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_7714602
_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
'As K1.35 Na3.15 O39.647 W9, 7.858(O), 10.8[H2O]'
_chemical_formula_sum            'As H5.9 Na3.1 O34 W9'
_chemical_formula_weight         2809.43
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_audit_creation_date             2023-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-08 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   30.08540(9)
_cell_length_b                   30.08540(9)
_cell_length_c                   30.08540(9)
_cell_measurement_reflns_used    228300
_cell_measurement_temperature    99.95(13)
_cell_measurement_theta_max      29.4260
_cell_measurement_theta_min      2.5150
_cell_volume                     27231.24(14)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_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    -15.00  31.00   1.00   60.00    --   -9.92 -99.00  90.00   46
  2  \w    -14.00  85.00   1.00   60.00    --   10.55  38.00  60.00   99
  3  \w    -42.00  43.00   1.00   60.00    --   10.55 -77.00-120.00   85
  4  \w    -42.00  43.00   1.00   60.00    --   10.55 -77.00 120.00   85
  5  \w    -78.00  99.00   1.00   60.00    --   10.55   0.00 -90.00  177
  6  \w    -14.00  85.00   1.00   60.00    --   10.55  38.00 -60.00   99
  7  \w      6.00  67.00   1.00   60.00    --   10.55-125.00 -52.00   61
  8  \w     19.00  84.00   1.00   60.00    --   10.55-151.00  72.37   65
  9  \w    -69.00 -30.00   1.00   60.00    --   -9.92 129.00  55.17   39
 10  \w    -15.00  31.00   1.00   60.00    --   -9.92 -99.00  30.00   46
 11  \w    -69.00 -30.00   1.00   60.00    --   -9.92 129.00  -0.05   39
 12  \w    -87.00 -44.00   1.00   60.00    --   -9.92 156.00-107.40   43
 13  \w    -79.00 -37.00   1.00   60.00    --   -9.92 145.00  73.51   42
 14  \w    -69.00 -30.00   1.00   60.00    --   -9.92 129.00 141.56   39
 15  \w    -59.00 -17.00   1.00   60.00    --   -9.92 113.00-176.28   42
 16  \w    -84.00 -41.00   1.00   60.00    --   -9.92 152.00 -11.01   43
 17  \w    -15.00  31.00   1.00   60.00    --   -9.92 -99.00 120.00   46
 18  \w    -78.00 -31.00   1.00   60.00    --   10.55   0.00-180.00   47
 19  \w     -1.00  62.00   1.00   60.00    --   10.55-117.00 -11.69   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0178142501
_diffrn_orient_matrix_UB_12      0.0065108499
_diffrn_orient_matrix_UB_13      -0.0140068501
_diffrn_orient_matrix_UB_21      0.0122626488
_diffrn_orient_matrix_UB_22      -0.0070589512
_diffrn_orient_matrix_UB_23      -0.0188636512
_diffrn_orient_matrix_UB_31      -0.0093963484
_diffrn_orient_matrix_UB_32      -0.0215427484
_diffrn_orient_matrix_UB_33      0.0019551516
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            476401
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.594
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49516
_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    2.741
_exptl_crystal_description       block
_exptl_crystal_F_000             19957
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_refine_diff_density_max         2.277
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0214P)^2^+2635.2891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2932
_reflns_number_total             3572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03883a2.cif
_cod_data_source_block           jcr268_auto_v1
_cod_depositor_comments
'Adding full bibliography for 7714599--7714602.cif.'
_cod_original_cell_volume        27231.2(2)
_cod_original_formula_sum        'Na3.1 H5.9 As1 W9 O34'
_cod_database_code               7714602
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Na7AsW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 08.05.2023, Mo, 100K'
_olex2_refinement_description
;
1. Shared sites
{Na1, K1}
2. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Na1) = Uanis(K1)
3. Others
 Fixed Sof: K1(0.225) Na1(0.025)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              79121
_shelx_fab_checksum              6391
_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 1.577
_oxdiff_exptl_absorpt_empirical_full_min 0.668