Synthesis, Characterization, and Thermal Properties of Homoleptic Rare-Earth Guanidinates: Promising Precursors for MOCVD and ALD of Rare-Earth Oxide Thin Films
Andrian P. Milanov; Roland A. Fischer; Anjana Devi; Inorganic Chemistry 47 (2008) 11405–11416; doi:10.1021/ic801432b

data_4306615
_publ_contact_author
;
        Anjana Devi
        Department of Inorganic Chemistry II
        Ruhr-University Bochum
        Universitaetsstr. 150
        44801 Bochum
        Germany
;
_publ_contact_author_email       anjana.devi@ruhr-uni-bochum.de
_publ_contact_author_fax         '049 234 321-4174'
_publ_contact_author_phone       '049 234 32-24150'
_publ_section_title
;
Synthesis, Characterization, and Thermal Properties of Homoleptic
Rare-Earth Guanidinates: Promising Precursors for MOCVD and ALD of
Rare-Earth Oxide Thin Films
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11405
_journal_page_last               11416
_journal_paper_doi               10.1021/ic801432b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C39 H82 Dy N9'
_chemical_formula_weight         839.64
_chemical_name_common            'Dy(^i^PrN)~2~CNEt~2~ (2c)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.215(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1555(12)
_cell_length_b                   13.1098(4)
_cell_length_c                   17.3510(7)
_cell_measurement_reflns_used    5053
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      36.690
_cell_measurement_theta_min      2.747
_cell_volume                     4596.2(4)
_computing_cell_refinement       'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_data_collection       'CrysAlis CCD 1.171.13, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '560 images at 1.0 deg. in \w and 15 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18529
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.923
_refine_diff_density_min         -1.978
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1216P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                2946
_reflns_number_total             4045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801432b_si_001_6.cif
_cod_data_source_block           cvd225
_cod_original_cell_volume        4596.2(3)
_cod_database_code               4306615