#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:10:59 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180469 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/38/7213825.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_7213825
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         '(C7 H11 N2 1+)2, (U O3 C4 H2 N4 S4 2-)'
_chemical_formula_sum            'C18 H24 N8 O3 S4 U'
_chemical_formula_weight         766.72
_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                 98.3050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3879(15)
_cell_length_b                   8.6863(10)
_cell_length_c                   23.486(3)
_cell_measurement_reflns_used    3807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.667
_cell_measurement_theta_min      5.608
_cell_volume                     2702.6(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 0.936
_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  0.0205
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14446
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.334
_diffrn_reflns_theta_min         1.753
_diffrn_source                   'fine-focused sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.350
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1464
_exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation'
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.714
_refine_diff_density_min         -1.508
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0151
_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)+(0.0084P)²+4.5197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0345
_refine_ls_wR_factor_ref         0.0347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3756
_reflns_number_total             3807
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42106f.txt
_cod_data_source_block           Compound_8
_cod_original_cell_volume        2702.6(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7213825
#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 0.59414(13) 0.45871(19) 0.38868(8) 0.0135(3) Uani 1 1 d . . .
C2 C 0.41103(13) -0.0071(2) 0.17340(7) 0.0158(3) Uani 1 1 d . . .
C3 C 0.63295(16) -0.1886(2) 0.55468(9) 0.0225(4) Uani 1 1 d . . .
H3 H 0.6316 -0.2946 0.5601 0.027 Uiso 1 1 calc R U .
C4 C 0.64323(15) -0.0940(2) 0.60149(8) 0.0191(4) Uani 1 1 d . . .
H4 H 0.6482 -0.1353 0.6383 0.023 Uiso 1 1 calc R U .
C5 C 0.64628(13) 0.0688(2) 0.59365(8) 0.0155(3) Uani 1 1 d . . .
C6 C 0.63364(14) 0.1225(2) 0.53581(8) 0.0191(4) Uani 1 1 d . . .
H6 H 0.6321 0.2278 0.5284 0.023 Uiso 1 1 calc R U .
C7 C 0.62385(15) 0.0214(2) 0.49144(8) 0.0224(4) Uani 1 1 d . . .
H7 H 0.6164 0.0585 0.4539 0.027 Uiso 1 1 calc R U .
C8 C 0.67583(16) 0.1067(3) 0.69730(9) 0.0285(5) Uani 1 1 d . . .
H8A H 0.6926 0.1905 0.7236 0.043 Uiso 1 1 calc R U .
H8B H 0.7300 0.0334 0.7016 0.043 Uiso 1 1 calc R U .
H8C H 0.6152 0.0578 0.7054 0.043 Uiso 1 1 calc R U .
C9 C 0.66288(19) 0.3319(3) 0.62931(12) 0.0330(5) Uani 1 1 d . . .
H9A H 0.6718 0.3835 0.6658 0.049 Uiso 1 1 calc R U .
H9B H 0.6006 0.3646 0.6071 0.049 Uiso 1 1 calc R U .
H9C H 0.7180 0.3570 0.6090 0.049 Uiso 1 1 calc R U .
N1 N 0.59219(12) 0.43326(18) 0.33982(7) 0.0172(3) Uani 1 1 d . . .
N2 N 0.43685(13) 0.11114(19) 0.19394(7) 0.0213(3) Uani 1 1 d . . .
N3 N 0.62462(13) -0.1319(2) 0.50058(7) 0.0218(3) Uani 1 1 d . . .
H3A H 0.6198 -0.1940 0.4718 0.026 Uiso 1 1 calc R U .
N4 N 0.66019(12) 0.1653(2) 0.63840(7) 0.0209(3) Uani 1 1 d . . .
O1 O 0.61064(10) 0.33494(16) 0.21682(6) 0.0191(3) Uani 1 1 d . . .
