A thiolate-bridged ruthenium–molybdenum complex featuring terminal nitrido and bridging amido ligands derived from the N–H and N–N bond cleavage of hydrazine
Li, Yahui; Su, Linan; Yang, Dawei; Di, Kai; Wang, Baomin; Qu, Jingping; Dalton Transactions  (2022) –; doi:10.1039/D2DT01378A

data_7710681
_publ_section_title
;
 A thiolate-bridged ruthenium--molybdenum complex featuring terminal
 nitrido and bridging amido ligands derived from the N--H and N--N bond
 cleavage of hydrazine
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01378A
_journal_year                    2022
_chemical_formula_moiety         'C26 H38 Mo N2 Ru S2'
_chemical_formula_sum            'C26 H38 Mo N2 Ru S2'
_chemical_formula_weight         639.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-02 deposited with the CCDC.	2022-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8725(14)
_cell_length_b                   16.2572(16)
_cell_length_c                   22.557(2)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    297.0
_cell_measurement_theta_max      29.522
_cell_measurement_theta_min      2.739
_cell_volume                     5453.9(9)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      297.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35336
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.064
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5501
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1368 before and 0.0827 after correction.
The Ratio of minimum to maximum transmission is 0.7373.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         5575
_refine_ls_number_restraints     1034
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0208P)^2^+13.3480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4132
_reflns_number_total             5575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01378a2.cif
_cod_data_source_block           1_CCDC3
_cod_original_cell_volume        5454.0(9)
_cod_database_code               7710681
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.891
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Mo02-S004 \\sim Mo-S0
 with sigma of 0.02
 S003-C00E \\sim S1-C7AA
 with sigma of 0.02
 S004-C00K \\sim S0-C7BA
 with sigma of 0.02
 C007-C00G \\sim C0-C8AA
 with sigma of 0.02
 C008-C00J \\sim C1-C9AA
 with sigma of 0.02
 C009-C00N \\sim C2-C0BA
 with sigma of 0.02
 C00A-C00L \\sim C0AA-C1BA
 with sigma of 0.02
 C00B-C00O \\sim C1AA-C2BA
 with sigma of 0.02
 C00C-C00R \\sim C2AA-C3BA
 with sigma of 0.02
 C00D-C00W \\sim C3AA-C00X
 with sigma of 0.02
 C00E-C00K \\sim C7AA-C7BA
 with sigma of 0.02
 C00E-C00M \\sim C7AA-C8BA
 with sigma of 0.02
 C00F-C00T \\sim C4AA-C4BA
 with sigma of 0.02
 C00H-C00S \\sim C5AA-C5BA
 with sigma of 0.02
 C00I-C00U \\sim C6AA-C6BA
 with sigma of 0.02
 C00K-C00Q \\sim C7BA-C9BA
 with sigma of 0.02
 C00M-C00V \\sim C8BA-C0CA
 with sigma of 0.02
 C00P-C00Q \\sim C1CA-C9BA
 with sigma of 0.02
 C00P-C00V \\sim C1CA-C0CA
 with sigma of 0.02
 Ru01-Mo02 \\sim Ru-Mo
 with sigma of 0.04
 Ru01-S003 \\sim Ru-S1
