New Chiral Cyclohexylhemicucurbit[6]uril
Aav, Riina; Shmatova, Elena; Reile, Indrek; Borissova, Maria; Topić, Filip; Rissanen, Kari; Organic Letters 15 (2013) 3786–; doi:10.1021/ol401766a

data_1512214
_publ_section_title
;
 New Chiral Cyclohexylhemicucurbit[6]uril
;
_journal_issue                   14
_journal_name_full               'Organic Letters'
_journal_page_first              3786
_journal_paper_doi               10.1021/ol401766a
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C48 H72 N12 O6), 7(C Cl4)'
_chemical_formula_sum            'C103 H144 Cl28 N24 O12'
_chemical_formula_weight         2903.01
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.62503(15)
_cell_length_b                   17.42571(16)
_cell_length_c                   94.3127(10)
_cell_measurement_reflns_used    11260
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      71.2919
_cell_measurement_theta_min      3.2775
_cell_volume                     27322.7(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis 2007)'
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       113
_diffrn_reflns_limit_l_min       -112
_diffrn_reflns_number            26058
_diffrn_reflns_point_group_measured_fraction_full 0.750
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.743
_diffrn_reflns_theta_min         4.689
_exptl_absorpt_coefficient_mu    5.621
_exptl_absorpt_correction_T_max  0.596
_exptl_absorpt_correction_T_min  0.266
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.36.21
(release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)
Numerical absorption correction based on gaussian integration over a
multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12016
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.105
_refine_diff_density_max         1.785
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 4824 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.042(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1775
_refine_ls_number_reflns         18553
_refine_ls_number_restraints     3370
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0847
_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^)+(0.0581P)^2^+388.2816P+0.0100sin\q]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2162
_reflns_Friedel_coverage         0.430
_reflns_Friedel_fraction_full    0.489
_reflns_Friedel_fraction_max     0.489
_reflns_number_gt                17287
_reflns_number_total             18553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol401766a_si_002.cif
_cod_data_source_block           aav1c
_cod_database_code               1512214
_shelx_estimated_absorpt_t_min   0.259
_shelx_estimated_absorpt_t_max   0.590
_shelxl_version_number           2012-9
_shelx_res_checksum              8426
_shelx_hkl_checksum              68055