Multisequential reversible phase transition materials with semiconducting and fluorescence properties: (C8H18BrN)2SnBr6
Liu, Yao; Li, Yu-Kong; Ying, Ting-Ting; Tan, Yu-Hui; Tang, Yun-Zhi; Han, Ding-Chong; Du, Peng-kang; Zhang, Hao; New Journal of Chemistry 45 (2021) 20721–20725; doi:10.1039/D1NJ04448F

data_7061014
_publ_section_title
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 Multisequential reversible phase transition materials with semiconducting
 and fluorescence properties: (C8H18BrN)2SnBr6
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_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20721
_journal_page_last               20725
_journal_paper_doi               10.1039/D1NJ04448F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'Br6 Sn, 2(C8 H18 Br N)'
_chemical_formula_sum            'C16 H36 Br8 N2 Sn'
_chemical_formula_weight         1014.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-10-02
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2021-10-06 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.855(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4401(14)
_cell_length_b                   14.7764(13)
_cell_length_c                   13.9147(12)
_cell_measurement_reflns_used    7294
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.451
_cell_measurement_theta_min      2.821
_cell_volume                     2968.7(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      300
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16738
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.822
_exptl_absorpt_coefficient_mu    11.636
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1421 before and 0.0930 after correction.
The Ratio of minimum to maximum transmission is 0.4097.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.270
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0.00116(10)
_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   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2625
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0610
_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^)+120.9526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1735
_reflns_number_total             2625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04448f2.cif
_cod_data_source_block           1_LTP
_cod_depositor_comments          'Adding full bibliography for 7061014.cif.'
_cod_database_code               7061014
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.204
_shelx_estimated_absorpt_t_min   0.128
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7A-C8B
 1.5 with sigma of 0.02
 N2-C7A = N2-C6A = N2-C6B
 1.51 with sigma of 0.02
 C8B-C7B
 1.5 with sigma of 0.02
 N2-C6A \\sim N2-C6B \\sim N2-C6B_$1 \\sim N2-C6A_$1 \\sim N2-C7A \\sim
N2-C7A_$1
 with sigma of 0.01
 C5B-C6B \\sim C5A-C6A
 with sigma of 0.01
 Br5B-C5B \\sim Br5A-C5A
 with sigma of 0.01
 Sn1-Br5 \\sim Sn1-Br4
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C5B \\sim C6A \\sim C6B \\sim C7A \\sim C8B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C8A \\sim C7B \\sim C8B \\sim C7A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Br4 \\sim Br5: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Br5B \\sim Br5A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C6B) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C5B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Br3(0.5) Br4(0.94) C8B(0.5) H8BA(0.5) H8BB(0.5) H8BC(0.5) C7A(0.5)
 H7AA(0.5) H7AB(0.5) Br5A(0.25) C6A(0.5) H6AA(0.5) H6AB(0.5) C5A(0.5) H5AA(0.5)
 H5AB(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) Br5B(0.25)
 C7B(0.5) H7BA(0.5) H7BB(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) Br5(0.06)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C4(H4A,H4B), C7A(H7AA,H7AB), C6A(H6AA,H6AB),
 C5A(H5AA,H5AB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7B(H7BA,H7BB)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8B(H8BA,H8BB,H8BC), C8A(H8AA,H8AB,H8AC)
;
_shelx_res_checksum              58035
_olex2_submission_special_instructions 'No special instructions were received'