#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2100159.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2100159 loop_ _publ_author_name 'Schmid, Siegbert' 'Wagner, Trixie' _publ_section_title ; Structure of KNbOB~2~O~5~ -- a commensurately modulated structure ; _journal_coeditor_code CK5006 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 361 _journal_page_last 366 _journal_volume 61 _journal_year 2005 _chemical_formula_moiety 'B8 K4 Nb4 O24' _chemical_formula_sum 'B32 K16 Nb16 O96' _chemical_formula_weight 3994.08 _chemical_name_systematic ; ? ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b n 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.3056(11) _cell_length_b 31.1632(18) _cell_length_c 9.1659(15) _cell_measurement_reflns_used 928 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.47 _cell_measurement_theta_min 1.31 _cell_volume 2086.8(5) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'three-circle goniometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 12617 _diffrn_reflns_theta_full 26.47 _diffrn_reflns_theta_max 26.47 _diffrn_reflns_theta_min 1.31 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 3.058 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 3.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1888 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.404 _refine_diff_density_min -0.568 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_extinction_coef 0.00051(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 4272 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.970 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0237 _refine_ls_shift/su_max 0.189 _refine_ls_shift/su_mean 0.015 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.0651 _reflns_number_gt 3768 _reflns_number_total 4272 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ck5006.cif _[local]_cod_data_source_block c:_shelx_knbobo_knb-t00 _[local]_cod_cif_authors_sg_H-M Pbn2~1~ _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2100159 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y, z+1/2' '-x, y+1/2, z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_type_symbol K-1 0.00601(11) 0.06419(4) 0.06652(12) 0.0273(3) Uani d 1 K K-2 0.00937(12) 0.18992(4) 0.06582(12) 0.0286(3) Uani d 1 K K-3 0.00190(12) 0.31374(4) 0.05438(12) 0.0277(3) Uani d 1 K K-4 -0.00881(11) 0.43877(4) 0.05738(12) 0.0252(2) Uani d 1 K Nb-1 0.03785(4) 0.099635(8) 0.66158(4) 0.00733(9) Uani d 1 Nb Nb-2 -0.01804(3) 0.225821(9) 0.66236(4) 0.00782(9) Uani d 1 Nb Nb-3 -0.01097(3) 0.350713(9) 0.66542(4) 0.00744(9) Uani d 1 Nb Nb-4 0.01162(3) 0.474595(9) 0.66392(4) 0.00744(9) Uani d 1 Nb B-1 0.3809(5) 0.12755(12) 0.8633(4) 0.0137(8) Uani d 1 B B-2 0.3057(5) 0.24716(13) 0.8885(5) 0.0140(8) Uani d 1 B B-3 0.3340(5) 0.36772(12) 0.8646(4) 0.0130(8) Uani d 1 B B-4 0.3417(5) 0.50490(13) 0.8734(4) 0.0141(9) Uani d 1 B B-5 0.2889(5) 0.61869(13) 0.8870(5) 0.0145(8) Uani d 1 B B-6 0.3612(5) 0.74498(13) 0.8616(4) 0.0140(9) Uani d 1 B B-7 0.3306(5) 0.87847(13) 0.8841(5) 0.0136(8) Uani d 1 B B-8 0.3268(5) 0.99105(12) 0.8767(5) 0.0140(9) Uani d 1 B O1-1 0.2063(3) 0.11303(9) 0.4914(3) 0.0150(6) Uani d 1 O O1-2 0.1874(4) 0.24127(9) 0.5296(3) 0.0180(7) Uani d 1 O O1-3 0.1425(3) 0.34980(8) 0.4868(3) 0.0163(6) Uani d 1 O O1-4 0.1986(4) 0.49345(10) 0.5115(3) 0.0154(6) Uani d 1 O O1-5 0.1597(5) 0.60295(10) 0.5163(3) 0.0200(8) Uani d 1 O O1-6 0.1760(3) 0.73273(9) 0.4844(3) 0.0191(6) Uani d 1 O O1-7 0.2137(3) 0.86917(9) 0.5288(3) 0.0136(6) Uani d 1 O O1-8 0.1571(4) 0.97204(9) 0.4976(3) 0.0159(7) Uani d 1 O O2-1 0.2416(4) 0.11112(10) 0.7887(3) 0.0265(7) Uani d 1 O O2-2 0.1416(4) 0.23778(9) 0.8274(3) 0.0196(7) Uani d 1 O O2-3 0.2081(3) 0.34490(8) 0.7879(3) 0.0146(6) Uani d 1 O O2-4 0.1841(4) 0.49283(9) 0.8121(3) 0.0199(7) Uani d 1 O O2-5 0.1347(4) 0.60389(10) 0.8224(3) 0.0192(7) Uani d 1 O O2-6 0.2348(3) 0.72312(8) 0.7864(3) 