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#$Date: 2016-03-25 16:16:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179961 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/55/7025596.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_7025596
loop_
_publ_author_name
'Seaman, Lani A.'
'Schnaars, David D.'
'Wu, Guang'
'Hayton, Trevor W.'
_publ_section_title
;
 Isolation of a uranyl amide by "ate" complex formation.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6635
_journal_page_last               6637
_journal_paper_doi               10.1039/c001976c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C48 H76 Li2 N4 O6 U'
_chemical_formula_weight         1057.04
_chemical_name_systematic
;
Complex 2
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.047(4)
_cell_angle_beta                 92.432(4)
_cell_angle_gamma                96.819(4)
_cell_formula_units_Z            1
_cell_length_a                   9.001(3)
_cell_length_b                   11.766(4)
_cell_length_c                   12.875(4)
_cell_measurement_temperature    150(2)
_cell_volume                     1220.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10192
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    3.375
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.255
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0438P)²+0.9791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                4838
_reflns_number_total             4843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001976c.txt
_cod_data_source_block           ls_4_14m
_cod_original_cell_volume        1220.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025596
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_calc_flag
_atom_site_refinement_flags
O1 O 0.6579(3) 0.4151(2) 0.4782(2) 0.0218(5) Uani 1 1 d .
U1 U 0.5000 0.5000 0.5000 0.01732(7) Uani 1 2 d S
O3 O 0.7105(3) 0.6759(2) 0.2313(2) 0.0223(5) Uani 1 1 d .
O2 O 0.4249(3) 0.7416(3) 0.3389(2) 0.0285(6) Uani 1 1 d .
N1 N 0.3543(3) 0.3053(3) 0.4804(3) 0.0190(6) Uani 1 1 d .
H1 H 0.420(5) 0.250(4) 0.448(4) 0.023 Uiso 1 1 calc .
N2 N 0.4573(4) 0.4658(3) 0.3020(3) 0.0220(7) Uani 1 1 d .
H2 H 0.364(5) 0.488(4) 0.302(4) 0.026 Uiso 1 1 calc .
C9 C 0.4381(4) 0.3558(3) 0.1968(3) 0.0191(7) Uani 1 1 d .
C1 C 0.2216(4) 0.2387(3) 0.4076(3) 0.0200(7) Uani 1 1 d .
C6 C 0.0817(4) 0.2772(4) 0.4395(3) 0.0216(8) Uani 1 1 d .
C10 C 0.5614(4) 0.2966(4) 0.1477(3) 0.0234(8) Uani 1 1 d .
C14 C 0.2926(4) 0.3019(4) 0.1374(3) 0.0226(8) Uani 1 1 d .
C2 C 0.2260(4) 0.1329(4) 0.3019(3) 0.0232(8) Uani 1 1 d .
C5 C -0.0477(4) 0.2128(4) 0.3642(4) 0.0274(9) Uani 1 1 d .
H5 H -0.1397 0.2394 0.3850 0.033 Uiso 1 1 calc R
C21 C 0.7874(5) 0.7987(4) 0.2521(3) 0.0293(9) Uani 1 1 d .
H21A H 0.7362 0.8311 0.2049 0.035 Uiso 1 1 calc R
H21B H 0.8894 0.7921 0.2313 0.035 Uiso 1 1 calc R
C11 C 0.5392(5) 0.1882(4) 0.0454(3) 0.0291(9) Uani 1 1 d .
H11 H 0.6218 0.1507 0.0138 0.035 Uiso 1 1 calc R
C23 C 0.6861(5) 0.5897(4) 0.1107(3) 0.0269(8) Uani 1 1 d .
H23A H 0.6394 0.6304 0.0690 0.032 Uiso 1 1 calc R
H23B H 0.6171 0.5151 0.1007 0.032 Uiso 1 1 calc R
C15 C 0.1564(5) 0.3595(4) 0.1866(4) 0.0297(9) Uani 1 1 d .
H15A H 0.0676 0.3091 0.1370 0.045 Uiso 1 1 calc R
H15B H 0.1648 0.4442 0.1925 0.045 Uiso 1 1 calc R
H15C H 0.1498 0.3620 0.2618 0.045 Uiso 1 1 calc R
C16 C 0.7180(5) 0.3498(4) 0.2091(4) 0.0302(9) Uani 1 1 d .
H16A H 0.7275 0.3326 0.2754 0.045 Uiso 1 1 calc R
H16B H 0.7358 0.4399 0.2331 0.045 Uiso 1 1 calc R
H16C H 0.7904 0.3108 0.1578 0.045 Uiso 1 1 calc R
C13 C 0.2752(5) 0.1908(4) 0.0349(3) 0.0301(9) Uani 1 1 d .
