Structural Transformation and Luminescence Response of Magic-Size Silver(I) Chalcogenide Clusters via Ligand-Exchange
Wu, Wei-Hong; Zeng, Hui-Min; Yu, Ze-Nan; Wang, Chao; Jiang, Zhan-Guo; Zhan, Cai-Hong; Chemical Communications  (2021) –; doi:10.1039/D1CC06007D

data_7129251
_publ_section_title
;
 Structural Transformation and Luminescence Response of Magic-Size
 Silver(I) Chalcogenide Clusters via Ligand-Exchange
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06007D
_journal_year                    2021
_chemical_formula_moiety         '3(F6 Sb), C138 H207 Ag32 S3'
_chemical_formula_sum            'C138 H207 Ag32 F18 S3 Sb3'
_chemical_formula_weight         6121.29
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2021-10-19 deposited with the CCDC.	2021-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                93.851(2)
_cell_angle_beta                 98.460(2)
_cell_angle_gamma                117.901(2)
_cell_formula_units_Z            2
_cell_length_a                   19.1661(9)
_cell_length_b                   19.2822(10)
_cell_length_c                   28.4193(13)
_cell_measurement_reflns_used    9640
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.28
_cell_volume                     9069.1(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            129189
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         2.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0770 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.8319.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_description       block
_exptl_crystal_F_000             5804
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         6.884
_refine_diff_density_min         -4.982
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1907
_refine_ls_number_reflns         36993
_refine_ls_number_restraints     1001
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1221P)^2^+154.9759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2407
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30696
_reflns_number_total             36993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06007d2.cif
_cod_data_source_block           a_a
_cod_database_code               7129251
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-C16
 1.5 with sigma of 0.02
3. Rigid bond restraints
 F7, F8, F10, F11, F12, F34, F1, F2, F3, F4, F5, F6, F04A, F18, F50, F113,
 F128, F139
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C1, C3, C0AA, C01A, C01B, C01C, C01D, C01E, C01F, C01G, C01H, C01I, C01K,
 C01L, C01M, C01P, C01Q, C01S, C01U, C01V, C01W, C01X, C01Y, C01Z, C02A, C02B,
 C02C, C02D, C02F, C02G, C02H, C02K, C02L, C02M, C02P, C02Q, C02R, C02S, C02T,
 C02U, C02Y, C03A, C03C, C03D, C03E, C03H, C03I, C03J, C03L, C03M, C03O, C03P,
 C03Q, C03R, C03T, C03U, C03V, C03X, C03Z, C04B, C04F, C04G, C04J, C04L, C04M,
 C04P, C1A, C2A, C3A, C4A, C5A, C6A, C11A, C12A, C13A, C14A, C15A, C16A, C21A,
 C22A, C23A, C24A, C25A, C26A, C10, C13, C14, C015, C15, C16, C016, C017, C17,
 C18, C018, C019, C20, C020, C21, C022, C023, C024, C026, C27, C027, C028, C28,
 C029, C29, C30, C030, C31, C032, C32, C033, C34, C034, C035, C036, C037, C038,
 C38, C039, C39, C041, C41, C42, C043, C44, C45, C047, C50, C54, C55, C73, C79,
 C126
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F10 \\sim F11 \\sim F12 \\sim F34 \\sim F1 \\sim F2 \\sim F3
\\sim F4 \\sim F5 \\sim F6 \\sim F04A \\sim F18 \\sim F50 \\sim F113 \\sim F128
\\sim F139: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C2 \\sim C1 \\sim C3 \\sim C0AA \\sim C01A \\sim C01B \\sim C01C \\sim C01D
\\sim C01E \\sim C01F \\sim C01G \\sim C01H \\sim C01I \\sim C01K \\sim C01L
