#------------------------------------------------------------------------------
#$Date: 2019-11-23 11:06:01 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233004 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/84/4348492.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_4348492
loop_
_publ_author_name
'Martin, Nicolas P.'
'Falaise, Clément'
'Volkringer, Christophe'
'Henry, Natacha'
'Farger, Pierre'
'Falk, Camille'
'Delahaye, Emilie'
'Rabu, Pierre'
'Loiseau, Thierry'
_publ_section_title
;
 Hydrothermal Crystallization of Uranyl Coordination Polymers Involving an
 Imidazolium Dicarboxylate Ligand: Effect of pH on the Nuclearity of
 Uranyl-Centered Subunits.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8697
_journal_page_last               8705
_journal_paper_doi               10.1021/acs.inorgchem.6b01232
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C14 H14 N4 O10 U'
_chemical_formula_weight         636.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 97.680(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2573(2)
_cell_length_b                   14.3164(5)
_cell_length_c                   14.6263(4)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.423
_cell_measurement_theta_min      2.8455
_cell_volume                     1713.54(9)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_min         1.999
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.541
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6109
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.467
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2166
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         29866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0321P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24783
_reflns_number_total             29866
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01232_si_001.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348492
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
OU1 O 0.9403(5) 0.1000(3) 0.0565(3) 0.0255(11) Uani 1 1 d . .
OU2 O 1.1202(5) 0.1259(3) 0.2883(3) 0.0283(11) Uani 1 1 d . .
O1B O 0.9852(5) -0.0595(3) 0.1838(3) 0.0278(11) Uani 1 1 d . .
O2B O 1.2216(5) -0.0096(3) 0.1506(3) 0.0284(11) Uani 1 1 d . .
C1B C 1.1240(8) -0.0756(5) 0.1607(4) 0.0211(14) Uani 1 1 d . .
N2B N 1.5723(6) -0.1598(4) 0.0768(3) 0.0232(12) Uani 1 1 d . .
N1B N 1.3473(6) -0.1802(3) 0.1338(3) 0.0208(12) Uani 1 1 d . .
C3B C 1.4123(8) -0.1495(4) 0.0609(4) 0.0219(14) Uani 1 1 d . .
H3B H 1.3543 -0.1249 0.0075 0.026 Uiso 1 1 calc R U
C2B C 1.1742(8) -0.1741(4) 0.1453(4) 0.0242(15) Uani 1 1 d . .
H2A H 1.1539 -0.2122 0.1975 0.029 Uiso 1 1 calc R U
H2B H 1.1086 -0.1987 0.0906 0.029 Uiso 1 1 calc R U
C4B C 1.4741(8) -0.2103(5) 0.1990(4) 0.0293(16) Uani 1 1 d . .
H4B H 1.4641 -0.2344 0.2570 0.035 Uiso 1 1 calc R U
O1A O 0.9245(6) 0.2672(3) 0.1626(3) 0.0291(11) Uani 1 1 d . .
O4B O 1.2563(5) 0.1932(3) 0.1354(3) 0.0274(11) Uani 1 1 d . .
O2A O 0.9519(6) 0.3115(3) 0.0181(3) 0.0367(12) Uani 1 1 d . .
N1A N 0.7248(6) 0.4474(4) 0.0160(3) 0.0239(12) Uani 1 1 d . .
O3B O 1.4471(6) 0.2700(3) 0.0723(3) 0.0374(13) Uani 1 1 d . .
C6B C 1.3163(8) 0.1406(5) -0.0094(4) 0.0272(16) Uani 1 1 d . .
H6A H 1.3332 0.0773 0.0134 0.033 Uiso 1 1 calc R U
H6B H 1.2043 0.1458 -0.0390 0.033 Uiso 1 1 calc R U
C1A C 0.8931(8) 0.3186(4) 0.0904(4) 0.0234(15) Uani 1 1 d . .
C7B C 1.3440(8) 0.2085(5) 0.0710(4) 0.0230(14) Uani 1 1 d . .
C2A C 0.7697(9) 0.3951(4) 0.1018(4) 0.0283(16) Uani 1 1 d . .
H2A1 H 0.6723 0.3673 0.1208 0.034 Uiso 1 1 calc R U
H2A2 H 0.8156 0.4377 0.1500 0.034 Uiso 1 1 calc R U
C3A C 0.7956(9) -0.0282(5) 0.4916(4) 0.0320(17) Uani 1 1 d . .
H3A H 0.8702 -0.0646 0.5293 0.038 Uiso 1 1 calc R U
C5B C 1.6127(9) -0.1984(5) 0.1634(4) 0.0300(17) Uani 1 1 d . .
H5B H 1.7172 -0.2132 0.1915 0.036 Uiso 1 1 calc R U
N2A N 0.6299(6) 0.0249(4) 0.3745(3) 0.0229(12) Uani 1 1 d . .
C5A C 0.6246(8) 0.0839(5) 0.4443(4) 0.0246(15) Uani 1 1 d . .
H5A H 0.5615 0.1378 0.4430 0.029 Uiso 1 1 calc R U
C4A C 0.7374(9) -0.0453(5) 0.4030(4) 0.0320(17) Uani 1 1 d . .
H4A H 0.7649 -0.0955 0.3677 0.038 Uiso 1 1 calc R U
O3A O 0.7893(5) 0.0969(3) 0.2418(3) 0.0307(11) Uani 1 1 d . .
