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_7714599
_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         'Na6 O48 Sb W6, 4(O)'
_chemical_formula_sum            'H Na6 O24 Sb W6'
_chemical_formula_weight         2194.79
_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     direct
_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                69.081(4)
_cell_angle_beta                 85.409(4)
_cell_angle_gamma                69.784(4)
_cell_formula_units_Z            1
_cell_length_a                   10.5698(5)
_cell_length_b                   10.9770(4)
_cell_length_c                   11.3410(5)
_cell_measurement_reflns_used    51314
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      32.5430
_cell_measurement_theta_min      2.6990
_cell_volume                     1151.98(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 1.5 (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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_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 0.952
_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    -27.00  62.00   1.00   12.50    --  -17.86  19.00-120.00   89
  2  \w    -42.00  15.00   1.00   12.50    --  -17.86 -77.00 -30.00   57
  3  \w    -94.00 -43.00   1.00   12.50    --  -17.86 154.00 173.50   51
  4  \w     -9.00  92.00   1.00   12.50    --   18.80  57.00-150.00  101
  5  \w    -42.00  51.00   1.00   12.50    --   18.80 -77.00  60.00   93
  6  \w     -9.00  92.00   1.00   12.50    --   18.80  57.00 -30.00  101
  7  \w    -53.00  47.00   1.00   12.50    --   18.80 -57.00 -60.00  100
  8  \w     -6.00  93.00   1.00   12.50    --   18.80  38.00 120.00   99
  9  \w     -6.00  93.00   1.00   12.50    --   18.80  38.00   0.00   99
 10  \w     -5.00  67.00   1.00   12.50    --   18.80-112.00-161.52   72
 11  \w    -93.00 -42.00   1.00   12.50    --  -17.86 153.00 -29.97   51
 12  \w    -42.00  15.00   1.00   12.50    --  -17.86 -77.00  90.00   57
 13  \w    -50.00  21.00   1.00   12.50    --  -17.86  77.00 120.00   71
 14  \w    -75.00 -28.00   1.00   12.50    --  -17.86 126.00  32.77   47
 15  \w    -75.00 -28.00   1.00   12.50    --  -17.86 126.00  80.20   47
 16  \w    -94.00 -43.00   1.00   12.50    --  -17.86 154.00-118.92   51
 17  \w     39.00 108.00   1.00   12.50    --   18.80 178.00 -60.00   69
 18  \w    -69.00 107.00   1.00   12.50    --   18.80   0.00-180.00  176
 19  \w    -69.00 107.00   1.00   12.50    --   18.80   0.00-120.00  176
 20  \w    -69.00 107.00   1.00   12.50    --   18.80   0.00 -90.00  176
 21  \w    -69.00 107.00   1.00   12.50    --   18.80   0.00-150.00  176
;
_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      0.0292666000
_diffrn_orient_matrix_UB_12      0.0308368000
_diffrn_orient_matrix_UB_13      -0.0561870000
_diffrn_orient_matrix_UB_21      0.0508210000
_diffrn_orient_matrix_UB_22      -0.0651084000
_diffrn_orient_matrix_UB_23      0.0082308000
_diffrn_orient_matrix_UB_31      -0.0410751000
_diffrn_orient_matrix_UB_32      -0.0149247000
_diffrn_orient_matrix_UB_33      -0.0356282000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72269
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.776
_diffrn_reflns_theta_min         2.303
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57141
_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    3.164
_exptl_crystal_description       block
_exptl_crystal_F_000             977
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         6.729
_refine_diff_density_min         -1.888
_refine_diff_density_rms         0.258
_refine_ls_extinction_coef       0.00212(8)
_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   1.136
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         8114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0290P)^2^+9.2027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7973
_reflns_number_total             8114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03883a2.cif
_cod_data_source_block           jcr255_auto
_cod_depositor_comments
'Adding full bibliography for 7714599--7714602.cif.'
_cod_original_cell_volume        1151.98(9)
_cod_original_formula_sum        'Na6 H1 Sb1 W6 O24'
_cod_database_code               7714599
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Na7SbW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 06.01.2023, Mo, 100K'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
;
_shelx_res_checksum              47671
_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 1.598
_oxdiff_exptl_absorpt_empirical_full_min 0.802