Thermochromism and piezochromism of an atomically precise high-nuclearity silver sulfide nanocluster.
Sun, Qiao-Qiao; Li, Qian; Li, Hai-Yang; Zhang, Miao-Miao; Sun, Meng-En; Li, Si; Quan, Zewei; Zang, Shuang-Quan; Chemical communications (Cambridge, England) 57 (2021) 2372–2375; doi:10.1039/d0cc07085h

data_7127868
_publ_section_title
;
 Thermochromism and piezochromism of an atomically precise high-nuclearity
 silver sulfide nanocluster.
;
_journal_issue                   19
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2372
_journal_page_last               2375
_journal_paper_doi               10.1039/d0cc07085h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C378 H300 Ag50 F36 P12 S43, 4(C5 H10 N2 O)'
_chemical_formula_sum            'C398 H340 Ag50 F36 N8 O4 P12 S43'
_chemical_formula_weight         13126.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-02 deposited with the CCDC.	2021-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.4521(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.0312(2)
_cell_length_b                   24.2172(2)
_cell_length_c                   33.2627(2)
_cell_measurement_reflns_used    69224
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7390
_cell_measurement_theta_min      2.6800
_cell_volume                     24081.6(3)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -83.00 -56.00   0.25    0.25    --    0.00 -38.00-150.00  108
  2  \w    -12.00  41.00   0.25    0.25    --    0.00  82.00 120.00  212
  3  \w    -40.00  17.00   0.25    0.25    --    0.00 -38.00  30.00  228
  4  \w    -72.00 -47.00   0.25    0.25    --    0.00 -38.00  30.00  100
  5  \w    -89.00  12.00   0.25    0.25    --    0.00 -38.00 -60.00  404
  6  \w     67.00 115.00   0.25    2.00    --   95.20 -15.00 -30.00  192
  7  \w     11.00  48.00   0.25    2.00    --   95.20 -15.00 -30.00  148
  8  \w     65.00 104.00   0.25    2.00    --   95.20 -45.00 -30.00  156
  9  \w     68.00  99.00   0.25    2.00    --   95.20  77.00   0.00  124
 10  \w      6.00 115.00   0.25    2.00    --   95.20 -30.00 -30.00  436
 11  \w    128.00 178.00   0.25    2.00    --   95.20  77.00   0.00  200
 12  \w      7.00 127.00   0.25    2.00    --   95.20 -82.00 -60.00  480
 13  \w      7.00  54.00   0.25    2.00    --   95.20 -61.00-120.00  188
 14  \w     21.00  49.00   0.25    2.00    --   95.20 -45.00 -30.00  112
 15  \w     86.00 173.00   0.25    2.00    --   95.20  77.00 -60.00  348
;
_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      -0.0180543000
_diffrn_orient_matrix_UB_12      0.0595318000
_diffrn_orient_matrix_UB_13      -0.0000846000
_diffrn_orient_matrix_UB_21      -0.0065338000
_diffrn_orient_matrix_UB_22      -0.0009100000
_diffrn_orient_matrix_UB_23      -0.0464873000
_diffrn_orient_matrix_UB_31      -0.0478361000
_diffrn_orient_matrix_UB_32      -0.0224019000
_diffrn_orient_matrix_UB_33      0.0016047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            139943
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        65.500
_diffrn_reflns_theta_max         65.500
_diffrn_reflns_theta_min         2.348
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.494
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       needle
_exptl_crystal_F_000             12716
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.062
_refine_diff_density_max         3.507
_refine_diff_density_min         -2.311
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2445
_refine_ls_number_reflns         41335
_refine_ls_number_restraints     710
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1621P)^2^+163.6168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2486
_refine_ls_wR_factor_ref         0.2581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34574
_reflns_number_total             41335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07085h2.cif
_cod_data_source_block           20190823d5_1_100_00
_cod_depositor_comments
'Adding full bibliography for 7127868--7127870.cif.'
