#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:39:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180443 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/12/7211252.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_7211252
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            'C14 H4 Cl2 N2 O15 U2'
_chemical_formula_weight         987.15
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8835(8)
_cell_length_b                   9.2545(8)
_cell_length_c                   28.075(3)
_cell_measurement_reflns_used    43356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      57.113
_cell_measurement_theta_min      4.634
_cell_volume                     2308.1(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43210
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.323
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.585
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.630(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0253
_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)+(0.0197P)²+11.1637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0559
_reflns_number_gt                5615
_reflns_number_total             5896
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3ce41655k.txt
_cod_data_source_block           Compound6
_cod_database_code               7211252
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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
C1 C 0.2428(7) 0.8249(7) 0.8862(2) 0.0103(12) Uani 1 1 d .
C2 C 0.3092(7) 0.9558(7) 0.8981(2) 0.0126(12) Uani 1 1 d .
H8 H 0.3560 0.9688 0.9274 0.015 Uiso 1 1 calc R
C3 C 0.3036(8) 1.0665(7) 0.8650(2) 0.0155(13) Uani 1 1 d .
C5 C 0.2288(8) 1.0477(7) 0.8213(2) 0.0177(13) Uani 1 1 d .
H6 H 0.2205 1.1224 0.7993 0.021 Uiso 1 1 calc R
C6 C 0.1676(7) 0.9113(7) 0.8126(2) 0.0144(13) Uani 1 1 d .
C7 C 0.0897(7) 0.8701(7) 0.7673(2) 0.0122(12) Uani 1 1 d .
C8 C 0.2440(7) 0.6936(7) 0.9176(2) 0.0130(13) Uani 1 1 d .
C9 C 0.1053(8) 0.7913(8) 1.1239(2) 0.0166(14) Uani 1 1 d .
C10 C 0.0380(7) 0.8210(7) 1.1680(2) 0.0185(14) Uani 1 1 d .
H11 H -0.0114 0.9082 1.1731 0.022 Uiso 1 1 calc R
C11 C 0.0462(8) 0.7195(8) 1.2034(2) 0.0192(14) Uani 1 1 d .
C12 C 0.1284(8) 0.5905(8) 1.1954(2) 0.0203(15) Uani 1 1 d .
H4 H 0.1414 0.5225 1.2195 0.024 Uiso 1 1 calc R
C13 C 0.1891(7) 0.5693(8) 1.1502(2) 0.0187(14) Uani 1 1 d .
C14 C 0.2789(9) 0.4367(9) 1.1368(2) 0.0259(16) Uani 1 1 d .
C15 C 0.1091(8) 0.8953(8) 1.0826(2) 0.0185(14) Uani 1 1 d .
N1 N 0.1742(6) 0.8037(6) 0.84413(18) 0.0133(11) Uani 1 1 d .
N2 N 0.1756(6) 0.6652(6) 1.11524(19) 0.0127(11) Uani 1 1 d .
O1 O 0.2251(6) 0.5030(5) 0.79833(15) 0.0177(10) Uani 1 1 d .
O2 O -0.1094(5) 0.6237(5) 0.85364(16) 0.0182(10) Uani 1 1 d .
O3 O 0.0151(6) 0.3287(5) 0.86215(18) 0.0255(12) Uani 1 1 d .
O4 O 0.0902(5) 0.9591(5) 0.73353(15) 0.0164(10) Uani 1 1 d .
O5 O 0.0277(6) 0.7490(5) 0.76665(15) 0.0164(10) Uani 1 1 d .
O6 O 0.1837(5) 0.5825(5) 0.90108(15) 0.0142(10) Uani 1 1 d .
O7 O 0.4615(6) 0.6859(6) 1.05086(16) 0.0221(11) Uani 1 1 d .
O8 O 0.1054(6) 0.5426(6) 1.02045(17) 0.0216(11) Uani 1 1 d .
O9 O 0.3994(7) 0.4127(5) 0.99349(19) 0.0316(14) Uani 1 1 d .
O10 O 0.3104(5) 0.7056(5) 0.95739(15) 0.0151(10) Uani 1 1 d .
O11 O 0.1792(6) 0.8473(5) 1.04603(16) 0.0204(11) Uani 1 1 d .
O12 O 0.3184(7) 0.4339(6) 1.09336(17) 0.0333(14) Uani 1 1 d .
O13 O 0.0482(8) 1.0150(6) 1.08633(17) 0.0307(13) Uani 1 1 d .
O14 O 0.3067(7) 0.3464(6) 1.16787(18) 0.0350(15) Uani 1 1 d .
OW1 O 0.442(4) 0.1546(14) 1.0383(4) 0.45(3) Uani 1 1 d .
U1 U 0.05606(3) 0.56143(2) 0.826105(8) 0.00998(5) Uani 1 1 d .
U2 U 0.28471(3) 0.61467(3) 1.035087(8) 0.01466(6) Uani 1 1 d .
Cl1 Cl 0.3896(2) 1.22886(18) 0.87759(6) 0.0248(4) Uani 1 1 d .
Cl2 Cl -0.0391(2) 0.7432(2) 1.25723(6) 0.0273(4) 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'
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'
Cl Cl 0.1484 0.1585 '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 122.1(6) . .
N1 C1 C8 113.6(5) . .
C2 C1 C8 124.2(5) . .
