#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:10:05 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179778 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/74/7007411.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_7007411
loop_
_publ_author_name
'Salmon, Lionel'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Synthesis and crystal structure of uranium(IV) complexes with
 calix[n]arenes (n = 4, 6 and 8): mononuclear, polynuclear and 1D
 polymeric species.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3629
_journal_page_last               3637
_journal_paper_doi               10.1039/b604712b
_journal_year                    2006
_chemical_formula_sum            'C58 H56 N4 O8 U'
_chemical_formula_weight         1175.10
_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                 120.446(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3919(5)
_cell_length_b                   17.0589(5)
_cell_length_c                   17.0640(5)
_cell_measurement_reflns_used    39725
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.47
_cell_volume                     5368.4(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (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 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and one 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  0.0816
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39725
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    3.080
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4943
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0705
_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)+(0.0978P)²+62.5699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                3752
_reflns_number_total             4943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604712b.txt
_cod_data_source_block           8.4py
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7007411
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 0.07612(3) 0.7500 0.0489(2) Uani 1 2 d S . .
O1 O 0.0030(3) 0.1627(3) 0.8431(4) 0.0396(14) Uani 1 1 d . . .
O2 O 0.1268(4) 0.1314(4) 0.8262(4) 0.0475(16) Uani 1 1 d . . .
H2 H 0.1612 0.1015 0.8181 0.057 Uiso 1 1 d R . .
O3 O -0.0704(5) 0.0008(4) 0.7947(5) 0.070(2) Uani 1 1 d . . .
O4 O 0.0772(5) -0.0033(4) 0.8770(5) 0.070(2) Uani 1 1 d . . .
N1 N 0.2409(6) 0.0571(6) 0.8410(7) 0.067(3) Uani 1 1 d . . .
N2 N 0.0000 0.3722(7) 0.7500 0.053(3) Uani 1 2 d S . .
C1 C -0.0599(5) 0.2367(6) 0.8999(6) 0.041(2) Uani 1 1 d . . .
C2 C 0.0044(5) 0.2123(5) 0.9063(6) 0.041(2) Uani 1 1 d . . .
C3 C 0.0729(5) 0.2378(5) 0.9792(6) 0.037(2) Uani 1 1 d . . .
C4 C 0.0737(6) 0.2872(6) 1.0444(6) 0.045(2) Uani 1 1 d . . .
H4 H 0.1178 0.3049 1.0922 0.054 Uiso 1 1 calc R . .
C5 C 0.0100(5) 0.3101(6) 1.0387(6) 0.047(2) Uani 1 1 d . . .
H5 H 0.0111 0.3430 1.0829 0.057 Uiso 1 1 calc R . .
C6 C -0.0550(6) 0.2849(6) 0.9686(7) 0.052(3) Uani 1 1 d . . .
H6 H -0.0974 0.3004 0.9668 0.063 Uiso 1 1 calc R . .
C7 C 0.1415(5) 0.2110(5) 0.9833(6) 0.041(2) Uani 1 1 d . . .
H7A H 0.1393 0.1547 0.9742 0.050 Uiso 1 1 calc R . .
H7B H 0.1824 0.2220 1.0433 0.050 Uiso 1 1 calc R . .
C8 C 0.1538(5) 0.2506(5) 0.9125(6) 0.041(2) Uani 1 1 d . . .
C9 C 0.1433(5) 0.2115(5) 0.8344(6) 0.042(2) Uani 1 1 d . . .
C10 C 0.1503(5) 0.2482(6) 0.7674(6) 0.046(2) Uani 1 1 d . . .
C11 C 0.1702(5) 0.3267(6) 0.7791(6) 0.043(2) Uani 1 1 d . . .
H11 H 0.1744 0.3528 0.7342 0.052 Uiso 1 1 calc R . .
C12 C 0.1837(5) 0.3667(6) 0.8568(7) 0.048(2) Uani 1 1 d . . .
H12 H 0.1995 0.4184 0.8655 0.058 Uiso 1 1 calc R . .
C13 C 0.1737(5) 0.3294(5) 0.9215(6) 0.042(2) Uani 1 1 d . . .
H13 H 0.1803 0.3574 0.9719 0.050 Uiso 1 1 calc R . .
C14 C 0.1311(6) 0.2077(7) 0.6782(7) 0.055(3) Uani 1 1 d . . .
H14A H 0.1693 0.2172 0.6646 0.066 Uiso 1 1 calc R . .
H14B H 0.1280 0.1516 0.6849 0.066 Uiso 1 1 calc R . .
C15 C -0.1205(11) -0.0756(10) 0.8639(14) 0.088(5) Uani 1 1 d . . .
H15A H -0.1199 -0.0525 0.9155 0.132 Uiso 1 1 calc R . .
H15B H -0.1162 -0.1315 0.8711 0.132 Uiso 1 1 calc R . .
H15C H -0.1652 -0.0628 0.8097 0.132 Uiso 1 1 calc R . .
C16 C -0.0612(10) -0.0459(9) 0.8568(11) 0.068(4) Uani 1 1 d . . .
