A Tertiary Carbon‒Iron Bond as an FeICl Synthon and the Reductive Alkylation of Diphosphine-Supported Iron(II) Chloride Complexes to Low-Valent Iron
Tondreau, Aaron M.; Scott, Brian L.; Boncella, James M.; Organometallics 35 (2016) 1643–; doi:10.1021/acs.organomet.6b00108

data_4088456
_publ_section_title
;
 A Tertiary Carbon--Iron Bond as an FeICl Synthon and the Reductive
 Alkylation of Diphosphine-Supported Iron(II) Chloride Complexes to
 Low-Valent Iron
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1643
_journal_paper_doi               10.1021/acs.organomet.6b00108
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C26 H31 Cl Fe N2 Si'
_chemical_formula_weight         490.94
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           Monoclinic'
_symmetry_space_group_name_H-M   'C 1 c 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                 117.3952(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7047(13)
_cell_length_b                   9.9238(8)
_cell_length_c                   17.9359(14)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.47
_cell_volume                     2639.9(4)
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 2013)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Bruker Triumph curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23499
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/3 - Bruker AXS area detector scaling and absorption correction '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         8016
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                7403
_reflns_number_total             8016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00108_si_002.cif
_cod_data_source_block           py2feclcphtms
_cod_depositor_comments
;

2020-10-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         245.47
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      Cc
_cod_original_formula_sum        'C13 H15.5 Cl0.5 Fe0.5 N1 Si0.5'
_cod_database_code               4088456