Employing a new 12-connected topological open-framework copper borovanadate as an effective heterogeneous catalyst for oxidation of benzyl-alkanes.
Feng, Yuquan; Ding, Chenghua; Fan, Huitao; Zhong, Zhiguo; Qiu, Dongfang; Shi, Hengzhen; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18731–18736; doi:10.1039/c5dt03425f

data_7036786
_publ_section_title
;
 Employing a new 12-connected topological open-framework copper
 borovanadate as an effective heterogeneous catalyst for oxidation of
 benzyl-alkanes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18731
_journal_page_last               18736
_journal_paper_doi               10.1039/c5dt03425f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C8 H48 B20 Cu2 N8 Na2 O68 V12, 2(C4 H16 Cu N4), 4(H2 O), 3(O)'
_chemical_formula_sum            'C16 H88 B20 Cu4 N16 Na2 O75 V12'
_chemical_formula_weight         2832.64
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_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_date             2015-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-09-30 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 121.510(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4021(15)
_cell_length_b                   25.291(3)
_cell_length_c                   16.5039(15)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.50
_cell_volume                     4413.3(9)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22271
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.287
_exptl_absorpt_correction_T_max  0.6836
_exptl_absorpt_correction_T_min  0.5877
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.622
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         7749
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0549P)^2^+12.9781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                6911
_reflns_number_total             7749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03425f2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7036786.cif.'
_cod_original_cell_volume        4413.3(8)
_cod_database_code               7036786
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H31 of O31, All N(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  H19 of O19, H32 of O32, H33 of O33, H4 of O4
2. Restrained distances
 O1W-H1WB = O1W-H1WA = O2W-H2WA = O2W-H2WB = O4W-H4WA = O4W-H4WB
 0.83 with sigma of 0.02
 H1WB-H1WA = H2WA-H2WB = H4WA-H4WB
 1.37 with sigma of 0.02
 C7-C8
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cu1 \\sim O15: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(O5W) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O5W(0.5) O6W(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 N7(H7A,H7B), N8(H8A,H8B), C1(H1C,H1D), C2(H2C,H2D), C3(H3C,H3D), C4(H4C,H4D),
 C5(H5C,H5D), C6(H6C,H6D), C7(H7C,H7D), C8(H8C,H8D)
5.b Idealised tetrahedral OH refined as rotating group:
 O4(H4), O19(H19), O32(H32), O33(H33)
;
_olex2_submission_special_instructions 'No special instructions were received'