Synthesis, X-ray, and Spectroscopic Study of Dissymmetric Tetrahedral Zinc(II) Complexes from Chiral Schiff Base Naphthaldiminate Ligands with Apparent Exception to the ECD Exciton Chirality.
Enamullah, Mohammed; Makhloufi, Gamall; Ahmed, Rifat; Joy, Baitul Alif; Islam, Mohammad Ariful; Padula, Daniele; Hunter, Howard; Pescitelli, Gennaro; Janiak, Christoph; Inorganic chemistry 55 (2016) 6449–6464; doi:10.1021/acs.inorgchem.6b00403

data_4347613
_publ_section_title
;
 Synthesis, X-ray, and Spectroscopic Study of Dissymmetric Tetrahedral
 Zinc(II) Complexes from Chiral Schiff Base Naphthaldiminate Ligands with
 Apparent Exception to the ECD Exciton Chirality.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6449
_journal_page_last               6464
_journal_paper_doi               10.1021/acs.inorgchem.6b00403
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C40 H36 N2 O4 Zn'
_chemical_formula_sum            'C40 H36 N2 O4 Zn'
_chemical_formula_weight         674.08
_chemical_name_systematic
;
bis{(S)-N-(p-methoxphenyl)ethyl-2-oxo-1-naphthaldiminato-\k^2^N,O}zinc(II)
;
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.771(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0424(8)
_cell_length_b                   18.9648(13)
_cell_length_c                   15.3577(10)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.986
_cell_measurement_theta_min      2.167
_cell_volume                     3320.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2 (Crystal Impact, 2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL2014 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41002
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.191
_diffrn_reflns_theta_min         1.765
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.9544
_exptl_absorpt_correction_T_min  0.7192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 6100 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         17758
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0364
_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^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                14875
_reflns_number_total             17758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Zn-2S.cif
_cod_data_source_block           znr29
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4347613
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2013-2
_shelx_res_checksum              60353
_shelx_hkl_checksum              80316