#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/31/2203187.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_2203187
loop_
_publ_author_name
'Borkowski, Lauren A.'
'Cahill, Christopher L.'
_publ_section_title
;
 A novel uranium-containing coordination polymer:
 poly[[aqua(benzene-1,3,5-tricarboxylato)dioxouranium(VI)] monohydrate]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m198
_journal_page_last               m200
_journal_paper_doi               10.1107/S1600536804000765
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[U O2 (C9 H4 O6) (H2 O)] , H2 O'
_chemical_formula_moiety         'C9 H6 O9 U , H2 O'
_chemical_formula_sum            'C9 H8 O10 U'
_chemical_formula_weight         514.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                70.507(5)
_cell_angle_beta                 75.840(5)
_cell_angle_gamma                87.002(5)
_cell_formula_units_Z            2
_cell_length_a                   7.8342(6)
_cell_length_b                   8.3781(7)
_cell_length_c                   10.6208(9)
_cell_measurement_reflns_used    1478
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.58
_cell_volume                     636.85(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'CrystalMaker (CrystalMaker, 2003)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω and φ'
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4649
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    12.792
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.681
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       blade
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.685
_refine_diff_density_min         -2.010
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2589
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0071P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                2237
_reflns_number_total             2589
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fl6076.cif
_cod_data_source_block           I
_cod_database_code               2203187
_cod_database_fobs_code          2203187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_type_symbol
U1 0.24849(4) 0.25189(4) 0.08559(3) 0.02078(11) Uani d . 1 U
O1 0.4334(8) 0.0295(7) 0.1976(6) 0.0297(15) Uani d . 1 O
O2 0.1934(7) 0.0812(8) 0.3316(6) 0.0339(16) Uani d . 1 O
O3 -0.0131(8) 0.3489(8) 0.1875(6) 0.0432(19) Uani d . 1 O
O4 0.2020(8) 0.4606(8) -0.1103(6) 0.0351(16) Uani d . 1 O
O5 0.8047(8) -0.5209(9) 0.6103(7) 0.0457(19) Uani d . 1 O
O6 0.8856(8) -0.3290(9) 0.3991(7) 0.052(2) Uani d . 1 O
H6 0.9805 -0.3751 0.4002 0.078 Uiso calc R 1 H
O7 0.1358(8) 0.1032(8) 0.0503(7) 0.0353(16) Uani d . 1 O
O8 0.4990(8) 0.2256(8) -0.0875(6) 0.0288(15) Uani d D 1 O
H8A 0.513(12) 0.138(8) -0.130(8) 0.043 Uiso d D 1 H
H8B 0.620(5) 0.241(11) -0.087(9) 0.043 Uiso d D 1 H
O9 0.3644(8) 0.3989(8) 0.1189(6) 0.0317(15) Uani d . 1 O
C1 0.3807(10) -0.1340(10) 0.4361(9) 0.0235(19) Uani d . 1 C
C2 0.2544(10) -0.2004(10) 0.5598(8) 0.023(2) Uani d . 1 C
H2 0.1426 -0.1558 0.5712 0.028 Uiso calc R 1 H
C3 0.2971(10) 0.6665(10) -0.3342(8) 0.0227(19) Uani d . 1 C
C4 0.4657(10) 0.6026(10) -0.3508(8) 0.0225(19) Uani d . 1 C
H4 0.4936 0.5124 -0.2802 0.027 Uiso calc R 1 H
C5 0.5921(10) -0.3268(11) 0.5277(9) 0.0229(19) Uani d . 1 C
C6 0.5475(10) -0.1977(10) 0.4211(8) 0.0216(19) Uani d . 1 C
H6A 0.6310 -0.1533 0.3383 0.026 Uiso calc R 1 H
C7 0.3328(11) -0.0009(11) 0.3180(9) 0.025(2) Uani d . 1 C
C8 0.1622(10) 0.5880(11) -0.2000(9) 0.0219(19) Uani d . 1 C
C9 0.7732(11) -0.4005(12) 0.5148(9) 0.029(2) Uani d . 1 C
OW1 0.1760(11) 0.7387(10) 0.0735(11) 0.077(3) Uani d D 1 O
HW1 0.097(14) 0.829(12) 0.044(14) 0.115 Uiso d D 1 H
HW2 0.170(18) 0.627(8) 0.143(10) 0.115 Uiso d D 1 H
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O9 U1 O7 . . 178.9(3) yes
O9 U1 O3 . . 89.5(3) ?
O7 U1 O3 . . 91.6(3) ?
O9 U1 O4 . . 89.9(3) ?
O7 U1 O4 . . 90.1(3) ?
O3 U1 O4 . . 82.2(2) ?
O9 U1 O8 . . 90.6(2) ?
O7 U1 O8 . . 88.3(3) ?
O3 U1 O8 . . 160.3(2) ?
O4 U1 O8 . . 78.0(2) ?
O9 U1 O1 . . 88.6(3) ?
O7 U1 O1 . . 90.9(2) ?
O3 U1 O1 . . 127.8(2) ?
O4 U1 O1 . . 149.88(19) ?
