Ce(IV) Complexes with Donor-Functionalized Alkoxide Ligands: Improved Precursors for Chemical Vapor Deposition of CeO2
Helen C. Aspinall; John Bacsa; Anthony C. Jones; Jacqueline S. Wrench; Kate Black; Paul R. Chalker; Peter J. King; Paul Marshall; Matthew Werner; Hywel O. Davies; Rajesh Odedra; Inorganic Chemistry 50 (2011) 11644–11652; doi:10.1021/ic201593s

data_4326891
_publ_section_title
;
 Ce(IV) Complexes with Donor-Functionalized Alkoxide Ligands: Improved
 Precursors for Chemical Vapor Deposition of CeO2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11644
_journal_page_last               11652
_journal_paper_doi               10.1021/ic201593s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '(Ce 4+)3, (C5 H11 O -)9, (C4 H9 O -), (O 2-)'
_chemical_formula_sum            'C49 H108 Ce3 O11'
_chemical_formula_weight         1293.73
_chemical_name_common            JW251
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   19.0918(17)
_cell_length_b                   19.0918(17)
_cell_length_c                   23.342(2)
_cell_measurement_temperature    100(2)
_cell_volume                     7368.2(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'SMART v.5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 diffractometer with APEX detector'
_diffrn_measurement_method       '\w scans with a narrow frame width'
_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  0.1072
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63149
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  0.9321
_exptl_absorpt_correction_T_min  0.8060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008-1 (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       needle
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
  The molecular formula includes diffuse solvent not included
  in the atom list. Disordered toluene molecules could be 
  discerned from the difference electron density, but the density 
   was too 
  diffuse to be modelled reliably.  
  PLATON/SQUEEZE calculates 1 large solvent voids in the unit cell
  volume = 1550 A^3^, with 724 electrons in each void, corresponding 
  to 8(C7 H10) and 8(C5 H12) and 2(C7 H10), 2(C5 H12) for each the 
  molecular formula unit.
;
_refine_diff_density_max         2.211
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+21.3941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                3584
_reflns_number_total             4686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201593s_si_002_3.cif
_cod_data_source_block           jw251m
_cod_database_code               4326891