Synthesis and Characterization of Volatile, Fluorine-Free β-Ketoiminate Lanthanide MOCVD Precursors and Their Implementation in Low-Temperature Growth of Epitaxial CeO2 Buffer Layers for Superconducting Electronics
Nikki L. Edleman; Anchuan Wang; John A. Belot; Andrew W. Metz; Jason R. Babcock; Amber M. Kawaoka; Jun Ni; Matthew V. Metz; Christine J. Flaschenriem; Charlotte L. Stern; Louise M. Liable-Sands; Arnold L. Rheingold; Paul R. Markworth; Robert P. H. Chang; Michael P. Chudzik; Carl R. Kannewurf; Tobin J. Marks; Inorganic Chemistry 41 (2002) 5005–5023; doi:10.1021/ic020299h

data_4318574
_publ_section_title
;
 Synthesis and Characterization of Volatile, Fluorine-Free \b-Ketoiminate
 Lanthanide MOCVD Precursors and Their Implementation in Low-Temperature
 Growth of Epitaxial CeO2 Buffer Layers for Superconducting Electronics
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5005
_journal_page_last               5023
_journal_paper_doi               10.1021/ic020299h
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C33 H60 Ce N3 O6'
_chemical_formula_weight         734.96
_chemical_name_common            'complex 4, Ce(tBuMeMe)3'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                112.8853(6)
_cell_angle_beta                 90.9699(11)
_cell_angle_gamma                99.5012(7)
_cell_formula_units_Z            8
_cell_length_a                   17.5040(2)
_cell_length_b                   21.1598(2)
_cell_length_c                   23.0715(2)
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     7733.61(14)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.851
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'Siemens P4_CCD'
_diffrn_measurement_method       'omega/phi scans'
_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  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0827
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49148
_diffrn_reflns_theta_full        28.13
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_correction_T_min  0.7928
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.987
_refine_diff_density_min         -2.307
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1549
_refine_ls_number_reflns         32224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.181
_refine_ls_shift/su_mean         0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                22312
_reflns_number_total             32224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020299h_1.cif
_cod_data_source_block           C33H60CeN3O6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        7733.63(12)
_cod_database_code               4318574