#------------------------------------------------------------------------------
#$Date: 2015-06-07 01:09:23 +0300 (Sun, 07 Jun 2015) $
#$Revision: 138539 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/02/7220260.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_7220260
loop_
_publ_author_name
'Thuéry, Pierre'
'Harrowfield, Jack'
_publ_section_title
;
 Solvent effects in solvo-hydrothermal synthesis of uranyl ion complexes
 with 1,3-adamantanediacetate
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              4006
_journal_paper_doi               10.1039/C5CE00401B
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C14 H20 O7 U'
_chemical_formula_weight         538.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-02-03 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                92.036(3)
_cell_angle_beta                 97.215(4)
_cell_angle_gamma                94.435(4)
_cell_formula_units_Z            2
_cell_length_a                   6.3900(3)
_cell_length_b                   9.8657(6)
_cell_length_c                   12.5336(9)
_cell_measurement_reflns_used    45680
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      3.28
_cell_volume                     780.72(8)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_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 (821 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  0.0686
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45680
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.280
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.427
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_correction_T_min  0.247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.290
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.164
_refine_diff_density_min         -2.028
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0159P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4311
_reflns_number_total             4756
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00401b1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7220260--7220264.cif.'
_cod_database_code               7220260
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
U1 U -0.00761(2) 0.24989(2) 0.41421(2) 0.01977(5) Uani 1 1 d . .
O1 O -0.1467(5) 0.1504(2) 0.3048(2) 0.0260(6) Uani 1 1 d . .
O2 O 0.1314(5) 0.3531(2) 0.5239(2) 0.0280(6) Uani 1 1 d . .
O3 O 0.0229(5) 0.4342(2) 0.2880(2) 0.0290(6) Uani 1 1 d . .
O4 O 0.2958(5) 0.3115(2) 0.3175(2) 0.0253(6) Uani 1 1 d . .
O5 O 0.2002(4) 1.0757(2) 0.4504(2) 0.0246(6) Uani 1 1 d . .
O6 O 0.2138(5) 0.8548(2) 0.4651(2) 0.0256(6) Uani 1 1 d . .
O7 O -0.3101(5) 0.3844(2) 0.4194(2) 0.0291(6) Uani 1 1 d . .
H7A H -0.2729 0.4678 0.4158 0.035 Uiso 1 1 d R U
H7B H -0.3988 0.3448 0.3550 0.035 Uiso 1 1 d R U
C1 C 0.2824(6) 0.6239(3) 0.1598(3) 0.0188(7) Uani 1 1 d . .
C2 C 0.3528(6) 0.7147(3) 0.2620(3) 0.0186(7) Uani 1 1 d . .
H2A H 0.5015 0.7009 0.2893 0.022 Uiso 1 1 calc R U
H2B H 0.2637 0.6887 0.3183 0.022 Uiso 1 1 calc R U
C3 C 0.3339(6) 0.8665(3) 0.2384(3) 0.0173(7) Uani 1 1 d . .
C4 C 0.1061(6) 0.8887(3) 0.1934(3) 0.0203(7) Uani 1 1 d . .
H4A H 0.0958 0.9857 0.1773 0.024 Uiso 1 1 calc R U
H4B H 0.0110 0.8659 0.2480 0.024 Uiso 1 1 calc R U
C5 C 0.0359(6) 0.7994(3) 0.0906(3) 0.0210(7) Uani 1 1 d . .
H5 H -0.1138 0.8138 0.0626 0.025 Uiso 1 1 calc R U
C6 C 0.0530(6) 0.6482(3) 0.1172(3) 0.0214(8) Uani 1 1 d . .
H6A H -0.0404 0.6237 0.1720 0.026 Uiso 1 1 calc R U
H6B H 0.0056 0.5895 0.0516 0.026 Uiso 1 1 calc R U
C7 C 0.4230(6) 0.6650(3) 0.0730(3) 0.0211(7) Uani 1 1 d . .
