#------------------------------------------------------------------------------
#$Date: 2020-02-04 22:42:09 +0200 (Tue, 04 Feb 2020) $
#$Revision: 247750 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/30/7703096.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_7703096
loop_
_publ_author_name
'Thuéry, Pierre'
'Atoini, Youssef'
'Harrowfield, Jack'
_publ_section_title
;
 Zero-, mono- and diperiodic uranyl ion complexes with the diphenate
 dianion: influences of transition metal ion coordination and differential
 UVI chelation.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              817
_journal_page_last               828
_journal_paper_doi               10.1039/c9dt04126e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C14 H8 O6 U'
_chemical_formula_weight         510.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                92.354(7)
_cell_angle_beta                 116.196(5)
_cell_angle_gamma                111.110(6)
_cell_formula_units_Z            2
_cell_length_a                   9.3038(10)
_cell_length_b                   9.3958(8)
_cell_length_c                   9.9840(15)
_cell_measurement_reflns_used    32551
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.73
_cell_volume                     709.40(16)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and ten ω scans with 2° steps (734 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  0.0909
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32551
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         3.728
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.464
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.389
_exptl_crystal_description       platelet
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.095
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0316
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2207
_reflns_number_total             2687
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04126e1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7703096--7703104.cif.'
_cod_database_code               7703096
_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 0.52224(3) 1.22322(3) 0.95942(2) 0.02171(9) Uani 1 1 d . .
O1 O 0.2961(5) 1.1632(5) 0.8955(4) 0.0220(11) Uani 1 1 d . .
O2 O 0.7496(5) 1.2802(5) 1.0286(4) 0.0218(11) Uani 1 1 d . .
O3 O 0.4169(5) 1.0895(5) 0.6961(4) 0.0265(11) Uani 1 1 d . .
O4 O 0.4694(5) 0.9443(5) 0.8614(4) 0.0235(11) Uani 1 1 d . .
O5 O 0.4194(5) 0.5780(5) 0.8546(4) 0.0234(11) Uani 1 1 d . .
O6 O 0.5449(5) 0.4235(5) 0.8288(4) 0.0258(11) Uani 1 1 d . .
C1 C 0.3010(7) 0.8128(7) 0.5924(6) 0.0186(14) Uani 1 1 d . .
C2 C 0.3809(8) 0.7169(8) 0.5828(6) 0.0216(15) Uani 1 1 d . .
C3 C 0.2793(8) 0.5792(8) 0.4654(6) 0.0277(17) Uani 1 1 d . .
H3 H 0.3323 0.5125 0.4560 0.033 Uiso 1 1 calc R U
C4 C 0.1013(9) 0.5378(8) 0.3618(7) 0.0297(17) Uani 1 1 d . .
H4 H 0.0321 0.4419 0.2851 0.036 Uiso 1 1 calc R U
C5 C 0.0272(8) 0.6402(8) 0.3733(7) 0.0286(18) Uani 1 1 d . .
H5 H -0.0921 0.6161 0.3010 0.034 Uiso 1 1 calc R U
C6 C 0.1254(8) 0.7752(8) 0.4881(6) 0.0236(15) Uani 1 1 d . .
H6 H 0.0734 0.8432 0.4964 0.028 Uiso 1 1 calc R U
C7 C 0.5750(8) 0.7654(8) 0.6819(6) 0.0218(15) Uani 1 1 d . .
C8 C 0.6425(8) 0.6777(7) 0.7813(6) 0.0205(15) Uani 1 1 d . .
C9 C 0.8228(8) 0.7158(8) 0.8606(6) 0.0254(16) Uani 1 1 d . .
H9 H 0.8652 0.6508 0.9227 0.030 Uiso 1 1 calc R U
C10 C 0.9393(8) 0.8483(8) 0.8482(7) 0.0282(17) Uani 1 1 d . .
H10 H 1.0629 0.8776 0.9047 0.034 Uiso 1 1 calc R U
C11 C 0.8735(8) 0.9393(8) 0.7514(6) 0.0258(17) Uani 1 1 d . .
H11 H 0.9529 1.0311 0.7427 0.031 Uiso 1 1 calc R U
C12 C 0.6935(8) 0.8963(7) 0.6685(6) 0.0229(16) Uani 1 1 d . .
