#------------------------------------------------------------------------------
#$Date: 2022-06-14 00:54:47 +0300 (Tue, 14 Jun 2022) $
#$Revision: 276004 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/02/7130225.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_7130225
loop_
_publ_author_name
'Tanuhadi, Elias'
'Rompel, Annette'
_publ_section_title
;
 Trisubstituted 4f -- and 4d Tungstoantimonates as artificial
 Phosphoesterases for Nerve Agent Degradation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02223K
_journal_year                    2022
_chemical_formula_moiety         'C6 K3 Na21 O148 P Sb3 W28 Yb3, 28.5(O)'
_chemical_formula_sum            'C6 H80 K3 Na21 O147 P Sb3 W28 Yb3'
_chemical_formula_weight         9167.93
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_primary     direct
_audit_creation_date             2022-06-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-05 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   30.5334(6)
_cell_length_b                   30.5334(6)
_cell_length_c                   14.4965(4)
_cell_measurement_reflns_used    100211
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.91
_cell_measurement_theta_min      2.09
_cell_volume                     11704.3(5)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 500K'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      '9595 frames, detector distance = 40 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            160304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.711
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'Axo Mo'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_type              'Incoatec IuS'
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    23.090
_exptl_absorpt_correction_T_max  0.0129
_exptl_absorpt_correction_T_min  0.0025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             12090
_exptl_crystal_recrystallization_method
'evaporation from aqueous buffer solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.918
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.336
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_coef       0.000069(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         4704
_refine_ls_number_restraints     1039
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0456
_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/[σ²(Fo²)+(0.0857P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3713
_reflns_number_total             4704
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc02223k1.cif
_cod_data_source_block           elta2431_yb
_cod_original_cell_volume        11704.3(6)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               7130225
_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   0.091
_shelx_estimated_absorpt_t_min   0.091
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9568
 0.0432
2. Restrained distances
 C1-C2
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
Uanis(O37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O27) \\sim Ueq, Uanis(O2S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O35) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33)
\\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O34) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Na1(0.5) O5S(0.5) O26(0.6) O4S(0.25) Na3(0.25) O32(0.25) O34(0.25)
 O33(0.25) O35(0.25) O37(0.25) O40(0.4)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
W1 W 0.68737(5) 0.54279(5) 0.38141(12) 0.0370(4) Uani 1 1 d . U . . .
W2 W 0.62406(5) 0.48452(5) 0.16432(12) 0.0343(4) Uani 1 1 d . U . . .
W3 W 0.51834(3) 0.48166(3) 0.23810(17) 0.0382(6) Uani 1 2 d S TU P . .
W4 W 0.58264(5) 0.53889(5) 0.46028(13) 0.0387(5) Uani 1 1 d . U . . .
W5 W 0.63697(5) 0.48434(5) 0.58086(12) 0.0381(4) Uani 1 1 d . U . . .
W6 W 0.666667 0.333333 0.3865(3) 0.0361(9) Uani 1 6 d S TU P . .
Yb1 Yb 0.72866(3) 0.45732(7) 0.24369(18) 0.0351(6) Uani 1 2 d S TU P . .
Sb1 Sb 0.58498(5) 0.41502(5) 0.3727(3) 0.0298(8) Uani 1 2 d S TU P . .
K1 K 0.7350(2) 0.4699(4) 0.4774(8) 0.033(3) Uani 1 2 d S TU P . .
P1 P 0.666667 0.333333 0.151(2) 0.039(6) Uani 1 6 d S TU P . .
Na1 Na 0.6489(19) 0.6204(18) 0.165(4) 0.083(11) Uani 0.5 1 d . U P A 2
Na2 Na 0.8118(3) 0.6236(7) 0.2569(18) 0.049(5) Uani 1 2 d S TU P . .
O1 O 0.5177(7) 0.3889(8) 0.433(2) 0.039(6) Uani 1 1 d . U . . .
O2 O 0.5628(6) 0.4372(6) 0.267(3) 0.039(6) Uani 1 2 d S TU P . .