0.0168(6) Uani d 1 O O2-7 0.1661(4) 0.86849(8) 0.8275(3) 0.0145(6) Uani d 1 O O2-8 0.1913(4) 0.97104(8) 0.8025(3) 0.0144(7) Uani d 1 O O3-1 0.0652(3) 0.04323(6) 0.6590(5) 0.0222(5) Uani d 1 O O3-2 0.0119(3) 0.16999(8) 0.6553(5) 0.0311(7) Uani d 1 O O3-3 -0.0693(3) 0.29562(6) 0.6704(4) 0.0188(5) Uani d 1 O O3-4 0.0709(3) 0.41939(6) 0.6655(4) 0.0153(4) Uani d 1 O O4-1 0.5534(3) 0.11972(9) 0.8035(3) 0.0191(6) Uani d 1 O O4-2 0.4612(3) 0.24331(10) 0.8032(3) 0.0191(6) Uani d 1 O O4-3 0.5117(3) 0.36810(10) 0.8053(3) 0.0193(6) Uani d 1 O O4-4 0.5045(3) 0.49294(10) 0.8057(3) 0.0198(7) Uani d 1 O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 K-1 0.0285(5) 0.0271(5) 0.0264(6) 0.0059(4) -0.0041(4) 0.0049(5) K-2 0.0312(5) 0.0287(6) 0.0259(6) -0.0071(4) 0.0003(4) 0.0069(5) K-3 0.0266(5) 0.0299(6) 0.0265(7) 0.0007(3) 0.0005(4) 0.0063(5) K-4 0.0228(5) 0.0267(5) 0.0259(6) 0.0031(3) -0.0016(4) 0.0037(4) Nb-1 0.00728(14) 0.00781(15) 0.00691(17) 0.00022(9) -0.0005(4) -0.00004(17) Nb-2 0.00839(13) 0.00783(16) 0.00724(17) 0.00034(8) -0.0001(2) 0.00023(17) Nb-3 0.00790(13) 0.00731(15) 0.00712(19) 0.00016(8) 0.0007(3) 0.00016(16) Nb-4 0.00756(13) 0.00765(16) 0.00710(17) -0.00011(8) 0.0006(3) 0.00010(17) B-1 0.011(2) 0.013(2) 0.017(2) 0.0020(15) -0.0005(15) 0.0036(16) B-2 0.010(2) 0.019(2) 0.012(2) 0.0011(16) -0.0046(15) 0.0019(17) B-3 0.0081(18) 0.017(2) 0.014(2) -0.0002(14) -0.0003(14) 0.0025(16) B-4 0.015(2) 0.016(2) 0.011(2) 0.0017(15) 0.0019(15) 0.0013(16) B-5 0.0094(19) 0.014(2) 0.020(2) 0.0011(15) -0.0027(17) -0.0026(18) B-6 0.011(2) 0.020(2) 0.011(2) 0.0039(15) -0.0012(14) 0.0002(16) B-7 0.013(2) 0.012(2) 0.016(2) 0.0038(15) -0.0001(16) 0.0019(17) B-8 0.0103(19) 0.013(2) 0.019(2) -0.0001(14) -0.0027(16) 0.0001(17) O1-1 0.0081(14) 0.0252(15) 0.0118(14) 0.0010(10) 0.0006(10) 0.0047(11) O1-2 0.0130(14) 0.0296(18) 0.0113(15) 0.0009(11) 0.0013(11) 0.0018(12) O1-3 0.0135(14) 0.0237(15) 0.0116(14) 0.0059(11) 0.0031(11) 0.0029(11) O1-4 0.0114(15) 0.0208(17) 0.0140(15) -0.0025(13) -0.0017(12) 0.0029(12) O1-5 0.0105(15) 0.038(2) 0.0114(14) 0.0073(12) 0.0034(12) 0.0099(13) O1-6 0.0152(14) 0.0290(16) 0.0132(14) 0.0098(11) 0.0025(11) 0.0031(12) O1-7 0.0085(13) 0.0195(15) 0.0127(13) 0.0004(10) -0.0016(11) 0.0022(11) O1-8 0.0120(15) 0.0201(16) 0.0156(14) 0.0034(11) 0.0033(11) 0.0060(12) O2-1 0.0167(16) 0.0433(18) 0.0194(15) -0.0046(13) -0.0061(13) -0.0073(14) O2-2 0.0135(15) 0.0312(16) 0.0140(14) -0.0036(11) -0.0007(12) 0.0014(12) O2-3 0.0129(13) 0.0133(13) 0.0177(14) 0.0003(10) -0.0017(10) -0.0024(11) O2-4 0.0153(16) 0.0256(19) 0.0186(16) -0.0009(13) -0.0073(13) -0.0068(13) O2-5 0.0161(17) 0.0301(18) 0.0116(15) -0.0070(12) -0.0047(12) 0.0022(12) O2-6 0.0108(13) 0.0227(14) 0.0169(14) 0.0044(11) -0.0036(11) -0.0011(12) O2-7 0.0113(13) 0.0204(15) 0.0117(13) 0.0002(10) -0.0024(11) -0.0035(11) O2-8 0.0129(15) 0.0160(15) 0.0142(14) -0.0006(10) -0.0029(11) 0.0021(11) O3-1 0.0257(12) 0.0123(11) 0.0285(14) -0.0009(8) 0.000(2) -0.0005(18) O3-2 0.0474(16) 0.0106(13) 0.0353(19) 0.0048(9) 0.008(2) -0.0005(18) O3-3 0.0214(11) 0.0107(10) 0.0243(14) 0.0001(8) 0.0004(19) -0.0017(17) O3-4 0.0156(11) 0.0095(10) 0.0207(12) 0.0012(8) 0.0021(18) 0.0014(17) O4-1 0.0116(12) 0.0354(17) 0.0105(14) 0.0012(11) -0.0012(11) -0.0082(12) O4-2 0.0149(13) 0.0331(18) 0.0095(15) 0.0004(11) -0.0007(10) -0.0031(12) O4-3 0.0160(13) 0.0324(18) 0.0095(15) -0.0023(10) 0.0025(10) -0.0073(12) O4-4 0.0165(14) 0.0301(18) 0.0128(16) 0.0036(10) -0.0006(10) -0.0075(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 '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' B B 0.0013 0.0007 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O2-5 K-1 O4-4 4_544 2_554 154.54(9) O2-5 K-1 O1-4 4_544 2_554 114.91(10) O4-4 K-1 O1-4 2_554 2_554 76.16(8) O2-5 K-1 O1-8 4_544 3_464 70.44(9) O4-4 K-1 O1-8 2_554 3_464 84.17(8) O1-4 K-1 O1-8 2_554 3_464 112.75(9) O2-5 K-1 O1-7 4_544 3_464 47.92(7) O4-4 