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_1574910
_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         'C51 H42 Ag Cl N3 P3, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C51.5 H43 Ag Cl2 N3 P3'
_chemical_formula_weight         975.57
_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             2023-09-25
_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                89.488(3)
_cell_angle_beta                 68.446(4)
_cell_angle_gamma                86.972(4)
_cell_formula_units_Z            2
_cell_length_a                   12.9844(6)
_cell_length_b                   13.1743(5)
_cell_length_c                   14.0881(5)
_cell_measurement_reflns_used    13795
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      30.5620
_cell_measurement_theta_min      1.6840
_cell_volume                     2238.12(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 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 1.000
_diffrn_measured_fraction_theta_max 0.844
_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    -54.00 -27.00   0.50    7.59    --    5.00  45.00 168.96   54
  2  \w     24.00  58.00   0.50    7.59    --  -10.70  45.00  -8.13   68
  3  \w    -99.00  24.00   0.50    7.59    --  -10.70  45.00 120.00  246
  4  \w     52.00  78.00   0.50    7.59    --  -10.70  45.00 120.00   52
  5  \w    -98.00  78.00   0.50    7.59    --  -10.70  45.00 175.79  352
  6  \w   -100.00  78.00   0.50    7.59    --  -10.70  45.00  60.00  356
;
_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      0.0175545000
_diffrn_orient_matrix_UB_12      -0.0343142000
_diffrn_orient_matrix_UB_13      0.0308156000
_diffrn_orient_matrix_UB_21      -0.0557488000
_diffrn_orient_matrix_UB_22      -0.0028694000
_diffrn_orient_matrix_UB_23      0.0340759000
_diffrn_orient_matrix_UB_31      -0.0065915000
_diffrn_orient_matrix_UB_32      -0.0414909000
_diffrn_orient_matrix_UB_33      -0.0286354000
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36867
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.014
_diffrn_reflns_theta_min         1.548
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79588
_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            'clear colourless'
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         12052
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.001
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9008
_reflns_number_total             12052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr01269d2.cif
_cod_data_source_block           mx10989
_cod_depositor_comments
'Adding full bibliography for 1574898--1574913.cif.'
_cod_original_formula_sum        'C51.50 H43 Ag Cl2 N3 P3'
_cod_database_code               1574910
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AgNOCClHP
_chemical_oxdiff_usercomment     'Mn Ce C H O N'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl2A-C52 = Cl2-C52
 1.76 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl2A \\sim C52: within 1.9A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.9A
4. Others
 Fixed Sof: Cl2(0.5) Cl2A(0.5) C52(0.5) H52A(0.5) H52B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
  C22(H22), 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), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51)
;
_shelx_res_checksum              48209
_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.385