O3 O 0.6953(9) 0.5382(8) 0.510(2) 0.045(5) Uani 1 1 d . U . . .
O4 O 0.7017(7) 0.4931(8) 0.3650(19) 0.037(5) Uani 1 1 d . U . . .
O5 O 0.7425(9) 0.5953(9) 0.364(2) 0.050(6) Uani 1 1 d . U . . .
O5S O 0.652(3) 0.621(2) 0.225(6) 0.071(17) Uani 0.5 1 d . U P B 1
O6 O 0.6552(8) 0.5306(8) 0.267(2) 0.043(5) Uani 1 1 d . U . . .
O7 O 0.6496(9) 0.5784(8) 0.418(2) 0.044(5) Uani 1 1 d . U . . .
O8 O 0.6544(7) 0.4514(8) 0.1966(18) 0.035(5) Uani 1 1 d . U . . .
O9 O 0.6601(9) 0.5183(9) 0.078(2) 0.048(6) Uani 1 1 d . U . . .
O10 O 0.5710(5) 0.4290(5) 0.099(3) 0.040(6) Uani 1 2 d S TU P . .
O11 O 0.5761(11) 0.5129(11) 0.164(2) 0.053(6) Uani 1 1 d . U . A 2
O12 O 0.4872(7) 0.5128(7) 0.200(3) 0.063(8) Uani 1 2 d S TU P A .
O13 O 0.5610(9) 0.5272(8) 0.3428(18) 0.041(5) Uani 1 1 d . U . . .
O14 O 0.5200(6) 0.4800(6) 0.495(3) 0.042(7) Uani 1 2 d S TU P . .
O15 O 0.5706(9) 0.5839(9) 0.494(2) 0.049(6) Uani 1 1 d . U . . .
O16 O 0.6079(9) 0.5304(8) 0.5735(18) 0.037(5) Uani 1 1 d . U . . .
O17 O 0.5686(6) 0.4314(6) 0.603(3) 0.042(7) Uani 1 2 d S TU P . .
O18 O 0.6599(9) 0.4990(10) 0.690(2) 0.048(6) Uani 1 1 d . U . . .
O19 O 0.6535(9) 0.4383(8) 0.543(2) 0.048(6) Uani 1 1 d . U . . .
O20 O 0.666667 0.333333 0.503(6) 0.066(15) Uani 1 6 d S TU P . .
O21 O 0.6999(8) 0.3998(15) 0.365(3) 0.066(9) Uani 1 2 d S TU P . .
O22 O 0.6942(6) 0.3884(13) 0.142(3) 0.058(8) Uani 1 2 d S TU P . .
O23 O 0.7430(7) 0.4859(13) 0.081(3) 0.045(7) Uani 1 2 d S TU P I .
O24 O 0.7703(6) 0.5405(13) 0.191(3) 0.047(7) Uani 1 2 d S TU P I .
O25 O 0.8522(6) 0.7044(12) 0.375(4) 0.067(13) Uani 1 2 d S TU P C 2
O26 O 0.582(2) 0.661(2) 0.276(5) 0.081(15) Uani 0.6 1 d . U P A 1
C1 C 0.7864(10) 0.573(2) 0.044(5) 0.064(14) Uani 1 2 d DS TU P I .
C2 C 0.7647(9) 0.5295(18) 0.113(5) 0.045(9) Uani 1 2 d DS TU P . .
O4S O 0.7892(13) 0.578(3) 0.616(5) 0.038(16) Uani 0.5 2 d S TU P D 2
O1S O 0.7234(14) 0.6401(12) 0.590(3) 0.076(10) Uani 1 1 d . U . . .
O2S O 0.6367(10) 0.3633(10) 0.636(4) 0.095(6) Uani 1 2 d S TU P . .
Na3 Na 0.4611(18) 0.5389(18) 0.037(7) 0.134(14) Uani 0.5 2 d S TU P A 1
O6S O 0.7350(12) 0.6891(11) 0.377(3) 0.071(9) Uani 1 1 d . U . . .
O27 O 0.6160(10) 0.6774(11) 0.175(2) 0.058(6) Uani 1 1 d . U . . .
