#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/37/7103743.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_7103743
loop_
_publ_author_name
'Jean-Claude Berthet'
'Michel Ephritikhine'
'Martine Nierlich'
_publ_section_title
;
A novel coordination geometry for the uranyl ion. 
Rhombohedral uranium environment in [UO2(OTf)2(bpy)2] and [UO2(phen)3][OTf]2
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b303255h
_journal_year                    2003
_chemical_formula_sum            'C22 H16 F6 N4 O8 S2 U'
_chemical_formula_weight         880.54
_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                102.13(3)
_cell_angle_beta                 92.66(3)
_cell_angle_gamma                102.87(3)
_cell_formula_units_Z            1
_cell_length_a                   6.0290(12)
_cell_length_b                   10.031(2)
_cell_length_c                   11.462(2)
_cell_measurement_reflns_used    4085
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     657.5(2)
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997)'
_computing_data_collection       'DENZO(Otwinowski& Minor,1997)'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick,1997)'
_computing_publication_material  'SHELXTL (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device       'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       'φ rotation 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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4085
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         3.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.429
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'MULABS in PLATON;Spek,1998'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.432
_refine_diff_density_min         -2.503
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0248
_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)+(0.0536P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                2015
_reflns_number_total             2016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303255h.txt
_cod_data_source_block           2jc
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7103743
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.0000 0.0000 0.0000 0.01439(11) Uani 1 2 d S . .
S S -0.01382(19) -0.26123(11) -0.27018(9) 0.0176(2) Uani 1 1 d . . .
F1 F -0.1756(6) -0.4296(3) -0.4770(3) 0.0376(8) Uani 1 1 d . . .
F2 F -0.3148(6) -0.2489(3) -0.4377(3) 0.0374(7) Uani 1 1 d . . .
F3 F -0.4249(6) -0.4172(4) -0.3480(3) 0.0427(8) Uani 1 1 d . . .
O1 O -0.2539(5) 0.0502(3) 0.0353(3) 0.0172(6) Uani 1 1 d . . .
O2 O -0.1380(6) -0.1861(3) -0.1808(3) 0.0191(7) Uani 1 1 d . . .
O3 O 0.0518(6) -0.3778(4) -0.2357(3) 0.0281(8) Uani 1 1 d . . .
O4 O 0.1512(6) -0.1717(4) -0.3221(3) 0.0306(8) Uani 1 1 d . . .
N1 N -0.2743(6) -0.2216(4) 0.0477(3) 0.0166(7) Uani 1 1 d . . .
N2 N 0.1156(7) -0.0961(4) 0.1822(3) 0.0181(8) Uani 1 1 d . . .
C1 C -0.4795(8) -0.2723(5) -0.0171(4) 0.0184(9) Uani 1 1 d . . .
H1B H -0.5009 -0.2447 -0.0885 0.022 Uiso 1 1 calc R . .
C2 C -0.6614(8) -0.3637(5) 0.0171(4) 0.0226(10) Uani 1 1 d . . .
H2A H -0.8013 -0.3951 -0.0295 0.027 Uiso 1 1 calc R . .
C3 C -0.6276(9) -0.4063(5) 0.1226(4) 0.0231(10) Uani 1 1 d . . .
H3B H -0.7448 -0.4682 0.1476 0.028 Uiso 1 1 calc R . .
C4 C -0.4190(9) -0.3563(5) 0.1901(4) 0.0220(10) Uani 1 1 d . . .
H4B H -0.3938 -0.3844 0.2609 0.026 Uiso 1 1 calc R . .
C5 C -0.2451(8) -0.2624(5) 0.1510(4) 0.0184(9) Uani 1 1 d . . .
C6 C -0.0199(8) -0.1993(4) 0.2217(4) 0.0166(9) Uani 1 1 d . . .
C7 C 0.0459(9) -0.2454(5) 0.3220(4) 0.0245(10) Uani 1 1 d . . .
H7A H -0.0517 -0.3173 0.3474 0.029 Uiso 1 1 calc R . .
C8 C 0.2603(9) -0.1815(5) 0.3829(4) 0.0259(10) Uani 1 1 d . . .
H8A H 0.3061 -0.2076 0.4517 0.031 Uiso 1 1 calc R . .
C9 C 0.4058(8) -0.0784(5) 0.3404(4) 0.0233(10) Uani 1 1 d . . .
H9A H 0.5520 -0.0364 0.3783 0.028 Uiso 1 1 calc R . .
