Synthesis and diverse crystal packing in o-, m- and p-bis(carbonylthioureido)benzenes containing bisferrocenes.
Duan, Xin E.; Jiang, Ze Jin; Tong, Hong Bo; Bai, Sheng Di; Acta crystallographica. Section C, Structural chemistry 81 (2025) –; doi:10.1107/S2053229625000282

data_2312739
_publ_section_title
;
 Synthesis and diverse crystal packing in o-, m- and
 p-bis(carbonylthioureido)benzenes containing bisferrocenes.
;
_journal_coeditor_code           QF3066
_journal_issue                   2
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229625000282
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          '[Fe2 (C5 H5)2 (C20 H16 N4 O2 S2)], C3 H6 O'
_chemical_formula_moiety         'C30 H26 Fe2 N4 O2 S2, C3 H6 O'
_chemical_formula_sum            'C33 H32 Fe2 N4 O3 S2'
_chemical_formula_weight         708.44
_chemical_melting_point_gt       463
_chemical_melting_point_lt       464
_chemical_name_systematic
;
3,3'-Bis(ferrocenylcarbonyl)-1,1'-(benzene-1,2-diyl)bis(thiourea)
acetone monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.6983(6)
_cell_length_b                   21.8868(11)
_cell_length_c                   22.6831(12)
_cell_measurement_reflns_used    9049
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.265
_cell_measurement_theta_min      2.582
_cell_volume                     6304.2(5)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62236
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.324
_diffrn_reflns_theta_min         2.616
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0357P)^2^+3.6860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                6551
_reflns_number_total             7854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qf3066sup1.cif
_cod_data_source_block           1
_cod_database_code               2312739
_shelx_estimated_absorpt_t_min   0.735
_shelx_estimated_absorpt_t_max   0.811
_shelx_hkl_checksum              29577
_shelx_res_checksum              64899
_cod_database_fobs_code 2312739