Transfer Hydrogenation of Aldehydes and Ketones in Air with Methanol and Ethanol by an Air-Stable Ruthenium–Triazole Complex
Ghosh, Rahul; Jana, Narayan Ch.; Panda, Surajit; Bagh, Bidraha; ACS Sustainable Chemistry & Engineering  (2021) –; doi:10.1021/acssuschemeng.1c00633

data_4518575
_publ_section_title
;
 Transfer Hydrogenation of Aldehydes and Ketones in Air with Methanol and
 Ethanol by an Air-Stable Ruthenium--Triazole Complex
;
_journal_name_full               'ACS Sustainable Chemistry &amp; Engineering'
_journal_paper_doi               10.1021/acssuschemeng.1c00633
_journal_year                    2021
_chemical_formula_moiety         'C24 H24 Cl N3 O Ru'
_chemical_formula_sum            'C24 H24 Cl N3 O Ru'
_chemical_formula_weight         506.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.033(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.8691(11)
_cell_length_b                   11.8858(4)
_cell_length_c                   19.9571(10)
_cell_measurement_reflns_used    24371
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.4380
_cell_measurement_theta_min      3.3220
_cell_volume                     4915.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -7.00  18.00   0.50   20.00    --    3.67-109.00 -37.00   50
  2  \w    -11.00  38.00   0.50   20.00    --   -3.98-109.00 -37.00   98
  3  \w    -20.00  38.00   0.50   20.00    --    3.67 -99.00-150.00  116
  4  \w    -65.00   5.00   0.50   20.00    --    3.67 -19.00  60.00  140
  5  \w     10.00  40.00   0.50   20.00    --    3.67 -99.00  90.00   60
  6  \w     -3.00  40.00   0.50   20.00    --    3.67 -99.00 120.00   86
  7  \w     19.00  57.00   0.50   20.00    --   -3.98  57.00-150.00   76
  8  \w    -45.00 -19.00   0.50   20.00    --   -3.98 -77.00 120.00   52
  9  \w    -67.00 -30.00   0.50   20.00    --   -3.98 -57.00-180.00   74
 10  \w     37.00  62.00   0.50   20.00    --   -3.98  38.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0327801000
_diffrn_orient_matrix_UB_12      -0.0144499000
_diffrn_orient_matrix_UB_13      0.0102977000
_diffrn_orient_matrix_UB_21      0.0065902000
_diffrn_orient_matrix_UB_22      0.0078649000
_diffrn_orient_matrix_UB_23      0.0377630000
_diffrn_orient_matrix_UB_31      -0.0073582000
_diffrn_orient_matrix_UB_32      -0.0573383000
_diffrn_orient_matrix_UB_33      0.0025655000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55914
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.330
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         9643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0390P)^2^+11.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8304
_reflns_number_total             9643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sc1c00633_si_002.cif
_cod_data_source_block           bb_012
_cod_depositor_comments
;

2025-09-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C192 H192 Cl8 N24 O8 Ru8'
_cod_original_formula_weight         4055.84
_cod_original_formula_moiety         '8(C24 H24 Cl N3 O Ru)'
_cod_original_formula_units_Z            1
_cod_database_code               4518575
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C192 H196 Cl8 N24 O8 Ru8 '
_diffrn_oxdiff_ac3_digest_frames
;
01794d5733d3791551260831c19acacf9800025b7a1
;
_diffrn_oxdiff_ac3_digest_hkl
;
01fc846e46536fa24ab48e91611578e9d38a24
;
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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(C15') = Uanis(C20') = Uanis(C19')
3.a Ternary CH refined with riding coordinates:
 C22'(H22'), C22(H22)
3.b Aromatic/amide H refined with riding coordinates:
 C1'(H1'), C17'(H17'), C20'(H20'), C1(H1), C10'(H10'), C10(H10), C11'(H11'),
 C16'(H16'), C13'(H13'), C19'(H19'), C12(H12), C11(H11), C19(H19), C12'(H12'),
 C16(H16), C17(H17), C13(H13), C7(H7), C4(H4), C8(H8), C20(H20), C8'(H8'),
 C7'(H7'), C6(H6), C4'(H4'), C6'(H6'), C5(H5), C5'(H5')
3.c Idealised Me refined as rotating group:
 C21'(H21D,H21E,H21F), C24'(H24D,H24E,H24F), C23'(H23D,H23E,H23F), C21(H21A,
 H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              72084
_shelx_hkl_checksum              57539
_shelx_fab_checksum              37334
_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 1.238
_oxdiff_exptl_absorpt_empirical_full_min 0.633