#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:05:35 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179651 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/04/4510499.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_4510499
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Increasing Complexity in the Uranyl Ion--Kemp’s Triacid System:
 From One- and Two-Dimensional Polymers to Uranyl--Copper(II) Dodeca- and
 Hexadecanuclear Species
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2665
_journal_paper_doi               10.1021/cg500353k
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C24 H42 O18 U'
_chemical_formula_weight         856.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 117.704(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1312(2)
_cell_length_b                   25.5646(11)
_cell_length_c                   8.1350(4)
_cell_measurement_reflns_used    38995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.94
_cell_volume                     1497.17(11)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and three ω scans with 2° steps (347 frames)'
_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  0.0231
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            38995
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.502
_exptl_absorpt_correction_T_max  0.489
_exptl_absorpt_correction_T_min  0.333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.151
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4459
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0316
_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)+(0.0298P)²+4.8878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                3506
_reflns_number_total             4459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg500353k_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4510499--4510507.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4510499
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
U U 0.0000 0.0000 0.5000 0.02117(6) Uani 1 2 d S
O1 O -0.0958(4) -0.02578(12) 0.6368(4) 0.0310(6) Uani 1 1 d .
O2 O -0.1238(4) -0.07651(11) 0.2992(4) 0.0262(6) Uani 1 1 d .
O3 O 0.1591(4) -0.08611(11) 0.5167(4) 0.0315(6) Uani 1 1 d .
O4 O -0.5094(4) -0.08205(15) 0.0407(4) 0.0400(8) Uani 1 1 d .
O5 O -0.4345(5) -0.12602(16) 0.3032(5) 0.0428(8) Uani 1 1 d .
H5 H -0.4801 -0.0960 0.3446 0.051 Uiso 1 1 d R
O6 O -0.2281(7) -0.04380(16) -0.0981(6) 0.0636(12) Uani 1 1 d U
O7 O 0.0766(8) -0.05519(16) 0.0741(6) 0.0609(11) Uani 1 1 d U
H7 H 0.1232 -0.0201 0.0720 0.073 Uiso 1 1 d R
O8 O 0.3168(5) -0.01009(12) 0.7580(5) 0.0413(9) Uani 1 1 d .
H8A H 0.3434 0.0207 0.8090 0.050 Uiso 1 1 d R
H8B H 0.3811 -0.0371 0.8377 0.050 Uiso 1 1 d R
O9 O -0.5178(8) -0.0595(3) 0.4848(10) 0.055(2) Uani 0.668(13) 1 d P
O10 O -0.5980(13) -0.0383(3) 0.3668(14) 0.027(3) Uani 0.332(13) 1 d P
C1 C 0.0137(5) -0.16045(15) 0.3120(6) 0.0262(8) Uani 1 1 d .
C2 C -0.1745(6) -0.18722(16) 0.2594(6) 0.0269(8) Uani 1 1 d .
H2A H -0.1627 -0.2246 0.2350 0.032 Uiso 1 1 calc R
H2B H -0.1972 -0.1856 0.3688 0.032 Uiso 1 1 calc R
C3 C -0.3477(6) -0.16527(17) 0.0914(5) 0.0292(8) Uani 1 1 d .
C4 C -0.3068(7) -0.15375(19) -0.0728(6) 0.0372(10) Uani 1 1 d .
H4A H -0.3272 -0.1866 -0.1441 0.045 Uiso 1 1 calc R
H4B H -0.4010 -0.1284 -0.1553 0.045 Uiso 1 1 calc R
C5 C -0.1152(8) -0.13246(16) -0.0331(7) 0.0377(11) Uani 1 1 d .
C6 C 0.0408(6) -0.15890(16) 0.1372(6) 0.0320(9) Uani 1 1 d .
H6A H 0.1586 -0.1404 0.1681 0.038 Uiso 1 1 calc R
H6B H 0.0543 -0.1953 0.1034 0.038 Uiso 1 1 calc R
C7 C 0.0171(5) -0.10506(15) 0.3816(6) 0.0250(7) Uani 1 1 d .
C8 C 0.1685(6) -0.19264(17) 0.4630(7) 0.0408(11) Uani 1 1 d .
H8C H 0.2891 -0.1769 0.4928 0.061 Uiso 1 1 calc R
H8D H 0.1644 -0.2285 0.4186 0.061 Uiso 1 1 calc R
H8E H 0.1514 -0.1932 0.5746 0.061 Uiso 1 1 calc R
C9 C -0.4333(6) -0.11915(19) 0.1428(6) 0.0325(9) Uani 1 1 d .
C10 C -0.5005(6) -0.2073(2) 0.0281(6) 0.0407(11) Uani 1 1 d .
H10A H -0.6111 -0.1948 -0.0815 0.061 Uiso 1 1 calc R
H10B H -0.5320 -0.2144 0.1285 0.061 Uiso 1 1 calc R
H10C H -0.4556 -0.2395 -0.0030 0.061 Uiso 1 1 calc R
C11 C -0.0820(10) -0.0713(2) -0.0094(8) 0.0497(13) Uani 1 1 d U
C12 C -0.0837(9) -0.1447(2) -0.2037(7) 0.0456(12) Uani 1 1 d U
H12A H 0.0345 -0.1294 -0.1844 0.068 Uiso 1 1 calc R
H12B H -0.1854 -0.1296 -0.3156 0.068 Uiso 1 1 calc R
H12C H -0.0805 -0.1826 -0.2185 0.068 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'
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 179.999(1) 3_556 .
