Synthesis and Characterization of the Titanium Bisamide Ti{N(H)AriPr6}2 (AriPr6= C6H3-2,6-(C6H2-2,4,6-iPr3)2 and Its TiCl{N(H)AriPr6}2 Precursor: Ti(II) →Ti(IV) Cyclization
Jessica N. Boynton; Jing-Dong Guo; Fernande Grandjean; James C. Fettinger; Shigeru Nagase; Gary J. Long; Philip P. Power; Inorganic Chemistry 52 (2013) 14216–14223; doi:10.1021/ic4021355

data_4337003
_publ_section_title
;
 Synthesis and Characterization of the Titanium Bisamide Ti{N(H)AriPr6}2
 (AriPr6= C6H3-2,6-(C6H2-2,4,6-iPr3)2 and Its TiCl{N(H)AriPr6}2 Precursor:
 Ti(II) \\rightarrow Ti(IV) Cyclization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14216
_journal_page_last               14223
_journal_paper_doi               10.1021/ic4021355
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C72 H100 Cl N2 Ti, C6 H14, C6 H12'
_chemical_formula_sum            'C84 H126 Cl N2 Ti'
_chemical_formula_weight         1247.21
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                87.7219(5)
_cell_angle_beta                 72.4363(4)
_cell_angle_gamma                65.1037(4)
_cell_formula_units_Z            2
_cell_length_a                   14.7300(5)
_cell_length_b                   15.2643(5)
_cell_length_c                   19.6629(6)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.21
_cell_volume                     3803.7(2)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2012.2-0) (Bruker, 2012)'
_computing_data_reduction        'SAINT (8.27b) (Bruker, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34082
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.167
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.9695
_exptl_absorpt_correction_T_min  0.9140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1366
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.161
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         17383
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+2.0838P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13601
_reflns_number_total             17383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4021355_si_002_1.cif
_cod_data_source_block           JB28FMI
_cod_original_cell_volume        3803.8(2)
_cod_database_code               4337003
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.970
_shelxl_version_number           2012-9
_shelx_res_checksum              30668