# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is © The Royal Society of Chemistry 2004


data_global
_journal_name_full               J.Mater.Chem.

_journal_coden_Cambridge         1145

_publ_contact_author_name        'Prof Adulfas Abrutis'
_publ_contact_author_address     
;
Chemistry
Vilnius University
Naugarduko 24
Vilnius
LT-2006
LITHUANIA
;

_publ_contact_author_email       ADULFAS.ABRUTIS@CHF.VU.LT

_publ_section_title              
;
New sterically hindered Hf, Zr and Y b-diketonates
as MOCVD precursors for oxide films.
;
loop_
_publ_author_name
'Adulfas Abrutis'
'Sergej V Pasko'
'Ausrine Bartsayte'
'Philippe Richard'
'Vida Kazlauskiene'

data_lyon6
_database_code_depnum_ccdc_archive 'CCDC 226824'

_audit_creation_date             2003-09-09
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#_audit_creation_method            SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H76 Hf O8'
_chemical_formula_weight         911.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.1660(2)
_cell_length_b                   17.3175(4)
_cell_length_c                   19.5311(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.037(1)
_cell_angle_gamma                90.00
_cell_volume                     4627.30(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    5187
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    2.301
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9177
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5284
_reflns_number_gt                4863
_reflns_threshold_expression     2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Ferrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^  2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+14.0268P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5284
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0725
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0663(2) 0.1358(2) 0.13347(16) 0.0301(7) Uani 1 1 d . . .
C2 C 0.0012(3) 0.0748(2) 0.13122(18) 0.0337(7) Uani 1 1 d . . .
H2 H 0.0102 0.0289 0.1089 0.040 Uiso 1 1 calc R . .
C3 C -0.0781(2) 0.0813(2) 0.16218(16) 0.0299(7) Uani 1 1 d . . .
C4 C 0.1409(3) 0.1308(2) 0.08996(17) 0.0358(8) Uani 1 1 d . . .
H4A H 0.1182 0.1631 0.0483 0.043 Uiso 1 1 calc R . .
H4B H 0.1417 0.0780 0.0735 0.043 Uiso 1 1 calc R . .
C5 C 0.2472(2) 0.15425(19) 0.12667(16) 0.0285(6) Uani 1 1 d . . .
C6 C 0.2789(3) 0.1120(3) 0.1978(2) 0.0489(10) Uani 1 1 d . . .
H6A H 0.2722 0.0574 0.1900 0.073 Uiso 1 1 calc R . .
H6B H 0.2384 0.1281 0.2277 0.073 Uiso 1 1 calc R . .
H6C H 0.3459 0.1242 0.2203 0.073 Uiso 1 1 calc R . .
C7 C 0.2573(3) 0.2409(2) 0.1383(3) 0.0466(10) Uani 1 1 d . . .
H7A H 0.2376 0.2670 0.0935 0.070 Uiso 1 1 calc R . .
H7B H 0.3242 0.2533 0.1609 0.070 Uiso 1 1 calc R . .
