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_7131695
_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         309.35
_chemical_name_systematic        R-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'
_atom_sites_solution_hydrogens   geom
_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                   11.6505(4)
_cell_length_b                   12.1341(4)
_cell_length_c                   16.4837(6)
_cell_measurement_reflns_used    14926
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.2680
_cell_measurement_theta_min      3.8210
_cell_volume                     2330.27(14)
_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  'SHELXL 2018/3 (Sheldrick, 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 0.995
_diffrn_measured_fraction_theta_max 0.887
_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     20.00  55.00   0.50    2.98    --   -0.30  73.00 -47.00   70
  2  \w     33.00  58.00   0.50    2.98    --   -0.30  51.00 165.00   50
  3  \w      7.00  87.00   0.50    2.98    --   -0.30  38.00  30.00  160
  4  \w    -13.00  89.00   0.50    2.98    --   -0.30  38.00 -90.00  204
  5  \w      3.00  47.00   0.50    2.98    --   -0.30  77.00   0.00   88
;
_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      -0.0580003000
_diffrn_orient_matrix_UB_12      0.0177744000
_diffrn_orient_matrix_UB_13      -0.0012008000
_diffrn_orient_matrix_UB_21      0.0136191000
_diffrn_orient_matrix_UB_22      0.0440008000
_diffrn_orient_matrix_UB_23      0.0267351000
_diffrn_orient_matrix_UB_31      0.0125154000
_diffrn_orient_matrix_UB_32      0.0341078000
_diffrn_orient_matrix_UB_33      -0.0337130000
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28131
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.206
_diffrn_reflns_theta_min         3.497
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90771
_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       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 4352 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         12085
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0096P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0478
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_full    0.877
_reflns_Friedel_fraction_max     0.704
_reflns_number_gt                11147
_reflns_number_total             12085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01461d2.cif
_cod_data_source_block           exp_6268
_cod_depositor_comments
;
Adding full bibliography for 7131695--7131696.cif.

2025-03-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C10 H28 Cl8 N4 Zn2'
_cod_original_formula_weight         618.70
_cod_original_formula_moiety         '2(Cl4 Zn), 2(C5 H14 N2)'
_cod_original_formula_units_Z            4
_cod_database_code               7131695
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.587
_shelx_estimated_absorpt_t_min   0.382
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C20(H20), C7(H7), C2(H2), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N6(H6D,H6E), N4(H4A,H4B), N8(H8C,H8D), N1(H1A,H1B), N2(H2A,H2B),
 N5(H5A,H5B), N7(H7A,H7B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C10(H10A,H10B), C012(H01A,H01B), C3(H3C,H3D),
 C12(H12A,H12B), C8(H8A,H8B), C4(H4C,H4D), C9(H9A,H9B)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C1(H1C,H1D,H1E), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              28074
_shelx_hkl_checksum              51765
_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 1.170
_oxdiff_exptl_absorpt_empirical_full_min 0.898