Immobilization of Keggin Polyoxovanadoniobate in Crystalline Solids as Effective Heterogeneous Catalysts towards Selective Oxidation of Benzyl-Alkanes
Hu, Jufang; Dong, Jing; Huang, Xianqiang; Chi, Yingnan; Lin, Zhengguo; Li, Jikun; Yang, Song; Ma, Hongwei; Hu, Changwen; Dalton Trans.  (2017) –; doi:10.1039/C7DT01122A

data_7043258
_publ_section_title
;
 Immobilization of Keggin Polyoxovanadoniobate in Crystalline Solids as
 Effective Heterogeneous Catalysts towards Selective Oxidation of
 Benzyl-Alkanes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01122A
_journal_year                    2017
_chemical_formula_moiety
'(Nb12 O42 P V2 H2.5 7.5-), 2(C6 H24 Co N6 3+), [Co (C2 N2 H8)2 (H2 O)2, 3+]0.5, 20(H2 O)'
_chemical_formula_sum            'C14 H100.5 Co2.5 N14 Nb12 O63 P V2'
_chemical_formula_weight         2868.67
_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_date             2017-06-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-05 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                93.4430(10)
_cell_angle_beta                 105.1070(10)
_cell_angle_gamma                117.0460(10)
_cell_formula_units_Z            1
_cell_length_a                   12.8884(4)
_cell_length_b                   14.1118(5)
_cell_length_c                   14.5289(5)
_cell_measurement_reflns_used    7326
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      2.44
_cell_volume                     2222.65(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22166
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.656
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_primary    'light yellow'
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1407
_refine_diff_density_max         2.290
_refine_diff_density_min         -2.468
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8414
_refine_ls_number_restraints     627
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0934P)^2^+23.7442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6012
_reflns_number_total             8414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01122a2.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C14 H100.50 Co2.50 N14 Nb12 O63 P V2'
_cod_database_code               7043258
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O1P(0.5) O2P(0.5) O3P(0.5) O4P(0.5) Co2(0.25) O1W(0.5) H1WA(0.5)
 H1WB(0.5) N7(0.5) H7A(0.5) H7B(0.5) N8(0.5) H8A(0.5) H8B(0.5) C7(0.5) H7C(0.5)
 H7D(0.5) C8(0.5) H8C(0.5) H8D(0.5) O3W(0.5) H3WA(0.5) H3WB(0.5) O4W(0.5)
 H4WA(0.5) H4WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 C1(H1C,H1D), C2(H2C,H2D), C3(H3C,H3D), C4(H4C,H4D), C5(H5C,H5D), C6(H6C,H6D),
 N7(H7A,H7B), N8(H8A,H8B), C7(H7C,H7D), C8(H8C,H8D)
;
_shelx_res_checksum              4209
_shelx_fab_checksum              59753
_olex2_submission_special_instructions 'No special instructions were received'