#------------------------------------------------------------------------------ #$Date: 2021-04-28 04:49:09 +0300 (Wed, 28 Apr 2021) $ #$Revision: 264607 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/72/7707202.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_7707202 loop_ _publ_author_name 'Niu, Jingyang' 'Yang, Zongfei' 'Shang, Jingjing' 'Yang, Yuanyuan' 'Ma, Pengtao' 'Wang, Jingping' _publ_section_title ; Synthesis, structure and stability of three V-substituted polyoxoniobate clusters based on [TeNb9O33]17- units ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00223F _journal_year 2021 _chemical_formula_moiety 'C6 H24 Cu3 K5 N6 Na1.5 Nb9 O50 Te V3, Na O6, 4.5(O)' _chemical_formula_sum 'C6 H24 Cu3 K5 N6 Na2.5 Nb9 O60.5 Te V3' _chemical_formula_weight 2708.52 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-11-27 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-12-01 deposited with the CCDC. 2021-04-27 downloaded from the CCDC. ; _cell_angle_alpha 79.580(16) _cell_angle_beta 82.368(16) _cell_angle_gamma 60.151(9) _cell_formula_units_Z 2 _cell_length_a 12.824(4) _cell_length_b 12.873(5) _cell_length_c 27.492(14) _cell_measurement_reflns_used 9986 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.299 _cell_measurement_theta_min 2.181 _cell_volume 3867(3) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON II' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'Helios multilayer optic' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_unetI/netI 0.0450 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 48854 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.100 _diffrn_reflns_theta_max 25.100 _diffrn_reflns_theta_min 2.262 _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 3.185 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1053 before and 0.0628 after correction. The Ratio of minimum to maximum transmission is 0.8550. The \l/2 correction factor is Not present.' _exptl_crystal_colour blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 2.326 _exptl_crystal_description block _exptl_crystal_F_000 2571 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _refine_diff_density_max 2.363 _refine_diff_density_min -2.126 _refine_diff_density_rms 0.186 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 863 _refine_ls_number_reflns 13753 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0457 _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^)+(0.0368P)^2^+52.4680P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1068 _refine_ls_wR_factor_ref 0.1136 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11722 _reflns_number_total 13753 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00223f2.cif _cod_data_source_block 2 _cod_original_formula_sum 'C6 H24 Cu3 K5 N6 Na2.50 Nb9 O60.50 Te V3' _cod_database_code 7707202 _shelx_shelxl_version_number 2018/3 _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 0.682 _shelx_estimated_absorpt_t_min 0.598 _diffrn_source_source 'Incoatc Ius 3.0 ' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H) groups 2. Restrained distances O23W-O23W_$1 2.65 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints Uanis(O16W) \\sim Ueq, Uanis(O16B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: O16W(0.5) O20W(0.5) O21W(0.5) O22W(0.5) O23W(0.5) O16B(0.5) O24W(0.5) 5.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), N1(H1C,H1D), N2(H2C,H2D), N3(H3C,H3D), N4(H4C,H4D), N5(H5C,H5D), N6(H6C,H6D) ; _shelx_res_file ; TITL 2.res in P-1 2.res created by SHELXL-2018/3 at 17:15:16 on 27-Nov-2020 REM Old TITL Integration of M5123 REM SHELXT solution in P-1 REM R1 0.209, Rweak 0.011, Alpha 0.056, Orientation as input REM Formula found by SHELXT: Nb26 O161 CELL 0.71073 12.8239 12.8731 27.4924 79.58 82.368 60.151 ZERR 2 0.0044 0.0048 0.0135 0.016 0.016 0.009 LATT 1 SFAC C H Cu K N Na Nb O Te V UNIT 12 48 6 10 12 5 18 121 2 6 EQIV $1 2-X,1-Y,1-Z DANG 2.65 0.01 O23W O23W_$1 ISOR 0.01 0.02 O16W O16B L.S. 10 PLAN 10 SIZE 0.18 0.16 0.13 TEMP -123.15 LIST 4 BOND $H HTAB ABIN fmap 2 acta OMIT -3 50.2 OMIT 0 0 4 OMIT -1 -2 1 OMIT 1 0 2 OMIT -1 1 2 OMIT 1 2 4 OMIT 0 1 8 OMIT -1 -3 4 OMIT 2 1 5 OMIT 1 1 2 OMIT 0 1 2 OMIT -1 -1 4 OMIT 1 -1 3 REM REM REM WGHT 0.036800 52.468002 FVAR 0.09576 C1 1 0.173298 1.278734 0.132097 11.00000 0.02858 0.03901 = 0.03493 0.01041 -0.01229 -0.01389 AFIX 23 H1A 2 0.206198 1.334642 0.129997 11.00000 -1.20000 H1B 2 0.091633 1.324790 0.119125 11.00000 -1.20000 AFIX 0 C2 1 0.254093 1.176499 0.101960 11.00000 0.04324 0.05035 = 0.02868 0.00527 -0.01164 -0.01356 AFIX 23 H2A 2 0.217322 1.125029 0.101229 11.00000 -1.20000 H2B 2 0.266048 1.209282 0.067505 11.00000 -1.20000 AFIX 0 C3 1 1.010658 0.735123 0.102851 11.00000 0.05577 0.04486 = 0.02764 -0.01106 -0.00132 -0.02722 AFIX 23 H3A 2 1.099298 0.699676 0.101372 11.00000 -1.20000 H3B 2 0.984020 0.754673 0.068614 11.00000 -1.20000 AFIX 0 C4 1 0.974580 0.646374 0.132663 11.00000 0.03034 0.03210 = 0.03940 -0.01857 0.00070 -0.01732 AFIX 23 H4A 2 0.887349 0.677230 0.130421 11.00000 -1.20000 H4B 2 1.019181 0.567853 0.119561 11.00000 -1.20000 AFIX 0 C5 1 0.702005 1.484972 0.103164 11.00000 0.04083 0.05676 = 0.01994 0.00327 -0.00152 -0.02996 AFIX 23 H5A 2 0.649031 1.573543 0.100961 11.00000 -1.20000 H5B 2 0.730004 1.463719 0.069222 11.00000 -1.20000 AFIX 0 C6 1 0.809902 1.445019 0.134209 11.00000 0.02738 0.03984 = 0.04162 -0.00026 0.00893 -0.02093 AFIX 23 H6A 2 0.868339 1.358668 0.132463 11.00000 -1.20000 H6B 2 0.850925 1.493034 0.121236 11.00000 -1.20000 AFIX 0 PART 1 CU1 3 0.339210 1.092675 0.199211 11.00000 0.01745 0.01689 = 0.02088 -0.00312 -0.00310 -0.00624 PART 0 CU2 3 0.956747 0.798083 0.199918 11.00000 0.01943 0.01734 = 0.02077 -0.00515 0.00090 -0.00983 CU3 3 0.636296 1.413267 0.200745 11.00000 0.01624 0.01975 = 0.02005 -0.00050 -0.00038 -0.01072 K1 4 1.153787 0.547912 0.301814 11.00000 0.01689 0.01656 = 0.05595 -0.00470 -0.00187 -0.00391 K2 4 0.628989 0.589755 0.303050 11.00000 0.02556 0.01911 = 0.07075 -0.01166 -0.00208 -0.01284 K3 4 0.111669 1.065610 0.305446 11.00000 0.01601 0.02823 = 0.14078 -0.01980 0.00182 -0.01277 K4 4 0.410275 0.189823 0.501370 11.00000 0.05094 0.02799 = 0.01755 -0.00062 0.00655 -0.01484 N1 5 0.167701 1.225249 0.184224 11.00000 0.03192 0.02872 = 0.03028 0.00058 -0.00874 -0.01943 AFIX 23 H1C 2 0.117049 1.193629 0.188094 11.00000 -1.20000 H1D 2 0.140971 1.282303 0.204883 11.00000 -1.20000 AFIX 0 N2 5 0.371551 1.104573 0.126204 11.00000 0.03130 0.04529 = 0.02733 0.00650 -0.00044 -0.00134 AFIX 23 H2C 2 0.417476 1.141260 0.116976 11.00000 -1.20000 H2D 2 0.412217 1.029391 0.116783 11.00000 -1.20000 AFIX 0 N3 5 0.953686 0.844983 0.126890 11.00000 0.07082 0.03339 = 0.02858 -0.00477 -0.00455 -0.02954 AFIX 23 H3C 2 0.876306 0.892788 0.117809 11.00000 -1.20000 H3D 2 0.994100 0.887339 0.117357 11.00000 -1.20000 AFIX 0 N4 5 1.003028 0.630543 0.185016 11.00000 0.01920 0.02986 = 0.03349 -0.00908 0.00473 -0.01192 AFIX 23 H4C 2 1.082855 0.579196 0.189172 11.00000 -1.20000 H4D 2 0.960138 0.599950 0.205510 11.00000 -1.20000 AFIX 0 N5 5 0.636245 1.421938 0.127820 11.00000 0.04044 0.07059 = 0.02673 -0.00827 0.00766 -0.04085 AFIX 23 H5C 2 0.672057 1.346036 0.119297 11.00000 -1.20000 H5D 2 0.559194 1.462352 0.118007 11.00000 -1.20000 AFIX 0 N6 5 0.765712 1.463627 0.185951 11.00000 0.02816 0.02201 = 0.03058 -0.00116 0.00117 -0.01344 AFIX 23 H6C 2 0.734492 1.542641 0.189777 11.00000 -1.20000 H6D 2 0.826835 1.417802 0.206813 11.00000 -1.20000 AFIX 0 NB1 7 0.455807 0.915660 0.293728 11.00000 0.00950 0.00942 = 0.01767 -0.00192 -0.00096 -0.00545 NB2 7 0.478361 1.400294 0.295560 11.00000 0.00950 0.00893 = 0.01693 -0.00267 0.00075 -0.00451 NB3 7 0.626122 1.201052 0.397450 11.00000 0.01337 0.01479 = 0.01260 -0.00357 0.00005 -0.00814 NB4 7 0.964007 0.894302 0.295127 11.00000 0.00829 0.01091 = 0.01546 -0.00258 -0.00057 -0.00432 NB5 7 0.449529 1.041810 0.395644 11.00000 0.01099 0.01357 = 0.01310 -0.00157 0.00124 -0.00705 NB6 7 0.785776 0.867186 0.396881 11.00000 0.01101 0.01429 = 0.01357 0.00083 -0.00118 -0.00465 NB7 7 0.801143 0.743374 0.292200 11.00000 0.00943 0.00844 = 0.01939 -0.00173 0.00011 -0.00388 NB8 7 0.304231 1.230505 