# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name W.Casey J.C.Fettinger C.A.Ohlin E.M.Villa _publ_contact_author_name 'William Casey' _publ_contact_author_email WHCASEY@UCDAVIS.EDU data_jf1660ffmi _database_code_depnum_ccdc_archive 'CCDC 715295' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Nb9 O28 Ti, 7(C4 H12 N), 22(H2 O)' _chemical_formula_sum 'C28 H128 N7 Nb9 O50 Ti' _chemical_formula_weight 2247.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.583(2) _cell_length_b 19.893(4) _cell_length_c 15.513(3) _cell_angle_alpha 90.020(2) _cell_angle_beta 105.549(2) _cell_angle_gamma 89.966(2) _cell_volume 4038.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9642 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 27.47 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method ? _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 1.416 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5402 _exptl_absorpt_correction_T_max 0.7477 _exptl_absorpt_process_details 'SADABS 2008/3 (Sheldrick, 2008)' _exptl_special_details ; A colorless block with approximate orthogonal dimensions 0.50 x 0.35 x 0.22mm3 was placed and optically centered on the Bruker APEX II1 CCD system at 90(2)K. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3\% wide omega-scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3\% wide scans, 15 seconds per frame and 606 frames were collected, at varying phi angles (phi=0\%, 90\%, 180\%, 270\%), for each series. The crystal to detector distance was 5.28cm, thus providing a complete sphere of data with processing to 2ThetaMax=55.24\%. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35282 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 18438 _reflns_number_gt 16888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.2-0) (Bruker, 2007)' _computing_cell_refinement 'SAINT (7.46A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.46A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 4GB of extended memory. A total of 49929 reflections were collected and corrected for Lorentz and polarization effects and numerical, face based, absorption using Blessing's method as incorporated into the program SADABS(2,3) with 18438 unique. The SHELXTL(4) program package was implemented to determine the probable space group and set up the initial files. The unit cell appears monoclinic with both alpha and gamma near 90.0 degrees. However, system symmetry and lack of systematic absences generated three possibilities, P2, Pm, or P2/m and after all three had had exhaustive attempts with strange fruitless results in each, the triclinic system was attempted. System symmetry, lack of systematic absences and intensity statistics indicated the potential centrosymmetric triclinic space group P-1 (no. 2). The structure was determined by direct methods with the successful location of a majority of the molecule of interest using the program XS(5). The structure was refined with XL(5). An initial result in P-1 proved appealing and when the twin law -1 0 0 0 1 0 0 0 -1 was included the structure converged quickly. When viewed down the 010 axis it becomes apparent that the molecule does not possess two-fold symmetry about this axis but is skewed from it. The tetramethylammonium anions are also problematic with a two fold rotation but are well ordered in P-1. It was therefore concluded that this system possesses a nearly monoclinic cell but is actually triclinic in nature. A multitude of refinement difference-Fourier cycles were required to locate the remaining non-hydrogen atoms. Water molecules were optimized when believed to be partial occupancy and hydrogen atoms were located whenever possible with difference-Fourier maps. All hydrogen atoms were optimized to have minimal interactions with neighboring water molecules. The data collected were merged based upon identical indices yielding 12276 data [R(int)=0.0212] that were truncated to 2ThetaMax=55.00\% resulting in 12262 data that were further merged in least-squares refinement to 6255 unique data [R(int)=0.0240]. All non-hydrogen atoms were refined anisotropically. The final structure was refined to convergence with R(F)=4.62%, wR(F2)=10.91%, GOF=1.053 for all 18438 unique reflections [R(F)=4.03%, wR(F2)=10.56% for those 16888 data with Fo > 4sigma(Fo)]. The final difference-Fourier map was possessed a multitude of peaks near the heavy atoms within the structure while the remainder of the map was featureless indicating that the structure is both correct and complete. References: 1. Bruker (2007) APEX (Version 2.2.0) and SAINT (Version 7.23a). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2007) Version 2007/3, 'Siemens Area Detector Absorption Correction' Universit\"at G\"ottingen: G\"ottingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G\"ottingen: G\"ottingen, Germany. ; _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^)+(0.0294P)^2^+21.8870P] 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 18438 _refine_ls_number_parameters 955 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.115 _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 0.13039(4) 0.58808(3) 0.22132(3) 0.01291(11) Uani 1 1 d . . . Nb2 Nb 0.14139(5) 0.75030(4) 0.22961(4) 0.01028(13) Uani 0.50 1 d P A 1 Ti2 Ti 0.14139(5) 0.75030(4) 0.22961(4) 0.01028(13) Uani 0.50 1 d P A 2 Nb3 Nb -0.06449(4) 0.67680(2) 0.09446(3) 0.01099(10) Uani 1 1 d . A . Nb4 Nb -0.09661(4) 0.59348(3) 0.27154(3) 0.01251(11) Uani 1 1 d . . . Nb5 Nb 0.10850(4) 0.66635(3) 0.40754(3) 0.01080(10) Uani 1 1 d . A . Nb6 Nb 0.11564(4) 0.83037(3) 0.41504(3) 0.01283(10) Uani 1 1 d . . . Nb7 Nb 0.15141(4) 0.91282(3) 0.23972(3) 0.01563(11) Uani 1 1 d . A . Nb8 Nb -0.05267(4) 0.84089(2) 0.10179(3) 0.01186(10) Uani 1 