#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:39:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180443 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/12/7211249.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_7211249
loop_
_publ_author_name
'Cantos, Paula M.'
'Pope, Simon J. A.'
'Cahill, Christopher L.'
_publ_section_title
;
 An exploration of homo- and heterometallic UO22+ hybrid materials
 containing chelidamic acid: synthesis, structure, and luminescence
 studies
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              9039
_journal_paper_doi               10.1039/c3ce41655k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C7 H2 N O13 U2'
_chemical_formula_weight         784.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.288(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.327(3)
_cell_length_b                   12.129(3)
_cell_length_c                   15.073(4)
_cell_measurement_reflns_used    41355
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      57.410
_cell_measurement_theta_min      4.380
_cell_volume                     1812.2(8)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'SMART V5.05 (Bruker-AXS)'
_computing_data_reduction        'SAINT (Bruker-AXS)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker Apex CCD II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39636
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.906
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.2904
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.874
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.659
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0381
_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)+(0.0528P)²+16.0474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                3767
_reflns_number_total             4496
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3ce41655k.txt
_cod_data_source_block           Compound3
_cod_original_cell_volume        1812.3(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7211249
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
C1 C 0.5066(8) 0.1648(7) 0.4464(5) 0.0240(16) Uani 1 1 d .
C2 C 0.5759(8) 0.2196(7) 0.5271(6) 0.0281(17) Uani 1 1 d .
H2 H 0.6506 0.1873 0.5683 0.034 Uiso 1 1 calc R
C3 C 0.5314(9) 0.3239(7) 0.5452(6) 0.0299(18) Uani 1 1 d .
C4 C 0.4147(9) 0.3668(7) 0.4807(6) 0.0317(19) Uani 1 1 d .
H4 H 0.3805 0.4353 0.4905 0.038 Uiso 1 1 calc R
C5 C 0.3527(8) 0.3065(6) 0.4037(5) 0.0225(15) Uani 1 1 d .
C6 C 0.2307(8) 0.3454(6) 0.3303(6) 0.0254(16) Uani 1 1 d .
C7 C 0.5485(7) 0.0560(6) 0.4171(6) 0.0234(16) Uani 1 1 d .
N1 N 0.3951(7) 0.2067(5) 0.3851(4) 0.0249(14) Uani 1 1 d .
O1 O 0.1787(6) 0.0285(5) 0.3011(4) 0.0362(14) Uani 1 1 d .
O2 O 0.3764(7) 0.1788(5) 0.1819(4) 0.0408(15) Uani 1 1 d .
O3 O 0.4770(6) 0.0193(5) 0.3407(4) 0.0362(15) Uani 1 1 d .
O4 O 0.1787(7) 0.2803(5) 0.2664(4) 0.0400(16) Uani 1 1 d .
O5 O 0.1880(6) 0.4431(5) 0.3366(4) 0.0319(13) Uani 1 1 d .
O6 O 0.6486(6) 0.0067(5) 0.4684(4) 0.0307(13) Uani 1 1 d .
O7 O 0.8142(9) 0.0388(7) 0.3443(5) 0.055(2) Uani 1 1 d .
O8 O 0.8583(7) -0.1786(6) 0.5090(5) 0.0493(18) Uani 1 1 d .
O9 O 0.6339(8) -0.1645(7) 0.3283(6) 0.063(2) Uani 1 1 d .
O10 O 0.8963(8) -0.1915(9) 0.3119(7) 0.087(3) Uani 1 1 d .
O11 O 0.9294(6) 0.0546(6) 0.5470(5) 0.0410(16) Uani 1 1 d .
O12 O 0.5896(6) 0.3804(5) 0.6202(4) 0.0374(16) Uani 1 1 d .
U1 U 0.27649(3) 0.10399(2) 0.24086(2) 0.02342(10) Uani 1 1 d .
U2 U 0.83824(3) -0.07060(3) 0.42753(2) 0.03201(11) Uani 1 1 d .
OW1 O 0.654(2) -0.3899(13) 0.3228(12) 0.152(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'
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
N1 C1 C2 123.1(7) . .
N1 C1 C7 112.9(6) . .
C2 C1 C7 124.0(7) . .
C1 C2 C3 119.0(7) . .
O12 C3 C2 122.9(7) . .
O12 C3 C4 119.6(8) . .
C2 C3 C4 117.5(7) . .
C5 C4 C3 119.3(8) . .
