Engineering robust polar chiral clathrate crystals
Christopher S. Frampton; Kamal A. Ketuly; A. Hamid A. Hadi; James H. Gall; David D. MacNicol; Chem.Commun. 49 (2013) 7198–; doi:10.1039/c3cc43012j

data_7109599
_publ_section_title
;
 Engineering robust polar chiral clathrate crystals
;
_journal_name_full               Chem.Commun.
_journal_page_first              7198
_journal_paper_doi               10.1039/c3cc43012j
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety
'3(C18 H20 O S),3(C18 H20 O2), (C Cl4), 0.5(H2 O)'
_chemical_formula_sum            'C109 H121 Cl4 O9.5 S3'
_chemical_formula_weight         1821.04
_chemical_name_common
;
S-Thiadianin's, R-Dianin's CCl4,H2O Quasiracemate
;
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   27.3283(4)
_cell_length_b                   27.3283(4)
_cell_length_c                   10.8327(3)
_cell_measurement_reflns_used    9616
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      75.8600
_cell_measurement_theta_min      3.2315
_cell_volume                     7006.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2001), <i>Mercury CSD 2.0</i> (Macrae <i>et al</i>., 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2001), <i>Mercury CSD 2.0</i> (Macrae <i>et al</i>., 2008)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 10.5598
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13784
_diffrn_reflns_theta_full        74.39
_diffrn_reflns_theta_max         74.39
_diffrn_reflns_theta_min         9.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2901
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.032(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6061
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                5976
_reflns_number_total             6061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43012j.txt
_cod_data_source_block           p11140
_cod_original_formula_sum        'C109 H121 Cl4 O9.50 S3'
_cod_database_code               7109599