Structural, Magnetic, EPR, and Electrochemical Characterizations of a Spin-Frustrated Trinuclear CrIII Polyoxometalate and Study of Its Reactivity with Lanthanum Cations
Jean-Daniel Compain; Pierre Mialane; Anne Dolbecq; Israël Martyr Mbomekallé; Jérôme Marrot; Francis Sécheresse; Carole Duboc; Eric Rivière; Inorganic Chemistry 49 (2010) 2851–2858; doi:10.1021/ic902341w

data_4315164
_publ_contact_author
;
      Dr P. Mialane
      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       mialane@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 83'
_publ_section_title
;
 Structural, Magnetic, EPR, and Electrochemical Characterizations of a
 Spin-Frustrated Trinuclear CrIII Polyoxometalate and Study of Its
 Reactivity with Lanthanum Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2851
_journal_page_last               2858
_journal_paper_doi               10.1021/ic902341w
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'Cr3 Cs4 H77 La2 O112 Si2 W20'
_chemical_formula_weight         6568.26
_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                78.0490(10)
_cell_angle_beta                 89.2950(10)
_cell_angle_gamma                71.4010(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7643(6)
_cell_length_b                   19.2319(9)
_cell_length_c                   21.1546(10)
_cell_measurement_reflns_used    16852
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.34
_cell_volume                     4807.1(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCDC 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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26271
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    26.659
_exptl_absorpt_correction_T_max  0.6177
_exptl_absorpt_correction_T_min  0.3491
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5774
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.424
_refine_diff_density_min         -4.779
_refine_diff_density_rms         0.660
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         16852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1786
_reflns_number_gt                12404
_reflns_number_total             16852
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic902341w_si_002_2.cif
_cod_data_source_block           2
_cod_original_formula_sum        'H77 Cr3 Cs4 La2 O112 Si2 W20'
_cod_database_code               4315164