K-1 O1-7 2_554 3_464 120.44(8) O1-4 K-1 O1-7 2_554 3_464 162.63(9) O1-8 K-1 O1-7 3_464 3_464 67.23(8) O2-5 K-1 O4-3 4_544 2_554 104.89(9) O4-4 K-1 O4-3 2_554 2_554 82.98(8) O1-4 K-1 O4-3 2_554 2_554 126.58(8) O1-8 K-1 O4-3 3_464 2_554 113.27(8) O1-7 K-1 O4-3 3_464 2_554 64.70(7) O2-5 K-1 B-5 4_544 4_544 24.88(9) O4-4 K-1 B-5 2_554 4_544 135.67(9) O1-4 K-1 B-5 2_554 4_544 138.83(10) O1-8 K-1 B-5 3_464 4_544 59.69(9) O1-7 K-1 B-5 3_464 4_544 24.97(9) O4-3 K-1 B-5 2_554 4_544 88.47(9) O2-5 K-1 O3-4 4_544 2_554 120.59(10) O4-4 K-1 O3-4 2_554 2_554 84.77(8) O1-4 K-1 O3-4 2_554 2_554 55.33(7) O1-8 K-1 O3-4 3_464 2_554 165.57(8) O1-7 K-1 O3-4 3_464 2_554 126.75(7) O4-3 K-1 O3-4 2_554 2_554 74.42(7) B-5 K-1 O3-4 4_544 2_554 134.27(9) O2-5 K-1 O2-8 4_544 3_464 114.61(8) O4-4 K-1 O2-8 2_554 3_464 43.29(7) O1-4 K-1 O2-8 2_554 3_464 115.34(8) O1-8 K-1 O2-8 3_464 3_464 53.12(6) O1-7 K-1 O2-8 3_464 3_464 79.18(7) O4-3 K-1 O2-8 2_554 3_464 74.52(7) B-5 K-1 O2-8 4_544 3_464 92.52(9) O3-4 K-1 O2-8 2_554 3_464 121.56(10) O2-5 K-1 O2-1 4_544 1_554 52.27(9) O4-4 K-1 O2-1 2_554 1_554 149.89(8) O1-4 K-1 O2-1 2_554 1_554 75.87(8) O1-8 K-1 O2-1 3_464 1_554 117.07(9) O1-7 K-1 O2-1 3_464 1_554 88.64(8) O4-3 K-1 O2-1 2_554 1_554 105.17(8) B-5 K-1 O2-1 4_544 1_554 74.19(9) O3-4 K-1 O2-1 2_554 1_554 70.22(8) O2-8 K-1 O2-1 3_464 1_554 166.69(8) O2-5 K-1 B-8 4_544 3_464 136.54(10) O4-4 K-1 B-8 2_554 3_464 21.38(8) O1-4 K-1 B-8 2_554 3_464 96.57(9) O1-8 K-1 B-8 3_464 3_464 70.04(9) O1-7 K-1 B-8 3_464 3_464 99.47(9) O4-3 K-1 B-8 2_554 3_464 75.29(9) B-5 K-1 B-8 4_544 3_464 114.73(9) O3-4 K-1 B-8 2_554 3_464 101.63(10) O2-8 K-1 B-8 3_464 3_464 22.25(8) O2-1 K-1 B-8 1_554 3_464 171.06(8) O2-5 K-1 Nb-4 4_544 2_554 132.37(8) O4-4 K-1 Nb-4 2_554 2_554 69.23(5) O1-4 K-1 Nb-4 2_554 2_554 31.43(6) O1-8 K-1 Nb-4 3_464 2_554 138.34(7) O1-7 K-1 Nb-4 3_464 2_554 154.22(6) O4-3 K-1 Nb-4 2_554 2_554 95.17(5) B-5 K-1 Nb-4 4_544 2_554 155.08(8) O3-4 K-1 Nb-4 2_554 2_554 27.50(3) O2-8 K-1 Nb-4 3_464 2_554 112.23(6) O2-1 K-1 Nb-4 1_554 2_554 81.08(5) B-8 K-1 Nb-4 3_464 2_554 89.98(7) O2-2 K-2 O4-3 1_554 2_554 162.30(9) O2-2 K-2 O1-7 1_554 3_464 120.54(9) O4-3 K-2 O1-7 2_554 3_464 69.01(8) O2-2 K-2 O1-3 1_554 2_554 74.52(9) O4-3 K-2 O1-3 2_554 2_554 88.23(8) O1-7 K-2 O1-3 3_464 2_554 110.83(8) O2-2 K-2 O4-2 1_554 2_554 99.78(9) O4-3 K-2 O4-2 2_554 2_554 83.44(8) O1-7 K-2 O4-2 3_464 2_554 125.69(8) O1-3 K-2 O4-2 2_554 2_554 114.15(7) O2-2 K-2 O2-3 1_554 2_554 117.85(8) O4-3 K-2 O2-3 2_554 2_554 46.10(7) O1-7 K-2 O2-3 3_464 2_554 110.86(8) O1-3 K-2 O2-3 2_554 2_554 55.51(6) O4-2 K-2 O2-3 2_554 2_554 73.75(7) O2-2 K-2 O1-2 1_554 2_554 46.04(7) O4-3 K-2 O1-2 2_554 2_554 124.06(8) O1-7 K-2 O1-2 3_464 2_554 166.54(10) O1-3 K-2 O1-2 2_554 2_554 69.17(8) O4-2 K-2 O1-2 2_554 2_554 63.23(7) O2-3 K-2 O1-2 2_554 2_554 80.59(7) O2-2 K-2 B-2 1_554 1_554 24.58(9) O4-3 K-2 B-2 2_554 1_554 140.51(9) O1-7 K-2 B-2 3_464 1_554 143.08(10) O1-3 K-2 B-2 2_554 1_554 61.78(9) O4-2 K-2 B-2 2_554 1_554 86.25(10) O2-3 K-2 B-2 2_554 1_554 94.44(9) O1-2 K-2 B-2 2_554 1_554 24.34(9) O2-2 K-2 O2-6 1_554 4_544 54.21(8) O4-3 K-2 O2-6 2_554 4_544 140.43(7) O1-7 K-2 O2-6 3_464 4_544 72.56(7) O1-3 K-2 O2-6 2_554 4_544 114.37(9) O4-2 K-2 O2-6 2_554 4_544 112.53(8) O2-3 K-2 O2-6 2_554 4_544 169.82(8) O1-2 K-2 O2-6 2_554 4_544 94.97(8) B-2 K-2 O2-6 1_554 4_544 78.38(9) O2-2 K-2 O3-3 1_554 2_454 118.36(9) O4-3 K-2 O3-3 2_554 2_454 79.34(8) O1-7 K-2 O3-3 3_464 2_454 53.25(7) O1-3 K-2 O3-3 2_554 2_454 162.56(7) O4-2 K-2 O3-3 2_554 2_454 76.80(8) O2-3 K-2 O3-3 2_554 2_454 119.60(10) O1-2 K-2 O3-3 2_554 2_454 128.08(7) B-2 K-2 O3-3 1_554 2_454 134.66(9) O2-6 K-2 O3-3 4_544 2_454 70.33(8) O2-2 K-2 B-3 1_554 2_554 140.67(9) O4-3 K-2 B-3 2_554 2_554 23.17(8) O1-7 K-2 B-3 3_464 2_554 90.54(9) O1-3 K-2 B-3 2_554 2_554 71.88(9) O4-2 K-2 B-3 2_554 2_554 76.37(9) O2-3 K-2 B-3 2_554 2_554 22.99(8) O1-2 K-2 B-3 2_554 