A new binuclear oxovanadium(v) complex as a catalyst in combination with pyrazinecarboxylic acid (PCA) for efficient alkane oxygenation by H2O2.
Sutradhar, Manas; Shvydkiy, Nikita V.; Guedes da Silva, M Fátima C; Kirillova, Marina V.; Kozlov, Yuriy N.; Pombeiro, Armando J. L.; Shul'pin, Georgiy B.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11791–11803; doi:10.1039/c3dt50584g

data_7021620
_publ_section_title
;
 A new binuclear oxovanadium(v) complex as a catalyst in combination with
 pyrazinecarboxylic acid (PCA) for efficient alkane oxygenation by H2O2.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11791
_journal_page_last               11803
_journal_paper_doi               10.1039/c3dt50584g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C30 H36 N4 O10 V2'
_chemical_formula_sum            'C30 H36 N4 O10 V2'
_chemical_formula_weight         714.51
_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                78.910(3)
_cell_angle_beta                 68.375(3)
_cell_angle_gamma                65.880(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8519(5)
_cell_length_b                   9.8955(6)
_cell_length_c                   10.3659(6)
_cell_measurement_reflns_used    8472
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.31
_cell_measurement_theta_min      2.26
_cell_volume                     769.45(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13491
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.8718
_exptl_absorpt_correction_T_min  0.7843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             370
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2794
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.9981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                2582
_reflns_number_total             2794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50584g.txt
_cod_data_source_block           SB10VO1
_cod_database_code               7021620