#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/19/8101910.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_8101910
loop_
_publ_author_name
'Bekaert, A.'
'Lemoine, P.'
'Brion, J. D.'
'Viossat, B.'
_publ_section_title
;
Crystal structure of bis(acetato-O,O')bis(μ-acetato-O,O')bis
(k³N-antipyrine-O]tetraoxodiuranium, U₂O₄(CH₃COO)₄[C₆H₅N₂C₃
(CH₃)₂HO]₂
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              45
_journal_page_last               46
_journal_volume                  221
_journal_year                    2006
_chemical_formula_structural     U2(O)4(CH3COO)4[C6H5N2C3(CH3)2HO]2
_chemical_formula_sum            'C30 H36 N4 O14 U2'
_chemical_formula_weight         1152.68
_chemical_name_systematic
;
bis[acetato-O,O']bis(μ-acetato-O,O')bis(\kN³-antipyrine-O]dioxouranium
;
_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                112.94(5)
_cell_angle_beta                 92.84(7)
_cell_angle_gamma                110.61(8)
_cell_formula_units_Z            1
_cell_length_a                   8.989(9)
_cell_length_b                   9.709(3)
_cell_length_c                   12.220(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.25
_cell_measurement_theta_min      7.87
_cell_volume                     897.5(14)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994) [7] '
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994) [7] '
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995) [8] '
_computing_molecular_graphics    'CAMERON [11]'
_computing_publication_material  'WinGX - Version 1.63.02 [12]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997) [10] '
_computing_structure_solution    'SIR92 [9]'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega/2theta
_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    0.0525
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3158
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  1
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.081
_exptl_absorpt_correction_T_max  0.1625
_exptl_absorpt_correction_T_min  0.0370
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'DIFABS - Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_density_meas      2.12(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.725
_refine_diff_density_min         -2.613
_refine_diff_density_rms         0.245
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0429
_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)+(0.0940P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                2816
_reflns_number_total             3158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1703.cff
_cod_data_source_block           bv93
_cod_original_cell_volume        897.5(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101910
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.54691(3) -0.07508(3) 0.25979(2) 0.03998(15) Uani 1 2 i d . . .
O1 O 0.4917(12) 0.0713(9) 0.2380(7) 0.067(2) Uani 1 2 i d . . .
O2 O 0.5975(12) -0.2230(10) 0.2782(8) 0.069(2) Uani 1 2 i d . . .
O3 O 0.5462(9) -0.2033(10) 0.0438(6) 0.067(2) Uani 1 2 i d . . .
O4 O 0.3172(9) -0.2954(9) 0.0940(6) 0.0601(16) Uani 1 2 i d . . .
C5 C 0.3983(13) -0.2956(12) 0.0135(9) 0.052(2) Uani 1 2 i d . . .
C6 C 0.3139(16) -0.4077(15) -0.1183(9) 0.072(3) Uani 1 2 i d . . .
H6A H 0.3909 -0.3951 -0.1690 0.107 Uiso 1 2 i calc R . .
H6B H 0.2277 -0.3803 -0.1401 0.107 Uiso 1 2 i calc R . .
H6C H 0.2694 -0.5190 -0.1294 0.107 Uiso 1 2 i calc R . .
O7 O 0.6554(9) 0.1054(9) 0.4654(6) 0.0574(17) Uani 1 2 i d . . .
O8 O 0.6805(9) 0.1411(11) 0.6536(6) 0.078(3) Uani 1 2 i d . . .
C9 C 0.7367(12) 0.1356(11) 0.5634(8) 0.052(2) Uani 1 2 i d . . .
C10 C 0.9158(14) 0.1670(19) 0.5741(13) 0.081(4) Uani 1 2 i d . . .
H10A H 0.9620 0.1893 0.6548 0.122 Uiso 1 2 i calc R . .
H10B H 0.9718 0.2593 0.5581 0.122 Uiso 1 2 i calc R . .
H10C H 0.9270 0.0723 0.5160 0.122 Uiso 1 2 i calc R . .
C11 C 0.9782(11) 0.1981(11) 0.0371(8) 0.0490(19) Uani 1 2 i d . . .
