#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/96/2239646.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_2239646
loop_
_publ_author_name
'Corfield, Peter W. R.'
_publ_section_title
;
 A cyclooctatrienone complex of diiron hexacarbonyl
;
_journal_coeditor_code           PK2527
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m254
_journal_paper_doi               10.1107/S1600536814012690
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Fe2 (C8 H8 O) (C O)6]'
_chemical_formula_moiety         'C14 H8 Fe2 O7'
_chemical_formula_sum            'C14 H8 Fe2 O7'
_chemical_formula_weight         399.90
_chemical_melting_point          428
_chemical_name_systematic
;
[μ-(2,6,7-η:3,4,5-η)-Cycloocta-2,4,6-trienone]bis(tricarbonyldiiron)(Fe---Fe)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.172(16)
_cell_angle_beta                 83.82(3)
_cell_angle_gamma                74.54(2)
_cell_formula_units_Z            2
_cell_length_a                   7.729(8)
_cell_length_b                   8.258(8)
_cell_length_c                   11.927(11)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    296(3)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      11.04
_cell_volume                     729.4(12)
_computing_cell_refinement       'Corfield (1972)'
_computing_data_collection       'Corfield (1972)'
_computing_data_reduction
;
data reduction followed procedures in Corfield et al. (1973),
with p = 0.06
[data were averaged with a local version of SORTAV (Blessing, 1989),
and a
four-dimensional scaling procedure (XABS2; Parkin et al., 1995)
was applied]
;
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
;
local superposition program (Corfield, 1972)
;
_diffrn_ambient_temperature      296(3)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Picker four-circle'
_diffrn_measurement_method       'θ/2θ scans'
_diffrn_radiation_monochromator  'oriented graphite 200 reflection'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4520
_diffrn_reflns_theta_full        29.92
_diffrn_reflns_theta_max         29.92
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        7.60(10)
_diffrn_standards_interval_count 500
_diffrn_standards_number         18
_exptl_absorpt_coefficient_mu    2.02
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Busing & Levy, 1957)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_meas      1.83
_exptl_crystal_density_method
;
flotation in bromobenzene/bromoform mixture
;
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.487
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0273
_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/[σ²(Fo²)+0.0840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                3687
_reflns_number_total             4227
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2527sup1.cf
_cod_data_source_block           I
_cod_database_code               2239646
_cod_database_fobs_code          2239646
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Fe Fe1 0.23879(3) 0.27972(3) 0.177172(18) 0.03093(8) Uani d . 1 1
Fe Fe2 0.53855(3) 0.14576(3) 0.29382(2) 0.03417(8) Uani d . 1 1
C C11 0.0206(3) 0.3694(2) 0.13055(15) 0.0413(4) Uani d . 1 1
