Self-assembly of Dawson-type H<sub>6</sub>P<sub>2</sub>W<sub>18</sub>O<sub>62</sub>@[Cu<sub>6</sub>O(TZI)<sub>3</sub>(H<sub>2</sub>O)<sub>6</sub>]<sub>4</sub> for high-performance aerobic oxidation desulfurization of fuel.
Qu, Wenjia; Wei, Pengpeng; Li, Jingfang; Liang, Liye; Ma, Liqiang; Li, Guangming; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12610–12619; doi:10.1039/d4dt01568a

data_7716521
_publ_section_title
;
 Self-assembly of Dawson-type
 H<sub>6</sub>P<sub>2</sub>W<sub>18</sub>O<sub>62</sub>@[Cu<sub>6</sub>O(TZI)<sub>3</sub>(H<sub>2</sub>O)<sub>6</sub>]<sub>4</sub>
 for high-performance aerobic oxidation desulfurization of fuel.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12610
_journal_page_last               12619
_journal_paper_doi               10.1039/d4dt01568a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'0.25(C864 H288 Cu192 N384 O608), 4(Mo1 O13 P0.25 V0.25 W1.75)'
_chemical_formula_sum            'C216 H72 Cu48 Mo4 N96 O204 P V W7'
_chemical_formula_weight         12078.23
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-23 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   44.5464(2)
_cell_length_b                   44.5464(2)
_cell_length_c                   44.5464(2)
_cell_measurement_reflns_used    13270
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.6770
_cell_measurement_theta_min      3.2930
_cell_volume                     88397.1(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_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     86.00 118.00   0.50    9.00    --   45.62 139.00-176.00   64
  2  \w     35.00  60.00   0.50   45.00    --  106.06 -53.00  62.00   50
  3  \w   -114.00 -85.00   0.50    9.00    --  -45.62-125.00-150.00   58
  4  \w    -68.00 -31.00   0.50   45.00    -- -102.00  61.00-120.00   74
  5  \w   -136.00 -90.00   0.50   45.00    -- -102.00 -40.00 163.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0127479000
_diffrn_orient_matrix_UB_12      0.0089419000
_diffrn_orient_matrix_UB_13      0.0309143000
_diffrn_orient_matrix_UB_21      0.0268648000
_diffrn_orient_matrix_UB_22      0.0153875000
_diffrn_orient_matrix_UB_23      -0.0155123000
_diffrn_orient_matrix_UB_31      -0.0177253000
_diffrn_orient_matrix_UB_32      0.0295867000
_diffrn_orient_matrix_UB_33      -0.0013443000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            23710
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.464
_diffrn_reflns_theta_min         3.290
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.908
_exptl_crystal_description       block
_exptl_crystal_F_000             23152
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.757
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         4273
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0935
_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^)+(0.1753P)^2^+765.7305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2696
_refine_ls_wR_factor_ref         0.2732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4015
_reflns_number_total             4273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01568a2.cif
_cod_data_source_block           4_sq
_cod_depositor_comments          'Adding full bibliography for 7716521.cif.'
_cod_original_cell_volume        88397.1(12)
_cod_database_code               7716521
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Cu C N O P'
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.702
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{W1, V1, Mo1}
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(W1) = Uanis(V1) = Uanis(Mo1)
Uanis(O6B) = Uanis(O6A)
4. Others
 Fixed Sof: O9(0.08333) O10(0.25) W1(0.14583) P1(0.02083) O7(0.25) V1(0.02083)
 Mo1(0.08333) O6A(0.25) O6B(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4)
;
_shelx_res_checksum              48961
_shelx_fab_checksum              58
_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 1.615
_oxdiff_exptl_absorpt_empirical_full_min 0.727