Supplementary Material (ESI) for Journal of Materials Chemistry
This journal is © The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge	1145

loop_
_publ_author_name
'Paul A. Williams'
'John L. Roberts'
'Anthony C. Jones'
'Jamie F. Bickley'
'Alexander Steiner'
'Paul Chalker'
'Hywel O. Davies'
'Timothy J. Leedham'

_publ_requested_journal       'Journal of Materials Chemistry'


_publ_contact_author_name     	'Prof Anthony C Jones'  
_publ_contact_author_address 
;
Department of Chemistry
University of Liverpool
Liverpool
L69 7ZD
UNITED KINGDOM
;

_publ_contact_author_email       'TONY@TJCONSULTANCY.DEMON.CO.UK'

_publ_section_title		
;
Novel mononuclear zirconium and hafnium alkoxides; Improved
precursors for the MOCVD of ZrO2 and HfO2
;


data_tony67m 
_database_code_CSD                  171865

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C18 H40 O6 Zr' 
_chemical_formula_weight          443.72 

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' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Zr'  'Zr'  -2.9673   0.5597 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            'Orthorhombic' 
_symmetry_space_group_name_H-M    'P 21 21 21'

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

_cell_length_a                    10.2970(12) 
_cell_length_b                    10.7861(12) 
_cell_length_c                    21.258(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2361.1(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     6142 
_cell_measurement_theta_min       5.380 
_cell_measurement_theta_max       55.981

_exptl_crystal_description        block	 
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.45 
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.2  
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.248 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              944 
_exptl_absorpt_coefficient_mu     0.491 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(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    'Bruker Apex CCD area detector'
_diffrn_measurement_method     	   '\w scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             14636 
_diffrn_reflns_av_R_equivalents   0.1032 
_diffrn_reflns_av_sigmaI/netI     0.0800 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          1.92 
_diffrn_reflns_theta_max          28.29 
_reflns_number_total              5439 
_reflns_number_gt                 4699 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection     'SMART (Bruker, 2000)'
_computing_cell_refinement     'SMART'
_computing_data_reduction     'SHELXTL (Bruker, 2000)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     	?
_computing_publication_material     'SHELXL97' 

_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^)+(0.0885P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.02(5) 
_refine_ls_number_reflns          5439 
_refine_ls_number_parameters      239 
_refine_ls_number_restraints      68 
_refine_ls_R_factor_all           0.0452 
_refine_ls_R_factor_gt            0.0389 
_refine_ls_wR_factor_ref          0.1030 
_refine_ls_wR_factor_gt           0.0990 
_refine_ls_goodness_of_fit_ref    0.728 
_refine_ls_restrained_S_all       0.746 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 

