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_4326830
_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         'C30 H26 Br2 N2 O2 Zn'
_chemical_formula_sum            'C30 H26 Br2 N2 O2 Zn'
_chemical_formula_weight         671.72
_chemical_name_systematic
; 
\L-Bis{(R)-N-(1-(4-bromophenyl)ethyl)salicylaldiminato-
\k^2^N,O}zinc(II) 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.064(2)
_cell_length_b                   10.522(2)
_cell_length_c                   26.340(5)
_cell_measurement_reflns_used    3620
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      21.753
_cell_measurement_theta_min      2.478
_cell_volume                     2789.2(9)
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16969
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    3.775
_exptl_absorpt_correction_T_max  0.9115
_exptl_absorpt_correction_T_min  0.2779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0141P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                4480
_reflns_number_total             5995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2009557_si_002_1.cif
_cod_data_source_block           l11znf
_cod_original_cell_volume        2789.4(10)
_cod_database_code               4326830