Transformations of silver(i) chalcogenide clusters induced by halide ions as dopant components rather than surface active species
Gao, Yu-Quan; Wu, Wei-Hong; Mao, Hui; Zhang, Ya-Ge; Zhan, Cai-Hong; Jiang, Zhan-Guo; CrystEngComm 25 (2023) 4934–4938; doi:10.1039/D3CE00716B

data_7247254
_publ_section_title
;
 Transformations of silver(i) chalcogenide clusters induced by halide ions
 as dopant components rather than surface active species
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              4934
_journal_page_last               4938
_journal_paper_doi               10.1039/D3CE00716B
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Ag45 Br6 C192, 4(F6 Sb)'
_chemical_formula_sum            'C192 Ag45 Br6 F24 Sb4'
_chemical_formula_weight         8582.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2023-07-03 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                110.987(9)
_cell_angle_beta                 114.356(9)
_cell_angle_gamma                99.657(9)
_cell_formula_units_Z            1
_cell_length_a                   18.711(5)
_cell_length_b                   20.882(6)
_cell_length_c                   21.381(6)
_cell_measurement_reflns_used    2707
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      15.98
_cell_measurement_theta_min      2.40
_cell_volume                     6599(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'BRUKER D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.1117
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19809
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        15.990
_diffrn_reflns_theta_max         15.990
_diffrn_reflns_theta_min         2.212
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.609
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.5679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1046 before and 0.0799 after correction.
The Ratio of minimum to maximum transmission is 0.7632.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_description       block
_exptl_crystal_F_000             3897
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.217
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.432
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         6412
_refine_ls_number_restraints     2663
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1824
_refine_ls_R_factor_gt           0.1302
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3554
_refine_ls_wR_factor_ref         0.4020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3739
_reflns_number_total             6412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00716b2.cif
_cod_data_source_block           aaa_a
_cod_depositor_comments
'Adding full bibliography for 7247254--7247256.cif.'
_cod_database_code               7247254
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.586
_olex2_refinement_description
;
1. Restrained distances
 Sb2-F3 = Sb2-F4 = Sb2-F6 = Sb2-F8
 1.88 with sigma of 0.02
 Sb2-F5 = Sb2-F7
 1.87 with sigma of 0.02
 Sb1-F1 = Sb1-F2 = Sb1-F10 = Sb1-F12
 1.88 with sigma of 0.02
 Sb1-F9 = Sb1-F11
 1.87 with sigma of 0.02
 C16-C18 = C18-C20
 1.54 with sigma of 0.02
 C36-C38 = C38-C40
 1.54 with sigma of 0.02
 C18-C22 = C18-C24
 1.55 with sigma of 0.02
 C26-C28 = C28-C30
 1.54 with sigma of 0.02
 C28-C32 = C28-C34
 1.55 with sigma of 0.02
 C38-C42 = C38-C44
 1.55 with sigma of 0.02
