Formation and Structures of Hafnocene Complexes in MAO- and AlBui3/CPh3[B(C6F5)4]-Activated Systems
Bryliakov, Konstantin P.; Talsi, Evgenii P.; Voskoboynikov, Alexander Z.; Lancaster, Simon J.; Bochmann, Manfred; Organometallics 27 (2008) 6333–; doi:10.1021/om800664p

data_4072201
_publ_section_title
;
 Formation and Structures of Hafnocene Complexes in MAO- and
 AlBui3/CPh3[B(C6F5)4]-Activated Systems
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6333
_journal_paper_doi               10.1021/om800664p
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C32 H35 Cl Hf Si'
_chemical_formula_structural
;
(C13H8CH2CH2-2-C12H9-1-CH3)Hf(Cl)(CH2Si(CH3)3)
;
_chemical_formula_sum            'C32 H35 Cl Hf Si'
_chemical_formula_weight         661.63
_chemical_name_common
;             
Compound 12, C2H4(Flu)(5,6-C3H6-2-2MeInd)Hf(Cl)CH2SiMe3
;
_chemical_name_systematic
;
(chloro)(9-[2-(2-methyl-5,6,7-trihydroindacen-1-yl)ethyl]-fluorenyl)
(trimethylsilylmethyl)hafnium
;
_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-97 and CrysAlis RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 116.194(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2434(6)
_cell_length_b                   10.0370(3)
_cell_length_c                   17.8692(5)
_cell_measurement_reflns_used    21716
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2775.06(16)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Bruker-Nonius Roper CCD camera on \k-goniostat
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21382
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    3.917
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+22.9373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                3784
_reflns_number_total             4852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800664p_si_001.cif
_cod_data_source_block           2008src0396
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2775.06(15)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4072201