#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:48:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179937 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/32/7023225.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_7023225
loop_
_publ_author_name
'Thuéry, Pierre'
'Rivière, Eric'
_publ_section_title
;
 Uranyl-copper(II) heterometallic oxalate complexes: coordination polymers
 and frameworks.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10551
_journal_page_last               10558
_journal_paper_doi               10.1039/c3dt51020d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C28 H20 Cu2 N14 O20 U2'
_chemical_formula_weight         1475.72
_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                103.449(3)
_cell_angle_beta                 110.754(3)
_cell_angle_gamma                110.069(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9169(6)
_cell_length_b                   10.9294(6)
_cell_length_c                   11.1783(5)
_cell_measurement_reflns_used    39442
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.35
_cell_volume                     973.80(10)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and seven ω scans with 2° steps (505 frames)'
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39442
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.470
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    2.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.130
_refine_diff_density_min         -2.320
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0288
_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)+(0.0178P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                5138
_reflns_number_total             5940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51020d.txt
_cod_data_source_block           3
_cod_original_cell_volume        973.81(10)
_cod_database_code               7023225
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
U U 0.265623(15) 0.181929(12) 0.435344(13) 0.01572(4) Uani 1 1 d .
Cu Cu 0.21630(5) -0.10800(4) 0.11947(4) 0.01763(9) Uani 1 1 d .
O1 O 0.1142(3) 0.1742(2) 0.2835(3) 0.0202(5) Uani 1 1 d .
O2 O 0.4225(3) 0.2013(3) 0.5890(3) 0.0200(5) Uani 1 1 d .
O3 O 0.0726(3) -0.0542(2) 0.3879(2) 0.0181(5) Uani 1 1 d .
O4 O -0.1093(3) -0.1842(2) 0.4406(3) 0.0191(5) Uani 1 1 d .
O5 O 0.4743(3) 0.3402(2) 0.3943(3) 0.0209(5) Uani 1 1 d .
O6 O 0.6527(3) 0.5656(2) 0.4541(3) 0.0213(5) Uani 1 1 d .
O7 O 0.3212(3) 0.0363(2) 0.3063(2) 0.0183(5) Uani 1 1 d .
H7 H 0.4227 0.0524 0.3333 0.022 Uiso 1 1 d R
O8 O 0.6360(3) 0.0950(3) 0.3804(3) 0.0305(6) Uani 1 1 d .
O9 O 0.5067(3) -0.0513(3) 0.1604(3) 0.0295(6) Uani 1 1 d .
O10 O 0.7601(3) 0.0059(3) 0.2898(3) 0.0283(6) Uani 1 1 d .
N1 N 0.2106(3) -0.2645(3) 0.1854(3) 0.0166(6) Uani 1 1 d .
N2 N 0.1870(3) -0.2542(3) -0.0515(3) 0.0188(6) Uani 1 1 d .
N3 N 0.2109(4) -0.4666(3) -0.1172(3) 0.0263(7) Uani 1 1 d .
N4 N 0.1988(4) -0.4929(3) 0.1215(3) 0.0224(7) Uani 1 1 d .
N5 N 0.2053(3) 0.0372(3) 0.0368(3) 0.0183(6) Uani 1 1 d .
N6 N 0.0456(3) 0.1451(3) -0.0538(3) 0.0168(6) Uani 1 1 d .
N7 N 0.6343(4) 0.0154(3) 0.2776(3) 0.0217(7) Uani 1 1 d .
C1 C -0.0099(4) -0.0687(3) 0.4514(4) 0.0175(7) Uani 1 1 d .
C2 C 0.5366(4) 0.4725(4) 0.4560(4) 0.0180(7) Uani 1 1 d .
C3 C 0.2138(4) -0.2654(4) 0.3060(4) 0.0197(7) Uani 1 1 d .
H3 H 0.2192 -0.1884 0.3682 0.024 Uiso 1 1 calc R
C4 C 0.2088(4) -0.3823(4) 0.3375(4) 0.0221(8) Uani 1 1 d .
