#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:59:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178968 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/97/4119759.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_4119759
loop_
_publ_author_name
'Daniel K. Unruh'
'Kyle Gojdas'
'Anna Libo'
'Tori Z. Forbes'
_publ_contact_author_address
;Department of Chemistry
University of Iowa
Chemistry Building W374
Iowa City, IA 52242
;
_publ_contact_author_email       tori-forbes@uiowa.edu
_publ_contact_author_fax         319-335-1270
_publ_contact_author_name        'Tori Z. Forbes'
_publ_contact_author_phone       319-384-1320
_publ_section_title
;
 Development of Metal-Organic Nanotubes Exhibiting Low-Temperature,
 Reversible Exchange of Confined "Ice Channels"
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7398
_journal_page_last               7401
_journal_paper_doi               10.1021/ja400303f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C60 H102 N18 O72 U6'
_chemical_formula_weight         3655.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            1
_cell_length_a                   22.5338(10)
_cell_length_b                   22.5338(10)
_cell_length_c                   6.5999(4)
_cell_measurement_reflns_used    9698
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.76
_cell_volume                     2902.3(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CrystalMaker v2.5.0'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega 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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            55033
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    8.450
_exptl_absorpt_correction_T_max  0.466
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_description       blocky
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4951
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0320P)²+4.3918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0547
_reflns_number_gt                4712
_reflns_number_total             4951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400303f_si_006.cif
_cod_data_source_block           hexanes
_cod_database_code               4119759
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
U1 U 0.792667(5) 0.172138(5) -0.332093(14) 0.01706(4) Uani 1 1 d .
O1 O 0.58593(11) 0.04935(11) -0.0622(3) 0.0245(4) Uani 1 1 d .
O2 O 0.68977(11) 0.08601(11) -0.1883(3) 0.0255(4) Uani 1 1 d .
O3 O 0.77036(12) 0.07617(12) -0.5342(3) 0.0256(4) Uani 1 1 d .
O4 O 0.83576(11) 0.14731(12) -0.1542(3) 0.0252(4) Uani 1 1 d .
O5 O 0.74728(12) 0.19701(12) -0.4983(4) 0.0322(5) Uani 1 1 d .
O6 O 0.86148(11) 0.28605(11) -0.2209(4) 0.0270(5) Uani 1 1 d .
O7 O 0.89003(12) 0.20969(13) -0.5371(3) 0.0319(5) Uani 1 1 d .
O8 O 0.67769(13) 0.05331(14) -0.7163(4) 0.0358(6) Uani 1 1 d .
O9 O 0.88151(16) 0.27857(16) -0.7657(4) 0.0451(7) Uani 1 1 d .
O10 O 0.87112(17) 0.38452(14) -0.1204(6) 0.0610(10) Uani 1 1 d .
OW1 O 0.9200(3) 0.0634(3) -0.0333(10) 0.1167(19) Uani 1 1 d .
OW2A O 0.9274(7) 0.0982(7) -0.4770(19) 0.108(3) Uiso 0.50 1 d P
OW2B O 0.8872(7) 0.0540(7) -0.4674(18) 0.107(3) Uiso 0.50 1 d P
N1 N 0.74410(14) 0.20977(13) -0.0363(4) 0.0283(6) Uani 1 1 d .
H1 H 0.7620 0.2027 0.0788 0.034 Uiso 1 1 calc R
N2 N 0.97613(13) 0.28004(13) -1.0109(4) 0.0235(5) Uani 1 1 d .
H2A H 1.0055 0.3227 -0.9672 0.028 Uiso 1 1 calc R
H2B H 0.9394 0.2802 -1.0638 0.028 Uiso 1 1 calc R
N3 N 0.53522(13) -0.00214(14) -0.6769(4) 0.0249(5) Uani 1 1 d .
