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_7247256
_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         'C360 H540 Ag148 Br30 S26'
_chemical_formula_sum            'C360 H540 Ag148 Br30 S26'
_chemical_formula_weight         24063.51
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_atom_sites_solution_hydrogens   difmap
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.517(4)
_cell_length_b                   30.517(4)
_cell_length_c                   35.190(6)
_cell_measurement_reflns_used    7359
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      17.96
_cell_measurement_theta_min      2.21
_cell_volume                     32772(8)
_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      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0919
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            58977
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        18.847
_diffrn_reflns_theta_max         18.847
_diffrn_reflns_theta_min         0.883
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.242
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_description       block
_exptl_crystal_F_000             22244
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.209
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.470
_refine_ls_extinction_coef       0.00025(4)
_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   1.511
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         6603
_refine_ls_number_restraints     1148
_refine_ls_restrained_S_all      1.388
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.1233
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.001
_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          0.3418
_refine_ls_wR_factor_ref         0.3783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4408
_reflns_number_total             6603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00716b2.cif
_cod_data_source_block           910_a
_cod_depositor_comments
'Adding full bibliography for 7247254--7247256.cif.'
_cod_original_cell_volume        32773(11)
_cod_database_code               7247256
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.521
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20-C22 = C22-C24
 1.54 with sigma of 0.02
 C32-C36 = C32-C38
 1.55 with sigma of 0.02
 C17-C35 = C35-C9
 1.54 with sigma of 0.02
 C35-C37 = C35-C19
 1.55 with sigma of 0.02
 C30-C32 = C32-C34
 1.54 with sigma of 0.02
 C22-C26 = C22-C28
 1.55 with sigma of 0.02
 C40-C42 = C42-C44
 1.54 with sigma of 0.02
 C42-C46 = C42-C48
 1.55 with sigma of 0.02
 C50-C52 = C52-C54
 1.54 with sigma of 0.02
 C52-C27 = C52-C7
 1.55 with sigma of 0.02
 C29-C15 = C15-C31
 1.54 with sigma of 0.02
 C15-C2 = C15-C33
 1.55 with sigma of 0.02
 C39-C5 = C5-C41
 1.54 with sigma of 0.02
 C5-C21 = C5-C43
 1.55 with sigma of 0.02
 C25-C51 = C51-C13
 1.54 with sigma of 0.02
 C23-C47 = C47-C3
 1.54 with sigma of 0.02
 C47-C49
 1.55 with sigma of 0.02
 C51-C53
 1.55 with sigma of 0.02
 C4-C37
 1.2 with sigma of 0.02
 C30-C36 = C30-C38
 2.52 with sigma of 0.04
 C17-C37 = C17-C19
 2.52 with sigma of 0.04
 C30-C34
 2.56 with sigma of 0.04
 C17-C9
 2.56 with sigma of 0.04
 C40-C46 = C40-C48
 2.52 with sigma of 0.04
 C20-C26 = C20-C28
 2.52 with sigma of 0.04
 C29-C2 = C29-C33
 2.52 with sigma of 0.04
 C50-C27 = C50-C7
 2.52 with sigma of 0.04
 C20-C24
 2.56 with sigma of 0.04
 C40-C44
 2.56 with sigma of 0.04
 C50-C54
 2.56 with sigma of 0.04
 C29-C31
 2.56 with sigma of 0.04
 C39-C41
 2.56 with sigma of 0.04
 C39-C21 = C39-C43
 2.52 with sigma of 0.04
 C25-C13
 2.56 with sigma of 0.04
 C25-C53
 2.52 with sigma of 0.04
 C23-C3
 2.56 with sigma of 0.04
