#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:12:01 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179561 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/30/4503017.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_4503017
loop_
_publ_author_name
'Mihalcea, Ionut'
'Henry, Natacha'
'Volkringer, Christophe'
'Loiseau, Thierry'
_publ_section_title
;
 Uranyl--Pyromellitate Coordination Polymers: Toward Three-Dimensional
 Open Frameworks with Large Channel Systems
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              526
_journal_paper_doi               10.1021/cg201509v
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety
' 3(U O2 2+).  1(C10 O8 H2 4-).  2(O H 1-).  2(H2 O)'
_chemical_formula_sum            'C10 H8 O18 U3'
_chemical_formula_weight         1130.25
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.846(2)
_cell_angle_beta                 100.440(2)
_cell_angle_gamma                96.940(2)
_cell_formula_units_Z            1
_cell_length_a                   5.5266(3)
_cell_length_b                   7.6559(3)
_cell_length_c                   11.3208(4)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.595
_cell_measurement_theta_min      2.744
_cell_volume                     456.66(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            70902
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    26.629
_exptl_absorpt_correction_T_max  0.2685
_exptl_absorpt_correction_T_min  0.1104
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.886
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0181
_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)+(0.0120P)²+3.3649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0457
_reflns_number_gt                2372
_reflns_number_total             2662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201509v_si_009.cif
_cod_data_source_block           ndupyro021_0m
_cod_original_cell_volume        456.66(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4503017
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 0.5000 1.0000 1.0000 0.01057(6) Uani 1 2 d S
U2 U 0.57879(3) 0.58571(2) 0.739045(15) 0.01158(5) Uani 1 1 d .
O81 O 0.4017(7) 0.6890(5) 0.3957(3) 0.0206(8) Uani 1 1 d .
O82 O 0.3102(7) 0.6139(5) 0.5646(3) 0.0201(8) Uani 1 1 d .
O1H O 0.7134(7) 0.7701(5) 0.9334(3) 0.0191(8) Uani 1 1 d .
O1W O 0.8710(7) 0.4313(5) 0.8560(3) 0.0208(8) Uani 1 1 d .
O71 O 0.8112(8) 0.9390(5) 1.1697(3) 0.0243(9) Uani 1 1 d .
O1U O 0.2585(7) 0.8303(5) 1.0132(3) 0.0198(8) Uani 1 1 d .
O22U O 0.3251(7) 0.4768(5) 0.7887(4) 0.0209(8) Uani 1 1 d .
O21U O 0.8391(7) 0.6847(5) 0.6918(4) 0.0231(8) Uani 1 1 d .
O72 O 0.5709(7) 1.1213(5) 1.2349(3) 0.0189(8) Uani 1 1 d .
C8 C 0.3053(9) 0.7143(6) 0.4881(4) 0.0130(9) Uani 1 1 d .
C7 C 0.7492(10) 1.0333(6) 1.2588(4) 0.0140(9) Uani 1 1 d .
C2 C 0.1614(9) 0.8693(6) 0.5029(4) 0.0128(9) Uani 1 1 d .
C1 C 0.1242(9) 0.9710(6) 0.6130(4) 0.0130(9) Uani 1 1 d .
C3 C 0.0373(10) 0.9027(7) 0.3928(4) 0.0152(10) Uani 1 1 d .
H3 H 0.0635 0.8375 0.3195 0.018 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'
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
O1U U1 O1U 180.0 2_677 .
O1U U1 O1H 87.89(16) 2_677 2_677
O1U U1 O1H 92.11(16) . 2_677
O1U U1 O1H 92.11(16) 2_677 .
O1U U1 O1H 87.89(16) . .
O1H U1 O1H 180.000(2) 2_677 .
O1U U1 O71 86.08(16) 2_677 .
O1U U1 O71 93.92(16) . .
O1H U1 O71 112.70(12) 2_677 .
O1H U1 O71 67.30(12) . .
O1U U1 O71 93.92(16) 2_677 2_677
O1U U1 O71 86.08(16) . 2_677
O1H U1 O71 67.30(12) 2_677 2_677
O1H U1 O71 112.70(12) . 2_677
O71 U1 O71 179.999(2) . 2_677
O1U U1 O72 88.34(15) 2_677 2_677
O1U U1 O72 91.66(15) . 2_677
O1H U1 O72 117.04(11) 2_677 2_677
O1H U1 O72 62.96(11) . 2_677
O71 U1 O72 129.65(11) . 2_677
O71 U1 O72 50.35(11) 2_677 2_677
O1U U1 O72 91.66(15) 2_677 .
O1U U1 O72 88.34(15) . .
O1H U1 O72 62.96(11) 2_677 .
O1H U1 O72 117.04(11) . .
O71 U1 O72 50.35(11) . .
O71 U1 O72 129.65(11) 2_677 .
O72 U1 O72 180.00(6) 2_677 .
O1U U1 C7 88.98(16) 2_677 .
O1U U1 C7 91.02(16) . .
O1H U1 C7 88.26(13) 2_677 .
O1H U1 C7 91.74(13) . .
O71 U1 C7 24.78(12) . .
O71 U1 C7 155.22(12) 2_677 .
O72 U1 C7 154.43(12) 2_677 .
O72 U1 C7 25.57(12) . .
