#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:11:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179279 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/99/4319911.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_4319911
loop_
_publ_author_name
'Janet A. Danis'
'Mavis R. Lin'
'Brian L. Scott'
'Bryan W. Eichhorn'
'Wolfgang H. Runde'
_publ_section_title
;
 Coordination Trends in Alkali Metal Crown Ether Uranyl Halide Complexes:
 The Series [A(Crown)]2[UO2X4] Where A = Li, Na, K and X = Cl, Br
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3389
_journal_page_last               3394
_journal_paper_doi               10.1021/ic0011056
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H48 Br4 K2 O14 U'
_chemical_formula_weight         1196.49
_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                 92.6590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2472(5)
_cell_length_b                   10.0343(5)
_cell_length_c                   19.7082(9)
_cell_measurement_temperature    293(2)
_cell_volume                     2024.28(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.945
_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    0.0225
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3928
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    8.216
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1148
_refine_diff_density_max         0.552
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0249
_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)+(0.0381P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                3564
_reflns_number_total             3928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0011056_1.cif
_cod_data_source_block           '[K(18-crown-6)]2[UO2Br4]'
_cod_database_code               4319911
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.5000 0.0000 0.02370(7) Uani 1 2 d S . .
Br1 Br 0.68532(4) 0.37687(4) 0.090042(19) 0.03380(10) Uani 1 1 d . . .
Br2 Br 0.45112(5) 0.68455(5) 0.10362(2) 0.05088(13) Uani 1 1 d . . .
K1 K 0.77940(8) 0.67218(7) 0.15803(4) 0.03012(18) Uani 1 1 d . . .
O1 O 0.3743(3) 0.3963(3) 0.02876(14) 0.0367(6) Uani 1 1 d . . .
O2 O 0.9462(3) 0.4782(3) 0.23197(15) 0.0387(7) Uani 1 1 d . . .
O3 O 1.0089(2) 0.5702(3) 0.10210(13) 0.0360(6) Uani 1 1 d . . .
O4 O 0.9301(3) 0.8257(3) 0.05727(13) 0.0372(6) Uani 1 1 d . . .
O5 O 0.7289(3) 0.9425(3) 0.12731(13) 0.0366(6) Uani 1 1 d . . .
O6 O 0.6749(2) 0.8459(2) 0.25599(13) 0.0302(6) Uani 1 1 d . . .
O7 O 0.7253(3) 0.5807(2) 0.29117(12) 0.0324(6) Uani 1 1 d . . .
C1 C 1.0179(4) 0.4013(4) 0.1858(2) 0.0392(9) Uani 1 1 d . . .
H1A H 0.9583 0.3494 0.1566 0.047 Uiso 1 1 calc R . .
H1B H 1.0757 0.3402 0.2107 0.047 Uiso 1 1 calc R . .
C2 C 1.0952(4) 0.4923(4) 0.1442(2) 0.0391(10) Uani 1 1 d . . .
H2A H 1.1487 0.5499 0.1735 0.047 Uiso 1 1 calc R . .
H2B H 1.1525 0.4410 0.1163 0.047 Uiso 1 1 calc R . .
C3 C 1.0751(4) 0.6428(4) 0.0523(2) 0.0395(9) Uani 1 1 d . . .
H3A H 1.1176 0.5819 0.0221 0.047 Uiso 1 1 calc R . .
H3B H 1.1413 0.6996 0.0740 0.047 Uiso 1 1 calc R . .
C4 C 0.9761(4) 0.7257(4) 0.01297(19) 0.0386(10) Uani 1 1 d . . .
H4A H 1.0157 0.7668 -0.0256 0.046 Uiso 1 1 calc R . .
H4B H 0.9040 0.6703 -0.0038 0.046 Uiso 1 1 calc R . .
C5 C 0.8355(5) 0.9099(4) 0.0243(2) 0.0431(10) Uani 1 1 d . . .
H5A H 0.7604 0.8582 0.0081 0.052 Uiso 1 1 calc R . .
H5B H 0.8724 0.9538 -0.0143 0.052 Uiso 1 1 calc R . .
C6 C 0.7957(5) 1.0111(4) 0.0753(2) 0.0439(11) Uani 1 1 d . . .
H6A H 0.8722 1.0563 0.0949 0.053 Uiso 1 1 calc R . .
