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_4001859
_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            'C18 B27 N18 O90 V18'
_chemical_formula_weight         3117.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   22.0072(6)
_cell_length_b                   22.0072(6)
_cell_length_c                   11.2578(4)
_cell_measurement_temperature    373(2)
_cell_volume                     4721.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2819
_diffrn_reflns_theta_full        66.55
_diffrn_reflns_theta_max         66.55
_diffrn_reflns_theta_min         4.02
_exptl_absorpt_coefficient_mu    15.511
_exptl_absorpt_correction_T_max  0.5110
_exptl_absorpt_correction_T_min  0.2576
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21t (release 14-08-2012 CrysAlis171 .NET)
(compiled Aug 14 2012,18:12:40)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_density_diffrn    2.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3006
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         1839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0991P)^2^+59.1074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.1870
_reflns_number_gt                1635
_reflns_number_total             1839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm401400m_si_004.cif
_cod_data_source_block           vb4
_cod_original_cell_volume        4721.9(3)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4001859