#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:10:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180469 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/38/7213818.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_7213818
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 N1 Br1 1+)2, (U1 O3 C4 H2 N4 S4 2-), (H2 O1)'
_chemical_formula_sum            'C14 H14 Br2 N6 O4 S4 U'
_chemical_formula_weight         857.38
_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                   6.4685(13)
_cell_length_b                   15.007(3)
_cell_length_c                   25.732(5)
_cell_measurement_reflns_used    8479
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.642
_cell_measurement_theta_min      5.429
_cell_volume                     2497.9(9)
_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 0.999
_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  0.0549
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            31174
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.421
_diffrn_reflns_theta_min         2.715
_diffrn_source                   'fine-focused sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.064
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5276
_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    2.267
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1576
_exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation'
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.391
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0243
_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)+(0.0225P)²+6.0525P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2830
_reflns_number_total             3212
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce42106f.txt
_cod_data_source_block           Compound_2
_cod_original_cell_volume        2497.8(8)
_cod_database_code               7213818
#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 0.1534(6) 0.1950(2) 0.11925(14) 0.0163(7) Uani 1 1 d . . .
C2 C 0.2729(5) -0.0690(2) 0.17645(13) 0.0150(7) Uani 1 1 d . . .
C5 C 0.7811(6) 0.9455(3) 0.11350(16) 0.0242(8) Uani 1 1 d . . .
H5 H 0.8186 0.8875 0.1220 0.029 Uiso 1 1 calc R U .
C6 C 0.7766(6) 0.9717(3) 0.06246(16) 0.0254(9) Uani 1 1 d . . .
H6 H 0.8086 0.9318 0.0360 0.030 Uiso 1 1 calc R U .
C7 C 0.7232(6) 1.0587(3) 0.05120(14) 0.0210(8) Uani 1 1 d . . .
C8 C 0.6736(6) 1.1183(3) 0.09088(15) 0.0208(7) Uani 1 1 d . . .
H8 H 0.6375 1.1769 0.0834 0.025 Uiso 1 1 calc R U .
C9 C 0.6793(6) 1.0883(3) 0.14101(15) 0.0204(7) Uani 1 1 d . . .
H9 H 0.6467 1.1268 0.1681 0.024 Uiso 1 1 calc R U .
N1 N 0.1327(5) 0.1826(2) 0.16407(12) 0.0203(7) Uani 1 1 d . . .
N2 N 0.2512(5) 0.0011(2) 0.19408(13) 0.0233(7) Uani 1 1 d . . .
N5 N 0.7315(5) 1.0037(2) 0.15134(12) 0.0201(7) Uani 1 1 d . . .
H5A H 0.7335 0.9861 0.1831 0.024 Uiso 1 1 calc R U .
O1 O -0.0948(5) 0.0870(2) 0.2500 0.0164(7) Uani 1 2 d S T P
O2 O 0.4227(5) 0.1652(2) 0.2500 0.0188(8) Uani 1 2 d S T P
OW1 O -0.0132(6) 0.2789(2) 0.2500 0.0191(8) Uani 1 2 d S T P
OW2 O 0.2942(6) 0.4084(3) 0.2500 0.0238(8) Uani 1 2 d S T P
S1 S 0.17640(18) 0.21257(7) 0.05792(4) 0.0283(2) Uani 1 1 d . . .
S2 S 0.30732(19) -0.16806(7) 0.15214(4) 0.0326(3) Uani 1 1 d . . .
Br1 Br 0.71268(6) 1.09859(3) -0.01801(2) 0.03017(10) Uani 1 1 d . . .
U1 U 0.16381(3) 0.12640(2) 0.2500 0.01124(6) 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'
Br Br -0.2901 2.4595 '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 178.7(4) . .
N2 C2 S2 179.0(4) . .
N5 C5 C6 120.1(4) . .
N5 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C5 C6 C7 118.5(4) . .
C5 C6 H6 120.8 . .
C7 C6 H6 120.8 . .
C6 C7 C8 120.6(4) . .
C6 C7 Br1 120.6(3) . .
C8 C7 Br1 118.8(3) . .
C9 C8 C7 118.3(4) . .
C9 C8 H8 120.9 . .
C7 C8 H8 120.9 . .
N5 C9 C8 120.4(3) . .
N5 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C1 N1 U1 163.7(3) . .
C2 N2 U1 164.7(3) . .
C9 N5 C5 122.1(3) . .
C9 N5 H5A 119.0 . .
C5 N5 H5A 119.0 . .
O2 U1 O1 179.71(16) . .
O2 U1 N1 87.90(9) . .
O1 U1 N1 92.20(9) . .
O2 U1 N1 87.90(9) . 6_556
O1 U1 N1 92.20(9) . 6_556
N1 U1 N1 137.19(15) . 6_556
O2 U1 N2 91.96(12) . .
O1 U1 N2 87.80(12) . .
N1 U1 N2 75.14(11) . .
N1 U1 N2 147.59(11) 6_556 .
O2 U1 N2 91.96(12) . 6_556
O1 U1 N2 87.80(12) . 6_556
N1 U1 N2 147.60(11) . 6_556
N1 U1 N2 75.14(11) 6_556 6_556
N2 U1 N2 72.48(16) . 6_556
O2 U1 OW1 97.40(15) . .
O1 U1 OW1 82.89(14) . .
N1 U1 OW1 69.18(8) . .
N1 U1 OW1 69.18(8) 6_556 .
N2 U1 OW1 142.63(8) . .
N2 U1 OW1 142.63(8) 6_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.176(5) .
C1 S1 1.607(4) .
C2 N2 1.155(4) .
C2 S2 1.628(4) .
C5 N5 1.347(5) .
C5 C6 1.371(6) .
C5 H5 0.9300 .
C6 C7 1.382(6) .
C6 H6 0.9300 .
C7 C8 1.394(5) .
C7 Br1 1.880(4) .
C8 C9 1.367(5) .
C8 H8 0.9300 .
C9 N5 1.339(5) .
C9 H9 0.9300 .
N1 U1 2.375(3) .
N2 U1 2.434(3) .
N5 H5A 0.8600 .
O1 U1 1.775(3) .
O2 U1 1.773(4) .
OW1 U1 2.559(3) .
U1 N1 2.375(3) 6_556
U1 N2 2.434(3) 6_556
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 S2 0.93 2.94 3.575(4) 126.4 7_675
C9 H9 O2 0.93 2.62 3.457(4) 149.9 1_565
N5 H5A O1 0.86 2.55 3.044(4) 117.8 1_665
N5 H5A OW2 0.86 2.09 2.919(4) 162.9 7_665
C8 H8 S2 0.93 2.94 3.575(4) 126.4 7_675
C9 H9 O2 0.93 2.62 3.457(4) 149.9 1_565
N5 H5A O1 0.86 2.55 3.044(4) 117.8 1_665
N5 H5A OW2 0.86 2.09 2.919(4) 162.9 7_665
