Sign control of circularly polarized luminescence of chiral Schiff-base Zn(II) complexes through coordination geometry changes
Ikeshita, Masahiro; Mizugaki, Momo; Ishikawa, Takahiro; Matsudaira, Kana; Kitahara, Maho; Imai, Yoshitane; Tsuno, Takashi; Chemical Communications  (2022) –; doi:10.1039/D2CC01959K

data_7130190
_publ_section_title
;
 Sign control of circularly polarized luminescence of chiral Schiff-base
 Zn(II) complexes through coordination geometry changes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01959K
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H16 N O Zn0.5'
_chemical_formula_sum            'C19 H16 N O Zn0.5'
_chemical_formula_weight         307.01
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-24 deposited with the CCDC.	2022-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.6028(2)
_cell_length_b                   8.6028(2)
_cell_length_c                   34.6337(8)
_cell_measurement_reflns_used    11776
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      27.1670
_cell_measurement_theta_min      2.7200
_cell_volume                     2219.78(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'Rigaku HyPix-3000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -71.00  96.00   0.50   21.82    --   20.00  54.00 -90.00  334
  2  \w    -74.00  71.00   0.50   21.82    --   20.00  54.00-180.00  290
  3  \w    -71.00  -3.00   0.50   21.82    --   20.00  54.00  30.00  136
  4  \w      4.00  66.00   0.50   21.82    --   20.00  54.00  30.00  124
  5  \w    -69.00 -44.00   0.50   21.82    --   20.00  54.00-120.00   50
  6  \w    -18.00   7.00   0.50   21.82    --   20.00  54.00-120.00   50
  7  \w     70.00  99.00   0.50   21.82    --   20.00  54.00-120.00   58
  8  \w    -23.00   6.00   0.50   21.82    --   20.00  54.00  60.00   58
  9  \w     50.00  85.00   0.50   21.82    --   20.00  54.00  60.00   70
 10  \w      0.00  25.00   0.50   21.82    --   20.00  54.00-150.00   50
 11  \w    -49.00 101.00   0.50   21.82    --   20.00  54.00 -30.00  300
;
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0377122000
_diffrn_orient_matrix_UB_12      0.0051122000
_diffrn_orient_matrix_UB_13      -0.0178334000
_diffrn_orient_matrix_UB_21      0.0610754000
_diffrn_orient_matrix_UB_22      -0.0181918000
_diffrn_orient_matrix_UB_23      -0.0100180000
_diffrn_orient_matrix_UB_31      -0.0625700000
_diffrn_orient_matrix_UB_32      -0.0933255000
_diffrn_orient_matrix_UB_33      0.0009546000
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            30053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.473
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_preparation       toluene/MeOH
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0283P)^2^+0.5351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                3975
_reflns_number_total             4401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01959k2.cif
_cod_data_source_block           exp_534
_cod_original_cell_volume        2219.78(12)
_cod_original_formula_sum        'C19 H16 N O Zn0.50'
_cod_database_code               7130190
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H32N2O2Zn
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00B(H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C004(H004), C008(H008), C00A(H00A), C00C(H00C), C00D(H00D), C00E(H00E),
 C00F(H00F), C00I(H00J), C00J(H00K), C00K(H00L), C00L(H00M), C00M(H00N)
2.c Idealised Me refined as rotating group:
 C00H(H00G,H00H,H00I)
;
_shelx_res_checksum              23150
_shelx_hkl_checksum              95192
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.118
_oxdiff_exptl_absorpt_empirical_full_min 0.919