#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:05:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178801 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/55/4105590.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_4105590
loop_
_publ_author_name
'Han-Yuan Gong'
'Brett M. Rambo'
'Elizabeth Karnas'
'Vincent M. Lynch'
'Karin M. Keller'
'Jonathan L. Sessler'
_publ_section_title
;
 Environmentally Responsive Threading, Dethreading, and Fixation of
 Anion-Induced Pseudorotaxanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1526
_journal_page_last               1533
_journal_paper_doi               10.1021/ja109102k
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C38 H34 N10 4+, 2(C8 H4 O4) 2-, 16(H2O)'
_chemical_formula_sum            'C54 H42 N10 O24'
_chemical_formula_weight         1214.98
_chemical_name_common
;
cyclo[2](2,6-di(1H-imidazol-1-yl)pyridine)[2](1,4-dimethylenebenzene) 
di-terephthalate_16 H20 
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.76(3)
_cell_angle_beta                 109.73(3)
_cell_angle_gamma                101.49(3)
_cell_formula_units_Z            1
_cell_length_a                   10.421(2)
_cell_length_b                   11.556(2)
_cell_length_c                   14.011(3)
_cell_measurement_reflns_used    5298
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.59
_cell_volume                     1511.7(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10501
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8339
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     341
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1687
_refine_ls_R_factor_gt           0.1062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0750P)²+6.1468P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2257
_refine_ls_wR_factor_ref         0.2814
_reflns_number_gt                2930
_reflns_number_total             5298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109102k_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        1511.5(5)
_cod_database_code               4105590
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 1.1532(5) 0.7888(4) 0.8159(4) 0.0521(12) Uani 1 1 d U . .
N2 N 0.9865(4) 0.6187(4) 0.7541(3) 0.0446(11) Uani 1 1 d U . .
N3 N 1.0068(4) 0.4222(4) 0.7220(3) 0.0425(11) Uani 1 1 d U . .
N4 N 1.0482(5) 0.2347(4) 0.6865(4) 0.0497(12) Uani 1 1 d U . .
N5 N 1.2516(5) 0.1978(4) 0.7058(4) 0.0516(12) Uani 1 1 d U . .
C1 C 1.2959(7) 0.8779(5) 0.8641(5) 0.0640(18) Uani 1 1 d U . .
H1A H 1.2853 0.9599 0.8719 0.077 Uiso 1 1 calc R . .
H1B H 1.3473 0.8680 0.8185 0.077 Uiso 1 1 calc R . .
C2 C 1.1287(6) 0.6683(5) 0.7963(4) 0.0458(13) Uani 1 1 d U . .
H2A H 1.1972 0.6256 0.8093 0.055 Uiso 1 1 calc R . .
C3 C 1.0254(8) 0.8176(6) 0.7867(6) 0.0696(19) Uani 1 1 d U . .
H3A H 1.0135 0.8957 0.7931 0.084 Uiso 1 1 calc R . .
C4 C 0.9204(7) 0.7128(6) 0.7473(5) 0.0638(18) Uani 1 1 d U . .
H4A H 0.8235 0.7050 0.7210 0.077 Uiso 1 1 calc R . .
C5 C 0.9183(5) 0.4903(5) 0.7206(4) 0.0433(13) Uani 1 1 d U . .
C6 C 0.7723(6) 0.4479(6) 0.6872(5) 0.0587(16) Uani 1 1 d U . .
H6A H 0.7147 0.4997 0.6876 0.070 Uiso 1 1 calc R . .
C7 C 0.7183(6) 0.3222(7) 0.6532(5) 0.0665(19) Uani 1 1 d U . .
H7A H 0.6211 0.2885 0.6301 0.080 Uiso 1 1 calc R . .
C8 C 0.8045(6) 0.2469(6) 0.6527(5) 0.0596(17) Uani 1 1 d U . .
H8A H 0.7687 0.1628 0.6300 0.072 Uiso 1 1 calc R . .
C9 C 0.9482(5) 0.3032(5) 0.6881(4) 0.0448(13) Uani 1 1 d U . .
C10 C 1.1879(6) 0.2837(5) 0.7221(5) 0.0498(14) Uani 1 1 d U . .
