#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:23:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179325 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/22/4322236.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_4322236
loop_
_publ_author_name
'Marianne P. Wilkerson'
'Carol J. Burns'
'Robert T. Paine'
'Brian L. Scott'
_publ_section_title
;
 Synthesis and Crystal Structure of UO2Cl2(THF)3: A Simple Preparation of
 an Anhydrous Uranyl Reagent
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4156
_journal_page_last               4158
_journal_paper_doi               10.1021/ic990159g
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C12 H24 Cl2 O5 U'
_chemical_formula_weight         557.24
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8225(4)
_cell_length_b                   16.7914(10)
_cell_length_c                   15.6088(9)
_cell_measurement_temperature    203
_cell_volume                     1785.85(18)
_computing_cell_refinement       'SAINT 4.051(Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.051 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 5.1 (Bruker, 1997)'
_computing_publication_material  'SHELXTL 5.1 (Bruker, 1997)'
_computing_structure_refinement  'SHELXTL 5.1 (Bruker, 1997)'
_computing_structure_solution    'SHELXTL 5.1 (Bruker, 1997)'
_diffrn_ambient_temperature      203
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'ω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3592
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.401
_exptl_absorpt_correction_T_max  0.20
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.725
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.799
_refine_ls_goodness_of_fit_obs   0.810
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.799
_refine_ls_restrained_S_obs      0.810
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_obs          0.0395
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1199
_refine_ls_wR_factor_obs         0.1070
_reflns_number_observed          2813
_reflns_number_total             3592
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990159g.cif
_cod_data_source_block           ccd42
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1785.9(2)
_cod_database_code               4322236
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
U1 U 0.07095(4) 0.71664(2) 0.89848(2) 0.03566(13) Uani 1 d . .
Cl1 Cl 0.1282(4) 0.56619(14) 0.8445(2) 0.0639(7) Uani 1 d . .
Cl2 Cl 0.2106(4) 0.8278(2) 1.0093(2) 0.0596(6) Uani 1 d . .
O1 O -0.1267(8) 0.6902(4) 0.9616(5) 0.052(2) Uani 1 d . .
O2 O 0.2572(8) 0.7464(4) 0.8308(4) 0.0483(14) Uani 1 d . .
O3 O -0.1561(8) 0.6959(4) 0.7724(4) 0.0439(14) Uani 1 d . .
O4 O 0.2602(8) 0.6467(4) 1.0123(4) 0.051(2) Uani 1 d . .
O5 O -0.1136(8) 0.8383(3) 0.8584(4) 0.0433(13) Uani 1 d . .
C1 C -0.3310(14) 0.6459(7) 0.7750(8) 0.066(3) Uani 1 d . .
H1A H -0.2979(14) 0.5942(7) 0.7996(8) 0.079 Uiso 1 calc R .
H1B H -0.4286(14) 0.6708(7) 0.8093(8) 0.079 Uiso 1 calc R .
C2 C -0.4035(30) 0.6376(13) 0.6880(10) 0.158(10) Uani 1 d . .
H2A H -0.5170(30) 0.6716(13) 0.6773(10) 0.190 Uiso 1 calc R .
H2B H -0.4430(30) 0.5829(13) 0.6769(10) 0.190 Uiso 1 calc R .
C3 C -0.2463(18) 0.6604(11) 0.6310(8) 0.096(5) Uani 1 d . .
H3A H -0.2977(18) 0.6947(11) 0.5852(8) 0.115 Uiso 1 calc R .
H3B H -0.1894(18) 0.6135(11) 0.6058(8) 0.115 Uiso 1 calc R .
C4 C -0.0968(17) 0.7033(7) 0.6863(7) 0.064(3) Uani 1 d . .
H4A H 0.0319(17) 0.6799(7) 0.6808(7) 0.077 Uiso 1 calc R .
H4B H -0.0912(17) 0.7590(7) 0.6699(7) 0.077 Uiso 1 calc R .
C5 C 0.1862(15) 0.5960(10) 1.0764(8) 0.091(5) Uani 1 d . .
H5A H 0.1357(15) 0.5472(10) 1.0505(8) 0.109 Uiso 1 calc R .
H5B H 0.0801(15) 0.6223(10) 1.1044(8) 0.109 Uiso 1 calc R .
C6 C 0.3452(18) 0.5781(11) 1.1388(10) 0.110(6) Uani 1 d . .
H6A H 0.3187(18) 0.6014(11) 1.1939(10) 0.132 Uiso 1 calc R .
H6B H 0.3582(18) 0.5210(11) 1.1460(10) 0.132 Uiso 1 calc R .
C7 C 0.5204(17) 0.6104(8) 1.1081(9) 0.082(4) Uani 1 d . .
H7A H 0.6205(17) 0.5695(8) 1.1058(9) 0.099 Uiso 1 calc R .
