#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:49:18 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154569 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/34/4513429.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_4513429
loop_
_publ_author_name
'Jayasinghe, Ashini S.'
'Unruh, Daniel K.'
'Kral, Andrew'
'Libo, Anna'
'Forbes, Tori Z.'
_publ_section_title
;
 Structural Features in Metal--Organic Nanotube Crystals That Influence
 Stability and Solvent Uptake
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4062
_journal_paper_doi               10.1021/acs.cgd.5b00653
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C10 H17 N3 O10 U'
_chemical_formula_weight         577.29
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-01T12:20:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.6558(14)
_cell_length_b                   22.6558(14)
_cell_length_c                   6.4981(5)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.75
_cell_volume                     2888.5(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  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_laue_measured_fraction_full 1
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            41764
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.333
_diffrn_reflns_theta_min         1.038
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.477
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       Blocky
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.097
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.018
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0191P)²+5.6325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0421
_reflns_number_gt                3360
_reflns_number_total             3526
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00653_si_003.cif
_cod_data_source_block           p-3
_cod_depositor_comments
'Adding full bibliography for 4513429--4513433.cif.'
_cod_original_cell_volume        2888.5(4)
_cod_database_code               4513429
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_calc_flag
U1 U 0.37909(2) 0.17258(2) 0.67330(2) 0.01056(5) Uani 1 d
O1 O 0.39631(12) 0.08674(11) 0.8161(3) 0.0152(5) Uani 1 d
O2 O 0.30953(12) 0.07749(12) 0.4684(3) 0.0155(5) Uani 1 d
O3 O 0.44916(12) 0.19816(12) 0.5044(4) 0.0190(5) Uani 1 d
O4 O 0.31156(12) 0.14735(12) 0.8547(3) 0.0159(5) Uani 1 d
O5 O 0.42390(12) 0.28558(11) 0.7886(3) 0.0158(5) Uani 1 d
O6 O 0.32302(12) 0.21304(12) 0.4687(3) 0.0183(5) Uani 1 d
O7 O 0.37935(12) 0.05401(13) 0.2879(4) 0.0214(5) Uani 1 d
O8 O 0.46454(12) 0.05042(11) 0.9333(3) 0.0141(5) Uani 1 d
O9 O 0.51403(13) 0.38414(12) 0.8846(4) 0.0275(6) Uani 1 d
O10 O 0.40051(13) 0.28424(14) 0.2432(4) 0.0259(6) Uani 1 d
N1 N 0.46573(14) 0.20939(14) 0.9716(4) 0.0154(6) Uani 1 d
H1 H 0.439 0.2008 1.1015 0.018 Uiso 1 calc
N2 N 0.28403(14) -0.02367(14) 0.0108(4) 0.0138(6) Uani 1 d
H2A H 0.2845 -0.0604 0.0657 0.017 Uiso 1 calc
H2B H 0.3269 0.006 -0.0343 0.017 Uiso 1 calc
N3 N 0.46354(14) -0.00246(14) 1.3181(4) 0.0141(6) Uani 1 d
H3A H 0.4679 -0.0336 1.2411 0.017 Uiso 1 calc
H3B H 0.4388 0.0117 1.2441 0.017 Uiso 1 calc
C1 C 0.32433(17) 0.04978(16) 0.3212(5) 0.0131(7) Uani 1 d
C2 C 0.45069(17) 0.09573(17) 0.9078(5) 0.0140(7) Uani 1 d
C3 C 0.48244(18) 0.32212(17) 0.8760(5) 0.0179(7) Uani 1 d
C4 C 0.49830(18) 0.16738(17) 0.9837(6) 0.0190(8) Uani 1 d
H4A H 0.5114 0.1656 1.128 0.023 Uiso 1 calc
H4B H 0.5403 0.1884 0.8992 0.023 Uiso 1 calc
C5 C 0.51449(19) 0.28265(17) 0.9660(6) 0.0239(8) Uani 1 d
H5A H 0.5544 0.2911 0.8818 0.029 Uiso 1 calc
H5B H 0.5307 0.2991 1.1073 0.029 Uiso 1 calc
C6 C 0.26516(17) 0.00983(17) 0.1738(5) 0.0146(7) Uani 1 d
H6A H 0.2255 -0.0252 0.2516 0.018 Uiso 1 calc
H6B H 0.2519 0.0411 0.1095 0.018 Uiso 1 calc
C7 C 0.34228(18) 0.24728(17) 0.3013(5) 0.0157(7) Uani 1 d
C8 C 0.53228(17) 0.05674(17) 1.3598(5) 0.0174(7) Uani 1 d
H8A H 0.5277 0.0926 1.433 0.021 Uiso 1 calc
H8B H 0.5561 0.0761 1.228 0.021 Uiso 1 calc
C9 C 0.23650(17) -0.04644(17) -0.1672(5) 0.0152(7) Uani 1 d
H9A H 0.2443 -0.0064 -0.2494 0.018 Uiso 1 calc
H9B H 0.1889 -0.0695 -0.1169 0.018 Uiso 1 calc
C10 C 0.42651(17) -0.03525(18) 1.5115(5) 0.0172(7) Uani 1 d
H10A H 0.3819 -0.0756 1.478 0.021 Uiso 1 calc
H10B H 0.418 -0.0028 1.5901 0.021 Uiso 1 calc
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 0 '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 0.006 '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_3
O3 U1 O4 176.88(11) .
