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_7707268
_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         'Nb9 O193 P6 W45 Zn4, 19(O)'
_chemical_formula_sum            'Nb9 O212 P6 W45 Zn4'
_chemical_formula_weight         12948.74
_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            2
_cell_length_a                   34.2369(4)
_cell_length_b                   34.2369(4)
_cell_length_c                   13.7551(2)
_cell_measurement_reflns_used    27600
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.1980
_cell_measurement_theta_min      3.9240
_cell_volume                     13963.1(3)
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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    -32.00  52.00   1.00    2.00    --   35.62 -56.00 127.00   84
  2  \w     91.00 175.00   1.00   22.46    --  107.12  56.00 -89.00   84
  3  \w     40.00 124.00   1.00   22.46    --  107.12 -56.00 127.00   84
  4  \w   -108.00 -35.00   1.00    2.00    --  -35.62-178.00 150.00   73
  5  \w     55.00 108.00   1.00    2.00    --   35.62-178.00-180.00   53
  6  \w      1.00  75.00   1.00    2.00    --   35.62 -99.00  60.00   74
  7  \w     38.00 110.00   1.00   22.46    --  107.12 -95.00  30.00   72
  8  \w     38.00 110.00   1.00   22.46    --  107.12 -95.00 150.00   72
  9  \w     91.00 175.00   1.00   22.46    --  107.12  54.00 -59.00   84
 10  \w    100.00 177.00   1.00   22.46    --  107.12 111.00 -60.00   77
 11  \w   -103.00  -9.00   1.00    2.00    --  -35.62 -77.00-180.00   94
 12  \w   -103.00 -19.00   1.00    2.00    --  -35.62 -57.00 -90.00   84
 13  \w   -103.00 -19.00   1.00    2.00    --  -35.62 -57.00  30.00   84
 14  \w     38.00 126.00   1.00   22.46    --  107.12   0.00-150.00   88
;
_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      0.0226437000
_diffrn_orient_matrix_UB_12      0.0415639000
_diffrn_orient_matrix_UB_13      0.0670648000
_diffrn_orient_matrix_UB_21      0.0250472000
_diffrn_orient_matrix_UB_22      -0.0205854000
_diffrn_orient_matrix_UB_23      0.0533841000
_diffrn_orient_matrix_UB_31      0.0394637000
_diffrn_orient_matrix_UB_32      0.0233639000
_diffrn_orient_matrix_UB_33      -0.0721854000
_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  0.0694
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            66285
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.588
_diffrn_reflns_theta_min         3.542
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    37.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28728
_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 white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    3.080
_exptl_crystal_description       prism
_exptl_crystal_F_000             11210
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.117
_refine_diff_density_min         -5.377
_refine_diff_density_rms         0.520
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         17909
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+2064.7737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2131
_refine_ls_wR_factor_ref         0.2235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14582
_reflns_number_total             17909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00924a2.cif
_cod_data_source_block           xwr20191224-2
_cod_depositor_comments
'Adding full bibliography for 7707266--7707269.cif.'
_cod_original_cell_volume        13963.1(4)
_cod_database_code               7707268
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'P1 W1 O1 Nb1 Zn1 '
_shelx_estimated_absorpt_t_max   0.255
_shelx_estimated_absorpt_t_min   0.071
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O4-Zn2
 2.1 with sigma of 0.02
 Zn2_$1-O3_$1
 2.1 with sigma of 0.02
 Zn2-O3
 2.1 with sigma of 0.01
 O1-Zn1
 2.13 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O7) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O84)
\\sim Ueq, Uanis(O82) \\sim Ueq, Uanis(O88) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O40) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(P19)
\\sim Ueq, Uanis(P20) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O52) \\sim Ueq,
Uanis(O6) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O66) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(Zn2)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O10) = Uanis(O1)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58069
_shelx_hkl_checksum              61331
_shelx_fab_checksum              23387
_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 2.835
_oxdiff_exptl_absorpt_empirical_full_min 0.485