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_4127036
_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            'C29 H33 N3 O Ru'
_chemical_formula_weight         540.65
_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-2014/7
_cell_angle_alpha                62.554(4)
_cell_angle_beta                 78.316(4)
_cell_angle_gamma                89.506(4)
_cell_formula_units_Z            2
_cell_length_a                   7.3957(7)
_cell_length_b                   13.6493(13)
_cell_length_c                   14.1277(12)
_cell_measurement_reflns_used    19586
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.635
_cell_measurement_theta_min      2.826
_cell_volume                     1233.5(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.962
_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  0.0982
_diffrn_reflns_av_unetI/netI     0.1233
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19586
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.635
_diffrn_reflns_theta_min         2.826
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       rod
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7224
_exptl_transmission_factor_min   0.6283
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0246P)^2^+0.8961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3892
_reflns_number_total             5524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13097_si_002.cif
_cod_data_source_block           2[Ru]
_cod_database_code               4127036
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              84138
_shelx_hkl_checksum              74868