0.291701 11.00000 0.00741 0.00866 = 0.01596 -0.00202 -0.00007 -0.00373 NB9 7 0.793430 1.239171 0.293096 11.00000 0.00922 0.01002 = 0.01558 -0.00248 -0.00040 -0.00569 O1 8 0.434716 1.348697 0.131226 11.00000 0.05770 0.08450 = 0.01886 0.00372 -0.00554 -0.05937 O1W 8 0.610635 0.688153 0.409099 11.00000 0.09325 0.05094 = 0.06089 -0.00726 -0.00231 -0.04717 O2W 8 0.781270 0.429219 0.381711 11.00000 0.03844 0.03548 = 0.05996 -0.02462 0.01650 -0.02505 O3W 8 1.072573 0.207958 0.383023 11.00000 0.02384 0.04873 = 0.05557 0.01641 -0.00501 -0.01998 O4W 8 1.272677 0.932326 0.198032 11.00000 0.02876 0.02690 = 0.03541 -0.00914 -0.00410 -0.01019 O5W 8 1.183063 0.732965 0.198533 11.00000 0.02576 0.02381 = 0.03682 -0.00729 0.00596 -0.01248 O6W 8 1.474136 0.641393 0.198912 11.00000 0.02170 0.02252 = 0.03603 0.00065 -0.00211 -0.00893 O7W 8 1.465622 0.833319 0.100909 11.00000 0.04936 0.06664 = 0.05180 -0.01202 0.00710 -0.04237 O8W 8 1.144494 0.942682 0.100907 11.00000 0.03957 0.04712 = 0.05283 0.00489 -0.01181 -0.01408 O9W 8 1.358051 0.623922 0.099838 11.00000 0.06868 0.03783 = 0.04916 -0.01547 -0.00547 -0.02138 O2 8 0.263027 1.490358 0.193880 11.00000 0.02226 0.01633 = 0.08201 0.00936 -0.02143 -0.00827 O3 8 1.028750 1.100700 0.189897 11.00000 0.01983 0.02565 = 0.09562 -0.01350 0.01292 -0.01473 O4 8 0.648845 0.911601 0.130393 11.00000 0.03056 0.05821 = 0.01841 -0.00341 -0.00158 -0.00177 O5 8 0.640209 0.725151 0.190629 11.00000 0.02570 0.03008 = 0.08911 -0.03732 -0.00228 -0.01068 O6 8 0.831592 0.789900 0.456882 11.00000 0.02089 0.02377 = 0.01918 0.00144 -0.00339 -0.00672 O7 8 0.864893 1.121009 0.131550 11.00000 0.08794 0.02834 = 0.01766 -0.00444 0.00252 -0.02452 O8 8 0.151598 1.334890 0.281676 11.00000 0.01019 0.01336 = 0.02280 -0.00239 -0.00239 -0.00221 O9 8 0.379562 1.558015 0.288014 11.00000 0.01864 0.01385 = 0.02413 -0.00375 0.00020 -0.00743 O10 8 0.853754 0.593484 0.281958 11.00000 0.01613 0.01475 = 0.02589 -0.00299 0.00189 -0.00744 O10W 8 1.234241 -0.121586 0.387784 11.00000 0.03684 0.04868 = 0.04394 -0.02316 0.01504 -0.03219 O11W 8 1.462914 -0.410828 0.386172 11.00000 0.03403 0.01899 = 0.04984 -0.00570 -0.01595 -0.00558 O12W 8 1.167990 -0.349683 0.387385 11.00000 0.02426 0.03443 = 0.05842 0.01378 -0.00394 -0.01410 O13W 8 -0.026322 0.029909 0.411589 11.00000 0.02502 0.05623 = 0.02513 0.00102 -0.00483 -0.02174 O14W 8 0.272418 0.384511 0.412231 11.00000 0.06046 0.05126 = 0.08786 0.01008 0.02690 0.00846 O15W 8 0.009439 0.496043 0.379167 11.00000 0.02840 0.02202 = 0.04294 -0.00672 -0.00671 -0.00849 PART 1 O16W 8 0.204592 -0.035291 0.486301 10.50000 0.00627 0.08448 = 0.04086 0.05104 -0.00824 -0.01304 PART 0 O11 8 1.121238 0.840628 0.287129 11.00000 0.01299 0.01827 = 0.02153 -0.00437 -0.00140 -0.00547 O12 8 0.399780 0.818887 0.286119 11.00000 0.01449 0.01545 = 0.02568 -0.00169 -0.00508 -0.00856 O13 8 0.618529 1.236252 0.457744 11.00000 0.02387 0.02919 = 0.01839 -0.00844 0.00287 -0.01489 O14 8 0.506370 1.370105 0.219837 11.00000 0.01239 0.01760 = 0.01796 -0.00055 -0.00099 -0.00804 O15 8 0.419787 0.929499 0.362814 11.00000 0.01662 0.01277 = 0.02149 -0.00054 -0.00078 -0.00997 O16 8 0.761735 0.834250 0.219773 11.00000 0.01305 0.01592 = 0.02072 -0.00212 -0.00222 -0.00662 O17 8 0.896642 1.294609 0.282623 11.00000 0.01857 0.01868 = 0.02066 -0.00095 -0.00229 -0.01185 O18 8 0.380216 1.236575 0.219600 11.00000 0.01693 0.01655 = 0.01739 -0.00452 0.00074 -0.01056 O19 8 0.631816 1.190889 0.307628 11.00000 0.00863 0.00845 = 0.01609 -0.00384 0.00033 -0.00391 O20 8 0.502202 0.959425 0.218792 11.00000 0.01583 0.01167 = 0.02100 -0.00140 -0.00265 -0.00658 O21 8 0.506121 1.368011 0.364526 11.00000 0.01782 0.01676 = 0.01672 -0.00336 0.00134 -0.00831 O22 8 0.505245 1.066777 0.306886 11.00000 0.00950 0.01104 = 0.01343 -0.00131 0.00143 -0.00703 O23 8 0.782695 1.213976 0.220830 11.00000 0.01331 0.01608 = 0.01729 -0.00240 -0.00180 -0.00746 O24 8 0.816722 0.726238 0.361805 11.00000 0.01947 0.01752 = 0.01971 -0.00302 0.00462 -0.01208 O25 8 0.387760 1.023257 0.455454 11.00000 0.01541 0.01827 = 0.01808 -0.00056 0.00111 -0.00602 O26 8 0.366813 1.338564 0.299112 11.00000 0.01059 0.01242 = 0.02060 -0.00271 0.00053 -0.00515 O27 8 0.300251 1.177820 0.361459 11.00000 0.01001 0.01550 = 0.01760 -0.00422 0.00106 -0.00283 O28 8 0.916623 0.956775 0.219400 11.00000 0.01824 0.01308 = 0.02027 -0.00263 -0.00079 -0.00944 O29 8 0.626179 0.803665 0.298580 11.00000 0.01018 0.01027 = 0.02392 -0.00168 -0.00135 -0.00467 O30 8 0.754858 1.241714 0.363096 11.00000 0.01338 0.02114 = 0.01907 -0.00406 -0.00134 -0.01069 O31 8 0.310747 1.080903 0.273272 11.00000 0.00925 0.01003 = 0.01871 -0.00355 -0.00318 -0.00400 O32 8 0.903830 1.063704 0.299814 11.00000 0.01398 0.01241 = 0.01811 -0.00436 -0.00137 -0.00731 O33 8 0.955010 0.754347 0.274093 11.00000 0.01162 0.01568 = 0.01863 -0.00511 0.00228 -0.00802 O34 8 0.639880 1.396402 0.274966 11.00000 0.00839 0.01249 = 0.02242 0.00117 -0.00016 -0.00579 O35 8 0.756151 0.940754 0.307212 11.00000 0.00922 0.01180 = 0.01473 -0.00381 0.00151 -0.00599 O36 8 0.947320 0.843258 0.364279 11.00000 0.01015 0.01832 = 0.01916 -0.00184 -0.00066 -0.00655 O38 8 0.744643 1.031734 0.402579 11.00000 0.01433 0.01522 = 0.01889 -0.00379 -0.00047 -0.00751 O39 8 0.617161 0.913272 0.402706 11.00000 0.01356 0.01430 = 0.01829 -0.00106 -0.00104 -0.00587 O40 8 0.498437 1.158326 0.403203 11.00000 0.01249 0.01625 = 0.01356 -0.00124 0.00003 -0.00654 TE1 9 0.636079 1.078079 0.271722 11.00000 0.00788 0.00891 = 0.01212 -0.00181 0.00005 -0.00459 V1 10 0.900575 1.098985 0.189684 11.00000 0.01742 0.01347 = 0.01862 -0.00284 0.00589 -0.00820 V2 10 0.639164 0.854773 0.189032 11.00000 0.01355 0.01931 = 0.02100 -0.00927 -0.00136 -0.00567 V3 10 0.393369 1.363358 0.190379 11.00000 0.01718 0.01784 = 0.01880 0.00434 -0.00630 -0.01161 NA1 6 1.317384 0.786090 0.141463 11.00000 0.02986 0.02942 = 0.02852 -0.00385 -0.00099 -0.01488 NA2 6 1.293543 -0.277163 0.336839 11.00000 0.01538 0.01626 = 0.02758 -0.00422 -0.00210 -0.00748 NA3 6 0.000000 0.000000 0.500000 10.50000 0.03303 0.04949 = 0.03164 -0.00611 -0.00122 -0.02443 PART 1 K5 4 0.961518 0.393605 0.327303 11.00000 0.05894 0.06378 = 0.07554 -0.01268 -0.00154 -0.02910 PART 0 O17W 8 1.145375 1.042772 0.003857 11.00000 0.10920 O18W 8 1.546431 0.806381 0.003845 11.00000 0.11396 O19W 8 1.309693 0.646432 0.002857 11.00000 0.13639 O20W 8 0.181391 -0.193441 0.491727 10.50000 0.05578 0.07759 = 0.04546 0.01157 -0.02428 -0.04241 O21W 8 0.715071 0.844061 0.037851 10.50000 0.06839 O22W 8 0.357380 1.409655 0.036661 10.50000 0.06438 O23W 8 0.950657 0.600877 0.520076 10.50000 0.06613 PART 2 O16B 8 0.149357 0.069673 0.483206 10.50000 0.06643 0.08335 = 0.03393 -0.03967 0.02573 -0.06380 PART 0 O24W 8 -0.021846 0.200991 0.496359 10.50000 0.08831 HKLF 4 REM 2.res in P-1 REM wR2 = 0.1136, GooF = S = 1.041, Restrained GooF = 1.042 for all data REM R1 = 0.0457 for 11722 Fo > 4sig(Fo) and 0.0561 for all 13753 data REM 863 parameters refined using 13 restraints END WGHT 0.0369 52.3878 REM Instructions for potential hydrogen bonds EQIV $3 x-1, y, z HTAB N1 O3_$3 HTAB N1 O8 HTAB N2 O7W_$3 HTAB N3 O8W EQIV $5 x+1, y-1, z HTAB N4 O2_$5 HTAB N4 O10 HTAB N5 O1 EQIV $4 x-1, y+1, z HTAB N5 O9W_$4 EQIV $6 x, y+1, z HTAB N6 O5_$6 HTAB N6 O17 REM Highest difference peak 2.363, deepest hole -2.126, 1-sigma level 0.186 Q1 1 0.6454 0.9437 0.0293 11.00000 0.05 2.36 Q2 1 1.0543 0.6317 0.5570 11.00000 0.05 2.09 Q3 1 0.1841 0.3218 0.4429 11.00000 0.05 1.94 Q4 1 0.3233 0.4253 0.4442 11.00000 0.05 1.92 Q5 1 0.1174 1.0559 0.3355 11.00000 0.05 1.60 Q6 1 0.4487 1.3882 0.0319 11.00000 0.05 1.60 Q7 1 0.7138 0.6153 0.4383 11.00000 0.05 1.57 Q8 1 0.4776 0.7422 0.4449 11.00000 0.05 1.50 Q9 1 0.6385 0.5651 0.3341 11.00000 0.05 1.41 Q10 1 0.2762 -0.2953 0.4765 11.00000 0.05 1.36 ; _shelx_res_checksum 27785 _shelx_fab_file ; -15 -8 1 4.2161 0.3137 -15 -7 1 -3.6816 0.4257 -15 -7 2 -1.6162 0.4591 -15 -6 1 -0.6552 0.3390 -14 -11 1 1.8580 0.3150 -14 -11 2 -1.0278 -0.4147 -14 -11 3 1.3476 -1.0064 -14 -10 1 -2.8368 -0.5501 -14 -10 2 -0.1391 -0.8911 -14 -10 3 0.3403 -1.1441 -14 -10 4 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-1.1674 -0.0446 15 6 0 -1.9397 -0.1297 