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_7062764
_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         'C53 H42 Cl N4 O P2 Ru S2, Cl O4, 3(C6 H6)'
_chemical_formula_sum            'C71 H60 Cl2 N4 O5 P2 Ru S2'
_chemical_formula_weight         1347.26
_chemical_name_systematic        C71H60Cl2N4O5RuS2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.9228(4)
_cell_length_b                   10.5794(2)
_cell_length_c                   18.1360(4)
_cell_measurement_reflns_used    6710
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.7680
_cell_measurement_theta_min      2.2240
_cell_volume                     3246.94(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     53.44 205.44   0.50    2.00  81.02  -9.84  31.50    --   304
  2  \w   -100.81  15.69   0.50    2.00    --   -9.84 -59.25  20.08  233
  3  \f      3.79 155.79   0.50    2.00  15.81  -9.84 -59.25    --   304
;
_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      -0.0049769000
_diffrn_orient_matrix_UB_12      -0.0053133000
_diffrn_orient_matrix_UB_13      -0.0387353000
_diffrn_orient_matrix_UB_21      0.0407834000
_diffrn_orient_matrix_UB_22      0.0127513000
_diffrn_orient_matrix_UB_23      -0.0051711000
_diffrn_orient_matrix_UB_31      0.0081910000
_diffrn_orient_matrix_UB_32      -0.0655894000
_diffrn_orient_matrix_UB_33      0.0021526000
_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  0.0755
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37392
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.646
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45292
_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    1.378
_exptl_crystal_description       plate
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 2306 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5920
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+2.2960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5340
_reflns_number_total             5920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04221a2.cif
_cod_data_source_block           '[2]ClO4'
_cod_depositor_comments
'Adding full bibliography for 7062764--7062766.cif.'
_cod_database_code               7062764
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.943
_reflns_odcompleteness_completeness 87.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.99
_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. Restrained distances
 C40-C41
 1.4 with sigma of 0.02
 C44-C43
 1.4 with sigma of 0.02
 C41-C40
 1.7 with sigma of 0.02
 C44-C39
 1.58 with sigma of 0.02
 C42-C43
 1.58 with sigma of 0.02
 C42-C41
 1.58 with sigma of 0.02
 C40-C39
 1.58 with sigma of 0.02
3. Others
 Fixed Sof: H17A(0.5) H17B(0.5) H17C(0.5) H16A(0.5) H16B(0.5) H16C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C31(H31), C22(H22), C29(H29), C21(H21), C19(H19), C25(H25),
 C23(H23), C5(H5), C28(H28), C32(H32), C35(H35), C34(H34), C37(H37), C4(H4),
 C26(H26), C11(H11), C7(H7), C12(H12), C40(H40), C33(H33), C36(H36), C14(H14),
 C27(H27), C39(H39), C44(H44), C38(H38), C41(H41), C43(H43), C42(H42)
4.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              88232
_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 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.595