Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2001


data_v2 

_database_code_CSD           152545

_journal_coden_Cambridge      186

_publ_contact_author
; Dr Alexander Z. Voskoboynikov
Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

_publ_contact_author_email        voskoboy@org.chem.msu.su

_publ_contact_letter
; reference number B009280K
;

_publ_section_title
;
ansa-Metallocenes with Ph2Si Bridge. Molecular structures of
Ph2Si(h5-fluorenyl)(h5-C5H4)HfCl2 and
[(9-fluorenyl)Ph2SiC5H4-h5]2HfCl2.
;

_publ_requested_journal           'J.Chem.Com., Dalton Trans.'

loop_
_publ_author_name
_publ_author_address

'Izmer, Vyacheslav V.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

'Agarkov, Anton Y.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

'Nosova, Valentina M.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

"Kuz'mina, Lyudmila G."
; N.S.Kurnakov Institute of General and Inorganic Chemistry
of Russian Academy of Science, 31 Leninskii prospect,
Moscow, 117907, Russia
;

'Howard, Judith A. K.'
; Department of Chemistry, University of Durham,
South Road, Durham, DH1 3LE, United Kingdom
;

'Beletskaya, Irina P.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

'Voskoboynikov, Alexander Z.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
Bis[(diphenyl-(fluoren-9-yl)-silyl)cyclopentadienyl]
dichloro-hafnium(IV)
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C61.50 H49 Cl5 Hf Si2' 
_chemical_formula_weight          1199.93 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

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' 
'Si'  'Si'   0.0817   0.0704 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Cl'  'Cl'   0.1484   0.1585 
'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            triclinic
_symmetry_space_group_name_H-M    'P -1'

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x, -y, -z' 

_cell_length_a                    13.5860(9) 
_cell_length_b                    14.0886(6) 
_cell_length_c                    15.9919(6) 
_cell_angle_alpha                 69.997(1) 
_cell_angle_beta                  71.314(2) 
_cell_angle_gamma                 89.535(1) 
_cell_volume                      2706.9(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        colorless
_exptl_crystal_colour             block
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.472 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1206 
_exptl_absorpt_coefficient_mu     2.257 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.5678
_exptl_absorpt_correction_T_max   0.8216