H3A H 0.5004 -0.0339 -0.7519 0.030 Uiso 1 1 calc R
H3B H 0.5742 0.0125 -0.7478 0.030 Uiso 1 1 calc R
C1 C 0.72877(15) 0.04916(15) -0.6827(4) 0.0219(6) Uani 1 1 d .
C2 C 0.64503(15) 0.09510(15) -0.0929(4) 0.0216(5) Uani 1 1 d .
C3 C 0.74876(16) 0.00991(16) -0.8280(4) 0.0233(6) Uani 1 1 d .
H3C H 0.7926 0.0411 -0.8897 0.028 Uiso 1 1 calc R
H3D H 0.7537 -0.0245 -0.7537 0.028 Uiso 1 1 calc R
C4 C 0.95385(16) 0.23230(17) -0.8358(4) 0.0255(6) Uani 1 1 d .
H4A H 0.9934 0.2407 -0.7557 0.031 Uiso 1 1 calc R
H4B H 0.9318 0.1854 -0.8840 0.031 Uiso 1 1 calc R
C5 C 0.52397(19) 0.05649(17) -0.6399(5) 0.0310(7) Uani 1 1 d .
H5A H 0.5194 0.0747 -0.7683 0.037 Uiso 1 1 calc R
H5B H 0.5632 0.0926 -0.5692 0.037 Uiso 1 1 calc R
C6 C 0.90412(16) 0.24271(17) -0.7056(4) 0.0266(6) Uani 1 1 d .
C7 C 0.66932(17) 0.16725(17) -0.0168(6) 0.0334(8) Uani 1 1 d .
H7A H 0.6474 0.1876 -0.0943 0.040 Uiso 1 1 calc R
H7B H 0.6564 0.1655 0.1241 0.040 Uiso 1 1 calc R
C8 C 0.53987(19) -0.0339(2) -0.4853(5) 0.0318(7) Uani 1 1 d .
H8A H 0.5797 -0.0011 -0.4091 0.038 Uiso 1 1 calc R
H8B H 0.5452 -0.0731 -0.5154 0.038 Uiso 1 1 calc R
C9 C 0.83973(18) 0.32233(17) -0.1318(6) 0.0359(8) Uani 1 1 d .
C10 C 0.76840(19) 0.28340(18) -0.0434(7) 0.0445(10) Uani 1 1 d .
H10A H 0.7687 0.3000 0.0924 0.053 Uiso 1 1 calc R
H10B H 0.7374 0.2914 -0.1254 0.053 Uiso 1 1 calc R
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'
U U -9.6767 9.6646 '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
O5 U1 O4 177.02(11) . .
O5 U1 O7 96.46(10) . .
O4 U1 O7 86.28(9) . .
O5 U1 O2 91.37(10) . .
O4 U1 O2 86.70(9) . .
O7 U1 O2 152.59(8) . .
O5 U1 O6 91.01(10) . .
O4 U1 O6 88.38(9) . .
O7 U1 O6 78.42(8) . .
O2 U1 O6 127.81(8) . .
O5 U1 O3 92.73(10) . .
O4 U1 O3 89.11(9) . .
O7 U1 O3 74.82(9) . .
O2 U1 O3 78.61(8) . .
O6 U1 O3 153.22(8) . .
O5 U1 N1 87.57(11) . .
O4 U1 N1 89.54(10) . .
O7 U1 N1 142.35(9) . .
O2 U1 N1 63.97(8) . .
O6 U1 N1 64.06(8) . .
O3 U1 N1 142.58(8) . .
C2 O2 U1 126.31(19) . .
C1 O3 U1 129.4(2) . .
C9 O6 U1 125.6(2) . .
C6 O7 U1 128.6(2) . .
C10 N1 C7 113.5(3) . .
C10 N1 U1 111.6(2) . .
C7 N1 U1 112.9(2) . .
C10 N1 H1 106.1 . .
C7 N1 H1 106.1 . .
U1 N1 H1 106.1 . .
