Selective Dilithiation of [Ti(η5-C5H5)(η8-C8H8)] and Subsequent Conversion into Neutral and Cationic ansa-Complexes
Holger Braunschweig; Marco Fuss; Thomas Kupfer; Krzysztof Radacki; Journal of the American Chemical Society 133 (2011) 5780–5783; doi:10.1021/ja2014218

data_4105997
_publ_contact_author_address
; Institut fuer Anorganische Chemie
Universitaet Wuerzburg
Am Hubland
97074 Wuerzburg, Germany
;
_publ_contact_author_email       H.Braunschweig@mail.uni-wuerzburg.de
_publ_contact_author_fax         +49-931-31-84623
_publ_contact_author_name        'Prof. Dr. Holger Braunschweig'
_publ_contact_author_phone       +49-931-31-85260
_publ_section_title
;
 Selective Dilithiation of [Ti(\h5-C5H5)(\h8-C8H8)] and Subsequent
 Conversion into Neutral and Cationic ansa-Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5780
_journal_page_last               5783
_journal_paper_doi               10.1021/ja2014218
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C44 H68 Li4 N6 Ti2, 2(C4 H8 O)'
_chemical_formula_sum            'C52 H84 Li4 N6 O2 Ti2'
_chemical_formula_weight         948.81
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.506(6)
_cell_angle_beta                 113.485(4)
_cell_angle_gamma                107.899(6)
_cell_formula_units_Z            1
_cell_length_a                   10.8890(10)
_cell_length_b                   11.824(2)
_cell_length_c                   12.4298(13)
_cell_measurement_reflns_used    9285
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.19
_cell_volume                     1308.8(3)
_computing_cell_refinement       'Saint+ ver. 7.53A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2008.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.53A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58768
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2008/1 (Brucker 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5900
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.8162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                5127
_reflns_number_total             5900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2014218_si_001.cif
_cod_data_source_block           C52H84Li4N6O2Ti2
_cod_database_code               4105997