#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:37:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178660 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/71/4077179.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4077179
loop_
_publ_author_name
'Neumüller, Bernhard'
'Petz, Wolfgang'
_publ_contact_author
;
        Wolfgang Petz
        Fachbereich Chemie
        Universität Marburg
        Hans-Meerwein-Strasse
        35032 Marburg
        Germany

        Bernhard Neumüller
        Fachbereich Chemie
        Universität Marburg
        Hans-Meerwein-Strasse
        35032 Marburg
        Germany
;
_publ_section_title
;
 Reaction of Fe2(CO)9with Lithium:  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/[σ²(Fo²)+(0.1043P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.03044(7) 0.14028(2) 0.04571(8) 0.0259(2) Uani 1 1 d .
Fe2 Fe 0.23308(7) 0.11200(2) 0.00632(8) 0.0255(2) Uani 1 1 d .
C1 C 0.1005(5) 0.15408(16) -0.1040(6) 0.0289(11) Uani 1 1 d .
O1 O 0.0737(4) 0.17972(12) -0.2059(5) 0.0435(10) Uani 1 1 d .
C2 C 0.0832(5) 0.08196(16) 0.0218(5) 0.0253(11) Uani 1 1 d .
O2 O 0.0500(3) 0.04368(9) 0.0255(4) 0.0253(8) Uani 1 1 d .
C3 C -0.1333(6) 0.14421(17) -0.0947(7) 0.0375(13) Uani 1 1 d .
O3 O -0.2406(4) 0.14910(14) -0.1884(5) 0.0569(12) Uani 1 1 d .
C4 C 0.0820(5) 0.19379(17) 0.1196(6) 0.0349(12) Uani 1 1 d .
O4 O 0.1165(5) 0.22888(13) 0.1655(5) 0.0588(12) Uani 1 1 d .
C5 C 0.0074(6) 0.12072(17) 0.2055(7) 0.0373(13) Uani 1 1 d .
O5 O -0.0125(5) 0.10753(15) 0.3039(5) 0.0651(13) Uani 1 1 d .
C6 C 0.2292(5) 0.07916(16) -0.1426(6) 0.0306(12) Uani 1 1 d .
O6 O 0.2273(4) 0.05793(13) -0.2407(5) 0.0482(10) Uani 1 1 d .
C7 C 0.3533(5) 0.15371(18) 0.0174(7) 0.0400(14) Uani 1 1 d .
O7 O 0.4269(4) 0.17977(14) 0.0144(6) 0.0663(14) Uani 1 1 d .
C8 C 0.3442(5) 0.08556(18) 0.1755(7) 0.0393(13) Uani 1 1 d .
O8 O 0.4168(5) 0.06835(17) 0.2834(6) 0.0733(15) Uani 1 1 d .
Li1 Li 0.0901(10) 0.2057(3) -0.3707(13) 0.048(3) Uani 1 1 d .
O9 O -0.0829(4) 0.20279(15) -0.5314(5) 0.0599(12) Uani 1 1 d .
C9 C -0.1902(10) 0.1784(4) -0.5286(11) 0.116(4) Uani 1 1 d .
H91 H -0.1719 0.1464 -0.5290 0.156(8) Uiso 1 1 calc R
H92 H -0.2022 0.1853 -0.4367 0.156(8) Uiso 1 1 calc R
C10 C -0.3055(10) 0.1895(6) -0.6550(13) 0.179(8) Uani 1 1 d .
H101 H -0.3709 0.2041 -0.6249 0.156(8) Uiso 1 1 calc R
H102 H -0.3476 0.1626 -0.7128 0.156(8) Uiso 1 1 calc R
C11 C -0.2666(10) 0.2190(5) -0.7451(15) 0.177(7) Uani 1 1 d .
H111 H -0.2898 0.2059 -0.8452 0.156(8) Uiso 1 1 calc R
H112 H -0.3149 0.2474 -0.7588 0.156(8) Uiso 1 1 calc R
C12 C -0.1284(8) 0.2261(3) -0.6723(9) 0.074(2) Uani 1 1 d .
H121 H -0.1088 0.2580 -0.6549 0.156(8) Uiso 1 1 calc R
H122 H -0.0832 0.2146 -0.7334 0.156(8) Uiso 1 1 calc R
O10 O 0.2404(4) 0.19152(13) -0.4118(5) 0.0547(12) Uani 1 1 d .
C13 C 0.3231(9) 0.2236(2) -0.4380(12) 0.089(3) Uani 1 1 d .
H131 H 0.3727 0.2410 -0.3460 0.156(8) Uiso 1 1 calc R
H132 H 0.2677 0.2440 -0.5189 0.156(8) Uiso 1 1 calc R
C14 C 0.4190(11) 0.1990(4) -0.4826(16) 0.129(4) Uani 1 1 d .
H141 H 0.4050 0.2069 -0.5858 0.156(8) Uiso 1 1 calc R
H142 H 0.5127 0.2057 -0.4134 0.156(8) Uiso 1 1 calc R
C15 C 0.3906(12) 0.1540(4) -0.4742(15) 0.124(4) Uani 1 1 d .