O28 O 0.4193(12) 0.5807(12) 0.129(5) 0.130(18) Uani 1 2 d S TU P . .
O29 O 0.5378(16) 0.6090(14) 0.114(3) 0.099(11) Uani 1 1 d . U . . .
O31 O 0.584(2) 0.539(2) -0.137(5) 0.18(2) Uani 1 1 d . U . . .
O32 O 0.532(3) 0.468(3) -0.062(10) 0.122(6) Uani 0.5 2 d S TU P E 2
O36 O 0.5221(11) 0.4779(11) 0.134(4) 0.094(12) Uani 1 2 d S TU P A 1
O30 O 0.6554(11) 0.6624(11) 0.334(3) 0.084(11) Uani 1 1 d . U . F 1
O34 O 0.6166(16) 0.3834(16) 0.063(7) 0.07(2) Uani 0.5 2 d S TU P G 1
O33 O 0.510(3) 0.490(3) -0.032(11) 0.126(3) Uani 0.5 2 d S TU P A 1
O35 O 0.623(2) 0.377(2) -0.003(9) 0.088(6) Uani 0.5 2 d S TU P H 2
O37 O 0.498(3) 0.502(3) -0.149(12) 0.15(2) Uani 0.5 2 d S TU P . .
O38 O 0.610(3) 0.471(3) -0.120(7) 0.26(4) Uani 1 1 d . U . . .
O39 O 0.871(3) 0.664(3) 0.361(6) 0.12(3) Uani 0.55(8) 1 d . U . I 1
O40 O 0.701(4) 0.608(3) -0.006(7) 0.09(3) Uani 0.4 1 d . U P J 2
O41 O 0.616(3) 0.6200(19) 0.069(3) 0.146(17) Uani 1 1 d . U . . .
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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'
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
O3 W1 O1 74.4(10) . 4_665 ?
O3 W1 O7 84.8(11) . . ?
O4 W1 O1 86.5(9) . 4_665 ?
O4 W1 O3 88.5(11) . . ?
O4 W1 O6 92.3(11) . . ?
O4 W1 O7 160.2(10) . . ?
O5 W1 O1 166.5(12) . 4_665 ?
O5 W1 O3 96.7(12) . . ?
O5 W1 O4 103.7(11) . . ?
O5 W1 O6 103.6(12) . . ?
O5 W1 O7 95.6(11) . . ?
O6 W1 O1 84.5(10) . 4_665 ?
O6 W1 O3 158.8(10) . . ?
O6 W1 O7 87.4(11) . . ?
O7 W1 O1 73.7(8) . 4_665 ?
O6 W2 O2 84.6(10) . . ?
O6 W2 O11 83.6(10) . . ?
O8 W2 O2 87.9(11) . . ?
O8 W2 O6 90.2(10) . . ?
O8 W2 O10 94.6(11) . . ?
O8 W2 O11 161.7(11) . . ?
O9 W2 O2 169.5(12) . . ?
O9 W2 O6 101.4(12) . . ?
O9 W2 O8 100.6(11) . . ?
O9 W2 O10 100.6(14) . . ?
O9 W2 O11 97.5(11) . . ?
O10 W2 O2 72.3(12) . . ?
O10 W2 O6 156.2(12) . . ?
O10 W2 O11 84.6(12) . . ?
O11 W2 O2 74.4(12) . . ?
O11 W3 O2 74.4(10) . . ?
O11 W3 O2 74.4(10) 4_665 . ?
O11 W3 O11 93.4(17) . 4_665 ?
O11 W3 O13 157.8(10) 4_665 . ?
O11 W3 O13 87.8(11) . . ?
O12 W3 O2 171.5(18) . . ?
O12 W3 O11 100.0(13) . 4_665 ?
O12 W3 O11 100.0(13) . . ?
O12 W3 O13 101.6(13) . 4_665 ?
O12 W3 O13 101.6(13) . . ?
O13 W3 O2 84.7(9) . . ?
O13 W3 O2 84.7(9) 4_665 . ?