H4 H 0.2110 -0.3852 0.4206 0.027 Uiso 1 1 calc R
C5 C 0.2005(4) -0.4932(4) 0.2422(4) 0.0227(8) Uani 1 1 d .
H5 H 0.1958 -0.5722 0.2619 0.027 Uiso 1 1 calc R
C6 C 0.2048(4) -0.3759(4) 0.1006(4) 0.0184(7) Uani 1 1 d .
C7 C 0.2015(4) -0.3669(4) -0.0316(4) 0.0190(7) Uani 1 1 d .
C8 C 0.1808(4) -0.2419(4) -0.1710(4) 0.0222(8) Uani 1 1 d .
H8 H 0.1683 -0.1669 -0.1901 0.027 Uiso 1 1 calc R
C9 C 0.1929(5) -0.3385(4) -0.2639(4) 0.0278(9) Uani 1 1 d .
H9 H 0.1905 -0.3294 -0.3452 0.033 Uiso 1 1 calc R
C10 C 0.2088(5) -0.4513(4) -0.2334(4) 0.0310(9) Uani 1 1 d .
H10 H 0.2181 -0.5173 -0.2951 0.037 Uiso 1 1 calc R
C11 C 0.3303(5) 0.1286(4) 0.0306(4) 0.0246(8) Uani 1 1 d .
H11 H 0.4281 0.1242 0.0613 0.030 Uiso 1 1 calc R
C12 C 0.3168(5) 0.2301(4) -0.0210(4) 0.0251(8) Uani 1 1 d .
H12 H 0.4032 0.2929 -0.0267 0.030 Uiso 1 1 calc R
C13 C 0.1704(4) 0.2343(4) -0.0636(4) 0.0216(8) Uani 1 1 d .
H13 H 0.1576 0.3003 -0.0999 0.026 Uiso 1 1 calc R
C14 C 0.0689(4) 0.0498(3) -0.0045(4) 0.0166(7) Uani 1 1 d .
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'
Cu Cu 0.3201 1.2651 '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'
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 U O1 176.36(10) . .
O2 U O7 89.73(10) . .
O1 U O7 92.02(10) . .
O2 U O3 95.42(9) . .
O1 U O3 88.10(9) . .
O7 U O3 75.88(8) . .
O2 U O4 87.66(10) . 2_556
O1 U O4 92.89(10) . 2_556
O7 U O4 142.27(8) . 2_556
O3 U O4 66.93(8) . 2_556
O2 U O6 88.69(10) . 2_666
O1 U O6 87.94(10) . 2_666
O7 U O6 141.01(8) . 2_666
O3 U O6 143.02(8) . 2_666
O4 U O6 76.57(8) 2_556 2_666
O2 U O5 89.34(10) . .
O1 U O5 88.03(10) . .
O7 U O5 75.20(8) . .
O3 U O5 150.65(8) . .
O4 U O5 142.34(8) 2_556 .
O6 U O5 65.83(8) 2_666 .
O7 Cu N1 93.63(11) . .
O7 Cu N5 90.84(11) . .
N1 Cu N5 175.06(12) . .
O7 Cu N2 159.48(11) . .
N1 Cu N2 80.29(12) . .
N5 Cu N2 96.21(12) . .
O7 Cu N6 98.63(10) . 2
N1 Cu N6 99.94(10) . 2
N5 Cu N6 77.28(10) . 2
N2 Cu N6 101.71(11) . 2
C1 O3 U 119.7(2) . .
C1 O4 U 119.4(2) . 2_556
C2 O5 U 120.0(2) . .
C2 O6 U 120.5(2) . 2_666
Cu O7 U 138.78(12) . .
Cu O7 H7 99.9 . .
U O7 H7 119.9 . .
C6 N1 C3 118.1(3) . .
C6 N1 Cu 115.8(2) . .
C3 N1 Cu 126.1(2) . .
C7 N2 C8 116.7(3) . .
C7 N2 Cu 113.9(2) . .
C8 N2 Cu 128.5(2) . .
C7 N3 C10 116.3(3) . .
