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_4332756
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H50 N6 O2 Ti, C6 H6'
_chemical_formula_sum            'C38 H56 N6 O2 Ti'
_chemical_formula_weight         676.80
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.651(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8179(8)
_cell_length_b                   12.6276(9)
_cell_length_c                   12.8169(9)
_cell_measurement_reflns_used    6687
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1890.9(2)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43494
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.607
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.51
_refine_ls_abs_structure_details 'Flack, 34 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9849
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6671
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000376
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 p=(max(Fo^2^,0) + 2Fc^2^)/3 
 Method = SHELXL 97 (Sheldrick, 1997) 
 w=1/[sigma^2^(F^2^) + 0.04 + 2.37p] 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1129
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1129
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                5407
_reflns_number_total             6671
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            ic060809ysup1.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4332756