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_4127037
_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            'C33 H42 N4 Ru'
_chemical_formula_weight         595.77
_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                75.816(3)
_cell_angle_beta                 73.171(4)
_cell_angle_gamma                89.508(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2644(8)
_cell_length_b                   11.3701(7)
_cell_length_c                   14.0186(10)
_cell_measurement_reflns_used    25624
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.583
_cell_measurement_theta_min      1.852
_cell_volume                     1514.83(19)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1609
_diffrn_reflns_av_unetI/netI     0.2602
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25624
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         1.852
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.7411
_exptl_absorpt_correction_T_min  0.6460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.207
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.0076(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1912
_refine_ls_R_factor_gt           0.0793
_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^)+(0.0825P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.2174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2967
_reflns_number_total             6913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13097_si_002.cif
_cod_data_source_block           3[Ru]
_cod_database_code               4127037
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              30550
_shelx_hkl_checksum              13841