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 1.1749(4) 0.0506(4) 0.88444(15) 0.0441(8) Uani 1 1 d . . . 
C2 C 1.2618(5) 0.1473(6) 0.8551(2) 0.0724(14) Uani 1 1 d . . . 
H2A H 1.2819 0.1235 0.8117 0.109 Uiso 1 1 calc R . . 
H2B H 1.3425 0.1536 0.8793 0.109 Uiso 1 1 calc R . . 
H2C H 1.2173 0.2277 0.8552 0.109 Uiso 1 1 calc R . . 
C3 C 1.2426(5) -0.0768(4) 0.88607(19) 0.0642(12) Uani 1 1 d . . . 
H3A H 1.3213 -0.0713 0.9119 0.096 Uiso 1 1 calc R . . 
H3B H 1.2661 -0.1015 0.8432 0.096 Uiso 1 1 calc R . . 
H3C H 1.1836 -0.1384 0.9042 0.096 Uiso 1 1 calc R . . 
C4 C 1.1383(4) 0.0861(4) 0.95157(16) 0.0528(10) Uani 1 1 d . . . 
H4A H 1.1027 0.0135 0.9743 0.063 Uiso 1 1 calc R . . 
H4B H 1.2154 0.1167 0.9746 0.063 Uiso 1 1 calc R . . 
C5 C 1.0046(5) 0.2295(4) 1.00694(16) 0.0524(10) Uani 1 1 d . . . 
H5A H 0.9630 0.1636 1.0315 0.079 Uiso 1 1 calc R . . 
H5B H 0.9435 0.2982 1.0012 0.079 Uiso 1 1 calc R . . 
H5C H 1.0818 0.2592 1.0293 0.079 Uiso 1 1 calc R . . 
C6 C 0.8227(3) 0.3983(3) 0.86180(14) 0.0350(6) Uani 1 1 d . . . 
C7 C 0.6948(4) 0.4698(3) 0.85910(18) 0.0496(9) Uani 1 1 d . . . 
H7A H 0.6271 0.4167 0.8410 0.074 Uiso 1 1 calc R . . 
H7B H 0.7057 0.5437 0.8328 0.074 Uiso 1 1 calc R . . 
H7C H 0.6695 0.4948 0.9017 0.074 Uiso 1 1 calc R . . 
C8 C 0.9258(4) 0.4728(3) 0.89694(16) 0.0441(8) Uani 1 1 d . . . 
H8A H 0.8987 0.4842 0.9407 0.066 Uiso 1 1 calc R . . 
H8B H 0.9362 0.5540 0.8768 0.066 Uiso 1 1 calc R . . 
H8C H 1.0085 0.4281 0.8958 0.066 Uiso 1 1 calc R . . 
C9 C 0.8670(3) 0.3718(3) 0.79442(14) 0.0386(7) Uani 1 1 d . . . 
H9A H 0.7928 0.3438 0.7684 0.046 Uiso 1 1 calc R . . 
H9B H 0.9045 0.4473 0.7751 0.046 Uiso 1 1 calc R . . 
C10 C 1.0172(4) 0.2448(4) 0.73811(15) 0.0439(8) Uani 1 1 d . . . 
H10A H 0.9484 0.2114 0.7112 0.066 Uiso 1 1 calc R . . 
H10B H 1.0860 0.1828 0.7430 0.066 Uiso 1 1 calc R . . 
H10C H 1.0534 0.3197 0.7188 0.066 Uiso 1 1 calc R . . 
C11 C 0.6795(4) 0.0288(4) 0.7582(2) 0.0510(9) Uani 1 1 d D . . 
C12 C 0.5945(8) 0.1412(7) 0.7445(4) 0.068(3) Uiso 0.607(15) 1 d PD A 1 
H12A H 0.5530 0.1691 0.7836 0.102 Uiso 0.607(15) 1 calc PR A 1 
H12B H 0.5275 0.1186 0.7139 0.102 Uiso 0.607(15) 1 calc PR A 1 
H12C H 0.6481 0.2082 0.7274 0.102 Uiso 0.607(15) 1 calc PR A 1 
C13 C 0.7400(7) -0.0078(8) 0.6941(3) 0.055(2) Uiso 0.607(15) 1 d PD A 1 
H13A H 0.7881 0.0628 0.6768 0.082 Uiso 0.607(15) 1 calc PR A 1 
H13B H 0.6708 -0.0316 0.6648 0.082 Uiso 0.607(15) 1 calc PR A 1 
H13C H 0.7993 -0.0780 0.7000 0.082 Uiso 0.607(15) 1 calc PR A 1 
C14 C 0.6045(10) -0.0782(9) 0.7857(5) 0.073(3) Uiso 0.607(15) 1 d PD A 1 
H14A H 0.6639 -0.1470 0.7944 0.110 Uiso 0.607(15) 1 calc PR A 1 
H14B H 0.5380 -0.1052 0.7558 0.110 Uiso 0.607(15) 1 calc PR A 1 
H14C H 0.5628 -0.0518 0.8250 0.110 Uiso 0.607(15) 1 calc PR A 1 
C12' C 0.5701(13) 0.1044(14) 0.7844(8) 0.085(5) Uiso 0.393(15) 1 d PD A 2 
H12D H 0.5538 0.0796 0.8280 0.128 Uiso 0.393(15) 1 calc PR A 2 
H12E H 0.4917 0.0905 0.7592 0.128 Uiso 0.393(15) 1 calc PR A 2 
H12F H 0.5934 0.1924 0.7831 0.128 Uiso 0.393(15) 1 calc PR A 2 
C13' C 0.7103(18) 0.0483(19) 0.6914(6) 0.094(5) Uiso 0.393(15) 1 d PD A 2 
H13D H 0.7324 0.1356 0.6844 0.141 Uiso 0.393(15) 1 calc PR A 2 
H13E H 0.6349 0.0262 0.6656 0.141 Uiso 0.393(15) 1 calc PR A 2 
H13F H 0.7843 -0.0039 0.6795 0.141 Uiso 0.393(15) 1 calc PR A 2 
C14' C 0.6425(13) -0.1080(9) 0.7722(6) 0.059(3) Uiso 0.393(15) 1 d PD A 2 
H14D H 0.7151 -0.1623 0.7608 0.088 Uiso 0.393(15) 1 calc PR A 2 
H14E H 0.5657 -0.1308 0.7475 0.088 Uiso 0.393(15) 1 calc PR A 2 
H14F H 0.6232 -0.1173 0.8171 0.088 Uiso 0.393(15) 1 calc PR A 2 
C15 C 0.7568(7) -0.0897(5) 0.9655(3) 0.0377(16) Uiso 0.603(10) 1 d PD B 1 
C16 C 0.6157(7) -0.0976(7) 0.9618(4) 0.059(2) Uiso 0.603(10) 1 d PD B 1 
H16A H 0.5777 -0.0168 0.9720 0.089 Uiso 0.603(10) 1 calc PR B 1 
H16B H 0.5844 -0.1597 0.9919 0.089 Uiso 0.603(10) 1 calc PR B 1 
H16C H 0.5901 -0.1218 0.9191 0.089 Uiso 0.603(10) 1 calc PR B 1 
C17 C 0.7990(9) -0.0730(7) 1.0363(3) 0.064(2) Uiso 0.603(10) 1 d PD B 1 
H17A H 0.8939 -0.0776 1.0395 0.096 Uiso 0.603(10) 1 calc PR B 1 
H17B H 0.7601 -0.1388 1.0619 0.096 Uiso 0.603(10) 1 calc PR B 1 
H17C H 0.7694 0.0079 1.0517 0.096 Uiso 0.603(10) 1 calc PR B 1 
C18 C 0.8384(9) -0.2007(7) 0.9398(4) 0.051(2) Uiso 0.603(10) 1 d PD B 1 
H18A H 0.8178 -0.2140 0.8953 0.077 Uiso 0.603(10) 1 calc PR B 1 
H18B H 0.8175 -0.2757 0.9637 0.077 Uiso 0.603(10) 1 calc PR B 1 
H18C H 0.9311 -0.1821 0.9442 0.077 Uiso 0.603(10) 1 calc PR B 1 
C15' C 0.8015(9) -0.0920(7) 0.9759(4) 0.034(2) Uiso 0.397(10) 1 d PD B 2 
C16' C 0.6640(12) -0.0741(14) 0.9975(8) 0.087(5) Uiso 0.397(10) 1 d PD B 2 
H16D H 0.6090 -0.0544 0.9612 0.130 Uiso 0.397(10) 1 calc PR B 2 
H16E H 0.6605 -0.0059 1.0279 0.130 Uiso 0.397(10) 1 calc PR B 2 
H16F H 0.6329 -0.1505 1.0174 0.130 Uiso 0.397(10) 1 calc PR B 2 
C17' C 0.8906(11) -0.0987(11) 1.0355(5) 0.061(3) Uiso 0.397(10) 1 d PD B 2 
H17D H 0.9817 -0.0923 1.0227 0.091 Uiso 0.397(10) 1 calc PR B 2 
H17E H 0.8765 -0.1779 1.0571 0.091 Uiso 0.397(10) 1 calc PR B 2 
H17F H 0.8691 -0.0303 1.0639 0.091 Uiso 0.397(10) 1 calc PR B 2 
C18' C 0.7984(14) -0.2086(10) 0.9343(5) 0.050(3) Uiso 0.397(10) 1 d PD B 2 
H18D H 0.7407 -0.1943 0.8983 0.075 Uiso 0.397(10) 1 calc PR B 2 
H18E H 0.7662 -0.2790 0.9589 0.075 Uiso 0.397(10) 1 calc PR B 2 
H18F H 0.8862 -0.2267 0.9191 0.075 Uiso 0.397(10) 1 calc PR B 2 
O1 O 1.0583(2) 0.0402(2) 0.84956(10) 0.0367(5) Uani 1 1 d . . . 
O2 O 1.0420(3) 0.1820(2) 0.94680(10) 0.0442(6) Uani 1 1 d . . . 
O3 O 0.8031(2) 0.28247(19) 0.89144(10) 0.0346(5) Uani 1 1 d . . . 
O4 O 0.9641(2) 0.2751(2) 0.79886(10) 0.0351(5) Uani 1 1 d . . . 
O5 O 0.7856(2) 0.0602(2) 0.79710(11) 0.0435(6) Uani 1 1 d . A . 
O6 O 0.8139(3) 0.0147(2) 0.93540(13) 0.0572(8) Uani 1 1 d . . . 
Zr1 Zr 0.88477(3) 0.11813(2) 0.869235(12) 0.03128(10) Uani 1 1 d . A . 

