#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:10:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180469 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/38/7213823.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_7213823
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         '(C6 H8 N1 1+)2, (U O3 C4 H2 N4 S4 2-)'
_chemical_formula_sum            'C16 H18 N6 O3 S4 U'
_chemical_formula_weight         708.63
_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                 95.282(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.761(2)
_cell_length_b                   16.018(4)
_cell_length_c                   16.129(4)
_cell_measurement_reflns_used    3692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      48.472
_cell_measurement_theta_min      5.073
_cell_volume                     2253.8(9)
_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 0.932
_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_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25394
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.443
_diffrn_reflns_theta_min         1.268
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.603
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1344
_exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.253
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         6584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0418
_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)+(0.0240P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5115
_reflns_number_total             6584
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42106f.txt
_cod_data_source_block           Compound_6
_cod_original_cell_volume        2253.8(10)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7213823
#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
C1 C 0.5468(9) 0.2500 0.0494(5) 0.0165(17) Uani 1 2 d S T P
C2 C 0.9645(9) 0.2500 0.1482(5) 0.0126(15) Uani 1 2 d S T P
C3 C 0.9989(8) 0.2500 0.3884(4) 0.0098(14) Uani 1 2 d S T P
C4 C 0.5552(8) 0.2500 0.4831(5) 0.0117(15) Uani 1 2 d S T P
C5 C 1.0370(6) 0.9660(4) 0.2499(3) 0.0129(11) Uani 1 1 d . . .
C6 C 0.5873(6) 0.6298(3) 0.2497(3) 0.0123(11) Uani 1 1 d . . .
C7 C 0.8036(7) -0.0188(4) 0.4135(3) 0.0176(12) Uani 1 1 d . . .
H7 H 0.8217 -0.0435 0.3632 0.021 Uiso 1 1 calc R U .
C8 C 0.7154(7) -0.0595(4) 0.4658(4) 0.0191(12) Uani 1 1 d . . .
H8 H 0.6741 -0.1116 0.4514 0.023 Uiso 1 1 calc R U .
C9 C 0.6874(6) -0.0220(4) 0.5420(3) 0.0151(12) Uani 1 1 d . . .
C10 C 0.7545(6) 0.0571(3) 0.5605(3) 0.0146(11) Uani 1 1 d . . .
H10 H 0.7395 0.0833 0.6106 0.018 Uiso 1 1 calc R U .
C11 C 0.8403(7) 0.0947(4) 0.5058(4) 0.0202(13) Uani 1 1 d . . .
H11 H 0.8826 0.1470 0.5180 0.024 Uiso 1 1 calc R U .
C12 C 0.5982(6) -0.0591(3) 0.5948(3) 0.0095(10) Uani 1 1 d . . .
H12A H 0.6375 -0.0474 0.6511 0.014 Uiso 1 1 calc R U .
H12B H 0.5980 -0.1184 0.5858 0.014 Uiso 1 1 calc R U .
H12C H 0.4955 -0.0382 0.5852 0.014 Uiso 1 1 calc R U .
C13 C 0.6767(6) 0.5730(4) 0.9793(4) 0.0173(12) Uani 1 1 d . . .
H13 H 0.6405 0.6203 0.9505 0.021 Uiso 1 1 calc R U .
C14 C 0.7663(6) 0.5183(3) 0.9423(4) 0.0152(11) Uani 1 1 d . . .
H14 H 0.7906 0.5280 0.8882 0.018 Uiso 1 1 calc R U .
C15 C 0.8240(6) 0.4457(3) 0.9859(4) 0.0131(11) Uani 1 1 d . . .
C16 C 0.7818(7) 0.4354(4) 1.0676(4) 0.0176(12) Uani 1 1 d . . .
H16 H 0.8171 0.3893 1.0989 0.021 Uiso 1 1 calc R U .
C17 C 0.6900(7) 0.4923(4) 1.1010(4) 0.0199(13) Uani 1 1 d . . .
H17 H 0.6620 0.4845 1.1547 0.024 Uiso 1 1 calc R U .
C18 C 0.9132(5) 0.3910(3) 0.9516(3) 0.0057(9) Uani 1 1 d . . .
H18A H 0.9705 0.4190 0.9119 0.009 Uiso 1 1 calc R U .
H18B H 0.8510 0.3482 0.9240 0.009 Uiso 1 1 calc R U .
H18C H 0.9827 0.3663 0.9942 0.009 Uiso 1 1 calc R U .
