Ruthenium-hydride-mediated stabilisation of the azo anion radical of azobis(benzothiazole) and its reversible electron-reservoir feature
Singh, Aditi; Seikh, Liton; Dey, Sanchaita; Lahiri, Goutam Kumar; New Journal of Chemistry 47 (2023) 19428–19438; doi:10.1039/D3NJ04221A

data_7062765
_publ_section_title
;
 Ruthenium-hydride-mediated stabilisation of the azo anion radical of
 azobis(benzothiazole) and its reversible electron-reservoir feature
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19428
_journal_page_last               19438
_journal_paper_doi               10.1039/D3NJ04221A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C51 H36 Cl3 N4 O P2 Ru S2, Cl O4, 2(C2 H3 N)'
_chemical_formula_sum            'C55 H42 Cl4 N6 O5 P2 Ru S2'
_chemical_formula_weight         1235.87
_chemical_name_systematic        C55H42Cl4N6O5P2RuS2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-19 deposited with the CCDC.	2023-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                98.711(3)
_cell_angle_beta                 91.236(3)
_cell_angle_gamma                94.357(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2190(5)
_cell_length_b                   12.8734(5)
_cell_length_c                   17.3515(6)
_cell_measurement_reflns_used    18332
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.4000
_cell_measurement_theta_min      1.8680
_cell_volume                     2688.60(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -339.92  19.88   0.70    2.00  15.81  -9.84 -59.25    --   514
  2  \w    -65.46   0.34   0.70    2.00    --  -19.34  94.56 145.16   94
  3  \w    -60.89   0.01   0.70    2.00    --  -14.77  94.56 -34.84   87
  4  \w   -100.81  15.39   0.70    2.00    --   -9.84 -59.25 -51.92  166
  5  \w   -100.81  15.39   0.70    2.00    --   -9.84 -59.25 164.08  166
  6  \w    -65.46   0.34   0.70    2.00    --  -19.34  94.56  73.16   94
  7  \f   -349.53  10.27   0.70    2.00   6.61  -9.84 -31.50    --   514
  8  \w    -65.46   0.34   0.70    2.00    --  -19.34  94.56   1.16   94
  9  \f    -10.27 349.53   0.70    2.00  81.02  -9.84  31.50    --   514
 10  \w    -51.04   0.06   0.70    2.00    --   -4.92  94.56 -34.84   73
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0405168000
_diffrn_orient_matrix_UB_12      0.0280765000
_diffrn_orient_matrix_UB_13      0.0209563000
_diffrn_orient_matrix_UB_21      0.0157126000
_diffrn_orient_matrix_UB_22      -0.0198481000
_diffrn_orient_matrix_UB_23      0.0342157000
_diffrn_orient_matrix_UB_31      0.0387886000
_diffrn_orient_matrix_UB_32      0.0441017000
_diffrn_orient_matrix_UB_33      0.0101153000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            121750
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.605
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         9466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0368P)^2^+7.5639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7854
_reflns_number_total             9466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04221a2.cif
_cod_data_source_block           '[3]ClO4'
_cod_depositor_comments
'Adding full bibliography for 7062764--7062766.cif.'
_cod_database_code               7062765
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.929
_reflns_odcompleteness_completeness 80.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.87
_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 Aromatic/amide H refined with riding coordinates:
 C14(H14), C29(H29), C12(H12), C11(H11), C38(H38), C39(H39), C23(H23),
 C24(H24), C5(H5), C27(H27), C33(H33), C25(H25), C26(H26), C51(H51), C37(H37),
 C30(H30), C31(H31), C32(H32), C44(H44), C45(H45), C36(H36), C35(H35), C7(H7),
 C4(H4), C43(H43), C19(H19), C47(H47), C50(H50), C41(H41), C17(H17), C18(H18),
 C48(H48), C42(H42), C49(H49), C21(H21), C20(H20)
2.b Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              2294
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.769
_oxdiff_exptl_absorpt_empirical_full_min 0.581