#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:10:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180469 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/38/7213824.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_7213824
loop_
_publ_author_name
'Surbella III, Robert G.'
'Cahill, Christopher L.'
_publ_section_title
;
 The exploration of supramolecular interactions stemming from the
 [UO2(NCS)4(H2O)]2− tecton and substituted pyridinium cations
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2352
_journal_paper_doi               10.1039/c3ce42106f
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         '(C5 H7 N2 1+)2, (U O3 C4 H2 N4  S4 2-)'
_chemical_formula_sum            'C14 H16 N8 O3 S4 U'
_chemical_formula_weight         710.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.2530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7580(7)
_cell_length_b                   16.0178(14)
_cell_length_c                   16.1291(14)
_cell_measurement_reflns_used    5880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.778
_cell_measurement_theta_min      5.072
_cell_volume                     2253.2(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 2013)'
_computing_data_collection       'APEX II (Bruker AXS, 2013)'
_computing_data_reduction        'SAINT (Bruker AXS, 2013)'
_computing_molecular_graphics    'Crystal Maker v.8.2.2 (Palmer 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker ApexII CCD'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39748
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         1.268
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.607
_exptl_absorpt_correction_T_max  0.745686
_exptl_absorpt_correction_T_min  0.537970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS, G. Sheldrick (2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method 'Slow Evaporation'
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.714
_refine_diff_density_min         -1.477
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0112P)²+10.5513P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4687
_reflns_number_total             5798
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42106f.txt
_cod_data_source_block           Compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2253.1(3)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7213824
#BEGIN Tags that were not found in dictionaries:
_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           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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
C5 C 0.5376(5) 0.9661(3) 0.7502(3) 0.0109(9) Uani 1 1 d . . .
C6 C 0.0883(5) 0.6292(3) 0.7501(3) 0.0120(9) Uani 1 1 d . . .
C1 C 0.9533(8) 0.7500 1.4491(4) 0.0121(13) Uani 1 2 d S T P
C2 C 0.5365(7) 0.7500 1.3527(4) 0.0088(12) Uani 1 2 d S T P
C3 C 0.5004(8) 0.7500 1.1109(4) 0.0116(13) Uani 1 2 d S T P
C4 C 0.9464(7) 0.7500 1.0165(4) 0.0131(14) Uani 1 2 d S T P
C7 C 0.3403(6) 0.4058(3) 0.0061(3) 0.0189(10) Uani 1 1 d . . .
H7 H 0.3839 0.3540 0.0190 0.023 Uiso 1 1 calc R U .
C8 C 0.2527(6) 0.4433(3) 0.0603(3) 0.0165(10) Uani 1 1 d . . .
H8 H 0.2360 0.4168 0.1100 0.020 Uiso 1 1 calc R U .
C9 C 0.1870(5) 0.5221(3) 0.0420(3) 0.0141(10) Uani 1 1 d . . .
C10 C 0.2166(6) 0.5593(3) -0.0343(3) 0.0191(11) Uani 1 1 d . . .
H10 H 0.1767 0.6117 -0.0487 0.023 Uiso 1 1 calc R U .
C11 C 0.3041(6) 0.5181(3) -0.0867(3) 0.0199(11) Uani 1 1 d . . .
H11 H 0.3221 0.5423 -0.1372 0.024 Uiso 1 1 calc R U .
C12 C 0.8092(6) 0.9924(3) 0.3987(3) 0.0176(10) Uani 1 1 d . . .
H12 H 0.8349 0.9852 0.3445 0.021 Uiso 1 1 calc R U .
C13 C 0.7197(6) 0.9351(3) 0.4325(3) 0.0174(10) Uani 1 1 d . . .
H13 H 0.6861 0.8884 0.4019 0.021 Uiso 1 1 calc R U .
C14 C 0.6771(5) 0.9462(3) 0.5143(3) 0.0125(9) Uani 1 1 d . . .
C15 C 0.7333(5) 1.0176(3) 0.5575(3) 0.0133(9) Uani 1 1 d . . .
H15 H 0.7083 1.0272 0.6115 0.016 Uiso 1 1 calc R U .
C16 C 0.8230(5) 1.0723(3) 0.5213(3) 0.0169(10) Uani 1 1 d . . .
H16 H 0.8590 1.1193 0.5506 0.020 Uiso 1 1 calc R U .
N5 N 0.5214(4) 0.8943(2) 0.7394(2) 0.0141(8) Uani 1 1 d . . .
N6 N 0.2082(5) 0.6605(3) 0.7590(3) 0.0163(9) Uani 1 1 d . . .
