203 109.5 . . ? C145 C146 H204 109.5 . . ? H203 C146 H204 109.5 . . ? C145 C146 H205 109.5 . . ? H203 C146 H205 109.5 . . ? H204 C146 H205 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Nb1 Nb2 O4 -91.56(14) . . . . ? O2 Nb1 Nb2 O4 85.96(14) . . . . ? O1 Nb1 Nb2 O3 89.73(14) . . . . ? O2 Nb1 Nb2 O3 -92.75(14) . . . . ? O2 Nb1 O1 C1 -148.5(6) . . . . ? Nb2 Nb1 O1 C1 29.1(6) . . . . ? O1 Nb1 O2 C28 -143.8(6) . . . . ? Nb2 Nb1 O2 C28 38.6(6) . . . . ? O4 Nb2 O3 C64 149.3(7) . . . . ? Nb1 Nb2 O3 C64 -32.0(7) . . . . ? O3 Nb2 O4 C91 140.4(7) . . . . ? Nb1 Nb2 O4 C91 -38.4(8) . . . . ? Nb1 O1 C1 C2 -82.1(7) . . . . ? Nb1 O1 C1 C6 97.1(6) . . . . ? O1 C1 C2 C3 163.5(4) . . . . ? C6 C1 C2 C3 -15.6(6) . . . . ? O1 C1 C2 C7 -20.3(6) . . . . ? C6 C1 C2 C7 160.6(4) . . . . ? C1 C2 C3 C4 7.5(7) . . . . ? C7 C2 C3 C4 -169.2(5) . . . . ? C2 C3 C4 C5 3.8(8) . . . . ? C2 C3 C4 C17 -178.3(5) . . . . ? C3 C4 C5 C6 -7.7(7) . . . . ? C17 C4 C5 C6 174.5(5) . . . . ? C4 C5 C6 C1 -0.2(7) . . . . ? C4 C5 C6 C18 177.8(4) . . . . ? O1 C1 C6 C5 -166.8(4) . . . . ? C2 C1 C6 C5 12.4(6) . . . . ? O1 C1 C6 C18 15.4(6) . . . . ? C2 C1 C6 C18 -165.5(4) . . . . ? C3 C2 C7 C8 166.7(4) . . . . ? C1 C2 C7 C8 -9.4(7) . . . . ? C3 C2 C7 C10 -71.1(5) . . . . ? C1 C2 C7 C10 112.8(5) . . . . ? C3 C2 C7 C9 46.9(6) . . . . ? C1 C2 C7 C9 -129.3(5) . . . . ? C2 C7 C8 C11 -176.2(4) . . . . ? C10 C7 C8 C11 59.4(5) . . . . ? C9 C7 C8 C11 -56.0(5) . . . . ? C8 C7 C9 C13 57.8(6) . . . . ? C2 C7 C9 C13 -177.0(5) . . . . ? C10 C7 C9 C13 -56.9(6) . . . . ? C8 C7 C10 C15 -58.2(5) . . . . ? C2 C7 C10 C15 174.6(4) . . . . ? C9 C7 C10 C15 56.7(5) . . . . ? C7 C8 C11 C16 -61.4(6) . . . . ? C7 C8 C11 C12 58.4(6) . . . . ? C16 C11 C12 C13 60.3(6) . . . . ? C8 C11 C12 C13 -58.9(6) . . . . ? C11 C12 C13 C14 -60.2(6) . . . . ? C11 C12 C13 C9 60.2(6) . . . . ? C7 C9 C13 C14 59.9(6) . . . . ? C7 C9 C13 C12 -61.7(7) . . . . ? C12 C13 C14 C15 59.6(6) . . . . ? C9 C13 C14 C15 -61.2(6) . . . . ? C13 C14 C15 C16 -58.6(6) . . . . ? C13 C14 C15 C10 61.8(6) . . . . ? C7 C10 C15 C14 -60.1(6) . . . . ? C7 C10 C15 C16 60.4(6) . . . . ? C12 C11 C16 C15 -60.5(5) . . . . ? C8 C11 C16 C15 60.5(6) . . . . ? C14 C15 C16 C11 59.6(6) . . . . ? C10 C15 C16 C11 -60.9(6) . . . . ? C5 C6 C18 C20 110.2(4) . . . . ? C1 C6 C18 C20 -72.0(5) . . . . ? C5 C6 C18 C19 -126.8(4) . . . . ? C1 C6 C18 C19 51.0(5) . . . . ? C5 C6 C18 C21 -10.0(5) . . . . ? C1 C6 C18 C21 167.8(4) . . . . ? C20 C18 C19 C22 -56.0(5) . . . . ? C6 C18 C19 C22 179.5(4) . . . . ? C21 C18 C19 C22 58.5(5) . . . . ? C6 C18 C20 C24 179.2(4) . . . . ? C19 C18 C20 C24 56.1(5) . . . . ? C21 C18 C20 C24 -57.5(5) . . . . ? C20 C18 C21 C26 57.9(5) . . . . ? C6 C18 C21 C26 -178.5(4) . . . . ? C19 C18 C21 C26 -58.9(5) . . . . ? C18 C19 C22 C23 57.5(5) . . . . ? C18 C19 C22 C27 -61.4(5) . . . . ? C27 C22 C23 C24 53.2(6) . . . . ? C19 C22 C23 C24 -63.9(5) . . . . ? C22 C23 C24 C25 -52.6(6) . . . . ? C22 C23 C24 C20 63.7(5) . . . . ? C18 C20 C24 C25 60.8(5) . . . . ? C18 C20 C24 C23 -58.4(5) . . . . ? C23 C24 C25 C26 52.7(7) . . . . ? C20 C24 C25 C26 -62.7(6) . . . . ? C24 C25 C26 C27 -54.2(7) . . . . ? C24 C25 C26 C21 61.1(6) . . . . ? C18 C21 C26 C25 -58.4(5) . . . . ? C18 C21 C26 C27 60.1(5) . . . . ? C25 C26 C27 C22 54.9(6) . . . . ? C21 C26 C27 C22 -60.5(6) . . . . ? C23 C22 C27 C26 -54.2(6) . . . . ? C19 C22 C27 C26 62.4(6) . . . . ? Nb1 O2 C28 C29 -91.1(7) . . . . ? Nb1 O2 C28 C33 88.1(7) . . . . ? O2 C28 C29 C30 165.0(4) . . . . ? C33 C28 C29 C30 -14.1(6) . . . . ? O2 C28 C29 C34 -19.7(6) . . . . ? C33 C28 C29 C34 161.2(4) . . . . ? C28 C29 C30 C31 3.2(6) . . . . ? C34 C29 C30 C31 -172.6(4) . . . . ? C29 C30 C31 C32 7.6(7) . . . . ? C29 C30 C31 C53 -171.7(4) . . . . ? C30 C31 C32 C33 -7.9(6) . . . . ? C53 C31 C32 C33 171.3(4) . . . . ? C31 C32 C33 C28 -2.4(6) . . . . ? C31 C32 C33 C54 174.8(4) . . . . ? O2 C28 C33 C32 -165.2(4) . . . . ? C29 C28 C33 C32 13.9(6) . . . . ? O2 C28 C33 C54 17.7(6) . . . . ? C29 C28 C33 C54 -163.2(4) . . . . ? C30 C29 C34 C46 -70.0(7) . . . . ? C28 C29 C34 C46 114.8(7) . . . . ? C30 C29 C34 C45 55.9(7) . . . . ? C28 C29 C34 C45 -119.3(7) . . . . ? C30 C29 C34 C35 124.9(5) . . . . ? C28 C29 C34 C35 -50.4(6) . . . . ? C30 C29 C34 C37 -110.3(5) . . . . ? C28 C29 C34 C37 74.5(6) . . . . ? C30 C29 C34 C36 6.9(5) . . . . ? C28 C29 C34 C36 -168.3(4) . . . . ? C30 C29 C34 C44 170.7(6) . . . . ? C28 C29 C34 C44 -4.5(7) . . . . ? C46 C34 C35 C38 20.1(11) . . . . ? C45 C34 C35 C38 -80.5(8) . . . . ? C37 C34 C35 C38 54.1(7) . . . . ? C29 C34 C35 C38 179.8(5) . . . . ? C36 C34 C35 C38 -59.6(6) . . . . ? C44 C34 C35 C38 75.6(8) . . . . ? C46 C34 C36 C40 -78.0(7) . . . . ? C45 C34 C36 C40 82.9(9) . . . . ? C35 C34 C36 C40 56.3(7) . . . . ? C37 C34 C36 C40 -62.0(6) . . . . ? C29 C34 C36 C40 175.9(5) . . . . ? C44 C34 C36 C40 16.1(10) . . . . ? C46 C34 C37 C42 85.6(10) . . . . ? C45 C34 C37 C42 21.3(12) . . . . ? C35 C34 C37 C42 -55.0(7) . . . . ? C29 C34 C37 C42 -178.9(5) . . . . ? C36 C34 C37 C42 60.1(6) . . . . ? C44 C34 C37 C42 -70.2(7) . . . . ? C34 C35 C38 C43 -56.5(8) . . . . ? C34 C35 C38 C39 63.6(7) . . . . ? C43 C38 C39 C40 59.4(9) . . . . ? C35 C38 C39 C40 -60.3(8) . . . . ? C38 C39 C40 C41 -59.1(9) . . . . ? C38 C39 C40 C36 57.4(8) . . . . ? C34 C36 C40 C39 -56.4(8) . . . . ? C34 C36 C40 C41 61.9(7) . . . . ? C39 C40 C41 C42 59.3(9) . . . . ? C36 C40 C41 C42 -59.6(8) . . . . ? C40 C41 C42 C43 -58.8(9) . . . . ? C40 C41 C42 C37 60.7(8) . . . . ? C34 C37 C42 C41 -62.5(8) . . . . ? C34 C37 C42 C43 58.0(7) . . . . ? C39 C38 C43 C42 -58.9(9) . . . . ? C35 C38 C43 C42 60.8(8) . . . . ? C41 C42 C43 C38 58.9(9) . . . . ? C37 C42 C43 C38 -61.6(8) . . . . ? C46 C34 C44 C47 63.0(10) . . . . ? C45 C34 C44 C47 -58.6(11) . . . . ? C35 C34 C44 C47 -80.9(10) . . . . ? C37 C34 C44 C47 78.0(9) . . . . ? C29 C34 C44 C47 -174.6(7) . . . . ? C36 C34 C44 C47 -15.1(13) . . . . ? C46 C34 C45 C49 -51.2(13) . . . . ? C35 C34 C45 C49 80.7(10) . . . . ? C37 C34 C45 C49 -14.3(16) . . . . ? C29 C34 C45 C49 -174.9(9) . . . . ? C36 C34 C45 C49 -71.2(10) . . . . ? C44 C34 C45 C49 64.2(11) . . . . ? C45 C34 C46 C51 53.2(12) . . . . ? C35 C34 C46 C51 -26.1(14) . . . . ? C37 C34 C46 C51 -85.5(12) . . . . ? C29 C34 C46 C51 174.4(8) . . . . ? C36 C34 C46 C51 68.3(9) . . . . ? C44 C34 C46 C51 -61.6(11) . . . . ? C34 C44 C47 C52 -60.4(12) . . . . ? C34 C44 C47 C48 57.3(12) . . . . ? C52 C47 C48 C49 53.1(16) . . . . ? C44 C47 C48 C49 -61.7(15) . . . . ? C47 C48 C49 C50 -51.0(17) . . . . ? C47 C48 C49 C45 63.5(14) . . . . ? C34 C45 C49 C48 -67.8(13) . . . . ? C34 C45 C49 C50 51.4(14) . . . . ? C48 C49 C50 C51 52.1(18) . . . . ? C45 C49 C50 C51 -62.1(16) . . . . ? C49 C50 C51 C52 -51.8(18) . . . . ? C49 C50 C51 C46 64.9(15) . . . . ? C34 C46 C51 C50 -57.3(14) . . . . ? C34 C46 C51 C52 60.1(13) . . . . ? C48 C47 C52 C51 -56.5(16) . . . . ? C44 C47 C52 C51 60.5(14) . . . . ? C50 C51 C52 C47 56.0(17) . . . . ? C46 C51 C52 C47 -59.8(15) . . . . ? C32 C33 C54 C56 110.8(4) . . . . ? C28 C33 C54 C56 -72.2(5) . . . . ? C32 C33 C54 C57 -9.3(5) . . . . ? C28 C33 C54 C57 167.8(4) . . . . ? C32 C33 C54 C55 -126.4(4) . . . . ? C28 C33 C54 C55 50.7(5) . . . . ? C56 C54 C55 C58 -55.2(4) . . . . ? C33 C54 C55 C58 179.3(3) . . . . ? C57 C54 C55 C58 59.3(4) . . . . ? C33 C54 C56 C60 179.2(3) . . . . ? C57 C54 C56 C60 -58.1(4) . . . . ? C55 C54 C56 C60 56.3(4) . . . . ? C56 C54 C57 C62 58.9(4) . . . . ? C33 C54 C57 C62 -176.6(3) . . . . ? C55 C54 C57 C62 -57.5(4) . . . . ? C54 C55 C58 C59 57.8(4) . . . . ? C54 C55 C58 C63 -62.1(4) . . . . ? C63 C58 C59 C60 58.9(4) . . . . ? C55 C58 C59 C60 -60.2(4) . . . . ? C54 C56 C60 C61 60.5(4) . . . . ? C54 C56 C60 C59 -59.1(4) . . . . ? C58 C59 C60 C61 -59.4(4) . . . . ? C58 C59 C60 C56 60.7(4) . . . . ? C56 C60 C61 C62 -59.7(4) . . . . ? C59 C60 C61 C62 59.7(4) . . . . ? C60 C61 C62 C63 -60.9(4) . . . . ? C60 C61 C62 C57 59.5(4) . . . . ? C54 C57 C62 C63 59.2(4) . . . . ? C54 C57 C62 C61 -61.0(4) . . . . ? C61 C62 C63 C58 60.3(5) . . . . ? C57 C62 C63 C58 -59.3(5) . . . . ? C59 C58 C63 C62 -59.3(5) . . . . ? C55 C58 C63 C62 60.5(5) . . . . ? Nb2 O3 C64 C65 -93.7(7) . . . . ? Nb2 O3 C64 C69 86.1(8) . . . . ? O3 C64 C65 C66 167.8(4) . . . . ? C69 C64 C65 C66 -12.0(6) . . . . ? O3 C64 C65 C70 -17.1(6) . . . . ? C69 C64 C65 C70 163.2(4) . . . . ? C64 C65 C66 C67 3.0(7) . . . . ? C70 C65 C66 C67 -172.3(5) . . . . ? C65 C66 C67 C68 5.0(7) . . . . ? C65 C66 C67 C80 -176.7(5) . . . . ? C66 C67 C68 C69 -4.7(7) . . . . ? C80 C67 C68 C69 177.1(5) . . . . ? C67 C68 C69 C64 -3.7(6) . . . . ? C67 C68 C69 C81 172.2(4) . . . . ? O3 C64 C69 C68 -167.5(4) . . . . ? C65 C64 C69 C68 12.2(6) . . . . ? O3 C64 C69 C81 17.2(6) . . . . ? C65 C64 C69 C81 -163.0(4) . . . . ? C66 C65 C70 C71 119.3(5) . . . . ? C64 C65 C70 C71 -55.7(6) . . . . ? C66 C65 C70 C73 -117.5(5) . . . . ? C64 C65 C70 C73 67.4(6) . . . . ? C66 C65 C70 C72 2.1(6) . . . . ? C64 C65 C70 C72 -172.9(4) . . . . ? C65 C70 C71 C74 -178.7(4) . . . . ? C73 C70 C71 C74 54.9(5) . . . . ? C72 C70 C71 C74 -58.3(5) . . . . ? C71 C70 C72 C76 57.7(6) . . . . ? C65 C70 C72 C76 176.7(4) . . . . ? C73 C70 C72 C76 -58.1(5) . . . . ? C71 C70 C73 C78 -55.1(5) . . . . ? C65 C70 C73 C78 -178.3(4) . . . . ? C72 C70 C73 C78 58.7(5) . . . . ? C70 C71 C74 C79 -58.0(5) . . . . ? C70 C71 C74 C75 61.3(6) . . . . ? C79 C74 C75 C76 59.0(6) . . . . ? C71 C74 C75 C76 -60.5(6) . . . . ? C74 C75 C76 C77 -60.5(6) . . . . ? C74 C75 C76 C72 60.1(6) . . . . ? C70 C72 C76 C75 -60.3(6) . . . . ? C70 C72 C76 C77 60.8(6) . . . . ? C75 C76 C77 C78 60.3(5) . . . . ? C72 C76 C77 C78 -60.2(6) . . . . ? C76 C77 C78 C79 -58.6(5) . . . . ? C76 C77 C78 C73 60.4(6) . . . . ? C70 C73 C78 C77 -62.0(5) . . . . ? C70 C73 C78 C79 57.7(5) . . . . ? C71 C74 C79 C78 60.4(5) . . . . ? C75 C74 C79 C78 -58.8(5) . . . . ? C77 C78 C79 C74 59.0(5) . . . . ? C73 C78 C79 C74 -60.1(5) . . . . ? C68 C69 C81 C83 68.9(5) . . . . ? C64 C69 C81 C83 -115.9(5) . . . . ? C68 C69 C81 C82 -168.7(4) . . . . ? C64 C69 C81 C82 6.6(6) . . . . ? C68 C69 C81 C84 -50.8(5) . . . . ? C64 C69 C81 C84 124.5(4) . . . . ? C83 C81 C82 C85 -57.4(5) . . . . ? C84 C81 C82 C85 58.0(5) . . . . ? C69 C81 C82 C85 177.9(4) . . . . ? C82 C81 C83 C87 57.7(5) . . . . ? C84 C81 C83 C87 -55.0(5) . . . . ? C69 C81 C83 C87 -174.6(4) . . . . ? C83 C81 C84 C89 56.8(5) . . . . ? C82 C81 C84 C89 -57.2(5) . . . . ? C69 C81 C84 C89 178.0(4) . . . . ? C81 C82 C85 C86 58.5(5) . . . . ? C81 C82 C85 C90 -61.1(5) . . . . ? C90 C85 C86 C87 57.4(6) . . . . ? C82 C85 C86 C87 -60.9(5) . . . . ? C85 C86 C87 C88 -55.6(6) . . . . ? C85 C86 C87 C83 62.3(5) . . . . ? C81 C83 C87 C88 58.2(6) . . . . ? C81 C83 C87 C86 -60.7(5) . . . . ? C86 C87 C88 C89 54.2(6) . . . . ? C83 C87 C88 C89 -62.8(6) . . . . ? C87 C88 C89 C90 -56.0(6) . . . . ? C87 C88 C89 C84 62.2(6) . . . . ? C81 C84 C89 C90 61.1(5) . . . . ? C81 C84 C89 C88 -59.1(5) . . . . ? C88 C89 C90 C85 56.3(6) . . . . ? C84 C89 C90 C85 -60.5(6) . . . . ? C86 C85 C90 C89 -57.0(6) . . . . ? C82 C85 C90 C89 60.7(6) . . . . ? Nb2 O4 C91 C96 92.0(8) . . . . ? Nb2 O4 C91 C92 -86.9(8) . . . . ? O4 C91 C92 C93 168.4(4) . . . . ? C96 C91 C92 C93 -10.4(6) . . . . ? O4 C91 C92 C97 -16.3(6) . . . . ? C96 C91 C92 C97 164.9(4) . . . . ? C91 C92 C93 C94 0.4(6) . . . . ? C97 C92 C93 C94 -175.3(4) . . . . ? C92 C93 C94 C95 7.5(7) . . . . ? C92 C93 C94 C116 -174.3(4) . . . . ? C93 C94 C95 C96 -5.7(7) . . . . ? C116 C94 C95 C96 176.0(4) . . . . ? C94 C95 C96 C91 -3.8(6) . . . . ? C94 C95 C96 C117 171.3(4) . . . . ? O4 C91 C96 C95 -166.8(4) . . . . ? C92 C91 C96 C95 12.0(6) . . . . ? O4 C91 C96 C117 18.7(6) . . . . ? C92 C91 C96 C117 -162.5(4) . . . . ? C93 C92 C97 C108 65.3(6) . . . . ? C91 C92 C97 C108 -110.0(6) . . . . ? C93 C92 C97 C100 -113.7(5) . . . . ? C91 C92 C97 C100 71.0(6) . . . . ? C93 C92 C97 C109 -56.4(6) . . . . ? C91 C92 C97 C109 128.3(6) . . . . ? C93 C92 C97 C98 120.7(5) . . . . ? C91 C92 C97 C98 -54.6(6) . . . . ? C93 C92 C97 C107 -174.8(6) . . . . ? C91 C92 C97 C107 10.0(7) . . . . ? C93 C92 C97 C99 5.4(5) . . . . ? C91 C92 C97 C99 -169.9(4) . . . . ? C108 C97 C98 C101 -82.5(8) . . . . ? C100 C97 C98 C101 53.6(7) . . . . ? C109 C97 C98 C101 -3.0(12) . . . . ? C92 C97 C98 C101 -178.4(5) . . . . ? C107 C97 C98 C101 73.0(7) . . . . ? C99 C97 C98 C101 -59.0(6) . . . . ? C108 C97 C99 C103 80.1(8) . . . . ? C100 C97 C99 C103 -59.0(8) . . . . ? C109 C97 C99 C103 -85.7(8) . . . . ? C92 C97 C99 C103 176.0(6) . . . . ? C98 C97 C99 C103 57.7(8) . . . . ? C107 C97 C99 C103 -3.9(11) . . . . ? C108 C97 C100 C105 2.4(11) . . . . ? C109 C97 C100 C105 86.6(7) . . . . ? C92 C97 C100 C105 -179.1(5) . . . . ? C98 C97 C100 C105 -54.2(7) . . . . ? C107 C97 C100 C105 -74.7(7) . . . . ? C99 C97 C100 C105 58.3(6) . . . . ? C97 C98 C101 C106 -57.1(8) . . . . ? C97 C98 C101 C102 62.1(8) . . . . ? C106 C101 C102 C103 58.3(11) . . . . ? C98 C101 C102 C103 -59.8(10) . . . . ? C101 C102 C103 C104 -57.9(12) . . . . ? C101 C102 C103 C99 57.3(11) . . . . ? C97 C99 C103 C102 -57.4(10) . . . . ? C97 C99 C103 C104 59.8(9) . . . . ? C102 C103 C104 C105 56.6(12) . . . . ? C99 C103 C104 C105 -59.9(10) . . . . ? C103 C104 C105 C100 61.9(9) . . . . ? C103 C104 C105 C106 -56.3(11) . . . . ? C97 C100 C105 C104 -62.6(8) . . . . ? C97 C100 C105 C106 57.5(8) . . . . ? C102 C101 C106 C105 -56.7(11) . . . . ? C98 C101 C106 C105 62.1(10) . . . . ? C104 C105 C106 C101 56.8(11) . . . . ? C100 C105 C106 C101 -62.4(10) . . . . ? C108 C97 C107 C110 -59.9(10) . . . . ? C100 C97 C107 C110 77.5(9) . . . . ? C109 C97 C107 C110 61.9(10) . . . . ? C92 C97 C107 C110 -178.7(8) . . . . ? C98 C97 C107 C110 -80.1(9) . . . . ? C99 C97 C107 C110 1.2(13) . . . . ? C100 C97 C108 C112 4.6(14) . . . . ? C109 C97 C108 C112 -55.8(11) . . . . ? C92 C97 C108 C112 -174.0(8) . . . . ? C98 C97 C108 C112 83.5(10) . . . . ? C107 C97 C108 C112 61.5(10) . . . . ? C99 C97 C108 C112 -68.9(9) . . . . ? C108 C97 C109 C114 55.7(10) . . . . ? C100 C97 C109 C114 -78.7(8) . . . . ? C92 C97 C109 C114 173.0(7) . . . . ? C98 C97 C109 C114 -2.5(14) . . . . ? C107 C97 C109 C114 -62.9(9) . . . . ? C99 C97 C109 C114 68.6(8) . . . . ? C97 C107 C110 C115 -60.3(13) . . . . ? C97 C107 C110 C111 59.1(13) . . . . ? C115 C110 C111 C112 56.2(19) . . . . ? C107 C110 C111 C112 -61.4(16) . . . . ? C110 C111 C112 C113 -54.2(19) . . . . ? C110 C111 C112 C108 61.6(15) . . . . ? C97 C108 C112 C113 54.0(15) . . . . ? C97 C108 C112 C111 -61.6(13) . . . . ? C111 C112 C113 C114 57(2) . . . . ? C108 C112 C113 C114 -58(2) . . . . ? C112 C113 C114 C115 -58(2) . . . . ? C112 C113 C114 C109 60.3(19) . . . . ? C97 C109 C114 C113 -55.8(14) . . . . ? C97 C109 C114 C115 62.5(12) . . . . ? C111 C110 C115 C114 -57.0(19) . . . . ? C107 C110 C115 C114 59.7(17) . . . . ? C113 C114 C115 C110 57.1(19) . . . . ? C109 C114 C115 C110 -61.5(16) . . . . ? C95 C96 C117 C120 -50.6(6) . . . . ? C91 C96 C117 C120 123.9(5) . . . . ? C95 C96 C117 C128 114.5(6) . . . . ? C91 C96 C117 C128 -70.9(7) . . . . ? C95 C96 C117 C119 71.6(6) . . . . ? C91 C96 C117 C119 -113.8(5) . . . . ? C95 C96 C117 C127 -121.6(5) . . . . ? C91 C96 C117 C127 52.9(6) . . . . ? C95 C96 C117 C118 -171.0(5) . . . . ? C91 C96 C117 C118 3.6(7) . . . . ? C95 C96 C117 C129 -7.8(6) . . . . ? C91 C96 C117 C129 166.8(5) . . . . ? C120 C117 C118 C121 55.8(8) . . . . ? C128 C117 C118 C121 -75.7(8) . . . . ? C96 C117 C118 C121 176.3(6) . . . . ? C119 C117 C118 C121 -64.1(8) . . . . ? C127 C117 C118 C121 84.4(9) . . . . ? C129 C117 C118 C121 16.3(11) . . . . ? C120 C117 C119 C123 -55.5(8) . . . . ? C128 C117 C119 C123 77.6(9) . . . . ? C96 C117 C119 C123 -174.9(6) . . . . ? C127 C117 C119 C123 24.9(12) . . . . ? C118 C117 C119 C123 61.0(8) . . . . ? C129 C117 C119 C123 -65.9(7) . . . . ? C128 C117 C120 C125 14.2(12) . . . . ? C96 C117 C120 C125 175.3(6) . . . . ? C119 C117 C120 C125 55.4(9) . . . . ? C127 C117 C120 C125 -81.5(8) . . . . ? C118 C117 C120 C125 -59.5(8) . . . . ? C129 C117 C120 C125 70.8(9) . . . . ? C117 C118 C121 C122 64.7(10) . . . . ? C117 C118 C121 C126 -55.6(10) . . . . ? C126 C121 C122 C123 59.0(13) . . . . ? C118 C121 C122 C123 -62.1(12) . . . . ? C117 C119 C123 C124 57.2(10) . . . . ? C117 C119 C123 C122 -60.2(10) . . . . ? C121 C122 C123 C124 -56.5(13) . . . . ? C121 C122 C123 C119 61.5(12) . . . . ? C119 C123 C124 C125 -61.1(11) . . . . ? C122 C123 C124 C125 56.3(12) . . . . ? C117 C120 C125 C126 61.5(10) . . . . ? C117 C120 C125 C124 -54.9(10) . . . . ? C123 C124 C125 C126 -58.6(12) . . . . ? C123 C124 C125 C120 58.2(11) . . . . ? C122 C121 C126 C125 -60.9(13) . . . . ? C118 C121 C126 C125 56.8(12) . . . . ? C120 C125 C126 C121 -57.4(11) . . . . ? C124 C125 C126 C121 59.0(11) . . . . ? C120 C117 C127 C130 77.4(8) . . . . ? C128 C117 C127 C130 -53.5(9) . . . . ? C96 C117 C127 C130 179.4(6) . . . . ? C119 C117 C127 C130 -20.5(12) . . . . ? C118 C117 C127 C130 -72.8(8) . . . . ? C129 C117 C127 C130 59.4(8) . . . . ? C120 C117 C128 C132 -19.7(13) . . . . ? C96 C117 C128 C132 -179.7(8) . . . . ? C119 C117 C128 C132 -90.3(11) . . . . ? C127 C117 C128 C132 57.0(10) . . . . ? C118 C117 C128 C132 72.1(9) . . . . ? C129 C117 C128 C132 -54.0(10) . . . . ? C120 C117 C129 C134 -85.3(10) . . . . ? C128 C117 C129 C134 56.3(9) . . . . ? C96 C117 C129 C134 -176.3(7) . . . . ? C119 C117 C129 C134 79.8(8) . . . . ? C127 C117 C129 C134 -59.2(9) . . . . ? C118 C117 C129 C134 -15.9(12) . . . . ? C117 C127 C130 C135 -61.2(10) . . . . ? C117 C127 C130 C131 55.8(10) . . . . ? C135 C130 C131 C132 54.2(14) . . . . ? C127 C130 C131 C132 -64.0(13) . . . . ? C130 C131 C132 C133 -55.1(16) . . . . ? C130 C131 C132 C128 63.8(13) . . . . ? C117 C128 C132 C133 58.0(13) . . . . ? C117 C128 C132 C131 -60.5(12) . . . . ? C131 C132 C133 C134 56.8(15) . . . . ? C128 C132 C133 C134 -56.9(14) . . . . ? C117 C129 C134 C135 59.8(11) . . . . ? C117 C129 C134 C133 -57.7(11) . . . . ? C132 C133 C134 C135 -60.3(14) . . . . ? C132 C133 C134 C129 58.3(13) . . . . ? C129 C134 C135 C130 -56.9(12) . . . . ? C133 C134 C135 C130 61.0(12) . . . . ? C131 C130 C135 C134 -58.9(12) . . . . ? C127 C130 C135 C134 57.6(11) . . . . ? C141 C136 C137 C138 -10(2) . . . . ? C136 C137 C138 C139 9(2) . . . . ? C137 C138 C139 C140 -2(2) . . . . ? C138 C139 C140 C141 -5(2) . . . . ? C139 C140 C141 C136 5(2) . . . . ? C137 C136 C141 C140 3(2) . . . . ? C142 C143 C144 C145 -78(3) . . . . ? C143 C144 C145 C146 159.9(16) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.646 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.110 data_[{(ArO)2Nb}{(ArO)Nb(O)}{OArCHC}(O)](benzene)(hexane)2.5 _database_code_depnum_ccdc_archive 'CCDC 902915' #TrackingRef '14202_web_deposit_cif_file_0_HiroyukiKawaguchi_1348537764.CIF-kawaguchi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C100 H126 Nb2 O6, C6 H6, 2.5(C6 H14)' _chemical_formula_sum 'C121 H167 Nb2 O6' _chemical_formula_weight 1903.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.793(7) _cell_length_b 17.972(7) _cell_length_c 18.964(7) _cell_angle_alpha 58.272(11) _cell_angle_beta 74.032(18) _cell_angle_gamma 83.67(2) _cell_volume 4955(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9217 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2046 _exptl_absorpt_coefficient_mu 0.289 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9526 _exptl_absorpt_correction_T_max 0.9717 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Mercury375R CCD (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 13.6612 _diffrn_reflns_number 53106 _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_sigmaI/netI 0.1819 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.52 _reflns_number_total 22676 _reflns_number_gt 12400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2009)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2009)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+8.3486P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22676 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1660 _refine_ls_R_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.2435 _refine_ls_wR_factor_gt 0.1839 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.20722(3) 0.22659(3) 0.23943(3) 0.02555(15) Uani 1 1 d . . . Nb2 Nb 0.12024(3) 0.33522(3) 0.31467(3) 0.02479(14) Uani 1 1 d . . . O1 O 0.2201(2) 0.3284(3) 0.2559(3) 0.0271(9) Uani 1 1 d . . . O2 O 0.1820(2) 0.2860(3) 0.1444(3) 0.0320(10) Uani 1 1 d . . . O3 O 0.1637(2) 0.1105(3) 0.2805(3) 0.0311(10) Uani 1 1 d . . . O4 O 0.3164(2) 0.2005(3) 0.2203(3) 0.0293(9) Uani 1 1 d . . . O5 O 0.0644(2) 0.4182(2) 0.2357(2) 0.0264(9) Uani 1 1 d . . . O6 O 0.1228(2) 0.3325(2) 0.4155(2) 0.0256(9) Uani 1 1 d . . . C1 C 0.0914(3) 0.2182(4) 0.3429(4) 0.0266(13) Uani 1 1 d . . . C2 C 0.0405(4) 0.1464(4) 0.3886(4) 0.0292(13) Uani 1 1 d . . . H1 H -0.001(4) 0.141(4) 0.436(4) 0.04(2) Uiso 1 1 d . . . C3 C 0.0952(4) 0.0638(4) 0.3143(4) 0.0301(14) Uani 1 1 d . . . C4 C 0.0833(4) 0.0069(4) 0.2868(4) 0.0320(14) Uani 1 1 d . . . C5 C 0.0115(4) -0.0409(4) 0.3275(4) 0.0335(14) Uani 1 1 d . . . H2 H 0.0019 -0.0795 0.3106 0.040 Uiso 1 1 calc R . . C6 C -0.0474(4) -0.0357(4) 0.3915(4) 0.0322(14) Uani 1 1 d . . . C7 C -0.0346(4) 0.0233(4) 0.4136(4) 0.0317(14) Uani 1 1 d . . . H3 H -0.0735 0.0287 0.4564 0.038 Uiso 1 1 calc R . . C8 C 0.0355(4) 0.0757(4) 0.3734(4) 0.0296(13) Uani 1 1 d . . . C9 C -0.1231(4) -0.0908(4) 0.4307(5) 0.0406(16) Uani 1 1 d . . . H4 H -0.1360 -0.1196 0.4933 0.061 Uiso 1 1 calc R . . H5 H -0.1166 -0.1353 0.4146 0.061 Uiso 1 1 calc R . . H6 H -0.1655 -0.0531 0.4093 0.061 Uiso 1 1 calc R . . C10 C 0.1430(4) 0.0006(4) 0.2141(4) 0.0311(14) Uani 1 1 d . . . C11 C 0.1558(4) 0.0917(4) 0.1293(4) 0.0372(15) Uani 1 1 d . . . H7 H 0.1056 0.1104 0.1130 0.045 Uiso 1 1 calc R . . H8 H 0.1737 0.1356 0.1383 0.045 Uiso 1 1 calc R . . C12 C 0.1139(4) -0.0642(4) 0.1952(5) 0.0409(17) Uani 1 1 d . . . H9 H 0.1050 -0.1235 0.2473 0.049 Uiso 1 1 calc R . . H10 H 0.0635 -0.0452 0.1795 0.049 Uiso 1 1 calc R . . C13 C 0.2212(4) -0.0292(4) 0.2358(5) 0.0378(16) Uani 1 1 d . . . H11 H 0.2135 -0.0877 0.2889 0.045 Uiso 1 1 calc R . . H12 H 0.2409 0.0120 0.2470 0.045 Uiso 1 1 calc R . . C14 C 0.2168(4) 0.0871(5) 0.0568(5) 0.0468(18) Uani 1 1 d . . . H13 H 0.2250 0.1465 0.0035 0.056 Uiso 1 1 calc R . . C15 C 0.1873(5) 0.0221(5) 0.0399(5) 0.054(2) Uani 1 1 d . . . H14 H 0.1377 0.0415 0.0227 0.065 Uiso 1 1 calc R . . H15 H 0.2263 0.0192 -0.0071 0.065 Uiso 1 1 calc R . . C16 C 0.1744(4) -0.0676(5) 0.1215(5) 0.051(2) Uani 1 1 d . . . H16 H 0.1548 -0.1101 0.1111 0.061 Uiso 1 1 calc R . . C17 C 0.2523(4) -0.0986(5) 0.1466(6) 0.053(2) Uani 1 1 d . . . H17 H 0.2443 -0.1576 0.1989 0.064 Uiso 1 1 calc R . . H18 H 0.2912 -0.1020 0.0998 0.064 Uiso 1 1 calc R . . C18 C 0.2828(4) -0.0340(5) 0.1630(5) 0.0455(18) Uani 1 1 d . . . H19 H 0.3335 -0.0534 0.1792 0.055 Uiso 1 1 calc R . . C19 C 0.2941(4) 0.0577(5) 0.0810(5) 0.0465(18) Uani 1 1 d . . . H20 H 0.3138 0.1000 0.0909 0.056 Uiso 1 1 calc R . . H21 H 0.3334 0.0561 0.0334 0.056 Uiso 1 1 calc R . . C20 C 0.3954(3) 0.2054(4) 0.2136(4) 0.0255(12) Uani 1 1 d . . . C21 C 0.4442(3) 0.2726(4) 0.1365(4) 0.0273(13) Uani 1 1 d . . . C22 C 0.5203(4) 0.2839(4) 0.1390(4) 0.0340(14) Uani 1 1 d . . . H22 H 0.5536 0.3295 0.0890 0.041 Uiso 1 1 calc R . . C23 C 0.5491(4) 0.2325(4) 0.2100(4) 0.0348(15) Uani 1 1 d . . . C24 C 0.5024(3) 0.1616(4) 0.2811(4) 0.0331(14) Uani 1 1 d . . . H23 H 0.5228 0.1240 0.3293 0.040 Uiso 1 1 calc R . . C25 C 0.4260(3) 0.1435(4) 0.2841(4) 0.0290(13) Uani 1 1 d . . . C26 C 0.4190(3) 0.3305(4) 0.0512(4) 0.0291(13) Uani 1 1 d . . . C27 C 0.3798(4) 0.2727(4) 0.0309(4) 0.0325(14) Uani 1 1 d . . . H24 H 0.4165 0.2280 0.0284 0.039 Uiso 1 1 calc R . . H25 H 0.3325 0.2417 0.0777 0.039 Uiso 1 1 calc R . . C28 C 0.3625(4) 0.4032(4) 0.0505(4) 0.0310(14) Uani 1 1 d . . . H26 H 0.3149 0.3759 0.0982 0.037 Uiso 1 1 calc R . . H27 H 0.3883 0.4424 0.0596 0.037 Uiso 1 1 calc R . . C29 C 0.4915(4) 0.3789(5) -0.0266(4) 0.0416(17) Uani 1 1 d . . . H28 H 0.5173 0.4183 -0.0177 0.050 Uiso 1 1 calc R . . H29 H 0.5295 0.3353 -0.0290 0.050 Uiso 1 1 calc R . . C30 C 0.3569(4) 0.3281(4) -0.0552(4) 0.0367(15) Uani 1 1 d . . . H30 H 0.3310 0.2888 -0.0649 0.044 Uiso 1 1 calc R . . C31 C 0.4304(4) 0.3725(5) -0.1289(4) 0.0438(17) Uani 1 1 d . . . H31 H 0.4161 0.4070 -0.1843 0.053 Uiso 1 1 calc R . . H32 H 0.4671 0.3277 -0.1310 0.053 Uiso 1 1 calc R . . C32 C 0.4691(4) 0.4330(5) -0.1128(4) 0.0405(16) Uani 1 1 d . . . H33 H 0.5171 0.4630 -0.1603 0.049 Uiso 1 1 calc R . . C33 C 0.4118(4) 0.5017(4) -0.1086(4) 0.0412(17) Uani 1 1 d . . . H34 H 0.4376 0.5417 -0.1004 0.049 Uiso 1 1 calc R . . H35 H 0.3964 0.5370 -0.1634 0.049 Uiso 1 1 calc R . . C34 C 0.3390(4) 0.4573(4) -0.0347(4) 0.0350(15) Uani 1 1 d . . . H36 H 0.3020 0.5027 -0.0328 0.042 Uiso 1 1 calc R . . C35 C 0.2990(4) 0.3964(4) -0.0509(4) 0.0371(15) Uani 1 1 d . . . H37 H 0.2514 0.3667 -0.0039 0.044 Uiso 1 1 calc R . . H38 H 0.2833 0.4316 -0.1055 0.044 Uiso 1 1 calc R . . C36 C 0.6295(4) 0.2519(5) 0.2111(5) 0.0450(18) Uani 1 1 d . . . H39 H 0.6397 0.2085 0.2666 0.067 Uiso 1 1 calc R . . H40 H 0.6314 0.3105 0.2023 0.067 Uiso 1 1 calc R . . H41 H 0.6692 0.2491 0.1652 0.067 Uiso 1 1 calc R . . C37 C 0.3844(4) 0.0545(4) 0.3588(4) 0.0309(14) Uani 1 1 d . . . C38 C 0.3731(4) 0.0007(4) 0.3201(4) 0.0386(16) Uani 1 1 d . . . H42 H 0.3404 0.0332 0.2791 0.046 Uiso 1 1 calc R . . H43 H 0.4246 -0.0066 0.2880 0.046 Uiso 1 1 calc R . . C39 C 0.3036(4) 0.0618(4) 0.4122(4) 0.0392(16) Uani 1 1 d . . . H44 H 0.3105 0.0932 0.4402 0.047 Uiso 1 1 calc R . . H45 H 0.2692 0.0963 0.3736 0.047 Uiso 1 1 calc R . . C40 C 0.4340(4) 0.0003(5) 0.4235(4) 0.0432(17) Uani 1 1 d . . . H46 H 0.4865 -0.0063 0.3924 0.052 Uiso 1 1 calc R . . H47 H 0.4409 0.0323 0.4509 0.052 Uiso 1 1 calc R . . C41 C 0.3343(4) -0.0890(4) 0.3888(5) 0.0457(18) Uani 1 1 d . . . H48 H 0.3274 -0.1215 0.3613 0.055 Uiso 1 1 calc R . . C42 C 0.2536(4) -0.0789(4) 0.4398(5) 0.0449(18) Uani 1 1 d . . . H49 H 0.2193 -0.0464 0.4007 0.054 Uiso 1 1 calc R . . H50 H 0.2285 -0.1373 0.4844 0.054 Uiso 1 1 calc R . . C43 C 0.2643(4) -0.0297(4) 0.4815(4) 0.0383(16) Uani 1 1 d . . . H51 H 0.2121 -0.0228 0.5142 0.046 Uiso 1 1 calc R . . C44 C 0.3167(4) -0.0806(5) 0.5431(5) 0.051(2) Uani 1 1 d . . . H52 H 0.3232 -0.0487 0.5707 0.062 Uiso 1 1 calc R . . H53 H 0.2920 -0.1390 0.5886 0.062 Uiso 1 1 calc R . . C45 C 0.3961(4) -0.0907(5) 0.4933(5) 0.053(2) Uani 1 1 d . . . H54 H 0.4304 -0.1235 0.5333 0.063 Uiso 1 1 calc R . . C46 C 0.3864(5) -0.1410(5) 0.4517(5) 0.058(2) Uani 1 1 d . . . H55 H 0.3617 -0.1997 0.4964 0.070 Uiso 1 1 calc R . . H56 H 0.4382 -0.1488 0.4203 0.070 Uiso 1 1 calc R . . C47 C 0.0212(3) 0.4902(4) 0.1900(4) 0.0270(13) Uani 1 1 d . . . C48 C -0.0458(3) 0.4769(4) 0.1707(4) 0.0274(13) Uani 1 1 d . . . C49 C -0.0947(3) 0.5485(4) 0.1397(4) 0.0312(14) Uani 1 1 d . . . H57 H -0.1402 0.5409 0.1270 0.037 Uiso 1 1 calc R . . C50 C -0.0797(4) 0.6293(4) 0.1270(4) 0.0327(14) Uani 1 1 d . . . C51 C -0.0077(3) 0.6414(4) 0.1369(4) 0.0280(13) Uani 1 1 d . . . H58 H 0.0061 0.6979 0.1233 0.034 Uiso 1 1 calc R . . C52 C 0.0451(3) 0.5747(4) 0.1657(4) 0.0276(13) Uani 1 1 d . . . C53 C -0.0630(3) 0.3939(4) 0.1707(4) 0.0264(13) Uani 1 1 d . . . C54 C 0.0091(3) 0.3777(4) 0.1138(4) 0.0281(13) Uani 1 1 d . . . H59 H 0.0209 0.4299 0.0551 0.034 Uiso 1 1 calc R . . H60 H 0.0550 0.3688 0.1370 0.034 Uiso 1 1 calc R . . C55 C -0.1333(3) 0.4056(4) 0.1334(4) 0.0286(13) Uani 1 1 d . . . H61 H -0.1231 0.4581 0.0749 0.034 Uiso 1 1 calc R . . H62 H -0.1806 0.4152 0.1694 0.034 Uiso 1 1 calc R . . C56 C -0.0839(3) 0.3110(4) 0.2627(4) 0.0291(13) Uani 1 1 d . . . H63 H -0.0412 0.3014 0.2905 0.035 Uiso 1 1 calc R . . H64 H -0.1324 0.3203 0.2977 0.035 Uiso 1 1 calc R . . C57 C -0.0047(4) 0.2972(4) 0.1097(4) 0.0311(14) Uani 1 1 d . . . H65 H 0.0430 0.2879 0.0729 0.037 Uiso 1 1 calc R . . C58 C -0.0745(4) 0.3116(4) 0.0725(4) 0.0340(15) Uani 1 1 d . . . H66 H -0.0832 0.2603 0.0690 0.041 Uiso 1 1 calc R . . H67 H -0.0636 0.3638 0.0138 0.041 Uiso 1 1 calc R . . C59 C -0.1484(4) 0.3248(4) 0.1296(4) 0.0347(15) Uani 1 1 d . . . H68 H -0.1938 0.3348 0.1046 0.042 Uiso 1 1 calc R . . C60 C -0.1660(3) 0.2433(4) 0.2207(4) 0.0328(14) Uani 1 1 d . . . H69 H -0.1750 0.1912 0.2187 0.039 Uiso 1 1 calc R . . H70 H -0.2138 0.2514 0.2573 0.039 Uiso 1 1 calc R . . C61 C -0.0959(4) 0.2296(4) 0.2588(4) 0.0316(14) Uani 1 1 d . . . H71 H -0.1066 0.1765 0.3178 0.038 Uiso 1 1 calc R . . C62 C -0.0220(4) 0.2172(4) 0.2008(4) 0.0327(14) Uani 1 1 d . . . H72 H 0.0232 0.2082 0.2249 0.039 Uiso 1 1 calc R . . H73 H -0.0298 0.1645 0.1991 0.039 Uiso 1 1 calc R . . C63 C -0.1355(4) 0.7021(4) 0.0964(5) 0.0416(17) Uani 1 1 d . . . H74 H -0.1608 0.6972 0.0591 0.062 Uiso 1 1 calc R . . H75 H -0.1066 0.7587 0.0644 0.062 Uiso 1 1 calc R . . H76 H -0.1754 0.6978 0.1459 0.062 Uiso 1 1 calc R . . C64 C 0.1312(3) 0.6015(4) 0.1546(4) 0.0272(13) Uani 1 1 d . . . C65 C 0.1885(3) 0.5703(4) 0.0972(4) 0.0270(13) Uani 1 1 d . . . H77 H 0.1841 0.5057 0.1268 0.032 Uiso 1 1 calc R . . H78 H 0.1740 0.5953 0.0424 0.032 Uiso 1 1 calc R . . C66 C 0.1550(3) 0.5639(4) 0.2390(4) 0.0290(13) Uani 1 1 d . . . H79 H 0.1198 0.5848 0.2749 0.035 Uiso 1 1 calc R . . H80 H 0.1500 0.4992 0.2712 0.035 Uiso 1 1 calc R . . C67 C 0.1423(4) 0.7029(4) 0.1052(4) 0.0307(14) Uani 1 1 d . . . H81 H 0.1277 0.7284 0.0503 0.037 Uiso 1 1 calc R . . H82 H 0.1067 0.7253 0.1395 0.037 Uiso 1 1 calc R . . C68 C 0.2736(3) 0.5993(4) 0.0788(4) 0.0313(14) Uani 1 1 d . . . H83 H 0.3094 0.5777 0.0430 0.038 Uiso 1 1 calc R . . C69 C 0.2953(3) 0.5604(4) 0.1638(4) 0.0307(14) Uani 1 1 d . . . H84 H 0.3501 0.5782 0.1527 0.037 Uiso 1 1 calc R . . H85 H 0.2911 0.4957 0.1947 0.037 Uiso 1 1 calc R . . C70 C 0.2399(3) 0.5932(4) 0.2194(4) 0.0322(14) Uani 1 1 d . . . H86 H 0.2549 0.5679 0.2746 0.039 Uiso 1 1 calc R . . C71 C 0.2484(4) 0.6925(4) 0.1716(4) 0.0367(15) Uani 1 1 d . . . H87 H 0.3031 0.7104 0.1605 0.044 Uiso 1 1 calc R . . H88 H 0.2139 0.7143 0.2072 0.044 Uiso 1 1 calc R . . C72 C 0.2264(4) 0.7324(4) 0.0867(4) 0.0338(15) Uani 1 1 d . . . H89 H 0.2309 0.7977 0.0559 0.041 Uiso 1 1 calc R . . C73 C 0.2809(4) 0.7000(4) 0.0301(4) 0.0360(15) Uani 1 1 d . . . H90 H 0.2660 0.7251 -0.0245 0.043 Uiso 1 1 calc R . . H91 H 0.3357 0.7191 0.0167 0.043 Uiso 1 1 calc R . . C74 C 0.1165(4) 0.3157(4) 0.4979(4) 0.0292(13) Uani 1 1 d . . . C75 C 0.0397(3) 0.3136(4) 0.5498(4) 0.0281(13) Uani 1 1 d . . . C76 C 0.0336(4) 0.2823(4) 0.6360(4) 0.0362(15) Uani 1 1 d . . . H92 H -0.0167 0.2784 0.6721 0.043 Uiso 1 1 calc R . . C77 C 0.0967(4) 0.2565(4) 0.6718(4) 0.0357(15) Uani 1 1 d . . . C78 C 0.1711(4) 0.2678(4) 0.6171(4) 0.0325(14) Uani 1 1 d . . . H93 H 0.2152 0.2539 0.6403 0.039 Uiso 1 1 