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_7707269
_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         'Mn4 Nb9 O193 P6 W45, 4(O), 6(C H O2)'
_chemical_formula_sum            'C6 H6 Mn4 Nb9 O209 P6 W45'
_chemical_formula_weight         12937.13
_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_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-21 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                   34.5750(3)
_cell_length_b                   34.5750(3)
_cell_length_c                   13.6491(2)
_cell_measurement_reflns_used    32089
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.1060
_cell_measurement_theta_min      4.1160
_cell_volume                     14130.5(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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(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 0.981
_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   -105.00  -8.00   1.00    3.50    --  -35.60 -76.00 -45.00   97
  2  \w     38.00 136.00   1.00   30.00    --  107.46 -76.00 -45.00   98
  3  \w     79.00 176.00   1.00   30.00    --  107.46  76.00  81.00   97
  4  \w     23.00  90.00   1.00    3.50    --   35.60-125.00-180.00   67
  5  \w    -33.00  54.00   1.00    3.50    --   35.60 -57.00  30.00   87
  6  \w     23.00  90.00   1.00    3.50    --   35.60-125.00  60.00   67
  7  \w    -33.00  54.00   1.00    3.50    --   35.60 -57.00-120.00   87
  8  \w     39.00 127.00   1.00   30.00    --  107.46 -61.00-150.00   88
  9  \w     36.00 112.00   1.00   30.00    --  107.46-111.00-120.00   76
 10  \w     36.00 112.00   1.00   30.00    --  107.46-111.00  90.00   76
 11  \w   -105.00  -7.00   1.00    3.50    --  -35.60 -77.00-180.00   98
 12  \w   -104.00 -17.00   1.00    3.50    --  -35.60 -57.00  30.00   87
 13  \w    -33.00  54.00   1.00    3.50    --   35.60 -57.00 150.00   87
 14  \w     17.00  92.00   1.00    3.50    --   35.60  57.00 -90.00   75
 15  \w      7.00 105.00   1.00    3.50    --   35.60  77.00 120.00   98
;
_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      -0.0407425000
_diffrn_orient_matrix_UB_12      0.0066718000
_diffrn_orient_matrix_UB_13      -0.0078969000
_diffrn_orient_matrix_UB_21      -0.0133456000
_diffrn_orient_matrix_UB_22      -0.0169586000
_diffrn_orient_matrix_UB_23      0.1058697000
_diffrn_orient_matrix_UB_31      0.0284716000
_diffrn_orient_matrix_UB_32      0.0480671000
_diffrn_orient_matrix_UB_33      0.0385347000
_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  0.0750
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            68752
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.382
_diffrn_reflns_theta_min         3.559
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    38.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30699
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.041
_exptl_crystal_description       block
_exptl_crystal_F_000             11206
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.692
_refine_diff_density_min         -3.042
_refine_diff_density_rms         0.535
_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     844
_refine_ls_number_reflns         17987
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+1926.4559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2073
_refine_ls_wR_factor_ref         0.2226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13792
_reflns_number_total             17987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00924a2.cif
_cod_data_source_block           xwr2020-7-18
_cod_depositor_comments
'Adding full bibliography for 7707266--7707269.cif.'
_cod_database_code               7707269
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'P1 W1 O1 Nb1 Mn1'
_shelx_estimated_absorpt_t_max   0.251
_shelx_estimated_absorpt_t_min   0.115
_reflns_odcompleteness_completeness 99.90
_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. Restrained distances
 Mn2-O4 = Mn1-O1
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O53)
\\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O3AA) \\sim Ueq,
Uanis(O8) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O59) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O63)
\\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(O13) \\sim Ueq,
Uanis(O8) \\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O58) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O67) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O72)
\\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(P2) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(O10)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O80) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O1(0.33333)
5.a Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C1AA(H1AA)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26958
_shelx_hkl_checksum              6265
_shelx_fab_checksum              28818
_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 2.270
_oxdiff_exptl_absorpt_empirical_full_min 0.274