Halogen-Ion-Driven Polymorphs for High-Performance Nonlinear Optical Crystalline Materials
Kang, Yuwei; Yang, Can; Wang, Yunjie; Wu, Qi; Chemical Science  (2026) –; doi:10.1039/D5SC10064J

data_1576616
_publ_section_title
;
 Halogen-ion-driven polymorphs for high-performance nonlinear optical
 crystalline materials.
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              8084
_journal_page_last               8089
_journal_paper_doi               10.1039/d5sc10064j
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'Br3 Sn, C8 H20 N'
_chemical_formula_sum            'C8 H20 Br3 N Sn'
_chemical_formula_weight         488.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-12-23 deposited with the CCDC.	2026-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.506(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.1273(7)
_cell_length_b                   33.1220(13)
_cell_length_c                   13.2631(5)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    223.0
_cell_measurement_theta_max      68.37
_cell_measurement_theta_min      3.52
_cell_volume                     5968.7(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      223.0
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18370
_diffrn_reflns_point_group_measured_fraction_full 0.780
_diffrn_reflns_point_group_measured_fraction_max 0.775
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.485
_diffrn_reflns_theta_min         2.668
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.760
_exptl_absorpt_correction_T_max  0.3201
_exptl_absorpt_correction_T_min  0.0961
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1631 before and 0.0979 after correction.
The Ratio of minimum to maximum transmission is 0.3002.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic whiteish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.175
_exptl_crystal_description       needle
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.953
_refine_diff_density_min         -2.786
_refine_diff_density_rms         0.537
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.147(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         8509
_refine_ls_number_restraints     798
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0839
_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^)+(0.1916P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2276
_reflns_Friedel_coverage         0.586
_reflns_Friedel_fraction_full    0.580
_reflns_Friedel_fraction_max     0.574
_reflns_number_gt                7963
_reflns_number_total             8509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc10064j2.cif
_cod_data_source_block           cu_154166_1_0m
_cod_depositor_comments
'Adding full bibliography for 1576615--1576616.cif.'
_cod_database_code               1576616
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.209
_shelx_estimated_absorpt_t_min   0.209
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.853(14)
 0.147(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C23-C31
 1.48 with sigma of 0.01
 C15-C29 = C25-C11
 1.48 with sigma of 0.01
 C21-C3
 1.48 with sigma of 0.01
 N4-C21 = N4-C15 = N4-C23 = N4-C25 = N3-C2 = N3-C17 = N3-C32 = N3-C22
 1.46 with sigma of 0.01
 N4-C29
 2.5 with sigma of 0.01
 N3-C8
 2.5 with sigma of 0.01
 C17-C8
 1.48 with sigma of 0.01
 H23b-H29c
 2.45 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6.a Riding coordinates:
 C11(H11a,H11b,H11c), C3(H3a,H3b,H3c), C31(H31a,H31b,H31c)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C10(H10a,H10b), C12(H12a,H12b), C14(H14a,H14b), C20(H20a,H20b),
 C22(H22a,H22b), C32(H32a,H32b), C2(H2a,H2b), C17(H17a,H17b), C9(H9a,H9b),
 C5(H5a,H5b), C21(H21a,H21b), C23(H23a,H23b), C25(H25a,H25b), C13(H13a,H13b),
 C15(H15a,H15b)
6.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C4(H4a,H4b,H4c), C8(H8a,H8b,H8c), C16(H16a,H16b,H16c),
 C18(H18a,H18b,H18c), C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C28(H28a,H28b,
 H28c), C30(H30a,H30b,H30c), C19(H19a,H19b,H19c), C27(H27a,H27b,H27c), C7(H7a,
 H7b,H7c), C29(H29a,H29b,H29c)
;
_olex2_submission_special_instructions 'No special instructions were received'