Synthesis of hafnium(IV) beta-ketoiminates as potential precursors for the MOCVD of HfO2
Diego Gonzalez-Flores; Siddappa A. Patil; Phillip A. Medina; Seth Dever; Chananate Uthaisar; Leslie W. Pineda; Mavis L. Montero; Joseph W. Ziller; Bradley D. Fahlman; Inorganica Chimica Acta 396 (2013) 60–65; doi:10.1016/j.ica.2012.10.002

data_1512971
_publ_section_title
;
 Synthesis of hafnium(IV) beta-ketoiminates as potential precursors for
 the MOCVD of HfO2
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              60
_journal_page_last               65
_journal_paper_doi               10.1016/j.ica.2012.10.002
_journal_volume                  396
_journal_year                    2013
_chemical_formula_sum            'C28 H40 Hf N4 O2'
_chemical_formula_weight         643.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.7347(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1654(7)
_cell_length_b                   9.0233(3)
_cell_length_c                   17.0661(6)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.66
_cell_measurement_theta_min      2.26
_cell_volume                     2771.89(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0115
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32445
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    3.794
_exptl_absorpt_correction_T_max  0.6423
_exptl_absorpt_correction_T_min  0.2961
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0134
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+1.5445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0334
_refine_ls_wR_factor_ref         0.0339
_reflns_number_gt                6485
_reflns_number_total             6832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-396-60-65-2.cif
_cod_data_source_block           cmu8
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1512971