#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:46:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179708 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/11/7001174.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_7001174
loop_
_publ_author_name
'Berthet, Jean-Claude'
'Siffredi, Gérald'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Synthesis and crystal structure of pentavalent uranyl complexes. The
 remarkable stability of UO2X (X = I, SO3CF3) in non-aqueous solutions
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3478
_journal_page_last               3494
_journal_paper_doi               10.1039/b820659g
_journal_year                    2009
_chemical_formula_moiety         'C21 H20 F3 N4 O5 S U'
_chemical_formula_sum            'C21 H20 F3 N4 O5 S U'
_chemical_formula_weight         735.50
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.720(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2614(8)
_cell_length_b                   12.2270(10)
_cell_length_c                   15.2571(10)
_cell_measurement_reflns_used    40910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.28
_cell_volume                     2445.3(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40910
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.785
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.483
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.00097(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2317
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0357
_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)+(0.0456P)²+25.2918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                1801
_reflns_number_total             2317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820659g.txt
_cod_data_source_block           19
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7001174
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 0.0000 0.99700(3) 0.7500 0.02845(18) Uani 1 2 d S . .
S1 S 0.0424(3) 0.6962(3) 0.7258(2) 0.0296(8) Uani 0.50 1 d PD . .
O1 O 0.0873(4) 1.0005(5) 0.6679(4) 0.0412(14) Uani 1 1 d . . .
O2 O 0.0000 0.7905(6) 0.7500 0.046(2) Uani 1 2 d S . .
O3 O 0.0353(9) 0.6841(11) 0.6313(7) 0.043(3) Uani 0.50 1 d P . .
O4 O 0.1412(8) 0.6793(10) 0.7787(7) 0.038(3) Uani 0.50 1 d P . .
F1 F 0.0000 0.4862(5) 0.7500 0.059(2) Uani 1 2 d S . .
F2 F -0.1282(7) 0.5849(8) 0.7117(6) 0.042(2) Uani 0.50 1 d P . .
F3 F -0.0423(7) 0.5866(8) 0.8439(6) 0.043(2) Uani 0.50 1 d P . .
N1 N 0.1526(5) 0.9413(5) 0.8700(4) 0.0326(14) Uani 1 1 d . . .
C1 C 0.2465(8) 0.9342(11) 0.8517(7) 0.069(3) Uani 1 1 d U . .
H1 H 0.2574 0.9480 0.7939 0.082 Uiso 1 1 calc R . .
C2 C 0.3295(8) 0.9075(11) 0.9141(7) 0.073(3) Uani 1 1 d U . .
H2 H 0.3941 0.9025 0.8976 0.087 Uiso 1 1 calc R . .
C3 C 0.3169(6) 0.8884(7) 1.0000(6) 0.044(2) Uani 1 1 d . . .
H3 H 0.3716 0.8706 1.0432 0.053 Uiso 1 1 calc R . .
C4 C 0.2200(7) 0.8965(8) 1.0193(6) 0.049(2) Uani 1 1 d . . .
H4 H 0.2072 0.8855 1.0769 0.059 Uiso 1 1 calc R . .
C5 C 0.1419(6) 0.9212(8) 0.9527(6) 0.046(2) Uani 1 1 d . . .
H5 H 0.0763 0.9239 0.9672 0.055 Uiso 1 1 calc R . .
N2 N 0.0860(4) 1.1695(4) 0.8265(4) 0.0476(19) Uani 1 1 d G . .
C6 C 0.1748(5) 1.2111(6) 0.8012(4) 0.069(3) Uani 1 1 d GU . .
H6 H 0.1991 1.1827 0.7518 0.082 Uiso 1 1 calc R . .
C7 C 0.2274(5) 1.2951(6) 0.8497(7) 0.107(5) Uani 1 1 d GU . .
H7 H 0.2868 1.3229 0.8328 0.129 Uiso 1 1 calc R . .
C8 C 0.1911(7) 1.3375(5) 0.9235(7) 0.121(5) Uani 1 1 d GU . .
