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#$Date: 2016-03-26 00:26:42 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180079 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/25/7052523.cif $
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#
# 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_7052523
loop_
_publ_author_name
'Mansikkamäki, Heidi'
'Nissinen, Maija'
'Schalley, Christoph A.'
'Rissanen, Kari'
_publ_section_title
;
 Self-assembling resorcinarene capsules: solid and gas phase studies on
 encapsulation of small alkyl ammonium cations
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              88
_journal_paper_doi               10.1039/b207875a
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C72 H96 Br N O22'
_chemical_formula_weight         1407.41
_space_group_IT_number           112
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2c'
_symmetry_space_group_name_H-M   'P -4 2 c'
_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            2
_cell_length_a                   14.2645(7)
_cell_length_b                   14.2645(7)
_cell_length_c                   18.4532(9)
_cell_measurement_temperature    173(2)
_cell_volume                     3754.8(3)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       collect
_computing_data_reduction        Denzo-SMN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13197
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_correction_T_min  0.8862
_exptl_absorpt_correction_type   'not used'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3284
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1313
_refine_ls_R_factor_gt           0.0878
_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)+(0.1366P)²+3.6499P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2231
_refine_ls_wR_factor_ref         0.2541
_reflns_number_gt                2230
_reflns_number_total             3284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207875a.txt
_cod_data_source_block           4(1)2Br4MeOH3H2O
_cod_database_code               7052523
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, -z+1/2'
'-x, -y, z'
'-x, y, -z+1/2'
'-y, -x, z+1/2'
'-y, x, -z'
'y, -x, -z'
'y, x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.5000 0.0000 -0.14062(13) 0.0803(8) Uani 0.50 2 d SP A 1
O71 O 0.5000 0.0000 -0.1036(12) 0.089(6) Uiso 0.50 2 d SP B 2
C1 C 0.7512(4) -0.0058(5) 0.0730(3) 0.0464(14) Uani 1 1 d . . .
C2 C 0.7860(4) 0.0641(5) 0.1170(3) 0.0473(16) Uani 1 1 d . . .
H2 H 0.8339 0.0475 0.1504 0.057 Uiso 1 1 calc R . .
C3 C 0.7562(4) 0.1582(5) 0.1164(3) 0.0487(16) Uani 1 1 d . . .
C4 C 0.6854(5) 0.1805(5) 0.0674(3) 0.0526(16) Uani 1 1 d . . .
O4 O 0.6560(4) 0.2724(3) 0.0645(3) 0.0716(14) Uani 1 1 d . . .
H4 H 0.6085 0.2765 0.0378 0.107 Uiso 1 1 calc R . .
C5 C 0.6478(5) 0.1134(5) 0.0215(3) 0.0573(18) Uani 1 1 d . . .
H5 H 0.6005 0.1303 -0.0123 0.069 Uiso 1 1 calc R . .
C6 C 0.6786(5) 0.0225(5) 0.0250(3) 0.0577(19) Uani 1 1 d . . .
O6 O 0.6411(4) -0.0467(4) -0.0186(2) 0.0679(14) Uani 1 1 d . . .
H6C H 0.5916 -0.0269 -0.0379 0.102 Uiso 0.50 1 calc PR . .
C7 C 0.7975(4) 0.2316(5) 0.1679(3) 0.0488(16) Uani 1 1 d . . .
H7 H 0.7816 0.2944 0.1472 0.059 Uiso 1 1 calc R . .
C8 C 0.7485(4) 0.2252(4) 0.2419(3) 0.0447(14) Uani 1 1 d . . .
C9 C 0.7851(4) 0.1725(5) 0.2976(3) 0.0463(15) Uani 1 1 d . . .
H9 H 0.8424 0.1403 0.2892 0.056 Uiso 1 1 calc R . .
C10 C 0.7430(4) 0.1633(4) 0.3659(3) 0.0448(15) Uani 1 1 d . . .
O11 O 0.6084(4) 0.2052(4) 0.4394(2) 0.0675(14) Uani 1 1 d . . .
H11 H 0.6310 0.1632 0.4661 0.101 Uiso 1 1 calc R . .
C11 C 0.6599(4) 0.2108(5) 0.3761(3) 0.0501(16) Uani 1 1 d . . .
C12 C 0.6196(5) 0.2642(5) 0.3213(4) 0.0603(18) Uani 1 1 d . . .
H12 H 0.5613 0.2949 0.3291 0.072 Uiso 1 1 calc R . .
