#------------------------------------------------------------------------------
#$Date: 2022-06-24 02:16:54 +0300 (Fri, 24 Jun 2022) $
#$Revision: 276211 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/05/7710577.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_7710577
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 H4 Br O8 U, C8 H6 Ag N4'
_chemical_formula_sum            'C17 H10 Ag Br N4 O8 U'
_chemical_formula_weight         824.10
_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
_audit_update_record
;
2022-05-20 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                102.0070(10)
_cell_angle_beta                 103.8250(10)
_cell_angle_gamma                108.3100(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9506(3)
_cell_length_b                   10.6865(4)
_cell_length_c                   12.1235(5)
_cell_measurement_reflns_used    6392
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.234
_cell_measurement_theta_min      4.647
_cell_volume                     1017.36(7)
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  'shelXle (C.B. Huebschle, rev 958)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0346
_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       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11435
_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         26.019
_diffrn_reflns_theta_min         2.109
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    10.930
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.690
_exptl_crystal_description       blocks
_exptl_crystal_F_000             756
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         3990
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0234
_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)+(0.0100P)²+2.1445P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3701
_reflns_number_total             3990
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01161a2.cif
_cod_data_source_block           Cmpd7_DMB2_24_A
_cod_database_code               7710577
_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 0.23581(2) 0.31707(2) 0.09320(2) 0.01494(5) Uani 1 1 d . . . . .
N1 N 0.4564(5) 0.1299(4) 0.4374(3) 0.0190(8) Uani 1 1 d . . . . .
C1 C -0.0499(6) 0.0147(5) 0.0413(4) 0.0202(10) Uani 1 1 d . . . . .
Ag1 Ag 0.51389(5) 0.07006(4) 0.26494(3) 0.02352(9) Uani 1 1 d . . . . .
O1 O 0.0906(4) 0.3437(3) -0.0178(3) 0.0210(7) Uani 1 1 d . . . . .
O2 O 0.3843(4) 0.2913(3) 0.2021(3) 0.0249(7) Uani 1 1 d . . . . .
N2 N 0.4452(5) 0.0847(4) 0.6195(3) 0.0194(8) Uani 1 1 d . . . . .
C2 C 0.5122(5) 0.5645(4) 0.0488(4) 0.0170(9) Uani 1 1 d . . . . .
O4 O 0.0030(4) 0.1376(3) 0.1082(3) 0.0221(7) Uani 1 1 d . . . . .
N4 N 0.6089(4) 0.1074(4) -0.0752(3) 0.0175(8) Uani 1 1 d . . . . .
O5 O 0.4357(4) 0.5445(3) 0.1213(3) 0.0212(7) Uani 1 1 d . . . . .
O7 O 0.1737(4) 0.4496(3) 0.2326(3) 0.0253(7) Uani 1 1 d . . . . .
O6 O 0.6044(4) 0.6782(3) 0.0464(3) 0.0203(7) Uani 1 1 d . . . . .
O8 O 0.2654(5) 0.4558(4) 0.4218(4) 0.0518(11) Uani 1 1 d . . . . .
O3 O -0.1730(4) -0.0850(3) 0.0356(3) 0.0237(7) Uani 1 1 d . . . . .
N3 N 0.6120(5) 0.1564(4) 0.1253(3) 0.0170(8) Uani 1 1 d . . . . .
C3 C 0.2013(6) 0.4987(5) 0.3436(4) 0.0241(11) Uani 1 1 d . . . . .
