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_4087304
_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         'C20 H29 I2 N O3 Ti'
_chemical_formula_sum            'C20 H29 I2 N O3 Ti'
_chemical_formula_weight         623.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.989(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.324(5)
_cell_length_b                   10.083(4)
_cell_length_c                   16.295(6)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.565
_cell_measurement_theta_min      2.386
_cell_volume                     2330.6(15)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26924
_diffrn_reflns_theta_full        28.91
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    3.035
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       red
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.572
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         5796
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+3.1831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                4934
_reflns_number_total             5796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00096_si_002.cif
_cod_data_source_block           s_0m
_cod_depositor_comments
'Adding full bibliography for 4087304--4087307.cif.'
_cod_original_cell_volume        2330.6(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4087304