A new polyoxometalate-based Mo/V coordinated crystalline hybrid and its catalytic activity in aerobic hydroxylation of benzene
Ge, Weilin; Long, Zhouyang; Cai, Xiaochun; Wang, Qian; Zhou, Yu; Xu, Yan; Wang, Jun; RSC Adv.  (2014) –; doi:10.1039/C4RA06736C

data_7218044
_publ_section_title
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 A new polyoxometalate-based Mo/V coordinated crystalline hybrid and its
 catalytic activity in aerobic hydroxylation of benzene
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA06736C
_journal_year                    2014
_chemical_formula_sum            'C60 H53 Mo12 N12 O50 P V4'
_chemical_formula_weight         3128.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.877(2)
_cell_angle_beta                 90.706(2)
_cell_angle_gamma                109.7960(10)
_cell_formula_units_Z            1
_cell_length_a                   11.4527(13)
_cell_length_b                   14.6366(17)
_cell_length_c                   14.6690(17)
_cell_measurement_reflns_used    3702
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.32
_cell_volume                     2222.7(4)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            15629
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  0.7824
_exptl_absorpt_correction_T_min  0.7386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00039(13)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         7737
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+1.3333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                5261
_reflns_number_total             7737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra06736c2.cif
_cod_data_source_block           a01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7218044