C1 C2 C3 118.0(6) . .
C2 C3 C5 120.8(6) . .
C2 C3 Cl1 119.4(5) . .
C5 C3 Cl1 119.8(5) . .
C6 C5 C3 116.7(6) . .
N1 C6 C5 122.8(6) . .
N1 C6 C7 113.2(5) . .
C5 C6 C7 124.0(6) . .
O5 C7 O4 125.3(6) . .
O5 C7 C6 116.5(5) . .
O4 C7 C6 118.2(6) . .
O6 C8 O10 126.8(6) . .
O6 C8 C1 116.5(5) . .
O10 C8 C1 116.7(5) . .
N2 C9 C10 121.9(7) . .
N2 C9 C15 113.8(6) . .
C10 C9 C15 124.3(6) . .
C11 C10 C9 119.0(6) . .
C10 C11 C12 119.3(6) . .
C10 C11 Cl2 122.1(6) . .
C12 C11 Cl2 118.6(5) . .
C13 C12 C11 117.6(6) . .
N2 C13 C12 122.9(7) . .
N2 C13 C14 113.9(6) . .
C12 C13 C14 123.1(6) . .
O14 C14 O12 127.6(7) . .
O14 C14 C13 118.7(6) . .
O12 C14 C13 113.7(6) . .
O13 C15 O11 126.2(7) . .
O13 C15 C9 119.8(6) . .
O11 C15 C9 114.0(6) . .
C6 N1 C1 119.6(6) . .
C6 N1 U1 120.8(4) . .
C1 N1 U1 119.6(4) . .
C13 N2 C9 119.2(6) . .
C13 N2 U2 120.4(4) . .
C9 N2 U2 120.4(4) . .
C7 O4 U1 144.1(4) . 4_556
C7 O5 U1 125.9(4) . .
C8 O6 U1 126.5(4) . .
C8 O10 U2 137.8(4) . .
C15 O11 U2 127.7(5) . .
C14 O12 U2 128.1(5) . .
O2 U1 O1 178.6(2) . .
O2 U1 O4 89.0(2) . 4_546
O1 U1 O4 91.87(19) . 4_546
O2 U1 O3 89.0(2) . .
O1 U1 O3 92.3(2) . .
O4 U1 O3 81.58(16) 4_546 .
O2 U1 O6 89.02(19) . .
O1 U1 O6 90.59(18) . .
O4 U1 O6 158.53(15) 4_546 .
O3 U1 O6 77.01(16) . .
O2 U1 O5 88.9(2) . .
O1 U1 O5 90.21(19) . .
O4 U1 O5 74.74(15) 4_546 .
O3 U1 O5 156.26(16) . .
O6 U1 O5 126.58(15) . .
O2 U1 N1 88.2(2) . .
O1 U1 N1 90.4(2) . .
O4 U1 N1 137.64(17) 4_546 .
O3 U1 N1 140.58(17) . .
O6 U1 N1 63.64(16) . .
O5 U1 N1 62.95(16) . .
O7 U2 O8 178.8(2) . .
O7 U2 O10 90.72(19) . .
O8 U2 O10 90.40(19) . .
O7 U2 O12 88.7(2) . .
O8 U2 O12 90.5(2) . .
O10 U2 O12 152.34(17) . .
O7 U2 O11 88.9(2) . .
O8 U2 O11 90.9(2) . .
O10 U2 O11 80.40(16) . .
O12 U2 O11 127.22(17) . .
O7 U2 O9 92.0(2) . .
O8 U2 O9 88.6(2) . .
O10 U2 O9 77.79(17) . .
O12 U2 O9 74.60(18) . .
O11 U2 O9 158.18(17) . .
O7 U2 N2 92.9(2) . .
O8 U2 N2 86.0(2) . .
O10 U2 N2 143.93(17) . .
O12 U2 N2 63.68(18) . .
O11 U2 N2 63.81(17) . .
O9 U2 N2 137.84(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.344(8) .
C1 C2 1.388(9) .
C1 C8 1.501(8) .
C2 C3 1.385(9) .
C3 C5 1.405(9) .
C3 Cl1 1.722(7) .
C5 C6 1.396(9) .
C6 N1 1.334(8) .
C6 C7 1.496(8) .
C7 O5 1.250(8) .
C7 O4 1.257(7) .
C8 O6 1.249(7) .
C8 O10 1.268(7) .
C9 N2 1.346(8) .
C9 C10 1.402(9) .
C9 C15 1.507(10) .
C10 C11 1.370(10) .
C11 C12 1.417(10) .
C11 Cl2 1.703(7) .
C12 C13 1.392(8) .
C13 N2 1.330(9) .
C13 C14 1.511(10) .
C14 O14 1.232(8) .
C14 O12 1.270(8) .
C15 O13 1.237(9) .
C15 O11 1.281(8) .
N1 U1 2.527(5) .
N2 U2 2.495(5) .
O1 U1 1.777(5) .
O2 U1 1.758(5) .
O3 U1 2.407(5) .
O4 U1 2.321(4) 4_556
O5 U1 2.421(4) .
O6 U1 2.399(4) .
O7 U2 1.760(5) .
O8 U2 1.775(5) .
O9 U2 2.429(5) .
O10 U2 2.349(4) .
O11 U2 2.368(5) .
O12 U2 2.359(5) .
U1 O4 2.321(4) 4_546