O1U U1 C7 91.02(16) 2_677 2_677
O1U U1 C7 88.98(16) . 2_677
O1H U1 C7 91.74(13) 2_677 2_677
O1H U1 C7 88.26(13) . 2_677
O71 U1 C7 155.22(12) . 2_677
O71 U1 C7 24.78(12) 2_677 2_677
O72 U1 C7 25.57(12) 2_677 2_677
O72 U1 C7 154.43(12) . 2_677
C7 U1 C7 180.000(1) . 2_677
O1U U1 U2 79.67(12) 2_677 2_677
O1U U1 U2 100.33(12) . 2_677
O1H U1 U2 29.61(9) 2_677 2_677
O1H U1 U2 150.39(9) . 2_677
O71 U1 U2 83.68(8) . 2_677
O71 U1 U2 96.32(8) 2_677 2_677
O72 U1 U2 143.90(7) 2_677 2_677
O72 U1 U2 36.10(7) . 2_677
C7 U1 U2 59.99(9) . 2_677
C7 U1 U2 120.01(9) 2_677 2_677
O1U U1 U2 100.33(12) 2_677 .
O1U U1 U2 79.67(12) . .
O1H U1 U2 150.39(9) 2_677 .
O1H U1 U2 29.61(9) . .
O71 U1 U2 96.32(8) . .
O71 U1 U2 83.68(8) 2_677 .
O72 U1 U2 36.10(7) 2_677 .
O72 U1 U2 143.90(7) . .
C7 U1 U2 120.01(9) . .
C7 U1 U2 59.99(9) 2_677 .
U2 U1 U2 180.000(1) 2_677 .
O21U U2 O22U 177.00(18) . .
O21U U2 O82 92.01(17) . .
O22U U2 O82 90.07(16) . .
O21U U2 O1H 90.34(17) . .
O22U U2 O1H 89.86(16) . .
O82 U2 O1H 132.56(12) . .
O21U U2 O81 87.99(16) . 2_666
O22U U2 O81 90.22(16) . 2_666
O82 U2 O81 80.28(12) . 2_666
O1H U2 O81 147.16(12) . 2_666
O21U U2 O1W 86.29(16) . .
O22U U2 O1W 90.89(15) . .
O82 U2 O1W 153.67(13) . .
O1H U2 O1W 73.76(12) . .
O81 U2 O1W 73.40(13) 2_666 .
O21U U2 O72 89.16(16) . 2_677
O22U U2 O72 93.64(16) . 2_677
O82 U2 O72 67.74(12) . 2_677
O1H U2 O72 64.93(12) . 2_677
O81 U2 O72 147.77(12) 2_666 2_677
O1W U2 O72 138.40(12) . 2_677
O21U U2 U1 99.98(13) . .
O22U U2 U1 81.62(12) . .
O82 U2 U1 103.84(9) . .
O1H U2 U1 29.64(9) . .
O81 U2 U1 170.80(9) 2_666 .
O1W U2 U1 102.33(9) . .
O72 U2 U1 38.13(8) 2_677 .
C8 O81 U2 129.5(3) . 2_666
C8 O82 U2 137.2(3) . .
U2 O1H U1 120.75(15) . .
C7 O71 U1 98.8(3) . .
C7 O72 U2 147.9(3) . 2_677
C7 O72 U1 93.4(3) . .
U2 O72 U1 105.77(12) 2_677 .
O81 C8 O82 124.4(4) . .
O81 C8 C2 116.8(4) . .
O82 C8 C2 118.7(4) . .
O71 C7 O72 117.4(4) . .
O71 C7 C1 118.9(4) . 2_677
O72 C7 C1 123.5(4) . 2_677
O71 C7 U1 56.5(2) . .
O72 C7 U1 61.0(2) . .
C1 C7 U1 173.9(3) 2_677 .
C3 C2 C1 117.8(4) . .
C3 C2 C8 114.7(4) . .
C1 C2 C8 127.4(4) . .
C3 C1 C2 118.8(4) 2_576 .
C3 C1 C7 114.2(4) 2_576 2_677
C2 C1 C7 126.9(4) . 2_677
C2 C3 C1 123.4(4) . 2_576
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1U 1.794(4) 2_677
U1 O1U 1.794(4) .
U1 O1H 2.319(3) 2_677
U1 O1H 2.319(3) .
U1 O71 2.490(4) .
U1 O71 2.490(4) 2_677
U1 O72 2.586(3) 2_677
U1 O72 2.586(3) .
U1 C7 2.952(5) .
U1 C7 2.952(5) 2_677
U1 U2 4.0312(2) 2_677
U1 U2 4.0312(2) .
U2 O21U 1.761(4) .
U2 O22U 1.776(4) .
U2 O82 2.308(4) .
U2 O1H 2.318(3) .
U2 O81 2.381(3) 2_666
U2 O1W 2.456(4) .
U2 O72 2.468(3) 2_677
O81 C8 1.252(6) .
O81 U2 2.381(3) 2_666
O82 C8 1.260(6) .
O71 C7 1.252(6) .
O72 C7 1.277(6) .
O72 U2 2.468(3) 2_677
C8 C2 1.507(6) .
C7 C1 1.500(6) 2_677
C2 C3 1.393(6) .
C2 C1 1.404(6) .
C1 C3 1.395(6) 2_576
C1 C7 1.500(6) 2_677
C3 C1 1.395(6) 2_576
