Regulation of metal valence states for enhancing second harmonic generation performance of chiral tin halides.
Wang, Yue; Cheng, Puxin; Han, Wenqing; Guan, Junjie; Li, Quanwen; Wang, Zhihua; Wang, Peihan; Zheng, Yongshen; Xu, Jialiang; Materials horizons 12 (2025) 9106–9113; doi:10.1039/d5mh01023c

data_1575321
_publ_section_title
;
 Regulation of metal valence states for enhancing second harmonic
 generation performance of chiral tin halides.
;
_journal_issue                   21
_journal_name_full               'Materials horizons'
_journal_page_first              9106
_journal_page_last               9113
_journal_paper_doi               10.1039/d5mh01023c
_journal_volume                  12
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Br6 Sn, 2(C6 H14 N)'
_chemical_formula_sum            'C12 H28 Br6 N2 Sn'
_chemical_formula_weight         798.501
_chemical_name_systematic        A2SnBr6
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_Int_Tables_number      5
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-06
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2025-06-02 deposited with the CCDC.	2025-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.444(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.8205(4)
_cell_length_b                   7.5406(2)
_cell_length_c                   7.1670(1)
_cell_measurement_reflns_used    5423
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2570
_cell_measurement_theta_min      4.2770
_cell_volume                     1115.73(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9666
_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    136.00 162.00   0.50    0.05    --  106.55  77.00   0.00   52
  2  \w     84.00 109.00   0.50    0.05    --  106.55  77.00   0.00   50
  3  \w     84.00 110.00   0.50    0.05    --  106.55  77.00 -60.00   52
  4  \w    100.00 126.00   0.50    0.05    --  106.55  45.00 -60.00   52
  5  \w    117.00 143.00   0.50    0.05    --  106.55  38.00-108.00   52
  6  \w     61.00 119.00   0.50    0.05    --   47.89  38.00-108.00  116
  7  \w     40.00 106.00   0.50    0.05    --  106.55 -77.00  30.00  132
  8  \w     36.00  75.00   0.50    0.05    --  106.55 -61.00 -30.00   78
  9  \w     34.00  60.00   0.50    0.05    --  106.55 -61.00 -60.00   52
 10  \w     38.00 105.00   0.50    0.05    --  106.55 -95.00-180.00  134
 11  \w     40.00  70.00   0.50    0.05    --  106.55-125.00  30.00   60
 12  \w     43.00  99.00   0.50    0.05    --  106.55 -95.00 120.00  112
 13  \w    -22.00  39.00   0.50    0.05    --   47.89 -38.00  96.00  122
 14  \w    -26.00  -1.00   0.50    0.05    --   47.89 -19.00 120.00   50
 15  \w    -25.00  24.00   0.50    0.05    --   47.89 -19.00 -60.00   98
 16  \w    -81.00 -36.00   0.50    0.05    --  -47.89 -57.00   0.00   90
 17  \w    -62.00 -25.00   0.50    0.05    --  -47.89 -77.00 -60.00   74
 18  \w    -70.00 -33.00   0.50    0.05    --  -47.89 -57.00 -60.00   74
 19  \w    -93.00 -68.00   0.50    0.05    --  -47.89 -77.00 -60.00   50
 20  \w   -116.00 -90.00   0.50    0.05    --  -47.89 -57.00 -60.00   52
 21  \w   -121.00 -95.00   0.50    0.05    --  -47.89 -38.00  96.00   52
 22  \w   -107.00 -82.00   0.50    0.05    -- -104.50 -77.00   0.00   50
 23  \w   -122.00 -91.00   0.50    0.05    -- -104.50 -61.00   0.00   62
 24  \w   -170.00-141.00   0.50    0.05    -- -104.50 -61.00  30.00   58
 25  \w   -174.00-148.00   0.50    0.05    -- -104.50 -61.00   0.00   52
 26  \w   -173.00-147.00   0.50    0.05    -- -104.50 -61.00  14.78   52
 27  \w   -165.00-139.00   0.50    0.05    -- -104.50 -62.00 -49.19   52
 28  \w   -114.00 -89.00   0.50    0.05    -- -104.50 -62.00 -49.19   50
 29  \w   -115.00 -90.00   0.50    0.05    -- -104.50 -61.00 -30.00   50
 30  \w   -115.00 -90.00   0.50    0.05    -- -104.50 -55.00  -0.72   50
 31  \w   -114.00 -88.00   0.50    0.05    -- -104.50 -61.00  14.78   52
