#------------------------------------------------------------------------------
#$Date: 2021-02-12 15:49:47 +0100 (vie 12 de feb de 2021) $
#$Revision: 261924 $
#$URL: svn://www.crystallography.net/cod/cif/1/56/03/1560365.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_1560365
loop_
_publ_author_name
'Jayasinghe, Ashini S.'
'Payne, Maurice K.'
'Forbes, Tori Z.'
_publ_section_title
;
 Synthesis and characterization of heterometallic uranyl
 pyridinedicarboxylate compounds
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              25
_journal_page_last               31
_journal_paper_doi               10.1016/j.jssc.2017.07.002
_journal_volume                  254
_journal_year                    2017
_chemical_formula_sum            'C14 H14 N2 O18 U Zn'
_chemical_formula_weight         801.67
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-06-23T16:37:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.82(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.751(17)
_cell_length_b                   7.149(7)
_cell_length_c                   10.905(10)
_cell_measurement_reflns_used    648
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.56
_cell_measurement_theta_min      2.77
_cell_volume                     1146(2)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CrystalMaker v2.5.0'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.128
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10131
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.462
_diffrn_reflns_theta_min         1.874
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.195
_exptl_absorpt_correction_T_max  0.4288
_exptl_absorpt_correction_T_min  0.3404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.6
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.0044(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1139
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0532P)²+6.4654P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0
_reflns_number_gt                850
_reflns_number_total             1139
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc2.cif
_cod_data_source_block           c2_m_new_a
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               1560365
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5 0.5 0.5 0.0472(5) Uani 1 4 d S T P . .
Zn2 Zn 0.5 0.5 1 0.0414(6) Uani 1 4 d DS T P . .
O1 O 0.5 0.2531(15) 0.5 0.059(3) Uani 1 2 d S T P . .
O2 O 0.3741(6) 0.5 0.3313(9) 0.058(3) Uani 1 2 d S T P . .
O3 O 0.2304(6) 0.5 0.2490(8) 0.056(3) Uani 1 2 d S T P . .
O4 O 0.3850(6) 0.5 0.8719(8) 0.054(3) Uani 1 2 d S T P . .
O5 O 0.4657(7) 0.546(3) 0.7098(10) 0.043(8) Uani 0.5 1 d . . P . .
O6 O 0.4311(7) 0.3009(13) 1.0949(8) 0.086(3) Uani 1 1 d D . . . .
H6A H 0.411(9) 0.310(9) 1.166(6) 0.103 Uiso 1 1 d D U . . .
H6B H 0.436(8) 0.182(3) 1.088(9) 0.103 Uiso 1 1 d D U . . .
OW1 O 0.0414(8) 0.5 0.1902(12) 0.078(4) Uani 1 2 d S T P . .
OW2 O 0.2646(11) 0.157(2) 0.9867(15) 0.080(6) Uani 0.5 1 d . . P A -1
N1 N 0.3292(7) 0.5 0.5543(9) 0.033(2) Uani 1 2 d S T P . .
C1 C 0.2888(9) 0.5 0.3360(12) 0.038(3) Uani 1 2 d S T P . .
C2 C 0.2602(8) 0.5 0.4665(11) 0.033(3) Uani 1 2 d S T P . .
C3 C 0.1701(8) 0.5 0.4951(12) 0.040(3) Uani 1 2 d S T P . .
H3 H 0.12189 0.5 0.431686 0.047 Uiso 1 2 calc R U P . .
C4 C 0.1522(9) 0.5 0.6153(12) 0.047(4) Uani 1 2 d S T P . .
H4 H 0.090915 0.5 0.635826 0.056 Uiso 1 2 calc R U P . .
C5 C 0.2225(8) 0.5 0.7084(13) 0.041(3) Uani 1 2 d S T P . .
H5 H 0.210836 0.5 0.792759 0.049 Uiso 1 2 calc R U P . .
C6 C 0.3104(9) 0.5 0.6726(12) 0.038(3) Uani 1 2 d S T P . .
C7 C 0.3932(9) 0.5 0.7608(13) 0.048(4) Uani 1 2 d S T P . .
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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 U1 O1 180 . 5_666
O1 U1 O5 97.9(5) . .
O1 U1 O5 82.1(5) 5_666 .
O1 U1 O5 82.1(5) . 5_666
O1 U1 O5 97.9(5) 5_666 5_666
O5 U1 O5 180 . 5_666
O1 U1 O5 82.1(5) . 6_565
O1 U1 O5 97.9(5) 5_666 6_565
O5 U1 O5 15.8(10) . 6_565
O5 U1 O5 164.2(10) 5_666 6_565
O1 U1 O5 97.9(5) . 2_656
O1 U1 O5 82.1(5) 5_666 2_656
O5 U1 O5 164.2(10) . 2_656
O5 U1 O5 15.8(10) 5_666 2_656
O5 U1 O5 180 6_565 2_656
O1 U1 O2 90.000(2) . .
O1 U1 O2 90.0000(10) 5_666 .
O5 U1 O2 119.8(3) . .
O5 U1 O2 60.2(3) 5_666 .
