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_7061695
_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         'C15 H12 Cl N O Ru'
_chemical_formula_sum            'C15 H12 Cl N O Ru'
_chemical_formula_weight         358.78
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc28xgym
_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                90
_cell_angle_beta                 117.249(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3837(9)
_cell_length_b                   15.434(2)
_cell_length_c                   12.6134(18)
_cell_measurement_reflns_used    2687
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5890
_cell_measurement_theta_min      2.2370
_cell_volume                     1277.9(3)
_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_type            EosS2
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_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  79.00   1.00   45.06    --   13.76  57.00 -60.00   78
  2  \w      1.00  27.00   1.00   45.06    --   13.76  77.00  30.00   26
  3  \w     42.00  73.00   1.00   45.06    --   13.76-137.00-143.00   31
  4  \w    -13.00  50.00   1.00   45.06    --  -15.95  57.00-180.00   63
;
_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      0.0513545000
_diffrn_orient_matrix_UB_12      0.0168387000
_diffrn_orient_matrix_UB_13      0.0526803000
_diffrn_orient_matrix_UB_21      -0.0211458000
_diffrn_orient_matrix_UB_22      0.0427595000
_diffrn_orient_matrix_UB_23      -0.0203916000
_diffrn_orient_matrix_UB_31      -0.0794734000
_diffrn_orient_matrix_UB_32      -0.0004835000
_diffrn_orient_matrix_UB_33      0.0285722000
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5778
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.024
_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    1.424
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.697
_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    1.8648
_exptl_crystal_description       block
_exptl_crystal_F_000             712.0
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.7521
_refine_diff_density_min         -0.6264
_refine_diff_density_rms         0.1507
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             9.0720
_refine_ls_goodness_of_fit_ref   1.0164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0164
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0303P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -8
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                1514
_reflns_number_total             2257
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj03121c2.cif
_cod_data_source_block           R8HQ
_cod_depositor_comments
'Adding full bibliography for 7061695--7061696.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C15 H12 Cl1 N O Ru'
_cod_database_code               7061695
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Riding coordinates:
 C13(H13), C15(H15), C12(H12), C11(H11), C10(H10), C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C2(H2), C1(H1), C6(H6), C3(H3)
;
_olex2_date_sample_data_collection 2018-06-28
_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 1.721
_oxdiff_exptl_absorpt_empirical_full_min 0.523