N1 N 0.5371(7) 0.2500 0.1224(4) 0.0159(14) Uani 1 2 d S T P
N2 N 0.8578(7) 0.2500 0.1857(4) 0.0139(14) Uani 1 2 d S T P
N3 N 0.8720(8) 0.2500 0.3605(4) 0.0224(16) Uani 1 2 d S T P
N4 N 0.5572(8) 0.2500 0.4096(4) 0.0178(15) Uani 1 2 d S T P
N5 N 1.0215(5) 0.8942(3) 0.2396(3) 0.0158(10) Uani 1 1 d . . .
N6 N 0.7081(5) 0.6607(3) 0.2588(3) 0.0147(10) Uani 1 1 d . . .
N7 N 0.8649(6) 0.0564(3) 0.4330(3) 0.0219(11) Uani 1 1 d . . .
H7A H 0.9206 0.0806 0.3989 0.026 Uiso 1 1 calc R U .
N8 N 0.6391(6) 0.5598(3) 1.0568(3) 0.0182(11) Uani 1 1 d . . .
H8A H 0.5812 0.5952 1.0789 0.022 Uiso 1 1 calc R U .
O1 O 0.6369(4) 0.1398(2) 0.2692(2) 0.0168(9) Uani 1 1 d . . .
O2 O 0.9738(6) 0.7500 0.3564(3) 0.0176(12) Uani 1 2 d S T P
O3 O 0.8938(6) 0.7500 0.1386(3) 0.0149(12) Uani 1 2 d S T P
OW1 O 0.3522(6) 0.2500 0.2610(4) 0.0236(14) Uani 1 2 d S T P
OW2 O 1.2086(6) 0.7500 0.2272(3) 0.0159(12) Uani 1 2 d S T P
S1 S 0.5555(3) 0.2500 -0.04947(13) 0.0201(4) Uani 1 2 d S T P
S2 S 1.1099(2) 0.2500 0.09112(12) 0.0140(4) Uani 1 2 d S T P
S3 S 1.1749(2) 0.2500 0.42978(14) 0.0227(5) Uani 1 2 d S T P
S4 S 0.5426(3) 0.2500 0.58146(13) 0.0183(4) Uani 1 2 d S T P
S5 S 1.06069(18) 1.06576(9) 0.26263(9) 0.0180(3) Uani 1 1 d . . .
S6 S 0.42167(15) 0.58262(9) 0.23438(9) 0.0145(3) Uani 1 1 d . . .
U1 U 0.63693(3) 0.2500 0.26921(2) 0.00971(8) Uani 1 2 d S T P
U2 U 0.93156(3) 0.7500 0.24751(2) 0.00930(8) 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
N1 C1 S1 178.7(7) . .
N2 C2 S2 177.3(7) . .
N3 C3 S3 178.6(7) . .
N4 C4 S4 176.9(7) . .
N5 C5 S5 178.9(5) . .
N6 C6 S6 177.1(5) . .
N7 C7 C8 121.4(5) . .
N7 C7 H7 119.3 . .
C8 C7 H7 119.3 . .
C7 C8 C9 119.4(6) . .
C7 C8 H8 120.3 . .
C9 C8 H8 120.3 . .
C12 C9 C8 121.4(5) . .
C12 C9 C10 121.0(5) . .
C8 C9 C10 117.6(5) . .
C11 C10 C9 120.3(5) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C10 C11 N7 120.3(6) . .
C10 C11 H11 119.9 . .
N7 C11 H11 119.9 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N8 C13 C14 120.9(5) . .
N8 C13 H13 119.6 . .
C14 C13 H13 119.6 . .
C13 C14 C15 120.2(5) . .
C13 C14 H14 119.9 . .
C15 C14 H14 119.9 . .
C18 C15 C16 121.8(5) . .
C18 C15 C14 121.8(5) . .
C16 C15 C14 116.4(5) . .
C17 C16 C15 120.4(5) . .
C17 C16 H16 119.8 . .
C15 C16 H16 119.8 . .
N8 C17 C16 120.5(6) . .
N8 C17 H17 119.7 . .
C16 C17 H17 119.7 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C1 N1 U1 155.1(6) . .
C2 N2 U1 178.2(6) . .
C3 N3 U1 165.5(6) . .
C4 N4 U1 164.2(6) . .
C5 N5 U2 162.8(4) . .
C6 N6 U2 164.5(4) . .
C7 N7 C11 121.0(5) . .
C7 N7 H7A 119.5 . .
C11 N7 H7A 119.5 . .
C13 N8 C17 121.5(5) . .
C13 N8 H8A 119.3 . .
C17 N8 H8A 119.3 . .
O1 U1 O1 180.0(3) 4_565 .
