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#$Date: 2025-08-21 01:01:10 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/18/4321881.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_4321881
loop_
_publ_author_name
'David L. Clark'
'Steven D. Conradson'
'Robert J. Donohoe'
'D. Webster Keogh'
'David E. Morris'
'Phillip D. Palmer'
'Robin D. Rogers'
'C. Drew Tait'
_publ_section_title
;
 Chemical Speciation of the Uranyl Ion under Highly Alkaline Conditions.
 Synthesis, Structures, and Oxo Ligand Exchange Dynamics
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1456
_journal_page_last               1466
_journal_paper_doi               10.1021/ic981137h
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural     DLC6
_chemical_formula_sum            'Co2 H50 N12 O19 U3'
_chemical_formula_weight         1354.47
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 120.384(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4130(4)
_cell_length_b                   12.1794(3)
_cell_length_c                   15.3721(4)
_cell_measurement_reflns_used    6961
_cell_measurement_temperature    173(2)
_cell_volume                     2812.35(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8742
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    18.462
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.199
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.526
_refine_diff_density_min         -2.581
_refine_diff_density_rms         0.317
_refine_ls_extinction_coef       0.00035(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.099
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_obs          0.0313
_refine_ls_shift/esd_max         -2.264
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      '0.0295, 0.0000'
_refine_ls_wR_factor_all         0.0808
_refine_ls_wR_factor_obs         0.0734
_reflns_number_observed          2860
_reflns_number_total             3282
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981137h.cif
_cod_data_source_block           dlc6
_cod_original_formula_sum        'H50 Co2 N12 O19 U3'
_cod_database_code               4321881
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
U1 U 1.0000 1.36126(2) 0.7500 0.00869(10) Uani 1 d S .
U2 U 1.0000 1.0000 0.5000 0.01068(11) Uani 1 d S .
U3 U 0.7500 0.7500 0.5000 0.01062(11) Uani 1 d S .
Co Co 0.79259(5) 1.39685(7) 0.35041(6) 0.0092(2) Uani 1 d . .
O1 O 1.0000 1.5091(5) 0.7500 0.0154(15) Uani 1 d S .
O2 O 1.0000 1.2111(5) 0.7500 0.019(2) Uani 1 d S .
O3 O 0.9698(3) 1.3675(4) 0.8773(4) 0.0154(10) Uani 1 d . .
H3 H 0.9760(54) 1.3046(14) 0.9024(42) 0.018 Uiso 1 calc R .
O4 O 1.1484(3) 1.3579(3) 0.8596(4) 0.0138(10) Uani 1 d . .
H4 H 1.1675(9) 1.4225(4) 0.8748(43) 0.017 Uiso 1 calc R .
O5 O 0.8823(3) 1.0088(4) 0.4638(4) 0.0158(10) Uani 1 d . .
O6 O 0.9506(4) 0.9646(4) 0.3356(4) 0.0226(11) Uani 1 d . .
H6 H 0.9847(31) 0.9192(52) 0.3310(4) 0.027 Uiso 1 calc R .
O7 O 0.9902(3) 1.1804(4) 0.4720(4) 0.0227(11) Uani 1 d . .
H7 H 1.0371(23) 1.2028(12) 0.4749(63) 0.027 Uiso 1 calc R .
O8 O 0.6448(4) 0.7601(4) 0.4984(4) 0.0210(11) Uani 1 d . .
O9 O 0.6850(4) 0.6870(4) 0.3408(4) 0.0190(11) Uani 1 d . .
H9 H 0.6304(11) 0.6776(66) 0.3185(22) 0.023 Uiso 1 calc R .
O10 O 0.7277(3) 0.9258(4) 0.4422(4) 0.0166(10) Uani 1 d . .
H10 H 0.7735(19) 0.9486(22) 0.4429(56) 0.020 Uiso 1 calc R .
O11 O 1.0000 1.1348(7) 0.2500 0.016(2) Uani 1 d S .
H11A H 1.0000 1.1841(7) 0.2500 0.019 Uiso 1 d SR .
H11B H 1.0016 1.1037(7) 0.2833 0.019 Uiso 0.50 d PR .
N1 N 0.7064(4) 1.3066(5) 0.2370(4) 0.0159(12) Uani 1 d . .
H1A H 0.6832(23) 1.2549(24) 0.2600(7) 0.019 Uiso 1 calc R .
H1B H 0.7342(7) 1.2730(29) 0.2076(21) 0.019 Uiso 1 calc R .
H1C H 0.6618(16) 1.3501(7) 0.1909(17) 0.019 Uiso 1 calc R .
N2 N 0.8236(4) 1.2704(4) 0.4422(4) 0.0129(11) Uani 1 d . .
H2A H 0.8708(19) 1.2342(22) 0.4456(27) 0.016 Uiso 1 calc R .
H2B H 0.7762(11) 1.2241(19) 0.4185(19) 0.016 Uiso 1 calc R .
H2C H 0.8382(29) 1.2945(5) 0.5047(9) 0.016 Uiso 1 calc R .
N3 N 0.8876(4) 1.3603(4) 0.3211(5) 0.0156(12) Uani 1 d . .
H3A H 0.9235(19) 1.3076(28) 0.3647(23) 0.019 Uiso 1 calc R .
H3B H 0.9203(20) 1.4214(10) 0.3282(35) 0.019 Uiso 1 calc R .
H3C H 0.8628(4) 1.3348(37) 0.2567(12) 0.019 Uiso 1 calc R .
N4 N 0.7594(4) 1.5282(5) 0.2630(4) 0.0150(12) Uani 1 d . .
