#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:14:39 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179528 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/25/4342523.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_4342523
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            'C24 H28 Cu O10 U'
_chemical_formula_weight         778.03
_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                 110.940(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3216(11)
_cell_length_b                   12.0844(8)
_cell_length_c                   11.9978(6)
_cell_measurement_reflns_used    40022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.37
_cell_volume                     2345.5(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and four ω scans with 2° steps (440 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  0.0396
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            40022
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.862
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light blue'
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.461
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0313
_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)+(0.0583P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                1873
_reflns_number_total             2229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic503004j_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 4342516--4342524.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4342523
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
U1 U 0.5000 0.5000 0.0000 0.02577(12) Uani 1 2 d S
Cu1 Cu 0.5000 0.25225(8) 0.2500 0.0225(2) Uani 1 2 d S
O1 O 0.5522(2) 0.4146(3) -0.0695(3) 0.0336(8) Uani 1 1 d .
O2 O 0.5868(2) 0.4327(3) 0.1817(3) 0.0309(8) Uani 1 1 d .
O3 O 0.6152(2) 0.2703(3) 0.2735(3) 0.0265(8) Uani 1 1 d .
O4 O 0.9131(2) 0.1459(3) 0.4954(3) 0.0305(8) Uani 1 1 d .
O5 O 0.9690(2) 0.3015(3) 0.5871(3) 0.0300(8) Uani 1 1 d .
C1 C 0.7296(3) 0.3701(4) 0.2568(4) 0.0233(10) Uani 1 1 d .
C2 C 0.7821(3) 0.3064(4) 0.3694(4) 0.0231(10) Uani 1 1 d .
H2A H 0.7652 0.2276 0.3620 0.028 Uiso 1 1 calc R
H2B H 0.7735 0.3377 0.4403 0.028 Uiso 1 1 calc R
C3 C 0.8741(3) 0.3157(4) 0.3841(4) 0.0237(10) Uani 1 1 d .
C4 C 0.9003(3) 0.4376(4) 0.3969(4) 0.0277(11) Uani 1 1 d .
H4A H 0.9594 0.4437 0.4065 0.033 Uiso 1 1 calc R
H4B H 0.8931 0.4698 0.4684 0.033 Uiso 1 1 calc R
C5 C 0.8466(4) 0.5009(4) 0.2842(6) 0.0353(14) Uani 1 1 d .
H5 H 0.8635 0.5805 0.2919 0.042 Uiso 1 1 calc R
C6 C 0.7554(4) 0.4926(4) 0.2700(5) 0.0297(12) Uani 1 1 d .
H6A H 0.7211 0.5344 0.1985 0.036 Uiso 1 1 calc R
H6B H 0.7470 0.5248 0.3406 0.036 Uiso 1 1 calc R
C7 C 0.7429(3) 0.3202(5) 0.1464(4) 0.0329(12) Uani 1 1 d .
H7A H 0.7261 0.2414 0.1373 0.039 Uiso 1 1 calc R
H7B H 0.7088 0.3603 0.0735 0.039 Uiso 1 1 calc R
C8 C 0.8352(3) 0.3302(6) 0.1631(4) 0.0392(14) Uani 1 1 d .
H8 H 0.8442 0.2979 0.0920 0.047 Uiso 1 1 calc R
C9 C 0.8874(3) 0.2667(5) 0.2748(4) 0.0305(12) Uani 1 1 d .
H9A H 0.9466 0.2718 0.2848 0.037 Uiso 1 1 calc R
H9B H 0.8714 0.1877 0.2664 0.037 Uiso 1 1 calc R
C10 C 0.8597(4) 0.4504(6) 0.1747(5) 0.0448(15) Uani 1 1 d .
H10A H 0.8260 0.4909 0.1018 0.054 Uiso 1 1 calc R
H10B H 0.9186 0.4573 0.1834 0.054 Uiso 1 1 calc R
C11 C 0.6376(3) 0.3569(4) 0.2370(4) 0.0252(10) Uani 1 1 d .
C12 C 0.9232(2) 0.2508(4) 0.4966(4) 0.0228(9) Uani 1 1 d .
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'
Cu Cu 0.3201 1.2651 '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 O1 180.0 5_665 .
O1 U1 O4 91.03(15) 5_665 8_455
O1 U1 O4 88.97(15) . 8_455
O1 U1 O4 88.97(15) 5_665 4_655
O1 U1 O4 91.03(15) . 4_655
O4 U1 O4 180.0 8_455 4_655
O1 U1 O2 91.74(15) 5_665 .
O1 U1 O2 88.26(15) . .
O4 U1 O2 87.26(12) 8_455 .
