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_1575317
_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         'Br6 Sn, C12 H28 N2'
_chemical_formula_sum            'C12 H28 Br6 N2 Sn'
_chemical_formula_weight         798.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-25
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2025-07-25 deposited with the CCDC.	2025-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.696(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.8427(7)
_cell_length_b                   7.5744(2)
_cell_length_c                   7.1881(3)
_cell_measurement_reflns_used    4014
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4680
_cell_measurement_theta_min      4.2790
_cell_volume                     1124.57(7)
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.967
_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    -65.00 -38.00   0.50    0.05    -- -104.50  61.00  90.00   54
  2  \w    -39.00  -7.00   0.50    0.05    --  -47.39  38.00 150.00   64
  3  \w    -37.00  14.00   0.50    0.05    --  -47.39  38.00  60.00  102
  4  \w    -68.00 -33.00   0.50    0.05    -- -104.50  61.00 -60.00   70
  5  \w    -67.00 -35.00   0.50    0.05    -- -104.50  61.00 -90.00   64
  6  \w     -8.00  19.00   0.50    0.05    --  -47.39  19.00-120.00   54
  7  \w    -56.00  24.00   0.50    0.05    --  -47.39  81.00 -58.00  160
  8  \w    -66.00 -39.00   0.50    0.05    -- -104.50  81.00 -58.00   54
  9  \w    133.00 176.00   0.50    0.05    --  105.93  30.00 -90.00   86
 10  \w    130.00 178.00   0.50    0.05    --  105.93  15.00-120.00   96
 11  \w     96.00 126.00   0.50    0.05    --  105.93  30.00 -90.00   60
 12  \w    115.00 176.00   0.50    0.05    --  105.93  61.00   0.00  122
 13  \w   -105.00 -26.00   0.50    0.05    --  -47.39 -77.00 120.00  158
 14  \w    -22.00   7.00   0.50    0.05    --   47.39 -19.00  30.00   58
 15  \w     33.00  69.00   0.50    0.05    --  105.93 -61.00 -30.00   72
 16  \w     85.00 173.00   0.50    0.05    --  105.93 125.00  60.00  176
 17  \w     90.00 176.00   0.50    0.05    --  105.93  81.00 -58.00  172
 18  \w     38.00  68.00   0.50    0.05    --  105.93 -61.00  60.00   60
 19  \w     40.00  65.00   0.50    0.05    --  105.93 -61.00  90.00   50
 20  \w    -14.00  66.00   0.50    0.05    --   47.39 -81.00 179.00  160
 21  \w     53.00  95.00   0.50    0.05    --  105.93 -81.00 179.00   84
 22  \w     61.00  95.00   0.50    0.05    --  105.93-125.00   0.00   68
 23  \w     65.00 107.00   0.50    0.05    --  105.93-125.00 -60.00   84
 24  \w     37.00 111.00   0.50    0.05    --  105.93-125.00-180.00  148
 25  \w   -161.00 -92.00   0.50    0.05    -- -104.50 -15.00  60.00  138
 26  \w   -172.00-135.00   0.50    0.05    -- -104.50 -45.00 120.00   74
 27  \w   -131.00 -93.00   0.50    0.05    -- -104.50 -45.00 120.00   76
 28  \w   -144.00-119.00   0.50    0.05    -- -104.50 -30.00  60.00   50
 29  \w   -169.00-120.00   0.50    0.05    -- -104.50 -61.00-120.00   98
 30  \w   -115.00 -90.00   0.50    0.05    -- -104.50 -61.00-120.00   50
 31  \w   -163.00 -95.00   0.50    0.05    -- -104.50 -61.00  60.00  136
 32  \w   -151.00-126.00   0.50    0.05    -- -104.50 -81.00 179.00   50
;
_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      0.0232978000
_diffrn_orient_matrix_UB_12      0.0867206000
_diffrn_orient_matrix_UB_13      0.1909263000
_diffrn_orient_matrix_UB_21      0.0296751000
_diffrn_orient_matrix_UB_22      0.1531611000
_diffrn_orient_matrix_UB_23      -0.1009089000
_diffrn_orient_matrix_UB_31      -0.0643451000
_diffrn_orient_matrix_UB_32      0.1019664000
_diffrn_orient_matrix_UB_33      -0.0109836000
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       24
_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       -8
_diffrn_reflns_number            5356
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.682
_diffrn_reflns_theta_min         4.281
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40811
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.358
_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         1.201
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0685P)^2^+1.4499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1137
_reflns_number_total             1219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5mh01023c2.cif
_cod_data_source_block           rac-4Sn
_cod_depositor_comments
'Adding full bibliography for 1575317--1575322.cif.'
_cod_database_code               1575317
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.413
_shelx_estimated_absorpt_t_min   0.099
_reflns_odcompleteness_completeness 99.09
_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. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5) H1E(0.5) C2(0.5) H2(0.5)
 H3A(0.5) H3B(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) H6A(0.5) H6B(0.5)
3.a Ternary CH refined with riding coordinates:
 C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_shelx_res_checksum              78294
_shelx_hkl_checksum              49730
_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 2.294
_oxdiff_exptl_absorpt_empirical_full_min 0.582