#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:39:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180443 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/12/7211250.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_7211250
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 N2 O18 U3'
_chemical_formula_weight         1202.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 106.0310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0704(10)
_cell_length_b                   8.3162(8)
_cell_length_c                   13.6240(13)
_cell_measurement_reflns_used    8013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.566
_cell_measurement_theta_min      5.803
_cell_volume                     1096.61(18)
_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    'SHELXS-97, G. Sheldrick (1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'Bruker Apex CCD II'
_diffrn_measurement_method       omega
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7704
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.32
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    22.193
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5382
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.757
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0306
_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)+(0.0201P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                2263
_reflns_number_total             2836
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3ce41655k.txt
_cod_data_source_block           Compound4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7211250
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 0.2758(8) 0.5409(9) 0.1157(5) 0.0121(15) Uani 1 1 d .
C2 C 0.1779(8) 0.4241(9) 0.1082(5) 0.0141(16) Uani 1 1 d .
H1 H 0.0846 0.4492 0.0832 0.017 Uiso 1 1 calc R
C3 C 0.2196(7) 0.2629(9) 0.1391(5) 0.0102(14) Uani 1 1 d .
C4 C 0.3617(7) 0.2412(9) 0.1849(5) 0.0105(15) Uani 1 1 d .
H2 H 0.3947 0.1414 0.2115 0.013 Uiso 1 1 calc R
C5 C 0.4521(8) 0.3668(9) 0.1904(5) 0.0120(15) Uani 1 1 d .
C6 C 0.6055(8) 0.3547(8) 0.2306(5) 0.0095(14) Uani 1 1 d .
C7 C 0.2432(9) 0.7125(9) 0.0816(5) 0.0147(16) Uani 1 1 d .
N1 N 0.4121(6) 0.5163(7) 0.1559(4) 0.0094(12) Uani 1 1 d .
O1 O 0.6014(6) 0.6704(6) 0.0395(3) 0.0158(11) Uani 1 1 d .
O2 O 0.5660(5) 0.8024(6) 0.2756(4) 0.0169(12) Uani 1 1 d .
O3 O 0.6733(5) 0.4814(6) 0.2272(3) 0.0137(11) Uani 1 1 d .
O4 O 0.3448(6) 0.8016(6) 0.0808(4) 0.0178(12) Uani 1 1 d .
O5 O 0.5969(5) 1.0088(6) 0.1001(3) 0.0130(11) Uani 1 1 d .
O6 O 0.6621(5) 0.2235(6) 0.2653(4) 0.0147(11) Uani 1 1 d .
O7 O 0.1182(5) 0.7564(6) 0.0558(4) 0.0142(11) Uani 1 1 d .
O8 O 0.1322(5) 0.1447(6) 0.1277(3) 0.0120(10) Uani 1 1 d .
O9 O -0.1160(5) 0.9513(6) 0.0730(3) 0.0136(11) Uani 1 1 d .
U1 U 0.58514(3) 0.73290(3) 0.158761(19) 0.00993(8) Uani 1 1 d .
U2 U 0.0000 1.0000 0.0000 0.00797(9) Uani 1 2 d S
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'
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 123.7(7) . .
N1 C1 C7 112.4(7) . .
C2 C1 C7 123.9(7) . .
C1 C2 C3 119.7(7) . .
C1 C2 H1 120.1 . .
C3 C2 H1 120.1 . .
O8 C3 C4 121.9(7) . .
O8 C3 C2 122.6(6) . .
C4 C3 C2 115.5(6) . .
C5 C4 C3 120.3(7) . .
C5 C4 H2 119.8 . .
C3 C4 H2 119.8 . .
N1 C5 C4 123.5(7) . .
N1 C5 C6 111.6(6) . .
C4 C5 C6 124.9(6) . .
O6 C6 O3 122.8(7) . .
O6 C6 C5 120.7(7) . .
O3 C6 C5 116.5(6) . .
O7 C7 O4 125.0(7) . .
O7 C7 C1 118.3(7) . .
O4 C7 C1 116.7(7) . .
C1 N1 C5 117.0(6) . .
C1 N1 U1 121.7(5) . .
C5 N1 U1 121.2(5) . .
C6 O3 U1 127.2(5) . .
C7 O4 U1 124.6(5) . .
C6 O6 U1 115.9(5) . 2_645
C7 O7 U2 135.3(5) . .
C3 O8 U2 137.8(4) . 1_545
O2 U1 O1 177.7(2) . .
O2 U1 O3 93.3(2) . .
O1 U1 O3 89.0(2) . .
O2 U1 O4 88.5(2) . .
O1 U1 O4 90.1(2) . .
O3 U1 O4 127.04(17) . .
O2 U1 O5 90.8(2) . .
O1 U1 O5 87.1(2) . .
O3 U1 O5 156.07(17) . .
O4 U1 O5 76.60(17) . .
O2 U1 O6 89.4(2) . 2_655
O1 U1 O6 91.7(2) . 2_655
O3 U1 O6 64.84(17) . 2_655
O4 U1 O6 168.04(17) . 2_655
O5 U1 O6 91.68(16) . 2_655
O2 U1 N1 90.1(2) . .
O1 U1 N1 90.9(2) . .
O3 U1 N1 63.41(18) . .
O4 U1 N1 63.66(18) . .
O5 U1 N1 140.21(17) . .
O6 U1 N1 128.12(17) 2_655 .
O9 U2 O9 180.0 . 3_575
O9 U2 O8 88.3(2) . 3_565
O9 U2 O8 91.7(2) 3_575 3_565
O9 U2 O8 91.7(2) . 1_565
O9 U2 O8 88.3(2) 3_575 1_565
O8 U2 O8 180.00(19) 3_565 1_565
O9 U2 O7 91.4(2) . 3_575
O9 U2 O7 88.6(2) 3_575 3_575
O8 U2 O7 94.16(17) 3_565 3_575
O8 U2 O7 85.84(17) 1_565 3_575
O9 U2 O7 88.6(2) . .
O9 U2 O7 91.4(2) 3_575 .
O8 U2 O7 85.84(17) 3_565 .
O8 U2 O7 94.16(17) 1_565 .
O7 U2 O7 180.0 3_575 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.345(9) .
C1 C2 1.368(10) .
C1 C7 1.508(10) .
C2 C3 1.433(10) .
C2 H1 0.9300 .
C3 O8 1.300(8) .
C3 C4 1.406(10) .
C4 C5 1.374(10) .
C4 H2 0.9300 .
C5 N1 1.351(9) .
C5 C6 1.493(10) .
C6 O6 1.261(8) .
C6 O3 1.264(8) .
C7 O7 1.264(9) .
C7 O4 1.266(9) .
N1 U1 2.499(6) .
O1 U1 1.757(5) .
O2 U1 1.753(5) .
O3 U1 2.361(5) .
O4 U1 2.428(5) .
O5 U1 2.444(5) .
O6 U1 2.470(5) 2_645
O7 U2 2.367(5) .
O8 U2 2.229(5) 1_545
O9 U2 1.778(5) .
U1 O6 2.470(5) 2_655
U2 O9 1.778(5) 3_575
U2 O8 2.229(5) 3_565
U2 O8 2.229(5) 1_565
U2 O7 2.367(5) 3_575