C17 C 0.0047(9) -0.0708(7) 0.9110(12) 0.083(4) Uani 1 1 d . . .
H17 H 0.0050 -0.1162 0.9413 0.099 Uiso 1 1 calc R . .
C18 C 0.0700(9) -0.0490(8) 0.9340(9) 0.084(4) Uani 1 1 d . . .
C19 C 0.1414(12) -0.0782(12) 1.0082(15) 0.105(7) Uani 1 1 d . . .
H19A H 0.1363 -0.0969 1.0577 0.158 Uiso 1 1 calc R . .
H19B H 0.1762 -0.0363 1.0290 0.158 Uiso 1 1 calc R . .
H19C H 0.1578 -0.1203 0.9856 0.158 Uiso 1 1 calc R . .
C20 C 0.2660(9) 0.0088(9) 0.9108(10) 0.094(4) Uani 1 1 d U . .
H20 H 0.2405 0.0037 0.9414 0.113 Uiso 1 1 calc R . .
C21 C 0.3288(10) -0.0347(11) 0.9403(13) 0.115(6) Uani 1 1 d U . .
H21 H 0.3436 -0.0712 0.9868 0.138 Uiso 1 1 calc R . .
C22 C 0.3693(9) -0.0217(10) 0.8976(12) 0.105(5) Uani 1 1 d U . .
H22 H 0.4129 -0.0478 0.9174 0.125 Uiso 1 1 calc R . .
C23 C 0.3432(7) 0.0304(7) 0.8256(9) 0.073(3) Uani 1 1 d U . .
H23 H 0.3682 0.0396 0.7951 0.088 Uiso 1 1 calc R . .
C24 C 0.2798(7) 0.0676(7) 0.8013(10) 0.072(3) Uani 1 1 d U . .
H24 H 0.2624 0.1030 0.7532 0.087 Uiso 1 1 calc R . .
C25 C 0.0089(6) 0.4119(6) 0.8249(8) 0.054(3) Uani 1 1 d . . .
H25 H 0.0147 0.3851 0.8757 0.065 Uiso 1 1 calc R . .
C26 C 0.0088(6) 0.4921(7) 0.8227(9) 0.066(3) Uani 1 1 d . . .
H26 H 0.0149 0.5203 0.8729 0.079 Uiso 1 1 calc R . .
C27 C 0.0000 0.5303(10) 0.7500 0.065(4) Uani 1 2 d SU . .
H27 H 0.0000 0.5848 0.7500 0.078 Uiso 1 2 calc SR . .
N3 N 0.2961(7) 0.2024(7) 0.6714(11) 0.076(6) Uani 0.50 1 d PGU . .
C28 C 0.3063(7) 0.2830(7) 0.6814(11) 0.080(7) Uani 0.50 1 d PGU . .
H28 H 0.2754 0.3139 0.6917 0.096 Uiso 0.50 1 calc PR . .
C29 C 0.3628(8) 0.3176(6) 0.6758(10) 0.055(5) Uani 0.50 1 d PGU . .
H29 H 0.3696 0.3716 0.6825 0.066 Uiso 0.50 1 calc PR . .
C30 C 0.4091(6) 0.2715(7) 0.6604(10) 0.044(4) Uani 0.50 1 d PGU . .
H30 H 0.4469 0.2947 0.6567 0.052 Uiso 0.50 1 calc PR . .
C31 C 0.3989(7) 0.1909(7) 0.6504(11) 0.072(7) Uani 0.50 1 d PGU . .
H31 H 0.4298 0.1600 0.6401 0.086 Uiso 0.50 1 calc PR . .
C32 C 0.3424(7) 0.1563(6) 0.6559(11) 0.051(5) Uani 0.50 1 d PGU . .
H32 H 0.3355 0.1023 0.6493 0.061 Uiso 0.50 1 calc PR . .
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'
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'
N N 0.0061 0.0033 '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 93.0(3) . 2_556 ?
O1 U O4 144.5(3) . 2_556 ?
O1 U O4 88.4(3) 2_556 2_556 ?
O1 U O4 88.4(2) . . ?
O1 U O4 144.5(3) 2_556 . ?
O4 U O4 110.4(4) 2_556 . ?
O1 U O3 85.5(2) . . ?
O1 U O3 145.3(3) 2_556 . ?
O4 U O3 74.0(3) 2_556 . ?
O4 U O3 70.1(3) . . ?
O1 U O3 145.3(3) . 2_556 ?
O1 U O3 85.5(2) 2_556 2_556 ?
O4 U O3 70.1(3) 2_556 2_556 ?
O4 U O3 74.0(3) . 2_556 ?
O3 U O3 114.7(4) . 2_556 ?
O1 U O2 74.9(2) . . ?
O1 U O2 75.2(2) 2_556 . ?
O4 U O2 138.9(3) 2_556 . ?
O4 U O2 70.9(3) . . ?
O3 U O2 136.6(2) . . ?
O3 U O2 71.2(3) 2_556 . ?
