Unusual Chiroptical Properties of the Cryptophane-222 Skeleton.
Pitrat, Delphine; Daugey, Nicolas; Jean, Marion; Vanthuyne, Nicolas; Wien, Frank; Ducasse, Laurent; Calin, Nathalie; Buffeteau, Thierry; Brotin, Thierry; The journal of physical chemistry. B 120 (2016) 12650–12659; doi:10.1021/acs.jpcb.6b09771

data_1554047
_publ_section_title
;
 Unusual Chiroptical Properties of the Cryptophane-222 Skeleton.
;
_journal_issue                   49
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              12650
_journal_page_last               12659
_journal_paper_doi               10.1021/acs.jpcb.6b09771
_journal_volume                  120
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H42 O6'
_chemical_formula_sum            'C48 H42 O6'
_chemical_formula_weight         714.81
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.5313(7)
_cell_length_b                   11.5313(7)
_cell_length_c                   27.9387(18)
_cell_measurement_reflns_used    13268
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.9160
_cell_measurement_theta_min      4.3210
_cell_volume                     3217.3(3)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'SHELXLe  (Sheldrick, 2011)'
_computing_publication_material  'SHELXLe  (Sheldrick, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40781
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.558
_diffrn_reflns_theta_min         4.427
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense colourless'
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1134
_exptl_crystal_size_max          0.1912
_exptl_crystal_size_mid          0.1575
_exptl_crystal_size_min          0.1305
_platon_squeeze_details
;
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.168 -0.168  0.000       153        45 ' '
   2  0.000  0.168  0.333       153        46 ' '
   3  0.168  1.000  0.667       153        46 ' '
   4  0.000  0.478  0.833        75         9 ' '
   5  0.477  0.000  0.167        75         9 ' '
   6  0.522  0.522  0.500        74         9 ' '
;
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1425 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.11(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0692P)^2^+0.7633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.726
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                3568
_reflns_number_total             3816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp6b09771_si_003.cif
_cod_data_source_block           cr222-
_cod_original_cell_volume        3217.3(4)
_cod_database_code               1554047
_shelxl_version_number           2013-4
_shelx_res_checksum              78997
_shelx_hkl_checksum              55630