Role of Ammonium Ions in the Formation of Ammonium Uranyl Peroxides and Uranyl Peroxo-oxalates
Blanchard, Florent; Ellart, Marine; Rivenet, Murielle; Vigier, Nicolas; Hablot, Isabelle; Morel, Bertrand; Grandjean, Stéphane; Abraham, Francis; Crystal Growth & Design 16 (2015) 200–; doi:10.1021/acs.cgd.5b01090

data_4516470
_publ_section_title
;
 Role of Ammonium Ions in the Formation of Ammonium Uranyl Peroxides and
 Uranyl Peroxo-oxalates
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              200
_journal_paper_doi               10.1021/acs.cgd.5b01090
_journal_volume                  16
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'O140 U28, N8 U0.25, 18(N), 8(O)'
_chemical_formula_sum            'N26 O148 U28.25'
_chemical_formula_weight         9456.13
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_audit_creation_date             2015-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.5052(13)
_cell_length_b                   20.5052(13)
_cell_length_c                   24.7010(16)
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.570
_cell_measurement_theta_min      2.368
_cell_volume                     10385.9(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            45720
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         1.404
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    22.026
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7929.6
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.130
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_refine_diff_density_max         4.563
_refine_diff_density_min         -1.157
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_refine_ls_abs_structure_details
;
 Flack x determined using 4216 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         10635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0457
_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/[\s^2^(Fo^2^)+(0.0765P)^2^+134.4339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9511
_reflns_number_total             10635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b01090_si_002.cif
_cod_data_source_block           u28
_cod_original_cell_volume        10385.9(15)
_cod_database_code               4516470
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8612(10) 0.1388(10)
;
_shelx_res_checksum              62910
_shelx_hkl_checksum              42002
_olex2_submission_special_instructions 'No special instructions were received'