O13 W3 O13 83.1(14) . 4_665 ?
O36 W3 O2 92(2) . . ?
O36 W3 O11 51.8(12) . 4_665 ?
O36 W3 O12 79(3) . . ?
O36 W3 O13 138.2(7) . 4_665 ?
O36 W3 O13 138.2(7) . . ?
O7 W4 O1 74.4(9) . 4_665 ?
O7 W4 O14 159.6(12) . . ?
O7 W4 O16 89.0(11) . . ?
O13 W4 O1 85.9(10) . 4_665 ?
O13 W4 O7 89.6(11) . . ?
O13 W4 O14 88.0(14) . . ?
O13 W4 O16 158.8(9) . . ?
O14 W4 O1 85.3(11) . 4_665 ?
O15 W4 O1 169.7(11) . 4_665 ?
O15 W4 O7 100.6(10) . . ?
O15 W4 O13 103.3(13) . . ?
O15 W4 O14 99.7(13) . . ?
O15 W4 O16 97.8(12) . . ?
O16 W4 O1 73.4(10) . 4_665 ?
O16 W4 O14 86.0(13) . . ?
O3 W5 O1 72.2(9) . 4_665 ?
O3 W5 O16 85.5(9) . . ?
O16 W5 O1 72.6(9) . 4_665 ?
O17 W5 O1 85.2(12) . 4_665 ?
O17 W5 O3 157.3(14) . . ?
O17 W5 O16 85.6(11) . . ?
O18 W5 O1 167.9(10) . 4_665 ?
O18 W5 O3 100.3(12) . . ?
O18 W5 O16 97.7(11) . . ?
O18 W5 O17 101.6(14) . . ?
O18 W5 O19 104.6(12) . . ?
O19 W5 O1 85.3(11) . 4_665 ?
O19 W5 O3 90.2(10) . . ?
O19 W5 O16 157.7(12) . . ?
O19 W5 O17 90.3(12) . . ?
O20 W6 O21 100.1(15) . 2_655 ?
O20 W6 O21 100.1(15) . 3_665 ?
O20 W6 O21 100.1(15) . . ?
O21 W6 O21 117.0(9) 3_665 . ?
O21 W6 O21 117.0(9) 2_655 . ?
O21 W6 O21 117.0(9) 3_665 2_655 ?
O4 Yb1 O4 68.9(10) 5_655 . ?
O4 Yb1 O23 124.8(8) . . ?
O4 Yb1 O23 124.8(8) 5_655 . ?
O8 Yb1 O4 72.8(8) . . ?
O8 Yb1 O4 72.8(8) 5_655 5_655 ?
O8 Yb1 O4 141.5(8) 5_655 . ?
O8 Yb1 O4 141.5(8) . 5_655 ?
O8 Yb1 O8 144.3(13) 5_655 . ?
O8 Yb1 O21 100.4(6) . . ?
O8 Yb1 O21 100.4(6) 5_655 . ?
O8 Yb1 O22 76.1(6) . . ?
O8 Yb1 O22 76.1(6) 5_655 . ?
O8 Yb1 O23 74.7(6) . . ?
O8 Yb1 O23 74.7(6) 5_655 . ?
O8 Yb1 O24 88.0(6) 5_655 . ?
O8 Yb1 O24 88.0(6) . . ?
O21 Yb1 O4 73.0(11) . 5_655 ?
O21 Yb1 O4 73.0(11) . . ?
O21 Yb1 O22 88.0(16) . . ?
O21 Yb1 O23 156.9(15) . . ?
O21 Yb1 O24 150.2(16) . . ?
O22 Yb1 O4 139.5(7) . . ?
O22 Yb1 O4 139.5(7) . 5_655 ?
O22 Yb1 O23 69.0(13) . . ?
O22 Yb1 O24 121.9(15) . . ?
O24 Yb1 O4 82.5(11) . . ?
O24 Yb1 O4 82.5(11) . 5_655 ?
O24 Yb1 O23 52.9(14) . . ?
O1 Sb1 O1 91.3(12) 4_665 . ?
