2-Aminopyrrolines: New Chiral Amidinate Ligands with a Rigid Well-Defined Molecular Structure and Their Coordination to TiIV
Ward, Benjamin D.; Risler, Hélène; Weitershaus, Katharina; Bellemin-Laponnaz, Stéphane; Wadepohl, Hubert; Gade, Lutz H.; Inorganic Chemistry 45 (2006) 7777–7787; doi:10.1021/ic060809y

data_4332758
_publ_section_title
;
 2-Aminopyrrolines:&#x00A0; New Chiral Amidinate Ligands with a Rigid
 Well-Defined Molecular Structure and Their Coordination to TiIV
;
_journal_issue                   19
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7777
_journal_page_last               7787
_journal_paper_doi               10.1021/ic060809y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C28 H42 N6 Ti'
_chemical_formula_sum            'C28 H42 N6 Ti'
_chemical_formula_weight         510.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.3150(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9730(5)
_cell_length_b                   8.2490(3)
_cell_length_c                   22.5880(10)
_cell_measurement_reflns_used    5273
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2791.10(18)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measured_fraction_theta_max 0.95
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_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  0.1001
_diffrn_reflns_av_sigmaI/netI    0.1734
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9818
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1997) 
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1823
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0833P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1871
_reflns_number_gt                3533
_reflns_number_total             6325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060809ysup1.cif
_cod_data_source_block           11
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4332758