Formation of a Ce(IV) Oxo Complex via Inner Sphere Nitrate Reduction.
Damon, Peter L.; Wu, Guang; Kaltsoyannis, Nikolas; Hayton, Trevor W.; Journal of the American Chemical Society 138 (2016) 12743–12746; doi:10.1021/jacs.6b07932

data_4130929
_publ_section_title
;
 Formation of a Ce(IV) Oxo Complex via Inner Sphere Nitrate Reduction.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12743
_journal_page_last               12746
_journal_paper_doi               10.1021/jacs.6b07932
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C32 H73 Ce Li N4 O5 Si3, C6 H6'
_chemical_formula_sum            'C38 H79 Ce Li N4 O5 Si3'
_chemical_formula_weight         903.38
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                85.344(4)
_cell_angle_beta                 78.547(4)
_cell_angle_gamma                63.000(4)
_cell_formula_units_Z            2
_cell_length_a                   11.745(3)
_cell_length_b                   12.572(3)
_cell_length_c                   18.886(4)
_cell_measurement_reflns_used    281
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.7455
_cell_measurement_theta_min      0.6601
_cell_volume                     2435.1(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'Omega scan'
_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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25647
_diffrn_reflns_theta_full        27.21
_diffrn_reflns_theta_max         27.21
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.8954
_exptl_absorpt_correction_T_min  0.8056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.784
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         10700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0362
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                8850
_reflns_number_total             10700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b07932_si_001.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        2435.2(9)
_cod_database_code               4130929