#------------------------------------------------------------------------------ #$Date: 2017-06-01 08:19:34 +0300 (Thu, 01 Jun 2017) $ #$Revision: 197132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/83/7228353.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7228353 loop_ _publ_author_name 'Li, Li' 'Niu, Yanjun' 'Dong, Kaili' 'Ma, Pengtao' 'Zhang, Chao' 'Niu, Jingyang' 'Wang, Jingping' _publ_section_title ; A Ni-containing decaniobate incorporating organic ligands: synthesis, structure, and catalysis for allylic alcohol epoxidation ; _journal_issue 46 _journal_name_full 'RSC Adv.' _journal_page_first 28696 _journal_paper_doi 10.1039/C7RA03254D _journal_volume 7 _journal_year 2017 _chemical_formula_moiety 'C4 H16 N4 Na8 Nb10 Ni3 O58, 2(O)' _chemical_formula_sum 'C4 H72 N4 Na8 Nb10 Ni3 O60' _chemical_formula_weight 2425.80 _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2016-07-09 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _audit_update_record ; 2017-01-09 deposited with the CCDC. 2017-05-17 downloaded from the CCDC. ; _cell_angle_alpha 61.8590(10) _cell_angle_beta 63.6420(10) _cell_angle_gamma 61.2230(10) _cell_formula_units_Z 1 _cell_length_a 12.5635(8) _cell_length_b 12.9279(9) _cell_length_c 13.1370(9) _cell_measurement_reflns_used 3147 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.25 _cell_measurement_theta_min 2.19 _cell_volume 1582.83(19) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS-1997 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8189 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.098 _diffrn_reflns_theta_max 25.098 _diffrn_reflns_theta_min 1.832 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.783 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0592 before and 0.0311 after correction. The Ratio of minimum to maximum transmission is 0.7994. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1186 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.718 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.163 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 5578 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0411 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+9.6880P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0992 _refine_ls_wR_factor_ref 0.1077 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4475 _reflns_number_total 5578 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ra03254d2.cif _cod_data_source_block njy1 _cod_database_code 7228353 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.768 _shelx_estimated_absorpt_t_min 0.426 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H) groups 2.a Secondary CH2 refined with riding coordinates: N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D) ; _shelx_res_file ; njy1.res created by SHELXL-2014/7 TITL NJY1 in P-1 CELL 0.71073 12.5635 12.9279 13.137 61.859 63.642 61.223 ZERR 1 0.0008 0.0009 0.0009 0.001 0.001 0.001 LATT 1 SFAC C N Nb Ni O H Na UNIT 4 4 10 3 60 72 8 L.S. 10 PLAN -20 SIZE 0.37 0.18 0.1 BOND $H HTAB fmap 2 acta OMIT -3 50.2 OMIT 2 5 2 OMIT 1 3 2 OMIT 6 -2 5 OMIT 3 1 4 OMIT 3 8 0 OMIT -3 -9 2 OMIT 0 -3 1 REM REM REM WGHT 0.046100 9.688001 FVAR 0.06067 NB1 3 0.596373 -0.123920 0.305442 11.00000 0.01200 0.01287 = 0.01455 -0.00701 -0.00171 -0.00370 NB2 3 0.607205 -0.296646 0.589111 11.00000 0.01292 0.00937 = 0.01671 -0.00402 -0.00329 -0.00302 NB3 3 0.749872 -0.120711 0.579415 11.00000 0.01128 0.01297 = 0.01658 -0.00648 -0.00423 -0.00230 NB4 3 0.739646 0.051756 0.294566 11.00000 0.01166 0.01221 = 0.01372 -0.00555 -0.00002 -0.00493 NB5 3 0.870369 -0.260199 0.374792 11.00000 0.00989 0.01338 = 0.01976 -0.00984 -0.00183 -0.00098 NI1 4 