##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section E. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_database_code_depnum_ccdc_archive 'CCDC 992448'
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Poly[diammonium
[diaqua(μ₇-benzene-1,2,3,4,5,6-hexacarboxylato)tetraoxidodiuranium(VI)]]
;
_chemical_name_common     ?
_chemical_formula_moiety     '2H4 N +, 2C6 H2 O9 U -'
_chemical_formula_sum     'C12 H12 N2 O18 U2'
_chemical_formula_iupac     '(N H4)2 [(U O2)2 (C12 O12) (H2 O)2]'
_chemical_formula_weight     948.2874
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/c'
_symmetry_space_group_name_Hall     '-P 2ybc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y-1/2, z-1/2'
_cell_length_a     8.0083(4)
_cell_length_b     10.2948(6)
_cell_length_c     11.7481(6)
_cell_angle_alpha     90.00
_cell_angle_beta     99.7330(10)
_cell_angle_gamma     90.00
_cell_volume     954.62(9)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     18686
_cell_measurement_theta_min     6.968
_cell_measurement_theta_max     60.584
_cell_measurement_temperature     100(2)
_exptl_crystal_description     rods
_exptl_crystal_colour     yellow
_exptl_crystal_size_max     0.4
_exptl_crystal_size_mid     0.3
_exptl_crystal_size_min     0.2
_exptl_crystal_density_diffrn     3.299
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     852
_exptl_absorpt_coefficient_mu     17.048
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1999)'
_exptl_absorpt_correction_T_min     0.4669
_exptl_absorpt_correction_T_max     0.7461
_exptl_special_details     ?
_diffrn_ambient_temperature     100(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker APEXII CCD'
_diffrn_measurement_method     'omega scans'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     18160
_diffrn_reflns_av_R_equivalents     0.0363
_diffrn_reflns_av_sigmaI/netI     0.0247
_diffrn_reflns_theta_min     2.65
_diffrn_reflns_theta_max     30.47
_diffrn_reflns_theta_full     25.00
_diffrn_measured_fraction_theta_max     0.927
_diffrn_measured_fraction_theta_full     0.993
_diffrn_reflns_limit_h_min     -11
_diffrn_reflns_limit_h_max     8
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     14
_diffrn_reflns_limit_l_min     -16
_diffrn_reflns_limit_l_max     16
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_refine_special_details
;
Refinement of F² against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F², conventional
R-factors R are based on F, with F set to zero for
negative F². The threshold expression of F² >
2σ(F²) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F² are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total     2912
_reflns_number_gt     2398
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0213
_refine_ls_R_factor_gt     0.0166
_refine_ls_wR_factor_gt     0.0333
_refine_ls_wR_factor_ref     0.0347
_refine_ls_goodness_of_fit_ref     1.044
_refine_ls_restrained_S_all     1.044
_refine_ls_number_reflns     2698
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0125P)²+1.2966P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.024
_refine_diff_density_min     -0.984
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    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'
    N N 0.0061 0.0033 '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'
_computing_data_collection     'APEX2 (Bruker, 2008)'
_computing_cell_refinement     'SAINT (Bruker, 2008)'
_computing_data_reduction     'SAINT (Bruker, 2008)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics
;
CrystalMaker (CrystalMaker, 2009) and
ORTEP-3 (Burnett & Johnson  1996)
;
_computing_publication_material     'WinGX (Farrugia, 2012)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_symmetry_multiplicity
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    U U1 0.412520(13) 0.721169(10) 0.152007(9) 0.00526(4) Uani d . 1 1 . .
    O O1 0.5032(3) 0.5786(2) 0.10655(18) 0.0103(4) Uani d . 1 1 . .
    O O2 0.3232(3) 0.8648(2) 0.19911(18) 0.0091(4) Uani d . 1 1 . .
    O O3 0.2643(3) 0.6031(2) 0.28641(18) 0.0082(4) Uani d . 1 1 . .
    O O5 0.1465(3) 0.6550(2) 0.05335(18) 0.0083(4) Uani d . 1 1 . .
    O O4 0.3585(3) 0.7973(2) -0.04722(18) 0.0096(4) Uani d . 1 1 . .
    O O8 0.6415(3) 0.8435(2) 0.10897(18) 0.0112(4) Uani d . 1 1 . .
    O O9 0.6149(3) 0.7076(2) 0.3302(2) 0.0125(5) Uani d . 1 1 . .
    O O7 0.8885(3) 0.7764(2) 0.21059(19) 0.0112(4) Uani d . 1 1 . .
    O O6 -0.1157(3) 0.6646(2) -0.04255(18) 0.0093(4) Uani d . 1 1 . .
    C C1 0.2569(4) 0.6268(3) 0.3903(2) 0.0065(6) Uani d . 1 1 . .
    C C2 0.1216(4) 0.5613(3) 0.4453(2) 0.0050(5) Uani d . 1 1 . .