O3 U1 O6 95.39(10) .
O4 U1 O6 87.35(9) .
O3 U1 O2 91.70(10) .
O4 U1 O2 90.34(9) .
O6 U1 O2 77.79(8) .
O3 U1 O5 90.73(10) .
O4 U1 O5 88.42(9) .
O6 U1 O5 77.08(8) .
O2 U1 O5 154.88(8) .
O3 U1 O1 91.31(9) .
O4 U1 O1 86.84(9) .
O6 U1 O1 154.24(8) .
O2 U1 O1 77.17(8) .
O5 U1 O1 127.77(8) .
O3 U1 N1 86.98(10) .
O4 U1 N1 89.95(10) .
O6 U1 N1 141.28(8) .
O2 U1 N1 140.88(8) .
O5 U1 N1 64.23(8) .
O1 U1 N1 63.79(8) .
C2 O1 U1 126.2(2) .
C1 O2 U1 130.9(2) .
C3 O5 U1 125.6(2) .
C7 O6 U1 129.7(2) .
C5 N1 C4 113.4(3) .
C5 N1 U1 111.6(2) .
C4 N1 U1 112.18(19) .
C6 N2 C9 112.9(3) .
C8 N3 C10 111.8(3) .
O7 C1 O2 127.1(3) .
O7 C1 C6 119.7(3) .
O2 C1 C6 113.2(3) .
O8 C2 O1 123.7(3) .
O8 C2 C4 120.7(3) .
O1 C2 C4 115.6(3) .
O9 C3 O5 125.6(3) .
O9 C3 C5 118.8(3) .
O5 C3 C5 115.5(3) .
N1 C4 C2 111.0(3) .
N1 C5 C3 111.4(3) .
N2 C6 C1 111.0(3) .
O10 C7 O6 127.2(3) .
O10 C7 C9 120.1(3) 6
O6 C7 C9 112.6(3) 6
N3 C8 C10 110.4(3) 4_658
N2 C9 C7 110.4(3) 5
N3 C10 C8 110.2(3) 4_658
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O3 1.772(2) .
U1 O4 1.784(2) .
U1 O6 2.321(2) .
U1 O2 2.346(2) .
U1 O5 2.355(2) .
U1 O1 2.357(2) .
U1 N1 2.582(3) .
O1 C2 1.290(4) .
O2 C1 1.278(4) .
O5 C3 1.292(4) .
O6 C7 1.279(4) .
O7 C1 1.221(4) .
O8 C2 1.225(4) .
O9 C3 1.218(4) .
O10 C7 1.217(4) .
N1 C5 1.464(4) .
N1 C4 1.469(4) .
N2 C6 1.485(4) .
N2 C9 1.486(4) .
N3 C8 1.486(4) .
N3 C10 1.487(4) .
C1 C6 1.523(4) .
C2 C4 1.514(5) .
C3 C5 1.522(5) .
C7 C9 1.516(5) 6
C8 C10 1.504(5) 4_658
C9 C7 1.516(5) 5
C10 C8 1.504(5) 4_658
