Evaluation of the stereoselectivity for titanium(IV)-based coordination entities induced by the enantiopure diphenylethene-1,2-diamine ligand
Macker, Emilie; Barloy, Laurent; Chaumont, Alain; Kyritsakas, Nathalie; Vincent, Bruno; Henry, Marc; Mobian, Pierre; Inorganica Chimica Acta 498 (2019) 119119–; doi:10.1016/j.ica.2019.119119

data_1565785
_publ_section_title
;
 Evaluation of the stereoselectivity for titanium(IV)-based coordination
 entities induced by the enantiopure diphenylethene-1,2-diamine ligand
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119119
_journal_paper_doi               10.1016/j.ica.2019.119119
_journal_volume                  498
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C112 H84 N4 O8 Ti2, 3(C7 H8) [+ solvent]'
_chemical_formula_sum            'C133 H108 N4 O8 Ti2'
_chemical_formula_weight         1986.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 102.885(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1564(10)
_cell_length_b                   26.3154(12)
_cell_length_c                   21.0515(9)
_cell_measurement_reflns_used    21000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      2.5
_cell_volume                     10885.0(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_unetI/netI     0.1645
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            216090
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.167
_diffrn_reflns_theta_min         1.258
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prism
_exptl_crystal_F_000             4168
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.578
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 10287 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2029
_refine_ls_number_reflns         59807
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.2053
_refine_ls_R_factor_gt           0.1021
_refine_ls_shift/su_max          0.0020
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2778
_refine_ls_wR_factor_ref         0.3446
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                29296
_reflns_number_total             59807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119119.cif
_cod_data_source_block           e3766a_b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1565785
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2014/6