#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/28/1512870.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_1512870
loop_
_publ_author_name
'Harri Sopo'
'Ari Väisänen'
'Reijo Sillanpää'
_publ_section_title
;
 Uranyl ion complexes with long chain aminoalcoholbis(phenolate)
 [O,N,O,O′] donor ligands
;
_journal_issue                   1
_journal_name_full               Polyhedron
_journal_page_first              184
_journal_page_last               196
_journal_paper_doi               10.1016/j.poly.2006.08.006
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C44 H60 N2 O8 U'
_chemical_formula_sum            'C44 H60 N2 O8 U'
_chemical_formula_weight         982.97
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                106.8500(10)
_cell_angle_beta                 91.9950(10)
_cell_angle_gamma                91.0010(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5394(2)
_cell_length_b                   9.6303(2)
_cell_length_c                   11.7396(3)
_cell_measurement_reflns_used    4029
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_volume                     1031.13(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8344
_diffrn_reflns_theta_full        28.11
_diffrn_reflns_theta_max         28.11
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.990
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+1.8241P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                4954
_reflns_number_total             4958
_reflns_threshold_expression     >2s(I)
_cod_data_source_file            2007-184_RS.txt
_cod_data_source_block           so98=1a
_cod_database_code               1512870
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
U U 0.0000 0.0000 0.0000 0.01809(5) Uani 1 2 d S
O1 O -0.0657(2) -0.1792(2) -0.07882(18) 0.0246(5) Uani 1 1 d .
O2 O 0.1783(2) -0.0257(2) -0.12322(18) 0.0232(4) Uani 1 1 d .
O3 O -0.1183(2) 0.0890(2) -0.13744(18) 0.0226(4) Uani 1 1 d .
O4 O 0.1672(4) 0.0830(3) -0.6305(3) 0.0610(9) Uani 1 1 d .
H4 H 0.173(6) 0.031(6) -0.712(5) 0.089(18) Uiso 1 1 d .
N8 N 0.0933(3) 0.1880(3) -0.2581(2) 0.0221(5) Uani 1 1 d .
H8 H 0.051(4) 0.117(4) -0.243(3) 0.029(10) Uiso 1 1 d .
C1 C 0.2375(3) -0.0884(3) -0.2267(3) 0.0218(6) Uani 1 1 d .
C2 C 0.2670(3) -0.2365(3) -0.2633(3) 0.0240(6) Uani 1 1 d .
C3 C 0.3292(3) -0.2937(4) -0.3727(3) 0.0293(7) Uani 1 1 d .
H3 H 0.3512 -0.3936 -0.3966 0.035 Uiso 1 1 calc R
C4 C 0.3602(4) -0.2101(4) -0.4477(3) 0.0332(8) Uani 1 1 d .
C5 C 0.3317(4) -0.0631(4) -0.4097(3) 0.0307(7) Uani 1 1 d .
H5 H 0.3529 -0.0036 -0.4590 0.037 Uiso 1 1 calc R
C6 C 0.2725(3) -0.0017(3) -0.2998(3) 0.0227(6) Uani 1 1 d .
C7 C 0.2479(3) 0.1574(3) -0.2534(3) 0.0247(6) Uani 1 1 d .
H7A H 0.2986 0.2093 -0.3017 0.030 Uiso 1 1 calc R
H7B H 0.2854 0.1941 -0.1701 0.030 Uiso 1 1 calc R
C9 C 0.0553(3) 0.3187(3) -0.1576(3) 0.0227(6) Uani 1 1 d .
H9A H 0.0962 0.3097 -0.0815 0.027 Uiso 1 1 calc R
H9B H 0.0965 0.4075 -0.1709 0.027 Uiso 1 1 calc R
C10 C -0.1007(3) 0.3332(3) -0.1486(2) 0.0214(6) Uani 1 1 d .
C11 C -0.1658(3) 0.4609(3) -0.1485(3) 0.0246(6) Uani 1 1 d .
H11 H -0.1109 0.5400 -0.1574 0.030 Uiso 1 1 calc R
C12 C -0.3094(3) 0.4757(3) -0.1358(3) 0.0265(7) Uani 1 1 d .