H13 H 0.1794 0.1543 -0.0028 0.036 Uiso 1 1 calc R
C3 C 0.0942(5) 0.0707(4) 0.2296(4) 0.0325(10) Uani 1 1 d .
H3 H 0.0983 0.0012 0.1598 0.039 Uiso 1 1 calc R
C18 C 0.2075(5) 0.8430(4) 0.3664(4) 0.0311(9) Uani 1 1 d .
H18A H 0.2217 0.9311 0.3789 0.037 Uiso 1 1 calc R
H18B H 0.1135 0.8246 0.3943 0.037 Uiso 1 1 calc R
C8 C 0.3736(5) 0.0886(4) 0.2658(4) 0.0313(9) Uani 1 1 d .
H8A H 0.3582 0.0217 0.1889 0.047 Uiso 1 1 calc R
H8B H 0.4135 0.0577 0.3176 0.047 Uiso 1 1 calc R
H8C H 0.4432 0.1582 0.2679 0.047 Uiso 1 1 calc R
C12 C 0.3974(5) 0.1340(4) -0.0115(4) 0.0324(9) Uani 1 1 d .
H12 H 0.3843 0.0603 -0.0801 0.039 Uiso 1 1 calc R
C4 C -0.0430(5) 0.1102(4) 0.2595(4) 0.0341(10) Uani 1 1 d .
H4 H -0.1304 0.0686 0.2102 0.041 Uiso 1 1 calc R
C20 C 0.3723(5) 0.7362(5) 0.2303(4) 0.0338(10) Uani 1 1 d .
H20A H 0.3811 0.6548 0.1680 0.041 Uiso 1 1 calc R
H20B H 0.4294 0.8028 0.2164 0.041 Uiso 1 1 calc R
C17 C 0.3382(5) 0.8156(5) 0.4256(4) 0.0396(11) Uani 1 1 d .
H17A H 0.3995 0.8943 0.4788 0.048 Uiso 1 1 calc R
H17B H 0.3014 0.7694 0.4687 0.048 Uiso 1 1 calc R
C19 C 0.2090(5) 0.7548(5) 0.2396(4) 0.0396(11) Uani 1 1 d .
H19A H 0.1442 0.6748 0.2186 0.048 Uiso 1 1 calc R
H19B H 0.1771 0.7934 0.1908 0.048 Uiso 1 1 calc R
Li1 Li 0.5910(7) 0.6443(6) 0.3438(5) 0.0239(13) Uani 1 1 d .
C7 C 0.0690(4) 0.3866(4) 0.5527(3) 0.0259(8) Uani 1 1 d .
H7A H -0.0346 0.3975 0.5600 0.039 Uiso 1 1 calc R
H7B H 0.1260 0.4626 0.5559 0.039 Uiso 1 1 calc R
H7C H 0.1077 0.3697 0.6145 0.039 Uiso 1 1 calc R
C22 C 0.7904(5) 0.8878(4) 0.3768(4) 0.0324(9) Uani 1 1 d .
H22A H 0.6894 0.8979 0.3959 0.049 Uiso 1 1 calc R
H22B H 0.8460 0.9687 0.3911 0.049 Uiso 1 1 calc R
H22C H 0.8378 0.8538 0.4233 0.049 Uiso 1 1 calc R
C24 C 0.8298(5) 0.5490(5) 0.0599(4) 0.0380(10) Uani 1 1 d .
H24A H 0.8926 0.6205 0.0592 0.057 Uiso 1 1 calc R
H24B H 0.8062 0.4839 -0.0174 0.057 Uiso 1 1 calc R
H24C H 0.8820 0.5167 0.1058 0.057 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'
Li Li -0.0003 0.0001 '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
O1 U1 O1 180.000(1) 2_666 .
O1 U1 N1 94.62(12) 2_666 .
O1 U1 N1 85.38(12) . .
O1 U1 N1 85.38(12) 2_666 2_666
O1 U1 N1 94.62(12) . 2_666
N1 U1 N1 180.0 . 2_666
O1 U1 N2 84.90(11) 2_666 .
O1 U1 N2 95.10(11) . .
N1 U1 N2 97.51(11) . .
N1 U1 N2 82.49(11) 2_666 .
O1 U1 N2 95.10(11) 2_666 2_666
O1 U1 N2 84.90(11) . 2_666
N1 U1 N2 82.49(11) . 2_666
N1 U1 N2 97.51(11) 2_666 2_666
N2 U1 N2 180.000(1) . 2_666
O1 U1 Li1 83.26(15) 2_666 .
