Two POM-based compounds containing Zn-capped Keggin anions as decent heterogeneous catalysts for sulfur oxidation and cycloaddition of CO2 reactions
Zhu, Yinhua; Yang, Jianbo; Liu, Xiaomei; Wang, Jilei; Ping, Qingdong; Du, Zeyu; Li, Jianian; Zang, Tingting; Mei, Hua; Xu, Yan; Dalton Transactions  (2022) –; doi:10.1039/D1DT04348J

data_7709332
_publ_section_title
;
 Two POM-based compounds containing Zn-capped Keggin anions as decent
 heterogeneous catalysts for sulfur oxidation and cycloaddition of CO2
 reactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04348J
_journal_year                    2022
_chemical_formula_sum            'C59 H99 Mo12 N8 O40 P Zn4'
_chemical_formula_weight         3004.19
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-11-01 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   32.635(2)
_cell_length_b                   32.635(2)
_cell_length_c                   34.282(3)
_cell_measurement_reflns_used    9569
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.593
_cell_measurement_theta_min      2.246
_cell_volume                     36512(4)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            128461
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.248
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_description       block
_exptl_crystal_F_000             23488
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 6355 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.489(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1124
_refine_ls_number_reflns         16094
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+259.7553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.963
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14269
_reflns_number_total             16094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04348j2.cif
_cod_data_source_block           a01_CCDC1
_cod_original_cell_volume        36512(6)
_cod_database_code               7709332
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.736
_exptl_absorpt_special_details   '(SADABS; Sheldrick, 2003)'
_shelx_res_checksum              71895
_shelx_hkl_checksum              40329