#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:16:37 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262474 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/78/7127891.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_7127891
loop_
_publ_author_name
'Wan, Rong'
'Liu, Zhen'
'Ma, Xinyi'
'Li, Huafeng'
'Ma, Pengtao'
'Zhang, Chao'
'Niu, Jingyang'
'Wang, Jingping'
_publ_section_title
;
 Discovery of two Na⁺-centered Silverton-type polyoxometalates
 {NaM₁₂O₄₂} (M = Mo, W).
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2172
_journal_page_last               2175
_journal_paper_doi               10.1039/d0cc07590f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '0.5(C48 H144 Na8 O108 Ru8 S24 W24), 3(O)'
_chemical_formula_sum            'C24 H72 Na4 O57 Ru4 S12 W12'
_chemical_formula_weight         4359.97
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2020-03-30 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9539(9)
_cell_length_b                   17.9539(9)
_cell_length_c                   17.9539(9)
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.78
_cell_volume                     5787.3(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.604
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.675
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0938 before and 0.0643 after correction. The Ratio of minimum to maximum transmission is 0.8077. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_description       block
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.008
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.249
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0433P)²+2.0371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2029
_reflns_number_total             2398
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc07590f2.cif
_cod_data_source_block           njy1
_cod_depositor_comments
'Adding full bibliography for 7127890--7127891.cif.'
_cod_original_cell_volume        5787.3(9)
_cod_database_code               7127891
_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   0.252
_shelx_estimated_absorpt_t_min   0.167
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.01(2) -0.01(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: Na2(0.25)
4.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'
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 -0.08577(2) 0.00242(3) -0.17284(2) 0.01905(13) Uani 1 1 d . . . . .
Ru1 Ru -0.18015(5) -0.18015(5) -0.18015(5) 0.0239(3) Uani 1 3 d S T P . .
S1 S -0.1429(2) -0.2232(2) -0.29125(19) 0.0383(8) Uani 1 1 d . . . . .
Na1 Na 0.0000 0.0000 0.0000 0.021(2) Uani 1 12 d S T P . .
Na2 Na -0.1896(3) 0.1896(3) -0.1896(3) 0.017(2) Uani 0.75 3 d S T P . .
O1 O -0.1224(3) 0.0025(6) -0.0738(3) 0.0209(12) Uani 1 1 d . . . . .
O2 O -0.1338(5) -0.0784(5) -0.2047(5) 0.027(2) Uani 1 1 d . . . . .
O3 O -0.1354(5) 0.0726(5) -0.2129(5) 0.029(2) Uani 1 1 d . . . . .
O4 O 0.0000 0.0000 -0.2384(4) 0.0244(18) Uani 1 2 d S T P . .
O5 O -0.1798(6) -0.2890(6) -0.3228(7) 0.059(3) Uani 1 1 d . . . . .
C1 C -0.1490(12) -0.1538(10) -0.3608(8) 0.072(5) Uani 1 1 d . . . . .
H1A H -0.1256 -0.1090 -0.3434 0.107 Uiso 1 1 calc R . . . .
H1B H -0.1243 -0.1707 -0.4052 0.107 Uiso 1 1 calc R . . . .
H1C H -0.2004 -0.1440 -0.3717 0.107 Uiso 1 1 calc R . . . .
C2 C -0.0459(8) -0.2409(15) -0.2923(10) 0.085(7) Uani 1 1 d . . . . .
H2A H -0.0198 -0.1989 -0.2720 0.127 Uiso 1 1 calc R . . . .
H2B H -0.0354 -0.2843 -0.2629 0.127 Uiso 1 1 calc R . . . .
H2C H -0.0298 -0.2492 -0.3426 0.127 Uiso 1 1 calc R . . . .
O1W O 0.0000 -0.2500 -0.5000 0.111(9) Uiso 1 4 d S T P . .
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'
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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
W1 W1 Na1 63.597(5) 2 . ?
O1 W1 W1 110.31(18) . 2 ?
O1 W1 W1 47.7(2) 12 2 ?
O1 W1 W1 44.7(2) 9 2 ?
O1 W1 Na1 47.80(15) 9 . ?
O1 W1 Na1 47.68(16) 12 . ?
O1 W1 Na1 46.71(18) . . ?
O1 W1 O1 81.2(5) . 12 ?
O1 W1 O1 73.1(3) 12 9 ?
O1 W1 O1 82.5(4) . 9 ?
O1 W1 O4 147.7(3) . . ?
O2 W1 W1 117.5(3) . 2 ?
O2 W1 Na1 119.5(3) . . ?
O2 W1 O1 88.6(3) . 9 ?
