Formic acid dehydrogenation by [Ru(η6-benzene)(L)Cl] catalysts: L = 2-methylquinolin-8-olate and quinolin-8-olate
Vatsa, Aditi; Padhi, Sumanta Kumar; New Journal of Chemistry 46 (2022) 15723–15731; doi:10.1039/D2NJ03121C

data_7061696
_publ_section_title
;
 Formic acid dehydrogenation by [Ru(\h6-benzene)(L)Cl] catalysts: L =
 2-methylquinolin-8-olate and quinolin-8-olate
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15723
_journal_page_last               15731
_journal_paper_doi               10.1039/D2NJ03121C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C16 H14 Cl N O Ru'
_chemical_formula_sum            'C16 H14 Cl N O Ru'
_chemical_formula_weight         372.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc28xgzn
_audit_creation_date             2021-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-28 deposited with the CCDC.	2022-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                91.151(7)
_cell_angle_beta                 91.017(7)
_cell_angle_gamma                98.196(7)
_cell_formula_units_Z            2
_cell_length_a                   7.5620(7)
_cell_length_b                   9.2366(8)
_cell_length_c                   9.7047(8)
_cell_measurement_reflns_used    5381
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1400
_cell_measurement_theta_min      2.6860
_cell_volume                     670.64(10)
_computing_cell_refinement
;
'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
;
_computing_data_collection
;
'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
;
_computing_data_reduction
;
'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0606
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9902
_diffrn_measured_fraction_theta_max 0.9902
_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     -1.00  67.00   1.00   15.91    --   13.76  57.00   0.00   68
  2  \w    -52.00  18.00   1.00   15.91    --   13.76 -57.00 -60.00   70
  3  \w    -79.00  -1.00   1.00   15.91    --  -15.95 -57.00 150.00   78
  4  \w    -41.00  51.00   1.00   15.91    --  -15.95  77.00-180.00   92
  5  \w    -84.00  -3.00   1.00   15.91    --  -15.95 -19.00-150.00   81
  6  \w    -80.00   7.00   1.00   15.91    --  -15.95 -77.00  60.00   87
  7  \w    -71.00 -21.00   1.00   15.91    --  -15.95 129.00-147.41   50
  8  \w    -79.00 -37.00   1.00   15.91    --  -15.95-178.00 -90.00   42
  9  \w    -67.00 -37.00   1.00   15.91    --  -15.95 123.00 -62.15   30
 10  \w    -76.00 -22.00   1.00   15.91    --  -15.95 137.00  37.29   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       \w-scans
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0457895000
_diffrn_orient_matrix_UB_12      0.0538743000
_diffrn_orient_matrix_UB_13      0.0459807000
_diffrn_orient_matrix_UB_21      -0.0692544000
_diffrn_orient_matrix_UB_22      -0.0150828000
_diffrn_orient_matrix_UB_23      0.0482140000
_diffrn_orient_matrix_UB_31      0.0457349000
_diffrn_orient_matrix_UB_32      -0.0537827000
_diffrn_orient_matrix_UB_33      0.0301261000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10363
_diffrn_reflns_theta_full        24.9971
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.8461
_exptl_crystal_description       block
_exptl_crystal_F_000             369.9242
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.7957
_refine_diff_density_min         -0.6459
_refine_diff_density_rms         0.1354
_refine_ls_d_res_high            0.8410
_refine_ls_d_res_low             9.7006
_refine_ls_goodness_of_fit_ref   0.9893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9893
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                2064
_reflns_number_total             2331
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj03121c2.cif
_cod_data_source_block           R2M8HQ
_cod_depositor_comments
;
Adding full bibliography for 7061695--7061696.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C32 H28 Cl2 N2 O2 Ru2'
_cod_original_formula_weight         745.63
_cod_original_formula_moiety         '2(C16 H14 Cl N O Ru)'
_cod_original_formula_units_Z            1
_cod_database_code               7061696
_chemical_oxdiff_formula         'C33 H30 N3 O3 Br1 '
_reflns_odcompleteness_completeness 100.00
_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.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C11(H11), C12(H12), C5(H5), C7(H7), C13(H13), C3(H3), C14(H14),
 C15(H15), C2(H2), C6(H6)
2.b Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c)
;
_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 2.602
_oxdiff_exptl_absorpt_empirical_full_min 0.560