B-α-[AsW9O33](9-) polyoxometalates incorporating hexanuclear uranium {U6O8}-like clusters bearing the U(IV) form or unprecedented mixed valence U(IV)/U(VI) involving direct U(VI)[double bond, length as m-dash]O-U(IV) bonding.
Duval, Sylvain; Sobanska, Sophie; Roussel, Pascal; Loiseau, Thierry; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19772–19776; doi:10.1039/c5dt02932e

data_7037050
_publ_section_title
;
 B-\a-[AsW9O33](9-) polyoxometalates incorporating hexanuclear uranium
 {U6O8}-like clusters bearing the U(IV) form or unprecedented mixed
 valence U(IV)/U(VI) involving direct U(VI)[double bond, length as
 m-dash]O-U(IV) bonding.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19772
_journal_page_last               19776
_journal_paper_doi               10.1039/c5dt02932e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '0.5(As6 Na30 O325.5 U12 W54), 6.25(O)'
_chemical_formula_sum            'As3 Na15 O169 U6 W27'
_chemical_formula_weight         9665.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-09 deposited with the CCDC.
2015-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.543(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7846(8)
_cell_length_b                   31.0033(14)
_cell_length_c                   17.7568(8)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.09
_cell_measurement_theta_min      2.27
_cell_volume                     7585.9(7)
_computing_data_collection       'Bruker APEX2'
_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      100.03
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0625
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            254548
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.179
_diffrn_reflns_theta_min         1.314
_exptl_absorpt_coefficient_mu    27.575
_exptl_absorpt_correction_T_max  0.3363
_exptl_absorpt_correction_T_min  0.1243
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 'numercal''
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    4.232
_exptl_crystal_description       block
_exptl_crystal_F_000             8332
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.494
_refine_diff_density_min         -2.468
_refine_diff_density_rms         0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     996
_refine_ls_number_reflns         20819
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+173.2665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15162
_reflns_number_total             20819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02932e2.cif
_cod_data_source_block           sd162
_cod_depositor_comments
'Adding full bibliography for 7037049--7037051.cif.'
_cod_database_code               7037050
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Na6B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
2. Others
 Sof(Na0A)=Sof(OW10)=Sof(O1A)=Sof(O1C)=1-FVAR(1)
 Sof(O1B)=0.5*(1-FVAR(2))
 Sof(OW61)=0.5*FVAR(2)
 Sof(Na1)=Sof(OW64)=Sof(OW62)=Sof(OW63)=FVAR(1)
 Fixed Sof: OW89(0.75) OW94(0.5) OW95(0.75) Na2(0.5) Na6B(0.5) OW78(0.375)
 OW82(0.5) OW97(0.25) OW69(0.7) NaW7(0.5) Na9(0.5) OW79(0.25) OW71(0.25)
 OW73(0.125) OW91(0.5) OW68(0.5) OW80(0.5) OW92(0.25) OW76(0.125) O4AA(0.5)
 O1D(0.3) O1E(0.25) O1F(0.25) O8AA(0.5) O6AA(0.25) O7AA(0.25) O1G(0.25)
 O0BA(0.125) O1H(0.25) O9AA(0.25) O1BA(0.25) O3BA(0.25) O2BA(0.25) O4BA(0.125)
 O1I(0.125) O6BA(0.25) O5BA(0.25)
;
_shelx_res_checksum              28311
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'