Diethyl 2,2'-(trisulfane-1,3-diyl)dibenzoate
Boukebbous, Khaled; Laifa, El Adoui; De Mallmann, Aimery; Taoufik, Mostafa; IUCrData 1 (2016) x161708–; doi:10.1107/S2414314616017089

data_1544529
_publ_section_title
;
 Diethyl 2,2'-(trisulfane-1,3-diyl)dibenzoate
;
_journal_issue                   11
_journal_name_full               IUCrData
_journal_page_first              x161708
_journal_paper_doi               10.1107/S2414314616017089
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C18 H18 O4 S3'
_chemical_formula_moiety         'C18 H18 O4 S3'
_chemical_formula_sum            'C18 H18 O4 S3'
_chemical_formula_weight         394.54
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 106.59(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.071(3)
_cell_length_b                   4.4304(11)
_cell_length_c                   27.422(9)
_cell_measurement_reflns_used    1198
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5200
_cell_measurement_theta_min      4.8540
_cell_volume                     1754.8(8)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
CRYSTALS (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_refinement
;
CRYSTALS (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku OF Xcalibur Atlas Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            6690
_diffrn_reflns_theta_full        26.515
_diffrn_reflns_theta_max         29.980
_diffrn_reflns_theta_min         3.547
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.89
_refine_diff_density_min         -1.00
_refine_ls_extinction_coef       29(8)
_refine_ls_extinction_method
;
Larson (1970), Equation 22
;
_refine_ls_goodness_of_fit_ref   0.9946
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.0002161
_refine_ls_shift/su_mean         0.0000194
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince,
1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.372E+04 0.520E+04 0.373E+04 0.166E+04 752.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1664
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                1653
_reflns_number_total             2177
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            wm4032sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               1544529
_cod_database_fobs_code          1544529