#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:14:39 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179528 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/25/4342517.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_4342517
loop_
_publ_author_name
'Thuéry, Pierre'
'Rivière, Eric'
'Harrowfield, Jack'
_publ_section_title
;
 Uranyl and uranyl-3d block cation complexes with
 1,3-adamantanedicarboxylate: crystal structures, luminescence, and
 magnetic properties.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2838
_journal_page_last               2850
_journal_paper_doi               10.1021/ic503004j
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C15 H21 N O7 U'
_chemical_formula_weight         565.36
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                101.364(5)
_cell_angle_beta                 112.692(4)
_cell_angle_gamma                105.953(5)
_cell_formula_units_Z            2
_cell_length_a                   8.8534(8)
_cell_length_b                   10.6080(11)
_cell_length_c                   10.8364(9)
_cell_measurement_reflns_used    51106
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.71
_cell_volume                     848.45(15)
_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    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 φ and 13 ω scans with 2° steps (695 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  0.0739
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            51106
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.602
_exptl_absorpt_correction_T_max  0.383
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0318
_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)+(0.0090P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                4261
_reflns_number_total             5181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic503004j_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4342516--4342524.cif.'
_cod_original_cell_volume        848.46(15)
_cod_database_code               4342517
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
U1 U 0.82382(2) 0.302407(13) 0.723434(14) 0.02188(5) Uani 1 1 d .
O1 O 1.0133(4) 0.3932(3) 0.7098(3) 0.0331(7) Uani 1 1 d .
O2 O 0.6341(4) 0.2059(3) 0.7350(3) 0.0322(7) Uani 1 1 d .
O3 O 0.6693(4) 0.1798(3) 0.4683(3) 0.0359(8) Uani 1 1 d .
O4 O 0.6343(4) 0.3723(2) 0.5389(3) 0.0309(7) Uani 1 1 d .
O5 O 0.1760(4) 0.4906(3) 0.1619(3) 0.0380(8) Uani 1 1 d .
O6 O 0.0007(4) 0.3229(3) -0.0450(3) 0.0322(7) Uani 1 1 d .
O7 O 0.8814(4) 0.0915(2) 0.6670(3) 0.0291(7) Uani 1 1 d .
N1 N 0.8538(5) -0.1217(3) 0.5487(3) 0.0265(8) Uani 1 1 d .
C1 C 0.5076(5) 0.2579(3) 0.2845(4) 0.0211(8) Uani 1 1 d .
C2 C 0.3673(6) 0.3227(3) 0.2605(4) 0.0202(8) Uani 1 1 d .
H2A H 0.2782 0.2739 0.2869 0.024 Uiso 1 1 calc R
H2B H 0.4251 0.4222 0.3216 0.024 Uiso 1 1 calc R
C3 C 0.2749(5) 0.3104(3) 0.1035(4) 0.0203(8) Uani 1 1 d .
C4 C 0.4173(6) 0.3897(4) 0.0667(4) 0.0275(9) Uani 1 1 d .
H4A H 0.3600 0.3848 -0.0337 0.033 Uiso 1 1 calc R
H4B H 0.4750 0.4892 0.1279 0.033 Uiso 1 1 calc R
C5 C 0.5568(6) 0.3267(4) 0.0890(4) 0.0293(9) Uani 1 1 d .
H5 H 0.6471 0.3784 0.0639 0.035 Uiso 1 1 calc R
C6 C 0.6481(6) 0.3385(4) 0.2458(4) 0.0286(9) Uani 1 1 d .
H6A H 0.7065 0.4378 0.3073 0.034 Uiso 1 1 calc R
H6B H 0.7403 0.2989 0.2618 0.034 Uiso 1 1 calc R
C7 C 0.4196(6) 0.1032(4) 0.1878(4) 0.0277(9) Uani 1 1 d .
