Reaction of Fe2(CO)9with Lithium: Preparation and Structures of Compounds with Strong Ion Pairing
Neumüller, Bernhard; Petz, Wolfgang; Organometallics 20 (2001) 163–; doi:10.1021/om000597r

data_4077180
_publ_section_title
;
 Reaction of Fe2(CO)9with Lithium:&#x00A0; Preparation and Structures of
 Compounds with Strong Ion Pairing
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              163
_journal_paper_doi               10.1021/om000597r
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         '[{(THF)~2~Na}{Fe~2~(CO)~8~}]~n~'
_chemical_formula_sum            'C24 H32 Fe2 Na2 O12'
_chemical_formula_weight         670.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary
;
  Patterson in space group Aba2; transformation into Cmca
;
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.982(1)
_cell_length_b                   12.998(2)
_cell_length_c                   23.862(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.71
_cell_volume                     3096.0(7)
_computing_cell_refinement       'IPDS (Stoe)'
_computing_data_collection       'IPDS (Stoe)'
_computing_data_reduction        'IPDS (Stoe)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997) PLATON-98 (Spek, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990) in Aba2'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'IPDS (Stoe)'
_diffrn_measurement_method       'IPDS (Stoe)'
_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  0.1675
_diffrn_reflns_av_sigmaI/netI    0.1213
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11241
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plates'
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.791
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                702
_reflns_number_total             1596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000597r.cif
_cod_data_source_block           pe4
_cod_original_sg_symbol_H-M      Cmca
_cod_database_code               4077180