Synthesis, Characterization and Reactivity of Group 4 Metallocene Bis(diphenylphosphino)acetylene Complexes-A Reactivity and Bonding Study
Martin Haehnel; Sven Hansen; Kathleen Schubert; Perdita Arndt; Anke Spannenberg; Haijun Jiao; Uwe Rosenthal; Journal of the American Chemical Society 135 (2013) 17556–17565; doi:10.1021/ja409320k

data_4121171
_publ_section_title
;
 Synthesis, Characterization and Reactivity of Group 4 Metallocene
 Bis(diphenylphosphino)acetylene Complexes-A Reactivity and Bonding Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17556
_journal_page_last               17565
_journal_paper_doi               10.1021/ja409320k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C46 H44 P2 Ti'
_chemical_formula_weight         706.65
_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                68.8320(10)
_cell_angle_beta                 73.9580(10)
_cell_angle_gamma                72.2450(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4225(2)
_cell_length_b                   12.4016(2)
_cell_length_c                   15.9682(3)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      2.31
_cell_volume                     1973.41(6)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            42877
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
Contributions of disordered solvent molecules were removed from the 
diffraction data with PLATON / SQUEEZE (van der Sluis & Spek, 1990; 
Spek, 2009). 
;
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         9797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0396P)^2^+0.3191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                7811
_reflns_number_total             9797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409320k_si_003.cif
_cod_data_source_block           ax0169
_cod_database_code               4121171