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_7062766
_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 H38 Cl N4 O P2 Ru S2, 0.8(Cl O4)'
_chemical_formula_sum            'C51 H38 Cl1.8 N4 O4.2 P2 Ru S2'
_chemical_formula_weight         1064.99
_chemical_name_systematic        C51H38Cl2N4O5P2RuS2
_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     dual
_audit_creation_date             2023-09-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-26 deposited with the CCDC.	2023-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.4970(3)
_cell_length_b                   14.2023(2)
_cell_length_c                   32.8171(5)
_cell_measurement_reflns_used    40908
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.9370
_cell_measurement_theta_min      1.6210
_cell_volume                     9087.1(2)
_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  20.08   0.80    2.00  15.81  -9.84 -59.25    --   450
  2  \w    -65.46   0.14   0.80    2.00    --  -19.34  94.56 145.16   82
  3  \w    -60.88  -0.08   0.80    2.00    --  -14.77  94.56 -34.84   76
  4  \w   -100.81  15.19   0.80    2.00    --   -9.84 -59.25 -51.92  145
  5  \w   -100.81  15.19   0.80    2.00    --   -9.84 -59.25 164.08  145
  6  \w    -65.46   0.14   0.80    2.00    --  -19.34  94.56  73.16   82
  7  \f   -349.73  10.27   0.80    2.00   6.61  -9.84 -31.50    --   450
  8  \w    -65.46   0.14   0.80    2.00    --  -19.34  94.56   1.16   82
  9  \f    -10.27 349.73   0.80    2.00  81.02  -9.84  31.50    --   450
 10  \w    -51.04   0.16   0.80    2.00    --   -4.92  94.56 -34.84   64
;
_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      0.0047685000
_diffrn_orient_matrix_UB_12      0.0279876000
_diffrn_orient_matrix_UB_13      -0.0176828000
_diffrn_orient_matrix_UB_21      0.0355551000
_diffrn_orient_matrix_UB_22      0.0032448000
_diffrn_orient_matrix_UB_23      0.0043387000
_diffrn_orient_matrix_UB_31      0.0060245000
_diffrn_orient_matrix_UB_32      -0.0412475000
_diffrn_orient_matrix_UB_33      -0.0116443000
_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  0.1580
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            390312
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.622
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45731
_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 pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       needle
_exptl_crystal_F_000             4338
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0421P)^2^+17.3334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6682
_reflns_number_total             8003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04221a2.cif
_cod_data_source_block           '[1]ClO4'
_cod_depositor_comments
'Adding full bibliography for 7062764--7062766.cif.'
_cod_original_formula_sum        'C51 H38 Cl1.80 N4 O4.20 P2 Ru S2'
_cod_database_code               7062766
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.924
_reflns_odcompleteness_completeness 89.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.91
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Cl2(0.8) O3(0.8) O2(0.8) O4(0.8) O5(0.8)
3.a Aromatic/amide H refined with riding coordinates:
 C45(H45), C7(H7), C44(H44), C47(H47), C51(H51), C39(H39), C11(H11), C12(H12),
 C37(H37), C38(H38), C48(H48), C17(H17), C6(H6), C41(H41), C13(H13), C14(H14),
 C30(H30), C5(H5), C49(H49), C4(H4), C33(H33), C50(H50), C21(H21), C43(H43),
 C27(H27), C29(H29), C36(H36), C35(H35), C26(H26), C31(H31), C18(H18), C23(H23),
  C20(H20), C42(H42), C32(H32), C19(H19), C25(H25), C24(H24)
;
_shelx_res_checksum              71184
_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 1.595
_oxdiff_exptl_absorpt_empirical_full_min 0.526