2_554 101.94(9) B-2 K-2 B-3 1_554 2_554 117.41(9) O2-6 K-2 B-3 4_544 2_554 163.08(8) O3-3 K-2 B-3 2_454 2_554 99.13(10) O2-2 K-2 B-5 1_554 4_544 100.67(10) O4-3 K-2 B-5 2_554 4_544 85.71(9) O1-7 K-2 B-5 3_464 4_544 21.51(8) O1-3 K-2 B-5 2_554 4_544 99.01(9) O4-2 K-2 B-5 2_554 4_544 144.62(8) O2-3 K-2 B-5 2_554 4_544 119.91(9) O1-2 K-2 B-5 2_554 4_544 146.04(9) B-2 K-2 B-5 1_554 4_544 121.83(11) O2-6 K-2 B-5 4_544 4_544 59.95(8) O3-3 K-2 B-5 2_454 4_544 68.12(8) B-3 K-2 B-5 2_554 4_544 104.22(10) O1-2 K-3 O1-6 2_554 3_464 109.89(9) O1-2 K-3 O4-2 2_554 2_554 67.72(8) O1-6 K-3 O4-2 3_464 2_554 86.76(8) O1-2 K-3 O2-7 2_554 4_544 128.39(9) O1-6 K-3 O2-7 3_464 4_544 77.80(8) O4-2 K-3 O2-7 2_554 4_544 160.74(8) O1-2 K-3 O2-3 2_554 1_554 74.51(7) O1-6 K-3 O2-3 3_464 1_554 113.29(9) O4-2 K-3 O2-3 2_554 1_554 141.56(7) O2-7 K-3 O2-3 4_544 1_554 56.94(8) O1-2 K-3 O2-6 2_554 3_464 109.39(8) O1-6 K-3 O2-6 3_464 3_464 56.18(7) O4-2 K-3 O2-6 2_554 3_464 45.12(7) O2-7 K-3 O2-6 4_544 3_464 115.72(7) O2-3 K-3 O2-6 1_554 3_464 169.36(8) O1-2 K-3 O4-1 2_554 2_554 124.21(8) O1-6 K-3 O4-1 3_464 2_554 113.21(8) O4-2 K-3 O4-1 2_554 2_554 81.01(8) O2-7 K-3 O4-1 4_544 2_554 94.45(8) O2-3 K-3 O4-1 1_554 2_554 116.28(8) O2-6 K-3 O4-1 3_464 2_554 70.27(7) O1-2 K-3 O1-1 2_554 2_554 83.30(7) O1-6 K-3 O1-1 3_464 2_554 151.87(9) O4-2 K-3 O1-1 2_554 2_554 121.37(8) O2-7 K-3 O1-1 4_544 2_554 74.70(8) O2-3 K-3 O1-1 1_554 2_554 44.70(7) O2-6 K-3 O1-1 3_464 2_554 144.28(8) O4-1 K-3 O1-1 2_554 2_554 75.04(7) O1-2 K-3 O2-2 2_554 1_554 43.59(7) O1-6 K-3 O2-2 3_464 1_554 75.74(8) O4-2 K-3 O2-2 2_554 1_554 91.56(8) O2-7 K-3 O2-2 4_544 1_554 95.66(9) O2-3 K-3 O2-2 1_554 1_554 64.50(8) O2-6 K-3 O2-2 3_464 1_554 111.06(8) O4-1 K-3 O2-2 2_554 1_554 167.79(8) O1-1 K-3 O2-2 2_554 1_554 101.09(7) O1-2 K-3 B-2 2_554 1_554 22.76(9) O1-6 K-3 B-2 3_464 1_554 97.71(9) O4-2 K-3 B-2 2_554 1_554 85.24(9) O2-7 K-3 B-2 4_544 1_554 107.99(10) O2-3 K-3 B-2 1_554 1_554 60.66(9) O2-6 K-3 B-2 3_464 1_554 119.41(9) O4-1 K-3 B-2 2_554 1_554 145.14(9) O1-1 K-3 B-2 2_554 1_554 85.35(9) O2-2 K-3 B-2 1_554 1_554 23.25(8) O1-2 K-3 B-3 2_554 1_554 72.02(9) O1-6 K-3 B-3 3_464 1_554 136.40(10) O4-2 K-3 B-3 2_554 1_554 129.31(9) O2-7 K-3 B-3 4_544 1_554 69.74(9) O2-3 K-3 B-3 1_554 1_554 23.27(8) O2-6 K-3 B-3 3_464 1_554 166.86(9) O4-1 K-3 B-3 2_554 1_554 97.90(9) O1-1 K-3 B-3 2_554 1_554 23.02(8) O2-2 K-3 B-3 1_554 1_554 79.27(9) B-2 K-3 B-3 1_554 1_554 67.05(10) O1-2 K-3 B-1 2_554 2_554 100.66(9) O1-6 K-3 B-1 3_464 2_554 130.85(9) O4-2 K-3 B-1 2_554 2_554 70.12(9) O2-7 K-3 B-1 4_544 2_554 111.79(9) O2-3 K-3 B-1 1_554 2_554 111.43(9) O2-6 K-3 B-1 3_464 2_554 77.99(9) O4-1 K-3 B-1 2_554 2_554 23.62(8) O1-1 K-3 B-1 2_554 2_554 66.73(8) O2-2 K-3 B-1 1_554 2_554 144.23(9) B-2 K-3 B-1 1_554 2_554 121.66(10) B-3 K-3 B-1 1_554 2_554 88.89(9) O1-5 K-4 O1-1 3_464 2_554 112.89(10) O1-5 K-4 O2-8 3_464 4_544 69.42(9) O1-1 K-4 O2-8 2_554 4_544 113.08(9) O1-5 K-4 O4-1 3_464 2_554 73.42(8) O1-1 K-4 O4-1 2_554 2_554 83.99(8) O2-8 K-4 O4-1 4_544 2_554 142.72(8) O1-5 K-4 O1-4 3_464 3_464 72.09(9) O1-1 K-4 O1-4 2_554 3_464 157.88(10) O2-8 K-4 O1-4 4_544 3_464 46.88(7) O4-1 K-4 O1-4 2_554 3_464 117.59(8) O1-5 K-4 O4-4 3_464 3_464 116.50(8) O1-1 K-4 O4-4 2_554 3_464 121.75(8) O2-8 K-4 O4-4 4_544 3_464 111.68(8) O4-1 K-4 O4-4 2_554 3_464 82.27(8) O1-4 K-4 O4-4 3_464 3_464 69.39(8) O1-5 K-4 O2-4 3_464 1_554 123.07(9) O1-1 K-4 O2-4 2_554 1_554 78.51(8) O2-8 K-4 O2-4 4_544 1_554 55.85(9) O4-1 K-4 O2-4 2_554 1_554 159.67(8) O1-4 K-4 O2-4 3_464 1_554 81.00(9) O4-4 K-4 O2-4 3_464 1_554 98.18(8) O1-5 K-4 O2-7 3_464 4_544 44.54(7) O1-1 K-4 O2-7 2_554 4_544 75.56(8) O2-8 K-4 O2-7 4_544 4_544 62.89(8) O4-1 K-4 O2-7 2_554 4_544 92.33(8) O1-4 K-4 O2-7 3_464 4_544 97.48(8) O4-4 K-4 O2-7 3_464 4_544 160.84(7) O2-4 K-4 O2-7 1_554 4_544 93.22(8) O1-5 K-4 O2-1 3_464 2_554 112.69(9) O1-1 K-4 O2-1 2_554 2_554 52.86(7) O2-8 K-4 O2-1 