Electron-Rich N-Heterocyclic Silylene (NHSi)-Iron Complexes: Synthesis, Structures, and Catalytic Ability of an Isolable Hydridosilylene-Iron Complex
Burgert Blom; Stephan Enthaler; Shigeyoshi Inoue; Elisabeth Irran; Matthias Driess; Journal of the American Chemical Society 135 (2013) 6703–6713; doi:10.1021/ja402480v

data_4119702
_publ_contact_author_address
;
Institute of Chemistry: Metalorganics and Inorganic Materials, 
Technische Universit\"at Berlin, Strasse des 17. Juni 135, Sekr. C2, 
D-10623 Berlin
;
_publ_contact_author_email       matthias.driess@tu-berlin.de
_publ_contact_author_fax         49-30-314-29732
_publ_contact_author_name        'Matthias Driess'
_publ_contact_author_phone       49-30-314-22265
_publ_section_title
;
 Electron-Rich N-Heterocyclic Silylene (NHSi)-Iron Complexes: Synthesis,
 Structures, and Catalytic Ability of an Isolable Hydridosilylene-Iron
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6703
_journal_page_last               6713
_journal_paper_doi               10.1021/ja402480v
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C27 H56 Fe N2 P4 Si'
_chemical_formula_weight         616.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
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_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
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CrysAlisPro, Oxford Diffraction Ltd.,
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
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_cell_formula_units_Z            4
_cell_length_a                   24.0190(12)
_cell_length_b                   15.0889(8)
_cell_length_c                   9.4039(5)
_cell_measurement_reflns_used    3684
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4771
_cell_measurement_theta_min      3.3351
_cell_volume                     3408.2(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0684
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_diffrn_reflns_limit_k_max       17
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.916
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         5185
_refine_ls_number_restraints     484
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+4.7202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                4792
_reflns_number_total             5185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402480v_si_001_3.cif
_cod_data_source_block           c:\compound5
_cod_database_code               4119702