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_7714600
_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 O76 P4 W14, 2.5(O)'
_chemical_formula_sum            'H6 Na6 O58 P4 W14'
_chemical_formula_weight         4091.72
_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             2023-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-08 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                99.1067(16)
_cell_angle_beta                 91.2955(16)
_cell_angle_gamma                104.3378(18)
_cell_formula_units_Z            1
_cell_length_a                   10.8321(2)
_cell_length_b                   12.6641(3)
_cell_length_c                   15.4456(3)
_cell_measurement_reflns_used    56046
_cell_measurement_temperature    99.92(18)
_cell_measurement_theta_max      29.3570
_cell_measurement_theta_min      2.8500
_cell_volume                     2022.70(8)
_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      99.92(18)
_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 0.932
_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    -86.00 -43.00   1.00   20.00    --   -9.92 154.00  82.20   43
  2  \w    -15.00  31.00   1.00   20.00    --   -9.92 -99.00   0.00   46
  3  \w    -86.00 -43.00   1.00   20.00    --   -9.92 154.00 163.41   43
  4  \w    -85.00 -42.00   1.00   20.00    --   -9.92 153.00 -28.92   43
  5  \w    -69.00  27.00   1.00   20.00    --   10.55 -19.00-180.00   96
  6  \w    -69.00  27.00   1.00   20.00    --   10.55 -19.00   0.00   96
  7  \w      2.00  63.00   1.00   20.00    --   10.55-120.00 -25.80   61
  8  \w    -14.00  85.00   1.00   20.00    --   10.55  38.00-180.00   99
  9  \w    -27.00  91.00   1.00   20.00    --   10.55  19.00   0.00  118
 10  \w    -84.00 -41.00   1.00   20.00    --   -9.92 152.00-104.93   43
 11  \w    -15.00  31.00   1.00   20.00    --   -9.92 -99.00 150.00   46
 12  \w    -85.00 -42.00   1.00   20.00    --   -9.92 153.00  17.67   43
 13  \w    -69.00 -30.00   1.00   20.00    --   -9.92 129.00 -46.76   39
 14  \w    -42.00  23.00   1.00   20.00    --   -9.92 -77.00-120.00   65
 15  \w    -43.00  21.00   1.00   20.00    --   -9.92  77.00 -90.00   64
 16  \w    -15.00  31.00   1.00   20.00    --   -9.92 -99.00 -60.00   46
 17  \w    -81.00 -38.00   1.00   20.00    --   -9.92 148.00  -8.82   43
 18  \w    -69.00 -30.00   1.00   20.00    --   -9.92 129.00-118.80   39
 19  \w    -43.00  21.00   1.00   20.00    --   -9.92  77.00   0.00   64
 20  \w    -42.00  23.00   1.00   20.00    --   -9.92 -77.00-150.00   65
 21  \w    -43.00  21.00   1.00   20.00    --   -9.92  77.00 -60.00   64
 22  \w    -78.00  30.00   1.00   20.00    --   10.55   0.00-150.00  108
 23  \w    -78.00  99.00   1.00   20.00    --   10.55   0.00-180.00  177
;
_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      0.0379700000
_diffrn_orient_matrix_UB_12      -0.0370519000
_diffrn_orient_matrix_UB_13      -0.0138964000
_diffrn_orient_matrix_UB_21      -0.0340321000
_diffrn_orient_matrix_UB_22      -0.0146716000
_diffrn_orient_matrix_UB_23      -0.0417207000
_diffrn_orient_matrix_UB_31      0.0445774000
_diffrn_orient_matrix_UB_32      0.0430380000
_diffrn_orient_matrix_UB_33      -0.0154399000
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            88070
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.455
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15221
_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    3.359
_exptl_crystal_description       block
_exptl_crystal_F_000             1790
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.567
_refine_diff_density_min         -4.396
_refine_diff_density_rms         0.305
_refine_ls_extinction_coef       0.00039(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   1.076
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         10454
_refine_ls_number_restraints     641
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+19.9366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10049
_reflns_number_total             10454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03883a2.cif
_cod_data_source_block           jcr253-2_auto
_cod_depositor_comments
'Adding full bibliography for 7714599--7714602.cif.'
_cod_original_cell_volume        2022.72(7)
_cod_original_formula_sum        'Na6 H6 P4 W14 O58'
_cod_database_code               7714600
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Na7PW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 15.02.2023, Mo, 100K'
_shelx_estimated_absorpt_t_max   0.123
_shelx_estimated_absorpt_t_min   0.060
_olex2_refinement_description
;
1. Restrained distances
 Na3-O9X \\sim Na3-O9W
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O16) \\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(P1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O17) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O9X) = Uanis(O9W)
3. 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
4. Others
 Sof(O9X)=1-FVAR(1)
 Sof(O9W)=FVAR(1)
 Fixed Sof: O28(0.25)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45535
_shelx_fab_checksum              57332
_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 3.400
_oxdiff_exptl_absorpt_empirical_full_min 0.560