Developing two high-nuclearity Ag nanoclusters with temperature-sensitive fluorescence properties.
Ye, Xiao-Lin; Rezayati, Sobhan; Bigdeli, Fahime; Yang, Le; Liu, Kuan-Guan; Wei, Jianyu; Morsali, Ali; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4298–4305; doi:10.1039/d5dt02009c

data_7720045
_publ_section_title
;
 Developing two high-nuclearity Ag nanoclusters with temperature-sensitive
 fluorescence properties.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4298
_journal_page_last               4305
_journal_paper_doi               10.1039/d5dt02009c
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety
'2(C156 H115 Ag19 Mo O18 P7), 3(C H4 O), 2(C F3 O3 S)'
_chemical_formula_sum            'C317 H242 Ag38 F6 Mo2 O45 P14 S2'
_chemical_formula_weight         9673.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-11-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-11-21 deposited with the CCDC.	2026-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.47(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   16.444(3)
_cell_length_b                   19.237(4)
_cell_length_c                   25.411(5)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.875
_cell_measurement_theta_min      2.695
_cell_volume                     7668(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_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      100(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            144557
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.895
_diffrn_reflns_theta_min         2.521
_exptl_absorpt_coefficient_mu    2.599
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0756 before and 0.0654 after correction.
The Ratio of minimum to maximum transmission is 0.8763.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4670
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 14752 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2016
_refine_ls_number_reflns         36566
_refine_ls_number_restraints     663
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0067P)^2^+6.3487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0488
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                33624
_reflns_number_total             36566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02009c2.cif
_cod_data_source_block           mo_230829b_a
_cod_depositor_comments
'Adding full bibliography for 7720045--7720046.cif.'
_cod_database_code               7720045
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.599
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately coated
 with PDMS (polydimethylsiloxane/Dimethicone, CAS: 9006-65-9 on a glass slide.
 A suitable single crystal was selected and mounted on a glass fiber using
 vacuum silicone grease as adhesive. The glass fiber with single crystal was
 mounted on copper pin with solid paraffin. Operator: DJ_Tokyo.
;
_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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O31A-C3 \\sim O31-C3
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim O21 \\sim O22 \\sim O23 \\sim C1 \\sim F1 \\sim F2 \\sim F3 \\sim O21A
\\sim S1A \\sim O22A \\sim O23A \\sim C1A \\sim F1A \\sim F2A \\sim F3A: within
3A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3A
O31 \\sim C3 \\sim O31A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O32 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Ag21 \\sim Ag19 \\sim Ag11 \\sim Ag20: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(O31) = Uanis(O31A)
4. Same fragment restrains
{S1A, F1A, F2A, F3A, O21A, O22A, O23A, C1A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{S1, F1, F2, F3, O21, O22, O23, C1}
5. Others
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O21A)=Sof(O22A)=Sof(O23A)=Sof(C1A)=1-
 FVAR(1)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O21)=Sof(O22)=Sof(O23)=Sof(C1)=FVAR(1)
 Sof(H3BD)=Sof(H3BE)=Sof(H3BF)=Sof(O31A)=Sof(H31A)=1-FVAR(2)
 Sof(O31)=Sof(H31)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(2)
 Sof(Ag21)=Sof(Ag20)=1-FVAR(3)
 Sof(Ag11)=Sof(Ag19)=FVAR(3)
 Fixed Sof: O32(0.5) H32(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
6.a Riding coordinates:
 O31(H31), O32(H32), O31A(H31A)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C54(H54), C55(H55),
 C56(H56), C57(H57), C58(H58), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
  C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C84(H84), C85(H85),
 C86(H86), C87(H87), C88(H88), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98),
  C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C124(H124), C125(H125),
 C126(H126), C127(H127), C128(H128), C132(H132), C133(H133), C134(H134),
 C135(H135), C136(H136), C142(H142), C143(H143), C144(H144), C145(H145),
 C146(H146), C152(H152), C153(H153), C154(H154), C155(H155), C156(H156),
 C162(H162), C163(H163), C164(H164), C165(H165), C166(H166), C172(H172),
 C173(H173), C174(H174), C175(H175), C176(H176), C182(H182), C183(H183),
 C184(H184), C185(H185), C186(H186), C192(H192), C193(H193), C194(H194),
 C195(H195), C196(H196), C202(H202), C203(H203), C204(H204), C205(H205),
 C206(H206), C212(H212), C213(H213), C214(H214), C215(H215), C216(H216),
 C222(H222), C223(H223), C224(H224), C225(H225), C226(H226), C232(H232),
 C233(H233), C234(H234), C235(H235), C236(H236)
6.c Idealised Me refined as rotating group:
 C3(H3AA,H3AB,H3AC), C3(H3BD,H3BE,H3BF), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              23620
_olex2_submission_special_instructions 'No special instructions were received'