#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:35:18 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179537 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/06/4500685.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_4500685
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            'C16 H8 N O17 U3'
_chemical_formula_weight         1200.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.294(2)
_cell_angle_beta                 105.175(2)
_cell_angle_gamma                101.557(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2962(3)
_cell_length_b                   13.3376(4)
_cell_length_c                   13.6850(4)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.42
_cell_measurement_theta_min      2.58
_cell_volume                     1208.64(7)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66799
_diffrn_reflns_theta_full        32.60
_diffrn_reflns_theta_max         32.60
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    20.132
_exptl_absorpt_correction_T_max  0.3526
_exptl_absorpt_correction_T_min  0.0711
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.265
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.370
_refine_ls_extinction_coef       0.00117(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         8737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0330P)²+2.1574P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                7148
_reflns_number_total             8737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200106j_si_002.cif
_cod_data_source_block           uft116_0m
_cod_database_code               4500685
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U1 U 0.52101(3) 0.911961(13) 0.095638(13) 0.02246(5) Uani 1 1 d .
U2 U 0.49493(3) 0.591995(12) 0.414964(12) 0.02415(5) Uani 1 1 d .
U3 U 0.31313(3) 0.281739(13) 0.274451(12) 0.02212(5) Uani 1 1 d .
N1 N 1.0000 1.0000 0.0000 0.0400(16) Uani 1 2 d S
N2 N 1.0683(12) 0.5765(7) 0.5783(7) 0.0299(18) Uani 0.50 1 d P
O1 O 0.5523(6) 0.2761(3) 0.2691(3) 0.0363(9) Uani 1 1 d .
O2 O 0.2484(7) 0.5934(3) 0.4071(3) 0.0397(9) Uani 1 1 d .
O3 O 0.7415(7) 0.5978(3) 0.4147(3) 0.0416(10) Uani 1 1 d .
O4 O 0.2123(6) 0.2516(3) 0.0887(3) 0.0284(8) Uani 1 1 d .
O5 O 0.2279(6) 0.0921(3) 0.2326(3) 0.0269(7) Uani 1 1 d .
O6 O 0.4351(8) 0.4200(3) 0.4177(3) 0.0451(12) Uani 1 1 d .
O7 O 0.3709(7) 0.4480(3) 0.2286(3) 0.0430(11) Uani 1 1 d .
O8 O 0.3865(7) 0.2240(3) 0.4347(3) 0.0348(9) Uani 1 1 d .
O9 O 0.4466(7) 0.9977(3) 0.2454(3) 0.0384(10) Uani 1 1 d .
O10 O 0.7741(6) 0.9785(4) 0.1563(4) 0.0438(10) Uani 1 1 d .
O11 O 0.6044(7) 0.7588(3) 0.0178(3) 0.0415(10) Uani 1 1 d .
O12 O 0.0696(7) 0.2810(4) 0.2722(4) 0.0428(10) Uani 1 1 d .
O13 O 0.5478(7) 0.9323(3) -0.0646(3) 0.0393(10) Uani 1 1 d .
O14 O 0.2681(6) 0.8431(4) 0.0375(4) 0.0441(10) Uani 1 1 d .
O15 O 0.5585(8) 0.8016(3) 0.2166(3) 0.0485(12) Uani 1 1 d .
O16 O 0.4163(7) 0.2152(3) 0.5933(3) 0.0341(9) Uani 1 1 d .
O17 O 0.4047(7) 0.6111(3) 0.2277(3) 0.0374(10) Uani 1 1 d .
C1 C 0.3526(8) 0.5154(4) 0.1765(3) 0.0235(9) Uani 1 1 d .
C2 C 0.3154(8) 0.0310(4) 0.2734(3) 0.0244(10) Uani 1 1 d .
C3 C 0.2909(8) 0.2860(3) 0.0253(3) 0.0236(9) Uani 1 1 d .
C4 C 0.3640(7) 0.1678(3) 0.4971(3) 0.0216(9) Uani 1 1 d .
C5 C 0.2771(7) 0.4838(4) 0.0584(3) 0.0220(9) Uani 1 1 d .
C6 C 0.2524(7) 0.3830(4) -0.0075(3) 0.0212(9) Uani 1 1 d .
C7 C 0.2807(7) 0.0501(3) 0.4589(4) 0.0205(9) Uani 1 1 d .
