(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_1563821
_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 rmad
_chemical_formula_moiety         'C32 H30 N2 O6 Si, 2(C H Cl3)'
_chemical_formula_sum            'C34 H32 Cl6 N2 O6 Si'
_chemical_formula_weight         805.40
_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   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5325(3)
_cell_length_b                   10.0173(4)
_cell_length_c                   37.6713(15)
_cell_measurement_reflns_used    30852
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.10
_cell_volume                     3597.2(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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      203(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            26633
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.833
_diffrn_reflns_theta_min         2.104
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.9175
_exptl_absorpt_correction_T_min  0.7393
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1974 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_coef       0.0044(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7376
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+4.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.950
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                5870
_reflns_number_total             7376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bg734_3.cif
_cod_data_source_block           bg734_3
_cod_database_code               1563821
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              6865
_shelx_hkl_checksum              72768