_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        'Siemens SMART CCD'
_diffrn_measurement_method        \w
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             19863 
_diffrn_reflns_av_R_equivalents   0.0639 
_diffrn_reflns_av_sigmaI/netI     0.0568 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.44 
_diffrn_reflns_theta_max          27.49 
_reflns_number_total              12276 
_reflns_number_observed           10576 
_reflns_observed_criterion        I>2\s(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 933 with very negative F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses 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 observed criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating R(obs) 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 w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+17.9727P] 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     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          11343 
_refine_ls_number_parameters      614 
_refine_ls_number_restraints      13 
_refine_ls_R_factor_all           0.0762 
_refine_ls_R_factor_obs           0.0589 
_refine_ls_wR_factor_all          0.2142 
_refine_ls_wR_factor_obs          0.1489 
_refine_ls_goodness_of_fit_all    1.072 
_refine_ls_goodness_of_fit_obs    1.059 
_refine_ls_restrained_S_all       1.418 
_refine_ls_restrained_S_obs       1.059 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
Hf1 Hf 0.72517(2) 0.55941(2) 0.56105(2) 0.02416(9) Uani 1 d . . 
Cl1 Cl 0.87900(12) 0.52161(12) 0.45445(11) 0.0320(3) Uani 1 d . . 
Cl2 Cl 0.61106(13) 0.42416(13) 0.56849(11) 0.0351(3) Uani 1 d . . 
Si1 Si 0.51375(13) 0.42542(13) 0.81138(12) 0.0248(3) Uani 1 d . . 
Si2 Si 0.91262(12) 0.80245(12) 0.36750(11) 0.0230(3) Uani 1 d . . 
C1 C 0.6531(5) 0.4768(5) 0.7363(4) 0.0261(12) Uani 1 d . . 
C2 C 0.7414(5) 0.4261(5) 0.7053(4) 0.0293(12) Uani 1 d . . 
H2A H 0.7396(5) 0.3516(5) 0.7170(4) 0.035 Uiso 1 calc R . 
C3 C 0.8331(5) 0.4952(5) 0.6664(5) 0.0332(14) Uani 1 d . . 
H3A H 0.9064(5) 0.4777(5) 0.6460(5) 0.040 Uiso 1 calc R . 
C4 C 0.8043(5) 0.5899(5) 0.6718(4) 0.0320(13) Uani 1 d . . 
H4A H 0.8534(5) 0.6504(5) 0.6574(4) 0.038 Uiso 1 calc R . 
C5 C 0.6938(5) 0.5776(5) 0.7172(4) 0.0269(12) Uani 1 d . . 
H5A H 0.6526(5) 0.6291(5) 0.7388(4) 0.032 Uiso 1 calc R . 
C6 C 0.5085(5) 0.4226(5) 0.9339(4) 0.0291(12) Uani 1 d . . 
H6A H 0.5204(5) 0.4933(5) 0.9321(4) 0.035 Uiso 1 calc R . 
C7 C 0.4065(6) 0.3691(5) 1.0107(5) 0.0355(15) Uani 1 d . . 
C8 C 0.3048(6) 0.3951(6) 1.0244(5) 0.043(2) Uani 1 d . . 
H8A H 0.2906(6) 0.4551(6) 0.9818(5) 0.051 Uiso 1 calc R . 
C9 C 0.2238(8) 0.3300(8) 1.1031(7) 0.064(3) Uani 1 d . . 
H9A H 0.1539(8) 0.3460(8) 1.1126(7) 0.077 Uiso 1 calc R . 
C10 C 0.2425(8) 0.2439(8) 1.1668(7) 0.066(3) Uani 1 d . . 
H10A H 0.1864(8) 0.2032(8) 1.2208(7) 0.080 Uiso 1 calc R . 
C11 C 0.3432(9) 0.2163(7) 1.1525(6) 0.060(3) Uani 1 d . . 
H11A H 0.3560(9) 0.1554(7) 1.1950(6) 0.072 Uiso 1 calc R . 
C12 C 0.4257(6) 0.2794(5) 1.0747(5) 0.039(2) Uani 1 d . . 
C13 C 0.5388(6) 0.2715(5) 1.0452(5) 0.039(2) Uani 1 d . . 
C14 C 0.5966(9) 0.1963(6) 1.0828(6) 0.053(2) Uani 1 d . . 
H14A H 0.5624(9) 0.1370(6) 1.1358(6) 0.064 Uiso 1 calc R . 
C15 C 0.7035(8) 0.2094(7) 1.0422(6) 0.053(2) Uani 1 d . . 
H15A H 0.7433(8) 0.1575(7) 1.0655(6) 0.064 Uiso 1 calc R . 
C16 C 0.7548(7) 0.3000(6) 0.9657(6) 0.047(2) Uani 1 d . . 
H16A H 0.8290(7) 0.3094(6) 0.9396(6) 0.056 Uiso 1 calc R . 
C17 C 0.6977(6) 0.3750(6) 0.9284(5) 0.0360(14) Uani 1 d . . 
H17A H 0.7322(6) 0.4361(6) 0.8779(5) 0.043 Uiso 1 calc R . 
C18 C 0.5883(6) 0.3591(5) 0.9665(4) 0.0324(13) Uani 1 d . . 
C19 C 0.4270(5) 0.5211(5) 0.7678(5) 0.0309(13) Uani 1 d . . 
C20 C 0.4057(6) 0.6014(6) 0.8011(5) 0.040(2) Uani 1 d . . 
H20A H 0.4297(6) 0.6033(6) 0.8502(5) 0.048 Uiso 1 calc R . 
C21 C 0.3507(7) 0.6779(7) 0.7643(6) 0.046(2) Uani 1 d . . 
H21A H 0.3400(7) 0.7332(7) 0.7862(6) 0.055 Uiso 1 calc R . 
C22 C 0.3106(6) 0.6747(7) 0.6949(6) 0.047(2) Uani 1 d . . 
H22A H 0.2715(6) 0.7267(7) 0.6706(6) 0.057 Uiso 1 calc R . 
C23 C 0.3284(5) 0.5953(6) 0.6621(5) 0.040(2) Uani 1 d . . 
H23A H 0.3007(5) 0.5922(6) 0.6154(5) 0.048 Uiso 1 calc R . 
C24 C 0.3866(5) 0.5197(6) 0.6970(5) 0.0338(14) Uani 1 d . . 
H24A H 0.3994(5) 0.4662(6) 0.6728(5) 0.041 Uiso 1 calc R . 
C25 C 0.4753(5) 0.2926(5) 0.8234(4) 0.0295(13) Uani 1 d . . 
C26 C 0.5346(6) 0.2133(5) 0.8499(5) 0.039(2) Uani 1 d . . 
H26A H 0.6003(6) 0.2278(5) 0.8548(5) 0.047 Uiso 1 calc R . 
C27 C 0.4983(7) 0.1131(6) 0.8691(7) 0.054(2) Uani 1 d . . 
