Stabilization of Tetravalent 4f (Ce), 5d (Hf), or 5f (Th, U) Clusters by the [α-SiW9O34](10-) Polyoxometalate.
Duval, Sylvain; Béghin, Sébastien; Falaise, Clément; Trivelli, Xavier; Rabu, Pierre; Loiseau, Thierry; Inorganic chemistry 54 (2015) 8271–8280; doi:10.1021/acs.inorgchem.5b00786

data_4344090
_publ_section_title
;
 Stabilization of Tetravalent 4f (Ce), 5d (Hf), or 5f (Th, U) Clusters by
 the [\a-SiW9O34](10-) Polyoxometalate.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8271
_journal_page_last               8280
_journal_paper_doi               10.1021/acs.inorgchem.5b00786
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'0.25(C16 H24 Cs12 Na28 O380.8 Si8 U16 W72), 2.5(O)'
_chemical_formula_sum            'C4 H6 Cs3 Na7 O97.7 Si2 U4 W18'
_chemical_formula_weight         6494.55
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.472(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.8519(12)
_cell_length_b                   19.0881(9)
_cell_length_c                   18.1113(9)
_cell_measurement_temperature    100(2)
_cell_volume                     8788.4(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45044
_diffrn_reflns_theta_full        26.57
_diffrn_reflns_theta_max         26.57
_diffrn_reflns_theta_min         1.33
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    32.206
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.2249
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS empirical'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    4.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11126
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.193
_refine_diff_density_min         -6.186
_refine_diff_density_rms         0.704
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         9060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+1207.0261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                7291
_reflns_number_total             9060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00786_si_003.cif
_cod_data_source_block           sd69
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity' tag as specified in the
replacement file
'/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 3376 2015-05-07 07:48:27Z andrius 

 Adding full bibliography for 4344089--4344090.cif.
;
_cod_original_formula_sum        'C4 H6 Cs3 Na7 O97.70 Si2 U4 W18'
_cod_database_code               4344090
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O5W(0.8) Na4W(0.5) O1W(0.8) OW14(0.6) O10W(0.75) O12W(0.7)
 Cs1F(0.5) O7W(0.7) O13W(0.5)
3.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'