#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:00:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178929 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/58/4115892.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4115892
loop_
_publ_author_name
'Jaheon Kim'
'In-Sun Jung'
'Soo-Young Kim'
'Eunsung Lee'
'Jin-Koo Kang'
'Shigeru Sakamoto'
'Kentaro Yamaguchi'
'Kimoon Kim'
_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            'C30 H38 N20 O14'
_chemical_formula_weight         902.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2314(8)
_cell_length_b                   18.8133(12)
_cell_length_c                   14.0361(9)
_cell_measurement_reflns_used    6105
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      24.10
_cell_measurement_theta_min      1.81
_cell_volume                     3494.0(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13435
_diffrn_reflns_theta_full        24.10
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         2855
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0447P)²+7.0174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                2286
_reflns_number_total             2855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993376p_2.cif
_cod_data_source_block           CB[5]
_cod_database_code               4115892
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O1 O -0.50793(17) 0.65429(12) 0.45488(16) 0.0281(6) Uani 1 1 d .
O2 O -0.35339(17) 0.59624(12) 0.29941(16) 0.0274(5) Uani 1 1 d .
O3 O -0.2633(2) 0.7500 0.2253(3) 0.0348(9) Uani 1 2 d S
O4 O -0.16409(17) 0.66319(13) 0.75227(19) 0.0378(6) Uani 1 1 d .
O5 O -0.00638(16) 0.60971(12) 0.59633(15) 0.0259(5) Uani 1 1 d .
O6 O 0.1154(2) 0.7500 0.4875(2) 0.0231(7) Uani 1 2 d S
N1 N -0.46474(19) 0.68550(13) 0.60909(18) 0.0211(6) Uani 1 1 d .
N2 N -0.41156(19) 0.58155(14) 0.55217(19) 0.0230(6) Uani 1 1 d .
N3 N -0.28540(18) 0.54634(14) 0.43519(19) 0.0217(6) Uani 1 1 d .
N4 N -0.18141(19) 0.57793(13) 0.31751(18) 0.0194(6) Uani 1 1 d .
N5 N -0.11417(18) 0.69087(13) 0.26028(19) 0.0193(6) Uani 1 1 d .
N6 N -0.33543(19) 0.68535(14) 0.73469(19) 0.0230(6) Uani 1 1 d .
N7 N -0.26849(19) 0.59024(14) 0.66413(19) 0.0243(6) Uani 1 1 d .
N8 N -0.14601(19) 0.54361(13) 0.55089(18) 0.0210(6) Uani 1 1 d .
N9 N -0.04684(18) 0.58959(13) 0.43832(18) 0.0186(6) Uani 1 1 d .
N10 N 0.03383(18) 0.69120(13) 0.36455(18) 0.0190(6) Uani 1 1 d .
C1 C -0.4648(2) 0.64300(16) 0.5301(2) 0.0201(7) Uani 1 1 d .
C2 C -0.3816(2) 0.53059(16) 0.4806(2) 0.0215(7) Uani 1 1 d .
H2A H -0.4347 0.5285 0.4310 0.026 Uiso 1 1 calc R
H2B H -0.3773 0.4830 0.5105 0.026 Uiso 1 1 calc R
C3 C -0.2808(2) 0.57675(15) 0.3462(2) 0.0200(7) Uani 1 1 d .
C4 C -0.1491(2) 0.62029(15) 0.2359(2) 0.0200(7) Uani 1 1 d .
H4A H -0.0940 0.5948 0.2027 0.024 Uiso 1 1 calc R
H4B H -0.2064 0.6246 0.1909 0.024 Uiso 1 1 calc R
C5 C -0.1741(3) 0.7500 0.2464(3) 0.0215(10) Uani 1 2 d S
C6 C -0.5249(3) 0.7500 0.6154(3) 0.0223(10) Uani 1 2 d S
H6A H -0.5754 0.7500 0.5633 0.027 Uiso 1 2 calc SR
H6B H -0.5622 0.7500 0.6765 0.027 Uiso 1 2 calc SR
C7 C -0.4223(2) 0.65070(16) 0.6926(2) 0.0202(7) Uani 1 1 d .
H7A H -0.4754 0.6401 0.7412 0.024 Uiso 1 1 calc R
C8 C -0.3764(2) 0.58113(16) 0.6498(2) 0.0203(7) Uani 1 1 d .
H8A H -0.4018 0.5383 0.6845 0.024 Uiso 1 1 calc R
C9 C -0.1890(2) 0.51590(16) 0.4635(2) 0.0190(7) Uani 1 1 d .
H9A H -0.1916 0.4628 0.4641 0.023 Uiso 1 1 calc R
C10 C -0.1147(2) 0.54396(15) 0.3851(2) 0.0180(7) Uani 1 1 d .
H10A H -0.0771 0.5039 0.3547 0.022 Uiso 1 1 calc R
C11 C -0.0082(2) 0.70874(15) 0.2715(2) 0.0178(7) Uani 1 1 d .
H11A H 0.0338 0.6890 0.2185 0.021 Uiso 1 1 calc R
C12 C -0.2473(2) 0.64888(18) 0.7208(2) 0.0251(8) Uani 1 1 d .
C13 C -0.1924(2) 0.53740(16) 0.6439(2) 0.0210(7) Uani 1 1 d .
H13A H -0.2235 0.4897 0.6494 0.025 Uiso 1 1 calc R
H13B H -0.1388 0.5408 0.6930 0.025 Uiso 1 1 calc R
C14 C -0.0610(2) 0.58500(16) 0.5351(2) 0.0189(7) Uani 1 1 d .
C15 C 0.0459(2) 0.61944(16) 0.3987(2) 0.0205(7) Uani 1 1 d .