C13 C 0.6647(4) 0.2725(4) 0.2554(4) 0.0517(15) Uani 1 1 d . . .
O13 O 0.6214(4) 0.3267(4) 0.2043(3) 0.0742(16) Uani 1 1 d . . .
H13 H 0.6259 0.3009 0.1636 0.111 Uiso 1 1 calc R . .
C14 C 0.7884(4) 0.1043(5) 0.4262(3) 0.0516(16) Uani 1 1 d . . .
H14 H 0.7692 0.1335 0.4732 0.062 Uiso 1 1 calc R . .
C29 C 0.9054(5) 0.2269(6) 0.1728(4) 0.064(2) Uani 1 1 d . . .
H29A H 0.9326 0.2410 0.1252 0.096 Uiso 1 1 calc R . .
H29B H 0.9245 0.1639 0.1879 0.096 Uiso 1 1 calc R . .
H29C H 0.9277 0.2728 0.2083 0.096 Uiso 1 1 calc R . .
C30 C 0.8955(5) 0.1074(5) 0.4240(3) 0.0566(17) Uani 1 1 d . . .
H30A H 0.9168 0.1724 0.4291 0.085 Uiso 1 1 calc R . .
H30B H 0.9175 0.0822 0.3776 0.085 Uiso 1 1 calc R . .
H30C H 0.9209 0.0696 0.4637 0.085 Uiso 1 1 calc R . .
N1 N 0.5000 0.0000 0.2500 0.048(2) Uani 1 4 d S . .
C50 C 0.5595(8) 0.0597(9) 0.2069(6) 0.134(5) Uani 1 1 d . . .
H50A H 0.5941 0.1024 0.2388 0.201 Uiso 1 1 calc R . .
H50B H 0.5210 0.0961 0.1732 0.201 Uiso 1 1 calc R . .
H50C H 0.6040 0.0211 0.1796 0.201 Uiso 1 1 calc R . .
O60 O 0.5147(5) 0.3077(5) -0.0244(3) 0.0999(19) Uiso 1 1 d D . .
C61 C 0.5144(18) 0.2851(18) -0.0950(10) 0.134(6) Uiso 0.560(18) 1 d PD C 1
C61B C 0.513(3) 0.3717(19) -0.0764(14) 0.134(6) Uiso 0.440(18) 1 d PD C 2
O70 O 0.5000 0.5000 0.2500 0.181(8) Uiso 1 4 d S . .
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'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
C2 C1 C6 115.1(6) . . ?
C2 C1 C14 122.9(5) . 2 ?
C6 C1 C14 121.9(6) . 2 ?
C1 C2 C3 125.2(6) . . ?
C4 C3 C2 116.2(6) . . ?
C4 C3 C7 121.7(6) . . ?
C2 C3 C7 122.1(5) . . ?
O4 C4 C5 121.1(6) . . ?
O4 C4 C3 117.6(6) . . ?
C5 C4 C3 121.3(6) . . ?
C6 C5 C4 120.0(6) . . ?
C5 C6 O6 121.6(6) . . ?
C5 C6 C1 122.2(7) . . ?
O6 C6 C1 116.2(6) . . ?
C3 C7 C8 109.6(5) . . ?
C3 C7 C29 112.9(6) . . ?
C8 C7 C29 113.6(5) . . ?
C9 C8 C13 117.1(5) . . ?
C9 C8 C7 121.5(5) . . ?
C13 C8 C7 121.4(5) . . ?
C8 C9 C10 124.0(6) . . ?
C11 C10 C9 116.4(6) . . ?
C11 C10 C14 122.1(5) . . ?
C9 C10 C14 121.5(6) . . ?
C10 C11 O11 122.9(6) . . ?
C10 C11 C12 121.7(6) . . ?
O11 C11 C12 115.2(6) . . ?
C13 C12 C11 119.6(6) . . ?
O13 C13 C12 116.4(6) . . ?
O13 C13 C8 122.5(5) . . ?
C12 C13 C8 121.1(6) . . ?
C1 C14 C30 112.3(6) 2 . ?
C1 C14 C10 111.7(4) 2 . ?
C30 C14 C10 112.6(5) . . ?
C50 N1 C50 107.6(10) 4_655 . ?
C50 N1 C50 113.1(10) 4_655 2 ?
C50 N1 C50 107.8(12) . 2 ?
C50 N1 C50 107.8(12) 4_655 3_655 ?
C50 N1 C50 113.1(10) . 3_655 ?
