#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/91/2239185.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2239185
loop_
_publ_author_name
'Cantos, Paula M.'
'Cahill, Christopher L.'
_publ_section_title
;
 Poly[diammonium
 [diaqua(μ₇-benzene-1,2,3,4,5,6-hexacarboxylato)tetraoxidodiuranium(VI)]]
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m142
_journal_page_last               m143
_journal_paper_doi               10.1107/S1600536814006047
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(N H4)2 [(U O2)2 (C12 O12) (H2 O)2]'
_chemical_formula_moiety         '2H4 N +, 2C6 H2 O9 U -'
_chemical_formula_sum            'C12 H12 N2 O18 U2'
_chemical_formula_weight         948.2874
_chemical_name_systematic
;
Poly[diammonium
[diaqua(μ₇-benzene-1,2,3,4,5,6-hexacarboxylato)tetraoxidodiuranium(VI)]]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 99.7330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0083(4)
_cell_length_b                   10.2948(6)
_cell_length_c                   11.7481(6)
_cell_measurement_reflns_used    18686
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.584
_cell_measurement_theta_min      6.968
_cell_volume                     954.62(9)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
;
CrystalMaker (CrystalMaker, 2009) and
ORTEP-3 (Burnett & Johnson  1996)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18160
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    17.048
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.984
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0125P)²+1.2966P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0333
_refine_ls_wR_factor_ref         0.0347
_reflns_number_gt                2398
_reflns_number_total             2912
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg2133sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2239185
_cod_database_fobs_code          2239185
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'
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_occupancy
_atom_site_symmetry_multiplicity
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_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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
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_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_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
