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_4350702
_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         'C39 H72 Co N4 Si4'
_chemical_formula_sum            'C39 H72 Co N4 Si4'
_chemical_formula_weight         768.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.835(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9510(7)
_cell_length_b                   16.794(2)
_cell_length_c                   23.1128(12)
_cell_measurement_reflns_used    5104
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      28.5380
_cell_measurement_theta_min      3.5020
_cell_volume                     4622.3(7)
_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
;
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)
;
_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      150.01(11)
_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      0.0171242000
_diffrn_orient_matrix_UB_12      -0.0363192000
_diffrn_orient_matrix_UB_13      -0.0121524000
_diffrn_orient_matrix_UB_21      -0.0561026000
_diffrn_orient_matrix_UB_22      -0.0141965000
_diffrn_orient_matrix_UB_23      -0.0013782000
_diffrn_orient_matrix_UB_31      -0.0099556000
_diffrn_orient_matrix_UB_32      0.0163520000
_diffrn_orient_matrix_UB_33      -0.0282571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18514
_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         25.350
_diffrn_reflns_theta_min         3.056
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37782
_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    1.104
_exptl_crystal_description       plate
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         8455
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0445P)^2^+2.8682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5861
_reflns_number_total             8455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501677k_si_002.cif
_cod_data_source_block           9
_cod_original_cell_volume        4622.5(7)
_cod_database_code               4350702
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C39 H72 N4 Co1 Si4'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C23 \\sim C22-C23A \\sim C22-C24 \\sim C22-C24A
 with sigma of 0.02
 C13-C14 \\sim C13-C14A \\sim C13-C15 \\sim C13-C15A
 with sigma of 0.02
3. Rigid bond restraints
 C24, C24A, C23, C23A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C14A, C15A, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C24 \\sim C24A \\sim C23 \\sim C23A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C14 \\sim C14A \\sim C15A \\sim C15: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.08
Uanis(C24) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C23A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H22A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23A)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(1)
 Sof(H13A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(H13)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C25(H25), C13(H13), C13(H13A), C10(H10), C22(H22), C22(H22A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C20(H20), C1(H1), C8(H8), C7(H7), C6(H6), C18(H18), C19(H19)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C35(H35A,H35B,
 H35C), C31(H31A,H31B,H31C), C36(H36A,H36B,H36C), C26(H26A,H26B,H26C), C11(H11A,
 H11B,H11C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C23(H23A,H23B,H23C),
 C15(H15A,H15B,H15C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C34(H34A,H34B,
 H34C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C14(H14A,H14B,H14C), C12(H12A,
 H12B,H12C), C39(H39A,H39B,H39C), C24A(H24D,H24E,H24F), C23A(H23D,H23E,H23F),
 C15A(H15D,H15E,H15F), C14A(H14D,H14E,H14F)
;
_shelx_res_checksum              75887
_shelx_hkl_checksum              14827
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'