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_4085751
_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_moiety         'C31 H42 Cl O P Ti'
_chemical_formula_sum            'C31 H42 Cl O P Ti'
_chemical_formula_weight         544.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.3650(6)
_cell_length_b                   23.435(2)
_cell_length_c                   32.712(3)
_cell_measurement_reflns_used    6442
_cell_measurement_temperature    115
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      2.55
_cell_volume                     5646.1(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean 9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            36528
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.630
_diffrn_reflns_theta_min         2.965
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0623 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.8472.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+2.6565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4508
_reflns_number_total             6272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00250_si_003.cif
_cod_data_source_block           3a
_cod_original_cell_volume        5646.2(8)
_cod_database_code               4085751
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.923
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C15(H15a,H15b), C17(H17a,H17b), C25(H25a,H25b), C18(H18a,
 H18b), C16(H16a,H16b), C21(H21a,H21b), C22(H22a,H22b), C24(H24a,H24b),
 C23(H23a,H23b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C31(H31), C27(H27), C7(H7), C30(H30), C5(H5), C29(H29), C28(H28),
 C4(H4), C3(H3), C6(H6), C10(H10), C8(H8), C9(H9)
2.d Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C12(H12a,H12b,H12c)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'