H27A H 0.5384(7) 0.0598(6) 0.8889(7) 0.064 Uiso 1 calc R . 
C28 C 0.4050(7) 0.0909(6) 0.8598(7) 0.054(2) Uani 1 d . . 
H28A H 0.3814(7) 0.0226(6) 0.8719(7) 0.065 Uiso 1 calc R . 
C29 C 0.3449(6) 0.1688(6) 0.8323(6) 0.045(2) Uani 1 d . . 
H29A H 0.2806(6) 0.1539(6) 0.8252(6) 0.054 Uiso 1 calc R . 
C30 C 0.3796(5) 0.2680(6) 0.8155(5) 0.038(2) Uani 1 d . . 
H30A H 0.3376(5) 0.3205(6) 0.7982(5) 0.046 Uiso 1 calc R . 
C1' C 0.7766(5) 0.7330(5) 0.4354(4) 0.0263(12) Uani 1 d . . 
C2' C 0.7163(5) 0.7442(5) 0.5212(4) 0.0273(12) Uani 1 d . . 
H2'A H 0.7405(5) 0.7861(5) 0.5518(4) 0.033 Uiso 1 calc R . 
C3' C 0.6115(5) 0.6997(5) 0.5495(4) 0.0301(13) Uani 1 d . . 
H3'A H 0.5505(5) 0.7055(5) 0.6020(4) 0.036 Uiso 1 calc R . 
C4' C 0.6070(5) 0.6615(5) 0.4788(5) 0.0323(13) Uani 1 d . . 
H4'A H 0.5421(5) 0.6334(5) 0.4745(5) 0.039 Uiso 1 calc R . 
C5' C 0.7079(5) 0.6815(5) 0.4099(5) 0.0294(13) Uani 1 d . . 
H5'A H 0.7259(5) 0.6691(5) 0.3491(5) 0.035 Uiso 1 calc R . 
C6' C 1.0093(5) 0.7527(5) 0.2785(4) 0.0269(12) Uani 1 d . . 
H6'A H 1.0321(5) 0.6865(5) 0.3106(4) 0.032 Uiso 1 calc R . 
C7' C 1.1007(5) 0.8369(5) 0.2233(5) 0.0317(13) Uani 1 d . . 
C8' C 1.1745(5) 0.8692(6) 0.2540(5) 0.0379(15) Uani 1 d . . 
H8'A H 1.1779(5) 0.8339(6) 0.3152(5) 0.045 Uiso 1 calc R . 
C9' C 1.2439(5) 0.9560(6) 0.1911(6) 0.046(2) Uani 1 d . . 
H9'A H 1.2941(5) 0.9808(6) 0.2107(6) 0.055 Uiso 1 calc R . 
C10' C 1.2410(6) 1.0066(6) 0.1011(6) 0.047(2) Uani 1 d . . 
H10B H 1.2891(6) 1.0652(6) 0.0601(6) 0.057 Uiso 1 calc R . 
C11' C 1.1686(6) 0.9725(6) 0.0699(6) 0.043(2) Uani 1 d . . 
H11B H 1.1673(6) 1.0070(6) 0.0078(6) 0.052 Uiso 1 calc R . 
C12' C 1.0978(5) 0.8866(5) 0.1315(5) 0.0327(13) Uani 1 d . . 
C13' C 1.0186(5) 0.8312(5) 0.1177(5) 0.0312(13) Uani 1 d . . 
C14' C 0.9933(6) 0.8439(6) 0.0359(5) 0.044(2) Uani 1 d . . 
H14B H 1.0242(6) 0.9008(6) -0.0206(5) 0.052 Uiso 1 calc R . 
C15' C 0.9228(7) 0.7717(7) 0.0400(5) 0.048(2) Uani 1 d . . 
H15B H 0.9040(7) 0.7802(7) -0.0142(5) 0.057 Uiso 1 calc R . 
C16' C 0.8778(7) 0.6860(6) 0.1218(6) 0.046(2) Uani 1 d . . 
H16B H 0.8314(7) 0.6360(6) 0.1218(6) 0.055 Uiso 1 calc R . 
C17' C 0.9014(6) 0.6741(6) 0.2039(5) 0.0362(14) Uani 1 d . . 
H17B H 0.8712(6) 0.6164(6) 0.2598(5) 0.043 Uiso 1 calc R . 
C18' C 0.9698(5) 0.7483(5) 0.2018(4) 0.0290(12) Uani 1 d . . 
C19' C 0.9712(5) 0.8000(4) 0.4600(4) 0.0253(11) Uani 1 d . . 
C20' C 1.0348(5) 0.7253(5) 0.4888(5) 0.0322(13) Uani 1 d . . 
H20B H 1.0516(5) 0.6771(5) 0.4583(5) 0.039 Uiso 1 calc R . 
C21' C 1.0739(6) 0.7196(6) 0.5606(5) 0.039(2) Uani 1 d . . 
H21B H 1.1178(6) 0.6693(6) 0.5784(5) 0.047 Uiso 1 calc R . 
C22' C 1.0469(6) 0.7902(6) 0.6060(5) 0.039(2) Uani 1 d . . 
H22B H 1.0720(6) 0.7871(6) 0.6558(5) 0.047 Uiso 1 calc R . 
C23' C 0.9847(6) 0.8636(5) 0.5793(5) 0.0351(14) Uani 1 d . . 
H23B H 0.9673(6) 0.9112(5) 0.6103(5) 0.042 Uiso 1 calc R . 
C24' C 0.9472(5) 0.8685(5) 0.5066(5) 0.0315(13) Uani 1 d . . 
H24B H 0.9043(5) 0.9197(5) 0.4887(5) 0.038 Uiso 1 calc R . 
C25' C 0.8881(5) 0.9362(5) 0.3039(4) 0.0281(12) Uani 1 d . . 
C26' C 0.9663(5) 1.0176(5) 0.2631(4) 0.0286(12) Uani 1 d . . 
H26B H 1.0337(5) 1.0062(5) 0.2678(4) 0.034 Uiso 1 calc R . 
C27' C 0.9479(6) 1.1154(5) 0.2154(5) 0.0333(13) Uani 1 d . . 
H27B H 1.0030(6) 1.1695(5) 0.1864(5) 0.040 Uiso 1 calc R . 
C28' C 0.8500(6) 1.1338(5) 0.2103(5) 0.039(2) Uani 1 d . . 
H28B H 0.8370(6) 1.2007(5) 0.1790(5) 0.047 Uiso 1 calc R . 
C29' C 0.7710(6) 1.0544(6) 0.2511(6) 0.047(2) Uani 1 d . . 
H29B H 0.7035(6) 1.0669(6) 0.2473(6) 0.056 Uiso 1 calc R . 
C30' C 0.7890(6) 0.9562(5) 0.2976(5) 0.0368(15) Uani 1 d . . 
H30B H 0.7338(6) 0.9023(5) 0.3253(5) 0.044 Uiso 1 calc R . 
C31 C 1.4525(24) 0.8734(25) 0.4000(27) 0.284(20) Uiso 1 d D . 
H31C H 1.4762(24) 0.8437(25) 0.4550(27) 0.341 Uiso 0.50 calc PR 2 
H31D H 1.4848(24) 0.8421(25) 0.3523(27) 0.341 Uiso 0.50 calc PR 2 
H31A H 1.4841(24) 0.9013(25) 0.3325(27) 0.341 Uiso 0.50 d PR 1 
H31B H 1.4794(24) 0.8106(25) 0.4249(27) 0.341 Uiso 0.50 d PR 1 
Cl3 Cl 1.3139(16) 0.8600(14) 0.4342(13) 0.418(10) Uiso 1 d D . 
Cl4 Cl 1.4678(30) 0.9638(41) 0.4517(40) 0.554(34) Uiso 0.50 d PD 1 
Cl4A Cl 1.4789(16) 1.0053(16) 0.3523(18) 0.256(9) Uiso 0.50 d PD 2 
C32 C 1.0552(54) 1.5268(52) 0.0696(18) 0.339(51) Uiso 0.50 d PD -3 
H32A H 1.0359(54) 1.5865(52) 0.0882(18) 0.406 Uiso 0.50 calc PR -3 
H32B H 1.1197(54) 1.5049(52) 0.0830(18) 0.406 Uiso 0.50 calc PR -3 
Cl6 Cl 0.9527(13) 1.4273(11) 0.1275(10) 0.178(5) Uiso 0.50 d PD -3 
Cl5 Cl 1.0706(10) 1.5538(10) -0.0496(9) 0.152(4) Uiso 0.50 d PD -3 

