Novel oxovanadium(iv) complexes with 4-acyl pyrazolone ligands: synthesis, crystal structure and catalytic activity towards the oxidation of benzylic alcohols
Parihar, Sanjay; Jadeja, R. N.; Gupta, Vivek K.; RSC Advances 4 (2014) 10295–; doi:10.1039/c3ra46896h

data_7239444
_publ_section_title
;
 Novel oxovanadium(iv) complexes with 4-acyl pyrazolone ligands:
 synthesis, crystal structure and catalytic activity towards the oxidation
 of benzylic alcohols
;
_journal_issue                   20
_journal_name_full               'RSC Advances'
_journal_page_first              10295
_journal_paper_doi               10.1039/c3ra46896h
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C36 H32 N4 O6 V, C2 H3 N'
_chemical_formula_sum            'C38 H35 N5 O6 V'
_chemical_formula_weight         708.65
_chemical_name_systematic
;
 Bis(5-methyl-4-benzoyl-2-p-tolyl-2,4-dihydro-pyrazol-3-one)V(IV)
 acetonitrile solvate 
;
_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_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.196(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2079(7)
_cell_length_b                   11.4667(5)
_cell_length_c                   18.6877(8)
_cell_measurement_reflns_used    5156
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9490
_cell_measurement_theta_min      3.3659
_cell_volume                     3558.5(3)
_computing_cell_refinement       'SAINT 6.45  (Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45  (Bruker, 2003)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  PLATON(Spek,1999)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0324
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14753
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.9366
_exptl_absorpt_correction_T_min  0.9070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2003'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6979
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0574P)^2^+0.3120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                4587
_reflns_number_total             6979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra46896h.txt
_cod_data_source_block           jadeja12
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7239444