A nickel-modified polyoxometalate towards a highly efficient catalyst for selective oxidation of hydrocarbons
Zhou, Lei; Liu, Juan; Ji, Wenbin; Huang, Hui; Hu, Hailiang; Liu, Yang; Kang, Zhenhui; Journal of Materials Chemistry A 2 (2014) 12686–; doi:10.1039/C4TA02214A

data_7235772
_publ_section_title
;
 A nickel-modified polyoxometalate towards a highly efficient catalyst for
 selective oxidation of hydrocarbons
;
_journal_issue                   32
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              12686
_journal_paper_doi               10.1039/C4TA02214A
_journal_volume                  2
_journal_year                    2014
_chemical_formula_moiety         '[Ni2(C16H15N3F2Si)7(H2O)(SiMo12O40)]H2O'
_chemical_formula_sum            'C112 H109 F14 Mo12 N21 Ni2 O42 Si8'
_chemical_formula_weight         4180.59
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.319(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.369(5)
_cell_length_b                   24.336(4)
_cell_length_c                   25.550(5)
_cell_measurement_reflns_used    5414
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.684
_cell_measurement_theta_min      2.334
_cell_volume                     14465(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1485
_diffrn_reflns_av_sigmaI/netI    0.1647
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            73009
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.8708
_exptl_absorpt_correction_T_min  0.8478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS, Sheldrick, 1996'
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             8232
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.996
_refine_diff_density_min         -1.499
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1903
_refine_ls_number_reflns         25217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1949
_refine_ls_R_factor_gt           0.0818
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.2224
_reflns_number_gt                12299
_reflns_number_total             25217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ta02214a2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7235772