3D Open-Framework Vanadoborate as a Highly Effective Heterogeneous Pre-catalyst for the Oxidation of Alkylbenzenes
Chen, Hong; Deng, Youqian; Yu, Zhengbao; Zhao, Huishuang; Yao, Qingxia; Zou, Xiaodong; Bäckvall, Jan-E.; Sun, Junliang; Chemistry of Materials 25 (2013) 5031–; doi:10.1021/cm401400m

data_4001857
_publ_section_title
;
 3D Open-Framework Vanadoborate as a Highly Effective Heterogeneous
 Pre-catalyst for the Oxidation of Alkylbenzenes
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5031
_journal_paper_doi               10.1021/cm401400m
_journal_volume                  25
_journal_year                    2013
_chemical_formula_sum            'C8 H36 B18 N6 O61 V12 Zn2'
_chemical_formula_weight         2129.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   32.79240(10)
_cell_length_b                   32.79240(10)
_cell_length_c                   28.3220(2)
_cell_measurement_temperature    293(2)
_cell_volume                     30455.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            135762
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.940
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             16640
_platon_squeeze_details
;
;
_refine_diff_density_max         1.854
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         7774
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                7489
_reflns_number_total             7774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm401400m_si_002.cif
_cod_data_source_block           a2
_cod_original_sg_symbol_H-M      I41/acd
_cod_database_code               4001857