Facile Access to Tetravalent Cerium Compounds: One-Electron Oxidation Using Iodine(III) Reagents
Peter Dröse; Alan R. Crozier; Samira Lashkari; Jochen Gottfriedsen; Steffen Blaurock; Cristian G. Hrib; Cäcilia Maichle-Mössmer; Christoph Schädle; Reiner Anwander; Frank T. Edelmann; Journal of the American Chemical Society 132 (2010) 14046–14047; doi:10.1021/ja107494h

data_4103256
_publ_section_title
;
 Facile Access to Tetravalent Cerium Compounds: One-Electron Oxidation
 Using Iodine(III) Reagents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14046
_journal_page_last               14047
_journal_paper_doi               10.1021/ja107494h
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C42 H75 Ce Cl N6 O3 Si6'
_chemical_formula_weight         1056.19
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.76(3)
_cell_angle_beta                 90.93(3)
_cell_angle_gamma                104.79(3)
_cell_formula_units_Z            2
_cell_length_a                   11.153(2)
_cell_length_b                   12.925(3)
_cell_length_c                   19.583(4)
_cell_measurement_reflns_used    782
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.22
_cell_measurement_theta_min      2.10
_cell_volume                     2693.1(11)
_computing_cell_refinement       'Stoe XAREA'
_computing_data_collection       'Stoe XAREA'
_computing_data_reduction        'Stoe XAREA'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'Bruker SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14472
_diffrn_reflns_theta_full        29.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.6465
_exptl_absorpt_correction_T_min  0.6422
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            black-red
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.603
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    'methyls rigid and other riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         14472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                11654
_reflns_number_total             14472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107494h_si_003.cif
_cod_data_source_block           ip2_228a
_cod_original_cell_volume        2693.1(9)
_cod_database_code               4103256