calc R . . C79 C 0.1838(3) 0.2987(4) 0.5297(4) 0.0292(13) Uani 1 1 d . . . C80 C -0.0356(3) 0.3448(4) 0.5175(4) 0.0277(13) Uani 1 1 d . . . C81 C -0.0229(4) 0.4387(4) 0.4377(4) 0.0319(14) Uani 1 1 d . . . H94 H -0.0061 0.4788 0.4520 0.038 Uiso 1 1 calc R . . H95 H 0.0192 0.4394 0.3907 0.038 Uiso 1 1 calc R . . C82 C -0.1042(4) 0.3471(4) 0.5876(4) 0.0358(15) Uani 1 1 d . . . H96 H -0.1151 0.2874 0.6390 0.043 Uiso 1 1 calc R . . H97 H -0.0885 0.3855 0.6044 0.043 Uiso 1 1 calc R . . C83 C -0.0638(4) 0.2817(4) 0.4951(4) 0.0329(14) Uani 1 1 d . . . H98 H -0.0223 0.2787 0.4497 0.040 Uiso 1 1 calc R . . H99 H -0.0744 0.2220 0.5465 0.040 Uiso 1 1 calc R . . C84 C -0.0984(4) 0.4715(4) 0.4072(4) 0.0321(14) Uani 1 1 d . . . H100 H -0.0881 0.5316 0.3549 0.039 Uiso 1 1 calc R . . C85 C -0.1629(4) 0.4735(4) 0.4775(4) 0.0405(16) Uani 1 1 d . . . H101 H -0.2110 0.4955 0.4573 0.049 Uiso 1 1 calc R . . H102 H -0.1469 0.5135 0.4924 0.049 Uiso 1 1 calc R . . C86 C -0.1793(4) 0.3806(5) 0.5569(4) 0.0407(16) Uani 1 1 d . . . H103 H -0.2215 0.3817 0.6037 0.049 Uiso 1 1 calc R . . C87 C -0.2048(4) 0.3176(5) 0.5353(4) 0.0414(17) Uani 1 1 d . . . H104 H -0.2536 0.3372 0.5163 0.050 Uiso 1 1 calc R . . H105 H -0.2150 0.2581 0.5870 0.050 Uiso 1 1 calc R . . C88 C -0.1395(4) 0.3161(4) 0.4637(4) 0.0368(15) Uani 1 1 d . . . H106 H -0.1565 0.2766 0.4481 0.044 Uiso 1 1 calc R . . C89 C -0.1235(4) 0.4083(4) 0.3853(4) 0.0355(15) Uani 1 1 d . . . H107 H -0.1712 0.4291 0.3644 0.043 Uiso 1 1 calc R . . H108 H -0.0816 0.4074 0.3389 0.043 Uiso 1 1 calc R . . C90 C 0.0874(4) 0.2220(5) 0.7655(4) 0.051(2) Uani 1 1 d . . . H109 H 0.1294 0.1822 0.7848 0.077 Uiso 1 1 calc R . . H110 H 0.0366 0.1905 0.7989 0.077 Uiso 1 1 calc R . . H111 H 0.0903 0.2711 0.7736 0.077 Uiso 1 1 calc R . . C91 C 0.2694(4) 0.3124(4) 0.4746(4) 0.0308(14) Uani 1 1 d . . . C92 C 0.2838(4) 0.4060(4) 0.3953(4) 0.0328(14) Uani 1 1 d . . . H112 H 0.2477 0.4153 0.3602 0.039 Uiso 1 1 calc R . . H113 H 0.2722 0.4487 0.4144 0.039 Uiso 1 1 calc R . . C93 C 0.2893(4) 0.2458(4) 0.4450(4) 0.0341(15) Uani 1 1 d . . . H114 H 0.2532 0.2516 0.4111 0.041 Uiso 1 1 calc R . . H115 H 0.2822 0.1857 0.4958 0.041 Uiso 1 1 calc R . . C94 C 0.3285(4) 0.3003(5) 0.5266(4) 0.0411(16) Uani 1 1 d . . . H116 H 0.3172 0.3417 0.5474 0.049 Uiso 1 1 calc R . . H117 H 0.3216 0.2401 0.5773 0.049 Uiso 1 1 calc R . . C95 C 0.3680(4) 0.4224(4) 0.3403(4) 0.0328(14) Uani 1 1 d . . . H118 H 0.3748 0.4832 0.2891 0.039 Uiso 1 1 calc R . . C96 C 0.3860(4) 0.3557(4) 0.3110(4) 0.0378(16) Uani 1 1 d . . . H119 H 0.4405 0.3660 0.2751 0.045 Uiso 1 1 calc R . . H120 H 0.3505 0.3633 0.2758 0.045 Uiso 1 1 calc R . . C97 C 0.3753(4) 0.2617(4) 0.3894(5) 0.0406(16) Uani 1 1 d . . . H121 H 0.3869 0.2190 0.3696 0.049 Uiso 1 1 calc R . . C98 C 0.4319(4) 0.2506(5) 0.4418(5) 0.0487(19) Uani 1 1 d . . . H122 H 0.4865 0.2612 0.4060 0.058 Uiso 1 1 calc R . . H123 H 0.4266 0.1900 0.4918 0.058 Uiso 1 1 calc R . . C99 C 0.4133(4) 0.3161(5) 0.4726(5) 0.0458(18) Uani 1 1 d . . . H124 H 0.4495 0.3083 0.5079 0.055 Uiso 1 1 calc R . . C100 C 0.4245(4) 0.4106(5) 0.3935(5) 0.0450(18) Uani 1 1 d . . . H125 H 0.4139 0.4534 0.4125 0.054 Uiso 1 1 calc R . . H126 H 0.4792 0.4211 0.3580 0.054 Uiso 1 1 calc R . . C101 C 0.4030(8) -0.3523(9) 0.3115(9) 0.129(5) Uiso 1 1 d . . . H127 H 0.3609 -0.3735 0.3014 0.194 Uiso 1 1 calc R . . H128 H 0.3950 -0.3781 0.3733 0.194 Uiso 1 1 calc R . . H129 H 0.4535 -0.3693 0.2881 0.194 Uiso 1 1 calc R . . C102 C 0.4022(8) -0.2594(9) 0.2705(9) 0.122(4) Uiso 1 1 d . . . H130 H 0.3501 -0.2435 0.2931 0.146 Uiso 1 1 calc R . . H131 H 0.4089 -0.2347 0.2084 0.146 Uiso 1 1 calc R . . C103 C 0.4606(7) -0.2186(8) 0.2802(8) 0.112(4) Uiso 1 1 d . . . H132 H 0.4537 -0.2426 0.3421 0.134 Uiso 1 1 calc R . . H133 H 0.4518 -0.1551 0.2531 0.134 Uiso 1 1 calc R . . C104 C 0.5456(7) -0.2313(9) 0.2411(8) 0.112(4) Uiso 1 1 d . . . H134 H 0.5523 -0.2104 0.1799 0.134 Uiso 1 1 calc R . . H135 H 0.5560 -0.2945 0.2707 0.134 Uiso 1 1 calc R . . C105 C 0.6061(12) -0.1815(14) 0.2485(14) 0.212(9) Uiso 1 1 d . . . H136 H 0.6046 -0.2056 0.3094 0.254 Uiso 1 1 calc R . . H137 H 0.5953 -0.1184 0.2219 0.254 Uiso 1 1 calc R . . C106 C 0.6893(12) -0.1960(13) 0.1980(13) 0.211(9) Uiso 1 1 d . . . H138 H 0.7310 -0.1688 0.2028 0.316 Uiso 1 1 calc R . . H139 H 0.6904 -0.1693 0.1374 0.316 Uiso 1 1 calc R . . H140 H 0.6973 -0.2589 0.2230 0.316 Uiso 1 1 calc R . . C107 C 0.6454(11) -0.0305(12) 0.3045(12) 0.197(8) Uiso 1 1 d U . . H141 H 0.6013 -0.0685 0.3188 0.295 Uiso 1 1 calc R . . H142 H 0.6268 0.0277 0.2915 0.295 Uiso 1 1 calc R . . H143 H 0.6686 -0.0558 0.3533 0.295 Uiso 1 1 calc R . . C108 C 0.7119(16) -0.0219(19) 0.2199(19) 0.302(12) Uiso 1 1 d DU . . H144 H 0.7288 -0.0789 0.2258 0.362 Uiso 1 1 calc R . . H145 H 0.6979 0.0174 0.1648 0.362 Uiso 1 1 calc R . . C109 C 0.7632(12) 0.0171(14) 0.2370(13) 0.204(8) Uiso 1 1 d DU . . H146 H 0.7616 -0.0188 0.2987 0.244 Uiso 1 1 calc R . . H147 H 0.7444 0.0756 0.2250 0.244 Uiso 1 1 calc R . . C110 C 0.8521(10) 0.0282(11) 0.1822(11) 0.155(6) Uiso 1 1 d U . . H148 H 0.8811 0.0667 0.1893 0.186 Uiso 1 1 calc R . . H149 H 0.8755 -0.0299 0.2071 0.186 Uiso 1 1 calc R . . C111 C 0.8640(8) 0.0621(9) 0.0947(9) 0.124(4) Uiso 1 1 d U . . H150 H 0.8368 0.1178 0.0705 0.148 Uiso 1 1 calc R . . H151 H 0.8394 0.0208 0.0873 0.148 Uiso 1 1 calc R . . C112 C 0.9532(7) 0.0801(8) 0.0408(8) 0.119(4) Uiso 1 1 d U . . H152 H 0.9557 0.1044 -0.0198 0.179 Uiso 1 1 calc R . . H153 H 0.9806 0.0251 0.0624 0.179 Uiso 1 1 calc R . . H154 H 0.9782 0.1220 0.0465 0.179 Uiso 1 1 calc R . . C113 C 0.6861(6) -0.5444(9) 0.3139(8) 0.136(5) Uiso 1 1 d G . . H155 H 0.7139 -0.5593 0.2728 0.164 Uiso 1 1 calc R . . C114 C 0.6936(6) -0.4600(8) 0.2970(7) 0.174(7) Uiso 1 1 d G . . H156 H 0.7266 -0.4172 0.2443 0.209 Uiso 1 1 calc R . . C115 C 0.6529(8) -0.4381(7) 0.3571(10) 0.186(7) Uiso 1 1 d G . . H157 H 0.6580 -0.3804 0.3455 0.223 Uiso 1 1 calc R . . C116 C 0.6047(7) -0.5007(11) 0.4342(8) 0.215(9) Uiso 1 1 d G . . H158 H 0.5768 -0.4858 0.4753 0.258 Uiso 1 1 calc R . . C117 C 0.5972(7) -0.5852(9) 0.4511(7) 0.219(9) Uiso 1 1 d G . . H159 H 0.5642 -0.6280 0.5038 0.262 Uiso 1 1 calc R . . C118 C 0.6379(7) -0.6070(6) 0.3910(9) 0.196(8) Uiso 1 1 d G . . H160 H 0.6328 -0.6647 0.4026 0.236 Uiso 1 1 calc R . . C119 C 0.4318(7) -0.1048(7) -0.0651(7) 0.100(4) Uiso 1 1 d . . . H161 H 0.4234 -0.0902 -0.1199 0.149 Uiso 1 1 calc R . . H162 H 0.3815 -0.1218 -0.0217 0.149 Uiso 1 1 calc R . . H163 H 0.4670 -0.1536 -0.0467 0.149 Uiso 1 1 calc R . . C120 C 0.4677(8) -0.0263(9) -0.0758(9) 0.121(4) Uiso 1 1 d . . . H164 H 0.5176 -0.0088 -0.1209 0.146 Uiso 1 1 calc R . . H165 H 0.4322 0.0229 -0.0958 0.146 Uiso 1 1 calc R . . C121 C 0.4833(7) -0.0407(7) 0.0034(8) 0.102(4) Uiso 1 1 d . . . H166 H 0.5208 -0.0880 0.0216 0.122 Uiso 1 1 calc R . . H167 H 0.4339 -0.0616 0.0493 0.122 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0217(3) 0.0257(3) 0.0308(3) -0.0166(2) -0.0040(2) -0.0012(2) Nb2 0.0229(3) 0.0256(3) 0.0276(3) -0.0155(2) -0.0048(2) -0.0001(2) O1 0.023(2) 0.028(2) 0.033(2) -0.0170(19) -0.0081(17) -0.0018(17) O2 0.030(2) 0.037(2) 0.034(2) -0.021(2) -0.0104(19) -0.0006(19) O3 0.024(2) 0.028(2) 0.046(3) -0.024(2) -0.0045(19) -0.0016(18) O4 0.023(2) 0.030(2) 0.035(2) -0.018(2) -0.0042(18) -0.0009(18) O5 0.027(2) 0.028(2) 0.026(2) -0.0146(18) -0.0074(17) -0.0012(18) O6 0.026(2) 0.027(2) 0.023(2) -0.0126(18) -0.0033(16) -0.0021(17) C1 0.029(3) 0.023(3) 0.027(3) -0.012(3) -0.009(2) 0.006(3) C2 0.026(3) 0.032(3) 0.029(3) -0.015(3) -0.007(3) 0.001(3) C3 0.031(3) 0.023(3) 0.038(4) -0.014(3) -0.014(3) 0.001(3) C4 0.027(3) 0.030(3) 0.041(4) -0.020(3) -0.008(3) 0.001(3) C5 0.037(4) 0.025(3) 0.041(4) -0.018(3) -0.012(3) -0.002(3) C6 0.030(3) 0.027(3) 0.030(3) -0.009(3) -0.007(3) -0.002(3) C7 0.031(3) 0.031(3) 0.030(3) -0.013(3) -0.007(3) -0.003(3) C8 0.032(3) 0.031(3) 0.028(3) -0.016(3) -0.007(3) -0.004(3) C9 0.030(4) 0.035(4) 0.053(4) -0.022(3) -0.002(3) -0.010(3) C10 0.035(3) 0.022(3) 0.038(4) -0.019(3) -0.004(3) -0.001(3) C11 0.036(4) 0.037(4) 0.049(4) -0.030(3) -0.008(3) 0.000(3) C12 0.036(4) 0.038(4) 0.061(5) -0.036(4) -0.006(3) -0.004(3) C13 0.033(4) 0.030(3) 0.056(4) -0.027(3) -0.010(3) 0.003(3) C14 0.047(4) 0.052(5) 0.050(5) -0.036(4) -0.007(4) 0.006(4) C15 0.052(5) 0.071(6) 0.059(5) -0.050(5) -0.004(4) -0.005(4) C16 0.051(5) 0.050(5) 0.070(6) -0.045(4) -0.009(4) -0.007(4) C17 0.047(5) 0.040(4) 0.083(6) -0.046(4) 0.000(4) -0.002(4) C18 0.028(4) 0.039(4) 0.076(5) -0.036(4) -0.010(3) 0.003(3) C19 0.037(4) 0.045(4) 0.060(5) -0.036(4) 0.002(3) -0.004(3) C20 0.017(3) 0.029(3) 0.036(3) -0.021(3) -0.005(2) 0.000(2) C21 0.024(3) 0.027(3) 0.035(3) -0.020(3) -0.007(3) 0.002(3) C22 0.025(3) 0.040(4) 0.042(4) -0.024(3) -0.006(3) 0.001(3) C23 0.027(3) 0.041(4) 0.043(4) -0.028(3) -0.003(3) -0.001(3) C24 0.026(3) 0.035(4) 0.042(4) -0.022(3) -0.012(3) 0.004(3) C25 0.024(3) 0.037(3) 0.033(3) -0.024(3) -0.008(3) 0.006(3) C26 0.020(3) 0.033(3) 0.034(3) -0.018(3) -0.003(2) -0.004(3) C27 0.036(4) 0.025(3) 0.035(4) -0.016(3) -0.004(3) -0.005(3) C28 0.028(3) 0.033(3) 0.037(4) -0.022(3) -0.008(3) 0.001(3) C29 0.023(3) 0.048(4) 0.040(4) -0.017(3) 0.002(3) -0.004(3) C30 0.047(4) 0.040(4) 0.032(4) -0.025(3) -0.010(3) 0.003(3) C31 0.046(4) 0.055(5) 0.035(4) -0.028(4) -0.004(3) 0.000(4) C32 0.031(4) 0.048(4) 0.031(4) -0.013(3) -0.006(3) -0.003(3) C33 0.048(4) 0.030(4) 0.038(4) -0.011(3) -0.010(3) -0.009(3) C34 0.032(3) 0.034(4) 0.034(4) -0.016(3) -0.007(3) 0.003(3) C35 0.030(3) 0.046(4) 0.030(3) -0.016(3) -0.004(3) -0.006(3) C36 0.026(3) 0.049(4) 0.059(5) -0.027(4) -0.011(3) -0.002(3) C37 0.028(3) 0.031(3) 0.030(3) -0.013(3) -0.005(3) -0.001(3) C38 0.030(3) 0.037(4) 0.049(4) -0.024(3) -0.007(3) 0.004(3) C39 0.030(4) 0.037(4) 0.044(4) -0.018(3) -0.006(3) 0.001(3) C40 0.033(4) 0.046(4) 0.044(4) -0.018(3) -0.014(3) 0.007(3) C41 0.047(4) 0.025(3) 0.064(5) -0.022(3) -0.015(4) 0.001(3) C42 0.045(4) 0.022(3) 0.052(4) -0.010(3) -0.007(3) -0.007(3) C43 0.031(4) 0.033(4) 0.039(4) -0.013(3) -0.002(3) -0.004(3) C44 0.057(5) 0.036(4) 0.039(4) -0.004(3) -0.012(4) -0.008(4) C45 0.048(5) 0.043(4) 0.051(5) -0.011(4) -0.019(4) 0.004(4) C46 0.045(5) 0.028(4) 0.066(5) -0.007(4) -0.001(4) 0.000(3) C47 0.024(3) 0.027(3) 0.028(3) -0.013(3) -0.005(2) 0.000(2) C48 0.021(3) 0.032(3) 0.029(3) -0.016(3) -0.006(2) -0.001(3) C49 0.025(3) 0.035(3) 0.041(4) -0.023(3) -0.013(3) 0.003(3) C50 0.030(3) 0.036(4) 0.039(4) -0.026(3) -0.009(3) 0.009(3) C51 0.025(3) 0.025(3) 0.031(3) -0.013(3) -0.005(2) 0.000(2) C52 0.028(3) 0.024(3) 0.030(3) -0.014(3) -0.004(3) -0.001(3) C53 0.026(3) 0.032(3) 0.026(3) -0.016(3) -0.010(2) 0.001(3) C54 0.029(3) 0.025(3) 0.031(3) -0.015(3) -0.008(3) 0.000(3) C55 0.023(3) 0.032(3) 0.030(3) -0.015(3) -0.008(2) 0.002(3) C56 0.027(3) 0.032(3) 0.026(3) -0.014(3) -0.003(2) -0.005(3) C57 0.034(3) 0.031(3) 0.031(3) -0.016(3) -0.011(3) 0.001(3) C58 0.043(4) 0.034(3) 0.035(4) -0.020(3) -0.018(3) 0.000(3) C59 0.032(3) 0.038(4) 0.036(4) -0.019(3) -0.009(3) -0.008(3) C60 0.028(3) 0.035(3) 0.032(3) -0.014(3) -0.004(3) -0.013(3) C61 0.034(3) 0.027(3) 0.035(3) -0.013(3) -0.015(3) 0.000(3) C62 0.037(4) 0.032(3) 0.040(4) -0.023(3) -0.016(3) 0.001(3) C63 0.042(4) 0.041(4) 0.052(4) -0.028(4) -0.021(3) 0.013(3) C64 0.022(3) 0.030(3) 0.031(3) -0.017(3) -0.005(2) 0.003(3) C65 0.023(3) 0.028(3) 0.027(3) -0.014(3) -0.006(2) 0.002(3) C66 0.031(3) 0.029(3) 0.031(3) -0.019(3) -0.004(3) -0.002(3) C67 0.033(3) 0.024(3) 0.032(3) -0.014(3) -0.003(3) -0.001(3) C68 0.022(3) 0.028(3) 0.040(4) -0.018(3) -0.001(3) -0.001(3) C69 0.027(3) 0.027(3) 0.039(4) -0.018(3) -0.007(3) -0.004(3) C70 0.026(3) 0.035(4) 0.038(4) -0.021(3) -0.007(3) -0.003(3) C71 0.039(4) 0.035(4) 0.041(4) -0.022(3) -0.007(3) -0.009(3) C72 0.038(4) 0.020(3) 0.042(4) -0.015(3) -0.010(3) -0.003(3) C73 0.033(4) 0.030(3) 0.040(4) -0.016(3) -0.005(3) -0.006(3) C74 0.036(3) 0.027(3) 0.028(3) -0.017(3) -0.008(3) 0.000(3) C75 0.028(3) 0.025(3) 0.030(3) -0.015(3) -0.003(3) -0.004(3) C76 0.044(4) 0.035(4) 0.028(3) -0.017(3) -0.003(3) 0.001(3) C77 0.038(4) 0.046(4) 0.029(3) -0.025(3) -0.006(3) 0.002(3) C78 0.031(3) 0.033(3) 0.034(3) -0.016(3) -0.013(3) 0.004(3) C79 0.030(3) 0.028(3) 0.031(3) -0.015(3) -0.009(3) -0.002(3) C80 0.021(3) 0.031(3) 0.035(3) -0.021(3) -0.006(3) 0.001(3) C81 0.032(3) 0.032(3) 0.038(4) -0.023(3) -0.008(3) 0.000(3) C82 0.035(4) 0.039(4) 0.038(4) -0.024(3) -0.007(3) 0.002(3) C83 0.031(3) 0.035(4) 0.035(4) -0.020(3) -0.005(3) -0.003(3) C84 0.035(3) 0.030(3) 0.032(3) -0.018(3) -0.008(3) 0.005(3) C85 0.034(4) 0.047(4) 0.050(4) -0.034(4) -0.003(3) 0.002(3) C86 0.040(4) 0.048(4) 0.036(4) -0.027(3) -0.002(3) 0.001(3) C87 0.029(3) 0.049(4) 0.038(4) -0.019(3) -0.003(3) -0.006(3) C88 0.037(4) 0.042(4) 0.035(4) -0.023(3) -0.004(3) -0.009(3) C89 0.032(3) 0.041(4) 0.031(3) -0.019(3) -0.002(3) -0.004(3) C90 0.046(4) 0.077(6) 0.034(4) -0.033(4) -0.008(3) 0.013(4) C91 0.030(3) 0.035(3) 0.029(3) -0.018(3) -0.007(3) 0.000(3) C92 0.038(4) 0.030(3) 0.027(3) -0.011(3) -0.011(3) -0.003(3) C93 0.031(3) 0.031(3) 0.039(4) -0.017(3) -0.007(3) -0.002(3) C94 0.039(4) 0.045(4) 0.039(4) -0.020(3) -0.012(3) 0.003(3) C95 0.032(3) 0.033(3) 0.033(4) -0.016(3) -0.009(3) -0.003(3) C96 0.032(4) 0.033(4) 0.041(4) -0.016(3) -0.005(3) 0.002(3) C97 0.037(4) 0.032(4) 0.051(4) -0.023(3) -0.008(3) 0.002(3) C98 0.034(4) 0.040(4) 0.055(5) -0.014(4) -0.011(3) 0.003(3) C99 0.030(4) 0.053(5) 0.048(4) -0.018(4) -0.017(3) 0.000(3) C100 0.033(4) 0.045(4) 0.056(5) -0.026(4) -0.011(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O2 1.704(4) . ? Nb1 O4 1.928(4) . ? Nb1 O3 1.968(4) . ? Nb1 O1 2.058(4) . ? Nb1 C1 2.377(6) . ? Nb1 Nb2 3.0481(11) . ? Nb2 O1 1.850(4) . ? Nb2 O5 1.896(4) . ? Nb2 O6 1.899(4) . ? Nb2 C1 1.968(6) . ? O3 C3 1.354(7) . ? O4 C20 1.385(6) . ? O5 C47 1.410(7) . ? O6 C74 1.400(7) . ? C1 C2 1.374(8) . ? C2 C8 1.459(8) . ? C2 H1 0.96(7) . ? C3 C8 1.406(8) . ? C3 C4 1.426(8) . ? C4 C5 1.404(8) . ? C4 C10 1.540(8) . ? C5 C6 1.407(9) . ? C5 H2 0.9500 . ? C6 C7 1.388(8) . ? C6 C9 1.522(8) . ? C7 C8 1.416(8) . ? C7 H3 0.9500 . ? C9 H4 0.9800 . ? C9 H5 0.9800 . ? C9 H6 0.9800 . ? C10 C13 1.519(9) . ? C10 C11 1.559(9) . ? C10 C12 1.560(8) . ? C11 C14 1.534(9) . ? C11 H7 0.9900 . ? C11 H8 0.9900 . ? C12 C16 1.536(9) . ? C12 H9 0.9900 . ? C12 H10 0.9900 . ? C13 C18 1.545(9) . ? C13 H11 0.9900 . ? C13 H12 0.9900 . ? C14 C19 1.521(10) . ? C14 C15 1.539(10) . ? C14 H13 1.0000 . ? C15 C16 1.519(11) . ? C15 H14 0.9900 . ? C15 H15 0.9900 . ? C16 C17 1.539(10) . ? C16 H16 1.0000 . ? C17 C18 1.533(9) . ? C17 H17 0.9900 . ? C17 H18 0.9900 . ? C18 C19 1.543(10) . ? C18 H19 1.0000 . ? C19 H20 0.9900 . ? C19 H21 0.9900 . ? C20 C25 1.422(8) . ? C20 C21 1.424(8) . ? C21 C22 1.408(8) . ? C21 C26 1.557(8) . ? C22 C23 1.377(9) . ? C22 H22 0.9500 . ? C23 C24 1.394(9) . ? C23 C36 1.517(8) . ? C24 C25 1.412(8) . ? C24 H23 0.9500 . ? C25 C37 1.554(8) . ? C26 C28 1.555(8) . ? C26 C27 1.562(8) . ? C26 C29 1.565(8) . ? C27 C30 1.547(9) . ? C27 H24 0.9900 . ? C27 H25 0.9900 . ? C28 C34 1.536(8) . ? C28 H26 0.9900 . ? C28 H27 0.9900 . ? C29 C32 1.541(9) . ? C29 H28 0.9900 . ? C29 H29 0.9900 . ? C30 C31 1.533(9) . ? C30 C35 1.534(9) . ? C30 H30 1.0000 . ? C31 C32 1.543(9) . ? C31 H31 0.9900 . ? C31 H32 0.9900 . ? C32 C33 1.534(9) . ? C32 H33 1.0000 . ? C33 C34 1.527(9) . ? C33 H34 0.9900 . ? C33 H35 0.9900 . ? C34 C35 1.564(9) . ? C34 H36 1.0000 . ? C35 H37 0.9900 . ? C35 H38 0.9900 . ? C36 H39 0.9800 . ? C36 H40 0.9800 . ? C36 H41 0.9800 . ? C37 C38 1.544(9) . ? C37 C40 1.544(8) . ? C37 C39 1.551(8) . ? C38 C41 1.522(9) . ? C38 H42 0.9900 . ? C38 H43 0.9900 . ? C39 C43 1.548(9) . ? C39 H44 0.9900 . ? C39 H45 0.9900 . ? C40 C45 1.536(10) . ? C40 H46 0.9900 . ? C40 H47 0.9900 . ? C41 C42 1.546(10) . ? C41 C46 1.548(10) . ? C41 H48 1.0000 . ? C42 C43 1.516(9) . ? C42 H49 0.9900 . ? C42 H50 0.9900 . ? C43 C44 1.535(9) . ? C43 H51 1.0000 . ? C44 C45 1.521(10) . ? C44 H52 0.9900 . ? C44 H53 0.9900 . ? C45 C46 1.527(11) . ? C45 H54 1.0000 . ? C46 H55 0.9900 . ? C46 H56 0.9900 . ? C47 C52 1.412(8) . ? C47 C48 1.416(8) . ? C48 C49 1.412(8) . ? C48 C53 1.556(8) . ? C49 C50 1.384(8) . ? C49 H57 0.9500 . ? C50 C51 1.399(8) . ? C50 C63 1.506(8) . ? C51 C52 1.402(8) . ? C51 H58 0.9500 . ? C52 C64 1.581(8) . ? C53 C55 1.543(8) . ? C53 C54 1.545(8) . ? C53 C56 1.559(8) . ? C54 C57 1.538(8) . ? C54 H59 0.9900 . ? C54 H60 0.9900 . ? C55 C59 1.548(8) . ? C55 H61 0.9900 . ? C55 H62 0.9900 . ? C56 C61 1.544(8) . ? C56 H63 0.9900 . ? C56 H64 0.9900 . ? C57 C58 1.526(8) . ? C57 C62 1.528(8) . ? C57 H65 1.0000 . ? C58 C59 1.540(9) . ? C58 H66 0.9900 . ? C58 H67 0.9900 . ? C59 C60 1.540(8) . ? C59 H68 1.0000 . ? C60 C61 1.541(8) . ? C60 H69 0.9900 . ? C60 H70 0.9900 . ? C61 C62 1.545(9) . ? C61 H71 1.0000 . ? C62 H72 0.9900 . ? C62 H73 0.9900 . ? C63 H74 0.9800 . ? C63 H75 0.9800 . ? C63 H76 0.9800 . ? C64 C66 1.540(8) . ? C64 C67 1.555(8) . ? C64 C65 1.562(8) . ? C65 C68 1.541(8) . ? C65 H77 0.9900 . ? C65 H78 0.9900 . ? C66 C70 1.536(8) . ? C66 H79 0.9900 . ? C66 H80 0.9900 . ? C67 C72 1.528(8) . ? C67 H81 0.9900 . ? C67 H82 0.9900 . ? C68 C69 1.529(8) . ? C68 C73 1.541(8) . ? C68 H83 1.0000 . ? C69 C70 1.543(8) . ? C69 H84 0.9900 . ? C69 H85 0.9900 . ? C70 C71 1.521(8) . ? C70 H86 1.0000 . ? C71 C72 1.528(9) . ? C71 H87 0.9900 . ? C71 H88 0.9900 . ? C72 C73 1.545(9) . ? C72 H89 1.0000 . ? C73 H90 0.9900 . ? C73 H91 0.9900 . ? C74 C79 1.419(8) . ? C74 C75 1.440(8) . ? C75 C76 1.396(8) . ? C75 C80 1.551(8) . ? C76 C77 1.382(9) . ? C76 H92 0.9500 . ? C77 C78 1.397(8) . ? C77 C90 1.507(9) . ? C78 C79 1.401(8) . ? C78 H93 0.9500 . ? C79 C91 1.552(8) . ? C80 C81 1.549(8) . ? C80 C82 1.554(8) . ? C80 C83 1.569(8) . ? C81 C84 1.542(8) . ? C81 H94 0.9900 . ? C81 H95 0.9900 . ? C82 C86 1.538(9) . ? C82 H96 0.9900 . ? C82 H97 0.9900 . ? C83 C88 1.557(9) . ? C83 H98 0.9900 . ? C83 H99 0.9900 . ? C84 C85 1.515(8) . ? C84 C89 1.540(8) . ? C84 H100 1.0000 . ? C85 C86 1.538(9) . ? C85 H101 0.9900 . ? C85 H102 0.9900 . ? C86 C87 1.533(9) . ? C86 H103 1.0000 . ? C87 C88 1.537(9) . ? C87 H104 0.9900 . ? C87 H105 0.9900 . ? C88 C89 1.521(9) . ? C88 H106 1.0000 . ? C89 H107 0.9900 . ? C89 H108 0.9900 . ? C90 H109 0.9800 . ? C90 H110 0.9800 . ? C90 H111 0.9800 . ? C91 C93 1.541(8) . ? C91 C92 1.542(8) . ? C91 C94 1.555(8) . ? C92 C95 1.528(8) . ? C92 H112 0.9900 . ? C92 H113 0.9900 . ? C93 C97 1.559(9) . ? C93 H114 0.9900 . ? C93 H115 0.9900 . ? C94 C99 1.532(9) . ? C94 H116 0.9900 . ? C94 H117 0.9900 . ? C95 C100 1.535(9) . ? C95 C96 1.538(9) . ? C95 H118 1.0000 . ? C96 C97 1.541(9) . ? C96 H119 0.9900 . ? C96 H120 0.9900 . ? C97 C98 1.529(10) . ? C97 H121 1.0000 . ? C98 C99 1.539(10) . ? C98 H122 0.9900 . ? C98 H123 0.9900 . ? C99 C100 1.551(10) . ? C99 H124 1.0000 . ? C100 H125 0.9900 . ? C100 H126 0.9900 . ? C101 C102 1.423(15) . ? C101 H127 0.9800 . ? C101 H128 0.9800 . ? C101 H129 0.9800 . ? C102 C103 1.438(15) . ? C102 H130 0.9900 . ? C102 H131 0.9900 . ? C103 C104 1.540(15) . ? C103 H132 0.9900 . ? C103 H133 0.9900 . ? C104 C105 1.55(2) . ? C104 H134 0.9900 . ? C104 H135 0.9900 . ? C105 C106 1.61(2) . ? C105 H136 0.9900 . ? C105 H137 0.9900 . ? C106 H138 0.9800 . ? C106 H139 0.9800 . ? C106 H140 0.9800 . ? C107 C108 1.65(3) . ? C107 H141 0.9800 . ? C107 H142 0.9800 . ? C107 H143 0.9800 . ? C108 C109 1.404(16) . ? C108 H144 0.9900 . ? C108 H145 0.9900 . ? C109 C110 1.60(2) . ? C109 H146 0.9900 . ? C109 H147 0.9900 . ? C110 C111 1.392(17) . ? C110 H148 0.9900 . ? C110 H149 0.9900 . ? C111 C112 1.595(16) . ? C111 H150 0.9900 . ? C111 H151 0.9900 . ? C112 H152 0.9800 . ? C112 H153 0.9800 . ? C112 H154 0.9800 . ? C113 C114 1.3900 . ? C113 C118 1.3900 . ? C113 H155 0.9500 . ? C114 C115 1.3900 . ? C114 H156 0.9500 . ? C115 C116 1.3900 . ? C115 H157 0.9500 . ? C116 C117 1.3900 . ? C116 H158 0.9500 . ? C117 C118 1.3900 . ? C117 H159 0.9500 . ? C118 H160 0.9500 . ? C119 C120 1.506(15) . ? C119 H161 0.9800 . ? C119 H162 0.9800 . ? C119 H163 0.9800 . ? C120 C121 1.486(15) . ? C120 H164 0.9900 . ? C120 H165 0.9900 . ? C121 C121 1.57(2) 2_655 ? C121 H166 0.9900 . ? C121 H167 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O4 110.34(19) . . ? O2 Nb1 O3 99.75(19) . . ? O4 Nb1 O3 97.82(17) . . ? O2 Nb1 O1 98.03(18) . . ? O4 Nb1 O1 96.17(16) . . ? O3 Nb1 O1 151.90(16) . . ? O2 Nb1 C1 104.1(2) . . ? O4 Nb1 C1 145.38(18) . . ? O3 Nb1 C1 79.54(18) . . ? O1 Nb1 C1 75.12(18) . . ? O2 Nb1 Nb2 95.88(14) . . ? O4 Nb1 Nb2 129.64(12) . . ? O3 Nb1 Nb2 119.74(12) . . ? O1 Nb1 Nb2 36.34(11) . . ? C1 Nb1 Nb2 40.21(14) . . ? O1 Nb2 O5 109.65(17) . . ? O1 Nb2 O6 110.41(17) . . ? O5 Nb2 O6 123.19(17) . . ? O1 Nb2 C1 90.6(2) . . ? O5 Nb2 C1 107.8(2) . . ? O6 Nb2 C1 110.3(2) . . ? O1 Nb2 Nb1 41.25(12) . . ? O5 Nb2 Nb1 106.83(12) . . ? O6 Nb2 Nb1 129.83(12) . . ? C1 Nb2 Nb1 51.23(17) . . ? Nb2 O1 Nb1 102.40(17) . . ? C3 O3 Nb1 142.1(4) . . ? C20 O4 Nb1 158.8(4) . . ? C47 O5 Nb2 164.8(4) . . ? C74 O6 Nb2 169.3(4) . . ? C2 C1 Nb2 150.3(5) . . ? C2 C1 Nb1 121.1(4) . . ? Nb2 C1 Nb1 88.6(2) . . ? C1 C2 C8 129.6(6) . . ? C1 C2 H1 119(4) . . ? C8 C2 H1 111(4) . . ? O3 C3 C8 118.8(5) . . ? O3 C3 C4 119.8(5) . . ? C8 C3 C4 121.3(6) . . ? C5 C4 C3 115.7(6) . . ? C5 C4 C10 121.3(5) . . ? C3 C4 C10 122.9(5) . . ? C4 C5 C6 124.6(6) . . ? C4 C5 H2 117.7 . . ? C6 C5 H2 117.7 . . ? C7 C6 C5 117.6(6) . . ? C7 C6 C9 122.7(6) . . ? C5 C6 C9 119.7(6) . . ? C6 C7 C8 120.9(6) . . ? C6 C7 H3 119.5 . . ? C8 C7 H3 119.5 . . ? C3 C8 C7 119.6(5) . . ? C3 C8 C2 121.7(5) . . ? C7 C8 C2 118.4(6) . . ? C6 C9 H4 109.5 . . ? C6 C9 H5 109.5 . . ? H4 C9 H5 109.5 . . ? C6 C9 H6 109.5 . . ? H4 C9 H6 109.5 . . ? H5 C9 H6 109.5 . . ? C13 C10 C4 111.2(5) . . ? C13 C10 C11 108.9(5) . . ? C4 C10 C11 109.8(5) . . ? C13 C10 C12 108.2(5) . . ? C4 C10 C12 112.0(5) . . ? C11 C10 C12 106.4(5) . . ? C14 C11 C10 110.4(5) . . ? C14 C11 H7 109.6 . . ? C10 C11 H7 109.6 . . ? C14 C11 H8 109.6 . . ? C10 C11 H8 109.6 . . ? H7 C11 H8 108.1 . . ? C16 C12 C10 110.5(5) . . ? C16 C12 H9 109.6 . . ? C10 C12 H9 109.6 . . ? C16 C12 H10 109.6 . . ? C10 C12 H10 109.6 . . ? H9 C12 H10 108.1 . . ? C10 C13 C18 112.3(6) . . ? C10 C13 H11 109.1 . . ? C18 C13 H11 109.1 . . ? C10 C13 H12 109.1 . . ? C18 C13 H12 109.1 . . ? H11 C13 H12 107.9 . . ? C19 C14 C11 110.3(6) . . ? C19 C14 C15 109.4(6) . . ? C11 C14 C15 109.6(6) . . ? C19 C14 H13 109.1 . . ? C11 C14 H13 109.1 . . ? C15 C14 H13 109.1 . . ? C16 C15 C14 108.7(6) . . ? C16 C15 H14 110.0 . . ? C14 C15 H14 110.0 . . ? C16 C15 H15 110.0 . . ? C14 C15 H15 110.0 . . ? H14 C15 H15 108.3 . . ? C15 C16 C12 110.6(6) . . ? C15 C16 C17 109.6(6) . . ? C12 C16 C17 109.5(6) . . ? C15 C16 H16 109.0 . . ? C12 C16 H16 109.0 . . ? C17 C16 H16 109.0 . . ? C18 C17 C16 109.5(6) . . ? C18 C17 H17 109.8 . . ? C16 C17 H17 109.8 . . ? C18 C17 H18 109.8 . . ? C16 C17 H18 109.8 . . ? H17 C17 H18 108.2 . . ? C17 C18 C19 109.0(6) . . ? C17 C18 C13 109.0(6) . . ? C19 C18 C13 108.4(5) . . ? C17 C18 H19 110.2 . . ? C19 C18 H19 110.2 . . ? C13 C18 H19 110.2 . . ? C14 C19 C18 109.9(6) . . ? C14 C19 H20 109.7 . . ? C18 C19 H20 109.7 . . ? C14 C19 H21 109.7 . . ? C18 C19 H21 109.7 . . ? H20 C19 H21 108.2 . . ? O4 C20 C25 119.3(5) . . ? O4 C20 C21 119.3(5) . . ? C25 C20 C21 121.4(5) . . ? C22 C21 C20 116.4(6) . . ? C22 C21 C26 119.6(5) . . ? C20 C21 C26 123.9(5) . . ? C23 C22 C21 123.6(6) . . ? C23 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? C22 C23 C24 118.1(6) . . ? C22 C23 C36 121.3(6) . . ? C24 C23 C36 120.7(6) . . ? C23 C24 C25 122.5(6) . . ? C23 C24 H23 118.8 . . ? C25 C24 H23 118.8 . . ? C24 C25 C20 116.9(6) . . ? C24 C25 C37 118.4(5) . . ? C20 C25 C37 124.5(5) . . ? C28 C26 C21 113.9(5) . . ? C28 C26 C27 108.8(5) . . ? C21 C26 C27 110.6(5) . . ? C28 C26 C29 105.9(5) . . ? C21 C26 C29 111.1(5) . . ? C27 C26 C29 106.0(5) . . ? C30 C27 C26 111.7(5) . . ? C30 C27 H24 109.3 . . ? C26 C27 H24 109.3 . . ? C30 C27 H25 109.3 . . ? C26 C27 H25 109.3 . . ? H24 C27 H25 107.9 . . ? C34 C28 C26 111.5(5) . . ? C34 C28 H26 109.3 . . ? C26 C28 H26 109.3 . . ? C34 C28 H27 109.3 . . ? C26 C28 H27 109.3 . . ? H26 C28 H27 108.0 . . ? C32 C29 C26 112.5(5) . . ? C32 C29 H28 109.1 . . ? C26 C29 H28 109.1 . . ? C32 C29 H29 109.1 . . ? C26 C29 H29 109.1 . . ? H28 C29 H29 107.8 . . ? C31 C30 C35 110.9(6) . . ? C31 C30 C27 109.8(6) . . ? C35 C30 C27 109.3(5) . . ? C31 C30 H30 109.0 . . ? C35 C30 H30 109.0 . . ? C27 C30 H30 109.0 . . ? C30 C31 C32 108.1(5) . . ? C30 C31 H31 110.1 . . ? C32 C31 H31 110.1 . . ? C30 C31 H32 110.1 . . ? C32 C31 H32 110.1 . . ? H31 C31 H32 108.4 . . ? C33 C32 C29 108.3(6) . . ? C33 C32 C31 110.0(5) . . ? C29 C32 C31 109.9(6) . . ? C33 C32 H33 109.5 . . ? C29 C32 H33 109.5 . . ? C31 C32 H33 109.5 . . ? C34 C33 C32 110.4(5) . . ? C34 C33 H34 109.6 . . ? C32 C33 H34 109.6 . . ? C34 C33 H35 109.6 . . ? C32 C33 H35 109.6 . . ? H34 C33 H35 108.1 . . ? C33 C34 C28 109.7(5) . . ? C33 C34 C35 108.1(5) . . ? C28 C34 C35 110.1(5) . . ? C33 C34 H36 109.6 . . ? C28 C34 H36 109.6 . . ? C35 C34 H36 109.6 . . ? C30 C35 C34 109.0(5) . . ? C30 C35 H37 109.9 . . ? C34 C35 H37 109.9 . . ? C30 C35 H38 109.9 . . ? C34 C35 H38 109.9 . . ? H37 C35 H38 108.3 . . ? C23 C36 H39 109.5 . . ? C23 C36 H40 109.5 . . ? H39 C36 H40 109.5 . . ? C23 C36 H41 109.5 . . ? H39 C36 H41 109.5 . . ? H40 C36 H41 109.5 . . ? C38 C37 C40 107.2(5) . . ? C38 C37 C39 108.6(5) . . ? C40 C37 C39 106.0(5) . . ? C38 C37 C25 107.9(5) . . ? C40 C37 C25 112.1(5) . . ? C39 C37 C25 114.8(5) . . ? C41 C38 C37 111.9(6) . . ? C41 C38 H42 109.2 . . ? C37 C38 H42 109.2 . . ? C41 C38 H43 109.2 . . ? C37 C38 H43 109.2 . . ? H42 C38 H43 107.9 . . ? C43 C39 C37 111.3(5) . . ? C43 C39 H44 109.4 . . ? C37 C39 H44 109.4 . . ? C43 C39 H45 109.4 . . ? C37 C39 H45 109.4 . . ? H44 C39 H45 108.0 . . ? C45 C40 C37 112.2(6) . . ? C45 C40 H46 109.2 . . ? C37 C40 H46 109.2 . . ? C45 C40 H47 109.2 . . ? C37 C40 H47 109.2 . . ? H46 C40 H47 107.9 . . ? C38 C41 C42 110.0(5) . . ? C38 C41 C46 109.4(6) . . ? C42 C41 C46 108.7(6) . . ? C38 C41 H48 109.6 . . ? C42 C41 H48 109.6 . . ? C46 C41 H48 109.6 . . ? C43 C42 C41 109.5(6) . . ? C43 C42 H49 109.8 . . ? C41 C42 H49 109.8 . . ? C43 C42 H50 109.8 . . ? C41 C42 H50 109.8 . . ? H49 C42 H50 108.2 . . ? C42 C43 C44 109.8(6) . . ? C42 C43 C39 110.1(6) . . ? C44 C43 C39 108.6(5) . . ? C42 C43 H51 109.4 . . ? C44 C43 H51 109.4 . . ? C39 C43 H51 109.4 . . ? C45 C44 C43 109.4(6) . . ? C45 C44 H52 109.8 . . ? C43 C44 H52 109.8 . . ? C45 C44 H53 109.8 . . ? C43 C44 H53 109.8 . . ? H52 C44 H53 108.2 . . ? C44 C45 C46 109.9(6) . . ? C44 C45 C40 109.2(6) . . ? C46 C45 C40 109.5(6) . . ? C44 C45 H54 109.4 . . ? C46 C45 H54 109.4 . . ? C40 C45 H54 109.4 . . ? C45 C46 C41 109.0(6) . . ? C45 C46 H55 109.9 . . ? C41 C46 H55 109.9 . . ? C45 C46 H56 109.9 . . ? C41 C46 H56 109.9 . . ? H55 C46 H56 108.3 . . ? O5 C47 C52 118.8(5) . . ? O5 C47 C48 120.0(5) . . ? C52 C47 C48 121.3(5) . . ? C49 C48 C47 116.9(5) . . ? C49 C48 C53 118.4(5) . . ? C47 C48 C53 124.3(5) . . ? C50 C49 C48 123.5(6) . . ? C50 C49 H57 118.3 . . ? C48 C49 H57 118.3 . . ? C49 C50 C51 116.6(6) . . ? C49 C50 C63 120.9(6) . . ? C51 C50 C63 122.3(6) . . ? C50 C51 C52 123.5(6) . . ? C50 C51 H58 118.2 . . ? C52 C51 H58 118.2 . . ? C51 C52 C47 117.0(5) . . ? C51 C52 C64 118.0(5) . . ? C47 C52 C64 124.2(5) . . ? C55 C53 C54 107.6(5) . . ? C55 C53 C48 111.5(5) . . ? C54 C53 C48 108.9(5) . . ? C55 C53 C56 106.1(5) . . ? C54 C53 C56 109.9(5) . . ? C48 C53 C56 112.6(5) . . ? C57 C54 C53 111.5(5) . . ? C57 C54 H59 109.3 . . ? C53 C54 H59 109.3 . . ? C57 C54 H60 109.3 . . ? C53 C54 H60 109.3 . . ? H59 C54 H60 108.0 . . ? C53 C55 C59 111.8(5) . . ? C53 C55 H61 109.3 . . ? C59 C55 H61 109.3 . . ? C53 C55 H62 109.3 . . ? C59 C55 H62 109.3 . . ? H61 C55 H62 107.9 . . ? C61 C56 C53 110.6(5) . . ? C61 C56 H63 109.5 . . ? C53 C56 H63 109.5 . . ? C61 C56 H64 109.5 . . ? C53 C56 H64 109.5 . . ? H63 C56 H64 108.1 . . ? C58 C57 C62 109.6(5) . . ? C58 C57 C54 109.3(5) . . ? C62 C57 C54 108.5(5) . . ? C58 C57 H65 109.8 . . ? C62 C57 H65 109.8 . . ? C54 C57 H65 109.8 . . ? C57 C58 C59 110.0(5) . . ? C57 C58 H66 109.7 . . ? C59 C58 H66 109.7 . . ? C57 C58 H67 109.7 . . ? C59 C58 H67 109.7 . . ? H66 C58 H67 108.2 . . ? C60 C59 C58 109.8(5) . . ? C60 C59 C55 109.4(5) . . ? C58 C59 C55 108.5(5) . . ? C60 C59 H68 109.7 . . ? C58 C59 H68 109.7 . . ? C55 C59 H68 109.7 . . ? C59 C60 C61 109.1(5) . . ? C59 C60 H69 109.9 . . ? C61 C60 H69 109.9 . . ? C59 C60 H70 109.9 . . ? C61 C60 H70 109.9 . . ? H69 C60 H70 108.3 . . ? C60 C61 C56 108.8(5) . . ? C60 C61 C62 109.0(5) . . ? C56 C61 C62 109.9(5) . . ? C60 C61 H71 109.7 . . ? C56 C61 H71 109.7 . . ? C62 C61 H71 109.7 . . ? C57 C62 C61 110.8(5) . . ? C57 C62 H72 109.5 . . ? C61 C62 H72 109.5 . . ? C57 C62 H73 109.5 . . ? C61 C62 H73 109.5 . . ? H72 C62 H73 108.1 . . ? C50 C63 H74 109.5 . . ? C50 C63 H75 109.5 . . ? H74 C63 H75 109.5 . . ? C50 C63 H76 109.5 . . ? H74 C63 H76 109.5 . . ? H75 C63 H76 109.5 . . ? C66 C64 C67 107.8(5) . . ? C66 C64 C65 109.3(5) . . ? C67 C64 C65 106.6(5) . . ? C66 C64 C52 114.9(5) . . ? C67 C64 C52 110.2(5) . . ? C65 C64 C52 107.7(5) . . ? C68 C65 C64 110.8(5) . . ? C68 C65 H77 109.5 . . ? C64 C65 H77 109.5 . . ? C68 C65 H78 109.5 . . ? C64 C65 H78 109.5 . . ? H77 C65 H78 108.1 . . ? C70 C66 C64 109.8(5) . . ? C70 C66 H79 109.7 . . ? C64 C66 H79 109.7 . . ? C70 C66 H80 109.7 . . ? C64 C66 H80 109.7 . . ? H79 C66 H80 108.2 . . ? C72 C67 C64 112.3(5) . . ? C72 C67 H81 109.2 . . ? C64 C67 H81 109.2 . . ? C72 C67 H82 109.2 . . ? C64 C67 H82 109.2 . . ? H81 C67 H82 107.9 . . ? C69 C68 C73 109.9(5) . . ? C69 C68 C65 109.0(5) . . ? C73 C68 C65 109.4(5) . . ? C69 C68 H83 109.5 . . ? C73 C68 H83 109.5 . . ? C65 C68 H83 109.5 . . ? C68 C69 C70 109.7(5) . . ? C68 C69 H84 109.7 . . ? C70 C69 H84 109.7 . . ? C68 C69 H85 109.7 . . ? C70 C69 H85 109.7 . . ? H84 C69 H85 108.2 . . ? C71 C70 C66 110.5(5) . . ? C71 C70 C69 108.9(5) . . ? C66 C70 C69 110.1(5) . . ? C71 C70 H86 109.1 . . ? C66 C70 H86 109.1 . . ? C69 C70 H86 109.1 . . ? C70 C71 C72 109.9(5) . . ? C70 C71 H87 109.7 . . ? C72 C71 H87 109.7 . . ? C70 C71 H88 109.7 . . ? C72 C71 H88 109.7 . . ? H87 C71 H88 108.2 . . ? C71 C72 C67 108.8(5) . . ? C71 C72 C73 110.0(5) . . ? C67 C72 C73 108.6(5) . . ? C71 C72 H89 109.8 . . ? C67 C72 H89 109.8 . . ? C73 C72 H89 109.8 . . ? C68 C73 C72 109.0(5) . . ? C68 C73 H90 109.9 . . ? C72 C73 H90 109.9 . . ? C68 C73 H91 109.9 . . ? C72 C73 H91 109.9 . . ? H90 C73 H91 108.3 . . ? O6 C74 C79 120.7(5) . . ? O6 C74 C75 117.9(5) . . ? C79 C74 C75 121.3(5) . . ? C76 C75 C74 116.5(6) . . ? C76 C75 C80 118.0(5) . . ? C74 C75 C80 125.5(5) . . ? C77 C76 C75 123.7(6) . . ? C77 C76 H92 118.1 . . ? C75 C76 H92 118.1 . . ? C76 C77 C78 117.7(6) . . ? C76 