15 6 1 -0.9560 0.4347 15 6 2 -2.3849 0.4754 15 6 3 -0.8690 0.2579 15 6 4 -1.2866 0.0534 15 6 5 0.5860 -0.1853 15 6 6 0.7410 0.1405 15 6 7 1.3424 0.0751 15 6 8 1.1215 0.2910 15 6 9 0.0911 -0.0282 15 7 0 -1.4129 0.1645 15 7 1 -3.7086 0.3778 15 7 2 -0.7250 0.3849 15 7 3 -2.8832 0.1610 15 7 4 0.4540 -0.1537 15 7 5 -1.3498 0.0223 15 7 6 1.1890 -0.0092 15 7 7 -0.7570 0.2808 15 7 8 0.1051 0.0272 15 7 9 -1.1692 0.0255 15 7 10 -0.9254 -0.1334 15 8 0 3.0353 0.1850 15 8 1 5.6409 0.4569 15 8 2 2.8381 0.3947 15 8 3 4.7633 0.0588 15 8 4 1.4446 0.0049 15 8 5 3.1291 -0.0439 15 8 6 0.0237 0.1855 15 8 7 0.9019 0.1012 15 8 8 -1.3175 0.0388 15 8 9 -0.7723 -0.0989 15 8 10 -0.7089 -0.1393 15 9 0 0.9875 0.8436 15 9 1 -0.7364 1.0297 15 9 2 -0.8797 0.5736 15 9 3 -2.4699 0.2743 15 9 4 -1.4316 0.0341 15 9 5 -1.5742 0.1140 15 9 6 -0.1131 0.1973 15 9 7 0.2487 0.1008 15 9 8 1.0201 0.0646 15 9 9 2.2135 -0.1231 15 9 10 2.0765 0.0742 15 10 3 -2.1768 -0.0928 15 10 4 -0.1388 -0.1444 15 10 5 -0.2322 0.0364 15 10 6 1.4074 0.0095 15 10 7 -0.2581 0.1223 0 0 0 0.0 0.0 ; _shelx_fab_checksum 32427 _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 _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1733(8) 1.2787(9) 0.1321(3) 0.036(2) Uani 1 1 d . . . . . H1A H 0.206198 1.334642 0.129997 0.044 Uiso 1 1 calc R . . . . H1B H 0.091633 1.324790 0.119125 0.044 Uiso 1 1 calc R . . . . C2 C 0.2541(9) 1.1765(10) 0.1020(4) 0.045(3) Uani 1 1 d . . . . . H2A H 0.217322 1.125029 0.101229 0.054 Uiso 1 1 calc R . . . . H2B H 0.266048 1.209282 0.067505 0.054 Uiso 1 1 calc R . . . . C3 C 1.0107(10) 0.7351(9) 0.1029(3) 0.041(2) Uani 1 1 d . . . . . H3A H 1.099298 0.699676 0.101372 0.049 Uiso 1 1 calc R . . . . H3B H 0.984020 0.754673 0.068614 0.049 Uiso 1 1 calc R . . . . C4 C 0.9746(8) 0.6464(8) 0.1327(3) 0.031(2) Uani 1 1 d . . . . . H4A H 0.887349 0.677230 0.130421 0.038 Uiso 1 1 calc R . . . . H4B H 1.019181 0.567853 0.119561 0.038 Uiso 1 1 calc R . . . . C5 C 0.7020(9) 1.4850(10) 0.1032(3) 0.038(2) Uani 1 1 d . . . . . H5A H 0.649031 1.573543 0.100961 0.045 Uiso 1 1 calc R . . . . H5B H 0.730004 1.463719 0.069222 0.045 Uiso 1 1 calc R . . . . C6 C 0.8099(8) 1.4450(9) 0.1342(3) 0.036(2) Uani 1 1 d . . . . . H6A H 0.868339 1.358668 0.132463 0.043 Uiso 1 1 calc R . . . . H6B H 0.850925 1.493034 0.121236 0.043 Uiso 1 1 calc R . . . . Cu1 Cu 0.33921(8) 1.09268(8) 0.19921(3) 0.0190(2) Uani 1 1 d . . . A 1 Cu2 Cu 0.95675(8) 0.79808(8) 0.19992(3) 0.0186(2) Uani 1 1 d . . . . . Cu3 Cu 0.63630(8) 1.41327(8) 0.20075(3) 0.0182(2) Uani 1 1 d . . . . . K1 K 1.15379(16) 0.54791(16) 0.30181(8) 0.0317(4) Uani 1 1 d . . . . . K2 K 0.62899(18) 0.58976(17) 0.30305(9) 0.0368(5) Uani 1 1 d . . . . . K3 K 0.11167(19) 1.0656(2) 0.30545(13) 0.0602(8) Uani 1 1 d . . . . . K4 K 0.4103(2) 0.18982(18) 0.50137(7) 0.0353(5) Uani 1 1 d . . . . . N1 N 0.1677(7) 1.2252(6) 0.1842(3) 0.0281(16) Uani 1 1 d . . . . . H1C H 0.117049 1.193629 0.188094 0.034 Uiso 1 1 calc R . . A . H1D H 0.140971 1.282303 0.204883 0.034 Uiso 1 1 calc R . . A . N2 N 0.3716(7) 1.1046(8) 0.1262(3) 0.044(2) Uani 1 1 d . . . . . H2C H 0.417476 1.141260 0.116976 0.053 Uiso 1 1 calc R . . A . H2D H 0.412217 1.029391 0.116783 0.053 Uiso 1 1 calc R . . A . N3 N 0.9537(9) 0.8450(7) 0.1269(3) 0.042(2) Uani 1 1 d . . . . . H3C H 0.876306 0.892788 0.117809 0.050 Uiso 1 1 calc R . . . . H3D H 0.994100 0.887339 0.117357 0.050 Uiso 1 1 calc R . . . . N4 N 1.0030(6) 0.6305(6) 0.1850(3) 0.0275(16) Uani 1 1 d . . . . . H4C H 1.082855 0.579196 0.189172 0.033 Uiso 1 1 calc R . . . . H4D H 0.960138 0.599950 0.205510 0.033 Uiso 1 1 calc R . . . . N5 N 0.6362(7) 1.4219(8) 0.1278(3) 0.040(2) Uani 1 1 d . . . . . H5C H 0.672057 1.346036 0.119297 0.049 Uiso 1 1 calc R . . . . H5D H 0.559194 1.462352 0.118007 0.049 Uiso 1 1 calc R . . . . N6 N 0.7657(6) 1.4636(6) 0.1860(3) 0.0270(16) Uani 1 1 d . . . . . H6C H 0.734492 1.542641 0.189777 0.032 Uiso 1 1 calc R . . . . H6D H 0.826835 1.417802 0.206813 0.032 Uiso 1 1 calc R . . . . Nb1 Nb 0.45581(6) 0.91566(6) 0.29373(2) 0.01177(14) Uani 1 1 d . . . . . Nb2 Nb 0.47836(6) 1.40029(6) 0.29556(2) 0.01178(14) Uani 1 1 d . . . . . Nb3 Nb 0.62612(6) 1.20105(6) 0.39745(2) 0.01284(14) Uani 1 1 d . . . . . Nb4 Nb 0.96401(6) 0.89430(6) 0.29513(2) 0.01159(14) Uani 1 1 d . . . . . Nb5 Nb 0.44953(6) 1.04181(6) 0.39564(2) 0.01229(14) Uani 1 1 d . . . . . Nb6 Nb 0.78578(6) 0.86719(6) 0.39688(2) 0.01395(15) Uani 1 1 d . . . . . Nb7 Nb 0.80114(6) 0.74337(6) 0.29220(2) 0.01272(14) Uani 1 1 d . . . . . Nb8 Nb 0.30423(5) 1.23050(6) 0.29170(2) 0.01076(14) Uani 1 1 d . . . . . Nb9 Nb 0.79343(6) 1.23917(6) 0.29310(2) 0.01107(14) Uani 1 1 d . . . . . O1 O 0.4347(6) 1.3487(7) 0.1312(2) 0.0438(18) Uani 1 1 d . . . . . O1W O 0.6106(8) 0.6882(7) 0.4091(3) 0.063(2) Uani 1 1 d . . . . . O2W O 0.7813(6) 0.4292(6) 0.3817(3) 0.0408(17) Uani 1 1 d . . . . . O3W O 1.0726(6) 0.2080(6) 0.3830(3) 0.0447(18) Uani 1 1 d . . . . . O4W O 1.2727(5) 0.9323(5) 0.1980(2) 0.0309(14) Uani 1 1 d . . . . . O5W O 1.1831(5) 0.7330(5) 0.1985(2) 0.0289(14) Uani 1 1 d . . . . . O6W O 1.4741(5) 0.6414(5) 0.1989(2) 0.0281(13) Uani 1 1 d . . . . . O7W O 1.4656(7) 0.8333(7) 0.1009(3) 0.0500(19) Uani 1 1 d . . . . . O8W O 1.1445(6) 0.9427(7) 0.1009(3) 0.0503(19) Uani 1 1 d . . . . . O9W O 1.3581(7) 0.6239(6) 0.0998(3) 0.052(2) Uani 1 1 d . . . . . O2 O 0.2630(5) 1.4904(5) 0.1939(3) 0.0410(18) Uani 1 1 d . . . . . O3 O 1.0288(5) 1.1007(6) 0.1899(3) 0.0463(19) Uani 1 1 d . . . . . O4 O 0.6488(6) 0.9116(7) 0.1304(2) 0.0448(18) Uani 1 1 d . . . . . O5 O 0.6402(6) 0.7252(6) 0.1906(3) 0.0454(19) Uani 1 1 d . . . . . O6 O 0.8316(5) 0.7899(5) 0.45688(19) 0.0235(12) Uani 1 1 d . . . . . O7 O 0.8649(7) 1.1210(6) 0.1315(2) 0.0467(19) Uani 1 1 d . . . . . O8 O 0.1516(4) 1.3349(4) 0.28168(19) 0.0169(11) Uani 1 1 d . . . . . O9 O 0.3796(5) 1.5580(5) 0.28801(19) 0.0190(11) Uani 1 1 d . . . . . O10 O 0.8538(5) 0.5935(5) 0.28196(19) 0.0192(11) Uani 1 1 d . . . . . O10W O 1.2342(6) -0.1216(6) 0.3878(2) 0.0374(16) Uani 1 1 d . . . . . O11W O 1.4629(6) -0.4108(5) 0.3862(2) 0.0359(15) Uani 1 1 d . . . . . O12W O 1.1680(6) -0.3497(6) 0.3874(3) 0.0418(17) Uani 1 1 d . . . . . O13W O -0.0263(5) 0.0299(6) 0.4116(2) 0.0351(15) Uani 1 1 d . . . . . O14W O 0.2724(8) 0.3845(8) 0.4122(4) 0.088(3) Uani 1 1 d . . . . . O15W O 0.0094(5) 0.4960(5) 0.3792(2) 0.0319(14) Uani 1 1 d . . . . . O16W O 0.2046(10) -0.0353(16) 0.4863(5) 0.056(5) Uani 0.5 1 d . U . B 1 O11 O 1.1212(4) 0.8406(5) 0.28713(19) 0.0182(11) Uani 1 1 d . . . . . O12 O 0.3998(4) 0.8189(4) 0.28612(19) 0.0177(11) Uani 1 1 d . . . . . O13 O 0.6185(5) 1.2363(5) 0.45774(19) 0.0226(12) Uani 1 1 d . . . . . O14 O 0.5064(4) 1.3701(4) 0.21984(18) 0.0159(11) Uani 1 1 d . . . . . O15 O 0.4198(4) 0.9295(4) 0.36281(19) 0.0160(11) Uani 1 1 d . . . . . O16 O 0.7617(4) 0.8342(4) 0.21977(19) 0.0167(11) Uani 1 1 d . . . . . O17 O 0.8966(5) 1.2946(5) 0.28262(19) 0.0182(11) Uani 1 1 d . . . . . O18 O 0.3802(4) 1.2366(4) 0.21960(18) 0.0157(11) Uani 1 1 d . . . . . O19 O 0.6318(4) 1.1909(4) 0.30763(17) 0.0109(10) Uani 1 1 d . . . . . O20 O 0.5022(4) 0.9594(4) 0.21879(19) 0.0161(11) Uani 1 1 d . . . . . O21 O 0.5061(5) 1.3680(5) 0.36453(18) 0.0172(11) Uani 1 1 d . . . . . O22 O 0.5052(4) 1.0668(4) 0.30689(17) 0.0107(10) Uani 1 1 d . . . . . O23 O 0.7827(4) 1.2140(4) 0.22083(18) 0.0153(11) Uani 1 1 d . . . . . O24 O 0.8167(5) 0.7262(5) 0.36181(19) 0.0180(11) Uani 1 1 d . . . . . O25 O 0.3878(5) 1.0233(5) 0.45545(19) 0.0187(11) Uani 1 1 d . . . . . O26 O 0.3668(4) 1.3386(4) 0.29911(18) 0.0148(11) Uani 1 1 d . . . . . O27 O 0.3003(4) 1.1778(4) 0.36146(18) 0.0158(11) Uani 1 1 d . . . . . O28 O 0.9166(5) 0.9568(4) 0.21940(18) 0.0163(11) Uani 1 1 d . . . . . O29 O 0.6262(4) 0.8037(4) 0.29858(19) 0.0150(11) Uani 1 1 d . . . . . O30 O 0.7549(4) 1.2417(5) 0.36310(18) 0.0166(11) Uani 1 1 d . . . . . O31 O 0.3107(4) 1.0809(4) 0.27327(18) 0.0125(10) Uani 1 1 d . . . . . O32 O 0.9038(4) 1.0637(4) 0.29981(18) 0.0140(10) Uani 1 1 d . . . . . O33 O 0.9550(4) 0.7543(4) 0.27409(18) 0.0146(11) Uani 1 1 d . . . . . O34 O 0.6399(4) 1.3964(4) 0.27497(18) 0.0147(11) Uani 1 1 d . . . . . O35 O 0.7562(4) 0.9408(4) 0.30721(17) 