H8 H 0.2262 1.3937 0.9560 0.146 Uiso 1 1 calc R . .
C9 C 0.1023(7) 1.2959(7) 0.9488(5) 0.116(5) Uani 1 1 d GU . .
H9 H 0.0780 1.3243 0.9981 0.139 Uiso 1 1 calc R . .
C10 C 0.0497(5) 1.2119(6) 0.9002(4) 0.071(3) Uani 1 1 d GU . .
H10 H -0.0097 1.1841 0.9171 0.085 Uiso 1 1 calc R . .
C11 C -0.0326(10) 0.5851(11) 0.7562(10) 0.035(4) Uani 0.50 1 d PD . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 O1 177.3(3) . 2_556 ?
O1 U O2 91.34(17) . . ?
O1 U O2 91.34(17) 2_556 . ?
O1 U N2 90.5(2) . . ?
O1 U N2 87.4(2) 2_556 . ?
O2 U N2 144.52(12) . . ?
O1 U N2 87.4(2) . 2_556 ?
O1 U N2 90.5(2) 2_556 2_556 ?
O2 U N2 144.52(12) . 2_556 ?
N2 U N2 71.0(2) . 2_556 ?
O1 U N1 91.7(2) . 2_556 ?
O1 U N1 89.0(2) 2_556 2_556 ?
O2 U N1 74.85(14) . 2_556 ?
N2 U N1 140.50(18) . 2_556 ?
N2 U N1 69.76(19) 2_556 2_556 ?
O1 U N1 89.0(2) . . ?
O1 U N1 91.7(2) 2_556 . ?
O2 U N1 74.85(14) . . ?
N2 U N1 69.76(19) . . ?
N2 U N1 140.50(18) 2_556 . ?
N1 U N1 149.7(3) 2_556 . ?
O2 S1 O3 113.1(6) . . ?
O2 S1 O4 110.3(5) . . ?
O3 S1 O4 117.5(7) . . ?
O2 S1 C11 107.8(6) . . ?
O3 S1 C11 103.1(7) . . ?
O4 S1 C11 103.9(7) . . ?
S1 O2 U 148.1(2) . . ?
C5 N1 C1 115.7(8) . . ?
C5 N1 U 122.6(5) . . ?
C1 N1 U 121.8(6) . . ?
N1 C1 C2 123.3(10) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 120.0(10) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 116.8(8) . . ?
C4 C3 H3 121.6 . . ?
C2 C3 H3 121.6 . . ?
C3 C4 C5 119.2(8) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 124.9(8) . . ?
N1 C5 H5 117.5 . . ?
C4 C5 H5 117.5 . . ?
C6 N2 C10 120.0 . . ?
C6 N2 U 120.5(3) . . ?
C10 N2 U 119.1(4) . . ?
N2 C6 C7 120.0 . . ?
N2 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 N2 120.0 . . ?
C9 C10 H10 120.0 . . ?
N2 C10 H10 120.0 . . ?
F1 C11 F2 105.2(10) . . ?
F1 C11 F3 99.6(10) . . ?
F2 C11 F3 105.8(11) . . ?
F1 C11 S1 119.2(9) . . ?
F2 C11 S1 112.9(9) . . ?
F3 C11 S1 112.5(9) . . ?
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 1.831(6) . ?
U O1 1.831(6) 2_556 ?
U O2 2.525(8) . ?
U N2 2.590(5) . ?
U N2 2.590(4) 2_556 ?
U N1 2.605(6) 2_556 ?
U N1 2.605(6) . ?
S1 O2 1.359(7) . ?
S1 O3 1.437(11) . ?
S1 O4 1.446(11) . ?
S1 C11 1.786(9) . ?
F1 C11 1.292(15) . ?
F2 C11 1.345(16) . ?
F3 C11 1.364(17) . ?
N1 C5 1.316(10) . ?
N1 C1 1.321(11) . ?
C1 C2 1.381(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.367(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.364(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(11) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
N2 C6 1.3900 . ?
N2 C10 1.3900 . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
