A cyclooctatrienone complex of diiron hexacarbonyl
Corfield, Peter W. R.; Acta Crystallographica Section E 70 (2014) m254–; doi:10.1107/S1600536814012690

data_2239646
_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
;
[\m-(2,6,7-\h:3,4,5-\h)-Cycloocta-2,4,6-trienone]bis(tricarbonyldiiron)(<i>Fe</i>---<i>Fe</i>)
;
_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 <i>et al.</i> (1973),
with p = 0.06
[data were averaged with a local version of SORTAV (Blessing, 1989),
and a
four-dimensional scaling procedure (XABS2; Parkin <i>et al.</i>, 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       '\q/2\q 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/[\s^2^(Fo^2^)+0.0840P] where P=(Fo^2^+2Fc^2^)/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>2\s(I)
_cod_data_source_file            pk2527sup1.cf
_cod_data_source_block           I
_cod_database_code               2239646
_cod_database_fobs_code          2239646