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_4105389
_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            'C29 H21 Mo O5 P Ti'
_chemical_formula_weight         624.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.5819(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.9896(4)
_cell_length_b                   10.02607(10)
_cell_length_c                   17.1398(2)
_cell_measurement_reflns_used    29903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.6839
_cell_measurement_theta_min      2.0793
_cell_volume                     5240.45(11)
_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 RED, 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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            98358
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment
;
The hydrogens of the five- and seven-membered rings were refined freely.
Other H atoms were included using a riding model.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7987
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                6080
_reflns_number_total             7987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9080056_si_003.cif
_cod_data_source_block           susy41
_cod_original_cell_volume        5240.45(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4105389