H6B H 0.7386 1.0771 0.0536 0.053 Uiso 1 1 calc R . .
C7 C 0.6972(5) 1.0294(4) 0.1811(2) 0.0406(10) Uani 1 1 d . . .
H7A H 0.6552 1.1091 0.1628 0.049 Uiso 1 1 calc R . .
H7B H 0.7760 1.0555 0.2068 0.049 Uiso 1 1 calc R . .
C8 C 0.6070(4) 0.9573(4) 0.2261(2) 0.0393(9) Uani 1 1 d . . .
H8A H 0.5786 1.0167 0.2613 0.047 Uiso 1 1 calc R . .
H8B H 0.5304 0.9269 0.1997 0.047 Uiso 1 1 calc R . .
C9 C 0.5910(4) 0.7738(4) 0.29867(19) 0.0360(9) Uani 1 1 d . . .
H9A H 0.5222 0.7305 0.2714 0.043 Uiso 1 1 calc R . .
H9B H 0.5510 0.8342 0.3300 0.043 Uiso 1 1 calc R . .
C10 C 0.6709(4) 0.6722(4) 0.33705(19) 0.0350(9) Uani 1 1 d . . .
H10A H 0.7404 0.7160 0.3637 0.042 Uiso 1 1 calc R . .
H10B H 0.6165 0.6247 0.3680 0.042 Uiso 1 1 calc R . .
C11 C 0.8070(5) 0.4852(4) 0.3245(2) 0.0445(11) Uani 1 1 d . . .
H11A H 0.7562 0.4314 0.3545 0.053 Uiso 1 1 calc R . .
H11B H 0.8750 0.5300 0.3518 0.053 Uiso 1 1 calc R . .
C12 C 0.8672(5) 0.3981(4) 0.2733(2) 0.0456(11) Uani 1 1 d . . .
H12A H 0.9203 0.3300 0.2961 0.055 Uiso 1 1 calc R . .
H12B H 0.7995 0.3544 0.2454 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'
K K 0.2009 0.2494 '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
_geom_angle_publ_flag
O1 U1 O1 180.00(17) 3_665 . ?
O1 U1 Br2 90.12(9) 3_665 . ?
O1 U1 Br2 89.88(9) . . ?
O1 U1 Br2 89.88(9) 3_665 3_665 ?
O1 U1 Br2 90.12(9) . 3_665 ?
Br2 U1 Br2 180.000(13) . 3_665 ?
O1 U1 Br1 88.87(9) 3_665 . ?
O1 U1 Br1 91.13(9) . . ?
Br2 U1 Br1 88.229(13) . . ?
Br2 U1 Br1 91.771(13) 3_665 . ?
O1 U1 Br1 91.13(9) 3_665 3_665 ?
O1 U1 Br1 88.87(9) . 3_665 ?
Br2 U1 Br1 91.771(13) . 3_665 ?
Br2 U1 Br1 88.229(13) 3_665 3_665 ?
Br1 U1 Br1 180.0 . 3_665 ?
O1 U1 K1 62.90(9) 3_665 . ?
O1 U1 K1 117.10(9) . . ?
Br2 U1 K1 51.101(14) . . ?
Br2 U1 K1 128.899(14) 3_665 . ?
Br1 U1 K1 48.850(13) . . ?
Br1 U1 K1 131.151(13) 3_665 . ?
O1 U1 K1 117.10(9) 3_665 3_665 ?
O1 U1 K1 62.90(9) . 3_665 ?
Br2 U1 K1 128.899(14) . 3_665 ?
Br2 U1 K1 51.101(14) 3_665 3_665 ?
Br1 U1 K1 131.150(13) . 3_665 ?
Br1 U1 K1 48.850(13) 3_665 3_665 ?
K1 U1 K1 180.0 . 3_665 ?
U1 Br1 K1 92.105(17) . . ?
U1 Br2 K1 89.891(17) . . ?
O5 K1 O3 114.25(8) . . ?
O5 K1 O6 59.07(7) . . ?
O3 K1 O6 146.08(8) . . ?
O5 K1 O7 117.67(8) . . ?
O3 K1 O7 116.15(8) . . ?
O6 K1 O7 58.61(7) . . ?
O5 K1 O2 147.30(9) . . ?
O3 K1 O2 58.59(8) . . ?
O6 K1 O2 107.36(8) . . ?