 with sigma of 0.04
 Ru01-S004 \\sim Ru-S0
 with sigma of 0.04
 Ru01-N005 \\sim Ru-N0
 with sigma of 0.04
 Ru01-N006 \\sim Ru-N1
 with sigma of 0.04
 Ru01-C007 \\sim Ru-C0
 with sigma of 0.04
 Ru01-C008 \\sim Ru-C1
 with sigma of 0.04
 Ru01-C009 \\sim Ru-C2
 with sigma of 0.04
 Ru01-C00A \\sim Ru-C0AA
 with sigma of 0.04
 Ru01-C00B \\sim Ru-C1AA
 with sigma of 0.04
 Ru01-C00C \\sim Ru-C2AA
 with sigma of 0.04
 Ru01-C00D \\sim Ru-C3AA
 with sigma of 0.04
 Ru01-C00E \\sim Ru-C7AA
 with sigma of 0.04
 Ru01-C00F \\sim Ru-C4AA
 with sigma of 0.04
 Ru01-C00G \\sim Ru-C8AA
 with sigma of 0.04
 Ru01-C00H \\sim Ru-C5AA
 with sigma of 0.04
 Ru01-C00I \\sim Ru-C6AA
 with sigma of 0.04
 Ru01-C00J \\sim Ru-C9AA
 with sigma of 0.04
 Ru01-C00L \\sim Ru-C1BA
 with sigma of 0.04
 Ru01-C00N \\sim Ru-C0BA
 with sigma of 0.04
 Ru01-C00O \\sim Ru-C2BA
 with sigma of 0.04
 Mo02-S003 \\sim Mo-S1
 with sigma of 0.04
 Mo02-N005 \\sim Mo-N0
 with sigma of 0.04
 Mo02-N006 \\sim Mo-N1
 with sigma of 0.04
 Mo02-C007 \\sim Mo-C0
 with sigma of 0.04
 Mo02-C008 \\sim Mo-C1
 with sigma of 0.04
 Mo02-C009 \\sim Mo-C2
 with sigma of 0.04
 Mo02-C00A \\sim Mo-C0AA
 with sigma of 0.04
 Mo02-C00B \\sim Mo-C1AA
 with sigma of 0.04
 Mo02-C00C \\sim Mo-C2AA
 with sigma of 0.04
 Mo02-C00D \\sim Mo-C3AA
 with sigma of 0.04
 Mo02-C00E \\sim Mo-C7AA
 with sigma of 0.04
 Mo02-C00F \\sim Mo-C4AA
 with sigma of 0.04
 Mo02-C00H \\sim Mo-C5AA
 with sigma of 0.04
 Mo02-C00I \\sim Mo-C6AA
 with sigma of 0.04
 Mo02-C00K \\sim Mo-C7BA
 with sigma of 0.04
 Mo02-C00R \\sim Mo-C3BA
 with sigma of 0.04
 Mo02-C00S \\sim Mo-C5BA
 with sigma of 0.04
 Mo02-C00T \\sim Mo-C4BA
 with sigma of 0.04
 Mo02-C00U \\sim Mo-C6BA
 with sigma of 0.04
 Mo02-C00W \\sim Mo-C00X
 with sigma of 0.04
 S003-S004 \\sim S1-S0
 with sigma of 0.04
 S003-N005 \\sim S1-N0
 with sigma of 0.04
 S003-N006 \\sim S1-N1
 with sigma of 0.04
 S003-C007 \\sim S1-C0
 with sigma of 0.04
 S003-C008 \\sim S1-C1
 with sigma of 0.04
 S003-C009 \\sim S1-C2
 with sigma of 0.04
 S003-C00A \\sim S1-C0AA
 with sigma of 0.04
 S003-C00B \\sim S1-C1AA
 with sigma of 0.04
 S003-C00C \\sim S1-C2AA
 with sigma of 0.04
 S003-C00D \\sim S1-C3AA
 with sigma of 0.04
 S003-C00F \\sim S1-C4AA
 with sigma of 0.04
 S003-C00H \\sim S1-C5AA
 with sigma of 0.04
 S003-C00I \\sim S1-C6AA
 with sigma of 0.04
 S003-C00K \\sim S1-C7BA
 with sigma of 0.04
 S003-C00M \\sim S1-C8BA
 with sigma of 0.04
 S004-N005 \\sim S0-N0
 with sigma of 0.04
 S004-N006 \\sim S0-N1
 with sigma of 0.04
 S004-C00C \\sim S0-C2AA
 with sigma of 0.04
 S004-C00D \\sim S0-C3AA
 with sigma of 0.04
 S004-C00E \\sim S0-C7AA
 with sigma of 0.04
 S004-C00F \\sim S0-C4AA
 with sigma of 0.04
 S004-C00H \\sim S0-C5AA
 with sigma of 0.04
 S004-C00I \\sim S0-C6AA
 with sigma of 0.04
 S004-C00Q \\sim S0-C9BA
 with sigma of 0.04
 N005-N006 \\sim N0-N1
 with sigma of 0.04
 N005-C007 \\sim N0-C0
 with sigma of 0.04
 N005-C008 \\sim N0-C1
 with sigma of 0.04
 N005-C009 \\sim N0-C2
 with sigma of 0.04
 N005-C00A \\sim N0-C0AA
 with sigma of 0.04
