#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/06/4500686.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_4500686
loop_
_publ_author_name
'Mihalcea, Ionut'
'Henry, Natacha'
'Loiseau, Thierry'
_publ_section_title
;
 Revisiting the Uranyl-phthalate System: Isolation and Crystal Structures
 of Two Types of Uranyl−Organic Frameworks (UOF)
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1940
_journal_paper_doi               10.1021/cg200106j
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C12 H9 O11 U1.5'
_chemical_formula_weight         686.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   30.5385(7)
_cell_length_b                   30.5385(7)
_cell_length_c                   5.8489(2)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.14
_cell_measurement_theta_min      2.31
_cell_volume                     4723.9(2)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART/SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            97670
_diffrn_reflns_theta_full        35.93
_diffrn_reflns_theta_max         35.93
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    15.483
_exptl_absorpt_correction_T_max  0.3706
_exptl_absorpt_correction_T_min  0.0354
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3684
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.610
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.310
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0187P)²+55.8897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                3910
_reflns_number_total             4662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200106j_si_003.cif
_cod_data_source_block           uft006
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C12 H9 O11 U1.50'
_cod_database_code               4500686
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U1 U 0.619797(5) 0.161322(5) 0.97126(2) 0.01750(4) Uani 1 1 d .
O1 O 0.63471(11) 0.21596(11) 0.8086(5) 0.0243(6) Uani 1 1 d .
O2 O 0.60511(13) 0.10691(13) 1.1315(6) 0.0322(7) Uani 1 1 d .
O3 O 0.66224(12) 0.13635(11) 0.6985(5) 0.0251(6) Uani 1 1 d .
O4 O 0.54429(10) 0.15692(12) 1.0997(5) 0.0226(5) Uani 1 1 d .
O5 O 0.70405(11) 0.19871(12) 1.0998(5) 0.0233(5) Uani 1 1 d .
O6 O 0.55653(12) 0.10891(12) 0.6996(5) 0.0258(6) Uani 1 1 d .
O7 O 0.63422(19) 0.2148(2) 1.3152(8) 0.0502(14) Uani 1 1 d .
H1O7 H 0.652(3) 0.224(3) 1.357(15) 0.05(3) Uiso 1 1 d .
H2O7 H 0.617(3) 0.212(3) 1.401(13) 0.05(2) Uiso 1 1 d .
C1 C 0.49667(13) 0.12987(14) 1.0923(6) 0.0164(6) Uani 1 1 d .
C2 C 0.52867(14) 0.11822(14) 0.5755(6) 0.0173(6) Uani 1 1 d .
C3 C 0.48826(14) 0.07561(14) 0.4409(6) 0.0180(6) Uani 1 1 d .
C4 C 0.47071(14) 0.08203(14) 1.2272(6) 0.0191(6) Uani 1 1 d .
C5 C 0.42995(16) 0.04060(16) 1.1226(8) 0.0270(8) Uani 1 1 d .
H5 H 0.4180 0.0447 0.9828 0.032 Uiso 1 1 calc R
C6 C 0.46479(17) 0.02766(16) 0.5424(8) 0.0269(8) Uani 1 1 d .
H6 H 0.4765 0.0231 0.6820 0.032 Uiso 1 1 calc R
C7 C 0.7706(2) 0.0909(2) 0.2300(10) 0.0360(11) Uani 1 1 d .
H7 H 0.7864 0.0751 0.1599 0.043 Uiso 1 1 calc R
C8 C 0.7471(2) 0.0738(2) 0.4415(10) 0.0391(11) Uani 1 1 d .
H8 H 0.7479 0.0470 0.5139 0.047 Uiso 1 1 calc R
OW1 O 0.6668(2) 0.3334(2) 0.6704(10) 0.165(15) Uiso 0.50 3 d SPR
OW2 O 0.6668(2) 0.3334(2) 1.3963(10) 0.32(3) Uiso 0.50 3 d SPR
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 U1 O1 179.66(17) . .
O2 U1 O5 89.35(13) . .
O1 U1 O5 90.61(12) . .
O2 U1 O4 89.78(14) . .
O1 U1 O4 90.47(12) . .
O5 U1 O4 136.38(10) . .
O2 U1 O6 89.01(14) . .
O1 U1 O6 90.85(12) . .
O5 U1 O6 148.96(11) . .
O4 U1 O6 74.61(11) . .
O2 U1 O3 88.70(14) . .
O1 U1 O3 90.97(12) . .
O5 U1 O3 74.61(11) . .
O4 U1 O3 148.96(11) . .
O6 U1 O3 74.37(11) . .
O2 U1 O7 93.83(19) . .
O1 U1 O7 86.47(18) . .
O5 U1 O7 68.39(13) . .
O4 U1 O7 68.16(13) . .
O6 U1 O7 142.64(13) . .
O3 U1 O7 142.86(13) . .
C1 O3 U1 129.6(2) 18_546 .
C1 O4 U1 142.9(3) . .
C2 O5 U1 143.6(3) 18_546 .
C2 O6 U1 130.2(3) . .
O3 C1 O4 122.5(3) 17_556 .
O3 C1 C4 117.7(3) 17_556 .
O4 C1 C4 119.8(3) . .
O6 C2 O5 123.1(4) . 17_556
O6 C2 C3 117.8(3) . .
O5 C2 C3 119.1(3) 17_556 .
C6 C3 C4 119.3(4) . 1_554
C6 C3 C2 117.1(3) . .
C4 C3 C2 123.5(3) 1_554 .
C5 C4 C3 119.4(4) . 1_556
C5 C4 C1 116.9(3) . .
C3 C4 C1 123.4(3) 1_556 .
C8 C5 C4 120.7(4) 17_556 .
C7 C6 C3 120.6(4) 17 .
C6 C7 C8 120.0(4) 18_545 .
C5 C8 C7 120.0(4) 18_546 .
OW2 OW2 OW1 179.5(15) 16_657 1_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.760(3) .
U1 O1 1.771(3) .
U1 O5 2.356(3) .
U1 O4 2.364(3) .
U1 O6 2.393(3) .
U1 O3 2.408(3) .
U1 O7 2.487(4) .
O3 C1 1.262(4) 18_546
O4 C1 1.264(4) .
O5 C2 1.269(4) 18_546
O6 C2 1.254(4) .
C1 O3 1.261(4) 17_556
C1 C4 1.492(5) .
C2 O5 1.269(4) 17_556
C2 C3 1.493(5) .
C3 C6 1.400(5) .
C3 C4 1.412(5) 1_554
C4 C5 1.396(5) .
C4 C3 1.412(5) 1_556
C5 C8 1.387(7) 17_556
C6 C7 1.386(7) 17
C7 C6 1.386(7) 18_545
C7 C8 1.394(8) .
C8 C5 1.387(7) 18_546
OW1 OW2 1.6032 1_554
OW2 OW2 0.736(12) 16_657
OW2 OW1 1.6032 1_556
