#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:48:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179937 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/32/7023227.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_7023227
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            'C16 H8 Cu N2 O10 U'
_chemical_formula_weight         689.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 107.188(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8103(6)
_cell_length_b                   16.5690(7)
_cell_length_c                   12.5158(7)
_cell_measurement_reflns_used    48655
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.10
_cell_volume                     1745.44(17)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and three ω scans with 2° steps (356 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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48655
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.549
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    2.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0363
_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)+(0.0082P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                3674
_reflns_number_total             5335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51020d.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7023227
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.41633(2) 0.679516(11) 0.928769(13) 0.01830(5) Uani 1 1 d .
Cu Cu 0.08077(8) 0.95031(4) 0.70284(4) 0.02464(15) Uani 1 1 d .
O1 O 0.6189(4) 0.7072(2) 0.9766(2) 0.0252(8) Uani 1 1 d .
O2 O 0.2136(4) 0.6509(2) 0.8805(2) 0.0263(8) Uani 1 1 d .
O3 O 0.3376(4) 0.80271(19) 0.8304(2) 0.0233(8) Uani 1 1 d .
O4 O 0.2260(4) 0.8557(2) 0.6600(3) 0.0289(9) Uani 1 1 d .
O5 O 0.4500(4) 0.6827(2) 0.7439(2) 0.0237(8) Uani 1 1 d .
O6 O 0.3872(4) 0.7402(2) 0.5760(2) 0.0256(8) Uani 1 1 d .
O7 O 0.4678(4) 0.54568(19) 0.8705(2) 0.0233(8) Uani 1 1 d .
O8 O 0.5161(4) 0.4162(2) 0.9199(2) 0.0240(8) Uani 1 1 d .
O9 O -0.0899(4) 0.9286(2) 0.5635(3) 0.0280(8) Uani 1 1 d .
O10 O -0.1500(4) 0.9663(2) 0.3830(3) 0.0283(8) Uani 1 1 d .
N1 N -0.0105(5) 0.8791(2) 0.7942(3) 0.0227(9) Uani 1 1 d .
N2 N 0.2021(5) 0.9955(2) 0.8499(3) 0.0238(10) Uani 1 1 d .
C1 C 0.3080(6) 0.8068(3) 0.7253(4) 0.0211(11) Uani 1 1 d .
C2 C 0.3898(6) 0.7383(3) 0.6762(3) 0.0208(11) Uani 1 1 d .
C3 C 0.4949(6) 0.4893(3) 0.9387(3) 0.0230(11) Uani 1 1 d .
C4 C -0.0700(6) 0.9695(3) 0.4846(4) 0.0269(12) Uani 1 1 d .
C5 C -0.1109(6) 0.8167(3) 0.7634(4) 0.0287(12) Uani 1 1 d .
H5 H -0.1583 0.8074 0.6875 0.034 Uiso 1 1 calc R
C6 C -0.1462(6) 0.7662(3) 0.8391(4) 0.0307(13) Uani 1 1 d .
H6 H -0.2143 0.7228 0.8138 0.037 Uiso 1 1 calc R
C7 C -0.0826(6) 0.7788(3) 0.9515(4) 0.0268(12) Uani 1 1 d .
H7 H -0.1043 0.7436 1.0030 0.032 Uiso 1 1 calc R
C8 C 0.0170(6) 0.8466(3) 0.9876(4) 0.0223(11) Uani 1 1 d .
C9 C 0.0547(6) 0.8925(3) 0.9055(4) 0.0205(11) Uani 1 1 d .
C10 C 0.1653(6) 0.9579(3) 0.9363(4) 0.0225(11) Uani 1 1 d .
C11 C 0.2289(6) 0.9800(3) 1.0491(4) 0.0255(12) Uani 1 1 d .
C12 C 0.1818(6) 0.9354(3) 1.1297(4) 0.0271(12) Uani 1 1 d .
H12 H 0.2205 0.9505 1.2045 0.033 Uiso 1 1 calc R
C13 C 0.0819(6) 0.8712(3) 1.1024(4) 0.0281(13) Uani 1 1 d .
H13 H 0.0551 0.8429 1.1584 0.034 Uiso 1 1 calc R
C14 C 0.3387(6) 1.0441(3) 1.0707(4) 0.0313(13) Uani 1 1 d .
H14 H 0.3860 1.0608 1.1440 0.038 Uiso 1 1 calc R
C15 C 0.3757(6) 1.0818(3) 0.9853(4) 0.0319(13) Uani 1 1 d .
H15 H 0.4467 1.1248 0.9999 0.038 Uiso 1 1 calc R
C16 C 0.3070(6) 1.0557(3) 0.8754(4) 0.0283(12) Uani 1 1 d .
H16 H 0.3355 1.0813 0.8180 0.034 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'
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'
Cu Cu 0.3201 1.2651 '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
O1 U O2 179.50(16) . .
O1 U O6 85.45(13) . 4_576
O2 U O6 94.95(13) . 4_576
O1 U O3 93.61(14) . .
O2 U O3 86.75(14) . .
O6 U O3 80.64(10) 4_576 .
O1 U O8 85.10(14) . 3_667
O2 U O8 94.68(14) . 3_667
O6 U O8 79.32(11) 4_576 3_667
O3 U O8 159.96(10) . 3_667
O1 U O7 94.58(14) . .
