A Giant Mo/Ta/W Ternary Mixed-Addenda Polyoxometalate with Efficient Photocatalytic Activity for Primary Amines Coupling.
Li, Shujun; Li, Gang; Ji, Panpan; Zhang, Jiangwei; Liu, Shuxia; Zhang, Jie; Chen, Xuenian; ACS applied materials & interfaces  (2019) –; doi:10.1021/acsami.9b16694

data_4516211
_publ_section_title
;
 A Giant Mo/Ta/W Ternary Mixed-Addenda Polyoxometalate with Efficient
 Photocatalytic Activity for Primary Amines Coupling.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.9b16694
_journal_year                    2019
_chemical_formula_moiety         'C6 H9 K3 Mo8 O399 P12 Ta18 W90'
_chemical_formula_sum            'C6 H9 K3 Mo8 O399 P12 Ta18 W90'
_chemical_formula_weight         27524.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.529(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.8886(7)
_cell_length_b                   24.9746(3)
_cell_length_c                   57.2531(12)
_cell_measurement_reflns_used    77488
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.500
_cell_measurement_theta_min      1.536
_cell_volume                     54387.2(17)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Synchrotron radiation X-ray'
_diffrn_radiation_wavelength     0.6229
_diffrn_reflns_av_R_equivalents  0.1072
_diffrn_reflns_av_unetI/netI     0.1815
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            227632
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.536
_exptl_absorpt_coefficient_mu    22.880
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ad
_exptl_crystal_density_diffrn    3.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             49416
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.825
_refine_diff_density_min         -4.644
_refine_diff_density_rms         0.606
_refine_ls_extinction_coef       0.000040(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     5158
_refine_ls_number_reflns         109898
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.1036
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1997
_refine_ls_wR_factor_ref         0.2525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                88611
_reflns_number_total             109898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b16694_si_002.cif
_cod_data_source_block           compound1
_cod_database_code               4516211
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 W68-O14
 1.92 with sigma of 0.02
 W1-O110
 2 with sigma of 0.02
 Ta5-O188
 2 with sigma of 0.02
 Mo3-O295
 2 with sigma of 0.02
 K2-O379
 2.5 with sigma of 0.02
 W19-O9AA
 1.6 with sigma of 0.02
 Mo1-O129 = Mo1-O274
 1.95 with sigma of 0.02
 Mo1-O284 = Mo1-O87 = Mo1-O247
 1.78 with sigma of 0.02
 C6-C2
 1.53 with sigma of 0.02
 O9-O14
 2.95 with sigma of 0.04
 O192-O14
 2.88 with sigma of 0.04
3. Restrained planarity
 O347, O74, C1, C4
 with sigma of 0.1
 O344, O85, C5, C3
 with sigma of 0.1
 O359, O324, C6, C2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(K1) = Uanis(K3) = Uanis(K2)
Uanis(O295) = Uanis(O37)
5.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              38848
_shelx_hkl_checksum              65518
_shelx_fab_checksum              39127
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'