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_1575320
_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         'Br3 Sn, Br, 2(C6 H14 N)'
_chemical_formula_sum            'C12 H28 Br4 N2 Sn'
_chemical_formula_weight         638.69
_chemical_name_systematic        A2SnBr4
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.34120(10)
_cell_length_b                   12.04860(10)
_cell_length_c                   25.9872(2)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.5980
_cell_measurement_theta_min      4.0330
_cell_volume                     1985.49(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  '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 1.000
_diffrn_measured_fraction_theta_max 0.977
_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     -5.00  27.00   0.50    0.05    --   47.80 -40.00 -72.00   64
  2  \w     44.00  70.00   0.50    0.05    --  106.64 -61.00 -90.00   52
  3  \w    117.00 178.00   0.50    0.05    --  106.64  15.00 150.00  122
  4  \w     41.00 104.00   0.50    0.05    --  106.64 -77.00 150.00  126
  5  \w     57.00  82.00   0.50    0.05    --  106.64-125.00  90.00   50
  6  \w     46.00  79.00   0.50    0.05    --  106.64 -95.00 120.00   66
  7  \w     36.00  93.00   0.50    0.05    --  106.64 -94.00  82.00  114
  8  \w    -21.00  76.00   0.50    0.05    --   47.80 -94.00  82.00  194
  9  \w    -21.00  12.00   0.50    0.05    --  -47.80  19.00-150.00   66
 10  \w    -68.00 -35.00   0.50    0.05    -- -104.50  61.00 -60.00   66
 11  \w    -68.00 -39.00   0.50    0.05    -- -104.50  61.00-150.00   58
 12  \w     -4.00  21.00   0.50    0.05    --  -47.80  19.00 -60.00   50
 13  \w    -65.00 -34.00   0.50    0.05    -- -104.50  61.00 120.00   62
 14  \w    -65.00 -36.00   0.50    0.05    -- -104.50 125.00   0.00   58
 15  \w   -110.00 -81.00   0.50    0.05    -- -104.50 125.00   0.00   58
 16  \w   -104.00 -78.00   0.50    0.05    -- -104.50  97.00 -70.00   52
 17  \w    -60.00 -34.00   0.50    0.05    -- -104.50  97.00 -70.00   52
 18  \w   -174.00 -96.00   0.50    0.05    -- -104.50 -40.00 -72.00  156
 19  \w   -164.00 -96.00   0.50    0.05    -- -104.50 -45.00 120.00  136
;
_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      0.1666087000
_diffrn_orient_matrix_UB_12      -0.0641316000
_diffrn_orient_matrix_UB_13      -0.0312908000
_diffrn_orient_matrix_UB_21      -0.1520272000
_diffrn_orient_matrix_UB_22      -0.0048076000
_diffrn_orient_matrix_UB_23      -0.0462164000
_diffrn_orient_matrix_UB_31      0.0900123000
_diffrn_orient_matrix_UB_32      0.1105086000
_diffrn_orient_matrix_UB_33      -0.0200580000
_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  0.0210
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.827
_diffrn_reflns_theta_min         4.044
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43922
_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 reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 1608 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(2)
_refine_ls_extinction_coef       0.00057(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0165
_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^)+(0.0265P)^2^+0.9800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0444
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                3987
_reflns_number_total             3997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5mh01023c2.cif
_cod_data_source_block           S-2Sn
_cod_depositor_comments
'Adding full bibliography for 1575317--1575322.cif.'
_cod_database_code               1575320
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.441
_reflns_odcompleteness_completeness 99.90
_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(H00S), C00G(H00I)
2.b Secondary CH2 refined with riding coordinates:
 N006(H00A,H00B), N007(H00O,H00P), C008(H00C,H00D), C009(H00Q,H00R), C00A(H00E,
 H00F), C00C(H00T,H00U), C00D(H00G,H00H), C00E(H00V,H00W), C00F(H00X,H00Y),
 C00I(H00M,H00N)
2.c Idealised Me refined as rotating group:
 C00H(H00J,H00K,H00L), C00J(H00Z,H,HA)
;
_shelx_res_checksum              41662
_shelx_hkl_checksum              43478
_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 1.598
_oxdiff_exptl_absorpt_empirical_full_min 0.752