C4 N2 C3 112.6(2) . 5_663
C4 N2 H2A 109.1 . .
C3 N2 H2A 109.1 5_663 .
C4 N2 H2B 109.1 . .
C3 N2 H2B 109.1 5_663 .
H2A N2 H2B 107.8 . .
C8 N3 C5 112.0(2) . .
C8 N3 H3A 109.2 . .
C5 N3 H3A 109.2 . .
C8 N3 H3B 109.2 . .
C5 N3 H3B 109.2 . .
H3A N3 H3B 107.9 . .
O8 C1 O3 126.6(3) . .
O8 C1 C3 119.7(3) . .
O3 C1 C3 113.6(3) . .
O1 C2 O2 123.6(3) . .
O1 C2 C7 120.3(3) . .
O2 C2 C7 116.1(3) . .
N2 C3 C1 110.9(3) 6_543 .
N2 C3 H3C 109.5 6_543 .
C1 C3 H3C 109.5 . .
N2 C3 H3D 109.5 6_543 .
C1 C3 H3D 109.5 . .
H3C C3 H3D 108.1 . .
N2 C4 C6 109.6(3) . .
N2 C4 H4A 109.7 . .
C6 C4 H4A 109.7 . .
N2 C4 H4B 109.7 . .
C6 C4 H4B 109.7 . .
H4A C4 H4B 108.2 . .
N3 C5 C8 110.4(3) . 4_654
N3 C5 H5A 109.6 . .
C8 C5 H5A 109.6 4_654 .
N3 C5 H5B 109.6 . .
C8 C5 H5B 109.6 4_654 .
H5A C5 H5B 108.1 . .
O9 C6 O7 127.0(3) . .
O9 C6 C4 120.3(3) . .
O7 C6 C4 112.8(3) . .
N1 C7 C2 110.6(3) . .
N1 C7 H7A 109.5 . .
C2 C7 H7A 109.5 . .
N1 C7 H7B 109.5 . .
C2 C7 H7B 109.5 . .
H7A C7 H7B 108.1 . .
N3 C8 C5 110.1(3) . 4_654
N3 C8 H8A 109.6 . .
C5 C8 H8A 109.6 4_654 .
N3 C8 H8B 109.6 . .
C5 C8 H8B 109.6 4_654 .
H8A C8 H8B 108.2 . .
O10 C9 O6 125.0(3) . .
O10 C9 C10 118.8(3) . .
O6 C9 C10 116.1(3) . .
N1 C10 C9 110.9(3) . .
N1 C10 H10A 109.5 . .
C9 C10 H10A 109.5 . .
N1 C10 H10B 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O5 1.771(2) .
U1 O4 1.782(2) .
U1 O7 2.346(2) .
U1 O2 2.354(2) .
U1 O6 2.356(2) .
U1 O3 2.371(2) .
U1 N1 2.580(3) .
O1 C2 1.226(4) .
O2 C2 1.289(4) .
O3 C1 1.280(4) .
O6 C9 1.287(4) .
O7 C6 1.286(4) .
O8 C1 1.221(4) .
O9 C6 1.217(4) .
O10 C9 1.216(4) .
OW2A OW2B 0.956(14) .
N1 C10 1.465(4) .
N1 C7 1.470(4) .
N1 H1 0.9100 .
N2 C4 1.485(4) .
N2 C3 1.489(4) 5_663
N2 H2A 0.9000 .
N2 H2B 0.9000 .
N3 C8 1.482(4) .
N3 C5 1.485(4) .
N3 H3A 0.9000 .
N3 H3B 0.9000 .
C1 C3 1.517(4) .
C2 C7 1.518(4) .
C3 N2 1.489(4) 6_543
C3 H3C 0.9700 .
C3 H3D 0.9700 .
C4 C6 1.520(4) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C8 1.510(5) 4_654
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C5 1.509(5) 4_654
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.511(5) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
