Multinuclear transition metal-containing polyoxometalates constructed from Nb/W mixed-addendum precursors: synthesis, structures and catalytic performance.
Xiao, Wanru; Li, Shujun; Zhao, Yue; Ma, Yubin; Li, Na; Zhang, Jie; Chen, Xuenian; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8690–8695; doi:10.1039/d1dt00924a

data_7707267
_publ_section_title
;
 Multinuclear transition metal-containing polyoxometalates constructed
 from Nb/W mixed-addendum precursors: synthesis, structures and catalytic
 performance.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8690
_journal_page_last               8695
_journal_paper_doi               10.1039/d1dt00924a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'Co4 Nb9 O193 P6 W45, 1(O)'
_chemical_formula_sum            'C9 H0.5 Co4 Nb9 O219.5 P6 W45'
_chemical_formula_weight         13151.57
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-14 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   33.8321(5)
_cell_length_b                   33.8321(5)
_cell_length_c                   13.5769(3)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.3000
_cell_measurement_theta_min      4.0040
_cell_volume                     13458.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_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   -104.00 -50.00   1.00    5.00    --  -35.62-159.00 -97.00   54
  2  \w     39.00 124.00   1.00   35.00    --  107.12 -53.00 -73.00   85
  3  \w     40.00 124.00   1.00   35.00    --  107.12 -54.00 125.00   84
  4  \w     93.00 169.00   1.00   35.00    --  107.12  28.00  68.00   76
  5  \w     19.00  99.00   1.00    5.00    --   35.62  38.00 120.00   80
  6  \w     75.00 105.00   1.00    5.00    --   35.62 178.00  90.00   30
  7  \w     38.00  80.00   1.00   35.00    --  107.12 -95.00-180.00   42
  8  \w     69.00 104.00   1.00   35.00    --  107.12 -95.00-150.00   35
  9  \w    105.00 177.00   1.00   35.00    --  107.12 111.00  90.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0514841000
_diffrn_orient_matrix_UB_12      0.0189883000
_diffrn_orient_matrix_UB_13      -0.0164082000
_diffrn_orient_matrix_UB_21      0.0063652000
_diffrn_orient_matrix_UB_22      -0.0039337000
_diffrn_orient_matrix_UB_23      0.1111859000
_diffrn_orient_matrix_UB_31      -0.0088247000
_diffrn_orient_matrix_UB_32      -0.0488546000
_diffrn_orient_matrix_UB_33      -0.0153714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36548
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.552
_diffrn_reflns_theta_min         3.588
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    40.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.245
_exptl_crystal_description       prism
_exptl_crystal_F_000             11415
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.139
_refine_diff_density_min         -2.310
_refine_diff_density_rms         0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         17157
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0846P)^2^+338.0468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12489
_reflns_number_total             17157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00924a2.cif
_cod_data_source_block           xwr20190930-1
_cod_depositor_comments
'Adding full bibliography for 7707266--7707269.cif.'
_cod_original_cell_volume        13458.3(5)
_cod_original_formula_sum        'C9 H0.50 Co4 Nb9 O219.50 P6 W45'
_cod_database_code               7707267
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'P1 W1 Nb1 C1 O1 N1 Co1 B1'
_shelx_estimated_absorpt_t_max   0.237
_shelx_estimated_absorpt_t_min   0.107
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 Co2-O4
 2.1 with sigma of 0.02
 O3-Co2
 2.05 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O00W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O1(0.33333)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86178
_shelx_hkl_checksum              10330
_shelx_fab_checksum              67730
_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 1.701
_oxdiff_exptl_absorpt_empirical_full_min 0.673