Redox induced S-S bond cleavage of 2,2'-dithiobisbenzothiazole - leading to a [2Ru-2S] core analogous to [2Fe-2S] cluster.
Dhara, Suman; Panda, Sanjib; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12408–12412; doi:10.1039/d1dt02211c

data_7707946
_publ_section_title
;
 Redox induced S-S bond cleavage of 2,2'-dithiobisbenzothiazole - leading
 to a [2Ru-2S] core analogous to [2Fe-2S] cluster.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12408
_journal_page_last               12412
_journal_paper_doi               10.1039/d1dt02211c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C44 H34 Cl N O P2 Ru S2, 2(C H2 Cl2)'
_chemical_formula_sum            'C46 H38 Cl5 N O P2 Ru S2'
_chemical_formula_weight         1025.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-10 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.332(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6447(4)
_cell_length_b                   16.6071(5)
_cell_length_c                   11.6908(3)
_cell_measurement_reflns_used    16233
_cell_measurement_temperature    152(3)
_cell_measurement_theta_max      32.3790
_cell_measurement_theta_min      2.2360
_cell_volume                     2236.96(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      152(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -10.56 149.94   0.50    6.00  81.02  -9.84  31.50    --   321
  2  \w    -81.21  26.29   0.50    6.00    --    9.90 -30.17  -6.99  215
  3  \w   -100.87  13.63   0.50    6.00    --   -9.90 -56.72  89.28  229
;
_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      0.0074509000
_diffrn_orient_matrix_UB_12      -0.0268492000
_diffrn_orient_matrix_UB_13      -0.0455378000
_diffrn_orient_matrix_UB_21      0.0376891000
_diffrn_orient_matrix_UB_22      -0.0240089000
_diffrn_orient_matrix_UB_23      0.0391854000
_diffrn_orient_matrix_UB_31      -0.0480645000
_diffrn_orient_matrix_UB_32      -0.0229934000
_diffrn_orient_matrix_UB_33      0.0122821000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22467
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.760
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69487
_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 light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.86
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.54
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 3424 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7771
_refine_ls_number_restraints     846
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0651
_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^)+(0.1035P)^2^+10.1723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1805
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                7638
_reflns_number_total             7771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02211c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7707944--7707946.cif.'
_cod_database_code               7707946
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30O1Cl1Ru1P2S2
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.528
_reflns_odcompleteness_completeness 86.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C46(H46A,H46B)
5.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C22(H22), C43(H43), C40(H40), C42(H42), C23(H23), C24(H24),
 C25(H25), C38(H38), C14(H14), C16(H16), C10(H10), C18(H18), C19(H19), C41(H41),
  C44(H44), C20(H20), C34(H34), C3(H3), C36(H36), C6(H6), C35(H35), C28(H28),
 C32(H32), C37(H37), C4(H4), C30(H30), C29(H29), C17(H17), C12(H12), C11(H11),
 C5(H5), C13(H13), C31(H31)
;
_shelx_res_checksum              74106
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.231
_oxdiff_exptl_absorpt_empirical_full_min 0.805