ansa-Metallocenes with a Ph2Si bridge: molecular structures of HfCl2[Ph2Si(η5-C13H8)(η5-C5H4)] and HfCl2[Ph2Si(C13H9)(η5-C5H4)]2
Vyacheslav V. Izmer; Anton Y. Agarkov; Valentina M. Nosova; Lyudmila G. Kuz'mina; Judith A. K. Howard; Irina P. Beletskaya; Alexander Z. Voskoboynikov; J. Chem. Soc., Dalton Trans.  (2001) 1131–1136; doi:10.1039/b009280k

data_7010454
_publ_contact_author
; Dr Alexander Z. Voskoboynikov
Department of Chemistry, Moscow State University
Leninskie Gory, Moscow 119899, Russia
;
_publ_section_title
;
 ansa-Metallocenes with a Ph2Si bridge: molecular structures of
 HfCl2[Ph2Si(\h5-C13H8)(\h5-C5H4)] and HfCl2[Ph2Si(C13H9)(\h5-C5H4)]2
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1131
_journal_page_last               1136
_journal_paper_doi               10.1039/b009280k
_journal_year                    2001
_chemical_formula_sum            'C61.5 H49 Cl5 Hf Si2'
_chemical_formula_weight         1199.93
_chemical_name_systematic
; 
Bis[(diphenyl-(fluoren-9-yl)-silyl)cyclopentadienyl]
dichloro-hafnium(IV)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                69.997(1)
_cell_angle_beta                 71.314(2)
_cell_angle_gamma                89.535(1)
_cell_formula_units_Z            2
_cell_length_a                   13.5860(9)
_cell_length_b                   14.0886(6)
_cell_length_c                   15.9919(6)
_cell_measurement_temperature    150(2)
_cell_volume                     2706.9(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19863
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    2.257
_exptl_absorpt_correction_T_max  0.8216
_exptl_absorpt_correction_T_min  0.5678
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      ?
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.106
_refine_diff_density_min         -2.383
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         11343
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.418
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_obs          0.0589
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+17.9727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2142
_refine_ls_wR_factor_obs         0.1489
_reflns_number_observed          10576
_reflns_number_total             12276
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            b009280k.txt
_cod_data_source_block           v2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+17.9727P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+17.9727P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C61.50 H49 Cl5 Hf Si2'
_cod_database_code               7010454