#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/42/4114204.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_4114204
loop_
_publ_author_name
'Margaret-Jane Crawford'
'Arkady Ellern'
'Heinrich Nöth'
'Max Suter'
_publ_contact_author
;
       Heinrich Nöth
       Institut für anorganische Chemie
       Universität München
       Butenandtstr. 5-13 (Haus D)
       81377 München
       Bundesrepublik Deutschland
;
_publ_contact_author_email       H.Noeth@lrz.uni-muenchen.de
_publ_contact_author_fax         '089 2180 7865'
_publ_contact_author_phone       '089 2180 7454'
_publ_section_title
;
 Synthesis and Structure of UO2I2(OH2)2.4Et2O: First Structurally
 Characterized U(VI)-I Bond and Lightest Missing Member of the UO2X2 (X =
 Halide) Series
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11778
_journal_page_last               11779
_journal_paper_doi               10.1021/ja030260r
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C8 H22 I2 O6 U'
_chemical_formula_weight         583.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-CIF-file updated by CIFRTF'
_cell_angle_alpha                68.412(2)
_cell_angle_beta                 67.056(2)
_cell_angle_gamma                75.297(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8306(11)
_cell_length_b                   9.2307(11)
_cell_length_c                   10.8926(14)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      1.00
_cell_measurement_theta_min      20.00
_cell_volume                     753.94(16)
_computing_cell_refinement       'SMART (V4.C50)'
_computing_data_collection       'SMART (V4.C50)'
_computing_data_reduction        'SAINT (V4.D50)'
_computing_molecular_graphics    'XP (SHELXTL-Ver.5)'
_computing_publication_material  'SHELXL (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Siemens SMART Area-detector'
_diffrn_measurement_method       Hemisphere
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2964
_diffrn_reflns_theta_full        21.72
_diffrn_reflns_theta_max         21.72
_diffrn_reflns_theta_min         2.13
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    12.815
_exptl_absorpt_correction_T_max  0.368678
_exptl_absorpt_correction_T_min  0.200711
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.569
_exptl_crystal_description       plates
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         1521
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          2.459
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0579P)²+1.2993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                1427
_reflns_number_total             1521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030260r_2.cif
_cod_data_source_block           publ_contact_author
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'mixed ' changed to 'mixed'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometrically' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_formula_sum        'C8 H22 U O6 I2'
_cod_database_code               4114204
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.5000 0.0000 0.0585(2) Uani 1 2 d S . .
I1 I 0.2356(3) 0.6403(3) 0.2048(2) 0.0779(18) Uani 0.685(5) 1 d P A 1
O1 O 0.5779(9) 0.3039(9) 0.1796(7) 0.0573(16) Uani 1 1 d . A .
O2 O 0.6396(7) 0.6157(7) -0.0137(7) 0.0714(17) Uani 1 1 d . A .
O5 O 0.258(3) 0.717(3) 0.083(2) 0.088(7) Uani 0.315(5) 1 d PD A 2
O6 O 0.337(2) 0.529(2) 0.257(2) 0.075(6) Uani 0.315(5) 1 d PD A 2
O7 O 0.133(3) 0.713(3) 0.310(3) 0.105(8) Uani 0.315(5) 1 d P A 2
N1 N 0.228(4) 0.639(4) 0.214(3) 0.000(12) Uiso 0.315(5) 1 d PD A 2
H1O H 0.658(12) 0.294(10) 0.209(8) 0.06(3) Uiso 1 1 d . . .
H2O H 0.533(10) 0.233(11) 0.225(8) 0.04(3) Uiso 1 1 d . . .
O3 O 0.4108(8) 0.0564(8) 0.3296(6) 0.0691(17) Uani 1 1 d . . .
O4 O 0.8354(9) 0.2992(9) 0.2444(8) 0.091(2) Uani 1 1 d . . .
C1 C 0.2720(17) 0.1831(16) 0.5050(12) 0.107(4) Uani 1 1 d . . .
H1A H 0.1648 0.1984 0.5764 0.128 Uiso 1 1 calc R . .
H1B H 0.2971 0.2839 0.4334 0.128 Uiso 1 1 calc R . .
H1C H 0.3588 0.1411 0.5486 0.128 Uiso 1 1 calc R . .
C2 C 0.2649(18) 0.0722(17) 0.4404(14) 0.108(4) Uani 1 1 d . . .
H2A H 0.2473 -0.0316 0.5117 0.130 Uiso 1 1 calc R . .
H2B H 0.1696 0.1094 0.4054 0.130 Uiso 1 1 calc R . .
C3 C 0.4146(14) -0.0496(14) 0.2597(12) 0.090(3) Uani 1 1 d . . .
H3A H 0.3887 -0.1529 0.3294 0.108 Uiso 1 1 calc R . .
H3B H 0.3281 -0.0087 0.2143 0.108 Uiso 1 1 calc R . .
C4 C 0.5726(16) -0.0700(14) 0.1563(12) 0.091(3) Uani 1 1 d . . .
H4A H 0.6558 -0.1251 0.2024 0.109 Uiso 1 1 calc R . .
H4B H 0.6044 0.0330 0.0931 0.109 Uiso 1 1 calc R . .