N1 N 0.9622(6) 0.7500 1.3778(4) 0.0153(12) Uani 1 2 d S T P
N2 N 0.6423(7) 0.7500 1.3144(3) 0.0130(11) Uani 1 2 d S T P
N3 N 0.6291(7) 0.7500 1.1388(4) 0.0172(13) Uani 1 2 d S T P
N4 N 0.9424(6) 0.7500 1.0894(3) 0.0138(12) Uani 1 2 d S T P
N7 N 0.3646(5) 0.4432(3) -0.0665(3) 0.0192(9) Uani 1 1 d . . .
H7A H 0.4200 0.4184 -0.1004 0.023 Uiso 1 1 calc R U .
N8 N 0.0986(5) 0.5593(3) 0.0941(3) 0.0204(9) Uani 1 1 d . . .
H8A H 0.0808 0.5351 0.1398 0.024 Uiso 1 1 calc R U .
H8B H 0.0593 0.6075 0.0819 0.024 Uiso 1 1 calc R U .
N9 N 0.8618(5) 1.0599(2) 0.4428(2) 0.0158(9) Uani 1 1 d . . .
H9 H 0.9202 1.0952 0.4208 0.019 Uiso 1 1 calc R U .
N10 N 0.5868(5) 0.8914(2) 0.5484(2) 0.0170(9) Uani 1 1 d . . .
H10A H 0.5616 0.8994 0.5981 0.020 Uiso 1 1 calc R U .
H10B H 0.5538 0.8481 0.5208 0.020 Uiso 1 1 calc R U .
O2 O 0.4731(5) 0.7500 0.8570(3) 0.0148(10) Uani 1 2 d S T P
O3 O 0.3928(5) 0.7500 0.6379(3) 0.0115(9) Uani 1 2 d S T P
O1 O 0.8633(4) 0.6398(2) 1.2305(2) 0.0158(7) Uani 1 1 d . . .
OW2 O 0.7082(5) 0.7500 0.7271(3) 0.0146(10) Uani 1 2 d S T P
OW1 O 1.1463(5) 0.7500 1.2387(3) 0.0239(12) Uani 1 2 d S T P
S5 S 0.56058(16) 1.06576(7) 0.76271(8) 0.0184(3) Uani 1 1 d . . .
S6 S -0.07808(13) 0.58262(8) 0.73429(7) 0.0144(2) Uani 1 1 d . . .
S1 S 0.9444(2) 0.7500 1.54952(11) 0.0199(4) Uani 1 2 d S T P
S2 S 0.38950(19) 0.7500 1.40896(10) 0.0136(3) Uani 1 2 d S T P
S3 S 0.3255(2) 0.7500 1.07023(12) 0.0214(4) Uani 1 2 d S T P
S4 S 0.9576(2) 0.7500 0.91821(11) 0.0177(4) Uani 1 2 d S T P
U2 U 0.43160(3) 0.7500 0.74748(2) 0.00881(6) Uani 1 2 d S T P
U1 U 0.86303(3) 0.7500 1.23076(2) 0.00926(6) 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 0.0000 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'
S S 0.1246 0.1234 '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
N5 C5 S5 178.6(4) . .
N6 C6 S6 177.5(4) . .
N1 C1 S1 178.9(6) . .
N2 C2 S2 178.6(6) . .
N3 C3 S3 178.5(6) . .
N4 C4 S4 178.2(6) . .
N7 C7 C8 120.5(5) . .
N7 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C7 C8 C9 120.4(5) . .
C7 C8 H8 119.8 . .
C9 C8 H8 119.8 . .
N8 C9 C8 121.2(4) . .
N8 C9 C10 121.6(5) . .
C8 C9 C10 117.2(4) . .
C11 C10 C9 119.6(5) . .
C11 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
N7 C11 C10 121.1(5) . .
N7 C11 H11 119.5 . .
C10 C11 H11 119.5 . .
N9 C12 C13 120.9(4) . .
N9 C12 H12 119.6 . .
C13 C12 H12 119.6 . .
C12 C13 C14 120.2(4) . .
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 . .
N10 C14 C15 121.6(4) . .
N10 C14 C13 121.3(4) . .
C15 C14 C13 117.0(4) . .
C16 C15 C14 120.4(4) . .
C16 C15 H15 119.8 . .
C14 C15 H15 119.8 . .
C15 C16 N9 121.2(4) . .
C15 C16 H16 119.4 . .
N9 C16 H16 119.4 . .
C5 N5 U2 162.8(4) . .
C6 N6 U2 164.8(4) . .
C1 N1 U1 155.5(5) . .
C2 N2 U1 178.9(5) . .
C3 N3 U1 164.8(5) . .
C4 N4 U1 165.2(5) . .
