Selective Lithiation and Phosphane-Functionalization of [(η7-C7H7)Ti(η5-C5H5)] (Troticene) and Its Use for the Preparation of Early-Late Heterobimetallic Complexes
Swagat K. Mohapatra; Susanne Büschel; Constantin Daniliuc; Peter G. Jones; Matthias Tamm; Journal of the American Chemical Society 131 (2009) 17014–17023; doi:10.1021/ja9080056

data_4105387
_publ_section_title
;
 Selective Lithiation and Phosphane-Functionalization of
 [(\h7-C7H7)Ti(\h5-C5H5)] (Troticene) and Its Use for the Preparation of
 Early-Late Heterobimetallic Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17014
_journal_page_last               17023
_journal_paper_doi               10.1021/ja9080056
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C49 H74 Li4 N6 Ti2'
_chemical_formula_weight         870.70
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.282(2)
_cell_angle_beta                 94.171(4)
_cell_angle_gamma                101.030(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0047(4)
_cell_length_b                   12.0319(4)
_cell_length_c                   17.3320(6)
_cell_measurement_reflns_used    14145
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1538
_cell_measurement_theta_min      2.0166
_cell_volume                     2450.22(14)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_molecular_graphics    'BRUKER XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.1121
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63649
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       prism
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.764
_refine_ls_hydrogen_treatment
;
The hydrogens of the five- and seven-membered rings were refined freely.
The hydrogens of the methyl groups were refined using rigid groups,
other H atoms were included using a riding model.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         11139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.764
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0197P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                6400
_reflns_number_total             11139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9080056_si_001.cif
_cod_data_source_block           swag01
_cod_database_code               4105387