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_4115128
_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            'C82 H100 Cl2.39 N9 O14'
_chemical_formula_weight         1520.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 100.137(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.171(2)
_cell_length_b                   20.108(3)
_cell_length_c                   15.371(2)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    173(2)
_cell_volume                     4007.3(10)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0936
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19266
_diffrn_reflns_theta_full        24.04
_diffrn_reflns_theta_max         24.04
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       plate
_exptl_crystal_F_000             1615
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6285
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1799
_refine_ls_R_factor_gt           0.0926
_refine_ls_shift/su_max          0.924
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1952P)^2^+3.7489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2594
_refine_ls_wR_factor_ref         0.3359
_reflns_number_gt                3142
_reflns_number_total             6285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027191l_s1_2.cif
_cod_data_source_block           4xTMACl(II)
_cod_original_cell_volume        4007.4(10)
_cod_database_code               4115128