Neutral and Zwitterionic Low-Coordinate Titanium Complexes Bearing the Terminal Phosphinidene Functionality. Structural, Spectroscopic, Theoretical, and Catalytic Studies Addressing the Ti-P Multiple Bond
Guangyu Zhao; Falguni Basuli; Uriah J. Kilgore; Hongjun Fan; Halikhedkar Aneetha; John C. Huffman; Gang Wu; Daniel J. Mindiola; Journal of the American Chemical Society 128 (2006) 13575–13585; doi:10.1021/ja064853o

data_4110971
_publ_section_title
;
 Neutral and Zwitterionic Low-Coordinate Titanium Complexes Bearing the
 Terminal Phosphinidene Functionality. Structural, Spectroscopic,
 Theoretical, and Catalytic Studies Addressing the Ti-P Multiple Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13575
_journal_page_last               13585
_journal_paper_doi               10.1021/ja064853o
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C55 H87 N2 P Ti, 0.5(C6 H14)'
_chemical_formula_sum            'C58 H94 N2 P Ti'
_chemical_formula_weight         898.22
_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                 93.21(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.854(18)
_cell_length_b                   21.04(2)
_cell_length_c                   18.74(3)
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      23.16
_cell_measurement_theta_min      2.31
_cell_volume                     5454(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local program)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
'   0.30 degree frames measured for 30.17 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.1135
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18817
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       irrregular
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.797
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         11975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.797
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                7099
_reflns_number_total             11975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064853osi20060707_082854.cif
_cod_data_source_block           05085
_cod_original_cell_volume        5453(12)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4110971