\\sim C01M \\sim C01P \\sim C01Q \\sim C01S \\sim C01U \\sim C01V \\sim C01W
\\sim C01X \\sim C01Y \\sim C01Z \\sim C02A \\sim C02B \\sim C02C \\sim C02D
\\sim C02F \\sim C02G \\sim C02H \\sim C02K \\sim C02L \\sim C02M \\sim C02P
\\sim C02Q \\sim C02R \\sim C02S \\sim C02T \\sim C02U \\sim C02Y \\sim C03A
\\sim C03C \\sim C03D \\sim C03E \\sim C03H \\sim C03I \\sim C03J \\sim C03L
\\sim C03M \\sim C03O \\sim C03P \\sim C03Q \\sim C03R \\sim C03T \\sim C03U
\\sim C03V \\sim C03X \\sim C03Z \\sim C04B \\sim C04F \\sim C04G \\sim C04J
\\sim C04L \\sim C04M \\sim C04P \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim
C5A \\sim C6A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A
\\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim C10
\\sim C13 \\sim C14 \\sim C015 \\sim C15 \\sim C16 \\sim C016 \\sim C017 \\sim
C17 \\sim C18 \\sim C018 \\sim C019 \\sim C20 \\sim C020 \\sim C21 \\sim C022
\\sim C023 \\sim C024 \\sim C026 \\sim C27 \\sim C027 \\sim C028 \\sim C28
\\sim C029 \\sim C29 \\sim C30 \\sim C030 \\sim C31 \\sim C032 \\sim C32 \\sim
C033 \\sim C34 \\sim C034 \\sim C035 \\sim C036 \\sim C037 \\sim C038 \\sim C38
\\sim C039 \\sim C39 \\sim C041 \\sim C41 \\sim C42 \\sim C043 \\sim C44 \\sim
C45 \\sim C047 \\sim C50 \\sim C54 \\sim C55 \\sim C73 \\sim C79 \\sim C126:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. Same fragment restrains
{C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C11A, C12A, C13A, C14A, C15A, C16A}
{C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C21A, C22A, C23A, C24A, C25A, C26A}
6. Others
 Fixed Sof: Sb0A(0.5) Sb2(0.5) Sb4(0.5) Sb5A(0.5) Ag0B(0.5) Ag0C(0.5)
 Ag0E(0.33333) Ag0F(0.5) Ag0G(0.5) Ag0J(0.5) Ag0K(0.5) Ag0L(0.5) Ag0M(0.5)
 Ag0N(0.5) Ag0P(0.5) Ag0Q(0.5) Ag0R(0.5) Ag0S(0.5) Ag0T(0.5) Ag0U(0.5)
 Ag0V(0.5) Ag0W(0.5) Ag0X(0.5) Ag1(0.5) Ag1B(0.5) Ag2(0.5) Ag2B(0.5) Ag3(0.5)
 Ag3B(0.33333) Ag4(0.5) Ag4A(0.5) Ag4B(0.33333) Ag5(0.5) Ag5B(0.5) Ag06(0.5)
 Ag6A(0.5) Ag7(0.5) Ag07(0.5) Ag7A(0.5) Ag8(0.5) Ag8A(0.5) Ag9(0.5) Ag9A(0.5)
 Ag10(0.5) Ag11(0.5) Ag12(0.5) Ag13(0.5) Ag14(0.5) Ag15(0.5)
7.a Me refined with riding coordinates:
 C03X(H1AA,HF,HG), C26A(H26A,H26B,H26C), C39(H39A,H39B,H39C), C54(H54A,H54B,
 H54C)
7.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C0AA(H0AA,H0AB,H0AC), C01A(H01A,H01B,H01C),
 C01G(H01D,H01E,H01F), C01Y(H01G,H01H,H01I), C02D(H02A,H02B,H02C), C02H(H02D,
 H02E,H02F), C02S(H02G,H02H,H02I), C02U(H02J,H02K,H02L), C03C(H03A,H03B,H03C),
 C03D(H03D,H03E,H03F), C03E(H03G,H03H,H03I), C03L(H03J,H03K,H03L), C03M(H03M,
 H03N,H03O), C03O(H03P,H03Q,H03R), C03Q(H03S,H03T,H03U), C03R(H03V,H03W,H03X),
 C03T(H03Y,H,HA), C03U(H03Z,HB,HC), C03V(H03,HD,HE), C03Z(H2AA,HH,HI),
 C04B(H04A,H04B,H04C), C04G(H04D,H04E,H04F), C04L(H04G,H04H,H04I), C04M(H04J,
 H04K,H04L), C04P(H04M,H04N,H04O), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC),
 C6A(H6AA,H6AB,H6AC), C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C16A(H16A,
 H16B,H16C), C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C15(H15D,H15E,H15F),
 C16(H16D,H16E,H16F), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C030(H3AA,HJ,HK), C31(H31A,H31B,H31C), C032(H7AA,HL,HM), C033(H8AA,
 HN,HO), C34(H34A,H34B,H34C), C036(H9AA,HP,HQ), C038(H0BA,HR,HS), C38(H38A,H38B,
 H38C), C039(H1BA,HT,HU), C041(H04P,H04Q,H04R), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C043(H04S,H04T,H04U), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C047(H04V,H04W,H04X), C50(H50A,H50B,H50C), C55(H55A,H55B,H55C), C73(H73A,H73B,
 H73C), C79(H79A,H79B,H79C), C126(H12A,H12B,H12C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'