#------------------------------------------------------------------------------ #$Date: 2021-04-28 04:49:09 +0300 (Wed, 28 Apr 2021) $ #$Revision: 264607 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/72/7707201.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_7707201 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 'C40 H32 Cu4 K N8 Nb9 O39 Te V2, 3(O), 2(C H6 N3)' _chemical_formula_sum 'C42 H44 Cu4 K N14 Nb9 O42 Te V2' _chemical_formula_weight 2775.84 _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 mixed _atom_sites_solution_primary dual _audit_creation_date 2020-07-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-25 deposited with the CCDC. 2021-04-27 downloaded from the CCDC. ; _cell_angle_alpha 63.501(2) _cell_angle_beta 71.908(3) _cell_angle_gamma 84.150(3) _cell_formula_units_Z 2 _cell_length_a 15.4162(15) _cell_length_b 18.9380(17) _cell_length_c 21.0858(19) _cell_measurement_reflns_used 7359 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.976 _cell_measurement_theta_min 2.405 _cell_volume 5232.1(8) _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 149.98 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON II' _diffrn_radiation_monochromator 'Helios multilayer optic' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1295 _diffrn_reflns_av_unetI/netI 0.1399 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 62433 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.098 _diffrn_reflns_theta_max 25.098 _diffrn_reflns_theta_min 2.163 _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 2.295 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1213 before and 0.0817 after correction. The Ratio of minimum to maximum transmission is 0.7464. The \l/2 correction factor is Not present.' _exptl_crystal_colour blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.762 _exptl_crystal_description block _exptl_crystal_F_000 2664 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.461 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.162 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1017 _refine_ls_number_reflns 18559 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 0.987 _refine_ls_R_factor_all 0.1415 _refine_ls_R_factor_gt 0.0694 _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^)+(0.0902P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1633 _refine_ls_wR_factor_ref 0.2055 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9272 _reflns_number_total 18559 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00223f2.cif _cod_data_source_block 1 _cod_database_code 7707201 _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 0.875 _shelx_estimated_absorpt_t_min 0.670 _diffrn_source_source 'Incoatc Ius 3.0 ' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H) groups 2. Restrained distances C42-N14 1.38 with sigma of 0.02 C22-C23 1.39 with sigma of 0.02 C21-C22 1.39 with sigma of 0.02 C23-C24 1.39 with sigma of 0.02 3. Rigid bond restraints C7, C8 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C23, C24 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C3) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(N12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 5.a Rotating group: N10(H10A,H10B), N11(H11A,H11B), N12(H12A,H12B), N13(H13A,H13B), N14(H14A,H14B) 5.b Aromatic/amide H refined with riding coordinates: C21(H21), C22(H22), C23(H23), C24(H24), C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C7(H7), C10(H10), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40) 5.c Fitted hexagon refined as free rotating group: N5(C21,C22,C23,C24,C25), C8(C7,C6,N2,C10,C9) 5.d X=CH2 refined with riding coordinates: N9(H9A,H9B) ; _shelx_res_file ; TITL 1_a.res in P-1 1.res created by SHELXL-2018/3 at 17:12:03 on 24-Jul-2020 REM Old TITL 1_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.257, Rweak 0.033, Alpha 0.084, Orientation as input REM Formula found by SHELXT: Nb10 Se4 S8 Cu2 C54 N16 O39 CELL 0.71073 15.4162 18.938 21.0858 63.501 71.908 84.15 ZERR 2 0.0015 0.0017 0.0019 0.002 0.003 0.003 LATT 1 SFAC C H Cu K N Nb O Te V UNIT 84 88 8 2 28 18 84 2 4 DFIX 1.38 C42 N14 DFIX 1.39 C22 C23 DFIX 1.39 C21 C22 DFIX 1.39 C23 C24 DELU C7 C8 DELU C23 C24 ISOR 0.01 0.02 C3 C24 O4W C42 ISOR 0.005 0.01 N12 L.S. 10 PLAN 10 SIZE 0.19 0.12 0.06 TEMP -123.17 LIST 4 ABIN fmap 2 acta OMIT -3 50.2 OMIT 2 -1 2 OMIT 2 -4 2 OMIT -2 -1 4 OMIT -1 2 1 OMIT 2 0 0 OMIT 2 0 1 OMIT 3 1 6 OMIT -1 4 0 OMIT 0 2 2 OMIT 1 -4 2 OMIT -3 -3 4 OMIT -3 3 0 OMIT 2 3 4 OMIT -1 0 3 OMIT 1 -2 2 OMIT -1 7 4 OMIT 2 -2 1 OMIT 1 6 5 OMIT -4 -2 2 OMIT 2 -4 6 OMIT 0 1 6 OMIT 1 -1 4 OMIT 5 3 4 OMIT -2 -5 3 OMIT 6 -2 1 OMIT -3 4 2 OMIT 3 0 4 OMIT 0 2 8 OMIT 3 1 7 OMIT 0 2 3 OMIT 2 0 3 OMIT 6 2 4 OMIT 4 -2 3 OMIT 6 1 8 OMIT 3 -2 2 OMIT -1 2 0 OMIT 1 2 0 OMIT -1 3 1 OMIT -2 0 1 OMIT 2 1 0 OMIT -2 2 1 OMIT -2 1 1 OMIT 0 4 0 OMIT -3 0 2 OMIT 1 7 9 OMIT 0 -3 1 OMIT -2 0 2 OMIT 1 -3 3 OMIT -1 4 2 OMIT -1 -1 1 OMIT 0 -2 1 OMIT 4 0 5 OMIT 2 -3 1 OMIT 2 2 5 REM REM REM WGHT 0.090200 FVAR 0.14483 TE1 8 0.692452 0.696176 0.746236 11.00000 0.04437 0.03797 = 0.03429 -0.01709 -0.00281 -0.00250 NB1 6 0.770397 0.899581 0.611443 11.00000 0.05479 0.03855 = 0.03955 -0.01260 -0.01049 -0.00574 NB2 6 0.713551 0.838461 0.817658 11.00000 0.05778 0.04096 = 0.04210 -0.02132 -0.00772 -0.00548 NB3 6 0.663351 0.639177 0.943050 11.00000 0.05442 0.04106 = 0.03593 -0.01925 -0.00190 -0.00422 NB4 6 0.678434 0.483615 0.871266 11.00000 0.05313 0.04007 = 0.03555 -0.01905 -0.00058 -0.00119 NB5 6 0.741942 0.540945 0.680272 11.00000 0.04876 0.04307 = 0.03616 -0.02009 -0.00043 -0.00024 NB6 6 0.786330 0.765707 0.542535 11.00000 0.04646 0.04568 = 0.03428 -0.01702 -0.00587 -0.00202 NB7 6 0.897460 0.552527 0.760514 11.00000 0.04694 0.04947 = 0.03819 -0.01868 -0.00256 0.00175 NB8 6 0.882643 0.706688 0.830141 11.00000 0.05066 0.05352 = 0.03950 -0.02009 -0.00959 -0.00605 NB9 6 0.943258 0.771489 0.625923 11.00000 0.04473 0.05059 = 0.03740 -0.01614 -0.00429 -0.00829 CU2 3 0.562365 0.826095 0.611137 11.00000 0.04910 0.04516 = 0.04409 -0.02084 -0.01218 0.00284 CU4 3 0.929377 0.633631 0.580424 11.00000 0.04528 0.05571 = 0.04130 -0.02207 -0.00140 0.00057 CU3 3 0.607343 0.380297 0.785162 11.00000 0.06556 0.04360 = 0.04929 -0.02578 -0.00408 -0.00285 CU1 3 0.557359 0.796748 0.984426 11.00000 0.07080 0.04767 = 0.04661 -0.02754 -0.00619 -0.00251 V1 9 0.501632 0.758244 0.874756 11.00000 0.05864 0.04012 = 0.03674 -0.02312 0.00520 -0.01026 V2 9 0.527395 0.538784 0.773544 11.00000 0.04766 0.04278 = 0.04249 -0.02302 0.00552 -0.00967 K1 4 0.407612 0.570499 0.929975 11.00000 0.05864 0.05290 = 0.04564 -0.02496 0.00174 -0.00726 O1W 7 0.453891 0.745599 0.718106 11.00000 0.06321 0.04504 = 0.04209 -0.00737 -0.00432 -0.00007 O2W 7 0.522889 0.321502 0.913492 11.00000 0.05550 0.04185 = 0.04529 -0.02038 -0.00066 -0.00105 O3W 7 0.860479 0.490065 0.964452 11.00000 0.07423 0.03685 = 0.02842 -0.00033 -0.01282 0.00815 O1 7 0.424671 0.753639 0.847319 11.00000 0.08107 0.07212 = 0.05380 -0.02742 0.00642 0.01651 O2 7 0.466938 0.793187 0.939815 11.00000 0.05612 0.05838 = 0.04609 -0.03071 -0.00740 -0.00018 O3 7 0.591436 0.821560 0.799309 11.00000 0.04567 0.06349 = 0.05158 -0.03480 -0.00787 0.00378 O4 7 0.792282 0.646418 0.600158 11.00000 0.04281 0.05177 = 0.04343 -0.03024 0.00072 -0.00042 O5 7 0.692216 0.922301 0.835461 11.00000 0.07970 0.04872 = 0.06368 -0.03326 -0.01142 -0.00897 O6 7 0.649205 0.755534 0.923728 11.00000 0.05462 0.03014 = 0.04858 -0.02324 -0.01128 -0.00217 O7 7 0.620528 0.593768 1.040318 11.00000 0.06884 0.04337 = 0.05188 -0.02313 -0.00421 -0.00152 O8 7 0.548422 0.661910 0.908962 11.00000 0.05146 0.04217 = 0.05202 -0.02204 -0.00025 -0.01139 O9 7 0.671123 0.547375 0.923071 11.00000 0.05692 0.04343 = 0.04786 -0.02306 0.00263 0.00179 O10 7 0.639624 0.390528 0.946087 11.00000 0.05611 0.04590 = 0.03252 -0.01553 0.00572 -0.01134 O11 7 0.680169 0.460520 0.783725 11.00000 0.03982 0.04600 = 0.04031 -0.02583 0.00131 -0.00552 O12 7 0.505746 0.449797 0.777753 11.00000 0.05529 0.05113 = 0.06047 -0.02445 -0.01256 -0.00750 O13 7 0.433899 0.587508 0.773778 11.00000 0.05671 0.05438 = 0.05981 -0.02345 -0.00319 -0.00329 O14 7 0.558535 0.532333 0.849359 11.00000 0.04694 0.05197 = 0.04146 -0.02770 0.00170 -0.00808 O15 7 0.614626 0.593486 0.690322 11.00000 0.05295 0.04435 = 0.03757 -0.01624 0.00482 -0.00290 O16 7 0.646889 0.744315 0.601057 11.00000 0.04584 0.04546 = 0.05217 -0.02660 -0.01319 0.00710 O17 7 0.635068 0.857994 0.655481 11.00000 0.04871 0.04474 = 0.04867 -0.02764 -0.01080 -0.00193 O18 7 0.763603 0.873062 0.530907 11.00000 0.04170 0.05431 = 0.04807 -0.02159 -0.01137 0.00316 O19 7 0.784088 0.758769 0.661121 11.00000 0.04979 0.03522 = 0.02773 -0.01204 -0.00092 0.00320 O20 7 