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_4115249
_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         '(C24 H38 O Ti), (C24 H20 B), (C4 H8 O)'
_chemical_formula_sum            'C52 H66 B O2 Ti'
_chemical_formula_weight         781.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   direct
_audit_creation_date             '2002-07-11  13:18:57'
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
 ?
;
_cell_angle_alpha                90
_cell_angle_beta                 90.060(8)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   17.995(2)
_cell_length_b                   13.483(1)
_cell_length_c                   18.008(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    130
_cell_measurement_theta_max      18.48
_cell_measurement_theta_min      16.18
_cell_volume                     4369.2(8)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'CAD4-UNIX software Version 5.1, 1994'
_computing_data_reduction        'HELENA (Spek, 1994)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 1994) 
 PLATON (Spek, 1994)
;
_computing_publication_material
;
 PLATON (Spek, 1990)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution
;
 DIRDIF-94 (Beurskens et al., 1994)
;
_diffrn_ambient_temperature      130(1)
_diffrn_detector_area_resol_mean ?'
_diffrn_measurement_device_type
;
  Enraf Nonius CAD-4F diffractometer
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_detector
;
  scintillation NaI crystal with photomultiplier
;
_diffrn_radiation_monochromator  'perpendicular mounted graphite'
_diffrn_radiation_source         'fine focus sealed Philips Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.055
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8816
_diffrn_reflns_reduction_process
;

 Intensity data were corrected for Lorentz and polarization effects,
  scale variation, for absorption and reduced to F~o~^2^
;
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        ' no decay, variation 1.3'
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.37
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    'constr - riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         7140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_gt           0.1322
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+4.11P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_reflns_number_gt                5287
_reflns_number_total             8368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027617w-3_s2_1.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4115249