 C56-C58 = C58-C60
 1.54 with sigma of 0.02
 C66-C68 = C68-C70
 1.54 with sigma of 0.02
 C58-C62 = C58-C64
 1.55 with sigma of 0.02
 C48-C52 = C48-C54
 1.55 with sigma of 0.02
 C46-C48 = C48-C50
 1.54 with sigma of 0.02
 C68-C72 = C68-C74
 1.55 with sigma of 0.02
 C90-C94 = C90-C96
 1.55 with sigma of 0.02
 C88-C90 = C90-C92
 1.54 with sigma of 0.02
 C17-C69 = C69-C35
 1.54 with sigma of 0.02
 C3-C49 = C49-C25
 1.54 with sigma of 0.02
 C49-C51 = C49-C13
 1.55 with sigma of 0.02
 C69-C71 = C69-C9
 1.55 with sigma of 0.02
 C53-C27 = C27-C55
 1.54 with sigma of 0.02
 C27-C7 = C27-C57
 1.55 with sigma of 0.02
 C29-C59 = C59-C15
 1.54 with sigma of 0.02
 C59-C61 = C59-C31
 1.55 with sigma of 0.02
 C63-C2 = C2-C65
 1.54 with sigma of 0.02
 C2-C33 = C2-C67
 1.55 with sigma of 0.02
 C37-C19 = C37-C77
 1.55 with sigma of 0.02
 C73-C37 = C37-C75
 1.54 with sigma of 0.02
 C5-C81 = C81-C41
 1.54 with sigma of 0.02
 C81-C83 = C81-C21
 1.55 with sigma of 0.02
 C43-C87 = C87-C11
 1.54 with sigma of 0.02
 C87-C89 = C87-C45
 1.55 with sigma of 0.02
 C91-C23 = C23-C93
 1.54 with sigma of 0.02
 C23-C47 = C23-C95
 1.55 with sigma of 0.02
 C85-C93
 1.2 with sigma of 0.02
 C26-C32 = C26-C34
 2.52 with sigma of 0.04
 C16-C20
 2.56 with sigma of 0.04
 C16-C22 = C16-C24
 2.52 with sigma of 0.04
 C26-C30
 2.56 with sigma of 0.04
 C36-C40
 2.56 with sigma of 0.04
 C36-C42 = C36-C44
 2.52 with sigma of 0.04
 C46-C50
 2.56 with sigma of 0.04
 C56-C60
 2.56 with sigma of 0.04
 C46-C52 = C46-C54
 2.52 with sigma of 0.04
 C66-C70
 2.56 with sigma of 0.04
 C66-C72 = C66-C74
 2.52 with sigma of 0.04
 C56-C62 = C56-C64
 2.52 with sigma of 0.04
 C88-C92
 2.56 with sigma of 0.04
 C88-C94 = C88-C96
 2.52 with sigma of 0.04
 C29-C15
 2.56 with sigma of 0.04
 C17-C35
 2.56 with sigma of 0.04
 C3-C25
 2.56 with sigma of 0.04
 C53-C55
 2.56 with sigma of 0.04
 C63-C65
 2.56 with sigma of 0.04
 C3-C51 = C3-C13
 2.52 with sigma of 0.04
 C53-C7 = C53-C57
 2.52 with sigma of 0.04
 C29-C61 = C29-C31
 2.52 with sigma of 0.04
 C63-C33 = C63-C67
 2.52 with sigma of 0.04
 C17-C71 = C17-C9
 2.52 with sigma of 0.04
 C73-C75
 2.56 with sigma of 0.04
 C73-C19 = C73-C77
 2.52 with sigma of 0.04
 C5-C41
 2.56 with sigma of 0.04
 C5-C83 = C5-C21
 2.52 with sigma of 0.04
 C43-C89 = C43-C45
 2.52 with sigma of 0.04
 C43-C11
 2.56 with sigma of 0.04
 C91-C93
 2.56 with sigma of 0.04
 C91-C47 = C91-C95
 2.52 with sigma of 0.04
 Sb1-F1 \\sim Sb1-F2 \\sim Sb1-F9 \\sim Sb1-F10 \\sim Sb1-F11 \\sim Sb1-F12
 with sigma of 0.02
 F1-F2 \\sim F1-F9 \\sim F1-F10 \\sim F1-F11 \\sim F2-F9 \\sim F2-F11 \\sim
F2-F12 \\sim F9-F10 \\sim F9-F12 ~
 F10-F11 \\sim F10-F12 \\sim F11-F12
 with sigma of 0.04
 Sb2-F3 \\sim Sb2-F4 \\sim Sb2-F5 \\sim Sb2-F6 \\sim Sb2-F7 \\sim Sb2-F8
 with sigma of 0.02
 F3-F4 \\sim F3-F5 \\sim F3-F6 \\sim F3-F7 \\sim F4-F5 \\sim F4-F7 \\sim F4-F8
\\sim F5-F6 \\sim F5-F8 \\sim F6-F7
 \\sim F6-F8 \\sim F7-F8
 with sigma of 0.04
 C36-C40 \\sim C36-C42 \\sim C36-C44
 with sigma of 0.04
 C38-C40 \\sim C38-C42 \\sim C38-C44 \\sim C38-C36
 with sigma of 0.02
 C40-C42 \\sim C40-C44 \\sim C42-C44
 with sigma of 0.04
 C18-C20 \\sim C18-C22 \\sim C18-C24 \\sim C18-C16
 with sigma of 0.02
 C20-C22 \\sim C20-C24 \\sim C22-C24
 with sigma of 0.04
 C16-C20 \\sim C16-C22 \\sim C16-C24
 with sigma of 0.04
 C28-C30 \\sim C28-C32 \\sim C28-C34 \\sim C28-C26
 with sigma of 0.02
