Versatile Coordination of Cyclopentadienyl-Arene Ligands and Its Role in Titanium-Catalyzed Ethylene Trimerization
Edwin Otten; Aurora A. Batinas; Auke Meetsma; Bart Hessen; Journal of the American Chemical Society 131 (2009) 5298–5312; doi:10.1021/ja810089f

data_4104167
_publ_contact_author_address
;
  Crystal Structure Center, Chemical Physics,
  Zernike Institute for Advanced Materials,
  University of Groningen,
  Nijenborgh 4,
  NL-9747 AG Groningen, The Netherlands.
;
_publ_contact_author_email       A.Meetsma@rug.nl
_publ_contact_author_fax         '+31 50 3634441'
_publ_contact_author_name
;
  Drs. A. Meetsma
;
_publ_contact_author_phone       '+31 50 3634368'
_publ_section_title
;
 Versatile Coordination of Cyclopentadienyl-Arene Ligands and Its Role in
 Titanium-Catalyzed Ethylene Trimerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5298
_journal_page_last               5312
_journal_paper_doi               10.1021/ja810089f
_journal_volume                  131
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C24 B F20, C16 H21 Ti'
_chemical_formula_sum            'C40 H21 B F20 Ti'
_chemical_formula_weight         940.27
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2009-02-09  09:05:58'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version :: 240908)
 SHELXL97-2 & Manual Editing
;
_cell_angle_alpha                90
_cell_angle_beta                 91.066(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.791(1)
_cell_length_b                   13.320(1)
_cell_length_c                   28.398(3)
_cell_measurement_reflns_used    9603
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.35
_cell_volume                     4081.1(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus '
_computing_molecular_graphics
;
 PLATON (Spek, 2003)
 PLUTO (Meetsma, 2008)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
 DIRDIF-08 (Beurskens et al., 2008)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28595
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT-Plus & SADABS (Bruker, 2007).
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.33
_exptl_absorpt_correction_T_max  0.9822
_exptl_absorpt_correction_T_min  0.8189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2001))'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         7155
_refine_ls_number_restraints     640
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1726
_refine_ls_wR_factor_ref         0.1916
_reflns_number_gt                4302
_reflns_number_total             7155
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja810089f_si_002.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4104167
_vrn_publ_code_void_volume       570.4
_vrn_publ_code_frame_time_sec    30.0
_vrn_publ_code_meas_time_hour    18.0