Understanding the decomposition process of the Pt1Ag24(SPhCl2)18 nanocluster at the atomic level
Jiang, Kefan; Ma, Along; Li, Yuansheng; Wang, Jiawei; Yin, Zhengmao; Wang, Shuxin; RSC Advances 14 (2024) 10574–10579; doi:10.1039/D4RA01274G

data_7248374
_publ_section_title
;
 Understanding the decomposition process of the Pt1Ag24(SPhCl2)18
 nanocluster at the atomic level
;
_journal_issue                   15
_journal_name_full               'RSC Advances'
_journal_page_first              10574
_journal_page_last               10579
_journal_paper_doi               10.1039/D4RA01274G
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety
'0.333(Ag24 Br12.071 C120 Cl15.88 Pt S20), 0.333(Ag24 Br13.14 C120 Cl13.72 Pt S20), 0.333(Ag24 Br12.58 C120 Cl14.84 Pt S20), 2.667(C24 P), 0.867[C24PH20]'
_chemical_formula_sum
'C184 H120.67 Ag24 Br12.49 Cl15.03 P2.67 Pt S20'
_chemical_formula_weight         7369.73
_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             2024-01-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-20 deposited with the CCDC.	2024-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                93.09
_cell_angle_beta                 90.67
_cell_angle_gamma                90.79
_cell_formula_units_Z            3
_cell_length_a                   26.638
_cell_length_b                   29.956
_cell_length_c                   31.053
_cell_measurement_reflns_used    1543
_cell_measurement_temperature    120
_cell_measurement_theta_max      130.15
_cell_measurement_theta_min      5.53
_cell_volume                     24739.000
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.86, Darmstadt 2018
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
 1559 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            165059
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.759
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    16.342
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10449
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.492
_refine_diff_density_min         -2.317
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3334
_refine_ls_number_reflns         86370
_refine_ls_number_restraints     3301
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1073P)^2^+7.5674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1850
_reflns_d_resolution_high        0.822
_reflns_d_resolution_low         13.317
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              29
_reflns_limit_h_min              -32
_reflns_limit_k_max              19
_reflns_limit_k_min              -36
_reflns_limit_l_max              37
_reflns_limit_l_min              -33
_reflns_number_gt                56187
_reflns_number_total             90081
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d4ra01274g2.cif
_cod_data_source_block           1
_cod_original_cell_volume        24739.4
_cod_database_code               7248374
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.394
_shelx_estimated_absorpt_t_min   0.267
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Cl30, Br17}
{Cl22, Br3}
{Cl24, Br15}
{Br10, Cl14}
{Br13, Cl28}
{Br14, Cl2}
{Cl5, Br4}
{Cl21, Br18}
{Br1, Cl10}
{Br2, Cl9}
{Br24, Cl13}
{Cl27, Br5}