O1 U1 N3 90.01(12) 4_565 .
O1 U1 N3 90.00(13) . .
O1 U1 N4 89.98(12) 4_565 .
O1 U1 N4 89.98(12) . .
N3 U1 N4 74.6(2) . .
O1 U1 N1 90.01(13) 4_565 .
O1 U1 N1 90.01(13) . .
N3 U1 N1 142.9(2) . .
N4 U1 N1 142.5(2) . .
O1 U1 N2 90.02(12) 4_565 .
O1 U1 N2 90.02(12) . .
N3 U1 N2 70.4(2) . .
N4 U1 N2 145.0(2) . .
N1 U1 N2 72.5(2) . .
O1 U1 OW1 89.98(12) 4_565 .
O1 U1 OW1 89.98(12) . .
N3 U1 OW1 145.7(2) . .
N4 U1 OW1 71.1(2) . .
N1 U1 OW1 71.4(2) . .
N2 U1 OW1 143.9(2) . .
O3 U2 O2 178.7(2) . .
O3 U2 N6 89.76(18) . 4_575
O2 U2 N6 91.27(18) . 4_575
O3 U2 N6 89.76(18) . .
O2 U2 N6 91.26(18) . .
N6 U2 N6 71.6(2) 4_575 .
O3 U2 N5 88.84(13) . 4_575
O2 U2 N5 90.74(13) . 4_575
N6 U2 N5 145.07(16) 4_575 4_575
N6 U2 N5 73.48(15) . 4_575
O3 U2 N5 88.84(13) . .
O2 U2 N5 90.74(13) . .
N6 U2 N5 73.48(15) 4_575 .
N6 U2 N5 145.07(15) . .
N5 U2 N5 141.4(2) 4_575 .
O3 U2 OW2 87.9(2) . .
O2 U2 OW2 90.8(2) . .
N6 U2 OW2 144.13(11) 4_575 .
N6 U2 OW2 144.13(11) . .
N5 U2 OW2 70.68(11) 4_575 .
N5 U2 OW2 70.68(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.188(10) .
C1 S1 1.604(9) .
C2 N2 1.160(10) .
C2 S2 1.638(8) .
C3 N3 1.160(10) .
C3 S3 1.622(8) .
C4 N4 1.188(9) .
C4 S4 1.601(8) .
C5 N5 1.167(7) .
C5 S5 1.623(6) .
C6 N6 1.165(7) .
C6 S6 1.635(6) .
C7 N7 1.344(7) .
C7 C8 1.361(8) .
C7 H7 0.9300 .
C8 C9 1.409(8) .
C8 H8 0.9300 .
C9 C12 1.347(7) .
C9 C10 1.417(8) .
C10 C11 1.353(8) .
C10 H10 0.9300 .
C11 N7 1.360(7) .
C11 H11 0.9300 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 N8 1.339(7) .
C13 C14 1.351(8) .
C13 H13 0.9300 .
C14 C15 1.428(8) .
C14 H14 0.9300 .
C15 C18 1.328(7) .
C15 C16 1.411(8) .
C16 C17 1.359(8) .
C16 H16 0.9300 .
C17 N8 1.349(7) .
C17 H17 0.9300 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
N1 U1 2.447(7) .
N2 U1 2.457(6) .
N3 U1 2.419(7) .
N4 U1 2.430(7) .
N5 U2 2.448(5) .
N6 U2 2.445(5) .
N7 H7A 0.8600 .
N8 H8A 0.8600 .
O1 U1 1.765(4) .
O2 U2 1.761(5) .
O3 U2 1.757(5) .
OW1 U1 2.486(6) .
OW2 U2 2.479(5) .
U1 O1 1.765(4) 4_565
U2 N6 2.445(5) 4_575
U2 N5 2.448(5) 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
_geom_hbond_site_symmetry_A
C7 H7 N6 0.93 2.65 3.422(7) 140.4 4_565
C8 H8 S4 0.93 2.94 3.832(6) 162.4 3_656
C10 H10 S6 0.93 2.98 3.799(6) 147.4 2_646
C14 H14 S5 0.93 2.93 3.836(6) 166.4 2_746
C16 H16 N2 0.93 2.64 3.557(7) 168.3 1_556
C17 H17 S6 0.93 3.01 3.631(6) 125.7 1_556
N7 H7A S5 0.86 2.63 3.374(5) 146.2 1_545
N8 H8A S1 0.86 2.78 3.488(5) 141.2 3_666
N8 H8A S6 0.86 2.99 3.601(5) 130.0 1_556
