#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:26:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179110 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/72/4307239.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_4307239
loop_
_publ_author_name
'Pierre Thuéry'
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      Bât. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       pierre.thuery@cea.fr
_publ_contact_author_fax         '33 1 69 08 66 40'
_publ_contact_author_name        'P. Thuéry'
_publ_contact_author_phone       '33 1 69 08 63 29'
_publ_section_title
;
Uranyl Ion Complexation by Citric and Citramalic Acids in the Presence of
Diamines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2307
_journal_page_last               2315
_journal_paper_doi               10.1021/ic061772k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C30 H56 N2 O28 U2'
_chemical_formula_weight         1368.83
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 115.634(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4966(10)
_cell_length_b                   20.177(3)
_cell_length_c                   14.2793(15)
_cell_measurement_reflns_used    57451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.56
_cell_volume                     4285.1(8)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and five ω scans with 2° steps'
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            57451
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.648
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_description       needle
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1135P)²+0.0064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                2794
_reflns_number_total             4054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061772ksi20060919_082125_1.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4307239
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
U U 0.13166(3) 0.28718(2) 0.31235(3) 0.0499(2) Uani 1 1 d . . .
O1 O 0.1196(6) 0.2007(5) 0.3200(6) 0.057(2) Uani 1 1 d . . .
O2 O 0.1479(5) 0.3733(5) 0.3053(6) 0.062(2) Uani 1 1 d . . .
O3 O -0.0007(5) 0.2952(4) 0.1565(6) 0.053(2) Uani 1 1 d . . .
O4 O 0.1545(6) 0.2744(5) 0.1598(7) 0.065(2) Uani 1 1 d . . .
O5 O 0.1157(5) 0.3022(5) -0.0037(7) 0.066(3) Uani 1 1 d . . .
O6 O -0.1835(5) 0.3013(4) 0.0071(6) 0.049(2) Uani 1 1 d . . .
O7 O -0.2092(5) 0.2336(5) -0.1249(6) 0.059(2) Uani 1 1 d . . .
O8 O -0.0771(8) 0.4067(6) -0.1330(8) 0.099(4) Uani 1 1 d . . .
O9 O 0.0562(8) 0.4516(7) -0.0426(9) 0.095(4) Uani 1 1 d . . .
O10 O 0.0914(12) -0.1254(9) 0.2590(14) 0.077(5) Uani 1 1 d D . .
O11 O 0.1048(10) 0.0509(9) 0.1566(15) 0.069(5) Uani 1 1 d D . .
O12 O 0.0849(10) 0.0459(8) 0.4411(12) 0.090(5) Uani 1 1 d D . .
O13 O 0.0000 -0.0108(14) 0.2500 0.069(7) Uani 1 2 d SU . .
O14 O 0.2380(12) 0.3216(8) -0.0865(19) 0.075(6) Uani 0.50 1 d P . .
O15 O 0.1290(10) 0.4320(11) -0.1761(13) 0.067(5) Uani 0.50 1 d P . .
O16 O 0.0967(18) 0.4886(15) -0.203(2) 0.068(7) Uani 0.50 1 d P . .
N1 N 0.1963(11) -0.0086(9) 0.3581(14) 0.074(6) Uani 1 1 d D . .
C1 C 0.0047(7) 0.3126(6) 0.0638(8) 0.048(3) Uani 1 1 d . . .
C2 C 0.0987(8) 0.2957(6) 0.0741(9) 0.052(3) Uani 1 1 d . . .
C3 C -0.0614(8) 0.2688(6) -0.0315(9) 0.052(3) Uani 1 1 d . . .
H3A H -0.0587 0.2849 -0.0941 0.062 Uiso 1 1 calc R . .
H3B H -0.0396 0.2235 -0.0206 0.062 Uiso 1 1 calc R . .
C4 C -0.1583(7) 0.2685(7) -0.0491(9) 0.053(3) Uani 1 1 d . . .
C5 C -0.0114(7) 0.3880(6) 0.0464(9) 0.053(3) Uani 1 1 d . . .