C77 C90 122.0(6) . . ? C78 C77 C90 120.2(6) . . ? C77 C78 C79 123.1(6) . . ? C77 C78 H93 118.5 . . ? C79 C78 H93 118.5 . . ? C78 C79 C74 116.9(6) . . ? C78 C79 C91 118.3(5) . . ? C74 C79 C91 124.7(5) . . ? C81 C80 C75 111.1(5) . . ? C81 C80 C82 107.0(5) . . ? C75 C80 C82 110.8(5) . . ? C81 C80 C83 109.2(5) . . ? C75 C80 C83 112.1(5) . . ? C82 C80 C83 106.4(5) . . ? C84 C81 C80 111.5(5) . . ? C84 C81 H94 109.3 . . ? C80 C81 H94 109.3 . . ? C84 C81 H95 109.3 . . ? C80 C81 H95 109.3 . . ? H94 C81 H95 108.0 . . ? C86 C82 C80 112.4(5) . . ? C86 C82 H96 109.1 . . ? C80 C82 H96 109.1 . . ? C86 C82 H97 109.1 . . ? C80 C82 H97 109.1 . . ? H96 C82 H97 107.9 . . ? C88 C83 C80 109.6(5) . . ? C88 C83 H98 109.7 . . ? C80 C83 H98 109.7 . . ? C88 C83 H99 109.7 . . ? C80 C83 H99 109.7 . . ? H98 C83 H99 108.2 . . ? C85 C84 C89 109.4(5) . . ? C85 C84 C81 110.1(5) . . ? C89 C84 C81 108.4(5) . . ? C85 C84 H100 109.6 . . ? C89 C84 H100 109.6 . . ? C81 C84 H100 109.6 . . ? C84 C85 C86 109.2(5) . . ? C84 C85 H101 109.8 . . ? C86 C85 H101 109.8 . . ? C84 C85 H102 109.8 . . ? C86 C85 H102 109.8 . . ? H101 C85 H102 108.3 . . ? C87 C86 C85 110.7(6) . . ? C87 C86 C82 108.2(5) . . ? C85 C86 C82 109.4(6) . . ? C87 C86 H103 109.5 . . ? C85 C86 H103 109.5 . . ? C82 C86 H103 109.5 . . ? C86 C87 C88 109.1(5) . . ? C86 C87 H104 109.9 . . ? C88 C87 H104 109.9 . . ? C86 C87 H105 109.9 . . ? C88 C87 H105 109.9 . . ? H104 C87 H105 108.3 . . ? C89 C88 C87 109.3(6) . . ? C89 C88 C83 109.7(5) . . ? C87 C88 C83 109.7(5) . . ? C89 C88 H106 109.3 . . ? C87 C88 H106 109.3 . . ? C83 C88 H106 109.3 . . ? C88 C89 C84 110.9(5) . . ? C88 C89 H107 109.5 . . ? C84 C89 H107 109.5 . . ? C88 C89 H108 109.5 . . ? C84 C89 H108 109.5 . . ? H107 C89 H108 108.1 . . ? C77 C90 H109 109.5 . . ? C77 C90 H110 109.5 . . ? H109 C90 H110 109.5 . . ? C77 C90 H111 109.5 . . ? H109 C90 H111 109.5 . . ? H110 C90 H111 109.5 . . ? C93 C91 C92 109.2(5) . . ? C93 C91 C79 111.7(5) . . ? C92 C91 C79 110.6(5) . . ? C93 C91 C94 106.8(5) . . ? C92 C91 C94 107.2(5) . . ? C79 C91 C94 111.1(5) . . ? C95 C92 C91 112.1(5) . . ? C95 C92 H112 109.2 . . ? C91 C92 H112 109.2 . . ? C95 C92 H113 109.2 . . ? C91 C92 H113 109.2 . . ? H112 C92 H113 107.9 . . ? C91 C93 C97 110.5(5) . . ? C91 C93 H114 109.5 . . ? C97 C93 H114 109.5 . . ? C91 C93 H115 109.5 . . ? C97 C93 H115 109.5 . . ? H114 C93 H115 108.1 . . ? C99 C94 C91 111.9(5) . . ? C99 C94 H116 109.2 . . ? C91 C94 H116 109.2 . . ? C99 C94 H117 109.2 . . ? C91 C94 H117 109.2 . . ? H116 C94 H117 107.9 . . ? C92 C95 C100 109.6(5) . . ? C92 C95 C96 109.1(5) . . ? C100 C95 C96 108.9(5) . . ? C92 C95 H118 109.7 . . ? C100 C95 H118 109.7 . . ? C96 C95 H118 109.7 . . ? C95 C96 C97 110.2(6) . . ? C95 C96 H119 109.6 . . ? C97 C96 H119 109.6 . . ? C95 C96 H120 109.6 . . ? C97 C96 H120 109.6 . . ? H119 C96 H120 108.1 . . ? C98 C97 C96 108.9(6) . . ? C98 C97 C93 110.1(6) . . ? C96 C97 C93 109.3(5) . . ? C98 C97 H121 109.5 . . ? C96 C97 H121 109.5 . . ? C93 C97 H121 109.5 . . ? C97 C98 C99 109.2(6) . . ? C97 C98 H122 109.8 . . ? C99 C98 H122 109.8 . . ? C97 C98 H123 109.8 . . ? C99 C98 H123 109.8 . . ? H122 C98 H123 108.3 . . ? C94 C99 C98 109.5(6) . . ? C94 C99 C100 109.4(6) . . ? C98 C99 C100 109.1(6) . . ? C94 C99 H124 109.6 . . ? C98 C99 H124 109.6 . . ? C100 C99 H124 109.6 . . ? C95 C100 C99 109.2(5) . . ? C95 C100 H125 109.8 . . ? C99 C100 H125 109.8 . . ? C95 C100 H126 109.8 . . ? C99 C100 H126 109.8 . . ? H125 C100 H126 108.3 . . ? C102 C101 H127 109.5 . . ? C102 C101 H128 109.5 . . ? H127 C101 H128 109.5 . . ? C102 C101 H129 109.5 . . ? H127 C101 H129 109.5 . . ? H128 C101 H129 109.5 . . ? C101 C102 C103 115.9(13) . . ? C101 C102 H130 108.3 . . ? C103 C102 H130 108.3 . . ? C101 C102 H131 108.3 . . ? C103 C102 H131 108.3 . . ? H130 C102 H131 107.4 . . ? C102 C103 C104 114.6(12) . . ? C102 C103 H132 108.6 . . ? C104 C103 H132 108.6 . . ? C102 C103 H133 108.6 . . ? C104 C103 H133 108.6 . . ? H132 C103 H133 107.6 . . ? C103 C104 C105 112.5(13) . . ? C103 C104 H134 109.1 . . ? C105 C104 H134 109.1 . . ? C103 C104 H135 109.1 . . ? C105 C104 H135 109.1 . . ? H134 C104 H135 107.8 . . ? C104 C105 C106 105.0(16) . . ? C104 C105 H136 110.8 . . ? C106 C105 H136 110.8 . . ? C104 C105 H137 110.8 . . ? C106 C105 H137 110.8 . . ? H136 C105 H137 108.8 . . ? C105 C106 H138 109.5 . . ? C105 C106 H139 109.5 . . ? H138 C106 H139 109.5 . . ? C105 C106 H140 109.5 . . ? H138 C106 H140 109.5 . . ? H139 C106 H140 109.5 . . ? C108 C107 H141 109.5 . . ? C108 C107 H142 109.5 . . ? H141 C107 H142 109.5 . . ? C108 C107 H143 109.5 . . ? H141 C107 H143 109.5 . . ? H142 C107 H143 109.5 . . ? C109 C108 C107 87.9(19) . . ? C109 C108 H144 114.0 . . ? C107 C108 H144 114.0 . . ? C109 C108 H145 114.0 . . ? C107 C108 H145 114.0 . . ? H144 C108 H145 111.2 . . ? C108 C109 C110 114(2) . . ? C108 C109 H146 108.7 . . ? C110 C109 H146 108.7 . . ? C108 C109 H147 108.7 . . ? C110 C109 H147 108.7 . . ? H146 C109 H147 107.6 . . ? C111 C110 C109 116.7(15) . . ? C111 C110 H148 108.1 . . ? C109 C110 H148 108.1 . . ? C111 C110 H149 108.1 . . ? C109 C110 H149 108.1 . . ? H148 C110 H149 107.3 . . ? C110 C111 C112 115.4(13) . . ? C110 C111 H150 108.4 . . ? C112 C111 H150 108.4 . . ? C110 C111 H151 108.4 . . ? C112 C111 H151 108.4 . . ? H150 C111 H151 107.5 . . ? C111 C112 H152 109.5 . . ? C111 C112 H153 109.5 . . ? H152 C112 H153 109.5 . . ? C111 C112 H154 109.5 . . ? H152 C112 H154 109.5 . . ? H153 C112 H154 109.5 . . ? C114 C113 C118 120.0 . . ? C114 C113 H155 120.0 . . ? C118 C113 H155 120.0 . . ? C115 C114 C113 120.0 . . ? C115 C114 H156 120.0 . . ? C113 C114 H156 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H157 120.0 . . ? C116 C115 H157 120.0 . . ? C117 C116 C115 120.0 . . ? C117 C116 H158 120.0 . . ? C115 C116 H158 120.0 . . ? C116 C117 C118 120.0 . . ? C116 C117 H159 120.0 . . ? C118 C117 H159 120.0 . . ? C117 C118 C113 120.0 . . ? C117 C118 H160 120.0 . . ? C113 C118 H160 120.0 . . ? C120 C119 H161 109.5 . . ? C120 C119 H162 109.5 . . ? H161 C119 H162 109.5 . . ? C120 C119 H163 109.5 . . ? H161 C119 H163 109.5 . . ? H162 C119 H163 109.5 . . ? C121 C120 C119 114.5(11) . . ? C121 C120 H164 108.6 . . ? C119 C120 H164 108.6 . . ? C121 C120 H165 108.6 . . ? C119 C120 H165 108.6 . . ? H164 C120 H165 107.6 . . ? C120 C121 C121 116.2(12) . 2_655 ? C120 C121 H166 108.2 . . ? C121 C121 H166 108.2 2_655 . ? C120 C121 H167 108.2 . . ? C121 C121 H167 108.2 2_655 . ? H166 C121 H167 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Nb1 Nb2 O1 -95.6(2) . . . . ? O4 Nb1 Nb2 O1 27.1(2) . . . . ? O3 Nb1 Nb2 O1 159.7(2) . . . . ? C1 Nb1 Nb2 O1 159.5(3) . . . . ? O2 Nb1 Nb2 O5 5.28(18) . . . . ? O4 Nb1 Nb2 O5 127.9(2) . . . . ? O3 Nb1 Nb2 O5 -99.50(19) . . . . ? O1 Nb1 Nb2 O5 100.8(2) . . . . ? C1 Nb1 Nb2 O5 -99.6(2) . . . . ? O2 Nb1 Nb2 O6 -170.4(2) . . . . ? O4 Nb1 Nb2 O6 -47.7(2) . . . . ? O3 Nb1 Nb2 O6 84.9(2) . . . . ? O1 Nb1 Nb2 O6 -74.8(2) . . . . ? C1 Nb1 Nb2 O6 84.8(3) . . . . ? O2 Nb1 Nb2 C1 104.9(3) . . . . ? O4 Nb1 Nb2 C1 -132.5(3) . . . . ? O3 Nb1 Nb2 C1 0.1(3) . . . . ? O1 Nb1 Nb2 C1 -159.5(3) . . . . ? O5 Nb2 O1 Nb1 -93.38(19) . . . . ? O6 Nb2 O1 Nb1 127.75(17) . . . . ? C1 Nb2 O1 Nb1 15.8(2) . . . . ? O2 Nb1 O1 Nb2 89.0(2) . . . . ? O4 Nb1 O1 Nb2 -159.37(18) . . . . ? O3 Nb1 O1 Nb2 -39.8(4) . . . . ? C1 Nb1 O1 Nb2 -13.50(18) . . . . ? O2 Nb1 O3 C3 -74.1(6) . . . . ? O4 Nb1 O3 C3 173.6(6) . . . . ? O1 Nb1 O3 C3 54.4(8) . . . . ? C1 Nb1 O3 C3 28.5(6) . . . . ? Nb2 Nb1 O3 C3 28.4(7) . . . . ? O2 Nb1 O4 C20 105.8(11) . . . . ? O3 Nb1 O4 C20 -150.7(10) . . . . ? O1 Nb1 O4 C20 4.9(11) . . . . ? C1 Nb1 O4 C20 -67.8(11) . . . . ? Nb2 Nb1 O4 C20 -10.9(11) . . . . ? O1 Nb2 O5 C47 -122.0(13) . . . . ? O6 Nb2 O5 C47 10.5(14) . . . . ? C1 Nb2 O5 C47 140.7(13) . . . . ? Nb1 Nb2 O5 C47 -165.5(13) . . . . ? O1 Nb2 O6 C74 -116(2) . . . . ? O5 Nb2 O6 C74 112(2) . . . . ? C1 Nb2 O6 C74 -17(2) . . . . ? Nb1 Nb2 O6 C74 -73(2) . . . . ? O1 Nb2 C1 C2 168.1(9) . . . . ? O5 Nb2 C1 C2 -81.0(9) . . . . ? O6 Nb2 C1 C2 56.1(10) . . . . ? Nb1 Nb2 C1 C2 -178.5(10) . . . . ? O1 Nb2 C1 Nb1 -13.32(18) . . . . ? O5 Nb2 C1 Nb1 97.58(19) . . . . ? O6 Nb2 C1 Nb1 -125.40(17) . . . . ? O2 Nb1 C1 C2 96.8(5) . . . . ? O4 Nb1 C1 C2 -89.4(6) . . . . ? O3 Nb1 C1 C2 -0.7(5) . . . . ? O1 Nb1 C1 C2 -168.5(5) . . . . ? Nb2 Nb1 C1 C2 179.2(6) . . . . ? O2 Nb1 C1 Nb2 -82.3(2) . . . . ? O4 Nb1 C1 Nb2 91.5(3) . . . . ? O3 Nb1 C1 Nb2 -179.9(2) . . . . ? O1 Nb1 C1 Nb2 12.37(17) . . . . ? Nb2 C1 C2 C8 163.9(7) . . . . ? Nb1 C1 C2 C8 -14.4(9) . . . . ? Nb1 O3 C3 C8 -37.2(9) . . . . ? Nb1 O3 C3 C4 139.9(5) . . . . ? O3 C3 C4 C5 178.0(5) . . . . ? C8 C3 C4 C5 -4.9(9) . . . . ? O3 C3 C4 C10 -4.9(9) . . . . ? C8 C3 C4 C10 172.1(6) . . . . ? C3 C4 C5 C6 0.1(9) . . . . ? C10 C4 C5 C6 -177.0(6) . . . . ? C4 C5 C6 C7 2.5(10) . . . . ? C4 C5 C6 C9 179.8(6) . . . . ? C5 C6 C7 C8 -0.5(9) . . . . ? C9 C6 C7 C8 -177.7(6) . . . . ? O3 C3 C8 C7 -175.9(5) . . . . ? C4 C3 C8 C7 7.0(9) . . . . ? O3 C3 C8 C2 10.1(9) . . . . ? C4 C3 C8 C2 -167.0(6) . . . . ? C6 C7 C8 C3 -4.2(9) . . . . ? C6 C7 C8 C2 170.0(6) . . . . ? C1 C2 C8 C3 12.2(10) . . . . ? C1 C2 C8 C7 -161.9(6) . . . . ? C5 C4 C10 C13 -122.3(6) . . . . ? C3 C4 C10 C13 60.8(8) . . . . ? C5 C4 C10 C11 117.0(6) . . . . ? C3 C4 C10 C11 -59.9(8) . . . . ? C5 C4 C10 C12 -1.1(8) . . . . ? C3 C4 C10 C12 -178.0(6) . . . . ? C13 C10 C11 C14 56.4(7) . . . . ? C4 C10 C11 C14 178.5(5) . . . . ? C12 C10 C11 C14 -60.0(7) . . . . ? C13 C10 C12 C16 -57.9(8) . . . . ? C4 C10 C12 C16 179.2(6) . . . . ? C11 C10 C12 C16 59.1(7) . . . . ? C4 C10 C13 C18 -178.7(5) . . . . ? C11 C10 C13 C18 -57.5(6) . . . . ? C12 C10 C13 C18 57.8(7) . . . . ? C10 C11 C14 C19 -58.7(7) . . . . ? C10 C11 C14 C15 61.9(8) . . . . ? C19 C14 C15 C16 61.1(8) . . . . ? C11 C14 C15 C16 -60.1(8) . . . . ? C14 C15 C16 C12 59.7(8) . . . . ? C14 C15 C16 C17 -61.2(7) . . . . ? C10 C12 C16 C15 -60.9(8) . . . . ? C10 C12 C16 C17 60.1(7) . . . . ? C15 C16 C17 C18 60.9(8) . . . . ? C12 C16 C17 C18 -60.6(8) . . . . ? C16 C17 C18 C19 -58.9(8) . . . . ? C16 C17 C18 C13 59.1(8) . . . . ? C10 C13 C18 C17 -59.4(7) . . . . ? C10 C13 C18 C19 59.0(7) . . . . ? C11 C14 C19 C18 60.4(7) . . . . ? C15 C14 C19 C18 -60.3(8) . . . . ? C17 C18 C19 C14 59.3(7) . . . . ? C13 C18 C19 C14 -59.2(7) . . . . ? Nb1 O4 C20 C25 97.8(11) . . . . ? Nb1 O4 C20 C21 -81.9(12) . . . . ? O4 C20 C21 C22 169.0(5) . . . . ? C25 C20 C21 C22 -10.7(8) . . . . ? O4 C20 C21 C26 -12.9(8) . . . . ? C25 C20 C21 C26 167.3(5) . . . . ? C20 C21 C22 C23 1.9(9) . . . . ? C26 C21 C22 C23 -176.2(6) . . . . ? C21 C22 C23 C24 4.8(10) . . . . ? C21 C22 C23 C36 -175.5(6) . . . . ? C22 C23 C24 C25 -3.2(9) . . . . ? C36 C23 C24 C25 177.2(6) . . . . ? C23 C24 C25 C20 -5.1(9) . . . . ? C23 C24 C25 C37 169.4(6) . . . . ? O4 C20 C25 C24 -167.6(5) . . . . ? C21 C20 C25 C24 12.2(8) . . . . ? O4 C20 C25 C37 18.3(8) . . . . ? C21 C20 C25 C37 -161.9(5) . . . . ? C22 C21 C26 C28 -105.7(6) . . . . ? C20 C21 C26 C28 76.3(7) . . . . ? C22 C21 C26 C27 131.3(6) . . . . ? C20 C21 C26 C27 -46.7(7) . . . . ? C22 C21 C26 C29 13.7(8) . . . . ? C20 C21 C26 C29 -164.2(6) . . . . ? C28 C26 C27 C30 56.2(6) . . . . ? C21 C26 C27 C30 -177.9(5) . . . . ? C29 C26 C27 C30 -57.3(6) . . . . ? C21 C26 C28 C34 -179.4(5) . . . . ? C27 C26 C28 C34 -55.4(6) . . . . ? C29 C26 C28 C34 58.2(6) . . . . ? C28 C26 C29 C32 -58.8(7) . . . . ? C21 C26 C29 C32 177.0(5) . . . . ? C27 C26 C29 C32 56.7(7) . . . . ? C26 C27 C30 C31 62.0(7) . . . . ? C26 C27 C30 C35 -59.8(7) . . . . ? C35 C30 C31 C32 59.9(7) . . . . ? C27 C30 C31 C32 -61.0(7) . . . . ? C26 C29 C32 C33 60.2(7) . . . . ? C26 C29 C32 C31 -60.1(7) . . . . ? C30 C31 C32 C33 -59.3(7) . . . . ? C30 C31 C32 C29 60.0(7) . . . . ? C29 C32 C33 C34 -58.9(7) . . . . ? C31 C32 C33 C34 61.3(7) . . . . ? C32 C33 C34 C28 59.8(7) . . . . ? C32 C33 C34 C35 -60.4(7) . . . . ? C26 C28 C34 C33 -60.6(7) . . . . ? C26 C28 C34 C35 58.3(6) . . . . ? C31 C30 C35 C34 -60.7(7) . . . . ? C27 C30 C35 C34 60.4(7) . . . . ? C33 C34 C35 C30 59.6(7) . . . . ? C28 C34 C35 C30 -60.3(6) . . . . ? C24 C25 C37 C38 -114.2(6) . . . . ? C20 C25 C37 C38 59.9(7) . . . . ? C24 C25 C37 C40 3.6(8) . . . . ? C20 C25 C37 C40 177.7(6) . . . . ? C24 C25 C37 C39 124.6(6) . . . . ? C20 C25 C37 C39 -61.4(8) . . . . ? C40 C37 C38 C41 57.7(7) . . . . ? C39 C37 C38 C41 -56.4(7) . . . . ? C25 C37 C38 C41 178.6(5) . . . . ? C38 C37 C39 C43 55.8(7) . . . . ? C40 C37 C39 C43 -59.1(7) . . . . ? C25 C37 C39 C43 176.6(5) . . . . ? C38 C37 C40 C45 -57.1(7) . . . . ? C39 C37 C40 C45 58.8(7) . . . . ? C25 C37 C40 C45 -175.3(6) . . . . ? C37 C38 C41 C42 58.8(7) . . . . ? C37 C38 C41 C46 -60.5(7) . . . . ? C38 C41 C42 C43 -59.6(8) . . . . ? C46 C41 C42 C43 60.2(7) . . . . ? C41 C42 C43 C44 -60.2(7) . . . . ? C41 C42 C43 C39 59.4(7) . . . . ? C37 C39 C43 C42 -58.8(7) . . . . ? C37 C39 C43 C44 61.5(7) . . . . ? C42 C43 C44 C45 60.0(7) . . . . ? C39 C43 C44 C45 -60.5(8) . . . . ? C43 C44 C45 C46 -60.3(8) . . . . ? C43 C44 C45 C40 59.9(8) . . . . ? C37 C40 C45 C44 -60.7(8) . . . . ? C37 C40 C45 C46 59.7(8) . . . . ? C44 C45 C46 C41 60.7(8) . . . . ? C40 C45 C46 C41 -59.3(8) . . . . ? C38 C41 C46 C45 60.0(8) . . . . ? C42 C41 C46 C45 -60.1(7) . . . . ? Nb2 O5 C47 C52 47.4(16) . . . . ? Nb2 O5 C47 C48 -131.4(12) . . . . ? O5 C47 C48 C49 168.2(5) . . . . ? C52 C47 C48 C49 -10.4(8) . . . . ? O5 C47 C48 C53 -19.7(9) . . . . ? C52 C47 C48 C53 161.6(5) . . . . ? C47 C48 C49 C50 0.6(9) . . . . ? C53 C48 C49 C50 -172.0(6) . . . . ? C48 C49 C50 C51 7.2(9) . . . . ? C48 C49 C50 C63 -178.0(6) . . . . ? C49 C50 C51 C52 -5.7(9) . . . . ? C63 C50 C51 C52 179.6(6) . . . . ? C50 C51 C52 C47 -3.5(9) . . . . ? C50 C51 C52 C64 166.7(6) . . . . ? O5 C47 C52 C51 -166.9(5) . . . . ? C48 C47 C52 C51 11.8(8) . . . . ? O5 C47 C52 C64 23.6(8) . . . . ? C48 C47 C52 C64 -157.7(6) . . . . ? C49 C48 C53 C55 1.0(7) . . . . ? C47 C48 C53 C55 -170.9(5) . . . . ? C49 C48 C53 C54 119.7(6) . . . . ? C47 C48 C53 C54 -52.3(7) . . . . ? C49 C48 C53 C56 -118.1(6) . . . . ? C47 C48 C53 C56 69.9(7) . . . . ? C55 C53 C54 C57 -57.9(6) . . . . ? C48 C53 C54 C57 -179.0(5) . . . . ? C56 C53 C54 C57 57.2(6) . . . . ? C54 C53 C55 C59 58.1(6) . . . . ? C48 C53 C55 C59 177.5(5) . . . . ? C56 C53 C55 C59 -59.6(6) . . . . ? C55 C53 C56 C61 60.9(6) . . . . ? C54 C53 C56 C61 -55.2(6) . . . . ? C48 C53 C56 C61 -176.8(5) . . . . ? C53 C54 C57 C58 59.9(6) . . . . ? C53 C54 C57 C62 -59.5(6) . . . . ? C62 C57 C58 C59 58.6(6) . . . . ? C54 C57 C58 C59 -60.1(7) . . . . ? C57 C58 C59 C60 -59.9(6) . . . . ? C57 C58 C59 C55 59.7(6) . . . . ? C53 C55 C59 C60 60.2(6) . . . . ? C53 C55 C59 C58 -59.6(6) . . . . ? C58 C59 C60 C61 60.2(6) . . . . ? C55 C59 C60 C61 -58.8(7) . . . . ? C59 C60 C61 C56 60.5(7) . . . . ? C59 C60 C61 C62 -59.4(6) . . . . ? C53 C56 C61 C60 -62.8(6) . . . . ? C53 C56 C61 C62 56.5(6) . . . . ? C58 C57 C62 C61 -58.8(6) . . . . ? C54 C57 C62 C61 60.5(6) . . . . ? C60 C61 C62 C57 59.4(6) . . . . ? C56 C61 C62 C57 -59.9(6) . . . . ? C51 C52 C64 C66 117.8(6) . . . . ? C47 C52 C64 C66 -72.8(7) . . . . ? C51 C52 C64 C67 -4.2(7) . . . . ? C47 C52 C64 C67 165.2(5) . . . . ? C51 C52 C64 C65 -120.2(6) . . . . ? C47 C52 C64 C65 49.2(7) . . . . ? C66 C64 C65 C68 -58.1(6) . . . . ? C67 C64 C65 C68 58.2(6) . . . . ? C52 C64 C65 C68 176.5(5) . . . . ? C67 C64 C66 C70 -57.7(6) . . . . ? C65 