0.0115(10) Uani 1 1 d . . . . . O36 O 0.9473(4) 0.8433(5) 0.36428(18) 0.0161(11) Uani 1 1 d . . . . . O38 O 0.7446(4) 1.0317(4) 0.40258(18) 0.0158(11) Uani 1 1 d . . . . . O39 O 0.6172(4) 0.9133(4) 0.40271(18) 0.0159(11) Uani 1 1 d . . . . . O40 O 0.4984(4) 1.1583(4) 0.40320(18) 0.0145(11) Uani 1 1 d . . . . . Te1 Te 0.63608(4) 1.07808(4) 0.27172(2) 0.00941(11) Uani 1 1 d . . . . . V1 V 0.90058(12) 1.09898(11) 0.18968(5) 0.0168(3) Uani 1 1 d . . . . . V2 V 0.63916(11) 0.85477(12) 0.18903(5) 0.0180(3) Uani 1 1 d . . . . . V3 V 0.39337(12) 1.36336(12) 0.19038(5) 0.0170(3) Uani 1 1 d . . . . . Na1 Na 1.3174(3) 0.7861(3) 0.14146(12) 0.0291(8) Uani 1 1 d . . . . . Na2 Na 1.2935(3) -0.2772(3) 0.33684(11) 0.0195(6) Uani 1 1 d . . . . . Na3 Na 0.000000 0.000000 0.500000 0.0360(12) Uani 1 2 d S T P . . K5 K 0.9615(3) 0.3936(3) 0.32730(12) 0.0661(8) Uani 1 1 d . . . C 1 O17W O 1.1454(11) 1.0428(11) 0.0039(5) 0.109(4) Uiso 1 1 d . . . . . O18W O 1.5464(12) 0.8064(12) 0.0038(5) 0.114(4) Uiso 1 1 d . . . . . O19W O 1.3097(14) 0.6464(14) 0.0029(5) 0.136(5) Uiso 1 1 d . . . . . O20W O 0.1814(14) -0.1934(15) 0.4917(5) 0.056(4) Uani 0.5 1 d . . . B . O21W O 0.7151(16) 0.8441(16) 0.0379(7) 0.068(5) Uiso 0.5 1 d . . . . . O22W O 0.3574(16) 1.4097(16) 0.0367(6) 0.064(5) Uiso 0.5 1 d . . . . . O23W O 0.9507(15) 0.6009(9) 0.5201(6) 0.066(5) Uiso 0.5 1 d D . . . . O16B O 0.1494(15) 0.0697(16) 0.4832(5) 0.047(4) Uani 0.5 1 d . U . B 2 O24W O -0.0218(19) 0.2010(19) 0.4964(8) 0.088(6) Uiso 0.5 1 d . . . B . 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 C1 0.029(5) 0.039(6) 0.035(5) 0.010(4) -0.012(4) -0.014(4) C2 0.043(6) 0.050(7) 0.029(5) 0.005(5) -0.012(4) -0.014(5) C3 0.056(7) 0.045(6) 0.028(5) -0.011(4) -0.001(5) -0.027(5) C4 0.030(5) 0.032(5) 0.039(5) -0.019(4) 0.001(4) -0.017(4) C5 0.041(6) 0.057(7) 0.020(5) 0.003(4) -0.002(4) -0.030(5) C6 0.027(5) 0.040(6) 0.042(6) 0.000(4) 0.009(4) -0.021(5) Cu1 0.0175(5) 0.0169(5) 0.0209(5) -0.0031(4) -0.0031(4) -0.0062(4) Cu2 0.0194(5) 0.0173(5) 0.0208(5) -0.0052(4) 0.0009(4) -0.0098(4) Cu3 0.0162(5) 0.0197(5) 0.0200(5) -0.0005(4) -0.0004(4) -0.0107(4) K1 0.0169(9) 0.0166(9) 0.0559(13) -0.0047(8) -0.0019(8) -0.0039(8) K2 0.0256(10) 0.0191(10) 0.0707(15) -0.0117(9) -0.0021(10) -0.0128(9) K3 0.0160(10) 0.0282(12) 0.141(3) -0.0198(14) 0.0018(13) -0.0128(10) K4 0.0509(13) 0.0280(10) 0.0175(9) -0.0006(8) 0.0065(8) -0.0148(10) N1 0.032(4) 0.029(4) 0.030(4) 0.001(3) -0.009(3) -0.019(4) N2 0.031(4) 0.045(5) 0.027(4) 0.007(4) 0.000(3) -0.001(4) N3 0.071(6) 0.033(5) 0.029(4) -0.005(3) -0.005(4) -0.030(5) N4 0.019(4) 0.030(4) 0.033(4) -0.009(3) 0.005(3) -0.012(3) N5 0.040(5) 0.071(6) 0.027(4) -0.008(4) 0.008(4) -0.041(5) N6 0.028(4) 0.022(4) 0.031(4) -0.001(3) 0.001(3) -0.013(3) Nb1 0.0095(3) 0.0094(3) 0.0177(3) -0.0019(2) -0.0010(2) -0.0054(3) Nb2 0.0095(3) 0.0089(3) 0.0169(3) -0.0027(2) 0.0008(2) -0.0045(3) Nb3 0.0134(3) 0.0148(3) 0.0126(3) -0.0036(3) 0.0001(2) -0.0081(3) Nb4 0.0083(3) 0.0109(3) 0.0155(3) -0.0026(2) -0.0006(2) -0.0043(3) Nb5 0.0110(3) 0.0136(3) 0.0131(3) -0.0016(2) 0.0012(2) -0.0071(3) Nb6 0.0110(3) 0.0143(3) 0.0136(3) 0.0008(3) -0.0012(2) -0.0047(3) Nb7 0.0094(3) 0.0084(3) 0.0194(3) -0.0017(3) 0.0001(2) -0.0039(3) Nb8 0.0074(3) 0.0087(3) 0.0160(3) -0.0020(2) -0.0001(2) -0.0037(3) Nb9 0.0092(3) 0.0100(3) 0.0156(3) -0.0025(2) -0.0004(2) -0.0057(3) O1 0.058(5) 0.084(5) 0.019(3) 0.004(3) -0.006(3) -0.059(4) O1W 0.093(7) 0.051(5) 0.061(5) -0.007(4) -0.002(5) -0.047(5) O2W 0.038(4) 0.035(4) 0.060(5) -0.025(3) 0.016(3) -0.025(3) O3W 0.024(3) 0.049(4) 0.056(4) 0.016(3) -0.005(3) -0.020(3) O4W 0.029(3) 0.027(3) 0.035(4) -0.009(3) -0.004(3) -0.010(3) O5W 0.026(3) 0.024(3) 0.037(4) -0.007(3) 0.006(3) -0.012(3) O6W 0.022(3) 0.023(3) 0.036(3) 0.001(3) -0.002(3) -0.009(3) O7W 0.049(4) 0.067(5) 0.052(5) -0.012(4) 0.007(4) -0.042(4) O8W 0.040(4) 0.047(4) 0.053(5) 0.005(4) -0.012(3) -0.014(4) O9W 0.069(5) 0.038(4) 0.049(5) -0.015(3) -0.005(4) -0.021(4) O2 0.022(3) 0.016(3) 0.082(5) 0.009(3) -0.021(3) -0.008(3) O3 0.020(3) 0.026(4) 0.096(6) -0.014(4) 0.013(3) -0.015(3) O4 0.031(4) 0.058(5) 0.018(3) -0.003(3) -0.002(3) -0.002(3) O5 0.026(3) 0.030(4) 0.089(6) -0.037(4) -0.002(3) -0.011(3) O6 0.021(3) 0.024(3) 0.019(3) 0.001(2) -0.003(2) -0.007(3) O7 0.088(6) 0.028(4) 0.018(3) -0.004(3) 0.003(3) -0.025(4) O8 0.010(3) 0.013(3) 0.023(3) -0.002(2) -0.002(2) -0.002(2) O9 0.019(3) 0.014(3) 0.024(3) -0.004(2) 0.000(2) -0.007(2) O10 0.016(3) 0.015(3) 0.026(3) -0.003(2) 0.002(2) -0.007(2) O10W 0.037(4) 0.049(4) 0.044(4) -0.023(3) 0.015(3) -0.032(3) O11W 0.034(4) 0.019(3) 0.050(4) -0.006(3) -0.016(3) -0.006(3) O12W 0.024(3) 0.034(4) 0.058(5) 0.014(3) -0.004(3) -0.014(3) O13W 0.025(3) 0.056(4) 0.025(3) 0.001(3) -0.005(3) -0.022(3) O14W 0.060(6) 0.051(5) 0.088(7) 0.010(5) 0.027(5) 0.008(5) O15W 0.028(3) 0.022(3) 0.043(4) -0.007(3) -0.007(3) -0.008(3) O16W 0.006(6) 0.084(11) 0.041(8) 0.051(7) -0.008(5) -0.013(6) O11 0.013(3) 0.018(3) 0.022(3) -0.004(2) -0.001(2) -0.005(2) O12 0.014(3) 0.015(3) 0.026(3) -0.002(2) -0.005(2) -0.009(2) O13 0.024(3) 0.029(3) 0.018(3) -0.008(2) 0.003(2) -0.015(3) O14 0.012(3) 0.018(3) 0.018(3) -0.001(2) -0.001(2) -0.008(2) O15 0.017(3) 0.013(3) 0.021(3) -0.001(2) -0.001(2) -0.010(2) O16 0.013(3) 0.016(3) 0.021(3) -0.002(2) -0.002(2) -0.007(2) O17 0.019(3) 0.019(3) 0.021(3) -0.001(2) -0.002(2) -0.012(2) O18 0.017(3) 0.017(3) 0.017(3) -0.005(2) 0.001(2) -0.011(2) O19 0.009(2) 0.008(2) 0.016(3) -0.0038(19) 0.0003(19) -0.004(2) O20 0.016(3) 0.012(3) 0.021(3) -0.001(2) -0.003(2) -0.007(2) O21 0.018(3) 0.017(3) 0.017(3) -0.003(2) 0.001(2) -0.008(2) O22 0.009(2) 0.011(2) 0.013(2) -0.0013(19) 0.0014(19) -0.007(2) O23 0.013(3) 0.016(3) 0.017(3) -0.002(2) -0.002(2) -0.007(2) O24 0.019(3) 0.018(3) 0.020(3) -0.003(2) 0.005(2) -0.012(2) O25 0.015(3) 0.018(3) 0.018(3) -0.001(2) 0.001(2) -0.006(2) O26 0.011(2) 0.012(3) 0.021(3) -0.003(2) 0.001(2) -0.005(2) O27 0.010(2) 0.016(3) 0.018(3) -0.004(2) 0.001(2) -0.003(2) O28 0.018(3) 0.013(3) 0.020(3) -0.003(2) -0.001(2) -0.009(2) O29 0.010(2) 0.010(2) 0.024(3) -0.002(2) -0.001(2) -0.005(2) O30 0.013(3) 0.021(3) 0.019(3) -0.004(2) -0.001(2) -0.011(2) O31 0.009(2) 0.010(2) 0.019(3) -0.004(2) -0.003(2) -0.004(2) O32 0.014(3) 0.012(3) 0.018(3) -0.004(2) -0.001(2) -0.007(2) O33 0.012(3) 0.016(3) 0.019(3) -0.005(2) 0.002(2) -0.008(2) O34 0.008(2) 0.012(3) 0.022(3) 0.001(2) 0.000(2) -0.006(2) O35 0.009(2) 0.012(2) 0.015(3) -0.0038(19) 0.0015(19) -0.006(2) O36 0.010(2) 0.018(3) 0.019(3) -0.002(2) -0.001(2) -0.007(2) O38 0.014(3) 0.015(3) 0.019(3) -0.004(2) 0.000(2) -0.008(2) O39 0.014(3) 0.014(3) 0.018(3) -0.001(2) -0.001(2) -0.006(2) O40 0.012(3) 0.016(3) 0.014(3) -0.001(2) 0.000(2) -0.007(2) Te1 0.0079(2) 0.0089(2) 0.0121(2) -0.00181(17) 0.00005(17) -0.00459(18) V1 0.0174(7) 0.0135(6) 0.0186(7) -0.0028(5) 0.0059(5) -0.0082(6) V2 0.0136(6) 0.0193(7) 0.0210(7) -0.0093(5) -0.0014(5) -0.0057(6) V3 0.0172(7) 0.0178(7) 0.0188(7) 0.0043(5) -0.0063(5) -0.0116(6) Na1 0.0299(19) 0.0294(19) 0.0285(18) -0.0038(14) -0.0010(14) -0.0149(16) Na2 0.0154(15) 0.0163(15) 0.0276(17) -0.0042(13) -0.0021(12) -0.0075(13) Na3 0.033(3) 0.049(3) 0.032(3) -0.006(2) -0.001(2) -0.024(3) K5 0.0589(17) 0.0638(18) 0.076(2) -0.0127(15) -0.0015(14) -0.0291(15) O20W 0.056(10) 0.078(11) 0.045(9) 0.012(8) -0.024(7) -0.042(9) O16B 0.066(9) 0.083(10) 0.034(7) -0.040(7) 0.026(7) -0.064(9) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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 _geom_angle_publ_flag H1A C1 H1B 108.4 . . ? C2 C1 H1A 110.1 . . ? C2 C1 H1B 110.1 . . ? N1 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? N1 C1 C2 108.0(8) . . ? C1 C2 H2A 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? N2 C2 C1 107.2(8) . . ? N2 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? H3A C3 H3B 108.4 . . ? C4 C3 H3A 110.0 . . ? C4 C3 H3B 110.0 . . ? N3 C3 H3A 110.0 . . ? N3 C3 H3B 110.0 . . ? N3 C3 C4 108.2(8) . . ? C3 C4 H4A 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N4 C4 C3 108.4(7) . . ? N4 C4 H4A 110.0 . . ? N4 C4 H4B 110.0 . . ? H5A C5 H5B 108.5 . . ? C6 C5 H5A 110.2 . . ? C6 C5 H5B 110.2 . . ? N5 C5 H5A 110.2 . . ? N5 