Oxidative addition chemistry of bis(4,5-dimethoxybenzo)-1,2,5,6-tetrathiocin with cyclopentadienyl metal carbonyl complexes and the mechanochemical transformation of CpCo(dmobdt) to [CpCo(dmobdt)]<sub>2</sub>.
El Rayes, Mary; Cutler, Daniel J.; Watanabe, Lara K.; Stephaniuk, Nadia T.; Hayward, John J.; D'Agostino, Mike; Macdonald, Charles L. B.; Pilkington, Melanie; Rawson, Jeremy M.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16163–16169; doi:10.1039/d5dt01691f

data_7719323
_publ_section_title
;
 Oxidative addition chemistry of
 bis(4,5-dimethoxybenzo)-1,2,5,6-tetrathiocin with cyclopentadienyl metal
 carbonyl complexes and the mechanochemical transformation of CpCo(dmobdt)
 to [CpCo(dmobdt)]<sub>2</sub>.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16163
_journal_page_last               16169
_journal_paper_doi               10.1039/d5dt01691f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C13 H13 Mo O2 S2), 2(C H Cl3)'
_chemical_formula_sum            'C28 H28 Cl6 Mo2 O4 S4'
_chemical_formula_weight         961.32
_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             2025-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                69.1010(10)
_cell_angle_beta                 78.2720(10)
_cell_angle_gamma                77.0780(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5225(4)
_cell_length_b                   13.8503(5)
_cell_length_c                   14.7916(6)
_cell_measurement_reflns_used    9235
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.83
_cell_volume                     1759.94(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            81432
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_min         2.495
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0698 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.9014.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.313
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+2.9696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7886
_reflns_number_total             8565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01691f2.cif
_cod_data_source_block           mo_me_120_chloroform_0m
_cod_depositor_comments
'Adding full bibliography for 7719321--7719327.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7719323
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.762
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C27(H27), C28(H28)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16), C6(H6), C11(H11), C25(H25), C19(H19), C13(H13), C10(H10),
 C12(H12), C26(H26), C9(H9), C22(H22), C23(H23), C24(H24)
1.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              93595
_olex2_submission_special_instructions 'No special instructions were received'