4_544 2_554 165.86(10) O4-1 K-4 O2-1 2_554 2_554 43.09(7) O1-4 K-4 O2-1 3_464 2_554 147.17(9) O4-4 K-4 O2-1 3_464 2_554 80.38(8) O2-4 K-4 O2-1 1_554 2_554 116.75(7) O2-7 K-4 O2-1 4_544 2_554 108.10(8) O1-5 K-4 B-8 3_464 4_544 63.05(9) O1-1 K-4 B-8 2_554 4_544 137.25(10) O2-8 K-4 B-8 4_544 4_544 24.22(9) O4-1 K-4 B-8 2_554 4_544 128.35(9) O1-4 K-4 B-8 3_464 4_544 24.05(8) O4-4 K-4 B-8 3_464 4_544 92.95(9) O2-4 K-4 B-8 1_554 4_544 71.98(9) O2-7 K-4 B-8 4_544 4_544 75.95(9) O2-1 K-4 B-8 2_554 4_544 169.54(10) O1-5 K-4 B-7 3_464 4_544 22.31(9) O1-1 K-4 B-7 2_554 4_544 97.23(10) O2-8 K-4 B-7 4_544 4_544 59.53(9) O4-1 K-4 B-7 2_554 4_544 86.48(9) O1-4 K-4 B-7 3_464 4_544 80.39(9) O4-4 K-4 B-7 3_464 4_544 137.67(9) O2-4 K-4 B-7 1_554 4_544 105.79(9) O2-7 K-4 B-7 4_544 4_544 23.18(8) O2-1 K-4 B-7 2_554 4_544 116.86(9) B-8 K-4 B-7 4_544 4_544 63.27(10) O1-5 K-4 O3-1 3_464 2_554 160.30(9) O1-1 K-4 O3-1 2_554 2_554 53.55(7) O2-8 K-4 O3-1 4_544 2_554 127.18(10) O4-1 K-4 O3-1 2_554 2_554 89.87(8) O1-4 K-4 O3-1 3_464 2_554 126.26(7) O4-4 K-4 O3-1 3_464 2_554 70.09(7) O2-4 K-4 O3-1 1_554 2_554 71.44(8) O2-7 K-4 O3-1 4_544 2_554 128.51(8) O2-1 K-4 O3-1 2_554 2_554 48.42(7) B-8 K-4 O3-1 4_544 2_554 136.58(9) B-7 K-4 O3-1 4_544 2_554 150.78(9) O3-1 Nb-1 O2-1 . . 96.07(14) O3-1 Nb-1 O2-5 . 4_545 98.69(15) O2-1 Nb-1 O2-5 . 4_545 91.70(14) O3-1 Nb-1 O1-5 . 4_545 97.23(15) O2-1 Nb-1 O1-5 . 4_545 165.51(14) O2-5 Nb-1 O1-5 4_545 4_545 91.95(10) O3-1 Nb-1 O1-1 . . 97.22(15) O2-1 Nb-1 O1-1 . . 87.60(11) O2-5 Nb-1 O1-1 4_545 . 164.06(12) O1-5 Nb-1 O1-1 4_545 . 85.06(12) O3-1 Nb-1 O3-2 . . 177.26(19) O2-1 Nb-1 O3-2 . . 84.09(13) O2-5 Nb-1 O3-2 4_545 . 84.04(13) O1-5 Nb-1 O3-2 4_545 . 82.35(13) O1-1 Nb-1 O3-2 . . 80.05(12) O3-1 Nb-1 K-4 . 2 65.02(8) O2-1 Nb-1 K-4 . 2 60.39(9) O2-5 Nb-1 K-4 4_545 2 143.74(9) O1-5 Nb-1 K-4 4_545 2 121.04(10) O1-1 Nb-1 K-4 . 2 46.90(8) O3-2 Nb-1 K-4 . 2 112.86(7) O3-1 Nb-1 K-1 . 1_556 74.74(14) O2-1 Nb-1 K-1 . 1_556 61.31(10) O2-5 Nb-1 K-1 4_545 1_556 41.85(9) O1-5 Nb-1 K-1 4_545 1_556 128.22(9) O1-1 Nb-1 K-1 . 1_556 146.10(7) O3-2 Nb-1 K-1 . 1_556 107.66(12) K-4 Nb-1 K-1 2 1_556 101.94(2) O3-1 Nb-1 K-4 . 2_455 79.39(8) O2-1 Nb-1 K-4 . 2_455 155.79(10) O2-5 Nb-1 K-4 4_545 2_455 65.86(10) O1-5 Nb-1 K-4 4_545 2_455 34.63(9) O1-1 Nb-1 K-4 . 2_455 116.50(8) O3-2 Nb-1 K-4 . 2_455 101.58(7) K-4 Nb-1 K-4 2 2_455 134.40(3) K-1 Nb-1 K-4 1_556 2_455 94.71(2) O3-2 Nb-2 O2-2 . . 98.27(16) O3-2 Nb-2 O2-6 . 4_545 94.58(13) O2-2 Nb-2 O2-6 . 4_545 92.41(12) O3-2 Nb-2 O1-2 . . 97.07(14) O2-2 Nb-2 O1-2 . . 88.67(12) O2-6 Nb-2 O1-2 4_545 . 168.02(11) O3-2 Nb-2 O1-6 . 4_545 98.50(16) O2-2 Nb-2 O1-6 . 4_545 162.65(12) O2-6 Nb-2 O1-6 4_545 4_545 90.65(11) O1-2 Nb-2 O1-6 . 4_545 84.89(12) O3-2 Nb-2 O3-3 . . 177.39(9) O2-2 Nb-2 O3-3 . . 83.53(12) O2-6 Nb-2 O3-3 4_545 . 83.43(10) O1-2 Nb-2 O3-3 . . 84.84(12) O1-6 Nb-2 O3-3 4_545 . 79.86(12) O3-2 Nb-2 K-2 . 1_556 75.05(15) O2-2 Nb-2 K-2 . 1_556 44.06(9) O2-6 Nb-2 K-2 4_545 1_556 58.17(8) O1-2 Nb-2 K-2 . 1_556 127.95(8) O1-6 Nb-2 K-2 4_545 1_556 146.78(8) O3-3 Nb-2 K-2 . 1_556 105.18(11) O3-2 Nb-2 K-3 . 2_455 77.81(9) O2-2 Nb-2 K-3 . 2_455 143.78(9) O2-6 Nb-2 K-3 4_545 2_455 52.72(8) O1-2 Nb-2 K-3 . 2_455 127.51(8) O1-6 Nb-2 K-3 4_545 2_455 45.77(8) O3-3 Nb-2 K-3 . 2_455 99.62(6) K-2 Nb-2 K-3 1_556 2_455 101.51(2) O3-2 Nb-2 K-3 . 2 64.98(8) O2-2 Nb-2 K-3 . 2 72.13(9) O2-6 Nb-2 K-3 4_545 2 151.22(8) O1-2 Nb-2 K-3 . 2 39.63(8) O1-6 Nb-2 K-3 4_545 2 111.43(8) O3-3 Nb-2 K-3 . 2 117.48(6) K-2 Nb-2 K-3 1_556 2 95.53(2) K-3 Nb-2 K-3 2_455 2 133.16(3) O3-3 Nb-3 O2-7 . 4_545 96.67(14) O3-3 Nb-3 O2-3 . . 95.29(12) O2-7 Nb-3 O2-3 4_545 . 93.69(12) O3-3 Nb-3 O1-3 . . 98.23(14) O2-7 Nb-3 O1-3 4_545 . 164.05(11) O2-3 Nb-3 O1-3 . . 90.58(11) O3-3 Nb-3 O1-7 . 4_545 96.62(13) O2-7 Nb-3 O1-7 4_545 4_545 88.01(11) O2-3 Nb-3 O1-7 . 4_545 167.69(10) O1-3 Nb-3 O1-7 . 4_545 84.66(11) O3-3 Nb-3 O3-4 . . 