C64 C66 C70 57.8(6) . . . . ? C52 C64 C66 C70 178.9(5) . . . . ? C66 C64 C67 C72 58.3(6) . . . . ? C65 C64 C67 C72 -58.9(6) . . . . ? C52 C64 C67 C72 -175.6(5) . . . . ? C64 C65 C68 C69 59.1(6) . . . . ? C64 C65 C68 C73 -61.1(6) . . . . ? C73 C68 C69 C70 59.9(6) . . . . ? C65 C68 C69 C70 -59.9(6) . . . . ? C64 C66 C70 C71 60.6(6) . . . . ? C64 C66 C70 C69 -59.7(6) . . . . ? C68 C69 C70 C71 -60.5(6) . . . . ? C68 C69 C70 C66 60.8(6) . . . . ? C66 C70 C71 C72 -60.5(7) . . . . ? C69 C70 C71 C72 60.5(7) . . . . ? C70 C71 C72 C67 58.5(7) . . . . ? C70 C71 C72 C73 -60.3(6) . . . . ? C64 C67 C72 C71 -58.7(6) . . . . ? C64 C67 C72 C73 61.0(7) . . . . ? C69 C68 C73 C72 -58.6(6) . . . . ? C65 C68 C73 C72 61.0(7) . . . . ? C71 C72 C73 C68 58.7(6) . . . . ? C67 C72 C73 C68 -60.3(7) . . . . ? Nb2 O6 C74 C79 114.4(19) . . . . ? Nb2 O6 C74 C75 -64(2) . . . . ? O6 C74 C75 C76 169.4(5) . . . . ? C79 C74 C75 C76 -8.8(8) . . . . ? O6 C74 C75 C80 -11.8(8) . . . . ? C79 C74 C75 C80 170.1(5) . . . . ? C74 C75 C76 C77 2.0(9) . . . . ? C80 C75 C76 C77 -176.9(6) . . . . ? C75 C76 C77 C78 4.2(10) . . . . ? C75 C76 C77 C90 -179.4(6) . . . . ? C76 C77 C78 C79 -4.1(10) . . . . ? C90 C77 C78 C79 179.4(6) . . . . ? C77 C78 C79 C74 -2.3(9) . . . . ? C77 C78 C79 C91 177.4(6) . . . . ? O6 C74 C79 C78 -169.2(5) . . . . ? C75 C74 C79 C78 8.9(9) . . . . ? O6 C74 C79 C91 11.1(9) . . . . ? C75 C74 C79 C91 -170.8(5) . . . . ? C76 C75 C80 C81 127.0(6) . . . . ? C74 C75 C80 C81 -51.9(7) . . . . ? C76 C75 C80 C82 8.2(7) . . . . ? C74 C75 C80 C82 -170.6(5) . . . . ? C76 C75 C80 C83 -110.6(6) . . . . ? C74 C75 C80 C83 70.6(7) . . . . ? C75 C80 C81 C84 -177.9(5) . . . . ? C82 C80 C81 C84 -56.8(6) . . . . ? C83 C80 C81 C84 58.0(6) . . . . ? C81 C80 C82 C86 56.9(6) . . . . ? C75 C80 C82 C86 178.1(5) . . . . ? C83 C80 C82 C86 -59.8(7) . . . . ? C81 C80 C83 C88 -56.8(6) . . . . ? C75 C80 C83 C88 179.7(5) . . . . ? C82 C80 C83 C88 58.4(6) . . . . ? C80 C81 C84 C85 60.7(6) . . . . ? C80 C81 C84 C89 -59.0(6) . . . . ? C89 C84 C85 C86 58.7(7) . . . . ? C81 C84 C85 C86 -60.4(7) . . . . ? C84 C85 C86 C87 -59.8(7) . . . . ? C84 C85 C86 C82 59.4(7) . . . . ? C80 C82 C86 C87 61.5(7) . . . . ? C80 C82 C86 C85 -59.2(7) . . . . ? C85 C86 C87 C88 59.4(7) . . . . ? C82 C86 C87 C88 -60.5(7) . . . . ? C86 C87 C88 C89 -58.6(7) . . . . ? C86 C87 C88 C83 61.8(7) . . . . ? C80 C83 C88 C89 58.7(7) . . . . ? C80 C83 C88 C87 -61.4(7) . . . . ? C87 C88 C89 C84 59.3(7) . . . . ? C83 C88 C89 C84 -61.0(7) . . . . ? C85 C84 C89 C88 -59.8(7) . . . . ? C81 C84 C89 C88 60.3(7) . . . . ? C78 C79 C91 C93 111.3(6) . . . . ? C74 C79 C91 C93 -69.0(8) . . . . ? C78 C79 C91 C92 -126.8(6) . . . . ? C74 C79 C91 C92 52.9(8) . . . . ? C78 C79 C91 C94 -7.8(8) . . . . ? C74 C79 C91 C94 171.8(6) . . . . ? C93 C91 C92 C95 -57.6(7) . . . . ? C79 C91 C92 C95 179.0(5) . . . . ? C94 C91 C92 C95 57.8(7) . . . . ? C92 C91 C93 C97 56.9(7) . . . . ? C79 C91 C93 C97 179.6(5) . . . . ? C94 C91 C93 C97 -58.8(7) . . . . ? C93 C91 C94 C99 59.5(7) . . . . ? C92 C91 C94 C99 -57.4(7) . . . . ? C79 C91 C94 C99 -178.4(5) . . . . ? C91 C92 C95 C100 -60.5(7) . . . . ? C91 C92 C95 C96 58.7(7) . . . . ? C92 C95 C96 C97 -59.5(7) . . . . ? C100 C95 C96 C97 60.2(7) . . . . ? C95 C96 C97 C98 -60.5(7) . . . . ? C95 C96 C97 C93 59.8(7) . . . . ? C91 C93 C97 C98 60.8(7) . . . . ? C91 C93 C97 C96 -58.7(7) . . . . ? C96 C97 C98 C99 60.7(7) . . . . ? C93 C97 C98 C99 -59.1(7) . . . . ? C91 C94 C99 C98 -60.2(7) . . . . ? C91 C94 C99 C100 59.4(8) . . . . ? C97 C98 C99 C94 58.5(7) . . . . ? C97 C98 C99 C100 -61.2(7) . . . . ? C92 C95 C100 C99 59.4(7) . . . . ? C96 C95 C100 C99 -59.9(7) . . . . ? C94 C99 C100 C95 -59.0(8) . . . . ? C98 C99 C100 C95 60.8(7) . . . . ? C101 C102 C103 C104 62.8(17) . . . . ? C102 C103 C104 C105 176.6(14) . . . . ? C103 C104 C105 C106 -175.5(13) . . . . ? C107 C108 C109 C110 169.2(16) . . . . ? C108 C109 C110 C111 46(3) . . . . ? C109 C110 C111 C112 174.8(14) . . . . ? C118 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 C117 0.0 . . . . ? C115 C116 C117 C118 0.0 . . . . ? C116 C117 C118 C113 0.0 . . . . ? C114 C113 C118 C117 0.0 . . . . ? C119 C120 C121 C121 -177.0(13) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.347 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.118 data_[{(ArO)2Nb}2(CH2)(O)](toluene)3.5 _database_code_depnum_ccdc_archive 'CCDC 902916' #TrackingRef '14202_web_deposit_cif_file_0_HiroyukiKawaguchi_1348537764.CIF-kawaguchi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C109 H142 Nb2 O5, 3.5(C7 H8)' _chemical_formula_sum 'C133.50 H170 Nb2 O5' _chemical_formula_weight 2040.52 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' Nb Nb -2.0727 0.6215 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.333(3) _cell_length_b 25.833(5) _cell_length_c 21.541(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.185(3) _cell_angle_gamma 90.00 _cell_volume 11314(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12187 _cell_measurement_theta_min 3.1074 _cell_measurement_theta_max 27.4507 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4372 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9723 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Saturn CCD (4x4 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 69689 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.47 _reflns_number_total 12895 _reflns_number_gt 10013 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+25.9946P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12895 _refine_ls_number_parameters 691 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2148 _refine_ls_wR_factor_gt 0.1988 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.498620(18) 0.231813(14) 0.313092(18) 0.02754(13) Uani 0.7646(11) 1 d P . 1 Nb2 Nb 0.43354(6) 0.23473(5) 0.24903(6) 0.0289(4) Uani 0.2354(11) 1 d P . 2 C1 C 0.5000 0.16827(18) 0.2500 0.0326(10) Uani 1 2 d S . . O1 O 0.5000 0.28716(13) 0.2500 0.0328(7) Uani 1 2 d S . . O2 O 0.40817(12) 0.23547(9) 0.33981(11) 0.0361(6) Uani 1 1 d . . . O3 O 0.58815(12) 0.23434(9) 0.34517(12) 0.0390(6) Uani 1 1 d . . . C2 C 0.35229(18) 0.23055(13) 0.37502(17) 0.0343(7) Uani 1 1 d . . . C3 C 0.29810(18) 0.26502(13) 0.36566(17) 0.0364(8) Uani 1 1 d . . . C4 C 0.23924(19) 0.25355(15) 0.39614(18) 0.0403(8) Uani 1 1 d . . . H1 H 0.2030 0.2763 0.3906 0.048 Uiso 1 1 calc R . . C5 C 0.23105(18) 0.21063(15) 0.43409(17) 0.0381(8) Uani 1 1 d . . . C6 C 0.28556(18) 0.18047(14) 0.44520(17) 0.0371(8) Uani 1 1 d . . . H2 H 0.2811 0.1518 0.4725 0.045 Uiso 1 1 calc R . . C7 C 0.34759(17) 0.18953(14) 0.41860(16) 0.0353(8) Uani 1 1 d . . . C8 C 0.29633(18) 0.31537(14) 0.32654(17) 0.0361(8) Uani 1 1 d . . . C9 C 0.36029(19) 0.32901(14) 0.29204(17) 0.0387(8) Uani 1 1 d . . . H3 H 0.3968 0.3318 0.3224 0.046 Uiso 1 1 calc R . . H4 H 0.3712 0.3008 0.2627 0.046 Uiso 1 1 calc R . . C10 C 0.2802(2) 0.36165(14) 0.37045(18) 0.0407(8) Uani 1 1 d . . . H5 H 0.2385 0.3546 0.3926 0.049 Uiso 1 1 calc R . . H6 H 0.3155 0.3653 0.4018 0.049 Uiso 1 1 calc R . . C11 C 0.2406(2) 0.31249(15) 0.27742(19) 0.0439(9) Uani 1 1 d . . . H7 H 0.2499 0.2839 0.2481 0.053 Uiso 1 1 calc R . . H8 H 0.1984 0.3049 0.2983 0.053 Uiso 1 1 calc R . . C12 C 0.3540(2) 0.38001(15) 0.25624(18) 0.0431(9) Uani 1 1 d . . . H9 H 0.3964 0.3875 0.2347 0.052 Uiso 1 1 calc R . . C13 C 0.3381(2) 0.42425(15) 0.3009(2) 0.0492(10) Uani 1 1 d . . . H10 H 0.3740 0.4280 0.3318 0.059 Uiso 1 1 calc R . . H11 H 0.3343 0.4572 0.2776 0.059 Uiso 1 1 calc R . . C14 C 0.2737(2) 0.41242(16) 0.33368(19) 0.0476(10) Uani 1 1 d . . . H12 H 0.2634 0.4412 0.3631 0.057 Uiso 1 1 calc R . . C15 C 0.2176(2) 0.40746(16) 0.28625(19) 0.0491(10) Uani 1 1 d . . . H13 H 0.1758 0.3997 0.3078 0.059 Uiso 1 1 calc R . . H14 H 0.2122 0.4404 0.2632 0.059 Uiso 1 1 calc R . . C16 C 0.2344(2) 0.36364(16) 0.24117(19) 0.0458(9) Uani 1 1 d . . . H15 H 0.1984 0.3603 0.2096 0.055 Uiso 1 1 calc R . . C17 C 0.2994(2) 0.37418(17) 0.20804(19) 0.0482(10) Uani 1 1 d . . . H16 H 0.3097 0.3452 0.1796 0.058 Uiso 1 1 calc R . . H17 H 0.2957 0.4062 0.1831 0.058 Uiso 1 1 calc R . . C18 C 0.16614(19) 0.19949(17) 0.46452(19) 0.0467(9) Uani 1 1 d . . . H18 H 0.1659 0.1638 0.4800 0.070 Uiso 1 1 calc R . . H19 H 0.1306 0.2039 0.4342 0.070 Uiso 1 1 calc R . . H20 H 0.1596 0.2235 0.4992 0.070 Uiso 1 1 calc R . . C19 C 0.40384(18) 0.15441(14) 0.44368(18) 0.0384(8) Uani 1 1 d . . . C20 C 0.47376(19) 0.16655(16) 0.42219(19) 0.0442(9) Uani 1 1 d . . . H21 H 0.4843 0.2030 0.4323 0.053 Uiso 1 1 calc R . . H22 H 0.4762 0.1625 0.3765 0.053 Uiso 1 1 calc R . . C21 C 0.3900(2) 0.09699(15) 0.4297(2) 0.0515(10) Uani 1 1 d . . . H23 H 0.3916 0.0913 0.3843 0.062 Uiso 1 1 calc R . . H24 H 0.3452 0.0881 0.4441 0.062 Uiso 1 1 calc R . . C22 C 0.4059(2) 0.16154(17) 0.51593(19) 0.0494(10) Uani 1 1 d . . . H25 H 0.4173 0.1979 0.5257 0.059 Uiso 1 1 calc R . . H26 H 0.3618 0.1545 0.5331 0.059 Uiso 1 1 calc R . . C23 C 0.5251(2) 0.13070(17) 0.4531(2) 0.0521(11) Uani 1 1 d . . . H27 H 0.5699 0.1394 0.4370 0.063 Uiso 1 1 calc R . . C24 C 0.5090(2) 0.07404(17) 0.4373(3) 0.0600(12) Uani 1 1 d . . . H28 H 0.5104 0.0689 0.3918 0.072 Uiso 1 1 calc R . . H29 H 0.5420 0.0509 0.4566 0.072 Uiso 1 1 calc R . . C25 C 0.4403(2) 0.06083(17) 0.4618(2) 0.0562(12) Uani 1 1 d . . . H30 H 0.4295 0.0239 0.4521 0.067 Uiso 1 1 calc R . . C26 C 0.4382(2) 0.06949(19) 0.5317(3) 0.0638(13) Uani 1 1 d . . . H31 H 0.4693 0.0456 0.5525 0.077 Uiso 1 1 calc R . . H32 H 0.3934 0.0619 0.5473 0.077 Uiso 1 1 calc R . . C27 C 0.4565(2) 0.12534(18) 0.5472(2) 0.0578(12) Uani 1 1 d . . . H33 H 0.4555 0.1305 0.5932 0.069 Uiso 1 1 calc R . . C28 C 0.5244(2) 0.13779(19) 0.5228(2) 0.0579(12) Uani 1 1 d . . . H34 H 0.5361 0.1739 0.5333 0.069 Uiso 1 1 calc R . . H35 H 0.5573 0.1146 0.5423 0.069 Uiso 1 1 calc R . . C29 C 0.62404(17) 0.23086(13) 0.39940(17) 0.0364(8) Uani 1 1 d . . . C30 C 0.61151(17) 0.26479(13) 0.44955(17) 0.0345(7) Uani 1 1 d . . . C31 C 0.63986(17) 0.25203(15) 0.50656(19) 0.0389(8) Uani 1 1 d . . . H36 H 0.6304 0.2735 0.5412 0.047 Uiso 1 1 calc R . . C32 C 0.68089(17) 0.20995(14) 0.51588(18) 0.0380(8) Uani 1 1 d . . . C33 C 0.69816(18) 0.18151(14) 0.46397(19) 0.0396(8) Uani 1 1 d . . . H37 H 0.7289 0.1542 0.4690 0.048 Uiso 1 1 calc R . . C34 C 0.67292(17) 0.19070(14) 0.40444(18) 0.0377(8) Uani 1 1 d . . . C35 C 0.57433(17) 0.31693(14) 0.44854(18) 0.0364(8) Uani 1 1 d . . . C36 C 0.53934(18) 0.33127(14) 0.38768(18) 0.0390(8) Uani 1 1 d . . . H38 H 0.5046 0.3054 0.3788 0.047 Uiso 1 1 calc R . . H39 H 0.5714 0.3304 0.3532 0.047 Uiso 1 1 calc R . . C37 C 0.62581(18) 0.35985(15) 0.46246(18) 0.0409(8) Uani 1 1 d . . . H40 H 0.6484 0.3519 0.5021 0.049 Uiso 1 1 calc R . . H41 H 0.6593 0.3600 0.4292 0.049 Uiso 1 1 calc R . . C38 C 0.52126(18) 0.31908(15) 0.50089(19) 0.0424(9) Uani 1 1 d . . . H42 H 0.4864 0.2933 0.4922 0.051 Uiso 1 1 calc R . . H43 H 0.5418 0.3102 0.5412 0.051 Uiso 1 1 calc R . . C39 C 0.50811(19) 0.38579(14) 0.39137(19) 0.0421(9) Uani 1 1 d . . . H44 H 0.4862 0.3942 0.3510 0.051 Uiso 1 1 calc R . . C40 C 0.5611(2) 0.42622(15) 0.4055(2) 0.0478(10) Uani 1 1 d . . . H45 H 0.5941 0.4266 0.3717 0.057 Uiso 1 1 calc R . . H46 H 0.5409 0.4610 0.4079 0.057 Uiso 1 1 calc R . . C41 C 0.59464(19) 0.41340(15) 0.46679(19) 0.0441(9) Uani 1 1 d . . . H47 H 0.6294 0.4398 0.4759 0.053 Uiso 1 1 calc R . . C42 C 0.5441(2) 0.41271(16) 0.5194(2) 0.0478(9) Uani 1 1 d . . . H48 H 0.5661 0.4035 0.5590 0.057 Uiso 1 1 calc R . . H49 H 0.5244 0.4475 0.5241 0.057 Uiso 1 1 calc R . . C43 C 0.4904(2) 0.37334(17) 0.5049(2) 0.0484(10) Uani 1 1 d . . . H50 H 0.4570 0.3738 0.5388 0.058 Uiso 1 1 calc R . . C44 C 0.45700(19) 0.38577(16) 0.4435(2) 0.0474(10) Uani 1 1 d . . . H51 H 0.4356 0.4201 0.4459 0.057 Uiso 1 1 calc R . . H52 H 0.4227 0.3596 0.4345 0.057 Uiso 1 1 calc R . . C45 C 0.7080(2) 0.19722(17) 0.57899(19) 0.0481(10) Uani 1 1 d . . . H53 H 0.7490 0.2163 0.5857 0.072 Uiso 1 1 calc R . . H54 H 0.7166 0.1600 0.5817 0.072 Uiso 1 1 calc R . . H55 H 0.6759 0.2070 0.6108 0.072 Uiso 1 1 calc R . . C46 C 0.6983(13) 0.1578(9) 0.3463(12) 0.042(5) Uani 0.662(7) 1 d P . 1 C47 C 0.7147(3) 0.1921(2) 0.2977(3) 0.0381(14) Uani 0.662(7) 1 d P . 1 H56 H 0.7483 0.2171 0.3121 0.046 Uiso 0.662(7) 1 calc PR . 1 H57 H 0.6752 0.2117 0.2845 0.046 Uiso 0.662(7) 1 calc PR . 1 C48 C 0.6491(3) 0.1154(2) 0.3330(3) 0.0401(14) Uani 0.662(7) 1 d P . 1 H58 H 0.6057 0.1303 0.3220 0.048 Uiso 0.662(7) 1 calc PR . 1 H59 H 0.6438 0.0927 0.3697 0.048 Uiso 0.662(7) 1 calc PR . 1 C49 C 0.7631(3) 0.1293(3) 0.3715(3) 0.0459(16) Uani 0.662(7) 1 d P . 1 H60 H 0.7955 0.1551 0.3865 0.055 Uiso 0.662(7) 1 calc PR . 1 H61 H 0.7520 0.1059 0.4063 0.055 Uiso 0.662(7) 1 calc PR . 1 C50 C 0.7415(4) 0.1605(3) 0.2428(3) 0.0430(16) Uani 0.662(7) 1 d P . 1 H62 H 0.7499 0.1843 0.2070 0.052 Uiso 0.662(7) 1 calc PR . 1 C51 C 0.6908(4) 0.1200(3) 0.2237(4) 0.0448(18) Uani 0.662(7) 1 d P . 1 H63 H 0.6496 0.1373 0.2106 0.054 Uiso 0.662(7) 1 calc PR . 1 H64 H 0.7076 0.0996 0.1883 0.054 Uiso 0.662(7) 1 calc PR . 1 C52 C 0.6774(3) 0.0846(2) 0.2779(3) 0.0459(16) Uani 0.662(7) 1 d P . 1 H65 H 0.6445 0.0580 0.2647 0.055 Uiso 0.662(7) 1 calc PR . 1 C53 C 0.7401(6) 0.0576(4) 0.2970(6) 0.052(2) Uani 0.662(7) 1 d P . 1 H66 H 0.7571 0.0370 0.2618 0.062 Uiso 0.662(7) 1 calc PR . 1 H67 H 0.7311 0.0338 0.3319 0.062 Uiso 0.662(7) 1 calc PR . 1 C54 C 0.7918(5) 0.0982(4) 0.3168(4) 0.051(2) Uani 0.662(7) 1 d P . 1 H68 H 0.8334 0.0805 0.3300 0.062 Uiso 0.662(7) 1 calc PR . 1 C55 C 0.8054(4) 0.1346(3) 0.2619(5) 0.0531(19) Uani 0.662(7) 1 d P . 1 H69 H 0.8381 0.1612 0.2742 0.064 Uiso 0.662(7) 1 calc PR . 1 H70 H 0.8235 0.1147 0.2266 0.064 Uiso 0.662(7) 1 calc PR . 1 C56 C 0.702(2) 0.1589(16) 0.356(2) 0.026(4) Uani 0.338(7) 1 d PU . 2 C57 C 0.6810(8) 0.1722(5) 0.2776(5) 0.050(3) Uani 0.338(7) 1 d PU . 2 H71 H 0.6329 0.1676 0.2726 0.060 Uiso 0.338(7) 1 calc PR . 2 H72 H 0.6911 0.2090 0.2689 0.060 Uiso 0.338(7) 1 calc PR . 2 C58 C 0.6891(9) 0.1019(5) 0.3545(6) 0.057(4) Uani 0.338(7) 1 d PU . 2 H73 H 0.6412 0.0972 0.3485 0.068 Uiso 0.338(7) 1 calc PR . 2 H74 H 0.7001 0.0878 0.3960 0.068 Uiso 0.338(7) 1 calc PR . 2 C59 C 0.7803(6) 0.1692(6) 0.3463(6) 0.052(3) Uani 0.338(7) 1 d PU . 2 H75 H 0.7864 0.2057 0.3335 0.063 Uiso 0.338(7) 1 calc PR . 2 H76 H 0.8030 0.1646 0.3867 0.063 Uiso 0.338(7) 1 calc PR . 2 C60 C 0.7157(12) 0.1388(7) 0.2291(8) 0.059(4) Uani 0.338(7) 1 d PU . 2 H77 H 0.6989 0.1471 0.1865 0.071 Uiso 0.338(7) 1 calc PR . 2 C61 C 0.7057(11) 0.0831(6) 0.2433(8) 0.076(4) Uani 0.338(7) 1 d PU . 2 H78 H 0.6589 0.0742 0.2360 0.091 Uiso 0.338(7) 1 calc PR . 2 H79 H 0.7325 0.0621 0.2143 0.091 Uiso 0.338(7) 1 calc PR . 2 C62 C 0.7234(16) 0.0691(11) 0.3073(13) 0.079(6) Uani 0.338(7) 1 d PU . 2 H80 H 0.7118 0.0320 0.3146 0.095 Uiso 0.338(7) 1 calc PR . 2 C63 C 0.7916(16) 0.0748(9) 0.3114(12) 0.088(7) Uani 0.338(7) 1 d PU . 2 H81 H 0.8129 0.0516 0.2810 0.106 Uiso 0.338(7) 1 calc PR . 2 H82 H 0.8065 0.0645 0.3534 0.106 Uiso 0.338(7) 1 calc PR . 2 C64 C 0.8137(11) 0.1341(9) 0.2981(10) 0.080(5) Uani 0.338(7) 1 d PU . 2 H83 H 0.8626 0.1377 0.3003 0.095 Uiso 0.338(7) 1 calc PR . 2 C65 C 0.7881(11) 0.1481(8) 0.2328(9) 0.079(5) Uani 0.338(7) 1 d PU . 2 H84 H 0.7976 0.1849 0.2239 0.095 Uiso 0.338(7) 1 calc PR . 2 H85 H 0.8108 0.1267 0.2013 0.095 Uiso 0.338(7) 1 calc PR . 