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_1550241
_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
'C48 H55.04 K N2 O6 Ru2, C20 H37.49 K O8, C4 H8 O, C1.94 H3.3 O0.58, C2.06 H4.12 O0.42'
_chemical_formula_sum            'C76 H107.92 K2 N2 O16 Ru2'
_chemical_formula_weight         1585.90
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 91.4431(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8109(8)
_cell_length_b                   28.5059(14)
_cell_length_c                   19.5850(10)
_cell_measurement_reflns_used    7560
_cell_measurement_temperature    102
_cell_measurement_theta_max      29.365
_cell_measurement_theta_min      1.7568
_cell_volume                     7708.0(7)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      101.8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1545
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            218987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.200
_exptl_absorpt_coefficient_mu    0.565
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       needle
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.073
_refine_diff_density_min         -2.675
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         19137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0775P)^2^+14.1727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16803
_reflns_number_total             19137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02864h2.cif
_cod_data_source_block           mo_xy_341_0m
_cod_database_code               1550241
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.707
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H46A)=Sof(H46B)=FVAR(1)
 Sof(H66C)=Sof(H66D)=1-FVAR(2)
 Sof(H68C)=Sof(H68D)=Sof(H69A)=Sof(H69B)=1-FVAR(3)
 Sof(H73A)=Sof(H73B)=1-FVAR(4)
 Sof(H72A)=Sof(H72B)=1-FVAR(5)
 Sof(H46C)=Sof(H46D)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=1-FVAR(6)
 Sof(C1A)=Sof(H1AB)=Sof(H1AC)=FVAR(6)
 Sof(O9A)=1-FVAR(7)
 Sof(O9)=FVAR(7)
 Sof(C71A)=Sof(H71C)=Sof(H71D)=1-FVAR(8)
 Sof(C71)=Sof(H71A)=Sof(H71B)=FVAR(8)
 Sof(C73A)=Sof(H73C)=Sof(H73D)=1-FVAR(9)
 Sof(C73)=FVAR(9)
 Sof(C72A)=Sof(H72C)=Sof(H72D)=1-FVAR(10)
 Sof(C72)=FVAR(10)
 Sof(H66A)=Sof(H66B)=Sof(O8A)=1-FVAR(11)
 Sof(O8)=FVAR(11)
 Sof(H68A)=Sof(H68B)=Sof(C69A)=Sof(H69C)=Sof(H69D)=1-FVAR(12)
 Sof(C69)=FVAR(12)
 Sof(H48C)=Sof(H48D)=Sof(O3A)=1-FVAR(13)
 Sof(O3)=Sof(H48A)=Sof(H48B)=FVAR(13)
 Sof(C70A)=Sof(H70A)=Sof(H70B)=1-FVAR(14)
 Sof(C70)=FVAR(14)
 Sof(O0AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C3A)=Sof(H3AB)=Sof(H3AC)=Sof(C1C)=
 Sof(H1CA)=Sof(H1CB)=1-FVAR(15)
 Sof(O0AA)=Sof(C1)=Sof(H1)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 FVAR(15)
 Sof(C2A)=Sof(H2AB)=Sof(H2AC)=1-FVAR(16)
 Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(16)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C14(H14), C5(H5), C6(H6), C22(H22), C30(H30), C29(H29), C21(H21),
 C43(H43)
3.b Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C45(H45A,H45B), C60(H60A,H60B), C61(H61A,H61B), C59(H59A,
 H59B), C40(H40A,H40B), C44(H44A,H44B), C53(H53A,H53B), C56(H56A,H56B),
 C42(H42A,H42B), C54(H54A,H54B), C41(H41A,H41B), C55(H55A,H55B), C39(H39A,H39B),
  C50(H50A,H50B), C38(H38A,H38B), C49(H49A,H49B), C52(H52A,H52B), C57(H57A,
 H57B), C46(H46A,H46B), C46(H46C,H46D), C51(H51A,H51B), C1A(H1AB,H1AC),
 C66(H66C,H66D), C66(H66A,H66B), C67(H67A,H67B), C68(H68C,H68D), C68(H68A,H68B),
  C69(H69A,H69B), C73(H73A,H73B), C72(H72A,H72B), C71(H71A,H71B), C64(H64A,
 H64B), C65(H65A,H65B), C63(H63A,H63B), C62(H62A,H62B), C48(H48A,H48B),
 C48(H48C,H48D), C1B(H1BA,H1BB), C71A(H71C,H71D), C73A(H73C,H73D), C72A(H72C,
 H72D), C69A(H69C,H69D), C70A(H70A,H70B), C2(H2A,H2B), C3(H3A,H3B), C9(H9A,H9B),
  C9A(H9AA,H9AB), C3A(H3AB,H3AC), C1C(H1CA,H1CB), C2A(H2AB,H2AC)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C19(H19), C8(H8), C27(H27), C18(H18), C10(H10), C3AA(H3AA),
 C11(H11), C35(H35), C16(H16), C25(H25), C26(H26), C17(H17), C32(H32), C34(H34),
  C33(H33), C1(H1)
3.d Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'