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 
Hf1 0.01976(13) 0.02758(14) 0.02382(13) -0.00770(9) -0.00715(9) -0.00305(8) 
Cl1 0.0266(7) 0.0324(7) 0.0304(7) -0.0088(6) -0.0038(6) 0.0024(6) 
Cl2 0.0329(8) 0.0398(8) 0.0324(7) -0.0134(6) -0.0102(6) -0.0106(6) 
Si1 0.0217(7) 0.0272(8) 0.0261(8) -0.0122(6) -0.0059(6) -0.0023(6) 
Si2 0.0207(7) 0.0257(7) 0.0217(7) -0.0059(6) -0.0086(6) -0.0003(6) 
C1 0.024(3) 0.033(3) 0.020(3) -0.009(2) -0.006(2) -0.006(2) 
C2 0.028(3) 0.031(3) 0.025(3) -0.004(2) -0.011(2) 0.001(2) 
C3 0.024(3) 0.045(4) 0.029(3) -0.010(3) -0.012(2) 0.003(3) 
C4 0.034(3) 0.037(3) 0.024(3) -0.005(3) -0.013(3) -0.009(3) 
C5 0.023(3) 0.031(3) 0.026(3) -0.009(2) -0.010(2) -0.001(2) 
C6 0.029(3) 0.032(3) 0.026(3) -0.013(2) -0.006(2) -0.006(2) 
C7 0.039(4) 0.037(3) 0.028(3) -0.019(3) 0.000(3) -0.014(3) 
C8 0.036(4) 0.048(4) 0.039(4) -0.024(3) 0.003(3) -0.010(3) 
C9 0.048(5) 0.074(6) 0.054(5) -0.029(5) 0.012(4) -0.027(5) 
C10 0.063(6) 0.071(6) 0.048(5) -0.028(5) 0.012(4) -0.039(5) 
C11 0.080(7) 0.045(4) 0.038(4) -0.011(4) -0.002(4) -0.030(4) 
C12 0.053(4) 0.034(3) 0.024(3) -0.012(3) -0.003(3) -0.013(3) 
C13 0.056(4) 0.034(3) 0.027(3) -0.012(3) -0.013(3) -0.009(3) 
C14 0.090(7) 0.036(4) 0.037(4) -0.010(3) -0.030(4) 0.006(4) 
C15 0.081(6) 0.048(5) 0.048(5) -0.022(4) -0.040(5) 0.022(4) 
C16 0.054(5) 0.053(5) 0.044(4) -0.020(4) -0.028(4) 0.011(4) 
C17 0.040(4) 0.042(4) 0.034(3) -0.018(3) -0.019(3) 0.005(3) 
C18 0.044(4) 0.033(3) 0.023(3) -0.011(3) -0.014(3) -0.002(3) 
C19 0.023(3) 0.040(3) 0.029(3) -0.014(3) -0.007(2) 0.002(2) 
C20 0.038(4) 0.052(4) 0.039(4) -0.026(3) -0.016(3) 0.008(3) 
C21 0.048(4) 0.054(5) 0.051(4) -0.035(4) -0.021(4) 0.021(4) 
C22 0.038(4) 0.068(5) 0.052(5) -0.032(4) -0.025(4) 0.029(4) 
C23 0.030(3) 0.062(5) 0.036(4) -0.022(3) -0.015(3) 0.009(3) 
C24 0.021(3) 0.048(4) 0.034(3) -0.020(3) -0.005(2) -0.001(3) 
C25 0.027(3) 0.032(3) 0.027(3) -0.013(2) -0.003(2) -0.006(2) 
C26 0.033(3) 0.033(3) 0.042(4) -0.011(3) -0.003(3) -0.004(3) 
C27 0.048(5) 0.032(4) 0.064(5) -0.012(4) -0.003(4) 0.005(3) 
C28 0.045(4) 0.038(4) 0.068(6) -0.025(4) 0.004(4) -0.012(3) 
C29 0.041(4) 0.045(4) 0.049(4) -0.019(3) -0.011(3) -0.017(3) 
C30 0.028(3) 0.041(4) 0.043(4) -0.010(3) -0.011(3) -0.005(3) 
C1' 0.023(3) 0.030(3) 0.026(3) -0.007(2) -0.011(2) 0.002(2) 
C2' 0.024(3) 0.025(3) 0.029(3) -0.005(2) -0.009(2) -0.002(2) 
C3' 0.019(3) 0.037(3) 0.028(3) -0.006(3) -0.006(2) -0.003(2) 
C4' 0.019(3) 0.041(3) 0.035(3) -0.007(3) -0.014(3) 0.003(2) 
C5' 0.020(3) 0.038(3) 0.029(3) -0.007(3) -0.011(2) -0.001(2) 
C6' 0.021(3) 0.026(3) 0.032(3) -0.010(2) -0.008(2) 0.001(2) 
C7' 0.024(3) 0.035(3) 0.030(3) -0.010(3) -0.003(2) 0.002(2) 
C8' 0.025(3) 0.045(4) 0.044(4) -0.016(3) -0.010(3) 0.002(3) 
C9' 0.020(3) 0.056(5) 0.055(5) -0.024(4) 0.000(3) -0.013(3) 
C10' 0.036(4) 0.047(4) 0.040(4) -0.009(3) 0.005(3) -0.016(3) 
C11' 0.037(4) 0.037(4) 0.042(4) -0.010(3) -0.001(3) -0.001(3) 
C12' 0.028(3) 0.031(3) 0.036(3) -0.014(3) -0.005(3) 0.004(3) 
C13' 0.032(3) 0.032(3) 0.032(3) -0.017(3) -0.008(3) 0.005(3) 
C14' 0.045(4) 0.052(4) 0.028(3) -0.011(3) -0.008(3) -0.001(3) 
C15' 0.051(5) 0.067(5) 0.033(4) -0.026(4) -0.016(3) 0.005(4) 
C16' 0.047(4) 0.053(4) 0.043(4) -0.024(4) -0.015(3) -0.004(3) 
C17' 0.034(3) 0.040(4) 0.034(3) -0.018(3) -0.006(3) -0.002(3) 
C18' 0.027(3) 0.031(3) 0.027(3) -0.011(2) -0.007(2) 0.005(2) 
C19' 0.024(3) 0.025(3) 0.025(3) -0.005(2) -0.010(2) -0.004(2) 
C20' 0.035(3) 0.029(3) 0.039(3) -0.013(3) -0.020(3) 0.002(3) 
C21' 0.043(4) 0.040(4) 0.045(4) -0.013(3) -0.030(3) 0.005(3) 
C22' 0.043(4) 0.042(4) 0.040(4) -0.016(3) -0.023(3) -0.001(3) 
C23' 0.040(4) 0.038(3) 0.031(3) -0.016(3) -0.012(3) -0.004(3) 
C24' 0.029(3) 0.029(3) 0.031(3) -0.003(2) -0.010(3) -0.004(2) 
C25' 0.031(3) 0.031(3) 0.022(3) -0.008(2) -0.009(2) 0.005(2) 
C26' 0.032(3) 0.028(3) 0.026(3) -0.009(2) -0.010(2) 0.004(2) 
C27' 0.040(4) 0.030(3) 0.028(3) -0.010(3) -0.008(3) 0.001(3) 
C28' 0.054(4) 0.031(3) 0.032(3) -0.006(3) -0.019(3) 0.008(3) 
C29' 0.038(4) 0.048(4) 0.055(5) -0.010(4) -0.025(4) 0.013(3) 
C30' 0.033(3) 0.033(3) 0.041(4) -0.005(3) -0.017(3) 0.006(3) 