0.500000 0.000000 0.500000 10.50000 0.00985 0.00978 = 0.01246 -0.00476 -0.00177 -0.00143 NI2 4 0.506507 -0.161802 0.772044 11.00000 0.01732 0.01527 = 0.01621 -0.00393 -0.00454 -0.00443 NA1 7 0.857409 -0.084336 0.077027 11.00000 0.03617 0.03624 = 0.02293 -0.01447 0.00138 -0.01816 NA2 7 0.939310 -0.341749 -0.010157 11.00000 0.03215 0.02826 = 0.03158 -0.01148 -0.00669 -0.01091 NA3 7 1.213835 -0.399845 -0.330336 11.00000 0.03865 0.03189 = 0.03187 -0.00882 -0.01029 -0.01717 NA4 7 1.222894 -0.227271 -0.632129 11.00000 0.07834 0.04675 = 0.04845 -0.00973 -0.02354 -0.03585 O1 5 1.021495 -0.358082 0.315381 11.00000 0.02772 O2 5 0.560421 -0.425608 0.700532 11.00000 0.02346 O3 5 0.549459 -0.127473 0.198569 11.00000 0.02293 O4 5 0.794235 0.176216 0.183988 11.00000 0.02586 O5 5 0.894406 -0.233450 0.498212 11.00000 0.01822 O6 5 0.809658 -0.123169 0.680049 11.00000 0.02547 O7 5 0.771960 -0.232631 0.272775 11.00000 0.01566 O8 5 0.886068 -0.092506 0.262897 11.00000 0.01743 O9 5 0.778586 -0.375857 0.505979 11.00000 0.01777 O10 5 0.778311 0.023493 0.437194 11.00000 0.01633 O11 5 0.662380 0.021004 0.207719 11.00000 0.01494 O12 5 0.546348 -0.254316 0.454609 11.00000 0.01548 O13 5 0.670724 -0.120002 0.441965 11.00000 0.01313 O14 5 0.674499 -0.258792 0.677769 11.00000 0.01654 O15 5 0.445836 -0.150205 0.637865 11.00000 0.01296 O16 5 0.562905 -0.009688 0.629630 11.00000 0.01304 0.01329 = 0.01372 -0.00442 -0.00488 -0.00223 N1 2 0.450408 -0.308994 0.905998 11.00000 0.02711 AFIX 23 H1A 6 0.367065 -0.282621 0.938670 11.00000 -1.20000 H1B 6 0.470227 -0.367006 0.875972 11.00000 -1.20000 AFIX 0 N2 2 0.567712 -0.172157 0.900881 11.00000 0.02889 AFIX 23 H2A 6 0.651869 -0.201313 0.880957 11.00000 -1.20000 H2B 6 0.540453 -0.096549 0.905553 11.00000 -1.20000 AFIX 0 C1 1 0.516732 -0.361291 0.997413 11.00000 0.03126 AFIX 23 H1C 6 0.602953 -0.414223 0.970547 11.00000 -1.20000 H1D 6 0.474283 -0.411715 1.072284 11.00000 -1.20000 AFIX 0 C2 1 0.517111 -0.256002 1.016851 11.00000 0.03518 AFIX 23 H2C 6 0.431651 -0.210248 1.054583 11.00000 -1.20000 H2D 6 0.568846 -0.289063 1.069721 11.00000 -1.20000 AFIX 0 O1W 5 1.294786 -0.235405 -0.487475 11.00000 0.02889 O2W 5 1.133600 -0.384934 -0.473910 11.00000 0.03280 O3W 5 1.304351 -0.060015 -0.790956 11.00000 0.03062 O4W 5 1.307104 -0.413466 -0.196677 11.00000 0.03046 O5W 5 1.121283 -0.560590 -0.203473 11.00000 0.03072 O6W 5 1.020927 -0.251146 -0.228050 11.00000 0.03878 O7W 5 1.042350 -0.251167 0.030381 11.00000 0.03376 O8W 5 0.854962 -0.467940 -0.009536 11.00000 0.03562 O9W 5 0.761397 -0.145414 -0.002896 11.00000 0.03296 O10W 5 1.254625 -0.332152 -0.759207 11.00000 0.04803 O11W 5 0.146779 0.461550 0.217580 11.00000 0.04775 O12W 5 0.886418 0.077030 -0.098941 11.00000 0.05620 O13W 5 1.047169 -0.048558 -0.607372 11.00000 0.08151 O14W 5 1.414726 -0.554119 -0.389510 11.00000 0.10711 HKLF 4 REM NJY1 in P-1 REM R1 = 0.0411 for 4475 Fo > 4sig(Fo) and 0.0545 for all 5578 data REM 238 parameters refined using 0 restraints END WGHT 0.0461 9.6884 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y, -z+1 HTAB N1 O4_$1 HTAB N1 O2 HTAB N2 O6 HTAB N2 O3_$1 REM Highest difference peak 1.718, deepest hole -1.041, 1-sigma level 0.163 Q1 1 1.3988 -0.5153 -0.4520 11.00000 0.05 1.72 Q2 1 1.1948 -0.5186 0.1821 11.00000 0.05 1.70 Q3 1 1.0419 -0.0581 -0.5522 11.00000 0.05 1.53 Q4 1 1.0546 -0.0418 -0.6640 11.00000 0.05 1.42 Q5 1 1.4454 -0.3609 -0.6927 11.00000 0.05 1.35 Q6 1 1.1116 -0.5614 0.2384 11.00000 0.05 1.33 Q7 1 1.4188 -0.5818 -0.3510 11.00000 0.05 1.33 Q8 1 0.9027 0.0283 -0.1180 11.00000 0.05 1.22 Q9 1 1.2464 -0.3334 -0.8020 11.00000 0.05 0.99 Q10 1 1.1586 -0.3743 -0.5175 11.00000 0.05 0.89 Q11 1 1.1055 -0.0935 0.0772 11.00000 0.05 