Diruthenium and triruthenium compounds of potential redox active non-chelated 1-N,1-N-benzothiadiazole bridge
Dey, Sanchaita; Hazari, Arijit Singha; Mobin, Shaikh M.; Lahiri, Goutam Kumar; Dalton Transactions  (2022) –; doi:10.1039/D2DT00533F

data_7710197
_publ_section_title
;
 Diruthenium and triruthenium compounds of potential redox active
 non-chelated &#xF068;1-N,&#xF068;1-N-benzothiadiazole bridge
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00533F
_journal_year                    2022
_chemical_formula_moiety
'0.988(C38 H40 N6 O8 Ru2 S3), Cl O4, 0.502(C H2 Cl2), 1[CH2Cl2]'
_chemical_formula_sum            'C39.05 H42.55 Cl4.01 N6 O11.89 Ru2 S3'
_chemical_formula_weight         1226.44
_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
_audit_creation_date             2022-04-28
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.04.21 svn.rca3783a0 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-05-02 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                115.273(2)
_cell_angle_beta                 97.684(2)
_cell_angle_gamma                90.042(2)
_cell_formula_units_Z            4
_cell_length_a                   14.9761(4)
_cell_length_b                   19.0200(5)
_cell_length_c                   19.8607(3)
_cell_measurement_reflns_used    29167
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.9780
_cell_measurement_theta_min      1.6800
_cell_volume                     5059.2(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 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            208250
_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         1.655
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.932
_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 brownish violet'
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.977
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1292
_refine_ls_number_reflns         17822
_refine_ls_number_restraints     428
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0858
_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^)+(0.1078P)^2^+23.7675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2247
_refine_ls_wR_factor_ref         0.2442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12900
_reflns_number_total             17822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00533f2.cif
_cod_data_source_block           3clo4
_cod_database_code               7710197
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O11-C63
 1.296 with sigma of 0.001
 O12-C65
 1.267 with sigma of 0.001
 C60-S10B
 1.291 with sigma of 0.001
 C58-O9
 1.272 with sigma of 0.001
 C47-C48
 1.309 with sigma of 0.001
 C48-C49
 1.4 with sigma of 0.02
 O24-O23 \\sim O24A-O23A
 with sigma of 0.04
 O22-O24 \\sim O22A-O24A
 with sigma of 0.04
 Cl2-O22 \\sim Cl2A-O22A
 with sigma of 0.02
 Cl2-O21 \\sim Cl2A-O21A
 with sigma of 0.02
 O21-O24 \\sim O21A-O24A
 with sigma of 0.04
 Cl2-O24 \\sim Cl2A-O24A
 with sigma of 0.02
 Cl2-O23 \\sim Cl2A-O23A
 with sigma of 0.02
 O22-O21 \\sim O22A-O21A
 with sigma of 0.04
 O22-O23 \\sim O22A-O23A
 with sigma of 0.04
 O21-O23 \\sim O21A-O23A
 with sigma of 0.04
 O19-O20 \\sim O19A-O20A
 with sigma of 0.04
 Cl1-O20 \\sim Cl1-O20A
 with sigma of 0.04
 O19-O18 \\sim O19A-O18A
 with sigma of 0.04
 O18-O20 \\sim O18A-O20A
 with sigma of 0.04
 Cl1-O17 \\sim Cl1-O17A
 with sigma of 0.02
 Cl1-O19 \\sim Cl1-O19A
 with sigma of 0.04
 Cl1-O18 \\sim Cl1-O18A
 with sigma of 0.04
 Cl83-C83 \\sim Cl85-C83 \\sim Cl85-C84 \\sim Cl83-C84
 with sigma of 0.001
3. Rigid bond restraints
 C48, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl2A \\sim Cl2 \\sim O22 \\sim O21 \\sim O24 \\sim O23 \\sim O21A \\sim O23A
\\sim O22A \\sim O24A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Cl1 \\sim O18 \\sim O19A \\sim O18A \\sim O19 \\sim O20A \\sim O20 \\sim O17
\\sim O17A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O9 \\sim S10B \\sim C61 \\sim C58 \\sim C60 \\sim C57 \\sim C59 \\sim C79 \\sim
N77 \\sim C78 \\sim N80 \\sim C77 \\sim O9B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C48 \\sim C49: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C78 \\sim C80 \\sim CXE \\sim CXF \\sim C81 \\sim C79 \\sim N77 \\sim S10B
\\sim N80: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
5. Rigid body (RIGU) restrains
 O21, Cl2, O22, O24, O23, O23A, Cl2A, O22A, O21A, O24A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(O23A)=Sof(Cl2A)=Sof(O22A)=Sof(O21A)=Sof(O24A)=1-FVAR(1)
 Sof(Cl2)=Sof(O22)=Sof(O21)=Sof(O24)=Sof(O23)=Sof(Cl3)=Sof(Cl6)=Sof(C82)=
 Sof(H82A)=Sof(H82B)=FVAR(1)
 Sof(O17A)=Sof(O19A)=Sof(O18A)=Sof(O20A)=1-FVAR(2)
 Sof(O17)=Sof(O19)=Sof(O18)=Sof(O20)=FVAR(2)
 Sof(S10B)=Sof(N77)=Sof(N80)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(O9B)=
 Sof(C80)=Sof(H80)=Sof(C78)=Sof(C79)=Sof(C81)=Sof(H81)=Sof(CXE)=Sof(HXE)=
 Sof(CXF)=Sof(HXF)=1-FVAR(3)
 Sof(S5)=Sof(O9)=Sof(N9)=Sof(C48)=Sof(H48)=Sof(C61)=Sof(H61A)=Sof(H61B)=
 Sof(H61C)=Sof(N10)=Sof(C58)=Sof(C50)=Sof(H50)=Sof(C60)=Sof(C49)=Sof(H49)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C46)=Sof(C45)=Sof(C47)=Sof(H47)=
 Sof(C59)=Sof(H59)=Sof(O10)=FVAR(3)
 Fixed Sof: Cl83(0.4) C84(0.2) H84A(0.2) H84B(0.2) Cl85(0.4) C83(0.2)
 H83A(0.2) H83B(0.2)
7.a Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C84(H84A,H84B), C83(H83A,H83B)
7.b Me refined with riding coordinates:
 C77(H77A,H77B,H77C)
7.c Aromatic/amide H refined with riding coordinates:
 C74(H74), C12(H12), C3(H3), C26(H26), C56(H56), C4(H4), C21(H21), C69(H69),
 C6(H6), C5(H5), C18(H18), C53(H53), C11(H11), C41(H41), C54(H54), C44(H44),
 C31(H31), C43(H43), C55(H55), C42(H42), C9(H9), C10(H10), C48(H48), C64(H64),
 C15(H15), C50(H50), C36(H36), C17(H17), C49(H49), C16(H16), C47(H47), C59(H59),
  C80(H80), C81(H81), CXE(HXE), CXF(HXF)
7.d Fitted hexagon refined as free rotating group:
 C80(C78,C79,C81,CXE,CXF)
7.e Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C19(H19A,H19B,
 H19C), C33(H33A,H33B,H33C), C72(H72A,H72B,H72C), C71(H71A,H71B,H71C), C76(H76A,
 H76B,H76C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C67(H67A,H67B,H67C),
 C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C38(H38A,H38B,H38C), C66(H66A,H66B,
 H66C), C57(H57A,H57B,H57C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 177 electrons were 
found in a volume of 541\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1[CH2Cl2] per Formula Unit 
which account for 168 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7071
_shelx_fab_checksum              16474
_olex2_submission_special_instructions 'No special instructions were received'