Vanadium complexes of different nuclearities in the catalytic oxidation of cyclohexane and cyclohexanol – An experimental and theoretical investigation
Sutradhar, M.; Martins, Luísa Margarida; Roy Barman, Tannistha; Kuznetsov, Maxim L.; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J. L.; New Journal of Chemistry 43 (2019) 17557–17570; doi:10.1039/C9NJ00348G

data_7058277
_publ_section_title
;
 Vanadium complexes of different nuclearities in the catalytic oxidation
 of cyclohexane and cyclohexanol -- An experimental and theoretical
 investigation
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17557
_journal_page_last               17570
_journal_paper_doi               10.1039/C9NJ00348G
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C33 H33 N6 O15 V3, 2(H2 O)'
_chemical_formula_sum            'C33 H37 N6 O17 V3'
_chemical_formula_weight         942.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-11-22 deposited with the CCDC.    2019-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                98.888(5)
_cell_angle_beta                 111.434(4)
_cell_angle_gamma                92.418(5)
_cell_formula_units_Z            2
_cell_length_a                   11.6728(12)
_cell_length_b                   13.1012(12)
_cell_length_c                   13.9688(12)
_cell_measurement_reflns_used    6123
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.33
_cell_measurement_theta_min      2.33
_cell_volume                     1953.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.934
_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  0.0793
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21572
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.449
_diffrn_reflns_theta_min         2.328
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6755
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1760
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+9.4895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.2215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3185
_reflns_number_total             6755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00348g2.cif
_cod_data_source_block           shelx
_cod_database_code               7058277
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              91617