Octakis(dimethyl sulfoxide-κ<i>O</i>)cerium(III) μ~6~-oxido-dodeca-μ~2~-oxido-hexaoxidohexamolybdate(VI) dimethyl sulfoxide tetrasolvate
Ben Khélifa, Arbia; Giorgi, Michel; Belkhiria, Mohamed Salah; Acta Crystallographica Section E 68 (2012) m938–m939; doi:10.1107/S1600536812025949

data_2235573
_publ_section_title
;
 Octakis(dimethyl sulfoxide-\k<i>O</i>)cerium(III)
 \m~6~-oxido-dodeca-\m~2~-oxido-hexaoxidohexamolybdate(VI) dimethyl
 sulfoxide tetrasolvate
;
_journal_coeditor_code           PV2546
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m938
_journal_page_last               m939
_journal_paper_doi               10.1107/S1600536812025949
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ce(C2 H6 O S)8]~2~ [Mo6 O19]3 , 4C2 H6 OS'
_chemical_formula_moiety
'2(C16 H48 Ce O8 S8 3+) , 3(Mo6 O19 2-) , 4(C2 H6 OS)'
_chemical_formula_sum            'C40 H120 Ce2 Mo18 O77 S20'
_chemical_formula_weight         4481.72
_chemical_name_systematic
;
Octakis(dimethyl sulfoxide-\k<i>O</i>)cerium(III)
\m~6~-oxido-dodeca-\m~2~-oxido-hexaoxidohexamolybdate(VI)
dimethyl sulfoxide tetrasolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.2810(10)
_cell_angle_beta                 98.4680(10)
_cell_angle_gamma                115.5800(10)
_cell_formula_units_Z            1
_cell_length_a                   13.4590(2)
_cell_length_b                   15.4688(3)
_cell_length_c                   17.6599(4)
_cell_measurement_reflns_used    80805
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.91
_cell_measurement_theta_min      2.33
_cell_volume                     3270.49(11)
_computing_cell_refinement
'HKL-Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction
'HKL-Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69065
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.75
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
During the refinement of the structure, a difference map showed
electron density peaks representing a highly disordered molecule of
solvent used for crystallization (DMSO) which could not be modeled
successfully.
The program PLATON (Spek, 2009) indicated potential solvent accessible
voids of 500.0 \%A^3^.
The sub-routine SQUEEZE in PLATON was used to remove the contribution
of the electron density from the observed data. The crystal density,
F(000) value, the molar mass are given without contribution of this
electron density.
;
_refine_diff_density_max         2.468
_refine_diff_density_min         -1.814
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         12827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+11.5151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                10059
_reflns_number_total             12827
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            pv2546.cif
_cod_data_source_block           I
_cod_original_cell_volume        3270.48(11)
_cod_database_code               2235573
_cod_database_fobs_code          2235573