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_7247255
_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         '4(F6 Sb), C192 H288 Ag45 Cl6'
_chemical_formula_sum            'C192 H288 Ag45 Cl6 F24 Sb4'
_chemical_formula_weight         8606.06
_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_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-08
_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                102.885(6)
_cell_angle_beta                 116.443(5)
_cell_angle_gamma                108.691(6)
_cell_formula_units_Z            1
_cell_length_a                   19.854(4)
_cell_length_b                   20.442(4)
_cell_length_c                   20.492(4)
_cell_measurement_reflns_used    4101
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      21.57
_cell_measurement_theta_min      2.46
_cell_volume                     6365(2)
_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      150.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0864
_diffrn_reflns_av_unetI/netI     0.0995
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35923
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        20.815
_diffrn_reflns_theta_max         20.815
_diffrn_reflns_theta_min         2.241
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.902
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0876 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.8700.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.245
_exptl_crystal_description       block
_exptl_crystal_F_000             4077
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.447
_refine_diff_density_min         -2.219
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.352
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1264
_refine_ls_number_reflns         13225
_refine_ls_number_restraints     1478
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.2004
_refine_ls_R_factor_gt           0.1303
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_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          0.3589
_refine_ls_wR_factor_ref         0.4174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6955
_reflns_number_total             13225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00716b2.cif
_cod_data_source_block           p-1_a
_cod_depositor_comments
'Adding full bibliography for 7247254--7247256.cif.'
_cod_original_cell_volume        6364(2)
_cod_database_code               7247255
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C81
 2.5 with sigma of 0.02
 C77-C47
 2.5 with sigma of 0.02
 C15-C75
 1.5 with sigma of 0.02
 C57-C21
 1.5 with sigma of 0.02
 C91-C87
 1.5 with sigma of 0.02
 C6-C8
 1.23 with sigma of 0.02
 C1-C14
 1.23 with sigma of 0.02
 C56-C74
 1.23 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
F1 \\sim F4 \\sim F5 \\sim F6 \\sim F9 \\sim F12: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
F2 \\sim F3 \\sim F7 \\sim F8 \\sim F10 \\sim F11: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
4.a Riding coordinates:
 C24(H24A,H24B,H24C), C47(H47A,H47B,H47C), C53(H53A,H53B,H53C), C77(H77A,H77B,
 H77C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C9(H9A,
 H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C45(H45A,H45B,H45C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C55(H55A,H55B,
 H55C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C63(H63A,
 H63B,H63C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C),
 C75(H75A,H75B,H75C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C84(H84A,H84B,
 H84C), C86(H86A,H86B,H86C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C91(H91A,
 H91B,H91C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C),
 C96(H96A,H96B,H96C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58320
_shelx_fab_checksum              95831
_olex2_submission_special_instructions 'No special instructions were received'