_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 
Hf1 Cl2 2.4132(15) . ? 
Hf1 Cl1 2.424(2) . ? 
Hf1 C2' 2.471(6) . ? 
Hf1 C1 2.489(6) . ? 
Hf1 C5 2.497(6) . ? 
Hf1 C3' 2.491(7) . ? 
Hf1 C4 2.496(6) . ? 
Hf1 C1' 2.504(6) . ? 
Hf1 C2 2.500(6) . ? 
Hf1 C3 2.515(6) . ? 
Hf1 C5' 2.523(6) . ? 
Hf1 C4' 2.530(6) . ? 
Si1 C25 1.875(6) . ? 
Si1 C19 1.884(7) . ? 
Si1 C1 1.877(6) . ? 
Si1 C6 1.924(6) . ? 
Si2 C19' 1.882(6) . ? 
Si2 C1' 1.889(6) . ? 
Si2 C25' 1.896(6) . ? 
Si2 C6' 1.927(6) . ? 
C1 C5 1.422(8) . ? 
C1 C2 1.429(9) . ? 
C2 C3 1.412(9) . ? 
C3 C4 1.411(10) . ? 
C4 C5 1.425(9) . ? 
C6 C18 1.508(10) . ? 
C6 C7 1.513(9) . ? 
C7 C12 1.413(11) . ? 
C7 C8 1.394(11) . ? 
C8 C9 1.405(11) . ? 
C9 C10 1.37(2) . ? 
C10 C11 1.39(2) . ? 
C11 C12 1.400(10) . ? 
C12 C13 1.470(12) . ? 
C13 C18 1.403(9) . ? 
C13 C14 1.398(12) . ? 
C14 C15 1.372(14) . ? 
C15 C16 1.418(13) . ? 
C16 C17 1.387(11) . ? 
C17 C18 1.401(10) . ? 
C19 C24 1.414(9) . ? 
C19 C20 1.399(10) . ? 
C20 C21 1.379(11) . ? 
C21 C22 1.396(11) . ? 
C22 C23 1.378(11) . ? 
C23 C24 1.390(10) . ? 
C25 C26 1.400(10) . ? 
C25 C30 1.404(9) . ? 
C26 C27 1.397(11) . ? 
C27 C28 1.374(13) . ? 
C28 C29 1.396(13) . ? 
C29 C30 1.385(10) . ? 
C1' C2' 1.416(9) . ? 
C1' C5' 1.422(8) . ? 
C2' C3' 1.425(8) . ? 
C3' C4' 1.426(10) . ? 
C4' C5' 1.413(9) . ? 
C6' C18' 1.505(9) . ? 
C6' C7' 1.528(8) . ? 
C7' C8' 1.390(10) . ? 
C7' C12' 1.407(10) . ? 
C8' C9' 1.402(10) . ? 
C9' C10' 1.383(12) . ? 
C10' C11' 1.390(12) . ? 
C11' C12' 1.400(10) . ? 
C12' C13' 1.449(9) . ? 
C13' C18' 1.407(9) . ? 
C13' C14' 1.409(10) . ? 
C14' C15' 1.372(12) . ? 
C15' C16' 1.401(12) . ? 
C16' C17' 1.405(10) . ? 
C17' C18' 1.389(9) . ? 
C19' C24' 1.387(9) . ? 
C19' C20' 1.406(9) . ? 
C20' C21' 1.391(9) . ? 
C21' C22' 1.402(11) . ? 
C22' C23' 1.371(11) . ? 
C23' C24' 1.392(9) . ? 
C25' C26' 1.390(9) . ? 
C25' C30' 1.400(9) . ? 
C26' C27' 1.394(9) . ? 
C27' C28' 1.375(10) . ? 
C28' C29' 1.379(11) . ? 
C29' C30' 1.391(10) . ? 
C31 Cl4A 1.74(3) . ? 
C31 Cl3 1.78(3) . ? 
C31 Cl4 1.79(3) . ? 
C32 Cl5 1.75(3) . ? 
C32 Cl6 1.75(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 
Cl2 Hf1 Cl1 94.29(6) . . ? 
Cl2 Hf1 C2' 132.73(15) . . ? 
Cl1 Hf1 C2' 112.27(15) . . ? 
Cl2 Hf1 C1 82.40(14) . . ? 
Cl1 Hf1 C1 127.1(2) . . ? 
C2' Hf1 C1 107.7(2) . . ? 
Cl2 Hf1 C5 113.48(14) . . ? 
Cl1 Hf1 C5 131.07(14) . . ? 
C2' Hf1 C5 78.1(2) . . ? 
C1 Hf1 C5 33.1(2) . . ? 
Cl2 Hf1 C3' 101.13(15) . . ? 
Cl1 Hf1 C3' 135.70(15) . . ? 
C2' Hf1 C3' 33.4(2) . . ? 
C1 Hf1 C3' 96.2(2) . . ? 
C5 Hf1 C3' 79.3(2) . . ? 
Cl2 Hf1 C4 135.2(2) . . ? 
Cl1 Hf1 C4 99.3(2) . . ? 
C2' Hf1 C4 79.9(2) . . ? 
C1 Hf1 C4 55.5(2) . . ? 
C5 Hf1 C4 33.2(2) . . ? 
C3' Hf1 C4 98.3(2) . . ? 
Cl2 Hf1 C1' 126.45(14) . . ? 
Cl1 Hf1 C1' 82.10(15) . . ? 
C2' Hf1 C1' 33.1(2) . . ? 
C1 Hf1 C1' 140.1(2) . . ? 
C5 Hf1 C1' 108.1(2) . . ? 
C3' Hf1 C1' 55.4(2) . . ? 
C4 Hf1 C1' 97.7(2) . . ? 
Cl2 Hf1 C2 82.3(2) . . ? 
Cl1 Hf1 C2 93.8(2) . . ? 
C2' Hf1 C2 130.9(2) . . ? 
C1 Hf1 C2 33.3(2) . . ? 
C5 Hf1 C2 54.2(2) . . ? 
C3' Hf1 C2 129.1(2) . . ? 
C4 Hf1 C2 54.5(2) . . ? 
C1' Hf1 C2 151.1(2) . . ? 
Cl2 Hf1 C3 112.0(2) . . ? 
Cl1 Hf1 C3 78.6(2) . . ? 
C2' Hf1 C3 111.1(2) . . ? 
C1 Hf1 C3 55.1(2) . . ? 
C5 Hf1 C3 54.2(2) . . ? 
C3' Hf1 C3 130.3(2) . . ? 
C4 Hf1 C3 32.7(2) . . ? 
C1' Hf1 C3 119.3(2) . . ? 
C2 Hf1 C3 32.7(2) . . ? 
Cl2 Hf1 C5' 93.59(15) . . ? 
Cl1 Hf1 C5' 83.5(2) . . ? 
C2' Hf1 C5' 54.1(2) . . ? 
C1 Hf1 C5' 149.2(2) . . ? 
C5 Hf1 C5' 130.6(2) . . ? 
C3' Hf1 C5' 54.5(2) . . ? 
C4 Hf1 C5' 130.1(2) . . ? 
C1' Hf1 C5' 32.9(2) . . ? 
C2 Hf1 C5' 174.9(2) . . ? 
C3 Hf1 C5' 149.6(2) . . ? 
Cl2 Hf1 C4' 79.5(2) . . ? 
Cl1 Hf1 C4' 113.5(2) . . ? 
C2' Hf1 C4' 54.5(2) . . ? 
C1 Hf1 C4' 117.5(2) . . ? 
C5 Hf1 C4' 110.7(2) . . ? 
C3' Hf1 C4' 33.0(2) . . ? 
C4 Hf1 C4' 130.7(2) . . ? 
C1' Hf1 C4' 54.7(2) . . ? 
C2 Hf1 C4' 148.0(2) . . ? 
C3 Hf1 C4' 163.3(2) . . ? 
C5' Hf1 C4' 32.5(2) . . ? 
C25 Si1 C19 114.2(3) . . ? 
C25 Si1 C1 114.8(3) . . ? 
C19 Si1 C1 108.1(3) . . ? 
C25 Si1 C6 107.8(3) . . ? 
C19 Si1 C6 108.4(3) . . ? 
C1 Si1 C6 102.8(3) . . ? 
C19' Si2 C1' 105.4(3) . . ? 
C19' Si2 C25' 110.9(3) . . ? 
C1' Si2 C25' 103.4(3) . . ? 
C19' Si2 C6' 108.0(3) . . ? 
C1' Si2 C6' 119.1(3) . . ? 
C25' Si2 C6' 109.8(3) . . ? 
C5 C1 C2 106.0(5) . . ? 
C5 C1 Si1 121.9(5) . . ? 
C2 C1 Si1 130.9(5) . . ? 
C5 C1 Hf1 73.7(3) . . ? 
C2 C1 Hf1 73.8(3) . . ? 
Si1 C1 Hf1 127.4(3) . . ? 
C3 C2 C1 109.1(6) . . ? 
C3 C2 Hf1 74.2(4) . . ? 
C1 C2 Hf1 72.9(3) . . ? 
C4 C3 C2 108.3(6) . . ? 
C4 C3 Hf1 72.9(4) . . ? 
C2 C3 Hf1 73.1(3) . . ? 
C3 C4 C5 107.3(6) . . ? 
C3 C4 Hf1 74.4(4) . . ? 
C5 C4 Hf1 73.5(3) . . ? 
C1 C5 C4 109.3(6) . . ? 
C1 C5 Hf1 73.1(3) . . ? 
C4 C5 Hf1 73.4(3) . . ? 
C18 C6 C7 102.6(6) . . ? 
C18 C6 Si1 111.0(4) . . ? 
C7 C6 Si1 112.5(4) . . ? 
C12 C7 C8 120.1(7) . . ? 
C12 C7 C6 109.5(6) . . ? 
C8 C7 C6 130.4(7) . . ? 
C7 C8 C9 118.0(9) . . ? 
C10 C9 C8 122.1(10) . . ? 
C9 C10 C11 120.2(8) . . ? 
C10 C11 C12 119.2(9) . . ? 
C7 C12 C11 120.4(8) . . ? 
C7 C12 C13 108.9(6) . . ? 
C11 C12 C13 130.7(8) . . ? 
C18 C13 C14 121.0(8) . . ? 
C18 C13 C12 107.9(7) . . ? 
C14 C13 C12 131.1(7) . . ? 
C15 C14 C13 119.1(8) . . ? 
C14 C15 C16 120.4(8) . . ? 
C17 C16 C15 120.6(8) . . ? 
C16 C17 C18 119.0(7) . . ? 
C13 C18 C17 119.7(7) . . ? 
C13 C18 C6 110.6(6) . . ? 
C17 C18 C6 129.7(6) . . ? 
C24 C19 C20 117.1(6) . . ? 
C24 C19 Si1 122.7(5) . . ? 
C20 C19 Si1 120.1(5) . . ? 
C21 C20 C19 121.5(7) . . ? 
C20 C21 C22 120.4(7) . . ? 
C23 C22 C21 119.4(7) . . ? 
C22 C23 C24 120.3(7) . . ? 
C23 C24 C19 121.2(7) . . ? 
C26 C25 C30 117.8(6) . . ? 
C26 C25 Si1 121.6(5) . . ? 
C30 C25 Si1 120.3(5) . . ? 
C25 C26 C27 120.6(7) . . ? 
C28 C27 C26 120.6(8) . . ? 
C27 C28 C29 119.9(7) . . ? 
C30 C29 C28 119.7(7) . . ? 
C29 C30 C25 121.5(7) . . ? 
C2' C1' C5' 106.5(5) . . ? 
C2' C1' Si2 120.5(4) . . ? 
C5' C1' Si2 131.9(5) . . ? 
C2' C1' Hf1 72.2(3) . . ? 
C5' C1' Hf1 74.3(4) . . ? 
Si2 C1' Hf1 127.8(3) . . ? 
C1' C2' C3' 109.6(6) . . ? 
C1' C2' Hf1 74.8(4) . . ? 
C3' C2' Hf1 74.1(4) . . ? 
C2' C3' C4' 106.8(5) . . ? 
C2' C3' Hf1 72.5(4) . . ? 
C4' C3' Hf1 75.0(4) . . ? 
C5' C4' C3' 107.9(5) . . ? 
C5' C4' Hf1 73.5(3) . . ? 
C3' C4' Hf1 72.0(4) . . ? 
C4' C5' C1' 109.2(6) . . ? 
C4' C5' Hf1 74.0(4) . . ? 
C1' C5' Hf1 72.8(3) . . ? 
C18' C6' C7' 102.0(5) . . ? 
C18' C6' Si2 113.1(4) . . ? 
C7' C6' Si2 104.9(4) . . ? 
C8' C7' C12' 121.7(6) . . ? 
C8' C7' C6' 129.2(6) . . ? 
C12' C7' C6' 109.1(6) . . ? 
C7' C8' C9' 117.3(7) . . ? 
C10' C9' C8' 121.7(7) . . ? 
C11' C10' C9' 120.8(7) . . ? 
C10' C11' C12' 118.8(7) . . ? 
C11' C12' C7' 119.7(7) . . ? 
C11' C12' C13' 131.2(7) . . ? 
C7' C12' C13' 109.0(6) . . ? 
C18' C13' C14' 120.4(6) . . ? 
C18' C13' C12' 108.6(6) . . ? 
C14' C13' C12' 130.7(7) . . ? 
C15' C14' C13' 118.2(7) . . ? 
C14' C15' C16' 122.0(7) . . ? 
C15' C16' C17' 119.9(7) . . ? 
C18' C17' C16' 118.8(7) . . ? 
C17' C18' C13' 120.5(6) . . ? 
C17' C18' C6' 129.3(6) . . ? 
C13' C18' C6' 110.1(6) . . ? 
C24' C19' C20' 117.6(6) . . ? 
C24' C19' Si2 120.7(5) . . ? 
C20' C19' Si2 121.6(5) . . ? 
C21' C20' C19' 122.0(6) . . ? 
C20' C21' C22' 118.2(7) . . ? 
C23' C22' C21' 120.7(6) . . ? 
C22' C23' C24' 120.1(6) . . ? 
C23' C24' C19' 121.4(6) . . ? 
C26' C25' C30' 117.8(6) . . ? 
C26' C25' Si2 121.7(5) . . ? 
C30' C25' Si2 120.5(5) . . ? 
C25' C26' C27' 121.3(6) . . ? 
C28' C27' C26' 120.2(6) . . ? 
C29' C28' C27' 119.5(6) . . ? 
C28' C29' C30' 120.8(7) . . ? 
C25' C30' C29' 120.4(7) . . ? 
Cl4A C31 Cl3 100.3(21) . . ? 
Cl3 C31 Cl4 98.6(22) . . ? 
Cl5 C32 Cl6 102.2(24) . . ? 

