A trigonal prismatic coordination geometry for vanadium in bis(2-oxidonaphthalene-1-carbaldehyde benzoylhydrazonato)vanadium(IV) dichloromethane hexane hemisolvate
Gao, Shan; Huo, Li-Hua; Zhao, Hui; Ng, Seik Weng; Acta Crystallographica Section E 61 (2005) m519–m521; doi:10.1107/S1600536805004174

data_2205238
_publ_section_title
;
 A trigonal prismatic coordination geometry for vanadium in
 bis(2-oxidonaphthalene-1-carbaldehyde benzoylhydrazonato)vanadium(IV)
 dichloromethane hexane hemisolvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m519
_journal_page_last               m521
_journal_paper_doi               10.1107/S1600536805004174
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[V (C18 H12 N2 O4)2], C H2 Cl2, 0.5C6 H14'
_chemical_formula_moiety         'C36 H24 N4 O4 V, C H2 Cl2, 0.5C6 H14'
_chemical_formula_sum            'C40 H33 Cl2 N4 O4 V'
_chemical_formula_weight         755.54
_chemical_name_systematic
;
bis(2-oxidonaphthalene-1-carbaldehyde benzoylhydrazonato)vanadium(IV)
dichloromethane hexane hemisolvate
;
_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                116.04(3)
_cell_angle_beta                 101.84(3)
_cell_angle_gamma                106.21(3)
_cell_formula_units_Z            2
_cell_length_a                   12.598(3)
_cell_length_b                   13.021(3)
_cell_length_c                   13.652(3)
_cell_measurement_reflns_used    15371
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1787.3(12)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17362
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.939
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8039
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.077
_refine_ls_R_factor_gt           0.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1036P)^2^+0.4047P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.160
_refine_ls_wR_factor_ref         0.174
_reflns_number_gt                5896
_reflns_number_total             8039
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6524.cif
_cod_data_source_block           I
_cod_original_cell_volume        1787.2(6)
_cod_database_code               2205238
_cod_database_fobs_code          2205238