Unusual Rearrangement of an N-Donor-Functionalized N-Heterocyclic Carbene Ligand on Group 8 Metals.
Liang, Qiuming; Salmon, Andrew; Kim, Patrick Jinhyung; Yan, Linfan; Song, Datong; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b13097

data_4127038
_publ_section_title
;
 Unusual Rearrangement of an N-Donor-Functionalized N-Heterocyclic Carbene
 Ligand on Group 8 Metals.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b13097
_journal_year                    2018
_chemical_formula_sum            'C65 H79 B Fe N4 O2'
_chemical_formula_weight         1014.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                76.008(3)
_cell_angle_beta                 77.143(3)
_cell_angle_gamma                86.820(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1306(7)
_cell_length_b                   14.1720(10)
_cell_length_c                   18.7468(13)
_cell_measurement_reflns_used    36450
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.757
_cell_measurement_theta_min      1.481
_cell_volume                     2797.5(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36450
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.757
_diffrn_reflns_theta_min         1.481
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'orange brown'
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         12462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0898
_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^)+(0.0894P)^2^+9.8894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2086
_refine_ls_wR_factor_ref         0.2648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8547
_reflns_number_total             12462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13097_si_002.cif
_cod_data_source_block           '[FeCP*(CNtBu)(HL)]BPh4'
_cod_database_code               4127038
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              90421
_shelx_hkl_checksum              82078