(S)-N-[(2-hydroxynaphthalen-1-yl)methylidene]valine ‒ A valuable ligand for the preparation of chiral complexes
Schwarzer, Sandra; Böhme, Uwe; Fels, Sabine; Günther, Betty; Brendler, Erica; Inorganica Chimica Acta 483 (2018) 136–147; doi:10.1016/j.ica.2018.08.011

data_1563822
_publ_section_title
;
 (S)-N-[(2-hydroxynaphthalen-1-yl)methylidene]valine -- A valuable ligand
 for the preparation of chiral complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              136
_journal_page_last               147
_journal_paper_doi               10.1016/j.ica.2018.08.011
_journal_volume                  483
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H25 N O3 Si, C H Cl3'
_chemical_formula_sum            'C29 H26 Cl3 N O3 Si'
_chemical_formula_weight         570.95
_chemical_melting_point          383
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7871(2)
_cell_length_b                   10.8431(2)
_cell_length_c                   25.8544(6)
_cell_measurement_reflns_used    8571
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      2.22
_cell_volume                     2743.73(10)
_computing_cell_refinement       'SMART (Bruker, 2007) '
_computing_data_collection       'SMART (Bruker, 2007) '
_computing_data_reduction        'SAINT (Bruker, 2007) '
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            18777
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.452
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.8699
_exptl_absorpt_correction_T_min  0.8244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 2453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.6905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6000
_reflns_number_total             6606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            k21FF_2.cif
_cod_data_source_block           k21FF_2
_cod_database_code               1563822
_shelx_res_checksum              80284
_shelx_hkl_checksum              47588