H4C H 0.5658 -0.1319 0.1028 0.109 Uiso 1 1 calc R . .
C5 C 0.9854(17) 0.246(3) 0.156(2) 0.197(10) Uani 1 1 d . . .
H5A H 1.0703 0.2213 0.2020 0.236 Uiso 1 1 calc R . .
H5B H 1.0190 0.3338 0.0692 0.236 Uiso 1 1 calc R . .
C6 C 0.988(2) 0.113(3) 0.1194(17) 0.148(7) Uani 1 1 d . . .
H6A H 1.1003 0.0853 0.0595 0.177 Uiso 1 1 calc R . .
H6B H 0.9099 0.1374 0.0689 0.177 Uiso 1 1 calc R . .
H6C H 0.9569 0.0243 0.2043 0.177 Uiso 1 1 calc R . .
C7 C 0.828(4) 0.428(4) 0.288(3) 0.222(13) Uani 1 1 d . . .
H7A H 0.9097 0.3968 0.3378 0.266 Uiso 1 1 calc R . .
H7B H 0.8705 0.5141 0.2018 0.266 Uiso 1 1 calc R . .
C8 C 0.702(5) 0.486(3) 0.361(3) 0.28(2) Uani 1 1 d . . .
H8A H 0.7298 0.5483 0.4024 0.331 Uiso 1 1 calc R . .
H8B H 0.6400 0.4017 0.4348 0.331 Uiso 1 1 calc R . .
H8C H 0.6335 0.5529 0.3031 0.331 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'
O O 0.0106 0.0060 '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'
N N 0.0061 0.0033 '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
O2 U1 O2 180.0(4) 2_665 .
O2 U1 O1 90.2(3) 2_665 .
O2 U1 O1 89.8(3) . .
O2 U1 O1 89.8(3) 2_665 2_665
O2 U1 O1 90.2(3) . 2_665
O1 U1 O1 180.0(4) . 2_665
O2 U1 O5 92.7(6) 2_665 .
O2 U1 O5 87.3(6) . .
O1 U1 O5 114.5(4) . .
O1 U1 O5 65.5(4) 2_665 .
O2 U1 O5 87.3(6) 2_665 2_665
O2 U1 O5 92.7(6) . 2_665
O1 U1 O5 65.5(4) . 2_665
O1 U1 O5 114.5(4) 2_665 2_665
O5 U1 O5 180.000(1) . 2_665
O2 U1 O6 93.7(5) 2_665 .
O2 U1 O6 86.3(5) . .
O1 U1 O6 64.5(4) . .
O1 U1 O6 115.5(4) 2_665 .
O5 U1 O6 50.0(6) . .
O5 U1 O6 130.0(6) 2_665 .
O2 U1 O6 86.3(5) 2_665 2_665
O2 U1 O6 93.7(5) . 2_665
O1 U1 O6 115.5(4) . 2_665
O1 U1 O6 64.5(4) 2_665 2_665
O5 U1 O6 130.0(6) . 2_665
O5 U1 O6 50.0(6) 2_665 2_665
O6 U1 O6 180.0(8) . 2_665
O2 U1 I1 89.5(2) 2_665 .
O2 U1 I1 90.5(2) . .
O1 U1 I1 90.20(15) . .
O1 U1 I1 89.80(15) 2_665 .
O5 U1 I1 24.5(4) . .
O5 U1 I1 155.5(4) 2_665 .
O6 U1 I1 26.1(4) . .
O6 U1 I1 153.9(4) 2_665 .
O2 U1 I1 90.5(2) 2_665 2_665
O2 U1 I1 89.5(2) . 2_665
O1 U1 I1 89.80(15) . 2_665
O1 U1 I1 90.20(15) 2_665 2_665
O5 U1 I1 155.5(4) . 2_665
O5 U1 I1 24.5(4) 2_665 2_665
O6 U1 I1 153.9(4) . 2_665
O6 U1 I1 26.1(4) 2_665 2_665
I1 U1 I1 180.0 . 2_665
N1 O5 U1 93.5(18) . .
N1 O6 U1 92.2(18) . .
O5 N1 O6 121(3) . .
O5 N1 O7 119(3) . .
O6 N1 O7 112(2) . .
C2 O3 C3 115.4(8) . .
C5 O4 C7 118.8(15) . .
O3 C2 C1 111.6(11) . .
C4 C3 O3 112.1(8) . .
O4 C5 C6 116.8(14) . .
C8 C7 O4 123(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.758(6) 2_665
U1 O2 1.758(6) .
U1 O1 2.321(7) .
U1 O1 2.321(7) 2_665
U1 O5 2.65(2) .
U1 O5 2.65(2) 2_665
U1 O6 2.680(19) .
U1 O6 2.680(19) 2_665
U1 I1 2.939(3) .
U1 I1 2.939(3) 2_665
O5 N1 1.29(2) .
O6 N1 1.30(2) .
O7 N1 1.34(5) .
O3 C2 1.400(14) .
O3 C3 1.432(11) .
O4 C5 1.39(2) .
O4 C7 1.41(2) .
C1 C2 1.464(16) .
C3 C4 1.431(15) .
C5 C6 1.42(3) .
C7 C8 1.21(4) .
