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_7160919
_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         'C26 H29 I N2 Ru'
_chemical_formula_sum            'C26 H29 I N2 Ru'
_chemical_formula_weight         597.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-11
_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                 104.0150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2763(4)
_cell_length_b                   11.1841(4)
_cell_length_c                   17.7735(6)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.89
_cell_measurement_theta_min      3.97
_cell_volume                     2367.65(14)
_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 0.999
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17284
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.955
_diffrn_reflns_theta_min         3.967
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.695
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.2930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1250 before and 0.0740 after correction. The Ratio of minimum to maximum transmission is 0.3888. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+4.0428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4355
_reflns_number_total             4643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01811k2.cif
_cod_data_source_block           11_CCDC1
_cod_database_code               7160919
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.277
_shelx_estimated_absorpt_t_min   0.217
_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.a Ternary CH refined with riding coordinates:
 C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C22(H22), C19(H19), C20(H20), C16(H16), C14(H14), C15(H15), C6(H6),
 C9(H9), C7(H7), C8(H8), C23(H23)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              42863
_shelx_hkl_checksum              61628
_olex2_submission_special_instructions 'No special instructions were received'