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_4322585
_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_sum            'C33 H32.5 N2.5 O6.5 V'
_chemical_formula_weight         619.07
_chemical_name_systematic
; 
 ? 
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.89(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.884(1)
_cell_length_b                   12.084(1)
_cell_length_c                   26.192(2)
_cell_measurement_temperature    293(2)
_cell_volume                     6247.9(8)
_computing_cell_refinement       'CONTROL (Rigaku, 1994)'
_computing_data_collection       'CONTROL (Rigaku, 1994)'
_computing_data_reduction        'CONTROL (Rigaku, 1994)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       RAXIS-IICS
_diffrn_measurement_method       'Weissenberg method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'RU300 Rigaku rotating Mo anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1287
_diffrn_reflns_av_sigmaI/netI    0.1235
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35532
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             2584
_exptl_crystal_preparation       'grown from acetonitrile solution'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.01
_refine_diff_density_max         .606
_refine_diff_density_min         -.459
_refine_diff_density_rms         .068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.950
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         10999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.1806
_refine_ls_R_factor_obs          0.0702
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2223
_refine_ls_wR_factor_obs         0.1556
_reflns_number_observed          5875
_reflns_number_total             13569
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9705958_2.cif
_cod_data_source_block           vana
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0951P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322585