0.735697 0.711838 0.812746 11.00000 0.06828 0.04095 = 0.03708 -0.02013 -0.01399 0.00093 O21 7 0.747400 0.598474 0.760932 11.00000 0.05356 0.03921 = 0.03700 -0.01924 -0.00399 0.01177 O22 7 0.757850 0.886316 0.710223 11.00000 0.04703 0.03761 = 0.04141 -0.01702 -0.00993 -0.00319 O23 7 0.829768 0.808202 0.831871 11.00000 0.06509 0.05389 = 0.03774 -0.01871 -0.00678 -0.01746 O24 7 0.792918 0.647584 0.930342 11.00000 0.05173 0.04373 = 0.03885 -0.02040 -0.01198 0.00160 O25 7 0.900547 0.882638 0.589017 11.00000 0.04251 0.06269 = 0.04054 -0.01927 -0.01125 -0.01296 O26 7 0.810245 0.471597 0.847414 11.00000 0.05110 0.04724 = 0.03884 -0.02028 0.00065 0.00063 O27 7 0.860303 0.516365 0.694903 11.00000 0.04143 0.04914 = 0.03961 -0.01665 -0.00102 0.00258 O28 7 1.000522 0.504103 0.761862 11.00000 0.05307 0.06233 = 0.05358 -0.01627 -0.01321 0.02181 O29 7 1.062620 0.789537 0.585387 11.00000 0.04261 0.06655 = 0.04795 -0.01964 -0.00494 -0.01729 O30 7 0.980621 0.705311 0.857328 11.00000 0.06557 0.08513 = 0.05649 -0.03258 -0.02332 -0.00421 O31 7 0.928341 0.763930 0.722174 11.00000 0.05713 0.05130 = 0.03362 -0.01521 -0.00404 -0.00679 O32 7 0.913145 0.771337 0.535899 11.00000 0.03819 0.05270 = 0.03601 -0.01799 0.00623 -0.00970 O33 7 0.933434 0.654611 0.664062 11.00000 0.04162 0.04987 = 0.03706 -0.01635 -0.00930 0.00114 O34 7 0.729216 0.488633 0.633775 11.00000 0.06332 0.07055 = 0.04457 -0.03744 -0.00956 0.00104 O35 7 0.790834 0.776800 0.454184 11.00000 0.06538 0.05649 = 0.02991 -0.01634 -0.01242 0.00510 O36 7 0.760458 1.002596 0.567257 11.00000 0.09338 0.04192 = 0.06550 -0.01521 -0.03875 0.00677 O37 7 0.896758 0.610898 0.815859 11.00000 0.04836 0.05155 = 0.04269 -0.01158 -0.01201 -0.00299 N1 5 0.480193 0.863230 1.031083 11.00000 0.09434 0.05376 = 0.04810 -0.04011 -0.00728 -0.00595 N3 5 0.481002 0.915465 0.604563 11.00000 0.04009 0.04331 = 0.05247 -0.02272 -0.01158 0.00143 N4 5 0.494274 0.814347 0.550354 11.00000 0.06638 0.05627 = 0.06822 -0.04178 -0.03719 0.02365 AFIX 66 N5 5 0.560606 0.310431 0.755568 11.00000 0.11394 0.06244 = 0.04381 -0.01854 -0.01712 -0.00587 C21 1 0.476119 0.315577 0.743363 11.00000 0.13985 0.09742 = 0.09020 -0.04104 -0.03679 -0.04010 AFIX 43 H21 2 0.434808 0.353617 0.751467 11.00000 -1.20000 AFIX 65 C22 1 0.452076 0.265066 0.719300 11.00000 0.18796 0.09679 = 0.13575 -0.05355 -0.08786 -0.01802 AFIX 43 H22 2 0.394332 0.268583 0.710959 11.00000 -1.20000 AFIX 65 C23 1 0.512519 0.209407 0.707442 11.00000 0.17495 0.09461 = 0.12375 -0.07175 -0.06491 0.00711 AFIX 43 H23 2 0.496086 0.174885 0.690997 11.00000 -1.20000 AFIX 65 C24 1 0.597007 0.204260 0.719647 11.00000 0.12773 0.08114 = 0.08300 -0.05059 -0.02171 0.00039 AFIX 43 H24 2 0.638317 0.166220 0.711542 11.00000 -1.20000 AFIX 65 C25 1 0.621051 0.254772 0.743709 11.00000 0.13710 0.07548 = 0.04945 -0.04315 0.00910 -0.01583 AFIX 0 N6 5 0.712385 0.307916 0.783220 11.00000 0.08576 0.05295 = 0.05388 -0.03072 0.01173 -0.00275 N7 5 0.942309 0.613510 0.493031 11.00000 0.04467 0.04172 = 0.04321 -0.01587 -0.00665 0.01036 N8 5 1.063798 0.623775 0.550245 11.00000 0.04942 0.06201 = 0.04238 -0.02359 0.00163 0.01215 N9 5 1.040219 0.843710 0.397970 11.00000 0.06839 0.06440 = 0.04303 -0.01264 -0.00599 -0.04297 AFIX 93 H9A 2 1.015658 0.808356 0.443879 11.00000 -1.20000 H9B 2 1.016672 0.849836 0.362877 11.00000 -1.20000 AFIX 0 N10 5 1.148503 0.944846 0.311240 11.00000 0.08644 0.08461 = 0.05952 -0.01843 0.02815 -0.00336 AFIX 7 H10A 2 1.206940 0.934538 0.293908 11.00000 -1.20000 H10B 2 1.119510 0.947134 0.279363 11.00000 -1.20000 AFIX 0 N11 5 1.147493 0.876693 0.437479 11.00000 0.07798 0.07432 = 0.10643 -0.01685 -0.02115 -0.02603 AFIX 7 H11A 2 1.170080 0.828014 0.454353 11.00000 -1.20000 H11B 2 1.194461 0.911430 0.421658 11.00000 -1.20000 AFIX 0 C1 1 0.397413 0.882442 1.033726 11.00000 0.06023 0.08180 = 0.07355 -0.03988 0.00783 -0.00336 AFIX 43 H1 2 0.366858 0.861050 1.012977 11.00000 -1.20000 AFIX 0 C2 1 0.349532 0.929899 1.062976 11.00000 0.10038 0.07823 = 0.07395 -0.04473 -0.00330 0.00706 AFIX 43 H2 2 0.290016 0.945104 1.059165 11.00000 -1.20000 AFIX 0 C3 1 0.390566 0.955063 1.098308 11.00000 0.10514 0.09159 = 0.09161 -0.05058 -0.00865 0.00963 AFIX 43 H3 2 0.359092 0.987827 1.120755 11.00000 -1.20000 AFIX 0 C4 1 0.474912 0.933795 1.101470 11.00000 0.11714 0.09002 = 0.04211 -0.04003 -0.00106 -0.03308 AFIX 43 H4 2 0.504708 0.950368 1.126109 11.00000 -1.20000 AFIX 0 C5 1 0.518361 0.884880 1.066028 11.00000 0.08639 0.05471 = 0.06467 -0.03565 -0.00886 0.01121 AFIX 66 C8 1 0.752355 0.848028 1.094317 11.00000 0.13304 0.24675 = 0.18173 -0.18409 -0.03861 -0.00545 AFIX 43 H8 2 0.789880 0.859554 1.117021 11.00000 -1.20000 AFIX 65 C7 1 0.665325 0.877286 1.098913 11.00000 0.12198 0.14241 = 0.12296 -0.08620 -0.02166 -0.03170 AFIX 43 H7 2 0.643369 0.908808 1.124759 11.00000 -1.20000 AFIX 65 C6 1 0.610420 0.860422 1.065692 11.00000 0.13828 0.06329 = 0.04186 -0.02269 -0.02414 -0.01922 N2 5 0.642544 0.814300 1.027876 11.00000 0.08611 0.09133 = 0.05749 -0.02849 -0.01514 -0.01114 C10 1 0.729573 0.785042 1.023279 11.00000 0.09131 0.13751 = 0.07616 -0.06170 -0.03740 -0.01322 AFIX 43 H10 2 0.751528 0.753520 0.997433 11.00000 -1.20000 AFIX 65 C9 1 0.784479 0.801906 1.056499 11.00000 0.14420 0.17379 = 0.18475 -0.12596 -0.08206 0.03039 AFIX 43 H9 2 0.843960 0.781909 1.053357 11.00000 -1.20000 AFIX 0 C11 1 0.477481 0.966891 0.632722 11.00000 0.07186 0.04195 = 0.05547 -0.02456 -0.02018 -0.00258 AFIX 43 H11 2 0.518118 0.960848 0.660513 11.00000 -1.20000 AFIX 0 C12 1 0.420188 1.026465 0.624197 11.00000 0.09388 0.03409 = 0.07861 -0.03547 -0.02608 0.02399 AFIX 43 H12 2 0.421686 1.061810 0.644681 11.00000 -1.20000 AFIX 0 C13 1 0.358295 1.036014 0.584893 11.00000 0.07121 0.04564 = 0.05823 -0.00814 -0.01387 0.01502 AFIX 43 H13 2 0.318143 1.078541 0.577767 11.00000 -1.20000 AFIX 0 C14 1 0.355619 0.983864 0.556616 11.00000 0.05512 0.06522 = 0.04334 -0.02525 -0.01459 0.00861 AFIX 43 H14 2 0.313258 0.988099 0.530729 11.00000 -1.20000 AFIX 0 C15 1 0.418981 0.923698 0.567975 11.00000 0.04034 0.03608 = 0.06574 -0.02073 -0.01256 -0.00830 C16 1 0.424262 0.863191 0.539246 11.00000 0.05677 0.05126 = 0.06002 -0.02079 -0.00933 -0.00265 C17 1 0.363737 0.860759 0.504015 11.00000 0.12066 0.06049 = 0.07650 -0.02526 -0.05174 0.01650 AFIX 43 H17 2 0.314638 0.895497 0.499282 11.00000 -1.20000 AFIX 0 C18 1 0.377710 0.803387 0.474514 11.00000 0.09148 0.10374 = 0.10367 -0.06996 -0.04626 0.02229 AFIX 43 H18 2 0.337601 0.798372 0.450327 11.00000 -1.20000 AFIX 0 C19 1 0.454528 0.754245 0.483151 11.00000 0.13103 0.10099 = 0.16836 -0.09226 -0.09363 0.06115 AFIX 43 H19 2 0.469197 0.717903 0.462028 11.00000 -1.20000 AFIX 0 C20 1 0.506722 0.761287 0.523173 11.00000 0.07363 0.06991 = 0.10413 -0.05544 -0.05637 0.02792 AFIX 43 H20 2 0.554667 0.725901 0.531854 11.00000 -1.20000 AFIX 0 C26 1 0.703391 0.257226 0.759143 11.00000 0.09277 0.05312 = 0.05439 -0.03511 -0.00739 0.01486 C27 1 0.773193 0.204509 0.754556 11.00000 0.10429 0.08692 = 0.12954 -0.06541 -0.01333 0.02459 AFIX 43 H27 2 0.766527 0.165088 0.739975 11.00000 -1.20000 AFIX 0 C28 1 0.850173 0.209502 0.770827 11.00000 0.08766 0.07375 = 0.12828 -0.05230 0.00595 0.02548 AFIX 43 H28 2 0.899815 0.176576 0.764970 11.00000 -1.20000 AFIX 0 C29 1 0.852990 0.263781 0.795892 11.00000 0.09207 0.08071 = 0.10792 -0.04873 -0.01761 0.01063 AFIX 43 H29 2 0.903662 0.266519 0.811424 11.00000 -1.20000 AFIX 0 C30 1 0.784108 0.314276 0.799020 11.00000 0.08967 0.03643 = 0.08657 -0.01838 -0.01005 0.01348 AFIX 43 H30 2 0.789272 0.354529 0.813025 11.00000 -1.20000 AFIX 0 C31 1 0.874274 0.607319 0.468775 11.00000 0.06174 0.06260 = 0.02528 -0.01891 -0.00306 0.00763 AFIX 43 H31 2 0.813433 0.615704 0.492348 11.00000 -1.20000 AFIX 0 C32 1 0.891433 0.589150 0.410739 11.00000 0.05738 0.08101 = 0.04655 -0.03757 -0.01263 0.01957 AFIX 43 H32 2 0.842473 0.583274 0.394822 11.00000 -1.20000 AFIX 0 C33 1 0.979928 0.579213 0.374855 11.00000 0.08476 0.04852 = 0.06095 -0.02900 -0.01659 0.00258 AFIX 43 H33 2 0.992324 0.565072 0.335069 11.00000 -1.20000 AFIX 0 C34 1 1.047323 0.589691 0.396734 11.00000 0.05888 0.05969 = 0.04598 -0.03024 0.00312 0.01272 AFIX 43 H34 2 1.108929 0.585795 0.371062 11.00000 -1.20000 AFIX 0 C35 1 1.028269 0.605759 0.455047 11.00000 0.05280 0.03626 = 0.04624 -0.00813 -0.00120 0.01063 C36 1 1.095965 0.614621 0.486819 11.00000 0.06682 0.04188 = 0.04930 -0.01943 0.00122 0.01364 C37 1 1.190807 0.613591 0.455362 11.00000 0.05291 0.07751 = 0.07741 -0.04199 0.01465 -0.00894 AFIX 43 H37 2 1.214300 0.609475 0.409872 11.00000 -1.20000 AFIX 0 C38 1 1.249879 0.618680 0.491731 11.00000 0.04575 0.10951 = 0.08202 -0.04970 0.00049 -0.00859 AFIX 43 H38 2 1.314030 0.617540 0.471471 11.00000 -1.20000 AFIX 0 C39 1 1.214700 0.625334 0.556864 11.00000 0.04062 0.10499 = 0.10211 -0.06277 -0.01437 -0.00294 AFIX 43 H39 2 1.254030 0.627386 0.582944 11.00000 -1.20000 AFIX 0 C40 1 1.121927 0.629008 0.584068 11.00000 0.06131 0.08157 = 0.04862 -0.01833 -0.00308 0.01196 AFIX 43 H40 2 1.098078 0.635479 0.628371 11.00000 -1.20000 AFIX 0 C41 1 1.110435 0.886370 0.382181 11.00000 0.09898 0.10756 = 0.03902 -0.03187 -0.01007 0.00154 N12 5 0.994805 0.919575 0.686806 11.00000 0.12107 0.03923 = 0.04791 -0.01759 0.02759 -0.01109 AFIX 7 H12A 2 0.988426 0.914425 0.735482 11.00000 -1.20000 H12B 2 0.934757 0.929868 0.684262 11.00000 -1.20000 AFIX 0 O4W 7 0.302208 0.449027 0.838452 11.00000 0.06547 0.18591 = 0.08764 -0.05456 -0.02938 -0.00583 O5W 7 0.627130 1.034586 0.704023 11.00000 0.15797 0.08996 = 0.16164 -0.06835 -0.08077 0.03581 N13 5 1.123550 1.024595 0.618463 11.00000 0.10191 0.09663 = 0.08392 -0.03592 -0.02228 -0.04416 AFIX 7 H13A 2 1.163830 1.042971 0.572908 11.00000 -1.20000 H13B 2 1.094842 1.066040 0.623908 11.00000 -1.20000 AFIX 0 N14 5 1.030526 0.991947 0.565772 11.00000 0.11469 0.12538 = 0.12173 -0.05584 -0.04768 -0.02432 AFIX 7 H14A 2 1.008668 0.948871 0.568642 11.00000 -1.20000 H14B 2 0.986749 1.026089 0.564856 11.00000 -1.20000 AFIX 0 C42 1 1.062056 0.975005 0.625063 11.00000 0.11133 0.09889 = 0.09866 -0.05187 -0.02988 0.00234 HKLF 4 REM 1_a.res in P-1 REM wR2 = 0.2055, GooF = S = 0.985, Restrained GooF = 0.987 for all data REM R1 = 0.0694 for 9272 Fo > 4sig(Fo) and 0.1415 for all 18559 data REM 1017 parameters refined using 36 restraints END WGHT 0.0907 0.0000 REM Highest difference peak 1.461, deepest hole -1.011, 1-sigma level 0.162 Q1 1 0.2640 0.5948 0.8917 11.00000 0.05 1.46 Q2 1 1.1425 0.7927 0.4366 11.00000 0.05 1.04 Q3 1 1.0365 0.9193 0.6952 11.00000 0.05 0.93 Q4 1 0.9445 1.0495 0.5529 11.00000 0.05 0.90 Q5 1 1.2818 0.9188 0.3588 11.00000 0.05 0.89 Q6 1 0.5627 0.7194 0.6543 11.00000 0.05 0.86 Q7 1 0.4683 0.7840 0.8622 11.00000 0.05 0.84 Q8 1 0.3072 0.4773 0.8314 11.00000 0.05 0.79 Q9 1 0.3326 0.3977 0.8499 11.00000 0.05 0.78 Q10 1 0.5369 0.8251 0.7298 11.00000 0.05 0.77 ; _shelx_res_checksum 95682 _shelx_fab_file ; -17 -2 1 32.9336 0.2003 -17 -1 1 0.5163 -0.0919 -17 0 1 -8.2117 -0.0491 -17 1 1 -5.0301 0.3828 -17 2 1 -12.9505 -0.0192 -17 3 1 8.8864 -0.2160 -17 4 1 -0.3740 0.2484 -16 -6 1 -3.4118 -0.1546 -16 -5 1 -13.4948 0.3545 -16 -5 2 5.2245 0.4316 -16 -4 1 -3.8639 -0.3646 -16 -4 2 -1.5152 0.0390 -16 -3 1 0.1945 0.3671 -16 -3 3 -0.3591 -0.0105 -16 -2 1 2.1032 0.2535 -16 -2 2 16.8101 0.1471 -16 -2 3 -7.1418 -0.1453 -16 -1 1 -3.1281 -0.8132 -16 -1 2 1.2563 -0.0088 -16 -1 3 6.0939 0.0931 -16 -1 4 10.6254 -0.1462 -16 0 1 0.9965 0.5806 -16 0 2 -4.7379 -0.2387 -16 0 3 9.0115 0.0986 -16 0 4 7.5407 0.0009 -16 1 1 3.3683 0.7660 -16 1 2 -8.5732 0.1176 -16 1 3 5.7376 -0.1166 -16 1 4 27.1415 0.0115 -16 2 1 -9.2422 -0.9886 -16 2 2 -5.5928 0.1974 -16 2 3 13.3672 -0.2117 -16 2 4 -6.6628 0.0875 -16 3 1 5.4636 -0.1818 -16 3 2 9.4799 -0.1420 -16 3 3 -2.8770 -0.0295 -16 3 4 9.0500 0.0730 -16 3 5 -1.3861 0.2431 -16 4 1 14.4177 0.3229 -16 4 2 6.8363 0.3529 -16 4 3 -3.9686 0.1786 -16 4 4 -3.1714 -0.0187 -16 5 1 19.3523 -0.4333 -16 5 2 12.0122 -0.2514 -16 5 3 7.9711 0.3131 -16 5 4 -1.3848 -0.3066 -16 6 1 -1.2278 0.0894 -16 6 2 8.9766 -0.1899 -16 6 3 -13.9481 0.0464 -16 6 4 -4.8610 0.2233 -16 7 1 -8.7865 0.4958 -16 7 2 -10.6756 -0.1878 -16 7 3 -4.0898 -0.1270 -16 8 1 -11.5935 0.0392 -16 8 2 -12.3086 0.3597 -15 -8 1 13.9753 -0.0087 -15 -7 1 5.1338 0.5513 -15 -7 2 2.1566 0.1356 -15 -6 1 5.8750 -0.2789 -15 -6 2 6.0559 0.0936 -15 -6 3 -5.4623 -0.0810 -15 -5 1 -7.9775 -0.4615 -15 -5 2 -1.2757 0.2919 -15 -5 3 13.7045 0.0467 -15 -5 4 -2.9175 0.0931 -15 -4 1 -0.5062 0.5837 -15 -4 2 -3.5716 -0.4557 -15 -4 3 -3.5320 0.0978 -15 -4 4 6.5241 -0.2151 -15 -3 1 1.0563 0.5500 -15 -3 2 0.4748 -0.0439 -15 -3 3 -6.0789 -0.2536 -15 -3 4 -3.9927 0.1375 -15 -3 5 -1.8663 -0.1604 -15 -2 1 -2.9737 -0.6688 -15 -2 2 1.6137 0.2635 -15 -2 3 2.8242 -0.0887 -15 -2 4 -15.0270 -0.1905 -15 -2 6 14.6797 -0.0300 -15 -1 1 -3.1591 0.1798 -15 -1 2 -5.9253 -0.3776 -15 -1 3 -8.1349 -0.0109 -15 -1 4 -5.9662 0.0544 -15 -1 5 -0.3761 -0.0452 -15 -1 6 -6.8405 0.1180 -15 0 1 -1.8744 0.4119 -15 0 2 -5.7370 0.3483 -15 0 3 1.1101 -0.0484 -15 0 4 2.0942 0.0778 -15 0 5 -1.6146 0.0890 -15 0 6 8.7262 -0.1031 -15 1 1 4.8303 -0.4213 -15 1 2 -0.5221 0.4568 -15 1 3 -4.1872 -0.0722 -15 1 4 9.7376 -0.0145 -15 1 5 18.6331 -0.0551 -15 1 6 -5.8838 -0.1129 -15 1 7 -2.7495 0.0297 -15 2 1 -13.3231 -1.0007 -15 2 2 -9.3735 -0.4294 -15 2 3 0.7708 0.1417 -15 2 4 5.1027 -0.0849 -15 2 5 -12.9555 0.1104 -15 2 6 1.8355 0.0207 -15 2 7 -1.0661 -0.0305 -15 3 1 -5.3069 0.6891 -15 3 2 -3.0564 -0.2363 -15 3 3 -3.3414 0.2544 -15 3 4 -2.8526 -0.0724 -15 3 5 6.1348 0.2355 -15 3 6 -11.4040 0.0665 -15 3 7 -8.3569 -0.1447 -15 4 1 -2.1147 0.4291 -15 4 2 6.5367 0.2130 -15 4 3 -0.6045 0.2470 -15 4 4 -11.3166 0.1480 -15 4 5 3.6151 -0.3212 -15 4 6 -9.2998 0.2243 -15 4 7 -8.1918 -0.1906 -15 5 1 8.3330 -0.4025 -15 5 2 9.3066 -0.2603 -15 5 3 7.4196 -0.3596 -15 5 4 10.8903 0.2229 -15 5 5 -6.6804 -0.1414 -15 5 6 -0.9253 -0.0804 -15 5 7 13.0472 0.1653 -15 6 1 -8.4200 0.6318 -15 6 2 1.6567 0.0177 -15 6 3 5.3438 -0.2469 -15 6 4 -5.3324 0.0123 -15 6 5 4.3124 0.1661 -15 6 6 2.0512 -0.1327 -15 6 7 -1.2841 0.1198 -15 7 1 8.0646 -0.1368 -15 7 2 -3.1388 0.4081 -15 7 3 -2.2631 -0.0246 -15 7 4 7.8929 -0.2227 -15 7 5 3.5711 0.0793 -15 7 6 -4.3426 -0.0418 -15 8 1 -10.6998 -0.8126 -15 8 2 -7.5648 -0.0540 -15 8 3 -4.1205 0.2700 -15 8 4 9.7640 -0.0160 -15 8 5 3.7268 -0.0898 -15 8 6 1.9133 0.0107 -15 9 1 -8.4304 0.6046 -15 9 2 -3.2855 -0.3866 -15 9 3 -3.9604 0.1149 -15 9 4 2.5571 -0.1226 -15 9 5 0.3679 0.0755 -15 10 1 -6.9091 0.5741 -15 10 2 -1.0083 -0.1191 -15 10 3 3.9890 -0.2937 -15 10 4 9.5035 0.2152 -15 11 1 2.9307 -0.6594 -14 -10 1 -2.9909 -0.0910 -14 -9 1 -6.5755 -0.6280 -14 -9 2 -2.9220 -0.2132 -14 -8 1 -1.7030 1.2514 -14 -8 2 2.2192 -0.1951 -14 -8 3 1.7881 -0.0826 -14 -7 1 -0.0965 -0.3928 -14 -7 2 -0.0810 0.4784 -14 -7 3 -4.7182 -0.0288 -14 -7 4 -0.1312 -0.0273 -14 -6 1 20.2614 -1.1446 -14 -6 2 -1.1052 -0.3069 -14 -6 3 6.8266 0.2239 -14 -6 4 -16.0163 -0.1295 -14 -6 5 -7.4352 0.0362 -14 -5 1 0.4225 1.3323 -14 -5 2 -0.4191 -0.3789 -14 -5 3 3.6897 0.0015 -14 -5 4 12.8765 -0.0662 -14 -5 5 -0.8701 0.0569 -14 -5 6 15.0628 0.0963 -14 -4 1 2.6808 0.3852 -14 -4 2 -2.8507 0.0836 -14 -4 3 -4.8083 -0.2166 -14 -4 4 3.9160 0.0118 -14 -4 5 7.9235 -0.1730 -14 -4 6 -14.1570 -0.0316 -14 -3 1 1.3290 -0.5971 -14 -3 2 1.4490 0.4438 -14 -3 3 1.3297 -0.3885 -14 -3 4 -3.7689 0.2500 -14 -3 5 -6.0669 0.0370 -14 -3 6 -9.1775 -0.0272 -14 -3 7 -9.0081 0.1815 -14 -2 1 -0.5652 -0.0863 -14 -2 2 2.3403 -0.1405 -14 -2 3 4.3748 0.0441 -14 -2 4 1.2102 -0.1396 -14 -2 5 -10.8015 0.1866 -14 -2 6 -11.4114 -0.1653 -14 -2 7 3.7787 0.0063 -14 -1 1 3.1905 -0.9826 -14 -1 2 0.8297 0.2464 -14 -1 3 -6.1963 0.4329 -14 -1 4 -6.2657 -0.2626 -14 -1 5 -6.9942 0.0934 -14 -1 6 -4.9853 0.0597 -14 -1 7 -6.8114 -0.0357 -14 -1 8 7.8544 0.1633 -14 0 1 4.6334 1.0131 -14 0 2 -3.4558 -0.1165 -14 0 3 -2.2047 0.2091 -14 0 4 0.3214 0.2676 -14 0 5 -9.4343 -0.0435 -14 0 6 -11.5841 0.0402 -14 0 7 5.6696 -0.1062 -14 0 8 13.1076 0.0947 -14 1 1 -0.1282 -0.8572 -14 1 2 7.9066 -0.0552 -14 1 3 6.1765 0.0027 -14 1 4 0.0865 -0.0715 -14 1 5 0.1689 -0.0473 -14 1 6 5.9416 -0.0810 -14 1 7 -7.6798 -0.0564 -14 1 8 7.1340 -0.0581 -14 1 9 4.0262 -0.0724 -14 2 1 6.8266 0.6972 -14 2 2 -7.3189 -0.6819 -14 2 3 -1.1978 -0.0935 -14 2 4 6.0493 0.0185 -14 2 5 -1.5618 0.0201 -14 2 6 -15.1591 0.0743 -14 2 7 14.7182 0.1305 -14 2 8 6.8133 -0.0462 -14 2 9 0.2613 0.0774 -14 3 1 -7.9601 0.3283 -14 3 2 -1.8991 0.5903 -14 3 3 -4.4493 -0.1031 -14 3 4 -5.9310 0.3396 -14 3 5 -0.9201 -0.1487 -14 3 6 1.0613 0.1442 -14 3 7 -8.9166 -0.0030 -14 3 8 5.4934 -0.1806 -14 3 9 -11.2609 -0.0086 -14 4 1 5.3759 -0.3623 -14 4 2 -8.0170 0.2181 -14 4 3 -4.8957 -0.0358 -14 4 4 -11.6821 -0.0884 -14 4 5 -7.8293 0.0386 -14 4 6 -0.9628 -0.3045 -14 4 7 -13.1535 0.1100 -14 4 8 2.0626 -0.0546 -14 4 9 17.1761 -0.0768 -14 5 1 -6.3137 -0.0605 -14 5 2 7.5211 -0.4665 -14 5 3 3.9732 -0.1349 -14 5 4 -0.8804 -0.2986 -14 5 5 8.0139 -0.0011 -14 5 6 -10.6987 0.0690 -14 5 7 0.9995 -0.0766 -14 5 8 17.3787 0.0630 -14 5 9 7.9060 0.1059 -14 6 1 2.6699 0.8334 -14 6 2 -13.7430 0.3929 -14 6 3 0.8563 -0.0048 -14 6 4 3.6918 -0.1111 -14 6 5 1.3353 0.0657 -14 6 6 2.3206 0.0558 -14 6 7 2.3956 -0.0287 -14 6 8 1.6826 0.0625 -14 6 9 -1.1525 -0.0282 -14 7 1 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5.8324 0.0497 16 4 10 -2.8704 0.0687 16 4 11 9.6105 -0.0072 16 4 12 -3.9538 -0.0599 16 4 13 -14.0912 -0.0113 16 4 14 -13.4702 0.0457 16 4 15 -2.4981 0.0463 16 4 16 -1.0114 0.0661 16 4 17 0.5183 -0.0024 16 4 18 -7.0710 0.0315 16 5 0 -15.9340 0.3568 16 5 1 -8.8225 -0.8186 