O2 U O7 84.92(15) . .
O6 U O7 146.09(10) 4_576 .
O3 U O7 133.05(10) . .
O8 U O7 66.93(9) 3_667 .
O1 U O5 85.48(12) . .
O2 U O5 94.36(12) . .
O6 U O5 144.22(11) 4_576 .
O3 U O5 65.50(10) . .
O8 U O5 134.08(11) 3_667 .
O7 U O5 69.20(10) . .
O10 Cu O9 85.57(13) 3_576 .
O10 Cu N1 171.20(16) 3_576 .
O9 Cu N1 93.95(15) . .
O10 Cu N2 94.20(15) 3_576 .
O9 Cu N2 162.21(16) . .
N1 Cu N2 83.56(16) . .
O10 Cu O4 94.09(14) 3_576 .
O9 Cu O4 90.04(14) . .
N1 Cu O4 94.70(15) . .
N2 Cu O4 107.71(15) . .
C1 O3 U 121.5(3) . .
C1 O4 Cu 125.7(3) . .
C2 O5 U 120.9(3) . .
C2 O6 U 146.0(3) . 4_575
C3 O7 U 119.9(3) . .
C3 O8 U 120.2(3) . 3_667
C4 O9 Cu 110.5(3) . .
C4 O10 Cu 110.7(3) . 3_576
C5 N1 C9 117.7(4) . .
C5 N1 Cu 129.9(3) . .
C9 N1 Cu 112.0(3) . .
C16 N2 C10 117.4(4) . .
C16 N2 Cu 130.6(3) . .
C10 N2 Cu 111.9(3) . .
O4 C1 O3 129.0(5) . .
O4 C1 C2 117.9(4) . .
O3 C1 C2 113.1(4) . .
O6 C2 O5 125.0(5) . .
O6 C2 C1 120.2(4) . .
O5 C2 C1 114.8(4) . .
O7 C3 O8 127.3(4) . .
O7 C3 C3 116.9(5) . 3_667
O8 C3 C3 115.8(5) . 3_667
O9 C4 O10 127.3(5) . .
O9 C4 C4 116.3(5) . 3_576
O10 C4 C4 116.4(5) . 3_576
N1 C5 C6 122.5(5) . .
N1 C5 H5 118.7 . .
C6 C5 H5 118.7 . .
C5 C6 C7 120.8(5) . .
C5 C6 H6 119.6 . .
C7 C6 H6 119.6 . .
C6 C7 C8 118.4(5) . .
C6 C7 H7 120.8 . .
C8 C7 H7 120.8 . .
C9 C8 C7 117.3(4) . .
C9 C8 C13 118.0(5) . .
C7 C8 C13 124.8(5) . .
N1 C9 C8 123.0(5) . .
N1 C9 C10 116.6(4) . .
C8 C9 C10 120.4(4) . .
N2 C10 C11 124.0(5) . .
N2 C10 C9 115.7(4) . .
C11 C10 C9 120.3(4) . .
C10 C11 C12 118.0(5) . .
C10 C11 C14 115.9(5) . .
C12 C11 C14 126.1(5) . .
C13 C12 C11 122.4(4) . .
C13 C12 H12 118.8 . .
C11 C12 H12 118.8 . .
C12 C13 C8 120.7(5) . .
C12 C13 H13 119.6 . .
C8 C13 H13 119.6 . .
C15 C14 C11 120.4(5) . .
C15 C14 H14 119.8 . .
C11 C14 H14 119.8 . .
C14 C15 C16 119.9(5) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
N2 C16 C15 122.4(5) . .
N2 C16 H16 118.8 . .
C15 C16 H16 118.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O1 1.767(3) .
U O2 1.773(3) .
U O6 2.347(3) 4_576
U O3 2.379(3) .
U O8 2.407(3) 3_667
U O7 2.419(3) .
U O5 2.419(3) .
Cu O10 1.955(3) 3_576
Cu O9 1.970(3) .
Cu N1 1.972(4) .
Cu N2 1.982(4) .
Cu O4 2.187(4) .
O3 C1 1.265(5) .
O4 C1 1.224(5) .
O5 C2 1.258(5) .
O6 C2 1.249(5) .
O6 U 2.347(3) 4_575
O7 C3 1.239(5) .
O8 C3 1.258(6) .
O8 U 2.407(3) 3_667
O9 C4 1.252(5) .
O10 C4 1.259(5) .
O10 Cu 1.955(3) 3_576
N1 C5 1.342(6) .
N1 C9 1.358(5) .
N2 C16 1.333(6) .
N2 C10 1.368(6) .
C1 C2 1.563(6) .
C3 C3 1.552(8) 3_667
C4 C4 1.553(10) 3_576
C5 C6 1.367(6) .
C5 H5 0.9300 .
C6 C7 1.369(6) .
C6 H6 0.9300 .
C7 C8 1.415(7) .
C7 H7 0.9300 .
C8 C9 1.396(6) .
C8 C13 1.439(6) .
C9 C10 1.431(7) .
C10 C11 1.405(6) .
C11 C12 1.408(7) .
C11 C14 1.408(7) .
C12 C13 1.358(7) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C15 1.359(7) .
C14 H14 0.9300 .
C15 C16 1.397(7) .
C15 H15 0.9300 .
C16 H16 0.9300 .
