Capturing ammonium nitrate in a synthetic uranium oxide hydrate phase: revealing the role of ammonium ions and anion inclusions.
Zhang, Yingjie; Ablott, Timothy A.; Nicholas, Maria K.; Karatchevtseva, Inna; Plášil, Jakub; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11112–11119; doi:10.1039/d4dt01372g

data_7716360
_publ_section_title
;
 Capturing ammonium nitrate in a synthetic uranium oxide hydrate phase:
 revealing the role of ammonium ions and anion inclusions.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11112
_journal_page_last               11119
_journal_paper_doi               10.1039/d4dt01372g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'O11 U3, N O3, 2(H4 N)'
_chemical_formula_sum            'H8 N3 O14 U3'
_chemical_formula_weight         988.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-05-08 deposited with the CCDC.	2024-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.387(3)
_cell_length_b                   7.4410(15)
_cell_length_c                   7.0020(14)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.989
_cell_measurement_theta_min      2.738
_cell_volume                     645.4(2)
_computing_cell_refinement       'BlueIce (McPhillips, et al., 2002)'
_computing_data_collection       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Eiger Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71079
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7396
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.989
_diffrn_reflns_theta_max         24.989
_diffrn_reflns_theta_min         2.738
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    37.627
_exptl_absorpt_correction_T_max  0.4314
_exptl_absorpt_correction_T_min  0.2494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1137 before and 0.0667 after correction.
The Ratio of minimum to maximum transmission is 0.5781.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.085
_exptl_crystal_description       plate
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         4.382
_refine_diff_density_min         -2.982
_refine_diff_density_rms         0.432
_refine_ls_abs_structure_details
;
 Flack x determined using 519 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1191
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                1165
_reflns_number_total             1191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01372g2.cif
_cod_data_source_block           cxasap_sadabs_s_aa
_cod_depositor_comments          'Adding full bibliography for 7716360.cif.'
_cod_database_code               7716360
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 N2-H2A
 1.05 with sigma of 0.02
 N2-H2C
 1.05 with sigma of 0.02
 N2-H2B
 1.05 with sigma of 0.02
 N2-H2D
 1.05 with sigma of 0.02
 H2D-H2A
 1.85 with sigma of 0.02
 H2C-H2A
 1.85 with sigma of 0.02
 H2C-H2D
 1.85 with sigma of 0.02
 H2A-H2B
 1.85 with sigma of 0.02
 H2B-H2C
 1.85 with sigma of 0.02
 H2B-H2D
 1.85 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O6) = Uanis(O7)
Uiso(H2A) = Uiso(H2B) = Uiso(H2C) = Uiso(H2D)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_shelx_res_checksum              92344
_shelx_hkl_checksum              3548
_olex2_submission_special_instructions 'No special instructions were received'