16 5 2 0.0963 0.2473 16 5 3 -12.1546 -0.0437 16 5 4 -3.5563 0.2645 16 5 5 -1.9297 0.0046 16 5 6 3.5702 0.1847 16 5 7 -1.9493 -0.1761 16 5 8 -2.8420 -0.0168 16 5 9 5.8872 0.0288 16 5 10 6.2667 -0.0464 16 5 11 -7.8112 -0.0370 16 5 12 0.6884 0.0581 16 5 13 -6.8904 -0.0247 16 5 14 -7.4029 0.0437 16 5 15 -8.8217 0.0420 16 5 16 9.1897 -0.0460 16 5 17 0.8217 -0.0018 16 5 18 1.3585 -0.1127 16 6 0 8.2127 0.1848 16 6 1 14.9573 0.5694 16 6 2 3.8683 -0.3578 16 6 3 8.7394 0.0486 16 6 4 -2.2198 0.0405 16 6 5 4.4895 -0.0155 16 6 6 8.1344 -0.0790 16 6 7 1.7804 0.1469 16 6 8 -5.8698 -0.1055 16 6 9 -7.3661 -0.0556 16 6 10 -11.6658 0.1123 16 6 11 -3.7924 -0.0405 16 6 12 -0.6632 0.1274 16 6 13 10.8535 0.0908 16 6 14 -17.3556 -0.0814 16 6 15 -5.4711 -0.0718 16 6 16 -12.4183 0.0150 16 6 17 0.3216 -0.1406 16 6 18 8.8677 0.0400 16 7 0 5.1665 -0.4155 16 7 1 18.9586 0.2920 16 7 2 10.4792 0.1948 16 7 3 12.4373 -0.0618 16 7 4 21.4517 -0.0845 16 7 5 -5.6237 -0.0752 16 7 6 -4.7336 -0.1538 16 7 7 -2.2050 -0.0009 16 7 8 -5.2165 0.0856 16 7 9 -4.7413 0.0065 16 7 10 -1.2857 -0.1039 16 7 11 2.0634 0.2277 16 7 12 7.2752 -0.1666 16 7 13 -9.7021 0.0683 16 7 14 -4.3570 -0.0210 16 7 15 -1.9201 -0.0242 16 7 16 0.9974 -0.0806 16 7 17 -1.4368 0.0769 16 7 18 7.6790 -0.0053 16 8 1 3.9582 -0.3970 16 8 2 -4.4043 0.1210 16 8 3 2.4466 -0.1004 16 8 4 7.2303 0.1100 16 8 5 4.5590 0.1143 16 8 6 -7.5558 0.0110 16 8 7 13.0472 -0.2133 16 8 8 3.2376 0.1046 16 8 9 -5.8609 0.0634 16 8 10 3.5816 0.1626 16 8 11 -4.6486 -0.0718 16 8 12 12.7075 0.0897 16 8 13 20.5586 -0.1037 16 8 14 10.3927 -0.0996 16 8 15 9.9672 0.1131 16 8 16 -1.6405 0.0718 16 8 17 -2.7590 -0.0235 16 8 18 4.7953 0.0273 16 9 2 -0.4150 -0.0657 16 9 3 0.6569 0.0064 16 9 4 12.7899 0.0277 16 9 5 7.1661 0.0110 16 9 6 -2.1673 0.0967 16 9 7 -8.7447 0.0271 16 9 8 18.8055 -0.0656 16 9 9 12.8961 -0.0812 16 9 10 -5.3362 -0.0095 16 9 11 7.6845 0.0834 16 9 12 3.7498 -0.0284 16 9 13 0.0233 -0.0781 16 9 14 2.7774 0.0026 16 9 15 -1.8938 -0.0269 16 9 16 -10.3227 0.0365 16 9 17 -22.3632 0.0046 16 9 18 -6.5044 0.0451 16 10 4 5.8261 -0.2055 16 10 5 6.7479 -0.1221 16 10 6 -0.7759 -0.0868 16 10 7 -2.2039 -0.0365 16 10 8 1.2334 -0.0174 16 10 9 -0.1623 0.0257 16 10 10 -8.6017 -0.0931 16 10 11 -1.8868 -0.0407 16 10 12 -7.6792 -0.0267 16 10 13 4.1819 0.1168 16 10 14 -4.7670 0.1091 16 10 15 -13.2432 -0.0223 16 10 16 -10.3129 -0.0530 16 10 17 -3.5472 0.1398 16 11 5 -9.3196 0.0307 16 11 6 -12.3347 -0.0055 16 11 7 -5.1142 0.0444 16 11 8 1.6701 -0.0159 16 11 9 1.2062 0.1119 16 11 10 -9.0605 0.0719 16 11 11 -24.1128 -0.0435 16 11 12 4.1629 0.0628 16 11 13 1.0231 -0.0584 16 11 14 8.5737 0.0081 16 11 15 1.0875 0.1028 16 11 16 -8.2132 0.0318 16 11 17 -9.0962 -0.1082 16 12 7 -7.5636 -0.0432 16 12 8 -7.0065 0.0805 16 12 9 9.2071 -0.2201 16 12 10 1.8474 0.0195 16 12 11 -7.3820 -0.0947 16 12 12 4.3867 -0.0272 16 12 13 13.8139 -0.1458 16 12 14 -1.8529 -0.0616 16 12 15 17.7589 0.0480 16 12 16 4.1283 -0.0164 16 13 11 2.8001 0.0250 16 13 12 13.5848 0.0387 16 13 13 9.1021 0.0405 17 -6 1 -4.8401 -0.4552 17 -6 2 -15.1197 0.2661 17 -6 3 -5.1547 -0.1745 17 -6 4 1.3884 0.1822 17 -6 5 -15.3002 0.0851 17 -6 6 -8.5402 -0.1242 17 -5 0 19.8694 0.6112 17 -5 1 -7.3714 -0.0062 17 -5 2 -3.0616 0.1065 17 -5 3 -6.1898 0.1043 17 -5 4 5.4497 -0.1106 17 -5 5 1.5029 -0.0368 17 -5 6 2.0989 0.1468 17 -5 7 1.7825 -0.0784 17 -5 8 14.0887 -0.0705 17 -4 0 10.4089 -0.3107 17 -4 1 0.1217 -0.0021 17 -4 2 -19.0146 -0.0984 17 -4 3 11.5765 0.1195 17 -4 4 -2.1136 -0.1363 17 -4 5 14.7363 -0.0032 17 -4 6 5.2414 -0.1482 17 -4 7 1.9099 -0.0478 17 -4 8 -4.7198 0.0292 17 -4 9 -3.5713 0.0508 17 -4 10 0.4509 -0.1763 17 -3 0 0.4966 0.0045 17 -3 1 -8.5874 -0.1377 17 -3 2 3.4120 -0.2228 17 -3 3 -8.3680 0.0748 17 -3 4 4.4313 -0.0345 17 -3 5 -2.3394 -0.0334 17 -3 6 -2.7894 0.1602 17 -3 7 -12.5042 -0.0307 17 -3 8 -2.5400 -0.0677 17 -3 9 7.7361 0.1339 17 -3 10 5.1457 0.1049 17 -3 11 2.4871 0.0417 17 -2 0 -9.1630 0.8333 17 -2 1 7.2268 0.0436 17 -2 2 8.0040 0.0909 17 -2 3 0.6954 -0.1823 17 -2 4 2.6207 0.2008 17 -2 5 8.6964 -0.1483 17 -2 6 -13.7134 0.0636 17 -2 7 -11.5340 0.0204 17 -2 8 7.7636 0.0437 17 -2 9 2.6444 -0.1512 17 -2 10 -2.3873 -0.0253 17 -2 11 -5.4486 -0.0423 17 -2 12 4.3918 -0.1139 17 -1 0 9.9961 -0.6410 17 -1 1 -0.3604 0.6598 17 -1 2 -4.1580 -0.3436 17 -1 3 -5.3205 0.0628 17 -1 4 3.1819 -0.1829 17 -1 5 9.8354 0.0563 17 -1 6 -13.9167 -0.1427 17 -1 7 -15.6750 0.0488 17 -1 8 -4.5413 0.0925 17 -1 9 -2.9115 -0.0218 17 -1 10 -16.1827 -0.0824 17 -1 11 -2.9505 -0.0190 17 -1 12 13.8905 -0.0491 17 -1 13 8.2019 0.0412 17 0 0 17.9185 -0.5295 17 0 1 15.6079 -0.5696 17 0 2 -16.2870 0.3118 17 0 3 -3.0622 -0.2485 17 0 4 7.0441 0.0456 17 0 5 -11.7156 0.1522 17 0 6 -12.0658 0.0421 17 0 7 -21.4810 -0.0498 17 0 8 -2.1277 0.0429 17 0 9 0.8608 0.0379 17 0 10 8.0881 0.0176 17 0 11 5.1786 0.1287 17 0 12 -6.1529 -0.1053 17 0 13 -5.0157 -0.0078 17 0 14 0.5398 0.0422 17 1 0 3.0469 0.6246 17 1 1 1.2249 -0.1702 17 1 2 2.0042 -0.0022 17 1 3 0.5170 0.0427 17 1 4 5.4211 0.0735 17 1 5 -0.2129 -0.0089 17 1 6 -7.4460 0.1976 17 1 7 -2.8211 -0.1113 17 1 8 -0.9163 -0.0580 17 1 9 11.2836 -0.0070 17 1 10 0.7608 0.0210 17 1 11 -12.6008 -0.0973 17 1 12 5.5686 0.2090 17 1 13 -5.8822 -0.0785 17 1 14 -1.1673 -0.0892 17 2 0 6.1897 -0.2632 17 2 1 -10.3503 0.4247 17 2 2 4.2756 0.0919 17 2 3 -6.8656 0.0947 17 2 4 -6.1119 -0.0756 17 2 5 3.4194 -0.0647 17 2 6 -7.6538 -0.1850 17 2 7 3.6289 0.2642 17 2 8 -8.2755 -0.0987 17 2 9 -3.7182 -0.0135 17 2 10 -3.2908 -0.0809 17 2 11 1.2343 0.0235 17 2 12 -3.6653 0.0230 17 2 13 -14.5967 -0.0265 17 2 14 -20.6554 0.0707 17 2 15 -13.3855 0.0984 17 3 0 9.1353 -0.3909 17 3 1 5.0024 -0.2562 17 3 2 -12.5012 -0.0795 17 3 3 -0.4495 0.2043 17 3 4 1.8773 -0.0009 17 3 5 0.9107 -0.0940 17 3 6 5.0867 0.0612 17 3 7 -2.1417 -0.1548 17 3 8 12.7379 -0.0171 17 3 9 2.3817 0.0489 17 3 10 1.6398 0.1211 17 3 11 11.7534 -0.0822 17 3 12 0.9251 -0.0608 17 3 13 -10.1419 0.1110 17 3 14 3.6532 -0.0642 17 3 15 9.6565 -0.0521 17 4 1 -19.6825 -0.0474 17 4 2 -9.6540 0.0079 17 4 3 -3.1998 -0.0106 17 4 4 1.2145 0.2296 17 4 5 -7.8240 0.1250 17 4 6 -9.0058 -0.0218 17 4 7 -0.1558 0.0106 17 4 8 10.6750 0.0262 17 4 9 8.1353 -0.0613 17 4 10 -4.9050 0.0451 17 4 11 -0.8767 0.0690 17 4 12 3.0949 0.0175 17 4 13 -11.8543 -0.0475 17 4 14 -10.6108 -0.0653 17 4 15 -0.3058 0.0364 17 4 16 6.5511 0.0533 17 5 1 -12.0130 0.1102 17 5 2 -12.2286 -0.1258 17 5 3 0.3908 -0.1101 17 5 4 -11.5182 -0.0887 17 5 5 -9.0374 0.0757 17 5 6 -8.9729 -0.0015 17 5 7 0.4716 -0.0257 17 5 8 1.6834 0.0774 17 5 9 1.4977 -0.1855 17 5 10 -0.9023 0.0029 17 5 11 7.4932 -0.0091 17 5 12 -2.5655 -0.0302 17 5 13 -2.8087 0.0207 17 5 14 -3.3791 0.0679 17 5 15 3.8907 -0.0268 17 5 16 5.4205 -0.0338 17 6 2 8.6624 0.2738 17 6 3 -4.7423 0.1339 17 6 4 6.2617 -0.2300 17 6 5 -7.8648 -0.0411 17 6 6 2.5283 -0.0743 17 6 7 11.6181 0.0853 17 6 8 7.8895 -0.1471 17 6 9 -2.7741 0.2523 17 6 10 -13.1988 -0.0941 17 6 11 -8.9125 0.0417 17 6 12 0.8057 0.0051 17 6 13 9.8376 0.0244 17 6 14 0.5466 0.0288 17 6 15 -10.0710 -0.0779 17 6 16 1.3370 -0.0235 17 7 3 0.2932 -0.1549 17 7 4 7.5792 0.0954 17 7 5 14.1701 -0.0299 17 7 6 -11.4771 -0.0247 17 7 7 -7.4266 -0.0821 17 7 8 -5.6845 0.1219 17 7 9 -16.8984 0.0327 17 7 10 -10.1270 0.0913 17 7 11 -6.4173 -0.0218 17 7 12 14.4708 0.0460 17 7 13 4.4678 -0.0406 17 7 14 -14.1202 -0.1213 17 7 15 -2.5614 0.0205 17 7 16 1.3081 -0.0243 17 8 4 3.9591 -0.1039 17 8 5 -0.1936 -0.0353 17 8 6 0.6957 0.2786 17 8 7 2.8981 0.0048 17 8 8 6.8438 0.0065 17 8 9 3.1614 0.0293 17 8 10 0.2240 -0.0167 17 8 11 0.0460 0.0394 17 8 12 -7.4386 -0.0768 17 8 13 17.4214 -0.0855 17 8 14 4.2475 0.0521 17 8 15 1.5327 -0.0490 17 9 6 3.9563 -0.1654 17 9 7 -0.4649 0.0974 17 9 8 12.9487 -0.0407 17 9 9 17.3450 -0.0942 17 9 10 6.9692 -0.1123 17 9 11 -1.0021 -0.1128 17 9 12 13.3107 -0.1680 17 9 13 15.1573 0.1852 17 9 14 11.6697 -0.0545 17 9 15 -4.1930 0.0392 17 10 8 6.8085 0.0319 17 10 9 16.5262 0.0290 17 10 10 -5.3960 0.0179 17 10 11 -1.7996 -0.0442 17 10 12 17.4199 0.1029 17 10 13 3.1805 -0.0614 17 10 14 -2.2174 0.0836 18 -2 4 -11.5070 -0.0680 18 -2 5 10.8859 0.0156 18 -2 6 0.0444 -0.1207 18 -2 7 -10.8068 -0.0528 18 -1 3 -2.3612 -0.0154 18 -1 4 -2.9826 -0.0418 18 -1 5 -0.9810 0.0435 18 -1 6 16.0233 0.1263 18 -1 7 -16.6142 -0.1708 18 -1 8 -7.9311 -0.0641 18 -1 9 -0.4673 0.2282 18 0 3 -20.7620 0.1426 18 0 4 1.4831 0.0952 18 0 5 8.3971 -0.0827 18 0 6 -8.8199 0.3277 18 0 7 -2.7226 0.0023 18 0 8 -19.1931 -0.0178 18 0 9 -15.2424 -0.0398 18 0 10 -2.8222 0.0441 18 1 3 -6.5772 0.0883 18 1 4 3.0550 0.0551 18 1 5 9.7223 0.0551 18 1 6 0.2957 -0.2827 18 1 7 -0.7458 0.1452 18 1 8 -7.6329 -0.0537 18 1 9 -9.3716 -0.1847 18 1 10 6.6618 0.1236 18 1 11 0.8332 -0.0010 18 2 4 -1.4788 -0.0382 18 2 5 2.3028 0.0030 18 2 6 3.7268 -0.2143 18 2 7 -5.9647 -0.1349 18 2 8 3.7187 0.0229 18 2 9 -12.5040 0.0771 18 2 10 -10.3503 0.0026 18 2 11 -9.0474 -0.0970 18 3 4 13.1848 0.0117 18 3 5 13.6417 0.0966 18 3 6 11.8588 0.0492 18 3 7 6.1248 -0.0271 18 3 8 -0.6358 0.0363 18 3 9 2.4517 -0.0606 18 3 10 -12.0627 0.0742 18 3 11 -1.6634 0.0810 18 3 12 2.5039 0.0324 18 4 5 0.6461 -0.0282 18 4 6 1.1808 0.2519 18 4 7 2.0667 -0.0288 18 4 8 0.4350 0.1234 18 4 9 13.4663 0.0214 18 4 10 -5.7013 -0.0990 18 4 11 -11.6028 0.0929 18 4 12 -3.3310 -0.0700 18 5 6 -17.2100 -0.0888 18 5 7 -9.0376 0.0362 18 5 8 0.2935 -0.0717 18 5 9 1.9438 0.1987 18 5 10 1.1032 -0.1190 18 5 11 -3.5010 -0.0848 18 5 12 3.2876 0.0579 18 6 7 -1.4774 0.0550 18 6 8 14.3801 0.0469 18 6 9 8.6522 -0.1499 18 6 10 -0.9212 0.1488 18 6 11 -10.5950 -0.0430 18 6 12 -2.1109 -0.0407 0 0 0 0.0 0.0 ; _shelx_fab_checksum 30020 _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 Te1 Te 0.69245(6) 0.69618(4) 0.74624(4) 0.0403(2) Uani 1 1 d . . . . . Nb1 Nb 0.77040(8) 0.89958(7) 0.61144(6) 0.0463(3) Uani 1 1 d . . . . . Nb2 Nb 0.71355(8) 0.83846(7) 0.81766(6) 0.0470(3) Uani 1 1 d . . . . . Nb3 Nb 0.66335(8) 0.63918(6) 0.94305(6) 0.0453(3) Uani 1 1 d . . . . . Nb4 Nb 0.67843(8) 0.48362(6) 0.87127(6) 0.0449(3) Uani 1 1 d . . . . . Nb5 Nb 0.74194(8) 0.54094(6) 0.68027(6) 0.0445(3) Uani 1 1 d . . . . . Nb6 Nb 0.78633(8) 0.76571(7) 0.54254(6) 0.0436(3) Uani 1 1 d . . . . . Nb7 Nb 0.89746(8) 0.55253(7) 0.76051(6) 0.0476(3) Uani 1 1 d . . . . . Nb8 Nb 0.88264(8) 0.70669(7) 0.83014(6) 0.0483(3) Uani 1 1 d . . . . . Nb9 Nb 0.94326(8) 0.77149(7) 0.62592(6) 0.0467(3) Uani 1 1 d . . . . . Cu2 Cu 0.56237(11) 0.82610(9) 0.61114(8) 0.0461(4) Uani 1 1 d . . . . . Cu4 Cu 0.92938(11) 0.63363(9) 0.58042(8) 0.0499(4) Uani 1 1 d . . . . . Cu3 Cu 0.60734(12) 0.38030(9) 0.78516(9) 0.0536(4) Uani 1 1 d . . . . . Cu1 Cu 0.55736(12) 0.79675(9) 0.98443(9) 0.0548(5) Uani 1 1 d . . . . . V1 V 0.50163(16) 0.75824(12) 0.87476(12) 0.0467(6) Uani 1 1 d . . . . . V2 V 0.52739(15) 0.53878(12) 0.77354(12) 0.0465(6) Uani 1 1 d . . . . . K1 K 0.4076(2) 0.57050(17) 0.92997(16) 0.0547(8) Uani 1 1 d . . . . . O1W O 0.4539(6) 0.7456(5) 0.7181(5) 0.057(2) Uani 1 1 d . . . . . O2W O 0.5229(6) 0.3215(4) 0.9135(4) 0.050(2) Uani 1 1 d . . . . . O3W O 0.8605(6) 0.4901(4) 0.9645(4) 0.053(2) Uani 1 1 d . . . . . O1 O 0.4247(7) 0.7536(6) 0.8473(5) 0.077(3) Uani 1 1 d . . . . . O2 O 0.4669(6) 0.7932(5) 0.9398(5) 0.052(2) Uani 1 1 d . . . . . O3 O 0.5914(5) 0.8216(5) 0.7993(5) 0.052(2) Uani 1 1 d . . . . . O4 O 0.7923(5) 0.6464(4) 0.6002(4) 0.046(2) Uani 1 1 d . . . . . O5 O 0.6922(6) 0.9223(5) 0.8355(5) 0.062(3) Uani 1 1 d . . . . . O6 O 0.6492(5) 0.7555(4) 0.9237(4) 0.043(2) Uani 1 1 d . . . . . O7 O 0.6205(6) 0.5938(5) 1.0403(5) 0.057(2) Uani 1 1 d . . . . . O8 O 0.5484(6) 0.6619(4) 0.9090(5) 0.051(2) Uani 1 1 d . . . . . O9 O 0.6711(6) 0.5474(4) 0.9231(5) 0.053(2) Uani 1 1 d . . . . . O10 O 0.6396(6) 0.3905(4) 0.9461(4) 0.049(2) Uani 1 1 d . . . . . O11 O 0.6802(5) 0.4605(4) 0.7837(4) 0.042(2) Uani 1 1 d . . . . . O12 O 0.5057(6) 0.4498(5) 0.7778(5) 0.056(2) Uani 1 1 d . . . . . O13 O 0.4339(6) 0.5875(5) 0.7738(5) 0.061(3) Uani 1 1 d . . . . . O14 O 0.5585(5) 0.5323(5) 0.8494(4) 0.047(2) Uani 1 1 d . . . . . O15 O 0.6146(6) 0.5935(4) 0.6903(4) 0.050(2) Uani 1 1 d . . . . . O16 O 0.6469(5) 0.7443(4) 0.6011(4) 0.047(2) Uani 1 1 d . . . . . O17 O 0.6351(5) 0.8580(4) 0.6555(4) 0.045(2) Uani 1 1 d . . . . . O18 O 0.7636(5) 0.8731(5) 0.5309(4) 0.049(2) Uani 1 1 d . . . . . O19 O 0.7841(5) 0.7588(4) 0.6611(4) 0.041(2) Uani 1 1 d . . . . . O20 O 0.7357(6) 0.7118(4) 0.8127(4) 0.048(2) Uani 1 1 d . . . . . O21 O 0.7474(5) 0.5985(4) 0.7609(4) 0.045(2) Uani 1 1 d . . . . . O22 O 0.7578(5) 0.8863(4) 0.7102(4) 0.043(2) Uani 1 1 d . . . . . O23 O 0.8298(6) 0.8082(5) 0.8319(4) 0.053(2) Uani 1 1 d . . . . . O24 O 0.7929(5) 0.6476(4) 0.9303(4) 0.044(2) Uani 1 1 d . . . . . O25 O 0.9005(5) 0.8826(5) 0.5890(4) 0.049(2) Uani 1 1 d . . . . . O26 O 0.8102(5) 0.4716(4) 0.8474(4) 0.049(2) Uani 1 1 d . . . . . O27 O 0.8603(5) 0.5164(5) 0.6949(4) 0.047(2) Uani 1 1 d . . . . . O28 O 1.0005(6) 0.5041(5) 0.7619(5) 0.062(3) Uani 1 1 d . . . . . O29 O 1.0626(5) 0.7895(5) 0.5854(5) 0.055(2) Uani 1 1 d . . . . . O30 O 0.9806(6) 0.7053(6) 0.8573(5) 0.067(3) Uani 1 1 d . . . . . O31 O 0.9283(6) 0.7639(5) 0.7222(4) 0.050(2) Uani 1 1 d . . . . . O32 O 0.9131(5) 0.7713(5) 0.5359(4) 0.046(2) Uani 1 1 d . . . . . O33 O 0.9334(5) 0.6546(4) 0.6641(4) 0.044(2) Uani 1 1 d . . . . . O34 O 0.7292(6) 0.4886(5) 0.6338(5) 0.056(2) Uani 1 1 d . . . . . O35 O 0.7908(6) 0.7768(5) 0.4542(4) 0.052(2) Uani 1 1 d . . . . . O36 O 0.7605(7) 1.0026(5) 0.5673(5) 0.067(3) Uani 1 1 d . . . . . O37 O 0.8968(5) 0.6109(5) 0.8159(4) 0.051(2) Uani 1 1 d . . . . . N1 N 0.4802(10) 0.8632(6) 1.0311(6) 0.061(3) Uani 1 1 d . . . . . N3 N 0.4810(7) 0.9155(6) 0.6046(6) 0.045(3) Uani 1 1 d . . . . . N4 N 0.4943(8) 0.8143(6) 0.5504(6) 0.055(3) Uani 1 1 d . . . . . N5 N 0.5606(8) 0.3104(5) 0.7556(5) 0.076(4) Uani 1 1 d . . . . . C21 C 0.4761(8) 0.3156(6) 0.7434(6) 0.105(7) Uani 1 1 d DG . . . . H21 H 0.434808 0.353617 0.751467 0.126 Uiso 1 1 calc R . . . . C22 C 0.4521(8) 0.2651(8) 0.7193(7) 0.127(8) Uani 1 1 d DG . . . . H22 H 0.394332 0.268583 0.710959 0.153 Uiso 1 1 calc R . . . . C23 C 0.5125(11) 0.2094(7) 0.7074(7) 0.117(7) Uani 1 1 d DG U . . . H23 H 0.496086 0.174885 0.690997 0.140 Uiso 1 1 calc R . . . . C24 C 0.5970(9) 0.2043(6) 0.7196(6) 0.094(5) Uani 1 1 d DG U . . . H24 H 0.638317 0.166220 0.711542 0.112 Uiso 1 1 calc R . . . . C25 C 0.6211(7) 0.2548(6) 0.7437(6) 0.089(6) Uani 1 1 d G . . . . N6 N 0.7124(10) 0.3079(7) 0.7832(7) 0.069(4) Uani 1 1 d . . . . . N7 N 0.9423(7) 0.6135(6) 0.4930(6) 0.047(3) Uani 1 1 d . . . . . N8 N 1.0638(7) 0.6238(6) 0.5502(6) 0.056(3) Uani 1 1 d . . . . . N9 N 1.0402(8) 0.8437(6) 0.3980(6) 0.062(3) Uani 1 1 d . . . . . H9A H 1.015658 0.808356 0.443879 0.074 Uiso 1 1 calc R . . . . H9B H 1.016672 0.849836 0.362877 0.074 Uiso 1 1 calc R . . . . N10 N 1.1485(10) 0.9448(7) 0.3112(7) 0.094(5) Uani 1 1 d . . . . . H10A H 1.206940 0.934538 0.293908 0.113 Uiso 1 1 d GR . . . . H10B H 1.119510 0.947134 0.279363 0.113 Uiso 1 1 d GR . . . . N11 N 1.1475(9) 0.8767(8) 0.4375(8) 0.094(5) Uani 1 1 d . . . . . H11A H 1.170080 0.828014 0.454353 0.113 Uiso 1 1 d GR . . . . H11B H 1.194461 0.911430 0.421658 0.113 Uiso 1 1 d GR . . . . C1 C 0.3974(12) 0.8824(9) 1.0337(9) 0.076(5) Uani 1 1 d . . . . . H1 H 0.366858 0.861050 1.012977 0.091 Uiso 1 1 calc R . . . . C2 C 0.3495(13) 0.9299(9) 1.0630(9) 0.086(5) Uani 1 1 d . . . . . H2 H 0.290016 0.945104 1.059165 0.103 Uiso 1 1 calc R . . . . C3 C 0.3906(15) 0.9551(11) 1.0983(11) 0.098(6) Uani 1 1 d . U . . . H3 H 0.359092 0.987827 1.120755 0.117 Uiso 1 1 calc R . . . . C4 C 0.4749(13) 0.9338(10) 1.1015(8) 0.082(5) Uani 1 1 d . . . . . H4 H 0.504708 0.950368 1.126109 0.098 Uiso 1 1 calc R . . . . C5 C 0.5184(12) 0.8849(8) 1.0660(9) 0.069(4) Uani 1 1 d . . . . . C8 C 0.7524(9) 0.8480(9) 1.0943(8) 0.153(10) Uani 1 1 d . U . . . H8 H 0.789880 0.859554 1.117021 0.184 Uiso 1 1 calc R . . . . C7 C 0.6653(10) 0.8773(7) 1.0989(7) 0.119(7) Uani 1 1 d G U . . . H7 H 0.643369 0.908808 1.124759 0.143 Uiso 1 1 calc R . . . . C6 C 0.6104(7) 0.8604(6) 1.0657(6) 0.080(5) Uani 1 1 d G . . . . N2 N 0.6425(8) 0.8143(6) 1.0279(5) 0.080(4) Uani 1 1 d G . . . . C10 C 0.7296(8) 0.7850(7) 1.0233(6) 0.091(6) Uani 1 1 d G . . . . H10 H 0.751528 0.753520 0.997433 0.109 Uiso 1 1 calc R . . . . C9 C 0.7845(7) 0.8019(9) 1.0565(8) 0.143(9) Uani 1 1 d G . . . . H9 H 0.843960 0.781909 1.053357 0.171 Uiso 1 1 calc R . . . . C11 C 0.4775(10) 0.9669(7) 0.6327(7) 0.054(4) Uani 1 1 d . . . . . H11 H 0.518118 0.960848 0.660513 0.065 Uiso 1 1 calc R . . . . C12 C 0.4202(11) 1.0265(7) 0.6242(8) 0.066(4) Uani 1 1 d . . . . . H12 H 0.421686 1.061810 0.644681 0.080 Uiso 1 1 calc R . . . . C13 C 0.3583(10) 1.0360(8) 0.5849(8) 0.066(4) Uani 1 1 d . . . . . H13 H 0.318143 1.078541 0.577767 0.080 Uiso 1 1 calc R . . . . C14 C 0.3556(9) 0.9839(8) 0.5566(7) 0.054(4) Uani 1 1 d . . . . . H14 H 0.313258 0.988099 0.530729 0.065 Uiso 1 1 calc R . . . . C15 C 0.4190(8) 0.9237(7) 0.5680(7) 0.048(3) Uani 1 1 d . . . . . C16 C 0.4243(10) 0.8632(8) 0.5392(8) 0.059(4) Uani 1 1 d . . . . . C17 C 0.3637(13) 0.8608(9) 0.5040(9) 0.083(5) Uani 1 1 d . . . . . H17 H 0.314638 0.895497 0.499282 0.100 Uiso 1 1 calc R . . . . C18 C 0.3777(12) 0.8034(10) 0.4745(10) 0.087(5) Uani 1 1 d . . . . . H18 H 0.337601 0.798372 0.450327 0.105 Uiso 1 1 calc R . . . . C19 C 0.4545(14) 0.7542(11) 0.4832(12) 0.112(7) Uani 1 1 d . . . . . H19 H 0.469197 0.717903 0.462028 0.135 Uiso 1 1 calc R . . . . C20 C 0.5067(11) 0.7613(9) 0.5232(9) 0.070(4) Uani 1 1 d . . . . . H20 H 0.554667 0.725901 