#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:54:25 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180160 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/56/7105691.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_7105691
loop_
_publ_author_name
'Victor Mougel'
'Biplab Biswas'
'Jacques Pecaut'
'Marinella Mazzanti'
_publ_section_title
;
 New insights into the acid mediated disproportionation of pentavalent
 uranyl.
;
_journal_name_full               Chem.Commun.
_journal_page_first              8648
_journal_paper_doi               10.1039/c0cc03443f
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C24 H20 N2 O6 U'
_chemical_formula_weight         670.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.493(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3216(9)
_cell_length_b                   10.0554(8)
_cell_length_c                   10.1130(8)
_cell_measurement_reflns_used    3800
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3968
_cell_measurement_theta_min      3.4824
_cell_volume                     1146.01(16)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details
;
1 omega 9.00 69.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 25.5614 37.0000 -90.0000 60

2 omega -96.00 3.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -27.4364 -77.0000 -60.0000 99

3 omega -52.00 36.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -27.4364 77.0000 60.0000 88

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6840
_diffrn_reflns_theta_full        32.52
_diffrn_reflns_theta_max         32.52
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    7.124
_exptl_absorpt_correction_T_max  0.1662
_exptl_absorpt_correction_T_min  0.0494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             636
_exptl_crystal_size_max          1.06
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.39
_refine_diff_density_max         5.148
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.375
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0582
_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)+(0.1044P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                2292
_reflns_number_total             3712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03443F.TXT
_cod_data_source_block           2
_cod_original_cell_volume        1146.00(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7105691
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C2 C 0.2078(6) -0.1215(6) 0.6301(7) 0.0346(13) Uani 1 1 d . . .
U1 U 0.0000 0.0000 0.5000 0.03180(12) Uani 1 2 d S . .
C1 C 0.4182(6) -0.1090(7) 0.7270(7) 0.0374(14) Uani 1 1 d . . .
H1 H 0.4263 -0.0300 0.6772 0.045 Uiso 1 1 calc R . .
C4 C 0.3922(7) -0.3406(8) 0.8708(8) 0.0441(16) Uani 1 1 d . . .
H4 H 0.3833 -0.4198 0.9201 0.053 Uiso 1 1 calc R . .
C5 C 0.2986(6) -0.2921(6) 0.7872(7) 0.0358(13) Uani 1 1 d . . .
H5 H 0.2251 -0.3383 0.7788 0.043 Uiso 1 1 calc R . .
O1 O 0.2143(5) -0.0082(4) 0.5771(6) 0.0395(11) Uani 1 1 d . . .
O3 O -0.0369(4) 0.0512(6) 0.6583(5) 0.0383(10) Uani 1 1 d . . .
O2 O 0.1122(4) -0.1858(5) 0.6129(6) 0.0435(12) Uani 1 1 d . . .
C9 C 0.3110(6) -0.1764(7) 0.7156(7) 0.0343(13) Uani 1 1 d . . .
N1 N 0.1113(5) 0.2246(6) 0.4909(6) 0.0380(12) Uani 1 1 d . . .