C8 C 0.2557(8) -0.0114(3) 0.3575(4) 0.0234(9) Uani 1 1 d .
C9 C 0.2300(8) -0.0021(4) 0.5302(4) 0.0300(11) Uani 1 1 d .
H9 H 0.2473 0.0377 0.5982 0.036 Uiso 1 1 calc R
C10 C 0.2358(8) 0.5650(4) 0.0138(4) 0.0255(10) Uani 1 1 d .
H10 H 0.2519 0.6319 0.0578 0.031 Uiso 1 1 calc R
C11 C 0.1718(9) 0.5484(5) -0.0942(4) 0.0336(12) Uani 1 1 d .
H11 H 0.1456 0.6033 -0.1227 0.040 Uiso 1 1 calc R
C12 C 0.1472(9) 0.4490(5) -0.1590(4) 0.0354(12) Uani 1 1 d .
H12 H 0.1019 0.4364 -0.2318 0.042 Uiso 1 1 calc R
C13 C 0.1540(9) -0.1122(4) 0.5020(5) 0.0356(12) Uani 1 1 d .
H13 H 0.1206 -0.1456 0.5505 0.043 Uiso 1 1 calc R
C14 C 0.1900(8) 0.3671(4) -0.1162(4) 0.0294(11) Uani 1 1 d .
H14 H 0.1766 0.3010 -0.1609 0.035 Uiso 1 1 calc R
C15 C 0.1817(9) -0.1215(4) 0.3310(5) 0.0338(12) Uani 1 1 d .
H15 H 0.1674 -0.1626 0.2640 0.041 Uiso 1 1 calc R
C16 C 0.1292(9) -0.1708(4) 0.4021(5) 0.0387(13) Uani 1 1 d .
H16 H 0.0765 -0.2443 0.3821 0.046 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O10 U1 O14 178.3(2) . .
O10 U1 O13 89.6(2) . .
O14 U1 O13 91.82(19) . .
O10 U1 O13 91.21(19) . 2_675
O14 U1 O13 90.1(2) . 2_675
O13 U1 O13 67.48(14) . 2_675
O10 U1 O11 89.76(19) . .
O14 U1 O11 89.78(19) . .
O13 U1 O11 74.55(13) . .
O13 U1 O11 142.01(13) 2_675 .
O10 U1 O9 91.00(19) . .
O14 U1 O9 88.44(19) . .
O13 U1 O9 141.47(13) . .
O13 U1 O9 73.98(13) 2_675 .
O11 U1 O9 143.98(13) . .
O10 U1 O15 87.9(2) . .
O14 U1 O15 90.4(2) . .
O13 U1 O15 145.22(13) . .
O13 U1 O15 147.23(13) 2_675 .
O11 U1 O15 70.76(13) . .
O9 U1 O15 73.28(14) . .
O10 U1 U1 90.49(15) . 2_675
O14 U1 U1 91.18(15) . 2_675
O13 U1 U1 33.83(9) . 2_675
O13 U1 U1 33.65(9) 2_675 2_675
O11 U1 U1 108.37(9) . 2_675
O9 U1 U1 107.63(9) . 2_675
O15 U1 U1 178.18(13) . 2_675
O2 U2 O3 174.81(18) . .
O2 U2 O6 91.92(19) . .
O3 U2 O6 92.1(2) . .
O2 U2 O6 92.10(19) . 2_666
O3 U2 O6 92.38(19) . 2_666
O6 U2 O6 68.99(15) . 2_666
O2 U2 O17 85.59(17) . .
O3 U2 O17 89.85(17) . .
O6 U2 O17 112.56(12) . .
O6 U2 O17 177.23(15) 2_666 .
O2 U2 O16 91.96(16) . 2_666
O3 U2 O16 83.90(17) . 2_666
O6 U2 O16 175.78(16) . 2_666
O6 U2 O16 112.53(12) 2_666 2_666
O17 U2 O16 66.09(11) . 2_666
O2 U2 O7 91.01(18) . .
O3 U2 O7 87.84(18) . .
O6 U2 O7 64.15(12) . .
O6 U2 O7 133.12(12) 2_666 .
O17 U2 O7 48.58(11) . .
O16 U2 O7 114.10(11) 2_666 .
