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_4078523
_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 F12 Fe4 N2 P2'
_chemical_formula_weight         1062.08
_chemical_properties_physical    air-sensitive
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   11.6407(2)
_cell_length_b                   14.0195(3)
_cell_length_c                   24.0667(4)
_cell_measurement_reflns_used    37817
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.95
_cell_measurement_theta_min      6.05
_cell_volume                     3927.61(13)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39328
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  0.8812
_exptl_absorpt_correction_T_min  0.7374
_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    1.796
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         8968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.147
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+1.4752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                8500
_reflns_number_total             8968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3002944_si_002.cif
_cod_data_source_block           cluster_2
_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               4078523