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_1575319
_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         798.51
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-15
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-25 deposited with the CCDC.	2025-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.556(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.8576(5)
_cell_length_b                   7.5452(2)
_cell_length_c                   7.1743(2)
_cell_measurement_reflns_used    4776
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1680
_cell_measurement_theta_min      4.2320
_cell_volume                     1119.25(5)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.962
_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    -27.00  23.00   0.50    0.05    --   47.39 -19.00-180.00  100
  2  \w    -26.00  28.00   0.50    0.05    --   47.39 -19.00  60.00  108
  3  \w     -9.00  27.00   0.50    0.05    --   47.39 -19.00 120.00   72
  4  \w     55.00  90.00   0.50    0.05    --   47.39-122.00 -22.00   70
  5  \w     42.00 107.00   0.50    0.05    --  106.55-122.00 -22.00  130
  6  \w     67.00 110.00   0.50    0.05    --  106.55-125.00  60.00   86
  7  \w     35.00 100.00   0.50    0.05    --  106.55 -95.00 120.00  130
  8  \w     35.00 104.00   0.50    0.05    --  106.55 -95.00 150.00  138
  9  \w     82.00 107.00   0.50    0.05    --  106.55-153.00 177.00   50
 10  \w     76.00 103.00   0.50    0.05    --   47.39-153.00 177.00   54
 11  \w     35.00  72.00   0.50    0.05    --  106.55 -61.00 -30.00   74
 12  \w     42.00  73.00   0.50    0.05    --  106.55 -61.00 -60.00   62
 13  \w     34.00  73.00   0.50    0.05    --  106.55 -61.00   0.00   78
 14  \w     49.00  74.00   0.50    0.05    --  106.55 -61.00  30.00   50
 15  \w    101.00 175.00   0.50    0.05    --  106.55  15.00 -60.00  148
 16  \w     92.00 165.00   0.50    0.05    --  106.55  61.00   0.00  146
 17  \w     99.00 177.00   0.50    0.05    --  106.55  61.00  30.00  156
 18  \w    128.00 174.00   0.50    0.05    --  106.55  45.00 150.00   92
 19  \w     96.00 123.00   0.50    0.05    --  106.55  45.00 150.00   54
 20  \w    123.00 150.00   0.50    0.05    --  106.55 122.00  58.00   54
 21  \w    102.00 128.00   0.50    0.05    --  106.55 153.00-141.00   52
 22  \w     65.00 115.00   0.50    0.05    --   47.39 153.00-141.00  100
 23  \w    -79.00 -46.00   0.50    0.05    -- -104.50 125.00-150.00   66
 24  \w    -92.00 -65.00   0.50    0.05    -- -104.50 153.00-141.00   54
 25  \w    -63.00 -36.00   0.50    0.05    -- -104.50 122.00  58.00   54
 26  \w   -109.00 -68.00   0.50    0.05    -- -104.50 122.00  58.00   82
 27  \w   -132.00 -77.00   0.50    0.05    -- -104.50 160.00 160.31  110
 28  \w     -7.00  19.00   0.50    0.05    --  -47.39  19.00  30.00   52
 29  \w   -132.00-105.00   0.50    0.05    -- -104.50 -77.00 -90.00   54
 30  \w   -164.00-136.00   0.50    0.05    -- -104.50 -77.00 -90.00   56
 31  \w   -174.00-114.00   0.50    0.05    -- -104.50 -30.00-180.00  120
 32  \w   -116.00 -38.00   0.50    0.05    --  -47.39 -57.00-120.00  156
 33  \w   -125.00 -89.00   0.50    0.05    -- -104.50-122.00 -22.00   72
 34  \w   -116.00 -55.00   0.50    0.05    --  -47.39-153.00 177.00  122
;
_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      -0.0141093000
_diffrn_orient_matrix_UB_12      -0.1929467000
_diffrn_orient_matrix_UB_13      0.0518983000
_diffrn_orient_matrix_UB_21      0.0586345000
_diffrn_orient_matrix_UB_22      -0.0631184000
_diffrn_orient_matrix_UB_23      -0.0923555000
_diffrn_orient_matrix_UB_31      0.0437358000
_diffrn_orient_matrix_UB_32      0.0221100000
_diffrn_orient_matrix_UB_33      0.1889261000
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_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            5032
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.408
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17483
_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    2.369
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.080
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details
;
 Flack x determined using 801 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2049
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0601P)^2^+2.7172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.835
_reflns_Friedel_fraction_max     0.767
_reflns_number_gt                2039
_reflns_number_total             2049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5mh01023c2.cif
_cod_data_source_block           S-4Sn
_cod_depositor_comments
'Adding full bibliography for 1575317--1575322.cif.'
_cod_database_code               1575319
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.412
_shelx_estimated_absorpt_t_min   0.099
_reflns_odcompleteness_completeness 99.35
_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:
 C00B(H00N)
2.b Secondary CH2 refined with riding coordinates:
 N005(H00A,H00B), C006(H00C,H00D), C007(H00E,H00F), C008(H00G,H00H), C00A(H00L,
 H00M)
2.c Idealised Me refined as rotating group:
 C009(H00I,H00J,H00K)
;
_shelx_res_checksum              4134
_shelx_hkl_checksum              46109
_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 2.579
_oxdiff_exptl_absorpt_empirical_full_min 0.582