Synthesis and characterization of Al and Si substituted polyoxometalates.
Raabe, Jan-Christian; Chitnis, Saurabh S.; Poller, Maximilian J.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9483–9488; doi:10.1039/d5dt00894h

data_7718803
_publ_section_title
;
 Synthesis and characterization of Al and Si substituted polyoxometalates.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9483
_journal_page_last               9488
_journal_paper_doi               10.1039/d5dt00894h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(Al0.5 O20 P0.5 W5.5), 4[C16H36N+]'
_chemical_formula_sum            'C64 H144 Al N4 O40 P W11'
_chemical_formula_weight         3690.12
_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'
_atom_sites_solution_primary     direct
_audit_creation_date             2025-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-05-06 deposited with the CCDC.	2025-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.4284(2)
_cell_length_b                   17.4284(2)
_cell_length_c                   17.4284(2)
_cell_measurement_reflns_used    22139
_cell_measurement_temperature    99.95(13)
_cell_measurement_theta_max      27.3480
_cell_measurement_theta_min      2.8310
_cell_volume                     5293.86(11)
_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      99.95(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  32.00   1.00   90.00    --   -8.55 -99.00  90.00   47
  2  \w    -19.00  82.00   1.00   90.00    --    9.33  57.00  90.00  101
  3  \w    -19.00  82.00   1.00   90.00    --    9.33  57.00 -30.00  101
  4  \w    -64.00  37.00   1.00   90.00    --    9.33 -57.00 -60.00  101
  5  \w    -42.00  42.00   1.00   90.00    --    9.33 -76.00 161.91   84
  6  \w     22.00  86.00   1.00   90.00    --    9.33-155.00 109.64   64
  7  \w    -15.00  84.00   1.00   90.00    --    9.33  38.00 -90.00   99
  8  \w     20.00  85.00   1.00   90.00    --    9.33-153.00 -36.94   65
  9  \w    -65.00 -27.00   1.00   90.00    --   -8.55 125.00 142.60   38
 10  \w    -84.00 -42.00   1.00   90.00    --   -8.55 153.00 -82.00   42
 11  \w    -84.00 -42.00   1.00   90.00    --   -8.55 153.00  15.58   42
 12  \w    -41.00  21.00   1.00   90.00    --   -8.55  77.00  90.00   62
 13  \w      7.00  67.00   1.00   90.00    --    9.33-127.00 178.60   60
;
_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      -0.0339847000
_diffrn_orient_matrix_UB_12      0.0160559000
_diffrn_orient_matrix_UB_13      -0.0155815000
_diffrn_orient_matrix_UB_21      -0.0214510000
_diffrn_orient_matrix_UB_22      -0.0313458000
_diffrn_orient_matrix_UB_23      0.0146998000
_diffrn_orient_matrix_UB_31      -0.0062034000
_diffrn_orient_matrix_UB_32      0.0205865000
_diffrn_orient_matrix_UB_33      0.0345203000
_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  0.0958
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65214
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.962
_diffrn_reflns_theta_min         2.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39767
_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    2.315
_exptl_crystal_description       plate
_exptl_crystal_F_000             3436
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         8.206
_refine_diff_density_min         -2.474
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         724
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0571
_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/[\s^2^(Fo^2^)+203.4304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                537
_reflns_number_total             724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00894h2.cif
_cod_data_source_block           jcr22-jcr13_auto_jcr_v1
_cod_depositor_comments          'Adding full bibliography for 7718803.cif.'
_cod_original_cell_volume        5293.9(2)
_cod_original_sg_symbol_H-M      Im-3m
_cod_database_code               7718803
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C87H187O40N5PAlW11
_chemical_oxdiff_usercomment     'Poller/Albert, 01.07.2024, Mo, 100K'
_shelx_estimated_absorpt_t_max   0.447
_shelx_estimated_absorpt_t_min   0.221
_diffrn_oxdiff_digest_hkl
;
01006f844450679c9e9affaecf1e2559f67cf5
;
_olex2_refinement_description
;
1. Shared sites
{W1, Al1}
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(W1) = Uanis(Al1)
3. Others
 Fixed Sof: W1(0.229167) Al1(0.020833) O1(0.083333)
 Fixed Uiso: P1(0.015)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32516
_shelx_hkl_checksum              1281
_shelx_fab_checksum              63209
_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.680