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_4121343
_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_absolute_configuration syn
_chemical_formula_sum            'C72 H72 Ce I Li3 N6 O6'
_chemical_formula_weight         1405.20
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      173
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.0951(4)
_cell_length_b                   15.0951(4)
_cell_length_c                   19.9811(8)
_cell_measurement_temperature    143(1)
_cell_volume                     3943.0(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49345
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.122
_refine_diff_density_min         -1.702
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6097
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                3555
_reflns_number_total             6097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja410688w_si_002_01.cif
_cod_data_source_block           UP4022
_cod_original_sg_symbol_H-M      'P 63 '
_cod_database_code               4121343