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_7707266
_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         'Cu1.333 Nb3 O67 P2 W15, 4.333(O)'
_chemical_formula_sum            'Cu1.33 Nb3 O62.33 P2 W15'
_chemical_formula_weight         4180.47
_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     dual
_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            6
_cell_length_a                   34.2443(4)
_cell_length_b                   34.2443(4)
_cell_length_c                   13.7584(2)
_cell_measurement_reflns_used    11232
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.4860
_cell_measurement_theta_min      4.1060
_cell_volume                     13972.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_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    -67.00 -13.00   1.00    3.00    --  -35.62 140.00-105.00   54
  2  \w    128.00 174.00   1.00   25.86    --  107.12 130.00  80.00   46
  3  \w     79.00 117.00   1.00   25.86    --  107.12-127.00  66.00   38
  4  \w     39.00  65.00   1.00   25.86    --  107.12-127.00  66.00   26
  5  \w     58.00  95.00   1.00    3.00    --   35.62-140.00-164.00   37
  6  \w    -24.00  51.00   1.00    3.00    --   35.62 -57.00-150.00   75
  7  \w     68.00  98.00   1.00    3.00    --   35.62  57.00 -90.00   30
  8  \w     63.00 124.00   1.00   25.86    --  107.12 -61.00-180.00   61
  9  \w     40.00 124.00   1.00   25.86    --  107.12 -45.00-120.00   84
 10  \w     65.00 128.00   1.00   25.86    --  107.12  -5.00-170.00   63
;
_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      0.0368461000
_diffrn_orient_matrix_UB_12      0.0501652000
_diffrn_orient_matrix_UB_13      0.0010722000
_diffrn_orient_matrix_UB_21      0.0365986000
_diffrn_orient_matrix_UB_22      -0.0134570000
_diffrn_orient_matrix_UB_23      -0.0069344000
_diffrn_orient_matrix_UB_31      -0.0019705000
_diffrn_orient_matrix_UB_32      0.0012211000
_diffrn_orient_matrix_UB_33      -0.1117663000
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32969
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.638
_diffrn_reflns_theta_min         3.541
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    37.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.981
_exptl_crystal_description       block
_exptl_crystal_F_000             10802
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.351
_refine_diff_density_min         -3.671
_refine_diff_density_rms         0.559
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         17739
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1063P)^2^+635.3656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2105
_refine_ls_wR_factor_ref         0.2266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13159
_reflns_number_total             17739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00924a2.cif
_cod_data_source_block           xwr20200905
_cod_depositor_comments
'Adding full bibliography for 7707266--7707269.cif.'
_cod_original_cell_volume        13972.5(4)
_cod_database_code               7707266
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'P1 O1 W1 Nb1 Cu1 '
_shelx_estimated_absorpt_t_max   0.257
_shelx_estimated_absorpt_t_min   0.118
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O6-Cu2
 2.1 with sigma of 0.01
 Cu2-O4
 2.03 with sigma of 0.01
 O4-O6
 3 with sigma of 0.01
 O3_$1-O7_$2
 3.1 with sigma of 0.01
 O6_$1-O7_$2
 3.1 with sigma of 0.01
 O7_$1-O5
 3.1 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(P21) \\sim Ueq, Uanis(P20) \\sim Ueq, Uanis(O34)
\\sim Ueq, Uanis(O78) \\sim Ueq, Uanis(O62) \\sim Ueq, Uanis(O40) \\sim Ueq,
Uanis(O3) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(Cu2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O54) \\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O37) \\sim Ueq, Uanis(O58) \\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(O35)
\\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O27) \\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(O43) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O3) = Uanis(O4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              59270
_shelx_hkl_checksum              14022
_shelx_fab_checksum              89022
_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 7.965
_oxdiff_exptl_absorpt_empirical_full_min 0.461