A low-valent dinuclear ruthenium diazadiene complex catalyzes the oxidation of dihydrogen and reversible hydrogenation of quinones
Yang, Xiuxiu; Gianetti, Thomas L.; Wörle, Michael D.; van Leest, Nicolaas P.; de Bruin, Bas; Grützmacher, Hansjörg; Chemical Science  (2019) –; doi:10.1039/C8SC02864H

data_1550238
_publ_section_title
;
 A low-valent dinuclear ruthenium diazadiene complex catalyzes the
 oxidation of dihydrogen and reversible hydrogenation of quinones
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC02864H
_journal_year                    2019
_chemical_formula_moiety         'C20 H24 Cl2 N2 Ru'
_chemical_formula_sum            'C20 H24 Cl2 N2 Ru'
_chemical_formula_weight         464.38
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-01 deposited with the CCDC.
2018-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                66.777(5)
_cell_angle_beta                 75.242(4)
_cell_angle_gamma                70.583(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2597(3)
_cell_length_b                   10.9580(5)
_cell_length_c                   12.6335(6)
_cell_measurement_reflns_used    6726
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0710
_cell_measurement_theta_min      3.1650
_cell_volume                     980.91(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details
;
  1 omega  -77.00    2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303  -77.0000    0.0000 79

  2 omega -102.00  -71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303  161.0000 -135.0000 31

  3 omega   20.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000 -180.0000 49

  4 omega  -41.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -57.0000   60.0000 84

  5 omega    9.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553   57.0000  -60.0000 82

  6 omega  -15.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553   19.0000 -120.0000 109
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0057416000
_diffrn_orient_matrix_UB_12      0.0097547000
_diffrn_orient_matrix_UB_13      0.0532375000
_diffrn_orient_matrix_UB_21      0.0095563000
_diffrn_orient_matrix_UB_22      -0.0714544000
_diffrn_orient_matrix_UB_23      0.0300133000
_diffrn_orient_matrix_UB_31      0.0913160000
_diffrn_orient_matrix_UB_32      -0.0110987000
_diffrn_orient_matrix_UB_33      -0.0086652000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11036
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.733
_diffrn_reflns_theta_min         2.786
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.067
_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     228
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0276P)^2^+0.2147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5722
_reflns_number_total             6415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02864h2.cif
_cod_data_source_block           exp_2130
_cod_database_code               1550238
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C20H30Ru2N2
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H4), C5(H5), C13(H6), C14(H9), N1(H13), C6(H20)
2.b Secondary CH2 refined with riding coordinates:
 C3(H21A,H21B), C2(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H8), C19(H12), C8(H15), C10(H16), C11(H17), C18(H19), C9(H22), C17(H23)
2.d Idealised Me refined as rotating group:
 C1(H18A,H18B,H18C), C4(H25A,H25B,H25C)
;
_shelx_res_checksum              3110
_olex2_submission_special_instructions 'No special instructions were received'