 C23-C49
 2.52 with sigma of 0.04
 C32-C34 \\sim C32-C36 \\sim C32-C38 \\sim C32-C30
 with sigma of 0.02
 C34-C36 \\sim C34-C38 \\sim C36-C38
 with sigma of 0.04
 C30-C34 \\sim C30-C36 \\sim C30-C38
 with sigma of 0.04
 C35-C9 \\sim C35-C37 \\sim C35-C19 \\sim C35-C17
 with sigma of 0.02
 C9-C37 \\sim C9-C19 \\sim C37-C19
 with sigma of 0.04
 C17-C9 \\sim C17-C37 \\sim C17-C19
 with sigma of 0.04
 C22-C24 \\sim C22-C26 \\sim C22-C28 \\sim C22-C20
 with sigma of 0.02
 C24-C26 \\sim C24-C28 \\sim C26-C28
 with sigma of 0.04
 C20-C24 \\sim C20-C26 \\sim C20-C28
 with sigma of 0.04
 C42-C44 \\sim C42-C46 \\sim C42-C48 \\sim C42-C40
 with sigma of 0.02
 C44-C46 \\sim C44-C48 \\sim C46-C48
 with sigma of 0.04
 C40-C44 \\sim C40-C46 \\sim C40-C48
 with sigma of 0.04
 C52-C54 \\sim C52-C27 \\sim C52-C7 \\sim C52-C50
 with sigma of 0.02
 C54-C27 \\sim C54-C7 \\sim C27-C7
 with sigma of 0.04
 C50-C54 \\sim C50-C27 \\sim C50-C7
 with sigma of 0.04
 C15-C31 \\sim C15-C2 \\sim C15-C33 \\sim C15-C29
 with sigma of 0.02
 C31-C2 \\sim C31-C33 \\sim C2-C33
 with sigma of 0.04
 C29-C31 \\sim C29-C2 \\sim C29-C33
 with sigma of 0.04
 C41-C21 \\sim C41-C43 \\sim C21-C43
 with sigma of 0.04
 C39-C41 \\sim C39-C21 \\sim C39-C43
 with sigma of 0.04
 C5-C41 \\sim C5-C21 \\sim C5-C43 \\sim C5-C39
 with sigma of 0.02
 C47-C3 \\sim C47-C49 \\sim C47-C23
 with sigma of 0.02
 C25-C13 \\sim C25-C53
 with sigma of 0.04
 C23-C3 \\sim C23-C49
 with sigma of 0.04
 C51-C13 \\sim C51-C53 \\sim C51-C25
 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 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 C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51
\\sim C52 \\sim C53 \\sim C54: within 3.8A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 3.8A
C30 \\sim C32 \\sim C34 \\sim C36 \\sim C38: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C9 \\sim C17 \\sim C19 \\sim C35 \\sim C37: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C7 \\sim C27 \\sim C50 \\sim C52 \\sim C54: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C20 \\sim C22 \\sim C24 \\sim C26 \\sim C28: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C40 \\sim C42 \\sim C44 \\sim C46 \\sim C48: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C2 \\sim C15 \\sim C29 \\sim C31 \\sim C33: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C5 \\sim C21 \\sim C39 \\sim C41 \\sim C43: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C13 \\sim C25 \\sim C51 \\sim C53: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C3 \\sim C23 \\sim C47 \\sim C49: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C30, C32, C34, C36, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C17, C19, C35, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C22, C24, C26, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C15, C29, C31, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C40, C42, C44, C46, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C27, C50, C52, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, C21, C39, C41, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C25, C51, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C23, C47, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C17(0.5) H17A(0.5) H17B(0.5)
 H17C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 H25A(0.5) H25B(0.5) H25C(0.5)
 Fixed X: C9(0.91414) C17(0.976969) C19(0.95515)
 Fixed Y: C9(0.625701) C17(0.572929) C19(0.59107)
 Fixed Z: C9(0.513161) C17(0.5265) C19(0.45912)
6.a Riding coordinates:
 C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25588
_shelx_fab_checksum              10839
_olex2_submission_special_instructions 'No special instructions were received'