    C C3 0.0179(4) 0.6342(3) 0.5063(2) 0.0054(5) Uani d . 1 1 . .
    C C5 0.8015(4) 0.8427(3) 0.1337(2) 0.0069(5) Uani d . 1 1 . .
    C C4 0.1018(4) 0.4272(3) 0.4383(2) 0.0064(6) Uani d . 1 1 . .
    C C6 0.0162(4) 0.7181(3) 0.0055(2) 0.0065(5) Uani d . 1 1 . .
    N N1 0.8845(4) 0.5051(3) 0.1615(3) 0.0107(5) Uani d . 1 1 . .
    H H1 0.852(5) 0.507(4) 0.089(4) 0.022(11) Uiso d . 1 1 . .
    H H2 0.980(6) 0.463(4) 0.185(4) 0.031(13) Uiso d . 1 1 . .
    H H3 0.813(6) 0.468(4) 0.190(4) 0.030(13) Uiso d . 1 1 . .
    H H4 0.905(6) 0.590(5) 0.190(4) 0.035(13) Uiso d . 1 1 . .
    H H6 0.571(6) 0.706(4) 0.381(4) 0.031(14) Uiso d . 1 1 . .
    H H5 0.716(7) 0.748(5) 0.355(4) 0.041(14) Uiso d . 1 1 . .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    U1 0.00418(6) 0.00674(6) 0.00524(5) -0.00009(4) 0.00189(4) 0.00013(4)
    O1 0.0106(11) 0.0116(11) 0.0092(10) 0.0035(9) 0.0032(8) 0.0001(8)
    O2 0.0094(11) 0.0093(11) 0.0096(10) -0.0007(8) 0.0045(8) -0.0028(8)
    O3 0.0085(11) 0.0096(10) 0.0069(10) -0.0019(8) 0.0023(8) -0.0015(8)
    O5 0.0059(10) 0.0079(10) 0.0106(10) 0.0008(8) -0.0001(8) 0.0004(8)
    O4 0.0090(11) 0.0132(11) 0.0073(10) 0.0058(8) 0.0034(8) 0.0035(8)
    O8 0.0062(11) 0.0136(11) 0.0141(11) -0.0020(9) 0.0027(8) 0.0039(9)
    O9 0.0083(12) 0.0229(14) 0.0068(11) -0.0051(10) 0.0026(9) 0.0000(9)
    O7 0.0112(11) 0.0108(11) 0.0118(11) 0.0005(9) 0.0029(9) 0.0057(9)
    O6 0.0091(11) 0.0083(10) 0.0103(10) 0.0009(9) 0.0011(8) 0.0003(9)
    C1 0.0055(14) 0.0061(14) 0.0081(13) 0.0026(11) 0.0014(11) 0.0018(10)
    C2 0.0024(13) 0.0100(14) 0.0027(12) -0.0001(11) 0.0005(10) -0.0005(10)
    C3 0.0047(13) 0.0054(13) 0.0055(13) 0.0001(10) -0.0005(10) -0.0001(10)
    C5 0.0099(14) 0.0047(13) 0.0074(13) -0.0004(11) 0.0056(11) -0.0023(11)
    C4 0.0040(14) 0.0094(14) 0.0061(13) 0.0015(11) 0.0016(10) -0.0001(11)
    C6 0.0062(14) 0.0082(14) 0.0065(13) -0.0007(11) 0.0048(10) 0.0005(11)
    N1 0.0113(15) 0.0110(14) 0.0108(14) 0.0006(11) 0.0045(11) 0.0019(11)
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are
estimated using the full covariance matrix. The cell s.u.'s are taken into
account individually in the estimation of s.u.'s in distances, angles and
torsion angles; correlations between s.u.'s in cell parameters are only used
when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    U1 O1 . 1.760(2) ?
    U1 O2 . 1.771(2) ?
    U1 O5 . 2.348(2) ?
    U1 O8 . 2.349(2) ?
    U1 O9 . 2.425(2) ?
    U1 O4 . 2.437(2) ?
    U1 O3 . 2.452(2) ?
    O3 C1 . 1.256(4) ?
    O5 C6 . 1.276(4) ?
    O4 C1 4_575 1.269(3) ?
    O8 C5 . 1.264(4) ?
    O7 C5 . 1.247(4) ?
    O6 C6 . 1.240(4) ?
    C1 O4 4_576 1.269(4) ?
    C1 C2 . 1.510(4) ?
    C2 C4 . 1.391(4) ?
    C2 C3 . 1.402(4) ?
    C3 C4 3_566 1.397(4) ?
    C3 C6 4_576 1.520(4) ?
    C5 C4 2_655 1.514(4) ?
    C4 C3 3_566 1.397(4) ?
    C4 C5 2_645 1.514(4) ?
    C6 C3 4_575 1.520(4) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 U1 O2 . . 179.34(10) ?