N12 N 1.0936(9) 0.2784(10) 0.1346(6) 0.0483(16) Uani 1 2 i d . . .
N13 N 1.0387(9) 0.2301(10) 0.2211(7) 0.0494(16) Uani 1 2 i d . . .
O14 O 0.8081(8) 0.0618(10) 0.2449(6) 0.0631(18) Uani 1 2 i d . . .
C14 C 0.8840(11) 0.1221(11) 0.1794(8) 0.0488(19) Uani 1 2 i d . . .
C15 C 0.8427(12) 0.0979(12) 0.0581(9) 0.053(2) Uani 1 2 i d . . .
H15 H 0.7434 0.0280 0.0034 0.064 Uiso 1 2 i calc R . .
C16 C 0.9980(15) 0.2223(14) -0.0777(8) 0.062(2) Uani 1 2 i d . . .
H16A H 0.8989 0.1530 -0.1386 0.092 Uiso 1 2 i calc R . .
H16B H 1.0854 0.1947 -0.1076 0.092 Uiso 1 2 i calc R . .
H16C H 1.0224 0.3344 -0.0596 0.092 Uiso 1 2 i calc R . .
C17 C 1.2605(14) 0.3913(19) 0.1549(12) 0.083(4) Uani 1 2 i d . . .
H17A H 1.3156 0.4291 0.2370 0.124 Uiso 1 2 i calc R . .
H17B H 1.2611 0.4827 0.1418 0.124 Uiso 1 2 i calc R . .
H17C H 1.3152 0.3366 0.0993 0.124 Uiso 1 2 i calc R . .
C18 C 1.1411(10) 0.3003(11) 0.3436(7) 0.0433(17) Uani 1 2 i d . . .
C19 C 1.2253(12) 0.2142(11) 0.3634(9) 0.053(2) Uani 1 2 i d . . .
H19 H 1.2163 0.1152 0.3026 0.064 Uiso 1 2 i calc R . .
C20 C 1.3243(14) 0.2828(15) 0.4785(10) 0.064(3) Uani 1 2 i d . . .
H20 H 1.3802 0.2266 0.4955 0.076 Uiso 1 2 i calc R . .
C21 C 1.3409(14) 0.4253(15) 0.5639(9) 0.064(3) Uani 1 2 i d . . .
H21 H 1.4100 0.4690 0.6391 0.077 Uiso 1 2 i calc R . .
C22 C 1.2580(16) 0.5093(14) 0.5434(11) 0.081(4) Uani 1 2 i d . . .
H22 H 1.2689 0.6084 0.6051 0.097 Uiso 1 2 i calc R . .
C23 C 1.1545(13) 0.4458(12) 0.4278(9) 0.058(2) Uani 1 2 i d . . .
H23 H 1.0988 0.5026 0.4113 0.069 Uiso 1 2 i 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'
U U -9.6767 9.6646 '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'
H H 0.0000 0.0000 '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
O2 U1 O1 178.6(3) . . ?
O2 U1 O14 92.1(4) . . ?
O1 U1 O14 88.7(4) . . ?
O2 U1 O8 90.8(4) . 2_656 ?
O1 U1 O8 88.9(4) . 2_656 ?
O14 U1 O8 159.5(3) . 2_656 ?
O2 U1 O7 91.5(3) . . ?
O1 U1 O7 89.7(3) . . ?
O14 U1 O7 81.5(3) . . ?
O8 U1 O7 78.1(3) 2_656 . ?
O2 U1 O3 88.9(4) . . ?
O1 U1 O3 90.1(3) . . ?
O14 U1 O3 75.3(3) . . ?
O8 U1 O3 125.0(3) 2_656 . ?
O7 U1 O3 156.8(3) . . ?
O2 U1 O4 88.7(3) . . ?
O1 U1 O4 89.9(3) . . ?
O14 U1 O4 127.7(2) . . ?
O8 U1 O4 72.7(3) 2_656 . ?
O7 U1 O4 150.8(3) . . ?
O3 U1 O4 52.4(2) . . ?
O2 U1 C5 89.5(3) . . ?
O1 U1 C5 89.2(3) . . ?
O14 U1 C5 101.4(3) . . ?