C5 H5B 110.2 . . ? N5 C5 C6 107.4(7) . . ? C5 C6 H6A 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N6 C6 C5 108.5(7) . . ? N6 C6 H6A 110.0 . . ? N6 C6 H6B 110.0 . . ? N1 Cu1 K3 70.0(2) . . ? N1 Cu1 Nb1 133.2(2) . . ? N1 Cu1 O18 89.6(2) . . ? N2 Cu1 K3 143.1(3) . . ? N2 Cu1 N1 85.9(3) . . ? N2 Cu1 Nb1 138.8(2) . . ? N2 Cu1 O18 102.0(3) . . ? N2 Cu1 O20 98.1(3) . . ? N2 Cu1 O31 178.4(3) . . ? Nb1 Cu1 K3 64.53(5) . . ? O18 Cu1 K3 105.08(13) . . ? O18 Cu1 Nb1 92.08(13) . . ? O20 Cu1 K3 105.74(16) . . ? O20 Cu1 N1 175.7(3) . . ? O20 Cu1 Nb1 42.50(15) . . ? O20 Cu1 O18 91.21(19) . . ? O20 Cu1 O31 80.8(2) . . ? O31 Cu1 K3 38.49(14) . . ? O31 Cu1 N1 95.2(2) . . ? O31 Cu1 Nb1 40.50(13) . . ? O31 Cu1 O18 76.77(18) . . ? N3 Cu2 K1 141.6(3) . . ? N3 Cu2 N4 85.8(3) . . ? N3 Cu2 Nb4 139.3(2) . . ? N3 Cu2 O16 101.6(3) . . ? N3 Cu2 O28 98.2(3) . . ? N3 Cu2 O33 178.4(3) . . ? N4 Cu2 K1 68.8(2) . . ? N4 Cu2 Nb4 132.9(2) . . ? N4 Cu2 O16 89.5(2) . . ? Nb4 Cu2 K1 65.66(5) . . ? O16 Cu2 K1 106.32(13) . . ? O16 Cu2 Nb4 92.12(13) . . ? O28 Cu2 K1 106.99(15) . . ? O28 Cu2 N4 175.8(3) . . ? O28 Cu2 Nb4 42.87(15) . . ? O28 Cu2 O16 91.24(19) . . ? O28 Cu2 O33 81.0(2) . . ? O33 Cu2 K1 40.03(14) . . ? O33 Cu2 N4 95.1(2) . . ? O33 Cu2 Nb4 40.19(14) . . ? O33 Cu2 O16 77.10(19) . . ? N5 Cu3 K2 142.5(3) . 1_565 ? N5 Cu3 N6 85.8(3) . . ? N5 Cu3 Nb2 139.4(2) . . ? N5 Cu3 O23 100.6(3) . . ? N5 Cu3 O34 177.5(3) . . ? N6 Cu3 K2 69.2(2) . 1_565 ? N6 Cu3 Nb2 133.0(2) . . ? N6 Cu3 O23 90.1(2) . . ? Nb2 Cu3 K2 65.32(5) . 1_565 ? O14 Cu3 K2 106.43(15) . 1_565 ? O14 Cu3 N5 98.0(3) . . ? O14 Cu3 N6 175.6(3) . . ? O14 Cu3 Nb2 42.80(15) . . ? O14 Cu3 O23 91.18(19) . . ? O14 Cu3 O34 81.3(2) . . ? O23 Cu3 K2 106.71(13) . 1_565 ? O23 Cu3 Nb2 91.82(13) . . ? O34 Cu3 K2 39.80(14) . 1_565 ? O34 Cu3 N6 95.0(2) . . ? O34 Cu3 Nb2 40.45(14) . . ? O34 Cu3 O23 77.00(19) . . ? Nb2 K1 Na2 63.73(6) 1_645 1_565 ? Nb2 K1 K5 126.37(7) 1_645 . ? Nb8 K1 Nb2 64.52(3) 1_645 1_645 ? Nb8 K1 Na2 126.53(7) 1_645 1_565 ? Nb8 K1 K5 63.35(6) 1_645 . ? O2 K1 Nb2 68.05(11) 1_645 1_645 ? O2 K1 Nb8 67.12(11) 1_645 1_645 ? O2 K1 O14W 128.08(18) 1_645 1_655 ? O2 K1 Na2 104.32(13) 1_645 1_565 ? O2 K1 K5 101.85(13) 1_645 . ? O8 K1 Nb2 92.70(11) 1_645 1_645 ? O8 K1 Nb8 29.07(10) 1_645 1_645 ? O8 K1 O2 69.69(15) 1_645 1_645 ? O8 K1 O9 119.62(15) 1_645 1_645 ? O8 K1 O12W 139.07(17) 1_645 1_565 ? O8 K1 O14W 86.7(2) 1_645 1_655 ? O8 K1 Na2 155.60(12) 1_645 1_565 ? O8 K1 K5 39.27(11) 1_645 . ? O9 K1 Nb2 29.10(10) 1_645 1_645 ? O9 K1 Nb8 92.90(11) 1_645 1_645 ? O9 K1 O2 71.91(16) 1_645 1_645 ? O9 K1 O12W 72.75(16) 1_645 1_565 ? O9 K1 O14W 82.2(2) 1_645 1_655 ? O9 K1 Na2 39.39(11) 1_645 1_565 ? O9 K1 K5 155.46(12) 1_645 . ? O12W K1 Nb2 85.42(13) 1_565 1_645 ? O12W K1 Nb8 124.31(14) 1_565 1_645 ? O12W K1 O2 143.34(18) 1_565 1_645 ? O12W K1 O14W 54.9(2) 1_565 1_655 ? O12W K1 Na2 39.39(13) 1_565 1_565 ? O12W K1 K5 114.39(14) 1_565 . ? O14W K1 Nb2 67.72(16) 1_655 1_645 ? O14W K1 Nb8 70.23(18) 1_655 1_645 ? O14W K1 Na2 78.8(2) 1_655 1_565 ? O14W K1 K5 83.7(2) 1_655 . ? O15W K1 Nb2 125.33(14) 1_655 1_645 ? O15W K1 Nb8 85.71(13) 1_655 1_645 ? O15W K1 O2 141.23(18) 1_655 1_645 ? O15W K1 O8 73.24(16) 1_655 1_645 ? O15W K1 O9 139.41(18) 1_655 1_645 ? O15W K1 O12W 74.80(18) 1_655 1_565 ? O15W K1 O14W 59.1(2) 1_655 1_655 ? O15W K1 Na2 114.18(15) 1_655 1_565 ? O15W K1 K5 39.60(13) 1_655 . ? O26 K1 Nb2 31.92(10) 1_645 1_645 ? O26 K1 Nb8 32.80(11) 1_645 1_645 ? O26 K1 O2 65.82(15) 1_645 1_645 ? O26 K1 O8 61.59(15) 1_645 1_645 ? O26 K1 O9 60.82(15) 1_645 1_645 ? O26 K1 O12W 104.30(17) 1_645 1_565 ? O26 K1 O14W 62.27(18) 1_645 1_655 ? O26 K1 O15W 105.58(17) 1_645 1_655 ? O26 K1 Na2 94.17(13) 1_645 1_565 ? O26 K1 K5 94.79(13) 1_645 . ? O33 K1 Nb2 143.74(12) . 1_645 ? O33 K1 Nb8 141.15(13) . 1_645 ? O33 K1 O2 96.42(16) . 1_645 ? O33 K1 O8 113.04(16) . 1_645 ? O33 K1 O9 115.99(16) . 1_645 ? O33 K1 O12W 90.37(17) . 1_565 ? O33 K1 O14W 135.50(19) . 1_655 ? O33 K1 O15W 87.71(17) . 1_655 ? O33 K1 O26 162.23(17) . 1_645 ? O33 K1 Na2 90.90(13) . 1_565 ? O33 K1 K5 88.01(13) . . ? K5 K1 Na2 153.77(9) . 1_565 ? Nb1 K2 Na2 63.58(6) . 1_465 ? Nb1 K2 K5 126.93(7) . . ? Nb7 K2 Nb1 64.45(4) . . ? Nb7 K2 Na2 126.22(7) . 1_465 ? Nb7 K2 K5 63.62(6) . . ? O1W K2 Nb1 67.99(15) . . ? O1W K2 Nb7 69.75(15) . . ? O1W K2 Na2 79.05(17) . 1_465 ? O1W K2 K5 84.64(18) . . ? O2W K2 Nb1 126.41(14) . . ? O2W K2 Nb7 86.25(14) . . ? O2W K2 O1W 59.8(2) . . ? O2W K2 O5 141.47(18) . . ? O2W K2 O10 74.10(17) . . ? O2W K2 O11W 75.41(18) . 1_465 ? O2W K2 O12 140.69(18) . . ? O2W K2 Na2 114.40(15) . 1_465 ? O2W K2 K5 40.41(14) . . ? O5 K2 Nb1 67.02(11) . . ? O5 K2 Nb7 66.82(11) . . ? O5 K2 O1W 127.16(18) . . ? O5 K2 Na2 103.86(13) . 1_465 ? O5 K2 K5 101.30(13) . . ? O10 K2 Nb1 92.50(11) . . ? O10 K2 Nb7 29.18(10) . . ? O10 K2 O1W 86.8(2) . . ? O10 K2 O5 69.05(16) . . ? O10 K2 O11W 140.32(18) . 1_465 ? O10 K2 O12 119.12(16) . . ? O10 K2 Na2 155.39(13) . 1_465 ? O10 K2 K5 39.50(12) . . ? O11W K2 Nb1 85.61(13) 1_465 . ? O11W K2 Nb7 124.66(14) 1_465 . ? O11W K2 O1W 55.8(2) 1_465 . ? O11W K2 O5 142.50(17) 1_465 . ? O11W K2 O12 73.04(16) 1_465 . ? O11W K2 Na2 39.00(13) 1_465 1_465 ? O11W K2 K5 115.82(15) 1_465 . ? O12 K2 Nb1 29.12(10) . . ? O12 K2 Nb7 92.78(11) . . ? O12 K2 O1W 83.01(19) . . ? O12 K2 O5 70.70(16) . . ? O12 K2 Na2 39.57(11) . 1_465 ? O12 K2 K5 156.03(12) . . ? O29 K2 Nb1 31.69(10) . . ? O29 K2 Nb7 32.94(10) . . ? O29 K2 O1W 62.19(18) . . ? O29 K2 O2W 106.63(17) . . ? O29 K2 O5 64.98(15) . . ? O29 K2 O10 61.72(15) . . ? O29 K2 O11W 104.51(17) . 1_465 ? O29 K2 O12 60.58(15) . . ? O29 K2 Na2 93.76(12) . 1_465 ? O29 K2 K5 95.47(12) . . ? O34 K2 Nb1 143.44(13) 1_545 . ? O34 K2 Nb7 140.25(13) 1_545 . ? O34 K2 O1W 136.86(19) 1_545 . ? O34 K2 O2W 87.47(17) 1_545 . ? O34 K2 O5 95.97(16) 1_545 . ? O34 K2 O10 112.01(16) 1_545 . ? O34 K2 O11W 91.27(17) 1_545 1_465 ? O34 K2 O12 115.88(16) 1_545 . ? O34 K2 O29 160.93(18) 1_545 . ? O34 K2 Na2 91.88(12) 1_545 1_465 ? O34 K2 K5 86.98(12) 1_545 . ? K5 K2 Na2 154.80(10) . 1_465 ? Nb4 K3 Na2 63.07(6) 1_455 1_465 ? Nb4 K3 K5 126.90(8) 1_455 1_465 ? Nb9 K3 Nb4 64.65(5) 1_455 1_455 ? Nb9 K3 Na2 126.24(7) 1_455 1_465 ? Nb9 K3 K5 63.22(6) 1_455 1_465 ? O3W K3 Nb4 127.30(15) 1_465 1_455 ? O3W K3 Nb9 85.83(14) 1_465 1_455 ? O3W K3 O3 140.05(19) 1_465 1_455 ? O3W K3 O10W 77.9(2) 1_465 1_465 ? O3W K3 O13W 59.26(18) 1_465 1_565 ? O3W K3 O11 142.6(2) 1_465 1_455 ? O3W K3 O17 73.46(17) 1_465 1_455 ? O3W K3 Na2 116.91(17) 1_465 1_465 ? O3W K3 K5 39.99(14) 1_465 1_465 ? O3 K3 Nb4 67.04(12) 1_455 1_455 ? O3 K3 Nb9 66.56(12) 1_455 1_455 ? O3 K3 Na2 102.84(13) 1_455 1_465 ? O3 K3 K5 100.24(14) 1_455 1_465 ? O10W K3 Nb4 85.49(13) 1_465 1_455 ? O10W K3 Nb9 125.98(15) 1_465 1_455 ? O10W K3 O3 141.59(18) 1_465 1_455 ? O10W K3 O13W 56.58(17) 1_465 1_565 ? O10W K3 O11 72.73(16) 1_465 1_455 ? O10W K3 Na2 38.98(13) 1_465 1_465 ? O10W K3 K5 117.93(16) 1_465 1_465 ? O13W K3 Nb4 69.79(12) 1_565 1_455 ? O13W K3 Nb9 70.75(12) 1_565 1_455 ? O13W K3 O3 128.67(16) 1_565 1_455 ? O13W K3 Na2 80.49(14) 1_565 1_465 ? O13W K3 K5 84.33(14) 1_565 1_465 ? O11 K3 Nb4 29.20(10) 1_455 1_455 ? O11 K3 Nb9 92.91(11) 1_455 1_455 ? O11 K3 O3 70.33(16) 1_455 1_455 ? O11 K3 O13W 85.02(17) 1_455 1_565 ? O11 K3 Na2 38.99(11) 1_455 1_465 ? O11 K3 K5 155.97(13) 1_455 1_465 ? O17 K3 Nb4 92.70(12) 1_455 1_455 ? O17 K3 Nb9 29.30(10) 1_455 1_455 ? O17 K3 O3 68.43(16) 1_455 1_455 ? O17 K3 O10W 142.34(19) 1_455 1_465 ? O17 K3 O13W 87.50(17) 1_455 1_565 ? O17 K3 O11 119.02(16) 1_455 1_455 ? O17 K3 Na2 155.43(13) 1_455 1_465 ? O17 K3 K5 39.03(11) 1_455 1_465 ? O31 K3 Nb4 141.13(14) . 1_455 ? O31 K3 Nb9 139.16(14) . 1_455 ? O31 K3 O3W 89.72(17) . 1_465 ? O31 K3 O3 93.08(17) . 1_455 ? O31 K3 O10W 92.36(17) . 1_465 ? O31 K3 O13W 138.26(18) . 1_565 ? O31 K3 O11 113.88(16) . 1_455 ? O31 K3 O17 111.25(17) . 1_455 ? O31 K3 O32 157.8(2) . 1_455 ? O31 K3 Na2 91.69(13) . 1_465 ? O31 K3 K5 88.11(12) . 