#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:56:23 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180281 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/67/7116771.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_7116771
loop_
_publ_author_name
'M. Basile'
'D. K. Unruh'
'K. Gojdas'
'E. Flores'
'L. Streicher'
'T. Z. Forbes'
_publ_section_title
;
 Chemical controls on uranyl citrate speciation and the self-assembly of
 nanoscale macrocycles and sandwich complexes in aqueous solutions
;
_journal_name_full               Chem.Commun.
_journal_page_first              5306
_journal_paper_doi               10.1039/C4cc08657K
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C12 H14 O20 U2, C2 H10 N2, 3(H2 O)'
_chemical_formula_sum            'C14 H30 N2 O23 U2'
_chemical_formula_weight         1070.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-28T08:13:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-10-28 deposited with the CCDC.
2014-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                97.9088(37)
_cell_angle_beta                 93.7875(37)
_cell_angle_gamma                104.2937(36)
_cell_formula_units_Z            1
_cell_length_a                   6.2109(8)
_cell_length_b                   9.9970(13)
_cell_length_c                   11.3778(15)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      2.57
_cell_volume                     674.38(15)
_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 v2.7.7'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16340
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         3.012
_exptl_absorpt_coefficient_mu    12.095
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.636
_exptl_crystal_description       blade
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.377
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.023
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0324P)²+1.1047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                3066
_reflns_number_total             3222
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc08657k2.cif
_cod_data_source_block           U2en
_cod_database_code               7116771
#BEGIN Tags that were not found in dictionaries:
_shelx_estimated_absorpt_t_min   0.176
_shelx_estimated_absorpt_t_max   0.794
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.13730(2) 0.69535(2) 0.56818(2) 0.02687(6) Uani 1 d . .
O1 O 0.1024(5) 0.4594(3) 0.5923(2) 0.0306(6) Uani 1 d . .
O2 O -0.0909(6) 0.7055(4) 0.6537(3) 0.0391(7) Uani 1 d . .
O3 O 0.6223(5) 0.6799(3) 0.8722(3) 0.0374(7) Uani 1 d . .
O4 O 0.3702(6) 0.6958(4) 0.4857(3) 0.0397(7) Uani 1 d . .
O5 O 0.3107(5) 0.9421(3) 0.6253(3) 0.0394(7) Uani 1 d . .
O6 O 0.3608(6) 0.7081(3) 0.7447(3) 0.0391(7) Uani 1 d . .
O7 O -0.0250(5) 0.8120(3) 0.4322(3) 0.0369(7) Uani 1 d . .
O8 O 0.2409(6) 0.4549(4) 0.9724(3) 0.0422(7) Uani 1 d . .
H8 H 0.2753 0.4156 1.0278 0.063 Uiso 1 calc . .
O9 O -0.2561(6) 0.8111(3) 0.2764(3) 0.0447(8) Uani 1 d . .
O10 O -0.0320(7) 0.2606(4) 0.9274(4) 0.0614(11) Uani 1 d . .
O11 O 0.7472(6) 0.9654(4) 0.6520(3) 0.0454(8) Uani 1 d . .
C1 C -0.1579(7) 0.7495(4) 0.3399(4) 0.0314(8) Uani 1 d . .
C2 C 0.4723(7) 0.6317(4) 0.7873(4) 0.0309(8) Uani 1 d . .
C3 C 0.1774(7) 0.4081(4) 0.6927(3) 0.0277(7) Uani 1 d . .
C4 C 0.0709(7) 0.3704(4) 0.9031(4) 0.0312(8) Uani 1 d . .
C5 C 0.4255(7) 0.4803(4) 0.7328(4) 0.0304(8) Uani 1 d . .
H5A H 0.4802 0.4296 0.7912 0.037 Uiso 1 calc . .
H5B H 0.5104 0.4733 0.6636 0.037 Uiso 1 calc . .
C6 C 0.0185(7) 0.4254(4) 0.7906(4) 0.0314(8) Uani 1 d . .
H6A H 0.0255 0.525 0.8114 0.038 Uiso 1 calc . .
H6B H -0.135 0.3769 0.7574 0.038 Uiso 1 calc . .
O12 O 0.0504(14) 0.0596(8) 1.1153(7) 0.0523(17) Uani 0.5 d A 1
H12A H 0.11(2) 0.159(3) 1.132(12) 0.079 Uiso 0.5 d B 1
H12B H 0.12(2) 0.015(11) 1.053(9) 0.079 Uiso 0.5 d C 1
C7 C 0.439(2) 0.0100(15) 0.9437(12) 0.036(3) Uani 0.5 d D 1
H7A H 0.4872 -0.0394 0.874 0.044 Uiso 0.5 calc D 1
H7B H 0.2777 -0.0284 0.944 0.044 Uiso 0.5 calc D 1
N1 N 0.4878(13) 0.1615(8) 0.9369(7) 0.0380(16) Uani 0.5 d D 1
H1A H 0.4427 0.2063 1.0009 0.057 Uiso 0.5 calc D 1
H1B H 0.4147 0.1741 0.87 0.057 Uiso 0.5 calc D 1
H1C H 0.6357 0.196 0.9355 0.057 Uiso 0.5 calc D 1
C8 C 0.536(2) 0.0231(16) 0.9421(13) 0.042(3) Uani 0.5 d E 2
H8A H 0.4153 -0.017 0.8775 0.051 Uiso 0.5 calc E 2
H8B H 0.5705 0.1252 0.95 0.051 Uiso 0.5 calc E 2
N2 N 0.2629(15) 0.0255(8) 1.0854(7) 0.0425(18) Uani 0.5 d F 2
H2A H 0.2161 -0.0027 1.1533 0.064 Uiso 0.5 calc F 2
H2B H 0.1537 -0.0107 1.0251 0.064 Uiso 0.5 calc F 2
H2C H 0.297 0.1195 1.0944 0.064 Uiso 0.5 calc F 2
H5C H 0.229(10) 1.011(5) 0.635(6) 0.064 Uiso 1 d . .
