#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/14/2221450.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2221450
loop_
_publ_author_name
'Yoshimura, Takashi'
'Kikunaga, Hidetoshi'
'Shinohara, Atsushi'
_publ_section_title
Poly[(μ₂-2-hydroxy-2-methylpropionato-κ³O¹,O²:O^1'^)(μ₂-2-hydroxy-2-methylpropionato-κ²O¹:κO^1'^)dioxidouranium(VI)]
_journal_coeditor_code           NG2546
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m355
_journal_page_last               m356
_journal_paper_doi               10.1107/S1600536809006059
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[U (C4 H7 O3)2 O2]'
_chemical_formula_moiety         'C8 H14 O8 U'
_chemical_formula_sum            'C8 H14 O8 U'
_chemical_formula_weight         476.22
_chemical_name_systematic
;
Poly[(μ₂-2-hydroxy-2-methylpropionato-
κ³O¹,O²:O^1'^)(μ₂-2-hydroxy-2-
methylpropionato-κ²O¹:κO^1'^)dioxidouranium(VI)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.246(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.009(2)
_cell_length_b                   8.237(2)
_cell_length_c                   17.552(6)
_cell_measurement_reflns_used    8716
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1289.0(6)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'TEXSAN (Rigaku/MSC, 2004)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae et al.,  2006)'
_computing_publication_material  'TEXSAN (Rigaku/MSC, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1994)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11887
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.0
_exptl_absorpt_coefficient_mu    12.622
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             872.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.99
_refine_diff_density_min         -2.15
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2949
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.079P)²+5.354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                2547
_reflns_number_total             2949
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2546.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2221450
_cod_database_fobs_code          2221450
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U(1) 0.63772(2) 0.19668(3) 0.624250(10) 0.01800(10) Uani d . 1.00 . .
O O(1) 0.7538(6) 0.3101(5) 0.5695(3) 0.0280(10) Uani d . 1.00 . .
O O(2) 0.5188(6) 0.0891(6) 0.6778(3) 0.0320(10) Uani d . 1.00 . .
O O(3) 0.4753(5) 0.4342(5) 0.6250(3) 0.0260(10) Uani d . 1.00 . .
O O(4) 0.6920(5) 0.3869(6) 0.7286(3) 0.0290(10) Uani d . 1.00 . .
O O(5) 0.6435(5) 0.6018(6) 0.7991(3) 0.0252(10) Uani d . 1.00 . .
O O(6) 0.2338(5) 0.4208(5) 0.5248(3) 0.0241(10) Uani d . 1.00 . .
O O(7) 0.7009(6) -0.0415(6) 0.5630(3) 0.0340(10) Uani d . 1.00 . .
O O(8) 0.4514(6) 0.1975(5) 0.5169(3) 0.0300(10) Uani d . 1.00 . .
C C(1) 0.6115(7) 0.5015(8) 0.7435(3) 0.0220(10) Uani d . 1.00 . .
C C(2) 0.4611(7) 0.5295(8) 0.6929(4) 0.0210(10) Uani d . 1.00 . .
C C(3) 0.3351(8) 0.4630(10) 0.7324(4) 0.036(2) Uani d . 1.00 . .
C C(4) 0.4392(10) 0.7064(7) 0.6704(5) 0.030(2) Uani d . 1.00 . .
C C(5) 0.3241(7) 0.1601(8) 0.4820(4) 0.0200(10) Uani d . 1.00 . .
C C(6) 0.1889(7) 0.2626(8) 0.4949(4) 0.0210(10) Uani d . 1.00 . .
C C(7) 0.1191(10) 0.1790(9) 0.5588(5) 0.039(2) Uani d . 1.00 . .
C C(8) 0.0781(10) 0.2800(10) 0.4211(5) 0.038(2) Uani d . 1.00 . .
H H(1) 0.3277 0.5253 0.7779 0.0356 Uiso calc . 1.00 . .
H H(2) 0.2423 0.4698 0.6980 0.0356 Uiso calc . 1.00 . .
H H(3) 0.3555 0.3516 0.7462 0.0356 Uiso calc . 1.00 . .
H H(4) 0.4388 0.7711 0.7159 0.0297 Uiso calc . 1.00 . .
H H(5) 0.3454 0.7192 0.6374 0.0297 Uiso calc . 1.00 . .
H H(6) 0.5196 0.7409 0.6438 0.0297 Uiso calc . 1.00 . .
H H(7) 0.0321 0.2384 0.5684 0.0386 Uiso calc . 1.00 . .
H H(8) 0.1908 0.1757 0.6048 0.0386 Uiso calc . 1.00 . .
H H(9) 0.0907 0.0703 0.5432 0.0386 Uiso calc . 1.00 . .
H H(10) -0.0100 0.3359 0.4322 0.0383 Uiso calc . 1.00 . .
H H(11) 0.0507 0.1746 0.4007 0.0383 Uiso calc . 1.00 . .
H H(12) 0.1237 0.3413 0.3841 0.0383 Uiso calc . 1.00 . .
H H(13) 0.4210 0.4724 0.5878 0.0255 Uiso calc . 1.00 . .