_refine_diff_density_max    3.106 
_refine_diff_density_min   -2.383 
_refine_diff_density_rms    0.181 

data_va 
_database_code_CSD           152546

_journal_coden_Cambridge      186

_publ_contact_author
; Dr Alexander Z. Voskoboynikov
Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

_publ_contact_author_email        voskoboy@org.chem.msu.su

_publ_contact_letter
; reference number B009280K
;

_publ_section_title
;
ansa-Metallocenes with Ph2Si Bridge. Molecular structures of
Ph2Si(h5-fluorenyl)(h5-C5H4)HfCl2 and
[(9-fluorenyl)Ph2SiC5H4-h5]2HfCl2.
;

_publ_requested_journal           'J.Chem.Com., Dalton Trans.'

loop_
_publ_author_name
_publ_author_address

'Izmer, Vyacheslav V.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

'Agarkov, Anton Y.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

'Nosova, Valentina M.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

"Kuz'mina, Lyudmila G."
; N.S.Kurnakov Institute of General and Inorganic Chemistry
of Russian Academy of Science, 31 Leninskii prospect,
Moscow, 117907, Russia
;

'Howard, Judith A. K.'
; Department of Chemistry, University of Durham,
South Road, Durham, DH1 3LE, United Kingdom
;

'Beletskaya, Irina P.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

'Voskoboynikov, Alexander Z.'
; Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;

_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
[h^5^-1-(diphenyl(h^5^-flyoren-9-yl)silyl)-cyclopentadienyl]-
dichloro-hafnium dichlormethane solvate 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C31 H24 Cl4 Hf Si' 
_chemical_formula_weight          744.88 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

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' 
'Si'  'Si'   0.0817   0.0704 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Cl'  'Cl'   0.1484   0.1585 
'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            monoclinic
_symmetry_space_group_name_H-M    'P 1 21/c 1'

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

_cell_length_a                    11.0830(2) 
_cell_length_b                    8.9801(2) 
_cell_length_c                    28.7654(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  101.096(1) 
_cell_angle_gamma                 90.00 
_cell_volume                      2809.4(1) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        block
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.05 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.761 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1456 
_exptl_absorpt_coefficient_mu     4.157 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4659
_exptl_absorpt_correction_T_max   0.8582