2 C66 C 0.1604(3) 0.0610(3) 0.4026(3) 0.0926(19) Uani 1 1 d . . . H86 H 0.1791 0.0956 0.3967 0.139 Uiso 1 1 calc R . . H87 H 0.1223 0.0632 0.4303 0.139 Uiso 1 1 calc R . . H88 H 0.1465 0.0470 0.3624 0.139 Uiso 1 1 calc R . . C67 C 0.2101(3) 0.02683(18) 0.4303(2) 0.0621(12) Uani 1 1 d . . . C68 C 0.2235(3) 0.02733(19) 0.4947(2) 0.0654(13) Uani 1 1 d . . . H89 H 0.2001 0.0503 0.5211 0.078 Uiso 1 1 calc R . . C69 C 0.2692(3) -0.0046(2) 0.5186(3) 0.0667(13) Uani 1 1 d . . . H90 H 0.2776 -0.0034 0.5619 0.080 Uiso 1 1 calc R . . C70 C 0.3045(3) -0.0393(2) 0.4826(3) 0.0732(15) Uani 1 1 d . . . H91 H 0.3364 -0.0616 0.5006 0.088 Uiso 1 1 calc R . . C71 C 0.2920(3) -0.0400(2) 0.4208(3) 0.0816(17) Uani 1 1 d . . . H92 H 0.3153 -0.0635 0.3950 0.098 Uiso 1 1 calc R . . C72 C 0.2456(3) -0.00710(19) 0.3946(2) 0.0620(12) Uani 1 1 d . . . H93 H 0.2384 -0.0081 0.3510 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0251(2) 0.0286(2) 0.0289(2) 0.00032(15) -0.00140(14) -0.00051(14) Nb2 0.0264(7) 0.0288(7) 0.0316(7) 0.0004(5) 0.0009(5) -0.0004(5) C1 0.034(2) 0.029(2) 0.034(2) 0.000 -0.003(2) 0.000 O1 0.0313(17) 0.0338(17) 0.0332(17) 0.000 -0.0001(14) 0.000 O2 0.0390(14) 0.0318(13) 0.0375(13) 0.0039(10) 0.0109(11) 0.0017(10) O3 0.0350(13) 0.0393(14) 0.0426(14) -0.0078(11) -0.0126(11) 0.0042(10) C2 0.0356(18) 0.0302(17) 0.0371(18) -0.0012(14) 0.0073(14) -0.0022(14) C3 0.0369(19) 0.0331(18) 0.0393(19) -0.0025(14) 0.0048(15) 0.0009(14) C4 0.037(2) 0.041(2) 0.043(2) 0.0009(16) 0.0052(16) 0.0054(16) C5 0.0354(19) 0.0393(19) 0.0395(19) -0.0028(15) 0.0060(15) -0.0040(15) C6 0.0370(19) 0.0384(19) 0.0359(19) 0.0034(15) 0.0026(15) -0.0032(15) C7 0.0352(18) 0.0335(18) 0.0373(19) -0.0001(14) 0.0024(15) -0.0016(14) C8 0.0383(19) 0.0341(18) 0.0360(18) 0.0029(14) 0.0040(15) 0.0051(15) C9 0.045(2) 0.0330(18) 0.0386(19) 0.0007(15) 0.0048(16) 0.0025(15) C10 0.046(2) 0.0369(19) 0.039(2) -0.0020(15) 0.0016(16) 0.0090(16) C11 0.043(2) 0.041(2) 0.047(2) -0.0033(17) -0.0001(17) 0.0012(16) C12 0.052(2) 0.036(2) 0.042(2) 0.0064(16) 0.0021(17) 0.0005(17) C13 0.057(3) 0.034(2) 0.057(3) 0.0075(18) -0.005(2) 0.0046(18) C14 0.058(3) 0.039(2) 0.046(2) -0.0039(17) -0.0059(19) 0.0121(18) C15 0.056(3) 0.044(2) 0.048(2) 0.0020(18) -0.0040(19) 0.0136(19) C16 0.049(2) 0.046(2) 0.042(2) 0.0008(17) -0.0063(18) 0.0062(18) C17 0.061(3) 0.046(2) 0.038(2) 0.0056(17) 0.0010(18) 0.0030(19) C18 0.041(2) 0.051(2) 0.049(2) 0.0064(18) 0.0057(17) -0.0052(18) C19 0.0361(19) 0.0363(19) 0.043(2) 0.0067(15) 0.0034(15) 0.0000(15) C20 0.041(2) 0.044(2) 0.048(2) 0.0107(17) -0.0023(17) -0.0028(17) C21 0.043(2) 0.040(2) 0.072(3) 0.004(2) -0.004(2) -0.0027(17) C22 0.049(2) 0.054(2) 0.046(2) 0.0097(19) 0.0034(18) 0.0002(19) C23 0.034(2) 0.053(2) 0.069(3) 0.023(2) -0.0061(19) -0.0050(17) C24 0.045(2) 0.048(3) 0.086(4) 0.006(2) 0.001(2) 0.006(2) C25 0.043(2) 0.040(2) 0.086(3) 0.012(2) -0.010(2) -0.0027(18) C26 0.047(2) 0.062(3) 0.083(4) 0.025(3) -0.011(2) -0.006(2) C27 0.056(3) 0.060(3) 0.057(3) 0.018(2) -0.012(2) 0.002(2) C28 0.049(2) 0.059(3) 0.065(3) 0.016(2) -0.016(2) -0.002(2) C29 0.0303(18) 0.0365(19) 0.042(2) -0.0015(15) -0.0103(15) -0.0006(14) C30 0.0273(17) 0.0341(18) 0.0420(19) -0.0038(14) -0.0043(14) -0.0033(13) C31 0.0317(18) 0.0379(19) 0.047(2) -0.0008(16) -0.0048(16) -0.0008(15) C32 0.0331(18) 0.0384(19) 0.042(2) 0.0025(15) -0.0031(15) -0.0056(15) C33 0.0306(18) 0.0358(19) 0.052(2) 0.0002(16) -0.0058(16) 0.0012(14) C34 0.0312(18) 0.0325(18) 0.049(2) -0.0016(15) -0.0059(15) -0.0012(14) C35 0.0294(17) 0.0341(18) 0.046(2) -0.0047(15) -0.0046(15) -0.0002(14) C36 0.0367(19) 0.0331(19) 0.047(2) -0.0052(15) -0.0059(16) 0.0027(14) C37 0.0365(19) 0.042(2) 0.044(2) -0.0053(16) -0.0023(16) -0.0068(16) C38 0.036(2) 0.040(2) 0.051(2) -0.0008(17) -0.0007(17) -0.0009(16) C39 0.041(2) 0.036(2) 0.049(2) -0.0022(16) -0.0018(17) 0.0050(16) C40 0.050(2) 0.035(2) 0.058(3) -0.0022(18) 0.0052(19) -0.0025(17) C41 0.041(2) 0.040(2) 0.051(2) -0.0093(17) 0.0005(17) -0.0072(16) C42 0.049(2) 0.042(2) 0.052(2) -0.0059(18) -0.0027(19) 0.0065(18) C43 0.043(2) 0.054(2) 0.048(2) -0.0052(19) 0.0106(18) 0.0049(18) C44 0.0322(19) 0.045(2) 0.065(3) 0.0011(19) -0.0032(18) 0.0060(16) C45 0.040(2) 0.053(2) 0.051(2) 0.0070(19) -0.0051(18) 0.0035(18) C46 0.041(7) 0.046(7) 0.039(11) -0.006(5) -0.010(6) 0.014(6) C47 0.038(3) 0.036(3) 0.040(3) 0.003(2) 0.003(3) 0.005(2) C48 0.040(3) 0.041(3) 0.040(3) 0.000(2) -0.004(3) -0.001(3) C49 0.045(3) 0.052(4) 0.041(3) -0.003(3) -0.006(3) 0.014(3) C50 0.035(4) 0.048(4) 0.046(4) 0.008(3) 0.002(3) 0.012(3) C51 0.056(5) 0.038(4) 0.040(4) -0.005(3) -0.004(3) 0.005(3) C52 0.056(4) 0.036(3) 0.046(4) -0.005(3) -0.004(3) 0.002(3) C53 0.068(6) 0.038(5) 0.048(5) 0.001(4) -0.002(4) 0.023(4) C54 0.061(5) 0.053(5) 0.039(4) -0.002(4) -0.009(3) 0.012(5) C55 0.041(4) 0.061(5) 0.057(5) -0.011(5) 0.009(4) 0.014(3) C56 0.033(8) 0.023(8) 0.022(9) -0.002(6) -0.015(7) -0.010(7) C57 0.063(8) 0.054(7) 0.033(6) -0.001(5) -0.010(5) 0.003(6) C58 0.089(10) 0.037(6) 0.043(7) 0.000(5) -0.002(7) 0.005(6) C59 0.040(6) 0.067(8) 0.051(7) 0.011(6) 0.007(5) 0.015(5) C60 0.093(12) 0.046(10) 0.039(7) -0.005(7) -0.010(9) 0.005(9) C61 0.123(13) 0.048(8) 0.056(8) -0.011(7) 0.007(9) 0.024(8) C62 0.131(16) 0.053(11) 0.054(10) -0.012(7) -0.002(12) 0.044(10) C63 0.144(15) 0.070(11) 0.050(10) 0.012(10) 0.026(10) 0.057(14) C64 0.072(10) 0.099(12) 0.068(10) 0.005(11) 0.010(9) 0.048(8) C65 0.092(11) 0.085(11) 0.060(9) 0.022(8) -0.002(9) 0.035(9) C66 0.104(5) 0.079(4) 0.096(5) -0.004(3) -0.002(4) 0.008(4) C67 0.070(3) 0.045(3) 0.071(3) 0.000(2) 0.004(3) -0.015(2) C68 0.088(4) 0.054(3) 0.053(3) -0.007(2) 0.014(3) -0.021(3) C69 0.082(4) 0.059(3) 0.059(3) 0.003(2) 0.004(3) -0.015(3) C70 0.079(4) 0.064(3) 0.077(4) -0.001(3) 0.006(3) -0.016(3) C71 0.085(4) 0.065(4) 0.095(5) -0.007(3) 0.023(4) -0.008(3) C72 0.080(3) 0.060(3) 0.046(3) -0.009(2) 0.009(2) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O2 1.931(2) . ? Nb1 O3 1.946(2) . ? Nb1 O1 1.973(2) . ? Nb1 C1 2.131(4) . ? Nb1 Nb1 2.7188(9) 2_655 ? Nb2 O1 1.913(3) . ? Nb2 O2 2.024(3) . ? Nb2 O3 2.075(3) 2_655 ? Nb2 C1 2.185(4) . ? Nb2 Nb2 2.703(3) 2_655 ? C1 Nb1 2.131(4) 2_655 ? C1 Nb2 2.185(4) 2_655 ? O1 Nb2 1.913(3) 2_655 ? O1 Nb1 1.973(2) 2_655 ? O2 C2 1.374(4) . ? O3 C29 1.378(4) . ? O3 Nb2 2.075(3) 2_655 ? C2 C7 1.419(5) . ? C2 C3 1.430(5) . ? C3 C4 1.399(5) . ? C3 C8 1.550(5) . ? C4 C5 1.388(5) . ? C4 H1 0.9500 . ? C5 C6 1.375(5) . ? C5 C18 1.503(5) . ? C6 C7 1.406(5) . ? C6 H2 0.9500 . ? C7 C19 1.556(5) . ? C8 C9 1.541(5) . ? C8 C11 1.550(5) . ? C8 C10 1.560(5) . ? C9 C12 1.532(5) . ? C9 H3 0.9900 . ? C9 H4 0.9900 . ? C10 C14 1.537(5) . ? C10 H5 0.9900 . ? C10 H6 0.9900 . ? C11 C16 1.540(5) . ? C11 H7 0.9900 . ? C11 H8 0.9900 . ? C12 C17 1.525(6) . ? C12 C13 1.528(6) . ? C12 H9 1.0000 . ? C13 C14 1.523(6) . ? C13 H10 0.9900 . ? C13 H11 0.9900 . ? C14 C15 1.534(6) . ? C14 H12 1.0000 . ? C15 C16 1.531(6) . ? C15 H13 0.9900 . ? C15 H14 0.9900 . ? C16 C17 1.528(6) . ? C16 H15 1.0000 . ? C17 H16 0.9900 . ? C17 H17 0.9900 . ? C18 H18 0.9800 . ? C18 H19 0.9800 . ? C18 H20 0.9800 . ? C19 C20 1.529(5) . ? C19 C21 1.539(5) . ? C19 C22 1.568(6) . ? C20 C23 1.546(5) . ? C20 H21 0.9900 . ? C20 H22 0.9900 . ? C21 C25 1.546(6) . ? C21 H23 0.9900 . ? C21 H24 0.9900 . ? C22 C27 1.543(6) . ? C22 H25 0.9900 . ? C22 H26 0.9900 . ? C23 C28 1.512(7) . ? C23 C24 1.538(6) . ? C23 H27 1.0000 . ? C24 C25 1.533(6) . ? C24 H28 0.9900 . ? C24 H29 0.9900 . ? C25 C26 1.523(7) . ? C25 H30 1.0000 . ? C26 C27 1.527(7) . ? C26 H31 0.9900 . ? C26 H32 0.9900 . ? C27 C28 1.515(6) . ? C27 H33 1.0000 . ? C28 H34 0.9900 . ? C28 H35 0.9900 . ? C29 C30 1.415(5) . ? C29 C34 1.440(5) . ? C30 C31 1.395(5) . ? C30 C35 1.545(5) . ? C31 C32 1.385(5) . ? C31 H36 0.9500 . ? C32 C33 1.384(5) . ? C32 C45 1.501(5) . ? C33 C34 1.400(5) . ? C33 H37 0.9500 . ? C34 C56 1.45(5) . ? C34 C46 1.60(3) . ? C35 C36 1.535(5) . ? C35 C37 1.553(5) . ? C35 C38 1.564(5) . ? C36 C39 1.547(5) . ? C36 H38 0.9900 . ? C36 H39 0.9900 . ? C37 C41 1.525(5) . ? C37 H40 0.9900 . ? C37 H41 0.9900 . ? C38 C43 1.538(6) . ? C38 H42 0.9900 . ? C38 H43 0.9900 . ? C39 C40 1.531(5) . ? C39 C44 1.532(6) . ? C39 H44 1.0000 . ? C40 C41 1.520(6) . ? C40 H45 0.9900 . ? C40 H46 0.9900 . ? C41 C42 1.533(6) . ? C41 H47 1.0000 . ? C42 C43 1.523(6) . ? C42 H48 0.9900 . ? C42 H49 0.9900 . ? C43 C44 1.520(6) . ? C43 H50 1.0000 . ? C44 H51 0.9900 . ? C44 H52 0.9900 . ? C45 H53 0.9800 . ? C45 H54 0.9800 . ? C45 H55 0.9800 . ? C46 C47 1.41(3) . ? C46 C48 1.51(2) . ? C46 C49 1.60(3) . ? C47 C50 1.538(9) . ? C47 H56 0.9900 . ? C47 H57 0.9900 . ? C48 C52 1.542(9) . ? C48 H58 0.9900 . ? C48 H59 0.9900 . ? C49 C54 1.544(11) . ? C49 H60 0.9900 . ? C49 H61 0.9900 . ? C50 C55 1.516(10) . ? C50 C51 1.524(10) . ? C50 H62 1.0000 . ? C51 C52 1.507(10) . ? C51 H63 0.9900 . ? C51 H64 0.9900 . ? C52 C53 1.509(12) . ? C52 H65 1.0000 . ? C53 C54 1.544(16) . ? C53 H66 0.9900 . ? C53 H67 0.9900 . ? C54 C55 1.539(13) . ? C54 H68 1.0000 . ? C55 H69 0.9900 . ? C55 H70 0.9900 . ? C56 C58 1.50(4) . ? C56 C59 1.62(5) . ? C56 C57 1.78(5) . ? C57 C60 1.53(2) . ? C57 H71 0.9900 . ? C57 H72 0.9900 . ? C58 C62 1.50(2) . ? C58 H73 0.9900 . ? C58 H74 0.9900 . ? C59 C64 1.54(2) . ? C59 H75 0.9900 . ? C59 H76 0.9900 . ? C60 C61 1.49(2) . ? C60 C65 1.49(3) . ? C60 H77 1.0000 . ? C61 C62 1.47(3) . ? C61 H78 0.9900 . ? C61 H79 0.9900 . ? C62 C63 1.40(4) . ? C62 H80 1.0000 . ? C63 C64 1.62(3) . ? C63 H81 0.9900 . ? C63 H82 0.9900 . ? C64 C65 1.54(2) . ? C64 H83 1.0000 . ? C65 H84 0.9900 . ? C65 H85 0.9900 . ? C66 C67 1.467(8) . ? C66 H86 0.9800 . ? C66 H87 0.9800 . ? C66 H88 0.9800 . ? C67 C72 1.373(7) . ? C67 C68 1.413(7) . ? C68 C69 1.344(8) . ? C68 H89 0.9500 . ? C69 C70 1.387(8) . ? C69 H90 0.9500 . ? C70 C71 1.353(8) . ? C70 H91 0.9500 . ? C71 C72 1.389(8) . ? C71 H92 0.9500 . ? C72 H93 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O3 141.55(11) . . ? O2 Nb1 O1 100.69(7) . . ? O3 Nb1 O1 101.82(8) . . ? O2 Nb1 C1 104.02(8) . . ? O3 Nb1 C1 103.77(8) . . ? O1 Nb1 C1 96.82(11) . . ? O2 Nb1 Nb1 108.70(8) . 2_655 ? O3 Nb1 Nb1 109.43(8) . 2_655 ? O1 Nb1 Nb1 46.44(7) . 2_655 ? C1 Nb1 Nb1 50.37(8) . 2_655 ? O1 Nb2 O2 99.50(9) . . ? O1 Nb2 O3 99.32(9) . 2_655 ? O2 Nb2 O3 152.96(12) . 2_655 ? O1 Nb2 C1 96.86(12) . . ? O2 Nb2 C1 99.08(9) . . ? O3 Nb2 C1 97.76(9) 2_655 . ? O1 Nb2 Nb2 45.06(8) . 2_655 ? O2 Nb2 Nb2 104.07(10) . 2_655 ? O3 Nb2 Nb2 102.97(10) 2_655 2_655 ? C1 Nb2 Nb2 51.80(8) . 2_655 ? Nb1 C1 Nb1 79.26(16) . 2_655 ? Nb1 C1 Nb2 53.00(10) . 2_655 ? Nb1 C1 Nb2 52.51(10) 2_655 2_655 ? Nb1 C1 Nb2 52.51(10) . . ? Nb1 C1 Nb2 53.00(10) 2_655 . ? Nb2 C1 Nb2 76.41(17) 2_655 . ? Nb2 O1 Nb2 89.88(16) 2_655 . ? Nb2 O1 Nb1 58.86(9) 2_655 2_655 ? Nb2 O1 Nb1 59.41(9) . 2_655 ? Nb2 O1 Nb1 59.41(9) 2_655 . ? Nb2 O1 Nb1 58.86(9) . . ? Nb1 O1 Nb1 87.11(14) 2_655 . ? C2 O2 Nb1 161.8(2) . . ? C2 O2 Nb2 138.3(2) . . ? Nb1 O2 Nb2 57.70(7) . . ? C29 O3 Nb1 142.3(2) . . ? C29 O3 Nb2 159.9(2) . 2_655 ? Nb1 O3 Nb2 57.14(7) . 2_655 ? O2 C2 C7 119.5(3) . . ? O2 C2 C3 120.2(3) . . ? C7 C2 C3 120.3(3) . . ? C4 C3 C2 117.5(3) . . ? C4 C3 C8 114.5(3) . . ? C2 C3 C8 128.0(3) . . ? C5 C4 C3 123.4(3) . . ? C5 C4 H1 118.3 . . ? C3 C4 H1 118.3 . . ? C6 C5 C4 117.2(3) . . ? C6 C5 C18 121.6(3) . . ? C4 C5 C18 121.1(3) . . ? C5 C6 C7 123.9(3) . . ? C5 C6 H2 118.0 . . ? C7 C6 H2 118.0 . . ? C6 C7 C2 117.1(3) . . ? C6 C7 C19 114.9(3) . . ? C2 C7 C19 127.9(3) . . ? C9 C8 C11 107.3(3) . . ? C9 C8 C3 115.8(3) . . ? C11 C8 C3 110.3(3) . . ? C9 C8 C10 107.3(3) . . ? C11 C8 C10 107.2(3) . . ? C3 C8 C10 108.5(3) . . ? C12 C9 C8 111.7(3) . . ? C12 C9 H3 109.3 . . ? C8 C9 H3 109.3 . . ? C12 C9 H4 109.3 . . ? C8 C9 H4 109.3 . . ? H3 C9 H4 107.9 . . ? C14 C10 C8 111.1(3) . . ? C14 C10 H5 109.4 . . ? C8 C10 H5 109.4 . . ? C14 C10 H6 109.4 . . ? C8 C10 H6 109.4 . . ? H5 C10 H6 108.0 . . ? C16 C11 C8 111.3(3) . . ? C16 C11 H7 109.4 . . ? C8 C11 H7 109.4 . . ? C16 C11 H8 109.4 . . ? C8 C11 H8 109.4 . . ? H7 C11 H8 108.0 . . ? C17 C12 C13 110.3(3) . . ? C17 C12 C9 108.5(3) . . ? C13 C12 C9 110.1(3) . . ? C17 C12 H9 109.3 . . ? C13 C12 H9 109.3 . . ? C9 C12 H9 109.3 . . ? C14 C13 C12 109.0(3) . . ? C14 C13 H10 109.9 . . ? C12 C13 H10 109.9 . . ? C14 C13 H11 109.9 . . ? C12 C13 H11 109.9 . . ? H10 C13 H11 108.3 . . ? C13 C14 C15 110.3(4) . . ? C13 C14 C10 109.7(3) . . ? C15 C14 C10 109.5(3) . . ? C13 C14 H12 109.1 . . ? C15 C14 H12 109.1 . . ? C10 C14 H12 109.1 . . ? C16 C15 C14 108.5(3) . . ? C16 C15 H13 110.0 . . ? C14 C15 H13 110.0 . . ? C16 C15 H14 110.0 . . ? C14 C15 H14 110.0 . . ? H13 C15 H14 108.4 . . ? C17 C16 C15 111.1(4) . . ? C17 C16 C11 108.7(3) . . ? C15 C16 C11 109.3(3) . . ? C17 C16 H15 109.2 . . ? C15 C16 H15 109.2 . . ? C11 C16 H15 109.2 . . ? C12 C17 C16 109.2(3) . . ? C12 C17 H16 109.8 . . ? C16 C17 H16 109.8 . . ? C12 C17 H17 109.8 . . ? C16 C17 H17 109.8 . . ? H16 C17 H17 108.3 . . ? C5 C18 H18 109.5 . . ? C5 C18 H19 109.5 . . ? H18 C18 H19 109.5 . . ? C5 C18 H20 109.5 . . ? H18 C18 H20 109.5 . . ? H19 C18 H20 109.5 . . ? C20 C19 C21 107.9(3) . . ? C20 C19 C7 117.3(3) . . ? C21 C19 C7 111.2(3) . . ? C20 C19 C22 104.7(3) . . ? C21 C19 C22 108.2(3) . . ? C7 C19 C22 107.1(3) . . ? C19 C20 C23 112.0(3) . . ? C19 C20 H21 109.2 . . ? C23 C20 H21 109.2 . . ? C19 C20 H22 109.2 . . ? C23 C20 H22 109.2 . . ? H21 C20 H22 107.9 . . ? C19 C21 C25 112.0(3) . . ? C19 C21 H23 109.2 . . ? C25 C21 H23 109.2 . . ? C19 C21 H24 109.2 . . ? C25 C21 H24 109.2 . . ? H23 C21 H24 107.9 . . ? C27 C22 C19 112.2(4) . . ? C27 C22 H25 109.2 . . ? C19 C22 H25 109.2 . . ? C27 C22 H26 109.2 . . ? C19 C22 H26 109.2 . . ? H25 C22 H26 107.9 . . ? C28 C23 C24 109.4(4) . . ? C28 C23 C20 110.3(4) . . ? C24 C23 C20 109.4(4) . . ? C28 C23 H27 109.3 . . ? C24 C23 H27 109.3 . . ? C20 C23 H27 109.3 . . ? C25 C24 C23 109.3(4) . . ? C25 C24 H28 109.8 . . ? C23 C24 H28 109.8 . . ? C25 C24 H29 109.8 . . ? C23 C24 H29 109.8 . . ? H28 C24 H29 108.3 . . ? C26 C25 C24 109.6(4) . . ? C26 C25 C21 109.4(4) . . ? C24 C25 C21 108.3(4) . . ? C26 C25 H30 109.8 . . ? C24 C25 H30 109.8 . . ? C21 C25 H30 109.8 . . ? C25 C26 C27 110.3(4) . . ? C25 C26 H31 109.6 . . ? C27 C26 H31 109.6 . . ? C25 C26 H32 109.6 . . ? C27 C26 H32 109.6 . . ? H31 C26 H32 108.1 . . ? C28 C27 C26 110.3(4) . . ? C28 C27 C22 109.0(4) . . ? C26 C27 C22 108.4(4) . . ? C28 C27 H33 109.7 . . ? C26 C27 H33 109.7 . . ? C22 C27 H33 109.7 . . ? C23 C28 C27 109.3(4) . . ? C23 C28 H34 109.8 . . ? C27 C28 H34 109.8 . . ? C23 C28 H35 109.8 . . ? C27 C28 H35 109.8 . . ? H34 C28 H35 108.3 . . ? O3 C29 C30 120.7(3) . . ? O3 C29 C34 118.3(3) . . ? C30 C29 C34 121.0(3) . . ? C31 C30 C29 116.8(3) . . ? C31 C30 C35 114.8(3) . . ? C29 C30 C35 128.2(3) . . ? C32 C31 C30 124.1(4) . . ? C32 C31 H36 118.0 . . ? C30 C31 H36 118.0 . . ? C33 C32 C31 117.0(3) . . ? C33 C32 C45 121.5(3) . . ? C31 C32 C45 121.5(4) . . ? C32 C33 C34 123.8(3) . . ? C32 C33 H37 118.1 . . ? C34 C33 H37 118.1 . . ? C33 C34 C29 116.2(3) . . ? C33 C34 C56 114(2) . . ? C29 C34 C56 130(2) . . ? C33 C34 C46 120.5(10) . . ? C29 C34 C46 123.2(10) . . ? C36 C35 C30 116.6(3) . . ? C36 C35 C37 107.6(3) . . ? C30 C35 C37 106.9(3) . . ? C36 C35 C38 106.7(3) . . ? C30 C35 C38 111.1(3) . . ? C37 C35 C38 107.5(3) . . ? C35 C36 C39 111.4(3) . . ? C35 C36 H38 109.3 . . ? C39 C36 H38 109.3 . . ? C35 C36 H39 109.3 . . ? C39 C36 H39 109.3 . . ? H38 C36 H39 108.0 . . ? C41 C37 C35 