O O11 -0.1162(2) 0.4219(2) 0.09807(15) 0.0624(4) Uani d . 1 1
C C12 0.3569(3) 0.2465(2) 0.03568(15) 0.0432(4) Uani d . 1 1
O O12 0.4271(3) 0.2256(2) -0.05374(13) 0.0677(5) Uani d . 1 1
C C13 0.2055(3) 0.0741(2) 0.18355(15) 0.0394(3) Uani d . 1 1
O O13 0.1684(3) -0.05060(18) 0.18661(14) 0.0580(4) Uani d . 1 1
C C14 0.7292(3) 0.0818(2) 0.37346(17) 0.0450(4) Uani d . 1 1
O O14 0.8500(2) 0.0358(2) 0.42302(17) 0.0682(5) Uani d . 1 1
C C15 0.6776(3) 0.1002(3) 0.16087(18) 0.0483(4) Uani d . 1 1
O O15 0.7697(3) 0.0716(3) 0.07895(15) 0.0752(5) Uani d . 1 1
C C16 0.4823(3) -0.0514(2) 0.31890(17) 0.0442(4) Uani d . 1 1
O O16 0.4551(3) -0.17724(19) 0.33981(16) 0.0674(5) Uani d . 1 1
C C1 0.0240(2) 0.4664(2) 0.35754(15) 0.0414(4) Uani d . 1 1
O O1 -0.13837(19) 0.4908(2) 0.38358(13) 0.0571(4) Uani d . 1 1
C C2 0.1512(2) 0.2959(2) 0.35132(13) 0.0361(3) Uani d . 1 1
H H2 0.0868 0.2108 0.3725 0.043 Uiso calc R 1 1
C C3 0.3129(2) 0.2703(2) 0.41251(14) 0.0372(3) Uani d . 1 1
H H3 0.3051 0.2147 0.4853 0.045 Uiso calc R 1 1
C C4 0.4485(2) 0.3564(2) 0.39688(15) 0.0409(4) Uani d . 1 1
H H4 0.5158 0.3642 0.4608 0.049 Uiso calc R 1 1
C C5 0.5108(3) 0.4085(2) 0.29046(17) 0.0421(4) Uani d . 1 1
H H5 0.6234 0.4426 0.2868 0.051 Uiso calc R 1 1
C C6 0.4023(3) 0.4619(2) 0.19756(16) 0.0404(4) Uani d . 1 1
H H6 0.4715 0.4828 0.1277 0.049 Uiso calc R 1 1
C C7 0.2215(3) 0.5506(2) 0.20695(17) 0.0437(4) Uani d . 1 1
H H7 0.1860 0.6237 0.1432 0.052 Uiso calc R 1 1
C C8 0.1071(3) 0.6065(2) 0.31726(19) 0.0508(5) Uani d . 1 1
H H8A 0.0130 0.7082 0.3068 0.061 Uiso calc R 1 1
H H8B 0.1809 0.6296 0.3726 0.061 Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.3463 0.8444 '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'
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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 1 1
-3 0 2
-1 1 0
4 0 5
-1 0 6
-8 1 0
-6 6 6
2 5 0
1 0 2
-1 -1 -1
3 0 -2
1 -1 0
-4 0 -5
1 0 -6
8 -1 0
6 -6 -6
-2 -5 0
-1 0 -2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C13 Fe1 C11 . 92.47(9) ?
C13 Fe1 C12 . 93.48(9) ?
C11 Fe1 C12 . 94.65(10) ?
C13 Fe1 C2 . 85.60(8) ?
C11 Fe1 C2 . 96.41(9) ?
C12 Fe1 C2 . 168.93(8) ?
C13 Fe1 C7 . 164.71(8) ?
C11 Fe1 C7 . 81.66(8) ?
C12 Fe1 C7 . 101.03(8) ?
C2 Fe1 C7 . 81.08(7) ?
C13 Fe1 C6 . 152.39(8) ?
C11 Fe1 C6 . 115.14(10) ?
C12 Fe1 C6 . 84.91(9) ?
C2 Fe1 C6 . 90.79(7) ?
C7 Fe1 C6 . 36.13(8) ?
C13 Fe1 Fe2 . 85.85(7) ?
C11 Fe1 Fe2 . 168.17(6) ?
C12 Fe1 Fe2 . 97.13(9) ?
C2 Fe1 Fe2 . 71.80(7) ?
C7 Fe1 Fe2 . 97.01(6) ?
C6 Fe1 Fe2 . 67.10(8) ?
C14 Fe2 C15 . 92.80(12) ?
C14 Fe2 C16 . 91.69(9) ?
C15 Fe2 C16 . 100.74(10) ?
C14 Fe2 C4 . 87.79(9) ?
C15 Fe2 C4 . 133.75(9) ?
C16 Fe2 C4 . 125.48(10) ?
C14 Fe2 C5 . 99.31(8) ?
C15 Fe2 C5 . 95.38(9) ?
C16 Fe2 C5 . 160.00(9) ?
C4 Fe2 C5 . 39.37(8) ?
C14 Fe2 C3 . 106.02(11) ?
C15 Fe2 C3 . 158.05(9) ?
C16 Fe2 C3 . 90.10(10) ?
C4 Fe2 C3 . 38.97(7) ?
C5 Fe2 C3 . 70.88(8) ?
C14 Fe2 Fe1 . 174.00(6) ?
C15 Fe2 Fe1 . 89.25(10) ?
C16 Fe2 Fe1 . 93.46(8) ?
C4 Fe2 Fe1 . 86.73(7) ?
C5 Fe2 Fe1 . 74.87(6) ?
C3 Fe2 Fe1 . 70.93(8) ?
O11 C11 Fe1 . 177.54(19) ?
O12 C12 Fe1 . 178.4(2) ?
O13 C13 Fe1 . 173.85(19) ?
O14 C14 Fe2 . 177.66(19) ?
C14 O14 O14 2_756 170.9(2) ?