C4A C 0.136(3) 0.6172(18) 0.3681(14) 0.017(4) Uani 0.5858(15) 1 d . U P A 1
C5A C 0.0839(14) 0.6697(11) 0.2790(9) 0.017(2) Uani 0.5858(15) 1 d . . P A 1
H5A H 0.084894 0.631377 0.201208 0.020 Uiso 0.5858(15) 1 calc R U P A 1
C6A C 0.0301(12) 0.7765(9) 0.2998(9) 0.027(2) Uani 0.5858(15) 1 d . . P A 1
H6A H -0.005935 0.811150 0.236575 0.032 Uiso 0.5858(15) 1 calc R U P A 1
C7A C 0.0281(12) 0.8338(9) 0.4122(10) 0.025(2) Uani 0.5858(15) 1 d . . P A 1
H7A H -0.007471 0.908662 0.427504 0.030 Uiso 0.5858(15) 1 calc R U P A 1
C8A C 0.0799(17) 0.7793(12) 0.5039(12) 0.018(3) Uani 0.5858(15) 1 d . . P A 1
C9A C 0.1338(12) 0.6713(10) 0.4819(9) 0.019(2) Uani 0.5858(15) 1 d . . P A 1
H9A H 0.168667 0.634657 0.543949 0.023 Uiso 0.5858(15) 1 calc R U P A 1
Br1A Br 0.07140(11) 0.85291(9) 0.65644(7) 0.0265(3) Uani 0.5858(15) 1 d . . P A
1
C4B C 0.152(4) 0.603(3) 0.393(2) 0.019(4) Uani 0.4142(15) 1 d . U P A 2
C5B C 0.112(2) 0.685(2) 0.3295(15) 0.029(4) Uani 0.4142(15) 1 d . U P A 2
H5B H 0.111987 0.667074 0.249504 0.034 Uiso 0.4142(15) 1 calc R U P A 2
C6B C 0.0689(17) 0.7966(15) 0.3775(16) 0.025(3) Uani 0.4142(15) 1 d . U P A 2
C7B C 0.067(3) 0.821(2) 0.491(2) 0.025(4) Uani 0.4142(15) 1 d . U P A 2
H7B H 0.040142 0.896787 0.524628 0.030 Uiso 0.4142(15) 1 calc R U P A 2
C8B C 0.1024(16) 0.7382(14) 0.5618(13) 0.029(3) Uani 0.4142(15) 1 d . U P A 2
H8B H 0.093234 0.753336 0.639514 0.035 Uiso 0.4142(15) 1 calc R U P A 2
C9B C 0.152(2) 0.6327(17) 0.5142(15) 0.029(3) Uani 0.4142(15) 1 d . U P A 2
H9B H 0.185581 0.580347 0.562359 0.035 Uiso 0.4142(15) 1 calc R U P A 2
Br1B Br 0.02086(18) 0.91150(13) 0.28882(11) 0.0370(4) Uani 0.4142(15) 1 d . . P
A 2
C14 C 0.5609(5) 0.0726(4) 0.0141(4) 0.0127(9) Uani 1 1 d . . . . .
C10 C 0.4734(5) 0.0594(4) 0.5160(4) 0.0159(9) Uani 1 1 d . . . . .
C15 C 0.7131(6) 0.2365(5) -0.0508(4) 0.0208(10) Uani 1 1 d . . . . .
H15 H 0.747423 0.265001 -0.112924 0.025 Uiso 1 1 calc R U . . .
C11 C 0.3985(6) 0.1917(5) 0.6481(4) 0.0221(10) Uani 1 1 d . . . . .
H11 H 0.377665 0.212643 0.721646 0.027 Uiso 1 1 calc R U . . .
C16 C 0.7737(6) 0.3310(5) 0.0615(4) 0.0205(10) Uani 1 1 d . . . . .
H16 H 0.849917 0.423021 0.078136 0.025 Uiso 1 1 calc R U . . .
C12 C 0.3799(6) 0.2720(5) 0.5744(4) 0.0251(11) Uani 1 1 d . . . . .
H12 H 0.349193 0.348639 0.596142 0.030 Uiso 1 1 calc R U . . .
C17 C 0.7188(6) 0.2859(5) 0.1481(4) 0.0222(10) Uani 1 1 d . . . . .
H17 H 0.757804 0.348501 0.226478 0.027 Uiso 1 1 calc R U . . .
C13 C 0.4083(6) 0.2354(5) 0.4671(4) 0.0222(10) Uani 1 1 d . . . . .
H13 H 0.393200 0.286556 0.412902 0.027 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'
B B 0.0013 0.0007 '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'
Br Br -0.2901 2.4595 '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 178.59(14) . . ?