H5A H -0.0700 0.3977 0.0435 0.064 Uiso 1 1 calc R . .
H5B H 0.0328 0.4103 0.1072 0.064 Uiso 1 1 calc R . .
C6 C -0.0079(9) 0.4179(8) -0.0448(11) 0.075(4) Uani 1 1 d . . .
C7 C 0.2329(17) -0.0731(9) 0.3964(19) 0.19(12) Uani 1 1 d DU . .
H7A H 0.2406 -0.0773 0.4674 0.224 Uiso 1 1 calc R . .
H7B H 0.2920 -0.0763 0.3974 0.224 Uiso 1 1 calc R . .
C8 C 0.1793(14) -0.1274(10) 0.337(3) 0.10(3) Uani 1 1 d DU . .
H8A H 0.2145 -0.1483 0.3059 0.119 Uiso 1 1 calc R . .
H8B H 0.1779 -0.1586 0.3881 0.119 Uiso 1 1 calc R . .
C9 C 0.0404(11) -0.1789(11) 0.2662(19) 0.086(7) Uani 1 1 d DU . .
H9A H 0.0549 -0.2161 0.2332 0.103 Uiso 1 1 calc R . .
H9B H 0.0641 -0.1897 0.3395 0.103 Uiso 1 1 calc R . .
C10 C 0.239(2) 0.0155(11) 0.2942(19) 0.136(16) Uani 1 1 d DU . .
H10A H 0.2453 -0.0217 0.2551 0.164 Uiso 1 1 calc R . .
H10B H 0.2987 0.0305 0.3402 0.164 Uiso 1 1 calc R . .
C11 C 0.1935(12) 0.0694(13) 0.2202(15) 0.084(9) Uani 1 1 d DU . .
H11A H 0.1940 0.1096 0.2578 0.100 Uiso 1 1 calc R . .
H11B H 0.2252 0.0782 0.1779 0.100 Uiso 1 1 calc R . .
C12 C 0.0531(16) 0.1034(14) 0.101(3) 0.104(11) Uani 1 1 d DU . .
H12A H 0.0847 0.1256 0.0659 0.124 Uiso 1 1 calc R . .
H12B H 0.0470 0.1347 0.1486 0.124 Uiso 1 1 calc R . .
C13 C 0.2196(18) 0.0337(12) 0.4485(15) 0.087(9) Uani 1 1 d DU . .
H13A H 0.2310 0.0765 0.4258 0.104 Uiso 1 1 calc R . .
H13B H 0.2779 0.0175 0.4975 0.104 Uiso 1 1 calc R . .
C14 C 0.1742(11) 0.050(2) 0.5131(18) 0.114(13) Uani 1 1 d DU . .
H14A H 0.1881 0.0180 0.5689 0.136 Uiso 1 1 calc R . .
H14B H 0.1895 0.0941 0.5423 0.136 Uiso 1 1 calc R . .
C15 C 0.0318(14) 0.0866(16) 0.473(2) 0.091(9) Uani 1 1 d DU . .
H15A H 0.0254 0.0644 0.5298 0.109 Uiso 1 1 calc R . .
H15B H 0.0648 0.1273 0.5007 0.109 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'
N N 0.0061 0.0033 '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'
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 U O2 177.9(4) . . ?
O1 U O3 92.5(3) . . ?
O2 U O3 88.9(3) . . ?
O1 U O6 92.8(3) . 2 ?
O2 U O6 87.2(3) . 2 ?
O3 U O6 140.8(3) . 2 ?
O1 U O4 90.9(4) . . ?
O2 U O4 88.1(4) . . ?
O3 U O4 65.9(3) . . ?
O6 U O4 152.7(3) 2 . ?
O1 U O3 85.4(4) . 2 ?
O2 U O3 96.6(4) . 2 ?
O3 U O3 68.2(3) . 2 ?
O6 U O3 73.6(3) 2 2 ?
O4 U O3 133.7(3) . 2 ?
O1 U O7 86.5(4) . 8_556 ?
O2 U O7 91.4(3) . 8_556 ?
O3 U O7 141.0(3) . 8_556 ?