_cod_original_cell_volume        24081.5(3)
_cod_database_code               7127868
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.87
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N8-C205 = N7-C202 = C202-C205
 1.5 with sigma of 0.01
 O4-C203 = O2-C195
 1.25 with sigma of 0.01
3. Restrained planarity
 F18, C134, C135, C136, C137, C138, C139
 with sigma of 0.01
 O2, N1, N3, C189, C190, C193, C195, C207
 with sigma of 0.01
 O4, N7, N8, C201, C202, C203, C204, C205
 with sigma of 0.01
4. Rigid bond restraints
 C171, C172
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C115, C116, C117, C118, C119, C120
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O4 \\sim N7 \\sim N8 \\sim C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O2 \\sim N1 \\sim N3 \\sim C189 \\sim C190 \\sim C193 \\sim C195 \\sim C207:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C177 \\sim C178 \\sim C179 \\sim C180 \\sim C181 \\sim C182: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C169 \\sim C170 \\sim C171 \\sim C173 \\sim C174: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C39 \\sim C42 \\sim C43 \\sim C44: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C115 \\sim C116 \\sim C117 \\sim C118 \\sim C119 \\sim C120: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
F18 \\sim C134 \\sim C135 \\sim C137: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C172 \\sim C173: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
F17 \\sim C127 \\sim C128 \\sim C129: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C60 \\sim C79 \\sim C108 \\sim C148 \\sim C168 \\sim C196: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
F18 \\sim C134 \\sim C135 \\sim C136 \\sim C137 \\sim C138 \\sim C139: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
F17 \\sim C124 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim C129: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
F12 \\sim C28 \\sim C159 \\sim C160 \\sim C166: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C147 \\sim C158 \\sim C183 \\sim C187 \\sim C198: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
F12 \\sim C28 \\sim C32 \\sim C114 \\sim C159 \\sim C160 \\sim C166: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C120 \\sim C119 \\sim C117 \\sim C116 \\sim C115 \\sim C118: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C165 \\sim C184 \\sim C150 \\sim C133 \\sim C70 \\sim C72: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C115 \\sim C116 \\sim C117 \\sim C118 \\sim C119 \\sim C120: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F12) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(C108)
\\sim Ueq, Uanis(C196) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(F6) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17)
\\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C91) \\sim Ueq,
Uanis(C98) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C116)
\\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq,
Uanis(C120) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C128) \\sim Ueq,
Uanis(C129) \\sim Ueq, Uanis(C134) \\sim Ueq, Uanis(C135) \\sim Ueq,
Uanis(C136) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(C144) \\sim Ueq,
Uanis(C145) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(C154) \\sim Ueq,
Uanis(C159) \\sim Ueq, Uanis(C160) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C163) \\sim Ueq, Uanis(C166) \\sim Ueq, Uanis(C176) \\sim Ueq,
Uanis(C183) \\sim Ueq, Uanis(C185) \\sim Ueq, Uanis(C186) \\sim Ueq,
Uanis(C198) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17)
\\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Others
 Sof(Ag27)=Sof(Ag28)=1-FVAR(1)
 Sof(Ag7)=Sof(Ag22)=FVAR(1)
 Fixed Sof: Ag25(0.5) Ag26(0.5) S22(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C38(H38A,H38B), C48(H48A,H48B), C49(H49A,H49B), C97(H97A,
 H97B), C98(H98A,H98B), C103(H10A,H10B), C104(H10C,H10D), C175(H17A,H17B),
 C189(H18A,H18B), C190(H19A,H19B), C202(H20G,H20H), C205(H20L,H20M)
7.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C13(H13), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
 C23(H23), C24(H24), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35),
  C37(H37), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
 C47(H47), C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57),
  C58(H58), C59(H59), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66),
 C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92),
  C94(H94), C95(H95), C100(H100), C101(H101), C102(H102), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C116(H116), C117(H117), C118(H118), C119(H119),
 C120(H120), C123(H123), C124(H124), C126(H126), C127(H127), C129(H129),
 C130(H130), C134(H134), C136(H136), C137(H137), C139(H139), C141(H141),
 C142(H142), C143(H143), C144(H144), C145(H145), C146(H146), C147(H147),
 C148(H148), C149(H149), C150(H150), C151(H151), C152(H152), C153(H153),
 C155(H155), C156(H156), C157(H157), C158(H158), C160(H160), C162(H162),
 C163(H163), C164(H164), C165(H165), C166(H166), C167(H167), C168(H168),
 C169(H169), C170(H170), C172(H172), C173(H173), C176(H176), C177(H177),
 C178(H178), C179(H179), C180(H180), C181(H181), C183(H183), C184(H184),
 C185(H185), C186(H186), C187(H187), C196(H196), C198(H198)
7.c Fitted hexagon refined as free rotating group:
 C39(C40,C41,C42,C43,C44), C115(C116,C117,C118,C119,C120), C124(C125,C126,C127,
 C128,C129), C134(C135,C136,C137,C138,C139), C169(C170,C171,C172,C173,C174),
 C177(C178,C179,C180,C181,C182)
7.d Idealised Me refined as rotating group:
 C193(H19C,H19D,H19E), C201(H20D,H20E,H20F), C204(H20I,H20J,H20K), C207(H20A,
 H20B,H20C)
;
_shelx_res_checksum              4398
_shelx_hkl_checksum              39946
_shelx_fab_checksum              44927
_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 3.116
_oxdiff_exptl_absorpt_empirical_full_min 0.577