New Cucurbituril Homologues: Syntheses, Isolation, Characterization, and X-ray Crystal Structures of Cucurbit[n]uril (n= 5, 7, and 8)
Jaheon Kim; In-Sun Jung; Soo-Young Kim; Eunsung Lee; Jin-Koo Kang; Shigeru Sakamoto; Kentaro Yamaguchi; Kimoon Kim; Journal of the American Chemical Society 122 (2000) 540–541; doi:10.1021/ja993376p

data_4115893
_publ_contact_author
;
Kimoon Kim
National Creative Research Initiative Center
for Smart Supramolecules and Department of Chemistry,
Pohang University of Science and Technology
San 31 Hyojadong, Pohang 790-784,South Korea
;
_publ_contact_author_email       kkim@postech.ac.kr
_publ_contact_author_fax         '82 562 279 8129'
_publ_contact_author_phone       '82 562 279 2113'
_publ_section_title
;
 New Cucurbituril Homologues: Syntheses, Isolation, Characterization, and
 X-ray Crystal Structures of Cucurbit[n]uril (n= 5, 7, and 8)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              540
_journal_page_last               541
_journal_paper_doi               10.1021/ja993376p
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C46 H96 N28 O50 S4'
_chemical_formula_weight         1969.75
_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                 92.5880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8547(2)
_cell_length_b                   20.1325(2)
_cell_length_c                   31.66160(10)
_cell_measurement_reflns_used    6665
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      1.88
_cell_volume                     8185.58(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker XP in SHELXTL'
_computing_publication_material  'Bruker XCIF in SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'omega and phi 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  0.0972
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            32190
_diffrn_reflns_theta_full        24.12
_diffrn_reflns_theta_max         24.12
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       plate
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         12695
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.1116
_refine_ls_shift/su_max          0.844
_refine_ls_shift/su_mean         0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1445P)^2^+40.6198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2859
_refine_ls_wR_factor_ref         0.3226
_reflns_number_gt                8935
_reflns_number_total             12695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993376p_3.cif
_cod_data_source_block           CB[7]
_cod_database_code               4115893