Studying how small silver clusters grow and their optical properties.
Peter, Blessing D.; Yi, Qiuhao; Luo, Zhixun; Nanoscale 17 (2025) 19821–19827; doi:10.1039/d5nr01269d

data_1575955
_publ_section_title
;
 Studying how small silver clusters grow and their optical properties.
;
_journal_issue                   34
_journal_name_full               Nanoscale
_journal_page_first              19821
_journal_page_last               19827
_journal_paper_doi               10.1039/d5nr01269d
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C49.655 H40.046 Ag2 N3 O3 P3, C O3'
_chemical_formula_sum            'C50.66 H40.04 Ag2 N3 O6 P3'
_chemical_formula_weight         1095.41
_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             2024-08-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-26 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                81.271(4)
_cell_angle_beta                 88.818(5)
_cell_angle_gamma                62.631(6)
_cell_formula_units_Z            2
_cell_length_a                   12.4790(8)
_cell_length_b                   12.5646(6)
_cell_length_c                   17.5146(8)
_cell_measurement_reflns_used    8115
_cell_measurement_temperature    170.01(10)
_cell_measurement_theta_max      25.4220
_cell_measurement_theta_min      1.8250
_cell_volume                     2406.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     59.00  86.00   0.50   35.00    --    5.00  45.00   0.00   54
  2  \w    -54.00 -26.00   0.50   35.00    --    5.00  45.00 150.00   56
  3  \w    -63.00 -36.00   0.50   35.00    --   -9.20  45.00   0.00   54
  4  \w    -95.00  19.00   0.50   35.00    --   -9.20  45.00 120.00  228
  5  \w    -97.00 -70.00   0.50   35.00    --   -9.20  45.00 150.00   54
  6  \w    -28.00  79.00   0.50   35.00    --   -9.20  45.00 150.00  214
  7  \w    -18.00  55.00   0.50   35.00    --   -9.20  45.00   0.00  146
  8  \w    -98.00  77.00   0.50   35.00    --   -9.20  45.00  60.00  350
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0394699000
_diffrn_orient_matrix_UB_12      0.0231899000
_diffrn_orient_matrix_UB_13      -0.0336683000
_diffrn_orient_matrix_UB_21      -0.0492200000
_diffrn_orient_matrix_UB_22      0.0318986000
_diffrn_orient_matrix_UB_23      0.0223896000
_diffrn_orient_matrix_UB_31      0.0113520000
_diffrn_orient_matrix_UB_32      0.0509118000
_diffrn_orient_matrix_UB_33      -0.0070108000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37648
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.241
_diffrn_reflns_theta_min         1.840
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.822
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         11877
_refine_ls_number_restraints     646
_refine_ls_restrained_S_all      2.008
_refine_ls_R_factor_all          0.2515
_refine_ls_R_factor_gt           0.1931
_refine_ls_shift/su_max          0.000
_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          0.5289
_refine_ls_wR_factor_ref         0.5558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7078
_reflns_number_total             11877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr01269d3.cif
_cod_data_source_block           mx15327
_cod_database_code               1575955
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AgCuNOPCH
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C20-C18 \\sim C20A-C18A
 with sigma of 0.02
 C20-C16 \\sim C20A-C16A
 with sigma of 0.02
 C18-C2 \\sim C18A-C2A
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
 C1-C22 \\sim C1A-C22A
 with sigma of 0.02
 C22-C16 \\sim C22A-C16A
 with sigma of 0.02