1_465 ? O32 K3 Nb4 31.84(10) 1_455 1_455 ? O32 K3 Nb9 32.99(11) 1_455 1_455 ? O32 K3 O3W 106.87(18) 1_455 1_465 ? O32 K3 O3 64.77(16) 1_455 1_455 ? O32 K3 O10W 105.21(18) 1_455 1_465 ? O32 K3 O13W 63.89(16) 1_455 1_565 ? O32 K3 O11 60.74(15) 1_455 1_455 ? O32 K3 O17 61.82(15) 1_455 1_455 ? O32 K3 Na2 93.61(13) 1_455 1_465 ? O32 K3 K5 95.23(13) 1_455 1_465 ? K5 K3 Na2 156.89(12) 1_465 1_465 ? Nb5 K4 Nb3 61.27(4) 1_545 1_545 ? Nb5 K4 Nb3 114.19(6) 2_666 1_545 ? Nb5 K4 Nb5 107.89(6) 1_545 2_666 ? Nb5 K4 Nb6 112.84(7) 1_545 2_666 ? Nb5 K4 Nb6 61.21(4) 2_666 2_666 ? Nb6 K4 Nb3 171.95(6) 2_666 1_545 ? O1W K4 Nb3 116.64(17) 2_666 1_545 ? O1W K4 Nb5 177.36(19) 2_666 1_545 ? O1W K4 Nb5 71.23(16) 2_666 2_666 ? O1W K4 Nb6 69.07(16) 2_666 2_666 ? O1W K4 O14W 110.7(3) 2_666 . ? O1W K4 O13 89.3(2) 2_666 1_545 ? O6 K4 Nb3 152.98(12) 2_666 1_545 ? O6 K4 Nb5 98.59(12) 2_666 1_545 ? O6 K4 Nb5 88.17(11) 2_666 2_666 ? O6 K4 Nb6 28.09(10) 2_666 2_666 ? O6 K4 O1W 83.9(2) 2_666 2_666 ? O6 K4 O14W 87.8(2) 2_666 . ? O6 K4 O13 166.13(16) 2_666 1_545 ? O14W K4 Nb3 69.09(17) . 1_545 ? O14W K4 Nb5 70.4(2) . 1_545 ? O14W K4 Nb5 175.3(2) . 2_666 ? O14W K4 Nb6 115.10(18) . 2_666 ? O13 K4 Nb3 28.04(10) 1_545 1_545 ? O13 K4 Nb5 101.09(12) 1_545 2_666 ? O13 K4 Nb5 88.46(11) 1_545 1_545 ? O13 K4 Nb6 155.12(12) 1_545 2_666 ? O13 K4 O14W 83.3(2) 1_545 . ? O25 K4 Nb3 86.30(12) 2_666 1_545 ? O25 K4 Nb3 88.68(12) 1_545 1_545 ? O25 K4 Nb5 90.09(12) 1_545 2_666 ? O25 K4 Nb5 89.73(12) 2_666 1_545 ? O25 K4 Nb5 28.53(10) 2_666 2_666 ? O25 K4 Nb5 28.57(10) 1_545 1_545 ? O25 K4 Nb6 84.80(12) 1_545 2_666 ? O25 K4 Nb6 88.24(12) 2_666 2_666 ? O25 K4 O1W 88.5(2) 2_666 2_666 ? O25 K4 O1W 152.84(19) 1_545 2_666 ? O25 K4 O6 75.71(16) 1_545 2_666 ? O25 K4 O6 112.99(16) 2_666 2_666 ? O25 K4 O14W 153.6(2) 2_666 . ? O25 K4 O14W 86.6(2) 1_545 . ? O25 K4 O13 114.20(16) 1_545 1_545 ? O25 K4 O13 78.78(16) 2_666 1_545 ? O25 K4 O25 83.24(17) 1_545 2_666 ? O39 K4 Nb3 146.39(13) 2_666 1_545 ? O39 K4 Nb5 32.50(10) 2_666 2_666 ? O39 K4 Nb5 121.20(13) 2_666 1_545 ? O39 K4 Nb6 30.27(10) 2_666 2_666 ? O39 K4 O1W 59.44(19) 2_666 2_666 ? O39 K4 O6 58.34(15) 2_666 2_666 ? O39 K4 O14W 144.5(2) 2_666 . ? O39 K4 O13 127.40(16) 2_666 1_545 ? O39 K4 O25 60.92(15) 2_666 2_666 ? O39 K4 O25 94.20(16) 2_666 1_545 ? O39 K4 O40 148.58(16) 2_666 1_545 ? O40 K4 Nb3 30.63(10) 1_545 1_545 ? O40 K4 Nb5 122.24(12) 1_545 2_666 ? O40 K4 Nb5 32.31(10) 1_545 1_545 ? O40 K4 Nb6 144.65(13) 1_545 2_666 ? O40 K4 O1W 146.0(2) 1_545 2_666 ? O40 K4 O6 124.56(16) 1_545 2_666 ? O40 K4 O14W 58.70(19) 1_545 . ? O40 K4 O13 58.67(14) 1_545 1_545 ? O40 K4 O25 95.20(16) 1_545 2_666 ? O40 K4 O25 60.84(15) 1_545 1_545 ? C1 N1 Cu1 106.0(5) . . ? C1 N1 H1C 110.5 . . ? C1 N1 H1D 110.5 . . ? Cu1 N1 H1C 110.5 . . ? Cu1 N1 H1D 110.5 . . ? H1C N1 H1D 108.7 . . ? C2 N2 Cu1 108.5(6) . . ? C2 N2 H2C 110.0 . . ? C2 N2 H2D 110.0 . . ? Cu1 N2 H2C 110.0 . . ? Cu1 N2 H2D 110.0 . . ? H2C N2 H2D 108.4 . . ? C3 N3 Cu2 108.8(6) . . ? C3 N3 H3C 109.9 . . ? C3 N3 H3D 109.9 . . ? Cu2 N3 H3C 109.9 . . ? Cu2 N3 H3D 109.9 . . ? H3C N3 H3D 108.3 . . ? C4 N4 Cu2 106.1(5) . . ? C4 N4 H4C 110.5 . . ? C4 N4 H4D 110.5 . . ? Cu2 N4 H4C 110.5 . . ? Cu2 N4 H4D 110.5 . . ? H4C N4 H4D 108.7 . . ? C5 N5 Cu3 109.3(6) . . ? C5 N5 H5C 109.8 . . ? C5 N5 H5D 109.8 . . ? Cu3 N5 H5C 109.8 . . ? Cu3 N5 H5D 109.8 . . ? H5C N5 H5D 108.3 . . ? C6 N6 Cu3 106.6(5) . . ? C6 N6 H6C 110.4 . . ? C6 N6 H6D 110.4 . . ? Cu3 N6 H6C 110.4 . . ? Cu3 N6 H6D 110.4 . . ? H6C N6 H6D 108.6 . . ? Cu1 Nb1 K2 126.19(5) . . ? Cu1 Nb1 K3 68.32(6) . . ? K2 Nb1 K3 118.81(5) . . ? O12 Nb1 Cu1 93.33(17) . . ? O12 Nb1 K2 54.56(17) . . ? O12 Nb1 K3 66.63(17) . . ? O12 Nb1 O15 101.4(2) . . ? O12 Nb1 O20 99.9(2) . . ? O12 Nb1 O22 172.5(2) . . ? O12 Nb1 O29 101.6(2) . . ? O12 Nb1 O31 100.3(2) . . ? O15 Nb1 Cu1 132.41(15) . . ? O15 Nb1 K2 98.42(15) . . ? O15 Nb1 K3 76.59(16) . . ? O15 Nb1 O20 157.9(2) . . ? O15 Nb1 O22 75.40(18) . . ? O15 Nb1 O29 96.8(2) . . ? O15 Nb1 O31 93.0(2) . . ? O20 Nb1 Cu1 39.52(14) . . ? O20 Nb1 K2 98.90(14) . . ? O20 Nb1 K3 106.59(15) . . ? O20 Nb1 O22 82.74(17) . . ? O22 Nb1 Cu1 84.20(12) . . ? O22 Nb1 K2 132.27(12) . . ? O22 Nb1 K3 105.87(12) . . ? O29 Nb1 Cu1 124.35(15) . . ? O29 Nb1 K2 47.53(15) . . ? O29 Nb1 K3 164.43(15) . . ? O29 Nb1 O20 84.9(2) . . ? O29 Nb1 O22 85.62(18) . . ? O29 Nb1 O31 153.7(2) . . ? O31 Nb1 Cu1 39.57(14) . . ? O31 Nb1 K2 153.97(14) . . ? O31 Nb1 K3 41.86(14) . . ? O31 Nb1 O20 77.08(19) . . ? O31 Nb1 O22 73.26(17) . . ? Cu3 Nb2 K1 124.68(5) . 1_465 ? Cu3 Nb2 K2 67.11(5) . 1_565 ? K1 Nb2 K2 118.11(5) 1_465 1_565 ? O9 Nb2 Cu3 93.39(17) . . ? O9 Nb2 K1 53.79(17) . 1_465 ? O9 Nb2 K2 65.87(17) . 1_565 ? O9 Nb2 O14 99.3(2) . . ? O9 Nb2 O19 173.0(2) . . ? O9 Nb2 O21 101.7(2) . . ? O9 Nb2 O26 101.4(2) . . ? O9 Nb2 O34 100.3(2) . . ? O14 Nb2 Cu3 39.15(13) . . ? O14 Nb2 K1 97.56(14) . 1_465 ? O14 Nb2 K2 104.68(14) . 1_565 ? O14 Nb2 O19 82.59(18) . . ? O19 Nb2 Cu3 83.84(12) . . ? O19 Nb2 K1 132.85(12) . 1_465 ? O19 Nb2 K2 107.12(12) . 1_565 ? O21 Nb2 Cu3 132.82(16) . . ? O21 Nb2 K1 99.61(16) . 1_465 ? O21 Nb2 K2 78.86(16) . 1_565 ? O21 Nb2 O14 158.1(2) . . ? O21 Nb2 O19 75.83(19) . . ? O21 Nb2 O26 97.4(2) . . ? O21 Nb2 O34 93.4(2) . . ? O26 Nb2 Cu3 123.21(15) . . ? O26 Nb2 K1 48.02(15) . 1_465 ? O26 Nb2 K2 165.22(15) . 1_565 ? O26 Nb2 O14 84.2(2) . . ? O26 Nb2 O19 85.49(18) . . ? O26 Nb2 O34 153.2(2) . . ? O34 Nb2 Cu3 39.63(14) . . ? O34 Nb2 K1 152.85(14) . 1_465 ? O34 Nb2 K2 41.53(14) . 1_565 ? O34 Nb2 O14 76.93(19) . . ? O34 Nb2 O19 73.43(18) . . ? O13 Nb3 K4 54.36(18) . 1_565 ? O13 Nb3 O19 169.1(2) . . ? O13 Nb3 O21 99.3(2) . . ? O13 Nb3 O30 100.9(2) . . ? O13 Nb3 O38 102.9(2) . . ? O13 Nb3 O40 101.4(2) . . ? O19 Nb3 K4 131.25(12) . 1_565 ? O21 Nb3 K4 94.53(15) . 1_565 ? O21 Nb3 O19 71.92(18) . . ? O30 Nb3 K4 155.02(15) . 1_565 ? O30 Nb3 O19 72.39(18) . . ? O30 Nb3 O21 85.2(2) . . ? O38 Nb3 K4 99.57(15) . 1_565 ? O38 Nb3 O19 85.90(18) . . ? O38 Nb3 O21 157.8(2) . . ? O38 Nb3 O30 89.0(2) . . ? O38 Nb3 O40 89.7(2) . . ? O40 Nb3 K4 47.05(15) . 1_565 ? O40 Nb3 O19 84.93(18) . . ? O40 Nb3 O21 87.4(2) . . ? O40 Nb3 O30 157.3(2) . . ? Cu2 Nb4 K1 66.79(4) . . ? Cu2 Nb4 K3 126.37(6) . 1_655 ? K3 Nb4 K1 118.85(5) 1_655 . ? O11 Nb4 Cu2 93.00(17) . . ? O11 Nb4 K1 66.10(17) . . ? O11 Nb4 K3 54.80(17) . 1_655 ? O11 Nb4 O28 99.4(2) . . ? O11 Nb4 O32 101.5(2) . . ? O11 Nb4 O33 100.1(2) . . ? O11 Nb4 O35 172.7(2) . . ? O11 Nb4 O36 101.5(2) . . ? O28 Nb4 Cu2 39.41(13) . . ? O28 Nb4 K1 104.77(14) . . ? O28 Nb4 K3 99.01(14) . 1_655 ? O28 Nb4 O35 82.28(18) . . ? O32 Nb4 Cu2 123.98(15) . . ? O32 Nb4 K1 165.16(15) . . ? O32 Nb4 K3 47.27(15) . 1_655 ? O32 Nb4 O28 84.7(2) . . ? O32 Nb4 O33 153.6(2) . . ? O32 Nb4 O35 85.76(18) . . ? O33 Nb4 Cu2 39.41(14) . . ? O33 Nb4 K1 41.24(14) . . ? O33 Nb4 K3 154.03(14) . 1_655 ? O33 Nb4 O28 76.88(19) . . ? O33 Nb4 O35 73.27(17) . . ? O35 Nb4 Cu2 83.76(11) . . ? O35 Nb4 K1 106.60(12) . . ? O35 Nb4 K3 132.14(12) . 1_655 ? O36 Nb4 Cu2 132.53(16) . . ? O36 Nb4 K1 78.35(16) . . ? O36 Nb4 K3 98.09(16) . 1_655 ? O36 Nb4 O28 158.2(2) . . ? O36 Nb4 O32 97.2(2) . . ? O36 Nb4 O33 93.3(2) . . ? O36 Nb4 O35 76.23(18) . . ? K4 Nb5 K4 72.11(6) 1_565 2_666 ? O15 Nb5 K4 149.61(15) . 1_565 ? O15 Nb5 K4 92.10(15) . 2_666 ? O15 Nb5 O22 72.44(18) . . ? O22 Nb5 K4 136.92(12) . 1_565 ? O22 Nb5 K4 134.04(12) . 2_666 ? O25 Nb5 K4 51.14(17) . 2_666 ? O25 Nb5 K4 50.17(18) . 1_565 ? O25 Nb5 O15 99.6(2) . . ? O25 Nb5 O22 169.7(2) . . ? O25 Nb5 O27 100.7(2) . . ? O25 Nb5 O39 100.7(2) . . ? O25 Nb5 O40 100.6(2) . . ? O27 Nb5 K4 95.98(15) . 1_565 ? O27 Nb5 K4 151.00(14) . 2_666 ? O27 Nb5 O15 85.5(2) . . ? O27 Nb5 O22 72.50(18) . . ? O39 Nb5 K4 49.85(15) . 2_666 ? O39 Nb5 K4 99.80(15) . 1_565 ? O39 Nb5 O15 88.3(2) . . ? O39 Nb5 O22 85.85(18) . . ? O39 Nb5 O27 158.3(2) . . ? O40 Nb5 K4 50.48(15) . 1_565 ? O40 Nb5 K4 101.52(15) . 2_666 ? O40 Nb5 O15 159.7(2) . . ? O40 Nb5 O22 87.32(18) . . ? O40 Nb5 O27 89.6(2) . . ? O40 Nb5 O39 89.1(2) . . ? O6 Nb6 K4 54.43(18) . 2_666 ? O6 Nb6 O24 100.1(2) . . ? O6 Nb6 O35 168.9(2) . . ? O6 Nb6 O36 99.8(2) . . ? O6 Nb6 O38 103.1(2) . . ? O6 Nb6 O39 101.2(2) . . ? O24 Nb6 K4 94.19(14) . 2_666 ? O24 Nb6 O35 71.65(18) . . ? O35 Nb6 K4 131.98(12) . 2_666 ? O36 Nb6 K4 153.84(15) . 2_666 ? O36 Nb6 O24 85.2(2) . . ? O36 Nb6 O35 72.58(18) . . ? O38 Nb6 K4 101.51(15) . 2_666 ? O38 Nb6 O24 156.7(2) . . ? O38 Nb6 O35 85.03(18) . . ? O38 Nb6 O36 88.1(2) . . ? O39 Nb6 K4 46.85(15) . 