H4A H 0.8096(4) 1.5610(22) 0.2710(27) 0.018 Uiso 1 calc R .
H4B H 0.7294(28) 1.5761(18) 0.2804(24) 0.018 Uiso 1 calc R .
H4C H 0.7242(26) 1.5078(7) 0.1975(6) 0.018 Uiso 1 calc R .
N5 N 0.8780(4) 1.4894(4) 0.4637(4) 0.0150(12) Uani 1 d . .
H5A H 0.8959(23) 1.5460(21) 0.4395(5) 0.018 Uiso 1 calc R .
H5B H 0.9261(14) 1.4483(10) 0.5067(18) 0.018 Uiso 1 calc R .
H5C H 0.8515(10) 1.5164(29) 0.4971(21) 0.018 Uiso 1 calc R .
N6 N 0.6944(4) 1.4298(5) 0.3742(4) 0.0138(11) Uani 1 d . .
H6A H 0.7103(12) 1.4863(25) 0.4189(27) 0.017 Uiso 1 calc R .
H6B H 0.6821(21) 1.3694(12) 0.3999(33) 0.017 Uiso 1 calc R .
H6C H 0.6452(10) 1.4490(37) 0.3150(7) 0.017 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
Co Co 0.3494 0.9721 '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
O1 U1 O2 180.000(4) . . ?
O1 U1 O4 91.04(10) . 2_756 ?
O2 U1 O4 88.96(11) . 2_756 ?
O1 U1 O4 91.04(11) . . ?
O2 U1 O4 88.96(10) . . ?
O4 U1 O4 177.9(2) 2_756 . ?
O1 U1 O3 88.08(11) . 2_756 ?
O2 U1 O3 91.92(11) . 2_756 ?
O4 U1 O3 92.0(2) 2_756 2_756 ?
O4 U1 O3 88.1(2) . 2_756 ?
O1 U1 O3 88.08(11) . . ?
O2 U1 O3 91.92(11) . . ?
O4 U1 O3 88.1(2) 2_756 . ?
O4 U1 O3 92.0(2) . . ?
O3 U1 O3 176.2(2) 2_756 . ?
O5 U2 O5 180.0 . 5_776 ?
O5 U2 O7 85.4(2) . . ?
O5 U2 O7 94.6(2) 5_776 . ?
O5 U2 O7 94.6(2) . 5_776 ?
O5 U2 O7 85.4(2) 5_776 5_776 ?
O7 U2 O7 179.998(1) . 5_776 ?
O5 U2 O6 86.4(2) . . ?
O5 U2 O6 93.6(2) 5_776 . ?
O7 U2 O6 91.4(2) . . ?
O7 U2 O6 88.6(2) 5_776 . ?
O5 U2 O6 93.6(2) . 5_776 ?
O5 U2 O6 86.4(2) 5_776 5_776 ?
O7 U2 O6 88.6(2) . 5_776 ?
O7 U2 O6 91.4(2) 5_776 5_776 ?
O6 U2 O6 179.998(1) . 5_776 ?
O8 U3 O8 179.997(2) . 7_666 ?
O8 U3 O9 93.4(2) . . ?
O8 U3 O9 86.6(2) 7_666 . ?
O8 U3 O9 86.6(2) . 7_666 ?
O8 U3 O9 93.4(2) 7_666 7_666 ?
O9 U3 O9 179.998(1) . 7_666 ?
O8 U3 O10 87.7(2) . . ?
O8 U3 O10 92.3(2) 7_666 . ?
O9 U3 O10 90.2(2) . . ?
O9 U3 O10 89.8(2) 7_666 . ?
O8 U3 O10 92.3(2) . 7_666 ?
O8 U3 O10 87.7(2) 7_666 7_666 ?
O9 U3 O10 89.8(2) . 7_666 ?
O9 U3 O10 90.2(2) 7_666 7_666 ?
O10 U3 O10 180.0 . 7_666 ?
N1 Co N6 86.2(2) . . ?
N1 Co N2 90.4(2) . . ?
N6 Co N2 88.6(2) . . ?
N1 Co N3 91.3(2) . . ?
N6 Co N3 177.5(2) . . ?
N2 Co N3 91.7(2) . . ?
N1 Co N5 179.2(2) . . ?
N6 Co N5 93.3(2) . . ?
N2 Co N5 90.2(2) . . ?
N3 Co N5 89.2(2) . . ?
N1 Co N4 91.2(3) . . ?
N6 Co N4 88.8(2) . . ?
N2 Co N4 176.8(2) . . ?
N3 Co N4 91.0(2) . . ?
N5 Co N4 88.2(2) . . ?
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 O1 1.801(6) . ?
U1 O2 1.829(6) . ?
U1 O4 2.261(5) 2_756 ?
U1 O4 2.261(5) . ?
U1 O3 2.270(4) 2_756 ?
U1 O3 2.270(4) . ?
U2 O5 1.835(5) . ?
U2 O5 1.835(5) 5_776 ?
U2 O7 2.229(5) . ?
U2 O7 2.229(5) 5_776 ?
U2 O6 2.262(5) . ?
U2 O6 2.262(5) 5_776 ?
U3 O8 1.823(5) . ?
U3 O8 1.823(5) 7_666 ?
U3 O9 2.249(5) . ?
U3 O9 2.249(5) 7_666 ?
U3 O10 2.275(5) . ?
U3 O10 2.275(5) 7_666 ?
Co N1 1.963(6) . ?
Co N6 1.963(5) . ?
Co N2 1.971(5) . ?
Co N3 1.973(5) . ?
Co N5 1.974(6) . ?
Co N4 1.978(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139134393
