#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/87/2228791.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_2228791
loop_
_publ_author_name
'Suzuki, Tomoya'
'Kawasaki, Takeshi'
'Ikeda, Yasuhisa'
_publ_section_title
;
 Bis(1,3-dimethyl-1,3-diazinan-2-one)dinitratodioxidouranium(VI)
;
_journal_coeditor_code           KJ2159
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m18
_journal_paper_doi               10.1107/S1600536810049883
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[U (N O3)2 O2 (C6 H12 N2 O)2]'
_chemical_formula_moiety         'C12 H24 N6 O10 U'
_chemical_formula_sum            'C12 H24 N6 O10 U'
_chemical_formula_weight         650.40
_chemical_name_systematic
;
Bis(1,3-dimethyl-1,3-diazinan-2-one)dinitratodioxidouranium(VI)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                115.611(2)
_cell_angle_beta                 113.348(2)
_cell_angle_gamma                91.041(2)
_cell_formula_units_Z            1
_cell_length_a                   7.8529(6)
_cell_length_b                   8.7706(6)
_cell_length_c                   9.1990(6)
_cell_measurement_reflns_used    6036
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.5
_cell_volume                     510.62(6)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2006)'
_computing_molecular_graphics    'CrystalMaker (CrystalMaker, 2007)'
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4800
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    8.009
_exptl_absorpt_correction_T_max  0.4466
_exptl_absorpt_correction_T_min  0.3430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.933
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0173
_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)+(0.0297P)²+0.4772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0445
_reflns_number_gt                2306
_reflns_number_total             2307
_reflns_threshold_expression     F²>2σ(F²)
_cod_data_source_file            kj2159.cif
_cod_data_source_block           I
_cod_database_code               2228791
_cod_database_fobs_code          2228791
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 U1 1.0000 0.0000 1.0000 0.02201(6) Uani d S 1 . .
O O1 1.1934(3) 0.1523(3) 1.0498(3) 0.0299(4) Uani d . 1 . .
O O2 0.7867(3) 0.0427(3) 0.7614(3) 0.0285(4) Uani d . 1 . .
O O3 1.0044(4) -0.1789(3) 0.6978(3) 0.0372(5) Uani d . 1 . .
O O4 1.1569(4) -0.2495(3) 0.9034(3) 0.0356(5) Uani d . 1 . .
O O5 1.1808(5) -0.3669(4) 0.6514(4) 0.0516(7) Uani d . 1 . .
N N1 1.1165(4) -0.2698(4) 0.7464(4) 0.0316(5) Uani d . 1 . .
N N2 0.7882(4) 0.2759(4) 0.7144(4) 0.0289(5) Uani d . 1 A .
N N3 0.5257(4) 0.1594(4) 0.7234(4) 0.0304(5) Uani d . 1 A .
C C1 0.7028(4) 0.1579(4) 0.7359(4) 0.0237(5) Uani d . 1 . .
C C2 0.7065(6) 0.4189(5) 0.6969(6) 0.0399(8) Uani d . 1 . .
H H2A 0.7498 0.4518 0.6248 0.048 Uiso calc PR 0.786(11) A 1
H H2B 0.7526 0.5210 0.8181 0.048 Uiso calc PR 0.786(11) A 1
H H2C 0.6480 0.3901 0.5684 0.048 Uiso calc PR 0.214(11) A 2
H H2D 0.8101 0.5246 0.7649 0.048 Uiso calc PR 0.214(11) A 2
C C3 0.4952(7) 0.3703(7) 0.6089(7) 0.0409(13) Uani d P 0.786(11) A 1
H H3A 0.4478 0.2848 0.4799 0.049 Uiso calc PR 0.786(11) A 1
H H3B 0.4444 0.4745 0.6165 0.049 Uiso calc PR 0.786(11) A 1
C C3B 0.558(2) 0.457(2) 0.765(2) 0.036(5) Uani d P 0.214(11) A 2
H H3C 0.6209 0.5204 0.8989 0.044 Uiso calc PR 0.214(11) A 2
H H3D 0.4844 0.5326 0.7225 0.044 Uiso calc PR 0.214(11) A 2
C C4 0.4252(5) 0.2925(6) 0.6999(6) 0.0429(8) Uani d . 1 . .
H H4A 0.4452 0.3857 0.8192 0.052 Uiso calc PR 0.786(11) A 1
H H4B 0.2868 0.2402 0.6258 0.052 Uiso calc PR 0.786(11) A 1
H H4C 0.3474 0.3176 0.7664 0.052 Uiso calc PR 0.214(11) A 2
H H4D 0.3375 0.2468 0.5705 0.052 Uiso calc PR 0.214(11) A 2
C C5 0.9791(5) 0.2755(6) 0.7260(5) 0.0398(8) Uani d . 1 . .
H H5A 1.0191 0.3695 0.7076 0.048 Uiso calc R 1 A .
H H5B 0.9778 0.1639 0.6328 0.048 Uiso calc R 1 . .
H H5C 1.0684 0.2928 0.8452 0.048 Uiso calc R 1 . .
C C6 0.4370(5) 0.0441(6) 0.7625(5) 0.0417(8) Uani d . 1 . .
H H6A 0.3096 0.0628 0.7468 0.050 Uiso calc R 1 A .
H H6B 0.5152 0.0687 0.8871 0.050 Uiso calc R 1 . .
