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_7010455
_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            'C31 H24 Cl4 Hf Si'
_chemical_formula_weight         744.88
_chemical_name_systematic
; 
[h^5^-1-(diphenyl(h^5^-flyoren-9-yl)silyl)-cyclopentadienyl]-
dichloro-hafnium dichlormethane solvate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.096(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0830(2)
_cell_length_b                   8.9801(2)
_cell_length_c                   28.7654(6)
_cell_measurement_temperature    150(2)
_cell_volume                     2809.40(10)
_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  0.1223
_diffrn_reflns_av_sigmaI/netI    0.0866
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            11778
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    4.157
_exptl_absorpt_correction_T_max  0.8582
_exptl_absorpt_correction_T_min  0.4659
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.925
_refine_diff_density_min         -2.382
_refine_diff_density_rms         0.219
_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_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.108
_refine_ls_goodness_of_fit_obs   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.228
_refine_ls_restrained_S_obs      1.136
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_obs          0.0620
_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^)+(0.0444P)^2^+56.6996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1679
_refine_ls_wR_factor_obs         0.1348
_reflns_number_observed          2652
_reflns_number_total             3487
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            b009280k.txt
_cod_data_source_block           va
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+56.6996P] 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^)+(0.0444P)^2^+56.6996P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2809.4(1)
_cod_database_code               7010455