#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/77/2007757.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2007757
loop_
_publ_author_name
'Guzman-Jimenez, Ilse Y.'
'Whitmire, Kenton H.'
_publ_section_title
;
 Bis(tetraethylammonium)
 tetra-μ-carbonyl-icosacarbonylhexairondithallate(2
 Fe---Fe)(8 Fe---Tl)(2--)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800053
_journal_paper_doi               10.1107/S0108270198099326
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '2(C8 H20 N )[Fe6 Tl2 (CO)24 ]'
_chemical_formula_structural     '[Et4N]2[Tl2Fe6(CO)24]'
_chemical_formula_sum            'C40 H40 Fe6 N2 O24 Tl2'
_chemical_formula_weight         1676.58
_chemical_name_systematic
; Ethanaminium, N,N,N-triethyl-,
tetra-.mu.-carbonyleicosacarbonyldithalla-
hexaferrate (2-) (2Fe-Fe) (8Fe-Tl) (2:1)
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.186(3)
_cell_length_b                   18.936(4)
_cell_length_c                   17.406(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      7.985
_cell_measurement_theta_min      3.630
_cell_volume                     5665(2)
_computing_cell_refinement
'MSC/AFC Software (Molecular Structure Corporation, 1995)'
_computing_data_collection
'MSC/AFC Software (Molecular Structure Corporation, 1995)'
_computing_data_reduction
'MSC/AFC Software (Molecular Structure Corporation, 1995)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1602
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            2047
_diffrn_reflns_theta_max         30.19
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.234
_exptl_absorpt_correction_T_max  0.235
_exptl_absorpt_correction_T_min  0.107
_exptl_absorpt_correction_type   'psi scans'
_exptl_absorpt_process_details
' (MSC/AFC, Molecular Structure Corporation, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.089
_refine_diff_density_min         -2.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.1755
_refine_ls_R_factor_obs          0.0492
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0689P)²+16.7215P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1690
_refine_ls_wR_factor_obs         0.1163
_reflns_number_observed          1043
_reflns_number_total             2047
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            qa0054.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+16.7215P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+16.7215P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5665.(2)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2007757
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Tl1 0.5000 0.06932(6) 0.07184(6) 0.0445(4) Uani d S 1 . Tl
Fe1 0.4305(2) 0.1662(2) 0.1731(2) 0.0541(8) Uani d . 1 . Fe
Fe2 0.5000 -0.0899(2) 0.0842(2) 0.0423(10) Uani d S 1 . Fe