N1 C5 C4 123.8(7) . .
N1 C5 C6 112.7(6) . .
C4 C5 C6 123.5(7) . .
O4 C6 O5 124.3(7) . .
O4 C6 C5 117.5(7) . .
O5 C6 C5 118.2(7) . .
O6 C7 O3 124.4(7) . .
O6 C7 C1 119.7(7) . .
O3 C7 C1 115.9(6) . .
C5 N1 C1 117.3(6) . .
C5 N1 U1 121.3(5) . .
C1 N1 U1 121.3(5) . .
C7 O3 U1 126.7(5) . .
C6 O4 U1 124.8(5) . .
C6 O5 U1 128.8(6) . 2
C7 O6 U2 128.1(6) . .
U2 O11 U2 110.7(3) 3_756 .
C3 O12 U1 144.8(6) . 4_666
O1 U1 O2 179.1(3) . .
O1 U1 O12 88.6(3) . 4_565
O2 U1 O12 92.3(3) . 4_565
O1 U1 O5 90.9(3) . 2_545
O2 U1 O5 89.0(3) . 2_545
O12 U1 O5 83.5(2) 4_565 2_545
O1 U1 O3 88.5(3) . .
O2 U1 O3 90.7(3) . .
O12 U1 O3 157.7(2) 4_565 .
O5 U1 O3 74.4(2) 2_545 .
O1 U1 O4 92.9(3) . .
O2 U1 O4 87.5(3) . .
O12 U1 O4 75.9(2) 4_565 .
O5 U1 O4 158.9(2) 2_545 .
O3 U1 O4 126.38(19) . .
O1 U1 N1 91.3(3) . .
O2 U1 N1 88.2(3) . .
O12 U1 N1 139.1(2) 4_565 .
O5 U1 N1 137.4(2) 2_545 .
O3 U1 N1 63.1(2) . .
O4 U1 N1 63.3(2) . .
O8 U2 O7 178.9(4) . .
O8 U2 O11 91.9(3) . 3_756
O7 U2 O11 89.3(3) . 3_756
O8 U2 O11 90.2(3) . .
O7 U2 O11 90.3(3) . .
O11 U2 O11 69.3(3) 3_756 .
O8 U2 O6 93.2(3) . .
O7 U2 O6 85.9(3) . .
O11 U2 O6 143.3(2) 3_756 .
O11 U2 O6 74.4(2) . .
O8 U2 O10 92.6(4) . .
O7 U2 O10 87.7(4) . .
O11 U2 O10 74.0(3) 3_756 .
O11 U2 O10 143.2(3) . .
O6 U2 O10 141.9(2) . .
O8 U2 O9 89.6(3) . .
O7 U2 O9 89.5(4) . .
O11 U2 O9 142.8(2) 3_756 .
O11 U2 O9 148.0(2) . .
O6 U2 O9 73.7(2) . .
O10 U2 O9 68.8(3) . .
O8 U2 U2 91.2(2) . 3_756
O7 U2 U2 89.7(3) . 3_756
O11 U2 U2 34.73(16) 3_756 3_756
O11 U2 U2 34.52(16) . 3_756
O6 U2 U2 108.75(14) . 3_756
O10 U2 U2 108.7(2) . 3_756
O9 U2 U2 177.4(2) . 3_756
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.356(10) .
C1 C2 1.395(11) .
C1 C7 1.495(11) .
C2 C3 1.398(12) .
C3 O12 1.315(10) .
C3 C4 1.419(12) .
C4 C5 1.369(11) .
C5 N1 1.343(10) .
C5 C6 1.501(10) .
C6 O4 1.245(10) .
C6 O5 1.278(9) .
C7 O6 1.255(9) .
C7 O3 1.262(10) .
N1 U1 2.507(6) .
O1 U1 1.788(6) .
O2 U1 1.786(6) .
O3 U1 2.420(6) .
O4 U1 2.441(6) .
O5 U1 2.355(6) 2
O6 U2 2.403(6) .
O7 U2 1.795(7) .
O8 U2 1.767(7) .
O9 U2 2.494(8) .
O10 U2 2.476(9) .
O11 U2 2.330(6) 3_756
O11 U2 2.342(7) .
O12 U1 2.258(6) 4_666
U1 O12 2.258(6) 4_565
U1 O5 2.355(6) 2_545
U2 O11 2.330(6) 3_756
U2 U2 3.8438(10) 3_756
