#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:28:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179846 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/42/7014206.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_7014206
loop_
_publ_author_name
'Salmon, Lionel'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Synthesis and crystal structure of uranium(IV) complexes with
 compartmental Schiff bases: from mononuclear species to tri- and
 tetranuclear clusters.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1635
_journal_page_last               1643
_journal_paper_doi               10.1039/b403459g
_journal_year                    2004
_chemical_formula_sum            'C46 H40 N4 O8 U'
_chemical_formula_weight         1014.85
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.144(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2340(9)
_cell_length_b                   15.5787(10)
_cell_length_c                   17.2083(10)
_cell_measurement_reflns_used    13741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.96
_cell_volume                     4059.1(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ 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  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13741
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    4.059
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.646
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0345
_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)+3.9610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                3235
_reflns_number_total             3833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b403459g.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7014206
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 0.527756(17) 0.2500 0.03022(9) Uani 1 2 d S . .
O1 O 0.0689(2) 0.3082(2) 0.4356(2) 0.0430(8) Uani 1 1 d . . .
O2 O -0.0194(2) 0.42532(19) 0.33014(19) 0.0340(7) Uani 1 1 d . . .
O3 O 0.0852(2) 0.6311(2) 0.2308(2) 0.0357(7) Uani 1 1 d . . .
O4 O 0.1774(2) 0.7508(2) 0.3294(2) 0.0403(8) Uani 1 1 d . . .
N1 N -0.1590(2) 0.4684(3) 0.1871(2) 0.0325(8) Uani 1 1 d . . .
N2 N -0.0708(2) 0.5916(2) 0.0963(2) 0.0336(9) Uani 1 1 d . . .
C1 C 0.1294(3) 0.2442(3) 0.4811(3) 0.0470(13) Uani 1 1 d . . .
H1A H 0.1034 0.2114 0.5136 0.071 Uiso 1 1 calc R . .
H1B H 0.1825 0.2711 0.5174 0.071 Uiso 1 1 calc R . .
H1C H 0.1431 0.2069 0.4430 0.071 Uiso 1 1 calc R . .
C2 C -0.0066(3) 0.2809(3) 0.3746(3) 0.0365(11) Uani 1 1 d . . .
C3 C -0.0530(3) 0.3472(3) 0.3190(3) 0.0351(11) Uani 1 1 d . . .
C4 C -0.1332(3) 0.3277(3) 0.2546(3) 0.0358(11) Uani 1 1 d . . .
C5 C -0.1663(4) 0.2427(3) 0.2469(3) 0.0419(12) Uani 1 1 d . . .
H5 H -0.2202 0.2297 0.2054 0.050 Uiso 1 1 calc R . .
C6 C -0.1196(4) 0.1792(3) 0.3001(3) 0.0488(14) Uani 1 1 d . . .
H6 H -0.1412 0.1233 0.2937 0.059 Uiso 1 1 calc R . .
C7 C -0.0397(4) 0.1986(3) 0.3637(3) 0.0434(13) Uani 1 1 d . . .
H7 H -0.0083 0.1552 0.3992 0.052 Uiso 1 1 calc R . .
C8 C -0.1853(3) 0.3923(3) 0.1968(3) 0.0350(11) Uani 1 1 d . . .
H8 H -0.2428 0.3774 0.1638 0.042 Uiso 1 1 calc R . .
C9 C -0.2228(3) 0.5227(3) 0.1232(3) 0.0358(10) Uani 1 1 d . . .
H9A H -0.2140 0.5825 0.1398 0.043 Uiso 1 1 calc R . .
H9B H -0.2827 0.5067 0.1169 0.043 Uiso 1 1 calc R . .
C10 C -0.2090(3) 0.5102(3) 0.0415(3) 0.0339(11) Uani 1 1 d . . .
C11 C -0.2697(3) 0.4651(3) -0.0229(3) 0.0385(11) Uani 1 1 d . . .
