Carbene rearrangements in three-coordinate N-heterocyclic carbene complexes of cobalt(II) bis(trimethylsilyl)amide.
Day, Benjamin M.; Pal, Kuntal; Pugh, Thomas; Tuck, Jessica; Layfield, Richard A.; Inorganic chemistry 53 (2014) 10578–10584; doi:10.1021/ic501677k

data_4350701
_publ_section_title
;
 Carbene rearrangements in three-coordinate N-heterocyclic carbene
 complexes of cobalt(II) bis(trimethylsilyl)amide.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10578
_journal_page_last               10584
_journal_paper_doi               10.1021/ic501677k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C23 H56 Co N4 Si4'
_chemical_formula_sum            'C23 H56 Co N4 Si4'
_chemical_formula_weight         560.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-22
_audit_creation_method
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Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.650(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3805(4)
_cell_length_b                   12.0557(4)
_cell_length_c                   12.0236(4)
_cell_measurement_reflns_used    3785
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      26.9750
_cell_measurement_theta_min      3.7770
_cell_volume                     1638.54(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0182658000
_diffrn_orient_matrix_UB_12      -0.0181293000
_diffrn_orient_matrix_UB_13      -0.0514385000
_diffrn_orient_matrix_UB_21      0.0086830000
_diffrn_orient_matrix_UB_22      -0.0543217000
_diffrn_orient_matrix_UB_23      0.0220522000
_diffrn_orient_matrix_UB_31      -0.0593949000
_diffrn_orient_matrix_UB_32      -0.0135585000
_diffrn_orient_matrix_UB_33      -0.0198376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.1040
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12362
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.118
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 2234 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6684
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5814
_reflns_number_total             6684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501677k_si_002.cif
_cod_data_source_block           8
_cod_database_code               4350701
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C20H20N4Si4Co1
_reflns_odcompleteness_completeness 99.77
_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:
 C2(H2), C3(H3)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C12(H12A,
 H12B,H12C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C20(H20A,H20B,H20C),
 C18(H18A,H18B,H18C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C6(H6A,
 H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              62367
_shelx_hkl_checksum              29318
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'