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_4104168
_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, C18 H25 Ti'
_chemical_formula_sum            'C42 H25 B F20 Ti'
_chemical_formula_weight         968.31
_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             '2006-01-27  08:24:21'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version :: 110805)
 SHELXL97-2 & Manual Editing
;
_cell_angle_alpha                90
_cell_angle_beta                 91.830(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0159(9)
_cell_length_b                   19.541(1)
_cell_length_c                   15.977(1)
_cell_measurement_reflns_used    6331
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.44
_cell_volume                     3749.5(4)
_computing_cell_refinement       'SAINTPLUS, Version 6.02A, (Bruker, 2000)'
_computing_data_collection       'SMART, Version 5.624, (Bruker, 2001)'
_computing_data_reduction        'XPREP, Version 5.1/NT, (Bruker, 2000)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2005)
 PLATON (Spek, 2003)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0862
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26584
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.9510
_exptl_absorpt_correction_T_min  0.8689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2001))'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         6618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0495P)^2^+0.6185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                4283
_reflns_number_total             6618
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja810089f_si_003.cif
_cod_data_source_block           Q1076
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4104168
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    8.0