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_7130191
_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         'C46 H36 N2 O2 Zn'
_chemical_formula_sum            'C46 H36 N2 O2 Zn'
_chemical_formula_weight         714.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-18
_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                90
_cell_formula_units_Z            4
_cell_length_a                   8.6225(9)
_cell_length_b                   28.466(2)
_cell_length_c                   14.1674(11)
_cell_measurement_reflns_used    3807
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      29.2170
_cell_measurement_theta_min      2.0180
_cell_volume                     3477.4(5)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_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 0.965
_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    -73.00 110.00   0.50  173.72    --   20.00  54.00-120.00  366
  2  \w    -56.00 -30.00   0.50  173.72    --   20.00  54.00 -90.00   52
  3  \w    -21.00  62.00   0.50  173.72    --   20.00  54.00 -90.00  166
  4  \w     67.00 105.50   0.50  173.72    --   20.00  54.00 -90.00   77
  5  \w      1.00  26.00   0.50  173.72    --   20.00  54.00  60.00   50
  6  \w     46.00  71.00   0.50  173.72    --   20.00  54.00  60.00   50
  7  \w    -73.00 -48.00   0.50  173.72    --   20.00  54.00 -60.00   50
  8  \w    -21.00  24.00   0.50  173.72    --   20.00  54.00 -60.00   90
  9  \w    -55.00  30.00   0.50  173.72    --   20.00  54.00 150.00  170
;
_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      0.0137308000
_diffrn_orient_matrix_UB_12      0.0167960000
_diffrn_orient_matrix_UB_13      -0.0360019000
_diffrn_orient_matrix_UB_21      -0.0022990000
_diffrn_orient_matrix_UB_22      -0.0180804000
_diffrn_orient_matrix_UB_23      -0.0344314000
_diffrn_orient_matrix_UB_31      -0.0810772000
_diffrn_orient_matrix_UB_32      0.0033688000
_diffrn_orient_matrix_UB_33      -0.0051866000
_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  0.1916
_diffrn_reflns_av_unetI/netI     0.3574
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31897
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.471
_diffrn_reflns_theta_min         2.028
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70332
_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    1.364
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_preparation       CH2Cl2/EtOH
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 899 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         10053
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.3027
_refine_ls_R_factor_gt           0.1377
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+3.1994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                4002
_reflns_number_total             10053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01959k2.cif
_cod_data_source_block           exp_417
_cod_database_code               7130191
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C46H36N2O2Zn
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Rigid bond restraints
 C00I, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C00I \\sim N2: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 1.7A
4.a Ternary CH refined with riding coordinates:
 C22(H22), C010(H010)
4.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C00C(H00C), C00D(H00D), C00E(H00E), C00H(H00H), C00I(H00I),
 C00J(H00J), C00L(H00L), C00M(H00M), C00N(H00N), C00P(H00P), C00R(H00R),
 C00V(H00V), C00W(H00W), C00Z(H00Z), C012(H012), C013(H013), C015(H015),
 C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B),
 C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F)
4.c Idealised Me refined as rotating group:
 C00U(H00A,H00B,H00F), C00Y(H00G,H00K,H00O)
;
_shelx_res_checksum              38159
_shelx_hkl_checksum              15374
_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 1.327
_oxdiff_exptl_absorpt_empirical_full_min 0.267