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_7037049
_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         'As3 C3.89 Na15.5 O153.47 U6 W27, 11(O)'
_chemical_formula_sum            'C3.89 As3 Na15.5 O164.47 U6 W27'
_chemical_formula_weight         9651.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.4544(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9019(5)
_cell_length_b                   35.9438(11)
_cell_length_c                   26.0511(9)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.34
_cell_volume                     16302.9(9)
_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      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0684
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            234505
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_min         1.377
_exptl_absorpt_coefficient_mu    25.661
_exptl_absorpt_correction_T_max  0.3584
_exptl_absorpt_correction_T_min  0.1348
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 'numerical''
_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    3.932
_exptl_crystal_description       plate
_exptl_crystal_F_000             16635
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.203
_refine_diff_density_min         -3.997
_refine_diff_density_rms         0.478
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         33291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0258P)^2^+1634.2810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24278
_reflns_number_total             33291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02932e2.cif
_cod_data_source_block           sd213
_cod_depositor_comments
'Adding full bibliography for 7037049--7037051.cif.'
_cod_original_cell_volume        16302.8(9)
_cod_original_formula_sum        'C3.89 As3 Na15.50 O164.47 U6 W27'
_cod_database_code               7037049
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uiso(C2) = Uiso(C1)
2. Others
 Sof(O1)=1-FVAR(1)
 Sof(O2)=Sof(O4)=Sof(C3)=Sof(C5)=Sof(C4)=Sof(C6)=FVAR(1)
 Fixed Sof: OW11(0.5) OW20(0.5) OW39(0.5) OW19(0.5) Na11(0.5) Na2(0.5)
 OW27(0.5) OW14(0.5) OW5(0.5) OW26(0.5) OW42(0.5) OW18(0.5) Na16(0.5) Na18(0.5)
 Na7(0.5) OW53(0.5) OW47(0.5) OW46(0.5) OW23(0.5) OW16(0.5) OW48(0.5) OW50(0.5)
 OW21(0.5) OW31(0.5) OW51(0.5) OW45(0.5) OW17(0.5) OW22(0.5) OW63(0.5)
 OW62(0.5) OW64(0.5)
;
_shelx_res_checksum              6730
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'