1 d . . . Nb9 Nb -0.08759(5) 0.75621(3) 0.27941(4) 0.00989(13) Uani 0.50 1 d P A 1 Ti9 Ti -0.08759(5) 0.75621(3) 0.27941(4) 0.00989(13) Uani 0.50 1 d P A 2 Nb10 Nb -0.07852(4) 0.91798(3) 0.28580(3) 0.01454(11) Uani 1 1 d . A . O1 O 0.2076(4) 0.5226(2) 0.1990(3) 0.0188(9) Uani 1 1 d . A . O2 O 0.2080(3) 0.6747(2) 0.2112(3) 0.0162(9) Uani 1 1 d . A . O3 O 0.0428(3) 0.6126(2) 0.1016(3) 0.0160(9) Uani 1 1 d . A . O4 O 0.0142(3) 0.54166(19) 0.2444(3) 0.0140(8) Uani 1 1 d . A . O5 O 0.1834(3) 0.6040(2) 0.3538(3) 0.0149(8) Uani 1 1 d . A . O6 O 0.2182(3) 0.8225(2) 0.2191(3) 0.0165(9) Uani 1 1 d . . . O7 O 0.0423(3) 0.7553(2) 0.1083(2) 0.0127(8) Uani 1 1 d . A . O8 O -0.1255(3) 0.6794(2) -0.0213(3) 0.0153(8) Uani 1 1 d . . . O9 O -0.1482(3) 0.6171(2) 0.1413(3) 0.0140(8) Uani 1 1 d . A . O10 O -0.1793(3) 0.5313(2) 0.2900(3) 0.0176(9) Uani 1 1 d . A . O11 O -0.0068(3) 0.6095(2) 0.3938(3) 0.0146(8) Uani 1 1 d . A . O12 O 0.1710(3) 0.6591(2) 0.5228(3) 0.0162(8) Uani 1 1 d . . . O13 O 0.1818(3) 0.7470(2) 0.3652(2) 0.0138(8) Uani 1 1 d . A . O14 O 0.0222(3) 0.68327(19) 0.2508(3) 0.0112(7) Uani 1 1 d . A . O15 O 0.1770(3) 0.8291(2) 0.5311(3) 0.0173(9) Uani 1 1 d . A . O16 O 0.1992(4) 0.8891(2) 0.3680(3) 0.0173(9) Uani 1 1 d . A . O17 O 0.2408(4) 0.9734(2) 0.2271(3) 0.0259(11) Uani 1 1 d . . . O18 O 0.0628(3) 0.8979(2) 0.1167(3) 0.0150(8) Uani 1 1 d . A . O19 O -0.1143(3) 0.8479(2) -0.0134(3) 0.0170(9) Uani 1 1 d . A . O20 O -0.1287(3) 0.7600(2) 0.1444(2) 0.0113(7) Uani 1 1 d . A . O21 O -0.1646(3) 0.6839(2) 0.2904(3) 0.0133(8) Uani 1 1 d . A . O22 O 0.0109(3) 0.7507(2) 0.4011(2) 0.0127(7) Uani 1 1 d . A . O23 O 0.0307(3) 0.8235(2) 0.2584(3) 0.0140(8) Uani 1 1 d . A . O24 O 0.0070(3) 0.8935(2) 0.4068(3) 0.0154(9) Uani 1 1 d . A . O25 O 0.0401(4) 0.9650(2) 0.2658(3) 0.0181(9) Uani 1 1 d . . . O26 O -0.1278(3) 0.9027(2) 0.1555(3) 0.0161(8) Uani 1 1 d . A . O27 O -0.1565(3) 0.8315(2) 0.2969(3) 0.0136(8) Uani 1 1 d . . . O28 O -0.1581(4) 0.9822(2) 0.3072(3) 0.0219(10) Uani 1 1 d . . . C31 C 0.9912(6) 0.8965(4) 0.6181(5) 0.0294(16) Uani 1 1 d . . . H31A H 1.0131 0.9362 0.6558 0.044 Uiso 1 1 calc R . . H31B H 1.0236 0.8966 0.5688 0.044 Uiso 1 1 calc R . . H31C H 1.0113 0.8557 0.6541 0.044 Uiso 1 1 calc R . . N31 N 0.8768(5) 0.8977(3) 0.5809(4) 0.0250(13) Uani 1 1 d . . . C32 C 0.8467(6) 0.9617(4) 0.5312(4) 0.0278(15) Uani 1 1 d . . . H32A H 0.7722 0.9632 0.5076 0.042 Uiso 1 1 calc R . . H32B H 0.8785 0.9642 0.4816 0.042 Uiso 1 1 calc R . . H32C H 0.8694 0.9997 0.5718 0.042 Uiso 1 1 calc R . . C33 C 0.8461(8) 0.8387(4) 0.5200(5) 0.038(2) Uani 1 1 d . . . H33A H 0.8642 0.7970 0.5543 0.056 Uiso 1 1 calc R . . H33B H 0.8818 0.8404 0.4729 0.056 Uiso 1 1 calc R . . H33C H 0.7722 0.8399 0.4928 0.056 Uiso 1 1 calc R . . C34 C 0.8280(6) 0.8929(4) 0.6567(5) 0.0298(16) Uani 1 1 d . . . H34A H 0.7536 0.8916 0.6328 0.045 Uiso 1 1 calc R . . H34B H 0.8473 0.9321 0.6958 0.045 Uiso 1 1 calc R . . H34C H 0.8514 0.8519 0.6910 0.045 Uiso 1 1 calc R . . C35 C 0.9819(6) 0.5897(4) 0.6030(5) 0.0307(16) Uani 1 1 d . . . H35A H 1.0031 0.5493 0.6393 0.046 Uiso 1 1 calc R . . H35B H 1.0046 0.6297 0.6399 0.046 Uiso 1 1 calc R . . H35C H 1.0128 0.5895 0.5527 0.046 Uiso 1 1 calc R . . N35 N 0.8692(4) 0.5907(3) 0.5685(3) 0.0181(11) Uani 1 1 d . . . C36 C 0.8356(6) 0.6519(4) 0.5142(5) 0.0262(15) Uani 1 1 d . . . H36A H 0.8540 0.6918 0.5522 0.039 Uiso 1 1 calc R . . H36B H 0.7613 0.6506 0.4887 0.039 Uiso 1 1 calc R . . H36C H 0.8692 0.6539 0.4657 0.039 Uiso 1 1 calc R . . C37 C 0.8380(7) 0.5303(4) 0.5098(5) 0.0335(18) Uani 1 1 d . . . H37A H 0.8701 0.5321 0.4603 0.050 Uiso 1 1 calc R . . H37B H 0.7635 0.5298 0.4858 0.050 Uiso 1 1 calc R . . H37C H 0.8600 0.4894 0.5449 0.050 Uiso 1 1 calc R . . C38 C 0.8234(5) 0.5886(4) 0.6457(4) 0.0248(14) Uani 1 1 d . . . H38A H 0.8509 0.5500 0.6838 0.037 Uiso 1 1 calc R . . H38B H 0.7491 0.5843 0.6235 0.037 Uiso 1 1 calc R . . H38C H 0.8402 0.6301 0.6805 0.037 Uiso 1 1 calc R . . C39 C 0.5750(5) 0.7590(5) 0.5205(5) 0.0357(17) Uani 1 1 d . . . H39A H 0.6111 0.7758 0.4780 0.054 Uiso 1 1 calc R . . H39B H 0.5918 0.7114 0.5331 0.054 Uiso 1 1 calc R . . H39C H 0.5961 0.7848 0.5762 0.054 Uiso 1 1 calc R . . N39 N 0.4636(5) 0.7663(4) 0.4816(4) 0.0379(16) Uani 1 1 d . . . C40 C 0.4381(9) 0.8363(8) 0.4513(14) 0.128(8) Uani 1 1 d . . . H40A H 0.4130 0.8606 0.4962 0.192 Uiso 1 1 calc R . . H40B H 0.3850 0.8360 0.3942 0.192 Uiso 1 1 calc R . . H40C H 0.4993 0.8587 0.4434 0.192 Uiso 1 1 calc R . . C41 C 0.4299(7) 0.7152(7) 0.4044(7) 0.075(4) Uani 1 1 d . . . H41A H 0.3561 0.7078 0.3914 0.112 Uiso 1 1 calc R . . H41B H 0.4659 0.6726 0.4219 0.112 Uiso 1 1 calc R . . H41C H 0.4464 0.7328 0.3510 0.112 Uiso 1 1 calc R . . C42 C 0.4078(5) 0.7491(5) 0.5483(5) 0.0317(15) Uani 1 1 d . . . H42A H 0.4310 0.7782 0.6008 0.048 Uiso 1 1 calc R . . H42B H 0.4209 0.7020 0.5664 0.048 Uiso 1 1 calc R . . H42C H 0.3343 0.7557 0.5219 0.048 Uiso 1 1 calc R . . C43 C 0.9254(7) 0.0822(5) 0.1083(6) 0.050(3) Uani 1 1 d . . . H43A H 0.9658 0.0879 0.0652 0.075 Uiso 1 1 calc R . . H43B H 0.9452 0.0403 0.1416 0.075 Uiso 1 1 calc R . . H43C H 0.9378 0.1202 0.1501 0.075 Uiso 1 1 calc R . . N43 N 0.8180(5) 0.0797(3) 0.0612(4) 0.0289(14) Uani 1 1 d . . . C44 C 0.7864(7) 0.1425(4) 0.0064(5) 0.0366(19) Uani 1 1 d . . . H44A H 0.7929 0.1814 0.0464 0.055 Uiso 1 1 calc R . . H44B H 0.7152 0.1382 -0.0292 0.055 Uiso 1 1 calc R . . H44C H 0.8306 0.1488 -0.0336 0.055 Uiso 1 1 calc R . . C45 C 0.8020(8) 0.0200(4) -0.0032(6) 0.047(2) Uani 1 1 d . . . H45A H 0.8420 0.0268 -0.0465 0.071 Uiso 1 1 calc R . . H45B H 0.7294 0.0164 -0.0349 0.071 Uiso 1 1 calc R . . H45C H 0.8244 -0.0214 0.0306 0.071 Uiso 1 1 calc R . . C46 C 0.7507(8) 0.0700(5) 0.1224(7) 0.053(3) Uani 1 1 d . . . H46A H 0.7631 0.0254 0.1501 0.080 Uiso 1 