Structure and bonding in three-coordinate N-heterocyclic carbene adducts of iron(II) bis(trimethylsilyl)amide
Richard A. Layfield; Joseph J. W. McDouall; Manfred Scheer; Christoph Schwarzmaier; Floriana Tuna; Chem.Commun. 47 (2011) 10623–10625; doi:10.1039/c1cc14576b

data_7106894
_publ_section_title
;
 Structure and bonding in three-coordinate N-heterocyclic carbene adducts
 of iron(II) bis(trimethylsilyl)amide
;
_journal_name_full               Chem.Commun.
_journal_page_first              10623
_journal_page_last               10625
_journal_paper_doi               10.1039/c1cc14576b
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C39 H72 Fe N4 Si4'
_chemical_formula_sum            'C39 H72 Fe N4 Si4'
_chemical_formula_weight         765.22
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                76.430(6)
_cell_angle_beta                 80.054(5)
_cell_angle_gamma                66.930(7)
_cell_formula_units_Z            2
_cell_length_a                   10.8510(8)
_cell_length_b                   11.3172(8)
_cell_length_c                   22.8051(13)
_cell_measurement_reflns_used    9350
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      63.5944
_cell_measurement_theta_min      4.0028
_cell_volume                     2494.4(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
(compiled Sep 13 2010,14:28:38)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
(compiled Sep 13 2010,14:28:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
(compiled Sep 13 2010,14:28:38)
;
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15902
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        63.72
_diffrn_reflns_theta_max         63.72
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    3.538
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
(compiled Sep 13 2010,14:28:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.019
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.2862
_exptl_crystal_size_mid          0.1423
_exptl_crystal_size_min          0.0853
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.6646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                7236
_reflns_number_total             7794
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c1cc14576b.txt
_cod_data_source_block           1
_cod_database_code               7106894