Tuning Reactivity and Electronic Properties through Ligand Reorganization within a Cerium Heterobimetallic Framework
Jerome R. Robinson; Zachary Gordon; Corwin H. Booth; Patrick J. Carroll; Patrick J. Walsh; Eric J. Schelter; Journal of the American Chemical Society 135 (2013) 19016–19024; doi:10.1021/ja410688w

data_4121346
_publ_section_title
;
 Tuning Reactivity and Electronic Properties through Ligand Reorganization
 within a Cerium Heterobimetallic Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19016
_journal_page_last               19024
_journal_paper_doi               10.1021/ja410688w
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C102 H96 Ce K2 O12'
_chemical_formula_weight         1732.11
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      76
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0895(11)
_cell_length_b                   20.0895(11)
_cell_length_c                   23.6913(13)
_cell_measurement_temperature    143(1)
_cell_volume                     9561.5(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            115967
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1093
_refine_ls_number_reflns         21914
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                17696
_reflns_number_total             21914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja410688w_si_002_04.cif
_cod_data_source_block           UP4054
_cod_original_sg_symbol_H-M      'P 41 '
_cod_database_code               4121346