Synthetic Endeavors toward Titanium Based Frustrated Lewis Pairs with Controlled Electronic and Steric Properties
Normand, Adrien T.; Richard, Philippe; Balan, Cédric; Daniliuc, Constantin G.; Kehr, Gerald; Erker, Gerhard; Le Gendre, Pierre; Organometallics  (2015) 150513110717003–; doi:10.1021/acs.organomet.5b00250

data_4085755
_publ_section_title
;
 Synthetic Endeavors toward Titanium Based Frustrated Lewis Pairs with
 Controlled Electronic and Steric Properties
;
_journal_name_full               Organometallics
_journal_page_first              150513110717003
_journal_paper_doi               10.1021/acs.organomet.5b00250
_journal_year                    2015
_chemical_formula_sum            'C59 H58 B O P Ti'
_chemical_formula_weight         872.73
_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                107.561(3)
_cell_angle_beta                 90.056(2)
_cell_angle_gamma                110.923(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6294(4)
_cell_length_b                   14.1385(5)
_cell_length_c                   14.6835(5)
_cell_measurement_reflns_used    5895
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     2317.41(15)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22187
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.17
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            'pale red'
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         7919
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.1052
_refine_ls_shift/su_max          0.000
_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^+10.6950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2260
_reflns_number_gt                5125
_reflns_number_total             7919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00250_si_009.cif
_cod_data_source_block           erk7681
_cod_original_cell_volume        2317.41(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085755