_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        'Siemens SMART CCD'
_diffrn_measurement_method        \w
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11778 
_diffrn_reflns_av_R_equivalents   0.1223 
_diffrn_reflns_av_sigmaI/netI     0.0866 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -5 
_diffrn_reflns_limit_k_max        5 
_diffrn_reflns_limit_l_min        -37 
_diffrn_reflns_limit_l_max        36 
_diffrn_reflns_theta_min          1.44 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3487 
_reflns_number_observed           2652 
_reflns_observed_criterion        I>2\s(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 329 with very negative F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses 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 observed criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating R(obs) 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 w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+56.6996P] 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     constr
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0012(2) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3158 
_refine_ls_number_parameters      185 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0957 
_refine_ls_R_factor_obs           0.0620 
_refine_ls_wR_factor_all          0.1679 
_refine_ls_wR_factor_obs          0.1348 
_refine_ls_goodness_of_fit_all    1.108 
_refine_ls_goodness_of_fit_obs    1.136 
_refine_ls_restrained_S_all       1.228 
_refine_ls_restrained_S_obs       1.136 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
Hf1 Hf 0.28985(5) 0.45498(9) 0.81172(2) 0.0207(3) Uani 1 d . . 
Cl1 Cl 0.1173(3) 0.5626(5) 0.75941(11) 0.0269(12) Uani 1 d . . 
Cl2 Cl 0.4386(3) 0.5044(5) 0.76257(11) 0.0263(13) Uani 1 d . . 
Si1 Si 0.3192(3) 0.2975(6) 0.91580(13) 0.0201(13) Uani 1 d . . 
C1 C 0.2781(11) 0.2193(18) 0.8554(4) 0.017(3) Uiso 1 d . . 
C2 C 0.1628(12) 0.2383(19) 0.8230(5) 0.024(3) Uiso 1 d . . 
H2A H 0.0807(12) 0.2440(19) 0.8325(5) 0.029 Uiso 1 calc R . 
C3 C 0.1806(12) 0.2263(19) 0.7756(5) 0.025(3) Uiso 1 d . . 
H3A H 0.1140(12) 0.2240(19) 0.7467(5) 0.030 Uiso 1 calc R . 
C4 C 0.3064(13) 0.2000(19) 0.7766(5) 0.025(3) Uiso 1 d . . 
H4A H 0.3444(13) 0.1766(19) 0.7486(5) 0.030 Uiso 1 calc R . 
C5 C 0.3690(13) 0.2013(19) 0.8254(5) 0.026(4) Uiso 1 d . . 
H5A H 0.4573(13) 0.1744(19) 0.8368(5) 0.032 Uiso 1 calc R . 
C6 C 0.3341(11) 0.4939(18) 0.8972(4) 0.016(3) Uiso 1 d . . 
C7 C 0.2323(11) 0.5999(17) 0.8806(4) 0.014(3) Uiso 1 d . . 
C8 C 0.1034(11) 0.5902(19) 0.8836(4) 0.021(3) Uiso 1 d . . 
H8A H 0.0712(11) 0.5058(19) 0.8969(4) 0.025 Uiso 1 calc R . 
C9 C 0.0308(13) 0.7072(19) 0.8664(5) 0.025(4) Uiso 1 d . . 
H9A H -0.0522(13) 0.7066(19) 0.8705(5) 0.030 Uiso 1 calc R . 
C10 C 0.0715(13) 0.8303(21) 0.8426(5) 0.032(4) Uiso 1 d . . 
H10A H 0.0159(13) 0.9076(21) 0.8304(5) 0.039 Uiso 1 calc R . 
C11 C 0.1911(12) 0.8366(21) 0.8376(5) 0.027(3) Uiso 1 d . . 
H11A H 0.2188(12) 0.9178(21) 0.8213(5) 0.033 Uiso 1 calc R . 
C12 C 0.2739(12) 0.7232(19) 0.8565(5) 0.022(3) Uiso 1 d . . 
C13 C 0.4021(12) 0.6994(19) 0.8571(5) 0.022(3) Uiso 1 d . . 
C14 C 0.4895(12) 0.7865(20) 0.8400(5) 0.027(4) Uiso 1 d . . 
H14A H 0.4641(12) 0.8747(20) 0.8226(5) 0.033 Uiso 1 calc R . 
C15 C 0.6100(12) 0.7462(20) 0.8480(5) 0.027(4) Uiso 1 d . . 
H15A H 0.6692(12) 0.8083(20) 0.8378(5) 0.032 Uiso 1 calc R . 
C16 C 0.6459(13) 0.6117(20) 0.8715(5) 0.029(4) Uiso 1 d . . 
H16A H 0.7298(13) 0.5830(20) 0.8759(5) 0.035 Uiso 1 calc R . 
C17 C 0.5651(11) 0.5192(19) 0.8886(4) 0.021(3) Uiso 1 d . . 
H17A H 0.5913(11) 0.4278(19) 0.9039(4) 0.025 Uiso 1 calc R . 
C18 C 0.4398(11) 0.5678(19) 0.8820(4) 0.017(3) Uiso 1 d . . 
C19 C 0.4673(12) 0.2126(19) 0.9469(5) 0.020(3) Uiso 1 d . . 
C20 C 0.5457(13) 0.2823(21) 0.9848(5) 0.029(4) Uiso 1 d . . 
H20A H 0.5233(13) 0.3768(21) 0.9954(5) 0.034 Uiso 1 calc R . 
C21 C 0.6550(13) 0.2172(21) 1.0074(5) 0.031(4) Uiso 1 d . . 
H21A H 0.7081(13) 0.2681(21) 1.0322(5) 0.038 Uiso 1 calc R . 
C22 C 0.6854(14) 0.0782(21) 0.9933(5) 0.033(4) Uiso 1 d . . 
H22A H 0.7589(14) 0.0320(21) 1.0092(5) 0.040 Uiso 1 calc R . 
C23 C 0.6117(13) 0.0051(21) 0.9568(5) 0.029(4) Uiso 1 d . . 
H23A H 0.6354(13) -0.0894(21) 0.9467(5) 0.035 Uiso 1 calc R . 
C24 C 0.5026(12) 0.0698(20) 0.9347(5) 0.023(3) Uiso 1 d . . 
H24A H 0.4497(12) 0.0161(20) 0.9105(5) 0.028 Uiso 1 calc R . 
C25 C 0.1923(12) 0.2772(19) 0.9497(5) 0.020(3) Uiso 1 d . . 
C26 C 0.0948(11) 0.1805(18) 0.9357(5) 0.020(3) Uiso 1 d . . 
H26A H 0.0903(11) 0.1230(18) 0.9077(5) 0.023 Uiso 1 calc R . 
C27 C 0.0015(13) 0.1671(21) 0.9630(5) 0.033(4) Uiso 1 d . . 
H27A H -0.0655(13) 0.1008(21) 0.9533(5) 0.040 Uiso 1 calc R . 
C28 C 0.0088(14) 0.2507(20) 1.0034(5) 0.032(4) Uiso 1 d . . 
H28A H -0.0536(14) 0.2409(20) 1.0217(5) 0.039 Uiso 1 calc R . 
C29 C 0.1034(13) 0.3471(22) 1.0180(5) 0.033(4) Uiso 1 d . . 
H29A H 0.1065(13) 0.4045(22) 1.0459(5) 0.039 Uiso 1 calc R . 
C30 C 0.1966(13) 0.3610(21) 0.9912(5) 0.031(4) Uiso 1 d . . 
H30A H 0.2629(13) 0.4278(21) 1.0013(5) 0.037 Uiso 1 calc R . 
C31 C 0.7257(14) 0.2942(21) 0.8081(5) 0.037(5) Uani 1 d . . 
H31A H 0.6508(14) 0.3564(21) 0.8049(5) 0.045 Uiso 1 calc R . 
H31B H 0.7159(14) 0.2279(21) 0.7802(5) 0.045 Uiso 1 calc R . 
Cl4 Cl 0.8532(4) 0.4108(6) 0.8084(2) 0.052(2) Uani 1 d . . 
Cl3 Cl 0.7381(5) 0.1849(7) 0.8592(2) 0.067(2) Uani 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 
Hf1 0.0208(3) 0.0274(8) 0.0152(3) -0.0004(3) 0.0065(2) -0.0003(3) 
Cl1 0.025(2) 0.036(4) 0.019(2) 0.000(2) 0.0031(12) 0.000(2) 
Cl2 0.023(2) 0.040(4) 0.019(2) -0.001(2) 0.0119(13) -0.002(2) 
Si1 0.023(2) 0.022(5) 0.016(2) 0.004(2) 0.0076(15) 0.002(2) 
C31 0.036(9) 0.046(18) 0.029(8) -0.006(8) 0.005(7) -0.003(9) 
Cl4 0.036(2) 0.040(5) 0.084(3) -0.007(3) 0.020(2) -0.003(2) 
Cl3 0.079(4) 0.070(6) 0.056(3) 0.020(3) 0.020(3) 0.011(3) 

