#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:10:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180469 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/38/7213822.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_7213822
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         708.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.078(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.654(2)
_cell_length_b                   9.0207(14)
_cell_length_c                   17.766(3)
_cell_measurement_reflns_used    6119
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.688
_cell_measurement_theta_min      4.588
_cell_volume                     2346.9(6)
_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 0.938
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12086
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.237
_diffrn_reflns_theta_min         2.294
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.301
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation'
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.895
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0223
_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)+(0.0155P)²+5.9979P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3049
_reflns_number_total             3284
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42106f.txt
_cod_data_source_block           Compound_5
_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        2347.0(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7213822
#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, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.08341(19) 0.9207(3) 0.57519(16) 0.0137(5) Uani 1 1 d . . .
C2 C -0.0683(2) 1.3933(3) 0.83704(16) 0.0146(5) Uani 1 1 d . . .
C3 C 0.7956(2) 0.7919(3) 0.62686(18) 0.0197(6) Uani 1 1 d . . .
H3 H 0.7721 0.8775 0.6480 0.024 Uiso 1 1 calc R U .
C4 C 0.77544(19) 0.6550(3) 0.65652(17) 0.0172(6) Uani 1 1 d . . .
H4 H 0.7385 0.6483 0.6979 0.021 Uiso 1 1 calc R U .
C5 C 0.81036(19) 0.5266(3) 0.62456(16) 0.0144(5) Uani 1 1 d . . .
C6 C 0.8645(2) 0.5430(3) 0.56165(18) 0.0215(6) Uani 1 1 d . . .
H6 H 0.8876 0.4596 0.5383 0.026 Uiso 1 1 calc R U .
C7 C 0.8834(2) 0.6809(4) 0.53444(18) 0.0241(7) Uani 1 1 d . . .
H7 H 0.9199 0.6912 0.4930 0.029 Uiso 1 1 calc R U .
C8 C 0.7923(2) 0.3770(3) 0.65764(18) 0.0212(6) Uani 1 1 d . . .
H8A H 0.7711 0.3107 0.6185 0.032 Uiso 1 1 calc R U .
H8B H 0.7466 0.3856 0.6948 0.032 Uiso 1 1 calc R U .
H8C H 0.8476 0.3388 0.6809 0.032 Uiso 1 1 calc R U .
N1 N 0.06178(17) 0.9590(3) 0.63466(14) 0.0162(5) Uani 1 1 d . . .
N2 N -0.04171(17) 1.2754(3) 0.82154(14) 0.0168(5) Uani 1 1 d . . .
N3 N 0.84913(18) 0.8015(3) 0.56763(15) 0.0200(5) Uani 1 1 d . . .
H3A H 0.8620 0.8876 0.5502 0.024 Uiso 1 1 calc R U .
O1 O -0.11170(13) 1.0554(2) 0.70819(11) 0.0161(4) Uani 1 1 d . . .
OW1 O 0.0000 0.7781(3) 0.7500 0.0226(7) Uani 1 2 d S T P
S1 S 0.11420(6) 0.86563(8) 0.49235(4) 0.01911(15) Uani 1 1 d . . .
S2 S -0.10687(6) 1.55634(8) 0.86052(4) 0.02167(15) Uani 1 1 d . . .
U1 U 0.0000 1.05536(2) 0.7500 0.00992(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 0.0000 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 179.4(3) . .
N2 C2 S2 178.5(3) . .
N3 C3 C4 119.9(3) . .
N3 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C3 C4 C5 120.1(3) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
C4 C5 C6 117.6(3) . .
C4 C5 C8 121.0(3) . .
C6 C5 C8 121.4(3) . .
C7 C6 C5 120.4(3) . .
C7 C6 H6 119.8 . .
C5 C6 H6 119.8 . .
N3 C7 C6 119.9(3) . .
N3 C7 H7 120.1 . .
C6 C7 H7 120.1 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C1 N1 U1 172.4(2) . .
C2 N2 U1 162.2(2) . .
C3 N3 C7 122.2(3) . .
C3 N3 H3A 118.9 . .
C7 N3 H3A 118.9 . .
O1 U1 O1 179.97(13) 2_556 .
O1 U1 N1 89.25(9) 2_556 .
O1 U1 N1 90.76(9) . .
O1 U1 N1 90.76(9) 2_556 2_556
O1 U1 N1 89.25(9) . 2_556
N1 U1 N1 138.08(11) . 2_556
O1 U1 N2 88.46(9) 2_556 2_556
O1 U1 N2 91.51(9) . 2_556
N1 U1 N2 75.21(8) . 2_556
N1 U1 N2 146.70(8) 2_556 2_556
O1 U1 N2 91.51(9) 2_556 .
O1 U1 N2 88.46(9) . .
N1 U1 N2 146.70(8) . .
N1 U1 N2 75.21(8) 2_556 .
N2 U1 N2 71.53(11) 2_556 .
O1 U1 OW1 90.02(6) 2_556 .
O1 U1 OW1 90.02(6) . .
N1 U1 OW1 69.04(6) . .
N1 U1 OW1 69.04(6) 2_556 .
N2 U1 OW1 144.24(6) 2_556 .
N2 U1 OW1 144.23(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.166(4) .
C1 S1 1.632(3) .
C2 N2 1.168(4) .
C2 S2 1.635(3) .
C3 N3 1.338(4) .
C3 C4 1.379(4) .
C3 H3 0.9300 .
C4 C5 1.395(4) .
C4 H4 0.9300 .
C5 C6 1.401(4) .
C5 C8 1.499(4) .
C6 C7 1.366(4) .
C6 H6 0.9300 .
C7 N3 1.343(4) .
C7 H7 0.9300 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
N1 U1 2.431(2) .
N2 U1 2.447(2) .
N3 H3A 0.8600 .
O1 U1 1.773(2) .
OW1 U1 2.501(3) .
U1 O1 1.773(2) 2_556
U1 N1 2.431(2) 2_556
U1 N2 2.447(2) 2_556