OW1 O 0.5000 0.6216(2) 0.2500 0.0255(4) Uani 1 2 d S T P
S1 S 0.59470(4) 0.49528(6) 0.45655(2) 0.02296(10) Uani 1 1 d . . .
S2 S 0.37640(4) -0.17429(5) 0.14580(2) 0.01942(9) Uani 1 1 d . . .
U1 U 0.5000 0.33647(2) 0.2500 0.01077(3) 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 178.94(17) . .
N2 C2 S2 178.78(18) . .
N3 C3 C4 121.56(18) . .
N3 C3 H3 119.2 . .
C4 C3 H3 119.2 . .
C3 C4 C5 119.63(18) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
N4 C5 C6 121.94(18) . .
N4 C5 C4 121.55(18) . .
C6 C5 C4 116.50(17) . .
C7 C6 C5 120.46(18) . .
C7 C6 H6 119.8 . .
C5 C6 H6 119.8 . .
N3 C7 C6 121.33(18) . .
N3 C7 H7 119.3 . .
C6 C7 H7 119.3 . .
N4 C8 H8A 109.5 . .
N4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N4 C9 H9A 109.5 . .
N4 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N4 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C1 N1 U1 148.78(14) . .
C2 N2 U1 171.36(15) . .
C7 N3 C3 120.45(17) . .
C7 N3 H3A 119.8 . .
C3 N3 H3A 119.8 . .
C5 N4 C8 120.74(18) . .
C5 N4 C9 120.59(18) . .
C8 N4 C9 118.65(18) . .
O1 U1 O1 179.14(9) 2_655 .
O1 U1 N1 91.85(6) 2_655 2_655
O1 U1 N1 88.45(6) . 2_655
O1 U1 N1 88.45(6) 2_655 .
O1 U1 N1 91.85(6) . .
N1 U1 N1 139.60(7) 2_655 .
O1 U1 N2 90.18(6) 2_655 2_655
O1 U1 N2 89.13(6) . 2_655
N1 U1 N2 146.82(5) 2_655 2_655
N1 U1 N2 73.55(5) . 2_655
O1 U1 N2 89.13(6) 2_655 .
O1 U1 N2 90.18(6) . .
N1 U1 N2 73.55(5) 2_655 .
N1 U1 N2 146.83(5) . .
N2 U1 N2 73.38(8) 2_655 .
O1 U1 OW1 90.43(4) 2_655 .
O1 U1 OW1 90.43(4) . .
N1 U1 OW1 69.80(4) 2_655 .
N1 U1 OW1 69.80(4) . .
N2 U1 OW1 143.31(4) 2_655 .
N2 U1 OW1 143.31(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.165(2) .
C1 S1 1.6242(18) .
C2 N2 1.165(2) .
C2 S2 1.6305(19) .
C3 N3 1.352(3) .
C3 C4 1.363(3) .
C3 H3 0.9300 .
C4 C5 1.428(3) .
C4 H4 0.9300 .
C5 N4 1.336(2) .
C5 C6 1.423(3) .
C6 C7 1.355(3) .
C6 H6 0.9300 .
C7 N3 1.349(3) .
C7 H7 0.9300 .
C8 N4 1.461(3) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 N4 1.464(3) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
N1 U1 2.4348(16) .
N2 U1 2.4409(16) .
N3 H3A 0.8600 .
O1 U1 1.7707(13) .
OW1 U1 2.476(2) .
U1 O1 1.7706(13) 2_655
U1 N1 2.4348(16) 2_655
U1 N2 2.4408(16) 2_655
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
C3 H3 S1 0.93 3.02 3.574(2) 119.5 1_545
C4 H4 O1 0.93 2.63 3.500(2) 155.6 6_556
C6 H6 S1 0.93 2.87 3.734(2) 154.4 .
C8 H8B N1 0.96 2.71 3.363(3) 125.5 7_656
N3 H3A S1 0.86 2.74 3.4056(18) 135.7 1_545
N3 H3A S2 0.86 2.78 3.4556(18) 137.2 2_655