C11 0.3798(12) 0.1933(12) 0.0936(13) 0.067(6) Uani d . 1 . C
O11 0.3419(9) 0.2114(10) 0.0422(10) 0.098(6) Uani d . 1 . O
C12 0.5000 0.2449(16) 0.1379(16) 0.048(7) Uani d S 1 . C
O12 0.5000 0.3079(11) 0.1090(10) 0.069(6) Uani d S 1 . O
C13 0.3923(12) 0.2321(10) 0.2390(13) 0.065(6) Uani d . 1 . C
O13 0.3673(10) 0.2759(9) 0.2835(10) 0.099(6) Uani d . 1 . O
C14 0.5000 0.1278(18) 0.249(2) 0.068(9) Uani d S 1 . C
O14 0.5000 0.1005(11) 0.3145(11) 0.068(6) Uani d S 1 . O
C15 0.3780(11) 0.0830(12) 0.1953(12) 0.063(6) Uani d . 1 . C
O15 0.3410(9) 0.0323(10) 0.2138(10) 0.096(6) Uani d . 1 . O
C21 0.5000 -0.1952(17) 0.0753(15) 0.046(7) Uani d S 1 . C
O21 0.5000 -0.2622(12) 0.0653(13) 0.082(7) Uani d S 1 . O
C22 0.5000 -0.0816(17) 0.1867(18) 0.059(8) Uani d S 1 . C
O22 0.5000 -0.0765(13) 0.2531(12) 0.084(7) Uani d S 1 . O
C23 0.5929(12) -0.0764(10) 0.0706(10) 0.050(5) Uani d . 1 . C
O23 0.6534(8) -0.0655(10) 0.0653(10) 0.092(5) Uani d . 1 . O
N1 0.8436(12) 0.0000 0.0000 0.062(7) Uani d S 1 . N
C1 0.7973(11) -0.0577(12) -0.0400(13) 0.071(6) Uani d . 1 . C
H1A 0.7641(11) -0.0341(12) -0.0770(13) 0.085 Uiso calc R 1 . H
H1B 0.7630(11) -0.0776(12) -0.0013(13) 0.085 Uiso calc R 1 . H
C2 0.8345(13) -0.1216(13) -0.0829(14) 0.096(8) Uani d . 1 . C
H2A 0.7940(13) -0.1510(13) -0.1035(14) 0.144 Uiso calc R 1 . H
H2B 0.8656(13) -0.1485(13) -0.0476(14) 0.144 Uiso calc R 1 . H
H2C 0.8666(13) -0.1046(13) -0.1240(14) 0.144 Uiso calc R 1 . H
C3 0.8912(13) -0.0409(17) 0.0577(18) 0.122(11) Uani d . 1 . C
H3A 0.9256(13) -0.0077(17) 0.0832(18) 0.147 Uiso calc R 1 . H
H3B 0.9239(13) -0.0736(17) 0.0294(18) 0.147 Uiso calc R 1 . H
C4 0.8493(19) -0.0825(16) 0.1190(16) 0.140(13) Uani d . 1 . C
H4A 0.8867(19) -0.1055(16) 0.1514(16) 0.210 Uiso calc R 1 . H
H4B 0.8165(19) -0.1172(16) 0.0953(16) 0.210 Uiso calc R 1 . H
H4C 0.8181(19) -0.0510(16) 0.1494(16) 0.210 Uiso calc R 1 . H
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'
N N 0.0061 0.0033 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Fe2 Tl1 Fe1 9_655 12_655 121.88(9) y
Fe2 Tl1 Fe1 9_655 . 121.88(9) y
Fe1 Tl1 Fe1 12_655 . 50.31(11) y
Fe2 Tl1 Fe2 9_655 . 102.26(9) y
Fe1 Tl1 Fe2 12_655 . 127.32(9) y
Fe1 Tl1 Fe2 . . 127.32(9) y
Fe2 Tl1 Tl1 9_655 9_655 54.57(8) y
Fe1 Tl1 Tl1 12_655 9_655 154.85(6) y
Fe1 Tl1 Tl1 . 9_655 154.85(6) y
Fe2 Tl1 Tl1 . 9_655 47.69(7) y
C11 Fe1 C13 . . 96.9(10) ?
C11 Fe1 C15 . . 100.1(10) ?
C13 Fe1 C15 . . 106.1(9) ?
C11 Fe1 C14 . . 169.6(11) ?
C13 Fe1 C14 . . 92.7(12) ?
C15 Fe1 C14 . . 80.7(10) ?
C11 Fe1 C12 . . 80.4(10) ?
C13 Fe1 C12 . . 84.1(10) ?
C15 Fe1 C12 . . 169.6(9) ?
C14 Fe1 C12 . . 97.0(10) ?
C11 Fe1 Fe1 . 12_655 120.5(7) ?
C13 Fe1 Fe1 . 12_655 111.1(7) ?
C15 Fe1 Fe1 . 12_655 119.1(6) ?
C14 Fe1 Fe1 . 12_655 51.7(7) ?
C12 Fe1 Fe1 . 12_655 53.5(5) ?
C11 Fe1 Tl1 . . 84.5(7) ?
C13 Fe1 Tl1 . . 175.8(7) ?
C15 Fe1 Tl1 . . 77.5(6) ?