2_666 ? O39 Nb6 O24 88.4(2) . . ? O39 Nb6 O35 86.17(18) . . ? O39 Nb6 O36 158.7(2) . . ? O39 Nb6 O38 89.9(2) . . ? K2 Nb7 K1 118.47(5) . . ? K2 Nb7 K5 60.90(6) . . ? O10 Nb7 K1 68.66(17) . . ? O10 Nb7 K2 52.95(17) . . ? O10 Nb7 O16 100.6(2) . . ? O10 Nb7 O24 102.6(2) . . ? O10 Nb7 O29 100.7(2) . . ? O10 Nb7 O33 99.6(2) . . ? O10 Nb7 O35 172.6(2) . . ? O10 Nb7 K5 25.09(18) . . ? O16 Nb7 K1 109.26(14) . . ? O16 Nb7 K2 99.48(14) . . ? O16 Nb7 O35 81.33(18) . . ? O16 Nb7 K5 124.84(15) . . ? O24 Nb7 K1 78.60(16) . . ? O24 Nb7 K2 95.34(16) . . ? O24 Nb7 O16 156.7(2) . . ? O24 Nb7 O29 94.0(2) . . ? O24 Nb7 O33 93.5(2) . . ? O24 Nb7 O35 75.46(19) . . ? O24 Nb7 K5 78.15(16) . . ? O29 Nb7 K1 164.96(15) . . ? O29 Nb7 K2 48.60(14) . . ? O29 Nb7 O16 82.6(2) . . ? O29 Nb7 O33 156.2(2) . . ? O29 Nb7 O35 86.61(18) . . ? O29 Nb7 K5 107.95(15) . . ? O33 Nb7 K1 38.64(14) . . ? O33 Nb7 K2 152.45(14) . . ? O33 Nb7 O16 81.6(2) . . ? O33 Nb7 O35 73.47(17) . . ? O33 Nb7 K5 95.70(15) . . ? O35 Nb7 K1 103.91(12) . . ? O35 Nb7 K2 134.05(12) . . ? O35 Nb7 K5 150.66(12) . . ? K5 Nb7 K1 57.91(5) . . ? K1 Nb8 K3 118.81(5) 1_465 . ? K1 Nb8 K5 60.90(6) 1_465 1_465 ? O8 Nb8 K1 53.33(17) . 1_465 ? O8 Nb8 K3 68.97(17) . . ? O8 Nb8 O18 100.7(2) . . ? O8 Nb8 O22 172.3(2) . . ? O8 Nb8 O26 101.3(2) . . ? O8 Nb8 O27 102.1(2) . . ? O8 Nb8 O31 99.3(2) . . ? O8 Nb8 K5 24.91(17) . 1_465 ? O18 Nb8 K1 98.57(14) . 1_465 ? O18 Nb8 K3 111.24(14) . . ? O18 Nb8 O22 81.65(18) . . ? O18 Nb8 K5 124.97(15) . 1_465 ? O22 Nb8 K1 133.90(12) . 1_465 ? O22 Nb8 K3 103.29(12) . . ? O22 Nb8 K5 150.57(12) . 1_465 ? O26 Nb8 K1 48.53(14) . 1_465 ? O26 Nb8 K3 163.73(15) . . ? O26 Nb8 O18 82.9(2) . . ? O26 Nb8 O22 86.30(18) . . ? O26 Nb8 O31 156.36(19) . . ? O26 Nb8 K5 107.51(15) . 1_465 ? O27 Nb8 K1 95.85(15) . 1_465 ? O27 Nb8 K3 76.46(16) . . ? O27 Nb8 O18 157.1(2) . . ? O27 Nb8 O22 75.57(18) . . ? O27 Nb8 O26 93.6(2) . . ? O27 Nb8 O31 93.4(2) . . ? O27 Nb8 K5 77.68(15) . 1_465 ? O31 Nb8 K1 152.38(14) . 1_465 ? O31 Nb8 K3 39.22(14) . . ? O31 Nb8 O18 81.92(19) . . ? O31 Nb8 O22 73.66(17) . . ? O31 Nb8 K5 96.04(14) . 1_465 ? K5 Nb8 K3 58.14(6) 1_465 . ? K3 Nb9 K2 118.98(5) 1_655 1_565 ? K3 Nb9 K5 61.19(6) 1_655 1_565 ? O17 Nb9 K2 69.00(17) . 1_565 ? O17 Nb9 K3 53.48(17) . 1_655 ? O17 Nb9 O19 172.4(2) . . ? O17 Nb9 O23 100.7(2) . . ? O17 Nb9 O30 102.5(2) . . ? O17 Nb9 O32 100.9(2) . . ? O17 Nb9 O34 99.1(2) . . ? O17 Nb9 K5 25.09(17) . 1_565 ? O19 Nb9 K2 103.43(11) . 1_565 ? O19 Nb9 K3 133.82(12) . 1_655 ? O19 Nb9 K5 150.92(12) . 1_565 ? O23 Nb9 K2 109.43(14) . 1_565 ? O23 Nb9 K3 100.10(15) . 1_655 ? O23 Nb9 O19 80.81(18) . . ? O23 Nb9 K5 124.86(14) . 1_565 ? O30 Nb9 K2 77.99(16) . 1_565 ? O30 Nb9 K3 94.81(16) . 1_655 ? O30 Nb9 O19 75.99(18) . . ? O30 Nb9 O23 156.7(2) . . ? O30 Nb9 O32 94.2(2) . . ? O30 Nb9 O34 93.2(2) . . ? O30 Nb9 K5 78.05(16) . 1_565 ? O32 Nb9 K2 165.07(14) . 1_565 ? O32 Nb9 K3 48.37(14) . 1_655 ? O32 Nb9 O19 86.67(18) . . ? O32 Nb9 O23 82.8(2) . . ? O32 Nb9 O34 156.6(2) . . ? O32 Nb9 K5 108.18(15) . 1_565 ? O34 Nb9 K2 37.99(14) . 1_565 ? O34 Nb9 K3 152.49(14) . 1_655 ? O34 Nb9 O19 73.68(18) . . ? O34 Nb9 O23 81.8(2) . . ? O34 Nb9 K5 95.02(15) . 1_565 ? K5 Nb9 K2 58.02(6) 1_565 1_565 ? K4 O1W K2 172.4(3) 2_666 . ? K5 O2W K2 90.5(2) . . ? K5 O3W K3 90.4(2) . 1_645 ? V3 O2 K1 115.9(3) . 1_465 ? V1 O3 K3 112.2(3) . 1_655 ? V2 O5 K2 114.0(3) . . ? Nb6 O6 K4 97.5(2) . 2_666 ? Nb8 O8 K1 97.6(2) . 1_465 ? Nb8 O8 K5 137.1(3) . 1_465 ? K5 O8 K1 90.77(17) 1_465 1_465 ? Nb2 O9 K1 97.1(2) . 1_465 ? Nb2 O9 Na2 138.4(3) . 1_475 ? Na2 O9 K1 90.13(18) 1_475 1_465 ? Nb7 O10 K2 97.9(2) . . ? Nb7 O10 K5 136.9(3) . . ? K5 O10 K2 91.07(18) . . ? Na2 O10W K3 90.8(2) . 1_645 ? Na2 O11W K2 91.1(2) . 1_645 ? Na2 O12W K1 89.4(2) . 1_545 ? Na3 O13W K3 139.6(2) . 1_545 ? K4 O14W K1 168.4(3) . 1_455 ? K5 O15W K1 92.1(2) 1_455 1_455 ? Nb4 O11 K3 96.0(2) . 1_655 ? Nb4 O11 Na2 137.0(3) . 1_565 ? Na2 O11 K3 89.95(18) 1_565 1_655 ? Nb1 O12 K2 96.3(2) . . ? Nb1 O12 Na2 137.2(3) . 1_465 ? Na2 O12 K2 89.24(17) 1_465 . ? Nb3 O13 K4 97.6(2) . 1_565 ? Cu3 O14 Nb2 98.0(2) . . ? V3 O14 Cu3 138.3(3) . . ? V3 O14 Nb2 119.9(3) . . ? Nb1 O15 Nb5 121.9(2) . . ? Nb7 O16 Cu2 93.29(19) . . ? V2 O16 Cu2 137.8(3) . . ? V2 O16 Nb7 122.7(3) . . ? Nb9 O17 K3 97.2(2) . 1_655 ? Nb9 O17 K5 136.7(3) . 1_565 ? K5 O17 K3 91.28(18) 1_565 1_655 ? Nb8 O18 Cu1 93.01(19) . . ? V3 O18 Cu1 138.9(3) . . ? V3 O18 Nb8 121.7(3) . . ? Nb2 O19 Nb3 89.95(15) . . ? Nb9 O19 Nb2 93.13(16) . . ? Nb9 O19 Nb3 89.93(15) . . ? Te1 O19 Nb2 121.1(2) . . ? Te1 O19 Nb3 133.7(2) . . ? Te1 O19 Nb9 118.5(2) . . ? Cu1 O20 Nb1 98.0(2) . . ? V2 O20 Cu1 137.8(3) . . ? V2 O20 Nb1 120.5(3) . . ? Nb2 O21 Nb3 122.3(3) . . ? Nb1 O22 Nb5 90.19(15) . . ? Nb8 O22 Nb1 93.10(16) . . ? Nb8 O22 Nb5 90.32(16) . . ? Te1 O22 Nb1 120.9(2) . . ? Te1 O22 Nb5 133.3(2) . . ? Te1 O22 Nb8 118.8(2) . . ? Nb9 O23 Cu3 93.13(19) . . ? V1 O23 Cu3 137.2(3) . . ? V1 O23 Nb9 123.3(3) . . ? Nb7 O24 Nb6 122.5(3) . . ? K4 O25 K4 96.76(17) 1_565 2_666 ? Nb5 O25 K4 100.3(2) . 2_666 ? Nb5 O25 K4 101.3(2) . 1_565 ? Nb2 O26 K1 100.1(2) . 1_465 ? Nb2 O26 Nb8 159.5(3) . . ? Nb8 O26 K1 98.67(19) . 1_465 ? Nb8 O27 Nb5 121.6(2) . . ? Cu2 O28 Nb4 97.7(2) . . ? V1 O28 Cu2 137.8(3) . . ? V1 O28 Nb4 121.1(3) . . ? Nb1 O29 K2 100.8(2) . . ? Nb1 O29 Nb7 159.1(3) . . ? Nb7 O29 K2 98.46(19) . . ? Nb9 O30 Nb3 121.6(2) . . ? Cu1 O31 K3 113.6(2) . . ? Cu1 O31 Nb1 99.9(2) . . ? Cu1 O31 Nb8 105.2(2) . . ? Nb1 O31 K3 107.4(2) . . ? Nb8 O31 K3 112.0(2) . . ? Nb8 O31 Nb1 118.2(2) . . ? Nb4 O32 K3 100.9(2) . 1_655 ? Nb4 O32 Nb9 158.9(3) . . ? Nb9 O32 K3 98.64(19) . 1_655 ? Cu2 O33 K1 111.0(2) . . ? Cu2 O33 Nb4 100.4(2) . . ? Cu2 O33 Nb7 104.9(2) . . ? Nb4 O33 K1 108.5(2) . . ? Nb7 O33 K1 113.0(2) . . ? Nb7 O33 Nb4 118.1(2) . . ? Cu3 O34 K2 111.3(2) . 1_565 ? Cu3 O34 Nb2 99.9(2) . . ? Cu3 O34 Nb9 104.9(2) . . ? Nb2 O34 K2 107.9(2) . 1_565 ? Nb9 O34 K2 114.0(2) . 1_565 ? Nb9 O34 Nb2 117.9(2) . . ? Nb4 O35 Nb6 89.65(16) . . ? Nb7 O35 Nb4 93.18(16) . . ? Nb7 O35 Nb6 90.37(16) . . ? Te1 O35 Nb4 120.7(2) . . ? Te1 O35 Nb6 133.5(2) . . ? Te1 O35 Nb7 119.1(2) . . ? Nb4 O36 Nb6 121.5(2) . . ? Nb3 O38 Nb6 148.8(3) . . ? Nb5 O39 K4 97.65(19) . 2_666 ? Nb6 O39 K4 102.9(2) . 2_666 ? Nb6 O39 Nb5 148.3(3) . . ? Nb3 O40 K4 102.3(2) . 1_565 ? Nb5 O40 K4 97.21(19) . 1_565 ? Nb5 O40 Nb3 148.3(3) . . ? O19 Te1 O22 96.1(2) . . ? O19 Te1 O35 96.4(2) . . ? O35 Te1 O22 96.1(2) . . ? O3 V1 O7 108.8(4) . . ? O3 V1 O23 111.4(3) . . ? O3 V1 O28 110.0(3) . . ? O7 V1 O23 108.4(3) . . ? O7 V1 O28 109.7(3) . . ? O23 V1 O28 108.5(2) . . ? O4 V2 O16 108.7(3) . . ? O4 V2 O20 109.6(3) . . ? O5 V2 O4 109.1(4) . . ? O5 V2 O16 111.2(3) . . ? O5 V2 O20 109.9(3) . . ? O16 V2 O20 108.4(2) . . ? O1 V3 O2 108.6(4) . . ? O1 V3 O14 109.4(3) . . ? O1 V3 O18 109.2(3) . . ? O2 V3 O14 109.9(3) . . ? O2 V3 O18 111.2(3) . . ? O18 V3 O14 108.6(2) . . ? O4W Na1 O6W 85.1(2) . . ? O5W Na1 O4W 84.4(2) . . ? O5W Na1 O6W 84.9(2) . . ? O7W Na1 O4W 88.1(3) . . ? O7W Na1 O5W 168.5(3) . . ? O7W Na1 O6W 85.8(3) . . ? O7W Na1 O8W 100.2(3) . . ? O8W Na1 O4W 85.1(3) . . ? O8W Na1 O5W 87.8(3) . . ? O8W Na1 O6W 168.3(3) . . ? O9W Na1 O4W 169.9(3) . . ? O9W Na1 O5W 87.4(3) . . ? O9W Na1 O6W 88.5(3) . . ? O9W Na1 O7W 99.2(3) . . ? O9W Na1 O8W 100.3(3) . . ? K1 Na2 K2 114.06(9) 1_545 1_645 ? K1 Na2 K3 115.11(9) 1_545 1_645 ? K2 Na2 K3 114.55(9) 1_645 1_645 ? O9 Na2 K1 50.47(14) 1_635 1_545 ? O9 Na2 K2 64.09(14) 1_635 1_645 ? O9 Na2 K3 133.49(17) 1_635 1_645 ? O9 Na2 O12 92.2(2) 1_635 1_645 ? O10W Na2 K1 136.13(18) . 1_545 ? O10W Na2 K2 108.79(18) . 1_645 ? O10W Na2 K3 50.21(19) . 1_645 ? O10W Na2 O9 172.6(2) . 1_635 ? O10W Na2 O12W 91.2(3) . . ? O10W Na2 O11 93.6(2) . 1_545 ? O10W Na2 O12 84.3(2) . 1_645 ? O11W Na2 K1 109.74(18) . 1_545 ? O11W Na2 K2 49.90(18) . 1_645 ? O11W Na2 K3 134.26(18) . 1_645 ? O11W Na2 O9 83.1(2) . 1_635 ? O11W Na2 O10W 90.6(2) . . ? O11W Na2 O12W 91.9(2) . . ? O11W Na2 O11 174.6(2) . 1_545 ? O11W Na2 O12 93.1(2) . 1_645 ? O12W Na2 K1 51.16(19) . 1_545 ? O12W Na2 K2 135.26(19) . 1_645 ? O12W Na2 K3 109.05(18) . 1_645 ? O12W Na2 O9 92.8(2) . 1_635 ? O12W Na2 O12 173.4(2) . 