1 calc R . . H46B H 0.6789 0.0736 0.0880 0.080 Uiso 1 1 calc R . . H46C H 0.7659 0.1046 0.1690 0.080 Uiso 1 1 calc R . . C47 C 0.4399(6) 0.6310(4) 0.1869(6) 0.0358(18) Uani 1 1 d . . . H47A H 0.3702 0.6262 0.1929 0.054 Uiso 1 1 calc R . . H47B H 0.4373 0.6402 0.1243 0.054 Uiso 1 1 calc R . . H47C H 0.4742 0.6681 0.2246 0.054 Uiso 1 1 calc R . . N47 N 0.4983(5) 0.5666(3) 0.2160(5) 0.0333(14) Uani 1 1 d . . . C48 C 0.5975(6) 0.5670(4) 0.1924(6) 0.0345(17) Uani 1 1 d . . . H48A H 0.6373 0.6064 0.2191 0.052 Uiso 1 1 calc R . . H48B H 0.5847 0.5686 0.1272 0.052 Uiso 1 1 calc R . . H48C H 0.6358 0.5260 0.2154 0.052 Uiso 1 1 calc R . . C49 C 0.4385(8) 0.5080(5) 0.1651(10) 0.068(4) Uani 1 1 d . . . H49A H 0.4855 0.4710 0.1628 0.102 Uiso 1 1 calc R . . H49B H 0.4037 0.5222 0.1040 0.102 Uiso 1 1 calc R . . H49C H 0.3879 0.4928 0.1954 0.102 Uiso 1 1 calc R . . C50 C 0.5199(13) 0.5605(6) 0.3141(7) 0.083(5) Uani 1 1 d . . . H50A H 0.5276 0.6054 0.3411 0.124 Uiso 1 1 calc R . . H50B H 0.5832 0.5350 0.3373 0.124 Uiso 1 1 calc R . . H50C H 0.4633 0.5370 0.3292 0.124 Uiso 1 1 calc R . . C51 C 0.8202(6) 0.3938(4) 0.1703(5) 0.0316(16) Uani 1 1 d . . . H51A H 0.8516 0.3546 0.2055 0.047 Uiso 1 1 calc R . . H51B H 0.7457 0.3894 0.1547 0.047 Uiso 1 1 calc R . . H51C H 0.8409 0.4348 0.2056 0.047 Uiso 1 1 calc R . . N51 N 0.8547(4) 0.3975(3) 0.0868(4) 0.0189(11) Uani 1 1 d . . . C52 C 0.8068(8) 0.4571(4) 0.0336(5) 0.043(2) Uani 1 1 d . . . H52A H 0.7326 0.4508 0.0134 0.064 Uiso 1 1 calc R . . H52B H 0.8341 0.4622 -0.0185 0.064 Uiso 1 1 calc R . . H52C H 0.8223 0.4976 0.0708 0.064 Uiso 1 1 calc R . . C53 C 0.9682(5) 0.4039(4) 0.1137(5) 0.0257(15) Uani 1 1 d . . . H53A H 0.9879 0.4440 0.1510 0.039 Uiso 1 1 calc R . . H53B H 0.9929 0.4080 0.0601 0.039 Uiso 1 1 calc R . . H53C H 0.9984 0.3640 0.1476 0.039 Uiso 1 1 calc R . . C54 C 0.8241(6) 0.3345(4) 0.0334(5) 0.0278(15) Uani 1 1 d . . . H54A H 0.8561 0.2957 0.0689 0.042 Uiso 1 1 calc R . . H54B H 0.8465 0.3370 -0.0215 0.042 Uiso 1 1 calc R . . H54C H 0.7496 0.3297 0.0179 0.042 Uiso 1 1 calc R . . C55 C 0.4813(5) 0.7927(4) -0.0044(5) 0.0346(18) Uani 1 1 d . . . H55A H 0.4627 0.8271 -0.0512 0.052 Uiso 1 1 calc R . . H55B H 0.4459 0.8017 0.0417 0.052 Uiso 1 1 calc R . . H55C H 0.4615 0.7483 -0.0306 0.052 Uiso 1 1 calc R . . N55 N 0.5933(4) 0.7942(3) 0.0364(4) 0.0258(12) Uani 1 1 d . . . C56 C 0.6268(7) 0.8614(5) 0.0734(8) 0.053(2) Uani 1 1 d . . . H56A H 0.6151 0.8942 0.0246 0.080 Uiso 1 1 calc R . . H56B H 0.6997 0.8600 0.1047 0.080 Uiso 1 1 calc R . . H56C H 0.5877 0.8745 0.1155 0.080 Uiso 1 1 calc R . . C57 C 0.6480(6) 0.7743(4) -0.0332(5) 0.0335(17) Uani 1 1 d . . . H57A H 0.6347 0.7269 -0.0488 0.050 Uiso 1 1 calc R . . H57B H 0.7217 0.7813 -0.0088 0.050 Uiso 1 1 calc R . . H57C H 0.6230 0.8021 -0.0868 0.050 Uiso 1 1 calc R . . C58 C 0.6203(5) 0.7442(4) 0.1107(4) 0.0305(15) Uani 1 1 d . . . H58A H 0.5925 0.7590 0.1597 0.046 Uiso 1 1 calc R . . H58B H 0.6948 0.7405 0.1324 0.046 Uiso 1 1 calc R . . H58C H 0.5913 0.7004 0.0887 0.046 Uiso 1 1 calc R . . O61 O 0.4195(4) 0.9396(4) 0.1741(4) 0.115(4) Uani 1 1 d D . . H61A H 0.3664 0.9495 0.1897 0.172 Uiso 1 1 d D . . H61B H 0.4546 0.9168 0.2170 0.172 Uiso 1 1 d D . . O62 O 0.4159(6) 0.7998(4) 0.1920(6) 0.068(2) Uani 1 1 d . . . O63 O 0.5972(8) 0.9768(6) 0.4057(11) 0.138(6) Uani 1 1 d . . . O64 O 0.6467(6) 0.8546(5) 0.3216(7) 0.074(2) Uani 1 1 d D . . H64A H 0.646(9) 0.8964(15) 0.330(10) 0.111 Uiso 1 1 d D . . H64B H 0.585(3) 0.843(6) 0.301(10) 0.111 Uiso 1 1 d D . . O65 O 0.6519(4) 0.7104(3) 0.3363(4) 0.0350(12) Uani 1 1 d D . . H65A H 0.648(6) 0.7517(10) 0.325(6) 0.053 Uiso 1 1 d D . . H65B H 0.707(4) 0.697(3) 0.327(6) 0.053 Uiso 1 1 d D . . O66 O 0.6360(3) 0.46460(12) 0.5559(4) 0.0403(13) Uani 1 1 d D . . H66A H 0.6073 0.5019 0.5596 0.060 Uiso 1 1 d D . . H66B H 0.6060 0.4279 0.5582 0.060 Uiso 1 1 d D . . O67 O 0.6683(3) 0.5930(3) 0.0075(3) 0.0276(10) Uani 1 1 d D . . H67A H 0.6918 0.5959 -0.0386 0.041 Uiso 1 1 d D . . H67B H 0.7242 0.6004 0.0476 0.041 Uiso 1 1 d D . . O68 O 0.5992(3) 0.9882(4) 0.6121(4) 0.094(3) Uani 1 1 d D . . H68A H 0.5391 0.9858 0.6168 0.140 Uiso 1 1 d D . . H68B H 0.6007 0.9662 0.5662 0.140 Uiso 1 1 d D . . O69 O 0.45673(10) 0.6113(3) 0.96587(8) 0.0351(12) Uani 1 1 d D . . H69A H 0.5203 0.6055 0.9783 0.053 Uiso 1 1 d D . . H69B H 0.4375 0.6161 0.9101 0.053 Uiso 1 1 d D . . O70 O 0.7390(3) 0.8981(2) 0.8393(4) 0.0470(17) Uani 1 1 d D . . H70A H 0.7898 0.8777 0.8718 0.071 Uiso 1 1 d D . . H70B H 0.7450 0.9367 0.8188 0.071 Uiso 1 1 d D . . O71 O 0.7454(3) 0.6027(2) 0.8543(3) 0.0244(10) Uani 1 1 d D . . H71A H 0.788(4) 0.624(3) 0.894(4) 0.037 Uiso 1 1 d D . . H71B H 0.776(5) 0.568(2) 0.844(5) 0.037 Uiso 1 1 d D . . O72 O 0.9429(6) 0.7635(3) 0.8674(4) 0.0542(19) Uani 1 1 d D . . H72A H 0.883(3) 0.751(6) 0.844(7) 0.081 Uiso 1 1 d D . . H72B H 0.941(7) 0.791(5) 0.908(6) 0.081 Uiso 1 1 d D . . O73 O 0.9593(4) 0.7363(3) 0.7014(4) 0.0390(13) Uani 1 1 d D . . H73A H 0.962(5) 0.740(6) 0.7559(14) 0.058 Uiso 1 1 d D . . H73B H 1.016(3) 0.749(6) 0.696(5) 0.058 Uiso 1 1 d D . . O74 O 0.5940(4) 0.6674(3) 0.7300(4) 0.0370(13) Uani 1 1 d D . . H74A H 0.598(6) 0.6260(10) 0.721(7) 0.056 Uiso 1 1 d D . . H74B H 0.543(5) 0.673(4) 0.750(6) 0.056 Uiso 1 1 d D . . O75 O 0.5977(5) 0.8123(3) 0.7324(4) 0.0414(14) Uani 1 1 d D . . H75A H 0.616(7) 0.8526(15) 0.741(7) 0.062 Uiso 1 1 d D . . H75B H 0.640(6) 0.789(4) 0.714(7) 0.062 Uiso 1 1 d D . . O76 O 0.5411(4) 0.5883(3) 0.5676(4) 0.0426(14) Uani 1 1 d . . . O77 O 0.4180(4) 0.6445(3) 0.7816(3) 0.0303(11) Uani 1 1 d D . . H77A H 0.380(5) 0.626(3) 0.736(4) 0.045 Uiso 1 1 d D . . H77B H 0.397(6) 0.6842(17) 0.784(5) 0.045 Uiso 1 1 d D . . O78 O 0.2817(3) 0.5730(2) 0.6554(3) 0.0226(10) Uani 1 1 d D . . H78A H 0.240(4) 0.546(3) 0.667(4) 0.019(19) Uiso 1 1 d D . . H78B H 0.253(4) 0.599(3) 0.614(4) 0.04(3) Uiso 1 1 d D . . O79 O 0.4217(4) 0.86017(14) 0.7745(3) 0.0426(15) Uani 1 1 d D . . H79A H 0.3851 0.8815 0.7308 0.064 Uiso 1 1 d D . . H79B H 0.4220 0.8199 0.7585 0.064 Uiso 1 1 d D . . O80 O 0.3057(4) 0.7566(3) 0.8092(3) 0.0347(11) Uani 1 1 d . . . O81 O 0.2828(4) 0.9283(2) 0.6417(3) 0.0265(10) Uani 1 1 d D . . H81A H 0.244(6) 0.895(3) 0.623(5) 0.040 Uiso 1 1 d D . . H81B H 0.294(7) 0.946(4) 0.596(3) 0.040 Uiso 1 1 d D . . O82 O 0.1470(4) 0.7442(3) 0.6564(3) 0.0218(9) Uani 1 1 d D . . H82A H 0.136(9) 0.7833(17) 0.636(5) 0.07(4) Uiso 1 1 d D . . H82B H 0.152(6) 0.719(3) 0.614(3) 0.02(2) Uiso 1 1 d D . . 