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_1575322
_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         638.694
_chemical_name_systematic        R2SnBr4
_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'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-26
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3457(1)
_cell_length_b                   12.0368(2)
_cell_length_c                   25.9787(4)
_cell_measurement_reflns_used    8827
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.7280
_cell_measurement_theta_min      3.4110
_cell_volume                     1984.30(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  '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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9744
_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    -62.00 -35.00   0.50    0.05    -- -104.50  61.00-180.00   54
  2  \w    -66.00 -40.00   0.50    0.05    -- -104.50  61.00 -30.00   52
  3  \w    -80.00 -42.00   0.50    0.05    -- -104.50  69.00  19.00   76
  4  \w     -9.00  28.00   0.50    0.05    --  -47.91  19.00-180.00   74
  5  \w    -23.00  25.00   0.50    0.05    --  -47.91  19.00   0.00   96
  6  \w    -65.00 -34.00   0.50    0.05    -- -104.50  61.00  60.00   62
  7  \w    -64.00 -39.00   0.50    0.05    -- -104.50  61.00  30.00   50
  8  \w   -173.00-118.00   0.50    0.05    -- -104.50 -15.00 -60.00  110
  9  \w   -174.00-130.00   0.50    0.05    -- -104.50 -30.00   0.00   88
 10  \w   -121.00 -96.00   0.50    0.05    -- -104.50 -30.00   0.00   50
 11  \w   -117.00 -90.00   0.50    0.05    -- -104.50 -53.00  42.00   54
 12  \w    -23.00   6.00   0.50    0.05    --   47.91 -19.00-120.00   58
 13  \w     34.00  62.00   0.50    0.05    --  106.52 -53.00  42.00   56
 14  \w     36.00  87.00   0.50    0.05    --  106.52 -77.00 -30.00  102
 15  \w     36.00  74.00   0.50    0.05    --  106.52 -69.00-113.00   76
 16  \w     35.00  66.00   0.50    0.05    --  106.52 -61.00-180.00   62
 17  \w     35.00 120.00   0.50    0.05    --   47.91  53.00-172.00  170
 18  \w     97.00 165.00   0.50    0.05    --  106.52  30.00 150.00  136
 19  \w     55.00  83.00   0.50    0.05    --  106.52-116.00 171.00   56
 20  \w     81.00 111.00   0.50    0.05    --  106.52-125.00  90.00   60
 21  \w     38.00  68.00   0.50    0.05    --  106.52-125.00  90.00   60
;
_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      0.0665053000
_diffrn_orient_matrix_UB_12      0.0682657000
_diffrn_orient_matrix_UB_13      0.0474495000
_diffrn_orient_matrix_UB_21      -0.1415506000
_diffrn_orient_matrix_UB_22      -0.0729265000
_diffrn_orient_matrix_UB_23      0.0343985000
_diffrn_orient_matrix_UB_31      0.1856595000
_diffrn_orient_matrix_UB_32      -0.0799910000
_diffrn_orient_matrix_UB_33      0.0091239000
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9744
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11071
_diffrn_reflns_point_group_measured_fraction_full 0.9994
_diffrn_reflns_point_group_measured_fraction_max 0.9559
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.92
_diffrn_reflns_theta_min         3.40
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62026
_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    2.138
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208.161
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.3706
_refine_diff_density_min         -0.4705
_refine_diff_density_rms         0.0954
_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   -0.016(3)
_refine_ls_d_res_high            0.7914
_refine_ls_d_res_low             12.9894
_refine_ls_goodness_of_fit_ref   1.0232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0232
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+1.5631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0438
_reflns_Friedel_coverage         0.930
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              32
_reflns_limit_l_min              -32
_reflns_number_gt                3894
_reflns_number_total             3989
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5mh01023c2.cif
_cod_data_source_block           R-2Sn
_cod_depositor_comments
'Adding full bibliography for 1575317--1575322.cif.'
_cod_original_cell_volume        1984.30(6)
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               1575322
_reflns_odcompleteness_completeness 99.95
_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:
 C008(H008), C00H(H00z)
2.b Secondary CH2 refined with riding coordinates:
 C009(H00c,H00d), C00A(H00p,H00q), C00B(H00r,H00s), C00C(H00e,H00f), C00D(H00t,
 H00u), C00F(H00g,H00h), C00G(H00y,H), C00I(H00i,H00j), N006(H00a,H00b),
 N007(H00n,H00o)
2.c Idealised Me refined as rotating group:
 C00E(H00v,H00w,H00x), C00J(H00k,H00l,H00m)
;
_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.806