Single crystal X-ray structure determination and temperature-dependent structural studies of the smectogenic compound 7OS5
Deptuch, Aleksandra; Jaworska-Gołab, Teresa; Kusz, Joachim; Ksiażek, Maria; Nagao, Keigo; Matsumoto, Takashi; Yamano, Akihito; Ossowska-Chruściel, Mirosława D.; Chruściel, Janusz; Marzec, Monika; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620014481

data_2108721
_publ_section_title
;
 Single crystal X-ray structure determination and temperature-dependent
 structural studies of the smectogenic compound 7OS5
;
_journal_coeditor_code           DK5101
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620014481
_journal_volume                  76
_journal_year                    2020
_chemical_formula_moiety         'C25 H34 O2 S'
_chemical_formula_sum            'C25 H34 O2 S'
_chemical_formula_weight         398.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   54.285(5)
_cell_length_b                   5.5843(3)
_cell_length_c                   14.8411(10)
_cell_measurement_reflns_used    5154
_cell_measurement_temperature    90(1)
_cell_measurement_theta_max      72.5200
_cell_measurement_theta_min      3.1830
_cell_volume                     4499.0(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28c 
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28c 
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28c 
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90(1)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34886
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.050
_diffrn_reflns_theta_min         3.256
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28c 
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       needle
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.53(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.1150
_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^)+(0.0856P)^2^+26.8267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2656
_refine_ls_wR_factor_ref         0.2987
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                5907
_reflns_number_total             8461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dk5101sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4499.0(5)
_cod_database_code               2108721
_cod_database_fobs_code          2108721
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.619
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              37382
_shelx_hkl_checksum              45712