Molecular and crystal structures of six poly(arylsulfinyl)- and poly(arylsulfanyl)ferrocenes.
Blockhaus, Tobias; Sünkel, Karlheinz; Acta crystallographica. Section C, Structural chemistry 80 (2024) 716–727; doi:10.1107/S2053229624009318

data_2312656
_publ_section_title
;
 Molecular and crystal structures of six poly(arylsulfinyl)- and
 poly(arylsulfanyl)ferrocenes.
;
_journal_coeditor_code           UX3008
_journal_issue                   'Pt 11'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              716
_journal_page_last               727
_journal_paper_doi               10.1107/S2053229624009318
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Fe (C5 H5) (C33 H29 O4 S4)], 0.75C4 H8 O2'
_chemical_formula_moiety         'C38 H34 Fe1 O4 S4, 0.75C4 H8 O2'
_chemical_formula_sum            'C41 H40 Fe O5.5 S4'
_chemical_formula_weight         804.82
_chemical_name_systematic
;
1,2,3,4-Tetrakis[(4-methylbenzene)sulfinyl]ferrocene
ethyl acetate 0.75-solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 97.106(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8893(7)
_cell_length_b                   8.2225(4)
_cell_length_c                   36.500(2)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    107(2)
_cell_measurement_theta_max      26.2155
_cell_measurement_theta_min      2.7206
_cell_volume                     3838.6(4)
_computing_cell_refinement
;
APEX2 (Bruker, 2011)
;
_computing_data_collection
;
APEX2 (Bruker, 2011)
;
_computing_data_reduction
;
SAINT (Bruker, 2011)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      107(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            59999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'rotating anode generator'
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.558
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4943 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.053(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         15634
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+8.7247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                13598
_reflns_number_total             15634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ux3008.cif
_cod_data_source_block           comp_4
_cod_depositor_comments
'Adding full bibliography for 2312653--2312658.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C41 H40 Fe1 O5.5 S4'
_cod_database_code               2312656
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              14612
_shelx_res_checksum              85245