O2 U2 O8 87.67(17) . 2_666
O3 U2 O8 91.92(17) . 2_666
O6 U2 O8 133.15(12) . 2_666
O6 U2 O8 64.21(11) 2_666 2_666
O17 U2 O8 114.10(11) . 2_666
O16 U2 O8 48.73(10) 2_666 2_666
O7 U2 O8 162.67(11) . 2_666
O2 U2 C1 87.25(17) . .
O3 U2 C1 89.60(17) . .
O6 U2 C1 88.66(12) . .
O6 U2 C1 157.62(12) 2_666 .
O17 U2 C1 23.93(11) . .
O16 U2 C1 89.85(11) 2_666 .
O7 U2 C1 24.68(11) . .
O8 U2 C1 138.02(11) 2_666 .
O2 U2 C4 91.12(16) . 2_666
O3 U2 C4 86.37(17) . 2_666
O6 U2 C4 157.43(12) . 2_666
O6 U2 C4 88.55(12) 2_666 2_666
O17 U2 C4 89.96(11) . 2_666
O16 U2 C4 24.05(11) 2_666 2_666
O7 U2 C4 138.14(11) . 2_666
O8 U2 C4 24.75(11) 2_666 2_666
C1 U2 C4 113.82(12) . 2_666
O2 U2 U2 92.44(13) . 2_666
O3 U2 U2 92.74(14) . 2_666
O6 U2 U2 34.52(9) . 2_666
O6 U2 U2 34.48(9) 2_666 2_666
O17 U2 U2 147.03(8) . 2_666
O16 U2 U2 146.85(8) 2_666 2_666
O7 U2 U2 98.66(8) . 2_666
O8 U2 U2 98.67(7) 2_666 2_666
C1 U2 U2 123.17(8) . 2_666
C4 U2 U2 123.00(8) 2_666 2_666
O2 U2 U3 90.01(13) . .
O3 U2 U3 92.08(14) . .
O6 U2 U3 27.65(9) . .
O6 U2 U3 96.62(9) 2_666 .
O17 U2 U3 84.92(8) . .
O16 U2 U3 150.68(8) 2_666 .
O7 U2 U3 36.60(8) . .
O8 U2 U3 160.57(7) 2_666 .
C1 U2 U3 61.02(8) . .
C4 U2 U3 174.66(8) 2_666 .
U2 U2 U3 62.150(5) 2_666 .
O12 U3 O1 176.4(2) . .
O12 U3 O6 91.0(2) . .
O1 U3 O6 92.60(19) . .
O12 U3 O4 89.33(17) . .
O1 U3 O4 87.79(16) . .
O6 U3 O4 137.77(13) . .
O12 U3 O5 90.58(18) . .
O1 U3 O5 86.99(16) . .
O6 U3 O5 137.96(12) . .
O4 U3 O5 84.25(12) . .
O12 U3 O7 93.16(19) . .
O1 U3 O7 87.81(18) . .
O6 U3 O7 68.87(12) . .
O4 U3 O7 68.96(12) . .
O5 U3 O7 152.88(12) . .
O12 U3 O8 93.48(18) . .
O1 U3 O8 88.14(17) . .
O6 U3 O8 68.70(12) . .
O4 U3 O8 153.39(12) . .
O5 U3 O8 69.28(11) . .
O7 U3 O8 137.11(12) . .
O12 U3 U2 90.37(15) . .
O1 U3 U2 92.62(13) . .
O6 U3 U2 28.15(9) . .
O4 U3 U2 109.62(8) . .
O5 U3 U2 166.11(8) . .
O7 U3 U2 40.81(8) . .
O8 U3 U2 96.83(8) . .
O12 U3 U2 90.22(15) . 2_666
O1 U3 U2 93.10(13) . 2_666
O6 U3 U2 27.89(9) . 2_666
O4 U3 U2 165.64(8) . 2_666
O5 U3 U2 110.10(8) . 2_666
O7 U3 U2 96.74(8) . 2_666
O8 U3 U2 40.94(8) . 2_666
U2 U3 U2 56.029(5) . 2_666
C3 O4 U3 134.2(3) . .
C2 O5 U3 130.4(3) . .
U3 O6 U2 124.20(16) . .
U3 O6 U2 124.76(16) . 2_666
U2 O6 U2 111.01(15) . 2_666
C1 O7 U3 160.2(3) . .
C1 O7 U2 94.5(3) . .
U3 O7 U2 102.60(13) . .
C4 O8 U3 158.3(3) . .