C14 Fe1 Tl1 . . 85.6(9) ?
C12 Fe1 Tl1 . . 92.3(7) ?
Fe1 Fe1 Tl1 12_655 . 64.85(6) y
C23 Fe2 C23 . 12_655 155.3(12) ?
C23 Fe2 C22 . . 97.5(6) ?
C23 Fe2 C22 12_655 . 97.5(6) ?
C23 Fe2 C21 . . 98.4(7) ?
C23 Fe2 C21 12_655 . 98.4(7) ?
C22 Fe2 C21 . . 99.5(13) ?
C23 Fe2 Tl1 . 9_655 80.4(6) ?
C23 Fe2 Tl1 12_655 9_655 80.4(6) ?
C22 Fe2 Tl1 . 9_655 166.8(10) ?
C21 Fe2 Tl1 . 9_655 93.7(8) ?
C23 Fe2 Tl1 . . 80.4(7) ?
C23 Fe2 Tl1 12_655 . 80.4(7) ?
C22 Fe2 Tl1 . . 89.0(10) ?
C21 Fe2 Tl1 . . 171.5(8) ?
Tl1 Fe2 Tl1 9_655 . 77.74(9) y
O11 C11 Fe1 . . 176.2(19) ?
O12 C12 Fe1 . 12_655 143.5(5) ?
O12 C12 Fe1 . . 143.5(5) ?
Fe1 C12 Fe1 12_655 . 73.1(11) ?
O13 C13 Fe1 . . 179.4(18) ?
O14 C14 Fe1 . 12_655 141.5(7) ?
O14 C14 Fe1 . . 141.5(7) ?
Fe1 C14 Fe1 12_655 . 76.6(13) ?
O15 C15 Fe1 . . 174.8(17) ?
O21 C21 Fe2 . . 177.(2) ?
O22 C22 Fe2 . . 180.(3) ?
O23 C23 Fe2 . . 176.(2) ?
C3 N1 C3 4 . 114.(3) ?
C3 N1 C1 4 . 110.4(14) ?
C3 N1 C1 . . 102.7(15) ?
C3 N1 C1 4 4 102.7(15) ?
C3 N1 C1 . 4 110.4(14) ?
C1 N1 C1 . 4 116.9(19) ?
N1 C1 C2 . . 124.2(16) ?
N1 C3 C4 . . 119.(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Tl1 Fe2 9_655 2.744(4) y
Tl1 Fe1 12_655 2.811(3) y
Tl1 Fe1 . 2.811(3) y
Tl1 Fe2 . 3.023(4) y
Tl1 Tl1 9_655 3.626(2) y
Fe1 C11 . 1.71(2) ?
Fe1 C13 . 1.82(2) ?
Fe1 C15 . 1.86(2) ?
Fe1 C14 . 1.93(3) ?
Fe1 C12 . 2.01(3) ?
Fe1 Fe1 12_655 2.389(5) y
Fe2 C23 . 1.63(2) ?
Fe2 C23 12_655 1.63(2) ?
Fe2 C22 . 1.79(3) ?
Fe2 C21 . 2.00(3) ?
Fe2 Tl1 9_655 2.744(4) y
C11 O11 . 1.16(2) ?
C12 O12 . 1.29(3) ?
C12 Fe1 12_655 2.01(3) ?
C13 O13 . 1.21(2) ?
C14 O14 . 1.25(4) ?
C14 Fe1 12_655 1.93(3) ?
C15 O15 . 1.20(2) ?
C21 O21 . 1.28(3) ?
C22 O22 . 1.16(3) ?
C23 O23 . 1.06(2) ?
N1 C3 4 1.51(3) ?
N1 C3 . 1.51(3) ?
N1 C1 . 1.52(2) ?
N1 C1 4 1.52(2) ?
C1 C2 . 1.56(3) ?
C3 C4 . 1.51(4) ?
