Titanium hydroamination catalysts bearing a 2-aminopyrrolinato spectator ligand: monitoring the individual reaction steps
Weitershaus, Katharina; Ward, Benjamin D.; Kubiak, Raphael; Müller, Carsten; Wadepohl, Hubert; Doye, Sven; Gade, Lutz H.; Dalton Transactions  (2009) 4586–4602; doi:10.1039/b902038a

data_7001424
_publ_section_title
;
 Titanium hydroamination catalysts bearing a 2-aminopyrrolinato
 spectator ligand: monitoring the individual reaction steps
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4586
_journal_page_last               4602
_journal_paper_doi               10.1039/b902038a
_journal_year                    2009
_chemical_formula_sum            'C44 H59 N3 Ti'
_chemical_formula_weight         677.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_kw16
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.994(4)
_cell_angle_beta                 96.108(4)
_cell_angle_gamma                108.513(4)
_cell_formula_units_Z            2
_cell_length_a                   9.5091(19)
_cell_length_b                   12.983(3)
_cell_length_c                   17.624(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1938.0(7)
_computing_cell_refinement
;
SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors
from Monte Carlo simulations.
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45869
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6762
_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            orange
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.073
_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   1.112
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         11314
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.3031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1588
_reflns_number_gt                7894
_reflns_number_total             11314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902038a.txt
_cod_data_source_block           complex_11
_cod_original_cell_volume        1937.9(7)
_cod_database_code               7001424
_audit_block_refno               625