A highly active and chemoselective homobimetallic ruthenium catalyst for one-pot reductive amination in water
Deshmukh, Gopal; Rana, Thakur Rochak Kumar; Yadav, Nikita; Rajaraman, Gopalan; Murugavel, Ramaswamy; Green Chemistry 26 (2024) 1610–1626; doi:10.1039/D3GC03374K

data_7247859
_publ_section_title
;
 A highly active and chemoselective homobimetallic ruthenium catalyst for
 one-pot reductive amination in water
;
_journal_issue                   3
_journal_name_full               'Green Chemistry'
_journal_page_first              1610
_journal_page_last               1626
_journal_paper_doi               10.1039/D3GC03374K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C58 H70 Cl2 N2 O2 Ru2, 2(C2 O), 0.5(C2 O2)'
_chemical_formula_sum            'C63 H70 Cl2 N2 O5 Ru2'
_chemical_formula_weight         1208.25
_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
_audit_creation_date             2023-08-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-28 deposited with the CCDC.	2023-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.474(4)
_cell_angle_beta                 89.037(4)
_cell_angle_gamma                78.850(4)
_cell_formula_units_Z            1
_cell_length_a                   10.8293(13)
_cell_length_b                   11.2973(14)
_cell_length_c                   12.2048(14)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.56
_cell_volume                     1452.3(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            51543
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.140
_diffrn_reflns_theta_max         25.140
_diffrn_reflns_theta_min         2.540
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6770
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0953 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.9085.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.553
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5178
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0703P)^2^+6.3295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4631
_reflns_number_total             5178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc03374k3.cif
_cod_data_source_block           rm_gd_241_0m
_cod_depositor_comments
'Adding full bibliography for 7247859--7247860.cif.'
_cod_database_code               7247859
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.750
_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. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3. Others
 Fixed Sof: O3(0.5)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C22(H22), C27(H27)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C19(H19), C20(H20), C25(H25)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              80303
_olex2_submission_special_instructions 'No special instructions were received'