Doping-Induced Anisotropic Self-Assembly of Silver Icosahedra in [Pt2Ag23Cl7(PPh3)10] Nanoclusters.
Bootharaju, Megalamane S.; Kozlov, Sergey M.; Cao, Zhen; Harb, Moussab; Maity, Niladri; Shkurenko, Aleksander; Parida, Manas R.; Hedhili, Mohamed N.; Eddaoudi, Mohamed; Mohammed, Omar F.; Bakr, Osman M.; Cavallo, Luigi; Basset, Jean-Marie; Journal of the American Chemical Society 139 (2017) 1053–1056; doi:10.1021/jacs.6b11875

data_4125839
_publ_section_title
;
 Doping-Induced Anisotropic Self-Assembly of Silver Icosahedra in
 [Pt2Ag23Cl7(PPh3)10] Nanoclusters.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1053
_journal_page_last               1056
_journal_paper_doi               10.1021/jacs.6b11875
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C180 H150 Ag23 Cl7 P10 Pt2'
_chemical_formula_sum            'C180 H150 Ag23 Cl7 P10 Pt2'
_chemical_formula_weight         5742.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.843(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.5654(9)
_cell_length_b                   23.626(2)
_cell_length_c                   30.091(2)
_cell_measurement_reflns_used    8931
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      40.22
_cell_measurement_theta_min      3.33
_cell_volume                     11434.8(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35250
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        39.971
_diffrn_reflns_theta_max         39.971
_diffrn_reflns_theta_min         1.512
_exptl_absorpt_coefficient_mu    19.313
_exptl_absorpt_correction_T_max  0.1169
_exptl_absorpt_correction_T_min  0.0360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1458 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.3080.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       prism
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         3.995
_refine_diff_density_min         -2.730
_refine_diff_density_rms         0.554
_refine_ls_extinction_coef       0.00016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   2.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         6877
_refine_ls_number_restraints     1246
_refine_ls_restrained_S_all      1.861
_refine_ls_R_factor_all          0.2247
_refine_ls_R_factor_gt           0.1646
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4440
_refine_ls_wR_factor_ref         0.4827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4435
_reflns_number_total             6877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11875_si_002.cif
_cod_data_source_block           ag23pt2
_cod_original_cell_volume        11435(1)
_cod_database_code               4125839
_shelx_estimated_absorpt_t_max   0.068
_shelx_estimated_absorpt_t_min   0.037
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C513-C513_$1
 -3.48 with sigma of 0.02
 P2-C212 \\sim P2-C216
 with sigma of 0.01
 P2-C222 \\sim P2-C226
 with sigma of 0.01
 P2-C232 \\sim P2-C236
 with sigma of 0.01
 P3-C312 \\sim P3-C316
 with sigma of 0.01
 P3-C322 \\sim P3-C326
 with sigma of 0.01
 P3-C332 \\sim P3-C336
 with sigma of 0.01
 P3-C342 \\sim P3-C346
 with sigma of 0.01
 P3-C352 \\sim P3-C356
 with sigma of 0.01
 P3-C362 \\sim P3-C366
 with sigma of 0.01
 P4-C412 \\sim P4-C416
 with sigma of 0.01
 P4-C422 \\sim P4-C426
 with sigma of 0.01
 P4-C432 \\sim P4-C436
 with sigma of 0.01
 P5-C512 \\sim P5-C516
 with sigma of 0.01
 P5-C522 \\sim P5-C526
 with sigma of 0.01
 P5-C532 \\sim P5-C536
 with sigma of 0.01
 P6-C612 \\sim P6-C616
 with sigma of 0.01
 P6-C622 \\sim P6-C626
 with sigma of 0.01
 P6-C632 \\sim P6-C636
 with sigma of 0.01
 P6-C642 \\sim P6-C646
 with sigma of 0.01
 P6-C652 \\sim P6-C656
 with sigma of 0.01
 P6-C662 \\sim P6-C666
 with sigma of 0.01
 P2-C211 \\sim P2-C221 \\sim P2-C231 \\sim P3-C311 \\sim P3-C321 \\sim P3-C331
