A pair of chiral organic-inorganic hybrid tin compounds showing reversible phase transition and enhanced SHG properties.
Jiang, Ting; Zou, Mingjun; Wu, Yaozhen; Zhou, Jie; Yin, Xin; Guo, Wenjing; Wei, Zhenhong; Cai, Hu; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14559–14565; doi:10.1039/d5dt01839k

data_1575700
_publ_section_title
;
 A pair of chiral organic-inorganic hybrid tin compounds showing
 reversible phase transition and enhanced SHG properties.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14559
_journal_page_last               14565
_journal_paper_doi               10.1039/d5dt01839k
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Cl6 Sn, C4 H12 N2'
_chemical_formula_sum            'C4 H12 Cl6 N2 Sn'
_chemical_formula_weight         419.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2025-07-17
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-07-30 deposited with the CCDC.	2025-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.339(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2249(3)
_cell_length_b                   7.2137(2)
_cell_length_c                   11.5197(4)
_cell_measurement_reflns_used    6573
_cell_measurement_temperature    469.99(10)
_cell_measurement_theta_max      26.7130
_cell_measurement_theta_min      2.9320
_cell_volume                     681.53(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.111a 64-bit (release 27-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      469.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     11.00  37.00   0.50    0.07    --   20.64  57.00-150.00   52
  2  \w     25.00  51.00   0.50    0.07    --   20.64  77.00-150.00   52
  3  \w     60.00  85.00   0.50    0.07    --   20.64  57.00-150.00   50
  4  \w    -20.00 103.00   0.50    0.07    --   20.64  38.00 -60.00  246
  5  \w    -13.00 102.00   0.50    0.07    --   20.64  57.00 150.00  230
  6  \w    -39.00 103.00   0.50    0.07    --   20.64  38.00 120.00  284
  7  \w    -67.00  46.00   0.50    0.07    --   20.64 -38.00  90.00  226
  8  \w     56.00  82.00   0.50    0.07    --   20.64 178.00  60.00   52
  9  \w     48.00  73.00   0.50    0.07    --   20.64 178.00 120.00   50
 10  \w     44.00  97.00   0.50    0.07    --   20.64-136.00 139.00  106
 11  \w     26.00  93.00   0.50    0.07    --   20.64-134.00 -42.00  134
 12  \w    -23.00  15.00   0.50    0.07    --  -20.64 -77.00 -90.00   76
 13  \w   -112.00 -67.00   0.50    0.07    --  -20.64 -77.00 -90.00   90
 14  \w    -82.00 -57.00   0.50    0.07    --  -20.64 136.00-156.00   50
 15  \w    -69.00 -22.00   0.50    0.07    --  -20.64 134.00  25.00   94
 16  \w    -19.00  10.00   0.50    0.07    --  -20.64  19.00-150.00   58
 17  \w     25.00  56.00   0.50    0.07    --  -20.64  19.00-120.00   62
 18  \w     17.00  58.00   0.50    0.07    --  -20.64  19.00-150.00   82
 19  \w     -6.00  44.00   0.50    0.07    --  -20.64  19.00-180.00  100
 20  \w    -24.00   3.00   0.50    0.07    --  -20.64  19.00-120.00   54
 21  \w    -17.00   9.00   0.50    0.07    --  -20.64  19.00 150.00   52
 22  \w    -19.00  62.00   0.50    0.07    --  -20.64  19.00  30.00  162
 23  \w    -14.00  13.00   0.50    0.07    --  -20.64 -99.00-180.00   54
 24  \w      5.00  35.00   0.50    0.07    --  -20.64 -99.00   0.00   60
 25  \w    -17.00  33.00   0.50    0.07    --  -20.64 -99.00 -90.00  100
 26  \w   -103.00 -46.00   0.50    0.07    --  -20.64-178.00-180.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0049400000
_diffrn_orient_matrix_UB_12      0.0143221000
_diffrn_orient_matrix_UB_13      0.0605579000
_diffrn_orient_matrix_UB_21      -0.0137884000
_diffrn_orient_matrix_UB_22      0.0958734000
_diffrn_orient_matrix_UB_23      -0.0101992000
_diffrn_orient_matrix_UB_31      -0.0852409000
_diffrn_orient_matrix_UB_32      -0.0163032000
_diffrn_orient_matrix_UB_33      -0.0066114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15401
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.014
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.111a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2784
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0494P)^2^+0.6367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2428
_reflns_number_total             2784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01839k2.cif
_cod_data_source_block           jt_autored
_cod_depositor_comments
'Adding full bibliography for 1575699--1575702.cif.'
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               1575700
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Sn Cl'
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.970
_diffrn_oxdiff_digest_hkl
;
4304fe0025c4213cf8b0b6cd5f3c8888484002
;
_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, All N(H,H,H) groups
2. Restrained distances
 H2B-N2 = N2-H2A
 0.89 with sigma of 0.02
 H2B-H2A
 1.449 with sigma of 0.04
 Cl3_$1-N2
 2.6 with sigma of 0.04
 H1A-Cl1_$3
 2.7 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C1(H1D,H1E), C4(H4A,H4B), C3(H3A,H3B)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              74380
_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 5.457
_oxdiff_exptl_absorpt_empirical_full_min 0.347