Heteroelements in polyoxometalates: a study on the influence of different group 15 elements on polyoxometalate formation.
Raabe, Jan-Christian; Jameel, Froze; Stein, Matthias; Albert, Jakob; Poller, Maximilian J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 454–466; doi:10.1039/d3dt03883a

data_7714601
_publ_section_title
;
 Heteroelements in polyoxometalates: a study on the influence of different
 group 15 elements on polyoxometalate formation.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              454
_journal_page_last               466
_journal_paper_doi               10.1039/d3dt03883a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Na8 O64 W12, 1.5(O4)'
_chemical_formula_sum            'Na8 O40 W12'
_chemical_formula_weight         3510.12
_chemical_name_systematic        'Paradodecatungstate B'
_chemical_properties_physical    Hygroscopic
_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_primary     heavy
_audit_creation_date             2023-03-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-09-08 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                82.286(3)
_cell_angle_beta                 66.379(3)
_cell_angle_gamma                64.875(3)
_cell_formula_units_Z            1
_cell_length_a                   11.7511(4)
_cell_length_b                   12.1744(4)
_cell_length_c                   12.4107(4)
_cell_measurement_reflns_used    55286
_cell_measurement_temperature    99.97(15)
_cell_measurement_theta_max      32.6870
_cell_measurement_theta_min      3.1860
_cell_volume                     1471.45(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -72.00 -24.00   1.00   15.00    --  -18.02 121.00  28.58   48
  2  \w    -42.00  15.00   1.00   15.00    --  -18.02 -77.00  30.00   57
  3  \w    -42.00  15.00   1.00   15.00    --  -18.02 -77.00-180.00   57
  4  \w    -94.00 -43.00   1.00   15.00    --  -18.02 154.00 178.42   51
  5  \w     -6.00  93.00   1.00   15.00    --   18.80  38.00  60.00   99
  6  \w    -22.00  99.00   1.00   15.00    --   18.80  19.00-150.00  121
  7  \w     -6.00  93.00   1.00   15.00    --   18.80  38.00 -30.00   99
  8  \w     39.00 108.00   1.00   15.00    --   18.80 178.00-120.00   69
  9  \w    -61.00  27.00   1.00   15.00    --   18.80 -19.00-150.00   88
 10  \w     39.00 108.00   1.00   15.00    --   18.80 178.00  60.00   69
 11  \w    -61.00  27.00   1.00   15.00    --   18.80 -19.00  30.00   88
 12  \w    -94.00 -43.00   1.00   15.00    --  -18.02 154.00 107.67   51
 13  \w    -42.00  15.00   1.00   15.00    --  -18.02 -77.00 120.00   57
 14  \w    -33.00  17.00   1.00   15.00    --  -18.02 -84.00 -93.00   50
 15  \w    -77.00 -30.00   1.00   15.00    --  -18.02 129.00  68.90   47
 16  \w    -87.00 -37.00   1.00   15.00    --  -18.02 145.00 -38.79   50
 17  \w   -107.00 -61.00   1.00   15.00    --  -18.02-178.00  60.00   46
 18  \w    -42.00  15.00   1.00   15.00    --  -18.02 -77.00   0.00   57
 19  \w   -107.00 -61.00   1.00   15.00    --  -18.02-178.00-180.00   46
 20  \w    -77.00 -30.00   1.00   15.00    --  -18.02 129.00 -82.14   47
 21  \w    -69.00 107.00   1.00   15.00    --   18.80   0.00-180.00  176
 22  \w    -69.00 107.00   1.00   15.00    --   18.80   0.00-150.00  176
 23  \w    -69.00 107.00   1.00   15.00    --   18.80   0.00-120.00  176
 24  \w    -69.00  32.00   1.00   15.00    --   18.80   0.00 -90.00  101
 25  \w      8.00  77.00   1.00   15.00    --   18.80-128.00-141.87   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0004483000
_diffrn_orient_matrix_UB_12      0.0412657000
_diffrn_orient_matrix_UB_13      -0.0461542000
_diffrn_orient_matrix_UB_21      -0.0706451000
_diffrn_orient_matrix_UB_22      0.0345389000
_diffrn_orient_matrix_UB_23      0.0302491000
_diffrn_orient_matrix_UB_31      0.0147696000
_diffrn_orient_matrix_UB_32      0.0353975000
_diffrn_orient_matrix_UB_33      0.0292085000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            93161
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.768
_diffrn_reflns_theta_min         2.289
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.961
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.596
_refine_diff_density_min         -11.466
_refine_diff_density_rms         0.465
_refine_ls_extinction_coef       0.00042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         10357
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0001P)^2^+93.5284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9939
_reflns_number_total             10357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03883a2.cif
_cod_data_source_block           jcr256_auto
_cod_depositor_comments
'Adding full bibliography for 7714599--7714602.cif.'
_cod_original_formula_sum        'Na8 W12 O40'
_cod_database_code               7714601
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Na7NW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 10.02.2023, Mo, 100K'
_shelx_estimated_absorpt_t_max   0.164
_shelx_estimated_absorpt_t_min   0.064
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O13) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O14) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O7W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O20) \\sim Ueq, Uanis(W6) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(O18) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(W3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93649
_shelx_fab_checksum              86631
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.266
_oxdiff_exptl_absorpt_empirical_full_min 0.625