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_1575318
_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_formula_moiety         'Br3 Sn, C6 H14 N'
_chemical_formula_sum            'C6 H14 Br3 N Sn'
_chemical_formula_weight         458.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-07-16
_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                 102.233(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.84820(10)
_cell_length_b                   8.29350(10)
_cell_length_c                   15.0756(2)
_cell_measurement_reflns_used    6479
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.5610
_cell_measurement_theta_min      2.9930
_cell_volume                     1203.36(3)
_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 2018/2 (Sheldrick, 2018)'
_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 0.998
_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     77.00 107.00   0.50    0.05    --  106.67-125.00-150.00   60
  2  \w     51.00  95.00   0.50    0.05    --  106.67 -95.00-120.00   88
  3  \w    -38.00  20.00   0.50    0.05    --  -47.76  38.00  60.00  116
  4  \w    -17.00  20.00   0.50    0.05    --  -47.76  33.00 -85.00   74
  5  \w    -15.00  23.00   0.50    0.05    --  -47.76  19.00-120.00   76
  6  \w    -66.00 -40.00   0.50    0.05    -- -104.50  61.00 -90.00   52
  7  \w    -88.00 -42.00   0.50    0.05    -- -104.50  77.00 -30.00   92
  8  \w   -121.00 -35.00   0.50    0.05    --  -47.76 -33.00 116.00  172
  9  \w   -125.00 -98.00   0.50    0.05    -- -104.50 -33.00 116.00   54
 10  \w     39.00  74.00   0.50    0.05    --  106.67 -61.00-180.00   70
 11  \w     38.00  74.00   0.50    0.05    --  106.67 -61.00-120.00   72
 12  \w     45.00  70.00   0.50    0.05    --  106.67 -61.00 -30.00   50
 13  \w     38.00  63.00   0.50    0.05    --  106.67 -61.00   0.00   50
 14  \w     34.00  67.00   0.50    0.05    --  106.67 -61.00 120.00   66
 15  \w     36.00  74.00   0.50    0.05    --  106.67 -61.00 150.00   76
 16  \w     51.00 106.00   0.50    0.05    --  106.67 -77.00  90.00  110
 17  \w    -16.00   9.00   0.50    0.05    --   47.76 -33.00 116.00   50
 18  \w     39.00  73.00   0.50    0.05    --  106.67 -61.00 -60.00   68
 19  \w     42.00  67.00   0.50    0.05    --  106.67 -61.00 -90.00   50
 20  \w     38.00  67.00   0.50    0.05    --  106.67 -61.00-150.00   58
 21  \w     98.00 178.00   0.50    0.05    --  106.67  33.00 -85.00  160
 22  \w    147.00 176.00   0.50    0.05    --  106.67 125.00 150.00   58
 23  \w    101.00 126.00   0.50    0.05    --  106.67 125.00 150.00   50
 24  \w     42.00 107.00   0.50    0.05    --   47.76  33.00 -85.00  130
;
_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      0.0373302000
_diffrn_orient_matrix_UB_12      -0.0757601000
_diffrn_orient_matrix_UB_13      0.0953945000
_diffrn_orient_matrix_UB_21      -0.1556208000
_diffrn_orient_matrix_UB_22      -0.0208223000
_diffrn_orient_matrix_UB_23      -0.0006329000
_diffrn_orient_matrix_UB_31      0.0025174000
_diffrn_orient_matrix_UB_32      -0.1683106000
_diffrn_orient_matrix_UB_33      -0.0428602000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7444
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.339
_diffrn_reflns_theta_min         4.927
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    28.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31140
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.531
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.221
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2435
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0416P)^2^+12.8894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2389
_reflns_number_total             2435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5mh01023c2.cif
_cod_data_source_block           rac-2Sn
_cod_depositor_comments
'Adding full bibliography for 1575317--1575322.cif.'
_cod_database_code               1575318
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.333
_shelx_estimated_absorpt_t_min   0.165
_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,H,H,H) groups
2. Restrained distances
 C8-C7 \\sim C9-C7 \\sim C9-C10 \\sim C11-C10
 with sigma of 0.02
 N2-C8 \\sim N2-C11
 with sigma of 0.02
3. Rigid bond restraints
 N2, C8, C7, C9, C10, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C8 \\sim C7 \\sim C9 \\sim C10 \\sim N2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C11) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
5. Others
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(N2)=Sof(H2A)=Sof(H2B)=Sof(C7)=Sof(H7)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2)=
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C7(H7)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), N2(H2A,H2B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
6.c Idealised Me refined as rotating group:
 C1(H1AA,H1AB,H1AC), C1(H1BD,H1BE,H1BF)
;
_shelx_res_checksum              93678
_shelx_hkl_checksum              17826
_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 2.169
_oxdiff_exptl_absorpt_empirical_full_min 0.701