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 0.052(2) 0.0501(19) 0.0303(17) 0.0021(14) -0.0031(14) 0.0045(16) 
C2 0.065(3) 0.105(4) 0.047(2) 0.010(2) -0.010(2) -0.021(3) 
C3 0.070(3) 0.079(3) 0.044(2) -0.002(2) -0.0074(19) 0.030(2) 
C4 0.071(3) 0.059(2) 0.0285(15) 0.0005(15) -0.0116(17) 0.0141(19) 
C5 0.087(3) 0.047(2) 0.0231(16) -0.0101(15) -0.0035(18) 0.007(2) 
C6 0.0473(17) 0.0321(15) 0.0257(14) 0.0025(13) -0.0042(13) 0.0010(12) 
C7 0.063(2) 0.0443(19) 0.042(2) 0.0016(15) -0.0028(17) 0.0130(16) 
C8 0.067(2) 0.0333(16) 0.0324(16) -0.0027(14) -0.0029(16) -0.0027(15) 
C9 0.0528(19) 0.0357(15) 0.0273(13) 0.0045(13) -0.0022(13) 0.0016(16) 
C10 0.063(2) 0.0509(19) 0.0180(14) -0.0016(14) 0.0088(15) -0.0062(17) 
C11 0.046(2) 0.047(2) 0.060(2) -0.0114(18) -0.0123(18) -0.0049(16) 
O1 0.0468(13) 0.0394(11) 0.0241(10) -0.0025(9) -0.0010(9) 0.0066(10) 
O2 0.0661(17) 0.0453(13) 0.0213(10) -0.0038(10) -0.0086(11) 0.0082(12) 
O3 0.0489(13) 0.0324(11) 0.0225(9) 0.0016(9) 0.0025(9) -0.0003(9) 
O4 0.0521(14) 0.0342(11) 0.0189(9) 0.0020(8) 0.0016(9) -0.0018(10) 
O5 0.0416(13) 0.0491(14) 0.0397(13) -0.0136(11) -0.0012(10) -0.0065(11) 
O6 0.090(2) 0.0380(14) 0.0432(14) 0.0072(11) 0.0272(14) -0.0035(13) 
Zr1 0.04518(16) 0.02818(13) 0.02047(13) 0.00014(11) 0.00416(12) -0.00238(12) 

_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 1.416(5) . ? 
C1 C2 1.509(6) . ? 
C1 C4 1.525(5) . ? 
C1 C3 1.541(5) . ? 
C4 O2 1.436(5) . ? 
C5 O2 1.430(4) . ? 
C6 O3 1.414(4) . ? 
C6 C8 1.526(5) . ? 
C6 C7 1.527(5) . ? 
C6 C9 1.531(4) . ? 
C9 O4 1.448(4) . ? 
C10 O4 1.440(4) . ? 
C11 O5 1.412(4) . ? 
C11 C13' 1.471(11) . ? 
C11 C12' 1.498(11) . ? 
C11 C14 1.507(8) . ? 
C11 C12 1.524(8) . ? 
C11 C13 1.550(7) . ? 
C11 C14' 1.553(9) . ? 
C15 O6 1.422(6) . ? 
C15 C16 1.457(9) . ? 
C15 C18 1.562(8) . ? 
C15 C17 1.578(8) . ? 
C15' O6 1.443(9) . ? 
C15' C16' 1.501(12) . ? 
C15' C18' 1.537(10) . ? 
C15' C17' 1.566(11) . ? 
O1 Zr1 2.018(2) . ? 
O2 Zr1 2.411(2) . ? 
O3 Zr1 2.018(2) . ? 
O4 Zr1 2.403(2) . ? 
O5 Zr1 1.945(2) . ? 
O6 Zr1 1.938(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 109.9(3) . . ? 
O1 C1 C4 107.5(3) . . ? 
C2 C1 C4 111.1(4) . . ? 
O1 C1 C3 109.0(3) . . ? 
C2 C1 C3 110.9(4) . . ? 
C4 C1 C3 108.3(3) . . ? 
O2 C4 C1 106.6(3) . . ? 
O3 C6 C8 110.3(3) . . ? 
O3 C6 C7 109.9(3) . . ? 
C8 C6 C7 110.6(3) . . ? 
O3 C6 C9 107.1(2) . . ? 
C8 C6 C9 110.4(3) . . ? 
C7 C6 C9 108.4(3) . . ? 
O4 C9 C6 106.2(2) . . ? 
O5 C11 C13' 111.4(8) . . ? 
O5 C11 C12' 103.5(7) . . ? 
C13' C11 C12' 116.3(10) . . ? 
O5 C11 C14 110.7(5) . . ? 
C13' C11 C14 126.6(9) . . ? 
C12' C11 C14 83.5(7) . . ? 
O5 C11 C12 111.4(4) . . ? 
C13' C11 C12 80.0(9) . . ? 
C12' C11 C12 37.4(6) . . ? 
C14 C11 C12 112.8(5) . . ? 
O5 C11 C13 105.4(4) . . ? 
C13' C11 C13 25.9(8) . . ? 
C12' C11 C13 140.2(8) . . ? 
C14 C11 C13 110.6(5) . . ? 
C12 C11 C13 105.5(5) . . ? 
O5 C11 C14' 107.8(5) . . ? 
C13' C11 C14' 112.0(9) . . ? 
C12' C11 C14' 105.1(8) . . ? 
C14 C11 C14' 21.9(5) . . ? 
C12 C11 C14' 130.6(6) . . ? 
C13 C11 C14' 91.4(6) . . ? 
O6 C15 C16 115.8(6) . . ? 
O6 C15 C18 103.1(5) . . ? 
C16 C15 C18 118.2(6) . . ? 
O6 C15 C17 103.0(5) . . ? 
C16 C15 C17 109.4(6) . . ? 
C18 C15 C17 105.9(6) . . ? 
O6 C15' C16' 99.4(8) . . ? 
O6 C15' C18' 108.2(7) . . ? 
C16' C15' C18' 105.2(9) . . ? 
O6 C15' C17' 117.9(7) . . ? 
C16' C15' C17' 108.1(9) . . ? 
C18' C15' C17' 116.1(9) . . ? 
C1 O1 Zr1 127.54(19) . . ? 
C5 O2 C4 112.4(3) . . ? 
C5 O2 Zr1 122.2(3) . . ? 
C4 O2 Zr1 107.8(2) . . ? 
C6 O3 Zr1 127.80(18) . . ? 
C10 O4 C9 111.5(2) . . ? 
C10 O4 Zr1 121.9(2) . . ? 
C9 O4 Zr1 108.25(17) . . ? 
C11 O5 Zr1 160.9(2) . . ? 
C15 O6 C15' 20.5(3) . . ? 
C15 O6 Zr1 159.7(3) . . ? 
C15' O6 Zr1 157.7(4) . . ? 
O6 Zr1 O5 100.95(12) . . ? 
O6 Zr1 O3 100.32(10) . . ? 
O5 Zr1 O3 104.35(10) . . ? 
O6 Zr1 O1 104.12(11) . . ? 
O5 Zr1 O1 99.64(10) . . ? 
O3 Zr1 O1 141.54(10) . . ? 
O6 Zr1 O4 170.30(9) . . ? 
O5 Zr1 O4 85.06(10) . . ? 
O3 Zr1 O4 70.63(8) . . ? 
O1 Zr1 O4 82.13(9) . . ? 
O6 Zr1 O2 85.45(12) . . ? 
O5 Zr1 O2 169.47(10) . . ? 
O3 Zr1 O2 82.46(9) . . ? 
O1 Zr1 O2 70.50(9) . . ? 
O4 Zr1 O2 89.79(8) . . ? 

loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
O1 C1 C4 O2 -44.6(4) . . . . ? 
C2 C1 C4 O2 75.8(4) . . . . ? 
C3 C1 C4 O2 -162.2(4) . . . . ? 
O3 C6 C9 O4 -44.9(3) . . . . ? 
C8 C6 C9 O4 75.1(3) . . . . ? 
C7 C6 C9 O4 -163.5(3) . . . . ? 
C2 C1 O1 Zr1 -98.9(4) . . . . ? 
C4 C1 O1 Zr1 22.2(4) . . . . ? 
C3 C1 O1 Zr1 139.4(3) . . . . ? 
C1 C4 O2 C5 -176.4(3) . . . . ? 
C1 C4 O2 Zr1 46.1(4) . . . . ? 
C8 C6 O3 Zr1 -95.8(3) . . . . ? 
C7 C6 O3 Zr1 142.0(2) . . . . ? 
C9 C6 O3 Zr1 24.4(3) . . . . ? 
C6 C9 O4 C10 -177.9(3) . . . . ? 
C6 C9 O4 Zr1 45.4(3) . . . . ? 
C13' C11 O5 Zr1 147.9(11) . . . . ? 
C12' C11 O5 Zr1 22.2(11) . . . . ? 
C14 C11 O5 Zr1 -65.8(10) . . . . ? 
C12 C11 O5 Zr1 60.6(10) . . . . ? 
C13 C11 O5 Zr1 174.5(7) . . . . ? 
C14' C11 O5 Zr1 -88.9(10) . . . . ? 
C16 C15 O6 C15' 164.2(15) . . . . ? 
C18 C15 O6 C15' -65.2(12) . . . . ? 
C17 C15 O6 C15' 44.8(12) . . . . ? 
C16 C15 O6 Zr1 -83.0(11) . . . . ? 
C18 C15 O6 Zr1 47.6(13) . . . . ? 
C17 C15 O6 Zr1 157.6(9) . . . . ? 
C16' C15' O6 C15 -37.9(12) . . . . ? 
C18' C15' O6 C15 71.6(13) . . . . ? 
C17' C15' O6 C15 -154.2(17) . . . . ? 
C16' C15' O6 Zr1 -160.3(11) . . . . ? 
C18' C15' O6 Zr1 -50.9(16) . . . . ? 
C17' C15' O6 Zr1 83.3(12) . . . . ? 
C15 O6 Zr1 O5 30.1(11) . . . . ? 
C15' O6 Zr1 O5 88.7(11) . . . . ? 
C15 O6 Zr1 O3 137.0(10) . . . . ? 
C15' O6 Zr1 O3 -164.4(11) . . . . ? 
C15 O6 Zr1 O1 -72.9(11) . . . . ? 
C15' O6 Zr1 O1 -14.3(11) . . . . ? 
C15 O6 Zr1 O4 157.7(9) . . . . ? 
C15' O6 Zr1 O4 -143.7(10) . . . . ? 
C15 O6 Zr1 O2 -141.5(11) . . . . ? 
C15' O6 Zr1 O2 -82.9(11) . . . . ? 
C11 O5 Zr1 O6 55.1(8) . . . . ? 
C11 O5 Zr1 O3 -48.7(8) . . . . ? 
C11 O5 Zr1 O1 161.6(8) . . . . ? 
C11 O5 Zr1 O4 -117.2(8) . . . . ? 
C11 O5 Zr1 O2 -178.2(6) . . . . ? 
C6 O3 Zr1 O6 176.7(2) . . . . ? 
C6 O3 Zr1 O5 -79.1(2) . . . . ? 
C6 O3 Zr1 O1 47.8(3) . . . . ? 
C6 O3 Zr1 O4 0.3(2) . . . . ? 
C6 O3 Zr1 O2 92.7(2) . . . . ? 
C1 O1 Zr1 O6 -77.7(3) . . . . ? 
C1 O1 Zr1 O5 178.4(2) . . . . ? 
C1 O1 Zr1 O3 50.2(3) . . . . ? 
C1 O1 Zr1 O4 94.8(3) . . . . ? 
C1 O1 Zr1 O2 2.2(2) . . . . ? 
C10 O4 Zr1 O6 -179.5(7) . . . . ? 
C9 O4 Zr1 O6 -48.2(8) . . . . ? 
C10 O4 Zr1 O5 -50.8(3) . . . . ? 
C9 O4 Zr1 O5 80.53(19) . . . . ? 
C10 O4 Zr1 O3 -157.9(3) . . . . ? 
C9 O4 Zr1 O3 -26.58(18) . . . . ? 
C10 O4 Zr1 O1 49.7(3) . . . . ? 
C9 O4 Zr1 O1 -179.00(19) . . . . ? 
C10 O4 Zr1 O2 120.1(3) . . . . ? 
C9 O4 Zr1 O2 -108.66(19) . . . . ? 
C5 O2 Zr1 O6 -53.5(3) . . . . ? 
C4 O2 Zr1 O6 79.0(2) . . . . ? 
C5 O2 Zr1 O5 178.6(5) . . . . ? 
C4 O2 Zr1 O5 -48.9(6) . . . . ? 
C5 O2 Zr1 O3 47.5(3) . . . . ? 
C4 O2 Zr1 O3 -180.0(2) . . . . ? 
C5 O2 Zr1 O1 -160.2(3) . . . . ? 
C4 O2 Zr1 O1 -27.7(2) . . . . ? 
C5 O2 Zr1 O4 118.0(3) . . . . ? 
C4 O2 Zr1 O4 -109.5(2) . . . . ? 

