Generation of Ti(II) Alkyne Trimerization Catalysts in the Absence of Strong Metal Reductants.
See, Xin Yi; Beaumier, Evan P.; Davis-Gilbert, Zachary W; Dunn, Peter L.; Larsen, Jacob A.; Pearce, Adam J.; Wheeler, T. Alex; Tonks, Ian A.; Organometallics 36 (2017) 1383–1390; doi:10.1021/acs.organomet.7b00096

data_4087306
_publ_section_title
;
 Generation of Ti(II) Alkyne Trimerization Catalysts in the Absence of
 Strong Metal Reductants.
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1383
_journal_page_last               1390
_journal_paper_doi               10.1021/acs.organomet.7b00096
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C57 H77 N5 Ti'
_chemical_formula_sum            'C57 H77 N5 Ti'
_chemical_formula_weight         880.13
_chemical_name_common            16121_0m
_chemical_name_systematic        Ti(NTol)(iPr2-N^N)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.510(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.516(2)
_cell_length_b                   14.4749(17)
_cell_length_c                   23.531(5)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.505
_cell_measurement_theta_min      2.9385
_cell_volume                     5116.3(14)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            133614
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.747
_diffrn_reflns_theta_min         2.942
_diffrn_source                   fine
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       Block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0610P)^2^+1.7097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9173
_reflns_number_total             10476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00096_si_002.cif
_cod_data_source_block           16121_0m
_cod_depositor_comments
'Adding full bibliography for 4087304--4087307.cif.'
_cod_original_cell_volume        5116.5(14)
_cod_database_code               4087306
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.875
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              18350
_shelx_hkl_checksum              80698