H15A H 0.0990 0.6188 0.4483 0.025 Uiso 1 1 calc R
H15B H 0.0689 0.5890 0.3454 0.025 Uiso 1 1 calc R
C16 C 0.0651(3) 0.7500 0.4134(3) 0.0197(10) Uani 1 2 d S
C17 C -0.3395(4) 0.7500 0.7913(3) 0.0248(10) Uani 1 2 d S
H17A H -0.2822 0.7500 0.8367 0.030 Uiso 1 2 calc SR
H17B H -0.4028 0.7500 0.8289 0.030 Uiso 1 2 calc SR
O3W O 0.2773(2) 0.64444(14) 0.4921(2) 0.0483(8) Uani 1 1 d D
O1W O -0.1284(9) 0.7500 0.5589(7) 0.185(5) Uani 1 2 d S
O2W O -0.2833(10) 0.7500 0.4565(9) 0.283(8) Uani 1 2 d S
H1W H 0.235(8) 0.678(5) 0.498(10) 0.339 Uiso 1 1 d D
H2W H 0.334(5) 0.664(7) 0.498(11) 0.339 Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 N1 C6 122.5(3) . .
C1 N1 C7 113.0(2) . .
C6 N1 C7 122.6(3) . .
C1 N2 C2 122.5(3) . .
C1 N2 C8 112.3(3) . .
C2 N2 C8 124.5(3) . .
C3 N3 C2 121.5(3) . .
C3 N3 C9 111.9(2) . .
C2 N3 C9 124.6(2) . .
C3 N4 C10 112.6(2) . .
C3 N4 C4 121.2(3) . .
C10 N4 C4 125.3(2) . .
C5 N5 C4 121.5(3) . .
C5 N5 C11 112.6(3) . .
C4 N5 C11 123.2(2) . .
C12 N6 C7 113.1(3) . .
C12 N6 C17 122.0(3) . .
C7 N6 C17 124.8(3) . .
C12 N7 C13 121.2(3) . .
C12 N7 C8 111.8(3) . .
C13 N7 C8 125.3(3) . .
C14 N8 C13 122.2(3) . .
C14 N8 C9 112.6(2) . .
C13 N8 C9 124.7(2) . .
C14 N9 C10 112.8(2) . .
C14 N9 C15 121.0(3) . .
C10 N9 C15 123.5(2) . .
C16 N10 C15 123.9(3) . .
C16 N10 C11 112.5(3) . .
C15 N10 C11 123.5(2) . .
O1 C1 N1 126.9(3) . .
O1 C1 N2 125.2(3) . .
N1 C1 N2 107.8(3) . .
N2 C2 N3 114.2(3) . .
O2 C3 N3 125.4(3) . .
O2 C3 N4 126.2(3) . .
N3 C3 N4 108.4(3) . .
N5 C4 N4 114.2(2) . .
O3 C5 N5 126.29(18) . .
O3 C5 N5 126.29(18) . 7_575
N5 C5 N5 107.4(4) . 7_575
N1 C6 N1 113.1(3) 7_575 .
N6 C7 N1 115.7(3) . .
N6 C7 C8 103.1(2) . .
N1 C7 C8 102.6(2) . .
N2 C8 N7 116.5(3) . .
N2 C8 C7 103.6(2) . .
N7 C8 C7 103.3(2) . .
N8 C9 N3 115.7(3) . .
N8 C9 C10 103.2(2) . .
N3 C9 C10 103.1(2) . .
N4 C10 N9 117.1(2) . .
N4 C10 C9 103.2(2) . .
N9 C10 C9 103.1(2) . .
N5 C11 N10 114.4(2) . .
N5 C11 C11 103.40(15) . 7_575
N10 C11 C11 103.09(15) . 7_575
O4 C12 N6 127.5(3) . .
O4 C12 N7 124.5(3) . .
N6 C12 N7 107.9(3) . .
N7 C13 N8 114.7(3) . .
O5 C14 N9 126.5(3) . .
O5 C14 N8 125.8(3) . .
N9 C14 N8 107.7(3) . .
N10 C15 N9 113.2(2) . .
O6 C16 N10 125.88(18) . .
O6 C16 N10 125.88(18) . 7_575
N10 C16 N10 108.2(4) . 7_575
N6 C17 N6 113.6(4) . 7_575
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.218(4) .
O2 C3 1.220(4) .
O3 C5 1.216(5) .
O4 C12 1.216(4) .
O5 C14 1.215(4) .
O6 C16 1.236(5) .
N1 C1 1.367(4) .
N1 C6 1.454(3) .
N1 C7 1.455(4) .
N2 C1 1.389(4) .
N2 C2 1.444(4) .
N2 C8 1.447(4) .
N3 C3 1.375(4) .
N3 C2 1.454(4) .
N3 C9 1.454(4) .
N4 C3 1.375(4) .
N4 C10 1.444(4) .
N4 C4 1.459(4) .
N5 C5 1.380(4) .
N5 C4 1.447(4) .
N5 C11 1.450(4) .
N6 C12 1.367(4) .
N6 C7 1.447(4) .
N6 C17 1.454(4) .
N7 C12 1.389(4) .
N7 C13 1.443(4) .
N7 C8 1.452(4) .
N8 C14 1.386(4) .
N8 C13 1.448(4) .
N8 C9 1.449(4) .
N9 C14 1.374(4) .
N9 C10 1.450(4) .
N9 C15 1.459(4) .
N10 C16 1.366(4) .
N10 C15 1.441(4) .
N10 C11 1.458(4) .
C5 N5 1.380(4) 7_575
C6 N1 1.454(3) 7_575
C7 C8 1.563(4) .
C9 C10 1.566(4) .
C11 C11 1.553(6) 7_575
C16 N10 1.366(4) 7_575
C17 N6 1.454(4) 7_575