O2 Sb1 O1 90.9(10) . . ?
O2 Sb1 O1 90.9(10) . 4_665 ?
O4 K1 O4 76.4(13) . 5_655 ?
O4 K1 O19 156.2(11) . 5_655 ?
O4 K1 O19 82.5(9) 5_655 5_655 ?
O4 K1 O19 82.5(9) . . ?
O4 K1 O19 156.2(11) 5_655 . ?
O4 K1 O21 73.9(10) 5_655 . ?
O4 K1 O21 73.9(10) . . ?
O19 K1 O19 115.5(13) . 5_655 ?
O19 K1 O21 89.9(9) . . ?
O19 K1 O21 89.9(9) 5_655 . ?
O22 P1 O22 119.2(7) 3_665 . ?
O22 P1 O22 119.2(7) . 2_655 ?
O22 P1 O22 119.2(7) 3_665 2_655 ?
O15 Na1 O11 120.3(19) 14_654 . ?
O27 Na1 O11 117(2) . . ?
O27 Na1 O15 123(2) . 14_654 ?
O41 Na1 O11 83(3) . . ?
O41 Na1 O15 123(3) . 14_654 ?
O41 Na1 O27 66(2) . . ?
O5 Na2 O5 88.7(15) 5_655 . ?
O5 Na2 O14 127.4(9) 5_655 14_654 ?
O5 Na2 O14 127.4(9) . 14_654 ?
O5 Na2 O15 168.3(12) . 18_554 ?
O5 Na2 O15 168.3(12) 5_655 14_654 ?
O5 Na2 O15 79.8(8) . 14_654 ?
O5 Na2 O15 79.8(8) 5_655 18_554 ?
O14 Na2 O15 60.3(7) 14_654 18_554 ?
O14 Na2 O15 60.4(7) 14_654 14_654 ?
O15 Na2 O15 111.5(13) 14_654 18_554 ?
O24 Na2 O5 88.4(11) . 5_655 ?
O24 Na2 O5 88.4(11) . . ?
O24 Na2 O14 124.2(17) . 14_654 ?
O24 Na2 O15 93.2(10) . 18_554 ?
O24 Na2 O15 93.2(10) . 14_654 ?
O39 Na2 O5 48(2) . 5_655 ?
O39 Na2 O5 95(3) 5_655 5_655 ?
O39 Na2 O5 95(3) . . ?
O39 Na2 O5 48(2) 5_655 . ?
O39 Na2 O14 88(2) 5_655 14_654 ?
O39 Na2 O14 88(2) . 14_654 ?
O39 Na2 O15 76(3) . 18_554 ?
O39 Na2 O15 131(2) . 14_654 ?
O39 Na2 O15 76(3) 5_655 14_654 ?
O39 Na2 O15 131(2) 5_655 18_554 ?
O39 Na2 O24 136(2) 5_655 . ?
O39 Na2 O24 136(2) . . ?
O39 Na2 O39 66(5) . 5_655 ?
W1 O1 W4 93.7(7) 4_665 4_665 ?
W1 O1 W5 95.0(9) 4_665 4_665 ?
W5 O1 W4 94.1(10) 4_665 4_665 ?
Sb1 O1 W1 114.6(11) . 4_665 ?
Sb1 O1 W4 137.3(12) . 4_665 ?
Sb1 O1 W5 113.3(9) . 4_665 ?
W2 O2 W2 94.6(15) 4_665 . ?
W2 O2 W3 92.7(11) . . ?
W2 O2 W3 92.7(11) 4_665 . ?
Sb1 O2 W2 115.1(10) . 4_665 ?
Sb1 O2 W2 115.1(10) . . ?
Sb1 O2 W3 137.4(18) . . ?
W1 O3 W5 118.0(12) . . ?
W1 O4 Yb1 139.5(14) . . ?
W1 O4 K1 121.2(13) . . ?
K1 O4 Yb1 94.3(8) . . ?
W1 O5 Na2 136.8(16) . . ?
W1 O5 O39 161(3) . 5_655 ?
O39 O5 Na2 60(3) 5_655 . ?
