Carboxamide carbonyl-ruthenium(ii) complexes: detailed structural and mechanistic studies in the transfer hydrogenation of ketones
Kumah, Robert T.; Vijayan, Paranthaman; Ojwach, Stephen O.; New Journal of Chemistry 46 (2022) 3146–3155; doi:10.1039/D1NJ05657C

data_7061241
_publ_section_title
;
 Carboxamide carbonyl-ruthenium(ii) complexes: detailed structural and
 mechanistic studies in the transfer hydrogenation of ketones
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3146
_journal_page_last               3155
_journal_paper_doi               10.1039/D1NJ05657C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C49 H37 Cl N4 O2 P2 Ru S'
_chemical_formula_sum            'C49 H37 Cl N4 O2 P2 Ru S'
_chemical_formula_weight         944.34
_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             2021-05-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-28 deposited with the CCDC.	2022-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.809(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.3269(17)
_cell_length_b                   12.2526(10)
_cell_length_c                   37.414(3)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100.05
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.45
_cell_volume                     9686.0(14)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.05
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            176145
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.300
_diffrn_reflns_theta_min         1.099
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       plate
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         23988
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0316P)^2^+9.4494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19547
_reflns_number_total             23988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05657c2.cif
_cod_data_source_block           Ru1
_cod_depositor_comments
;
Adding full bibliography for 7061239--7061241.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C98 H74 Cl2 N8 O4 P4 Ru2 S2'
_cod_original_formula_weight         1888.69
_cod_original_formula_moiety         '2(C49 H37 Cl N4 O2 P2 Ru S)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        9685.9(14)
_cod_database_code               7061241
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.875
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim C50: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
O2 \\sim C49: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O2) = Uanis(C49)
Uanis(O4) = Uanis(C50)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), 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), C38(H38), C39(H39),
  C40(H40), C41(H41), C46(H46), C47(H47), C48(H48), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71),
 C72(H72), C73(H73), C74(H74), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
  C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C88(H88), C89(H89),
 C90(H90), C91(H91), C95(H95), C96(H96), C97(H97)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53947
_shelx_fab_checksum              31573
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'