#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/07/7050756.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_7050756
loop_
_publ_author_name
'Masci, Bernardo'
'Nierlich, Martine'
'Thuéry, Pierre'
_publ_section_title
;
 Trigonal versus tetragonal or pentagonal coordination of the uranyl
 ion by hexahomotrioxacalix[3]arenes: solid state and solution
 investigations
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              120
_journal_paper_doi               10.1039/b108947c
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C33 H43 N O8 U'
_chemical_formula_weight         819.71
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.3031(6)
_cell_length_b                   19.6564(8)
_cell_length_c                   19.6680(8)
_cell_measurement_reflns_used    41417
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.63
_cell_volume                     6302.8(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_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41417
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.202
_exptl_absorpt_correction_T_max  0.594
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent intense orange'
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0295
_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)+(0.0059P)²+10.8520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                4467
_reflns_number_total             5961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108947c.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7050756
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.284079(9) -0.305462(8) 0.544024(8) 0.02330(5) Uani 1 1 d . . .
O1 O 0.27679(17) -0.25560(15) 0.44251(14) 0.0265(7) Uani 1 1 d . . .
O2 O 0.1441(2) -0.34366(15) 0.47659(14) 0.0294(7) Uani 1 1 d . . .
O3 O 0.23754(17) -0.40386(15) 0.58349(16) 0.0275(7) Uani 1 1 d . . .
O4 O 0.23573(18) -0.32866(15) 0.71471(16) 0.0294(7) Uani 1 1 d . . .
O5 O 0.36970(17) -0.26676(15) 0.62229(15) 0.0262(7) Uani 1 1 d . . .
O6 O 0.30964(18) -0.15144(16) 0.54161(16) 0.0322(7) Uani 1 1 d . . .
O7 O 0.36645(18) -0.35320(16) 0.50751(15) 0.0300(7) Uani 1 1 d . . .
O8 O 0.20114(17) -0.25762(14) 0.57967(14) 0.0219(6) Uani 1 1 d . . .
C1 C 0.2251(3) -0.1430(2) 0.4448(2) 0.0261(10) Uani 1 1 d . . .
C2 C 0.2141(3) -0.2127(2) 0.4324(2) 0.0246(9) Uani 1 1 d . . .
C3 C 0.1371(3) -0.2382(2) 0.4145(2) 0.0269(10) Uani 1 1 d . . .
C4 C 0.0725(3) -0.1927(3) 0.4042(2) 0.0340(11) Uani 1 1 d . . .
H4 H 0.0213 -0.2096 0.3920 0.041 Uiso 1 1 calc R . .
C5 C 0.0826(3) -0.1231(3) 0.4118(2) 0.0364(12) Uani 1 1 d . . .
C6 C 0.1591(3) -0.0986(3) 0.4336(2) 0.0340(12) Uani 1 1 d . . .
H6 H 0.1662 -0.0522 0.4407 0.041 Uiso 1 1 calc R . .
C7 C 0.0124(3) -0.0743(3) 0.3998(3) 0.0509(16) Uani 1 1 d . . .
H7A H -0.0286 -0.0960 0.3723 0.076 Uiso 1 1 calc R . .
H7B H 0.0324 -0.0345 0.3769 0.076 Uiso 1 1 calc R . .
H7C H -0.0111 -0.0614 0.4427 0.076 Uiso 1 1 calc R . .
C8 C 0.1262(3) -0.3140(3) 0.4104(2) 0.0338(12) Uani 1 1 d . . .
H8A H 0.0703 -0.3246 0.3973 0.041 Uiso 1 1 calc R . .
H8B H 0.1628 -0.3327 0.3764 0.041 Uiso 1 1 calc R . .
C9 C 0.1162(3) -0.4131(2) 0.4842(2) 0.0293(10) Uani 1 1 d . . .
H9A H 0.1582 -0.4444 0.4688 0.035 Uiso 1 1 calc R . .
H9B H 0.0671 -0.4204 0.4573 0.035 Uiso 1 1 calc R . .
C10 C 0.0981(3) -0.4248(2) 0.5586(2) 0.0247(10) Uani 1 1 d . . .
C11 C 0.1611(3) -0.4145(2) 0.6061(2) 0.0247(10) Uani 1 1 d . . .
