Synthesis, Electrochemistry, and Reactivity of Cerium(III/IV) Methylene-Bis-Phenolate Complexes
Brian D. Mahoney; Nicholas A. Piro; Patrick J. Carroll; Eric J. Schelter; Inorganic Chemistry 52 (2013) 5970–5977; doi:10.1021/ic400202r

data_4334879
_publ_section_title
;
 Synthesis, Electrochemistry, and Reactivity of Cerium(III/IV)
 Methylene-Bis-Phenolate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5970
_journal_page_last               5977
_journal_paper_doi               10.1021/ic400202r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C68 H92 Ce Li N2 O7'
_chemical_formula_weight         1196.50
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.044(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9237(11)
_cell_length_b                   19.4090(12)
_cell_length_c                   18.0250(12)
_cell_measurement_temperature    143(1)
_cell_volume                     6254.9(7)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            144657
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.358
_refine_diff_density_min         -2.580
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.474(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1457
_refine_ls_number_reflns         28576
_refine_ls_number_restraints     1484
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+22.5169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                26277
_reflns_number_total             28576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400202r_si_002_3.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P n '
_cod_database_code               4334879