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_7710196
_publ_section_title
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 Diruthenium and triruthenium compounds of potential redox active
 non-chelated &#xF068;1-N,&#xF068;1-N-benzothiadiazole bridge
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00533F
_journal_year                    2022
_chemical_formula_moiety         'C30 H38 N4 O8 Ru2 S, Cl O4, 1[H2O], 1[H2O]'
_chemical_formula_sum            'C30 H42 Cl N4 O14 Ru2 S'
_chemical_formula_weight         952.335
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2022-04-27
_audit_creation_method
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Olex2 1.5-dev
(compiled 2022.04.21 svn.rca3783a0 for OlexSys, GUI svn.r6444)
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_audit_update_record
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2022-05-02 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
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_cell_angle_alpha                94.487(10)
_cell_angle_beta                 104.937(9)
_cell_angle_gamma                90.671(11)
_cell_formula_units_Z            2
_cell_length_a                   12.479(4)
_cell_length_b                   12.682(4)
_cell_length_c                   12.995(3)
_cell_measurement_reflns_used    32813
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.30
_cell_volume                     1979.9(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.9915
_diffrn_measured_fraction_theta_max 0.9915
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.9915
_diffrn_reflns_Laue_measured_fraction_max 0.9915
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            86977
_diffrn_reflns_point_group_measured_fraction_full 0.9915
_diffrn_reflns_point_group_measured_fraction_max 0.9915
_diffrn_reflns_theta_full        25.1425
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1321 before and 0.0730 after correction.
The Ratio of minimum to maximum transmission is 0.8823.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             962.206
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.7094
_refine_diff_density_min         -0.3958
_refine_diff_density_rms         0.0784
_refine_ls_d_res_high            0.8364
_refine_ls_d_res_low             9.2900
_refine_ls_goodness_of_fit_ref   1.1047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    57
_refine_ls_number_parameters     507
_refine_ls_number_reflns         7018
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.0948
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          -0.0017
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+2.7932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                6232
_reflns_number_total             7018
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt00533f2.cif
_cod_data_source_block           1clo4
_cod_database_code               7710196
_olex2_refinement_description
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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
 Cl2-O9 = Cl2-O10 = Cl2-O11 = Cl2-O12
 1.5 with sigma of 0.02
 O11-O12 \\sim O11A-O12A
 with sigma of 0.04
 Cl2-O9 \\sim Cl2-O10 \\sim Cl2-O11 \\sim Cl2-O12
 with sigma of 0.02
 O10-O11 \\sim O10A-O11A
 with sigma of 0.04
 O9-O11 \\sim O9A-O11A
 with sigma of 0.04
 O9-O11 \\sim O10-O12 \\sim O9-O12 \\sim O10-O11 \\sim O9-O10 \\sim O11-O12
 with sigma of 0.04
 Cl2-O9 \\sim Cl2A-O9A
 with sigma of 0.02
 Cl2-O10 \\sim Cl2A-O10A
 with sigma of 0.02
 Cl2-O11 \\sim Cl2A-O11A
 with sigma of 0.02
 Cl2-O12 \\sim Cl2A-O12A
 with sigma of 0.02
 O9-O10 \\sim O9A-O10A
 with sigma of 0.04
 O9-O12 \\sim O9A-O12A
 with sigma of 0.04
 O10-O12 \\sim O10A-O12A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim O9 \\sim O10 \\sim O11 \\sim O12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 Cl2, O9, O10, O11, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2A, O9A, O10A, O11A, O12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl2A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=1-FVAR(1)
 Sof(Cl2)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C21(H21), C4(H4), C14(H14), C9(H9), C26(H26)
6.b Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C16(H16a,H16b,H16c), C24(H24a,H24b,H24c), C30(H30a,H30b,
 H30c), C18(H18a,H18b,H18c), C28(H28a,H28b,H28c), C23(H23a,H23b,H23c), C19(H19a,
 H19b,H19c), C7(H7a,H7b,H7c), C11(H11a,H11b,H11c)
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_smtbx_masks_special_details
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A solvent mask was calculated and 40 electrons were 
found in a volume of 166\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1[H2O], 1[H2O] per Formula Unit 
which account for 40 electrons per unit cell.
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_olex2_submission_special_instructions 'No special instructions were received'