O2 U1 O7 92.76(13) . . ?
O1 U1 O7 88.25(13) . . ?
O2 U1 O5 90.32(13) . . ?
O1 U1 O5 88.90(12) . . ?
O7 U1 O5 79.26(11) . . ?
O2 U1 O4 93.27(13) . . ?
O1 U1 O4 87.86(12) . . ?
O7 U1 O4 81.31(10) . . ?
O5 U1 O4 160.39(10) . . ?
O2 U1 O3 88.32(13) . 2 ?
O1 U1 O3 91.36(12) . 2 ?
O7 U1 O3 147.44(11) . 2 ?
O5 U1 O3 133.29(10) . 2 ?
O4 U1 O3 66.14(10) . 2 ?
O2 U1 O6 93.54(12) . 2_665 ?
O1 U1 O6 85.06(12) . 2_665 ?
O7 U1 O6 144.47(11) . 2_665 ?
O5 U1 O6 65.78(10) . 2_665 ?
O4 U1 O6 133.07(10) . 2_665 ?
O3 U1 O6 67.72(9) 2 2_665 ?
C13 N1 C10 116.8(4) . . ?
C13 N1 Ag1 123.4(3) . . ?
C10 N1 Ag1 119.7(3) . . ?
O3 C1 O4 127.0(4) . . ?
O3 C1 C1 116.8(5) . 2 ?
O4 C1 C1 116.2(5) . 2 ?
N1 Ag1 N3 143.69(13) . . ?
N1 Ag1 N4 139.15(13) . 2_655 ?
N3 Ag1 N4 70.72(12) . 2_655 ?
N1 Ag1 N2 70.42(12) . 2_656 ?
N3 Ag1 N2 138.63(12) . 2_656 ?
N4 Ag1 N2 95.00(12) 2_655 2_656 ?
C10 N2 C11 116.8(4) . . ?
C10 N2 Ag1 115.3(3) . 2_656 ?
C11 N2 Ag1 127.9(3) . 2_656 ?
O6 C2 O5 126.9(4) . . ?
O6 C2 C2 116.6(5) . 2_665 ?
O5 C2 C2 116.5(5) . 2_665 ?
C1 O4 U1 120.6(3) . . ?
C15 N4 C14 116.8(4) . . ?
C15 N4 Ag1 127.3(3) . 2_655 ?
C14 N4 Ag1 115.9(3) . 2_655 ?
C2 O5 U1 120.8(3) . . ?
C3 O7 U1 145.2(3) . . ?
C2 O6 U1 119.3(3) . 2_665 ?
C1 O3 U1 119.9(3) . 2 ?
C14 N3 C17 116.8(4) . . ?
C14 N3 Ag1 118.6(3) . . ?
C17 N3 Ag1 124.6(3) . . ?
O8 C3 O7 125.1(4) . . ?
O8 C3 C4B 110.5(11) . . ?
O7 C3 C4B 124.2(11) . . ?
O8 C3 C4A 124.1(7) . . ?
O7 C3 C4A 110.8(7) . . ?
C5A C4A C9A 119.9(16) . . ?
C5A C4A C3 120.6(13) . . ?
C9A C4A C3 119.5(12) . . ?
C4A C5A C6A 121.4(12) . . ?
C4A C5A H5A 119.3 . . ?
C6A C5A H5A 119.3 . . ?
C5A C6A C7A 120.2(9) . . ?
C5A C6A H6A 119.9 . . ?
C7A C6A H6A 119.9 . . ?
C6A C7A C8A 118.8(9) . . ?
C6A C7A H7A 120.6 . . ?
C8A C7A H7A 120.6 . . ?
C9A C8A C7A 120.6(11) . . ?
C9A C8A Br1A 120.2(10) . . ?
C7A C8A Br1A 119.1(10) . . ?
C8A C9A C4A 119.2(11) . . ?
C8A C9A H9A 120.4 . . ?
C4A C9A H9A 120.4 . . ?
C5B C4B C3 120(2) . . ?