1_645 ? O11 Na2 K1 64.82(14) 1_545 1_545 ? O11 Na2 K2 131.39(17) 1_545 1_645 ? O11 Na2 K3 51.06(14) 1_545 1_645 ? O11 Na2 O9 93.0(2) 1_545 1_635 ? O11 Na2 O12W 84.5(2) 1_545 . ? O11 Na2 O12 90.9(2) 1_545 1_645 ? O12 Na2 K1 130.61(17) 1_645 1_545 ? O12 Na2 K2 51.19(13) 1_645 1_645 ? O12 Na2 K3 64.33(14) 1_645 1_645 ? O13W Na3 O13W 180.0 2_556 . ? O13W Na3 O20W 90.1(4) 2_556 . ? O13W Na3 O20W 89.9(4) 2_556 2_556 ? O13W Na3 O20W 89.9(4) . . ? O13W Na3 O20W 90.1(4) . 2_556 ? O13W Na3 O16B 89.9(4) . . ? O13W Na3 O16B 90.1(4) . 2_556 ? O13W Na3 O16B 90.1(4) 2_556 . ? O13W Na3 O16B 89.9(4) 2_556 2_556 ? O13W Na3 O24W 92.0(5) . . ? O13W Na3 O24W 88.0(5) . 2_556 ? O13W Na3 O24W 88.0(5) 2_556 . ? O13W Na3 O24W 92.0(5) 2_556 2_556 ? O16W Na3 O13W 87.8(4) 2_556 . ? O16W Na3 O13W 92.2(4) . . ? O16W Na3 O13W 87.8(4) . 2_556 ? O16W Na3 O13W 92.2(4) 2_556 2_556 ? O16W Na3 O16W 180.0 2_556 . ? O16W Na3 O20W 126.8(6) . 2_556 ? O16W Na3 O20W 53.2(6) 2_556 2_556 ? O16W Na3 O20W 126.8(6) 2_556 . ? O16W Na3 O20W 53.2(6) . . ? O16W Na3 O16B 27.7(5) 2_556 2_556 ? O16W Na3 O16B 152.3(5) . 2_556 ? O16W Na3 O24W 103.5(7) 2_556 . ? O16W Na3 O24W 76.5(7) . . ? O16W Na3 O24W 76.5(7) 2_556 2_556 ? O16W Na3 O24W 103.5(7) . 2_556 ? O20W Na3 O20W 180.0 . 2_556 ? O20W Na3 O16B 99.2(5) . 2_556 ? O20W Na3 O16B 99.2(5) 2_556 . ? O20W Na3 O16B 80.8(5) 2_556 2_556 ? O20W Na3 O16B 80.8(5) . . ? O20W Na3 O24W 129.7(6) 2_556 2_556 ? O20W Na3 O24W 129.7(6) . . ? O20W Na3 O24W 50.3(6) 2_556 . ? O20W Na3 O24W 50.3(6) . 2_556 ? O16B Na3 O16B 180.0 2_556 . ? O24W Na3 O16B 49.0(6) . . ? O24W Na3 O16B 131.0(6) 2_556 . ? O24W Na3 O16B 49.0(6) 2_556 2_556 ? O24W Na3 O16B 131.0(6) . 2_556 ? O24W Na3 O24W 180.0 . 2_556 ? K1 K5 K2 116.90(9) . . ? K1 K5 Nb7 61.77(6) . . ? K1 K5 Nb8 55.76(6) . 1_645 ? K1 K5 Nb9 155.48(10) . 1_545 ? K2 K5 Nb7 55.48(5) . . ? K2 K5 Nb8 155.57(10) . 1_645 ? K2 K5 Nb9 62.25(6) . 1_545 ? K3 K5 K1 117.03(9) 1_645 . ? K3 K5 K2 117.62(9) 1_645 . ? K3 K5 Nb7 156.77(11) 1_645 . ? K3 K5 Nb8 61.48(6) 1_645 1_645 ? K3 K5 Nb9 55.59(6) 1_645 1_545 ? Nb8 K5 Nb7 114.50(8) 1_645 . ? Nb9 K5 Nb7 114.68(8) 1_545 . ? Nb9 K5 Nb8 113.67(8) 1_545 1_645 ? O2W K5 K1 132.96(18) . . ? O2W K5 K2 49.11(19) . . ? O2W K5 K3 106.23(18) . 1_645 ? O2W K5 Nb7 85.51(17) . . ? O2W K5 Nb8 154.6(2) . 1_645 ? O2W K5 Nb9 67.12(16) . 1_545 ? O3W K5 K1 106.37(18) . . ? O3W K5 K2 132.59(18) . . ? O3W K5 K3 49.7(2) . 1_645 ? O3W K5 Nb7 153.0(2) . . ? O3W K5 Nb8 67.60(16) . 1_645 ? O3W K5 Nb9 86.14(19) . 1_545 ? O3W K5 O2W 87.4(3) . . ? O8 K5 K1 49.95(14) 1_645 . ? O8 K5 K2 137.97(17) 1_645 . ? O8 K5 K3 68.70(14) 1_645 1_645 ? O8 K5 Nb7 101.26(15) 1_645 . ? O8 K5 Nb8 17.97(12) 1_645 1_645 ? O8 K5 Nb9 112.36(16) 1_645 1_545 ? O8 K5 O2W 172.4(3) 1_645 . ? O8 K5 O3W 85.0(2) 1_645 . ? O8 K5 O10 96.9(2) 1_645 . ? O8 K5 O15W 90.5(2) 1_645 1_655 ? O10 K5 K1 68.83(15) . . ? O10 K5 K2 49.43(14) . . ? O10 K5 K3 139.16(18) . 1_645 ? O10 K5 Nb7 18.02(13) . . ? O10 K5 Nb8 113.29(16) . 1_645 ? O10 K5 Nb9 101.21(16) . 1_545 ? O10 K5 O2W 90.6(2) . . ? O10 K5 O3W 171.0(3) . . ? O10 K5 O15W 83.6(2) . 1_655 ? O15W K5 K1 48.35(17) 1_655 . ? O15W K5 K2 106.65(17) 1_655 . ? O15W K5 K3 132.26(18) 1_655 1_645 ? O15W K5 Nb7 66.34(16) 1_655 . ? O15W K5 Nb8 85.39(17) 1_655 1_645 ? O15W K5 Nb9 155.56(19) 1_655 1_545 ? O15W K5 O2W 89.0(2) 1_655 . ? O15W K5 O3W 87.5(3) 1_655 . ? O17 K5 K1 137.65(17) 1_545 . ? O17 K5 K2 69.58(15) 1_545 . ? O17 K5 K3 49.69(14) 1_545 1_645 ? O17 K5 Nb7 113.66(16) 1_545 . ? O17 K5 Nb8 100.00(16) 1_545 1_645 ? O17 K5 Nb9 18.21(13) 1_545 1_545 ? O17 K5 O2W 84.7(2) 1_545 . ? O17 K5 O3W 91.6(2) 1_545 . ? O17 K5 O8 95.6(2) 1_545 1_645 ? O17 K5 O10 97.0(2) 1_545 . ? O17 K5 O15W 173.7(2) 1_545 1_655 ? 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 C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.517(14) . ? C1 N1 1.483(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 N2 1.492(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.509(13) . ? C3 N3 1.467(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 N4 1.485(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.534(13) . ? C5 N5 1.469(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 N6 1.475(11) . ? Cu1 K3 3.943(3) . ? Cu1 N1 2.042(7) . ? Cu1 N2 1.989(8) . ? Cu1 Nb1 3.1111(17) . ? Cu1 O18 2.334(5) . ? Cu1 O20 1.999(5) . ? Cu1 O31 2.012(5) . ? Cu2 K1 3.888(3) . ? Cu2 N3 1.989(8) . ? Cu2 N4 2.038(7) . ? Cu2 Nb4 3.1219(17) . ? Cu2 O16 2.311(5) . ? Cu2 O28 2.000(5) . ? Cu2 O33 2.015(5) . ? Cu3 K2 3.887(3) 1_565 ? Cu3 N5 1.988(8) . ? Cu3 N6 2.034(7) . ? Cu3 Nb2 3.1147(16) . ? Cu3 O14 1.986(5) . ? Cu3 O23 2.319(5) . ? Cu3 O34 2.017(5) . ? K1 Nb2 3.608(2) 1_645 ? K1 Nb8 3.594(2) 1_645 ? K1 O2 3.158(8) 1_645 ? K1 O8 2.908(5) 1_645 ? K1 O9 2.934(6) 1_645 ? K1 O12W 2.963(8) 1_565 ? K1 O14W 3.418(10) 1_655 ? K1 O15W 2.840(7) 1_655 ? K1 O26 2.724(5) 1_645 ? K1 O33 2.680(5) . ? K1 Na2 3.804(4) 1_565 ? K1 K5 3.799(4) . ? K2 Nb1 3.618(2) . ? K2 Nb7 3.582(2) . ? K2 O1W 3.319(8) . ? K2 O2W 2.872(8) . ? K2 O5 3.285(9) . ? K2 O10 2.886(6) . ? K2 O11W 2.911(7) 1_465 ? K2 O12 2.965(5) . ? K2 O29 2.716(5) . ? K2 O34 2.670(5) 1_545 ? K2 Na2 3.805(4) 1_465 ? K2 K5 3.799(4) . ? K3 Nb4 3.613(2) 1_455 ? K3 Nb9 3.575(3) 1_455 ? K3 O3W 2.894(9) 1_465 ? K3 O3 3.365(9) 1_455 ? K3 O10W 2.933(8) 1_465 ? K3 O13W 3.288(7) 1_565 ? K3 O11 2.969(6) 1_455 ? K3 O17 2.896(6) 1_455 ? K3 O31 2.679(5) . ? K3 O32 2.703(5) 1_455 ? K3 Na2 3.817(4) 1_465 ? K3 K5 3.797(4) 1_465 ? K4 Nb3 3.741(2) 1_545 ? K4 Nb5 3.620(2) 2_666 ? K4 Nb5 3.605(3) 1_545 ? K4 Nb6 3.730(2) 2_666 ? K4 O1W 3.066(8) 2_666 ? K4 O6 3.060(6) 2_666 ? K4 O14W 3.151(9) . ? K4 O13 3.067(6) 1_545 ? K4 O25 2.823(6) 1_545 ? K4 O25 2.865(6) 2_666 ? K4 O39 2.791(5) 2_666 ? K4 O40 2.803(5) 1_545 ? N1 H1C 0.9100 . ? N1 H1D 0.9100 . ? N2 H2C 0.9100 . ? N2 H2D 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N4 H4C 0.9100 . ? N4 H4D 0.9100 . ? N5 H5C 0.9100 . ? N5 H5D 0.9100 . ? N6 H6C 0.9100 . ? N6 H6D 0.9100 . ? Nb1 O12 1.771(5) . ? Nb1 O15 1.913(5) . ? Nb1 O20 2.122(5) . ? Nb1 O22 2.421(5) . ? Nb1 O29 1.934(5) . ? Nb1 O31 2.051(5) . ? Nb2 O9 1.768(5) . ? Nb2 O14 2.138(5) . ? Nb2 O19 2.412(5) . ? Nb2 O21 1.908(5) . ? Nb2 O26 1.937(5) . ? Nb2 O34 2.052(5) . ? Nb3 O13 1.774(5) . ? Nb3 O19 2.486(5) . ? Nb3 O21 2.045(5) . ? Nb3 O30 2.039(5) . ? Nb3 O38 1.931(5) . ? Nb3 O40 1.951(5) . ? Nb4 O11 1.772(5) . ? Nb4 O28 2.143(5) . ? Nb4 O32 1.941(5) . ? Nb4 O33 2.048(5) . ? Nb4 O35 2.413(5) . ? Nb4 O36 1.916(5) . ? Nb5 O15 2.040(5) . ? Nb5 O22 2.460(5) . ? Nb5 O25 1.757(5) . ? Nb5 O27 2.040(5) . ? Nb5 O39 1.962(5) . ? Nb5 O40 1.942(5) . ? Nb6 O6 1.771(5) . ? Nb6 O24 2.048(5) . ? Nb6 O35 2.483(5) . ? Nb6 O36 2.040(5) . ? Nb6 O38 1.943(5) . ? Nb6 O39 1.928(5) . ? Nb7 O10 1.763(5) . ? Nb7 O16 2.104(5) . ? Nb7 O24 1.912(5) . ? Nb7 O29 1.969(5) . ? Nb7 O33 2.038(5) . ? Nb7 O35 2.412(5) . ? Nb7 K5 3.895(3) . ? Nb8 O8 1.762(5) . ? Nb8 O18 2.096(5) . ? Nb8 O22 2.413(5) . ? Nb8 O26 1.969(5) . ? Nb8 O27 1.918(5) . ? Nb8 O31 2.038(5) . ? Nb8 K5 3.886(3) 1_465 ? Nb9 O17 1.763(5) . ? Nb9 O19 2.411(5) . ? Nb9 O23 2.103(5) . ? Nb9 O30 1.924(5) . ? Nb9 O32 1.969(5) . ? Nb9 O34 2.037(5) . ? Nb9 K5 3.868(3) 1_565 ? O1 V3 1.656(6) . ? O2W K5 2.463(7) . ? O3W K5 2.440(7) . ? O4W Na1 2.457(7) . ? O5W Na1 2.442(7) . ? O6W Na1 2.461(7) . ? O7W Na1 2.360(8) . ? O8W Na1 2.370(8) . ? O9W Na1 2.358(8) . ? O2 V3 1.664(6) . ? O3 V1 1.656(6) . ? O4 V2 1.661(6) . ? O5 V2 1.655(6) . ? O7 V1 1.657(6) . ? O8 K5 2.405(6) 1_465 ? O9 Na2 2.414(6) 1_475 ? O10 K5 2.417(6) . ? O10W Na2 2.401(7) . ? O11W Na2 2.395(7) . ? O12W Na2 2.414(7) . ? O13W Na3 2.433(6) . ? O15W K5 2.423(7) 1_455 ? O16W Na3 2.418(12) . ? O11 Na2 2.401(6) 1_565 ? O12 Na2 2.424(6) 1_465 ? O14 V3 1.796(5) . ? O16 V2 1.764(5) . ? O17 K5 2.391(6) 1_565 ? O18 V3 1.761(5) . ? O19 Te1 1.874(5) . ? O20 V2 1.797(5) . ? O22 Te1 1.879(5) . ? O23 V1 1.760(5) . ? O28 V1 1.786(5) . ? O35 Te1 1.874(5) . ? Na3 O20W 2.442(17) . ? Na3 O20W 2.442(17) 2_556 ? Na3 O16B 2.452(13) . ? Na3 O16B 2.452(13) 2_556 ? Na3 O24W 2.44(2) 2_556 ? Na3 O24W 2.44(2) . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.500 0.000 246.7 67.0 ? 2 0.500 0.500 0.500 91.5 27.1 ?