#------------------------------------------------------------------------------
#$Date: 2022-06-24 02:16:54 +0300 (Fri, 24 Jun 2022) $
#$Revision: 276211 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/05/7710579.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_7710579
loop_
_publ_author_name
'Brager, Dominique M.'
'Marwitz, Alexander C.'
'Cahill, Christopher L.'
_publ_section_title
;
 A spectroscopic, structural, and computational study of Ag-oxo
 interactions in Ag⁺/UO₂²⁺ complexes.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt01161a
_journal_year                    2022
_chemical_formula_moiety         'C9 H3 Cl2 O8 U, C8 H6 Ag N4'
_chemical_formula_sum            'C17 H9 Ag Cl2 N4 O8 U'
_chemical_formula_weight         814.08
_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_update_record
;
2022-05-20 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                99.151(5)
_cell_angle_beta                 98.695(5)
_cell_angle_gamma                107.432(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0510(13)
_cell_length_b                   10.4720(14)
_cell_length_c                   12.0195(16)
_cell_measurement_reflns_used    6474
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.41
_cell_volume                     1048.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13266
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.097
_diffrn_reflns_theta_min         2.088
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    8.953
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    2.578
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.754
_refine_diff_density_min         -3.136
_refine_diff_density_rms         0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4622
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0423
_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)+(0.0538P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3990
_reflns_number_total             4622
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01161a2.cif
_cod_data_source_block           Cmpd6_DMB2_25_C
_cod_database_code               7710579
_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.
;
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.28240(2) 0.69071(3) 0.91534(2) 0.01306(9) Uani 1 1 d . . . . .
Ag1 Ag 0.03197(7) 0.93936(7) 0.74656(4) 0.02360(15) Uani 1 1 d . . . . .
Cl1 Cl 0.2082(2) 0.4246(2) 0.41768(15) 0.0320(5) Uani 1 1 d . . . . .
Cl2 Cl 0.5129(3) 0.1027(2) 0.71951(16) 0.0335(5) Uani 1 1 d . . . . .
O1 O 0.4000(5) 0.6539(5) 1.0297(4) 0.0164(10) Uani 1 1 d . . . . .
O2 O 0.1616(6) 0.7268(6) 0.8029(4) 0.0198(11) Uani 1 1 d . . . . .
O3 O -0.0938(5) 0.3235(6) 0.9575(4) 0.0198(11) Uani 1 1 d . . . . .
O4 O 0.0839(5) 0.4653(5) 0.8837(4) 0.0174(10) Uani 1 1 d . U . . .
O5 O 0.5176(5) 0.8672(5) 0.9015(4) 0.0169(10) Uani 1 1 d . . . . .
O6 O 0.6832(5) 1.0837(5) 0.9707(4) 0.0167(10) Uani 1 1 d . . . . .
O7 O 0.3688(5) 0.5520(6) 0.7932(4) 0.0216(11) Uani 1 1 d . . . . .
O8 O 0.3652(7) 0.6305(6) 0.6300(5) 0.0310(13) Uani 1 1 d . . . . .
N1 N 0.0834(7) 0.8879(7) 0.5691(5) 0.0211(13) Uani 1 1 d . . . . .
N2 N 0.0411(7) 0.9111(7) 0.3739(5) 0.0210(13) Uani 1 1 d . . . . .
N3 N 0.1191(6) 1.1049(6) 0.9198(5) 0.0159(12) Uani 1 1 d . . . . .
N4 N 0.1013(6) 1.1490(7) 1.1157(4) 0.0178(12) Uani 1 1 d . . . . .
C1 C -0.0032(7) 0.4391(7) 0.9532(5) 0.0143(13) Uani 1 1 d . U . . .
C2 C 0.5580(8) 0.9848(8) 0.9634(6) 0.0167(14) Uani 1 1 d . . . . .
C3 C 0.3648(8) 0.5397(8) 0.6838(6) 0.0202(15) Uani 1 1 d . U . . .
C4 C 0.3662(8) 0.4028(8) 0.6239(6) 0.0181(14) Uani 1 1 d . U . . .
C5 C 0.3102(8) 0.3485(8) 0.5053(6) 0.0214(15) Uani 1 1 d . U . . .
C6 C 0.3288(9) 0.2276(9) 0.4519(6) 0.0261(17) Uani 1 1 d . U . . .