W1 O6 W2 147.7(13) . . ?
W4 O7 W1 118.1(11) . . ?
W2 O8 Yb1 145.9(11) . . ?
W2 O10 W2 120(2) 4_665 . ?
W2 O11 Na1 100.0(15) . . ?
W3 O11 W2 118.5(14) . . ?
W3 O11 Na1 124.7(15) . . ?
W3 O12 Na3 139(3) . . ?
W4 O13 W3 153.0(14) . . ?
W4 O14 W4 149(2) 4_665 . ?
W4 O14 Na2 100.5(10) . 9_565 ?
W4 O14 Na2 100.5(10) 4_665 9_565 ?
W4 O15 Na1 125.8(16) . 9_565 ?
W4 O15 Na2 98.3(10) . 9_565 ?
Na1 O15 Na2 133.0(15) 9_565 9_565 ?
W4 O16 W5 119.9(12) . . ?
W5 O17 W5 148.8(19) 4_665 . ?
W5 O19 K1 116.8(11) . . ?
W6 O21 Yb1 141(3) . . ?
W6 O21 K1 129(2) . . ?
Yb1 O21 K1 90.4(14) . . ?
P1 O22 Yb1 136(3) . . ?
C2 O23 Yb1 86(3) . . ?
Yb1 O24 Na2 137(2) . . ?
C2 O24 Yb1 95(3) . . ?
C2 O24 Na2 128(4) . . ?
C1 C1 C2 90(10) 5_655 . ?
O23 C2 C1 117(6) . . ?
O23 C2 C1 117(6) . 5_655 ?
O24 C2 O23 126(5) . . ?
O24 C2 C1 116(5) . 5_655 ?
O24 C2 C1 116(5) . . ?
C1 C2 C1 0(4) 5_655 . ?
O28 Na3 O12 89(3) . . ?
O28 Na3 O29 80(3) . 4_665 ?
O28 Na3 O29 80(3) . . ?
O28 Na3 O33 170(5) . . ?
O29 Na3 O12 65(2) 4_665 . ?
O29 Na3 O12 65(2) . . ?
O29 Na3 O29 126(4) . 4_665 ?
O29 Na3 O33 96(3) . . ?
O29 Na3 O33 96(3) 4_665 . ?
O33 Na3 O12 81(4) . . ?
O37 O33 Na3 90(8) . . ?
O5 O39 Na2 72(3) 5_655 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 2.26(2) 4_665 ?
W1 O3 1.90(3) . ?
W1 O4 1.79(2) . ?
W1 O5 1.66(2) . ?
W1 O6 1.86(3) . ?
W1 O7 2.01(2) . ?
W2 O2 2.26(3) . ?
W2 O6 1.94(3) . ?
W2 O8 1.74(2) . ?
W2 O9 1.64(3) . ?
W2 O10 1.912(19) . ?
W2 O11 2.04(2) . ?
W3 O2 2.39(3) . ?
W3 O11 1.87(3) . ?
W3 O11 1.87(3) 4_665 ?
W3 O12 1.74(4) . ?
W3 O13 2.03(2) 4_665 ?
W3 O13 2.03(2) . ?
W3 O36 1.52(5) . ?
W4 O1 2.33(2) 4_665 ?
W4 O7 1.88(2) . ?
W4 O13 1.80(3) . ?
W4 O14 1.924(11) . ?
W4 O15 1.66(2) . ?
W4 O16 1.89(3) . ?
W5 O1 2.28(3) 4_665 ?
W5 O3 2.00(3) . ?
W5 O16 2.00(2) . ?
W5 O17 1.923(9) . ?
W5 O18 1.70(3) . ?
W5 O19 1.80(2) . ?
W6 O20 1.69(8) . ?
W6 O21 1.78(4) 3_665 ?
W6 O21 1.78(4) 2_655 ?
W6 O21 1.78(4) . ?
Yb1 O4 2.42(2) . ?
Yb1 O4 2.42(2) 5_655 ?
Yb1 O8 2.29(2) 5_655 ?
