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_7231069
_publ_section_title
;
 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 Na4.35 O155.2 U2 W40, Na O6, 38.55(O0.55)'
_chemical_formula_sum            'As4 Na5.35 O182.4 U2 W40'
_chemical_formula_weight         11171.14
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_audit_creation_date             2017-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-04-05 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.8185(5)
_cell_length_b                   19.8185(5)
_cell_length_c                   26.1867(6)
_cell_measurement_reflns_used    4904
_cell_measurement_temperature    99.96
_cell_measurement_theta_max      24.54
_cell_measurement_theta_min      2.43
_cell_volume                     10285.4(4)
_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      99.96
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0920
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26582
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_min         1.555
_exptl_absorpt_coefficient_mu    24.579
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4086
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS numerical'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.607
_exptl_crystal_description       block
_exptl_crystal_F_000             9588
_exptl_crystal_recrystallization_method
'crystallized from slow evaporation of the solvent'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.415
_refine_diff_density_min         -2.392
_refine_diff_density_rms         0.301
_refine_ls_abs_structure_details
;
 Flack x determined using 3024 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.041(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10354
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0743
_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^)+(0.0451P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                7806
_reflns_number_total             10354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00873f2.cif
_cod_data_source_block           hb44c_sq
_cod_original_cell_volume        10285.4(6)
_cod_original_formula_sum        'As4 Na5.35 O182.40 U2 W40'
_cod_database_code               7231069
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 U1-OW20_$1
 2.5 with sigma of 0.01
2. Others
 Fixed Sof: U1(0.5) Na3(0.1375) OW19(0.3) OW17(0.3) Na1(0.5) OW20(0.5)
 Na4(0.45) OW2(0.75) OW1(0.75) O36(0.25) OW14(0.5) OW15(0.5) OW13(0.5)
 OW8(0.25) OW12(0.25) OW16(0.25) OW11(0.25) OW18(0.25) OW3(0.25) OW4(0.25)
 O37(0.25) OW10(0.25)
;
_shelx_res_checksum              96704
_shelx_fab_checksum              74286
_olex2_exptl_crystal_mounting_method 'Mounted on a mitegen loop'
_olex2_submission_special_instructions 'No special instructions were received'