Total CCl4 guest alignment in a quasiracemic clathrate closely related to Dianin’s compound
Frampton, Christopher Stephen; Gall, James H.; MacNicol, David D.; CrystEngComm  (2017) –; doi:10.1039/C7CE01275F

data_7228859
_publ_section_title
;
 Total CCl4 guest alignment in a quasiracemic clathrate closely related to
 Dianin&#x2019;s compound
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01275F
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H20 O2,C17 H18 O2,1/3(C Cl4)'
_chemical_formula_sum            'C35.33333 H38 Cl1.33333 O4'
_chemical_formula_weight         573.92
_chemical_name_common
'JACQ03 Quasiracemate, 4S-Dianins, 2S,4R nor analogue0.33 Tetrachloromethane solvate'
_chemical_name_systematic
'4S-4-p-hydroxyphenyl-2,2,4-trimethylchroman, 2S,4R-4-p-hydroxyphenyl-2,4-dimethylchroman, 0.33 Tetrachloromethane solvate'
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-04-03 deposited with the CCDC.
2017-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   26.5576(5)
_cell_length_b                   26.5576(5)
_cell_length_c                   11.1274(4)
_cell_measurement_reflns_used    9035
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      76.1340
_cell_measurement_theta_min      3.3255
_cell_volume                     6796.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2001), <i>Mercury CSD 3.5.1</i> (Macrae <i>et al</i>., 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2001), <i>Mercury CSD 3.5.1</i> (Macrae <i>et al</i>., 2008)
;
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 10.5598
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16141
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.483
_diffrn_reflns_theta_min         5.532
_exptl_absorpt_coefficient_mu    1.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2742
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CCl4'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 2554 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(6)
_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     378
_refine_ls_number_reflns         5821
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0600P)^2^+4.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.902
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                5617
_reflns_number_total             5821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01275f2.cif
_cod_data_source_block           p11028_1
_cod_depositor_comments
;

2018-12-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C106 H114 Cl4 O12'
_cod_original_formula_weight         1721.77
_cod_original_formula_moiety         '3(C18 H20 O2),3(C17 H18 O2),C Cl4'
_cod_original_formula_units_Z            3
_cod_original_cell_volume        6796.8(4)
_cod_database_code               7228859
_shelx_estimated_absorpt_t_min   0.632
_shelx_estimated_absorpt_t_max   0.786
_shelxl_version_number           2014/6
_shelx_res_checksum              52073