Crystal-glass phase transition enabling reversible fluorescence switching in zero-dimensional antimony halides
Yin, Meijuan; Li, Baihan; Yi, Zishuo; Zhang, Yuchi; Xia, Zhiguo; Xu, Yan; Chemical Communications  (2023) –; doi:10.1039/D3CC03752E

data_7132073
_publ_section_title
;
 Crystal-glass phase transition enabling reversible fluorescence switching
 in zero-dimensional antimony halides
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03752E
_journal_year                    2023
_chemical_formula_moiety         'Cl5 Sb, 2(C19 H18 P)'
_chemical_formula_sum            'C38 H36 Cl5 P2 Sb'
_chemical_formula_weight         853.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2gqr54
_audit_creation_date             2023-08-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-01 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1192(3)
_cell_length_b                   15.8880(7)
_cell_length_c                   13.1790(5)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.56
_cell_volume                     1862.90(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33175
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.038
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  0.0104
_exptl_absorpt_correction_T_min  0.0013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0772 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.1250.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.825
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0818
_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^)+(0.0390P)^2^+11.9116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.1766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3057
_reflns_number_total             3289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03752e2.cif
_cod_data_source_block           a
_cod_database_code               7132073
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl1(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C3(H3), C19(H19), C13(H13), C16(H16), C18(H18), C4(H4),
 C10(H10), C17(H17), C11(H11), C6(H6), C7(H7), C5(H5), C12(H12)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              451
_shelx_hkl_checksum              5533
_olex2_submission_special_instructions 'No special instructions were received'