H5D H 0.468(3) 0.966(7) 0.633(6) 0.064 Uiso 1 d . .
H11A H 0.800(11) 0.884(5) 0.634(6) 0.064 Uiso 1 d . .
H11B H 0.816(6) 1.016(6) 0.593(4) 0.064 Uiso 1 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 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_1
_geom_angle_site_symmetry_3
O4 U1 O2 176.72(14) . .
O4 U1 O6 90.19(14) . .
O2 U1 O6 89.13(14) . .
O4 U1 O1 91.12(13) . .
O2 U1 O1 91.80(13) . .
O6 U1 O1 75.18(10) . .
O4 U1 O7 92.46(14) . .
O2 U1 O7 86.48(14) . .
O6 U1 O7 148.84(11) . .
O1 U1 O7 135.74(10) . .
O4 U1 O5 84.65(14) . .
O2 U1 O5 92.08(14) . .
O6 U1 O5 76.25(11) . .
O1 U1 O5 151.09(10) . .
O7 U1 O5 73.11(11) . .
O1 U1 O5 139.00(10) 2_566 .
O4 U1 U1 90.76(11) . 2_566
O2 U1 U1 92.49(11) . 2_566
O6 U1 U1 109.96(8) . 2_566
O1 U1 U1 34.78(6) . 2_566
O7 U1 U1 101.04(7) . 2_566
O1 U1 U1 34.60(6) 2_566 2_566
O5 U1 U1 172.35(8) . 2_566
C3 O1 U1 128.1(2) . .
C3 O1 U1 120.6(2) . 2_566
U1 O1 U1 110.61(10) . 2_566
U1 O5 H5C 123(4) . .
U1 O5 H5D 115(4) . .
H5C O5 H5D 122(6) . .
C2 O6 U1 136.2(3) . .
C1 O7 U1 123.9(3) . .
C4 O8 H8 109.5 . .
H11A O11 H11B 98(5) . .
O9 C1 O7 122.9(4) . .
O9 C1 C3 121.5(4) . 2_566
O7 C1 C3 115.5(3) . 2_566
O3 C2 O6 121.6(4) . .
O3 C2 C5 119.2(4) . .
O6 C2 C5 119.2(4) . .
O1 C3 C5 110.7(3) . .
O1 C3 C1 109.8(3) . 2_566
C5 C3 C1 107.0(3) . 2_566
O1 C3 C6 107.8(3) . .
C5 C3 C6 114.2(3) . .
C1 C3 C6 107.2(3) 2_566 .
O10 C4 O8 123.2(4) . .
O10 C4 C6 123.9(4) . .
O8 C4 C6 112.9(4) . .
C2 C5 C3 114.7(3) . .
C2 C5 H5A 108.6 . .
C3 C5 H5A 108.6 . .
C2 C5 H5B 108.6 . .
C3 C5 H5B 108.6 . .
H5A C5 H5B 107.6 . .
C4 C6 C3 114.6(3) . .
C4 C6 H6A 108.6 . .
C3 C6 H6A 108.6 . .
C4 C6 H6B 108.6 . .
C3 C6 H6B 108.6 . .
H6A C6 H6B 107.6 . .
H12A O12 H12B 114(5) . .
N1 C7 C7 109.1(13) . 2_657
N1 C7 H7A 109.9 . .
C7 C7 H7A 109.9 2_657 .
N1 C7 H7B 109.9 . .
C7 C7 H7B 109.9 2_657 .
H7A C7 H7B 108.3 . .
C7 N1 H1A 109.5 . .
C7 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C7 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
N2 C8 C8 108.3(15) 2_657 2_657
N2 C8 H8A 110 2_657 .
C8 C8 H8A 110 2_657 .
N2 C8 H8B 110 2_657 .
C8 C8 H8B 110 2_657 .
H8A C8 H8B 108.4 . .
C8 N2 H2A 109.5 2_657 .
C8 N2 H2B 109.5 2_657 .
H2A N2 H2B 109.5 . .
C8 N2 H2C 109.5 2_657 .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O4 1.775(3) .
U1 O2 1.786(3) .
U1 O6 2.335(3) .
U1 O1 2.370(3) .
U1 O7 2.375(3) .
U1 O5 2.413(3) .
O1 C3 1.412(4) .
O3 C2 1.251(5) .
O5 H5C 0.95(2) .
O5 H5D 0.943(19) .
O6 C2 1.271(5) .
O7 C1 1.275(5) .
O8 C4 1.310(5) .
O8 H8 0.83 .
O9 C1 1.234(5) .
O10 C4 1.204(6) .
O11 H11A 0.96(2) .
O11 H11B 0.96(2) .
C1 C3 1.540(5) 2_566
C2 C5 1.503(6) .
C3 C5 1.540(5) .
C3 C6 1.557(6) .
C4 C6 1.508(5) .
C5 H5A 0.98 .
C5 H5B 0.98 .
C6 H6A 0.98 .
C6 H6B 0.98 .
O12 H12A 0.96(2) .
O12 H12B 0.96(2) .
C7 N1 1.483(16) .
C7 C7 1.51(3) 2_657
C7 H7A 0.98 .
C7 H7B 0.98 .
N1 H1A 0.9 .
N1 H1B 0.9 .
N1 H1C 0.9 .
C8 N2 1.485(16) 2_657
C8 C8 1.51(3) 2_657
C8 H8A 0.98 .
C8 H8B 0.98 .
N2 H2A 0.9 .
N2 H2B 0.9 .
N2 H2C 0.9 .
