Four alkoxohexavanadate-based pd-polyoxovanadates as robust heterogeneous catalysts for oxidation of benzyl-alkanes.
Li, Ji-Kun; Huang, Xian-Qiang; Yang, Song; Ma, Hong-Wei; Chi, Ying-Nan; Hu, Chang-Wen; Inorganic chemistry 54 (2015) 1454–1461; doi:10.1021/ic502447b

data_4342329
_publ_section_title
;
 Four alkoxohexavanadate-based pd-polyoxovanadates as robust heterogeneous
 catalysts for oxidation of benzyl-alkanes.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1454
_journal_page_last               1461
_journal_paper_doi               10.1021/ic502447b
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C38 H58 N6 O24 Pd2 V6'
_chemical_formula_sum            'C38 H58 N6 O24 Pd2 V6'
_chemical_formula_weight         1501.34
_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-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 98.513(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.949(4)
_cell_length_b                   24.934(6)
_cell_length_c                   13.822(3)
_cell_measurement_reflns_used    3160
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.70
_cell_measurement_theta_min      2.21
_cell_volume                     5436(2)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.1148
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26240
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.528
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.714
_exptl_absorpt_correction_T_max  0.7954
_exptl_absorpt_correction_T_min  0.6739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.259
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       0.00024(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9504
_refine_ls_number_restraints     1399
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1552
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1496P)^2^+7.2122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2286
_refine_ls_wR_factor_ref         0.2849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4920
_reflns_number_total             9504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502447b_si_002.cif
_cod_data_source_block           1ma
_cod_depositor_comments
'Adding full bibliography for 4342328--4342332.cif.'
_cod_database_code               4342329
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.795
_shelxl_version_number           2014/6
_shelx_res_checksum              83978
_shelx_hkl_checksum              2297