#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:10:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180469 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/38/7213820.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_7213820
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 H5 I N 1+)2,(U O3 C4 H2 N4 S4 2-),(H2 O)'
_chemical_formula_sum            'C14 H14 I2 N6 O4 S4 U'
_chemical_formula_weight         950.45
_chemical_properties_physical    thermochromic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      57
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7452(4)
_cell_length_b                   15.1032(8)
_cell_length_c                   25.9377(14)
_cell_measurement_reflns_used    3790
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      44.268
_cell_measurement_theta_min      5.394
_cell_volume                     2642.4(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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_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  0.0612
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26739
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.323
_diffrn_reflns_theta_min         2.697
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.826
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5821
_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    2.379
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1720
_exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation'
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.043
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0358
_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)+(0.0252P)²+4.5113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2658
_reflns_number_total             3910
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42106f.txt
_cod_data_source_block           Compound_3RT
_cod_database_code               7213820
#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, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -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 0.6572(8) 0.3061(4) 0.8790(2) 0.0478(13) Uani 1 1 d . . .
C2 C 0.7643(8) 0.5683(4) 0.8223(2) 0.0466(13) Uani 1 1 d . . .
C3 C 0.1748(9) 0.4100(5) 0.8575(2) 0.0618(16) Uani 1 1 d . . .
H3 H 0.1413 0.3716 0.8309 0.074 Uiso 1 1 calc R U .
C4 C 0.1741(9) 0.3811(4) 0.9070(2) 0.0570(14) Uani 1 1 d . . .
H4 H 0.1408 0.3228 0.9146 0.068 Uiso 1 1 calc R U .
C5 C 0.2230(8) 0.4389(4) 0.9457(2) 0.0530(14) Uani 1 1 d . . .
C6 C 0.2711(9) 0.5247(4) 0.9339(3) 0.0655(17) Uani 1 1 d . . .
H6 H 0.3027 0.5646 0.9600 0.079 Uiso 1 1 calc R U .
C7 C 0.2720(10) 0.5511(5) 0.8837(3) 0.0681(18) Uani 1 1 d . . .
H7 H 0.3063 0.6089 0.8751 0.082 Uiso 1 1 calc R U .
N1 N 0.6335(8) 0.3188(3) 0.83534(17) 0.0613(13) Uani 1 1 d . . .
N2 N 0.7454(8) 0.4992(3) 0.8051(2) 0.0680(14) Uani 1 1 d . . .
N3 N 0.2235(7) 0.4936(4) 0.8471(2) 0.0617(13) Uani 1 1 d . . .
H3A H 0.2235 0.5110 0.8156 0.074 Uiso 1 1 calc R U .
O1 O 0.4149(8) 0.4111(3) 0.7500 0.0520(13) Uani 1 2 d S T P
O2 O 0.9098(8) 0.3383(4) 0.7500 0.0588(14) Uani 1 2 d S T P
OW1 O 0.5026(8) 0.2201(3) 0.7500 0.0536(14) Uani 1 2 d S T P
OW2 O 0.8064(9) 0.0914(4) 0.7500 0.0676(16) Uani 1 2 d S T P
S1 S 0.6837(3) 0.28651(14) 0.93915(6) 0.0797(5) Uani 1 1 d . . .
S2 S 0.7942(4) 0.66619(11) 0.84522(7) 0.0893(7) Uani 1 1 d . . .
I1 I 0.21818(7) 0.39716(3) 1.02238(2) 0.07331(15) Uani 1 1 d . . .
U1 U 0.66311(4) 0.37449(2) 0.7500 0.03907(9) 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'
I I -0.4742 1.8119 '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 178.1(6) . .
N2 C2 S2 178.5(6) . .
N3 C3 C4 119.8(6) . .
N3 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C3 C4 C5 119.2(6) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C4 C5 C6 119.8(6) . .
C4 C5 I1 120.1(5) . .
C6 C5 I1 120.1(4) . .
C7 C6 C5 119.3(6) . .
C7 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
N3 C7 C6 119.4(6) . .
N3 C7 H7 120.3 . .
C6 C7 H7 120.3 . .
C1 N1 U1 163.0(5) . .
C2 N2 U1 164.6(5) . .
C7 N3 C3 122.5(6) . .
C7 N3 H3A 118.8 . .
C3 N3 H3A 118.8 . .
O2 U1 O1 179.9(2) . .
O2 U1 N1 88.24(14) . .
O1 U1 N1 91.78(14) . .
O2 U1 N1 88.24(14) . 6_557
O1 U1 N1 91.78(14) . 6_557
N1 U1 N1 137.3(2) . 6_557
O2 U1 N2 91.4(2) . 6_557
O1 U1 N2 88.52(19) . 6_557
N1 U1 N2 147.34(18) . 6_557
N1 U1 N2 75.26(17) 6_557 6_557
O2 U1 N2 91.4(2) . .
O1 U1 N2 88.52(19) . .
N1 U1 N2 75.25(17) . .
N1 U1 N2 147.35(18) 6_557 .
N2 U1 N2 72.1(3) 6_557 .
O2 U1 OW1 96.7(2) . .
O1 U1 OW1 83.3(2) . .
N1 U1 OW1 69.12(12) . .
N1 U1 OW1 69.12(12) 6_557 .
N2 U1 OW1 143.09(13) 6_557 .
N2 U1 OW1 143.09(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.159(6) .
C1 S1 1.599(6) .
C2 N2 1.141(6) .
C2 S2 1.607(6) .
C3 N3 1.332(8) .
C3 C4 1.355(8) .
C3 H3 0.9300 .
C4 C5 1.370(8) .
C4 H4 0.9300 .
C5 C6 1.371(8) .
C5 I1 2.087(6) .
C6 C7 1.363(9) .
C6 H6 0.9300 .
C7 N3 1.327(8) .
C7 H7 0.9300 .
N1 U1 2.376(5) .
N2 U1 2.430(5) .
N3 H3A 0.8600 .
O1 U1 1.763(5) .
O2 U1 1.751(5) .
OW1 U1 2.570(5) .
U1 N1 2.376(5) 6_557
U1 N2 2.430(5) 6_557