H7C H 0.2165 0.2573 0.1679 0.070 Uiso 1 1 calc R . .
C8 C 0.3117(3) 0.1286(2) 0.0787(2) 0.0397(8) Uani 1 1 d . . .
H8A H 0.2918 0.1553 0.0342 0.060 Uiso 1 1 calc R . .
H8B H 0.3048 0.0740 0.0707 0.060 Uiso 1 1 calc R . .
H8C H 0.3787 0.1406 0.1012 0.060 Uiso 1 1 calc R . .
C9 C -0.1588(3) 0.0201(2) 0.14783(18) 0.0322(7) Uani 1 1 d . . .
H9 H -0.2175 0.0453 0.1548 0.039 Uiso 1 1 calc R . .
C10 C -0.1850(4) -0.0107(3) 0.0737(2) 0.0641(14) Uani 1 1 d . . .
H10A H -0.2005 0.0315 0.0407 0.096 Uiso 1 1 calc R . .
H10B H -0.2406 -0.0442 0.0671 0.096 Uiso 1 1 calc R . .
H10C H -0.1307 -0.0391 0.0656 0.096 Uiso 1 1 calc R . .
C11 C -0.1341(4) -0.0442(3) 0.2010(2) 0.0662(14) Uani 1 1 d . . .
H11A H -0.1176 -0.0230 0.2480 0.099 Uiso 1 1 calc R . .
H11B H -0.0795 -0.0728 0.1937 0.099 Uiso 1 1 calc R . .
H11C H -0.1895 -0.0779 0.1952 0.099 Uiso 1 1 calc R . .
C12 C -0.1945(2) 0.32788(18) 0.17357(15) 0.0232(6) Uani 1 1 d . . .
C13 C -0.1498(2) 0.38414(19) 0.14247(17) 0.0293(7) Uani 1 1 d . . .
H13 H -0.1878 0.4239 0.1176 0.035 Uiso 1 1 calc R . .
C14 C -0.0497(2) 0.38326(18) 0.14713(16) 0.0272(6) Uani 1 1 d . . .
C15 C -0.3047(2) 0.3296(2) 0.16313(17) 0.0303(7) Uani 1 1 d . . .
H15A H -0.3265 0.3828 0.1566 0.036 Uiso 1 1 calc R . .
H15B H -0.3191 0.3108 0.2061 0.036 Uiso 1 1 calc R . .
C16 C -0.3644(2) 0.2816(2) 0.09982(17) 0.0311(7) Uani 1 1 d . . .
C17 C -0.4710(3) 0.2811(3) 0.1037(3) 0.0600(13) Uani 1 1 d . . .
H17A H -0.4748 0.2592 0.1481 0.090 Uiso 1 1 calc R . .
H17B H -0.5095 0.2507 0.0654 0.090 Uiso 1 1 calc R . .
H17C H -0.4956 0.3330 0.1000 0.090 Uiso 1 1 calc R . .
C18 C -0.3270(3) 0.1984(2) 0.1038(2) 0.0489(10) Uani 1 1 d . . .
H18A H -0.3294 0.1760 0.1483 0.073 Uiso 1 1 calc R . .
H18B H -0.2607 0.1982 0.1001 0.073 Uiso 1 1 calc R . .
H18C H -0.3672 0.1689 0.0657 0.073 Uiso 1 1 calc R . .
C19 C -0.3599(3) 0.3164(3) 0.02941(19) 0.0489(10) Uani 1 1 d . . .
H19A H -0.3832 0.3686 0.0265 0.073 Uiso 1 1 calc R . .
H19B H -0.4000 0.2867 -0.0087 0.073 Uiso 1 1 calc R . .
H19C H -0.2935 0.3158 0.0259 0.073 Uiso 1 1 calc R . .
C20 C -0.0052(2) 0.4436(2) 0.10879(18) 0.0315(7) Uani 1 1 d . . .
H20 H -0.0586 0.4739 0.0789 0.038 Uiso 1 1 calc R . .
C21 C 0.0584(4) 0.4975(3) 0.1615(2) 0.0544(11) Uani 1 1 d . . .
H21A H 0.0861 0.5356 0.1367 0.082 Uiso 1 1 calc R . .
H21B H 0.1099 0.4687 0.1927 0.082 Uiso 1 1 calc R . .
H21C H 0.0197 0.5226 0.1886 0.082 Uiso 1 1 calc R . .
C22 C 0.0498(3) 0.4054(3) 0.0609(2) 0.0488(10) Uani 1 1 d . . .
H22A H 0.0064 0.3719 0.0281 0.073 Uiso 1 1 calc R . .
H22B H 0.1033 0.3759 0.0891 0.073 Uiso 1 1 calc R . .
H22C H 0.0745 0.4444 0.0352 0.073 Uiso 1 1 calc R . .
Hf1 Hf 0.0000 0.234541(10) 0.2500 0.01919(6) Uani 1 2 d S . .
O1 O 0.06525(15) 0.19734(13) 0.16759(11) 0.0263(4) Uani 1 1 d . . .
