Three Pd-decavanadates with a controllable molar ratio of Pd to decavanadate and their heterogeneous aerobic oxidation of benzylic C-H bonds.
Huang, Xianqiang; Li, Jikun; Shen, Guodong; Xin, Nana; Lin, Zhengguo; Chi, Yingnan; Dou, Jianmin; Li, Dacheng; Hu, Changwen; Dalton transactions (Cambridge, England : 2003) 47 (2018) 726–733; doi:10.1039/c7dt03898d

data_7044912
_publ_section_title
;
 Three Pd-decavanadates with a controllable molar ratio of Pd to
 decavanadate and their heterogeneous aerobic oxidation of benzylic C-H
 bonds.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              726
_journal_page_last               733
_journal_paper_doi               10.1039/c7dt03898d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'H52 N12 O36 Pd3 V10'
_chemical_formula_sum            'H52 N12 O36 Pd3 V10'
_chemical_formula_weight         1625.13
_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   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-11-12 deposited with the CCDC.
2017-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                115.251(2)
_cell_angle_beta                 108.0690(10)
_cell_angle_gamma                98.8730(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5424(8)
_cell_length_b                   11.2379(9)
_cell_length_c                   11.8608(11)
_cell_measurement_reflns_used    2854
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.171
_cell_measurement_theta_min      3.302
_cell_volume                     1031.12(16)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.979
_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  0.0186
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5199
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.043
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  0.5377
_exptl_absorpt_correction_T_min  0.4371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0375P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2948
_reflns_number_total             3550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03898d2.cif
_cod_data_source_block           131105c
_cod_depositor_comments
'Adding full bibliography for 7044911--7044914.cif.'
_cod_original_cell_volume        1031.12(15)
_cod_database_code               7044912
_shelx_estimated_absorpt_t_min   0.437
_shelx_estimated_absorpt_t_max   0.538
_shelxl_version_number           2014/6
_shelx_res_checksum              34651