#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318069.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_4318069
loop_
_publ_author_name
'Marianne P. Wilkerson'
'Carol J. Burns'
'David E. Morris'
'Robert T. Paine'
'Brian L. Scott'
_publ_contact_author             'Carol J. Burns'
_publ_contact_author_email       cjb@lanl.gov
_publ_section_title
;
 Steric Control of Substituted Phenoxide Ligands on Product Structures of
 Uranyl Aryloxide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3110
_journal_page_last               3120
_journal_paper_doi               10.1021/ic011080q
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C40 H44 Cl8 O12 U2'
_chemical_formula_weight         1476.41
_chemical_name_systematic
;
Bis-m-2,6-dichlorophenoxy-bis[2,6-dichlorophenoxy
(dioxo)bis(tetrahydrofuran)uranium(VI)]
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   31.836(5)
_cell_length_b                   31.836(5)
_cell_length_c                   13.690(3)
_cell_measurement_temperature    203(2)
_cell_volume                     12016(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device_type  'Siemens P4'
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3002
_diffrn_reflns_theta_max         19.97
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.509
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XEMP in SHELXTL 4.2/360 (Siemens)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             6300
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2388
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0553P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                1669
_reflns_number_total             2388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011080q_2.cif
_cod_data_source_block           mar2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4318069
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.53547(3) 0.03902(3) 0.12284(5) 0.0237(3) Uani 1 1 d . . .
Cl1 Cl 0.60918(18) -0.00966(18) -0.0536(4) 0.0386(14) Uani 1 1 d . . .
Cl2 Cl 0.5480(2) 0.11490(19) -0.1473(4) 0.0493(16) Uani 1 1 d . . .
Cl3 Cl 0.63224(19) 0.0392(2) 0.3468(4) 0.0483(15) Uani 1 1 d . . .
Cl4 Cl 0.5609(2) 0.1608(2) 0.3141(4) 0.0550(17) Uani 1 1 d . . .
O1 O 0.5561(4) -0.0013(4) 0.1445(8) 0.026(3) Uani 1 1 d . . .
O2 O 0.5138(4) 0.0787(4) 0.1007(8) 0.025(3) Uani 1 1 d . . .
O3 O 0.5405(4) 0.0277(4) -0.0525(8) 0.023(3) Uani 1 1 d . . .
O4 O 0.5742(4) 0.0799(4) 0.2570(9) 0.035(3) Uani 1 1 d . . .
O5 O 0.6165(4) 0.1038(5) 0.0728(9) 0.039(4) Uani 1 1 d . . .
O6 O 0.4809(4) 0.0034(4) 0.2604(8) 0.034(3) Uani 1 1 d . . .
C1 C 0.5815(7) 0.0554(7) -0.1052(14) 0.025(5) Uani 1 1 d . . .
C2 C 0.6161(7) 0.0415(7) -0.1140(12) 0.025(5) Uani 1 1 d . . .
C3 C 0.6579(7) 0.0674(8) -0.1735(14) 0.036(6) Uani 1 1 d U . .
H3 H 0.6802 0.0567 -0.1793 0.043 Uiso 1 1 calc R . .
C4 C 0.6654(8) 0.1078(8) -0.2217(15) 0.052(7) Uani 1 1 d . . .
H4 H 0.6931 0.1255 -0.2595 0.062 Uiso 1 1 calc R . .
C5 C 0.6310(7) 0.1221(7) -0.2136(14) 0.036(6) Uani 1 1 d U . .
H5 H 0.6358 0.1499 -0.2457 0.043 Uiso 1 1 calc R . .
C6 C 0.5897(6) 0.0955(6) -0.1585(14) 0.024(5) Uani 1 1 d . . .
C7 C 0.5974(6) 0.1020(7) 0.3363(15) 0.027(5) Uani 1 1 d . . .
C8 C 0.6283(7) 0.0899(7) 0.3895(14) 0.029(5) Uani 1 1 d . . .