_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 
Hf1 Cl1 2.398(3) . ? 
Hf1 Cl2 2.411(3) . ? 
Hf1 C5 2.45(2) . ? 
Hf1 C6 2.437(12) . ? 
Hf1 C2 2.46(2) . ? 
Hf1 C1 2.48(2) . ? 
Hf1 C3 2.51(2) . ? 
Hf1 C4 2.52(2) . ? 
Hf1 C7 2.552(13) . ? 
Hf1 C18 2.566(13) . ? 
Hf1 C13 2.73(2) . ? 
Hf1 C12 2.75(2) . ? 
Si1 C1 1.848(13) . ? 
Si1 C19 1.874(14) . ? 
Si1 C25 1.868(13) . ? 
Si1 C6 1.86(2) . ? 
C1 C2 1.44(2) . ? 
C1 C5 1.46(2) . ? 
C2 C3 1.42(2) . ? 
C3 C4 1.41(2) . ? 
C4 C5 1.44(2) . ? 
C6 C18 1.48(2) . ? 
C6 C7 1.48(2) . ? 
C7 C12 1.43(2) . ? 
C7 C8 1.45(2) . ? 
C8 C9 1.36(2) . ? 
C9 C10 1.42(2) . ? 
C10 C11 1.36(2) . ? 
C11 C12 1.41(2) . ? 
C12 C13 1.43(2) . ? 
C13 C14 1.41(2) . ? 
C13 C18 1.40(2) . ? 
C14 C15 1.36(2) . ? 
C15 C16 1.40(2) . ? 
C16 C17 1.38(2) . ? 
C17 C18 1.43(2) . ? 
C19 C20 1.41(2) . ? 
C19 C24 1.40(2) . ? 
C20 C21 1.39(2) . ? 
C21 C22 1.37(2) . ? 
C22 C23 1.37(2) . ? 
C23 C24 1.38(2) . ? 
C25 C26 1.38(2) . ? 
C25 C30 1.40(2) . ? 
C26 C27 1.42(2) . ? 
C27 C28 1.37(2) . ? 
C28 C29 1.36(2) . ? 
C29 C30 1.41(2) . ? 
C31 Cl3 1.75(2) . ? 
C31 Cl4 1.76(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 
Cl1 Hf1 Cl2 96.37(12) . . ? 
Cl1 Hf1 C5 134.0(4) . . ? 
Cl2 Hf1 C5 90.0(3) . . ? 
Cl1 Hf1 C6 123.8(3) . . ? 
Cl2 Hf1 C6 122.5(3) . . ? 
C5 Hf1 C6 88.6(5) . . ? 
Cl1 Hf1 C2 89.6(3) . . ? 
Cl2 Hf1 C2 134.1(4) . . ? 
C5 Hf1 C2 55.9(5) . . ? 
C6 Hf1 C2 89.4(5) . . ? 
Cl1 Hf1 C1 123.3(3) . . ? 
Cl2 Hf1 C1 124.3(3) . . ? 
C5 Hf1 C1 34.4(4) . . ? 
C6 Hf1 C1 68.4(5) . . ? 
C2 Hf1 C1 33.9(4) . . ? 
Cl1 Hf1 C3 78.9(4) . . ? 
Cl2 Hf1 C3 103.8(3) . . ? 
C5 Hf1 C3 55.5(5) . . ? 
C6 Hf1 C3 121.5(5) . . ? 
C2 Hf1 C3 33.2(4) . . ? 
C1 Hf1 C3 56.1(4) . . ? 
Cl1 Hf1 C4 103.0(3) . . ? 
Cl2 Hf1 C4 79.7(3) . . ? 
C5 Hf1 C4 33.7(4) . . ? 
C6 Hf1 C4 121.2(5) . . ? 
C2 Hf1 C4 54.8(5) . . ? 
C1 Hf1 C4 56.2(5) . . ? 
C3 Hf1 C4 32.5(4) . . ? 
Cl1 Hf1 C7 89.6(3) . . ? 
Cl2 Hf1 C7 131.5(3) . . ? 
C5 Hf1 C7 119.1(4) . . ? 
C6 Hf1 C7 34.5(4) . . ? 
C2 Hf1 C7 93.8(5) . . ? 
C1 Hf1 C7 89.8(4) . . ? 
C3 Hf1 C7 124.5(4) . . ? 
C4 Hf1 C7 145.3(5) . . ? 
Cl1 Hf1 C18 130.7(4) . . ? 
Cl2 Hf1 C18 88.7(3) . . ? 
C5 Hf1 C18 94.8(5) . . ? 
C6 Hf1 C18 34.4(4) . . ? 
C2 Hf1 C18 120.6(4) . . ? 
C1 Hf1 C18 91.5(5) . . ? 
C3 Hf1 C18 147.0(5) . . ? 
C4 Hf1 C18 126.0(5) . . ? 
C7 Hf1 C18 53.7(4) . . ? 
Cl1 Hf1 C13 102.2(3) . . ? 
Cl2 Hf1 C13 80.3(3) . . ? 
C5 Hf1 C13 123.8(5) . . ? 
C6 Hf1 C13 54.4(5) . . ? 
C2 Hf1 C13 142.5(4) . . ? 
C1 Hf1 C13 120.5(4) . . ? 
C3 Hf1 C13 175.7(4) . . ? 
C4 Hf1 C13 149.3(4) . . ? 
C7 Hf1 C13 51.5(4) . . ? 
C18 Hf1 C13 30.5(4) . . ? 
Cl1 Hf1 C12 80.0(3) . . ? 
Cl2 Hf1 C12 103.1(3) . . ? 
C5 Hf1 C12 142.5(4) . . ? 
C6 Hf1 C12 54.6(5) . . ? 
C2 Hf1 C12 122.7(4) . . ? 
C1 Hf1 C12 119.7(4) . . ? 
C3 Hf1 C12 147.3(4) . . ? 
C4 Hf1 C12 175.8(4) . . ? 
C7 Hf1 C12 30.9(4) . . ? 
C18 Hf1 C12 51.4(4) . . ? 
C13 Hf1 C12 30.3(4) . . ? 
C1 Si1 C19 109.2(6) . . ? 
C1 Si1 C25 112.3(6) . . ? 
C19 Si1 C25 112.9(6) . . ? 
C1 Si1 C6 96.3(6) . . ? 
C19 Si1 C6 113.9(7) . . ? 
C25 Si1 C6 111.1(7) . . ? 
C2 C1 C5 105.0(11) . . ? 
C2 C1 Si1 126.2(11) . . ? 
C5 C1 Si1 121.8(10) . . ? 
C2 C1 Hf1 72.4(9) . . ? 
C5 C1 Hf1 71.6(9) . . ? 
Si1 C1 Hf1 97.1(7) . . ? 
C3 C2 C1 110.0(12) . . ? 
C3 C2 Hf1 75.2(9) . . ? 
C1 C2 Hf1 73.7(9) . . ? 
C4 C3 C2 108.3(12) . . ? 
C4 C3 Hf1 74.5(9) . . ? 
C2 C3 Hf1 71.6(9) . . ? 
C3 C4 C5 107.9(12) . . ? 
C3 C4 Hf1 73.0(10) . . ? 
C5 C4 Hf1 70.2(9) . . ? 
C4 C5 C1 108.7(12) . . ? 
C4 C5 Hf1 76.1(10) . . ? 
C1 C5 Hf1 74.0(9) . . ? 
C18 C6 C7 102.3(12) . . ? 
C18 C6 Si1 128.9(11) . . ? 
C7 C6 Si1 126.7(10) . . ? 
C18 C6 Hf1 77.6(7) . . ? 
C7 C6 Hf1 77.0(7) . . ? 
Si1 C6 Hf1 98.2(6) . . ? 
C12 C7 C8 119.2(13) . . ? 
C12 C7 C6 110.9(11) . . ? 
C8 C7 C6 129.8(13) . . ? 
C12 C7 Hf1 82.3(8) . . ? 
C8 C7 Hf1 114.3(9) . . ? 
C6 C7 Hf1 68.5(7) . . ? 
C9 C8 C7 117.0(14) . . ? 
C8 C9 C10 123.9(13) . . ? 
C11 C10 C9 119.3(16) . . ? 
C10 C11 C12 120.3(16) . . ? 
C11 C12 C13 133.1(15) . . ? 
C11 C12 C7 120.0(12) . . ? 
C13 C12 C7 106.9(13) . . ? 
C11 C12 Hf1 123.2(10) . . ? 
C13 C12 Hf1 73.9(9) . . ? 
C7 C12 Hf1 66.7(8) . . ? 
C14 C13 C18 119.4(13) . . ? 
C14 C13 C12 131.4(16) . . ? 
C18 C13 C12 109.2(13) . . ? 
C14 C13 Hf1 124.1(10) . . ? 
C18 C13 Hf1 68.3(8) . . ? 
C12 C13 Hf1 75.8(9) . . ? 
C15 C14 C13 120.9(16) . . ? 
C14 C15 C16 119.2(15) . . ? 
C17 C16 C15 123.1(14) . . ? 
C16 C17 C18 116.7(15) . . ? 
C13 C18 C17 120.6(13) . . ? 
C13 C18 C6 110.7(11) . . ? 
C17 C18 C6 128.7(14) . . ? 
C13 C18 Hf1 81.2(8) . . ? 
C17 C18 Hf1 116.6(10) . . ? 
C6 C18 Hf1 68.1(7) . . ? 
C20 C19 C24 116.1(13) . . ? 
C20 C19 Si1 122.9(13) . . ? 
C24 C19 Si1 120.9(10) . . ? 
C21 C20 C19 121.9(16) . . ? 
C22 C21 C20 119.1(15) . . ? 
C23 C22 C21 121.2(15) . . ? 
C22 C23 C24 119.5(17) . . ? 
C23 C24 C19 122.0(14) . . ? 
C26 C25 C30 118.7(12) . . ? 
C26 C25 Si1 122.2(10) . . ? 
C30 C25 Si1 119.1(11) . . ? 
C25 C26 C27 120.2(14) . . ? 
C28 C27 C26 119.4(15) . . ? 
C29 C28 C27 121.6(15) . . ? 
C28 C29 C30 119.4(16) . . ? 
C29 C30 C25 120.6(15) . . ? 
Cl3 C31 Cl4 113.4(9) . . ? 

_refine_diff_density_max    0.925 
_refine_diff_density_min   -2.382 
_refine_diff_density_rms    0.219