Thermodynamically Controlled Synthesis of a Chiral Tetra-cavitand Nanocapsule and Mechanism of Enantiomerization.
Junling Sun; James L. Bennett; Thomas J. Emge; Ralf Warmuth; Journal of the American Chemical Society 133 (2011) 3268–3271; doi:10.1021/ja110475w

data_4105750
_publ_section_title
;
 Thermodynamically Controlled Synthesis of a Chiral Tetra-cavitand
 Nanocapsule and Mechanism of Enantiomerization.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3268
_journal_page_last               3271
_journal_paper_doi               10.1021/ja110475w
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C272 H352 N16 O32, 9(C H CL3), 4.5(C H4 O)'
_chemical_formula_sum            'C285.5 H373 Cl27 N16 O36.5'
_chemical_formula_weight         5570.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.593(1)
_cell_angle_beta                 87.137(1)
_cell_angle_gamma                64.968(1)
_cell_formula_units_Z            2
_cell_length_a                   19.4713(12)
_cell_length_b                   21.8175(13)
_cell_length_c                   38.491(2)
_cell_measurement_reflns_used    8587
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.88
_cell_measurement_theta_min      2.30
_cell_volume                     14454.2(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            105126
_diffrn_reflns_theta_full        23.90
_diffrn_reflns_theta_max         23.90
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       lathe
_exptl_crystal_F_000             5898
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.852
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.435
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3757
_refine_ls_number_reflns         44634
_refine_ls_number_restraints     6604
_refine_ls_restrained_S_all      1.405
_refine_ls_R_factor_all          0.1671
_refine_ls_R_factor_gt           0.1240
_refine_ls_shift/su_max          0.159
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3483
_refine_ls_wR_factor_ref         0.3855
_reflns_number_gt                28708
_reflns_number_total             44634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja110475w_si_001.cif
_cod_data_source_block           tetramer
_cod_original_formula_sum        'C285.50 H373 Cl27 N16 O36.50'
_cod_database_code               4105750