Complexation of tetravalent uranium cations by the As4W40O140 cryptand
DUFAYE, Maxime; Duval, Sylvain; Hirsou, Bastien; Stoclet, Grégory; Loiseau, Thierry; CrystEngComm  (2018) –; doi:10.1039/C8CE00873F

data_7231071
_publ_section_title
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 Complexation of tetravalent uranium cations by the As4W40O140 cryptand
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE00873F
_journal_year                    2018
_chemical_formula_moiety         'As4 C3.5 Na6.5 O157 U2 W40, Na, 29.5(O)'
_chemical_formula_sum            'C3.5 As4 Na7.5 O186.5 U2 W40'
_chemical_formula_weight         11328.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2017-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-05 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                106.064(2)
_cell_angle_beta                 96.373(2)
_cell_angle_gamma                90.129(2)
_cell_formula_units_Z            4
_cell_length_a                   19.5645(7)
_cell_length_b                   26.6677(10)
_cell_length_c                   38.3039(15)
_cell_measurement_reflns_used    9674
_cell_measurement_temperature    99.97
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.22
_cell_volume                     19074.3(13)
_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      99.97
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.1420
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            212649
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.421
_diffrn_reflns_theta_min         1.293
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.516
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1312 before and 0.0613 after correction. The Ratio of minimum to maximum transmission is 0.5475. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.945
_exptl_crystal_description       block
_exptl_crystal_F_000             19486
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.701
_refine_diff_density_min         -3.441
_refine_diff_density_rms         0.580
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2421
_refine_ls_number_reflns         77648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+2394.6665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                46991
_reflns_number_total             77648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00873f2.cif
_cod_data_source_block           hb41_sq
_cod_depositor_comments
;

2024-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C7 As8 Na15 O373 U4 W80'
_cod_original_formula_weight         22656.40
_cod_original_formula_moiety         'As8 C7 Na13 O314 U4 W80, 2(Na), 59(O)'
_cod_original_formula_units_Z            2
_cod_database_code               7231071
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.177
_shelx_estimated_absorpt_t_min   0.109
_olex2_refinement_description
;
1. Others
 Fixed Sof: O5W(0.5) O55W(0.5) O6W(0.5) O9W(0.5) O31W(0.5) O28W(0.5)
;
_shelx_res_checksum              84220
_shelx_fab_checksum              58533
_olex2_exptl_crystal_mounting_method 'mitegen loop'
_olex2_submission_special_instructions 'No special instructions were received'