H6 H 0.296847 0.196898 0.370506 0.031 Uiso 1 1 calc R U . . .
C7 C 0.3941(9) 0.1519(9) 0.5175(6) 0.0268(17) Uani 1 1 d . . . . .
H7 H 0.405927 0.068765 0.481944 0.032 Uiso 1 1 calc R U . . .
C8 C 0.4415(8) 0.2006(9) 0.6361(6) 0.0222(16) Uani 1 1 d . . . . .
C9 C 0.4296(8) 0.3236(8) 0.6881(6) 0.0214(16) Uani 1 1 d . . . . .
H9 H 0.465063 0.355281 0.769271 0.026 Uiso 1 1 calc R U . . .
C10 C 0.0341(8) 0.9450(8) 0.4847(6) 0.0191(15) Uani 1 1 d . . . . .
C11 C 0.1050(9) 0.8136(9) 0.3460(6) 0.0272(18) Uani 1 1 d . . . . .
H11 H 0.109188 0.785640 0.267700 0.033 Uiso 1 1 calc R U . . .
C12 C 0.1651(10) 0.7523(9) 0.4275(7) 0.0298(18) Uani 1 1 d . . . . .
H12 H 0.212891 0.684983 0.407519 0.036 Uiso 1 1 calc R U . . .
C13 C 0.1519(9) 0.7943(9) 0.5397(6) 0.0264(17) Uani 1 1 d . . . . .
H13 H 0.193130 0.755146 0.597993 0.032 Uiso 1 1 calc R U . . .
C14 C 0.0604(7) 1.0711(8) 1.0102(5) 0.0155(14) Uani 1 1 d . . . . .
C15 C 0.2085(8) 1.2742(8) 1.1311(6) 0.0222(16) Uani 1 1 d . . . . .
H15 H 0.240584 1.332217 1.205836 0.027 Uiso 1 1 calc R U . . .
C16 C 0.2741(8) 1.3222(8) 1.0433(6) 0.0198(15) Uani 1 1 d . . . . .
H16 H 0.348786 1.411540 1.054788 0.024 Uiso 1 1 calc R U . . .
C17 C 0.2230(8) 1.2300(9) 0.9358(6) 0.0218(16) Uani 1 1 d . . . . .
H17 H 0.264153 1.258139 0.872205 0.026 Uiso 1 1 calc R U . . .
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
O2 U1 O1 178.8(2) . . ?
O2 U1 O7 94.12(19) . . ?
O1 U1 O7 86.74(19) . . ?
O2 U1 O5 93.0(2) . . ?
O1 U1 O5 87.95(19) . . ?
O7 U1 O5 83.71(17) . . ?
O2 U1 O4 88.6(2) . . ?
O1 U1 O4 90.69(19) . . ?
O7 U1 O4 75.86(17) . . ?
O5 U1 O4 159.57(16) . . ?
O2 U1 O6 87.9(2) . 2_677 ?
O1 U1 O6 91.76(19) . 2_677 ?
O7 U1 O6 150.21(18) . 2_677 ?
O5 U1 O6 66.50(15) . 2_677 ?
O4 U1 O6 133.93(15) . 2_677 ?
O2 U1 O3 94.39(19) . 2_567 ?
O1 U1 O3 84.37(18) . 2_567 ?
O7 U1 O3 140.47(19) . 2_567 ?
O5 U1 O3 134.15(17) . 2_567 ?
O4 U1 O3 65.85(16) . 2_567 ?
O6 U1 O3 68.65(17) 2_677 2_567 ?
N1 Ag1 N4 144.9(2) . 2_577 ?
N1 Ag1 N3 143.0(2) . . ?
N4 Ag1 N3 71.2(2) 2_577 . ?
N1 Ag1 N2 70.0(2) . 2_576 ?
N4 Ag1 N2 126.13(19) 2_577 2_576 ?
N3 Ag1 N2 95.8(2) . 2_576 ?
C1 O3 U1 119.2(4) . 2_567 ?
C1 O4 U1 120.3(4) . . ?
C2 O5 U1 120.4(4) . . ?
C2 O6 U1 119.5(4) . 2_677 ?
C3 O7 U1 130.4(4) . . ?
C13 N1 C10 116.4(6) . . ?
C13 N1 Ag1 123.4(5) . . ?