H7C H 0.5719 0.6496 0.0985 0.025 Uiso 1 1 calc R U
H7D H 0.3776 0.6076 0.0065 0.025 Uiso 1 1 calc R U
C8 C 0.4075(7) 0.8147(3) 0.0482(3) 0.0239(8) Uani 1 1 d . .
H8 H 0.5019 0.8397 -0.0072 0.029 Uiso 1 1 calc R U
C9 C 0.4779(6) 0.9031(3) 0.1512(3) 0.0235(8) Uani 1 1 d . .
H9A H 0.4709 1.0003 0.1352 0.028 Uiso 1 1 calc R U
H9B H 0.6265 0.8887 0.1784 0.028 Uiso 1 1 calc R U
C10 C 0.1810(7) 0.8373(3) 0.0052(3) 0.0245(8) Uani 1 1 d . .
H10A H 0.1359 0.7804 -0.0616 0.029 Uiso 1 1 calc R U
H10B H 0.1706 0.9339 -0.0121 0.029 Uiso 1 1 calc R U
C11 C 0.3121(7) 0.4734(3) 0.1807(3) 0.0247(8) Uani 1 1 d . .
H11A H 0.2651 0.4203 0.1122 0.030 Uiso 1 1 calc R U
H11B H 0.4658 0.4647 0.1983 0.030 Uiso 1 1 calc R U
C12 C 0.2027(7) 0.4061(3) 0.2671(3) 0.0235(8) Uani 1 1 d . .
C13 C 0.4112(6) 0.9617(3) 0.3378(3) 0.0221(8) Uani 1 1 d . .
H13A H 0.5491 0.9339 0.3713 0.027 Uiso 1 1 calc R U
H13B H 0.4357 1.0553 0.3134 0.027 Uiso 1 1 calc R U
C14 C 0.2637(6) 0.9644(3) 0.4224(3) 0.0198(7) 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'
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 179.04(11) . .
O1 U1 O5 88.86(12) . 1_545
O2 U1 O5 92.04(12) . 1_545
O1 U1 O6 91.60(10) . 2_566
O2 U1 O6 88.81(10) . 2_566
O5 U1 O6 83.82(9) 1_545 2_566
O1 U1 O7 89.86(12) . .
O2 U1 O7 89.42(12) . .
O5 U1 O7 157.80(8) 1_545 .
O6 U1 O7 74.06(9) 2_566 .
O1 U1 O4 93.75(10) . .
O2 U1 O4 86.14(10) . .
O5 U1 O4 77.81(8) 1_545 .
O6 U1 O4 160.74(11) 2_566 .
O7 U1 O4 124.39(8) . .
O1 U1 O3 86.81(10) . .
O2 U1 O3 92.36(11) . .
O5 U1 O3 130.16(8) 1_545 .
O6 U1 O3 145.88(10) 2_566 .
O7 U1 O3 71.86(8) . .
O4 U1 O3 53.05(9) . .
C12 O3 U1 93.9(2) . .
C12 O4 U1 93.3(2) . .
C14 O5 U1 149.8(3) . 1_565
C14 O6 U1 145.6(2) . 2_566
U1 O7 H7A 110.4 . .
U1 O7 H7B 99.0 . .
H7A O7 H7B 113.8 . .
C2 C1 C6 108.9(3) . .
C2 C1 C11 111.3(3) . .
C6 C1 C11 112.8(3) . .
C2 C1 C7 109.0(3) . .
C6 C1 C7 108.0(3) . .
C11 C1 C7 106.7(3) . .
C1 C2 C3 110.8(3) . .
C1 C2 H2A 109.5 . .
C3 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
C3 C2 H2B 109.5 . .
H2A C2 H2B 108.1 . .
C4 C3 C13 111.1(3) . .
C4 C3 C2 110.1(3) . .
C13 C3 C2 112.5(3) . .
C4 C3 C9 108.2(3) . .
C13 C3 C9 107.2(2) . .
