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_4342331
_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         'C36 H50 N6 O23 Pd2 V6'
_chemical_formula_sum            'C36 H50 N6 O23 Pd2 V6'
_chemical_formula_weight         1453.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                89.615(7)
_cell_angle_beta                 75.262(7)
_cell_angle_gamma                84.946(7)
_cell_formula_units_Z            1
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_cell_length_b                   10.709(2)
_cell_length_c                   12.472(3)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.76
_cell_measurement_theta_min      2.26
_cell_volume                     1362.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_diffrn_measured_fraction_theta_max 0.975
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_Laue_measured_fraction_full 0.958
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_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_l_max       14
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_diffrn_reflns_number            12571
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.047
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_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_max  0.7963
_exptl_absorpt_correction_T_min  0.6852
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_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.981
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_refine_ls_extinction_coef       0.0037(7)
_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   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4712
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2712
_reflns_number_total             4712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502447b_si_004.cif
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_cod_depositor_comments
'Adding full bibliography for 4342328--4342332.cif.'
_cod_original_cell_volume        1363.0(5)
_cod_database_code               4342331
_shelx_estimated_absorpt_t_min   0.685
_shelx_estimated_absorpt_t_max   0.796
_shelxl_version_number           2014/6
_shelx_res_checksum              47471
_shelx_hkl_checksum              55716