#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:19:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180257 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/43/7114324.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_7114324
loop_
_publ_author_name
'Karmazin, Lydia'
'Mazzanti, Marinella'
'Pécaut, Jacques'
_publ_section_title
;
 Unique crown thioether complexes of f elements: the crystal structure of
 U(iii) and La(iii) complexes of 1,4,7-trithiacyclononane
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              654
_journal_paper_doi               10.1039/b200315p
_journal_year                    2002
_chemical_formula_sum            'C10 H18 I3 N2 S3 U'
_chemical_formula_weight         881.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.1070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3393(10)
_cell_length_b                   9.1135(6)
_cell_length_c                   15.1154(10)
_cell_measurement_temperature    193(2)
_cell_volume                     2080.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13056
_diffrn_reflns_theta_full        28.97
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    12.547
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.095
_refine_diff_density_min         -1.640
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.316
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                3470
_reflns_number_total             4996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200315p.txt
_cod_data_source_block           struc_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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_sg_symbol_H-M      P21/c
_cod_database_code               7114324
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U U -0.245356(8) 0.415856(12) -0.114757(8) 0.01874(3) Uani 1 1 d .
I1 I -0.377444(15) 0.60515(2) -0.032097(15) 0.02988(6) Uani 1 1 d .
I2 I -0.256842(16) 0.60929(3) -0.289036(15) 0.03168(6) Uani 1 1 d .
I3 I -0.123931(15) 0.28447(2) 0.057059(14) 0.02955(6) Uani 1 1 d .
S1 S -0.41984(6) 0.34291(10) -0.23680(6) 0.0323(3) Uani 1 1 d .
S2 S -0.23764(6) 0.11275(9) -0.19288(6) 0.0308(2) Uani 1 1 d .
S3 S -0.35836(6) 0.19234(9) -0.03214(5) 0.0248(2) Uani 1 1 d .
N1 N -0.1487(2) 0.6390(3) -0.0484(2) 0.0350(9) Uani 1 1 d .
N2 N -0.0920(2) 0.3844(3) -0.1697(2) 0.0405(10) Uani 1 1 d .
C1 C -0.4038(3) 0.1787(5) -0.3004(2) 0.0436(13) Uani 1 1 d .
H1A H -0.444(3) 0.088(5) -0.272(3) 0.087(16) Uiso 1 1 d .
H1B H -0.429(2) 0.187(3) -0.354(2) 0.035(10) Uiso 1 1 d .
C2 C -0.3088(3) 0.1381(5) -0.3021(2) 0.0490(13) Uani 1 1 d .
H2A H -0.280(2) 0.236(3) -0.324(2) 0.033(9) Uiso 1 1 d .
H2B H -0.302(3) 0.035(5) -0.324(3) 0.069(13) Uiso 1 1 d .
C3 C -0.2956(3) -0.0226(4) -0.1372(3) 0.0362(11) Uani 1 1 d .
H3A H -0.352(2) -0.038(3) -0.1718(18) 0.019(8) Uiso 1 1 d .
H3B H -0.2661(17) -0.104(3) -0.1312(16) 0.000(6) Uiso 1 1 d .
C4 C -0.3073(3) 0.0167(4) -0.0445(2) 0.0362(11) Uani 1 1 d .
H4A H -0.252(2) 0.027(4) -0.012(2) 0.034(10) Uiso 1 1 d .
H4B H -0.3289(19) -0.069(3) -0.0095(17) 0.013(8) Uiso 1 1 d .
C5 C -0.4663(2) 0.1625(4) -0.0993(2) 0.0335(10) Uani 1 1 d .
H5A H -0.479(3) 0.064(4) -0.132(3) 0.064(13) Uiso 1 1 d .
H5B H -0.4905(18) 0.175(3) -0.0610(17) 0.010(8) Uiso 1 1 d .
C6 C -0.4969(2) 0.2810(4) -0.1662(3) 0.0406(12) Uani 1 1 d .
H6A H -0.507(3) 0.376(4) -0.137(2) 0.051(12) Uiso 1 1 d .
H6B H -0.5427(18) 0.239(3) -0.2060(17) 0.014(8) Uiso 1 1 d .
C11 C -0.1174(2) 0.7337(4) -0.0095(2) 0.0323(10) Uani 1 1 d .
C12 C -0.0748(3) 0.8573(4) 0.0429(2) 0.0389(12) Uani 1 1 d .
H12A H -0.0117 0.8363 0.0621 0.039(10) Uiso 1 1 calc R
H12B H -0.1025 0.8723 0.0960 0.12(2) Uiso 1 1 calc R
H12C H -0.0818 0.9462 0.0059 0.011(7) Uiso 1 1 calc R
C13 C -0.0311(2) 0.3914(4) -0.2017(2) 0.0334(11) Uani 1 1 d .
C14 C 0.0483(2) 0.4009(5) -0.2426(2) 0.0439(12) Uani 1 1 d .
H14A H 0.0345 0.3668 -0.3050 0.075(14) Uiso 1 1 calc R
H14B H 0.0950 0.3393 -0.2089 0.13(2) Uiso 1 1 calc R
H14C H 0.0685 0.5030 -0.2414 0.117(19) Uiso 1 1 calc R
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'
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 U N2 74.24(10)
N1 U S2 143.64(7)
N2 U S2 71.30(7)
N1 U S1 141.47(7)
N2 U S1 121.46(7)
S2 U S1 69.72(2)
N1 U S3 132.98(7)
N2 U S3 130.62(7)
S2 U S3 67.43(2)
S1 U S3 66.65(2)
N1 U I1 77.18(7)
N2 U I1 150.57(7)
S2 U I1 138.092(19)
S1 U I1 78.328(19)
S3 U I1 75.479(17)
N1 U I2 80.23(7)
N2 U I2 73.76(7)
S2 U I2 100.693(19)
S1 U I2 72.618(18)
S3 U I2 139.211(16)
I1 U I2 94.670(8)
N1 U I3 76.44(6)
N2 U I3 77.76(7)
S2 U I3 85.215(17)
S1 U I3 138.161(18)
S3 U I3 73.020(16)
I1 U I3 102.331(8)
I2 U I3 147.094(8)
C6 S1 C1 102.58(18)
C6 S1 U 107.78(12)
C1 S1 U 108.28(13)
C3 S2 C2 103.97(19)
C3 S2 U 112.69(12)
C2 S2 U 100.34(14)
C5 S3 C4 100.41(17)
C5 S3 U 113.46(12)
C4 S3 U 105.01(13)
C11 N1 U 167.6(3)
C13 N2 U 168.3(3)
C2 C1 S1 115.6(3)
C1 C2 S2 116.2(3)
C4 C3 S2 115.1(2)
C3 C4 S3 115.9(2)
C6 C5 S3 114.8(3)
C5 C6 S1 117.5(3)
N1 C11 C12 179.0(4)
N2 C13 C14 179.6(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
U N1 2.611(3)
U N2 2.644(3)
U S2 3.0146(9)
U S1 3.0456(9)
U S3 3.0779(9)
U I1 3.0872(3)
U I2 3.1488(3)
U I3 3.1543(3)
S1 C6 1.817(4)
S1 C1 1.819(4)
S2 C3 1.812(4)
S2 C2 1.827(4)
S3 C5 1.804(3)
S3 C4 1.806(4)
N1 C11 1.105(4)
N2 C13 1.127(5)
C1 C2 1.507(6)
C3 C4 1.488(5)
C5 C6 1.498(5)
C11 C12 1.464(5)
C13 C14 1.461(6)