O7 K1 O2 57.59(8) . . ?
O5 K1 O4 57.25(7) . . ?
O3 K1 O4 57.69(7) . . ?
O6 K1 O4 110.87(7) . . ?
O7 K1 O4 154.29(8) . . ?
O2 K1 O4 111.34(8) . . ?
O5 K1 Br1 135.46(6) . . ?
O3 K1 Br1 75.85(6) . . ?
O6 K1 Br1 134.22(6) . . ?
O7 K1 Br1 91.06(5) . . ?
O2 K1 Br1 76.32(6) . . ?
O4 K1 Br1 109.55(5) . . ?
O5 K1 Br2 74.63(6) . . ?
O3 K1 Br2 134.40(6) . . ?
O6 K1 Br2 78.39(6) . . ?
O7 K1 Br2 93.93(6) . . ?
O2 K1 Br2 135.10(7) . . ?
O4 K1 Br2 107.30(6) . . ?
Br1 K1 Br2 69.830(18) . . ?
O5 K1 U1 96.70(6) . . ?
O3 K1 U1 96.06(6) . . ?
O6 K1 U1 117.34(6) . . ?
O7 K1 U1 111.69(6) . . ?
O2 K1 U1 115.37(6) . . ?
O4 K1 U1 94.01(5) . . ?
Br1 K1 U1 39.046(11) . . ?
Br2 K1 U1 39.009(11) . . ?
C1 O2 C12 112.6(3) . . ?
C1 O2 K1 110.4(2) . . ?
C12 O2 K1 109.0(2) . . ?
C2 O3 C3 112.4(3) . . ?
C2 O3 K1 118.5(2) . . ?
C3 O3 K1 121.1(2) . . ?
C5 O4 C4 112.2(3) . . ?
C5 O4 K1 104.3(2) . . ?
C4 O4 K1 103.9(2) . . ?
C7 O5 C6 111.8(3) . . ?
C7 O5 K1 118.4(2) . . ?
C6 O5 K1 121.7(2) . . ?
C9 O6 C8 110.2(3) . . ?
C9 O6 K1 110.2(2) . . ?
C8 O6 K1 113.0(2) . . ?
C11 O7 C10 112.5(3) . . ?
C11 O7 K1 120.6(2) . . ?
C10 O7 K1 118.4(2) . . ?
O2 C1 C2 109.0(3) . . ?
O3 C2 C1 109.2(3) . . ?
O3 C3 C4 107.9(3) . . ?
O4 C4 C3 108.0(3) . . ?
O4 C5 C6 107.3(3) . . ?
O5 C6 C5 107.9(3) . . ?
O5 C7 C8 108.3(3) . . ?
O6 C8 C7 108.7(3) . . ?
O6 C9 C10 108.3(3) . . ?
O7 C10 C9 110.0(3) . . ?
O7 C11 C12 109.7(3) . . ?
O2 C12 C11 108.7(3) . . ?
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 1.769(2) 3_665 ?
U1 O1 1.769(2) . ?
U1 Br2 2.8188(4) . ?
U1 Br2 2.8188(4) 3_665 ?
U1 Br1 2.8230(4) . ?
U1 Br1 2.8230(4) 3_665 ?
U1 K1 4.4783(8) . ?
U1 K1 4.4783(8) 3_665 ?
Br1 K1 3.3744(9) . ?
Br2 K1 3.4852(10) . ?
K1 O5 2.821(3) . ?
K1 O3 2.834(3) . ?
K1 O6 2.847(2) . ?
K1 O7 2.858(2) . ?
K1 O2 2.933(3) . ?
K1 O4 2.998(3) . ?
O2 C1 1.423(5) . ?
O2 C12 1.423(5) . ?
O3 C2 1.419(5) . ?
O3 C3 1.419(4) . ?
O4 C5 1.421(5) . ?
O4 C4 1.424(4) . ?
O5 C7 1.421(5) . ?
O5 C6 1.435(5) . ?
O6 C9 1.427(4) . ?
O6 C8 1.429(5) . ?
O7 C11 1.414(5) . ?
O7 C10 1.421(4) . ?
C1 C2 1.481(6) . ?
C3 C4 1.501(6) . ?
C5 C6 1.498(6) . ?
C7 C8 1.497(6) . ?
C9 C10 1.492(6) . ?
C11 C12 1.490(6) . ?