C7 C 0.5131(7) -0.1551(8) 0.8095(8) 0.0445(16) Uani 1 1 d . . .
H7 H 0.5863 -0.1082 0.8168 0.053 Uiso 1 1 calc R . .
C13 C 0.1387(8) 0.4494(8) 0.5573(8) 0.0442(16) Uani 1 1 d . . .
H13 H 0.1176 0.5212 0.6114 0.053 Uiso 1 1 calc R . .
C14 C 0.0849(7) 0.3267(7) 0.5657(7) 0.0392(14) Uani 1 1 d . . .
H14 H 0.0271 0.3151 0.6269 0.047 Uiso 1 1 calc R . .
C8 C 0.5011(7) -0.2715(8) 0.8824(8) 0.0490(18) Uani 1 1 d . . .
H8 H 0.5661 -0.3041 0.9396 0.059 Uiso 1 1 calc R . .
C10 C 0.2498(7) 0.3621(8) 0.3922(8) 0.0459(17) Uani 1 1 d . . .
H10 H 0.3062 0.3723 0.3292 0.055 Uiso 1 1 calc R . .
C11 C 0.1936(7) 0.2409(7) 0.4064(7) 0.0397(14) Uani 1 1 d . . .
H11 H 0.2144 0.1674 0.3543 0.048 Uiso 1 1 calc R . .
C15 C 0.2227(9) 0.4662(10) 0.4703(9) 0.051(2) Uani 1 1 d . . .
H15 H 0.2617 0.5494 0.4643 0.061 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
O2 C2 O1 119.3(6) . . ?
O2 C2 C9 120.4(6) . . ?
O1 C2 C9 120.3(6) . . ?
O2 C2 U1 59.8(3) . . ?
O1 C2 U1 59.9(4) . . ?
C9 C2 U1 171.9(5) . . ?
O3 U1 O3 180.0 . 3_556 ?
O3 U1 O2 87.6(2) . . ?
O3 U1 O2 92.4(2) 3_556 . ?
O3 U1 O2 92.4(2) . 3_556 ?
O3 U1 O2 87.6(2) 3_556 3_556 ?
O2 U1 O2 180.0(2) . 3_556 ?
O3 U1 O1 88.0(2) . 3_556 ?
O3 U1 O1 92.0(2) 3_556 3_556 ?
O2 U1 O1 127.87(15) . 3_556 ?
O2 U1 O1 52.13(15) 3_556 3_556 ?
O3 U1 O1 92.0(2) . . ?
O3 U1 O1 88.0(2) 3_556 . ?
O2 U1 O1 52.13(15) . . ?
O2 U1 O1 127.87(15) 3_556 . ?
O1 U1 O1 179.999(1) 3_556 . ?
O3 U1 N1 93.7(2) . 3_556 ?
O3 U1 N1 86.3(2) 3_556 3_556 ?
O2 U1 N1 63.62(17) . 3_556 ?
O2 U1 N1 116.38(17) 3_556 3_556 ?
O1 U1 N1 64.89(15) 3_556 3_556 ?
O1 U1 N1 115.11(15) . 3_556 ?
O3 U1 N1 86.3(2) . . ?
O3 U1 N1 93.7(2) 3_556 . ?
O2 U1 N1 116.38(17) . . ?
O2 U1 N1 63.62(17) 3_556 . ?
O1 U1 N1 115.11(15) 3_556 . ?
O1 U1 N1 64.89(15) . . ?
N1 U1 N1 180.0 3_556 . ?
O3 U1 C2 87.9(2) . . ?
O3 U1 C2 92.1(2) 3_556 . ?
O2 U1 C2 26.05(17) . . ?
O2 U1 C2 153.95(17) 3_556 . ?
O1 U1 C2 153.80(16) 3_556 . ?
O1 U1 C2 26.20(16) . . ?
N1 U1 C2 89.57(18) 3_556 . ?
N1 U1 C2 90.43(18) . . ?
O3 U1 C2 92.1(2) . 3_556 ?
O3 U1 C2 87.9(2) 3_556 3_556 ?
O2 U1 C2 153.95(17) . 3_556 ?
O2 U1 C2 26.05(17) 3_556 3_556 ?
O1 U1 C2 26.20(16) 3_556 3_556 ?
O1 U1 C2 153.80(16) . 3_556 ?
N1 U1 C2 90.43(18) 3_556 3_556 ?
N1 U1 C2 89.57(18) . 3_556 ?
C2 U1 C2 180.0 . 3_556 ?
C7 C1 C9 120.8(7) . . ?
C5 C4 C8 119.4(7) . . ?
C4 C5 C9 120.5(7) . . ?
C2 O1 U1 93.9(4) . . ?
C2 O2 U1 94.2(4) . . ?
C1 C9 C5 120.0(6) . . ?
C1 C9 C2 119.9(6) . . ?
C5 C9 C2 120.0(6) . . ?
C14 N1 C11 118.7(7) . . ?
C14 N1 U1 121.2(5) . . ?
C11 N1 U1 120.1(5) . . ?
C1 C7 C8 119.5(7) . . ?
C15 C13 C14 119.2(8) . . ?
N1 C14 C13 122.1(8) . . ?
C7 C8 C4 119.8(7) . . ?
C15 C10 C11 118.9(8) . . ?
N1 C11 C10 122.0(7) . . ?
C10 C15 C13 119.1(8) . . ?
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
C2 O2 1.258(8) . ?
C2 O1 1.265(7) . ?
C2 C9 1.491(9) . ?
C2 U1 2.858(7) . ?
U1 O3 1.769(5) . ?
U1 O3 1.769(5) 3_556 ?
U1 O2 2.476(5) . ?
U1 O2 2.476(5) 3_556 ?
U1 O1 2.478(5) 3_556 ?
U1 O1 2.478(5) . ?
U1 N1 2.592(6) 3_556 ?
U1 N1 2.592(6) . ?
U1 C2 2.858(7) 3_556 ?
C1 C7 1.377(10) . ?
C1 C9 1.385(9) . ?
C4 C5 1.380(10) . ?
C4 C8 1.410(11) . ?
C5 C9 1.385(9) . ?
N1 C14 1.326(9) . ?
N1 C11 1.334(9) . ?
C7 C8 1.397(11) . ?
C13 C15 1.366(13) . ?
C13 C14 1.382(11) . ?
C10 C15 1.365(12) . ?
C10 C11 1.388(10) . ?