C13 C -0.3871(3) 0.3573(4) -0.1235(3) 0.0267(7) Uani 1 1 d .
H13 H -0.4854 0.3663 -0.1145 0.032 Uiso 1 1 calc R
C14 C -0.3272(3) 0.2267(3) -0.1240(3) 0.0246(6) Uani 1 1 d .
C15 C -0.1808(3) 0.2148(3) -0.1356(2) 0.0207(6) Uani 1 1 d .
C16 C 0.0425(4) 0.1899(4) -0.3809(3) 0.0282(7) Uani 1 1 d .
H16A H -0.0612 0.1812 -0.3865 0.034 Uiso 1 1 calc R
H16B H 0.0790 0.1045 -0.4406 0.034 Uiso 1 1 calc R
C17 C 0.0881(4) 0.3266(4) -0.4108(3) 0.0352(8) Uani 1 1 d .
H17A H 0.1886 0.3481 -0.3872 0.042 Uiso 1 1 calc R
H17B H 0.0340 0.4090 -0.3639 0.042 Uiso 1 1 calc R
C18 C 0.0666(5) 0.3138(5) -0.5439(3) 0.0496(11) Uani 1 1 d .
H18A H -0.0261 0.2660 -0.5718 0.059 Uiso 1 1 calc R
H18B H 0.0635 0.4130 -0.5525 0.059 Uiso 1 1 calc R
C19 C 0.1741(5) 0.2328(4) -0.6235(3) 0.0491(11) Uani 1 1 d .
H19A H 0.1587 0.2440 -0.7042 0.059 Uiso 1 1 calc R
H19B H 0.2686 0.2736 -0.5928 0.059 Uiso 1 1 calc R
C20 C 0.2322(4) -0.3330(4) -0.1872(3) 0.0326(7) Uani 1 1 d .
H20A H 0.2530 -0.4336 -0.2296 0.049 Uiso 1 1 calc R
H20B H 0.1323 -0.3264 -0.1700 0.049 Uiso 1 1 calc R
H20C H 0.2885 -0.3019 -0.1123 0.049 Uiso 1 1 calc R
C21 C 0.4225(5) -0.2769(5) -0.5668(3) 0.0521(11) Uani 1 1 d .
H21A H 0.3603 -0.3559 -0.6146 0.078 Uiso 1 1 calc R
H21B H 0.5146 -0.3153 -0.5547 0.078 Uiso 1 1 calc R
H21C H 0.4333 -0.2028 -0.6084 0.078 Uiso 1 1 calc R
C22 C -0.3797(4) 0.6151(4) -0.1390(3) 0.0357(8) Uani 1 1 d .
H22A H -0.4085 0.6087 -0.2213 0.053 Uiso 1 1 calc R
H22B H -0.3135 0.6974 -0.1076 0.053 Uiso 1 1 calc R
H22C H -0.4624 0.6289 -0.0901 0.053 Uiso 1 1 calc R
C23 C -0.4116(4) 0.0986(4) -0.1106(3) 0.0332(8) Uani 1 1 d .
H23A H -0.5103 0.1243 -0.1006 0.050 Uiso 1 1 calc R
H23B H -0.3755 0.0724 -0.0406 0.050 Uiso 1 1 calc R
H23C H -0.4037 0.0159 -0.1819 0.050 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
O1 U O1 180.00(17) . 2
O1 U O2 89.74(9) . 2
O1 U O2 90.26(9) 2 2
O1 U O2 90.26(9) . .
O1 U O2 89.74(9) 2 .
O2 U O2 180.00(10) 2 .
O1 U O3 90.66(9) . 2
O1 U O3 89.34(9) 2 2
O2 U O3 84.96(7) 2 2
O2 U O3 95.04(7) . 2
O1 U O3 89.34(9) . .
O1 U O3 90.66(9) 2 .
O2 U O3 95.04(7) 2 .
O2 U O3 84.96(7) . .
O3 U O3 180.00(9) 2 .
C1 O2 U 151.86(19) . .