177.77(15) O2-7 Nb-3 O3-4 4_545 . 83.25(11) O2-3 Nb-3 O3-4 . . 82.49(10) O1-3 Nb-3 O3-4 . . 82.07(12) O1-7 Nb-3 O3-4 4_545 . 85.61(10) O3-3 Nb-3 K-3 . 1_556 71.55(14) O2-7 Nb-3 K-3 4_545 1_556 51.46(8) O2-3 Nb-3 K-3 . 1_556 53.64(8) O1-3 Nb-3 K-3 . 1_556 140.02(8) O1-7 Nb-3 K-3 4_545 1_556 133.99(7) O3-4 Nb-3 K-3 . 1_556 106.80(10) O3-3 Nb-3 K-2 . 2_455 58.29(8) O2-7 Nb-3 K-2 4_545 2_455 74.45(8) O2-3 Nb-3 K-2 . 2_455 148.37(7) O1-3 Nb-3 K-2 . 2_455 108.93(8) O1-7 Nb-3 K-2 4_545 2_455 43.56(8) O3-4 Nb-3 K-2 . 2_455 123.73(6) K-3 Nb-3 K-2 1_556 2_455 98.28(2) O3-3 Nb-3 K-2 . 2 85.36(8) O2-7 Nb-3 K-2 4_545 2 143.14(8) O2-3 Nb-3 K-2 . 2 49.60(8) O1-3 Nb-3 K-2 . 2 44.49(8) O1-7 Nb-3 K-2 4_545 2 128.47(7) O3-4 Nb-3 K-2 . 2 93.36(6) K-3 Nb-3 K-2 1_556 2 95.58(2) K-2 Nb-3 K-2 2_455 2 133.72(3) O3-4 Nb-4 O2-4 . . 96.89(14) O3-4 Nb-4 O2-8 . 4_545 97.17(13) O2-4 Nb-4 O2-8 . 4_545 93.10(13) O3-4 Nb-4 O1-8 . 4_545 96.91(14) O2-4 Nb-4 O1-8 . 4_545 164.79(12) O2-8 Nb-4 O1-8 4_545 4_545 91.51(11) O3-4 Nb-4 O1-4 . . 96.97(14) O2-4 Nb-4 O1-4 . . 87.71(9) O2-8 Nb-4 O1-4 4_545 . 165.63(11) O1-8 Nb-4 O1-4 4_545 . 84.28(12) O3-4 Nb-4 O3-1 . 4 179.09(17) O2-4 Nb-4 O3-1 . 4 84.01(12) O2-8 Nb-4 O3-1 4_545 4 82.87(11) O1-8 Nb-4 O3-1 4_545 4 82.19(12) O1-4 Nb-4 O3-1 . 4 82.95(12) O3-4 Nb-4 K-4 . 1_556 73.46(13) O2-4 Nb-4 K-4 . 1_556 56.17(9) O2-8 Nb-4 K-4 4_545 1_556 48.18(9) O1-8 Nb-4 K-4 4_545 1_556 134.82(8) O1-4 Nb-4 K-4 . 1_556 139.91(8) O3-1 Nb-4 K-4 4 1_556 107.17(11) O3-4 Nb-4 K-1 . 2 58.09(8) O2-4 Nb-4 K-1 . 2 69.99(9) O2-8 Nb-4 K-1 4_545 2 146.19(8) O1-8 Nb-4 K-1 4_545 2 112.58(9) O1-4 Nb-4 K-1 . 2 46.80(8) O3-1 Nb-4 K-1 4 2 122.26(7) K-4 Nb-4 K-1 1_556 2 99.53(2) O3-4 Nb-4 K-1 . 2_455 86.59(7) O2-4 Nb-4 K-1 . 2_455 147.68(9) O2-8 Nb-4 K-1 4_545 2_455 54.63(9) O1-8 Nb-4 K-1 4_545 2_455 39.98(9) O1-4 Nb-4 K-1 . 2_455 123.89(8) O3-1 Nb-4 K-1 4 2_455 92.70(6) K-4 Nb-4 K-1 1_556 2_455 94.87(2) K-1 Nb-4 K-1 2 2_455 135.23(3) O2-1 B-1 O1-3 . 2 122.6(3) O2-1 B-1 O4-1 . . 115.0(3) O1-3 B-1 O4-1 2 . 122.5(3) O2-1 B-1 K-3 . 2 88.4(2) O1-3 B-1 K-3 2 2 116.1(2) O4-1 B-1 K-3 . 2 63.26(18) O1-2 B-2 O2-2 2 . 119.3(4) O1-2 B-2 O4-2 2 . 122.4(3) O2-2 B-2 O4-2 . . 118.3(4) O1-2 B-2 K-2 2 1_556 71.9(2) O2-2 B-2 K-2 . 1_556 59.9(2) O4-2 B-2 K-2 . 1_556 141.6(3) O1-2 B-2 K-3 2 1_556 55.2(2) O2-2 B-2 K-3 . 1_556 74.9(2) O4-2 B-2 K-3 . 1_556 147.3(3) K-2 B-2 K-3 1_556 1_556 71.05(9) O1-1 B-3 O2-3 2 . 122.3(3) O1-1 B-3 O4-3 2 . 122.2(3) O2-3 B-3 O4-3 . . 115.4(3) O1-1 B-3 K-3 2 1_556 67.93(19) O2-3 B-3 K-3 . 1_556 61.74(19) O4-3 B-3 K-3 . 1_556 148.6(2) O1-1 B-3 K-2 2 2 171.3(3) O2-3 B-3 K-2 . 2 62.86(19) O4-3 B-3 K-2 . 2 52.79(17) K-3 B-3 K-2 1_556 2 112.34(11) O2-4 B-4 O1-8 . 2_565 120.8(3) O2-4 B-4 O4-4 . . 118.3(3) O1-8 B-4 O4-4 2_565 . 120.9(3) O2-4 B-4 K-4 . 3_565 93.5(2) O1-8 B-4 K-4 2_565 3_565 115.0(2) O4-4 B-4 K-4 . 3_565 60.47(19) O2-5 B-5 O1-7 . 2_565 120.2(3) O2-5 B-5 O4-1 . 4_655 117.3(3) O1-7 B-5 O4-1 2_565 4_655 122.5(3) O2-5 B-5 K-1 . 4_556 58.9(2) O1-7 B-5 K-1 2_565 4_556 69.2(2) O4-1 B-5 K-1 4_655 4_556 149.1(3) O2-5 B-5 K-2 . 4_556 84.4(2) O1-7 B-5 K-2 2_565 4_556 50.74(18) O4-1 B-5 K-2 4_655 4_556 139.4(3) K-1 B-5 K-2 4_556 4_556 71.21(8) O2-6 B-6 O1-6 . 2_565 123.5(3) O2-6 B-6 O4-2 . 4_655 115.0(3) O1-6 B-6 O4-2 2_565 4_655 121.5(3) O2-6 B-6 K-3 . 3_565 61.57(19) O1-6 B-6 K-3 2_565 3_565 174.5(3) O4-2 B-6 K-3 4_655 3_565 53.46(18) O2-6 B-6 K-2 . 3_565 96.2(2) O1-6 B-6 K-2 2_565 3_565 113.8(2) O4-2 B-6 K-2 4_655 3_565 56.58(19) K-3 B-6 K-2 3_565 3_565 66.22(8) O1-5 B-7 O2-7 2_565 . 119.6(4) O1-5 B-7 O4-3 2_565 4_655 121.5(4) O2-7 B-7 O4-3 . 4_655 118.9(3) O1-5 B-7 K-4 2_565 4_556 51.5(2) O2-7 B-7 K-4 . 4_556 72.0(2) O4-3 B-7 K-4 4_655 4_556 159.8(3) O1-5 B-7 K-3 2_565 4_556 83.3(2) O2-7 B-7 K-3 . 4_556 54.72(19) O4-3 B-7 K-3 4_655 4_556 131.7(3) K-4 B-7 K-3 4_556 4_556 68.47(8) O1-4 B-8 O2-8 2_565 . 121.9(4) O1-4 B-8 O4-4 2_565 4_655 122.5(3) O2-8 B-8 O4-4 . 