Acetonitrilechlorotris(η^5^-cyclopentadienyl)vanadium(IV) tetrachloroferrate(III)
Honzíček, Jan; Císařová, Ivana; Vinklárek, Jaromír; Acta Crystallographica Section E 61 (2005) m149–m151; doi:10.1107/S1600536804032830

data_2204984
_publ_section_title
;
 Acetonitrilechlorotris(\h^5^-cyclopentadienyl)vanadium(IV)
 tetrachloroferrate(III)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m149
_journal_page_last               m151
_journal_paper_doi               10.1107/S1600536804032830
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[V (C5 H5)2 Cl (C2 H3 N)] [Fe Cl4]'
_chemical_formula_moiety         'C12 H13 Cl N V , Cl4 Fe'
_chemical_formula_sum            'C12 H13 Cl5 Fe N V'
_chemical_formula_weight         455.27
_chemical_name_systematic
;Acetonitrilechlorobis(\h^5^-cyclopentadienyl)vanadium(IV)
 tetrachloroiron(III)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3730(2)
_cell_length_b                   13.5290(3)
_cell_length_c                   17.2680(3)
_cell_measurement_reflns_used    27318
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1722.47(7)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26509
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.147
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.405
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Gaussian (Coppens & Hamilton, 1970)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.381
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   -0.003(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.6271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0535
_reflns_number_gt                3789
_reflns_number_total             3946
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ww6317.cif
_cod_data_source_block           I
_cod_database_code               2204984
_cod_database_fobs_code          2204984