Studies of iron-mediated Pauson‒Khand reactions of 1,1-disubstituted-allenylsilanes: mechanistic implications for a reactive three-membered iron metallacycle
Williams, David R.; Shah, Akshay A.; Mazumder, Shivnath; Baik, Mu-Hyun; Chemical Science 4 (2013) 238–; doi:10.1039/c2sc21404k

data_1514830
_publ_section_title
;
 Studies of iron-mediated Pauson--Khand reactions of
 1,1-disubstituted-allenylsilanes: mechanistic implications for a reactive
 three-membered iron metallacycle
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              238
_journal_paper_doi               10.1039/c2sc21404k
_journal_volume                  4
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H18 Fe1 O4 Si1'
_chemical_formula_sum            'C20 H18 Fe O4 Si'
_chemical_formula_weight         406.29
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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
_audit_creation_date             10-12-15
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 100.773(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1510(8)
_cell_length_b                   29.386(3)
_cell_length_c                   9.6851(10)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1999.4(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21632
_diffrn_reflns_theta_full        29.135
_diffrn_reflns_theta_max         30.036
_diffrn_reflns_theta_min         2.141
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.491
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9951
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         11113
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0025925
_refine_ls_shift/su_mean         0.0004175
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.66P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0910
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0910
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              41
_reflns_limit_k_min              -41
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                9275
_reflns_number_total             11113
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      27.26
_oxford_refine_ls_r_factor_ref   0.0443
_oxford_refine_ls_scale          0.18657(6)
_oxford_reflns_number_all        11113
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_10118_0m in P2(1)'
_cod_data_source_file            c2sc21404k.txt
_cod_data_source_block           10118
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C20 H18 Fe1 O4 Si1'
_cod_database_code               1514830