Yb1 O8 2.29(2) . ?
Yb1 O21 2.32(4) . ?
Yb1 O22 2.34(4) . ?
Yb1 O23 2.47(4) . ?
Yb1 O24 2.33(4) . ?
Sb1 O1 1.99(2) . ?
Sb1 O1 1.99(2) 4_665 ?
Sb1 O2 1.93(4) . ?
K1 O4 2.22(3) . ?
K1 O4 2.22(3) 5_655 ?
K1 O19 2.37(2) . ?
K1 O19 2.37(2) 5_655 ?
K1 O21 2.47(5) . ?
P1 O22 1.46(3) 3_665 ?
P1 O22 1.46(3) 2_655 ?
P1 O22 1.46(3) . ?
Na1 O11 2.90(6) . ?
Na1 O15 2.71(5) 14_654 ?
Na1 O27 2.41(6) . ?
Na1 O41 1.72(7) . ?
Na2 O5 2.41(3) . ?
Na2 O5 2.41(3) 5_655 ?
Na2 O14 2.59(4) 14_654 ?
Na2 O15 2.85(3) 18_554 ?
Na2 O15 2.85(3) 14_654 ?
Na2 O24 2.40(4) . ?
Na2 O39 2.20(8) . ?
Na2 O39 2.20(7) 5_655 ?
O5 O39 1.87(8) 5_655 ?
O12 Na3 2.74(10) . ?
O23 C2 1.24(6) . ?
O24 C2 1.17(7) . ?
O25 O25 0.00(11) 5_655 ?
O26 O27 1.72(7) . ?
C1 C1 0.00000(7) 5_655 ?
C1 C2 1.52(3) . ?
Na3 O28 2.59(12) . ?
Na3 O29 2.51(6) 4_665 ?
Na3 O29 2.51(6) . ?
Na3 O33 2.77(17) . ?
O33 O37 1.8(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Yb1 O23 C2 O24 0.00(3) . . . . ?
Yb1 O23 C2 C1 180.000(8) . . . 5_655 ?
Yb1 O23 C2 C1 180.000(8) . . . . ?
Yb1 O24 C2 O23 0.00(3) . . . . ?
Yb1 O24 C2 C1 180.000(11) . . . . ?
Yb1 O24 C2 C1 180.000(11) . . . 5_655 ?
Na2 O24 C2 O23 180.00(2) . . . . ?
Na2 O24 C2 C1 0.000(13) . . . . ?
Na2 O24 C2 C1 0.000(13) . . . 5_655 ?
O1 W1 O4 Yb1 123.9(16) 4_665 . . . ?
O1 W1 O4 K1 -88.4(13) 4_665 . . . ?
O1 W1 O5 Na2 -180(70) 4_665 . . . ?
O1 W1 O5 O39 -29(14) 4_665 . . 5_655 ?
O1 W1 O6 W2 -69(2) 4_665 . . . ?
O1 W4 O7 W1 2.4(13) 4_665 . . . ?
O1 W4 O13 W3 61(3) 4_665 . . . ?
O1 W4 O15 Na1 54(7) 4_665 . . 9_565 ?
O1 W4 O15 Na2 -109(6) 4_665 . . 9_565 ?
O1 W4 O16 W5 0.3(11) 4_665 . . . ?
O1 W5 O19 K1 86.8(14) 4_665 . . . ?
O2 W2 O8 Yb1 -130(3) . . . . ?
O2 W3 O11 W2 2.2(13) . . . . ?
O2 W3 O11 Na1 -126(2) . . . . ?
O3 W1 O4 Yb1 -161.7(16) . . . . ?
O3 W1 O4 K1 -14.0(13) . . . . ?
O3 W1 O5 Na2 132(2) . . . . ?
O3 W1 O5 O39 -77(11) . . . 5_655 ?
O3 W1 O6 W2 -75(4) . . . . ?
O3 W5 O19 K1 14.6(15) . . . . ?
O4 W1 O5 Na2 42(2) . . . . ?
O4 W1 O5 O39 -167(11) . . . 5_655 ?