{Br19, Cl38}
{Cl19, Br9}
{Cl3, Br30}
{Cl32, Br25}
{Cl35, Br6}
{Cl26, Br16}
{Cl34, Br7}
3. Restrained distances
 Cl20-C144
 1.75 with sigma of 0.01
 Cl33-C61
 1.75 with sigma of 0.01
 Cl31-C147
 1.75 with sigma of 0.01
 Cl19-C146
 1.9 with sigma of 0.01
 C276-Cl19 \\sim Cl19-C273
 with sigma of 0.02
 C142-Cl20 \\sim Cl20-C135
 with sigma of 0.02
 C235-Cl33 \\sim Cl33-C171
 with sigma of 0.02
 C276-Cl31 \\sim Cl31-C274
 with sigma of 0.02
 C126-Cl9 \\sim Cl9-C235
 with sigma of 0.02
4. Restrained planarity
 Cl15, Cl26, C45, C82, C145, C270, C271, C272
 with sigma of 0.1
 Cl19, C23, C146, C147, C273, C274, C276
 with sigma of 0.1
 Cl20, C135, C140, C142, C144
 with sigma of 0.1
 Cl33, C30, C61, C171, C235
 with sigma of 0.1
 Cl33, C61, C126, C235
 with sigma of 0.1
 Cl31, C23, C147, C274, C276
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Cl31 \\sim S7 \\sim C23 \\sim C146 \\sim C147 \\sim C273 \\sim C274 \\sim C276
\\sim Br9: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
Ag36 \\sim Cl15 \\sim S29 \\sim C45 \\sim C82 \\sim C145 \\sim C270 \\sim C271
\\sim C272 \\sim Br16: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3.8A
S26 \\sim C80 \\sim C141 \\sim C143 \\sim C264 \\sim C266 \\sim C268 \\sim
Br29: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
P3 \\sim C4 \\sim C11 \\sim C33 \\sim C42 \\sim C76 \\sim C78 \\sim C91 \\sim
C128 \\sim C136 \\sim C137 \\sim C139 \\sim C160 \\sim C166 \\sim C176 \\sim
C186 \\sim C198 \\sim C248 \\sim C253 \\sim C255 \\sim C257 \\sim C260 \\sim
C261 \\sim C263 \\sim C269: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
S3 \\sim C19 \\sim C116 \\sim C118 \\sim C214 \\sim C216 \\sim C218 \\sim Br26:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
Cl15 \\sim C45 \\sim C82 \\sim C145 \\sim C270 \\sim C271 \\sim C272 \\sim
Br16: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl31 \\sim C23 \\sim C146 \\sim C147 \\sim C273 \\sim C274 \\sim C276 \\sim
Br9: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
Cl33 \\sim S21 \\sim C28 \\sim C30 \\sim C61 \\sim C126 \\sim C171 \\sim C235:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C146) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl9) \\sim Ueq, Uanis(Br2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Br9) \\sim Ueq, Uanis(Cl19) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl30) = Uanis(Br17)
Uanis(Cl32) = Uanis(Br25)
Uanis(Cl27) = Uanis(Br5)
Uanis(Br2) = Uanis(Cl9)
Uanis(Cl22) = Uanis(Br3)
Uanis(Cl19) = Uanis(Br9)
Uanis(Cl24) = Uanis(Br15)
Uanis(Cl26) = Uanis(Br16)
Uanis(Br10) = Uanis(Cl14)
Uanis(Br24) = Uanis(Cl13)
Uanis(Br13) = Uanis(Cl28)
Uanis(Br19) = Uanis(Cl38)
Uanis(Br14) = Uanis(Cl2)
Uanis(Cl3) = Uanis(Br30)
Uanis(Cl5) = Uanis(Br4)
Uanis(Cl35) = Uanis(Br6)
Uanis(Cl21) = Uanis(Br18)
Uanis(Br1) = Uanis(Cl10)
Uanis(Cl34) = Uanis(Br7)
6. Others
 Fixed Sof: Cl4(0.79) Cl5(0.93) Cl6(0.56) Cl7(0.6) Cl9(0.59) Cl10(0.56)
 Cl13(0.5) Cl21(0.6) Cl23(0.93) Cl27(0.79) Cl33(0.59) Cl37(0.5) Br1(0.44)
 Br2(0.41) Br4(0.07) Br5(0.21) Br18(0.4) Br24(0.5) Cl3(0.45) Cl8(0.78)
 Cl11(0.78) Cl15(0.6) Cl17(0.61) Cl19(0.35) Cl25(0.3) Cl26(0.6) Cl29(0.45)
 Cl31(0.35) Cl32(0.61) Cl34(0.78) Cl35(0.78) Cl38(0.3) Br6(0.22) Br7(0.22)