112.3(3) . . ? C41 C37 H40 109.1 . . ? C35 C37 H40 109.1 . . ? C41 C37 H41 109.1 . . ? C35 C37 H41 109.1 . . ? H40 C37 H41 107.9 . . ? C43 C38 C35 110.8(3) . . ? C43 C38 H42 109.5 . . ? C35 C38 H42 109.5 . . ? C43 C38 H43 109.5 . . ? C35 C38 H43 109.5 . . ? H42 C38 H43 108.1 . . ? C40 C39 C44 109.5(3) . . ? C40 C39 C36 110.0(3) . . ? C44 C39 C36 108.5(3) . . ? C40 C39 H44 109.6 . . ? C44 C39 H44 109.6 . . ? C36 C39 H44 109.6 . . ? C41 C40 C39 109.7(3) . . ? C41 C40 H45 109.7 . . ? C39 C40 H45 109.7 . . ? C41 C40 H46 109.7 . . ? C39 C40 H46 109.7 . . ? H45 C40 H46 108.2 . . ? C40 C41 C37 109.2(3) . . ? C40 C41 C42 110.2(3) . . ? C37 C41 C42 108.3(3) . . ? C40 C41 H47 109.7 . . ? C37 C41 H47 109.7 . . ? C42 C41 H47 109.7 . . ? C43 C42 C41 109.7(3) . . ? C43 C42 H48 109.7 . . ? C41 C42 H48 109.7 . . ? C43 C42 H49 109.7 . . ? C41 C42 H49 109.7 . . ? H48 C42 H49 108.2 . . ? C44 C43 C42 110.8(4) . . ? C44 C43 C38 108.9(3) . . ? C42 C43 C38 109.2(3) . . ? C44 C43 H50 109.3 . . ? C42 C43 H50 109.3 . . ? C38 C43 H50 109.3 . . ? C43 C44 C39 109.6(3) . . ? C43 C44 H51 109.8 . . ? C39 C44 H51 109.8 . . ? C43 C44 H52 109.8 . . ? C39 C44 H52 109.8 . . ? H51 C44 H52 108.2 . . ? C32 C45 H53 109.5 . . ? C32 C45 H54 109.5 . . ? H53 C45 H54 109.5 . . ? C32 C45 H55 109.5 . . ? H53 C45 H55 109.5 . . ? H54 C45 H55 109.5 . . ? C47 C46 C48 118.1(18) . . ? C47 C46 C34 108.9(16) . . ? C48 C46 C34 108.6(16) . . ? C47 C46 C49 110.1(17) . . ? C48 C46 C49 106.0(15) . . ? C34 C46 C49 104.2(15) . . ? C46 C47 C50 108.9(12) . . ? C46 C47 H56 109.9 . . ? C50 C47 H56 109.9 . . ? C46 C47 H57 109.9 . . ? C50 C47 H57 109.9 . . ? H56 C47 H57 108.3 . . ? C46 C48 C52 105.8(11) . . ? C46 C48 H58 110.6 . . ? C52 C48 H58 110.6 . . ? C46 C48 H59 110.6 . . ? C52 C48 H59 110.6 . . ? H58 C48 H59 108.7 . . ? C54 C49 C46 107.1(11) . . ? C54 C49 H60 110.3 . . ? C46 C49 H60 110.3 . . ? C54 C49 H61 110.3 . . ? C46 C49 H61 110.3 . . ? H60 C49 H61 108.6 . . ? C55 C50 C51 110.3(7) . . ? C55 C50 C47 109.3(6) . . ? C51 C50 C47 109.2(6) . . ? C55 C50 H62 109.3 . . ? C51 C50 H62 109.3 . . ? C47 C50 H62 109.3 . . ? C52 C51 C50 109.4(6) . . ? C52 C51 H63 109.8 . . ? C50 C51 H63 109.8 . . ? C52 C51 H64 109.8 . . ? C50 C51 H64 109.8 . . ? H63 C51 H64 108.2 . . ? C51 C52 C53 109.7(7) . . ? C51 C52 C48 110.6(6) . . ? C53 C52 C48 110.2(7) . . ? C51 C52 H65 108.8 . . ? C53 C52 H65 108.8 . . ? C48 C52 H65 108.8 . . ? C52 C53 C54 109.6(8) . . ? C52 C53 H66 109.7 . . ? C54 C53 H66 109.7 . . ? C52 C53 H67 109.7 . . ? C54 C53 H67 109.7 . . ? H66 C53 H67 108.2 . . ? C55 C54 C49 109.7(7) . . ? C55 C54 C53 109.0(8) . . ? C49 C54 C53 107.8(8) . . ? C55 C54 H68 110.1 . . ? C49 C54 H68 110.1 . . ? C53 C54 H68 110.1 . . ? C50 C55 C54 108.9(6) . . ? C50 C55 H69 109.9 . . ? C54 C55 H69 109.9 . . ? C50 C55 H70 109.9 . . ? C54 C55 H70 109.9 . . ? H69 C55 H70 108.3 . . ? C34 C56 C58 120(3) . . ? C34 C56 C59 114(3) . . ? C58 C56 C59 109(3) . . ? C34 C56 C57 118(3) . . ? C58 C56 C57 97(3) . . ? C59 C56 C57 94(2) . . ? C60 C57 C56 115(2) . . ? C60 C57 H71 108.4 . . ? C56 C57 H71 108.4 . . ? C60 C57 H72 108.4 . . ? C56 C57 H72 108.4 . . ? H71 C57 H72 107.5 . . ? C56 C58 C62 119(3) . . ? C56 C58 H73 107.5 . . ? C62 C58 H73 107.5 . . ? C56 C58 H74 107.5 . . ? C62 C58 H74 107.5 . . ? H73 C58 H74 107.0 . . ? C64 C59 C56 115(2) . . ? C64 C59 H75 108.5 . . ? C56 C59 H75 108.5 . . ? C64 C59 H76 108.5 . . ? C56 C59 H76 108.5 . . ? H75 C59 H76 107.5 . . ? C61 C60 C65 106.2(16) . . ? C61 C60 C57 110.0(16) . . ? C65 C60 C57 109.3(17) . . ? C61 C60 H77 110.4 . . ? C65 C60 H77 110.4 . . ? C57 C60 H77 110.4 . . ? C62 C61 C60 113.4(18) . . ? C62 C61 H78 108.9 . . ? C60 C61 H78 108.9 . . ? C62 C61 H79 108.9 . . ? C60 C61 H79 108.9 . . ? H78 C61 H79 107.7 . . ? C63 C62 C61 106(3) . . ? C63 C62 C58 111(2) . . ? C61 C62 C58 112.7(19) . . ? C63 C62 H80 109.0 . . ? C61 C62 H80 109.0 . . ? C58 C62 H80 109.0 . . ? C62 C63 C64 111(2) . . ? C62 C63 H81 109.4 . . ? C64 C63 H81 109.4 . . ? C62 C63 H82 109.4 . . ? C64 C63 H82 109.4 . . ? H81 C63 H82 108.0 . . ? C59 C64 C65 109.2(14) . . ? C59 C64 C63 108.3(17) . . ? C65 C64 C63 107(2) . . ? C59 C64 H83 110.8 . . ? C65 C64 H83 110.8 . . ? C63 C64 H83 110.8 . . ? C60 C65 C64 110.0(18) . . ? C60 C65 H84 109.7 . . ? C64 C65 H84 109.7 . . ? C60 C65 H85 109.7 . . ? C64 C65 H85 109.7 . . ? H84 C65 H85 108.2 . . ? C67 C66 H86 109.5 . . ? C67 C66 H87 109.5 . . ? H86 C66 H87 109.5 . . ? C67 C66 H88 109.5 . . ? H86 C66 H88 109.5 . . ? H87 C66 H88 109.5 . . ? C72 C67 C68 117.1(5) . . ? C72 C67 C66 121.3(5) . . ? C68 C67 C66 121.5(5) . . ? C69 C68 C67 120.0(5) . . ? C69 C68 H89 120.0 . . ? C67 C68 H89 120.0 . . ? C68 C69 C70 122.8(5) . . ? C68 C69 H90 118.6 . . ? C70 C69 H90 118.6 . . ? C71 C70 C69 117.6(6) . . ? C71 C70 H91 121.2 . . ? C69 C70 H91 121.2 . . ? C70 C71 C72 121.1(6) . . ? C70 C71 H92 119.4 . . ? C72 C71 H92 119.4 . . ? C67 C72 C71 121.4(5) . . ? C67 C72 H93 119.3 . . ? C71 C72 H93 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Nb1 C1 Nb1 102.85(8) . . . 2_655 ? O3 Nb1 C1 Nb1 -103.99(9) . . . 2_655 ? O1 Nb1 C1 Nb1 0.0 . . . 2_655 ? O2 Nb1 C1 Nb2 153.60(9) . . . 2_655 ? O3 Nb1 C1 Nb2 -53.23(10) . . . 2_655 ? O1 Nb1 C1 Nb2 50.75(5) . . . 2_655 ? Nb1 Nb1 C1 Nb2 50.75(5) 2_655 . . 2_655 ? O2 Nb1 C1 Nb2 51.64(10) . . . . ? O3 Nb1 C1 Nb2 -155.19(10) . . . . ? O1 Nb1 C1 Nb2 -51.21(5) . . . . ? Nb1 Nb1 C1 Nb2 -51.21(5) 2_655 . . . ? O1 Nb2 C1 Nb1 53.49(5) . . . . ? O2 Nb2 C1 Nb1 -47.32(9) . . . . ? O3 Nb2 C1 Nb1 153.92(10) 2_655 . . . ? Nb2 Nb2 C1 Nb1 53.49(5) 2_655 . . . ? O1 Nb2 C1 Nb1 -53.00(5) . . . 2_655 ? O2 Nb2 C1 Nb1 -153.81(10) . . . 2_655 ? O3 Nb2 C1 Nb1 47.43(9) 2_655 . . 2_655 ? Nb2 Nb2 C1 Nb1 -53.00(5) 2_655 . . 2_655 ? O1 Nb2 C1 Nb2 0.0 . . . 2_655 ? O2 Nb2 C1 Nb2 -100.81(10) . . . 2_655 ? O3 Nb2 C1 Nb2 100.43(9) 2_655 . . 2_655 ? O2 Nb2 O1 Nb2 100.44(9) . . . 2_655 ? O3 Nb2 O1 Nb2 -99.06(10) 2_655 . . 2_655 ? C1 Nb2 O1 Nb2 0.0 . . . 2_655 ? O2 Nb2 O1 Nb1 153.61(10) . . . 2_655 ? O3 Nb2 O1 Nb1 -45.89(9) 2_655 . . 2_655 ? C1 Nb2 O1 Nb1 53.17(4) . . . 2_655 ? Nb2 Nb2 O1 Nb1 53.17(4) 2_655 . . 2_655 ? O2 Nb2 O1 Nb1 46.83(9) . . . . ? O3 Nb2 O1 Nb1 -152.68(10) 2_655 . . . ? C1 Nb2 O1 Nb1 -53.61(4) . . . . ? Nb2 Nb2 O1 Nb1 -53.61(4) 2_655 . . . ? O2 Nb1 O1 Nb2 -160.85(9) . . . 2_655 ? O3 Nb1 O1 Nb2 50.53(10) . . . 2_655 ? C1 Nb1 O1 Nb2 -55.13(6) . . . 2_655 ? Nb1 Nb1 O1 Nb2 -55.13(6) 2_655 . . 2_655 ? O2 Nb1 O1 Nb2 -50.10(10) . . . . ? O3 Nb1 O1 Nb2 161.27(9) . . . . ? C1 Nb1 O1 Nb2 55.61(6) . . . . ? Nb1 Nb1 O1 Nb2 55.61(6) 2_655 . . . ? O2 Nb1 O1 Nb1 -105.71(8) . . . 2_655 ? O3 Nb1 O1 Nb1 105.66(8) . . . 2_655 ? C1 Nb1 O1 Nb1 0.0 . . . 2_655 ? O3 Nb1 O2 C2 -33.1(8) . . . . ? O1 Nb1 O2 C2 -158.1(7) . . . . ? C1 Nb1 O2 C2 102.1(7) . . . . ? Nb1 Nb1 O2 C2 154.5(7) 2_655 . . . ? O3 Nb1 O2 Nb2 172.21(14) . . . . ? O1 Nb1 O2 Nb2 47.25(9) . . . . ? C1 Nb1 O2 Nb2 -52.63(10) . . . . ? Nb1 Nb1 O2 Nb2 -0.18(7) 2_655 . . . ? O1 Nb2 O2 C2 142.6(3) . . . . ? O3 Nb2 O2 C2 9.0(5) 2_655 . . . ? C1 Nb2 O2 C2 -118.8(3) . . . . ? Nb2 Nb2 O2 C2 -171.5(3) 2_655 . . . ? O1 Nb2 O2 Nb1 -48.97(9) . . . . ? O3 Nb2 O2 Nb1 177.5(2) 2_655 . . . ? C1 Nb2 O2 Nb1 49.61(10) . . . . ? Nb2 Nb2 O2 Nb1 -3.11(6) 2_655 . . . ? O2 Nb1 O3 C29 15.6(4) . . . . ? O1 Nb1 O3 C29 140.2(3) . . . . ? C1 Nb1 O3 C29 -119.6(3) . . . . ? Nb1 Nb1 O3 C29 -172.0(3) 2_655 . . . ? O2 Nb1 O3 Nb2 -171.47(13) . . . 2_655 ? O1 Nb1 O3 Nb2 -46.83(9) . . . 2_655 ? C1 Nb1 O3 Nb2 53.31(10) . . . 2_655 ? Nb1 Nb1 O3 Nb2 0.89(7) 2_655 . . 2_655 ? Nb1 O2 C2 C7 -27.9(9) . . . . ? Nb2 O2 C2 C7 119.2(3) . . . . ? Nb1 O2 C2 C3 155.1(6) . . . . ? Nb2 O2 C2 C3 -57.8(5) . . . . ? O2 C2 C3 C4 170.8(3) . . . . ? C7 C2 C3 C4 -6.2(5) . . . . ? O2 C2 C3 C8 -10.9(6) . . . . ? C7 C2 C3 C8 172.2(3) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C8 C3 C4 C5 -179.1(3) . . . . ? C3 C4 C5 C6 4.8(6) . . . . ? C3 C4 C5 C18 -178.5(4) . . . . ? C4 C5 C6 C7 -2.6(6) . . . . ? C18 C5 C6 C7 -179.2(4) . . . . ? C5 C6 C7 C2 -3.8(6) . . . . ? C5 C6 C7 C19 173.2(3) . . . . ? O2 C2 C7 C6 -168.8(3) . . . . ? C3 C2 C7 C6 8.2(5) . . . . ? O2 C2 C7 C19 14.6(5) . . . . ? C3 C2 C7 C19 -168.4(3) . . . . ? C4 C3 C8 C9 -179.7(3) . . . . ? C2 C3 C8 C9 1.9(5) . . . . ? C4 C3 C8 C11 -57.5(4) . . . . ? C2 C3 C8 C11 124.1(4) . . . . ? C4 C3 C8 C10 59.6(4) . . . . ? C2 C3 C8 C10 -118.7(4) . . . . ? C11 C8 C9 C12 57.8(4) . . . . ? C3 C8 C9 C12 -178.5(3) . . . . ? C10 C8 C9 C12 -57.1(4) . . . . ? C9 C8 C10 C14 57.5(4) . . . . ? C11 C8 C10 C14 -57.5(4) . . . . ? C3 C8 C10 C14 -176.6(3) . . . . ? C9 C8 C11 C16 -57.3(4) . . . . ? C3 C8 C11 C16 175.7(3) . . . . ? C10 C8 C11 C16 57.7(4) . . . . ? C8 C9 C12 C17 -61.1(4) . . . . ? C8 C9 C12 C13 59.7(4) . . . . ? C17 C12 C13 C14 60.0(4) . . . . ? C9 C12 C13 C14 -59.7(4) . . . . ? C12 C13 C14 C15 -60.5(4) . . . . ? C12 C13 C14 C10 60.2(4) . . . . ? C8 C10 C14 C13 -60.5(4) . . . . ? C8 C10 C14 C15 60.7(4) . . . . ? C13 C14 C15 C16 59.6(4) . . . . ? C10 C14 C15 C16 -61.3(4) . . . . ? C14 C15 C16 C17 -58.7(4) . . . . ? C14 C15 C16 C11 61.2(4) . . . . ? C8 C11 C16 C17 60.3(4) . . . . ? C8 C11 C16 C15 -61.1(4) . . . . ? C13 C12 C17 C16 -58.8(4) . . . . ? C9 C12 C17 C16 61.9(4) . . . . ? C15 C16 C17 C12 58.6(4) . . . . ? C11 C16 C17 C12 -61.7(4) . . . . ? C6 C7 C19 C20 -173.1(3) . . . . ? C2 C7 C19 C20 3.6(6) . . . . ? C6 C7 C19 C21 62.1(4) . . . . ? C2 C7 C19 C21 -121.2(4) . . . . ? C6 C7 C19 C22 -55.8(4) . . . . ? C2 C7 C19 C22 120.8(4) . . . . ? C21 C19 C20 C23 -56.6(5) . . . . ? C7 C19 C20 C23 177.0(3) . . . . ? C22 C19 C20 C23 58.5(4) . . . . ? C20 C19 C21 C25 57.8(5) . . . . ? C7 C19 C21 C25 -172.3(3) . . . . ? C22 C19 C21 C25 -55.0(5) . . . . ? C20 C19 C22 C27 -59.2(4) . . . . ? C21 C19 C22 C27 55.7(4) . . . . ? C7 C19 C22 C27 175.6(3) . . . . ? C19 C20 C23 C28 -61.3(5) . . . . ? C19 C20 C23 C24 59.0(5) . . . . ? C28 C23 C24 C25 60.7(5) . . . . ? C20 C23 C24 C25 -60.1(5) . . . . ? C23 C24 C25 C26 -58.7(5) . . . . ? C23 C24 C25 C21 60.6(5) . . . . ? C19 C21 C25 C26 58.7(5) . . . . ? C19 C21 C25 C24 -60.7(5) . . . . ? C24 C25 C26 C27 57.6(5) . . . . ? C21 C25 C26 C27 -61.0(5) . . . . ? C25 C26 C27 C28 -58.3(5) . . . . ? C25 C26 C27 C22 61.0(5) . . . . ? C19 C22 C27 C28 61.2(5) . . . . ? C19 C22 C27 C26 -58.9(5) . . . . ? C24 C23 C28 C27 -61.2(5) . . . . ? C20 C23 C28 C27 59.2(5) . . . . ? C26 C27 C28 C23 59.9(5) . . . . ? C22 C27 C28 C23 -59.0(5) . . . . ? Nb1 O3 C29 C30 -57.6(5) . . . . ? Nb2 O3 C29 C30 140.0(5) 2_655 . . . ? Nb1 O3 C29 C34 120.3(4) . . . . ? Nb2 O3 C29 C34 -42.2(8) 2_655 . . . ? O3 C29 C30 C31 167.0(3) . . . . ? C34 C29 C30 C31 -10.8(5) . . . . ? O3 C29 C30 C35 -18.0(6) . . . . ? C34 C29 C30 C35 164.2(3) . . . . ? C29 C30 C31 C32 2.7(5) . . . . ? C35 C30 C31 C32 -173.0(3) . . . . ? C30 C31 C32 C33 5.0(6) . . . . ? C30 C31 C32 C45 -177.8(4) . . . . ? C31 C32 C33 C34 -4.8(6) . . . . ? C45 C32 C33 C34 178.0(4) . . . . ? C32 C33 C34 C29 -2.9(5) . . . . ? C32 C33 C34 C56 175.1(15) . . . . ? C32 C33 C34 C46 176.9(10) . . . . ? O3 C29 C34 C33 -166.9(3) . . . . ? C30 C29 C34 C33 10.9(5) . . . . ? O3 C29 C34 C56 15.4(19) . . . . ? C30 C29 C34 C56 -166.7(18) . . . . ? O3 C29 C34 C46 13.2(11) . . . . ? C30 C29 C34 C46 -168.9(10) . . . . ? C31 C30 C35 C36 -177.0(3) . . . . ? C29 C30 C35 C36 7.9(5) . . . . ? C31 C30 C35 C37 62.6(4) . . . . ? C29 C30 C35 C37 -112.5(4) . . . . ? C31 C30 C35 C38 -54.4(4) . . . . ? C29 C30 C35 C38 130.5(4) . . . . ? C30 C35 C36 C39 -176.2(3) . . . . ? C37 C35 C36 C39 -56.2(4) . . . . ? C38 C35 C36 C39 59.0(4) . . . . ? C36 C35 C37 C41 57.5(4) . . . . ? C30 C35 C37 C41 -176.5(3) . . . . ? C38 C35 C37 C41 -57.1(4) . . . . ? C36 C35 C38 C43 -58.9(4) . . . . ? C30 C35 C38 C43 173.0(3) . . . . ? C37 C35 C38 C43 56.3(4) . . . . ? C35 C36 C39 C40 58.7(4) . . . . ? C35 C36 C39 C44 -61.0(4) . . . . ? C44 C39 C40 C41 59.8(4) . . . . ? C36 C39 C40 C41 -59.3(4) . . . . ? C39 C40 C41 C37 59.6(4) . . . . ? C39 C40 C41 C42 -59.3(4) . . . . ? C35 C37 C41 C40 -60.0(4) . . . . ? C35 C37 C41 C42 60.1(4) . . . . ? C40 C41 C42 C43 58.0(4) . . . . ? C37 C41 C42 C43 -61.5(4) . . . . ? C41 C42 C43 C44 -57.9(4) . . . . ? C41 C42 C43 C38 62.1(4) . . . . ? C35 C38 C43 C44 61.1(4) . . . . ? C35 C38 C43 C42 -60.1(4) . . . . ? C42 C43 C44 C39 58.8(4) . . . . ? C38 C43 C44 C39 -61.3(4) . . . . ? C40 C39 C44 C43 -59.3(4) . . . . ? C36 C39 C44 C43 60.8(4) . . . . ? C33 C34 C46 C47 -131.0(13) . . . . ? C29 C34 C46 C47 48.8(19) . . . . ? C56 C34 C46 C47 -117(19) . . . . ? C33 C34 C46 C48 99.1(15) . . . . ? C29 C34 C46 C48 -81.1(16) . . . . ? C56 C34 C46 C48 114(19) . . . . ? C33 C34 C46 C49 -13.5(16) . . . . ? C29 C34 C46 C49 166.3(7) . . . . ? C56 C34 C46 C49 1(17) . . . . ? C48 C46 C47 C50 -58(2) . . . . ? C34 C46 C47 C50 177.9(11) . . . . ? C49 C46 C47 C50 64.2(16) . . . . ? C47 C46 C48 C52 57(2) . . . . ? C34 C46 C48 C52 -178.7(11) . . . . ? C49 C46 C48 C52 -67.2(15) . . . . ? C47 C46 C49 C54 -61.4(16) . . . . ? C48 C46 C49 C54 67.4(16) . . . . ? C34 C46 C49 C54 -178.0(10) . . . . ? C46 C47 C50 C55 -64.7(14) . . . . ? C46 C47 C50 C51 56.1(13) . . . . ? C55 C50 C51 C52 60.5(9) . . . . ? C47 C50 C51 C52 -59.7(8) . . . . ? C50 C51 C52 C53 -60.5(9) . . . . ? C50 C51 C52 C48 61.2(8) . . . . ? C46 C48 C52 C51 -55.5(12) . . . . ? C46 C48 C52 C53 65.9(13) . . . . ? C51 C52 C53 C54 60.6(10) . . . . ? C48 C52 C53 C54 -61.4(10) . . . . ? C46 C49 C54 C55 56.9(12) . . . . ? C46 C49 C54 C53 -61.6(12) . . . . ? C52 C53 C54 C55 -59.7(10) . . . . ? C52 C53 C54 C49 59.3(10) . . . . ? C51 C50 C55 C54 -59.6(9) . . . . ? C47 C50 C55 C54 60.5(8) . . . . ? C49 C54 C55 C50 -59.1(9) . . . . ? C53 C54 C55 C50 58.8(10) . . . . ? C33 C34 C56 C58 69(4) . . . . ? C29 C34 C56 C58 -113(3) . . . . ? C46 C34 C56 C58 -97(19) . . . . ? C33 C34 C56 C59 -64(3) . . . . ? C29 C34 C56 C59 114(3) . . . . ? C46 C34 C56 C59 130(20) . . . . ? C33 C34 C56 C57 -172.9(16) . . . . ? C29 C34 C56 C57 5(3) . . . . ? C46 C34 C56 C57 21(17) . . . . ? C34 C56 C57 C60 178(2) . . . . ? C58 C56 C57 C60 -53(3) . . . . ? C59 C56 C57 C60 57(2) . . . . ? C34 C56 C58 C62 -176(3) . . . . ? C59 C56 C58 C62 -41(4) . . . . ? C57 C56 C58 C62 56(3) . . . . ? C34 C56 C59 C64 177(2) . . . . ? C58 C56 C59 C64 39(4) . . . . ? C57 C56 C59 C64 -60(2) . . . . ? C56 C57 C60 C61 54(2) . . . . ? C56 C57 C60 C65 -62(2) . . . . ? C65 C60 C61 C62 66(2) . . . . ? C57 C60 C61 C62 -52(3) . . . . ? C60 C61 C62 C63 -68(2) . . . . ? C60 C61 C62 C58 54(3) . . . . ? C56 C58 C62 C63 56(4) . . . . ? C56 C58 C62 C61 -63(4) . . . . ? C61 C62 C63 C64 61(2) . . . . ? C58 C62 C63 C64 -61(3) . . . . ? C56 C59 C64 C65 69(3) . . . . ? C56 C59 C64 C63 -47(3) . . . . ? C62 C63 C64 C59 59(3) . . . . ? C62 C63 C64 C65 -58(2) . . . . ? C61 C60 C65 C64 -59(2) . . . . ? C57 C60 C65 C64 60(2) . . . . ? C59 C64 C65 C60 -62(2) . . . . ? C63 C64 C65 C60 55(2) . . . . ? C72 C67 C68 C69 -0.2(7) . . . . ? C66 C67 C68 C69 179.7(5) . . . . ? C67 C68 C69 C70 -0.5(8) . . . . ? C68 C69 C70 C71 0.4(8) . . . . ? C69 C70 C71 C72 0.4(8) . . . . ? C68 C67 C72 C71 1.0(7) . . . . ? C66 C67 C72 C71 -178.9(5) . . . . ? C70 C71 C72 C67 -1.1(8) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.262 0.250 584 72 ' ' 2 0.000 0.738 0.750 584 72 ' ' 3 0.500 0.762 0.250 584 72 ' ' 4 0.500 0.238 0.750 584 72 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.881 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.082