H151 H 0.4747 0.1380 -0.4148 0.156(8) Uiso 1 1 calc R
H152 H 0.3510 0.1412 -0.5762 0.156(8) Uiso 1 1 calc R
C16 C 0.2976(9) 0.1487(2) -0.4047(10) 0.076(2) Uani 1 1 d .
H161 H 0.2273 0.1268 -0.4601 0.156(8) Uiso 1 1 calc R
H162 H 0.3453 0.1388 -0.2994 0.156(8) Uiso 1 1 calc R
Li2 Li 0.0431(8) -0.0048(3) -0.1144(9) 0.0291(18) Uani 1 1 d .
O11 O -0.0833(4) 0.01182(12) -0.3104(4) 0.0393(9) Uani 1 1 d .
C17 C -0.1815(6) -0.0179(2) -0.4149(7) 0.0533(17) Uani 1 1 d .
H171 H -0.1981 -0.0432 -0.3613 0.156(8) Uiso 1 1 calc R
H172 H -0.1503 -0.0292 -0.4892 0.156(8) Uiso 1 1 calc R
C18 C -0.3068(6) 0.0093(2) -0.4908(7) 0.0517(16) Uani 1 1 d .
H181 H -0.3708 0.0033 -0.4462 0.156(8) Uiso 1 1 calc R
H182 H -0.3508 0.0025 -0.5992 0.156(8) Uiso 1 1 calc R
C19 C -0.2612(6) 0.0575(2) -0.4657(6) 0.0455(15) Uani 1 1 d .
H191 H -0.2865 0.0729 -0.5624 0.156(8) Uiso 1 1 calc R
H192 H -0.3014 0.0732 -0.4063 0.156(8) Uiso 1 1 calc R
C20 C -0.1100(6) 0.0548(2) -0.3805(7) 0.0535(17) Uani 1 1 d .
H201 H -0.0662 0.0578 -0.4497 0.156(8) Uiso 1 1 calc R
H202 H -0.0766 0.0784 -0.3040 0.156(8) Uiso 1 1 calc R
O12 O 0.2176(4) -0.02852(12) -0.0553(4) 0.0394(9) Uani 1 1 d .
C21 C 0.2892(7) -0.0461(2) -0.1351(9) 0.062(2) Uani 1 1 d .
H211 H 0.3426 -0.0229 -0.1554 0.156(8) Uiso 1 1 calc R
H212 H 0.2270 -0.0593 -0.2313 0.156(8) Uiso 1 1 calc R
C22 C 0.3784(9) -0.0806(3) -0.0318(13) 0.102(4) Uani 1 1 d .
H221 H 0.3308 -0.1092 -0.0453 0.156(8) Uiso 1 1 calc R
H222 H 0.4599 -0.0850 -0.0493 0.156(8) Uiso 1 1 calc R
C23 C 0.4127(7) -0.0622(3) 0.1201(11) 0.086(3) Uani 1 1 d .
H231 H 0.4317 -0.0861 0.1951 0.156(8) Uiso 1 1 calc R
H232 H 0.4915 -0.0425 0.1514 0.156(8) Uiso 1 1 calc R
C24 C 0.2911(6) -0.0374(2) 0.1021(7) 0.0560(18) Uani 1 1 d .
H241 H 0.2358 -0.0550 0.1397 0.156(8) Uiso 1 1 calc R
H242 H 0.3161 -0.0094 0.1591 0.156(8) Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C3 Fe1 C4 107.9(2) . .
C3 Fe1 C5 103.6(3) . .
C4 Fe1 C5 94.7(2) . .
C3 Fe1 C2 103.4(2) . .
C4 Fe1 C2 147.0(2) . .
C5 Fe1 C2 87.9(2) . .
C3 Fe1 C1 89.5(2) . .
C4 Fe1 C1 87.4(2) . .
C5 Fe1 C1 165.3(2) . .
C2 Fe1 C1 82.5(2) . .
C3 Fe1 Fe2 125.06(19) . .
C4 Fe1 Fe2 102.67(18) . .
C5 Fe1 Fe2 118.22(18) . .
C2 Fe1 Fe2 48.87(14) . .
C1 Fe1 Fe2 47.27(15) . .
C6 Fe2 C8 106.9(2) . .
C6 Fe2 C7 102.1(3) . .
C8 Fe2 C7 93.5(3) . .
C6 Fe2 C1 99.2(2) . .
C8 Fe2 C1 153.4(2) . .
C7 Fe2 C1 86.1(2) . .
C6 Fe2 C2 94.3(2) . .
C8 Fe2 C2 89.3(2) . .
C7 Fe2 C2 161.8(2) . .
C1 Fe2 C2 83.5(2) . .
C6 Fe2 Fe1 126.63(17) . .
C8 Fe2 Fe1 107.89(19) . .