O1 U1 Li1 96.74(15) . .
N1 U1 Li1 139.09(13) . .
N1 U1 Li1 40.91(13) 2_666 .
N2 U1 Li1 41.58(14) . .
N2 U1 Li1 138.42(14) 2_666 .
O1 U1 Li1 96.74(15) 2_666 2_666
O1 U1 Li1 83.26(15) . 2_666
N1 U1 Li1 40.91(13) . 2_666
N1 U1 Li1 139.09(13) 2_666 2_666
N2 U1 Li1 138.42(14) . 2_666
N2 U1 Li1 41.58(14) 2_666 2_666
Li1 U1 Li1 180.00(17) . 2_666
C21 O3 C23 112.7(3) . .
C21 O3 Li1 123.3(3) . .
C23 O3 Li1 120.9(3) . .
C17 O2 C20 109.6(3) . .
C17 O2 Li1 132.0(3) . .
C20 O2 Li1 118.4(3) . .
C1 N1 Li1 130.6(3) . 2_666
C1 N1 U1 128.2(2) . .
Li1 N1 U1 90.5(2) 2_666 .
C9 N2 Li1 128.2(3) . .
C9 N2 U1 132.7(2) . .
Li1 N2 U1 89.7(2) . .
N2 C9 C10 121.5(3) . .
N2 C9 C14 120.2(3) . .
C10 C9 C14 118.3(3) . .
N1 C1 C6 120.2(3) . .
N1 C1 C2 120.9(3) . .
C6 C1 C2 118.8(3) . .
C5 C6 C1 119.3(4) . .
C5 C6 C7 119.3(4) . .
C1 C6 C7 121.4(3) . .
C11 C10 C9 120.3(4) . .
C11 C10 C16 119.7(4) . .
C9 C10 C16 120.0(3) . .
C13 C14 C9 119.4(4) . .
C13 C14 C15 119.8(4) . .
C9 C14 C15 120.7(3) . .
C3 C2 C1 120.0(4) . .
C3 C2 C8 119.8(4) . .
C1 C2 C8 120.1(3) . .
C4 C5 C6 121.8(4) . .
O3 C21 C22 109.7(3) . .
C10 C11 C12 121.6(4) . .
O3 C23 C24 112.8(3) . .
C12 C13 C14 121.3(4) . .
C4 C3 C2 121.2(4) . .
C17 C18 C19 103.9(3) . .
C13 C12 C11 119.0(4) . .
C5 C4 C3 118.8(4) . .
O2 C20 C19 105.1(3) . .
O2 C17 C18 107.8(3) . .
C20 C19 C18 103.1(3) . .
O3 Li1 O2 98.0(3) . .
O3 Li1 N1 130.5(3) . 2_666
O2 Li1 N1 105.1(3) . 2_666
O3 Li1 N2 122.0(3) . .
O2 Li1 N2 98.2(3) . .
N1 Li1 N2 97.3(3) 2_666 .
O3 Li1 U1 153.7(3) . .
O2 Li1 U1 107.5(3) . .
N1 Li1 U1 48.60(16) 2_666 .
N2 Li1 U1 48.73(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 U1 1.797(3) .
U1 O1 1.797(3) 2_666
U1 N1 2.408(3) .
U1 N1 2.408(3) 2_666
U1 N2 2.413(3) .
U1 N2 2.413(3) 2_666
U1 Li1 3.210(7) .
U1 Li1 3.210(7) 2_666
O3 C21 1.435(5) .
O3 C23 1.439(4) .
O3 Li1 1.970(7) .
O2 C17 1.423(5) .
O2 C20 1.431(5) .
O2 Li1 2.002(7) .
N1 C1 1.407(4) .
N1 Li1 2.102(7) 2_666
N2 C9 1.407(5) .
N2 Li1 2.131(7) .
C9 C10 1.409(5) .
C9 C14 1.418(5) .
C1 C6 1.408(5) .
C1 C2 1.409(5) .
C6 C5 1.394(5) .
C6 C7 1.501(5) .
C10 C11 1.377(6) .
C10 C16 1.510(5) .
C14 C13 1.396(6) .
C14 C15 1.505(6) .
C2 C3 1.390(6) .
C2 C8 1.505(6) .
C5 C4 1.384(6) .
C21 C22 1.497(6) .
C11 C12 1.380(6) .
C23 C24 1.511(6) .
C13 C12 1.380(6) .
C3 C4 1.384(7) .
C18 C17 1.514(6) .
C18 C19 1.520(6) .
C20 C19 1.513(6) .
Li1 N1 2.102(7) 2_666
