Synthesis of <i>N</i>-alkylated amines <i>via</i> alcohol dehydrogenation catalyzed by a bis-azo-diamido coordinated ruthenium(III) complex.
Halder, Supriyo; Naskar, Srijita; Malik, Sampad; Roy, Dipika; Pramanik, Kausikisankar; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14331–14348; doi:10.1039/d5dt01716e

data_7719311
_publ_section_title
;
 Synthesis of <i>N</i>-alkylated amines <i>via</i> alcohol dehydrogenation
 catalyzed by a bis-azo-diamido coordinated ruthenium(III) complex.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14331
_journal_page_last               14348
_journal_paper_doi               10.1039/d5dt01716e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C36 H29 Cl N6 P Ru'
_chemical_formula_sum            'C36 H29 Cl N6 P Ru'
_chemical_formula_weight         713.14
_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             2025-01-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-24 deposited with the CCDC.	2025-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                93.284(2)
_cell_angle_beta                 105.880(2)
_cell_angle_gamma                113.925(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1769(8)
_cell_length_b                   11.2766(8)
_cell_length_c                   16.0950(12)
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.48
_cell_volume                     1593.9(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8-Quest SCXRD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64436
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.749
_diffrn_reflns_theta_min         2.624
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.5635
_exptl_absorpt_correction_T_min  0.5066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1084 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.8990.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.047
_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     406
_refine_ls_number_reflns         8243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.6273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7356
_reflns_number_total             8243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01716e2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7719311.cif.'
_cod_database_code               7719311
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.852
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N6(H6), C3(H3), C4(H4), C5(H5), C6(H6A), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              90806
_olex2_submission_special_instructions 'No special instructions were received'