C7A C 0.6522(8) 0.0631(4) 0.2088(4) 0.0230(14) Uani 1 1 d . .
C6A C 0.5416(8) 0.0351(5) 0.2808(4) 0.0281(16) Uani 1 1 d . .
H6A1 H 0.4571 0.0820 0.2817 0.034 Uiso 1 1 calc R U
H6A2 H 0.4885 -0.0236 0.2623 0.034 Uiso 1 1 calc R U
O4A O 0.5987(6) 0.0521(4) 0.1282(3) 0.0467(15) Uani 1 1 d . .
U1 U 1.02761(3) 0.11468(2) 0.17245(2) 0.01746(8) 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'
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
C1B O1B U1 91.4(4) . .
C1B O2B U1 95.1(4) . .
O1B C1B O2B 120.8(6) . .
O1B C1B C2B 119.6(6) . .
O2B C1B C2B 119.6(6) . .
O1B C1B U1 62.4(3) . .
O2B C1B U1 58.7(3) . .
C2B C1B U1 174.8(4) . .
C3B N2B C5B 108.6(5) . .
C3B N2B C6B 124.5(5) . 3_855
C5B N2B C6B 126.6(5) . 3_855
C3B N1B C4B 107.7(5) . .
C3B N1B C2B 125.2(5) . .
C4B N1B C2B 126.8(5) . .
N2B C3B N1B 108.9(5) . .
N1B C2B C1B 111.6(5) . .
C5B C4B N1B 107.5(5) . .
C1A O1A U1 128.0(4) . .
C7B O4B U1 144.2(4) . .
C5A N1A C3A 108.8(5) 4_565 4_565
C5A N1A C2A 124.4(6) 4_565 .
C3A N1A C2A 126.1(5) 4_565 .
N2B C6B C7B 111.0(5) 3_855 .
O2A C1A O1A 127.1(6) . .
O2A C1A C2A 120.1(6) . .
O1A C1A C2A 112.8(5) . .
O3B C7B O4B 124.9(6) . .
O3B C7B C6B 120.3(6) . .
O4B C7B C6B 114.7(6) . .
N1A C2A C1A 111.8(5) . .
C4A C3A N1A 107.3(6) . 4_566
C4B C5B N2B 107.2(6) . .
C5A N2A C4A 108.6(5) . .
C5A N2A C6A 126.1(6) . .
C4A N2A C6A 125.2(5) . .
N1A C5A N2A 108.2(6) 4_566 .
C3A C4A N2A 107.0(6) . .
C7A O3A U1 129.5(4) . .
O4A C7A O3A 127.6(6) . .
O4A C7A C6A 117.3(6) . .
O3A C7A C6A 115.0(5) . .
N2A C6A C7A 113.5(5) . .
OU1 U1 OU2 177.86(19) . .
OU1 U1 O4B 94.23(17) . .
OU2 U1 O4B 85.32(17) . .
OU1 U1 O1A 87.33(16) . .
OU2 U1 O1A 94.66(17) . .
O4B U1 O1A 80.47(16) . .
OU1 U1 O3A 98.30(18) . .
OU2 U1 O3A 82.89(18) . .
O4B U1 O3A 155.32(15) . .
O1A U1 O3A 78.97(16) . .
OU1 U1 O2B 88.76(17) . .
OU2 U1 O2B 89.10(18) . .
O4B U1 O2B 75.79(15) . .
O1A U1 O2B 155.58(16) . .
O3A U1 O2B 125.45(15) . .
OU1 U1 O1B 84.45(16) . .
OU2 U1 O1B 94.18(17) . .
O4B U1 O1B 128.11(15) . .
O1A U1 O1B 150.70(16) . .
O3A U1 O1B 74.49(15) . .
O2B U1 O1B 52.33(14) . .
OU1 U1 C1B 84.82(17) . .
OU2 U1 C1B 93.22(18) . .
O4B U1 C1B 101.90(17) . .
O1A U1 C1B 171.93(15) . .
O3A U1 C1B 100.34(17) . .
O2B U1 C1B 26.19(15) . .
O1B U1 C1B 26.21(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
OU1 U1 1.764(4) .
OU2 U1 1.770(4) .
O1B C1B 1.259(7) .
O1B U1 2.527(5) .
O2B C1B 1.263(7) .
O2B U1 2.444(4) .
C1B C2B 1.496(9) .
C1B U1 2.850(7) .
N2B C3B 1.318(8) .
N2B C5B 1.381(7) .
N2B C6B 1.461(8) 3_855
N1B C3B 1.331(7) .
N1B C4B 1.387(7) .
N1B C2B 1.464(8) .
C4B C5B 1.330(9) .
O1A C1A 1.284(7) .
O1A U1 2.341(4) .
O4B C7B 1.281(7) .
O4B U1 2.323(4) .
O2A C1A 1.225(7) .
N1A C5A 1.324(7) 4_565
N1A C3A 1.365(8) 4_565
N1A C2A 1.466(7) .
O3B C7B 1.223(7) .
C6B N2B 1.461(8) 3_855
C6B C7B 1.519(8) .
C1A C2A 1.520(9) .
C3A C4A 1.343(8) .
C3A N1A 1.365(8) 4_566
N2A C5A 1.330(7) .
N2A C4A 1.369(8) .
N2A C6A 1.472(7) .
C5A N1A 1.324(7) 4_566
O3A C7A 1.266(7) .
O3A U1 2.345(4) .
C7A O4A 1.213(7) .
C7A C6A 1.536(9) .
