Controllable Synthesis of Lindqvist Alkoxopolyoxovanadate Clusters as Heterogeneous Catalysts for Sulfoxidation of Sulfides.
Li, Ji-Kun; Dong, Jing; Wei, Chuan-Ping; Yang, Song; Chi, Ying-Nan; Xu, Yan-Qing; Hu, Chang-Wen; Inorganic chemistry 56 (2017) 5748–5756; doi:10.1021/acs.inorgchem.7b00366

data_4345729
_publ_section_title
;
 Controllable Synthesis of Lindqvist Alkoxopolyoxovanadate Clusters as
 Heterogeneous Catalysts for Sulfoxidation of Sulfides.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5748
_journal_page_last               5756
_journal_paper_doi               10.1021/acs.inorgchem.7b00366
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C50 H62 Co2 N4 O27 V6'
_chemical_formula_sum            'C50 H62 Co2 N4 O27 V6'
_chemical_formula_weight         1574.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.3780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0869(4)
_cell_length_b                   11.1026(4)
_cell_length_c                   24.7041(9)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.46
_cell_volume                     3040.85(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29683
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.837
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  0.7847
_exptl_absorpt_correction_T_min  0.6455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.484
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0628P)^2^+4.5109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4812
_reflns_number_total             5653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00366_si_005.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4345729--4345733.cif.'
_cod_database_code               4345729
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.646
_shelx_estimated_absorpt_t_max   0.785
_shelx_res_checksum              41516
_shelx_hkl_checksum              78841