O4 U1 O2 92.74(12) 4_655 .
O1 U1 O2 88.26(15) 5_665 5_665
O1 U1 O2 91.74(15) . 5_665
O4 U1 O2 92.74(12) 8_455 5_665
O4 U1 O2 87.26(12) 4_655 5_665
O2 U1 O2 180.0 . 5_665
O3 Cu1 O3 167.0(2) . 2_655
O3 Cu1 O5 89.52(13) . 7_656
O3 Cu1 O5 94.83(13) 2_655 7_656
O3 Cu1 O5 94.83(13) . 8_455
O3 Cu1 O5 89.52(13) 2_655 8_455
O5 Cu1 O5 140.9(2) 7_656 8_455
C11 O2 U1 146.8(3) . .
C11 O3 Cu1 118.6(3) . .
C12 O4 U1 132.2(3) . 4_645
C12 O5 Cu1 124.7(3) . 7_656
C11 C1 C2 109.9(4) . .
C11 C1 C6 111.3(4) . .
C2 C1 C6 109.4(4) . .
C11 C1 C7 107.0(4) . .
C2 C1 C7 109.6(4) . .
C6 C1 C7 109.6(4) . .
C1 C2 C3 109.0(4) . .
C1 C2 H2A 109.9 . .
C3 C2 H2A 109.9 . .
C1 C2 H2B 109.9 . .
C3 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
C9 C3 C12 110.6(4) . .
C9 C3 C4 109.1(4) . .
C12 C3 C4 110.7(4) . .
C9 C3 C2 109.8(4) . .
C12 C3 C2 106.8(4) . .
C4 C3 C2 109.8(4) . .
C3 C4 C5 108.9(4) . .
C3 C4 H4A 109.9 . .
C5 C4 H4A 109.9 . .
C3 C4 H4B 109.9 . .
C5 C4 H4B 109.9 . .
H4A C4 H4B 108.3 . .
C6 C5 C10 109.9(5) . .
C6 C5 C4 110.0(5) . .
C10 C5 C4 108.9(5) . .
C6 C5 H5 109.3 . .
C10 C5 H5 109.3 . .
C4 C5 H5 109.3 . .
C5 C6 C1 109.0(4) . .
C5 C6 H6A 109.9 . .
C1 C6 H6A 109.9 . .
C5 C6 H6B 109.9 . .
C1 C6 H6B 109.9 . .
H6A C6 H6B 108.3 . .
C8 C7 C1 108.9(4) . .
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 . .
C10 C8 C9 110.1(5) . .
C10 C8 C7 109.4(5) . .
C9 C8 C7 109.6(4) . .
C10 C8 H8 109.2 . .
C9 C8 H8 109.2 . .
C7 C8 H8 109.2 . .
C8 C9 C3 109.5(4) . .
C8 C9 H9A 109.8 . .
C3 C9 H9A 109.8 . .
C8 C9 H9B 109.8 . .
C3 C9 H9B 109.8 . .
H9A C9 H9B 108.2 . .
C8 C10 C5 109.8(4) . .
C8 C10 H10A 109.7 . .
C5 C10 H10A 109.7 . .
C8 C10 H10B 109.7 . .
C5 C10 H10B 109.7 . .
H10A C10 H10B 108.2 . .
O3 C11 O2 122.7(4) . .
O3 C11 C1 117.9(4) . .
O2 C11 C1 119.4(4) . .
O5 C12 O4 122.5(4) . .
O5 C12 C3 119.6(4) . .
O4 C12 C3 117.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.764(4) 5_665
U1 O1 1.765(4) .
U1 O4 2.306(3) 8_455
U1 O4 2.306(3) 4_655
U1 O2 2.309(3) .
U1 O2 2.309(3) 5_665
Cu1 O3 1.926(3) .
Cu1 O3 1.926(3) 2_655
Cu1 O5 1.944(3) 7_656
Cu1 O5 1.944(3) 8_455
O2 C11 1.279(6) .
O3 C11 1.248(6) .
O4 C12 1.280(6) .
O4 U1 2.306(3) 4_645
O5 C12 1.252(6) .
O5 Cu1 1.944(3) 7_656
C1 C11 1.533(7) .
C1 C2 1.538(6) .
C1 C6 1.538(6) .
C1 C7 1.546(7) .
C2 C3 1.545(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C9 1.530(6) .
C3 C12 1.530(6) .
C3 C4 1.532(7) .
C4 C5 1.543(8) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.530(9) .
C5 C10 1.538(9) .
C5 H5 1.0000 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.543(7) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C10 1.506(10) .
C8 C9 1.528(7) .
C8 H8 1.0000 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
