#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:10:59 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180469 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/38/7213821.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_7213821
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 H5 N2 S1 1+)2, (U O3 C4 H2 N4 S4 2-), 4(H2 O)'
_chemical_formula_sum            'C16 H20 N8 O7 S6 U'
_chemical_formula_weight         866.81
_chemical_properties_physical    thermochromic
_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                 102.363(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.407(3)
_cell_length_b                   8.8724(17)
_cell_length_c                   24.900(5)
_cell_measurement_reflns_used    6848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.896
_cell_measurement_theta_min      5.546
_cell_volume                     2893.2(10)
_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 0.926
_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  0.0707
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15491
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.430
_diffrn_reflns_theta_min         1.674
_diffrn_source                   'fine-focused sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.093
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            'Orange (293(2)K) Yellow (100(2)K)'
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.160
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0295P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3882
_reflns_number_total             4076
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42106f.txt
_cod_data_source_block           Compound_4
_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        2893.1(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7213821
#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 0.4037(3) 0.1815(4) 0.11145(14) 0.0144(7) Uani 1 1 d . . .
C2 C 0.4364(3) -0.2521(4) 0.15680(14) 0.0146(7) Uani 1 1 d . . .
C8 C 0.6536(3) 0.5379(4) 0.07266(16) 0.0187(8) Uani 1 1 d . . .
H8 H 0.6515 0.6325 0.0564 0.022 Uiso 1 1 calc R U .
C7 C 0.6394(3) 0.4103(4) 0.04033(16) 0.0204(8) Uani 1 1 d . . .
H7 H 0.6271 0.4177 0.0022 0.024 Uiso 1 1 calc R U .
C6 C 0.6438(3) 0.2694(4) 0.06601(14) 0.0113(6) Uani 1 1 d . . .
C5 C 0.6603(3) 0.2615(4) 0.12280(14) 0.0145(7) Uani 1 1 d . . .
H5 H 0.6628 0.1688 0.1405 0.017 Uiso 1 1 calc R U .
C4 C 0.6731(3) 0.3937(4) 0.15255(15) 0.0164(7) Uani 1 1 d . . .
H4 H 0.6837 0.3905 0.1907 0.020 Uiso 1 1 calc R U .
C3 C 0.6355(3) -0.0261(4) 0.06873(15) 0.0158(7) Uani 1 1 d . . .
N1 N 0.4259(3) 0.1480(4) 0.15760(13) 0.0224(7) Uani 1 1 d . . .
N2 N 0.4588(2) -0.1622(3) 0.19212(12) 0.0175(6) Uani 1 1 d . . .
N4 N 0.6704(2) 0.5260(4) 0.12710(13) 0.0149(6) Uani 1 1 d . . .
H4A H 0.6799 0.6068 0.1466 0.018 Uiso 1 1 calc R U .
N3 N 0.6396(3) -0.1187(4) 0.10112(14) 0.0219(7) Uani 1 1 d . . .
O1 O 0.6236(2) 0.0625(3) 0.23526(12) 0.0160(5) Uani 1 1 d . . .
OW1 O 0.5000 0.3340(4) 0.2500 0.0241(9) Uani 1 2 d S T P
S1 S 0.36805(8) 0.22702(11) 0.04706(4) 0.0206(2) Uani 1 1 d . . .
S2 S 0.40734(7) -0.38318(11) 0.11048(4) 0.01862(19) Uani 1 1 d . . .
S3 S 0.62962(7) 0.11247(10) 0.02148(3) 0.01559(18) Uani 1 1 d . . .
U1 U 0.5000 0.06292(2) 0.2500 0.00872(6) Uani 1 2 d S T P
OW2 O 0.68623(19) 0.7215(3) 0.21744(10) 0.0149(5) Uani 1 1 d . . .
OW3 O 0.3215(2) -0.5323(3) 0.20876(11) 0.0163(5) Uani 1 1 d . . .
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 177.8(3) . .
N2 C2 S2 177.0(3) . .
N4 C8 C7 120.1(3) . .
N4 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C8 C7 C6 118.7(3) . .
C8 C7 H7 120.7 . .
C6 C7 H7 120.7 . .
C5 C6 C7 119.6(3) . .
C5 C6 S3 125.0(3) . .
C7 C6 S3 115.4(3) . .
C4 C5 C6 118.7(3) . .
C4 C5 H5 120.7 . .
C6 C5 H5 120.7 . .
N4 C4 C5 120.5(3) . .
N4 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
N3 C3 S3 179.3(4) . .
C1 N1 U1 169.9(3) . .
C2 N2 U1 168.1(3) . .
C8 N4 C4 122.5(3) . .
C8 N4 H4A 118.8 . .
C4 N4 H4A 118.8 . .
C3 S3 C6 98.83(16) . .
O1 U1 O1 179.76(14) 2_655 .
O1 U1 OW1 90.12(7) 2_655 .
O1 U1 OW1 90.12(7) . .
O1 U1 N1 90.89(12) 2_655 2_655
O1 U1 N1 89.19(12) . 2_655
OW1 U1 N1 71.86(8) . 2_655
O1 U1 N1 89.18(12) 2_655 .
O1 U1 N1 90.89(12) . .
OW1 U1 N1 71.86(8) . .
N1 U1 N1 143.71(17) 2_655 .
O1 U1 N2 90.99(11) 2_655 .
O1 U1 N2 88.81(11) . .
OW1 U1 N2 144.43(7) . .
N1 U1 N2 143.66(11) 2_655 .
N1 U1 N2 72.61(11) . .
O1 U1 N2 88.81(11) 2_655 2_655
O1 U1 N2 90.99(11) . 2_655
OW1 U1 N2 144.42(7) . 2_655
N1 U1 N2 72.61(11) 2_655 2_655
N1 U1 N2 143.66(11) . 2_655
N2 U1 N2 71.15(15) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.162(5) .
C1 S1 1.623(4) .
C2 N2 1.178(5) .
C2 S2 1.625(4) .
C8 N4 1.330(5) .
C8 C7 1.378(5) .
C8 H8 0.9300 .
C7 C6 1.400(5) .
C7 H7 0.9300 .
C6 C5 1.385(5) .
C6 S3 1.764(3) .
C5 C4 1.379(5) .
C5 H5 0.9300 .
C4 N4 1.330(5) .
C4 H4 0.9300 .
C3 N3 1.144(5) .
C3 S3 1.692(4) .
N1 U1 2.423(3) .
N2 U1 2.456(3) .
N4 H4A 0.8600 .
O1 U1 1.772(3) .
OW1 U1 2.405(4) .
U1 O1 1.772(3) 2_655
U1 N1 2.423(3) 2_655
U1 N2 2.456(3) 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
C8 H8 S1 0.93 2.82 3.599(4) 141.7 5_665
C7 H7 S2 0.93 2.76 3.680(4) 169.6 5_655
