Structure of the Decamethyl Titanocene Cation, a Metallocene with Two Agostic C-H Bonds, and Its Interaction with Fluorocarbons
Marco W. Bouwkamp; Jeanette de Wolf; Isabel del Hierro Morales; Jeroen Gercama; Auke Meetsma; Sergei I. Troyanov; Bart Hessen; Jan H. Teuben; Journal of the American Chemical Society 124 (2002) 12956–12957; doi:10.1021/ja027617w

data_4115251
_publ_contact_author_address
;
     Crystal Structure Center,
     Inorganic Solid State Chemistry Laboratory
     Chemical Physics,
     Materials Science Center,
     Groningen University,
     Nijenborgh 4,
     NL-9747 AG Groningen,
     The Netherlands.
;
_publ_contact_author_email       A.Meetsma@fwn.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
;
 Structure of the Decamethyl Titanocene Cation, a Metallocene with Two
 Agostic C-H Bonds, and Its Interaction with Fluorocarbons
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12956
_journal_page_last               12957
_journal_paper_doi               10.1021/ja027617w
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C20 H30 Ti, C24 H20 B'
_chemical_formula_sum            'C44 H50 B Ti'
_chemical_formula_weight         637.56
_chemical_name_systematic
;
 ?
;
_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   difmap
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   direct
_audit_creation_date             '2002-04-08  11:32:23'
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
 ?
;
_cell_angle_alpha                97.131(1)
_cell_angle_beta                 90.604(1)
_cell_angle_gamma                91.970(1)
_cell_formula_units_Z            4
_cell_length_a                   13.3636(7)
_cell_length_b                   15.0600(7)
_cell_length_c                   17.7873(9)
_cell_measurement_reflns_used    3994
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      23.49
_cell_measurement_theta_min      2.29
_cell_volume                     3549.6(3)
_computing_cell_refinement       'SAINT, Bruker Version 6.02A, 2000'
_computing_data_collection       'SMART, Bruker Version 5.624, 2001'
_computing_data_reduction        'XPREP, Bruker Version 5.1/NT, 2000'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2001) 
 PLATON (Spek, 1994)
;
_computing_publication_material
;
 PLATON (Spek, 1990)
 SHELXL (Sheldrick, 1997)
;
_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 '4096x4096 / 62x62 (binned 512)'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
  Bruker Smart Apex 
;
_diffrn_measurement_method       'phi and omega 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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25797
_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        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_correction_T_min  0.9016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2000))'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         12451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                7628
_reflns_number_total             12451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027617w-3_s2_3.cif
_cod_data_source_block           global
_cod_database_code               4115251
_vrn_publ_code_void_volume       0.0
_vrn_publ_code_frame_time        20.0
_vrn_publ_code_meas_time         13.0