Chirality and Diastereoselection of Δ/Λ-Configured Tetrahedral Zinc Complexes through Enantiopure Schiff Base Complexes: Combined Vibrational Circular Dichroism, Density Functional Theory, 1H NMR, and X-ray Structural Studies
Anne-Christine Chamayou; Steffen Lüdeke; Volker Brecht; Teresa B. Freedman; Laurence A. Nafie; Christoph Janiak; Inorganic Chemistry 50 (2011) 11363–11374; doi:10.1021/ic2009557

data_4326831
_publ_contact_author_address
;Institut f\"ur Anorganische Chemie und Strukturchemie
Universit\"at D\"usseldorf
Universit\"atsstr. 1
40225 D\"usseldorf
Germany
;
_publ_contact_author_email       janiak@uni-duesseldorf.de
_publ_contact_author_name        'Christoph Janiak'
_publ_contact_author_phone       +49-211-8112286
_publ_section_title
;
 Chirality and Diastereoselection of \D/\L-Configured Tetrahedral Zinc
 Complexes through Enantiopure Schiff Base Complexes: Combined Vibrational
 Circular Dichroism, Density Functional Theory, 1H NMR, and X-ray
 Structural Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11363
_journal_page_last               11374
_journal_paper_doi               10.1021/ic2009557
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C32 H32 N2 O4 Zn'
_chemical_formula_sum            'C32 H32 N2 O4 Zn'
_chemical_formula_weight         573.97
_chemical_name_systematic
; 
\D-Bis{(S)-N-(1-(4-methoxyphenyl)ethyl)salicylaldiminato-
\k^2^N,O}zinc(II) 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.810(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1814(2)
_cell_length_b                   9.9745(2)
_cell_length_c                   17.0287(4)
_cell_measurement_reflns_used    4288
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      21.003
_cell_measurement_theta_min      2.366
_cell_volume                     1389.49(5)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34711
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.9863
_exptl_absorpt_correction_T_min  0.7840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       needle
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6077
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                4647
_reflns_number_total             6077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2009557_si_002_2.cif
_cod_data_source_block           l5znf
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4326831