C2 C3 C9 107.7(3) . .
C3 C4 C5 110.4(3) . .
C3 C4 H4A 109.6 . .
C5 C4 H4A 109.6 . .
C3 C4 H4B 109.6 . .
C5 C4 H4B 109.6 . .
H4A C4 H4B 108.1 . .
C4 C5 C10 109.4(3) . .
C4 C5 C6 108.9(3) . .
C10 C5 C6 109.5(3) . .
C4 C5 H5 109.7 . .
C10 C5 H5 109.7 . .
C6 C5 H5 109.7 . .
C1 C6 C5 110.4(3) . .
C1 C6 H6A 109.6 . .
C5 C6 H6A 109.6 . .
C1 C6 H6B 109.6 . .
C5 C6 H6B 109.6 . .
H6A C6 H6B 108.1 . .
C8 C7 C1 110.7(3) . .
C8 C7 H7C 109.5 . .
C1 C7 H7C 109.5 . .
C8 C7 H7D 109.5 . .
C1 C7 H7D 109.5 . .
H7C C7 H7D 108.1 . .
C10 C8 C7 109.5(3) . .
C10 C8 C9 109.9(3) . .
C7 C8 C9 109.3(3) . .
C10 C8 H8 109.4 . .
C7 C8 H8 109.4 . .
C9 C8 H8 109.4 . .
C8 C9 C3 110.4(3) . .
C8 C9 H9A 109.6 . .
C3 C9 H9A 109.6 . .
C8 C9 H9B 109.6 . .
C3 C9 H9B 109.6 . .
H9A C9 H9B 108.1 . .
C8 C10 C5 109.3(3) . .
C8 C10 H10A 109.8 . .
C5 C10 H10A 109.8 . .
C8 C10 H10B 109.8 . .
C5 C10 H10B 109.8 . .
H10A C10 H10B 108.3 . .
C12 C11 C1 119.0(3) . .
C12 C11 H11A 107.6 . .
C1 C11 H11A 107.6 . .
C12 C11 H11B 107.6 . .
C1 C11 H11B 107.6 . .
H11A C11 H11B 107.0 . .
O3 C12 O4 119.6(3) . .
O3 C12 C11 123.0(4) . .
O4 C12 C11 117.4(4) . .
C14 C13 C3 115.4(3) . .
C14 C13 H13A 108.4 . .
C3 C13 H13A 108.4 . .
C14 C13 H13B 108.4 . .
C3 C13 H13B 108.4 . .
H13A C13 H13B 107.5 . .
O5 C14 O6 122.3(3) . .
O5 C14 C13 119.1(3) . .
O6 C14 C13 118.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.760(3) .
U1 O2 1.780(3) .
U1 O5 2.276(3) 1_545
U1 O6 2.343(2) 2_566
U1 O7 2.434(3) .
U1 O4 2.461(2) .
U1 O3 2.465(2) .
O3 C12 1.258(5) .
O4 C12 1.287(5) .
O5 C14 1.253(4) .
O5 U1 2.276(3) 1_565
O6 C14 1.260(4) .
O6 U1 2.343(2) 2_566
O7 H7A 0.8432 .
O7 H7B 0.9772 .
C1 C2 1.535(4) .
C1 C6 1.536(5) .
C1 C11 1.539(4) .
C1 C7 1.542(4) .
C2 C3 1.548(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.529(5) .
C3 C13 1.539(4) .
C3 C9 1.550(4) .
C4 C5 1.534(4) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C10 1.539(4) .
C5 C6 1.548(4) .
C5 H5 1.0000 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.528(5) .
C7 H7C 0.9900 .
C7 H7D 0.9900 .
C8 C10 1.516(6) .
C8 C9 1.531(4) .
C8 H8 1.0000 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.508(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C13 C14 1.506(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
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
O7 H7A O2 0.84 2.00 2.779(3) 153.5 2_566
O7 H7B O4 0.98 1.95 2.709(4) 132.8 1_455
