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_7231070
_publ_section_title
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 Complexation of tetravalent uranium cations by the As4W40O140 cryptand
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE00873F
_journal_year                    2018
_chemical_formula_moiety
'0.5(As8 C7 Na18 O365.6 U8 W80), 2(Na2 O6.5), 30.2(O)'
_chemical_formula_sum            'C3.5 As4 Na13 O226 U4 W40'
_chemical_formula_weight         12562.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n :2'
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_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                   23.184(2)
_cell_length_b                   29.532(3)
_cell_length_c                   14.5168(13)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.49
_cell_measurement_theta_min      3.18
_cell_volume                     9939.2(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            171581
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.544
_diffrn_reflns_theta_min         1.386
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.660
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.4632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1706 before and 0.0689 after correction. The Ratio of minimum to maximum transmission is 0.6222. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    4.198
_exptl_crystal_description       block
_exptl_crystal_F_000             10864
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         6.439
_refine_diff_density_min         -5.936
_refine_diff_density_rms         0.636
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         10581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0703P)^2^+871.8262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9155
_reflns_number_total             10581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00873f2.cif
_cod_data_source_block           md20dx8
_cod_original_formula_sum        'C3.50 As4 Na13 O226 U4 W40'
_cod_database_code               7231070
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Others
 Sof(OW29)=1-FVAR(1)
 Sof(OW8)=FVAR(1)
 Sof(OW30)=1-FVAR(2)
 Sof(OW22)=FVAR(2)
 Fixed Sof: O45(0.75) OW9(0.7) OW10(0.5) OW11(0.5) OW6(0.25) OW4(0.25)
 C1(0.375) OW23(0.5) OW26(0.3) OW25(0.5) OW24(0.25) Na5(0.5) OW28(0.25)
;
_shelx_res_checksum              418
_olex2_exptl_crystal_mounting_method 'mitegen loop'
_olex2_submission_special_instructions 'No special instructions were received'