C9 C 0.6541(7) 0.1143(8) 0.4699(15) 0.037(6) Uani 1 1 d . . .
H9 H 0.6736 0.1044 0.5011 0.045 Uiso 1 1 calc R . .
C10 C 0.6520(7) 0.1516(8) 0.5039(14) 0.039(6) Uani 1 1 d U . .
H10 H 0.6701 0.1683 0.5584 0.047 Uiso 1 1 calc R . .
C11 C 0.6220(7) 0.1663(8) 0.4574(14) 0.042(6) Uani 1 1 d U . .
H11 H 0.6193 0.1919 0.4825 0.051 Uiso 1 1 calc R . .
C12 C 0.5969(7) 0.1426(7) 0.3747(14) 0.030(5) Uani 1 1 d . . .
C13 C 0.6601(8) 0.1031(9) 0.0979(18) 0.065(8) Uani 1 1 d . . .
H13A H 0.6562 0.0873 0.1605 0.078 Uiso 1 1 calc R . .
H13B H 0.6669 0.0853 0.0489 0.078 Uiso 1 1 calc R . .
C14 C 0.6990(13) 0.1520(13) 0.102(3) 0.144(15) Uani 1 1 d U . .
H14A H 0.7117 0.1600 0.1684 0.172 Uiso 1 1 calc R . .
H14B H 0.7250 0.1566 0.0589 0.172 Uiso 1 1 calc R . .
C15 C 0.6797(11) 0.1811(11) 0.074(3) 0.161(18) Uani 1 1 d . . .
H15A H 0.6922 0.1944 0.0097 0.193 Uiso 1 1 calc R . .
H15B H 0.6906 0.2080 0.1191 0.193 Uiso 1 1 calc R . .
C16 C 0.6266(8) 0.1546(8) 0.0706(19) 0.064(7) Uani 1 1 d . . .
H16A H 0.6145 0.1615 0.0112 0.077 Uiso 1 1 calc R . .
H16B H 0.6128 0.1620 0.1267 0.077 Uiso 1 1 calc R . .
C17 C 0.4933(8) -0.0214(8) 0.3367(16) 0.058(7) Uani 1 1 d . . .
H17A H 0.5236 0.0009 0.3686 0.070 Uiso 1 1 calc R . .
H17B H 0.4957 -0.0482 0.3096 0.070 Uiso 1 1 calc R . .
C18 C 0.4507(10) -0.0393(10) 0.4073(18) 0.080(9) Uani 1 1 d . . .
H18A H 0.4245 -0.0708 0.3876 0.096 Uiso 1 1 calc R . .
H18B H 0.4606 -0.0416 0.4731 0.096 Uiso 1 1 calc R . .
C19 C 0.4352(9) -0.0015(11) 0.4017(16) 0.079(9) Uani 1 1 d . . .
H19A H 0.4001 -0.0168 0.4017 0.095 Uiso 1 1 calc R . .
H19B H 0.4478 0.0204 0.4571 0.095 Uiso 1 1 calc R . .
C20 C 0.4557(7) 0.0257(8) 0.3081(16) 0.046(7) Uani 1 1 d . . .
H20A H 0.4299 0.0234 0.2666 0.055 Uiso 1 1 calc R . .
H20B H 0.4782 0.0597 0.3214 0.055 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'
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
O1 U1 O2 179.1(5) . . ?
O1 U1 O4 89.2(5) . . ?
O2 U1 O4 91.4(5) . . ?
O1 U1 O6 88.2(5) . . ?
O2 U1 O6 91.3(5) . . ?
O4 U1 O6 72.0(4) . . ?
O1 U1 O3 89.0(4) . . ?
O2 U1 O3 90.9(4) . . ?
O4 U1 O3 146.7(4) . . ?
O6 U1 O3 141.0(4) . . ?
O1 U1 O5 92.4(5) . . ?
O2 U1 O5 88.4(5) . . ?
O4 U1 O5 72.4(4) . . ?
O6 U1 O5 144.5(4) . . ?
O3 U1 O5 74.5(4) . . ?