C50 N1 C50 107.6(10) 2 3_655 ?
C61B O60 C61 57.4(15) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.379(9) . ?
C1 C6 1.421(9) . ?
C1 C14 1.503(9) 2 ?
C2 C3 1.407(9) . ?
C3 C4 1.394(9) . ?
C3 C7 1.532(10) . ?
C4 O4 1.377(8) . ?
C4 C5 1.387(10) . ?
C5 C6 1.370(10) . ?
C6 O6 1.381(8) . ?
C7 C8 1.536(8) . ?
C7 C29 1.543(9) . ?
C8 C9 1.377(8) . ?
C8 C13 1.395(8) . ?
C9 C10 1.403(8) . ?
C10 C11 1.379(9) . ?
C10 C14 1.538(9) . ?
O11 C11 1.382(7) . ?
C11 C12 1.391(10) . ?
C12 C13 1.381(9) . ?
C13 O13 1.367(7) . ?
C14 C1 1.503(9) 2 ?
C14 C30 1.530(9) . ?
N1 C50 1.442(9) 4_655 ?
N1 C50 1.442(9) . ?
N1 C50 1.442(9) 2 ?
N1 C50 1.442(9) 3_655 ?
O60 C61B 1.324(19) . ?
O60 C61 1.342(18) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O60 0.84 1.82 2.648(8) 168.8 .
O6 H6C O71 0.84 1.82 2.638(14) 162.9 .
O6 H6C Br1 0.84 2.33 3.093(5) 150.6 .
O11 H11 O6 0.84 1.93 2.732(7) 159.6 2
O13 H13 O4 0.84 1.92 2.738(7) 164.1 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.0(8) . . . . ?
C14 C1 C2 C3 177.4(5) 2 . . . ?
C1 C2 C3 C4 0.4(8) . . . . ?
C1 C2 C3 C7 179.1(5) . . . . ?
C2 C3 C4 O4 -178.8(5) . . . . ?
C7 C3 C4 O4 2.5(8) . . . . ?
C2 C3 C4 C5 -0.6(9) . . . . ?
C7 C3 C4 C5 -179.3(6) . . . . ?
O4 C4 C5 C6 179.6(6) . . . . ?
C3 C4 C5 C6 1.4(10) . . . . ?
C4 C5 C6 O6 178.4(6) . . . . ?
C4 C5 C6 C1 -2.0(10) . . . . ?
C2 C1 C6 C5 1.8(8) . . . . ?
C14 C1 C6 C5 -176.6(6) 2 . . . ?
C2 C1 C6 O6 -178.6(5) . . . . ?
C14 C1 C6 O6 3.0(8) 2 . . . ?
C4 C3 C7 C8 96.1(6) . . . . ?
C2 C3 C7 C8 -82.5(6) . . . . ?
C4 C3 C7 C29 -136.2(6) . . . . ?
C2 C3 C7 C29 45.2(7) . . . . ?
C3 C7 C8 C9 94.3(6) . . . . ?
C29 C7 C8 C9 -33.1(8) . . . . ?
C3 C7 C8 C13 -85.6(7) . . . . ?
C29 C7 C8 C13 147.1(6) . . . . ?
C13 C8 C9 C10 0.5(9) . . . . ?
C7 C8 C9 C10 -179.4(5) . . . . ?
C8 C9 C10 C11 0.1(9) . . . . ?
C8 C9 C10 C14 -179.1(6) . . . . ?
C9 C10 C11 O11 177.1(6) . . . . ?
C14 C10 C11 O11 -3.7(9) . . . . ?
C9 C10 C11 C12 0.6(9) . . . . ?
C14 C10 C11 C12 179.8(6) . . . . ?
C10 C11 C12 C13 -1.9(10) . . . . ?
O11 C11 C12 C13 -178.6(6) . . . . ?
C11 C12 C13 O13 -179.4(6) . . . . ?
C11 C12 C13 C8 2.5(10) . . . . ?
C9 C8 C13 O13 -179.7(6) . . . . ?
C7 C8 C13 O13 0.1(9) . . . . ?
C9 C8 C13 C12 -1.8(9) . . . . ?
C7 C8 C13 C12 178.1(6) . . . . ?
C11 C10 C14 C1 86.9(7) . . . 2 ?
C9 C10 C14 C1 -93.9(7) . . . 2 ?
C11 C10 C14 C30 -145.5(6) . . . . ?
C9 C10 C14 C30 33.7(8) . . . . ?