O5 U1 O2 119.8(3) 6_565 .
O5 U1 O2 60.2(3) 2_656 .
O1 U1 O2 90.0000(10) . 5_666
O1 U1 O2 90.000(2) 5_666 5_666
O5 U1 O2 60.2(3) . 5_666
O5 U1 O2 119.8(3) 5_666 5_666
O5 U1 O2 60.2(3) 6_565 5_666
O5 U1 O2 119.8(3) 2_656 5_666
O2 U1 O2 180 . 5_666
O1 U1 N1 90.000(2) . .
O1 U1 N1 90.000(2) 5_666 .
O5 U1 N1 60.3(3) . .
O5 U1 N1 119.7(3) 5_666 .
O5 U1 N1 60.3(3) 6_565 .
O5 U1 N1 119.7(3) 2_656 .
O2 U1 N1 60.1(3) . .
O2 U1 N1 119.9(3) 5_666 .
O1 U1 N1 90.000(2) . 5_666
O1 U1 N1 90.000(3) 5_666 5_666
O5 U1 N1 119.7(3) . 5_666
O5 U1 N1 60.3(3) 5_666 5_666
O5 U1 N1 119.7(3) 6_565 5_666
O5 U1 N1 60.3(3) 2_656 5_666
O2 U1 N1 119.9(3) . 5_666
O2 U1 N1 60.1(3) 5_666 5_666
N1 U1 N1 180 . 5_666
O6 Zn2 O6 86.6(6) . 6_565
O6 Zn2 O6 93.4(6) . 2_657
O6 Zn2 O6 180 6_565 2_657
O6 Zn2 O6 180.0(4) . 5_667
O6 Zn2 O6 93.4(6) 6_565 5_667
O6 Zn2 O6 86.6(6) 2_657 5_667
O6 Zn2 O4 94.0(3) . 5_667
O6 Zn2 O4 94.0(3) 6_565 5_667
O6 Zn2 O4 86.0(3) 2_657 5_667
O6 Zn2 O4 86.0(3) 5_667 5_667
O6 Zn2 O4 86.0(3) . .
O6 Zn2 O4 86.0(3) 6_565 .
O6 Zn2 O4 94.0(3) 2_657 .
O6 Zn2 O4 94.0(3) 5_667 .
O4 Zn2 O4 180 5_667 .
C1 O2 U1 130.5(8) . .
C7 O4 Zn2 120.9(8) . .
O5 O5 C7 75.1(10) 6_565 .
O5 O5 U1 82.1(5) 6_565 .
C7 O5 U1 128.5(10) . .
Zn2 O6 H6A 128(4) . .
Zn2 O6 H6B 126(4) . .
H6A O6 H6B 102(4) . .
C2 N1 C6 118.7(10) . .
C2 N1 U1 121.6(8) . .
C6 N1 U1 119.7(8) . .
O3 C1 O2 127.2(12) . .
O3 C1 C2 119.5(12) . .
O2 C1 C2 113.2(11) . .
N1 C2 C3 121.6(11) . .
N1 C2 C1 114.6(11) . .
C3 C2 C1 123.8(11) . .
C4 C3 C2 118.9(12) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 C5 120.8(12) . .
C3 C4 H4 119.6 . .
C5 C4 H4 119.6 . .
C6 C5 C4 116.9(12) . .
C6 C5 H5 121.6 . .
C4 C5 H5 121.6 . .
N1 C6 C5 123.1(12) . .
N1 C6 C7 113.3(11) . .
C5 C6 C7 123.6(12) . .
O4 C7 O5 125.4(12) . 6_565
O4 C7 O5 125.4(12) . .
O5 C7 O5 29.7(19) 6_565 .
O4 C7 C6 119.6(12) . .
O5 C7 C6 112.7(12) 6_565 .
O5 C7 C6 112.7(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.765(11) .
U1 O1 1.765(11) 5_666
U1 O5 2.407(11) .
U1 O5 2.407(11) 5_666
U1 O5 2.407(11) 6_565
U1 O5 2.407(11) 2_656
U1 O2 2.502(9) .
U1 O2 2.502(9) 5_666
U1 N1 2.636(10) .
U1 N1 2.636(10) 5_666
Zn2 O6 2.076(8) .
Zn2 O6 2.076(8) 6_565
Zn2 O6 2.076(8) 2_657
Zn2 O6 2.076(8) 5_667
Zn2 O4 2.105(9) 5_667
Zn2 O4 2.105(9) .
O2 C1 1.265(15) .
O3 C1 1.227(15) .
O4 C7 1.228(15) .
O5 O5 0.66(4) 6_565
O5 C7 1.289(17) .
O6 H6A 0.85(2) .
O6 H6B 0.86(2) .
N1 C2 1.338(16) .
N1 C6 1.341(16) .
C1 C2 1.518(18) .
C2 C3 1.389(17) .
C3 C4 1.358(18) .
C3 H3 0.95 .
C4 C5 1.389(18) .
C4 H4 0.95 .
C5 C6 1.385(18) .
C5 H5 0.95 .
C6 C7 1.490(19) .