C15 O3 U 135.77(17) . .
C19 O4 H4 107(3) . .
C16 N8 C7 111.9(2) . .
C16 N8 C9 115.1(2) . .
C7 N8 C9 111.9(2) . .
C16 N8 H8 107(3) . .
C7 N8 H8 106(2) . .
C9 N8 H8 104(2) . .
O2 C1 C2 122.3(3) . .
O2 C1 C6 118.5(3) . .
C2 C1 C6 119.3(3) . .
C3 C2 C1 118.7(3) . .
C3 C2 C20 120.3(3) . .
C1 C2 C20 120.9(3) . .
C4 C3 C2 122.6(3) . .
C4 C3 H3 118.7 . .
C2 C3 H3 118.7 . .
C3 C4 C5 118.0(3) . .
C3 C4 C21 121.0(3) . .
C5 C4 C21 121.0(3) . .
C4 C5 C6 120.9(3) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C5 C6 C1 120.4(3) . .
C5 C6 C7 122.2(3) . .
C1 C6 C7 117.4(3) . .
C6 C7 N8 111.1(2) . .
C6 C7 H7A 109.4 . .
N8 C7 H7A 109.4 . .
C6 C7 H7B 109.4 . .
N8 C7 H7B 109.4 . .
H7A C7 H7B 108.0 . .
C10 C9 N8 111.9(2) . .
C10 C9 H9A 109.2 . .
N8 C9 H9A 109.2 . .
C10 C9 H9B 109.2 . .
N8 C9 H9B 109.2 . .
H9A C9 H9B 107.9 . .
C11 C10 C15 119.9(3) . .
C11 C10 C9 121.7(3) . .
C15 C10 C9 118.4(3) . .
C10 C11 C12 121.5(3) . .
C10 C11 H11 119.2 . .
C12 C11 H11 119.2 . .
C11 C12 C13 117.8(3) . .
C11 C12 C22 120.9(3) . .
C13 C12 C22 121.3(3) . .
C14 C13 C12 122.9(3) . .
C14 C13 H13 118.5 . .
C12 C13 H13 118.5 . .
C13 C14 C15 118.2(3) . .
C13 C14 C23 122.8(3) . .
C15 C14 C23 118.9(3) . .
O3 C15 C10 120.2(3) . .
O3 C15 C14 120.1(3) . .
C10 C15 C14 119.6(3) . .
N8 C16 C17 113.1(3) . .
N8 C16 H16A 109.0 . .
C17 C16 H16A 109.0 . .
N8 C16 H16B 109.0 . .
C17 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
C16 C17 C18 112.9(3) . .
C16 C17 H17A 109.0 . .
C18 C17 H17A 109.0 . .
C16 C17 H17B 109.0 . .
C18 C17 H17B 109.0 . .
H17A C17 H17B 107.8 . .
C19 C18 C17 116.2(3) . .
C19 C18 H18A 108.2 . .
C17 C18 H18A 108.2 . .
C19 C18 H18B 108.2 . .
C17 C18 H18B 108.2 . .
H18A C18 H18B 107.4 . .
O4 C19 C18 110.8(3) . .
O4 C19 H19A 109.5 . .
C18 C19 H19A 109.5 . .
O4 C19 H19B 109.5 . .
C18 C19 H19B 109.5 . .
H19A C19 H19B 108.1 . .
C2 C20 H20A 109.5 . .
C2 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C2 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C4 C21 H21A 109.5 . .
C4 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C4 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C12 C22 H22A 109.5 . .
C12 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C12 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C14 C23 H23A 109.5 . .
C14 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C14 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O1 1.795(2) .
U O1 1.795(2) 2
U O2 2.242(2) 2
U O2 2.242(2) .
U O3 2.307(2) 2
U O3 2.307(2) .
O2 C1 1.339(3) .
O3 C15 1.354(3) .
O4 C19 1.421(5) .
O4 H4 0.95(6) .
N8 C16 1.510(4) .
N8 C7 1.511(4) .
N8 C9 1.514(4) .
N8 H8 0.85(4) .
