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_1550239
_publ_section_title
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 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         'C72 H65 N4 Ru4, C20 H40 K O8, 2(C4 H8 O)'
_chemical_formula_sum            'C100 H121 K N4 O10 Ru4'
_chemical_formula_weight         1982.38
_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   mixed
_audit_creation_date             2017-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-03-01 deposited with the CCDC.
2018-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                110.2733(15)
_cell_angle_beta                 96.1280(15)
_cell_angle_gamma                106.3224(15)
_cell_formula_units_Z            1
_cell_length_a                   9.3201(4)
_cell_length_b                   15.1082(7)
_cell_length_c                   17.7752(9)
_cell_measurement_reflns_used    12541
_cell_measurement_temperature    101
_cell_measurement_theta_max      29.3560
_cell_measurement_theta_min      1.7568
_cell_volume                     2194.55(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      101.2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            87809
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.316
_exptl_absorpt_coefficient_mu    0.786
_exptl_crystal_colour            'clear brownish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         8951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+3.9135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8129
_reflns_number_total             8951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02864h2.cif
_cod_data_source_block           mo_xy_283_2_thf_0m
_cod_database_code               1550239
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C46A)=Sof(H46C)=Sof(H46D)=1-FVAR(1)
 Sof(C46)=Sof(H46A)=Sof(H46B)=FVAR(1)
 Sof(C45A)=Sof(H45C)=Sof(H45D)=1-FVAR(2)
 Sof(C45)=Sof(H45A)=Sof(H45B)=FVAR(2)
 Sof(C44A)=Sof(H44C)=Sof(H44D)=1-FVAR(3)
 Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(3)
 Sof(C43A)=Sof(H43C)=Sof(H43D)=1-FVAR(4)
 Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(4)
 Sof(O2A)=1-FVAR(5)
 Sof(O2)=FVAR(5)
 Sof(O1A)=Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C50A)=Sof(H50C)=Sof(H50D)=
 Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(6)
 Sof(O1)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C49)=
 Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=FVAR(6)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C13(H13), C5(H5), C14(H14), C22(H22), C2(H2), C3(H3), C29(H29),
 C21(H21), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C42(H42A,H42B), C38(H38A,H38B), C39(H39A,H39B), C48(H48A,
 H48B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C46(H46A,H46B),
 C43(H43A,H43B), C45(H45A,H45B), C44(H44A,H44B), C46A(H46C,H46D), C45A(H45C,
 H45D), C44A(H44C,H44D), C43A(H43C,H43D), C47A(H47C,H47D), C50A(H50C,H50D),
 C49A(H49C,H49D), C48A(H48C,H48D)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C24(H24), C8(H8), C27(H27), C11(H11), C19(H19), C18(H18), C25(H25),
 C35(H35), C10(H10), C32(H32), C17(H17), C9(H9), C26(H26), C34(H34), C33(H33)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'