N-Heterocyclic Carbene Ruthenium Complexes Synthesized by Hydrogen-Bonding-Assisted Strategy for Dehydrogenative Rearrangement of Esters
Gong, Zhi-Yuan; Tao, Sheng; Li, Xiao-Bin; Wang, Tao; Chen, Fei; Du, Zhi-Hong; Bo, Chun-Bo; Li, Min; Liu, Ning; Organic & Biomolecular Chemistry  (2025) –; doi:10.1039/D5OB01811K

data_7160920
_publ_section_title
;
 N-Heterocyclic Carbene Ruthenium Complexes Synthesized by
 Hydrogen-Bonding-Assisted Strategy for Dehydrogenative Rearrangement of
 Esters
;
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D5OB01811K
_journal_year                    2025
_chemical_formula_moiety         'C17 H18 I2 N2 Ru, C H2 Cl2'
_chemical_formula_sum            'C18 H20 Cl2 I2 N2 Ru'
_chemical_formula_weight         690.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-03 deposited with the CCDC.	2025-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                74.7750(10)
_cell_angle_beta                 71.8530(10)
_cell_angle_gamma                83.6420(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3565(2)
_cell_length_b                   11.5771(3)
_cell_length_c                   11.7765(3)
_cell_measurement_reflns_used    8955
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.27
_cell_measurement_theta_min      3.96
_cell_volume                     1044.12(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11482
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.260
_diffrn_reflns_theta_min         3.959
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.674
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1205 before and 0.0670 after correction. The Ratio of minimum to maximum transmission is 0.4037. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_description       needle
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.992
_refine_diff_density_min         -1.897
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4024
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0802P)^2^+2.6453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3810
_reflns_number_total             4024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01811k2.cif
_cod_data_source_block           11_CCDC2
_cod_database_code               7160920
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.128
_shelx_estimated_absorpt_t_min   0.070
_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
 C17-C12
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C18(H18A,H18B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              20858
_shelx_hkl_checksum              50485
_olex2_submission_special_instructions 'No special instructions were received'