Manganese(III)-Containing Wells-Dawson Sandwich-Type Polyoxometalates: Comparison with their Manganese(II) Counterparts
Mounim Lebrini; Israël M. Mbomekallé; Anne Dolbecq; Jérôme Marrot; Patrick Berthet; Joseline Ntienoue; Francis Sécheresse; Jacky Vigneron; Arnaud Etcheberry; Inorganic Chemistry 50 (2011) 6437–6448; doi:10.1021/ic102237x

data_4325576
_publ_contact_author
;
      Dr Israel Marty Mbomekalle
      Institut Lavoisier, ILV, UMR CNRS 8180
      Universit\'e de Versailles Saint-Quentin-en-Yvelines
      45 Avenue des Etats Unis
      78035 Versailles cedex
      France
;
_publ_contact_author_email       Israel.Mbomekalle@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 83'
_publ_contact_author_phone       '(33) 1 39 25 44 19'
_publ_section_title
;
 Manganese(III)-Containing Wells-Dawson Sandwich-Type Polyoxometalates:
 Comparison with their Manganese(II) Counterparts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6437
_journal_page_last               6448
_journal_paper_doi               10.1021/ic102237x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'As4 H112 Mn3 Na15 O168 W30'
_chemical_formula_weight         9125.75
_chemical_name_systematic
; 

 ? 

;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.59(2)
_cell_angle_beta                 83.89(2)
_cell_angle_gamma                75.20(2)
_cell_formula_units_Z            1
_cell_length_a                   12.733(5)
_cell_length_b                   15.855(7)
_cell_length_c                   19.475(8)
_cell_measurement_reflns_used    6997
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.66
_cell_volume                     3779(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            232324
_diffrn_reflns_theta_full        30.14
_diffrn_reflns_theta_max         30.14
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    24.005
_exptl_absorpt_correction_T_max  0.3270
_exptl_absorpt_correction_T_min  0.1608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.010
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.167
_refine_diff_density_min         -3.019
_refine_diff_density_rms         0.391
_refine_ls_extinction_coef       0.00096(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         21844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1999P)^2^+98.9815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2350
_refine_ls_wR_factor_ref         0.2533
_reflns_number_gt                18489
_reflns_number_total             21844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102237x_si_001_3.cif
_cod_data_source_block           4
_cod_original_formula_sum        'H112 As4 Mn3 Na15 O168 W30'
_cod_database_code               4325576