C7 Fe2 Fe1 114.78(18) . .
C1 Fe2 Fe1 49.72(15) . .
C2 Fe2 Fe1 47.60(14) . .
O1 C1 Fe2 140.4(4) . .
O1 C1 Fe1 136.3(4) . .
Fe2 C1 Fe1 83.0(2) . .
C1 O1 Li1 155.7(5) . .
O2 C2 Fe1 140.1(4) . .
O2 C2 Fe2 136.2(4) . .
Fe1 C2 Fe2 83.54(19) . .
C2 O2 Li2 142.3(4) . 3
C2 O2 Li2 127.3(4) . .
Li2 O2 Li2 89.4(4) 3 .
O3 C3 Fe1 176.5(5) . .
O4 C4 Fe1 178.5(5) . .
C4 O4 Li1 146.9(6) . 4_566
O5 C5 Fe1 177.2(6) . .
O6 C6 Fe2 179.3(5) . .
O7 C7 Fe2 175.4(6) . .
O8 C8 Fe2 179.0(6) . .
O1 Li1 O9 105.8(5) . .
O1 Li1 O10 119.6(5) . .
O9 Li1 O10 117.9(6) . .
O1 Li1 O4 108.6(6) . 4_565
O9 Li1 O4 102.3(5) . 4_565
O10 Li1 O4 100.7(5) . 4_565
C9 O9 C12 108.7(6) . .
C9 O9 Li1 124.5(6) . .
C12 O9 Li1 126.7(5) . .
C10 C9 O9 108.3(8) . .
C9 C10 C11 107.6(9) . .
C12 C11 C10 108.6(9) . .
C11 C12 O9 106.2(7) . .
C13 O10 C16 109.1(6) . .
C13 O10 Li1 124.0(5) . .
C16 O10 Li1 126.5(5) . .
O10 C13 C14 107.1(7) . .
C15 C14 C13 105.3(8) . .
C14 C15 C16 110.5(8) . .
O10 C16 C15 104.9(7) . .
O12 Li2 O11 128.6(5) . .
O12 Li2 O2 106.4(4) . 3
O11 Li2 O2 108.0(4) . 3
O12 Li2 O2 109.1(4) . .
O11 Li2 O2 107.6(4) . .
O2 Li2 O2 90.6(4) 3 .
O12 Li2 Li2 115.7(5) . 3
O11 Li2 Li2 115.7(5) . 3
O2 Li2 Li2 45.4(3) 3 3
O2 Li2 Li2 45.2(3) . 3
C20 O11 C17 106.2(4) . .
C20 O11 Li2 129.5(4) . .
C17 O11 Li2 124.1(4) . .
O11 C17 C18 105.5(5) . .
C17 C18 C19 105.8(5) . .
C20 C19 C18 104.3(5) . .
O11 C20 C19 105.6(5) . .
C21 O12 C24 109.3(5) . .
C21 O12 Li2 133.9(5) . .
C24 O12 Li2 116.1(4) . .
O12 C21 C22 104.1(6) . .
C23 C22 C21 103.6(7) . .
C24 C23 C22 103.6(6) . .
O12 C24 C23 107.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C3 1.754(6) .
Fe1 C4 1.770(5) .
Fe1 C5 1.794(6) .
Fe1 C2 1.906(5) .
Fe1 C1 1.971(5) .
Fe1 Fe2 2.5649(10) .
Fe2 C6 1.756(5) .
Fe2 C8 1.788(6) .
Fe2 C7 1.800(6) .
Fe2 C1 1.898(5) .
Fe2 C2 1.944(5) .
C1 O1 1.203(6) .
O1 Li1 1.877(11) .
C2 O2 1.221(5) .
O2 Li2 1.988(9) 3
O2 Li2 1.993(9) .
C3 O3 1.162(7) .
C4 O4 1.156(6) .
O4 Li1 2.015(11) 4_566
C5 O5 1.150(7) .
C6 O6 1.153(6) .
C7 O7 1.141(7) .
C8 O8 1.151(7) .
Li1 O9 1.898(12) .
Li1 O10 1.908(10) .
Li1 O4 2.015(11) 4_565
O9 C9 1.402(9) .
O9 C12 1.445(8) .
C9 C10 1.394(13) .
C10 C11 1.445(14) .
C11 C12 1.399(11) .
O10 C13 1.426(8) .
O10 C16 1.432(7) .
C13 C14 1.500(11) .
C14 C15 1.409(13) .
C15 C16 1.459(12) .
Li2 O12 1.897(9) .
Li2 O11 1.911(9) .
Li2 O2 1.988(9) 3
Li2 Li2 2.800(17) 3
O11 C20 1.444(7) .
O11 C17 1.449(7) .
C17 C18 1.507(8) .
C18 C19 1.528(9) .
C19 C20 1.518(8) .
O12 C21 1.428(7) .
O12 C24 1.438(7) .
C21 C22 1.502(10) .
C22 C23 1.487(12) .
C23 C24 1.480(10) .
