Sensing the chirality of various organic solvents by helically arranged π-blades.
Shimizu, Yuki; Shoji, Yoshiaki; Hashizume, Daisuke; Nagata, Yuuya; Fukushima, Takanori; Chemical communications (Cambridge, England) 54 (2018) 12314–12317; doi:10.1039/c8cc06277c

data_7122322
_publ_section_title
;
 Sensing the chirality of various organic solvents by helically arranged
 \p-blades.
;
_journal_issue                   87
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12314
_journal_page_last               12317
_journal_paper_doi               10.1039/c8cc06277c
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C138 H144 O3 Si3, C H Cl3'
_chemical_formula_sum            'C139 H145 Cl3 O3 Si3'
_chemical_formula_weight         2054.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-08-27 deposited with the CCDC.
2018-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.27587(13)
_cell_length_b                   24.1176(2)
_cell_length_c                   37.3535(3)
_cell_measurement_reflns_used    193309
_cell_measurement_temperature    90
_cell_measurement_theta_max      31.3900
_cell_measurement_theta_min      1.6710
_cell_volume                     13761.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       CrystalClear
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -60.00 120.00   0.30   64.00    --   30.00  50.00   0.00  600
  2  \w    -60.00 120.00   0.30   64.00    --   30.00  50.00  45.00  600
  3  \w    -60.00 120.00   0.30   64.00    --   30.00  50.00  90.00  600
  4  \w    -60.00 120.00   0.30   64.00    --   30.00  50.00 135.00  600
  5  \w    -60.00 120.00   0.30   64.00    --   30.00  50.00 180.00  600
  6  \w    -60.00 120.00   0.30   64.00    --   30.00  50.00 225.00  600
  7  \w    -60.00 120.00   0.30   64.00    --   30.00  50.00 270.00  600
  8  \w    -60.00 120.00   0.30   64.00    --   30.00  50.00 315.00  600
  9  \w    -60.00 120.00   0.30   64.00    --   30.00   0.00   0.00  600
;
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0087467000
_diffrn_orient_matrix_UB_12      0.0119404000
_diffrn_orient_matrix_UB_13      -0.0169815000
_diffrn_orient_matrix_UB_21      0.0186176000
_diffrn_orient_matrix_UB_22      0.0253824000
_diffrn_orient_matrix_UB_23      0.0058418000
_diffrn_orient_matrix_UB_31      0.0416253000
_diffrn_orient_matrix_UB_32      -0.0088375000
_diffrn_orient_matrix_UB_33      -0.0061739000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            404394
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.578
_diffrn_source                   'Fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.991
_exptl_crystal_description       needle
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 11821 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.054(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1449
_refine_ls_number_reflns         31595
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+3.1689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                28317
_reflns_number_total             31595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06277c2.cif
_cod_data_source_block           Helix
_cod_depositor_comments
'Adding full bibliography for 7122321--7122322.cif.'
_cod_database_code               7122322
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.996
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              68458
_shelx_fab_checksum              16432