O1 U O2 92.46(12) 3_556 .
O1 U O2 87.54(12) . .
O1 U O2 87.54(12) 3_556 3_556
O1 U O2 92.46(12) . 3_556
O2 U O2 180.00(15) . 3_556
O1 U O8 90.96(14) 3_556 3_556
O1 U O8 89.04(14) . 3_556
O2 U O8 64.67(9) . 3_556
O2 U O8 115.33(9) 3_556 3_556
O1 U O8 89.04(14) 3_556 .
O1 U O8 90.96(14) . .
O2 U O8 115.32(9) . .
O2 U O8 64.68(9) 3_556 .
O8 U O8 179.998(2) 3_556 .
O1 U O3 90.33(12) 3_556 3_556
O1 U O3 89.67(12) . 3_556
O2 U O3 128.31(9) . 3_556
O2 U O3 51.69(9) 3_556 3_556
O8 U O3 63.68(10) 3_556 3_556
O8 U O3 116.33(10) . 3_556
O1 U O3 89.67(12) 3_556 .
O1 U O3 90.33(12) . .
O2 U O3 51.69(9) . .
O2 U O3 128.31(9) 3_556 .
O8 U O3 116.32(10) 3_556 .
O8 U O3 63.67(10) . .
O3 U O3 180.0 3_556 .
C7 O2 U 96.8(2) . .
C7 O3 U 92.8(2) . .
C9 O5 H5 114.5 . .
C11 O7 H7 128.2 . .
U O8 H8A 103.9 . .
U O8 H8B 134.6 . .
H8A O8 H8B 114.0 . .
C7 C1 C8 109.7(3) . .
C7 C1 C6 109.5(3) . .
C8 C1 C6 109.8(4) . .
C7 C1 C2 111.1(3) . .
C8 C1 C2 108.9(3) . .
C6 C1 C2 107.7(3) . .
C3 C2 C1 117.6(3) . .
C3 C2 H2A 107.9 . .
C1 C2 H2A 107.9 . .
C3 C2 H2B 107.9 . .
C1 C2 H2B 107.9 . .
H2A C2 H2B 107.2 . .
C9 C3 C10 103.4(4) . .
C9 C3 C2 112.6(3) . .
C10 C3 C2 107.8(4) . .
C9 C3 C4 113.5(4) . .
C10 C3 C4 107.9(4) . .
C2 C3 C4 111.1(3) . .
C5 C4 C3 119.3(4) . .
C5 C4 H4A 107.5 . .
C3 C4 H4A 107.5 . .
C5 C4 H4B 107.5 . .
C3 C4 H4B 107.5 . .
H4A C4 H4B 107.0 . .
C6 C5 C4 111.5(3) . .
C6 C5 C12 107.9(4) . .
C4 C5 C12 108.2(4) . .
C6 C5 C11 107.7(4) . .
C4 C5 C11 118.3(4) . .
C12 C5 C11 102.5(3) . .
C5 C6 C1 115.7(3) . .
C5 C6 H6A 108.4 . .
C1 C6 H6A 108.4 . .
C5 C6 H6B 108.4 . .
C1 C6 H6B 108.4 . .
H6A C6 H6B 107.4 . .
O2 C7 O3 118.6(4) . .
O2 C7 C1 119.2(4) . .
O3 C7 C1 122.2(3) . .
C1 C8 H8C 109.5 . .
C1 C8 H8D 109.5 . .
H8C C8 H8D 109.5 . .
C1 C8 H8E 109.5 . .
H8C C8 H8E 109.5 . .
H8D C8 H8E 109.5 . .
O4 C9 O5 122.7(4) . .
O4 C9 C3 124.5(4) . .
O5 C9 C3 112.5(4) . .
C3 C10 H10A 109.5 . .
C3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O7 C11 O6 126.6(6) . .
O7 C11 C5 118.5(5) . .
O6 C11 C5 114.5(6) . .
C5 C12 H12A 109.5 . .
C5 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C5 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 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 1.756(3) 3_556
U O1 1.757(3) .
U O2 2.445(3) .
U O2 2.445(3) 3_556
U O8 2.465(3) 3_556
U O8 2.465(3) .
U O3 2.525(3) 3_556
U O3 2.525(3) .
O2 C7 1.258(5) .
O3 C7 1.263(5) .
O4 C9 1.222(6) .
O5 C9 1.322(5) .
O5 H5 0.9767 .
O6 C11 1.276(7) .
O7 C11 1.217(8) .
O7 H7 0.9777 .
O8 H8A 0.8701 .
O8 H8B 0.9239 .
C1 C7 1.520(5) .
C1 C8 1.528(6) .
C1 C6 1.538(6) .
C1 C2 1.544(5) .
C2 C3 1.541(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C9 1.523(6) .
C3 C10 1.540(6) .
C3 C4 1.548(6) .
C4 C5 1.536(7) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.533(7) .
C5 C12 1.555(6) .
C5 C11 1.584(7) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C8 H8C 0.9800 .
C8 H8D 0.9800 .
C8 H8E 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 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
O5 H5 O9 0.98 1.61 2.542(7) 157.9 .
O5 H5 O10 0.98 1.81 2.776(9) 167.3 .
O7 H7 O6 0.98 1.81 2.781(6) 173.0 3
O8 H8A O2 0.87 2.13 2.627(4) 115.8 3_556
O8 H8A O4 0.87 2.06 2.881(5) 157.2 3_556
O8 H8B O4 0.92 1.86 2.766(5) 164.4 1_656