 C30-C32 \\sim C30-C34 \\sim C32-C34
 with sigma of 0.04
 C26-C30 \\sim C26-C32 \\sim C26-C34
 with sigma of 0.04
 C56-C60 \\sim C56-C62 \\sim C56-C64
 with sigma of 0.04
 C48-C50 \\sim C48-C52 \\sim C48-C54 \\sim C48-C46
 with sigma of 0.02
 C60-C62 \\sim C60-C64 \\sim C62-C64
 with sigma of 0.04
 C68-C70 \\sim C68-C72 \\sim C68-C74 \\sim C68-C66
 with sigma of 0.02
 C70-C72 \\sim C70-C74 \\sim C72-C74
 with sigma of 0.04
 C66-C70 \\sim C66-C72 \\sim C66-C74
 with sigma of 0.04
 C50-C52 \\sim C50-C54 \\sim C52-C54
 with sigma of 0.04
 C46-C50 \\sim C46-C52 \\sim C46-C54
 with sigma of 0.04
 C58-C60 \\sim C58-C62 \\sim C58-C64 \\sim C58-C56
 with sigma of 0.02
 C88-C92 \\sim C88-C94 \\sim C88-C96
 with sigma of 0.04
 C90-C92 \\sim C90-C94 \\sim C90-C96 \\sim C90-C88
 with sigma of 0.02
 C92-C94 \\sim C92-C96 \\sim C94-C96
 with sigma of 0.04
 C59-C15 \\sim C59-C61 \\sim C59-C31 \\sim C59-C29
 with sigma of 0.02
 C29-C15 \\sim C29-C61 \\sim C29-C31
 with sigma of 0.04
 C15-C61 \\sim C15-C31 \\sim C61-C31
 with sigma of 0.04
 C2-C65 \\sim C2-C33 \\sim C2-C67 \\sim C2-C63
 with sigma of 0.02
 C17-C35 \\sim C17-C71 \\sim C17-C9
 with sigma of 0.04
 C65-C33 \\sim C65-C67 \\sim C33-C67
 with sigma of 0.04
 C63-C65 \\sim C63-C33 \\sim C63-C67
 with sigma of 0.04
 C69-C35 \\sim C69-C71 \\sim C69-C9 \\sim C69-C17
 with sigma of 0.02
 C35-C71 \\sim C35-C9 \\sim C71-C9
 with sigma of 0.04
 C49-C25 \\sim C49-C51 \\sim C49-C13 \\sim C49-C3
 with sigma of 0.02
 C25-C51 \\sim C25-C13 \\sim C51-C13
 with sigma of 0.04
 C3-C25 \\sim C3-C51 \\sim C3-C13
 with sigma of 0.04
 C27-C55 \\sim C27-C7 \\sim C27-C57 \\sim C27-C53
 with sigma of 0.02
 C55-C7 \\sim C55-C57 \\sim C7-C57
 with sigma of 0.04
 C53-C55 \\sim C53-C7 \\sim C53-C57
 with sigma of 0.04
 C75-C19 \\sim C75-C77 \\sim C19-C77
 with sigma of 0.04
 C37-C75 \\sim C37-C19 \\sim C37-C77 \\sim C37-C73
 with sigma of 0.02
 C73-C75 \\sim C73-C19 \\sim C73-C77
 with sigma of 0.04
 C41-C83 \\sim C41-C21 \\sim C83-C21
 with sigma of 0.04
 C81-C41 \\sim C81-C83 \\sim C81-C21 \\sim C81-C5
 with sigma of 0.02
 C5-C41 \\sim C5-C83 \\sim C5-C21
 with sigma of 0.04
 C43-C11 \\sim C43-C89 \\sim C43-C45
 with sigma of 0.04
 C11-C89 \\sim C11-C45 \\sim C89-C45
 with sigma of 0.04
 C87-C11 \\sim C87-C89 \\sim C87-C45 \\sim C87-C43
 with sigma of 0.02
 C91-C93 \\sim C91-C47 \\sim C91-C95
 with sigma of 0.04
 C93-C47 \\sim C93-C95 \\sim C47-C95
 with sigma of 0.04
 C23-C93 \\sim C23-C47 \\sim C23-C95 \\sim C23-C91
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Sb2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
Sb1 \\sim F1 \\sim F2 \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C26 \\sim C28 \\sim C30 \\sim C32 \\sim C34: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C16 \\sim C18 \\sim C20 \\sim C22 \\sim C24: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C36 \\sim C38 \\sim C40 \\sim C42 \\sim C44: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C56 \\sim C58 \\sim C60 \\sim C62 \\sim C64: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C46 \\sim C48 \\sim C50 \\sim C52 \\sim C54: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C66 \\sim C68 \\sim C70 \\sim C72 \\sim C74: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C88 \\sim C90 \\sim C92 \\sim C94 \\sim C96: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C3 \\sim C49 \\sim C25 \\sim