O15 C15 Fe2 . 177.8(2) ?
O16 C16 Fe2 . 175.41(18) ?
O1 C1 C2 . 122.70(18) y
O1 C1 C8 . 122.10(18) y
C2 C1 C8 . 114.90(17) y
C3 C2 C1 . 117.09(15) y
C3 C2 Fe1 . 107.62(12) ?
C1 C2 Fe1 . 99.86(11) ?
C3 C2 H2 . 110.6 ?
C1 C2 H2 . 110.6 ?
Fe1 C2 H2 . 110.6 ?
C4 C3 C2 . 127.37(16) y
C4 C3 Fe2 . 66.83(11) ?
C2 C3 Fe2 . 105.68(12) ?
C4 C3 H3 . 114.9 ?
C2 C3 H3 . 114.9 ?
Fe2 C3 H3 . 114.9 ?
C5 C4 C3 . 123.23(16) y
C5 C4 Fe2 . 72.62(12) ?
C3 C4 Fe2 . 74.20(11) ?
C5 C4 H4 . 118.0 ?
C3 C4 H4 . 118.0 ?
Fe2 C4 H4 . 118.0 ?
C4 C5 C6 . 125.64(18) y
C4 C5 Fe2 . 68.01(10) ?
C6 C5 Fe2 . 102.46(11) ?
C4 C5 H5 . 115.9 ?
C6 C5 H5 . 115.9 ?
Fe2 C5 H5 . 115.9 ?
C7 C6 C5 . 126.10(18) y
C7 C6 Fe1 . 71.86(12) ?
C5 C6 Fe1 . 108.79(12) ?
C7 C6 H6 . 113.9 ?
C5 C6 H6 . 113.9 ?
Fe1 C6 H6 . 113.9 ?
C6 C7 C8 . 124.40(19) y
C6 C7 Fe1 . 72.01(10) ?
C8 C7 Fe1 . 108.43(12) ?
C6 C7 H7 . 114.6 ?
C8 C7 H7 . 114.6 ?
Fe1 C7 H7 . 114.6 ?
C7 C8 C1 . 107.95(15) y
C7 C8 H8A . 110.1 ?
C1 C8 H8A . 110.1 ?
C7 C8 H8B . 110.1 ?
C1 C8 H8B . 110.1 ?
H8A C8 H8B . 108.4 ?
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
Fe1 C13 . 1.783(2) ?
Fe1 C11 . 1.796(2) ?
Fe1 C12 . 1.818(2) ?
Fe1 C2 . 2.109(2) ?
Fe1 C7 . 2.236(3) ?
Fe1 C6 . 2.238(2) ?
Fe1 Fe2 . 2.795(2) ?
Fe2 C14 . 1.795(2) ?
Fe2 C15 . 1.802(3) ?
Fe2 C16 . 1.807(2) ?
Fe2 C4 . 2.062(2) ?
Fe2 C5 . 2.123(3) ?
Fe2 C3 . 2.158(2) ?
C11 O11 . 1.138(3) ?
C12 O12 . 1.137(3) ?
C13 O13 . 1.140(2) ?
C14 O14 . 1.135(3) ?
O14 O14 2_756 3.042(4) ?
C15 O15 . 1.133(3) ?
C16 O16 . 1.133(3) ?
C1 O1 . 1.223(3) y
C1 C2 . 1.484(3) y
C2 C3 . 1.480(3) y
C2 H2 . 0.9800 ?
C3 C4 . 1.411(3) y
C3 H3 . 0.9800 ?
C4 C5 . 1.411(3) y
C4 H4 . 0.9800 ?
C5 C6 . 1.454(3) y
C5 H5 . 0.9800 ?
C6 C7 . 1.387(3) y
C6 H6 . 0.9800 ?
C7 C8 . 1.508(3) y
C7 H7 . 0.9800 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C8 C1 . 1.515(3) y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C1 C2 C3 C4 -58.8(2)
C2 C3 C4 C5 -36.3(3)
C3 C4 C5 C6 32.9(3)
C4 C5 C6 C7 34.9(3)
C5 C6 C7 C8 0.0(3)
C6 C7 C8 C1 -88.8(2)
C7 C8 C1 C2 46.3(2)
C8 C1 C2 C3 57.0(2)
O1 C1 C2 C3 -129.21(19)
O1 C1 C8 C7 -127.55(19)
