Uncommon carbene-to-azole ligand rearrangement of N-heterocyclic carbenes in a ruthenium system.
Zhang, Bo; Duan, Yu'ai; Zhang, Xin; Guo, Shuai; Chemical communications (Cambridge, England) 57 (2021) 6879–6882; doi:10.1039/d1cc01871j

data_7128489
_publ_section_title
;
 Uncommon carbene-to-azole ligand rearrangement of N-heterocyclic carbenes
 in a ruthenium system.
;
_journal_issue                   56
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6879
_journal_page_last               6882
_journal_paper_doi               10.1039/d1cc01871j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C25 H32 Cl N3 O Ru'
_chemical_formula_sum            'C25 H32 Cl N3 O Ru'
_chemical_formula_weight         527.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-04-26
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2021-04-02 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.9650(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.68636(12)
_cell_length_b                   17.1382(3)
_cell_length_c                   18.5598(3)
_cell_measurement_reflns_used    6710
_cell_measurement_temperature    108.85(10)
_cell_measurement_theta_max      29.5820
_cell_measurement_theta_min      3.5890
_cell_volume                     2400.25(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      108.85(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0971
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.8441
_diffrn_measurement_details
;
  1 omega  -46.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -57.0000   60.0000 34

  2 omega  -44.00  -18.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -57.0000   30.0000 26

  3 omega   -2.00   24.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  -99.0000   60.0000 26

  4 omega   16.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335   37.0000  -90.0000 44

  5 omega    3.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335   37.0000  -30.0000 82

  6 omega    4.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7335   57.0000   60.0000 60

  7 omega  -60.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4210  117.0000   -2.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0239224000
_diffrn_orient_matrix_UB_12      0.0283635000
_diffrn_orient_matrix_UB_13      -0.0279599000
_diffrn_orient_matrix_UB_21      -0.0048043000
_diffrn_orient_matrix_UB_22      -0.0295512000
_diffrn_orient_matrix_UB_23      -0.0270745000
_diffrn_orient_matrix_UB_31      -0.0907531000
_diffrn_orient_matrix_UB_32      -0.0059135000
_diffrn_orient_matrix_UB_33      0.0011305000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13603
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+1.1275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                4270
_reflns_number_total             4711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1cc01871j2.cif
_cod_data_source_block           exp_5438
_cod_depositor_comments
'Adding full bibliography for 7128489--7128493.cif.'
_cod_database_code               7128489
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32