C12 C 0.1441(3) -0.4146(2) 0.6755(2) 0.0276(10) Uani 1 1 d . . .
C13 C 0.0645(3) -0.4302(2) 0.6968(2) 0.0286(10) Uani 1 1 d . . .
H13 H 0.0528 -0.4304 0.7431 0.034 Uiso 1 1 calc R . .
C14 C 0.0020(3) -0.4456(2) 0.6508(2) 0.0273(10) Uani 1 1 d . . .
C15 C 0.0196(3) -0.4411(2) 0.5815(2) 0.0283(11) Uani 1 1 d . . .
H15 H -0.0218 -0.4492 0.5500 0.034 Uiso 1 1 calc R . .
C16 C -0.0825(3) -0.4670(2) 0.6758(3) 0.0354(12) Uani 1 1 d . . .
H16A H -0.0915 -0.5140 0.6650 0.053 Uiso 1 1 calc R . .
H16B H -0.1236 -0.4397 0.6540 0.053 Uiso 1 1 calc R . .
H16C H -0.0856 -0.4607 0.7241 0.053 Uiso 1 1 calc R . .
C17 C 0.2114(3) -0.3981(2) 0.7251(2) 0.0300(10) Uani 1 1 d . . .
H17A H 0.1920 -0.4043 0.7713 0.036 Uiso 1 1 calc R . .
H17B H 0.2577 -0.4282 0.7178 0.036 Uiso 1 1 calc R . .
C18 C 0.3105(3) -0.3121(2) 0.7497(2) 0.0271(10) Uani 1 1 d . . .
H18A H 0.3549 -0.3406 0.7335 0.033 Uiso 1 1 calc R . .
H18B H 0.3041 -0.3194 0.7982 0.033 Uiso 1 1 calc R . .
C19 C 0.3290(3) -0.2384(2) 0.7356(2) 0.0255(10) Uani 1 1 d . . .
C20 C 0.3543(3) -0.2196(2) 0.6696(2) 0.0236(10) Uani 1 1 d . . .
C21 C 0.3627(3) -0.1505(2) 0.6541(2) 0.0258(10) Uani 1 1 d . . .
C22 C 0.3500(3) -0.1024(2) 0.7042(2) 0.0307(11) Uani 1 1 d . . .
H22 H 0.3559 -0.0566 0.6933 0.037 Uiso 1 1 calc R . .
C23 C 0.3285(3) -0.1200(2) 0.7707(2) 0.0263(10) Uani 1 1 d . . .
C24 C 0.3177(2) -0.1888(2) 0.7847(2) 0.0259(10) Uani 1 1 d . . .
H24 H 0.3024 -0.2018 0.8283 0.031 Uiso 1 1 calc R . .
C25 C 0.3159(3) -0.0664(2) 0.8250(3) 0.0374(12) Uani 1 1 d . . .
H25A H 0.2622 -0.0469 0.8203 0.056 Uiso 1 1 calc R . .
H25B H 0.3565 -0.0314 0.8201 0.056 Uiso 1 1 calc R . .
H25C H 0.3210 -0.0869 0.8691 0.056 Uiso 1 1 calc R . .
C26 C 0.3795(3) -0.1302(2) 0.5809(2) 0.0319(11) Uani 1 1 d . . .
H26A H 0.3868 -0.0813 0.5775 0.038 Uiso 1 1 calc R . .
H26B H 0.4289 -0.1523 0.5645 0.038 Uiso 1 1 calc R . .
C27 C 0.3049(3) -0.1204(2) 0.4756(2) 0.0306(11) Uani 1 1 d . . .
H27A H 0.3506 -0.1348 0.4475 0.037 Uiso 1 1 calc R . .
H27B H 0.3063 -0.0712 0.4796 0.037 Uiso 1 1 calc R . .
N N 0.0860(2) -0.16289(19) 0.6209(2) 0.0305(9) Uani 1 1 d . . .
H1 H 0.1212 -0.1871 0.5915 0.037 Uiso 1 1 d R . .
C28 C 0.1088(3) -0.1876(4) 0.6887(3) 0.0540(16) Uani 1 1 d . . .
H28A H 0.1629 -0.1706 0.7000 0.065 Uiso 1 1 calc R . .
