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_4105820
_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            'C40 H63 Fe O P3 Si2'
_chemical_formula_weight         764.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.549(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0922(4)
_cell_length_b                   17.9941(10)
_cell_length_c                   20.9965(9)
_cell_measurement_temperature    100(2)
_cell_volume                     4177.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            76145
_diffrn_reflns_theta_full        65.18
_diffrn_reflns_theta_max         65.18
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    4.742
_exptl_absorpt_correction_T_max  0.5365
_exptl_absorpt_correction_T_min  0.4506
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0455P)^2^+2.1428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                6154
_reflns_number_total             7129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109678y_si_002_3.cif
_cod_data_source_block           d8_09038
_cod_database_code               4105820