Lewis Acid Chemistry of a Cationic [CCH] Subunit in a Bisdisphenoidal Eight-Atom Tetrairon‒Tetracarbon Cluster
Okazaki, Masaaki; Taniwaki, Wataru; Miyagi, Kazuki; Takano, Masato; Kaneko, Satoshi; Ozawa, Fumiyuki; Organometallics 32 (2013) 1951–; doi:10.1021/om400035q

data_4080498
_publ_section_title
;
 Lewis Acid Chemistry of a Cationic [CCH] Subunit in a Bisdisphenoidal
 Eight-Atom Tetrairon--Tetracarbon Cluster
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1951
_journal_paper_doi               10.1021/om400035q
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_sum            'C34 H38 F12 Fe4 N3 P2'
_chemical_formula_weight         1002.01
_chemical_properties_physical    'air-sensitive, paramagnetic'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 111.275(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3972(6)
_cell_length_b                   16.1594(7)
_cell_length_c                   11.5132(8)
_cell_measurement_reflns_used    14488
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.15
_cell_volume                     1802.5(2)
_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      93(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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14511
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed Xray tube'
_exptl_absorpt_coefficient_mu    1.761
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.467
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         6455
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0307P)^2^+1.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                6145
_reflns_number_total             6455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400035q_si_002.cif
_cod_data_source_block           6
_cod_original_cell_volume        1802.53(18)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4080498