4_655 115.5(3) O1-4 B-8 K-4 2_565 4_556 67.4(2) O2-8 B-8 K-4 . 4_556 60.50(19) O4-4 B-8 K-4 4_655 4_556 151.7(3) O1-4 B-8 K-1 2_565 3_565 163.5(3) O2-8 B-8 K-1 . 3_565 69.3(2) O4-4 B-8 K-1 4_655 3_565 47.56(18) K-4 B-8 K-1 4_556 3_565 114.92(11) B-3 O1-1 Nb-1 2_554 . 128.7(2) B-3 O1-1 K-4 2_554 2 128.2(2) Nb-1 O1-1 K-4 . 2 101.16(11) B-3 O1-1 K-3 2_554 2 89.1(2) Nb-1 O1-1 K-3 . 2 114.51(11) K-4 O1-1 K-3 2 2 81.10(7) B-2 O1-2 Nb-2 2_554 . 132.9(3) B-2 O1-2 K-3 2_554 2 102.0(2) Nb-2 O1-2 K-3 . 2 113.94(12) B-2 O1-2 K-2 2_554 2 83.7(2) Nb-2 O1-2 K-2 . 2 129.81(12) K-3 O1-2 K-2 2 2 80.72(7) B-1 O1-3 Nb-3 2_554 . 128.0(2) B-1 O1-3 K-2 2_554 2 122.8(2) Nb-3 O1-3 K-2 . 2 107.07(11) B-8 O1-4 Nb-4 2_564 . 130.0(3) B-8 O1-4 K-1 2_564 2 119.7(2) Nb-4 O1-4 K-1 . 2 101.77(11) B-8 O1-4 K-4 2_564 3_565 88.5(2) Nb-4 O1-4 K-4 . 3_565 125.26(12) K-1 O1-4 K-4 2 3_565 83.17(7) B-7 O1-5 Nb-1 2_564 4 132.2(3) B-7 O1-5 K-4 2_564 3_565 106.2(2) Nb-1 O1-5 K-4 4 3_565 121.62(13) B-6 O1-6 Nb-2 2_564 4 128.0(2) B-6 O1-6 K-3 2_564 3_565 128.0(2) Nb-2 O1-6 K-3 4 3_565 103.99(11) B-5 O1-7 Nb-3 2_564 4 131.5(2) B-5 O1-7 K-2 2_564 3_565 107.7(2) Nb-3 O1-7 K-2 4 3_565 107.25(11) B-5 O1-7 K-1 2_564 3_565 85.8(2) Nb-3 O1-7 K-1 4 3_565 130.31(12) K-2 O1-7 K-1 3_565 3_565 83.93(7) B-4 O1-8 Nb-4 2_564 4 129.7(3) B-4 O1-8 K-1 2_564 3_565 113.1(2) Nb-4 O1-8 K-1 4 3_565 113.85(12) B-1 O2-1 Nb-1 . . 167.4(3) B-1 O2-1 K-4 . 2 93.4(2) Nb-1 O2-1 K-4 . 2 88.90(10) B-1 O2-1 K-1 . 1_556 99.6(2) Nb-1 O2-1 K-1 . 1_556 88.97(10) K-4 O2-1 K-1 2 1_556 125.58(10) B-2 O2-2 Nb-2 . . 153.2(3) B-2 O2-2 K-2 . 1_556 95.6(2) Nb-2 O2-2 K-2 . 1_556 107.22(12) B-2 O2-2 K-3 . 1_556 81.9(2) Nb-2 O2-2 K-3 . 1_556 116.12(12) K-2 O2-2 K-3 1_556 1_556 77.60(8) B-3 O2-3 Nb-3 . . 143.1(2) B-3 O2-3 K-3 . 1_556 95.0(2) Nb-3 O2-3 K-3 . 1_556 94.90(9) B-3 O2-3 K-2 . 2 94.2(2) Nb-3 O2-3 K-2 . 2 101.53(11) K-3 O2-3 K-2 1_556 2 138.54(9) B-4 O2-4 Nb-4 . . 159.7(3) B-4 O2-4 K-4 . 1_556 103.7(2) Nb-4 O2-4 K-4 . 1_556 93.01(11) B-5 O2-5 Nb-1 . 4 153.4(3) B-5 O2-5 K-1 . 4_556 96.2(2) Nb-1 O2-5 K-1 4 4_556 110.08(13) B-6 O2-6 Nb-2 . 4 146.9(2) B-6 O2-6 K-3 . 3_565 96.2(2) Nb-2 O2-6 K-3 4 3_565 97.30(11) B-6 O2-6 K-2 . 4_556 97.7(2) Nb-2 O2-6 K-2 4 4_556 91.55(9) K-3 O2-6 K-2 3_565 4_556 139.26(8) B-7 O2-7 Nb-3 . 4 151.5(3) B-7 O2-7 K-3 . 4_556 103.5(2) Nb-3 O2-7 K-3 4 4_556 97.50(10) B-7 O2-7 K-4 . 4_556 84.8(2) Nb-3 O2-7 K-4 4 4_556 118.69(11) K-3 O2-7 K-4 4_556 4_556 77.65(7) B-8 O2-8 Nb-4 . 4 148.7(2) B-8 O2-8 K-4 . 4_556 95.3(2) Nb-4 O2-8 K-4 4 4_556 101.33(12) B-8 O2-8 K-1 . 3_565 88.5(2) Nb-4 O2-8 K-1 4 3_565 96.87(11) K-4 O2-8 K-1 4_556 3_565 136.96(9) Nb-1 O3-1 Nb-4 . 4_545 158.73(13) Nb-1 O3-1 K-4 . 2 87.00(8) Nb-4 O3-1 K-4 4_545 2 113.88(9) Nb-2 O3-2 Nb-1 . . 175.8(2) Nb-3 O3-3 Nb-2 . . 156.05(13) Nb-3 O3-3 K-2 . 2_455 95.30(9) Nb-2 O3-3 K-2 . 2_455 106.43(8) Nb-4 O3-4 Nb-3 . . 150.25(11) Nb-4 O3-4 K-1 . 2 94.42(9) Nb-3 O3-4 K-1 . 2 113.95(8) B-5 O4-1 B-1 4_645 . 122.6(3) B-5 O4-1 K-4 4_645 2 120.4(2) B-1 O4-1 K-4 . 2 108.2(2) B-5 O4-1 K-3 4_645 2 122.0(2) B-1 O4-1 K-3 . 2 93.1(2) K-4 O4-1 K-3 2 2 80.47(7) B-2 O4-2 B-6 . 4_645 122.7(3) B-2 O4-2 K-3 . 2 124.9(2) B-6 O4-2 K-3 4_645 2 103.7(2) B-2 O4-2 K-2 . 2 113.9(2) B-6 O4-2 K-2 4_645 2 100.6(2) K-3 O4-2 K-2 2 2 81.34(8) B-7 O4-3 B-3 4_645 . 124.3(3) B-7 O4-3 K-2 4_645 2 126.1(2) B-3 O4-3 K-2 . 2 104.0(2) B-7 O4-3 K-1 4_645 2 104.3(2) B-3 O4-3 K-1 . 2 104.1(2) K-2 O4-3 K-1 2 2 83.30(8) B-8 O4-4 B-4 4_645 . 123.9(3) B-8 O4-4 K-1 4_645 2 111.1(2) B-4 O4-4 K-1 . 2 119.4(2) B-8 O4-4 K-4 4_645 3_565 113.4(2) B-4 O4-4 K-4 . 