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 0.0152(2) 0.0125(2) 0.0105(2) 0.00037(18) 0.00259(19) 0.0028(2) Nb2 0.0114(3) 0.0105(3) 0.0087(3) -0.0003(2) 0.0022(2) -0.0009(3) Ti2 0.0114(3) 0.0105(3) 0.0087(3) -0.0003(2) 0.0022(2) -0.0009(3) Nb3 0.0132(2) 0.0105(2) 0.0086(2) -0.00070(18) 0.00168(17) -0.00027(19) Nb4 0.0130(2) 0.0129(2) 0.0106(2) 0.00128(18) 0.00140(18) -0.00186(19) Nb5 0.0115(2) 0.0113(2) 0.0088(2) 0.00097(18) 0.00132(17) 0.00062(19) Nb6 0.0168(2) 0.0110(2) 0.0094(2) -0.00119(18) 0.00133(18) -0.0012(2) Nb7 0.0199(3) 0.0129(2) 0.0132(2) 0.00106(19) 0.0030(2) -0.0044(2) Nb8 0.0146(2) 0.0104(2) 0.0097(2) 0.00107(18) 0.00185(18) 0.00022(19) Nb9 0.0113(3) 0.0097(3) 0.0080(3) 0.0004(2) 0.0014(2) 0.0009(3) Ti9 0.0113(3) 0.0097(3) 0.0080(3) 0.0004(2) 0.0014(2) 0.0009(3) Nb10 0.0200(3) 0.0113(2) 0.0114(2) -0.00083(19) 0.0026(2) 0.0020(2) O1 0.021(2) 0.020(2) 0.016(2) -0.0012(17) 0.0082(18) 0.0051(18) O2 0.016(2) 0.018(2) 0.0139(19) -0.0003(16) 0.0028(16) 0.0007(17) O3 0.019(2) 0.017(2) 0.0106(19) -0.0003(15) 0.0015(16) -0.0023(17) O4 0.022(2) 0.0076(17) 0.0123(19) 0.0007(14) 0.0037(16) 0.0010(16) O5 0.014(2) 0.015(2) 0.0121(19) 0.0010(15) -0.0011(16) -0.0004(16) O6 0.019(2) 0.016(2) 0.0145(19) -0.0027(16) 0.0041(16) -0.0016(17) O7 0.0166(19) 0.0114(19) 0.0096(17) -0.0020(15) 0.0025(15) -0.0013(17) O8 0.017(2) 0.017(2) 0.0115(18) -0.0024(15) 0.0020(15) -0.0012(17) O9 0.014(2) 0.0139(19) 0.0139(19) -0.0018(15) 0.0027(16) -0.0030(16) O10 0.013(2) 0.022(2) 0.015(2) 0.0053(17) 0.0008(16) -0.0060(17) O11 0.020(2) 0.0096(19) 0.0147(19) 0.0027(15) 0.0060(17) -0.0018(16) O12 0.018(2) 0.016(2) 0.0140(19) 0.0040(16) 0.0021(16) -0.0001(17) O13 0.0149(19) 0.0119(18) 0.0143(18) 0.0003(16) 0.0033(15) 0.0000(17) O14 0.0111(18) 0.0111(18) 0.0089(17) -0.0003(14) -0.0013(14) -0.0004(15) O15 0.023(2) 0.016(2) 0.0114(18) 0.0015(16) 0.0030(16) -0.0011(18) O16 0.023(2) 0.014(2) 0.014(2) 0.0004(15) 0.0030(17) -0.0056(17) O17 0.031(3) 0.020(2) 0.024(2) 0.0042(19) 0.005(2) -0.008(2) O18 0.017(2) 0.015(2) 0.0133(19) 0.0012(15) 0.0048(16) -0.0006(16) O19 0.019(2) 0.016(2) 0.0126(19) 0.0009(15) -0.0002(16) 0.0007(17) O20 0.0121(18) 0.0116(19) 0.0085(16) -0.0006(14) -0.0001(14) -0.0005(15) O21 0.0116(19) 0.014(2) 0.0130(18) 0.0026(15) 0.0012(15) 0.0021(15) O22 0.0149(19) 0.0141(19) 0.0090(17) 0.0038(16) 0.0030(14) 0.0026(17) O23 0.018(2) 0.0117(18) 0.0117(18) 0.0001(16) 0.0028(15) -0.0011(17) O24 0.021(2) 0.015(2) 0.0102(18) 0.0007(15) 0.0048(16) -0.0004(17) O25 0.025(2) 0.0116(19) 0.015(2) 0.0023(16) 0.0008(17) -0.0027(17) O26 0.019(2) 0.0120(19) 0.0159(19) -0.0001(16) 0.0034(17) -0.0001(16) O27 0.0155(19) 0.0124(19) 0.0126(18) 0.0004(15) 0.0031(15) 0.0009(16) O28 0.028(3) 0.017(2) 0.018(2) 0.0003(17) 0.0028(19) 0.0071(19) C31 0.033(4) 0.029(4) 0.027(3) -0.003(3) 0.009(3) 0.003(3) N31 0.041(4) 0.019(3) 0.017(3) -0.004(2) 0.011(2) -0.005(2) C32 0.041(4) 0.023(3) 0.017(3) -0.001(3) 0.004(3) -0.008(3) C33 0.066(6) 0.022(4) 0.030(4) -0.013(3) 0.022(4) -0.025(4) C34 0.044(4) 0.024(3) 0.026(3) -0.003(3) 0.016(3) -0.007(3) C35 0.024(4) 0.038(4) 0.027(4) 0.008(3) 0.003(3) 0.008(3) N35 0.018(3) 0.019(3) 0.016(2) 0.004(2) 0.002(2) -0.002(2) C36 0.030(4) 0.024(3) 0.021(3) 0.006(3) 0.001(3) 0.007(3) C37 0.055(5) 0.023(3) 0.028(4) -0.006(3) 0.021(4) -0.008(3) C38 0.022(3) 0.033(4) 0.023(3) 0.001(3) 0.013(3) -0.011(3) C39 0.018(3) 0.053(5) 0.034(4) 0.000(4) 0.003(3) -0.001(3) N39 0.021(3) 0.062(5) 0.033(3) 0.008(3) 0.010(3) 0.007(3) C40 0.033(6) 0.136(14) 0.23(2) 0.131(14) 0.053(9) 0.033(7) C41 0.023(4) 0.158(13) 0.047(5) -0.033(7) 0.016(4) -0.017(6) C42 0.016(3) 0.046(4) 0.034(4) 0.004(4) 0.008(3) 0.004(3) C43 0.039(5) 0.059(6) 0.042(5) 0.022(4) -0.006(4) -0.019(4) N43 0.032(3) 0.033(3) 0.028(3) 0.014(3) 0.019(3) 0.013(3) C44 0.058(5) 0.024(4) 0.037(4) 0.014(3) 0.028(4) 0.017(4) C45 0.064(6) 0.035(5) 0.042(5) 0.011(4) 0.013(5) -0.002(4) C46 0.058(6) 0.061(6) 0.057(6) 0.032(5) 0.045(5) 0.026(5) C47 0.020(3) 0.039(4) 0.050(5) -0.003(4) 0.011(3) 0.003(3) N47 0.023(3) 0.030(3) 0.051(4) -0.003(3) 0.017(3) -0.008(3) C48 0.019(3) 0.045(5) 0.042(4) 0.009(3) 0.012(3) 0.000(3) C49 0.033(5) 0.039(5) 0.132(11) -0.027(6) 0.023(6) -0.022(4) C50 0.166(15) 0.050(6) 0.054(6) 0.023(5) 0.068(8) 0.035(8) C51 0.033(4) 0.046(4) 0.021(3) -0.008(3) 0.016(3) -0.012(3) N51 0.015(2) 0.023(3) 0.019(2) -0.001(2) 0.003(2) 0.001(2) C52 0.064(6) 0.035(4) 0.025(4) 0.007(3) 0.003(4) 0.017(4) C53 0.017(3) 0.034(4) 0.029(3) -0.012(3) 0.010(3) -0.003(3) C54 0.033(4) 0.024(3) 0.028(3) -0.012(3) 0.010(3) -0.013(3) C55 0.011(3) 0.047(5) 0.040(4) 0.008(3) -0.004(3) 0.003(3) N55 0.011(3) 0.026(3) 0.036(3) 0.003(2) 0.000(2) -0.002(2) C56 0.034(5) 0.045(5) 0.079(7) -0.013(5) 0.012(5) -0.008(4) C57 0.026(4) 0.044(4) 0.032(4) 0.010(3) 0.010(3) -0.003(3) C58 0.021(3) 0.045(4) 0.023(3) 0.012(3) 0.002(3) 0.002(3) O61 0.093(8) 0.060(6) 0.226(14) -0.003(7) 0.105(9) 0.002(5) O62 0.044(4) 0.085(6) 0.082(6) -0.007(4) 0.030(4) 0.006(4) O63 0.054(6) 0.102(8) 0.266(17) 0.054(10) 0.059(9) -0.010(6) O64 0.036(4) 0.088(6) 0.108(7) -0.009(6) 0.038(4) -0.022(4) O65 