Circularly polarized luminescence and nonlinear optical harmonic generation based on chiral zinc halides.
Han, Xiao; Cheng, Puxin; Han, Wenqing; Shi, Rongchao; Guan, Junjie; Li, Geng; Xu, Jialiang; Chemical communications (Cambridge, England) 59 (2023) 7447–7450; doi:10.1039/d3cc01461d

data_7131696
_publ_section_title
;
 Circularly polarized luminescence and nonlinear optical harmonic
 generation based on chiral zinc halides.
;
_journal_issue                   48
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7447
_journal_page_last               7450
_journal_paper_doi               10.1039/d3cc01461d
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'Cl4 Zn, C5 H14 N2'
_chemical_formula_sum            'C5 H14 Cl4 N2 Zn'
_chemical_formula_weight         309.39
_chemical_name_systematic        S-MP-ZnCl
_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'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-04
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-13 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.02(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.6567(4)
_cell_length_b                   12.1248(4)
_cell_length_c                   16.4859(5)
_cell_measurement_reflns_used    14198
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.2640
_cell_measurement_theta_min      3.7550
_cell_volume                     2330.04(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-beta (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.9930
_diffrn_measured_fraction_theta_max 0.8794
_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    -36.00 -10.00   0.50    2.37    --   -0.30 -37.00   8.00   52
  2  \w     34.00  59.00   0.50    2.37    --   -0.30  37.00 164.00   50
  3  \w    -40.00  23.00   0.50    2.37    --   -0.30 -82.00  30.00  126
  4  \w     -9.00  17.00   0.50    2.37    --   -0.30  57.00 -30.00   52
  5  \w     45.00  88.00   0.50    2.37    --   -0.30  57.00 -30.00   86
  6  \w    -31.00  46.00   0.50    2.37    --   -0.30  77.00-180.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0192210000
_diffrn_orient_matrix_UB_12      0.0555272000
_diffrn_orient_matrix_UB_13      -0.0011431000
_diffrn_orient_matrix_UB_21      -0.0506773000
_diffrn_orient_matrix_UB_22      -0.0169047000
_diffrn_orient_matrix_UB_23      -0.0203853000
_diffrn_orient_matrix_UB_31      -0.0275989000
_diffrn_orient_matrix_UB_32      -0.0074839000
_diffrn_orient_matrix_UB_33      0.0378734000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.9930
_diffrn_reflns_Laue_measured_fraction_max 0.8794
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25218
_diffrn_reflns_point_group_measured_fraction_full 0.9071
_diffrn_reflns_point_group_measured_fraction_max 0.7618
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       plate
_exptl_crystal_F_000             1255.804
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.4484
_refine_diff_density_min         -0.4526
_refine_diff_density_rms         0.0894
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_d_res_high            0.6901
_refine_ls_d_res_low             5.4953
_refine_ls_goodness_of_fit_ref   1.0239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     438
_refine_ls_number_reflns         11317
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0239
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+0.5476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.634
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              22
_reflns_limit_l_min              -22
_reflns_number_gt                10564
_reflns_number_total             11317
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc01461d2.cif
_cod_data_source_block           s-zn-Cl
_cod_depositor_comments
;
Adding full bibliography for 7131695--7131696.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C20 H56 Cl16 N8 Zn4'
_cod_original_formula_weight         1237.545
_cod_original_formula_moiety         '4(Cl4 Zn), 4(C5 H14 N2)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7131696
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.957
 0.043
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C7(H7), C17(H17), C2(H2), C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 N8(H8a,H8b), N4(H4a,H4b), N2(H2a,H2b), N3(H3a,H3b), N1(H1a,H1b), N5(H5c,H5d),
 N6(H6d,H6e), N7(H7a,H7b), C15(H15a,H15b), C5(H5a,H5b), C14(H14a,H14b),
 C10(H10a,H10b), C19(H19a,H19b), C13(H13a,H13b), C4(H4c,H4d), C9(H9a,H9b),
 C20(H20a,H20b), C3(H3c,H3d), C8(H8c,H8d), C18(H18a,H18b)
3.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C16(H16a,H16b,H16c), C11(H11a,H11b,H11c), C1(H1c,H1d,H1e)
;
_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 1.182
_oxdiff_exptl_absorpt_empirical_full_min 0.894