O1 U O2 75.2(2) . 2_556 ?
O1 U O2 74.9(2) 2_556 2_556 ?
O4 U O2 70.9(3) 2_556 2_556 ?
O4 U O2 138.9(3) . 2_556 ?
O3 U O2 71.2(3) . 2_556 ?
O3 U O2 136.6(2) 2_556 2_556 ?
O2 U O2 136.1(3) . 2_556 ?
C2 O1 U 175.0(5) . . ?
C9 O2 U 124.5(5) . . ?
C16 O3 U 139.2(11) . . ?
C18 O4 U 136.5(9) . . ?
C20 N1 C24 118.3(12) . . ?
C25 N2 C25 120.8(13) 2_556 . ?
C2 C1 C6 117.5(9) . . ?
C2 C1 C14 119.2(8) . 2_556 ?
C6 C1 C14 123.3(9) . 2_556 ?
O1 C2 C1 120.1(8) . . ?
O1 C2 C3 118.8(8) . . ?
C1 C2 C3 121.2(8) . . ?
C4 C3 C2 118.2(8) . . ?
C4 C3 C7 122.1(9) . . ?
C2 C3 C7 119.7(8) . . ?
C5 C4 C3 120.5(9) . . ?
C6 C5 C4 120.4(9) . . ?
C5 C6 C1 122.2(10) . . ?
C3 C7 C8 112.6(7) . . ?
C13 C8 C9 117.1(8) . . ?
C13 C8 C7 120.5(8) . . ?
C9 C8 C7 122.3(8) . . ?
C10 C9 O2 119.3(8) . . ?
C10 C9 C8 122.7(9) . . ?
O2 C9 C8 118.0(8) . . ?
C9 C10 C11 118.3(9) . . ?
C9 C10 C14 122.3(10) . . ?
C11 C10 C14 119.2(9) . . ?
C12 C11 C10 120.8(9) . . ?
C13 C12 C11 119.8(10) . . ?
C12 C13 C8 121.2(9) . . ?
C1 C14 C10 111.9(8) 2_556 . ?
O3 C16 C17 117.0(15) . . ?
O3 C16 C15 122.0(17) . . ?
C17 C16 C15 120.8(14) . . ?
C18 C17 C16 137.0(14) . . ?
C17 C18 O4 117.2(13) . . ?
C17 C18 C19 130.0(15) . . ?
O4 C18 C19 111.9(16) . . ?
N1 C20 C21 122.5(17) . . ?
C20 C21 C22 117.8(18) . . ?
C23 C22 C21 119.0(15) . . ?
C24 C23 C22 117.5(15) . . ?
N1 C24 C23 124.7(14) . . ?
C26 C25 N2 118.1(11) . . ?
C27 C26 C25 120.9(12) . . ?
C26 C27 C26 121.3(16) . 2_556 ?
C28 N3 C32 120.0 . . ?
C29 C28 N3 120.0 . . ?
C30 C29 C28 120.0 . . ?
C29 C30 C31 120.0 . . ?
C32 C31 C30 120.0 . . ?
C31 C32 N3 120.0 . . ?
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 2.146(6) . ?
U O1 2.146(6) 2_556 ?
U O4 2.374(7) 2_556 ?
U O4 2.374(7) . ?
U O3 2.381(8) . ?
U O3 2.381(8) 2_556 ?
U O2 2.522(7) . ?
U O2 2.522(7) 2_556 ?
O1 C2 1.360(11) . ?
O2 C9 1.400(11) . ?
O3 C16 1.259(16) . ?
O4 C18 1.314(16) . ?
N1 C20 1.319(18) . ?
N1 C24 1.324(18) . ?
N2 C25 1.373(12) 2_556 ?
N2 C25 1.373(12) . ?
C1 C2 1.387(14) . ?
C1 C6 1.393(13) . ?
C1 C14 1.510(14) 2_556 ?
C2 C3 1.428(14) . ?
C3 C4 1.389(12) . ?
C3 C7 1.504(13) . ?
C4 C5 1.375(14) . ?
C5 C6 1.365(14) . ?
C7 C8 1.518(12) . ?
C8 C13 1.395(13) . ?
C8 C9 1.403(13) . ?
C9 C10 1.377(13) . ?
C10 C11 1.389(14) . ?
C10 C14 1.526(14) . ?
C11 C12 1.385(14) . ?
C12 C13 1.382(13) . ?
C14 C1 1.510(14) 2_556 ?
C15 C16 1.43(2) . ?
C16 C17 1.30(2) . ?
C17 C18 1.30(2) . ?
C18 C19 1.49(3) . ?
C20 C21 1.39(2) . ?
C21 C22 1.40(3) . ?
C22 C23 1.38(2) . ?
C23 C24 1.358(17) . ?
C25 C26 1.369(15) . ?
C26 C27 1.328(15) . ?
C27 C26 1.328(15) 2_556 ?
N3 C28 1.3900 . ?
N3 C32 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C31 C32 1.3900 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 N1 0.96 1.72 2.648(12) 160.8 .
