#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:10:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180469 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/38/7213819.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_7213819
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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.068(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6151(18)
_cell_length_b                   14.993(4)
_cell_length_c                   25.896(7)
_cell_measurement_reflns_used    7627
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      57.987
_cell_measurement_theta_min      5.434
_cell_volume                     2567.9(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.940
_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  0.0642
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            36812
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.404
_diffrn_reflns_theta_min         1.570
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.082
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5827
_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    2.448
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation'
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.062
_refine_diff_density_max         5.291
_refine_diff_density_min         -3.046
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0570
_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)+115.1768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5970
_reflns_number_total             7328
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42106f.txt
_cod_data_source_block           Compound_3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7213819
#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+1/2'
'-x, -y, -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
C1 C 0.6522(16) 0.8051(7) 0.8864(4) 0.016(2) Uani 1 1 d . .
C2 C 0.7825(17) 1.0709(8) 0.8234(4) 0.017(2) Uani 1 1 d . .
C3 C 0.7582(16) 1.0628(7) 0.6770(4) 0.0141(19) Uani 1 1 d . .
C4 C 0.6512(15) 0.8013(7) 0.6263(4) 0.0131(19) Uani 1 1 d . .
C5 C 0.2965(17) 1.0419(8) -0.1074(4) 0.019(2) Uani 1 1 d . .
H5 H 0.3427 1.0991 -0.1146 0.023 Uiso 1 1 calc R U
C6 C 0.2842(17) 1.0137(8) -0.0572(4) 0.020(2) Uani 1 1 d . .
H6 H 0.3207 1.0517 -0.0302 0.024 Uiso 1 1 calc R U
C7 C 0.2169(15) 0.9281(8) -0.0470(4) 0.017(2) Uani 1 1 d . .
C8 C 0.1660(15) 0.8728(7) -0.0881(4) 0.016(2) Uani 1 1 d . .
H8 H 0.1245 0.8145 -0.0820 0.019 Uiso 1 1 calc R U
C9 C 0.1770(16) 0.9042(8) -0.1380(4) 0.020(2) Uani 1 1 d . .
H9 H 0.1395 0.8679 -0.1657 0.023 Uiso 1 1 calc R U
C10 C 0.2572(17) 0.4376(8) 1.1254(4) 0.020(2) Uani 1 1 d . .
H10 H 0.2805 0.3787 1.1352 0.024 Uiso 1 1 calc R U
C11 C 0.2659(17) 0.4626(7) 1.0739(4) 0.019(2) Uani 1 1 d . .
H11 H 0.2963 0.4211 1.0485 0.023 Uiso 1 1 calc R U
C12 C 0.2278(15) 0.5516(8) 1.0611(4) 0.016(2) Uani 1 1 d . .
C13 C 0.1820(18) 0.6116(8) 1.0988(4) 0.022(2) Uani 1 1 d . .
H13 H 0.1553 0.6708 1.0902 0.027 Uiso 1 1 calc R U
C14 C 0.1755(17) 0.5846(8) 1.1490(4) 0.018(2) Uani 1 1 d . .
H14 H 0.1438 0.6252 1.1748 0.022 Uiso 1 1 calc R U
N1 N 0.6332(15) 0.8158(7) 0.8415(4) 0.0188(19) Uani 1 1 d . .
N2 N 0.7480(15) 0.9973(6) 0.8110(4) 0.0191(19) Uani 1 1 d . .
N3 N 0.7453(15) 0.9963(7) 0.6998(4) 0.022(2) Uani 1 1 d . .
N4 N 0.6215(15) 0.8143(7) 0.6706(4) 0.0192(19) Uani 1 1 d . .
N5 N 0.2418(14) 0.9870(7) -0.1462(4) 0.0183(19) Uani 1 1 d . .
H5A H 0.2488 1.0060 -0.1774 0.022 Uiso 1 1 calc R U
N6 N 0.2148(14) 0.4996(7) 1.1609(4) 0.0189(19) Uani 1 1 d . .
H6A H 0.2128 0.4839 1.1929 0.023 Uiso 1 1 calc R U
O1 O 0.4064(11) 0.9110(5) 0.7557(3) 0.0143(14) Uani 1 1 d . .
O2 O 0.9119(12) 0.8340(6) 0.7556(3) 0.0215(17) Uani 1 1 d . .
OW1 O 0.4862(11) 0.7181(5) 0.7548(3) 0.0144(14) Uani 1 1 d . .
OW2 O 0.7902(12) 0.5919(5) 0.7402(3) 0.0177(15) Uani 1 1 d . .