 Br9(0.65) Br16(0.4) Br19(0.7) Br25(0.39) Br30(0.55) Cl1(0.32) Cl2(0.81)
 Cl14(0.32) Cl16(0.81) Cl18(0.66) Cl20(0.4) Cl22(0.58) Cl24(0.66) Cl28(0.4)
 Cl30(0.66) Cl36(0.66) Cl39(0.58) Br3(0.42) Br10(0.68) Br13(0.6) Br14(0.19)
 Br15(0.34) Br17(0.34)
7.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C18(H18), C22(H22), C126(H126), C28(H28), C235(H235), C31(H31),
 C34(H34), C36(H36), C40(H40), C46(H46), C53(H53), C55(H55), C59(H59), C60(H60),
  C64(H64), C66(H66), C72(H72), C75(H75), C90(H90), C92(H92), C94(H94),
 C110(H110), C112(H112), C117(H117), C125(H125), C151(H151), C161(H161),
 C169(H169), C217(H217), C220(H220), C226(H226), C242(H242), C265(H265),
 C39(H39), C241(H241), C73(H73), C45(H45), C271(H271), C82(H82), C93(H93),
 C168(H168), C170(H170), C95(H95), C99(H99), C182(H182), C101(H101), C247(H247),
  C249(H249), C134(H134), C273(H273), C23(H23), C276(H276), C206(H206),
 C208(H208), C114(H114), C214(H214), C116(H116), C19(H19), C218(H218),
 C122(H122), C227(H227), C229(H229), C124(H124), C250(H250), C252(H252),
 C32(H32), C13(H13), C26(H26), C49(H49), C71(H71), C86(H86), C108(H108),
 C109(H109), C200(H200), C202(H202), C111(H111), C121(H121), C43(H43),
 C138(H138), C142(H142), C141(H141), C80(H80), C266(H266), C268(H268),
 C148(H148), C149(H149), C157(H157), C165(H165), C173(H173), C177(H177),
 C181(H181), C191(H191), C193(H193), C203(H203), C207(H207), C221(H221),
 C231(H231), C232(H232), C238(H238), C267(H267), C1(H1), C10(H10), C17(H17),
 C20(H20), C29(H29), C38(H38), C47(H47), C62(H62), C88(H88), C115(H115),
 C131(H131), C133(H133), C153(H153), C175(H175), C179(H179), C189(H189),
 C199(H199), C211(H211), C212(H212), C240(H240), C15(H15), C154(H154), C87(H87),
  C50(H50), C158(H158), C37(H37), C63(H63), C67(H67), C233(H233), C105(H105),
 C223(H223), C74(H74), C83(H83), C107(H107), C120(H120), C162(H162), C164(H164),
  C188(H188), C194(H194), C237(H237), C11(H11), C33(H33), C76(H76), C253(H253),
 C136(H136), C255(H255), C257(H257), C78(H78), C260(H260), C139(H139), C4(H4),
 C263(H263), C91(H91), C128(H128), C137(H137), C160(H160), C166(H166),
 C176(H176), C186(H186), C198(H198), C14(H14), C48(H48), C54(H54), C58(H58),
 C152(H152), C209(H209), C96(H96), C185(H185), C65(H65), C85(H85), C97(H97),
 C103(H103), C178(H178), C192(H192), C197(H197), C213(H213), C239(H239),
 C244(H244), C258(H258), C275(H275)
7.b Fitted hexagon refined as free rotating group:
 C30(C126,C28,C171,C61,C235), C217(C25,C220,C222,C224,C226), C39(C241,C130,
 C243,C73,C245), C45(C270,C145,C271,C82,C272), C93(C168,C9,C170,C95,C172),
 C99(C180,C56,C182,C101,C184), C132(C247,C21,C249,C134,C251), C146(C273,C23,
 C274,C147,C276), C206(C113,C208,C35,C210,C114), C214(C116,C216,C19,C218,C118),
 C225(C122,C227,C69,C229,C124), C250(C252,C254,C256,C32,C259), C109(C200,C5,
 C202,C111,C204), C135(C43,C138,C140,C142,C144), C141(C264,C80,C266,C143,C268),
 C15(C154,C87,C156,C50,C158), C63(C67,C233,C190,C105,C223), C76(C253,C136,C255,
 C42,C257), C78(C260,C139,C261,C4,C263), C58(C152,C183,C209,C96,C185)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62887
_shelx_hkl_checksum              2343
_shelx_fab_checksum              96884
_olex2_submission_special_instructions 'No special instructions were received'