H7A H 0.5107 0.0627 0.2022 0.033 Uiso 1 1 calc R
H7B H 0.3313 0.0497 0.2124 0.033 Uiso 1 1 calc R
C8 C 0.3280(6) 0.0937(4) 0.0322(4) 0.0303(10) Uani 1 1 d .
H8 H 0.2698 -0.0065 -0.0303 0.036 Uiso 1 1 calc R
C9 C 0.1871(6) 0.1558(4) 0.0095(4) 0.0276(9) Uani 1 1 d .
H9A H 0.0976 0.1042 0.0340 0.033 Uiso 1 1 calc R
H9B H 0.1258 0.1470 -0.0918 0.033 Uiso 1 1 calc R
C10 C 0.4668(7) 0.1730(4) -0.0065(4) 0.0363(11) Uani 1 1 d .
H10A H 0.5568 0.1315 0.0067 0.044 Uiso 1 1 calc R
H10B H 0.4084 0.1656 -0.1076 0.044 Uiso 1 1 calc R
C11 C 0.6061(6) 0.2703(4) 0.4386(4) 0.0261(9) Uani 1 1 d .
C12 C 0.1405(6) 0.3778(3) 0.0727(4) 0.0217(8) Uani 1 1 d .
C13 C 0.7951(6) -0.0215(4) 0.5649(4) 0.0255(9) Uani 1 1 d .
H13 H 0.6806 -0.0357 0.4951 0.031 Uiso 1 1 calc R
C14 C 0.7468(6) -0.2528(4) 0.4284(4) 0.0334(10) Uani 1 1 d .
H14A H 0.6388 -0.2465 0.3621 0.050 Uiso 1 1 calc R
H14B H 0.7145 -0.3294 0.4632 0.050 Uiso 1 1 calc R
H14C H 0.8156 -0.2703 0.3794 0.050 Uiso 1 1 calc R
C15 C 1.0282(6) -0.1081(4) 0.6509(4) 0.0330(10) Uani 1 1 d .
H15A H 1.0973 -0.0108 0.7142 0.049 Uiso 1 1 calc R
H15B H 1.0904 -0.1364 0.5999 0.049 Uiso 1 1 calc R
H15C H 1.0139 -0.1680 0.7072 0.049 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'
N N 0.0061 0.0033 '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 U1 O2 178.08(11) . .
O1 U1 O5 90.79(12) . 2_666
O2 U1 O5 91.11(12) . 2_666
O1 U1 O6 90.76(13) . 1_656
O2 U1 O6 89.25(13) . 1_656
O5 U1 O6 81.77(10) 2_666 1_656
O1 U1 O3 89.71(12) . .
O2 U1 O3 89.39(12) . .
O5 U1 O3 126.16(10) 2_666 .
O6 U1 O3 152.05(9) 1_656 .
O1 U1 O7 87.81(11) . .
O2 U1 O7 90.29(11) . .
O5 U1 O7 164.42(10) 2_666 .
O6 U1 O7 82.73(9) 1_656 .
O3 U1 O7 69.37(9) . .
O1 U1 O4 91.36(12) . .
O2 U1 O4 89.44(12) . .
O5 U1 O4 73.11(9) 2_666 .
O6 U1 O4 154.82(9) 1_656 .
O3 U1 O4 53.06(8) . .
O7 U1 O4 122.43(8) . .
C11 O3 U1 94.5(2) . .
C11 O4 U1 93.3(2) . .
C12 O5 U1 164.6(3) . 2_666
C12 O6 U1 154.2(3) . 1_454
C13 O7 U1 132.7(3) . .
C13 N1 C15 121.6(3) . .
C13 N1 C14 121.8(4) . .
C15 N1 C14 116.6(3) . .
C11 C1 C2 112.1(3) . .
C11 C1 C7 110.1(3) . .
C2 C1 C7 110.2(3) . .
C11 C1 C6 106.9(3) . .
C2 C1 C6 108.7(3) . .
C7 C1 C6 108.7(3) . .