O2 W1 O1 97.7(4) . . ?
O2 W1 O1 161.7(4) . 12 ?
O2 W1 O4 99.9(3) . . ?
O3 W1 W1 123.0(3) . 2 ?
O3 W1 Na1 128.3(3) . . ?
O3 W1 O1 167.2(4) . 9 ?
O3 W1 O1 95.8(4) . 12 ?
O3 W1 O1 102.4(4) . . ?
O3 W1 O2 102.3(3) . . ?
O3 W1 O4 100.1(3) . . ?
O4 W1 W1 37.41(18) . 2 ?
O4 W1 Na1 101.00(18) . . ?
O4 W1 O1 73.7(3) . 12 ?
O4 W1 O1 71.1(2) . 9 ?
S1 Ru1 S1 93.55(14) . 5 ?
S1 Ru1 S1 93.55(14) 9 5 ?
S1 Ru1 S1 93.55(14) . 9 ?
O2 Ru1 S1 89.7(3) . . ?
O2 Ru1 S1 89.7(3) 9 9 ?
O2 Ru1 S1 91.2(3) . 5 ?
O2 Ru1 S1 91.2(3) 9 . ?
O2 Ru1 S1 91.2(3) 5 9 ?
O2 Ru1 S1 174.1(3) 5 . ?
O2 Ru1 S1 89.7(3) 5 5 ?
O2 Ru1 S1 174.1(3) . 9 ?
O2 Ru1 S1 174.1(3) 9 5 ?
O2 Ru1 O2 85.3(4) . 9 ?
O2 Ru1 O2 85.3(4) 9 5 ?
O2 Ru1 O2 85.3(4) . 5 ?
O5 S1 Ru1 119.0(5) . . ?
O5 S1 C1 105.4(8) . . ?
O5 S1 C2 107.2(9) . . ?
C1 S1 Ru1 111.5(6) . . ?
C1 S1 C2 100.4(11) . . ?
C2 S1 Ru1 111.4(6) . . ?
O1 Na1 O1 178.0(5) 2 4 ?
O1 Na1 O1 62.2(4) 2 8 ?
O1 Na1 O1 62.2(4) 5 4 ?
O1 Na1 O1 62.2(4) 10 4 ?
O1 Na1 O1 116.61(12) 2 6 ?
O1 Na1 O1 65.3(4) 6 4 ?
O1 Na1 O1 62.2(4) 9 8 ?
O1 Na1 O1 65.3(4) 9 . ?
O1 Na1 O1 115.86(12) 9 6 ?
O1 Na1 O1 178.0(5) 3 . ?
O1 Na1 O1 65.3(4) 11 4 ?
O1 Na1 O1 117.9(3) 2 . ?
O1 Na1 O1 178.0(5) 12 10 ?
O1 Na1 O1 115.86(12) 10 . ?
O1 Na1 O1 65.3(4) 3 8 ?
O1 Na1 O1 62.2(4) 6 . ?
O1 Na1 O1 65.3(4) 10 8 ?
O1 Na1 O1 178.0(5) 7 5 ?
O1 Na1 O1 115.86(12) 3 6 ?
O1 Na1 O1 116.61(12) 3 5 ?
O1 Na1 O1 116.61(12) 10 6 ?
O1 Na1 O1 115.86(12) 11 2 ?
O1 Na1 O1 116.61(12) 7 4 ?
O1 Na1 O1 62.2(4) 9 2 ?
O1 Na1 O1 62.2(4) 5 10 ?
O1 Na1 O1 65.3(4) 7 2 ?
O1 Na1 O1 116.61(12) 11 8 ?
O1 Na1 O1 62.2(3) 3 2 ?
O1 Na1 O1 117.9(3) 7 8 ?
O1 Na1 O1 115.86(12) 5 2 ?
O1 Na1 O1 62.2(3) 5 8 ?
O1 Na1 O1 117.9(3) 11 12 ?
O1 Na1 O1 115.86(12) 12 8 ?
O1 Na1 O1 62.2(3) 9 12 ?
O1 Na1 O1 65.3(4) 11 6 ?
O1 Na1 O1 65.3(4) 7 12 ?
O1 Na1 O1 62.2(3) 7 6 ?
O1 Na1 O1 116.61(12) 3 12 ?
O1 Na1 O1 117.9(3) 5 6 ?
O1 Na1 O1 116.61(12) 5 12 ?
O1 Na1 O1 62.2(4) 12 6 ?
O1 Na1 O1 65.3(4) 2 12 ?
O1 Na1 O1 178.0(5) 8 6 ?
O1 Na1 O1 62.2(3) 11 10 ?
O1 Na1 O1 116.61(12) 9 4 ?