 32  \w   -115.00 -90.00   0.50    0.05    -- -104.50 -56.00  13.68   50
 33  \w   -115.00 -90.00   0.50    0.05    -- -104.50 -54.00  41.49   50
 34  \w   -126.00 -89.00   0.50    0.05    -- -104.50 -61.00  30.00   74
 35  \w   -120.00 -95.00   0.50    0.05    -- -104.50 -51.00 -33.20   50
 36  \w   -118.00 -92.00   0.50    0.05    -- -104.50 -45.00 -60.00   52
 37  \w   -117.00 -92.00   0.50    0.05    -- -104.50 -45.00 -30.00   50
 38  \w   -124.00 -93.00   0.50    0.05    -- -104.50 -46.00   6.13   62
 39  \w   -129.00 -92.00   0.50    0.05    -- -104.50 -30.00  30.00   74
 40  \w   -137.00 -92.00   0.50    0.05    -- -104.50 -38.00  96.00   90
 41  \w   -173.00-133.00   0.50    0.05    -- -104.50 -54.00  41.49   80
 42  \w   -167.00-104.00   0.50    0.05    -- -104.50 -30.00 -90.00  126
 43  \w    -63.00 -37.00   0.50    0.05    -- -104.50  61.00-120.00   52
 44  \w    -68.00 -33.00   0.50    0.05    -- -104.50  61.00 -90.00   70
 45  \w    -62.00 -35.00   0.50    0.05    -- -104.50  61.00 -60.00   54
 46  \w    -40.00  15.00   0.50    0.05    --  -47.89  38.00-108.00  110
 47  \w    -67.00 -41.00   0.50    0.05    -- -104.50  61.00  30.00   52
 48  \w    -59.00 -33.00   0.50    0.05    -- -104.50  61.00  60.00   52
 49  \w    -64.00 -32.00   0.50    0.05    -- -104.50  61.00 120.00   64
 50  \w    -20.00   6.00   0.50    0.05    --  -47.89  19.00  60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0046110000
_diffrn_orient_matrix_UB_12      0.0990320000
_diffrn_orient_matrix_UB_13      -0.1858459000
_diffrn_orient_matrix_UB_21      -0.0741610000
_diffrn_orient_matrix_UB_22      -0.0107836000
_diffrn_orient_matrix_UB_23      -0.0492294000
_diffrn_orient_matrix_UB_31      -0.0069432000
_diffrn_orient_matrix_UB_32      0.1783542000
_diffrn_orient_matrix_UB_33      0.1001537000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.9982
_diffrn_reflns_Laue_measured_fraction_max 0.9666
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6296
_diffrn_reflns_point_group_measured_fraction_full 0.9595
_diffrn_reflns_point_group_measured_fraction_max 0.9105
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.25
_diffrn_reflns_theta_min         4.28
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.663
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.377
_exptl_crystal_description       block
_exptl_crystal_F_000             741.460
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.7403
_refine_diff_density_min         -1.4634
_refine_diff_density_rms         0.2254
_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   -0.003(7)
_refine_ls_d_res_high            0.7937
_refine_ls_d_res_low             10.3225
_refine_ls_goodness_of_fit_ref   0.9421
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    21
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2127
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.9421
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+0.2538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.845
_reflns_limit_h_max              25
_reflns_limit_h_min              -26
_reflns_limit_k_max              9
_reflns_limit_k_min              -9
_reflns_limit_l_max              8
_reflns_limit_l_min              -8
_reflns_number_gt                2086
_reflns_number_total             2127
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5mh01023c2.cif
_cod_data_source_block           R-4Sn
_cod_depositor_comments
'Adding full bibliography for 1575317--1575322.cif.'
_cod_original_sg_symbol_Hall     ' C 2y'
_cod_database_code               1575321
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C00A(H00k)
2.b Secondary CH2 refined with riding coordinates:
 C006(H00c,H00d), C007(H00e,H00f), C008(H00g,H00h), C009(H00i,H00j), N005(H00a,
 H00b)
2.c Idealised Me refined as rotating group:
 C00B(H00l,H00m,H00n)
;
_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 3.315
_oxdiff_exptl_absorpt_empirical_full_min 0.736