Mono- and Dilithiation of [(η7-C7H7)Ti(η5-C5Me5)] (Pentamethyltroticene) for the Synthesis of Troticenyl Monophosphanes and [2]Troticenophanes with C‒P and C‒Si Bridges
Tagne Kuate, Alain C.; Mohapatra, Swagat K.; Daniliuc, Constantin G.; Jones, Peter G.; Tamm, Matthias; Organometallics 31 (2012) 8544–; doi:10.1021/om300927r

data_4079667
_publ_section_title
;
 Mono- and Dilithiation of [(\h7-C7H7)Ti(\h5-C5Me5)]
 (Pentamethyltroticene) for the Synthesis of Troticenyl Monophosphanes and
 [2]Troticenophanes with C--P and C--Si Bridges
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              8544
_journal_paper_doi               10.1021/om300927r
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C29 H38 P Ti'
_chemical_formula_weight         465.46
_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                102.585(6)
_cell_angle_beta                 99.292(8)
_cell_angle_gamma                116.434(8)
_cell_formula_units_Z            2
_cell_length_a                   11.1956(10)
_cell_length_b                   11.2091(8)
_cell_length_c                   11.5927(10)
_cell_measurement_reflns_used    7296
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6465
_cell_measurement_theta_min      4.0869
_cell_volume                     1214.5(2)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_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 10.3543
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11728
_diffrn_reflns_theta_full        72.50
_diffrn_reflns_theta_max         75.83
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    3.691
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0909
_reflns_number_gt                4216
_reflns_number_total             4975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300927r_si_001.cif
_cod_data_source_block           swag31
_cod_original_cell_volume        1214.52(17)
_cod_database_code               4079667