O2 O -0.08798(16) 0.13541(13) 0.20068(11) 0.0267(4) Uani 1 1 d . . .
O3 O -0.14968(15) 0.27170(12) 0.20957(12) 0.0244(4) Uani 1 1 d . . .
O4 O 0.00903(15) 0.33338(13) 0.18232(11) 0.0266(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0343(17) 0.0338(18) 0.0214(14) 0.0008(13) 0.0055(12) 0.0024(13)
C2 0.0371(17) 0.0313(18) 0.0337(16) -0.0084(14) 0.0111(14) -0.0026(14)
C3 0.0336(16) 0.0296(17) 0.0243(14) 0.0008(13) 0.0037(12) -0.0028(13)
C4 0.0405(18) 0.041(2) 0.0293(16) -0.0084(14) 0.0158(14) -0.0027(15)
C5 0.0322(16) 0.0265(17) 0.0286(15) -0.0009(12) 0.0110(12) 0.0039(13)
C6 0.043(2) 0.069(3) 0.0359(19) 0.0120(19) 0.0121(16) 0.014(2)
C7 0.047(2) 0.035(2) 0.070(3) -0.0142(19) 0.037(2) -0.0086(17)
C8 0.0385(19) 0.044(2) 0.0429(19) -0.0040(16) 0.0213(16) 0.0046(16)
C9 0.0336(16) 0.0268(17) 0.0360(16) -0.0074(13) 0.0084(13) -0.0073(13)
C10 0.071(3) 0.082(4) 0.037(2) -0.007(2) 0.010(2) -0.040(3)
C11 0.090(4) 0.050(3) 0.052(2) 0.012(2) 0.006(2) -0.034(3)
C12 0.0217(13) 0.0246(15) 0.0230(13) -0.0046(11) 0.0053(11) -0.0012(11)
C13 0.0261(15) 0.0251(16) 0.0351(16) 0.0038(13) 0.0055(13) 0.0029(12)
C14 0.0300(15) 0.0234(16) 0.0281(15) -0.0020(12) 0.0074(12) 0.0006(12)
C15 0.0217(14) 0.0359(18) 0.0334(16) 0.0018(14) 0.0070(12) 0.0049(13)
C16 0.0228(15) 0.0378(19) 0.0298(15) 0.0051(13) 0.0015(12) -0.0026(13)
C17 0.0268(19) 0.093(4) 0.056(3) -0.004(2) 0.0026(18) -0.012(2)
C18 0.051(2) 0.034(2) 0.048(2) 0.0011(18) -0.0109(18) -0.0091(18)
C19 0.051(2) 0.058(3) 0.0322(18) 0.0086(17) 0.0013(16) -0.0081(19)
C20 0.0332(16) 0.0279(17) 0.0353(16) 0.0066(13) 0.0125(13) -0.0002(13)
C21 0.074(3) 0.043(2) 0.048(2) 0.0001(18) 0.019(2) -0.029(2)
C22 0.063(3) 0.051(2) 0.042(2) 0.0086(18) 0.0303(19) 0.003(2)
Hf1 0.01630(9) 0.01937(10) 0.02284(9) 0.000 0.00677(6) 0.000
O1 0.0297(11) 0.0263(12) 0.0257(10) -0.0055(9) 0.0122(8) -0.0048(9)
O2 0.0289(11) 0.0232(11) 0.0273(10) -0.0011(9) 0.0061(8) -0.0069(9)
O3 0.0156(9) 0.0256(12) 0.0305(11) 0.0041(9) 0.0034(8) 0.0005(8)
O4 0.0223(10) 0.0277(11) 0.0316(11) 0.0069(9) 0.0104(8) -0.0001(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.259(4) . ?
C1 C2 1.396(5) . ?
C1 C4 1.521(4) . ?
C2 C3 1.411(5) . ?
C2 H2 0.9300 . ?
C3 O2 1.232(4) . ?
C3 C9 1.531(4) . ?
C4 C5 1.544(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C7 1.520(5) . ?
C5 C6 1.530(5) . ?
C5 C8 1.534(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.497(5) . ?
C9 C11 1.500(5) . ?
C9 H9 0.9800 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 O3 1.270(4) . ?
C12 C13 1.385(4) . ?
C12 C15 1.521(4) . ?
C13 C14 1.397(4) . ?
C13 H13 0.9300 . ?
C14 O4 1.271(4) . ?
C14 C20 1.515(4) . ?
C15 C16 1.547(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C19 1.518(5) . ?
C16 C18 1.529(6) . ?
C16 C17 1.532(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.503(5) . ?