0.85 Q12 1 1.1020 -0.4009 -0.4248 11.00000 0.05 0.85 Q13 1 1.2998 -0.2596 -0.4491 11.00000 0.05 0.83 Q14 1 1.0746 -0.2829 0.0875 11.00000 0.05 0.81 Q15 1 1.0270 -0.3804 0.3632 11.00000 0.05 0.78 Q16 1 0.8219 -0.4126 -0.0235 11.00000 0.05 0.75 Q17 1 1.0191 -0.3203 0.2633 11.00000 0.05 0.74 Q18 1 0.9441 -0.4655 0.2118 11.00000 0.05 0.74 Q19 1 0.8834 -0.5030 0.0064 11.00000 0.05 0.72 Q20 1 0.7609 0.1964 0.1565 11.00000 0.05 0.71 ; _shelx_res_checksum 2143 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Nb1 Nb 0.59637(5) -0.12392(5) 0.30544(5) 0.01312(14) Uani 1 1 d . . . Nb2 Nb 0.60720(5) -0.29665(5) 0.58911(5) 0.01386(14) Uani 1 1 d . . . Nb3 Nb 0.74987(5) -0.12071(5) 0.57941(5) 0.01361(14) Uani 1 1 d . . . Nb4 Nb 0.73965(5) 0.05176(5) 0.29457(5) 0.01304(14) Uani 1 1 d . . . Nb5 Nb 0.87037(5) -0.26020(5) 0.37479(5) 0.01473(15) Uani 1 1 d . . . Ni1 Ni 0.5000 0.0000 0.5000 0.0117(2) Uani 1 2 d S T P Ni2 Ni 0.50651(8) -0.16180(8) 0.77204(8) 0.0174(2) Uani 1 1 d . . . Na1 Na 0.8574(3) -0.0843(3) 0.0770(3) 0.0310(7) Uani 1 1 d . . . Na2 Na 0.9393(3) -0.3417(3) -0.0102(3) 0.0306(7) Uani 1 1 d . . . Na3 Na 1.2138(3) -0.3998(3) -0.3303(3) 0.0324(7) Uani 1 1 d . . . Na4 Na 1.2229(4) -0.2273(3) -0.6321(3) 0.0515(9) Uani 1 1 d . . . O1 O 1.0215(5) -0.3581(4) 0.3154(4) 0.0277(11) Uiso 1 1 d . . . O2 O 0.5604(4) -0.4256(4) 0.7005(4) 0.0235(11) Uiso 1 1 d . . . O3 O 0.5495(4) -0.1275(4) 0.1986(4) 0.0229(10) Uiso 1 1 d . . . O4 O 0.7942(4) 0.1762(4) 0.1840(4) 0.0259(11) Uiso 1 1 d . . . O5 O 0.8944(4) -0.2335(4) 0.4982(4) 0.0182(10) Uiso 1 1 d . . . O6 O 0.8097(4) -0.1232(4) 0.6800(4) 0.0255(11) Uiso 1 1 d . . . O7 O 0.7720(4) -0.2326(4) 0.2728(4) 0.0157(9) Uiso 1 1 d . . . O8 O 0.8861(4) -0.0925(4) 0.2629(4) 0.0174(9) Uiso 1 1 d . . . O9 O 0.7786(4) -0.3759(4) 0.5060(4) 0.0178(10) Uiso 1 1 d . . . O10 O 0.7783(4) 0.0235(4) 0.4372(4) 0.0163(9) Uiso 1 1 d . . . O11 O 0.6624(4) 0.0210(4) 0.2077(4) 0.0149(9) Uiso 1 1 d . . . O12 O 0.5463(4) -0.2543(4) 0.4546(4) 0.0155(9) Uiso 1 1 d . . . O13 O 0.6707(4) -0.1200(4) 0.4420(4) 0.0131(9) Uiso 1 1 d . . . O14 O 0.6745(4) -0.2588(4) 0.6778(4) 0.0165(9) Uiso 1 1 d . . . O15 O 0.4458(4) -0.1502(4) 0.6379(4) 0.0130(9) Uiso 1 1 d . . . O16 O 0.5629(4) -0.0097(4) 0.6296(4) 0.0140(9) Uani 1 1 d . . . N1 N 0.4504(6) -0.3090(5) 0.9060(5) 0.0271(14) Uiso 1 1 d . . . H1A H 0.3671 -0.2826 0.9387 0.033 Uiso 1 1 calc R . . H1B H 0.4702 -0.3670 0.8760 0.033 Uiso 1 1 calc R . . N2 N 0.5677(6) -0.1722(6) 0.9009(5) 0.0289(14) Uiso 1 1 d . . . H2A H 0.6519 -0.2013 0.8810 0.035 Uiso 1 1 calc R . . H2B H 0.5405 -0.0965 0.9056 0.035 Uiso 1 1 calc R . . C1 C 0.5167(7) -0.3613(7) 0.9974(7) 0.0313(17) Uiso 1 1 d . . . H1C H 0.6030 -0.4142 0.9705 0.038 Uiso 1 1 calc R . . H1D H 0.4743 -0.4117 1.0723 0.038 Uiso 1 1 calc R . . C2 C 0.5171(8) -0.2560(7) 1.0169(7) 0.0352(18) Uiso 1 1 d . . . H2C H 0.4317 -0.2102 1.0546 0.042 Uiso 1 1 calc R . . H2D H 0.5688 -0.2891 1.0697 0.042 Uiso 1 1 calc R . . O1W O 1.2948(5) -0.2354(5) -0.4875(4) 0.0289(11) Uiso 1 1 d . . . O2W O 1.1336(5) -0.3849(5) -0.4739(5) 0.0328(12) Uiso 1 1 d . . . O3W O 1.3044(5) -0.0600(5) -0.7910(5) 0.0306(12) Uiso 1 1 d . . . O4W O 1.3071(5) -0.4135(5) -0.1967(5) 0.0305(12) Uiso 1 1 d . . . O5W O 1.1213(5) -0.5606(5) -0.2035(5) 0.0307(12) Uiso 1 1 d . . . O6W O 1.0209(5) -0.2511(5) -0.2280(5) 0.0388(13) Uiso 1 1 d . . . O7W O 1.0424(5) -0.2512(5) 0.0304(5) 0.0338(12) Uiso 1 1 d . . . O8W O 0.8550(5) -0.4679(5) -0.0095(5) 0.0356(13) Uiso 1 1 d . . . O9W O 0.7614(5) -0.1454(5) -0.0029(5) 0.0330(12) Uiso 1 1 d . . . O10W O 1.2546(6) -0.3322(6) -0.7592(6) 0.0480(15) Uiso 1 1 d . . . O11W O 0.1468(6) 0.4616(6) 0.2176(6) 0.0477(15) Uiso 1 1 d . . . O12W