Bile Acid-Based Cage Compounds with Lipophilic Outer Shells and Inner Cavities
Bai, Xinyan; Barnes, Charles; Pascal, Jr, Robert A.; Chen, Xueyi; Dias, Jerry Ray; Organic Letters 13 (2011) 3064–3067; doi:10.1021/ol200953h

data_1502210
_publ_section_title
;
 Bile Acid-Based Cage Compounds with Lipophilic Outer Shells and Inner
 Cavities
;
_journal_coden_ASTM              ORLEF7
_journal_issue                   12
_journal_name_full               'Organic Letters'
_journal_page_first              3064
_journal_page_last               3067
_journal_paper_doi               10.1021/ol200953h
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_formula_moiety         '2(C56 H84 O8), C H2 Cl2, 3(C H4 O)'
_chemical_formula_sum            'C56 H84 O8'
_chemical_formula_weight         1951.52
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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                96.611(4)
_cell_angle_beta                 116.223(3)
_cell_angle_gamma                108.050(4)
_cell_formula_units_Z            2
_cell_length_a                   15.090(4)
_cell_length_b                   15.095(7)
_cell_length_c                   15.132(4)
_cell_measurement_reflns_used    6930
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.6
_cell_measurement_theta_min      2.3
_cell_volume                     2808.6(17)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SUPERFLIP (Palatinus and Chapuis, J. Appl. Cryst. (2007). 40, 786-790)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23264
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method 'Evaporation from CH2Cl2 + MeOH'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1153
_refine_ls_number_reflns         8054
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1618P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2132
_reflns_number_gt                6256
_reflns_number_total             8054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol200953h_si_001.cif
_cod_data_source_block           GrubbsDimer
_cod_database_code               1502210