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_4115891
_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            'C80 H144 Cl2 N40 O50 S'
_chemical_formula_weight         2569.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.9620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8327(3)
_cell_length_b                   18.5925(2)
_cell_length_c                   22.4398(6)
_cell_measurement_reflns_used    5786
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      24.08
_cell_measurement_theta_min      1.85
_cell_volume                     5700.7(2)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'omega and phi scana'
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22492
_diffrn_reflns_theta_full        24.08
_diffrn_reflns_theta_max         24.08
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             2708
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.723
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0048(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         8887
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.1023
_refine_ls_shift/su_max          0.536
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1808P)^2^+11.3868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2811
_refine_ls_wR_factor_ref         0.3113
_reflns_number_gt                6744
_reflns_number_total             8887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993376p_1.cif
_cod_data_source_block           2
_cod_database_code               4115891