O 0.8864(6) 0.0770(6) -0.0989(6) 0.0562(17) Uiso 1 1 d . . . O13W O 1.0472(8) -0.0486(8) -0.6074(7) 0.082(2) Uiso 1 1 d . . . O14W O 1.4147(10) -0.5541(9) -0.3895(9) 0.107(3) Uiso 1 1 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 0.0120(3) 0.0129(3) 0.0146(3) -0.0070(2) -0.0017(2) -0.0037(2) Nb2 0.0129(3) 0.0094(3) 0.0167(3) -0.0040(2) -0.0033(2) -0.0030(2) Nb3 0.0113(3) 0.0130(3) 0.0166(3) -0.0065(2) -0.0042(2) -0.0023(2) Nb4 0.0117(3) 0.0122(3) 0.0137(3) -0.0056(2) 0.0000(2) -0.0049(2) Nb5 0.0099(3) 0.0134(3) 0.0198(3) -0.0098(2) -0.0018(2) -0.0010(2) Ni1 0.0098(5) 0.0098(5) 0.0125(6) -0.0048(4) -0.0018(4) -0.0014(4) Ni2 0.0173(4) 0.0153(4) 0.0162(4) -0.0039(3) -0.0045(3) -0.0044(3) Na1 0.0362(17) 0.0362(17) 0.0229(16) -0.0145(13) 0.0014(13) -0.0182(14) Na2 0.0321(17) 0.0283(16) 0.0316(17) -0.0115(13) -0.0067(13) -0.0109(13) Na3 0.0387(18) 0.0319(16) 0.0319(17) -0.0088(13) -0.0103(14) -0.0172(14) Na4 0.078(3) 0.047(2) 0.048(2) -0.0097(17) -0.0235(19) -0.036(2) O16 0.013(2) 0.013(2) 0.014(2) -0.0044(18) -0.0049(18) -0.0022(18) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Nb2 Nb1 Nb5 59.572(17) . . Nb2 Nb1 Na1 122.39(5) . . Nb5 Nb1 Na1 62.83(5) . . Ni1 Nb1 Nb2 58.585(14) . . Ni1 Nb1 Nb5 84.524(17) . . Ni1 Nb1 Na1 117.57(5) . . Ni2 Nb1 Nb2 120.64(2) 2_656 . Ni2 Nb1 Nb5 114.87(2) 2_656 . Ni2 Nb1 Ni1 62.053(19) 2_656 . Ni2 Nb1 Na1 84.54(5) 2_656 . O3 Nb1 Nb2 135.64(15) . . O3 Nb1 Nb5 132.89(15) . . O3 Nb1 Ni1 142.52(15) . . O3 Nb1 Ni2 93.70(15) . 2_656 O3 Nb1 Na1 85.16(16) . . O3 Nb1 O7 100.1(2) . . O3 Nb1 O11 101.47(19) . . O3 Nb1 O12 104.22(19) . . O3 Nb1 O13 176.90(18) . . O3 Nb1 O16 100.73(19) . 2_656 O7 Nb1 Nb2 81.31(13) . . O7 Nb1 Nb5 32.75(13) . . O7 Nb1 Ni1 117.24(13) . . O7 Nb1 Ni2 127.66(12) . 2_656 O7 Nb1 Na1 47.37(13) . . O7 Nb1 O11 86.63(17) . . O7 Nb1 O12 92.13(17) . . O7 Nb1 O13 77.29(16) . . O7 Nb1 O16 158.08(17) . 2_656 O11 Nb1 Nb2 122.81(12) . . O11 Nb1 Nb5 81.29(12) . . O11 Nb1 Ni1 79.28(12) . . O11 Nb1 Ni2 41.07(12) . 2_656 O11 Nb1 Na1 46.21(13) . . O11 Nb1 O13 76.76(15) . . O11 Nb1 O16 82.76(16) . 2_656 O12 Nb1 Nb2 31.96(12) . . O12 Nb1 Nb5 83.75(12) . . O12 Nb1 Ni1 78.33(12) . . O12 Nb1 Ni2 132.71(12) . 2_656 O12 Nb1 Na1 139.47(13) . . O12 Nb1 O11 154.09(17) . . O12 Nb1 O13 77.72(15) . . O12 Nb1 O16 89.18(17) . 2_656 O13 Nb1 Nb2 46.05(9) . . O13 Nb1 Nb5 44.56(10) . . O13 Nb1 Ni1 39.97(10) . . O13 Nb1 Ni2 86.61(10) . 2_656 O13 Nb1 Na1 91.80(11) . . O16 Nb1 Nb2 88.41(11) 2_656 . O16 Nb1 Nb5 126.04(12) 2_656 . O16 Nb1 Ni1 41.84(11) 2_656 . O16 Nb1 Ni2 44.13(11) 2_656 2_656 O16 Nb1 Na1 128.36(13) 2_656 . O16 Nb1 O13 81.63(15) 2_656 . Nb5 Nb2 Nb1 60.247(17) . . Ni1 Nb2 Nb1 57.334(13) . . Ni1 Nb2 Nb5 84.236(16) . . Ni2 Nb2 Nb1 118.61(2) . . Ni2 Nb2 Nb5 114.81(2) . . Ni2 Nb2 Ni1 61.274(18) . . O2 Nb2 Nb1 135.93(15) . . O2 Nb2 Nb5 135.60(15) . . O2 Nb2 Ni1 140.12(15) . . O2 Nb2 Ni2 92.70(15) . . O2 Nb2 O9 102.8(2) . . O2 Nb2 O12 104.22(19) . . O2 Nb2 O13 178.43(18) . . O2 Nb2 O14 102.15(19) . . O2 Nb2 O15 99.55(19) . . O9 Nb2 Nb1 80.86(13) . . O9 Nb2 Nb5 32.82(13) . . O9 Nb2 Ni1 117.05(13) . . O9 Nb2 Ni2 130.25(13) . . O9 Nb2 O12 91.20(18) . . O9 Nb2 O13 77.74(16) . . O9 Nb2 O14 89.61(18) . . O9 Nb2 O15 157.22(17) . . O12 Nb2 Nb1 31.94(12) . . O12 Nb2 Nb5 84.36(12) . . O12 Nb2 Ni1 77.21(12) . . O12 Nb2 Ni2 130.48(12) . . O12 Nb2 O13 77.20(15) . . O12 Nb2 O14 152.75(17) . . O12 Nb2 O15 87.45(17) . . O13 Nb2 Nb1 45.54(10) . . O13 Nb2 Nb5 44.93(10) . . O13 Nb2 Ni1 39.31(9) . . O13 Nb2 Ni2 85.83(10) . . O14 Nb2 Nb1 121.88(12) . . O14 Nb2 Nb5 81.66(12) . . O14 Nb2 Ni1 78.20(12) . . O14 Nb2 Ni2 40.71(12) . . O14 Nb2 O13 76.36(15) . . O14 Nb2 O15 81.48(16) . . O15 Nb2 Nb1 86.11(11) . . O15 