Titanium Hydrazinediido Half-Sandwich Complexes: Highly Active Catalysts for the Hydrohydrazination of Terminal Alkynes at Ambient Temperature
Weitershaus, Katharina; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 28 (2009) 4898–; doi:10.1021/om900641e

data_4070183
_publ_section_title
;
 Titanium Hydrazinediido Half-Sandwich Complexes: Highly Active Catalysts
 for the Hydrohydrazination of Terminal Alkynes at Ambient Temperature
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4898
_journal_paper_doi               10.1021/om900641e
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C34 H43 N5 Ti'
_chemical_formula_weight         569.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_block_code                ga_kw25
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.644(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.483(2)
_cell_length_b                   17.855(3)
_cell_length_c                   15.233(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3119.9(10)
_computing_cell_refinement       'SAINT (Bruker AXS, 1997-2008)'
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2008)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector (Bruker AXS Smart 1000)'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            62584
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.11
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+4.2544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                4572
_reflns_number_total             7153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900641e_si_001.cif
_cod_data_source_block           complex_2a
_cod_original_cell_volume        3120.0(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4070183
_audit_block_refno               822