    O1 U1 O5 . . 89.70(9) ?
    O2 U1 O5 . . 90.90(9) ?
    O1 U1 O8 . . 90.27(9) ?
    O2 U1 O8 . . 89.48(9) ?
    O5 U1 O8 . . 136.52(7) ?
    O1 U1 O9 . . 87.94(9) ?
    O2 U1 O9 . . 91.41(9) ?
    O5 U1 O9 . . 145.87(8) ?
    O8 U1 O9 . . 77.55(8) ?
    O1 U1 O4 . . 89.55(8) ?
    O2 U1 O4 . . 90.93(8) ?
    O5 U1 O4 . . 67.67(7) ?
    O8 U1 O4 . . 68.85(7) ?
    O9 U1 O4 . . 146.29(8) ?
    O1 U1 O3 . . 92.95(9) ?
    O2 U1 O3 . . 86.99(8) ?
    O5 U1 O3 . . 71.12(7) ?
    O8 U1 O3 . . 152.22(7) ?
    O9 U1 O3 . . 75.01(8) ?
    O4 U1 O3 . . 138.70(7) ?
    C1 O3 U1 . . 129.60(19) ?
    C6 O5 U1 . . 132.53(19) ?
    C1 O4 U1 4_575 . 138.25(19) ?
    C5 O8 U1 . . 138.1(2) ?
    O3 C1 O4 . 4_576 123.4(3) ?
    O3 C1 C2 . . 119.0(3) ?
    O4 C1 C2 4_576 . 117.6(2) ?
    C4 C2 C3 . . 119.3(3) ?
    C4 C2 C1 . . 120.1(3) ?
    C3 C2 C1 . . 120.6(3) ?
    C4 C3 C2 3_566 . 120.5(3) ?
    C4 C3 C6 3_566 4_576 116.7(2) ?
    C2 C3 C6 . 4_576 122.5(3) ?
    O7 C5 O8 . . 126.2(3) ?
    O7 C5 C4 . 2_655 116.3(3) ?
    O8 C5 C4 . 2_655 117.5(3) ?
    C2 C4 C3 . 3_566 120.1(3) ?
    C2 C4 C5 . 2_645 122.6(3) ?
    C3 C4 C5 3_566 2_645 117.2(3) ?
    O6 C6 O5 . . 123.0(3) ?
    O6 C6 C3 . 4_575 117.0(3) ?
    O5 C6 C3 . 4_575 120.0(3) ?
loop_
    _geom_hbond_atom_site_label_d
    _geom_hbond_atom_site_label_h
    _geom_hbond_atom_site_label_a
    _geom_hbond_site_symmetry_d
    _geom_hbond_site_symmetry_h
    _geom_hbond_site_symmetry_a
    _geom_hbond_distance_dh
    _geom_hbond_distance_ha
    _geom_hbond_distance_da
    _geom_hbond_angle_dha
    _geom_hbond_publ_flag
    O9 H6 O4 ? ? 4_576 0.74(5) 2.02(5) 2.700(3) 152(5) yes
    O9 H5 O6 . . 4_676 0.91(6) 1.88(5) 2.744(3) 158(4) yes
    O9 H5 O7 . . . 0.91(6) 2.38(5) 2.884(3) 115(4) yes
    N1 H3 O2 . . 2_645 0.81(5) 2.12(5) 2.908(4) 165(5) yes
    N1 H1 O5 . . 3_665 0.85(4) 2.36(4) 2.990(4) 131(3) yes
    N1 H1 O6 . . 1_655 0.85(4) 2.29(4) 2.905(4) 130(3) yes
    N1 H4 O7 . . . 0.94(5) 1.94(5) 2.851(4) 162(5) yes
data_publication_text
_journal_date_recd_electronic     2013-12-17
_journal_date_accepted     2014-03-18
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2014
_journal_volume     70
_journal_issue      4
_journal_page_first     m142
_journal_page_last     m143
_journal_paper_category     QM
_journal_paper_doi     10.1107/S1600536814006047
_journal_coeditor_code     GG2133
_publ_contact_author_name     'Christopher L. Cahill'
_publ_contact_author_address
;
725 21st St. N.W. Washington, D.C. 20052 USA
;
_publ_contact_author_email     'cahill@gwu.edu'
_publ_contact_author_fax     '(202)994-5873'
_publ_contact_author_phone     '(202)994-6959'
_publ_section_title
;
Poly[diammonium
[diaqua(μ₇-benzene-1,2,3,4,5,6-hexacarboxylato)tetraoxidodiuranium(VI)]]
;
_publ_section_title_footnote     .
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Cantos, Paula M.' .
;
Department of Chemistry
The George Washington University
725 21st St NW
Washington, DC 20052
USA
;
    'Cahill, Christopher L.' .
;
Department of Chemistry
The George Washington University
725 21st St NW
Washington, DC 20052
USA
;
_publ_section_synopsis     .