C10 C 0.3273(8) -0.0396(5) 0.2399(4) 0.0207(9) Uani 1 1 d . . .
H10A H 0.4251 0.0287 0.2107 0.025 Uiso 1 1 calc R . .
C11 C -0.2462(9) -0.3431(5) -0.3899(4) 0.0243(10) Uani 1 1 d . . .
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 180.0 . 2 ?
O1 U O2 100.75(12) . . ?
O1 U O2 79.25(12) 2 . ?
O1 U O2 79.25(12) . 2 ?
O1 U O2 100.75(12) 2 2 ?
O2 U O2 180.0 . 2 ?
O1 U N2 104.17(13) . . ?
O1 U N2 75.83(13) 2 . ?
O2 U N2 112.59(11) . . ?
O2 U N2 67.41(11) 2 . ?
O1 U N2 75.83(13) . 2 ?
O1 U N2 104.17(13) 2 2 ?
O2 U N2 67.41(11) . 2 ?
O2 U N2 112.59(11) 2 2 ?
N2 U N2 180.00(8) . 2 ?
O1 U N1 74.13(13) . . ?
O1 U N1 105.87(13) 2 . ?
O2 U N1 68.12(11) . . ?
O2 U N1 111.88(11) 2 . ?
N2 U N1 60.77(12) . . ?
N2 U N1 119.23(12) 2 . ?
O1 U N1 105.87(13) . 2 ?
O1 U N1 74.13(13) 2 2 ?
O2 U N1 111.88(11) . 2 ?
O2 U N1 68.12(11) 2 2 ?
N2 U N1 119.23(12) . 2 ?
N2 U N1 60.77(12) 2 2 ?
N1 U N1 180.0 . 2 ?
O4 S O3 117.3(2) . . ?
O4 S O2 114.2(2) . . ?
O3 S O2 113.6(2) . . ?
O4 S C11 104.9(2) . . ?
O3 S C11 104.2(2) . . ?
O2 S C11 99.9(2) . . ?
S O2 U 131.25(19) . . ?
C1 N1 C5 117.7(4) . . ?
C1 N1 U 117.9(3) . . ?
C5 N1 U 122.2(3) . . ?
C6 N2 C10 117.8(4) . . ?
C6 N2 U 124.3(3) . . ?
C10 N2 U 117.9(3) . . ?
N1 C1 C2 123.7(4) . . ?
C3 C2 C1 118.0(4) . . ?
C4 C3 C2 119.5(4) . . ?
C3 C4 C5 119.3(4) . . ?
N1 C5 C4 121.9(4) . . ?
N1 C5 C6 115.8(4) . . ?
C4 C5 C6 122.3(4) . . ?
N2 C6 C7 122.7(4) . . ?
N2 C6 C5 115.3(4) . . ?
C7 C6 C5 122.0(4) . . ?
C8 C7 C6 118.5(4) . . ?
C9 C8 C7 119.5(4) . . ?
C10 C9 C8 118.2(4) . . ?
N2 C10 C9 123.3(4) . . ?
F2 C11 F1 107.5(4) . . ?
F2 C11 F3 108.6(4) . . ?
F1 C11 F3 108.3(4) . . ?
F2 C11 S 111.6(3) . . ?
F1 C11 S 110.0(4) . . ?
F3 C11 S 110.7(3) . . ?
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 1.754(3) . ?
U O1 1.754(3) 2 ?
U O2 2.448(3) . ?
U O2 2.448(3) 2 ?
U N2 2.605(4) . ?
U N2 2.605(4) 2 ?
U N1 2.633(4) . ?
U N1 2.633(4) 2 ?
S O4 1.425(4) . ?
S O3 1.437(4) . ?
S O2 1.476(3) . ?
S C11 1.832(5) . ?
F1 C11 1.330(6) . ?
F2 C11 1.318(6) . ?
F3 C11 1.336(6) . ?
N1 C1 1.347(6) . ?
N1 C5 1.348(6) . ?
N2 C6 1.341(6) . ?
N2 C10 1.352(6) . ?
C1 C2 1.392(7) . ?
C2 C3 1.385(7) . ?
C3 C4 1.378(7) . ?
C4 C5 1.404(7) . ?
C5 C6 1.484(6) . ?
C6 C7 1.399(6) . ?
C7 C8 1.388(7) . ?
C8 C9 1.387(7) . ?
C9 C10 1.386(7) . ?
