#------------------------------------------------------------------------------
#$Date: 2021-07-05 20:33:57 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267158 $
#$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
'Yang, Zongfei'
'Shang, Jingjing'
'Yang, Yuanyuan'
'Ma, Pengtao'
'Niu, Jingyang'
'Wang, Jingping'
_publ_section_title
;
Synthesis, structures and stability of three V-substituted polyoxoniobate
clusters based on [TeNb9O33]17- units.
;
_journal_issue 22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 7610
_journal_page_last 7620
_journal_paper_doi 10.1039/d1dt00223f
_journal_volume 50
_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_depositor_comments
'Adding full bibliography for 7707201--7707203.cif.'
_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
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16 4 3 4.1323 0.2641
16 4 4 -1.7603 0.0082
16 4 5 -0.9728 0.1110
16 4 6 -2.4443 -0.0912
16 4 7 0.2332 0.1006
16 4 8 14.5838 0.0150
16 4 9 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 ?