0.531854 0.084 Uiso 1 1 calc R . . . . C26 C 0.7034(12) 0.2572(8) 0.7591(8) 0.067(4) Uani 1 1 d . . . . . C27 C 0.7732(15) 0.2045(11) 0.7546(12) 0.107(7) Uani 1 1 d . . . . . H27 H 0.766527 0.165088 0.739975 0.128 Uiso 1 1 calc R . . . . C28 C 0.8502(14) 0.2095(11) 0.7708(12) 0.105(7) Uani 1 1 d . . . . . H28 H 0.899815 0.176576 0.764970 0.126 Uiso 1 1 calc R . . . . C29 C 0.8530(13) 0.2638(10) 0.7959(10) 0.094(6) Uani 1 1 d . . . . . H29 H 0.903662 0.266519 0.811424 0.113 Uiso 1 1 calc R . . . . C30 C 0.7841(13) 0.3143(8) 0.7990(9) 0.079(5) Uani 1 1 d . . . . . H30 H 0.789272 0.354529 0.813025 0.095 Uiso 1 1 calc R . . . . C31 C 0.8743(10) 0.6073(7) 0.4688(6) 0.053(4) Uani 1 1 d . . . . . H31 H 0.813433 0.615704 0.492348 0.064 Uiso 1 1 calc R . . . . C32 C 0.8914(10) 0.5892(8) 0.4107(7) 0.060(4) Uani 1 1 d . . . . . H32 H 0.842473 0.583274 0.394822 0.072 Uiso 1 1 calc R . . . . C33 C 0.9799(11) 0.5792(8) 0.3749(8) 0.064(4) Uani 1 1 d . . . . . H33 H 0.992324 0.565072 0.335069 0.077 Uiso 1 1 calc R . . . . C34 C 1.0473(10) 0.5897(8) 0.3967(7) 0.058(4) Uani 1 1 d . . . . . H34 H 1.108929 0.585795 0.371062 0.069 Uiso 1 1 calc R . . . . C35 C 1.0283(9) 0.6058(7) 0.4550(7) 0.053(4) Uani 1 1 d . . . . . C36 C 1.0960(10) 0.6146(7) 0.4868(8) 0.059(4) Uani 1 1 d . . . . . C37 C 1.1908(10) 0.6136(9) 0.4554(9) 0.074(5) Uani 1 1 d . . . . . H37 H 1.214300 0.609475 0.409872 0.089 Uiso 1 1 calc R . . . . C38 C 1.2499(11) 0.6187(10) 0.4917(9) 0.080(5) Uani 1 1 d . . . . . H38 H 1.314030 0.617540 0.471471 0.096 Uiso 1 1 calc R . . . . C39 C 1.2147(10) 0.6253(10) 0.5569(10) 0.077(5) Uani 1 1 d . . . . . H39 H 1.254030 0.627386 0.582944 0.092 Uiso 1 1 calc R . . . . C40 C 1.1219(10) 0.6290(9) 0.5841(8) 0.072(5) Uani 1 1 d . . . . . H40 H 1.098078 0.635479 0.628371 0.086 Uiso 1 1 calc R . . . . C41 C 1.1104(13) 0.8864(11) 0.3822(8) 0.084(5) Uani 1 1 d . . . . . N12 N 0.9948(10) 0.9196(6) 0.6868(7) 0.082(4) Uani 1 1 d . U . . . H12A H 0.988426 0.914425 0.735482 0.099 Uiso 1 1 d GR . . . . H12B H 0.934757 0.929868 0.684262 0.099 Uiso 1 1 d GR . . . . O4W O 0.3022(7) 0.4490(9) 0.8385(7) 0.113(4) Uani 1 1 d . U . . . O5W O 0.6271(10) 1.0346(7) 0.7040(8) 0.125(5) Uani 1 1 d . . . . . N13 N 1.1235(10) 1.0246(8) 0.6185(8) 0.093(5) Uani 1 1 d . . . . . H13A H 1.163830 1.042971 0.572908 0.112 Uiso 1 1 d GR . . . . H13B H 1.094842 1.066040 0.623908 0.112 Uiso 1 1 d GR . . . . N14 N 1.0305(11) 0.9919(10) 0.5658(9) 0.114(6) Uani 1 1 d D . . . . H14A H 1.008668 0.948871 0.568642 0.137 Uiso 1 1 d GR . . . . H14B H 0.986749 1.026089 0.564856 0.137 Uiso 1 1 d GR . . . . C42 C 1.0621(14) 0.9750(11) 0.6251(10) 0.100(6) Uani 1 1 d D U . . . 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 Te1 0.0444(5) 0.0380(4) 0.0343(4) -0.0171(4) -0.0028(4) -0.0025(4) Nb1 0.0548(8) 0.0385(6) 0.0395(7) -0.0126(5) -0.0105(6) -0.0057(6) Nb2 0.0578(8) 0.0410(6) 0.0421(7) -0.0213(6) -0.0077(6) -0.0055(6) Nb3 0.0544(8) 0.0411(6) 0.0359(6) -0.0192(5) -0.0019(5) -0.0042(6) Nb4 0.0531(8) 0.0401(6) 0.0356(6) -0.0190(5) -0.0006(5) -0.0012(5) Nb5 0.0488(7) 0.0431(6) 0.0362(6) -0.0201(6) -0.0004(5) -0.0002(5) Nb6 0.0465(7) 0.0457(7) 0.0343(6) -0.0170(5) -0.0059(5) -0.0020(5) Nb7 0.0469(7) 0.0495(7) 0.0382(7) -0.0187(6) -0.0026(5) 0.0018(6) Nb8 0.0507(8) 0.0535(7) 0.0395(7) -0.0201(6) -0.0096(6) -0.0060(6) Nb9 0.0447(7) 0.0506(7) 0.0374(7) -0.0161(6) -0.0043(5) -0.0083(6) Cu2 0.0491(10) 0.0452(9) 0.0441(9) -0.0208(8) -0.0122(7) 0.0028(7) Cu4 0.0453(10) 0.0557(10) 0.0413(9) -0.0221(8) -0.0014(7) 0.0006(8) Cu3 0.0656(11) 0.0436(9) 0.0493(10) -0.0258(8) -0.0041(8) -0.0028(8) Cu1 0.0708(12) 0.0477(9) 0.0466(10) -0.0275(8) -0.0062(8) -0.0025(8) V1 0.0586(15) 0.0401(12) 0.0367(12) -0.0231(10) 0.0052(11) -0.0103(11) V2 0.0477(14) 0.0428(12) 0.0425(13) -0.0230(11) 0.0055(10) -0.0097(10) K1 0.0586(19) 0.0529(17) 0.0456(17) -0.0250(15) 0.0017(14) -0.0073(15) O1W 0.063(6) 0.045(5) 0.042(5) -0.007(4) -0.004(4) 0.000(4) O2W 0.056(6) 0.042(5) 0.045(5) -0.020(4) -0.001(4) -0.001(4) O3W 0.074(6) 0.037(5) 0.028(5) 0.000(4) -0.013(4) 0.008(4) O1 0.081(8) 0.072(7) 0.054(6) -0.027(5) 0.006(5) 0.017(6) O2 0.056(6) 0.058(5) 0.046(5) -0.031(5) -0.007(4) 0.000(4) O3 0.046(5) 0.063(6) 0.052(5) -0.035(5) -0.008(4) 0.004(4) O4 0.043(5) 0.052(5) 0.043(5) -0.030(4) 0.001(4) 0.000(4) O5 0.080(7) 0.049(5) 0.064(6) -0.033(5) -0.011(5) -0.009(5) O6 0.055(5) 0.030(4) 0.049(5) -0.023(4) -0.011(4) -0.002(4) O7 0.069(6) 0.043(5) 0.052(6) -0.023(4) -0.004(5) -0.002(4) O8 0.051(5) 0.042(5) 0.052(5) -0.022(4) 0.000(4) -0.011(4) O9 0.057(6) 0.043(5) 0.048(5) -0.023(4) 0.003(4) 0.002(4) O10 0.056(6) 0.046(5) 0.033(5) -0.016(4) 0.006(4) -0.011(4) O11 0.040(5) 0.046(5) 0.040(5) -0.026(4) 0.001(4) -0.006(4) O12 0.055(6) 0.051(5) 0.060(6) -0.024(5) -0.013(5) -0.007(4) O13 0.057(6) 0.054(5) 0.060(6) -0.023(5) -0.003(5) -0.003(5) O14 0.047(5) 0.052(5) 0.041(5) -0.028(4) 0.002(4) -0.008(4) O15 0.053(5) 0.044(5) 0.038(5) -0.016(4) 0.005(4) -0.003(4) O16 0.046(5) 0.045(5) 0.052(5) -0.027(4) -0.013(4) 0.007(4) O17 0.049(5) 0.045(5) 0.049(5) -0.028(4) -0.011(4) -0.002(4) O18 0.042(5) 0.054(5) 0.048(5) -0.022(4) -0.011(4) 0.003(4) O19 0.050(5) 0.035(4) 0.028(4) -0.012(4) -0.001(4) 0.003(4) O20 0.068(6) 0.041(5) 0.037(5) -0.020(4) -0.014(4) 0.001(4) O21 0.054(5) 0.039(4) 0.037(5) -0.019(4) -0.004(4) 0.012(4) O22 0.047(5) 0.038(4) 0.041(5) -0.017(4) -0.010(4) -0.003(4) O23 0.065(6) 0.054(5) 0.038(5) -0.019(4) -0.007(4) -0.017(5) O24 0.052(5) 0.044(5) 0.039(5) -0.020(4) -0.012(4) 0.002(4) O25 0.043(5) 0.063(5) 0.041(5) -0.019(4) -0.011(4) -0.013(4) O26 0.051(5) 0.047(5) 0.039(5) -0.020(4) 0.001(4) 0.001(4) O27 0.041(5) 0.049(5) 0.040(5) -0.017(4) -0.001(4) 0.003(4) O28 0.053(6) 0.062(6) 0.054(6) -0.016(5) -0.013(5) 0.022(5) O29 0.043(5) 0.067(6) 0.048(5) -0.020(5) -0.005(4) -0.017(4) O30 0.066(7) 0.085(7) 0.056(6) -0.033(6) -0.023(5) -0.004(5) O31 0.057(6) 0.051(5) 0.034(5) -0.015(4) -0.004(4) -0.007(4) O32 0.038(5) 0.053(5) 0.036(5) -0.018(4) 0.006(4) -0.010(4) O33 0.042(5) 0.050(5) 0.037(5) -0.016(4) -0.009(4) 0.001(4) O34 0.063(6) 0.071(6) 0.045(5) -0.037(5) -0.010(4) 0.001(5) O35 0.065(6) 0.056(5) 0.030(5) -0.016(4) -0.012(4) 0.005(5) O36 0.093(8) 0.042(5) 0.066(7) -0.015(5) -0.039(6) 0.007(5) O37 0.048(5) 0.052(5) 0.043(5) -0.012(4) -0.012(4) -0.003(4) N1 0.094(11) 0.054(7) 0.048(7) -0.040(6) -0.007(7) -0.006(7) N3 0.040(6) 0.043(6) 0.052(7) -0.023(5) -0.012(5) 0.001(5) N4 0.066(8) 0.056(7) 0.068(8) -0.042(6) -0.037(6) 0.024(6) N5 0.114(12) 0.062(8) 0.044(7) -0.019(7) -0.017(7) -0.006(8) C21 0.140(19) 0.097(14) 0.090(14) -0.041(12) -0.037(13) -0.040(13) C22 0.19(2) 0.097(15) 0.14(2) -0.054(15) -0.088(18) -0.018(16) C23 0.175(18) 0.095(14) 0.124(18) -0.072(14) -0.065(17) 0.007(15) C24 0.128(10) 0.081(8) 0.083(9) -0.051(7) -0.022(7) 0.000(7) C25 0.137(18) 0.075(11) 0.049(10) -0.043(9) 0.009(10) -0.016(12) N6 0.086(10) 0.053(8) 0.054(8) -0.031(6) 0.012(7) -0.003(7) N7 0.045(7) 0.042(6) 0.043(6) -0.016(5) -0.007(5) 0.010(5) N8 0.049(7) 0.062(7) 0.042(7) -0.024(6) 0.002(6) 0.012(6) N9 0.068(8) 0.064(7) 0.043(7) -0.013(6) -0.006(6) -0.043(7) N10 0.086(10) 0.085(10) 0.060(9) -0.018(8) 0.028(7) -0.003(9) N11 0.078(10) 0.074(9) 0.106(13) -0.017(9) -0.021(9) -0.026(8) C1 0.060(11) 0.082(11) 0.074(11) -0.040(10) 0.008(9) -0.003(9) C2 0.100(14) 0.078(11) 0.074(12) -0.045(10) -0.003(10) 0.007(10) C3 0.105(10) 0.092(9) 0.092(9) -0.051(8) -0.009(7) 0.010(8) C4 0.117(15) 0.090(12) 0.042(9) -0.040(9) -0.001(9) -0.033(11) C5 0.086(12) 0.055(9) 0.065(10) -0.036(9) -0.009(9) 0.011(9) C8 0.133(18) 0.25(3) 0.18(2) -0.18(2) -0.039(18) -0.005(18) C7 0.122(15) 0.142(19) 0.123(17) -0.086(16) -0.022(15) -0.032(14) C6 0.138(17) 0.063(10) 0.042(9) -0.023(8) -0.024(10) -0.019(11) N2 0.086(11) 0.091(10) 0.057(8) -0.028(8) -0.015(7) -0.011(8) C10 0.091(14) 0.138(16) 0.076(12) -0.062(12) -0.037(11) -0.013(13) C9 0.14(2) 0.17(2) 0.18(3) -0.13(2) -0.082(19) 0.030(18) C11 0.072(10) 0.042(8) 0.055(9) -0.025(7) -0.020(7) -0.003(7) C12 0.094(12) 0.034(7) 0.079(11) -0.035(8) -0.026(10) 0.024(8) C13 0.071(11) 0.046(8) 0.058(10) -0.008(8) -0.014(8) 0.015(8) C14 0.055(9) 0.065(9) 0.043(8) -0.025(7) -0.015(7) 0.009(7) C15 0.040(8) 0.036(7) 0.066(9) -0.021(7) -0.013(7) -0.008(6) C16 0.057(9) 0.051(8) 0.060(10) -0.021(8) -0.009(7) -0.003(7) C17 0.121(16) 0.060(10) 0.077(12) -0.025(9) -0.052(11) 0.016(10) C18 0.091(13) 0.104(13) 0.104(14) -0.070(12) -0.046(11) 0.022(11) C19 0.131(18) 0.101(14) 0.17(2) -0.092(15) -0.094(17) 0.061(13) C20 0.074(11) 0.070(10) 0.104(13) -0.055(10) -0.056(10) 0.028(8) C26 0.093(13) 0.053(9) 0.054(9) -0.035(8) -0.007(9) 0.015(9) C27 0.104(16) 0.087(13) 0.130(18) -0.065(13) -0.013(14) 0.025(13) C28 0.088(15) 0.074(12) 0.128(18) -0.052(12) 0.006(13) 0.025(11) C29 