C11 N7 C7 121.2(4) . .
C11 N7 H7A 119.4 . .
C7 N7 H7A 119.4 . .
C9 N8 H8A 120.0 . .
C9 N8 H8B 120.0 . .
H8A N8 H8B 120.0 . .
C12 N9 C16 120.3(4) . .
C12 N9 H9 119.8 . .
C16 N9 H9 119.8 . .
C14 N10 H10A 120.0 . .
C14 N10 H10B 120.0 . .
H10A N10 H10B 120.0 . .
O3 U2 O2 179.2(2) . .
O3 U2 N6 89.65(15) . .
O2 U2 N6 90.98(15) . .
O3 U2 N6 89.65(15) . 4_575
O2 U2 N6 90.98(15) . 4_575
N6 U2 N6 71.78(19) . 4_575
O3 U2 N5 88.85(10) . 4_575
O2 U2 N5 90.89(11) . 4_575
N6 U2 N5 73.37(13) . 4_575
N6 U2 N5 145.12(13) 4_575 4_575
O3 U2 N5 88.85(10) . .
O2 U2 N5 90.89(11) . .
N6 U2 N5 145.12(13) . .
N6 U2 N5 73.37(13) 4_575 .
N5 U2 N5 141.42(18) 4_575 .
O3 U2 OW2 88.16(18) . .
O2 U2 OW2 91.07(19) . .
N6 U2 OW2 144.05(9) . .
N6 U2 OW2 144.05(10) 4_575 .
N5 U2 OW2 70.72(9) 4_575 .
N5 U2 OW2 70.72(9) . .
O1 U1 O1 179.7(2) 4_575 .
O1 U1 N3 89.99(11) 4_575 .
O1 U1 N3 89.99(11) . .
O1 U1 N4 89.85(10) 4_575 .
O1 U1 N4 89.85(10) . .
N3 U1 N4 74.05(18) . .
O1 U1 N1 90.10(11) 4_575 .
O1 U1 N1 90.10(11) . .
N3 U1 N1 143.09(19) . .
N4 U1 N1 142.86(18) . .
O1 U1 N2 90.14(11) 4_575 .
O1 U1 N2 90.14(11) . .
N3 U1 N2 70.81(19) . .
N4 U1 N2 144.86(19) . .
N1 U1 N2 72.29(18) . .
O1 U1 OW1 89.93(11) 4_575 .
O1 U1 OW1 89.92(11) . .
N3 U1 OW1 145.28(18) . .
N4 U1 OW1 71.23(17) . .
N1 U1 OW1 71.62(17) . .
N2 U1 OW1 143.91(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C5 N5 1.171(6) .
C5 S5 1.619(5) .
C6 N6 1.160(6) .
C6 S6 1.636(5) .
C1 N1 1.160(8) .
C1 S1 1.629(6) .
C2 N2 1.159(8) .
C2 S2 1.642(7) .
C3 N3 1.175(8) .
C3 S3 1.610(7) .
C4 N4 1.180(8) .
C4 S4 1.597(7) .
C7 N7 1.348(6) .
C7 C8 1.356(7) .
C7 H7 0.9300 .
C8 C9 1.408(7) .
C8 H8 0.9300 .
C9 N8 1.334(6) .
C9 C10 1.413(7) .
C10 C11 1.362(7) .
C10 H10 0.9300 .
C11 N7 1.340(6) .
C11 H11 0.9300 .
C12 N9 1.352(6) .
C12 C13 1.353(7) .
C12 H12 0.9300 .
C13 C14 1.414(6) .
C13 H13 0.9300 .
C14 N10 1.334(6) .
C14 C15 1.406(6) .
C15 C16 1.344(6) .
C15 H15 0.9300 .
C16 N9 1.356(6) .
C16 H16 0.9300 .
N5 U2 2.448(4) .
N6 U2 2.446(4) .
N1 U1 2.449(6) .
N2 U1 2.457(6) .
N3 U1 2.417(6) .
N4 U1 2.443(5) .
N7 H7A 0.8600 .
N8 H8A 0.8600 .
N8 H8B 0.8600 .
N9 H9 0.8600 .
N10 H10A 0.8600 .
N10 H10B 0.8600 .
O2 U2 1.770(5) .
O3 U2 1.768(4) .
O1 U1 1.765(3) .
OW2 U2 2.475(4) .
OW1 U1 2.472(5) .
U2 N6 2.446(4) 4_575
U2 N5 2.448(4) 4_575
U1 O1 1.765(3) 4_575
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C15 H15 S5 0.93 2.93 3.841(5) 167.0
N10 H10A N5 0.86 2.34 3.185(6) 167.7