O1 Na1 O1 117.9(3) 9 10 ?
O1 Na1 O1 117.9(3) 3 4 ?
O1 Na1 O1 115.86(12) 7 10 ?
O1 Na1 O1 65.3(4) 3 10 ?
O1 Na1 O1 115.86(12) 12 4 ?
O1 Na1 O1 178.0(5) 11 9 ?
O1 Na1 O1 115.86(12) 8 4 ?
O1 Na1 O1 62.2(4) 11 7 ?
O1 Na1 O1 116.61(12) 11 . ?
O1 Na1 O1 116.61(12) 9 7 ?
O1 Na1 O1 115.86(12) 7 . ?
O1 Na1 O1 62.2(4) 11 3 ?
O1 Na1 O1 65.3(4) 5 . ?
O1 Na1 O1 115.86(12) 9 3 ?
O1 Na1 O1 62.2(4) 12 . ?
O1 Na1 O1 62.2(4) 7 3 ?
O1 Na1 O1 116.61(12) 8 . ?
O1 Na1 O1 115.86(12) 11 5 ?
O1 Na1 O1 62.2(3) 4 . ?
O1 Na1 O1 65.3(4) 9 5 ?
O1 Na1 O1 116.61(12) 2 10 ?
O3 Na2 O3 82.1(4) . 12 ?
O3 Na2 O3 82.1(4) . 6 ?
O3 Na2 O3 82.1(4) 12 6 ?
O3 Na2 O5 86.0(3) 12 16_454 ?
O3 Na2 O5 163.9(4) 6 23_454 ?
O3 Na2 O5 86.0(3) . 23_454 ?
O3 Na2 O5 107.1(4) 6 16_454 ?
O3 Na2 O5 107.1(4) . 18_454 ?
O3 Na2 O5 107.1(4) 12 23_454 ?
O3 Na2 O5 163.9(4) 12 18_454 ?
O3 Na2 O5 86.0(3) 6 18_454 ?
O3 Na2 O5 163.9(4) . 16_454 ?
O5 Na2 O5 87.1(4) 18_454 23_454 ?
O5 Na2 O5 87.1(4) 16_454 23_454 ?
O5 Na2 O5 87.1(4) 18_454 16_454 ?
W1 O1 W1 134.4(6) . 6 ?
W1 O1 W1 134.4(5) . 5 ?
W1 O1 W1 87.6(2) 6 5 ?
W1 O1 Na1 93.7(3) 6 . ?
W1 O1 Na1 91.0(3) 5 . ?
W1 O1 Na1 100.8(2) . . ?
W1 O2 Ru1 148.3(5) . . ?
W1 O3 Na2 143.4(6) . . ?
W1 O4 W1 105.2(4) . 2 ?
S1 O5 Na2 122.5(6) . 15_444 ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
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 W1 3.0809(7) 2 ?
W1 Na1 3.4644(4) . ?
W1 O1 1.896(6) . ?
W1 O1 2.281(9) 9 ?
W1 O1 2.167(9) 12 ?
W1 O2 1.782(9) . ?
W1 O3 1.703(9) . ?
W1 O4 1.939(5) . ?
Ru1 S1 2.242(4) . ?
Ru1 S1 2.242(4) 9 ?
Ru1 S1 2.242(4) 5 ?
Ru1 O2 2.056(10) . ?
Ru1 O2 2.056(10) 5 ?
Ru1 O2 2.056(10) 9 ?
S1 O5 1.469(10) . ?
S1 C1 1.768(16) . ?
S1 C2 1.770(16) . ?
Na1 O1 2.567(6) 10 ?
Na1 O1 2.567(6) 5 ?
Na1 O1 2.567(6) 3 ?
Na1 O1 2.567(6) 6 ?
Na1 O1 2.567(6) 12 ?
Na1 O1 2.567(6) . ?
Na1 O1 2.567(6) 8 ?
Na1 O1 2.567(6) 11 ?
Na1 O1 2.567(6) 4 ?
Na1 O1 2.567(6) 9 ?
Na1 O1 2.567(6) 7 ?
Na1 O1 2.567(6) 2 ?
Na2 O3 2.354(11) . ?
Na2 O3 2.354(11) 12 ?
Na2 O3 2.354(11) 6 ?
Na2 O5 2.385(12) 16_454 ?
Na2 O5 2.385(12) 23_454 ?
Na2 O5 2.385(12) 18_454 ?
O1 W1 2.167(9) 6 ?
O1 W1 2.280(9) 5 ?
O4 W1 1.939(5) 2 ?
O5 Na2 2.385(12) 15_444 ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.01(2)
2 -0.01(2)
