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_4342330
_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         'C46 H82 N8 O25 Pd2 V6'
_chemical_formula_sum            'C46 H82 N8 O25 Pd2 V6'
_chemical_formula_weight         1665.63
_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'
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_cell_angle_beta                 73.385(6)
_cell_angle_gamma                78.023(5)
_cell_formula_units_Z            1
_cell_length_a                   10.7283(8)
_cell_length_b                   11.9106(6)
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_cell_measurement_reflns_used    3358
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      3.19
_cell_volume                     1573.04(19)
_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.996
_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  0.0177
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.975
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_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9314
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         3.194
_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
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_refine_diff_density_max         1.061
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_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.454
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0789P)^2^+2.9975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                4476
_reflns_number_total             5546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502447b_si_006.cif
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_cod_depositor_comments
'Adding full bibliography for 4342328--4342332.cif.'
_cod_database_code               4342330
_shelx_estimated_absorpt_t_min   0.707
_shelx_estimated_absorpt_t_max   0.796
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_shelx_res_checksum              20373
_shelx_hkl_checksum              3802