0.023(3) 0.047(3) 0.037(3) 0.005(3) 0.012(2) 0.003(2) O66 0.026(3) 0.036(3) 0.051(4) 0.002(3) -0.002(3) -0.002(2) O67 0.012(2) 0.042(3) 0.025(2) -0.002(2) -0.0024(18) -0.006(2) O68 0.062(6) 0.127(9) 0.086(7) 0.008(6) 0.011(5) -0.022(6) O69 0.019(2) 0.058(4) 0.028(3) 0.006(2) 0.005(2) 0.003(2) O70 0.035(3) 0.040(3) 0.047(3) 0.024(3) -0.023(3) -0.017(3) O71 0.016(2) 0.023(2) 0.028(2) -0.0101(19) -0.0049(19) 0.0031(18) O72 0.106(6) 0.029(3) 0.042(4) 0.001(3) 0.045(4) 0.002(3) O73 0.044(3) 0.042(3) 0.033(3) -0.009(2) 0.015(2) -0.013(3) O74 0.023(3) 0.051(4) 0.033(3) 0.012(3) 0.002(2) -0.001(3) O75 0.041(3) 0.042(3) 0.038(3) -0.003(3) 0.005(3) -0.007(3) O76 0.033(3) 0.046(3) 0.041(3) 0.003(3) -0.005(2) -0.003(3) O77 0.025(3) 0.038(3) 0.027(3) -0.001(2) 0.005(2) -0.003(2) O78 0.014(2) 0.021(2) 0.028(2) 0.0053(19) -0.0038(18) -0.0089(18) O79 0.031(3) 0.038(3) 0.050(4) 0.013(3) -0.004(3) 0.002(3) O80 0.037(3) 0.030(3) 0.029(2) 0.002(2) -0.006(2) -0.004(2) O81 0.025(3) 0.022(2) 0.029(2) -0.0061(19) 0.001(2) 0.000(2) O82 0.026(2) 0.022(2) 0.016(2) -0.0004(18) 0.0028(17) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.763(4) . ? Nb1 O4 1.943(4) . ? Nb1 O3 1.979(4) . ? Nb1 O5 2.012(4) . ? Nb1 O2 2.048(5) . ? Nb1 O14 2.512(4) . ? Nb1 Nb2 3.2314(10) . ? Nb1 Nb3 3.3466(8) . ? Nb2 O6 1.809(4) . ? Nb2 O2 1.815(4) . ? Nb2 O7 2.001(4) . ? Nb2 O13 2.028(4) . ? Nb2 O14 2.190(4) . ? Nb2 O23 2.222(4) . ? Nb2 Nb7 3.2381(10) . ? Nb2 Nb3 3.3486(9) . ? Nb2 Nb5 3.3574(9) . ? Nb3 O8 1.766(4) . ? Nb3 O9 1.918(4) . ? Nb3 O3 1.919(5) . ? Nb3 O7 2.104(4) . ? Nb3 O20 2.112(4) . ? Nb3 O14 2.398(4) . ? Nb3 Nb8 3.2686(9) . ? Nb3 Nb4 3.3362(8) . ? Nb4 O10 1.746(4) . ? Nb4 O4 1.960(4) . ? Nb4 O11 1.986(4) . ? Nb4 O9 2.009(4) . ? Nb4 O21 2.078(4) . ? Nb4 O14 2.486(4) . ? Nb4 Nb9 3.2405(10) . ? Nb4 Nb5 3.3415(8) . ? Nb5 O12 1.768(4) . ? Nb5 O11 1.898(4) . ? Nb5 O5 1.929(4) . ? Nb5 O13 2.086(4) . ? Nb5 O22 2.124(4) . ? Nb5 O14 2.423(4) . ? Nb5 Nb6 3.2655(9) . ? Nb6 O15 1.770(4) . ? Nb6 O16 1.906(4) . ? Nb6 O24 1.914(4) . ? Nb6 O22 2.102(4) . ? Nb6 O13 2.127(4) . ? Nb6 O23 2.398(4) . ? Nb6 Nb7 3.3220(9) . ? Nb6 Nb9 3.3336(9) . ? Nb6 Nb10 3.3429(8) . ? Nb7 O17 1.759(5) . ? Nb7 O25 1.963(5) . ? Nb7 O16 1.977(4) . ? Nb7 O18 1.986(4) . ? Nb7 O6 2.076(5) . ? Nb7 O23 2.487(4) . ? Nb7 Nb8 3.3367(8) . ? Nb8 O19 1.764(4) . ? Nb8 O18 1.900(4) . ? Nb8 O26 1.925(4) . ? Nb8 O20 2.111(4) . ? Nb8 O7 2.121(4) . ? Nb8 O23 2.414(4) . ? Nb8 Nb10 3.3403(9) . ? Nb9 O21 1.814(4) . ? Nb9 O27 1.824(4) . ? Nb9 O22 2.003(4) . ? Nb9 O20 2.020(4) . ? Nb9 O23 2.183(4) . ? Nb9 O14 2.209(4) . ? Nb9 Nb10 3.2210(10) . ? Nb10 O28 1.761(5) . ? Nb10 O25 1.958(5) . ? Nb10 O26 1.975(4) . ? Nb10 O24 1.986(4) . ? Nb10 O27 2.052(4) . ? Nb10 O23 2.500(4) . ? C31 N31 1.505(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N31 C32 1.486(9) . ? N31 C33 1.495(8) . ? N31 C34 1.500(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N35 1.480(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N35 C36 1.483(8) . ? N35 C38 1.490(8) . ? N35 C37 1.499(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 N39 1.478(9) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? N39 C42 1.478(9) . ? N39 C40 1.482(14) . ? N39 C41 1.543(13) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 N43 1.446(10) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N43 C46 1.496(9) . ? N43 C44 1.508(9) . ? N43 C45 1.528(11) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N47 1.510(10) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? N47 C50 1.475(12) . ? N47 C48 1.488(9) . ? N47 C49 1.518(11) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 N51 1.493(8) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? N51 C52 1.490(9) . ? N51 C53 1.491(8) . ? N51 C54 1.498(8) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N55 1.483(8) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? N55 C56 1.477(11) . ? N55 C58 1.491(9) . ? N55 C57 1.518(9) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? O61 H61A 0.8434 . ? O61 H61B 0.8411 . ? O64 H64A 0.84(5) . ? O64 H64B 0.85(7) . ? O65 H65A 0.84(2) . ? O65 H65B 0.84(6) . ? O66 H66A 0.8469 . ? O66 H66B 0.8422 . ? O67 H67A 0.8604 . ? O67 H67B 0.8558 . ? O68 H68A 0.8404 . ? O68 H68B 0.8402 . ? O69 H69A 0.8406 . ? O69 H69B 0.8402 . ? O70 H70A 0.8414 . ? O70 H70B 0.8444 . ? O71 H71A 0.84(6) . ? O71 H71B 0.84(5) . ? O72 H72A 0.84(6) . ? O72 H72B 0.84(10) . ? O73 H73A 0.84(3) . ? O73 H73B 0.84(6) . ? O74 H74A 0.84(3) . ? O74 H74B 0.84(8) . ? O75 H75A 0.84(5) . ? O75 H75B 0.85(8) . ? O77 H77A 0.84(6) . ? O77 H77B 0.84(4) . ? O78 H78A 0.84(6) . ? O78 H78B 0.84(6) . ? O79 H79A 0.8404 . ? O79 H79B 0.8393 . ? O81 H81A 0.85(7) . ? O81 H81B 0.84(7) . ? O82 H82A 0.84(4) . ? O82 H82B 0.84(6) . ? 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 O4 103.92(19) . . ? O1 Nb1 O3 103.71(19) . . ? O4 Nb1 O3 88.65(18) . . ? O1 Nb1 O5 104.34(19) . . ? O4 Nb1 O5 88.45(18) . . ? O3 Nb1 O5 151.66(18) . . ? O1 Nb1 O2 105.1(2) . . ? O4 Nb1 O2 150.95(17) . . ? O3 Nb1 O2 85.04(17) . . ? O5 Nb1 O2 83.94(17) . . ? O1 Nb1 O14 178.57(18) . . ? O4 Nb1 O14 77.37(15) . . ? O3 Nb1 O14 75.62(16) . . ? O5 Nb1 O14 76.25(15) . . ? O2 Nb1 O14 73.60(16) . . ? O1 Nb1 Nb2 136.15(15) . . ? O4 Nb1 Nb2 119.92(12) . . ? O3 Nb1 Nb2 78.55(13) . . ? O5 Nb1 Nb2 78.57(12) . . ? O2 Nb1 Nb2 31.04(12) . . ? O14 Nb1 Nb2 42.56(10) . . ? O1 Nb1 Nb3 133.80(15) . . ? O4 Nb1 Nb3 78.80(12) . . ? O3 Nb1 Nb3 30.32(13) . . ? O5 Nb1 Nb3 121.85(12) . . ? O2 Nb1 Nb3 81.57(12) . . ? O14 Nb1 Nb3 45.63(9) . . ? Nb2 Nb1 Nb3 61.172(18) . . ? O6 Nb2 O2 108.64(17) . . ? O6 Nb2 O7 97.71(18) . . ? O2 Nb2 O7 97.57(18) . . ? O6 Nb2 O13 96.72(18) . . ? O2 Nb2 O13 97.37(18) . . ? O7 Nb2 O13 154.68(15) . . ? O6 Nb2 O14 164.87(18) . . ? O2 Nb2 O14 86.47(18) . . ? O7 