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_7247860
_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         'C29 H36 Cl N O Ru'
_chemical_formula_sum            'C29 H36 Cl N O Ru'
_chemical_formula_weight         551.11
_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             2023-07-18
_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                90
_cell_angle_beta                 99.3510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.39840(10)
_cell_length_b                   12.30260(10)
_cell_length_c                   18.3366(2)
_cell_measurement_reflns_used    26802
_cell_measurement_temperature    104.5(7)
_cell_measurement_theta_max      25.0270
_cell_measurement_theta_min      2.2440
_cell_volume                     2537.17(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      104.5(7)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -126.01 105.99   1.00    5.00   6.61  -9.84 -31.50    --   232
  2  \w   -100.81  15.19   1.00    5.00    --   -9.84 -59.25 -51.92  116
  3  \w   -100.81  15.19   1.00    5.00    --   -9.84 -59.25-123.92  116
  4  \w   -100.81  15.19   1.00    5.00    --   -9.84 -59.25 164.08  116
  5  \w    -60.89   0.11   1.00    5.00    --  -14.77  94.56 -34.84   61
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0343273000
_diffrn_orient_matrix_UB_12      0.0477498000
_diffrn_orient_matrix_UB_13      0.0015899000
_diffrn_orient_matrix_UB_21      -0.0495906000
_diffrn_orient_matrix_UB_22      -0.0258992000
_diffrn_orient_matrix_UB_23      -0.0214170000
_diffrn_orient_matrix_UB_31      -0.0184909000
_diffrn_orient_matrix_UB_32      -0.0192443000
_diffrn_orient_matrix_UB_33      0.0328024000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44264
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         2.251
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0261P)^2^+2.5289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4281
_reflns_number_total             4454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc03374k3.cif
_cod_data_source_block           rm_gd_312
_cod_depositor_comments
'Adding full bibliography for 7247859--7247860.cif.'
_cod_database_code               7247860
_shelx_shelxl_version_number     2018/3
_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:
 C14(H14), C17(H17), C26(H26)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C25(H25), C21(H21), C7(H7), C24(H24), C2(H2), C3(H3), C12(H12),
 C5(H5), C10(H10), C4(H4), C11(H11)
2.c Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C27(H27a,H27b,H27c), C19(H19a,H19b,H19c), C16(H16a,H16b,
 H16c), C15(H15a,H15b,H15c), C28(H28a,H28b,H28c), C18(H18a,H18b,H18c)
;
_shelx_res_checksum              54599
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.555
_oxdiff_exptl_absorpt_empirical_full_min 0.501