C10 N1 Ag1 120.0(4) . . ?
C11 N2 C10 117.0(6) . . ?
C11 N2 Ag1 128.0(4) . 2_576 ?
C10 N2 Ag1 114.4(4) . 2_576 ?
C17 N3 C14 116.9(6) . . ?
C17 N3 Ag1 125.5(4) . . ?
C14 N3 Ag1 117.5(5) . . ?
C14 N4 C15 116.6(6) . . ?
C14 N4 Ag1 117.0(5) . 2_577 ?
C15 N4 Ag1 126.3(5) . 2_577 ?
O4 C1 O3 127.2(6) . . ?
O4 C1 C1 116.6(8) . 2_567 ?
O3 C1 C1 116.2(7) . 2_567 ?
O5 C2 O6 126.9(6) . . ?
O5 C2 C2 117.1(8) . 2_677 ?
O6 C2 C2 116.0(8) . 2_677 ?
O8 C3 O7 125.3(7) . . ?
O8 C3 C4 120.4(6) . . ?
O7 C3 C4 114.2(6) . . ?
C5 C4 C9 116.7(7) . . ?
C5 C4 C3 124.0(6) . . ?
C9 C4 C3 119.3(6) . . ?
C6 C5 C4 121.7(6) . . ?
C6 C5 Cl1 116.3(5) . . ?
C4 C5 Cl1 121.9(6) . . ?
C7 C6 C5 120.2(6) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C8 C7 C6 118.4(7) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
C9 C8 C7 121.2(7) . . ?
C9 C8 Cl2 119.9(5) . . ?
C7 C8 Cl2 118.9(6) . . ?
C8 C9 C4 121.5(6) . . ?
C8 C9 H9 119.3 . . ?
C4 C9 H9 119.3 . . ?
N2 C10 N1 125.4(6) . . ?
N2 C10 C10 116.6(7) . 2_576 ?
N1 C10 C10 118.0(7) . 2_576 ?
N2 C11 C12 122.1(7) . . ?
N2 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C13 C12 C11 116.5(7) . . ?
C13 C12 H12 121.7 . . ?
C11 C12 H12 121.7 . . ?
N1 C13 C12 122.5(7) . . ?
N1 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
N4 C14 N3 125.8(7) . . ?
N4 C14 C14 117.9(7) . 2_577 ?
N3 C14 C14 116.3(7) . 2_577 ?
N4 C15 C16 122.9(7) . . ?
N4 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
C15 C16 C17 115.3(7) . . ?
C15 C16 H16 122.3 . . ?
C17 C16 H16 122.3 . . ?
N3 C17 C16 122.4(6) . . ?
N3 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.768(4) . ?
U1 O1 1.773(4) . ?
U1 O7 2.287(5) . ?
U1 O5 2.413(5) . ?
U1 O4 2.432(5) . ?
U1 O6 2.441(5) 2_677 ?
U1 O3 2.445(5) 2_567 ?
Ag1 N1 2.267(6) . ?
Ag1 N4 2.340(6) 2_577 ?
Ag1 N3 2.345(6) . ?
Ag1 N2 2.458(6) 2_576 ?
Cl1 C5 1.735(7) . ?
Cl2 C8 1.733(8) . ?
O3 C1 1.256(9) . ?
O4 C1 1.240(8) . ?
O5 C2 1.249(9) . ?
O6 C2 1.266(8) . ?
O7 C3 1.294(8) . ?
O8 C3 1.231(9) . ?
N1 C13 1.338(9) . ?
N1 C10 1.343(8) . ?
N2 C11 1.338(10) . ?
N2 C10 1.339(8) . ?
N3 C17 1.328(10) . ?
N3 C14 1.331(8) . ?
N4 C14 1.326(9) . ?
N4 C15 1.342(10) . ?
C1 C1 1.541(13) 2_567 ?
C2 C2 1.538(13) 2_677 ?
C3 C4 1.503(10) . ?
C4 C5 1.401(9) . ?
C4 C9 1.403(10) . ?
C5 C6 1.395(11) . ?
C6 C7 1.393(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(11) . ?
C9 H9 0.9500 . ?
C10 C10 1.484(13) 2_576 ?
C11 C12 1.384(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(10) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C14 1.516(15) 2_577 ?
C15 C16 1.377(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.404(10) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