O1 U1 O3 90.1(5) . 10_655 ?
O2 U1 O3 89.0(4) . 10_655 ?
O4 U1 O3 146.8(4) . 10_655 ?
O6 U1 O3 74.7(4) . 10_655 ?
O3 U1 O3 66.4(4) . 10_655 ?
O5 U1 O3 140.7(4) . 10_655 ?
C1 O3 U1 122.5(10) . . ?
C1 O3 U1 123.9(10) . 10_655 ?
U1 O3 U1 113.6(4) . 10_655 ?
C7 O4 U1 177.2(13) . . ?
C13 O5 C16 109.7(15) . . ?
C13 O5 U1 122.3(12) . . ?
C16 O5 U1 119.0(11) . . ?
C20 O6 C17 107.5(14) . . ?
C20 O6 U1 123.9(11) . . ?
C17 O6 U1 118.6(10) . . ?
O3 C1 C6 123.9(16) . . ?
O3 C1 C2 119.7(17) . . ?
C6 C1 C2 116.1(17) . . ?
C1 C2 C3 121.9(18) . . ?
C1 C2 Cl1 120.8(15) . . ?
C3 C2 Cl1 117.3(15) . . ?
C4 C3 C2 120.0(19) . . ?
C3 C4 C5 118.7(19) . . ?
C6 C5 C4 121(2) . . ?
C5 C6 C1 122.6(18) . . ?
C5 C6 Cl2 119.7(16) . . ?
C1 C6 Cl2 117.5(15) . . ?
O4 C7 C12 123.2(17) . . ?
O4 C7 C8 123.9(19) . . ?
C12 C7 C8 112.7(19) . . ?
C9 C8 C7 124.0(19) . . ?
C9 C8 Cl3 119.2(16) . . ?
C7 C8 Cl3 116.8(16) . . ?
C10 C9 C8 121(2) . . ?
C9 C10 C11 119.4(19) . . ?
C12 C11 C10 120(2) . . ?
C11 C12 C7 122.9(19) . . ?
C11 C12 Cl4 120.9(17) . . ?
C7 C12 Cl4 116.2(15) . . ?
C14 C13 O5 108(2) . . ?
C15 C14 C13 106(3) . . ?
C14 C15 C16 113(3) . . ?
C15 C16 O5 101(2) . . ?
O6 C17 C18 102.9(16) . . ?
C19 C18 C17 104.7(19) . . ?
C20 C19 C18 106.3(18) . . ?
O6 C20 C19 106.7(18) . . ?
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 O1 1.735(11) . ?
U1 O2 1.743(11) . ?
U1 O4 2.232(13) . ?
U1 O6 2.425(12) . ?
U1 O3 2.444(11) . ?
U1 O5 2.461(12) . ?
U1 O3 2.480(11) 10_655 ?
Cl1 C2 1.739(19) . ?
Cl2 C6 1.726(18) . ?
Cl3 C8 1.778(19) . ?
Cl4 C12 1.732(19) . ?
O3 C1 1.36(2) . ?
O3 U1 2.480(11) 10_655 ?
O4 C7 1.30(2) . ?
O5 C13 1.44(2) . ?
O5 C16 1.48(2) . ?
O6 C20 1.46(2) . ?
O6 C17 1.48(2) . ?
C1 C6 1.38(2) . ?
C1 C2 1.38(2) . ?
C2 C3 1.42(2) . ?
C3 C4 1.36(3) . ?
C4 C5 1.39(3) . ?
C5 C6 1.38(2) . ?
C7 C12 1.40(3) . ?
C7 C8 1.42(2) . ?
C8 C9 1.36(3) . ?
C9 C10 1.31(3) . ?
C10 C11 1.41(3) . ?
C11 C12 1.37(3) . ?
C13 C14 1.42(3) . ?
C14 C15 1.40(4) . ?
C15 C16 1.47(3) . ?
C17 C18 1.52(3) . ?
C18 C19 1.51(3) . ?
C19 C20 1.50(3) . ?