O4 W1 O6 W2 17(2) . . . . ?
O5 W1 O4 Yb1 -65.1(18) . . . . ?
O5 W1 O4 K1 82.6(15) . . . . ?
O5 W1 O6 W2 122(2) . . . . ?
O6 W1 O4 Yb1 39.5(16) . . . . ?
O6 W1 O4 K1 -172.8(12) . . . . ?
O6 W1 O5 Na2 -54(2) . . . . ?
O6 W1 O5 O39 97(11) . . . 5_655 ?
O6 W2 O8 Yb1 -45(2) . . . . ?
O7 W1 O4 Yb1 128(3) . . . . ?
O7 W1 O4 K1 -84(3) . . . . ?
O7 W1 O5 Na2 -143(2) . . . . ?
O7 W1 O5 O39 8(11) . . . 5_655 ?
O7 W1 O6 W2 -143(2) . . . . ?
O7 W4 O13 W3 135(3) . . . . ?
O7 W4 O15 Na1 -6(2) . . . 9_565 ?
O7 W4 O15 Na2 -168.5(11) . . . 9_565 ?
O7 W4 O16 W5 -73.6(14) . . . . ?
O9 W2 O8 Yb1 57(3) . . . . ?
O10 W2 O8 Yb1 158(3) . . . . ?
O11 W2 O8 Yb1 -115(3) . . . . ?
O11 W3 O11 W2 -70.6(19) 4_665 . . . ?
O11 W3 O11 Na1 161.4(14) 4_665 . . . ?
O12 W3 O11 W2 -171.3(17) . . . . ?
O12 W3 O11 Na1 61(2) . . . . ?
O13 W3 O11 W2 22(4) 4_665 . . . ?
O13 W3 O11 W2 87.3(16) . . . . ?
O13 W3 O11 Na1 -106(3) 4_665 . . . ?
O13 W3 O11 Na1 -40.8(19) . . . . ?
O13 W3 O12 Na3 137.4(7) . . . . ?
O13 W3 O12 Na3 -137.4(7) 4_665 . . . ?
O13 W4 O7 W1 -83.4(15) . . . . ?
O13 W4 O15 Na1 -98(2) . . . 9_565 ?
O13 W4 O15 Na2 99.4(12) . . . 9_565 ?
O13 W4 O16 W5 13(4) . . . . ?
O14 W4 O7 W1 0(5) . . . . ?
O14 W4 O13 W3 -25(3) . . . . ?
O14 W4 O15 Na1 172(2) . . . 9_565 ?
O14 W4 O15 Na2 9.1(16) . . . 9_565 ?
O14 W4 O16 W5 86.6(15) . . . . ?
O15 W4 O7 W1 173.2(16) . . . . ?
O15 W4 O13 W3 -124(3) . . . . ?
O15 W4 O16 W5 -174.2(13) . . . . ?
O16 W4 O7 W1 75.5(15) . . . . ?
O16 W4 O13 W3 49(5) . . . . ?
O16 W4 O15 Na1 85(2) . . . 9_565 ?
O16 W4 O15 Na2 -78.1(11) . . . 9_565 ?
O16 W5 O19 K1 93(3) . . . . ?
O17 W5 O19 K1 171.9(17) . . . . ?
O18 W5 O19 K1 -86.1(17) . . . . ?
O20 W6 O21 Yb1 180.000(11) . . . . ?
O20 W6 O21 K1 0.000(6) . . . . ?
O21 W6 O21 Yb1 -73(2) 2_655 . . . ?
O21 W6 O21 Yb1 73(2) 3_665 . . . ?
O21 W6 O21 K1 107(2) 2_655 . . . ?
O21 W6 O21 K1 -107(2) 3_665 . . . ?
O22 P1 O22 Yb1 99(4) 2_655 . . . ?
O22 P1 O22 Yb1 -99(4) 3_665 . . . ?
C1 C1 C2 O23 -90(100) 5_655 . . . ?
C1 C1 C2 O24 90(100) 5_655 . . . ?
O36 W3 O12 Na3 0.000(16) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9568
2 0.0432
