Atomically precise chiral silver clusters based on non-chiral ligands for acid/base stimulated luminescence response.
Wang, Shuaibo; He, Weimiao; Cui, Yujia; Zhou, Zhan; Ma, Lufang; Zang, Shuang-Quan; Nanoscale 15 (2023) 12679–12685; doi:10.1039/d3nr03095d

data_1569435
_publ_section_title
;
 Atomically precise chiral silver clusters based on non-chiral ligands for
 acid/base stimulated luminescence response.
;
_journal_issue                   30
_journal_name_full               Nanoscale
_journal_page_first              12679
_journal_page_last               12685
_journal_paper_doi               10.1039/d3nr03095d
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C124 H98 Ag5.95 N16 P8 S4, 2(H2 O)'
_chemical_formula_sum            'C124 H102 Ag5.95 N16 O2 P8 S4'
_chemical_formula_weight         2866.04
_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             2023-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-05 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                94.0460(10)
_cell_angle_beta                 91.3660(10)
_cell_angle_gamma                109.9500(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4279(2)
_cell_length_b                   17.4914(3)
_cell_length_c                   26.3185(4)
_cell_measurement_reflns_used    25635
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      74.0590
_cell_measurement_theta_min      2.7210
_cell_volume                     6219.58(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -77.00 -51.00   0.50    0.50    --    0.00 -38.00  90.00   52
  2  \w    -88.00 -30.00   0.50    0.50    --    0.00 -57.00-150.00  116
  3  \w    -16.00  85.00   0.50    0.50    --    0.00  38.00  90.00  202
  4  \w    -18.00  29.00   0.50    0.50    --    0.00  38.00 -30.00   94
  5  \w     52.00  89.00   0.50    0.50    --    0.00  38.00 -30.00   74
  6  \w    -26.00  19.00   0.50    0.50    --    0.00 -38.00  90.00   90
  7  \w     -4.00  22.00   0.50    0.50    --    0.00  38.00  30.00   52
  8  \w      6.00 122.00   0.50    2.20    --   95.80 -15.00 120.00  232
  9  \w      6.00 103.00   0.50    2.20    --   95.80 -61.00 120.00  194
 10  \w      7.00  33.00   0.50    2.20    --   95.80 -82.00  30.00   52
 11  \w      6.00 128.00   0.50    2.20    --   95.80 -82.00 120.00  244
 12  \w     12.00 120.00   0.50    2.20    --   95.80 -61.00 -90.00  216
 13  \w     88.00 128.00   0.50    2.20    --   95.80 -82.00 -30.00   80
 14  \w     77.00 106.00   0.50    2.20    --   95.80 -45.00 -30.00   58
 15  \w     17.00 128.00   0.50    2.20    --   95.80 -82.00 -90.00  222
 16  \w     76.00 108.00   0.50    2.20    --   95.80  30.00 120.00   64
 17  \w     93.00 118.00   0.50    2.20    --   95.80 -82.00-180.00   50
 18  \w     75.00 176.00   0.50    2.20    --   95.80  45.00  60.00  202
 19  \w    128.00 184.00   0.50    2.20    --   95.80  30.00 120.00  112
 20  \w     10.00  65.00   0.50    2.20    --   95.80 -61.00   0.00  110
 21  \w     73.00 100.00   0.50    2.20    --   95.80 -82.00  30.00   54
 22  \w     29.00 107.00   0.50    2.20    --   95.80 -82.00  60.00  156
 23  \w     97.00 123.00   0.50    2.20    --   95.80 -82.00 150.00   52
 24  \w     38.00 112.00   0.50    2.20    --   95.80 -30.00 120.00  148
 25  \w     84.00 109.00   0.50    2.20    --   95.80 -82.00 -60.00   50
 26  \w     97.00 148.00   0.50    2.20    --   95.80  82.00  90.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0946156000
_diffrn_orient_matrix_UB_12      -0.0274402000
_diffrn_orient_matrix_UB_13      -0.0350083000
_diffrn_orient_matrix_UB_21      0.0576055000
_diffrn_orient_matrix_UB_22      -0.0204841000
_diffrn_orient_matrix_UB_23      -0.0443715000
_diffrn_orient_matrix_UB_31      -0.0258184000
_diffrn_orient_matrix_UB_32      -0.0875711000
_diffrn_orient_matrix_UB_33      0.0160659000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65292
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        65.500
_diffrn_reflns_theta_max         65.499
_diffrn_reflns_theta_min         2.697
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellowish yellow'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             2875
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.411
_refine_diff_density_min         -2.480
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1504
_refine_ls_number_reflns         21270
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+46.5089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16582
_reflns_number_total             21270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr03095d2.cif
_cod_data_source_block           Ag6-Rac
_cod_depositor_comments
'Adding full bibliography for 1569433--1569435.cif.'
_cod_database_code               1569435
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.453
_shelx_estimated_absorpt_t_min   0.352
_reflns_odcompleteness_completeness 99.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 S3-C123 = S4-C126
 1.75 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C123) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(N19)
\\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(N17) \\sim Ueq,
Uanis(N16) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(S4) \\sim Ueq, Uanis(S3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C120) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag7) = Uanis(Ag6)
4. Others
 Sof(Ag7)=1-FVAR(1)
 Sof(Ag6)=FVAR(1)
 Sof(N14)=Sof(H14)=Sof(N16)=Sof(C126)=Sof(N15)=Sof(C125)=Sof(H125)=Sof(S4)=1-
 FVAR(2)
 Sof(S3)=Sof(C124)=Sof(H124)=Sof(C123)=Sof(N17)=Sof(N19)=Sof(H19A)=Sof(N18)=
 FVAR(2)
 Fixed Sof: Ag2(0.95)
5.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 N14(H14), C107(H107), C101(H101), C90(H90), C9(H9), C117(H117), C103(H103),
 C91(H91), C108(H108), C14(H14A), C92(H92), C95(H95), C88(H88), C34(H34),
 C40(H40), C35(H35), C7(H7A), C22(H22), C84(H84), C116(H116), C80(H80),
 C42(H42), C121(H121), C99(H99), C16(H16), C113(H113), C18(H18), C89(H89),
 C110(H110), C85(H85), C39(H39), C72(H72), C2(H2), C77(H77), C12(H12), C76(H76),
  C63(H63), C74(H74), C97(H97), C45(H45), C114(H114), C83(H83), C6(H6),
 C11(H11), C112(H112), C102(H102), C87(H87), C73(H73), C15(H15), C96(H96),
 C66(H66), C44(H44), C115(H115), C31(H31), C36(H36), C33(H33), C10(H10),
 C47(H47), C5(H5), C106(H106), C21(H21), C98(H98), C29(H29), C4(H4), C58(H58),
 C70(H70), C105(H105), C38(H38), C78(H78), C32(H32), C48(H48), C59(H59),
 C19(H19), C67(H67), C86(H86), C62(H62), C3(H3), C68(H68), C20(H20), C69(H69),
 C61(H61), C79(H79), C54(H54), C28(H28), C51(H51), C125(H125), C37(H37),
 C25(H25), C120(H120), C49(H49), C50(H50), C55(H55), C27(H27), C56(H56),
 C57(H57), C60(H60), C26(H26), C124(H124), N19(H19A)
;
_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 1.756
_oxdiff_exptl_absorpt_empirical_full_min 0.431