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_1574911
_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         'C102 H84 Ag2 Cl N6 P6, 2(C H2 Cl2), 1[]'
_chemical_formula_sum            'C104 H88 Ag2 Cl5 N6 P6'
_chemical_formula_weight         2000.61
_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             2025-06-16
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-17 deposited with the CCDC.	2025-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                79.654(3)
_cell_angle_beta                 74.705(3)
_cell_angle_gamma                64.242(4)
_cell_formula_units_Z            1
_cell_length_a                   12.7430(4)
_cell_length_b                   12.7623(5)
_cell_length_c                   16.6375(6)
_cell_measurement_reflns_used    18917
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      29.5830
_cell_measurement_theta_min      1.7610
_cell_volume                     2344.01(17)
_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 2019/3 (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 1.000
_diffrn_measured_fraction_theta_max 0.847
_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    -56.00 -30.00   0.50    1.59    --    5.00  45.00 160.37   52
  2  \w   -100.00  78.00   0.50    1.59    --  -10.70  45.00  83.68  356
  3  \w    -56.00 -29.00   0.50    1.59    --  -10.70  45.00  13.93   54
  4  \w     -9.00  56.00   0.50    1.59    --  -10.70  45.00  13.93  130
  5  \w    -99.00  13.00   0.50    1.59    --  -10.70  45.00 150.00  224
  6  \w     22.00  51.00   0.50    1.59    --  -10.70  45.00 -17.18   58
  7  \w    -27.00  77.00   0.50    1.59    --  -10.70  45.00 170.77  208
  8  \w    -76.00 -50.00   0.50    1.59    --  -10.70  45.00 170.77   52
;
_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      0.0231744000
_diffrn_orient_matrix_UB_12      -0.0500435000
_diffrn_orient_matrix_UB_13      -0.0228077000
_diffrn_orient_matrix_UB_21      0.0515514000
_diffrn_orient_matrix_UB_22      -0.0236513000
_diffrn_orient_matrix_UB_23      0.0174024000
_diffrn_orient_matrix_UB_31      -0.0282949000
_diffrn_orient_matrix_UB_32      -0.0276699000
_diffrn_orient_matrix_UB_33      0.0337846000
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.967
_diffrn_reflns_theta_min         1.777
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77535
_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    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             1023
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12643
_refine_ls_number_restraints     488
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0647P)^2^+4.7009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10212
_reflns_number_total             12643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr01269d2.cif
_cod_data_source_block           mx11413_sq
_cod_depositor_comments
'Adding full bibliography for 1574898--1574913.cif.'
_cod_database_code               1574911
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         AgAuNOClPCH
_diffrn_oxdiff_ac3_digest_frames
;
01982436daae2e7d9d11ff0a8d5e888f8400028e213
;
_diffrn_oxdiff_ac3_digest_hkl
;
015c25ad3101699fde11449aa82d11f64b02b4
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C19A-C18 = C20A-C19A = C21A-C20A = C21A-C22 = C21-C20 = C20-C19 = C22-C21 =
 C19-C18 = C15-C14 = C16-C15 = C17-C16 = C17-C12 = C17A-C12 = C16A-C17A = C15A-
 C16A = C15A-C14 = C51-C46 = C51-C50 = C50-C49 = C49-C48 = C48-C47 = C47-C46 =
 C57-C56 = C58-C57 = C62-C58 = C62-C60 = C61-C60 = C61-C56
 1.39 with sigma of 0.01
3. Restrained planarity
 C18, N2A, C19A, C20A, C21A, C22A
 with sigma of 0.01
 C18, N2, C19, C20, C21, C22
 with sigma of 0.01
 C12, C13A, C14A, C15A, C16A, C17A
 with sigma of 0.01
 C12, C13, C14, C15, C16, C17
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C18 \\sim N2 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim N2A \\sim C19A \\sim
C20A \\sim C21A \\sim C22A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C56 \\sim C57 \\sim
C58 \\sim C60 \\sim C61 \\sim C62: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C13A \\sim C14A
\\sim C15A \\sim C16A \\sim C17A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
Uanis(N2) \\sim Ueq, Uanis(N2A) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
5. Others
 Sof(C56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C60)=Sof(H60)=Sof(C61)=
 Sof(H61)=Sof(C62)=Sof(H62)=1-FVAR(1)
 Sof(C46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(C50)=
 Sof(H50)=Sof(C51)=Sof(H51)=FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(H16A)=Sof(C17A)=Sof(H17A)=1-FVAR(2)
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=
 Sof(C17)=Sof(H17)=FVAR(2)
 Sof(N2A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=
 Sof(C22A)=Sof(H22A)=1-FVAR(3)
 Sof(N2)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C13(H13), C14(H14), C15(H15), C16(H16),
  C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A),
 C17A(H17A), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A), C57(H57), C58(H58),
  C60(H60), C61(H61), C62(H62)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49010
_shelx_fab_checksum              84819
_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 1.521
_oxdiff_exptl_absorpt_empirical_full_min 0.495