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_7710680
_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 H34 Br2 Mo Ru S2'
_chemical_formula_sum            'C26 H34 Br2 Mo Ru S2'
_chemical_formula_weight         767.48
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-24 deposited with the CCDC.	2022-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4661(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.8970(6)
_cell_length_b                   31.824(2)
_cell_length_c                   19.9124(14)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.422
_cell_measurement_theta_min      2.381
_cell_volume                     5627.6(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      180.0
_diffrn_measured_fraction_theta_full 0.999
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.147
_exptl_absorpt_coefficient_mu    3.984
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5158
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1068 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.6918.
The \l/2 correction factor is 0.00150.
;
_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    1.812
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.618
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.00023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0561
_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^)+75.1030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8967
_reflns_number_total             9959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01378a2.cif
_cod_data_source_block           1_CCDC2
_cod_database_code               7710680
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.503
_shelx_estimated_absorpt_t_min   0.381
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C11(H11), C17(H17), C22(H22), C27(H27), C29(H29), C32(H32), C46(H46)
;
_shelx_res_checksum              46732
_olex2_submission_special_instructions 'No special instructions were received'