High-resolution X-ray diffraction determination of the electron density of 1-(8-PhSC10H6)SS(C10H6SPh-8′)-1′ with the QTAIM approach: evidence for S4 σ(4c–6e) at the naphthalene peri-positions
Tsubomoto, Yutaka; Hayashi, Satoko; Nakanishi, Waro; Mapp, Lucy K.; Coles, Simon J.; RSC Advances 8 (2018) 9651–; doi:10.1039/C7RA13636F

data_7230263
_publ_section_title
;
 High-resolution X-ray diffraction determination of the electron density
 of 1-(8-PhSC10H6)SS(C10H6SPh-8&#x2032;)-1&#x2032; with the QTAIM
 approach: evidence for S4 \s(4c--6e) at the naphthalene peri-positions
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              9651
_journal_paper_doi               10.1039/C7RA13636F
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C32 H22 S4'
_chemical_formula_sum            'C32 H22 S4'
_chemical_formula_weight         534.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_update_record
;
2017-12-20 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.471(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4959(5)
_cell_length_b                   23.8566(11)
_cell_length_c                   10.3499(5)
_cell_measurement_reflns_used    245978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      1.9310
_cell_measurement_theta_min      61.9040
_cell_volume                     2485.2(2)
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            579910
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_max         60.085
_diffrn_reflns_theta_min         1.707
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.49414
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1076
_refine_ls_number_reflns         35199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.02
_refine_ls_R_factor_gt           0.016
_refine_ls_shift/su_max          0.611758E-11
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
        calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.023
_reflns_number_gt                34342
_reflns_number_total             37520
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c7ra13636f2.cif
_cod_data_source_block           1
_cod_database_code               7230263