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_1575701
_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
_chemical_name_systematic        1
_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             2025-07-14
_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                 94.450(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2181(5)
_cell_length_b                   7.2079(4)
_cell_length_c                   11.5107(6)
_cell_measurement_reflns_used    6897
_cell_measurement_temperature    470.02(10)
_cell_measurement_theta_max      29.3940
_cell_measurement_theta_min      3.1300
_cell_volume                     679.78(7)
_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      470.02(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     48.00 104.00   0.50    0.10    --   21.05 178.00 120.00  112
  2  \w    -25.00 104.00   0.50    0.10    --   21.05  77.00-120.00  258
  3  \w    -18.00 102.00   0.50    0.10    --   21.05  57.00-150.00  240
  4  \w    -18.00 102.00   0.50    0.10    --   21.05  57.00  30.00  240
  5  \w    -24.00 104.00   0.50    0.10    --   21.05  19.00 120.00  256
  6  \w    -24.00  62.00   0.50    0.10    --  -20.74  19.00 150.00  172
  7  \w    -24.00  62.00   0.50    0.10    --  -20.74  19.00 -60.00  172
  8  \w    -79.00   3.00   0.50    0.10    --  -20.74 104.00-156.00  164
  9  \w    -24.00  62.00   0.50    0.10    --  -20.74  19.00-180.00  172
 10  \w     45.00 104.00   0.50    0.10    --   21.05-178.00  90.00  118
 11  \w      3.00  79.00   0.50    0.10    --   21.05-104.00 102.00  152
 12  \w    -17.00  35.00   0.50    0.10    --  -20.74 -99.00  30.00  104
;
_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      0.0355058000
_diffrn_orient_matrix_UB_12      -0.0850824000
_diffrn_orient_matrix_UB_13      -0.0159513000
_diffrn_orient_matrix_UB_21      0.0785351000
_diffrn_orient_matrix_UB_22      0.0409022000
_diffrn_orient_matrix_UB_23      0.0070785000
_diffrn_orient_matrix_UB_31      0.0068977000
_diffrn_orient_matrix_UB_32      -0.0275955000
_diffrn_orient_matrix_UB_33      0.0592825000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0123
_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       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4905
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_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    3.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24775
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_description       needle
_exptl_crystal_F_000             404
_exptl_crystal_preparation       none
_exptl_crystal_recrystallization_method none
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         4905
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0867P)^2^+0.5189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4615
_reflns_number_total             4905
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9924\% 
around [0.99 -0.00 -0.11] (reciprocal) or [1.00 -0.00 -0.00] (direct)
;
_cod_data_source_file            d5dt01839k2.cif
_cod_data_source_block           0424-1-470k-twin2_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1575699--1575702.cif.'
_cod_original_cell_volume        679.78(6)
_cod_original_sg_symbol_H-M      'P  21'
_cod_database_code               1575701
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Sn Cl'
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.752
_diffrn_oxdiff_digest_hkl
;
4304cde74b3e6cf810e71af44b0a29dad3aa07
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.563(2)
 0.437(2)
2. 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
3. Restrained distances
 C4-C1 = C2-C1 = C2-C3
 1.54 with sigma of 0.02
 C2-C3 = C4-C1
 1.54 with sigma of 0.01
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C2(H2c,H2d)
4.c Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_shelx_res_checksum              71556
_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 2.782
_oxdiff_exptl_absorpt_empirical_full_min 0.564
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2