Nb2 Nb5 124.56(11) . . O15 Nb2 Ni1 40.64(11) . . O15 Nb2 Ni2 43.51(11) . . O15 Nb2 O13 79.79(15) . . Nb5 Nb3 Nb4 60.109(17) . . Ni1 Nb3 Nb4 57.307(13) . . Ni1 Nb3 Nb5 84.265(16) . . Ni2 Nb3 Nb4 118.81(2) . . Ni2 Nb3 Nb5 115.03(2) . . Ni2 Nb3 Ni1 61.504(19) . . O5 Nb3 Nb4 80.78(13) . . O5 Nb3 Nb5 32.00(13) . . O5 Nb3 Ni1 116.27(13) . . O5 Nb3 Ni2 129.35(13) . . O5 Nb3 O10 90.38(18) . . O5 Nb3 O13 76.84(16) . . O5 Nb3 O14 88.43(17) . . O5 Nb3 O16 156.86(18) . . O6 Nb3 Nb4 134.75(15) . . O6 Nb3 Nb5 134.42(16) . . O6 Nb3 Ni1 141.32(16) . . O6 Nb3 Ni2 94.21(16) . . O6 Nb3 O5 102.4(2) . . O6 Nb3 O10 103.6(2) . . O6 Nb3 O13 179.21(19) . . O6 Nb3 O14 103.4(2) . . O6 Nb3 O16 100.33(19) . . O10 Nb3 Nb4 31.39(12) . . O10 Nb3 Nb5 83.04(13) . . O10 Nb3 Ni1 77.62(12) . . O10 Nb3 Ni2 131.66(13) . . O10 Nb3 O13 76.73(16) . . O10 Nb3 O14 152.58(17) . . O10 Nb3 O16 88.43(17) . . O13 Nb3 Nb4 45.49(9) . . O13 Nb3 Nb5 44.84(10) . . O13 Nb3 Ni1 39.43(9) . . O13 Nb3 Ni2 86.10(10) . . O14 Nb3 Nb4 121.80(12) . . O14 Nb3 Nb5 81.53(12) . . O14 Nb3 Ni1 78.40(12) . . O14 Nb3 Ni2 41.00(12) . . O14 Nb3 O13 76.33(15) . . O14 Nb3 O16 82.16(17) . . O16 Nb3 Nb4 86.30(11) . . O16 Nb3 Nb5 125.11(12) . . O16 Nb3 Ni1 41.11(11) . . O16 Nb3 Ni2 43.86(11) . . O16 Nb3 O13 80.40(15) . . Nb3 Nb4 Na1 121.63(5) . . Nb5 Nb4 Nb3 59.566(16) . . Nb5 Nb4 Na1 62.08(5) . . Ni1 Nb4 Nb3 58.302(14) . . Ni1 Nb4 Nb5 84.493(16) . . Ni1 Nb4 Na1 115.51(5) . . Ni2 Nb4 Nb3 120.40(2) 2_656 . Ni2 Nb4 Nb5 114.97(2) 2_656 . Ni2 Nb4 Ni1 62.096(19) 2_656 . Ni2 Nb4 Na1 83.41(5) 2_656 . O4 Nb4 Nb3 134.18(16) . . O4 Nb4 Nb5 134.04(16) . . O4 Nb4 Ni1 141.47(16) . . O4 Nb4 Ni2 94.20(15) . 2_656 O4 Nb4 Na1 88.95(16) . . O4 Nb4 O8 101.3(2) . . O4 Nb4 O10 103.1(2) . . O4 Nb4 O11 103.49(19) . . O4 Nb4 O13 178.57(19) . . O4 Nb4 O15 100.29(19) . 2_656 O8 Nb4 Nb3 81.85(13) . . O8 Nb4 Nb5 32.77(13) . . O8 Nb4 Ni1 117.19(13) . . O8 Nb4 Ni2 127.19(13) . 2_656 O8 Nb4 Na1 47.30(14) . . O8 Nb4 O10 91.50(18) . . O8 Nb4 O11 85.98(17) . . O8 Nb4 O13 77.26(16) . . O8 Nb4 O15 157.39(17) . 2_656 O10 Nb4 Nb3 31.32(12) . . O10 Nb4 Nb5 82.49(12) . . O10 Nb4 Ni1 78.47(12) . . O10 Nb4 Ni2 133.47(13) . 2_656 O10 Nb4 Na1 138.78(13) . . O10 Nb4 O11 153.25(17) . . O10 Nb4 O13 77.09(16) . . O10 Nb4 O15 90.02(17) . 2_656 O11 Nb4 Nb3 122.30(12) . . O11 Nb4 Nb5 81.07(12) . . O11 Nb4 Ni1 79.08(12) . . O11 Nb4 Ni2 41.22(12) . 2_656 O11 Nb4 Na1 44.65(13) . . O11 Nb4 O13 76.39(15) . . O11 Nb4 O15 82.59(16) . 2_656 O13 Nb4 Nb3 45.91(10) . . O13 Nb4 Nb5 44.54(10) . . O13 Nb4 Ni1 39.95(10) . . O13 Nb4 Ni2 86.63(10) . 2_656 O13 Nb4 Na1 90.00(11) . . O15 Nb4 Nb3 87.87(11) 2_656 . O15 Nb4 Nb5 125.51(11) 2_656 . O15 Nb4 Ni1 41.35(11) 2_656 . O15 Nb4 Ni2 44.08(11) 2_656 2_656 O15 Nb4 Na1 126.89(13) 2_656 . O15 Nb4 O13 81.12(15) 2_656 . Nb1 Nb5 Nb4 61.756(16) . . Nb1 Nb5 Na1 59.07(5) . . Nb2 Nb5 Nb1 60.180(17) . . Nb2 Nb5 Nb3 62.272(17) . . Nb2 Nb5 Nb4 92.059(19) . . Nb2 Nb5 Na1 119.24(5) . . Nb3 Nb5 Nb1 91.902(19) . . Nb3 Nb5 Nb4 60.325(17) . . Nb3 Nb5 Na1 120.74(5) . . Nb4 Nb5 Na1 60.42(5) . . O1 Nb5 Nb1 132.92(16) . . O1 Nb5 Nb2 136.83(16) . . O1 Nb5 Nb3 135.02(16) . . O1 Nb5 Nb4 131.08(16) . . O1 Nb5 Na1 87.22(17) . . O1 Nb5 O5 103.8(2) . . O1 Nb5 O7 101.5(2) . . O1 Nb5 O8 99.5(2) . . O1 Nb5 O9 105.3(2) . . O1 Nb5 O13 176.38(19) . . O5 Nb5 Nb1 123.23(13) . . O5 Nb5 Nb2 82.30(13) . . O5 Nb5 Nb3 31.33(12) . . O5 Nb5 Nb4 80.51(12) . . O5 Nb5 Na1 134.30(13) . . O5 Nb5 O7 154.66(18) . . O5 Nb5 O8 88.03(18) . . O5 Nb5 O9 89.15(18) . . O5 Nb5 O13 77.70(16) . . O7 Nb5 Nb1 31.47(12) . . O7 Nb5 Nb2 80.95(12) . . O7 Nb5 Nb3 123.34(12) . . O7 Nb5 Nb4 81.23(12) . . O7 Nb5 Na1 44.66(13) . . O7 Nb5 O13 76.97(16) . . O8 Nb5 Nb1 80.88(12) . . O8 Nb5 Nb2 123.54(12) . . O8 Nb5 Nb3 81.66(13) . . O8 Nb5 Nb4 31.56(12) . . O8 Nb5 Na1 46.27(13) . . O8 Nb5 O7 85.54(17) . . O8 Nb5 O13 77.15(16) . . O9 Nb5 Nb1 79.92(12) . . O9 Nb5 Nb2 31.52(12) . . O9 Nb5 Nb3 83.05(13) . . O9 Nb5 Nb4 123.57(12) . . O9 Nb5 Na1 131.09(13) . . O9 Nb5 O7 86.44(17) . . O9 Nb5 O8 154.95(18) . . O9 Nb5 O13 77.93(16) . . O13 Nb5 Nb1 45.53(10) . . O13 Nb5 Nb2 46.42(10) . . O13 Nb5 Nb3 46.38(10) . . O13 Nb5 Nb4 45.64(10) . . O13 Nb5 Na1 89.41(11) . . Nb1 Ni1 Nb1 180.000(17) 2_656 . Nb1 Ni1 Nb3 80.693(14) . 