Nb2 O14 80.41(16) . . ? O13 Nb2 O14 80.24(16) . . ? O6 Nb2 O23 86.32(18) . . ? O2 Nb2 O23 165.03(18) . . ? O7 Nb2 O23 80.51(16) . . ? O13 Nb2 O23 79.77(16) . . ? O14 Nb2 O23 78.56(13) . . ? O6 Nb2 Nb1 144.22(15) . . ? O2 Nb2 Nb1 35.58(14) . . ? O7 Nb2 Nb1 90.02(13) . . ? O13 Nb2 Nb1 90.34(13) . . ? O14 Nb2 Nb1 50.89(11) . . ? O23 Nb2 Nb1 129.46(11) . . ? O6 Nb2 Nb7 36.24(14) . . ? O2 Nb2 Nb7 144.88(14) . . ? O7 Nb2 Nb7 90.26(13) . . ? O13 Nb2 Nb7 89.18(13) . . ? O14 Nb2 Nb7 128.64(11) . . ? O23 Nb2 Nb7 50.08(11) . . ? Nb1 Nb2 Nb7 179.40(2) . . ? O6 Nb2 Nb3 134.07(14) . . ? O2 Nb2 Nb3 84.70(14) . . ? O7 Nb2 Nb3 36.36(12) . . ? O13 Nb2 Nb3 125.74(12) . . ? O14 Nb2 Nb3 45.63(10) . . ? O23 Nb2 Nb3 85.15(11) . . ? Nb1 Nb2 Nb3 61.110(18) . . ? Nb7 Nb2 Nb3 118.93(2) . . ? O6 Nb2 Nb5 132.61(13) . . ? O2 Nb2 Nb5 84.18(14) . . ? O7 Nb2 Nb5 126.41(12) . . ? O13 Nb2 Nb5 35.89(12) . . ? O14 Nb2 Nb5 46.11(10) . . ? O23 Nb2 Nb5 85.10(11) . . ? Nb1 Nb2 Nb5 61.361(19) . . ? Nb7 Nb2 Nb5 118.06(2) . . ? Nb3 Nb2 Nb5 91.40(2) . . ? O8 Nb3 O9 103.87(19) . . ? O8 Nb3 O3 102.72(19) . . ? O9 Nb3 O3 94.83(18) . . ? O8 Nb3 O7 101.81(17) . . ? O9 Nb3 O7 152.17(16) . . ? O3 Nb3 O7 89.80(17) . . ? O8 Nb3 O20 102.86(17) . . ? O9 Nb3 O20 90.08(16) . . ? O3 Nb3 O20 151.93(16) . . ? O7 Nb3 O20 73.82(15) . . ? O8 Nb3 O14 175.03(17) . . ? O9 Nb3 O14 80.24(16) . . ? O3 Nb3 O14 79.51(16) . . ? O7 Nb3 O14 73.65(14) . . ? O20 Nb3 O14 74.13(14) . . ? O8 Nb3 Nb8 90.64(14) . . ? O9 Nb3 Nb8 129.36(13) . . ? O3 Nb3 Nb8 129.30(13) . . ? O7 Nb3 Nb8 39.50(11) . . ? O20 Nb3 Nb8 39.29(10) . . ? O14 Nb3 Nb8 84.55(9) . . ? O8 Nb3 Nb4 136.31(14) . . ? O9 Nb3 Nb4 32.66(12) . . ? O3 Nb3 Nb4 83.48(13) . . ? O7 Nb3 Nb4 121.60(10) . . ? O20 Nb3 Nb4 85.97(10) . . ? O14 Nb3 Nb4 48.04(10) . . ? Nb8 Nb3 Nb4 118.94(2) . . ? O8 Nb3 Nb1 134.04(14) . . ? O9 Nb3 Nb1 84.64(13) . . ? O3 Nb3 Nb1 31.38(12) . . ? O7 Nb3 Nb1 85.21(11) . . ? O20 Nb3 Nb1 122.46(10) . . ? O14 Nb3 Nb1 48.48(10) . . ? Nb8 Nb3 Nb1 118.83(2) . . ? Nb4 Nb3 Nb1 60.734(18) . . ? O8 Nb3 Nb2 135.18(14) . . ? O9 Nb3 Nb2 120.94(12) . . ? O3 Nb3 Nb2 76.16(13) . . ? O7 Nb3 Nb2 34.33(10) . . ? O20 Nb3 Nb2 77.63(10) . . ? O14 Nb3 Nb2 40.73(10) . . ? Nb8 Nb3 Nb2 61.116(18) . . ? Nb4 Nb3 Nb2 88.47(2) . . ? Nb1 Nb3 Nb2 57.72(2) . . ? O10 Nb4 O4 103.1(2) . . ? O10 Nb4 O11 102.39(19) . . ? O4 Nb4 O11 88.78(18) . . ? O10 Nb4 O9 105.32(18) . . ? O4 Nb4 O9 89.34(17) . . ? O11 Nb4 O9 151.92(17) . . ? O10 Nb4 O21 105.1(2) . . ? O4 Nb4 O21 151.74(17) . . ? O11 Nb4 O21 84.79(17) . . ? O9 Nb4 O21 83.72(17) . . ? O10 Nb4 O14 178.03(17) . . ? O4 Nb4 O14 77.72(15) . . ? O11 Nb4 O14 75.81(15) . . ? O9 Nb4 O14 76.42(15) . . ? O21 Nb4 O14 74.02(15) . . ? O10 Nb4 Nb9 136.21(16) . . ? O4 Nb4 Nb9 120.62(12) . . ? O11 Nb4 Nb9 78.27(12) . . ? O9 Nb4 Nb9 78.67(12) . . ? O21 Nb4 Nb9 31.12(12) . . ? O14 Nb4 Nb9 42.90(10) . . ? O10 Nb4 Nb3 135.99(14) . . ? O4 Nb4 Nb3 78.88(12) . . ? O11 Nb4 Nb3 121.61(12) . . ? O9 Nb4 Nb3 31.01(12) . . ? O21 Nb4 Nb3 81.20(11) . . ? O14 Nb4 Nb3 45.83(9) . . ? Nb9 Nb4 Nb3 61.469(17) . . ? O10 Nb4 Nb5 131.96(14) . . ? O4 Nb4 Nb5 78.77(12) . . ? O11 Nb4 Nb5 29.89(12) . . ? O9 Nb4 Nb5 122.73(12) . . ? O21 Nb4 Nb5 82.08(11) . . ? O14 Nb4 Nb5 46.32(9) . . ? Nb9 Nb4 Nb5 61.699(18) . . ? Nb3 Nb4 Nb5 91.90(2) . . ? O12 Nb5 O11 102.91(19) . . ? O12 Nb5 O5 102.67(19) . . ? O11 Nb5 O5 94.79(19) . . ? O12 Nb5 O13 103.91(18) . . ? O11 Nb5 O13 150.83(17) . . ? O5 Nb5 O13 90.37(17) . . ? O12 Nb5 O22 103.66(17) . . ? O11 Nb5 O22 88.86(17) . . ? O5 Nb5 O22 151.87(15) . . ? O13 Nb5 O22 73.85(15) . . ? O12 Nb5 O14 176.65(17) . . ? O11 Nb5 O14 78.90(16) . . ? O5 Nb5 O14 79.90(16) . . ? O13 Nb5 O14 73.78(14) . . ? O22 Nb5 O14 73.45(14) . . ? O12 Nb5 Nb6 92.50(14) . . ? O11 Nb5 Nb6 128.02(13) . . ? O5 Nb5 Nb6 130.00(13) . . ? O13 Nb5 Nb6 39.64(11) . . ? O22 Nb5 Nb6 39.16(11) . . ? O14 Nb5 Nb6 84.18(9) . . ? O12 Nb5 Nb4 134.14(14) . . ? O11 Nb5 Nb4 31.42(13) . . ? O5 Nb5 Nb4 84.01(12) . . ? O13 Nb5 Nb4 121.55(11) . . ? O22 Nb5 Nb4 84.77(11) . . ? O14 Nb5 Nb4 47.91(10) . . ? Nb6 Nb5 Nb4 117.90(2) . . ? O12 Nb5 Nb2 137.60(14) . . ? O11 Nb5 Nb2 119.48(13) . . ? O5 Nb5 Nb2 76.24(12) . . ? O13 Nb5 Nb2 34.74(11) . . ? O22 Nb5 Nb2 77.71(10) . . ? O14 Nb5 Nb2 40.62(10) . . ? Nb6 Nb5 Nb2 61.490(19) . . ? Nb4 Nb5 Nb2 88.23(2) . . ? O15 Nb6 O16 103.5(2) . . ? O15 Nb6 O24 102.8(2) . . ? O16 Nb6 O24 95.74(19) . . ? O15 Nb6 O22 102.39(17) . . ? O16 Nb6 O22 151.55(16) . . ? O24 Nb6 O22 89.95(17) . . ? O15 Nb6 O13 103.22(18) . . ? O16 Nb6 O13 89.16(18) . . ? O24 Nb6 O13 151.60(17) . . ? O22 Nb6 O13 73.47(15) . . ? O15 Nb6 O23 175.84(17) . . ? O16 Nb6 O23 79.66(16) . . ? O24 Nb6 O23 79.48(16) . . ? O22 Nb6 O23 74.01(14) . . ? O13 Nb6 O23 73.91(15) . . ? O15 Nb6 Nb5 91.32(15) . . ? O16 Nb6 Nb5 127.90(14) . . ? O24 Nb6 Nb5 129.59(13) . . ? O22 Nb6 Nb5 39.64(11) . . ? O13 Nb6 Nb5 38.74(11) . . ? O23 Nb6 Nb5 84.57(10) . . ? O15 Nb6 Nb7 135.06(15) . . ? O16 Nb6 Nb7 31.82(13) . . ? O24 Nb6 Nb7 84.33(13) . . ? O22 Nb6 Nb7 122.14(10) . . ? O13 Nb6 Nb7 85.34(11) . . ? O23 Nb6 Nb7 48.30(10) . . ? Nb5 Nb6 Nb7 118.30(2) . . ? O15 Nb6 Nb9 136.05(15) . . ? O16 Nb6 Nb9 120.47(13) . . ? O24 Nb6 Nb9 75.83(13) . . ? O22 Nb6 Nb9 34.72(10) . . ? O13 Nb6 Nb9 77.58(11) . . ? O23 Nb6 Nb9 40.82(10) . . ? Nb5 Nb6 Nb9 61.534(18) . . ? Nb7 Nb6 Nb9 88.87(2) . . ? O15 Nb6 Nb10 134.28(15) . . ? O16 Nb6 Nb10 84.58(14) . . ? O24 Nb6 Nb10 31.65(12) . . ? O22 Nb6 Nb10 85.87(11) . . ? O13 Nb6 Nb10 122.04(11) . . ? O23 Nb6 Nb10 48.25(10) . . ? Nb5 Nb6 Nb10 119.22(2) . . ? Nb7 Nb6 Nb10 61.089(19) . . ? Nb9 Nb6 Nb10 57.69(2) . . ? O17 Nb7 O25 104.7(2) . . ? O17 Nb7 O16 103.0(2) . . ? O25 Nb7 O16 88.98(19) . . ? O17 Nb7 O18 104.7(2) . . ? O25 Nb7 O18 88.55(18) . . ? O16 Nb7 O18 151.84(18) . . ? O17 Nb7 O6 