0.092(14) 0.081(12) 0.108(15) -0.049(12) -0.018(11) 0.011(11) C30 0.090(14) 0.036(8) 0.087(13) -0.018(8) -0.010(11) 0.013(9) C31 0.062(9) 0.063(9) 0.025(7) -0.019(7) -0.003(6) 0.008(7) C32 0.057(10) 0.081(10) 0.047(8) -0.038(8) -0.013(7) 0.020(8) C33 0.085(12) 0.049(8) 0.061(10) -0.029(8) -0.017(9) 0.003(8) C34 0.059(10) 0.060(9) 0.046(8) -0.030(7) 0.003(7) 0.013(7) C35 0.053(9) 0.036(7) 0.046(8) -0.008(6) -0.001(7) 0.011(6) C36 0.067(10) 0.042(8) 0.049(9) -0.019(7) 0.001(8) 0.014(7) C37 0.053(10) 0.078(11) 0.077(11) -0.042(9) 0.015(9) -0.009(8) C38 0.046(10) 0.110(14) 0.082(12) -0.050(11) 0.000(9) -0.009(9) C39 0.041(9) 0.105(13) 0.102(14) -0.063(11) -0.014(9) -0.003(9) C40 0.061(11) 0.082(11) 0.049(9) -0.018(8) -0.003(8) 0.012(9) C41 0.099(14) 0.108(14) 0.039(10) -0.032(10) -0.010(9) 0.002(12) N12 0.121(8) 0.039(5) 0.048(6) -0.018(5) 0.028(6) -0.011(6) O4W 0.065(7) 0.186(11) 0.088(8) -0.055(8) -0.029(6) -0.006(7) O5W 0.158(13) 0.090(9) 0.162(14) -0.068(9) -0.081(11) 0.036(9) N13 0.102(12) 0.097(10) 0.084(11) -0.036(9) -0.022(8) -0.044(9) N14 0.115(14) 0.125(14) 0.122(14) -0.056(12) -0.048(11) -0.024(11) C42 0.111(10) 0.099(9) 0.099(10) -0.052(8) -0.030(8) 0.002(8) 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' 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 O19 Te1 O21 96.6(3) . . ? O20 Te1 O19 95.8(4) . . ? O20 Te1 O21 95.4(3) . . ? O17 Nb1 O19 77.4(3) . . ? O18 Nb1 O17 81.6(3) . . ? O18 Nb1 O19 75.6(3) . . ? O22 Nb1 O17 84.8(3) . . ? O22 Nb1 O18 159.0(3) . . ? O22 Nb1 O19 85.9(3) . . ? O22 Nb1 O25 93.9(3) . . ? O25 Nb1 O17 151.6(3) . . ? O25 Nb1 O18 90.6(3) . . ? O25 Nb1 O19 74.3(3) . . ? O36 Nb1 O17 102.5(4) . . ? O36 Nb1 O18 99.0(4) . . ? O36 Nb1 O19 174.6(4) . . ? O36 Nb1 O22 99.5(4) . . ? O36 Nb1 O25 105.7(4) . . ? O3 Nb2 O20 78.1(3) . . ? O5 Nb2 O3 102.9(4) . . ? O5 Nb2 O6 97.2(4) . . ? O5 Nb2 O20 171.6(3) . . ? O5 Nb2 O22 101.8(4) . . ? O5 Nb2 O23 103.5(4) . . ? O6 Nb2 O3 82.1(3) . . ? O6 Nb2 O20 74.6(3) . . ? O22 Nb2 O3 82.8(3) . . ? O22 Nb2 O6 157.9(3) . . ? O22 Nb2 O20 86.6(3) . . ? O23 Nb2 O3 153.3(3) . . ? O23 Nb2 O6 91.0(3) . . ? O23 Nb2 O20 75.2(3) . . ? O23 Nb2 O22 95.4(3) . . ? O6 Nb3 K1 147.9(2) . 2_667 ? O6 Nb3 O20 75.6(3) . . ? O7 Nb3 K1 51.1(3) . 2_667 ? O7 Nb3 O6 99.5(3) . . ? O7 Nb3 O8 103.8(4) . . ? O7 Nb3 O9 100.2(4) . . ? O7 Nb3 O20 171.9(4) . . ? O7 Nb3 O24 100.4(4) . . ? O8 Nb3 K1 93.5(2) . 2_667 ? O8 Nb3 O6 80.3(3) . . ? O8 Nb3 O20 82.0(3) . . ? O9 Nb3 K1 49.3(2) . 2_667 ? O9 Nb3 O6 157.7(3) . . ? O9 Nb3 O8 85.1(3) . . ? O9 Nb3 O20 85.8(3) . . ? O20 Nb3 K1 135.08(19) . 2_667 ? O24 Nb3 K1 105.7(2) . 2_667 ? O24 Nb3 O6 90.8(3) . . ? O24 Nb3 O8 155.3(3) . . ? O24 Nb3 O9 95.6(3) . . ? O24 Nb3 O20 73.5(3) . . ? O9 Nb4 K1 50.4(2) . 2_667 ? O9 Nb4 O11 156.6(3) . . ? O9 Nb4 O14 87.6(3) . . ? O9 Nb4 O21 86.0(3) . . ? O9 Nb4 O26 97.2(4) . . ? O10 Nb4 K1 50.8(3) . 2_667 ? O10 Nb4 O9 101.2(4) . . ? O10 Nb4 O11 100.0(3) . . ? O10 Nb4 O14 102.4(4) . . ? O10 Nb4 O21 171.0(3) . . ? O10 Nb4 O26 100.6(4) . . ? O11 Nb4 K1 148.4(2) . 2_667 ? O11 Nb4 O21 74.0(3) . . ? O14 Nb4 K1 94.9(2) . 2_667 ? O14 Nb4 O11 78.3(3) . . ? O14 Nb4 O21 83.2(3) . . ? O21 Nb4 K1 136.4(2) . 2_667 ? O26 Nb4 K1 107.1(2) . 2_667 ? O26 Nb4 O11 88.5(3) . . ? O26 Nb4 O14 155.1(3) . . ? O26 Nb4 O21 72.8(3) . . ? O4 Nb5 Cu4 39.3(2) . . ? O4 Nb5 O11 157.0(3) . . ? O4 Nb5 O15 85.8(3) . . ? O4 Nb5 O21 83.6(3) . . ? O11 Nb5 Cu4 141.5(2) . . ? O11 Nb5 O15 83.8(3) . . ? O11 Nb5 O21 74.3(3) . . ? O15 Nb5 Cu4 124.4(2) . . ? O15 Nb5 O21 79.8(3) . . ? O21 Nb5 Cu4 84.77(19) . . ? O27 Nb5 Cu4 51.4(2) . . ? O27 Nb5 O4 89.4(3) . . ? O27 Nb5 O11 91.7(3) . . ? O27 Nb5 O15 155.6(3) . . ? O27 Nb5 O21 75.8(3) . . ? O34 Nb5 Cu4 102.3(3) . . ? O34 Nb5 O4 104.4(4) . . ? O34 Nb5 O11 97.6(4) . . ? O34 Nb5 O15 99.1(4) . . ? O34 Nb5 O21 171.9(3) . . ? O34 Nb5 O27 105.3(4) . . ? O4 Nb6 Cu4 39.2(2) . . ? O4 Nb6 O16 83.7(3) . . ? O4 Nb6 O19 80.7(3) . . ? O16 Nb6 Cu4 121.9(2) . . ? O16 Nb6 O19 78.3(3) . . ? O18 Nb6 Cu4 141.0(2) . . ? O18 Nb6 O4 155.6(3) . . ? O18 Nb6 O16 84.5(3) . . ? O18 Nb6 O19 76.0(3) . . ? O19 Nb6 Cu4 81.79(18) . . ? O32 Nb6 Cu4 48.3(2) . . ? O32 Nb6 O4 86.3(3) . . ? O32 Nb6 O16 152.9(3) . . ? O32 Nb6 O18 94.7(3) . . ? O32 Nb6 O19 75.3(3) . . ? O35 Nb6 Cu4 99.7(3) . . ? O35 Nb6 O4 102.6(3) . . ? O35 Nb6 O16 103.5(4) . . ? O35 Nb6 O18 100.9(4) . . ? O35 Nb6 O19 176.4(3) . . ? O35 Nb6 O32 103.2(4) . . ? O26 Nb7 O21 72.5(3) . . ? O26 Nb7 O27 88.5(3) . . ? O26 Nb7 O33 154.6(3) . . ? O27 Nb7 O21 74.7(3) . . ? O27 Nb7 O33 82.1(3) . . ? O28 Nb7 O21 170.4(4) . . ? O28 Nb7 O26 101.3(4) . . ? O28 Nb7 O27 98.2(4) . . ? O28 Nb7 O33 103.4(4) . . ? O28 Nb7 O37 102.0(4) . . ? O33 Nb7 O21 82.3(3) . . ? O37 Nb7 O21 85.6(3) . . ? O37 Nb7 O26 91.2(3) . . ? O37 Nb7 O27 159.4(3) . . ? O37 Nb7 O33 89.6(3) . . ? O23 Nb8 O20 74.1(3) . . ? O24 Nb8 O20 72.5(3) . . ? O24 Nb8 O23 88.3(3) . . ? O30 Nb8 O20 169.7(4) . . ? O30 Nb8 O23 99.6(4) . . ? O30 Nb8 O24 99.5(4) . . ? O30 Nb8 O31 102.4(4) . . ? O30 Nb8 O37 100.7(4) . . ? O31 Nb8 O20 85.7(3) . . ? O31 Nb8 O23 88.2(3) . . ? O31 Nb8 O24 158.1(3) . . ? O37 Nb8 O20 85.9(3) . . ? O37 Nb8 O23 159.6(3) . . ? O37 Nb8 O24 89.5(3) . . ? O37 Nb8 O31 86.3(3) . . ? O19 Nb9 Cu4 82.16(19) . . ? O25 Nb9 Cu4 131.0(2) . . ? O25 Nb9 O19 74.7(3) . . ? O25 Nb9 O32 84.6(3) . . ? O29 Nb9 Cu4 96.1(3) . . ? O29 Nb9 O19 171.3(3) . . ? O29 Nb9 O25 100.5(4) . . ? O29 Nb9 O31 101.2(4) . . ? O29 Nb9 O32 97.8(3) . . ? O29 Nb9 O33 101.1(4) . . ? O31 Nb9 Cu4 128.7(2) . . ? O31 Nb9 O19 86.4(3) . . ? O31 Nb9 O25 92.6(3) . . ? O31 Nb9 O32 161.0(3) . . ? O31 Nb9 O33 92.6(3) . . ? O32 Nb9 Cu4 47.4(2) . . ? O32 Nb9 O19 74.7(3) . . ? O33 Nb9 Cu4 36.5(2) . . ? O33 Nb9 O19 82.7(3) . . ? O33 Nb9 O25 156.4(3) . . ? O33 Nb9 O32 83.1(3) . . ? O16 Cu2 O1W 98.0(3) . . ? O16 Cu2 N3 171.2(4) . . ? O16 Cu2 N4 92.3(4) . . ? O17 Cu2 O1W 98.9(3) . . ? O17 Cu2 O16 92.5(3) . . ? O17 Cu2 N3 92.1(4) . . ? O17 Cu2 N4 169.0(4) . . ? N3 Cu2 O1W 88.7(4) . . ? N3 Cu2 N4 81.9(4) . . ? N4 Cu2 O1W 90.2(4) . . ? Nb5 Cu4 Nb6 77.09(5) . . ? Nb5 Cu4 Nb9 107.44(5) . . ? Nb6 Cu4 Nb9 65.49(4) . . ? O4 Cu4 Nb5 38.2(2) . . ? O4 Cu4 Nb6 39.4(2) . . ? O4 Cu4 Nb9 89.9(2) . . ? O4 Cu4 O32 75.9(3) . . ? O32 Cu4 Nb5 111.33(19) . . ? O32 Cu4 Nb6 37.54(19) . . ? O32 Cu4 Nb9 40.7(2) . . ? O33 Cu4 Nb5 88.6(2) . . ? O33 Cu4 Nb6 90.2(2) . . ? O33 Cu4 Nb9 36.5(2) . . ? O33 Cu4 O4 93.8(3) . . ? O33 Cu4 O32 76.5(3) . . ? N7 Cu4 Nb5 97.7(3) . . ? N7 Cu4 Nb6 94.5(3) . . ? N7 Cu4 Nb9 142.3(3) . . ? N7 Cu4 O4 93.2(4) . . ? N7 Cu4 O32 104.2(3) . . ? N7 Cu4 O33 172.8(4) . . ? N8 Cu4 Nb5 144.5(3) . . ? N8 Cu4 Nb6 138.4(3) . . ? N8 Cu4 Nb9 93.2(3) . . ? N8 Cu4 O4 173.9(4) . . ? N8 Cu4 O32 103.2(4) . . ? N8 Cu4 O33 91.8(4) . . ? N8 Cu4 N7 81.1(5) . . ? O2W Cu3 V2 88.8(2) . . ? O11 Cu3 V2 59.4(2) . . ? O11 Cu3 O2W 99.3(3) . . ? O11 Cu3 N5 162.3(4) . . ? O11 Cu3 N6 93.0(5) . . ? O12 Cu3 V2 30.7(2) . . ? O12 Cu3 O2W 82.9(3) . . ? O12 Cu3 O11 90.1(3) . . ? O12 Cu3 N5 95.1(4) . . ? O12 Cu3 N6 174.1(5) . . ? N5 Cu3 V2 124.2(4) . . ? N5 Cu3 O2W 98.1(3) . . ? N5 Cu3 N6 80.5(6) . . ? N6 Cu3 V2 152.0(4) . . ? N6 Cu3 O2W 101.4(4) . . ? O2W Cu1 V1 90.5(2) 2_667 . ? O2 Cu1 V1 29.7(2) . . ? O2 Cu1 O2W 84.0(3) . 2_667 ? O2 Cu1 O6 91.7(3) . . ? O2 Cu1 N1 92.4(5) . . ? O2 Cu1 N2 172.3(4) . . ? O6 Cu1 V1 61.9(2) . . ? O6 Cu1 O2W 102.5(3) . 2_667 ? O6 Cu1 N1 166.5(4) . . ? N1 Cu1 V1 121.3(4) . . ? N1 Cu1 O2W 90.8(4) . 2_667 ? N2 Cu1 V1 155.4(4) . . ? N2 Cu1 O2W 100.0(4) . 2_667 ? N2 Cu1 O6 93.9(4) . . ? N2 Cu1 N1 81.0(5) . . ? Cu1 V1 K1 120.99(9) . . ? O1 V1 Cu1 145.5(4) . . ? O1 V1 K1 61.7(4) . . ? O1 V1 O2 111.3(5) . . ? O1 V1 O3 109.7(5) . . ? O1 V1 O8 108.4(5) . . ? O2 V1 Cu1 34.3(3) . . ? O2 V1 K1 115.0(3) . . ? O2 V1 O3 109.0(4) . . ? O2 V1 O8 112.5(4) . . ? O3 V1 Cu1 91.2(3) . . ? O3 V1 K1 135.2(3) . . ? O3 V1 O8 105.8(4) . . ? O8 V1 Cu1 90.9(3) . . ? O8 V1 K1 49.4(3) . . ? Cu3 V2 K1 122.93(9) . . ? O12 V2 Cu3 35.4(3) . . ? O12 V2 K1 116.2(3) . . ? O12 V2 O14 114.6(4) . . ? O12 V2 O15 110.0(4) . . ? O13 V2 Cu3 143.3(3) . . ? O13 V2 K1 60.2(3) . . ? O13 V2 O12 108.1(4) . . ? O13 V2 O14 106.0(4) . . ? O13 V2 O15 109.1(4) . . ? O14 V2 Cu3 93.4(3) . . ? O14 V2 K1 47.4(3) . . ? O14 V2 O15 108.9(4) . . ? O15 V2 Cu3 92.8(3) . . ? O15 V2 K1 133.7(3) . . ? Nb3 K1 K1 63.57(7) 2_667 2_667 ? Nb4 K1 Nb3 62.67(5) 2_667 2_667 ? Nb4 K1 K1 62.96(7) 2_667 2_667 ? V1 K1 Nb3 155.77(11) . 2_667 ? V1 K1 Nb4 96.83(8) . 2_667 ? V1 K1 V2 99.80(8) . . ? V1 K1 K1 96.45(10) . 2_667 ? V2 K1 Nb3 96.00(8) . 2_667 ? V2 K1 Nb4 154.48(10) . 2_667 ? V2 K1 K1 95.89(10) . 2_667 ? O1 K1 Nb3 166.4(2) . 2_667 ? O1 K1 Nb4 107.2(2) . 2_667 ? O1 K1 V1 25.1(2) . . ? O1 K1 V2 95.87(19) . . ? O1 K1 K1 121.6(2) . 