2_656 Nb1 Ni1 Nb3 99.307(14) . . Nb1 Ni1 Nb3 99.308(14) 2_656 2_656 Nb1 Ni1 Nb3 80.692(14) 2_656 . Nb1 Ni1 Nb4 66.556(14) 2_656 2_656 Nb1 Ni1 Nb4 113.444(15) . 2_656 Nb1 Ni1 Nb4 113.443(14) 2_656 . Nb1 Ni1 Nb4 66.557(14) . . Nb3 Ni1 Nb3 180.0 . 2_656 Nb4 Ni1 Nb3 115.609(15) 2_656 . Nb4 Ni1 Nb3 115.609(15) . 2_656 Nb4 Ni1 Nb3 64.392(15) 2_656 2_656 Nb4 Ni1 Nb3 64.391(15) . . Nb4 Ni1 Nb4 180.0 2_656 . O13 Ni1 Nb1 130.28(11) 2_656 . O13 Ni1 Nb1 130.28(11) . 2_656 O13 Ni1 Nb1 49.72(11) 2_656 2_656 O13 Ni1 Nb1 49.72(11) . . O13 Ni1 Nb3 49.59(11) . . O13 Ni1 Nb3 130.41(11) 2_656 . O13 Ni1 Nb3 130.41(11) . 2_656 O13 Ni1 Nb3 49.59(11) 2_656 2_656 O13 Ni1 Nb4 49.85(11) 2_656 2_656 O13 Ni1 Nb4 49.85(11) . . O13 Ni1 Nb4 130.15(11) 2_656 . O13 Ni1 Nb4 130.15(11) . 2_656 O13 Ni1 O13 180.0 . 2_656 O13 Ni1 O15 89.95(16) 2_656 2_656 O13 Ni1 O15 89.95(16) . . O13 Ni1 O15 90.05(16) . 2_656 O13 Ni1 O15 90.05(16) 2_656 . O13 Ni1 O16 90.33(16) . 2_656 O13 Ni1 O16 89.67(16) 2_656 2_656 O13 Ni1 O16 90.33(16) 2_656 . O13 Ni1 O16 89.67(16) . . O15 Ni1 Nb1 87.98(11) . 2_656 O15 Ni1 Nb1 92.02(11) 2_656 2_656 O15 Ni1 Nb1 92.02(11) . . O15 Ni1 Nb1 87.98(11) 2_656 . O15 Ni1 Nb3 92.43(11) . 2_656 O15 Ni1 Nb3 87.57(11) . . O15 Ni1 Nb3 87.57(11) 2_656 2_656 O15 Ni1 Nb3 92.43(11) 2_656 . O15 Ni1 Nb4 40.41(11) 2_656 . O15 Ni1 Nb4 139.59(11) . . O15 Ni1 Nb4 40.41(11) . 2_656 O15 Ni1 Nb4 139.59(11) 2_656 2_656 O15 Ni1 O15 180.0(2) 2_656 . O15 Ni1 O16 82.88(16) 2_656 2_656 O15 Ni1 O16 97.12(16) 2_656 . O15 Ni1 O16 97.12(16) . 2_656 O15 Ni1 O16 82.88(16) . . O16 Ni1 Nb1 40.82(11) 2_656 . O16 Ni1 Nb1 139.19(11) 2_656 2_656 O16 Ni1 Nb1 40.82(11) . 2_656 O16 Ni1 Nb1 139.18(11) . . O16 Ni1 Nb3 139.76(11) . 2_656 O16 Ni1 Nb3 40.24(11) 2_656 2_656 O16 Ni1 Nb3 139.76(11) 2_656 . O16 Ni1 Nb3 40.24(11) . . O16 Ni1 Nb4 91.75(11) 2_656 2_656 O16 Ni1 Nb4 91.74(11) . . O16 Ni1 Nb4 88.25(11) 2_656 . O16 Ni1 Nb4 88.25(11) . 2_656 O16 Ni1 O16 180.0 2_656 . Nb1 Ni2 Nb2 120.75(3) 2_656 . Nb1 Ni2 Nb3 83.30(2) 2_656 . Nb3 Ni2 Nb2 67.89(2) . . Nb4 Ni2 Nb1 68.37(2) 2_656 2_656 Nb4 Ni2 Nb2 83.39(3) 2_656 . Nb4 Ni2 Nb3 120.79(3) 2_656 . O11 Ni2 Nb1 41.10(12) 2_656 2_656 O11 Ni2 Nb2 123.65(12) 2_656 . O11 Ni2 Nb3 123.18(12) 2_656 . O11 Ni2 Nb4 41.60(12) 2_656 2_656 O11 Ni2 O14 155.41(18) 2_656 . O11 Ni2 O15 81.01(16) 2_656 . O11 Ni2 O16 81.02(16) 2_656 . O11 Ni2 N1 98.8(2) 2_656 . O11 Ni2 N2 99.3(2) 2_656 . O14 Ni2 Nb1 122.61(12) . 2_656 O14 Ni2 Nb2 40.50(12) . . O14 Ni2 Nb3 40.77(12) . . O14 Ni2 Nb4 122.49(12) . 2_656 O14 Ni2 O15 80.45(16) . . O14 Ni2 O16 80.32(16) . . O14 Ni2 N1 99.3(2) . . O14 Ni2 N2 99.0(2) . . O15 Ni2 Nb1 89.14(11) . 2_656 O15 Ni2 Nb2 42.65(11) . . O15 Ni2 Nb3 89.31(11) . . O15 Ni2 Nb4 42.05(11) . 2_656 O15 Ni2 O16 81.24(16) . . O16 Ni2 Nb1 42.29(11) . 2_656 O16 Ni2 Nb2 89.39(12) . . O16 Ni2 Nb3 42.17(11) . . O16 Ni2 Nb4 89.76(11) . 2_656 N1 Ni2 Nb1 138.02(17) . 2_656 N1 Ni2 Nb2 89.28(17) . . N1 Ni2 Nb3 137.97(17) . . N1 Ni2 Nb4 89.03(17) . 2_656 N1 Ni2 O15 97.1(2) . . N1 Ni2 O16 178.3(2) . . N1 Ni2 N2 83.7(2) . . N2 Ni2 Nb1 90.60(17) . 2_656 N2 Ni2 Nb2 137.05(18) . . N2 Ni2 Nb3 89.87(17) . . N2 Ni2 Nb4 138.47(18) . 