C4 O8 U2 94.0(3) . 2_666
U3 O8 U2 102.08(12) . 2_666
C2 O9 U1 143.0(4) 1_565 .
C3 O11 U1 152.4(4) 2_665 .
U1 O13 U1 112.52(14) . 2_675
C4 O16 U2 99.5(3) . 2_666
C1 O17 U2 99.7(3) . .
O17 C1 O7 117.1(4) . .
O17 C1 C5 120.3(4) . .
O7 C1 C5 122.6(4) . .
O17 C1 U2 56.4(2) . .
O7 C1 U2 60.8(2) . .
C5 C1 U2 176.2(3) . .
O9 C2 O5 124.1(4) 1_545 .
O9 C2 C8 115.4(4) 1_545 .
O5 C2 C8 120.4(4) . .
O11 C3 O4 123.7(4) 2_665 .
O11 C3 C6 115.2(4) 2_665 .
O4 C3 C6 120.9(4) . .
O16 C4 O8 117.5(4) . .
O16 C4 C7 120.5(4) . .
O8 C4 C7 122.1(4) . .
O16 C4 U2 56.5(2) . 2_666
O8 C4 U2 61.2(2) . 2_666
C7 C4 U2 174.7(3) . 2_666
C10 C5 C6 119.4(4) . .
C10 C5 C1 115.3(4) . .
C6 C5 C1 125.2(4) . .
C14 C6 C5 118.7(4) . .
C14 C6 C3 114.0(4) . .
C5 C6 C3 127.3(4) . .
C9 C7 C8 118.3(4) . .
C9 C7 C4 117.6(4) . .
C8 C7 C4 124.1(4) . .
C15 C8 C7 119.4(4) . .
C15 C8 C2 115.3(4) . .
C7 C8 C2 125.2(4) . .
C13 C9 C7 121.6(5) . .
C11 C10 C5 121.6(5) . .
C12 C11 C10 118.9(5) . .
C11 C12 C14 120.5(5) . .
C16 C13 C9 119.1(5) . .
C6 C14 C12 120.9(5) . .
C16 C15 C8 121.2(5) . .
C13 C16 C15 120.4(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O10 1.764(4) .
U1 O14 1.767(4) .
U1 O13 2.319(4) .
U1 O13 2.330(3) 2_675
U1 O11 2.364(4) .
U1 O9 2.374(3) .
U1 O15 2.438(4) .
U1 U1 3.8662(3) 2_675
U2 O2 1.778(4) .
U2 O3 1.786(5) .
U2 O6 2.257(4) .
U2 O6 2.260(4) 2_666
U2 O17 2.555(3) .
U2 O16 2.558(3) 2_666
U2 O7 2.650(4) .
U2 O8 2.660(3) 2_666
U2 C1 3.025(4) .
U2 C4 3.027(4) 2_666
U2 U2 3.7228(3) 2_666
U2 U3 3.9569(3) .
U3 O12 1.767(4) .
U3 O1 1.782(4) .
U3 O6 2.220(4) .
U3 O4 2.373(3) .
U3 O5 2.382(3) .
U3 O7 2.417(4) .
U3 O8 2.442(3) .
U3 U2 3.9691(3) 2_666
O4 C3 1.272(6) .
O5 C2 1.265(6) .
O6 U2 2.260(4) 2_666
O7 C1 1.267(5) .
O8 C4 1.270(5) .
O8 U2 2.660(3) 2_666
O9 C2 1.246(6) 1_565
O11 C3 1.248(6) 2_665
O13 U1 2.330(3) 2_675
O16 C4 1.251(5) .
O16 U2 2.558(3) 2_666
O17 C1 1.245(5) .
C1 C5 1.498(6) .
C2 O9 1.246(6) 1_545
C2 C8 1.509(7) .
C3 O11 1.248(6) 2_665
C3 C6 1.509(6) .
C4 C7 1.486(6) .
C4 U2 3.027(4) 2_666
C5 C10 1.398(6) .
C5 C6 1.399(6) .
C6 C14 1.392(6) .
C7 C9 1.396(6) .
C7 C8 1.398(6) .
C8 C15 1.390(7) .
C9 C13 1.390(7) .
C10 C11 1.381(7) .
C11 C12 1.377(8) .
C12 C14 1.395(7) .
C13 C16 1.368(9) .
C15 C16 1.375(8) .
