Crystal structures of eight- and ten-membered cyclic bisanisylphosphonothioyl disulfanes and comparison with their <i>P</i>-ferrocenyl analogues
Przychodzeń, Witold; Chojnacki, Jarosław; Acta Crystallographica Section E 74 (2018) 212–216; doi:10.1107/S2056989018001068

data_2242361
_publ_section_title
;
 Crystal structures of eight- and ten-membered cyclic
 bisanisylphosphonothioyl disulfanes and comparison with their
 <i>P</i>-ferrocenyl analogues
;
_journal_coeditor_code           ZP2026
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              212
_journal_page_last               216
_journal_paper_doi               10.1107/S2056989018001068
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C16 H18 O4 P2 S4'
_chemical_formula_moiety         'C16 H18 O4 P2 S4'
_chemical_formula_sum            'C16 H18 O4 P2 S4'
_chemical_formula_weight         464.48
_chemical_name_systematic
2,5-Bis(4-methoxyphenyl)-1,6,3,4,2\l^5^,5\l^5^-dioxadithiadiphosphocane-2,5-dithione
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2415(3)
_cell_length_b                   7.2415(3)
_cell_length_c                   39.516(2)
_cell_measurement_reflns_used    6759
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.4367
_cell_measurement_theta_min      2.0556
_cell_volume                     2072.19(16)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2011)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '4-axis \k geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction KM-4 CCD'
_diffrn_measurement_method       '\w scans, 0.40 deg width'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            14211
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.988
_diffrn_reflns_theta_min         2.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.216
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.45(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.5163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                1839
_reflns_number_total             2019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zp2026sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        2072.2(2)
_cod_database_code               2242361
_cod_database_fobs_code          2242361
_shelx_res_checksum              25356