H10A H 1.2337 0.3654 0.7536 0.060 Uiso 1 1 calc R . .
C11 C 1.0223(7) 0.1117(5) 0.6438(5) 0.0593(17) Uani 1 1 d U . .
H11A H 0.9339 0.0553 0.6128 0.071 Uiso 1 1 calc R . .
C12 C 1.1475(7) 0.0885(5) 0.6551(5) 0.0612(17) Uani 1 1 d U . .
H12A H 1.1617 0.0136 0.6333 0.073 Uiso 1 1 calc R . .
C13 C 1.4053(6) 0.2170(5) 0.7367(5) 0.0552(16) Uani 1 1 d U . .
H13A H 1.4485 0.3017 0.7428 0.066 Uiso 1 1 calc R . .
H13B H 1.4233 0.1682 0.6824 0.066 Uiso 1 1 calc R . .
C14 C 1.4739(6) 0.1845(5) 0.8391(5) 0.0483(14) Uani 1 1 d U . .
C15 C 1.5801(6) 0.1251(5) 0.8491(5) 0.0525(15) Uani 1 1 d U . .
H15A H 1.6018 0.0997 0.7915 0.063 Uiso 1 1 calc R . .
C16 C 1.6533(6) 0.1038(5) 0.9444(5) 0.0541(15) Uani 1 1 d U . .
H16A H 1.7247 0.0648 0.9508 0.065 Uiso 1 1 calc R . .
C17 C 1.6207(6) 0.1402(5) 1.0303(5) 0.0525(15) Uani 1 1 d U . .
C18 C 1.5119(7) 0.1937(5) 1.0196(5) 0.0590(17) Uani 1 1 d U . .
H18A H 1.4874 0.2152 1.0765 0.071 Uiso 1 1 calc R . .
C19 C 1.4377(7) 0.2161(5) 0.9238(5) 0.0596(17) Uani 1 1 d U . .
H19A H 1.3640 0.2523 0.9170 0.071 Uiso 1 1 calc R . .
C20 C 1.2470(6) 0.4065(5) 1.0688(5) 0.0517(15) Uani 1 1 d U . .
C21 C 1.1193(6) 0.4540(5) 1.0309(4) 0.0440(13) Uani 1 1 d U . .
C22 C 0.9821(6) 0.3767(5) 0.9924(5) 0.0497(14) Uani 1 1 d U . .
H22A H 0.9690 0.2935 0.9862 0.060 Uiso 1 1 calc R . .
C23 C 0.8655(6) 0.4231(5) 0.9634(5) 0.0487(14) Uani 1 1 d U . .
H23A H 0.7751 0.3706 0.9396 0.058 Uiso 1 1 calc R . .
C24 C 0.7492(8) 0.2840(9) 0.4003(6) 0.089(2) Uani 1 1 d DU . .
C25 C 0.8844(7) 0.3950(9) 0.4529(6) 0.092(2) Uani 1 1 d DU . .
C26 C 0.8634(10) 0.5105(9) 0.4709(6) 0.095(3) Uani 1 1 d U . .
H26A H 0.7715 0.5183 0.4502 0.114 Uiso 1 1 calc R . .
C27 C 0.9868(10) 0.6238(12) 0.5235(7) 0.129(4) Uani 1 1 d U . .
H27A H 0.9739 0.7008 0.5382 0.155 Uiso 1 1 calc R . .
O1 O 1.3678(4) 0.4805(4) 1.0992(5) 0.0870(17) Uani 1 1 d U . .
O1WA O 0.4080(19) 0.3473(16) 0.4702(17) 0.169(8) Uani 0.75 1 d PU A 1
O1WB O 0.405(3) 0.328(3) 0.467(3) 0.064(9) Uani 0.25 1 d PU B 2
O1WC O 0.582(3) 0.4684(19) 0.4150(16) 0.099(7) Uani 0.25 1 d PU C 3
O1WD O 0.5406(9) 0.5056(7) 0.3191(8) 0.118(3) Uani 0.75 1 d PU D 4
O2 O 1.2294(4) 0.2954(4) 1.0683(4) 0.0672(13) Uani 1 1 d U . .