103.5(2) . . ? O25 Nb7 O6 151.83(18) . . ? O16 Nb7 O6 84.80(18) . . ? O18 Nb7 O6 84.25(17) . . ? O17 Nb7 O23 177.6(2) . . ? O25 Nb7 O23 77.59(16) . . ? O16 Nb7 O23 76.15(16) . . ? O18 Nb7 O23 75.92(16) . . ? O6 Nb7 O23 74.24(16) . . ? O17 Nb7 Nb2 134.47(18) . . ? O25 Nb7 Nb2 120.82(12) . . ? O16 Nb7 Nb2 78.94(12) . . ? O18 Nb7 Nb2 78.33(12) . . ? O6 Nb7 Nb2 31.01(12) . . ? O23 Nb7 Nb2 43.23(10) . . ? O17 Nb7 Nb6 133.36(16) . . ? O25 Nb7 Nb6 78.60(12) . . ? O16 Nb7 Nb6 30.54(13) . . ? O18 Nb7 Nb6 121.92(12) . . ? O6 Nb7 Nb6 82.23(12) . . ? O23 Nb7 Nb6 46.05(9) . . ? Nb2 Nb7 Nb6 62.147(18) . . ? O17 Nb7 Nb8 134.62(16) . . ? O25 Nb7 Nb8 78.75(13) . . ? O16 Nb7 Nb8 122.32(13) . . ? O18 Nb7 Nb8 30.09(12) . . ? O6 Nb7 Nb8 81.49(12) . . ? O23 Nb7 Nb8 46.19(9) . . ? Nb2 Nb7 Nb8 61.545(18) . . ? Nb6 Nb7 Nb8 91.96(2) . . ? O19 Nb8 O18 103.18(19) . . ? O19 Nb8 O26 103.02(19) . . ? O18 Nb8 O26 94.70(19) . . ? O19 Nb8 O20 103.80(18) . . ? O18 Nb8 O20 150.99(16) . . ? O26 Nb8 O20 89.47(16) . . ? O19 Nb8 O7 103.26(17) . . ? O18 Nb8 O7 90.10(17) . . ? O26 Nb8 O7 151.41(16) . . ? O20 Nb8 O7 73.50(15) . . ? O19 Nb8 O23 176.30(17) . . ? O18 Nb8 O23 79.26(16) . . ? O26 Nb8 O23 79.41(16) . . ? O20 Nb8 O23 73.31(14) . . ? O7 Nb8 O23 73.83(14) . . ? O19 Nb8 Nb3 92.21(14) . . ? O18 Nb8 Nb3 129.22(13) . . ? O26 Nb8 Nb3 128.77(13) . . ? O20 Nb8 Nb3 39.31(10) . . ? O7 Nb8 Nb3 39.12(11) . . ? O23 Nb8 Nb3 84.10(9) . . ? O19 Nb8 Nb7 134.63(15) . . ? O18 Nb8 Nb7 31.61(12) . . ? O26 Nb8 Nb7 83.92(13) . . ? O20 Nb8 Nb7 121.22(10) . . ? O7 Nb8 Nb7 85.61(11) . . ? O23 Nb8 Nb7 48.03(10) . . ? Nb3 Nb8 Nb7 118.39(2) . . ? O19 Nb8 Nb10 134.38(14) . . ? O18 Nb8 Nb10 83.93(13) . . ? O26 Nb8 Nb10 31.51(12) . . ? O20 Nb8 Nb10 84.83(10) . . ? O7 Nb8 Nb10 121.94(10) . . ? O23 Nb8 Nb10 48.27(10) . . ? Nb3 Nb8 Nb10 118.19(2) . . ? Nb7 Nb8 Nb10 60.968(18) . . ? O21 Nb9 O27 107.77(17) . . ? O21 Nb9 O22 97.14(18) . . ? O27 Nb9 O22 98.28(17) . . ? O21 Nb9 O20 96.99(17) . . ? O27 Nb9 O20 96.49(17) . . ? O22 Nb9 O20 155.35(15) . . ? O21 Nb9 O23 165.29(18) . . ? O27 Nb9 O23 86.93(18) . . ? O22 Nb9 O23 80.90(16) . . ? O20 Nb9 O23 80.31(15) . . ? O21 Nb9 O14 86.31(17) . . ? O27 Nb9 O14 165.87(17) . . ? O22 Nb9 O14 80.64(16) . . ? O20 Nb9 O14 80.23(15) . . ? O23 Nb9 O14 78.98(14) . . ? O21 Nb9 Nb10 143.90(13) . . ? O27 Nb9 Nb10 36.14(13) . . ? O22 Nb9 Nb10 90.86(13) . . ? O20 Nb9 Nb10 89.52(11) . . ? O23 Nb9 Nb10 50.79(11) . . ? O14 Nb9 Nb10 129.77(11) . . ? O21 Nb9 Nb4 36.30(13) . . ? O27 Nb9 Nb4 144.07(14) . . ? O22 Nb9 Nb4 89.43(13) . . ? O20 Nb9 Nb4 90.10(11) . . ? O23 Nb9 Nb4 129.00(11) . . ? O14 Nb9 Nb4 50.02(11) . . ? Nb10 Nb9 Nb4 179.60(2) . . ? O21 Nb9 Nb6 133.85(13) . . ? O27 Nb9 Nb6 85.05(13) . . ? O22 Nb9 Nb6 36.71(12) . . ? O20 Nb9 Nb6 126.14(11) . . ? O23 Nb9 Nb6 45.92(11) . . ? O14 Nb9 Nb6 85.87(10) . . ? Nb10 Nb9 Nb6 61.301(19) . . ? Nb4 Nb9 Nb6 118.86(2) . . ? O28 Nb10 O25 104.8(2) . . ? O28 Nb10 O26 104.3(2) . . ? O25 Nb10 O26 88.77(18) . . ? O28 Nb10 O24 103.49(19) . . ? O25 Nb10 O24 88.26(18) . . ? O26 Nb10 O24 151.88(18) . . ? O28 Nb10 O27 103.7(2) . . ? O25 Nb10 O27 151.51(18) . . ? O26 Nb10 O27 85.20(17) . . ? O24 Nb10 O27 84.20(17) . . ? O28 Nb10 O23 177.71(19) . . ? O25 Nb10 O23 77.35(16) . . ? O26 Nb10 O23 76.38(15) . . ? O24 Nb10 O23 75.69(16) . . ? O27 Nb10 O23 74.17(15) . . ? O28 Nb10 Nb9 135.25(17) . . ? O25 Nb10 Nb9 119.91(13) . . ? O26 Nb10 Nb9 79.38(12) . . ? O24 Nb10 Nb9 77.97(12) . . ? O27 Nb10 Nb9 31.60(12) . . ? O23 Nb10 Nb9 42.57(10) . . ? O28 Nb10 Nb8 134.75(15) . . ? O25 Nb10 Nb8 78.70(13) . . ? O26 Nb10 Nb8 30.63(13) . . ? O24 Nb10 Nb8 121.76(13) . . ? O27 Nb10 Nb8 82.06(11) . . ? O23 Nb10 Nb8 46.11(9) . . ? Nb9 Nb10 Nb8 61.788(17) . . ? O28 Nb10 Nb6 133.66(15) . . ? O25 Nb10 Nb6 78.10(13) . . ? O26 Nb10 Nb6 122.04(13) . . ? O24 Nb10 Nb6 30.39(13) . . ? O27 Nb10 Nb6 81.63(11) . . ? O23 Nb10 Nb6 45.71(9) . . ? Nb9 Nb10 Nb6 61.010(19) . . ? Nb8 Nb10 Nb6 91.53(2) . . ? Nb2 O2 Nb1 113.4(2) . . ? Nb3 O3 Nb1 118.3(2) . . ? Nb1 O4 Nb4 119.86(19) . . ? Nb5 O5 Nb1 117.2(2) . . ? Nb2 O6 Nb7 112.7(2) . . ? Nb2 O7 Nb3 109.30(18) . . ? Nb2 O7 Nb8 109.42(18) . . ? Nb3 O7 Nb8 101.38(16) . . ? Nb3 O9 Nb4 116.3(2) . . ? Nb5 O11 Nb4 118.7(2) . . ? Nb2 O13 Nb5 109.36(19) . . ? Nb2 O13 Nb6 109.17(19) . . ? Nb5 O13 Nb6 101.62(15) . . ? Nb2 O14 Nb9 101.32(16) . . ? Nb2 O14 Nb3 93.64(15) . . ? Nb9 O14 Nb3 93.64(14) . . ? Nb2 O14 Nb5 93.27(14) . . ? Nb9 O14 Nb5 93.47(15) . . ? Nb3 O14 Nb5 168.93(18) . . ? Nb2 O14 Nb4 171.6(2) . . ? Nb9 O14 Nb4 87.08(15) . . ? Nb3 O14 Nb4 86.13(13) . . ? Nb5 O14 Nb4 85.77(13) . . ? Nb2 O14 Nb1 86.55(15) . . ? Nb9 O14 Nb1 172.1(2) . . ? Nb3 O14 Nb1 85.89(13) . . ? Nb5 O14 Nb1 85.91(12) . . ? Nb4 O14 Nb1 85.05(12) . . ? Nb6 O16 Nb7 117.6(2) . . ? Nb8 O18 Nb7 118.3(2) . . ? Nb9 O20 Nb8 109.33(17) . . ? Nb9 O20 Nb3 108.90(18) . . ? Nb8 O20 Nb3 101.41(15) . . ? Nb9 O21 Nb4 112.6(2) . . ? Nb9 O22 Nb6 108.57(18) . . ? Nb9 O22 Nb5 109.76(19) . . ? Nb6 O22 Nb5 101.19(16) . . ? Nb9 O23 Nb2 101.13(16) . . ? Nb9 O23 Nb6 93.26(15) . . ? Nb2 O23 Nb6 94.21(15) . . ? Nb9 O23 Nb8 94.17(15) . . ? Nb2 O23 Nb8 92.98(15) . . ? Nb6 O23 Nb8 168.48(19) . . ? Nb9 O23 Nb7 172.2(2) . . ? Nb2 O23 Nb7 86.69(15) . . ? Nb6 O23 Nb7 85.66(13) . . ? Nb8 O23 Nb7 85.79(13) . . ? Nb9 O23 Nb10 86.64(15) . . ? Nb2 O23 Nb10 172.2(2) . . ? Nb6 O23 Nb10 86.04(13) . . ? Nb8 O23 Nb10 85.62(13) . . ? Nb7 O23 Nb10 85.55(12) . . ? Nb6 O24 Nb10 118.0(2) . . ? Nb10 O25 Nb7 119.5(2) . . ? Nb8 O26 Nb10 117.9(2) . . ? Nb9 O27 Nb10 112.3(2) . . ? N31 C31 H31A 109.5 . . ? N31 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N31 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 N31 C33 110.7(6) . . ? C32 N31 C34 110.1(6) . . ? C33 N31 C34 109.8(6) . . ? C32 N31 C31 109.0(6) . . ? C33 N31 C31 108.3(6) . . ? C34 N31 C31 109.0(6) . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C33 H33A 109.5 . . ? N31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N31 C34 H34A 109.5 . . ? N31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N35 C35 H35A 109.5 . . ? N35 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N35 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C35 N35 C36 110.3(6) . . ? C35 N35 C38 108.9(5) . . ? C36 N35 C38 110.4(6) . . ? C35 N35 C37 107.9(6) . . ? C36 N35 C37 108.6(5) . . ? C38 N35 C37 110.8(5) . . ? N35 C36 H36A 109.5 . . ? N35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N35 C37 H37A 109.5 . . ? N35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N35 C38 H38A 109.5 . . ? N35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N39 C39 H39A 109.5 . . ? N39 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N39 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 N39 C39 110.7(6) . . ? C42 N39 C40 108.6(8) . . ? C39 N39 C40 110.4(8) . . ? C42 N39 C41 106.8(7) . . ? C39 N39 C41 108.1(7) . . ? C40 N39 C41 112.2(11) . . ? N39 C40 H40A 109.5 . . ? N39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N39 C41 H41A 109.5 . . ? N39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N39 C42 H42A 109.5 . . ? N39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N43 C43 H43A 109.5 . . ? N43 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N43 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C43 N43 C46 112.9(7) . . ? C43 N43 C44 110.6(7) . . ? C46 N43 C44 109.5(6) . . ? C43 N43 C45 107.8(7) . . ? C46 N43 C45 108.0(7) . . ? C44 N43 C45 107.8(6) . . ? N43 C44 H44A 109.5 . . ? N43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N43 C45 H45A 109.5 . . ? N43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N43 C46 H46A 109.5 . . ? N43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N47 C47 H47A 109.5 . . ? N47 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N47 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C50 N47 C48 108.2(8) . . ? C50 N47 C47 108.8(7) . . ? C48 N47 C47 111.1(6) . . ? C50 N47 C49 113.9(9) . . ? C48 N47 C49 105.6(7) . . ? C47 N47 C49 109.3(7) . . ? N47 C48 H48A 109.5 . . ? N47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N47 C49 H49A 109.5 . . ? N47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N47 C50 H50A 109.5 . . ? N47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N51 C51 H51A 109.5 . . ? N51 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N51 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C52 N51 C53 110.6(6) . . ? C52 N51 C51 109.2(6) . . ? C53 N51 C51 107.6(5) . . ? C52 N51 C54 110.1(6) . . ? C53 N51 C54 109.8(5) . . ? C51 N51 C54 109.4(5) . . ? N51 C52 H52A 109.5 . . ? N51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N51 C53 H53A 109.5 . . ? N51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N51 C54 H54A 109.5 . . ? N51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N55 C55 H55A 109.5 . . ? N55 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N55 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C56 N55 C55 111.0(6) . . ? C56 N55 C58 108.5(7) . . ? C55 N55 C58 109.1(6) . . ? C56 N55 C57 110.7(6) . . ? C55 N55 C57 109.4(6) . . ? C58 N55 C57 108.0(5) . . ? N55 C56 H56A 109.5 . . ? N55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N55 C57 H57A 109.5 . . ? N55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N55 C58 H58A 109.5 . . ? N55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? H61A O61 H61B 104.2 . . ? H64A O64 H64B 106(12) . . ? H65A O65 H65B 106(7) . . ? H66A O66 H66B 121.3 . . ? H67A O67 H67B 97.9 . . ? H68A O68 H68B 106.9 . . ? H69A O69 H69B 105.6 . . ? H70A O70 H70B 121.1 . . ? H71A O71 H71B 106(6) . . ? H72A O72 H72B 107(10) . . ? H73A O73 H73B 106(7) . . ? H74A O74 H74B 107(8) . . ? H75A O75 H75B 112(9) . . ? H77A O77 H77B 108(7) . . ? H78A O78 H78B 111(6) . . ? H79A O79 H79B 107.0 . . ? H81A O81 H81B 106(7) . . ? H82A O82 H82B 108(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O61 H61A O17 0.84 2.00 2.844(6) 180. . O61 H61B O62 0.84 2.39 2.796(12) 110.0 . O64 H64A O63 0.84(5) 2.19(9) 2.921(17) 146(14) . O64 H64B O62 0.85(7) 2.61(11) 3.418(12) 161(14) . O65 H65A O64 0.84(2) 2.05(2) 2.875(11) 169(9) . O65 H65B O21 0.84(6) 1.99(6) 2.819(7) 167(7) 1_655 O66 H66B O76 0.84 2.41 2.845(7) 113. 2_666 O66 H66A O76 0.85 1.96 2.806(7) 180. . O66 H66B O76 0.84 2.41 2.845(7) 113. 2_666 O67 H67A O71 0.86 1.99 2.851(7) 180. 1_554 O67 H67B O9 0.86 1.97 2.824(6) 179. 1_655 O68 H68A O63 0.84 1.94 2.698(11) 150. 2_676 O68 H68B O63 0.84 2.49 3.202(17) 144. . O69 H69A O67 0.84 1.95 2.795(4) 180. 1_556 O69 H69B O77 0.84 2.02 2.842(5) 166. . O70 H70A O19 0.84 1.99 2.783(5) 156. 1_656 O70 H70B O17 0.84 1.95 2.798(5) 179. 2_676 O71 H71A O8 0.84(6) 1.87(6) 2.705(6) 175(7) 1_656 O71 H71B O1 0.84(5) 1.96(3) 2.754(6) 157(7) 2_666 O72 H72B O19 0.84(10) 1.96(9) 2.759(7) 160(9) 1_656 O73 H73A O72 0.84(3) 1.87(3) 2.697(8) 166(10) . O73 H73B O82 0.84(6) 2.03(4) 2.822(7) 157(10) 1_655 O74 H74A O76 0.84(3) 2.42(9) 2.891(9) 117(8) . O74 H74B O77 0.84(8) 1.97(7) 2.755(8) 155(7) . O75 H75A O70 0.84(5) 2.14(8) 2.765(8) 131(10) . O77 H77A O78 0.84(6) 1.89(3) 2.710(7) 165(9) . O77 H77B O80 0.84(6) 2.01(4) 2.797(8) 156(9) . O78 H78A O10 0.84(6) 1.95(6) 2.757(6) 163(6) 2_566 O78 H78B O12 0.84(6) 1.96(6) 2.786(6) 174(7) . O79 H79A O81 0.84 1.92 2.749(6) 170. . O79 H79B O80 0.84 2.32 2.735(8) 111. . O81 H81A O15 0.85(7) 1.97(4) 2.753(6) 153(7) . O81 H81B O63 0.84(7) 2.13(6) 2.722(11) 127(6) 2_676 O82 H82A O15 0.84(4) 2.06(6) 2.687(6) 131(7) . O82 H82B O12 0.84(6) 1.92(6) 2.761(6) 176(8) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.721 _refine_diff_density_min -1.778 _refine_diff_density_rms 0.151