H11 H -0.3217 0.4462 -0.0174 0.046 Uiso 1 1 calc R . .
C12 C -0.2546(3) 0.4474(3) -0.0959(3) 0.0430(13) Uani 1 1 d . . .
H12 H -0.2964 0.4173 -0.1389 0.052 Uiso 1 1 calc R . .
C13 C -0.1780(3) 0.4746(3) -0.1045(3) 0.0399(11) Uani 1 1 d . . .
H13 H -0.1668 0.4609 -0.1523 0.048 Uiso 1 1 calc R . .
C14 C -0.1169(3) 0.5226(3) -0.0418(3) 0.0377(10) Uani 1 1 d . . .
H14 H -0.0657 0.5421 -0.0485 0.045 Uiso 1 1 calc R . .
C15 C -0.1322(3) 0.5416(3) 0.0315(3) 0.0346(11) Uani 1 1 d . . .
C16 C -0.0525(3) 0.6663(3) 0.0740(3) 0.0360(11) Uani 1 1 d . . .
H16 H -0.0795 0.6798 0.0178 0.043 Uiso 1 1 calc R . .
C17 C 0.0049(3) 0.7312(3) 0.1260(3) 0.0358(11) Uani 1 1 d . . .
C18 C 0.0692(3) 0.7108(3) 0.2029(3) 0.0323(11) Uani 1 1 d . . .
C19 C 0.1198(3) 0.7781(3) 0.2547(3) 0.0372(11) Uani 1 1 d . . .
C20 C 0.1059(3) 0.8621(3) 0.2269(3) 0.0419(12) Uani 1 1 d . . .
H20 H 0.1391 0.9059 0.2604 0.050 Uiso 1 1 calc R . .
C21 C 0.0424(4) 0.8820(3) 0.1489(3) 0.0458(13) Uani 1 1 d . . .
H21 H 0.0335 0.9387 0.1310 0.055 Uiso 1 1 calc R . .
C22 C -0.0065(3) 0.8179(3) 0.0992(3) 0.0423(12) Uani 1 1 d . . .
H22 H -0.0477 0.8314 0.0470 0.051 Uiso 1 1 calc R . .
C23 C 0.2290(4) 0.8150(3) 0.3858(3) 0.0500(14) Uani 1 1 d . . .
H23A H 0.2649 0.8448 0.3607 0.075 Uiso 1 1 calc R . .
H23B H 0.2663 0.7881 0.4365 0.075 Uiso 1 1 calc R . .
H23C H 0.1904 0.8551 0.3979 0.075 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 U O2 87.26(16) 6_556 . ?
O2 U O3 101.23(11) 6_556 . ?
O2 U O3 148.63(11) . . ?
O2 U O3 148.63(11) 6_556 6_556 ?
O2 U O3 101.23(11) . 6_556 ?
O3 U O3 87.17(16) . 6_556 ?
O2 U N1 79.92(11) 6_556 . ?
O2 U N1 69.90(11) . . ?
O3 U N1 141.09(12) . . ?
O3 U N1 74.98(12) 6_556 . ?
O2 U N1 69.90(11) 6_556 6_556 ?
O2 U N1 79.92(11) . 6_556 ?
O3 U N1 74.98(12) . 6_556 ?
O3 U N1 141.09(12) 6_556 6_556 ?
N1 U N1 138.02(17) . 6_556 ?
O2 U N2 141.49(11) 6_556 6_556 ?
O2 U N2 75.96(11) . 6_556 ?
O3 U N2 78.95(11) . 6_556 ?
O3 U N2 69.61(11) 6_556 6_556 ?
N1 U N2 123.87(11) . 6_556 ?
N1 U N2 73.13(11) 6_556 6_556 ?
O2 U N2 75.96(11) 6_556 . ?
O2 U N2 141.49(11) . . ?
O3 U N2 69.61(11) . . ?
O3 U N2 78.95(11) 6_556 . ?
N1 U N2 73.13(11) . . ?
N1 U N2 123.87(11) 6_556 . ?
