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_7719327
_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), 0.5[C6H14], 0.5[C6H14]'
_chemical_formula_sum            'C26 H26 Mo2 O4 S4'
_chemical_formula_weight         722.59
_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                112.2790(10)
_cell_angle_beta                 113.8440(10)
_cell_angle_gamma                90.8890(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7679(3)
_cell_length_b                   11.8647(3)
_cell_length_c                   14.0768(4)
_cell_measurement_reflns_used    8742
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      3.19
_cell_volume                     1630.08(8)
_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      170.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0795
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58464
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_min         1.893
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1073 before and 0.0726 after correction.
The Ratio of minimum to maximum transmission is 0.8482.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         8093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0274P)^2^+0.8008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6492
_reflns_number_total             8093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01691f2.cif
_cod_data_source_block           mo_me122m_0m
_cod_depositor_comments
'Adding full bibliography for 7719321--7719327.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7719327
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.795
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16), C22(H22), C11(H11), C13(H13), C24(H24), C19(H19), C6(H6),
 C25(H25), C12(H12), C23(H23), C9(H9), C26(H26), C10(H10)
1.b 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              91063
_shelx_fab_checksum              22343
_olex2_submission_special_instructions 'No special instructions were received'