Spontaneous resolution of a Δ/Λ-chiral-at-metal pseudo-tetrahedral Schiff-base zinc complex to a racemic conglomerate with C–H⋯O organized 41- and 43-helices
Enamullah, Mohammed; Vasylyeva, Vera; Quddus, Mohammad Abdul; Islam, Mohammad Khairul; Höfert, Simon-Patrick; Janiak, Christoph; CrystEngComm 20 (2018) 4724–; doi:10.1039/C8CE00839F

data_7231050
_publ_section_title
;
 Spontaneous resolution of a \D/\L-chiral-at-metal pseudo-tetrahedral
 Schiff-base zinc complex to a racemic conglomerate with C--H&#x22EF;O
 organized 41- and 43-helices
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4724
_journal_paper_doi               10.1039/C8CE00839F
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H18 N4 O2 Zn'
_chemical_formula_sum            'C24 H18 N4 O2 Zn'
_chemical_formula_weight         459.79
_chemical_name_systematic
\L-bis[N-2-(pyridyl)salicylaldiminato-\k^2^N,O]zinc(II)
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-05-20 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8592(4)
_cell_length_b                   9.8592(4)
_cell_length_c                   21.1220(10)
_cell_measurement_reflns_used    9607
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.569
_cell_measurement_theta_min      2.280
_cell_volume                     2053.14(15)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'DIAMOND 4.3.1 (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD area detector'
_diffrn_measurement_method       '\w scans, \f 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  0.0241
_diffrn_reflns_av_unetI/netI     0.0049
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            98864
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.673
_diffrn_reflns_theta_min         2.280
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/dichloromethane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 927 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0160
_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^)+(0.0196P)^2^+0.6280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0442
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2368
_reflns_number_total             2387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00839f2.cif
_cod_data_source_block           mo_SH_ZnS2N_1M_0m_a
_cod_depositor_comments
'Adding full bibliography for 7231045--7231052.cif.'
_cod_original_cell_volume        2053.14(19)
_cod_database_code               7231050
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.749
_shelx_res_checksum              55338