C51 \\sim C13: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C29 \\sim C59 \\sim C15 \\sim C61 \\sim C31: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C53 \\sim C27 \\sim C55 \\sim C7 \\sim C57: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C63 \\sim C2 \\sim C65 \\sim C33 \\sim C67: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C17 \\sim C69 \\sim C35 \\sim C71 \\sim C9: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C73 \\sim C37 \\sim C75 \\sim C19 \\sim C77: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C85: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C5 \\sim C81 \\sim C41 \\sim C83 \\sim C21: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C43 \\sim C87 \\sim C11 \\sim C89 \\sim C45: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C91 \\sim C23 \\sim C93 \\sim C47 \\sim C95: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C1 \\sim C4 \\sim C6 \\sim C8 \\sim C10 \\sim C12 \\sim C14 \\sim C16 \\sim C18
\\sim C20 \\sim C22 \\sim C24 \\sim C26 \\sim C28 \\sim C30 \\sim C32 \\sim C34
\\sim C36 \\sim C38 \\sim C40 \\sim C42 \\sim C44 \\sim C46 \\sim C48 \\sim C50
\\sim C52 \\sim C54 \\sim C56 \\sim C58 \\sim C60 \\sim C62 \\sim C64 \\sim C66
\\sim C68 \\sim C70 \\sim C72 \\sim C74 \\sim C76 \\sim C78 \\sim C80 \\sim C82
\\sim C84 \\sim C86 \\sim C88 \\sim C90 \\sim C92 \\sim C94 \\sim C96 \\sim C3
\\sim C49 \\sim C25 \\sim C51 \\sim C13 \\sim C53 \\sim C27 \\sim C55 \\sim C7
\\sim C57 \\sim C29 \\sim C59 \\sim C15 \\sim C61 \\sim C31 \\sim C63 \\sim C2
\\sim C65 \\sim C33 \\sim C67 \\sim C17 \\sim C69 \\sim C35 \\sim C71 \\sim C9
\\sim C73 \\sim C37 \\sim C75 \\sim C19 \\sim C77 \\sim C39 \\sim C79 \\sim C5
\\sim C81 \\sim C41 \\sim C83 \\sim C21 \\sim C85 \\sim C43 \\sim C87 \\sim C11
\\sim C89 \\sim C45 \\sim C91 \\sim C23 \\sim C93 \\sim C47 \\sim C95: within
3.8A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 3.8A
3. Rigid body (RIGU) restrains
 Sb2, F3, F4, F5, F6, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Sb1, F1, F2, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C18, C20, C22, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C38, C40, C42, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C28, C30, C32, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C58, C60, C62, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C48, C50, C52, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C66, C68, C70, C72, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C88, C90, C92, C94, C96
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C49, C25, C51, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C59, C15, C61, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C69, C35, C71, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C27, C55, C7, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C63, C2, C65, C33, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C73, C37, C75, C19, C77
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, C81, C41, C83, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C85
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, C87, C11, C89, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C23, C93, C47, C95
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82852
_shelx_fab_checksum              52629
_olex2_submission_special_instructions 'No special instructions were received'