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_4079670
_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            'C34 H31 Mo O5 P Ti'
_chemical_formula_weight         694.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.788(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7310(8)
_cell_length_b                   9.0707(4)
_cell_length_c                   20.6103(10)
_cell_measurement_reflns_used    11673
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2830
_cell_measurement_theta_min      2.2407
_cell_volume                     3078.0(3)
_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 16.1419
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, 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  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58664
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98305
_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    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment
;
The hydrogens of the seven membered ring were refined with free
coordinates but fixed displacement parameters.  
The methyls were refined using a rigid model and others were riding. 
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6290
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0306
_refine_ls_wR_factor_ref         0.0315
_reflns_number_gt                4283
_reflns_number_total             6290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300927r_si_001.cif
_cod_data_source_block           atag18
_cod_original_cell_volume        3078.0(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4079670