H H6C 0.4266 -0.0769 0.6799 0.050 Uiso calc R 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O1 . 2_757 180 y
O1 U1 O2 . 2_757 87.26(9) ?
O1 U1 O2 2_757 2_757 92.74(9) ?
O1 U1 O2 . . 92.74(9) y
O1 U1 O2 2_757 . 87.26(9) ?
O2 U1 O2 2_757 . 180 ?
O1 U1 O4 . . 92.17(9) y
O1 U1 O4 2_757 . 87.83(10) ?
O2 U1 O4 2_757 . 65.69(8) ?
O2 U1 O4 . . 114.31(8) ?
O1 U1 O4 . 2_757 87.83(10) ?
O1 U1 O4 2_757 2_757 92.17(10) ?
O2 U1 O4 2_757 2_757 114.31(8) ?
O2 U1 O4 . 2_757 65.69(8) y
O4 U1 O4 . 2_757 180 ?
O1 U1 O3 . . 86.07(10) y
O1 U1 O3 2_757 . 93.93(10) ?
O2 U1 O3 2_757 . 115.08(7) ?
O2 U1 O3 . . 64.92(7) y
O4 U1 O3 . . 50.20(8) y
O4 U1 O3 2_757 . 129.80(8) ?
O1 U1 O3 . 2_757 93.93(10) ?
O1 U1 O3 2_757 2_757 86.07(10) ?
O2 U1 O3 2_757 2_757 64.92(7) ?
O2 U1 O3 . 2_757 115.08(7) ?
O4 U1 O3 . 2_757 129.80(8) ?
O4 U1 O3 2_757 2_757 50.20(8) ?
O3 U1 O3 . 2_757 180 ?
C1 O2 U1 . . 139.9(2) y
N1 O3 U1 . . 96.59(18) ?
N1 O4 U1 . . 97.71(17) ?
O5 N1 O4 . . 122.5(3) ?
O5 N1 O3 . . 122.6(3) ?
O4 N1 O3 . . 114.9(3) ?
C1 N2 C5 . . 120.3(3) ?
C1 N2 C2 . . 122.8(3) ?
C5 N2 C2 . . 116.5(3) ?
C1 N3 C6 . . 120.6(3) ?
C1 N3 C4 . . 122.8(3) ?
C6 N3 C4 . . 115.9(3) ?
O2 C1 N2 . . 119.8(3) ?
O2 C1 N3 . . 120.7(3) ?
N2 C1 N3 . . 119.5(3) ?
N2 C2 C3 . . 111.4(3) ?
N2 C2 C3B . . 113.2(7) ?
N2 C2 H2A . . 109.3 ?
C3 C2 H2A . . 109.3 ?
N2 C2 H2B . . 109.3 ?
C3 C2 H2B . . 109.3 ?
H2A C2 H2B . . 108.0 ?
N2 C2 H2C . . 108.9 ?
C3B C2 H2C . . 108.9 ?
N2 C2 H2D . . 108.9 ?
C3B C2 H2D . . 108.9 ?
H2C C2 H2D . . 107.7 ?
C2 C3 C4 . . 110.5(4) ?
C2 C3 H3A . . 109.6 ?
C4 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
C4 C3 H3B . . 109.6 ?
H3A C3 H3B . . 108.1 ?
C4 C3B C2 . . 110.3(9) ?
C4 C3B H3C . . 109.6 ?
C2 C3B H3C . . 109.6 ?
C4 C3B H3D . . 109.6 ?
C2 C3B H3D . . 109.6 ?
H3C C3B H3D . . 108.1 ?
N3 C4 C3B . . 112.7(7) ?
N3 C4 C3 . . 111.4(3) ?
C3B C4 C3 . . 45.7(7) ?
N3 C4 H4A . . 109.4 ?
C3 C4 H4A . . 109.4 ?
N3 C4 H4B . . 109.4 ?
C3 C4 H4B . . 109.4 ?
H4A C4 H4B . . 108.0 ?
N3 C4 H4C . . 109.1 ?
C3B C4 H4C . . 109.1 ?
N3 C4 H4D . . 109.1 ?
C3B C4 H4D . . 109.1 ?
H4C C4 H4D . . 107.8 ?
N2 C5 H5A . . 109.5 ?
N2 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
N2 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
N3 C6 H6A . . 109.5 ?
N3 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
N3 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.774(2) y
U1 O1 2_757 1.774(2) ?
U1 O2 2_757 2.363(2) ?
U1 O2 . 2.363(2) y
U1 O4 . 2.526(2) y
U1 O4 2_757 2.526(2) ?
U1 O3 . 2.549(2) y
U1 O3 2_757 2.549(2) ?
O2 C1 . 1.271(4) y
O3 N1 . 1.277(4) ?
O4 N1 . 1.277(4) ?
O5 N1 . 1.211(4) ?
N2 C1 . 1.348(4) ?
N2 C5 . 1.460(4) ?
N2 C2 . 1.460(4) ?
N3 C1 . 1.350(4) ?
N3 C6 . 1.458(4) ?
N3 C4 . 1.466(4) ?
C2 C3 . 1.484(6) ?
C2 C3B . 1.514(15) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C2 H2C . 0.9900 ?
C2 H2D . 0.9900 ?
C3 C4 . 1.521(6) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3B C4 . 1.494(16) ?
C3B H3C . 0.9900 ?
C3B H3D . 0.9900 ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C4 H4C . 0.9900 ?
C4 H4D . 0.9900 ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 H5C . 0.9800 ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