3_565 96.7(2) K-1 O4-4 K-4 2 3_565 82.12(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance K-1 O2-5 4_544 2.756(3) K-1 O4-4 2_554 2.825(3) K-1 O1-4 2_554 2.853(3) K-1 O1-8 3_464 2.859(3) K-1 O1-7 3_464 2.999(3) K-1 O4-3 2_554 3.043(3) K-1 B-5 4_544 3.199(4) K-1 O3-4 2_554 3.262(2) K-1 O2-8 3_464 3.342(3) K-1 O2-1 1_554 3.404(3) K-1 B-8 3_464 3.572(4) K-1 Nb-4 2_554 3.8311(10) K-2 O2-2 1_554 2.817(3) K-2 O4-3 2_554 2.848(3) K-2 O1-7 3_464 2.859(3) K-2 O1-3 2_554 2.920(3) K-2 O4-2 2_554 3.018(3) K-2 O2-3 2_554 3.096(3) K-2 O1-2 2_554 3.101(3) K-2 B-2 1_554 3.242(4) K-2 O2-6 4_544 3.288(3) K-2 O3-3 2_454 3.385(3) K-2 B-3 2_554 3.470(4) K-2 B-5 4_544 3.516(4) K-3 O1-2 2_554 2.853(3) K-3 O1-6 3_464 2.859(3) K-3 O4-2 2_554 2.904(3) K-3 O2-7 4_544 2.957(3) K-3 O2-3 1_554 3.029(3) K-3 O2-6 3_464 3.106(3) K-3 O4-1 2_554 3.111(3) K-3 O1-1 2_554 3.176(3) K-3 O2-2 1_554 3.313(3) K-3 B-2 1_554 3.398(4) K-3 B-3 1_554 3.426(4) K-3 B-1 2_554 3.478(4) K-4 O1-5 3_464 2.774(3) K-4 O1-1 2_554 2.803(3) K-4 O2-8 4_544 2.871(3) K-4 O4-1 2_554 2.919(3) K-4 O1-4 3_464 3.034(3) K-4 O4-4 3_464 3.117(3) K-4 O2-4 1_554 3.143(3) K-4 O2-7 4_544 3.249(3) K-4 O2-1 2_554 3.275(3) K-4 B-8 4_544 3.285(4) K-4 B-7 4_544 3.403(4) K-4 O3-1 2_554 3.418(3) Nb-1 O3-1 . 1.769(2) Nb-1 O2-1 . 1.924(3) Nb-1 O2-5 4_545 1.944(3) Nb-1 O1-5 4_545 1.967(3) Nb-1 O1-1 . 2.031(3) Nb-1 O3-2 . 2.201(2) Nb-1 K-4 2 3.7660(10) Nb-1 K-1 1_556 3.8795(13) Nb-1 K-4 2_455 4.1572(10) Nb-2 O3-2 . 1.755(2) Nb-2 O2-2 . 1.946(3) Nb-2 O2-6 4_545 1.951(3) Nb-2 O1-2 . 1.991(3) Nb-2 O1-6 4_545 2.010(3) Nb-2 O3-3 . 2.208(2) Nb-2 K-2 1_556 3.8687(13) Nb-2 K-3 2_455 3.8723(11) Nb-2 K-3 2 4.0887(11) Nb-3 O3-3 . 1.770(2) Nb-3 O2-7 4_545 1.949(3) Nb-3 O2-3 . 1.963(3) Nb-3 O1-3 . 1.984(3) Nb-3 O1-7 4_545 2.023(3) Nb-3 O3-4 . 2.2223(19) Nb-3 K-3 1_556 3.7480(13) Nb-3 K-2 2_455 3.9617(11) Nb-3 K-2 2 3.9831(11) Nb-4 O3-4 . 1.7740(19) Nb-4 O2-4 . 1.938(3) Nb-4 O2-8 4_545 1.955(3) Nb-4 O1-8 4_545 1.962(3) Nb-4 O1-4 . 2.041(3) Nb-4 O3-1 4 2.212(2) Nb-4 K-4 1_556 3.7782(13) Nb-4 K-1 2 3.8311(10) Nb-4 K-1 2_455 4.0692(11) B-1 O2-1 . 1.329(5) B-1 O1-3 2 1.345(5) B-1 O4-1 . 1.396(4) B-1 K-3 2 3.478(4) B-2 O1-2 2 1.344(5) B-2 O2-2 . 1.355(5) B-2 O4-2 . 1.384(5) B-2 K-2 1_556 3.242(4) B-2 K-3 1_556 3.398(4) B-3 O1-1 2 1.340(5) B-3 O2-3 . 1.359(5) B-3 O4-3 . 1.407(4) B-3 K-3 1_556 3.426(4) B-3 K-2 2 3.470(4) B-4 O2-4 . 1.335(5) B-4 O1-8 2_565 1.346(5) B-4 O4-4 . 1.392(4) B-4 K-4 3_565 3.559(4) B-5 O2-5 . 1.354(5) B-5 O1-7 2_565 1.354(5) B-5 O4-1 4_655 1.383(5) B-5 K-1 4_556 3.199(4) B-5 K-2 4_556 3.516(4) B-6 O2-6 . 1.339(5) B-6 O1-6 2_565 1.350(5) B-6 O4-2 4_655 1.404(5) B-6 K-3 3_565 3.512(4) B-6 K-2 3_565 3.555(4) B-7 O1-5 2_565 1.345(5) B-7 O2-7 . 1.345(5) B-7 O4-3 4_655 1.398(5) B-7 K-4 4_556 3.403(4) B-7 K-3 4_556 3.522(4) B-8 O1-4 2_565 1.339(5) B-8 O2-8 . 1.353(5) B-8 O4-4 4_655 1.395(5) B-8 K-4 4_556 3.285(4) B-8 K-1 3_565 3.572(4) O1-1 B-3 2_554 1.340(5) O1-1 K-4 2 2.803(3) O1-1 K-3 2 3.176(3) O1-2 B-2 2_554 1.344(5) O1-2 K-3 2 2.853(3) O1-2 K-2 2 3.101(3) O1-3 B-1 2_554 1.345(5) O1-3 K-2 2 2.920(3) O1-4 B-8 2_564 1.339(5) O1-4 K-1 2 2.853(3) O1-4 K-4 3_565 3.034(3) O1-5 B-7 2_564 1.345(5) O1-5 Nb-1 4 1.967(3) O1-5 K-4 3_565 2.774(3) O1-6 B-6 2_564 1.350(5) O1-6 Nb-2 4 2.010(3) O1-6 K-3 3_565 2.859(3) O1-7 B-5 2_564 1.354(5) O1-7 Nb-3 4 2.023(3) O1-7 K-2 3_565 2.859(3) O1-7 K-1 3_565 2.999(3) O1-8 B-4 2_564 1.346(5) O1-8 Nb-4 4 1.962(3) O1-8 K-1 3_565 2.859(3) O2-1 K-4 2 3.275(3) O2-1 K-1 1_556 3.404(3) O2-2 K-2 1_556 2.817(3) O2-2 K-3 1_556 3.313(3) O2-3 K-3 1_556 3.029(3) O2-3 K-2 2 3.096(3) O2-4 K-4 1_556 3.143(3) O2-5 Nb-1 4 1.944(3) O2-5 K-1 4_556 2.756(3) O2-6 Nb-2 4 1.951(3) O2-6 K-3 3_565 3.106(3) O2-6 K-2 4_556 3.288(3) O2-7 Nb-3 4 1.949(3) O2-7 K-3 4_556 2.957(3) O2-7 K-4 4_556 3.249(3) O2-8 Nb-4 4 1.955(3) O2-8 K-4 4_556 2.871(3) O2-8 K-1 3_565 3.342(3) O3-1 Nb-4 4_545 2.212(2) O3-1 K-4 2 3.418(3) O3-3 K-2 2_455 3.385(3) O3-4 K-1 2 3.262(2) O4-1 B-5 4_645 1.383(5) O4-1 K-4 2 2.919(3) O4-1 K-3 2 3.111(3) O4-2 B-6 4_645 1.404(5) O4-2 K-3 2 2.904(3) O4-2 K-2 2 3.018(3) O4-3 B-7 4_645 1.398(5) O4-3 K-2 2 2.848(3) O4-3 K-1 2 3.043(3) O4-4 B-8 4_645 1.395(5) O4-4 K-1 2 2.825(3) O4-4 K-4 3_565 3.117(3)