C20 C22 1.515(5) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
Hf1 O1 2.152(2) 2 ?
Hf1 O1 2.152(2) . ?
Hf1 O3 2.160(2) 2 ?
Hf1 O3 2.160(2) . ?
Hf1 O4 2.187(2) 2 ?
Hf1 O4 2.187(2) . ?
Hf1 O2 2.192(2) . ?
Hf1 O2 2.192(2) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 124.0(3) . . ?
O1 C1 C4 116.7(3) . . ?
C2 C1 C4 119.2(3) . . ?
C1 C2 C3 121.2(3) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
O2 C3 C2 123.5(3) . . ?
O2 C3 C9 116.1(3) . . ?
C2 C3 C9 120.3(3) . . ?
C1 C4 C5 117.4(3) . . ?
C1 C4 H4A 108.0 . . ?
C5 C4 H4A 108.0 . . ?
C1 C4 H4B 108.0 . . ?
C5 C4 H4B 108.0 . . ?
H4A C4 H4B 107.2 . . ?
C7 C5 C6 110.0(3) . . ?
C7 C5 C8 109.2(3) . . ?
C6 C5 C8 109.6(3) . . ?
C7 C5 C4 111.9(3) . . ?
C6 C5 C4 108.5(3) . . ?
C8 C5 C4 107.7(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C11 111.1(4) . . ?
C10 C9 C3 114.2(3) . . ?
C11 C9 C3 111.0(3) . . ?
C10 C9 H9 106.7 . . ?
C11 C9 H9 106.7 . . ?
C3 C9 H9 106.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3 C12 C13 124.2(3) . . ?
O3 C12 C15 115.9(3) . . ?
C13 C12 C15 119.8(3) . . ?
C12 C13 C14 122.4(3) . . ?
C12 C13 H13 118.8 . . ?
C14 C13 H13 118.8 . . ?
O4 C14 C13 123.6(3) . . ?
O4 C14 C20 116.0(3) . . ?
C13 C14 C20 120.4(3) . . ?
C12 C15 C16 115.2(3) . . ?
C12 C15 H15A 108.5 . . ?
C16 C15 H15A 108.5 . . ?
C12 C15 H15B 108.5 . . ?
C16 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C19 C16 C18 108.9(3) . . ?
C19 C16 C17 108.7(3) . . ?
C18 C16 C17 109.0(3) . . ?
C19 C16 C15 111.6(3) . . ?
C18 C16 C15 110.8(3) . . ?
C17 C16 C15 107.8(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C22 112.4(3) . . ?
C21 C20 C14 110.0(3) . . ?
C22 C20 C14 110.6(3) . . ?
C21 C20 H20 107.9 . . ?
C22 C20 H20 107.9 . . ?
C14 C20 H20 107.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O1 Hf1 O1 145.16(12) 2 . ?
O1 Hf1 O3 112.78(8) 2 2 ?
O1 Hf1 O3 77.95(8) . 2 ?
O1 Hf1 O3 77.95(8) 2 . ?
O1 Hf1 O3 112.78(8) . . ?
O3 Hf1 O3 145.33(11) 2 . ?
O1 Hf1 O4 71.24(8) 2 2 ?
O1 Hf1 O4 142.21(8) . 2 ?
O3 Hf1 O4 75.62(8) 2 2 ?
O3 Hf1 O4 77.40(8) . 2 ?
O1 Hf1 O4 142.21(8) 2 . ?
O1 Hf1 O4 71.24(8) . . ?
O3 Hf1 O4 77.40(8) 2 . ?
O3 Hf1 O4 75.62(8) . . ?
O4 Hf1 O4 76.97(12) 2 . ?
O1 Hf1 O2 77.80(8) 2 . ?
O1 Hf1 O2 75.08(8) . . ?
O3 Hf1 O2 141.84(8) 2 . ?
O3 Hf1 O2 71.36(8) . . ?
O4 Hf1 O2 139.72(8) 2 . ?
O4 Hf1 O2 117.59(8) . . ?
O1 Hf1 O2 75.08(8) 2 2 ?
O1 Hf1 O2 77.80(8) . 2 ?
O3 Hf1 O2 71.36(8) 2 2 ?
O3 Hf1 O2 141.84(8) . 2 ?
O4 Hf1 O2 117.59(8) 2 2 ?
O4 Hf1 O2 139.72(8) . 2 ?
O2 Hf1 O2 76.90(12) . 2 ?
C1 O1 Hf1 135.7(2) . . ?
C3 O2 Hf1 136.2(2) . . ?
C12 O3 Hf1 137.13(19) . . ?
C14 O4 Hf1 136.58(19) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.050
_refine_diff_density_min         -1.859
_refine_diff_density_rms         0.100