O2W O 0.696(2) -0.0802(15) 0.5475(19) 0.088(5) Uani 0.50 1 d PU E 1
O2W' O 0.733(3) -0.1223(19) 0.552(2) 0.120(8) Uani 0.50 1 d PU F 2
O3 O 0.7534(7) 0.1665(7) 0.3948(5) 0.121(2) Uani 1 1 d U . .
O3W O 0.4453(10) -0.0169(9) 0.5832(9) 0.151(4) Uani 0.85 1 d PU G 1
O3WB O 0.404(9) 0.034(7) 0.528(7) 0.18(3) Uani 0.15 1 d PU H 2
O4 O 0.6366(5) 0.3125(4) 0.3643(4) 0.0867(17) Uani 1 1 d U . .
O4W O 1.620(2) 0.459(2) 1.195(2) 0.098(7) Uani 0.25 1 d PU I 1
O4W' O 1.6377(5) 0.4793(4) 1.1122(4) 0.0486(13) Uani 0.75 1 d PU J 2
O6W O 1.0546(10) 0.0695(7) 0.9406(8) 0.091(3) Uani 0.88 1 d PU K 1
O6W' O 1.070(10) 0.107(7) 0.970(7) 0.12(3) Uani 0.13 1 d PU L 2
O7W O 0.8084(5) 0.0010(4) 0.7628(4) 0.0815(15) Uani 1 1 d U . .
O8W O 1.3672(5) 0.1875(5) 1.2179(4) 0.0923(17) Uani 1 1 d U . .
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
C2 N1 C3 108.9(5) . .
C2 N1 C1 125.3(5) . .
C3 N1 C1 125.7(5) . .
C2 N2 C4 108.5(5) . .
C2 N2 C5 124.7(4) . .
C4 N2 C5 126.8(5) . .
C5 N3 C9 115.9(4) . .
C10 N4 C11 107.4(5) . .
C10 N4 C9 123.9(4) . .
C11 N4 C9 128.6(5) . .
C10 N5 C12 108.0(5) . .
C10 N5 C13 125.2(5) . .
C12 N5 C13 126.8(5) . .
N1 C1 C17 111.0(5) . 2_867
N1 C1 H1A 109.4 . .
C17 C1 H1A 109.4 2_867 .
N1 C1 H1B 109.4 . .
C17 C1 H1B 109.4 2_867 .
H1A C1 H1B 108.0 . .
N1 C2 N2 108.0(5) . .
N1 C2 H2A 126.0 . .
N2 C2 H2A 126.0 . .
C4 C3 N1 108.3(5) . .
C4 C3 H3A 125.9 . .
N1 C3 H3A 125.9 . .
C3 C4 N2 106.2(5) . .
C3 C4 H4A 126.9 . .
N2 C4 H4A 126.9 . .
N3 C5 C6 125.7(5) . .
N3 C5 N2 113.6(4) . .
C6 C5 N2 120.6(5) . .
C5 C6 C7 115.3(6) . .
C5 C6 H6A 122.4 . .
C7 C6 H6A 122.4 . .
C8 C7 C6 121.7(6) . .
C8 C7 H7A 119.1 . .
C6 C7 H7A 119.1 . .
C7 C8 C9 116.1(6) . .
C7 C8 H8A 121.9 . .
C9 C8 H8A 121.9 . .
N3 C9 C8 125.2(5) . .
N3 C9 N4 113.4(4) . .
C8 C9 N4 121.4(5) . .
N5 C10 N4 109.6(5) . .
N5 C10 H10A 125.2 . .
N4 C10 H10A 125.2 . .
C12 C11 N4 107.9(5) . .
C12 C11 H11A 126.0 . .
N4 C11 H11A 126.0 . .
C11 C12 N5 106.9(5) . .
C11 C12 H12A 126.5 . .
N5 C12 H12A 126.5 . .
N5 C13 C14 112.9(5) . .
N5 C13 H13A 109.0 . .
C14 C13 H13A 109.0 . .
N5 C13 H13B 109.0 . .
C14 C13 H13B 109.0 . .
