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_4306612
_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            'C27 H60 Dy N9'
_chemical_formula_weight         673.34
_chemical_name_common            'Dy(^i^PrN)~2~CNMe~2~ (1c)'
_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                91.639(2)
_cell_angle_beta                 95.779(2)
_cell_angle_gamma                115.322(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7312(3)
_cell_length_b                   11.2048(3)
_cell_length_c                   16.1286(5)
_cell_measurement_reflns_used    10547
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      2.535
_cell_volume                     1738.53(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13788
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_T_max  0.660
_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    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0485
_reflns_number_gt                5348
_reflns_number_total             6092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801432b_si_001_3.cif
_cod_data_source_block           cvd207a
_cod_original_cell_volume        1738.53(9)
_cod_database_code               4306612