C5B C4B C9B 118(3) . . ?
C3 C4B C9B 121.5(19) . . ?
C4B C5B C6B 123(2) . . ?
C4B C5B H5B 118.7 . . ?
C6B C5B H5B 118.7 . . ?
C7B C6B C5B 118.5(16) . . ?
C7B C6B Br1B 119.9(15) . . ?
C5B C6B Br1B 121.6(14) . . ?
C6B C7B C8B 122.1(19) . . ?
C6B C7B H7B 119.0 . . ?
C8B C7B H7B 119.0 . . ?
C9B C8B C7B 118.2(15) . . ?
C9B C8B H8B 120.9 . . ?
C7B C8B H8B 120.9 . . ?
C8B C9B C4B 120.3(18) . . ?
C8B C9B H9B 119.8 . . ?
C4B C9B H9B 119.8 . . ?
N3 C14 N4 125.3(4) . . ?
N3 C14 C14 117.8(4) . 2_655 ?
N4 C14 C14 117.0(4) . 2_655 ?
N2 C10 N1 125.5(4) . . ?
N2 C10 C10 116.9(5) . 2_656 ?
N1 C10 C10 117.6(5) . 2_656 ?
N4 C15 C16 122.4(4) . . ?
N4 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
N2 C11 C12 122.2(4) . . ?
N2 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C17 C16 C15 116.8(4) . . ?
C17 C16 H16 121.6 . . ?
C15 C16 H16 121.6 . . ?
C11 C12 C13 116.7(4) . . ?
C11 C12 H12 121.7 . . ?
C13 C12 H12 121.7 . . ?
N3 C17 C16 121.9(4) . . ?
N3 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
N1 C13 C12 122.0(4) . . ?
N1 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
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(3) . ?
U1 O1 1.771(3) . ?
U1 O7 2.262(3) . ?
U1 O5 2.420(3) . ?
U1 O4 2.423(3) . ?
U1 O3 2.449(3) 2 ?
U1 O6 2.461(3) 2_665 ?
N1 C13 1.339(6) . ?
N1 C10 1.342(5) . ?
N1 Ag1 2.283(3) . ?
C1 O3 1.245(5) . ?
C1 O4 1.261(5) . ?
C1 C1 1.540(8) 2 ?
Ag1 N3 2.311(3) . ?
Ag1 N4 2.401(4) 2_655 ?
Ag1 N2 2.435(4) 2_656 ?
N2 C10 1.329(5) . ?
N2 C11 1.344(5) . ?
C2 O6 1.247(5) . ?
C2 O5 1.250(5) . ?
C2 C2 1.534(8) 2_665 ?
N4 C15 1.322(6) . ?
N4 C14 1.336(5) . ?
O7 C3 1.271(5) . ?
O8 C3 1.234(6) . ?
N3 C14 1.332(5) . ?
N3 C17 1.337(6) . ?
C3 C4B 1.40(3) . ?
C3 C4A 1.55(2) . ?
C4A C5A 1.371(18) . ?
C4A C9A 1.39(2) . ?
C5A C6A 1.372(14) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.380(12) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.408(16) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.386(16) . ?
C8A Br1A 1.883(14) . ?
C9A H9A 0.9500 . ?
C4B C5B 1.36(3) . ?
C4B C9B 1.43(3) . ?
C5B C6B 1.42(3) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.36(3) . ?
C6B Br1B 1.873(15) . ?
C7B C8B 1.41(2) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.40(2) . ?
C8B H8B 0.9500 . ?
C9B H9B 0.9500 . ?
C14 C14 1.501(8) 2_655 ?
C10 C10 1.501(8) 2_656 ?
C15 C16 1.378(6) . ?
C15 H15 0.9500 . ?
C11 C12 1.379(6) . ?
C11 H11 0.9500 . ?
C16 C17 1.373(6) . ?
C16 H16 0.9500 . ?
C12 C13 1.385(6) . ?
C12 H12 0.9500 . ?
C17 H17 0.9500 . ?
C13 H13 0.9500 . ?
