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_7160918
_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         'C25 H29 I N3 Ru, I, C H4 O'
_chemical_formula_sum            'C26 H33 I2 N3 O Ru'
_chemical_formula_weight         758.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-27 deposited with the CCDC.	2025-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.551(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.7159(9)
_cell_length_b                   9.3500(3)
_cell_length_c                   21.0421(6)
_cell_measurement_reflns_used    9790
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.17
_cell_measurement_theta_min      3.22
_cell_volume                     5392.3(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0833
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31003
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.276
_diffrn_reflns_theta_min         3.225
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.860
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1473 before and 0.0851 after correction. The Ratio of minimum to maximum transmission is 0.4575. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.922
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0604P)^2^+30.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4665
_reflns_number_total             5318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01811k2.cif
_cod_data_source_block           11
_cod_database_code               7160918
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.121
_shelx_estimated_absorpt_t_min   0.098
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C9(H9), C15(H15), C14(H14), C6(H6), C12(H12), C8(H8),
 C7(H7), C18(H18), C13(H13), C21(H21)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              4431
_shelx_hkl_checksum              19405
_olex2_submission_special_instructions 'No special instructions were received'