H12 H 0.6507 0.9576 0.6013 0.027 Uiso 1 1 calc R U
C13 C 0.4021(7) 0.9583(8) 0.7207(7) 0.0233(16) Uani 1 1 d . .
C14 C 0.5273(8) 0.5494(8) 0.8239(6) 0.0220(15) 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 178.06(17) . .
O1 U1 O5 88.39(17) . 2_677
O2 U1 O5 91.27(16) . 2_677
O1 U1 O6 94.72(17) . 1_565
O2 U1 O6 87.11(17) . 1_565
O5 U1 O6 81.53(15) 2_677 1_565
O1 U1 O4 88.79(16) . 2_677
O2 U1 O4 89.29(16) . 2_677
O5 U1 O4 88.25(14) 2_677 2_677
O6 U1 O4 169.08(14) 1_565 2_677
O1 U1 O3 83.54(16) . .
O2 U1 O3 97.54(15) . .
O5 U1 O3 154.87(16) 2_677 .
O6 U1 O3 75.50(15) 1_565 .
O4 U1 O3 115.22(15) 2_677 .
O1 U1 O4 91.11(17) . .
O2 U1 O4 88.31(17) . .
O5 U1 O4 152.56(13) 2_677 .
O6 U1 O4 125.82(13) 1_565 .
O4 U1 O4 64.31(14) 2_677 .
O3 U1 O4 51.74(13) . .
C13 O3 U1 97.0(4) . .
C13 O4 U1 148.7(4) . 2_677
C13 O4 U1 90.9(4) . .
U1 O4 U1 115.69(14) 2_677 .
C14 O5 U1 129.0(4) . 2_677
C14 O6 U1 140.5(4) . 1_545
C2 C1 C6 121.3(6) . .
C2 C1 C13 120.2(5) . .
C6 C1 C13 118.5(6) . .
C1 C2 C3 118.1(6) . .
C1 C2 C7 121.8(6) . .
C3 C2 C7 119.7(6) . .
C4 C3 C2 121.2(7) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C5 C4 C3 118.7(6) . .
C5 C4 H4 120.7 . .
C3 C4 H4 120.7 . .
C6 C5 C4 120.5(6) . .
C6 C5 H5 119.7 . .
C4 C5 H5 119.7 . .
C5 C6 C1 120.1(7) . .
C5 C6 H6 120.0 . .
C1 C6 H6 120.0 . .
C12 C7 C8 118.0(6) . .
C12 C7 C2 119.4(6) . .
C8 C7 C2 122.5(5) . .
C9 C8 C7 121.5(6) . .
C9 C8 C14 116.3(6) . .
C7 C8 C14 121.7(5) . .
C10 C9 C8 119.7(6) . .
C10 C9 H9 120.2 . .
C8 C9 H9 120.2 . .
C9 C10 C11 119.2(6) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
C12 C11 C10 120.5(6) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C7 121.0(6) . .
C11 C12 H12 119.5 . .
C7 C12 H12 119.5 . .
O3 C13 O4 119.2(6) . .
O3 C13 C1 122.1(5) . .
O4 C13 C1 118.6(6) . .
O6 C14 O5 124.1(6) . .
O6 C14 C8 118.4(6) . .
O5 C14 C8 117.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.756(4) .
U1 O2 1.761(4) .
U1 O5 2.307(4) 2_677
U1 O6 2.334(4) 1_565
U1 O4 2.425(4) 2_677
U1 O3 2.453(4) .
U1 O4 2.550(5) .
O3 C13 1.237(8) .
O4 C13 1.296(6) .
O4 U1 2.425(4) 2_677
O5 C14 1.279(7) .
O5 U1 2.307(4) 2_677
O6 C14 1.251(8) .
O6 U1 2.334(4) 1_545
C1 C2 1.383(9) .
C1 C6 1.389(8) .
C1 C13 1.503(8) .
C2 C3 1.399(9) .
C2 C7 1.497(8) .
C3 C4 1.398(8) .
C3 H3 0.9500 .
C4 C5 1.397(9) .
C4 H4 0.9500 .
C5 C6 1.371(9) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C12 1.383(8) .
C7 C8 1.396(8) .
C8 C9 1.393(8) .
C8 C14 1.515(8) .
C9 C10 1.378(8) .
C9 H9 0.9500 .
C10 C11 1.401(9) .
C10 H10 0.9500 .
C11 C12 1.383(8) .
C11 H11 0.9500 .
C12 H12 0.9500 .
