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_7710679
_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, F6 P'
_chemical_formula_sum            'C26 H34 Br2 F6 Mo P Ru S2'
_chemical_formula_weight         912.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-21 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                   28.2657(16)
_cell_length_b                   8.3531(5)
_cell_length_c                   27.0412(16)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      27.384
_cell_measurement_theta_min      2.438
_cell_volume                     6384.6(6)
_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      230.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38817
_diffrn_reflns_point_group_measured_fraction_full 0.809
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.438
_exptl_absorpt_coefficient_mu    3.602
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5882
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0923 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.7889.
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    1.899
_exptl_crystal_description       block
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.562(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         9073
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0518P)^2^+12.4120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.583
_reflns_Friedel_fraction_full    0.610
_reflns_Friedel_fraction_max     0.610
_reflns_number_gt                8010
_reflns_number_total             9073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01378a2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7710679
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.533
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.438(12)
 0.562(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 C56, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C102) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C3(H3A,H3B,H3C), C2(H2A,H2B,
 H2C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C1(H1A,
 H1B,H1C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C),
 C104(H10A,H10B,H10C), C103(H10D,H10E,H10F), C102(H10G,H10H,H10I), C101(H10J,
 H10K,H10L), C100(H10M,H10N,H10O)
5.b Aromatic/amide H refined with riding coordinates:
 C56(H56), C61(H61), C69(H69), C76(H76), C110(H110), C109(H109), C106(H106),
 C105(H105)
;
_shelx_res_checksum              44979
_olex2_submission_special_instructions 'No special instructions were received'