H13A C13 H13B 107.8 . .
C19 C14 C15 119.3(6) . .
C19 C14 C13 121.7(5) . .
C15 C14 C13 118.9(5) . .
C16 C15 C14 120.2(6) . .
C16 C15 H15A 119.9 . .
C14 C15 H15A 119.9 . .
C15 C16 C17 120.3(6) . .
C15 C16 H16A 119.9 . .
C17 C16 H16A 119.9 . .
C18 C17 C16 119.7(6) . .
C18 C17 C1 119.6(6) . 2_867
C16 C17 C1 120.7(6) . 2_867
C17 C18 C19 120.5(6) . .
C17 C18 H18A 119.8 . .
C19 C18 H18A 119.8 . .
C14 C19 C18 120.0(6) . .
C14 C19 H19A 120.0 . .
C18 C19 H19A 120.0 . .
O2 C20 O1 123.0(6) . .
O2 C20 C21 119.0(5) . .
O1 C20 C21 118.0(5) . .
C23 C21 C22 118.1(5) 2_767 .
C23 C21 C20 120.6(5) 2_767 .
C22 C21 C20 121.3(5) . .
C23 C22 C21 120.5(5) . .
C23 C22 H22A 119.8 . .
C21 C22 H22A 119.8 . .
C21 C23 C22 121.4(5) 2_767 .
C21 C23 H23A 119.3 2_767 .
C22 C23 H23A 119.3 . .
O4 C24 O3 122.4(7) . .
O4 C24 C25 114.2(8) . .
O3 C24 C25 123.4(8) . .
C27 C25 C26 122.9(9) 2_766 .
C27 C25 C24 119.7(9) 2_766 .
C26 C25 C24 117.4(7) . .
C25 C26 C27 121.7(9) . .
C25 C26 H26A 119.2 . .
C27 C26 H26A 119.2 . .
C25 C27 C26 115.4(11) 2_766 .
C25 C27 H27A 122.3 2_766 .
C26 C27 H27A 122.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C2 1.333(7) .
N1 C3 1.378(8) .
N1 C1 1.493(7) .
N2 C2 1.357(7) .
N2 C4 1.397(7) .
N2 C5 1.438(7) .
N3 C5 1.324(7) .
N3 C9 1.327(7) .
N4 C10 1.335(7) .
N4 C11 1.389(7) .
N4 C9 1.433(7) .
N5 C10 1.332(7) .
N5 C12 1.392(7) .
N5 C13 1.471(7) .
C1 C17 1.512(9) 2_867
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9300 .
C3 C4 1.353(9) .
C3 H3A 0.9300 .
C4 H4A 0.9300 .
C5 C6 1.388(7) .
C6 C7 1.390(9) .
C6 H6A 0.9300 .
C7 C8 1.371(9) .
C7 H7A 0.9300 .
C8 C9 1.387(8) .
C8 H8A 0.9300 .
C10 H10A 0.9300 .
C11 C12 1.346(9) .
C11 H11A 0.9300 .
C12 H12A 0.9300 .
C13 C14 1.513(8) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C19 1.382(8) .
C14 C15 1.394(8) .
C15 C16 1.383(9) .
C15 H15A 0.9300 .
C16 C17 1.386(8) .
C16 H16A 0.9300 .
C17 C18 1.373(8) .
C17 C1 1.512(9) 2_867
C18 C19 1.396(9) .
C18 H18A 0.9300 .
C19 H19A 0.9300 .
C20 O2 1.259(7) .
C20 O1 1.263(7) .
C20 C21 1.502(8) .
C21 C23 1.384(7) 2_767
C21 C22 1.399(7) .
C22 C23 1.387(8) .
C22 H22A 0.9300 .
C23 C21 1.384(7) 2_767
C23 H23A 0.9300 .
C24 O4 1.243(9) .
C24 O3 1.359(10) .
C24 C25 1.570(8) .
C25 C27 1.340(12) 2_766
C25 C26 1.394(12) .
C26 C27 1.518(12) .
C26 H26A 0.9300 .
C27 C25 1.340(12) 2_766
C27 H27A 0.9300 .
