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_4332759
_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         'C40 H50 N6 Ti1'
_chemical_formula_sum            'C40 H50 N6 Ti'
_chemical_formula_weight         662.78
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 117.311(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.222(3)
_cell_length_b                   12.1398(15)
_cell_length_c                   15.759(2)
_cell_measurement_reflns_used    11637
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     3607.4(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.961
_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  0.038
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45209
_diffrn_reflns_theta_full        30.786
_diffrn_reflns_theta_max         32.068
_diffrn_reflns_theta_min         1.995
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.61
_refine_diff_density_min         -1.07
_refine_ls_abs_structure_details 'Racemic Twin'
_refine_ls_abs_structure_Flack   0.239(18)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         11637
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.000183
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 49.2 78.0 46.8 19.6 4.74 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1186
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1186
_reflns_limit_h_max              31
_reflns_limit_h_min              -31
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              -23
_reflns_number_gt                8940
_reflns_number_total             11667
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            ic060809ysup1.cif
_cod_data_source_block           14
_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      'C 1 c 1 '
_cod_original_formula_sum        'C40 H50 N6 Ti1'
_cod_database_code               4332759