_diffrn_measured_fraction_theta_max    0.947 
_diffrn_reflns_theta_full              28.29 
_diffrn_measured_fraction_theta_full   0.947 
_refine_diff_density_max    0.670 
_refine_diff_density_min   -0.899 
_refine_diff_density_rms    0.075 

data_tony68m 
_database_code_CSD                  171866

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C18 H40 Hf O6' 
_chemical_formula_weight          530.99 

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' 
'O'  'O'   0.0106   0.0060 
'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' 

_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    'P 21 21 21' 

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

_cell_length_a                    10.1972(8) 
_cell_length_b                    10.7413(8) 
_cell_length_c                    21.3221(17) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2335.4(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     5852 
_cell_measurement_theta_min       5.384 
_cell_measurement_theta_max       56.535 


_exptl_crystal_description        'plate'
_exptl_crystal_colour             Colourless 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.510 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1072 
_exptl_absorpt_coefficient_mu     4.492 
_exptl_absorpt_correction_type    'Sadabs, Bruker, 2000' 
_exptl_absorpt_correction_T_min   0.2123 
_exptl_absorpt_correction_T_max   0.5522 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(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    'Bruker Apex CCD area detector'
_diffrn_measurement_method     	   '\w scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             13992 
_diffrn_reflns_av_R_equivalents   0.0224 
_diffrn_reflns_av_sigmaI/netI     0.0331 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          1.91 
_diffrn_reflns_theta_max          28.27 
_reflns_number_total              5260 
_reflns_number_gt                 5156 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection     'SMART (Bruker, 2000)'
_computing_cell_refinement     'SMART'
_computing_data_reduction     'SHELXTL (Bruker, 2000)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     	?
_computing_publication_material     'SHELXL97'

_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^)+(0.0243P)^2^+2.6270P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.036(12) 
_refine_ls_number_reflns          5260 
_refine_ls_number_parameters      235 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0254 
_refine_ls_R_factor_gt            0.0247 
_refine_ls_wR_factor_ref          0.0609 
_refine_ls_wR_factor_gt           0.0606 
_refine_ls_goodness_of_fit_ref    1.077 
_refine_ls_restrained_S_all       1.077 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 