H28B H 0.1117 -0.2369 0.6877 0.065 Uiso 1 1 calc R . .
C29 C 0.0491(4) -0.1662(5) 0.7441(3) 0.092(3) Uani 1 1 d . . .
H29A H 0.0473 -0.1175 0.7466 0.138 Uiso 1 1 calc R . .
H29B H 0.0670 -0.1843 0.7870 0.138 Uiso 1 1 calc R . .
H29C H -0.0046 -0.1834 0.7337 0.138 Uiso 1 1 calc R . .
C30 C 0.0054(3) -0.1882(3) 0.5958(3) 0.0396(12) Uani 1 1 d . . .
H30A H -0.0376 -0.1682 0.6234 0.048 Uiso 1 1 calc R . .
H30B H -0.0023 -0.1722 0.5496 0.048 Uiso 1 1 calc R . .
C31 C -0.0044(4) -0.2628(3) 0.5965(4) 0.080(3) Uani 1 1 d . . .
H31A H 0.0401 -0.2835 0.5722 0.121 Uiso 1 1 calc R . .
H31B H -0.0554 -0.2748 0.5752 0.121 Uiso 1 1 calc R . .
H31C H -0.0044 -0.2787 0.6427 0.121 Uiso 1 1 calc R . .
C32 C 0.0862(4) -0.0871(3) 0.6111(4) 0.0586(17) Uani 1 1 d . . .
H32A H 0.0702 -0.0775 0.5645 0.070 Uiso 1 1 calc R . .
H32B H 0.0447 -0.0676 0.6405 0.070 Uiso 1 1 calc R . .
C33 C 0.1641(4) -0.0526(3) 0.6245(4) 0.075(2) Uani 1 1 d . . .
H33A H 0.1760 -0.0545 0.6723 0.112 Uiso 1 1 calc R . .
H33B H 0.1602 -0.0060 0.6104 0.112 Uiso 1 1 calc R . .
H33C H 0.2072 -0.0747 0.5996 0.112 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
O7 U O8 179.38(13) . . ?
O7 U O5 89.20(12) . . ?
O8 U O5 91.34(12) . . ?
O7 U O3 86.55(12) . . ?
O8 U O3 93.59(11) . . ?
O5 U O3 105.79(11) . . ?
O7 U O1 84.90(12) . . ?
O8 U O1 94.56(11) . . ?
O5 U O1 120.39(11) . . ?
O3 U O1 132.78(11) . . ?
O7 U O2 106.66(12) . . ?
O8 U O2 72.84(11) . . ?
O5 U O2 162.72(10) . . ?
O3 U O2 69.27(10) . . ?
O1 U O2 69.07(10) . . ?
O7 U O6 114.27(12) . . ?
O8 U O6 65.71(11) . . ?
O5 U O6 65.43(10) . . ?
O3 U O6 156.33(10) . . ?
O1 U O6 63.73(10) . . ?
O2 U O6 112.15(8) . . ?
O7 U O4 119.26(11) . . ?
O8 U O4 61.29(10) . . ?
O5 U O4 61.09(9) . . ?
O3 U O4 58.02(9) . . ?
O1 U O4 155.60(9) . . ?
O2 U O4 104.02(8) . . ?
O6 U O4 100.12(8) . . ?
C9 O2 C8 114.0(3) . . ?
C17 O4 C18 112.5(3) . . ?
C26 O6 C27 113.9(3) . . ?
C6 C1 C2 118.8(4) . . ?
C6 C1 C27 122.9(4) . . ?
C2 C1 C27 118.1(4) . . ?
O1 C2 C3 119.8(4) . . ?
O1 C2 C1 119.4(4) . . ?
C3 C2 C1 120.6(4) . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 C8 118.4(4) . . ?
C4 C3 C8 122.5(4) . . ?
C5 C4 C3 121.8(4) . . ?
C4 C5 C6 118.4(5) . . ?
C4 C5 C7 121.3(5) . . ?
C6 C5 C7 120.2(5) . . ?
C1 C6 C5 121.1(5) . . ?
O2 C8 C3 109.0(4) . . ?
O2 C9 C10 107.8(3) . . ?
C15 C10 C11 119.3(4) . . ?
