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_1574907
_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, C H2 Cl2, N O3, C H4 O'
_chemical_formula_sum            'C70 H62 Ag Cl2 N5 O4 P4'
_chemical_formula_weight         1339.89
_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             2025-05-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-14 deposited with the CCDC.	2025-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                89.788(3)
_cell_angle_beta                 89.154(3)
_cell_angle_gamma                82.330(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9246(5)
_cell_length_b                   13.9944(4)
_cell_length_c                   19.0615(7)
_cell_measurement_reflns_used    13149
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      29.9920
_cell_measurement_theta_min      1.8000
_cell_volume                     3152.1(2)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.896
_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    -87.00   8.00   0.50    3.50    --  -10.70  45.00  92.62  190
  2  \w     31.00  76.00   0.50    3.50    --  -10.70  45.00  92.62   90
  3  \w    -95.00  57.00   0.50    3.50    --  -10.70  45.00  43.17  304
;
_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      -0.0029323000
_diffrn_orient_matrix_UB_12      0.0502597000
_diffrn_orient_matrix_UB_13      0.0060398000
_diffrn_orient_matrix_UB_21      0.0239062000
_diffrn_orient_matrix_UB_22      0.0059462000
_diffrn_orient_matrix_UB_23      -0.0337710000
_diffrn_orient_matrix_UB_31      -0.0549815000
_diffrn_orient_matrix_UB_32      0.0073544000
_diffrn_orient_matrix_UB_33      -0.0144213000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.927
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12981
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.817
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33357
_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    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.789
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         12981
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0630
_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^)+(0.1157P)^2^+2.1725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10712
_reflns_number_total             12981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr01269d2.cif
_cod_data_source_block           mx111110_tw
_cod_depositor_comments
'Adding full bibliography for 1574898--1574913.cif.'
_cod_database_code               1574907
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         AgNOPCHCl
_diffrn_oxdiff_ac3_digest_frames
;
01115762aa26950a2a38fccedba7919309000260b72
;
_diffrn_oxdiff_ac3_digest_hkl
;
010be9c115f93cad49ae31738b4ae3eafa3440
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.735(3)
 0.265(3)
2. 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,H) groups
3. Restrained distances
 O4-C70A = O4-C70
 1.43 with sigma of 0.01
4. Others
 Sof(H4B)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=1-FVAR(1)
 Sof(H4A)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B)
5.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),
 C13(H13), 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), 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)
5.c Tetrahedral OH refined with riding coordinates:
 O4(H4A), O4(H4B)
5.d Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C70A(H70D,H70E,H70F)
;
_shelx_res_checksum              84935
_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 2.437
_oxdiff_exptl_absorpt_empirical_full_min 0.643