C1 C2 1.402(4) .
C1 C6 1.404(4) .
C2 C3 1.400(4) .
C2 C20 1.504(4) .
C3 C4 1.390(5) .
C3 H3 0.9500 .
C4 C5 1.390(5) .
C4 C21 1.507(5) .
C5 C6 1.398(4) .
C5 H5 0.9500 .
C6 C7 1.496(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C9 C10 1.502(4) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.388(4) .
C10 C15 1.408(4) .
C11 C12 1.388(4) .
C11 H11 0.9500 .
C12 C13 1.394(4) .
C12 C22 1.520(4) .
C13 C14 1.390(4) .
C13 H13 0.9500 .
C14 C15 1.411(4) .
C14 C23 1.511(4) .
C16 C17 1.519(5) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.537(5) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 C19 1.486(6) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
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
O4 H4 O3 0.95(6) 1.86(6) 2.766(4) 159(5) 2_554
N8 H8 O3 0.85(4) 2.13(4) 2.811(3) 137(3) .
N8 H8 O2 0.85(4) 2.54(4) 3.042(3) 119(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
O1 U O2 C1 21.5(4) .
O1 U O2 C1 -158.5(4) 2
O2 U O2 C1 -171(100) 2
O3 U O2 C1 112.2(4) 2
O3 U O2 C1 -67.8(4) .
O1 U O3 C15 148.4(3) .
O1 U O3 C15 -31.6(3) 2
O2 U O3 C15 58.7(3) 2
O2 U O3 C15 -121.3(3) .
O3 U O3 C15 -96(100) 2
U O2 C1 C2 -62.8(5) .
U O2 C1 C6 118.0(4) .
O2 C1 C2 C3 -179.9(3) .
C6 C1 C2 C3 -0.7(4) .
O2 C1 C2 C20 0.4(5) .
C6 C1 C2 C20 179.5(3) .
C1 C2 C3 C4 -1.4(5) .
C20 C2 C3 C4 178.3(3) .
C2 C3 C4 C5 2.1(5) .
C2 C3 C4 C21 -177.8(4) .
C3 C4 C5 C6 -0.6(5) .
C21 C4 C5 C6 179.3(3) .
C4 C5 C6 C1 -1.5(5) .
C4 C5 C6 C7 176.6(3) .
O2 C1 C6 C5 -178.7(3) .
C2 C1 C6 C5 2.1(5) .
O2 C1 C6 C7 3.2(4) .
C2 C1 C6 C7 -176.0(3) .
C5 C6 C7 N8 108.0(3) .
C1 C6 C7 N8 -73.9(3) .
C16 N8 C7 C6 -81.2(3) .
C9 N8 C7 C6 147.9(2) .
C16 N8 C9 C10 61.3(3) .
C7 N8 C9 C10 -169.6(2) .
N8 C9 C10 C11 -126.6(3) .
N8 C9 C10 C15 55.7(3) .
C15 C10 C11 C12 0.1(4) .
C9 C10 C11 C12 -177.6(3) .
C10 C11 C12 C13 -0.3(5) .
C10 C11 C12 C22 -178.5(3) .
C11 C12 C13 C14 -0.2(5) .
C22 C12 C13 C14 178.0(3) .
C12 C13 C14 C15 0.9(5) .
C12 C13 C14 C23 180.0(3) .
U O3 C15 C10 84.3(3) .
U O3 C15 C14 -97.4(3) .
C11 C10 C15 O3 179.0(3) .
C9 C10 C15 O3 -3.2(4) .
C11 C10 C15 C14 0.6(4) .
C9 C10 C15 C14 178.4(3) .
C13 C14 C15 O3 -179.5(3) .
C23 C14 C15 O3 1.5(4) .
C13 C14 C15 C10 -1.1(4) .
C23 C14 C15 C10 179.8(3) .
C7 N8 C16 C17 -75.1(3) .
C9 N8 C16 C17 54.1(4) .
N8 C16 C17 C18 166.7(3) .
C16 C17 C18 C19 -79.0(5) .
C17 C18 C19 O4 67.9(5) .