2_667 ? O7 K1 Nb3 27.72(17) 2_667 2_667 ? O7 K1 Nb4 90.38(18) 2_667 2_667 ? O7 K1 V1 164.9(2) 2_667 . ? O7 K1 V2 69.30(18) 2_667 . ? O7 K1 K1 75.0(2) 2_667 2_667 ? O7 K1 O1 159.8(3) 2_667 . ? O7 K1 O13 78.4(2) 2_667 . ? O8 K1 Nb3 131.7(2) . 2_667 ? O8 K1 Nb4 93.0(2) . 2_667 ? O8 K1 V1 30.22(18) . . ? O8 K1 V2 91.70(19) . . ? O8 K1 K1 68.25(19) . 2_667 ? O8 K1 O1 54.4(3) . . ? O8 K1 O7 136.5(3) . 2_667 ? O8 K1 O9 116.8(3) . 2_667 ? O8 K1 O10 72.9(2) . 2_667 ? O8 K1 O13 102.8(3) . . ? O9 K1 Nb3 31.26(16) 2_667 2_667 ? O9 K1 Nb4 31.58(17) 2_667 2_667 ? O9 K1 V1 127.9(2) 2_667 . ? O9 K1 V2 126.70(18) 2_667 . ? O9 K1 K1 60.66(19) 2_667 2_667 ? O9 K1 O1 137.4(3) 2_667 . ? O9 K1 O7 58.9(2) 2_667 2_667 ? O9 K1 O10 59.7(2) 2_667 2_667 ? O9 K1 O13 135.3(3) 2_667 . ? O10 K1 Nb3 90.89(16) 2_667 2_667 ? O10 K1 Nb4 28.23(15) 2_667 2_667 ? O10 K1 V1 69.43(16) 2_667 . ? O10 K1 V2 163.8(2) 2_667 . ? O10 K1 K1 74.11(19) 2_667 2_667 ? O10 K1 O1 79.4(2) 2_667 . ? O10 K1 O7 118.6(2) 2_667 2_667 ? O10 K1 O13 159.8(3) 2_667 . ? O13 K1 Nb3 105.69(18) . 2_667 ? O13 K1 Nb4 164.17(19) . 2_667 ? O13 K1 V1 96.71(18) . . ? O13 K1 V2 27.54(17) . . ? O13 K1 K1 123.4(2) . 2_667 ? O13 K1 O1 82.3(3) . . ? O14 K1 Nb3 92.48(18) . 2_667 ? O14 K1 Nb4 131.5(2) . 2_667 ? O14 K1 V1 92.50(18) . . ? O14 K1 V2 29.03(18) . . ? O14 K1 K1 68.71(19) . 2_667 ? O14 K1 O1 101.1(3) . . ? O14 K1 O7 72.9(2) . 2_667 ? O14 K1 O8 72.6(3) . . ? O14 K1 O9 116.1(3) . 2_667 ? O14 K1 O10 136.3(3) . 2_667 ? O14 K1 O13 55.9(3) . . ? Cu3 O2W Cu1 144.8(4) . 2_667 ? V1 O1 K1 93.2(4) . . ? V1 O2 Cu1 116.0(5) . . ? V1 O3 Nb2 119.8(4) . . ? Nb5 O4 Nb6 153.5(4) . . ? Nb5 O4 Cu4 102.5(4) . . ? Cu4 O4 Nb6 101.4(3) . . ? Nb3 O6 Nb2 116.4(4) . . ? Cu1 O6 Nb2 114.9(3) . . ? Cu1 O6 Nb3 126.5(4) . . ? Nb3 O7 K1 101.2(4) . 2_667 ? Nb3 O8 K1 134.2(4) . . ? V1 O8 Nb3 123.8(4) . . ? V1 O8 K1 100.4(4) . . ? Nb3 O9 K1 99.4(3) . 2_667 ? Nb4 O9 Nb3 160.9(5) . . ? Nb4 O9 K1 98.0(3) . 2_667 ? Nb4 O10 K1 100.9(3) . 2_667 ? Nb5 O11 Nb4 118.1(4) . . ? Cu3 O11 Nb4 128.2(4) . . ? Cu3 O11 Nb5 112.4(4) . . ? V2 O12 Cu3 113.9(5) . . ? V2 O13 K1 92.2(4) . . ? Nb4 O14 K1 132.6(4) . . ? V2 O14 Nb4 122.8(4) . . ? V2 O14 K1 103.5(4) . . ? V2 O15 Nb5 114.9(4) . . ? Cu2 O16 Nb6 124.4(4) . . ? Cu2 O17 Nb1 128.7(4) . . ? Nb6 O18 Nb1 118.5(4) . . ? Te1 O19 Nb1 117.4(3) . . ? Te1 O19 Nb6 118.5(4) . . ? Te1 O19 Nb9 135.9(4) . . ? Nb1 O19 Nb6 89.2(2) . . ? Nb9 O19 Nb1 91.9(3) . . ? Nb9 O19 Nb6 92.2(3) . . ? Te1 O20 Nb2 118.5(4) . . ? Te1 O20 Nb3 118.9(4) . . ? Te1 O20 Nb8 134.1(4) . . ? Nb3 O20 Nb2 93.1(3) . . ? Nb3 O20 Nb8 92.3(3) . . ? Nb8 O20 Nb2 89.9(3) . . ? Te1 O21 Nb4 118.4(4) . . ? Te1 O21 Nb5 117.9(4) . . ? Te1 O21 Nb7 134.6(4) . . ? Nb4 O21 Nb5 93.4(3) . . ? Nb7 O21 Nb4 92.3(3) . . ? Nb7 O21 Nb5 90.4(3) . . ? Nb1 O22 Nb2 156.8(4) . . ? Nb2 O23 Nb8 120.7(4) . . ? Nb3 O24 Nb8 121.7(4) . . ? Nb1 O25 Nb9 119.1(4) . . ? Nb4 O26 Nb7 122.4(4) . . ? Nb5 O27 Nb7 119.1(4) . . ? Nb9 O31 Nb8 150.3(5) . . ? Nb6 O32 Nb9 117.7(4) . . ? Nb6 O32 Cu4 94.2(3) . . ? Nb9 O32 Cu4 91.8(3) . . ? Nb9 O33 Nb7 142.0(4) . . ? Cu4 O33 Nb7 108.9(4) . . ? Cu4 O33 Nb9 106.9(3) . . ? Nb7 O37 Nb8 152.9(4) . . ? C1 N1 Cu1 128.5(11) . . ? C1 N1 C5 116.9(14) . . ? C5 N1 Cu1 114.5(12) . . ? C11 N3 Cu2 128.8(9) . . ? C11 N3 C15 116.3(11) . . ? C15 N3 Cu2 114.9(8) . . ? C16 N4 Cu2 115.4(9) . . ? C20 N4 Cu2 127.2(9) . . ? C20 N4 C16 117.2(12) . . ? C21 N5 Cu3 125.1(7) . . ? C21 N5 C25 120.0 . . ? C25 N5 Cu3 114.8(7) . . ? N5 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C25 120.0 . . ? N5 C25 C26 112.7(10) . . ? C24 C25 N5 120.0 . . ? C24 C25 C26 127.3(10) . . ? C26 N6 Cu3 113.5(13) . . ? C30 N6 Cu3 123.5(11) . . ? C30 N6 C26 122.8(16) . . ? C31 N7 Cu4 126.1(8) . . ? C31 N7 C35 117.6(12) . . ? C35 N7 Cu4 116.3(10) . . ? C36 N8 Cu4 113.3(10) . . ? C40 N8 Cu4 126.5(10) . . ? C40 N8 C36 120.1(12) . . ? N1 C1 C2 126.4(18) . . ? C1 C2 C3 117(2) . . ? C4 C3 C2 120.1(19) . . ? C3 C4 C5 116.9(17) . . ? N1 C5 C4 122.6(16) . . ? N1 C5 C6 117.0(13) . . ? C6 C5 C4 120.4(16) . . ? C7 C8 C9 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C6 C5 127.2(10) . . ? N2 C6 C5 112.8(10) . . ? N2 C6 C7 120.0 . . ? C6 N2 Cu1 114.7(7) . . ? C6 N2 C10 120.0 . . ? C10 N2 Cu1 125.3(7) . . ? C9 C10 N2 120.0 . . ? C10 C9 C8 120.0 . . ? N3 C11 C12 124.1(13) . . ? C11 C12 C13 119.3(13) . . ? C14 C13 C12 119.9(13) . . ? C13 C14 C15 116.5(13) . . ? N3 C15 C14 123.8(12) . . ? N3 C15 C16 114.1(11) . . ? C14 C15 C16 122.1(12) . . ? N4 C16 C15 113.3(13) . . ? N4 C16 C17 125.0(14) . . ? C17 C16 C15 121.6(14) . . ? C16 C17 C18 117.5(16) . . ? C19 C18 C17 117.4(15) . . ? C20 C19 C18 118.1(16) . . ? N4 C20 C19 124.5(14) . . ? N6 C26 C25 118.3(14) . . ? N6 C26 C27 118.3(18) . . ? C27 C26 C25 123.2(16) . . ? C28 C27 C26 120.4(19) . . ? C27 C28 C29 116.9(19) . . ? C30 C29 C28 121(2) . . ? N6 C30 C29 120.5(18) . . ? N7 C31 C32 120.5(13) . . ? C31 C32 C33 120.0(14) . . ? C34 C33 C32 119.0(14) . . ? C33 C34 C35 119.7(14) . . ? N7 C35 C36 112.0(13) . . ? C34 C35 N7 123.0(14) . . ? C34 C35 C36 124.9(13) . . ? N8 C36 C35 117.0(13) . . ? N8 C36 C37 119.6(15) . . ? C37 C36 C35 123.5(14) . . ? C38 C37 C36 119.2(15) . . ? C39 C38 C37 119.5(15) . . ? C40 C39 C38 119.2(16) . . ? N8 C40 C39 122.3(15) . . ? N9 C41 N10 121.6(16) . . ? N9 C41 N11 120.0(14) . . ? N11 C41 N10 118.4(18) . . ? N13 C42 N12 133.5(17) . . ? N13 C42 N14 119.1(17) . . ? N14 C42 N12 103.7(17) . . ? 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 Te1 O19 1.868(7) . ? Te1 O20 1.869(8) . ? Te1 O21 1.889(7) . ? Nb1 O17 2.077(8) . ? Nb1 O18 2.007(8) . ? Nb1 O19 2.405(7) . ? Nb1 O22 1.932(8) . ? Nb1 O25 1.941(8) . ? Nb1 O36 1.762(8) . ? Nb2 O3 2.117(8) . ? Nb2 O5 1.766(8) . ? Nb2 O6 2.063(8) . ? Nb2 O20 2.431(8) . ? Nb2 O22 1.937(8) . ? Nb2 O23 1.897(9) . ? Nb3 K1 3.703(3) 2_667 ? Nb3 O6 2.056(7) . ? Nb3 O7 1.756(9) . ? Nb3 O8 2.050(9) . ? Nb3 O9 1.948(8) . ? Nb3 O20 2.392(8) . ? Nb3 O24 1.945(8) . ? Nb4 K1 3.656(3) 2_667 ? Nb4 O9 1.933(8) . ? Nb4 O10 1.761(7) . ? Nb4 O11 2.070(8) . ? Nb4 O14 2.070(8) . ? Nb4 O21 2.386(7) . ? Nb4 O26 1.951(8) . ? Nb5 Cu4 3.1338(19) . ? Nb5 O4 1.984(8) . ? Nb5 O11 2.006(7) . ? Nb5 O15 2.102(8) . ? Nb5 O21 2.418(8) . ? Nb5 O27 1.921(8) . ? Nb5 O34 1.734(8) . ? Nb6 Cu4 3.153(2) . ? Nb6 O4 2.041(8) . ? Nb6 O16 2.096(8) . ? Nb6 O18 1.944(8) . ? Nb6 O19 2.434(8) . ? Nb6 O32 1.927(8) . ? Nb6 O35 1.759(8) . ? Nb7 O21 2.386(8) . ? Nb7 O26 1.974(8) . ? Nb7 O27 2.032(9) . ? Nb7 O28 1.753(8) . ? Nb7 O33 2.047(7) . ? Nb7 O37 1.930(9) . ? Nb8 O20 2.391(9) . ? Nb8 O23 2.021(9) . ? Nb8 O24 2.005(8) . ? Nb8 O30 1.768(9) . ? Nb8 O31 1.952(8) . ? Nb8 O37 1.948(9) . ? Nb9 Cu4 3.203(2) . ? Nb9 O19 2.337(8) . ? Nb9 O25 2.011(8) . ? Nb9 O29 1.767(8) . ? Nb9 O31 1.910(8) . ? Nb9 O32 2.091(8) . ? Nb9 O33 1.993(8) . ? Cu2 O1W 2.306(8) . ? Cu2 O16 1.963(8) . ? Cu2 O17 1.946(8) . ? Cu2 N3 1.981(10) . ? Cu2 N4 1.983(10) . ? Cu4 O4 2.034(8) . ? Cu4 O32 2.361(8) . ? Cu4 O33 1.993(8) . ? Cu4 N7 1.991(11) . ? Cu4 N8 1.985(11) . ? Cu3 V2 3.060(3) . ? Cu3 O2W 2.382(8) . ? Cu3 O11 1.963(8) . ? Cu3 O12 1.939(9) . ? Cu3 N5 1.967(8) . ? Cu3 N6 2.015(14) . ? Cu1 V1 3.080(3) . ? Cu1 O2W 2.406(8) 2_667 ? Cu1 O2 1.929(9) . ? Cu1 O6 1.947(8) . ? Cu1 N1 2.010(11) . ? Cu1 N2 1.945(8) . ? V1 K1 3.522(3) . ? V1 O1 1.497(11) . ? V1 O2 1.699(8) . ? V1 O3 1.776(8) . ? V1 O8 1.803(8) . ? V2 K1 3.523(4) . ? V2 O12 1.709(8) . ? V2 O13 1.630(9) . ? V2 O14 1.758(8) . ? V2 O15 1.777(8) . ? K1 K1 4.539(6) 2_667 ? K1 O1 3.105(10) . ? K1 O7 2.937(8) 2_667 ? K1 O8 2.718(8) . ? K1 O9 2.846(8) 2_667 ? K1 O10 2.887(8) 2_667 ? K1 O13 3.060(10) . ? K1 O14 2.669(8) . ? N1 C1 1.282(18) . ? N1 C5 1.283(18) . ? N3 C11 1.338(15) . ? N3 C15 1.362(15) . ? N4 C16 1.355(16) . ? N4 C20 1.335(16) . ? N5 C21 1.3900 . ? N5 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.415(19) . ? N6 C26 1.305(18) . ? N6 C30 1.28(2) . ? N7 C31 1.337(16) . ? N7 C35 1.351(15) . ? N8 C36 1.357(16) . ? N8 C40 1.341(18) . ? N9 C41 1.284(19) . ? N10 C41 1.385(18) . ? N11 C41 1.39(2) . ? C1 C2 1.35(2) . ? C2 C3 1.36(2) . ? C3 C4 1.33(2) . ? C4 C5 1.43(2) . ? C5 C6 1.446(18) . ? C8 C7 1.3900 . ? C8 C9 1.3900 . ? C7 C6 1.3900 . ? C6 N2 1.3900 . ? N2 C10 1.3900 . ? C10 C9 1.3900 . ? C11 C12 1.342(17) . ? C12 C13 1.40(2) . ? C13 C14 1.372(19) . ? C14 C15 1.409(17) . ? C15 C16 1.502(18) . ? C16 C17 1.38(2) . ? C17 C18 1.44(2) . ? C18 C19 1.44(2) . ? C19 C20 1.39(2) . ? C26 C27 1.40(2) . ? C27 C28 1.36(3) . ? C28 C29 1.36(2) . ? C29 C30 1.36(2) . ? C31 C32 1.357(17) . ? C32 C33 1.379(19) . ? C33 C34 1.324(19) . ? C34 C35 1.335(18) . ? C35 C36 1.46(2) . ? C36 C37 1.408(19) . ? C37 C38 1.39(2) . ? C38 C39 1.37(2) . ? C39 C40 1.373(19) . ? N12 C42 1.43(2) . ? N13 C42 1.34(2) . ? N14 C42 1.375(15) . ? 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 0.569 -0.556 -0.569 1779.4 392.9 ?