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 -0.1717(5) 0.4521(5) 0.1153(2) 0.0387(11) Uani 1 1 d . . . 
C2 C -0.2595(6) 0.3551(7) 0.1440(3) 0.0580(15) Uani 1 1 d . . . 
H2A H -0.2150 0.2742 0.1433 0.087 Uiso 1 1 calc R . . 
H2B H -0.3411 0.3497 0.1198 0.087 Uiso 1 1 calc R . . 
H2C H -0.2796 0.3781 0.1874 0.087 Uiso 1 1 calc R . . 
C3 C -0.2396(6) 0.5808(6) 0.1147(3) 0.0546(15) Uani 1 1 d . . . 
H3A H -0.2674 0.6024 0.1573 0.082 Uiso 1 1 calc R . . 
H3B H -0.3163 0.5778 0.0871 0.082 Uiso 1 1 calc R . . 
H3C H -0.1780 0.6438 0.0993 0.082 Uiso 1 1 calc R . . 
C4 C -0.1339(5) 0.4171(4) 0.0486(2) 0.0412(11) Uani 1 1 d . . . 
H4A H -0.2114 0.3864 0.0253 0.049 Uiso 1 1 calc R . . 
H4B H -0.0976 0.4902 0.0262 0.049 Uiso 1 1 calc R . . 
C5 C 0.0008(6) 0.2713(5) -0.0063(2) 0.0443(12) Uani 1 1 d . . . 
H5A H -0.0761 0.2349 -0.0269 0.066 Uiso 1 1 calc R . . 
H5B H 0.0677 0.2069 -0.0004 0.066 Uiso 1 1 calc R . . 
H5C H 0.0363 0.3383 -0.0325 0.066 Uiso 1 1 calc R . . 
C6 C 0.1783(4) 0.0998(4) 0.1381(2) 0.0318(8) Uani 1 1 d . . . 
C7 C 0.3063(5) 0.0281(5) 0.1407(3) 0.0438(11) Uani 1 1 d . . . 
H7A H 0.3343 0.0071 0.0980 0.066 Uiso 1 1 calc R . . 
H7B H 0.2937 -0.0485 0.1649 0.066 Uiso 1 1 calc R . . 
H7C H 0.3736 0.0795 0.1609 0.066 Uiso 1 1 calc R . . 
C8 C 0.0743(5) 0.0268(4) 0.1018(2) 0.0386(10) Uani 1 1 d . . . 
H8A H -0.0091 0.0723 0.1030 0.058 Uiso 1 1 calc R . . 
H8B H 0.0627 -0.0553 0.1211 0.058 Uiso 1 1 calc R . . 
H8C H 0.1024 0.0168 0.0582 0.058 Uiso 1 1 calc R . . 
C9 C 0.1320(4) 0.1260(4) 0.20451(18) 0.0346(8) Uani 1 1 d . . . 
H9A H 0.0926 0.0504 0.2232 0.041 Uiso 1 1 calc R . . 
H9B H 0.2064 0.1528 0.2311 0.041 Uiso 1 1 calc R . . 
C10 C -0.0183(5) 0.2556(5) 0.2606(2) 0.0383(11) Uani 1 1 d . . . 
H10A H -0.0535 0.1804 0.2804 0.057 Uiso 1 1 calc R . . 
H10B H -0.0888 0.3168 0.2554 0.057 Uiso 1 1 calc R . . 
H10C H 0.0509 0.2909 0.2871 0.057 Uiso 1 1 calc R . . 
C11 C 0.3216(5) 0.4673(5) 0.2437(2) 0.0382(10) Uani 1 1 d . . . 
C12 C 0.4090(10) 0.3559(9) 0.2538(5) 0.062(3) Uiso 0.644(14) 1 d P A 1 
H12A H 0.3605 0.2915 0.2766 0.093 Uiso 0.644(14) 1 calc PR A 1 
H12B H 0.4861 0.3808 0.2782 0.093 Uiso 0.644(14) 1 calc PR A 1 
H12C H 0.4372 0.3230 0.2131 0.093 Uiso 0.644(14) 1 calc PR A 1 
C13 C 0.2639(10) 0.5008(10) 0.3073(5) 0.054(3) Uiso 0.644(14) 1 d P A 1 
H13A H 0.2185 0.5810 0.3043 0.081 Uiso 0.644(14) 1 calc PR A 1 
H13B H 0.3344 0.5067 0.3383 0.081 Uiso 0.644(14) 1 calc PR A 1 
H13C H 0.2014 0.4363 0.3201 0.081 Uiso 0.644(14) 1 calc PR A 1 
C14 C 0.3957(11) 0.5734(10) 0.2162(5) 0.065(3) Uiso 0.644(14) 1 d P A 1 
H14A H 0.4481 0.5438 0.1807 0.098 Uiso 0.644(14) 1 calc PR A 1 
H14B H 0.4539 0.6091 0.2481 0.098 Uiso 0.644(14) 1 calc PR A 1 
H14C H 0.3341 0.6372 0.2017 0.098 Uiso 0.644(14) 1 calc PR A 1 
C12' C 0.4350(13) 0.3984(10) 0.2146(8) 0.068(6) Uiso 0.356(14) 1 d PR A 2 
H12A' H 0.4154 0.3091 0.2136 0.102 Uiso 0.356(14) 1 d PR A 2 
H12B' H 0.5144 0.4126 0.2396 0.102 Uiso 0.356(14) 1 d PR A 2 
H12C' H 0.4492 0.4287 0.1718 0.102 Uiso 0.356(14) 1 d PR A 2 
C13' C 0.300(3) 0.424(3) 0.3078(12) 0.094(8) Uiso 0.356(14) 1 d P A 2 
H13A' H 0.2152 0.4553 0.3229 0.141 Uiso 0.356(14) 1 calc PR A 2 
H13B' H 0.3701 0.4552 0.3349 0.141 Uiso 0.356(14) 1 calc PR A 2 
H13C' H 0.2995 0.3329 0.3085 0.141 Uiso 0.356(14) 1 calc PR A 2 
C14' C 0.3586(17) 0.6054(16) 0.2317(8) 0.050(4) Uiso 0.356(14) 1 d P A 2 
H14A' H 0.3847 0.6158 0.1878 0.075 Uiso 0.356(14) 1 calc PR A 2 
H14B' H 0.4316 0.6290 0.2591 0.075 Uiso 0.356(14) 1 calc PR A 2 
H14C' H 0.2827 0.6586 0.2406 0.075 Uiso 0.356(14) 1 calc PR A 2 
C15 C 0.2365(6) 0.5891(5) 0.0339(3) 0.0481(13) Uani 1 1 d . . . 
C16 C 0.1783(8) 0.7026(5) 0.0644(3) 0.0622(17) Uani 1 1 d . . . 
H16A H 0.0829 0.7022 0.0586 0.093 Uiso 1 1 calc R . . 
H16B H 0.2153 0.7776 0.0451 0.093 Uiso 1 1 calc R . . 
H16C H 0.1987 0.7021 0.1093 0.093 Uiso 1 1 calc R . . 
C17 C 0.3859(7) 0.5966(7) 0.0371(4) 0.085(2) Uani 1 1 d . . . 
H17A H 0.4136 0.6012 0.0810 0.128 Uiso 1 1 calc R . . 
H17B H 0.4159 0.6711 0.0147 0.128 Uiso 1 1 calc R . . 
H17C H 0.4239 0.5224 0.0175 0.128 Uiso 1 1 calc R . . 
C18 C 0.1944(12) 0.5759(7) -0.0332(3) 0.107(4) Uani 1 1 d . . . 
H18A H 0.2162 0.4921 -0.0482 0.161 Uiso 1 1 calc R . . 
H18B H 0.2400 0.6378 -0.0589 0.161 Uiso 1 1 calc R . . 
H18C H 0.0995 0.5889 -0.0363 0.161 Uiso 1 1 calc R . . 
Hf1 Hf 0.118379(15) 0.380435(13) 0.131704(7) 0.02578(5) Uani 1 1 d . . . 
O1 O -0.0546(3) 0.4610(3) 0.15074(14) 0.0324(7) Uani 1 1 d . A . 
O2 O -0.0368(3) 0.3210(3) 0.05379(14) 0.0359(7) Uani 1 1 d . A . 
O3 O 0.1997(3) 0.2165(3) 0.10836(14) 0.0298(6) Uani 1 1 d . A . 
O4 O 0.0352(3) 0.2244(3) 0.20005(14) 0.0300(6) Uani 1 1 d . A . 
O5 O 0.2147(3) 0.4366(3) 0.20442(15) 0.0361(7) Uani 1 1 d . A . 
O6 O 0.1950(4) 0.4837(3) 0.06722(17) 0.0443(9) Uani 1 1 d . A . 