 N005-C00B \\sim N0-C1AA
 with sigma of 0.04
 N005-C00C \\sim N0-C2AA
 with sigma of 0.04
 N005-C00D \\sim N0-C3AA
 with sigma of 0.04
 N005-C00F \\sim N0-C4AA
 with sigma of 0.04
 N005-C00H \\sim N0-C5AA
 with sigma of 0.04
 N005-C00I \\sim N0-C6AA
 with sigma of 0.04
 N006-C007 \\sim N1-C0
 with sigma of 0.04
 N006-C008 \\sim N1-C1
 with sigma of 0.04
 N006-C009 \\sim N1-C2
 with sigma of 0.04
 N006-C00A \\sim N1-C0AA
 with sigma of 0.04
 N006-C00B \\sim N1-C1AA
 with sigma of 0.04
 N006-C00C \\sim N1-C2AA
 with sigma of 0.04
 N006-C00D \\sim N1-C3AA
 with sigma of 0.04
 N006-C00F \\sim N1-C4AA
 with sigma of 0.04
 N006-C00H \\sim N1-C5AA
 with sigma of 0.04
 N006-C00I \\sim N1-C6AA
 with sigma of 0.04
 C007-C008 \\sim C0-C1
 with sigma of 0.04
 C007-C009 \\sim C0-C2
 with sigma of 0.04
 C007-C00A \\sim C0-C0AA
 with sigma of 0.04
 C007-C00B \\sim C0-C1AA
 with sigma of 0.04
 C007-C00J \\sim C0-C9AA
 with sigma of 0.04
 C007-C00O \\sim C0-C2BA
 with sigma of 0.04
 C008-C009 \\sim C1-C2
 with sigma of 0.04
 C008-C00A \\sim C1-C0AA
 with sigma of 0.04
 C008-C00B \\sim C1-C1AA
 with sigma of 0.04
 C008-C00G \\sim C1-C8AA
 with sigma of 0.04
 C008-C00L \\sim C1-C1BA
 with sigma of 0.04
 C009-C00A \\sim C2-C0AA
 with sigma of 0.04
 C009-C00B \\sim C2-C1AA
 with sigma of 0.04
 C009-C00L \\sim C2-C1BA
 with sigma of 0.04
 C009-C00O \\sim C2-C2BA
 with sigma of 0.04
 C00A-C00B \\sim C0AA-C1AA
 with sigma of 0.04
 C00A-C00J \\sim C0AA-C9AA
 with sigma of 0.04
 C00A-C00N \\sim C0AA-C0BA
 with sigma of 0.04
 C00B-C00G \\sim C1AA-C8AA
 with sigma of 0.04
 C00B-C00N \\sim C1AA-C0BA
 with sigma of 0.04
 C00C-C00D \\sim C2AA-C3AA
 with sigma of 0.04
 C00C-C00F \\sim C2AA-C4AA
 with sigma of 0.04
 C00C-C00H \\sim C2AA-C5AA
 with sigma of 0.04
 C00C-C00I \\sim C2AA-C6AA
 with sigma of 0.04
 C00C-C00T \\sim C2AA-C4BA
 with sigma of 0.04
 C00C-C00W \\sim C2AA-C00X
 with sigma of 0.04
 C00D-C00F \\sim C3AA-C4AA
 with sigma of 0.04
 C00D-C00H \\sim C3AA-C5AA
 with sigma of 0.04
 C00D-C00I \\sim C3AA-C6AA
 with sigma of 0.04
 C00D-C00R \\sim C3AA-C3BA
 with sigma of 0.04
 C00D-C00S \\sim C3AA-C5BA
 with sigma of 0.04
 C00E-C00Q \\sim C7AA-C9BA
 with sigma of 0.04
 C00E-C00V \\sim C7AA-C0CA
 with sigma of 0.04
 C00F-C00H \\sim C4AA-C5AA
 with sigma of 0.04
 C00F-C00I \\sim C4AA-C6AA
 with sigma of 0.04
 C00F-C00R \\sim C4AA-C3BA
 with sigma of 0.04
 C00F-C00U \\sim C4AA-C6BA
 with sigma of 0.04
 C00H-C00I \\sim C5AA-C6AA
 with sigma of 0.04
 C00H-C00U \\sim C5AA-C6BA
 with sigma of 0.04
 C00H-C00W \\sim C5AA-C00X
 with sigma of 0.04
 C00I-C00S \\sim C6AA-C5BA
 with sigma of 0.04
 C00I-C00T \\sim C6AA-C4BA
 with sigma of 0.04
 C00K-C00M \\sim C7BA-C8BA
 with sigma of 0.04
 C00K-C00P \\sim C7BA-C1CA
 with sigma of 0.04
 C00M-C00P \\sim C8BA-C1CA
 with sigma of 0.04
 C00Q-C00V \\sim C9BA-C0CA
 with sigma of 0.04
3. Rigid bond restraints
 Mo02, S003
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Mo02 \\sim S003: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001
S004 \\sim Ru01 \\sim Mo02 \\sim S003 \\sim N005 \\sim N006 \\sim C007 \\sim