N2 U N2 136.21(16) 6_556 . ?
C2 O1 C1 117.2(4) . . ?
C19 O4 C23 117.3(4) . . ?
C8 N1 C9 116.6(4) . . ?
C16 N2 C15 115.4(4) . . ?
O1 C2 C7 126.5(5) . . ?
O1 C2 C3 113.7(4) . . ?
C7 C2 C3 119.9(5) . . ?
O2 C3 C4 122.1(4) . . ?
O2 C3 C2 118.8(4) . . ?
C4 C3 C2 119.2(4) . . ?
C3 C4 C5 119.2(5) . . ?
C3 C4 C8 122.4(4) . . ?
C5 C4 C8 118.4(5) . . ?
C6 C5 C4 120.7(5) . . ?
C5 C6 C7 120.0(5) . . ?
C2 C7 C6 121.0(5) . . ?
N1 C8 C4 125.9(4) . . ?
N1 C9 C10 108.5(4) . . ?
C11 C10 C15 119.1(4) . . ?
C11 C10 C9 120.6(4) . . ?
C15 C10 C9 120.3(4) . . ?
C10 C11 C12 121.2(4) . . ?
C13 C12 C11 119.8(5) . . ?
C12 C13 C14 120.2(4) . . ?
C13 C14 C15 120.2(4) . . ?
C14 C15 C10 119.3(4) . . ?
C14 C15 N2 121.2(4) . . ?
C10 C15 N2 119.5(4) . . ?
N2 C16 C17 127.7(4) . . ?
C18 C17 C22 119.3(5) . . ?
C18 C17 C16 121.5(4) . . ?
C22 C17 C16 119.1(5) . . ?
O3 C18 C17 122.7(4) . . ?
O3 C18 C19 118.0(4) . . ?
C17 C18 C19 119.4(4) . . ?
O4 C19 C20 126.4(4) . . ?
O4 C19 C18 114.0(4) . . ?
C20 C19 C18 119.5(5) . . ?
C19 C20 C21 120.8(5) . . ?
C22 C21 C20 119.9(5) . . ?
C21 C22 C17 121.0(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
U O2 2.205(3) 6_556 ?
U O2 2.205(3) . ?
U O3 2.223(3) . ?
U O3 2.223(3) 6_556 ?
U N1 2.583(4) . ?
U N1 2.583(4) 6_556 ?
U N2 2.667(4) 6_556 ?
U N2 2.667(4) . ?
O1 C2 1.363(6) . ?
O1 C1 1.419(6) . ?
O1 O2 2.608(4) . ?
O2 C3 1.319(5) . ?
O2 N1 2.760(5) . ?
O2 O3 4.263(4) . ?
O3 C18 1.323(5) . ?
O3 O4 2.601(4) . ?
O3 N2 2.815(5) . ?
O4 C19 1.357(6) . ?
O4 C23 1.435(6) . ?
N1 C8 1.291(6) . ?
N1 C9 1.476(6) . ?
N1 N2 3.129(5) . ?
N2 C16 1.293(6) . ?
N2 C15 1.428(6) . ?
C2 C7 1.377(7) . ?
C2 C3 1.424(7) . ?
C3 C4 1.405(7) . ?
C4 C5 1.417(6) . ?
C4 C8 1.453(7) . ?
C5 C6 1.375(7) . ?
C6 C7 1.395(7) . ?
C9 C10 1.514(6) . ?
C10 C11 1.381(6) . ?
C10 C15 1.407(6) . ?
C11 C12 1.392(7) . ?
C12 C13 1.372(7) . ?
C13 C14 1.391(7) . ?
C14 C15 1.401(6) . ?
C16 C17 1.446(7) . ?
C17 C18 1.396(7) . ?
C17 C22 1.417(6) . ?
C18 C19 1.427(6) . ?
C19 C20 1.384(7) . ?
C20 C21 1.400(7) . ?
C21 C22 1.367(7) . ?
