Synthesis and Structure of Cubane-Type Tetrairon Clusters Possessing μ3-Isonitrile Ligands. Reductive Coupling of Two Isonitriles on Redox-Responsive Tetrairon Reaction Sites
Okazaki, Masaaki; Suto, Kosei; Kudo, Naotsugu; Takano, Masato; Ozawa, Fumiyuki; Organometallics 31 (2012) 4110–; doi:10.1021/om3002944

data_4078524
_publ_section_title
;
 Synthesis and Structure of Cubane-Type Tetrairon Clusters Possessing
 \m3-Isonitrile Ligands. Reductive Coupling of Two Isonitriles on
 Redox-Responsive Tetrairon Reaction Sites
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4110
_journal_paper_doi               10.1021/om3002944
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_sum            'C40 H40 Fe4 N2'
_chemical_formula_weight         772.14
_chemical_properties_physical    air-sensitive
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.6939(5)
_cell_length_b                   20.5307(9)
_cell_length_c                   26.4471(11)
_cell_measurement_reflns_used    40346
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.77
_cell_measurement_theta_min      6.09
_cell_volume                     6349.5(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXISIP'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            55083
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.8386
_exptl_absorpt_correction_T_min  0.5289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         7193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0293P)^2^+2.4781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                6208
_reflns_number_total             7193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3002944_si_002.cif
_cod_data_source_block           ydkr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4078524