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_7106895
_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         'C33 H60 Fe N4 Si4'
_chemical_formula_structural     'C33 H60 Fe N4 Si4'
_chemical_formula_sum            'C33 H60 Fe N4 Si4'
_chemical_formula_weight         681.06
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Nov 12 10:27:12 2010'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 99.705(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6461(3)
_cell_length_b                   14.2890(3)
_cell_length_c                   16.7741(3)
_cell_measurement_reflns_used    5173
_cell_measurement_temperature    123
_cell_measurement_theta_max      70.4559
_cell_measurement_theta_min      4.0986
_cell_volume                     3932.72(13)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.971
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7577
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         70.66
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    4.432
_exptl_absorpt_correction_T_max  0.438
_exptl_absorpt_correction_T_min  0.281
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
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    1.150
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.4431
_exptl_crystal_size_mid          0.3543
_exptl_crystal_size_min          0.2560
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.1949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                3554
_reflns_number_total             3675
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc14576b.txt
_cod_data_source_block           ralr20
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7106895