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_1574902
_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
'3(C22.667 H18.667 Ag0.333 N1.333 P1.333), 0.167[], 0.333[], 0.167[], 0.167[], 0.333[], 0.667[], 0.167[]'
_chemical_formula_sum            'C68 H56 Ag N4 P4'
_chemical_formula_weight         1160.91
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-12-26 deposited with the CCDC.	2025-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.9512(6)
_cell_length_b                   13.9512(6)
_cell_length_c                   51.4858(19)
_cell_measurement_reflns_used    10310
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      27.2480
_cell_measurement_theta_min      1.6880
_cell_volume                     8678.4(6)
_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      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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   -100.00  77.08   0.38   15.00    --  -10.70  45.00   0.00  466
  2  \w     17.00  45.12   0.38   15.00    --  -10.70  45.00   0.00   74
  3  \w     13.00  41.12   0.38   15.00    --  -10.70  45.00  30.59   74
;
_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      0.0559600000
_diffrn_orient_matrix_UB_12      0.0277467000
_diffrn_orient_matrix_UB_13      0.0042961000
_diffrn_orient_matrix_UB_21      0.0181984000
_diffrn_orient_matrix_UB_22      0.0135763000
_diffrn_orient_matrix_UB_23      -0.0130224000
_diffrn_orient_matrix_UB_31      -0.0013613000
_diffrn_orient_matrix_UB_32      0.0498668000
_diffrn_orient_matrix_UB_33      0.0012095000
_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  0.1154
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            55283
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         1.685
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89917
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             3594
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.456
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         13304
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1727
_refine_ls_R_factor_gt           0.1187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1514P)^2^+27.9716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3111
_refine_ls_wR_factor_ref         0.3508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7190
_reflns_number_total             13304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr01269d2.cif
_cod_data_source_block           mx10853b_sq
_cod_depositor_comments
'Adding full bibliography for 1574898--1574913.cif.'
_cod_original_cell_volume        8678.4(8)
_cod_database_code               1574902
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNBPAg
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{N2, C23}
{C46, N4}
{N6, C6A}
3. Restrained distances
 C5-C6 = C6-C1 = C2-C1 = C2-C3 = C4-C3 = C4-C5
 1.39 with sigma of 0.01
 C69-C1 = C79-C69 = C80-C79 = C81-C80 = C82-C81 = C82-C1
 1.39 with sigma of 0.01
 C54-C53 = C55-C54 = C56-C55 = C57-C56 = C58-C57 = C58-C53
 1.39 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C80 \\sim C81 \\sim C79
\\sim C82 \\sim C69: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
Uanis(C82) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) = Uanis(C23)
Uanis(N6) = Uanis(C6A)
Uanis(C46) = Uanis(N4)
5. Others
 Sof(C80)=Sof(H80)=Sof(C81)=Sof(H81)=Sof(C79)=Sof(H79)=Sof(C82)=Sof(H82)=
 Sof(C69)=Sof(H69)=1-FVAR(1)
 Sof(C6)=Sof(H6)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=Sof(C2)=
 Sof(H2)=FVAR(1)
 Fixed Sof: C23(0.66666) H23(0.66666) H22(0.333333) H22A(0.66666) C46(0.66666)
 H46(0.66666) H45(0.66666) H45A(0.333333) N6(0.333333) H68(0.333333)
 H68A(0.66666) N2(0.333333) N4(0.333333) C6A(0.66666) H6A(0.66666)
6.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C12(H12), C11(H11),
 C10(H10), C9(H9), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C22(H22A), C35(H35), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C34(H34), C33(H33), C32(H32), C31(H31), C37(H37),
  C38(H38), C39(H39), C40(H40), C46(H46), C45(H45), C45(H45A), C44(H44),
 C43(H43), C42(H42), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54),
  C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62),
 C63(H63), C65(H65), C66(H66), C67(H67), C68(H68), C68(H68A), C6A(H6A),
 C80(H80), C81(H81), C79(H79), C82(H82), C69(H69)
;
_shelx_res_checksum              45305
_shelx_fab_checksum              34747
_platon_squeeze_void_probe_radius 1.20
_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.765