Silylation of Iron-Bound Carbon Monoxide Affords a Terminal Fe Carbyne
Yunho Lee; Jonas C. Peters; Journal of the American Chemical Society 133 (2011) 4438–4446; doi:10.1021/ja109678y

data_4105822
_publ_section_title
;
 Silylation of Iron-Bound Carbon Monoxide Affords a Terminal Fe Carbyne
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4438
_journal_page_last               4446
_journal_paper_doi               10.1021/ja109678y
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C68 H65 B Cl F24 Fe P3 Si'
_chemical_formula_weight         1561.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.2470(10)
_cell_angle_beta                 100.4700(10)
_cell_angle_gamma                100.0890(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7131(2)
_cell_length_b                   16.3092(3)
_cell_length_c                   19.1176(4)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_volume                     3633.37(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70589
_diffrn_reflns_theta_full        68.96
_diffrn_reflns_theta_max         68.96
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    3.688
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.951
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         12892
_refine_ls_number_restraints     992
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.181
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+5.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                12690
_reflns_number_total             12892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109678y_si_002_5.cif
_cod_data_source_block           d8_08062_0m-yunho
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_original_cell_volume        3633.36(12)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4105822