Redox-Responsive Recombination of Carbon-Carbon Bonds on Flexible Tetrairon Cores
Masaaki Okazaki; Masato Takano; Fumiyuki Ozawa; Journal of the American Chemical Society 131 (2009) 1684–1685; doi:10.1021/ja809540w

data_4103891
_publ_contact_author_address
'Institute for Chemical Research, Kyoto University'
_publ_contact_author_email       mokazaki@scl.kyoto-u.ac.jp
_publ_contact_author_fax         81-774-38-3039
_publ_contact_author_name        'Masaaki Okazaki'
_publ_contact_author_phone       81-774-38-3029
_publ_section_title
;
 Redox-Responsive Recombination of Carbon-Carbon Bonds on Flexible
 Tetrairon Cores
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1684
_journal_page_last               1685
_journal_paper_doi               10.1021/ja809540w
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration unk
_chemical_formula_sum            'C38 H48 F12 Fe4 P2 Si2'
_chemical_formula_weight         1074.28
_chemical_properties_physical    air-sensitive
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.366(10)
_cell_length_b                   11.366(10)
_cell_length_c                   29.309(27)
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.4647
_cell_volume                     3279(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26788
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.508
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.8166
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Higashi
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1638
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.148
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.26(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         5006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0955P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                4443
_reflns_number_total             5006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809540w_si_002.cif
_cod_data_source_block           okazaki
_cod_database_code               4103891