O6 U O7 78.1(3) 2 8_556 ?
O4 U O7 75.2(3) . 8_556 ?
O3 U O7 150.1(3) 2 8_556 ?
C1 O3 U 119.7(6) . . ?
C1 O3 U 128.4(6) . 2 ?
U O3 U 111.2(3) . 2 ?
C2 O4 U 121.2(8) . . ?
C4 O6 U 125.3(7) . 2 ?
C4 O7 U 129.0(8) . 8_455 ?
C8 O10 C9 111.7(10) . . ?
C12 O11 C11 112.5(11) . . ?
C14 O12 C15 109.5(10) . . ?
C7 N1 C10 107.8(10) . . ?
C7 N1 C13 106.7(9) . . ?
C10 N1 C13 110.3(19) . . ?
O3 C1 C2 109.1(9) . . ?
O3 C1 C5 108.7(10) . . ?
C2 C1 C5 109.3(10) . . ?
O3 C1 C3 111.5(10) . . ?
C2 C1 C3 104.4(10) . . ?
C5 C1 C3 113.7(9) . . ?
O4 C2 O5 123.2(11) . . ?
O4 C2 C1 117.3(11) . . ?
O5 C2 C1 119.5(10) . . ?
C4 C3 C1 115.5(10) . . ?
O6 C4 O7 124.6(11) . . ?
O6 C4 C3 121.1(10) . . ?
O7 C4 C3 114.3(12) . . ?
C6 C5 C1 118.7(11) . . ?
O9 C6 O8 119.9(14) . . ?
O9 C6 C5 124.3(12) . . ?
O8 C6 C5 115.8(13) . . ?
N1 C7 C8 114.6(12) . . ?
O10 C8 C7 127.9(18) . . ?
C9 C9 O10 124.8(14) 2 . ?
N1 C10 C11 117.8(17) . . ?
O11 C11 C10 109(2) . . ?
O11 C12 C15 115(2) . 2 ?
N1 C13 C14 133(2) . . ?
O12 C14 C13 100.9(19) . . ?
C12 C15 O12 118(3) 2 . ?
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
U O1 1.765(9) . ?
U O2 1.768(10) . ?
U O3 2.354(7) . ?
U O6 2.356(8) 2 ?
U O4 2.380(9) . ?
U O3 2.393(8) 2 ?
U O7 2.415(8) 8_556 ?
U U 3.9176(8) 2 ?
O3 C1 1.408(14) . ?
O3 U 2.393(8) 2 ?
O4 C2 1.246(14) . ?
O5 C2 1.265(15) . ?
O5 O14 2.773(19) . ?
O6 C4 1.243(15) . ?
O6 U 2.356(8) 2 ?
O7 C4 1.259(14) . ?
O7 U 2.415(8) 8_455 ?
O8 C6 1.302(16) . ?
O8 O16 2.77(3) 2_554 ?
O9 C6 1.245(17) . ?
O9 O15 2.69(2) . ?
O9 O16 2.76(3) . ?
O10 C8 1.40(4) . ?
O10 C9 1.40(3) . ?
O10 O13 2.73(3) . ?
O11 C12 1.38(4) . ?
O11 C11 1.40(3) . ?
O11 O13 2.88(2) . ?
O12 C14 1.39(3) . ?
O12 C15 1.41(3) . ?
O12 O13 2.722(19) . ?
O13 N1 2.924(17) . ?
O14 O15 2.80(3) . ?
O15 O16 1.25(3) . ?
O16 O2 2.90(3) 6_565 ?
N1 C7 1.44(3) . ?
N1 C10 1.46(4) . ?
N1 C13 1.45(3) . ?
C1 C2 1.531(16) . ?
C1 C5 1.546(17) . ?
C1 C3 1.593(16) . ?
C3 C4 1.507(17) . ?
C5 C6 1.459(18) . ?
C7 C8 1.43(4) . ?
C9 C9 1.21(3) 2 ?
C10 C11 1.48(3) . ?
C12 C15 1.38(3) 2 ?
C13 C14 1.46(4) . ?
C15 C12 1.38(3) 2 ?