 P004-C20 \\sim P004-C20A
 with sigma of 0.04
 P004-C1 \\sim P004-C1A
 with sigma of 0.04
 P004-C22 \\sim P004-C22A
 with sigma of 0.04
 P004-C16 \\sim P004-C16A
 with sigma of 0.04
 C20-C2 \\sim C20A-C2A
 with sigma of 0.04
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C18-C1 \\sim C18A-C1A
 with sigma of 0.04
 C18-C16 \\sim C18A-C16A
 with sigma of 0.04
 C2-C22 \\sim C2A-C22A
 with sigma of 0.04
 C1-C16 \\sim C1A-C16A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C017 \\sim C00S \\sim C20 \\sim C18 \\sim C2 \\sim C1 \\sim C22 \\sim C16 \\sim
C20A \\sim C18A \\sim C2A \\sim C1A \\sim C22A \\sim C16A \\sim C00E \\sim C3
\\sim C01J \\sim C12: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
C10: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
1.7A
O17 \\sim O7 \\sim O11: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
N5 \\sim C23 \\sim C4 \\sim C14 \\sim C13 \\sim C6: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 1.7A
C01A \\sim C00Q \\sim C012 \\sim C7 \\sim C01O \\sim C5: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C00Y \\sim C010 \\sim C019 \\sim C01R \\sim C01D \\sim C013: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
Uanis(C16A) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C20A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C1A)
\\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C017) \\sim Ueq, Uanis(C00S) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C01J) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C00E)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(C10)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C00Q) \\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C01O)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C01A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C00Y) \\sim Ueq, Uanis(C010) \\sim Ueq, Uanis(C013) \\sim Ueq,
Uanis(C019) \\sim Ueq, Uanis(C01R) \\sim Ueq, Uanis(C01D) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00V) \\sim Ueq, Uanis(C011) \\sim Ueq, Uanis(C00P) \\sim Ueq,
Uanis(C00B) \\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C00H) \\sim Ueq,
Uanis(C00I) \\sim Ueq, Uanis(C00L) \\sim Ueq, Uanis(C00C) \\sim Ueq,
Uanis(C00D) \\sim Ueq, Uanis(C00J) \\sim Ueq, Uanis(C015) \\sim Ueq,
Uanis(C01H) \\sim Ueq, Uanis(C00N) \\sim Ueq, Uanis(C00R) \\sim Ueq,
Uanis(C00M) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C20A)=Sof(H20A)=Sof(C18A)=Sof(H18A)=Sof(C2A)=Sof(H2A)=Sof(C1A)=Sof(H1A)=
 Sof(C22A)=Sof(C16A)=Sof(H16A)=1-FVAR(1)
 Sof(C20)=Sof(H20)=Sof(C18)=Sof(H18)=Sof(C2)=Sof(H2)=Sof(C1)=Sof(H1)=Sof(C22)=
 Sof(C16)=Sof(H16)=FVAR(1)
 Sof(C00Q)=Sof(H00Q)=Sof(C012)=Sof(C01A)=Sof(H01A)=Sof(C01O)=Sof(H01O)=Sof(C5)=
 Sof(H5)=Sof(C7)=Sof(H7)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00H(H00H), C00I(H00I), C00J(H00J), C00L(H00L),
 C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00T(H00T),
 C00U(H00U), C00V(H00V), C00X(H00X), C00Z(H00Z), C010(H010), C011(H011),
 C013(H013), C015(H015), C017(H017), C00S(H00S), C3(H3), C01J(H01J), C12(H12),
 C019(H019), C01A(H01A), C01D(H01D), C01H(H01H), C01O(H01O), C01R(H01R),
 C20(H20), C18(H18), C2(H2), C1(H1), C16(H16), C20A(H20A), C18A(H18A), C2A(H2A),
  C1A(H1A), C16A(H16A), C13(H13), C6(H6), C23(H23), C14(H14), C5(H5), C7(H7)
5.b Fitted hexagon refined as free rotating group:
 C017(C00S,C3,C01J,C12,C00E), C20(C18,C2,C1,C22,C16), C20A(C18A,C2A,C1A,C22A,
 C16A), C13(C6,C23,N5,C4,C14)
;
_shelx_res_checksum              32903
_shelx_hkl_checksum              63001
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.732
_oxdiff_exptl_absorpt_empirical_full_min 0.432