Normal-to-Abnormal Rearrangement and NHC Activation in Three-Coordinate Iron(II) Carbene Complexes
Benjamin M. Day; Thomas Pugh; Daniël Hendriks; Célia Fonseca Guerra; David J. Evans; F. Matthias Bickelhaupt; Richard A. Layfield; Journal of the American Chemical Society 135 (2013) 13338–13341; doi:10.1021/ja408589p

data_4120786
_publ_section_title
;
 Normal-to-Abnormal Rearrangement and NHC Activation in Three-Coordinate
 Iron(II) Carbene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13338
_journal_page_last               13341
_journal_paper_doi               10.1021/ja408589p
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C26 H60 Fe N6 Si4'
_chemical_formula_sum            'C26 H60 Fe N6 Si4'
_chemical_formula_weight         625.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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     iterative
_audit_creation_date             2013-04-05
_audit_creation_method
;
  Olex2 1.2
  (compiled Mar 21 2013 11:16:32, GUI svn.r4446)
;
_cell_angle_alpha                90
_cell_angle_beta                 126.451(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.705(2)
_cell_length_b                   9.3643(6)
_cell_length_c                   18.1068(15)
_cell_measurement_reflns_used    3384
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.0730
_cell_measurement_theta_min      3.5900
_cell_volume                     3642.2(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8542
_diffrn_measurement_details
;
  1 omega   49.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9454  178.0000 -180.0000 51

  2 omega  -77.00  -41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798 -178.0000  -90.0000 36

  3 omega  -86.00  -51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -57.0000 -150.0000 35

  4 omega  -90.00  -56.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798 -178.0000   60.0000 34

  5 omega  -90.00   11.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -37.0000 -120.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0124035000
_diffrn_orient_matrix_UB_12      -0.0461868000
_diffrn_orient_matrix_UB_13      -0.0228243000
_diffrn_orient_matrix_UB_21      -0.0189152000
_diffrn_orient_matrix_UB_22      0.0423133000
_diffrn_orient_matrix_UB_23      -0.0238306000
_diffrn_orient_matrix_UB_31      0.0322540000
_diffrn_orient_matrix_UB_32      0.0425911000
_diffrn_orient_matrix_UB_33      -0.0010370000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7787
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.582
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Pale brown'
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.064
_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     177
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+4.5822P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3078
_reflns_number_total             3735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja408589p_si_002_3.cif
_cod_data_source_block           platon
_cod_database_code               4120786
_chemical_oxdiff_formula         C17H38N4Si4Fe1
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              86493
_shelxl_version_number           2013-2