C008 \\sim C009 \\sim C00A \\sim C00B \\sim C00C \\sim C00D \\sim C00F \\sim
C00H \\sim C00I \\sim C00E \\sim C00G \\sim C00J \\sim C00N \\sim C00L \\sim
C00O \\sim C00R \\sim C00W \\sim C00T \\sim C00S \\sim C00U \\sim C00K \\sim
C00M \\sim C00Q \\sim C00V \\sim C00P \\sim S1 \\sim S0 \\sim Mo \\sim C7BA
\\sim N0 \\sim N1 \\sim C2AA \\sim C3AA \\sim C5AA \\sim C6AA \\sim C4AA \\sim
Ru \\sim C7AA \\sim C9BA \\sim C3BA \\sim C00X \\sim C5BA \\sim C6BA \\sim C4BA
\\sim C0 \\sim C1 \\sim C2 \\sim C0AA \\sim C1AA \\sim C8BA \\sim C1CA \\sim
C8AA \\sim C9AA \\sim C0BA \\sim C1BA \\sim C2BA \\sim C0CA: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(S0)=Sof(Ru)=Sof(Mo)=Sof(S1)=Sof(N0)=Sof(H0A)=Sof(H0B)=Sof(N1)=Sof(H1A)=
 Sof(H1B)=Sof(C0)=Sof(C1)=Sof(C2)=Sof(C0AA)=Sof(C1AA)=Sof(C2AA)=Sof(C3AA)=
 Sof(C4AA)=Sof(C5AA)=Sof(C6AA)=Sof(C7AA)=Sof(C8AA)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=Sof(C9AA)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C0BA)=Sof(H0BA)=
 Sof(H0BB)=Sof(H0BC)=Sof(C1BA)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2BA)=
 Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3BA)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=
 Sof(C00X)=Sof(H3AA)=Sof(HH)=Sof(HI)=Sof(C4BA)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=
 Sof(C5BA)=Sof(H5BA)=Sof(H5BB)=Sof(H5BC)=Sof(C6BA)=Sof(H6BA)=Sof(H6BB)=
 Sof(H6BC)=Sof(C7BA)=Sof(C8BA)=Sof(H8BA)=Sof(C9BA)=Sof(H9BA)=Sof(C0CA)=
 Sof(H0CA)=Sof(C1CA)=Sof(H1CA)=1-FVAR(1)
 Sof(Ru01)=Sof(Mo02)=Sof(S003)=Sof(S004)=Sof(N005)=Sof(H00A)=Sof(H00B)=
 Sof(N006)=Sof(H00C)=Sof(H00D)=Sof(C007)=Sof(C008)=Sof(C009)=Sof(C00A)=
 Sof(C00B)=Sof(C00C)=Sof(C00D)=Sof(C00E)=Sof(C00F)=Sof(C00G)=Sof(H00E)=
 Sof(H00F)=Sof(H00G)=Sof(C00H)=Sof(C00I)=Sof(C00J)=Sof(H00H)=Sof(H00I)=
 Sof(H00J)=Sof(C00K)=Sof(C00L)=Sof(H00K)=Sof(H00L)=Sof(H00M)=Sof(C00M)=
 Sof(H00N)=Sof(C00N)=Sof(H00O)=Sof(H00P)=Sof(H00Q)=Sof(C00O)=Sof(H00R)=
 Sof(H00S)=Sof(H00T)=Sof(C00P)=Sof(H00U)=Sof(C00Q)=Sof(H00V)=Sof(C00R)=
 Sof(H00W)=Sof(H00X)=Sof(H00Y)=Sof(C00S)=Sof(H00Z)=Sof(H)=Sof(HA)=Sof(C00T)=
 Sof(H00)=Sof(HB)=Sof(HC)=Sof(C00U)=Sof(H0AA)=Sof(HD)=Sof(HE)=Sof(C00V)=
 Sof(H1AA)=Sof(C00W)=Sof(H2AA)=Sof(HF)=Sof(HG)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 N005(H00A,H00B), N006(H00C,H00D), N0(H0A,H0B), N1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C00M(H00N), C00P(H00U), C00Q(H00V), C00V(H1AA), C8BA(H8BA), C9BA(H9BA),
 C0CA(H0CA), C1CA(H1CA)
6.c Idealised Me refined as rotating group:
 C00G(H00E,H00F,H00G), C00J(H00H,H00I,H00J), C00L(H00K,H00L,H00M), C00N(H00O,
 H00P,H00Q), C00O(H00R,H00S,H00T), C00R(H00W,H00X,H00Y), C00S(H00Z,H,HA),
 C00T(H00,HB,HC), C00U(H0AA,HD,HE), C00W(H2AA,HF,HG), C8AA(H8AA,H8AB,H8AC),
 C9AA(H9AA,H9AB,H9AC), C0BA(H0BA,H0BB,H0BC), C1BA(H1BA,H1BB,H1BC), C2BA(H2BA,
 H2BB,H2BC), C3BA(H3BA,H3BB,H3BC), C00X(H3AA,HH,HI), C4BA(H4BA,H4BB,H4BC),
 C5BA(H5BA,H5BB,H5BC), C6BA(H6BA,H6BB,H6BC)
;
_shelx_res_checksum              1919
_olex2_submission_special_instructions 'No special instructions were received'