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 0.037(2) 0.044(2) 0.035(3) 0.0000(19) -0.0042(18) 0.004(2) 
C2 0.049(3) 0.078(4) 0.047(3) -0.001(3) -0.007(2) -0.018(3) 
C3 0.054(3) 0.065(3) 0.045(3) -0.005(2) -0.005(2) 0.028(3) 
C4 0.045(3) 0.045(2) 0.033(2) 0.0005(18) -0.013(2) 0.009(2) 
C5 0.065(4) 0.047(3) 0.021(2) -0.008(2) -0.007(2) 0.004(3) 
C6 0.040(2) 0.0296(19) 0.026(2) 0.0016(17) -0.0038(16) 0.0023(16) 
C7 0.050(3) 0.038(2) 0.044(3) 0.004(2) -0.006(2) 0.013(2) 
C8 0.050(3) 0.035(2) 0.031(2) -0.0046(19) -0.004(2) -0.0008(19) 
C9 0.045(2) 0.0315(18) 0.0268(18) 0.0045(16) -0.0024(16) -0.002(2) 
C10 0.053(3) 0.045(3) 0.017(2) 0.0002(18) 0.0073(19) -0.004(2) 
C11 0.031(2) 0.040(2) 0.044(3) -0.009(2) -0.0099(19) -0.0021(19) 
C15 0.074(4) 0.029(2) 0.041(3) 0.004(2) 0.018(2) -0.003(2) 
C16 0.085(5) 0.035(3) 0.066(4) 0.000(3) 0.010(3) 0.010(3) 
C17 0.079(5) 0.073(4) 0.103(6) 0.016(4) 0.049(4) -0.009(4) 
C18 0.220(12) 0.072(5) 0.030(3) 0.015(3) 0.003(5) -0.057(6) 
Hf1 0.03168(8) 0.02406(7) 0.02160(7) 0.00047(6) 0.00105(6) -0.00193(7) 
O1 0.0351(16) 0.0361(15) 0.0260(15) -0.0045(12) -0.0040(12) 0.0060(13) 
O2 0.0475(19) 0.0374(16) 0.0229(15) -0.0032(13) -0.0091(13) 0.0077(14) 
O3 0.0365(16) 0.0275(14) 0.0253(14) 0.0027(12) 0.0034(12) 0.0025(12) 
O4 0.0392(17) 0.0316(15) 0.0192(14) 0.0013(12) 0.0029(12) -0.0020(13) 
O5 0.0340(16) 0.0419(17) 0.0322(16) -0.0075(14) -0.0042(13) -0.0055(14) 
O6 0.065(2) 0.0327(17) 0.0350(18) 0.0075(14) 0.0187(17) -0.0046(16) 

_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 1.416(6) . ? 
C1 C2 1.503(7) . ? 
C1 C4 1.522(7) . ? 
C1 C3 1.545(7) . ? 
C4 O2 1.435(5) . ? 
C5 O2 1.440(6) . ? 
C6 O3 1.421(5) . ? 
C6 C7 1.516(6) . ? 
C6 C9 1.520(6) . ? 
C6 C8 1.529(6) . ? 
C9 O4 1.448(5) . ? 
C10 O4 1.441(5) . ? 
C11 O5 1.414(5) . ? 
C11 C13' 1.46(3) . ? 
C11 C14 1.488(11) . ? 
C11 C12' 1.507(12) . ? 
C11 C12 1.507(11) . ? 
C11 C13 1.520(11) . ? 
C11 C14' 1.552(17) . ? 
C15 O6 1.402(6) . ? 
C15 C18 1.500(9) . ? 
C15 C16 1.503(7) . ? 
C15 C17 1.527(10) . ? 
Hf1 O6 1.932(3) . ? 
Hf1 O5 1.932(3) . ? 
Hf1 O1 2.006(3) . ? 
Hf1 O3 2.009(3) . ? 
Hf1 O4 2.377(3) . ? 
Hf1 O2 2.382(3) . ? 

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 109.4(4) . . ? 
O1 C1 C4 107.5(4) . . ? 
C2 C1 C4 111.1(4) . . ? 
O1 C1 C3 108.8(4) . . ? 
C2 C1 C3 110.9(5) . . ? 
C4 C1 C3 109.0(4) . . ? 
O2 C4 C1 106.3(3) . . ? 
O3 C6 C7 109.4(4) . . ? 
O3 C6 C9 107.5(3) . . ? 
C7 C6 C9 109.1(4) . . ? 
O3 C6 C8 109.5(4) . . ? 
C7 C6 C8 110.8(4) . . ? 
C9 C6 C8 110.5(4) . . ? 
O4 C9 C6 106.6(3) . . ? 
O5 C11 C13' 111.3(11) . . ? 
O5 C11 C14 109.7(6) . . ? 
C13' C11 C14 133.6(12) . . ? 
O5 C11 C12' 103.5(8) . . ? 
C13' C11 C12' 110.2(13) . . ? 
C14 C11 C12' 79.8(5) . . ? 
O5 C11 C12 110.8(5) . . ? 
C13' C11 C12 72.8(12) . . ? 
C14 C11 C12 111.3(6) . . ? 
C12' C11 C12 38.3(6) . . ? 
O5 C11 C13 106.6(5) . . ? 
C13' C11 C13 35.2(11) . . ? 
C14 C11 C13 111.5(7) . . ? 
C12' C11 C13 141.3(9) . . ? 
C12 C11 C13 106.8(6) . . ? 
O5 C11 C14' 108.2(7) . . ? 
C13' C11 C14' 119.7(13) . . ? 
C14 C11 C14' 23.0(7) . . ? 
C12' C11 C14' 102.4(8) . . ? 
C12 C11 C14' 129.7(8) . . ? 
C13 C11 C14' 90.9(8) . . ? 
O6 C15 C18 108.7(5) . . ? 
O6 C15 C16 108.5(4) . . ? 
C18 C15 C16 112.1(6) . . ? 
O6 C15 C17 108.7(5) . . ? 
C18 C15 C17 109.4(6) . . ? 
C16 C15 C17 109.4(6) . . ? 
O6 Hf1 O5 100.75(15) . . ? 
O6 Hf1 O1 104.59(15) . . ? 
O5 Hf1 O1 98.63(13) . . ? 
O6 Hf1 O3 99.21(14) . . ? 
O5 Hf1 O3 105.22(13) . . ? 
O1 Hf1 O3 142.29(13) . . ? 
O6 Hf1 O4 170.21(12) . . ? 
O5 Hf1 O4 84.80(12) . . ? 
O1 Hf1 O4 82.33(12) . . ? 
O3 Hf1 O4 71.41(11) . . ? 
O6 Hf1 O2 85.77(15) . . ? 
O5 Hf1 O2 168.90(13) . . ? 
O1 Hf1 O2 70.87(12) . . ? 
O3 Hf1 O2 82.34(12) . . ? 
O4 Hf1 O2 90.09(11) . . ? 
C1 O1 Hf1 127.2(3) . . ? 
C4 O2 C5 112.5(3) . . ? 
C4 O2 Hf1 108.6(2) . . ? 
C5 O2 Hf1 122.9(3) . . ? 
C6 O3 Hf1 126.8(2) . . ? 
C10 O4 C9 111.7(3) . . ? 
C10 O4 Hf1 121.3(3) . . ? 
C9 O4 Hf1 108.2(2) . . ? 
C11 O5 Hf1 160.1(3) . . ? 
C15 O6 Hf1 161.2(3) . . ? 

loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
O1 C1 C4 O2 43.9(5) . . . . ? 
C2 C1 C4 O2 -75.7(5) . . . . ? 
C3 C1 C4 O2 161.7(4) . . . . ? 
O3 C6 C9 O4 44.4(4) . . . . ? 
C7 C6 C9 O4 162.9(3) . . . . ? 
C8 C6 C9 O4 -75.0(4) . . . . ? 
C2 C1 O1 Hf1 98.1(5) . . . . ? 
C4 C1 O1 Hf1 -22.6(5) . . . . ? 
C3 C1 O1 Hf1 -140.6(3) . . . . ? 
O6 Hf1 O1 C1 78.6(4) . . . . ? 
O5 Hf1 O1 C1 -177.8(3) . . . . ? 
O3 Hf1 O1 C1 -48.8(4) . . . . ? 
O4 Hf1 O1 C1 -94.3(3) . . . . ? 
O2 Hf1 O1 C1 -1.6(3) . . . . ? 
C1 C4 O2 C5 175.3(4) . . . . ? 
C1 C4 O2 Hf1 -45.3(4) . . . . ? 
O6 Hf1 O2 C4 -79.9(3) . . . . ? 
O5 Hf1 O2 C4 46.6(8) . . . . ? 
O1 Hf1 O2 C4 27.1(3) . . . . ? 
O3 Hf1 O2 C4 -179.8(3) . . . . ? 
O4 Hf1 O2 C4 109.0(3) . . . . ? 
O6 Hf1 O2 C5 54.4(4) . . . . ? 
O5 Hf1 O2 C5 -179.2(6) . . . . ? 
O1 Hf1 O2 C5 161.4(4) . . . . ? 
O3 Hf1 O2 C5 -45.5(3) . . . . ? 
O4 Hf1 O2 C5 -116.8(3) . . . . ? 
C7 C6 O3 Hf1 -141.7(3) . . . . ? 
C9 C6 O3 Hf1 -23.3(4) . . . . ? 
C8 C6 O3 Hf1 96.7(4) . . . . ? 
O6 Hf1 O3 C6 -178.2(3) . . . . ? 
O5 Hf1 O3 C6 77.9(3) . . . . ? 
O1 Hf1 O3 C6 -49.4(4) . . . . ? 
O4 Hf1 O3 C6 -1.1(3) . . . . ? 
O2 Hf1 O3 C6 -93.8(3) . . . . ? 
C6 C9 O4 C10 178.7(4) . . . . ? 
C6 C9 O4 Hf1 -45.3(3) . . . . ? 
O6 Hf1 O4 C10 174.6(8) . . . . ? 
O5 Hf1 O4 C10 49.6(3) . . . . ? 
O1 Hf1 O4 C10 -49.9(3) . . . . ? 
O3 Hf1 O4 C10 157.5(4) . . . . ? 
O2 Hf1 O4 C10 -120.6(3) . . . . ? 
O6 Hf1 O4 C9 43.7(9) . . . . ? 
O5 Hf1 O4 C9 -81.3(2) . . . . ? 
O1 Hf1 O4 C9 179.2(2) . . . . ? 
O3 Hf1 O4 C9 26.7(2) . . . . ? 
O2 Hf1 O4 C9 108.6(2) . . . . ? 
C13' C11 O5 Hf1 -137.3(15) . . . . ? 
C14 C11 O5 Hf1 64.9(11) . . . . ? 
C12' C11 O5 Hf1 -18.9(12) . . . . ? 
C12 C11 O5 Hf1 -58.4(12) . . . . ? 
C13 C11 O5 Hf1 -174.2(9) . . . . ? 
C14' C11 O5 Hf1 89.2(12) . . . . ? 
O6 Hf1 O5 C11 -53.4(10) . . . . ? 
O1 Hf1 O5 C11 -160.2(9) . . . . ? 
O3 Hf1 O5 C11 49.3(10) . . . . ? 
O4 Hf1 O5 C11 118.4(9) . . . . ? 
O2 Hf1 O5 C11 -178.7(8) . . . . ? 
C18 C15 O6 Hf1 -132.3(12) . . . . ? 
C16 C15 O6 Hf1 -10.2(15) . . . . ? 
C17 C15 O6 Hf1 108.7(12) . . . . ? 
O5 Hf1 O6 C15 -56.4(13) . . . . ? 
O1 Hf1 O6 C15 45.6(13) . . . . ? 
O3 Hf1 O6 C15 -164.0(12) . . . . ? 
O4 Hf1 O6 C15 179.7(10) . . . . ? 
O2 Hf1 O6 C15 114.5(13) . . . . ? 

_diffrn_measured_fraction_theta_max    0.949 
_diffrn_reflns_theta_full              28.27 
_diffrn_measured_fraction_theta_full   0.949 
_refine_diff_density_max    1.463 
_refine_diff_density_min   -0.623 
_refine_diff_density_rms    0.109