Hydrogen Bonds Seal Single-Molecule Capsules
Jerry L. Atwood; Agnieszka Szumna; Journal of the American Chemical Society 124 (2002) 10646–10647; doi:10.1021/ja027191l

data_4115127
_publ_section_title
;
 Hydrogen Bonds Seal Single-Molecule Capsules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10646
_journal_page_last               10647
_journal_paper_doi               10.1021/ja027191l
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C91 H101 Cl16 N10 O14'
_chemical_formula_weight         2126.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.002(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.299(3)
_cell_length_b                   24.192(4)
_cell_length_c                   23.679(4)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    173(2)
_cell_volume                     9850(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    XSeed
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61879
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_F_000             4404
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.383
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1221
_refine_ls_number_reflns         21683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          2.218
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+12.4485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2286
_reflns_number_gt                12444
_reflns_number_total             21683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027191l_s1_1.cif
_cod_data_source_block           4xTMACl(I)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4115127