S1 S 0.6745(5) 0.7891(2) 0.94747(10) 0.0230(6) Uani 1 1 d . .
S2 S 0.8399(5) 1.17301(19) 0.83880(11) 0.0223(6) Uani 1 1 d . .
S3 S 0.7736(5) 1.1577(2) 0.64634(11) 0.0233(6) Uani 1 1 d . .
S4 S 0.6895(5) 0.7846(2) 0.56605(11) 0.0262(6) Uani 1 1 d . .
I1 I 0.19684(11) 0.88243(5) 0.02845(3) 0.01939(16) Uani 1 1 d . .
I2 I 0.23389(11) 0.58964(5) 0.98357(3) 0.01983(16) Uani 1 1 d . .
U1 U 0.65864(6) 0.87120(2) 0.75542(2) 0.01003(9) 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'
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
N1 C1 S1 178.8(11)
N2 C2 S2 177.2(11)
N3 C3 S3 178.3(10)
N4 C4 S4 179.3(11)
N5 C5 C6 120.0(11)
N5 C5 H5 120.0
C6 C5 H5 120.0
C5 C6 C7 119.4(10)
C5 C6 H6 120.3
C7 C6 H6 120.3
C6 C7 C8 118.8(10)
C6 C7 I1 120.7(8)
C8 C7 I1 120.4(9)
C9 C8 C7 119.9(11)
C9 C8 H8 120.0
C7 C8 H8 120.0
N5 C9 C8 119.4(11)
N5 C9 H9 120.3
C8 C9 H9 120.3
N6 C10 C11 119.0(11)
N6 C10 H10 120.5
C11 C10 H10 120.5
C10 C11 C12 118.4(10)
C10 C11 H11 120.8
C12 C11 H11 120.8
C13 C12 C11 120.1(11)
C13 C12 I2 121.0(9)
C11 C12 I2 118.8(8)
C14 C13 C12 119.8(12)
C14 C13 H13 120.1
C12 C13 H13 120.1
N6 C14 C13 119.6(11)
N6 C14 H14 120.2
C13 C14 H14 120.2
C1 N1 U1 163.8(9)
C2 N2 U1 159.3(9)
C3 N3 U1 168.4(9)
C4 N4 U1 160.6(8)
C9 N5 C5 122.4(10)
C9 N5 H5A 118.8
C5 N5 H5A 118.8
C14 N6 C10 123.1(10)
C14 N6 H6A 118.5
C10 N6 H6A 118.5
O2 U1 O1 178.7(4)
O2 U1 N4 88.4(3)
O1 U1 N4 92.5(3)
O2 U1 N1 88.3(3)
O1 U1 N1 91.8(3)
N4 U1 N1 137.2(3)
O2 U1 N3 90.7(4)
O1 U1 N3 88.6(3)
N4 U1 N3 75.6(3)
N1 U1 N3 147.1(3)
O2 U1 N2 91.3(4)
O1 U1 N2 87.4(3)
N4 U1 N2 147.8(3)
N1 U1 N2 74.9(3)
N3 U1 N2 72.3(3)
O2 U1 OW1 98.0(3)
O1 U1 OW1 83.3(3)
N4 U1 OW1 68.5(3)
N1 U1 OW1 69.8(3)
N3 U1 OW1 142.6(3)
N2 U1 OW1 143.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.178(14)
C1 S1 1.603(11)
C2 N2 1.170(15)
C2 S2 1.625(12)
C3 N3 1.163(14)
C3 S3 1.633(11)
C4 N4 1.184(14)
C4 S4 1.604(11)
C5 N5 1.343(15)
C5 C6 1.371(16)
C5 H5 0.9300
C6 C7 1.385(16)
C6 H6 0.9300
C7 C8 1.386(15)
C7 I1 2.077(10)
C8 C9 1.378(15)
C8 H8 0.9300
C9 N5 1.332(15)
C9 H9 0.9300
C10 N6 1.341(15)
C10 C11 1.388(16)
C10 H10 0.9300
C11 C12 1.397(16)
C11 H11 0.9300
C12 C13 1.365(16)
C12 I2 2.089(11)
C13 C14 1.363(16)
C13 H13 0.9300
C14 N6 1.336(15)
C14 H14 0.9300
N1 U1 2.388(9)
N2 U1 2.442(10)
N3 U1 2.440(10)
N4 U1 2.365(9)
N5 H5A 0.8600
N6 H6A 0.8600
O1 U1 1.773(7)
O2 U1 1.765(8)
OW1 U1 2.564(7)
