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_1512970
_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            'C37 H52 Hf N4 O2'
_chemical_formula_weight         763.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.1855(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1333(4)
_cell_length_b                   10.3317(3)
_cell_length_c                   31.2018(10)
_cell_measurement_reflns_used    9275
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.72
_cell_measurement_theta_min      2.37
_cell_volume                     3552.5(2)
_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 0.935
_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  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            41882
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.973
_exptl_absorpt_correction_T_max  0.6986
_exptl_absorpt_correction_T_min  0.4722
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         8784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0160
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+2.6655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0379
_refine_ls_wR_factor_ref         0.0384
_reflns_number_gt                8352
_reflns_number_total             8784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-396-60-65-1.cif
_cod_data_source_block           cmu5
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1512970