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_7719322
_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         'C20 H18 Fe2 O4 S2'
_chemical_formula_sum            'C20 H18 Fe2 O4 S2'
_chemical_formula_weight         498.16
_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
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                114.8730(10)
_cell_angle_beta                 100.4090(10)
_cell_angle_gamma                96.4530(10)
_cell_formula_units_Z            2
_cell_length_a                   6.8958(2)
_cell_length_b                   12.3838(4)
_cell_length_c                   12.7343(4)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      3.15
_cell_volume                     948.48(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II with Photon 100 CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54441
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.562
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'Incoatec IuS'
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0225P)^2^+0.4503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5283
_reflns_number_total             5696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01691f2.cif
_cod_data_source_block           cmpnd3
_cod_depositor_comments
'Adding full bibliography for 7719321--7719327.cif.'
_cod_database_code               7719322
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.843
_exptl_absorpt_special_details
;
SADABS 2016/2 Bruker AXS, Madison WI, USA
;
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C18(H18), C3(H3), C15(H15), C20(H20), C14(H14), C19(H19), C13(H13),
 C17(H17), C12(H12), C16(H16), C11(H11)
1.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              37976