2_656 N2 Ni2 O15 179.2(2) . . N2 Ni2 O16 98.0(2) . . Nb1 Na1 Nb4 60.35(5) . . Nb1 Na1 Nb5 58.10(5) . . Nb1 Na1 Na2 97.16(8) . . Nb4 Na1 Nb5 57.50(5) . . Nb4 Na1 Na2 151.20(10) . . Nb5 Na1 Na2 96.16(8) . . O7 Na1 Nb1 34.62(10) . . O7 Na1 Nb4 73.14(12) . . O7 Na1 Nb5 34.23(10) . . O7 Na1 Na2 78.28(13) . . O7 Na1 O8 65.02(15) . . O8 Na1 Nb1 73.54(12) . . O8 Na1 Nb4 33.81(10) . . O8 Na1 Nb5 34.46(10) . . O8 Na1 Na2 127.28(15) . . O11 Na1 Nb1 36.56(10) . . O11 Na1 Nb4 35.72(10) . . O11 Na1 Nb5 72.84(12) . . O11 Na1 Na2 131.55(15) . . O11 Na1 O7 66.43(15) . . O11 Na1 O8 65.46(15) . . O7W Na1 Nb1 123.72(16) . . O7W Na1 Nb4 132.78(17) . . O7W Na1 Nb5 84.18(15) . . O7W Na1 Na2 43.13(14) . . O7W Na1 O7 90.79(19) . . O7W Na1 O8 99.06(19) . . O7W Na1 O11 156.0(2) . . O7W Na1 O9W 85.5(2) . . O9W Na1 Nb1 77.39(14) . . O9W Na1 Nb4 133.63(16) . . O9W Na1 Nb5 115.86(15) . . O9W Na1 Na2 43.45(14) . . O9W Na1 O7 83.05(18) . . O9W Na1 O8 147.7(2) . . O9W Na1 O11 98.32(19) . . O12W Na1 Nb1 132.3(2) . . O12W Na1 Nb4 102.96(19) . . O12W Na1 Nb5 152.9(2) . . O12W Na1 Na2 105.7(2) . . O12W Na1 O7 166.6(2) . . O12W Na1 O8 118.9(2) . . O12W Na1 O11 102.7(2) . . O12W Na1 O7W 100.8(2) . . O12W Na1 O9W 91.2(2) . . Na1 Na2 Na3 123.56(9) . . Na2 Na2 Na1 156.64(15) 2_745 . Na2 Na2 Na3 68.51(10) 2_745 . O5W Na2 Na1 81.54(15) 2_745 . O5W Na2 Na2 79.36(16) 2_745 2_745 O5W Na2 Na3 143.13(16) 2_745 . O5W Na2 O6W 174.9(2) 2_745 . O5W Na2 O7W 85.3(2) 2_745 . O5W Na2 O8W 81.47(19) 2_745 2_745 O5W Na2 O9W 93.1(2) 2_745 . O6W Na2 Na1 99.25(16) . . O6W Na2 Na2 98.63(18) . 2_745 O6W Na2 Na3 32.96(14) . . O6W Na2 O8W 93.9(2) . 2_745 O6W Na2 O9W 90.9(2) . . O7W Na2 Na1 41.30(14) . . O7W Na2 Na2 123.20(19) . 2_745 O7W Na2 Na3 97.20(15) . . O7W Na2 O6W 92.0(2) . . O7W Na2 O8W 82.63(19) . 2_745 O7W Na2 O9W 83.62(19) . . O8W Na2 Na1 122.30(16) 2_745 . O8W Na2 Na1 142.99(18) . . O8W Na2 Na2 41.28(13) 2_745 2_745 O8W Na2 Na2 47.00(15) . 2_745 O8W Na2 Na3 87.46(16) . . O8W Na2 Na3 62.57(14) 2_745 . O8W Na2 O5W 83.4(2) . 2_745 O8W Na2 O6W 98.7(2) . . O8W Na2 O7W 166.4(2) . . O8W Na2 O8W 88.3(2) . 2_745 O8W Na2 O9W 104.5(2) . . O9W Na2 Na1 43.36(14) . . O9W Na2 Na2 150.85(19) . 2_745 O9W Na2 Na3 123.73(16) . . O9W Na2 O8W 165.6(2) . 2_745 Na4 Na3 Na2 131.47(11) . . O1W Na3 Na2 120.62(16) . . O1W Na3 Na4 42.94(14) . . O1W Na3 O6W 93.6(2) . . O2W Na3 Na2 114.99(16) . . O2W Na3 Na4 43.82(14) . . O2W Na3 O1W 86.71(19) . . O2W Na3 O4W 176.2(2) . . O2W Na3 O5W 82.48(19) . . O2W Na3 O6W 99.8(2) . . O2W Na3 O14W 93.2(3) . . O4W Na3 Na2 68.66(14) . . O4W Na3 Na4 133.17(17) . . O4W Na3 O1W 90.43(19) . . O4W Na3 O6W 82.9(2) . . O4W Na3 O14W 84.3(3) . . O5W Na3 Na2 65.31(15) . . O5W Na3 Na4 126.23(17) . . O5W Na3 O1W 169.2(2) . . O5W Na3 O4W 100.3(2) . . O5W Na3 O6W 88.9(2) . . O5W Na3 O14W 90.3(3) . . O6W Na3 Na2 31.71(14) . . O6W Na3 Na4 100.79(17) . . O14W Na3 Na2 138.2(3) . . O14W Na3 Na4 90.3(3) . . O14W Na3 O1W 89.6(3) . . O14W Na3 O6W 166.8(3) . . O1W Na4 Na3 43.92(14) . . O1W Na4 O2W 87.2(2) . . O1W Na4 O3W 93.0(2) . . O1W Na4 O10W 145.7(3) . . O2W Na4 Na3 43.36(14) . . O2W Na4 O3W 177.5(3) . . O3W Na4 Na3 136.97(18) . . O10W Na4 Na3 118.25(19) . . O10W Na4 O2W 83.5(2) . . O10W Na4 O3W 97.7(2) . . O13W Na4 Na3 99.1(2) . . O13W Na4 O1W 91.9(3) . . O13W Na4 O2W 99.0(3) . . O13W Na4 O3W 78.5(3) . . O13W Na4 O10W 122.2(3) . . Nb3 O5 Nb5 116.7(2) . . Nb1 O7 Nb5 115.8(2) . . Nb1 O7 Na1 98.01(18) . . Nb5 O7 Na1 101.10(18) . . Nb4 O8 Nb5 115.7(2) . . Nb4 O8 Na1 98.89(18) . . Nb5 O8 Na1 99.27(18) . . Nb2 O9 Nb5 115.7(2) . . Nb3 O10 Nb4 117.3(2) . . Nb1 O11 Nb4 115.0(2) . . Nb1 O11 Na1 97.23(17) . . Nb4 O11 Na1 99.63(17) . . Ni2 O11 Nb1 97.84(18) 2_656 . Ni2 O11 Nb4 97.18(18) 2_656 . Ni2 O11 Na1 150.1(2) 2_656 . Nb1 O12 Nb2 116.1(2) . . Nb1 O13 Nb2 88.41(13) . . Nb1 O13 Nb3 178.62(19) . . Nb1 O13 Nb4 91.87(14) . . Nb2 O13 Nb3 91.10(14) . . Nb4 O13 Nb2 178.4(2) . . Nb4 O13 Nb3 88.59(13) . . Nb5 O13 Nb1 89.92(14) . . Nb5 O13 Nb2 88.65(13) . . Nb5 O13 Nb3 88.79(13) . . Nb5 O13 Nb4 89.82(14) . . Ni1 O13 Nb1 90.32(15) . . Ni1 O13 Nb2 91.34(15) . . Ni1 O13 Nb3 90.98(15) . . Ni1 O13 Nb4 90.19(15) . . Ni1 O13 Nb5 179.8(2) . . Nb2 O14 Ni2 98.80(18) . . Nb3 O14 Nb2 116.0(2) . . Nb3 O14 Ni2 98.24(18) . . Nb2 O15 Ni2 93.84(16) . . Nb4 O15 Nb2 160.3(2) 2_656 . Nb4 O15 Ni1 98.25(17) 2_656 . Nb4 O15 Ni2 93.87(17) 2_656 . Ni1 O15 Nb2 98.58(17) . . Ni1 O15 Ni2 98.25(16) . . Nb1 O16 Nb3 161.2(2) 2_656 . Nb1 O16 Ni1 97.34(16) 2_656 . Nb1 O16 Ni2 93.58(17) 2_656 . Nb3 O16 Ni1 98.65(17) . . Nb3 O16 Ni2 93.97(16) . . Ni1 O16 Ni2 97.63(17) . . Ni2 N1 H1A 110.2 . . Ni2 N1 H1B 110.2 . . H1A N1 H1B 108.5 . . C1 N1 Ni2 107.5(4) . . C1 N1 H1A 110.2 . . C1 N1 H1B 110.2 . . Ni2 N2 H2A 110.0 . . Ni2 N2 H2B 110.0 . . H2A N2 H2B 108.4 . . C2 N2 Ni2 108.3(5) . . C2 N2 H2A 110.0 . . C2 N2 H2B 110.0 . . N1 C1 H1C 109.9 . . N1 C1 H1D 109.9 . . N1 C1 C2 109.0(6) . . H1C C1 H1D 108.3 . . C2 C1 H1C 109.9 . . C2 C1 H1D 109.9 . . N2 C2 C1 109.4(7) . . N2 C2 H2C 109.8 . . N2 C2 H2D 109.8 . . C1 C2 H2C 109.8 . . C1 C2 H2D 109.8 . . H2C C2 H2D 108.2 . . Na4 O1W Na3 93.1(2) . . Na3 O2W Na4 92.8(2) . . Na2 O5W Na3 132.6(2) 2_745 . Na2 O6W Na3 115.3(2) . . Na1 O7W Na2 95.6(2) . . Na2 O8W Na2 91.7(2) . 2_745 Na1 O9W Na2 93.2(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Nb1 Nb2 3.3467(8) . Nb1 Nb5 3.3489(8) . Nb1 Ni1 3.1324(6) . Nb1 Ni2 3.0619(10) 2_656 Nb1 Na1 3.384(3) . Nb1 O3 1.773(5) . Nb1 O7 1.941(4) . Nb1 O11 2.032(4) . Nb1 O12 1.972(4) . Nb1 O13 2.390(4) . Nb1 O16 2.064(4) 2_656 Nb2 Nb5 3.3261(8) . Nb2 Ni1 3.1755(6) . Nb2 Ni2 3.0892(10) . Nb2 O2 1.773(5) . Nb2 O9 1.929(4) . Nb2 O12 1.973(4) . Nb2 O13 2.410(4) . Nb2 O14 2.030(4) . Nb2 O15 2.098(4) . Nb3 Nb4 3.3573(8) . Nb3 Nb5 3.3317(8) . Nb3 Ni1 3.1677(6) . Nb3 Ni2 3.0757(10) . Nb3 O5 1.939(4) . Nb3 O6 1.770(5) . Nb3 O10 1.964(4) . Nb3 O13 2.412(4) . Nb3 O14 2.029(4) . Nb3 O16 2.070(4) . Nb4 Nb5 3.3501(8) . Nb4 Ni1 3.1332(6) . Nb4 Ni2 3.0571(10) 2_656 Nb4 Na1 3.455(3) . Nb4 O4 1.773(5) . Nb4 O8 1.945(4) . Nb4 O10 1.968(4) . Nb4 O11 2.046(4) . Nb4 O13 2.395(4) . Nb4 O15 2.052(4) 2_656 Nb5 Na1 3.510(3) . Nb5 O1 1.766(5) . Nb5 O5 1.976(4) . Nb5 O7 2.012(4) . Nb5 O8 2.012(4) . Nb5 O9 2.000(4) . Nb5 O13 2.350(4) . Ni1 Nb1 3.1324(6) 2_656 Ni1 Nb3 3.1677(6) 2_656 Ni1 Nb4 3.1332(6) 2_656 Ni1 O13 2.012(4) . Ni1 O13 2.012(4) 2_656 Ni1 O15 2.092(4) . Ni1 O15 2.091(4) 2_656 Ni1 O16 2.107(4) . Ni1 O16 2.107(4) 2_656 Ni2 Nb1 3.0619(10) 2_656 Ni2 Nb4 3.0571(10) 2_656 Ni2 O11 2.031(4) 2_656 Ni2 O14 2.039(4) . Ni2 O15 2.132(4) . Ni2 O16 2.136(4) . Ni2 N1 2.061(6) . Ni2 N2 2.078(6) . Na1 Na2 3.563(4) . Na1 O7 2.514(5) . Na1 O8 2.570(5) . Na1 O11 2.462(5) . Na1 O7W 2.363(6) . Na1 O9W 2.450(6) . Na1 O12W 2.294(7) . Na2 Na2 3.530(6) 2_745 Na2 Na3 4.214(4) . Na2 O5W 2.395(6) 2_745 Na2 O6W 2.450(6) . Na2 O7W 2.448(6) . Na2 O8W 2.330(6) . Na2 O8W 2.583(6) 2_745 Na2 O9W 2.454(6) . Na3 Na4 3.494(5) . Na3 O1W 2.428(6) . Na3 O2W 2.402(6) . Na3 O4W 2.413(6) . Na3 O5W 2.406(6) . Na3 O6W 2.537(6) . Na3 O14W 2.414(11) . Na4 O1W 2.384(6) . Na4 O2W 2.422(6) . Na4 O3W 2.461(6) . Na4 O10W 2.410(7) . Na4 O13W 2.341(9) . O11 Ni2 2.030(4) 2_656 O15 Nb4 2.052(4) 2_656 O16 Nb1 2.064(4) 2_656 N1 H1A 0.8900 . N1 H1B 0.8900 . N1 C1 1.474(9) . N2 H2A 0.8900 . N2 H2B 0.8900 . N2 C2 1.465(9) . C1 H1C 0.9700 . C1 H1D 0.9700 . C1 C2 1.501(10) . C2 H2C 0.9700 . C2 H2D 0.9700 . O5W Na2 2.395(6) 2_745 O8W Na2 2.583(6) 2_745