Thermal Dehydrogenation of Oxovanadium(IV) Complexes with Schiff Base Ligands Derived from meso-1,2-Diphenyl-1,2-ethanediamine in the Solid State
Gakuse Hoshina; Masanobu Tsuchimoto; Shigeru Ohba; Kiyohiko Nakajima; Hidehiro Uekusa; Yuji Ohashi; Hiroyuki Ishida; Masaaki Kojima; Inorganic Chemistry 37 (1998) 142–145; doi:10.1021/ic9705958

data_4322584
_publ_contact_author
; Dr. Masanobu Tsuchimoto
  Department of Chemistry
  Faculty of Science and Technology
  Keio University
  Hiyoshi 3-14-1, Kohoku-ku
  Yokohama, 223
  Japan
;
_publ_contact_author_email       ' tmoto@chem.keio.ac.jp'
_publ_contact_author_fax         '(81) 45 563 5967'
_publ_contact_author_phone       '(81) 45 563 1141 ext 3913'
_publ_section_title
;
 Thermal Dehydrogenation of Oxovanadium(IV) Complexes with Schiff Base
 Ligands Derived from meso-1,2-Diphenyl-1,2-ethanediamine in the Solid
 State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              142
_journal_page_last               145
_journal_paper_doi               10.1021/ic9705958
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         '(C32 H30 N2 O5 V)(H2 O)'
_chemical_formula_sum            'C32 H32 N2 O6 V'
_chemical_formula_weight         591.6
_chemical_name_systematic
;                                                                          
{N,N'-di-3-ethoxysalicylidene-(R,S)(S,R)-1,2-diphenyl-1,2-ethanediamine}
oxovanadium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source           'International Tables Vol.IV(1974)'
_audit_creation_date             97-05-10
_audit_creation_method           'manual editing'
_audit_update_record
;
?   
;
_cell_angle_alpha                90.000000(0)
_cell_angle_beta                 112.482(8)
_cell_angle_gamma                90.000000(0)
_cell_formula_units_Z            4
_cell_length_a                   16.528(2)
_cell_length_b                   11.031(2)
_cell_length_c                   17.189(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      15.005
_cell_measurement_theta_min      14.570
_cell_volume                     2895.7(7)
_computing_cell_refinement
; AFC/MSC Diffractometer Control System  
(Rigaku Corporation, 1993)
;
_computing_data_collection       ' AFC/MSC Diffractometer Control System  '
_computing_data_reduction        'local programs'
_computing_molecular_graphics    CRYSTAN-GM
_computing_publication_material  CRYSTAN-GM
_computing_structure_refinement  CRYSTAN-GM
_computing_structure_solution
' CRYSTAN-GM (Edwards, Gilmore, Mackay & Stewart, 1995)'
_diffrn_measurement_device_type  'Rigaku AFC-5'
_diffrn_measurement_method       '\q-2\q scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6891
_diffrn_reflns_theta_max         27.5
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.9374
_exptl_absorpt_correction_T_min  0.9215
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'(Coppens, Leiserowitz & Rabinovich, 1965)                     '
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1236.0
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.28
_refine_ls_hydrogen_treatment    refU
_refine_ls_number_parameters     402
_refine_ls_number_reflns         4029
_refine_ls_R_factor_obs          0.061
_refine_ls_shift/esd_max         0.04
_refine_ls_shift/esd_mean        0.0035
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w=1/[\s ^2^(F) + 0.000225F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.049
_reflns_number_observed          4029
_reflns_number_total             6664
_reflns_threshold_expression     '|F~o~| > 3\s(|F~o~|)'
_cod_data_source_file            ic9705958_1.cif
_cod_data_source_block           no5
_cod_original_cell_volume        2895.8(7)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C32 H32 N2 O6 V1    '
_cod_database_code               4322584