C3 C2 C1 109.9(3) . .
C3 C2 H2A 109.7 . .
C1 C2 H2A 109.7 . .
C3 C2 H2B 109.7 . .
C1 C2 H2B 109.7 . .
H2A C2 H2B 108.2 . .
C12 C3 C9 110.7(3) . .
C12 C3 C2 113.0(3) . .
C9 C3 C2 109.3(3) . .
C12 C3 C4 106.0(3) . .
C9 C3 C4 109.4(3) . .
C2 C3 C4 108.3(3) . .
C5 C4 C3 110.5(3) . .
C5 C4 H4A 109.6 . .
C3 C4 H4A 109.6 . .
C5 C4 H4B 109.6 . .
C3 C4 H4B 109.6 . .
H4A C4 H4B 108.1 . .
C4 C5 C6 109.1(3) . .
C4 C5 C10 109.3(4) . .
C6 C5 C10 109.9(3) . .
C4 C5 H5 109.5 . .
C6 C5 H5 109.5 . .
C10 C5 H5 109.5 . .
C5 C6 C1 109.4(3) . .
C5 C6 H6A 109.8 . .
C1 C6 H6A 109.8 . .
C5 C6 H6B 109.8 . .
C1 C6 H6B 109.8 . .
H6A C6 H6B 108.2 . .
C8 C7 C1 109.1(3) . .
C8 C7 H7A 109.9 . .
C1 C7 H7A 109.9 . .
C8 C7 H7B 109.9 . .
C1 C7 H7B 109.9 . .
H7A C7 H7B 108.3 . .
C7 C8 C9 110.0(3) . .
C7 C8 C10 109.5(4) . .
C9 C8 C10 109.9(3) . .
C7 C8 H8 109.1 . .
C9 C8 H8 109.1 . .
C10 C8 H8 109.1 . .
C8 C9 C3 109.8(3) . .
C8 C9 H9A 109.7 . .
C3 C9 H9A 109.7 . .
C8 C9 H9B 109.7 . .
C3 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
C5 C10 C8 109.4(3) . .
C5 C10 H10A 109.8 . .
C8 C10 H10A 109.8 . .
C5 C10 H10B 109.8 . .
C8 C10 H10B 109.8 . .
H10A C10 H10B 108.2 . .
O4 C11 O3 119.0(4) . .
O4 C11 C1 121.5(3) . .
O3 C11 C1 119.5(3) . .
O5 C12 O6 121.8(4) . .
O5 C12 C3 118.9(4) . .
O6 C12 C3 119.2(3) . .
O7 C13 N1 123.8(4) . .
O7 C13 H13 118.1 . .
N1 C13 H13 118.1 . .
N1 C14 H14A 109.5 . .
N1 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N1 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N1 C15 H15A 109.5 . .
N1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
N1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.768(3) .
U1 O2 1.775(3) .
U1 O5 2.299(2) 2_666
U1 O6 2.316(3) 1_656
U1 O3 2.427(3) .
U1 O7 2.443(2) .
U1 O4 2.458(3) .
O3 C11 1.271(5) .
O4 C11 1.262(4) .
O5 C12 1.252(4) .
O5 U1 2.299(2) 2_666
O6 C12 1.262(5) .
O6 U1 2.316(3) 1_454
O7 C13 1.251(4) .
N1 C13 1.316(5) .
N1 C15 1.458(5) .
N1 C14 1.463(5) .
C1 C11 1.514(5) .
C1 C2 1.541(5) .
C1 C7 1.545(4) .
C1 C6 1.553(5) .
C2 C3 1.536(5) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C12 1.514(5) .
C3 C9 1.536(5) .
C3 C4 1.547(5) .
C4 C5 1.523(6) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.535(5) .
C5 C10 1.532(5) .
C5 H5 1.0000 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.530(5) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.526(6) .
C8 C10 1.537(6) .
C8 H8 1.0000 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C13 H13 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