O8 U1 O1 . . 71.89(19) ?
O9 U1 O2 . . 88.3(2) ?
O7 U1 O2 . . 92.1(3) ?
O3 U1 O2 . . 75.2(2) ?
O4 U1 O2 . . 157.42(19) ?
O8 U1 O2 . . 124.5(2) ?
O1 U1 O2 . . 52.59(18) ?
O9 U1 C7 . . 88.0(3) ?
O7 U1 C7 . . 92.0(3) ?
O3 U1 C7 . . 101.4(2) ?
O4 U1 C7 . . 175.8(2) ?
O8 U1 C7 . . 98.3(2) ?
O1 U1 C7 . . 26.4(2) ?
O2 U1 C7 . . 26.1(2) ?
C7 O1 U1 . . 94.4(5) ?
C7 O2 U1 . . 94.6(5) ?
C8 O3 U1 2_565 . 159.3(6) ?
C8 O4 U1 . . 168.7(6) ?
C9 O6 H6 . . 109.5 ?
U1 O8 H8A . . 126(5) ?
U1 O8 H8B . . 125(5) ?
H8A O8 H8B . . 100(7) ?
C6 C1 C2 . . 120.0(8) ?
C6 C1 C7 . . 119.9(7) ?
C2 C1 C7 . . 120.0(7) ?
C3 C2 C1 1_546 . 119.4(7) ?
C3 C2 H2 1_546 . 120.3 ?
C1 C2 H2 . . 120.3 ?
C2 C3 C4 1_564 . 120.1(7) ?
C2 C3 C8 1_564 . 121.0(7) ?
C4 C3 C8 . . 118.9(7) ?
C5 C4 C3 1_564 . 120.0(8) ?
C5 C4 H4 1_564 . 120.0 ?
C3 C4 H4 . . 120.0 ?
C6 C5 C4 . 1_546 119.6(7) ?
C6 C5 C9 . . 122.3(7) ?
C4 C5 C9 1_546 . 118.1(8) ?
C1 C6 C5 . . 120.8(8) ?
C1 C6 H6A . . 119.6 ?
C5 C6 H6A . . 119.6 ?
O2 C7 O1 . . 118.4(8) ?
O2 C7 C1 . . 122.4(8) ?
O1 C7 C1 . . 119.2(7) ?
O2 C7 U1 . . 59.3(4) ?
O1 C7 U1 . . 59.2(4) ?
C1 C7 U1 . . 178.3(6) ?
O3 C8 O4 2_565 . 123.6(8) ?
O3 C8 C3 2_565 . 117.2(7) ?
O4 C8 C3 . . 119.1(7) ?
O5 C9 O6 . . 124.8(8) ?
O5 C9 C5 . . 120.0(8) ?
O6 C9 C5 . . 115.2(8) ?
HW1 OW1 HW2 . . 139(10) ?
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 O9 . 1.741(6) yes
U1 O7 . 1.750(6) yes
U1 O3 . 2.315(5) yes
U1 O4 . 2.323(6) yes
U1 O8 . 2.396(5) yes
U1 O1 . 2.463(6) yes
U1 O2 . 2.465(6) yes
U1 C7 . 2.859(9) ?
O1 C7 . 1.277(9) ?
O2 C7 . 1.264(9) ?
O3 C8 2_565 1.252(9) ?
O4 C8 . 1.255(10) ?
O5 C9 . 1.233(10) ?
O6 C9 . 1.296(10) ?
O6 H6 . 0.8200 ?
O8 H8A . 0.97(7) ?
O8 H8B . 0.97(5) ?
C1 C6 . 1.378(10) ?
C1 C2 . 1.396(11) ?
C1 C7 . 1.487(12) ?
C2 C3 1_546 1.389(11) ?
C2 H2 . 0.9300 ?
C3 C2 1_564 1.389(11) ?
C3 C4 . 1.393(10) ?
C3 C8 . 1.514(11) ?
C4 C5 1_564 1.387(11) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.382(11) ?
C5 C4 1_546 1.387(11) ?
C5 C9 . 1.511(11) ?
C6 H6A . 0.9300 ?
C8 O3 2_565 1.252(9) ?
OW1 HW1 . 0.97(11) ?
OW1 HW2 . 0.97(9) ?
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
O8 H8A O1 2_655 0.97(7) 1.77(7) 2.732(8) 172(9) yes
O8 H8B OW1 2_665 0.97(5) 1.66(5) 2.624(10) 176(9) yes
O6 H6 O5 2_746 0.82 1.85 2.669(8) 176 yes
OW1 HW1 O7 2_565 0.97(11) 2.25(8) 3.086(10) 144(11) yes
OW1 HW1 O7 1_565 0.97(11) 2.36(11) 2.987(10) 122(10) yes
OW1 HW2 O9 . 0.97(9) 2.42(11) 3.083(10) 125(10) yes
OW1 HW2 O5 2_656 0.97(9) 2.53(10) 3.280(12) 134(10) yes
OW1 HW2 O3 . 0.97(9) 2.64(10) 3.363(11) 131(10) yes
