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_2312655
_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) (C26 H23 O3 S3)]'
_chemical_formula_moiety         'C31 H28 Fe O3 S3'
_chemical_formula_sum            'C31 H28 Fe O3 S3'
_chemical_formula_weight         600.56
_chemical_name_systematic
;
1,2,3-Tris[(4-methylbenzene)sulfinyl]ferrocene
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                93.379(2)
_cell_angle_beta                 91.120(2)
_cell_angle_gamma                98.051(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8298(5)
_cell_length_b                   9.8573(6)
_cell_length_c                   17.4937(11)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.7546
_cell_measurement_theta_min      2.6283
_cell_volume                     1334.02(14)
_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
;
SHELXT2014 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21012
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.761
_diffrn_reflns_theta_min         3.229
_diffrn_source                   'rotating anode generator'
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.297
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4237 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         10957
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                9889
_reflns_number_total             10957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ux3008.cif
_cod_data_source_block           comp_3a
_cod_depositor_comments
'Adding full bibliography for 2312653--2312658.cif.'
_cod_database_code               2312655
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              68839
_shelx_res_checksum              9441