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_4077179
_publ_contact_author
;
        Wolfgang Petz
        Fachbereich Chemie
        Universit\"at Marburg
        Hans-Meerwein-Strasse
        35032 Marburg
        Germany

        Bernhard Neum\"uller
        Fachbereich Chemie
        Universit\"at Marburg
        Hans-Meerwein-Strasse
        35032 Marburg
        Germany
;
_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~Li}~2~{Fe~2~(CO)~8}]'
_chemical_formula_sum            'C24 H32 Fe2 Li2 O12'
_chemical_formula_weight         638.08
_chemical_name_systematic
; 
 ? 
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.82(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.000(1)
_cell_length_b                   30.312(3)
_cell_length_c                   9.833(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      11.0
_cell_volume                     2975.8(6)
_computing_cell_refinement       'EXPRESS (Enraf-Nonius)'
_computing_data_collection       'EXPRESS (Enraf-Nonius)'
_computing_data_reduction        'XCAD4 (Univ. of Marburg)'
_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)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CAD4 (Enraf-Nonius)'
_diffrn_measurement_method       omega-scan
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5550
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '7200 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '9 psi-scans'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columns
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0562
_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^)+(0.1043P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1707
_reflns_number_gt                3444
_reflns_number_total             4994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000597r.cif
_cod_data_source_block           pe3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_publ_contact_autor' tag replaced with '_publ_contact_author'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        2975.8(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077179