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_7710678
_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 H36 Mo N2 Ru S2'
_chemical_formula_sum            'C26 H36 Mo N2 Ru S2'
_chemical_formula_weight         637.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 92.836(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1999(11)
_cell_length_b                   10.4937(9)
_cell_length_c                   19.7054(16)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.234
_cell_measurement_theta_min      2.481
_cell_volume                     2726.2(4)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      294.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0712
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32086
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.457
_diffrn_reflns_theta_min         2.199
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6309
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1016 before and 0.0647 after correction.
The Ratio of minimum to maximum transmission is 0.8461.
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    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0106P)^2^+10.0340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4542
_reflns_number_total             6858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01378a2.cif
_cod_data_source_block           2
_cod_database_code               7710678
_shelx_shelxl_version_number     2018/3
_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.a Secondary CH2 refined with riding coordinates:
 N005(H00a,H00b)
2.b Aromatic/amide H refined with riding coordinates:
 C00B(H00c), C00I(H00I), C00M(H00M), C00R(H00u)
2.c Idealised Me refined as rotating group:
 C00J(H00d,H00e,H00f), C00K(H00g,H00h,H00j), C00O(H00k,H00l,H00n), C00P(H00o,
 H00p,H00q), C00Q(H00r,H00s,H00t), C00S(H00v,H00w,H00x), C00T(H00y,H,Ha),
 C00U(H00z,Hb,Hc), C00V(H00,Hd,He), C00W(H0aa,Hf,Hg)
;
_shelx_res_checksum              24062
_olex2_submission_special_instructions 'No special instructions were received'