Redetermination of (acetonitrile-κ<i>N</i>)dicarbonyl(η^5^-cyclopentadienyl)iron(II) tetrafluoridoborate
Kückmann, Theresa; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section E 68 (2012) m966–; doi:10.1107/S1600536812027857

data_2235670
_publ_section_title
;
 Redetermination of
 (acetonitrile-\k<i>N</i>)dicarbonyl(\h^5^-cyclopentadienyl)iron(II)
 tetrafluoridoborate
;
_journal_coeditor_code           WM2643
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m966
_journal_paper_doi               10.1107/S1600536812027857
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Fe (C5 H5) (C2 H3 N) (C O)2] B F4'
_chemical_formula_moiety         'C9 H8 Fe N O2 +, B F4 -'
_chemical_formula_sum            'C9 H8 B F4 Fe N O2'
_chemical_formula_weight         304.82
_chemical_name_systematic
;
(acetonitrile-\k<i>N</i>)dicarbonyl(\h^5^-cyclopentadienyl)iron(II)
tetrafluoridoborate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.192(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8842(7)
_cell_length_b                   15.289(2)
_cell_length_c                   11.4353(12)
_cell_measurement_reflns_used    6543
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      3.6
_cell_volume                     1198.7(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6372
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.55
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  0.8596
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>MULABS</i>; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.430
_refine_diff_density_min         -0.873
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2222
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0822P)^2^+3.3996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                1976
_reflns_number_total             2222
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2643.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2235670
_cod_database_fobs_code          2235670