H7B H 0.5696(17) 0.6528(8) 1.1455(9) 0.099 Uiso 1 calc R .
C8 C 0.4694(13) 0.6423(8) 1.0194(8) 0.070(3) Uani 1 d . .
H8A H 0.5266(13) 0.6946(8) 1.0122(8) 0.084 Uiso 1 calc R .
H8B H 0.5177(13) 0.6070(8) 0.9760(8) 0.084 Uiso 1 calc R .
C9 C -0.3182(14) 0.8489(6) 0.8710(8) 0.064(3) Uani 1 d . .
H9A H -0.3530(14) 0.8239(6) 0.9242(8) 0.077 Uiso 1 calc R .
H9B H -0.3962(14) 0.8250(6) 0.8241(8) 0.077 Uiso 1 calc R .
C10 C -0.3545(19) 0.9359(7) 0.8744(10) 0.086(4) Uani 1 d . .
H10A H -0.4306(19) 0.9534(7) 0.8237(10) 0.103 Uiso 1 calc R .
H10B H -0.4252(19) 0.9496(7) 0.9247(10) 0.103 Uiso 1 calc R .
C11 C -0.1577(18) 0.9734(6) 0.8784(10) 0.086(4) Uani 1 d . .
H11A H -0.1600(18) 1.0234(6) 0.8472(10) 0.104 Uiso 1 calc R .
H11B H -0.1130(18) 0.9834(6) 0.9374(10) 0.104 Uiso 1 calc R .
C12 C -0.0316(15) 0.9164(6) 0.8389(7) 0.061(3) Uani 1 d . .
H12A H 0.1021(15) 0.9210(6) 0.8626(7) 0.073 Uiso 1 calc R .
H12B H -0.0322(15) 0.9248(6) 0.7774(7) 0.073 Uiso 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O2 U1 O1 176.2(3) . . ?
O2 U1 O4 101.6(3) . . ?
O1 U1 O4 82.2(3) . . ?
O2 U1 O5 89.3(3) . . ?
O1 U1 O5 87.4(2) . . ?
O4 U1 O5 145.9(2) . . ?
O2 U1 O3 90.2(2) . . ?
O1 U1 O3 86.8(3) . . ?
O4 U1 O3 143.1(2) . . ?
O5 U1 O3 67.8(2) . . ?
O2 U1 Cl2 86.9(2) . . ?
O1 U1 Cl2 94.1(2) . . ?
O4 U1 Cl2 73.1(2) . . ?
O5 U1 Cl2 75.4(2) . . ?
O3 U1 Cl2 143.10(15) . . ?
O2 U1 Cl1 87.6(2) . . ?
O1 U1 Cl1 93.8(2) . . ?
O4 U1 Cl1 72.4(2) . . ?
O5 U1 Cl1 141.0(2) . . ?
O3 U1 Cl1 73.38(15) . . ?
Cl2 U1 Cl1 143.06(8) . . ?
C4 O3 C1 110.3(8) . . ?
C4 O3 U1 122.8(6) . . ?
C1 O3 U1 122.6(6) . . ?
C5 O4 C8 107.6(7) . . ?
C5 O4 U1 127.2(5) . . ?
C8 O4 U1 124.8(5) . . ?
C9 O5 C12 107.7(7) . . ?
C9 O5 U1 123.9(5) . . ?
C12 O5 U1 126.9(5) . . ?
C2 C1 O3 105.8(10) . . ?
C1 C2 C3 108.7(11) . . ?
C2 C3 C4 105.9(10) . . ?
O3 C4 C3 106.6(9) . . ?
O4 C5 C6 108.4(9) . . ?
C7 C6 C5 107.9(10) . . ?
C6 C7 C8 106.7(9) . . ?
O4 C8 C7 105.9(8) . . ?
O5 C9 C10 107.0(9) . . ?
C11 C10 C9 105.5(9) . . ?
C12 C11 C10 105.0(9) . . ?
C11 C12 O5 105.2(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.765(6) . ?
U1 O1 1.766(6) . ?
U1 O4 2.443(6) . ?
U1 O5 2.464(5) . ?
U1 O3 2.467(6) . ?
U1 Cl2 2.687(2) . ?
U1 Cl1 2.698(2) . ?
O3 C4 1.428(13) . ?
O3 C1 1.462(11) . ?
O4 C5 1.426(11) . ?
O4 C8 1.428(10) . ?
O5 C9 1.430(11) . ?
O5 C12 1.464(10) . ?
C1 C2 1.43(2) . ?
C2 C3 1.48(2) . ?
C3 C4 1.49(2) . ?
C5 C6 1.45(2) . ?
C6 C7 1.42(2) . ?
C7 C8 1.51(2) . ?
C9 C10 1.484(15) . ?
C10 C11 1.48(2) . ?
C11 C12 1.445(15) . ?
