Oxidovanadium(iv), oxidomolybdenum(vi) and cobalt(iii) complexes of o-phenylenediamine derivatives: oxidative dehydrogenation and photoluminescence
Chaudhuri, Satyabrata; Bera, Sachinath; Biswas, Manas Kumar; Roy, Amit Saha; Weyhermüller, Thomas; Ghosh, Prasanta; Inorg. Chem. Front. 1 (2014) 331–; doi:10.1039/C3QI00103B

data_4348005
_publ_section_title
;
 Oxidovanadium(iv), oxidomolybdenum(vi) and cobalt(iii) complexes of
 o-phenylenediamine derivatives: oxidative dehydrogenation and
 photoluminescence
;
_journal_issue                   4
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              331
_journal_paper_doi               10.1039/C3QI00103B
_journal_volume                  1
_journal_year                    2014
_chemical_compound_source        methanole
_chemical_formula_moiety         'C33 H35 N3 O2 V, 0.5(C H4 O)'
_chemical_formula_sum            'C33.5 H37 N3 O2.5 V'
_chemical_formula_weight         572.60
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_block_code                WGT-PG-500-06
_audit_creation_date             2011-03-09
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.22(5)
_cell_angle_beta                 83.19(5)
_cell_angle_gamma                88.86(5)
_cell_formula_units_Z            2
_cell_length_a                   9.340(3)
_cell_length_b                   11.616(7)
_cell_length_c                   13.836(4)
_cell_measurement_reflns_used    21602
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.8945
_cell_measurement_theta_min      2.6297
_cell_volume                     1447.6(11)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0929
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18275
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.97759
_exptl_absorpt_correction_T_min  0.95674
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0661P)^2^+1.0490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1707
_reflns_number_gt                5603
_reflns_number_total             8372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00103b2.cif
_cod_data_source_block           4
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_formula_sum        'C33.50 H37 N3 O2.50 V'
_cod_database_code               4348005