H H(14) 0.2178 0.4883 0.4902 0.0241 Uiso calc . 1.00 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
U U -9.677 9.665
;International Tables for Crystallography
(1992, 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_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O(1) U(1) O(2) . . . 178.3(2) no
O(1) U(1) O(3) . . . 88.9(2) no
O(1) U(1) O(4) . . . 89.9(2) no
O(1) U(1) O(5) . . 2_646 88.5(2) no
O(1) U(1) O(7) . . . 89.5(2) no
O(1) U(1) O(8) . . . 88.5(2) no
O(2) U(1) O(3) . . . 89.4(2) no
O(2) U(1) O(4) . . . 89.7(2) no
O(2) U(1) O(5) . . 2_646 93.0(2) no
O(2) U(1) O(7) . . . 91.7(2) no
O(2) U(1) O(8) . . . 90.6(2) no
O(3) U(1) O(4) . . . 62.10(10) no
O(3) U(1) O(5) . . 2_646 135.7(2) no
O(3) U(1) O(7) . . . 148.9(2) no
O(3) U(1) O(8) . . . 68.9(2) no
O(4) U(1) O(5) . . 2_646 73.7(2) no
O(4) U(1) O(7) . . . 149.0(2) no
O(4) U(1) O(8) . . . 131.0(2) no
O(5) U(1) O(7) 2_646 . . 75.3(2) no
O(5) U(1) O(8) 2_646 . . 155.1(2) no
O(7) U(1) O(8) . . . 80.0(2) no
U(1) O(3) C(2) . . . 124.2(3) no
U(1) O(3) H(13) . . . 126.3 no
C(2) O(3) H(13) . . . 109.5 no
U(1) O(4) C(1) . . . 126.5(4) no
U(1) O(5) C(1) 2_656 . . 136.7(4) no
C(6) O(6) H(14) . . . 109.5 no
U(1) O(7) C(5) . . 3_656 154.9(4) no
U(1) O(8) C(5) . . . 153.0(5) no
O(4) C(1) O(5) . . . 125.3(6) no
O(4) C(1) C(2) . . . 119.3(5) no
O(5) C(1) C(2) . . . 115.4(6) no
O(3) C(2) C(1) . . . 102.7(5) no
O(3) C(2) C(3) . . . 109.9(5) no
O(3) C(2) C(4) . . . 109.3(5) no
C(1) C(2) C(3) . . . 109.9(5) no
C(1) C(2) C(4) . . . 111.6(6) no
C(3) C(2) C(4) . . . 112.9(6) no
C(2) C(3) H(1) . . . 109.5 no
C(2) C(3) H(2) . . . 109.5 no
C(2) C(3) H(3) . . . 109.5 no
H(1) C(3) H(2) . . . 109.5 no
H(1) C(3) H(3) . . . 109.5 no
H(2) C(3) H(3) . . . 109.5 no
C(2) C(4) H(4) . . . 109.5 no
C(2) C(4) H(5) . . . 109.5 no
C(2) C(4) H(6) . . . 109.5 no
H(4) C(4) H(5) . . . 109.5 no
H(4) C(4) H(6) . . . 109.5 no
H(5) C(4) H(6) . . . 109.5 no
O(7) C(5) O(8) 3_656 . . 124.4(6) no
O(7) C(5) C(6) 3_656 . . 116.7(6) no
O(8) C(5) C(6) . . . 119.0(6) no
O(6) C(6) C(5) . . . 111.4(5) no
O(6) C(6) C(7) . . . 105.3(5) no
O(6) C(6) C(8) . . . 109.8(6) no
C(5) C(6) C(7) . . . 106.3(6) no
C(5) C(6) C(8) . . . 111.5(6) no
C(7) C(6) C(8) . . . 112.2(6) no
C(6) C(7) H(7) . . . 109.5 no
C(6) C(7) H(8) . . . 109.5 no
C(6) C(7) H(9) . . . 109.5 no
H(7) C(7) H(8) . . . 109.5 no
H(7) C(7) H(9) . . . 109.5 no
H(8) C(7) H(9) . . . 109.5 no
C(6) C(8) H(10) . . . 109.5 no
C(6) C(8) H(11) . . . 109.5 no
C(6) C(8) H(12) . . . 109.5 no
H(10) C(8) H(11) . . . 109.5 no
H(10) C(8) H(12) . . . 109.5 no
H(11) C(8) H(12) . . . 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U(1) O(1) . . 1.783(5) yes
U(1) O(2) . . 1.762(6) yes
U(1) O(3) . . 2.444(5) yes
U(1) O(4) . . 2.407(5) yes
U(1) O(5) . 2_646 2.355(4) yes
U(1) O(7) . . 2.346(5) yes
U(1) O(8) . . 2.336(5) yes
O(3) C(2) . . 1.449(8) no
O(3) H(13) . . 0.820 no
O(4) C(1) . . 1.241(8) no
O(5) C(1) . . 1.280(8) no
O(6) C(6) . . 1.441(8) no
O(6) H(14) . . 0.820 no
O(7) C(5) . 3_656 1.257(8) no
O(8) C(5) . . 1.259(8) no
C(1) C(2) . . 1.528(8) no
C(2) C(3) . . 1.510(10) no
C(2) C(4) . . 1.514(9) no
C(3) H(1) . . 0.960 no
C(3) H(2) . . 0.960 no
C(3) H(3) . . 0.960 no
C(4) H(4) . . 0.960 no
C(4) H(5) . . 0.960 no
C(4) H(6) . . 0.960 no
C(5) C(6) . . 1.525(10) no
C(6) C(7) . . 1.530(10) no
C(6) C(8) . . 1.523(10) no
C(7) H(7) . . 0.960 no
C(7) H(8) . . 0.960 no
C(7) H(9) . . 0.960 no
C(8) H(10) . . 0.960 no
C(8) H(11) . . 0.960 no
C(8) H(12) . . 0.960 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O(3) H(13) O(6) . . . 0.820 1.927 2.597(6) 138.188 yes
O(6) H(14) O(1) . . 3_666 0.820 1.999 2.777(6) 158.201 yes