C15 C10 C9 121.9(4) . . ?
C11 C10 C9 118.6(4) . . ?
O3 C11 C12 120.8(4) . . ?
O3 C11 C10 118.8(4) . . ?
C12 C11 C10 120.4(4) . . ?
C11 C12 C13 118.6(4) . . ?
C11 C12 C17 119.3(4) . . ?
C13 C12 C17 122.1(4) . . ?
C14 C13 C12 122.1(4) . . ?
C15 C14 C13 118.0(4) . . ?
C15 C14 C16 121.3(4) . . ?
C13 C14 C16 120.7(4) . . ?
C10 C15 C14 121.3(4) . . ?
O4 C17 C12 108.4(3) . . ?
O4 C18 C19 107.5(3) . . ?
C24 C19 C20 119.7(4) . . ?
C24 C19 C18 121.5(4) . . ?
C20 C19 C18 118.7(4) . . ?
O5 C20 C21 120.2(4) . . ?
O5 C20 C19 120.9(4) . . ?
C21 C20 C19 118.9(4) . . ?
C22 C21 C20 119.6(4) . . ?
C22 C21 C26 121.6(4) . . ?
C20 C21 C26 118.6(4) . . ?
C21 C22 C23 122.4(4) . . ?
C24 C23 C22 117.3(4) . . ?
C24 C23 C25 121.2(4) . . ?
C22 C23 C25 121.5(4) . . ?
C19 C24 C23 122.0(4) . . ?
O6 C26 C21 106.9(3) . . ?
O6 C27 C1 106.5(3) . . ?
C28 N C30 114.5(4) . . ?
C28 N C32 116.4(5) . . ?
C30 N C32 106.9(4) . . ?
N C28 C29 113.4(5) . . ?
C31 C30 N 115.1(4) . . ?
C33 C32 N 116.0(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 O7 1.789(3) . ?
U O8 1.790(3) . ?
U O5 2.213(3) . ?
U O3 2.218(3) . ?
U O1 2.227(3) . ?
U O2 2.744(3) . ?
U O6 3.056(3) . ?
U O4 3.478(3) . ?
O1 C2 1.340(5) . ?
O1 O2 2.850(4) . ?
O1 O6 2.877(4) . ?
O1 O5 3.853(4) . ?
O1 O3 4.073(4) . ?
O2 C9 1.446(5) . ?
O2 C8 1.456(5) . ?
O2 O3 2.853(4) . ?
O3 C11 1.339(5) . ?
O3 O4 2.974(4) . ?
O3 O5 3.534(4) . ?
O4 C17 1.436(5) . ?
O4 C18 1.437(5) . ?
O4 O5 3.091(4) . ?
O5 C20 1.337(5) . ?
O5 O6 2.935(4) . ?
O6 C26 1.439(5) . ?
O6 C27 1.437(5) . ?
C1 C6 1.403(6) . ?
C1 C2 1.403(6) . ?
C1 C27 1.503(6) . ?
C2 C3 1.395(6) . ?
C3 C4 1.397(6) . ?
C3 C8 1.502(7) . ?
C4 C5 1.386(7) . ?
C5 C6 1.404(7) . ?
C5 C7 1.512(7) . ?
C9 C10 1.510(6) . ?
C10 C15 1.394(6) . ?
C10 C11 1.405(6) . ?
C11 C12 1.394(6) . ?
C12 C13 1.398(6) . ?
C12 C17 1.503(6) . ?
C13 C14 1.396(6) . ?
C14 C15 1.395(6) . ?
C14 C16 1.521(6) . ?
C18 C19 1.505(6) . ?
C19 C24 1.386(6) . ?
C19 C20 1.411(6) . ?
C20 C21 1.400(6) . ?
C21 C22 1.381(6) . ?
C21 C26 1.518(6) . ?
C22 C23 1.396(6) . ?
C23 C24 1.390(6) . ?
C23 C25 1.516(6) . ?
N C28 1.468(6) . ?
N C30 1.489(6) . ?
N C32 1.502(6) . ?
C28 C29 1.519(7) . ?
C30 C31 1.476(8) . ?
C32 C33 1.464(8) . ?
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
N H1 O8 0.94 1.92 2.766(5) 148.5 .