C6 N4 C5 114.8(3) . .
C14 N5 C11 117.5(3) . .
C14 N5 Cu 118.1(2) . .
C11 N5 Cu 124.2(2) . .
C14 N6 C13 116.8(3) . .
C14 N6 Cu 109.8(2) . 2
C13 N6 Cu 133.3(2) . 2
O10 N7 O8 120.2(3) . .
O10 N7 O9 119.7(3) . .
O8 N7 O9 120.0(3) . .
O4 C1 O3 126.3(3) . .
O4 C1 C1 117.2(4) . 2_556
O3 C1 C1 116.5(3) . 2_556
O5 C2 O6 126.9(3) . .
O5 C2 C2 116.6(3) . 2_666
O6 C2 C2 116.5(4) . 2_666
N1 C3 C4 119.6(3) . .
N1 C3 H3 120.2 . .
C4 C3 H3 120.2 . .
C5 C4 C3 118.0(3) . .
C5 C4 H4 121.0 . .
C3 C4 H4 121.0 . .
N4 C5 C4 123.0(3) . .
N4 C5 H5 118.5 . .
C4 C5 H5 118.5 . .
N1 C6 N4 126.6(3) . .
N1 C6 C7 114.9(3) . .
N4 C6 C7 118.5(3) . .
N3 C7 N2 126.4(3) . .
N3 C7 C6 119.4(3) . .
N2 C7 C6 114.2(3) . .
N2 C8 C9 120.7(3) . .
N2 C8 H8 119.6 . .
C9 C8 H8 119.6 . .
C8 C9 C10 118.2(4) . .
C8 C9 H9 120.9 . .
C10 C9 H9 120.9 . .
N3 C10 C9 121.6(4) . .
N3 C10 H10 119.2 . .
C9 C10 H10 119.2 . .
N5 C11 C12 121.1(4) . .
N5 C11 H11 119.4 . .
C12 C11 H11 119.4 . .
C13 C12 C11 117.5(3) . .
C13 C12 H12 121.2 . .
C11 C12 H12 121.2 . .
N6 C13 C12 121.6(3) . .
N6 C13 H13 119.2 . .
C12 C13 H13 119.2 . .
N5 C14 N6 125.4(3) . .
N5 C14 C14 117.7(4) . 2
N6 C14 C14 116.9(4) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O2 1.768(2) .
U O1 1.784(2) .
U O7 2.239(2) .
U O3 2.421(2) .
U O4 2.421(2) 2_556
U O6 2.443(2) 2_666
U O5 2.464(2) .
Cu O7 1.933(2) .
Cu N1 2.005(3) .
Cu N5 2.028(3) .
Cu N2 2.039(3) .
Cu N6 2.289(3) 2
O3 C1 1.254(4) .
O4 C1 1.253(4) .
O4 U 2.421(2) 2_556
O5 C2 1.253(4) .
O6 C2 1.259(4) .
O6 U 2.443(2) 2_666
O7 H7 0.8799 .
O8 N7 1.260(4) .
O9 N7 1.263(4) .
O10 N7 1.249(4) .
N1 C6 1.327(4) .
N1 C3 1.339(4) .
N2 C7 1.346(4) .
N2 C8 1.356(4) .
N3 C7 1.327(5) .
N3 C10 1.341(5) .
N4 C6 1.338(4) .
N4 C5 1.344(5) .
N5 C14 1.333(4) .
N5 C11 1.335(4) .
N6 C14 1.335(4) .
N6 C13 1.346(4) .
N6 Cu 2.289(3) 2
C1 C1 1.537(7) 2_556
C2 C2 1.544(7) 2_666
C3 C4 1.392(5) .
C3 H3 0.9300 .
C4 C5 1.370(5) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C7 1.494(5) .
C8 C9 1.368(5) .
C8 H8 0.9300 .
C9 C10 1.397(6) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.387(5) .
C11 H11 0.9300 .
C12 C13 1.379(5) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C14 1.480(6) 2
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O7 H7 O8 0.88 1.84 2.719(4) 175.0