O8 U1 C5 98.9(3) 2_656 . ?
O7 U1 C5 176.8(2) . . ?
O3 U1 C5 26.1(3) . . ?
O4 U1 C5 26.3(3) . . ?
O2 U1 U1 82.9(3) . 2_656 ?
O1 U1 U1 97.8(3) . 2_656 ?
O14 U1 U1 115.10(19) . 2_656 ?
O8 U1 U1 45.25(19) 2_656 2_656 ?
O7 U1 U1 34.51(19) . 2_656 ?
O3 U1 U1 166.84(19) . 2_656 ?
O4 U1 U1 116.87(17) . 2_656 ?
C5 U1 U1 142.8(2) . 2_656 ?
C5 O3 U1 94.5(6) . . ?
C5 O4 U1 93.5(6) . . ?
O4 C5 O3 119.4(9) . . ?
O4 C5 C6 118.9(10) . . ?
O3 C5 C6 121.7(9) . . ?
O4 C5 U1 60.2(5) . . ?
O3 C5 U1 59.3(5) . . ?
C6 C5 U1 176.8(8) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C9 O7 U1 146.9(7) . . ?
C9 O8 U1 149.4(7) . 2_656 ?
O8 C9 O7 123.8(10) . . ?
O8 C9 C10 117.1(10) . . ?
O7 C9 C10 119.1(9) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N12 C11 C15 109.5(8) . . ?
N12 C11 C16 122.5(9) . . ?
C15 C11 C16 128.0(9) . . ?
C11 N12 N13 108.4(7) . . ?
C11 N12 C17 129.9(8) . . ?
N13 N12 C17 121.5(8) . . ?
C14 N13 N12 110.1(7) . . ?
C14 N13 C18 128.0(7) . . ?
N12 N13 C18 121.8(7) . . ?
C14 O14 U1 141.4(6) . . ?
O14 C14 N13 120.9(8) . . ?
O14 C14 C15 133.6(9) . . ?
N13 C14 C15 105.5(8) . . ?
C11 C15 C14 106.4(9) . . ?
C11 C15 H15 126.8 . . ?
C14 C15 H15 126.8 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N12 C17 H17A 109.5 . . ?
N12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 123.3(8) . . ?
C23 C18 N13 119.4(8) . . ?
C19 C18 N13 117.2(8) . . ?
C18 C19 C20 116.9(9) . . ?
C18 C19 H19 121.5 . . ?
C20 C19 H19 121.5 . . ?
C21 C20 C19 121.7(9) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C20 C21 C22 120.8(10) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C23 120.2(9) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C18 C23 C22 116.9(9) . . ?
C18 C23 H23 121.5 . . ?
C22 C23 H23 121.5 . . ?
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 O2 1.738(7) . ?
U1 O1 1.765(8) . ?
U1 O14 2.312(7) . ?
U1 O8 2.352(7) 2_656 ?
U1 O7 2.336(7) . ?
U1 O3 2.439(7) . ?
U1 O4 2.458(8) . ?
U1 C5 2.827(10) . ?
U1 U1 5.656(5) 2_656 ?
O3 C5 1.249(13) . ?
O4 C5 1.253(12) . ?
C5 C6 1.512(14) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
O7 C9 1.242(11) . ?
O8 C9 1.225(11) . ?
O8 U1 2.352(7) 2_656 ?
C9 C10 1.519(14) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N12 1.300(12) . ?
C11 C15 1.373(13) . ?
C11 C16 1.520(13) . ?
N12 N13 1.362(10) . ?
N12 C17 1.452(14) . ?
N13 C14 1.334(12) . ?
N13 C18 1.476(11) . ?
O14 C14 1.261(12) . ?
C14 C15 1.415(13) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C23 1.343(13) . ?
C18 C19 1.384(12) . ?
C19 C20 1.394(14) . ?
C19 H19 0.9300 . ?
C20 C21 1.320(16) . ?
C20 H20 0.9300 . ?
C21 C22 1.360(17) . ?
C21 H21 0.9300 . ?
C22 C23 1.424(16) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O7 C9 O8 -114.3(13) . . . . ?
U1 O7 C9 C10 65.3(16) . . . . ?
