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_1574908
_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
'C68 H56 Ag N4 P4, 0.795(C H2 Cl2), N O3, C2 H6 O'
_chemical_formula_sum            'C70.79 H63.59 Ag Cl1.59 N5 O4 P4'
_chemical_formula_weight         1336.51
_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   mixed
_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                91.203(2)
_cell_angle_beta                 91.613(2)
_cell_angle_gamma                96.934(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9103(3)
_cell_length_b                   13.7805(4)
_cell_length_c                   19.6808(5)
_cell_measurement_reflns_used    27491
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      30.9660
_cell_measurement_theta_min      1.6880
_cell_volume                     3204.34(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.840
_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    -79.00 -51.00   0.50   10.95    --  -10.80  45.00 132.78   56
  2  \w    -15.00  11.00   0.50   10.95    --  -10.80  45.00 132.78   52
  3  \w     53.00  78.00   0.50   10.95    --  -10.80  45.00 132.78   50
  4  \w    -74.00 -38.00   0.50   10.95    --  -10.80  45.00  60.00   72
  5  \w    -26.00  69.00   0.50   10.95    --  -10.80  45.00  60.00  190
  6  \w   -100.00 -64.00   0.50   10.95    --  -10.80  45.00 -17.71   72
  7  \w    -44.00  77.00   0.50   10.95    --  -10.80  45.00 -17.71  242
  8  \w   -100.00 -47.00   0.50   10.95    --  -10.80  45.00 150.00  106
  9  \w    -48.00  78.00   0.50   10.95    --  -10.80  45.00 177.71  252
;
_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      -0.0206780000
_diffrn_orient_matrix_UB_12      -0.0312015000
_diffrn_orient_matrix_UB_13      -0.0278585000
_diffrn_orient_matrix_UB_21      -0.0543099000
_diffrn_orient_matrix_UB_22      0.0155395000
_diffrn_orient_matrix_UB_23      0.0031012000
_diffrn_orient_matrix_UB_31      0.0150137000
_diffrn_orient_matrix_UB_32      0.0384070000
_diffrn_orient_matrix_UB_33      -0.0226860000
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52013
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.972
_diffrn_reflns_theta_min         1.723
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72387
_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    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             1379
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         17117
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0626P)^2^+1.8241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14727
_reflns_number_total             17117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr01269d2.cif
_cod_data_source_block           mx11116
_cod_depositor_comments
'Adding full bibliography for 1574898--1574913.cif.'
_cod_database_code               1574908
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         AgNOPCHCl
_diffrn_oxdiff_ac3_digest_frames
;
0146bc64521475ee915f74d8c07b20a20c000257355
;
_diffrn_oxdiff_ac3_digest_hkl
;
01afdb2e4fa162fdef0f48e928cdc2f3002e5a
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-C71
 1.43 with sigma of 0.01
 Cl1A-C72 = Cl2A-C72 = Cl1-C72A = Cl2-C72A
 1.76 with sigma of 0.01
 C70-C71
 1.54 with sigma of 0.01
3. Rigid bond restraints
 C67, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C72 \\sim Cl1A \\sim Cl2A \\sim Cl2 \\sim C72A \\sim Cl1: within 1.9A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.9A
5. Others
 Sof(Cl1)=Sof(Cl2)=Sof(C72A)=Sof(H72A)=Sof(H72B)=FVAR(1)
 Sof(Cl2A)=Sof(Cl1A)=Sof(C72)=Sof(H72C)=Sof(H72D)=FVAR(2)
6.a Riding coordinates:
 O4(H4A)
6.b Secondary CH2 refined with riding coordinates:
 C72A(H72A,H72B), C71(H71A,H71B), C72(H72C,H72D)
6.c 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),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), 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), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66),
 C67(H67), C68(H68)
6.d Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C)
;
_shelx_res_checksum              16990
_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 1.540
_oxdiff_exptl_absorpt_empirical_full_min 0.649