Guanidinate-stabilized monomeric hafnium amide complexes as promising precursors for MOCVD of HfO2.
Milanov, Andrian; Bhakta, Raghunandan; Baunemann, Arne; Becker, Hans-Werner; Thomas, Reji; Ehrhart, Peter; Winter, Manuela; Devi, Anjana; Inorganic chemistry 45 (2006) 11008–11018; doi:10.1021/ic061056i

data_4350518
_publ_section_title
;
 Guanidinate-stabilized monomeric hafnium amide complexes as promising
 precursors for MOCVD of HfO2.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11008
_journal_page_last               11018
_journal_paper_doi               10.1021/ic061056i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C24 H56.66667 Hf N8'
_chemical_formula_weight         635.93
_chemical_name_systematic
; 
bis-(dimethylamido)-bis-(N,N-diisopropyl-2-dimethylamido-guanidinato) 
hafnium(IV)
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_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                 116.313(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   19.8714(13)
_cell_length_b                   29.6787(13)
_cell_length_c                   17.5709(8)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.66
_cell_volume                     9288.9(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      105(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '1109 images at 1.0 deg. in \w and 25 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  0.1018
_diffrn_reflns_av_sigmaI/netI    0.1372
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59725
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    3.394
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   'Gaussian face-indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         10215
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                7111
_reflns_number_total             10215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061056isi20060613_055714.cif
_cod_data_source_block           cvd62
_cod_depositor_comments
;

2021-08-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        9288.9(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C72 H170 Hf3 N24'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1907.79
_cod_database_code               4350518