Reactions of Bromoacetylene with Primary Amine on a Butterfly-Type Tetrairon Core to Give Isonitrile and Methyne through Oxidation and Deprotonation
Okazaki, Masaaki; Tsuchimoto, Takahiro; Nakazawa, Yuki; Takano, Masato; Ozawa, Fumiyuki; Organometallics 30 (2011) 3487–; doi:10.1021/om200493b

data_4065003
_publ_section_title
;
 Reactions of Bromoacetylene with Primary Amine on a Butterfly-Type
 Tetrairon Core to Give Isonitrile and Methyne through Oxidation and
 Deprotonation
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3487
_journal_paper_doi               10.1021/om200493b
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_sum            'C32 H40 F6 Fe4 N P'
_chemical_formula_weight         807.02
_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                   9.2394(18)
_cell_length_b                   18.231(3)
_cell_length_c                   18.435(4)
_cell_measurement_reflns_used    10881
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4851
_cell_measurement_theta_min      3.1216
_cell_volume                     3105.3(10)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25430
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_T_max  0.8600
_exptl_absorpt_correction_T_min  0.4432
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Coorporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.367
_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   0.012(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                6531
_reflns_number_total             7091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200493b_si_002.cif
_cod_data_source_block           ydkr
_cod_database_code               4065003