Half-sandwich ruthenium complexes with acylhydrazone ligands: synthesis and catalytic activity in the <i>N</i>-alkylation of hydrazides.
Li, Heng; Wang, Ke; Yang, Lin; Luo, Yu-Zhou; Yao, Zi-Jian; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2797–2806; doi:10.1039/d3dt04078j

data_7714854
_publ_section_title
;
 Half-sandwich ruthenium complexes with acylhydrazone ligands: synthesis
 and catalytic activity in the <i>N</i>-alkylation of hydrazides.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2797
_journal_page_last               2806
_journal_paper_doi               10.1039/d3dt04078j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C29 H29 Cl N2 O2 Ru'
_chemical_formula_sum            'C29 H29 Cl N2 O2 Ru'
_chemical_formula_weight         574.06
_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
_audit_creation_date             2023-07-30
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) 
;
_audit_update_record
;
2023-12-06 deposited with the CCDC.	2023-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.153(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.2188(18)
_cell_length_b                   12.3812(8)
_cell_length_c                   16.2184(11)
_cell_measurement_reflns_used    9299
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      72.23
_cell_measurement_theta_min      3.41
_cell_volume                     5197.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      203.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37396
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.218
_diffrn_reflns_theta_min         3.415
_exptl_absorpt_coefficient_mu    6.052
_exptl_absorpt_correction_T_max  0.6225
_exptl_absorpt_correction_T_min  0.3697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1496 before and 0.0758 after correction. 
The Ratio of minimum to maximum transmission is 0.5939. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.249
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+7.5580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4896
_reflns_number_total             5095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04078j2.cif
_cod_data_source_block           cu_230727c_a
_cod_depositor_comments          'Adding full bibliography for 7714854.cif.'
_cod_database_code               7714854
_shelx_estimated_absorpt_t_max   0.643
_shelx_estimated_absorpt_t_min   0.264
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Ternary CH refined with riding coordinates: 
 C21(H21), C22(H22), C24(H24), C25(H25), C26(H26) 
2.b Aromatic/amide H refined with riding coordinates: 
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C11(H11), C12(H12), C13(H13), 
 C14(H14), C16(H16), C17(H17), C18(H18) 
2.c Idealised Me refined as rotating group: 
 C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B, 
 H29C) 
;
_shelx_res_checksum              77596
_shelx_shelxl_version_number     2019/2
_olex2_submission_special_instructions 'No special instructions were received'