Chiroptical properties of cryptophane-111
Buffeteau, Thierry; Pitrat, Delphine; Daugey, Nicolas; Calin, Nathalie; Jean, Marion; Vanthuyne, Nicolas; Ducasse, Laurent; Wien, Frank; Brotin, Thierry; Phys. Chem. Chem. Phys.  (2017) –; doi:10.1039/C7CP02045G

data_7228640
_publ_section_title
;
 Chiroptical properties of cryptophane-111
;
_journal_name_full               'Phys. Chem. Chem. Phys.'
_journal_paper_doi               10.1039/C7CP02045G
_journal_year                    2017
_chemical_formula_moiety         'C45 H36 O6, C H2 Cl2'
_chemical_formula_sum            'C46 H38 Cl2 O6'
_chemical_formula_weight         757.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-03-13 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.655(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6304(4)
_cell_length_b                   10.6493(5)
_cell_length_c                   16.3294(8)
_cell_measurement_reflns_used    11663
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.9250
_cell_measurement_theta_min      4.2480
_cell_volume                     1788.45(14)
_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 0.9932
_diffrn_measured_fraction_theta_max 0.9928
_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  0.0831
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25119
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.893
_diffrn_reflns_theta_min         4.299
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.065
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.322
_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    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             792
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.33785
_exptl_crystal_size_mid          0.2757
_exptl_crystal_size_min          0.08735
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 2497 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.010(13)
_refine_ls_extinction_coef       0.0033(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6318
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0875P)^2^+0.2755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                5850
_reflns_number_total             6318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cp02045g2.cif
_cod_data_source_block           cr111_2
_cod_database_code               7228640
_shelxl_version_number           2013-4
_shelx_res_checksum              13242
_shelx_hkl_checksum              59519