Mixed amide–malonate compound of hafnium as a novel monomeric precursor for MOCVD of HfO2 thin films
Milanov, A.; Bhakta, R.; Thomas, R.; Ehrhart, P.; Winter, M.; Waser, R.; Devi, A.; Journal of Materials Chemistry 16 (2006) 437–; doi:10.1039/b509380e

data_7203103
_publ_section_title
;
 Mixed amide--malonate compound of hafnium as a novel monomeric
 precursor for MOCVD of HfO2 thin films
;
_journal_issue                   5
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              437
_journal_paper_doi               10.1039/b509380e
_journal_volume                  16
_journal_year                    2006
_chemical_formula_sum            'C30 H58 Hf N2 O8'
_chemical_formula_weight         753.27
_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                83.458(5)
_cell_angle_beta                 86.262(7)
_cell_angle_gamma                84.888(7)
_cell_formula_units_Z            4
_cell_length_a                   13.3247(11)
_cell_length_b                   16.2200(14)
_cell_length_c                   17.2825(14)
_cell_measurement_reflns_used    2332
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9988
_cell_measurement_theta_min      2.5303
_cell_volume                     3690.4(5)
_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    'SHELXTL-PLUS(Sheldrick, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '586 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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27444
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    2.870
_exptl_absorpt_correction_T_max  0.59645
_exptl_absorpt_correction_T_min  0.46240
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   'Gaussian face-indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.330
_refine_diff_density_min         -2.108
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         12924
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0964P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                8924
_reflns_number_total             12924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b509380e.txt
_cod_data_source_block           cvd21
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203103