\\sim P3-C341 \\sim P3-C351
 \\sim P3-C361 \\sim P4-C411 \\sim P4-C421 \\sim P4-C431 \\sim P5-C511 \\sim
P5-C521 \\sim P5-C531 \\sim P6-
 C611 \\sim P6-C621 \\sim P6-C631 \\sim P6-C641 \\sim P6-C651 \\sim P6-C661
 with sigma of 0.01
3. Restrained planarity
 P2, C211, C212, C213, C214, C215, C216
 with sigma of 0.02
 P2, C221, C222, C223, C224, C225, C226
 with sigma of 0.02
 P2, C231, C232, C233, C234, C235, C236
 with sigma of 0.02
 P3, C311, C312, C313, C314, C315, C316
 with sigma of 0.02
 P3, C321, C322, C323, C324, C325, C326
 with sigma of 0.02
 P3, C331, C332, C333, C334, C335, C336
 with sigma of 0.02
 P3, C341, C342, C343, C344, C345, C346
 with sigma of 0.02
 P3, C351, C352, C353, C354, C355, C356
 with sigma of 0.02
 P3, C361, C362, C363, C364, C365, C366
 with sigma of 0.02
 P4, C411, C412, C413, C414, C415, C416
 with sigma of 0.02
 P4, C421, C422, C423, C424, C425, C426
 with sigma of 0.02
 P4, C431, C432, C433, C434, C435, C436
 with sigma of 0.02
 P5, C511, C512, C513, C514, C515, C516
 with sigma of 0.02
 P5, C521, C522, C523, C524, C525, C526
 with sigma of 0.02
 P5, C531, C532, C533, C534, C535, C536
 with sigma of 0.02
 P6, C611, C612, C613, C614, C615, C616
 with sigma of 0.02
 P6, C621, C622, C623, C624, C625, C626
 with sigma of 0.02
 P6, C631, C632, C633, C634, C635, C636
 with sigma of 0.02
 P6, C641, C642, C643, C644, C645, C646
 with sigma of 0.02
 P6, C651, C652, C653, C654, C655, C656
 with sigma of 0.02
 P6, C661, C662, C663, C664, C665, C666
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C221 \\sim C222 \\sim C223 \\sim C224 \\sim C225 \\sim C226: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C231 \\sim C232 \\sim C233 \\sim C234 \\sim C235 \\sim C236: within 2A with
sigma of 0.06 and sigma for terminal atoms of 0.12
C311 \\sim C312 \\sim C313 \\sim C314 \\sim C315 \\sim C316: within 2A with
sigma of 0.05 and sigma for terminal atoms of 0.1
C321 \\sim C322 \\sim C323 \\sim C324 \\sim C325 \\sim C326: within 2A with
sigma of 0.05 and sigma for terminal atoms of 0.1
C331 \\sim C332 \\sim C333 \\sim C334 \\sim C335 \\sim C336: within 2A with
sigma of 0.05 and sigma for terminal atoms of 0.1
C341 \\sim C342 \\sim C343 \\sim C344 \\sim C345 \\sim C346: within 2A with
sigma of 0.06 and sigma for terminal atoms of 0.12
C351 \\sim C352 \\sim C353 \\sim C354 \\sim C355 \\sim C356: within 2A with
sigma of 0.05 and sigma for terminal atoms of 0.1
C361 \\sim C362 \\sim C363 \\sim C364 \\sim C365 \\sim C366: within 2A with
sigma of 0.05 and sigma for terminal atoms of 0.1
C411 \\sim C412 \\sim C413 \\sim C414 \\sim C415 \\sim C416: within 2A with
sigma of 0.07 and sigma for terminal atoms of 0.14
C421 \\sim C422 \\sim C423 \\sim C424 \\sim C425 \\sim C426: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C431 \\sim C432 \\sim C433 \\sim C434 \\sim C435 \\sim C436: within 2A with
sigma of 0.05 and sigma for terminal atoms of 0.1
C511 \\sim C512 \\sim C513 \\sim C514 \\sim C515 \\sim C516: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C521 \\sim C522 \\sim C523 \\sim C524 \\sim C525 \\sim C526: within 2A with
sigma of 0.07 and sigma for terminal atoms of 0.14
C531 \\sim C532 \\sim C533 \\sim C534 \\sim C535 \\sim C536: within 2A with
sigma of 0.05 and sigma for terminal atoms of 0.1
C611 \\sim C612 \\sim C613 \\sim C614 \\sim C615 \\sim C616: within 2A with
sigma of 0.06 and sigma for terminal atoms of 0.12
C621 \\sim C622 \\sim C623 \\sim C624 \\sim C625 \\sim C626: within 2A with
sigma of 0.06 and sigma for terminal atoms of 0.12
C631 \\sim C632 \\sim C633 \\sim C634 \\sim C635 \\sim C636: within 2A with
sigma of 0.05 and sigma for terminal atoms of 0.1
C641 \\sim C642 \\sim C643 \\sim C644 \\sim C645 \\sim C646: within 2A with
sigma of 0.06 and sigma for terminal atoms of 0.12
C651 \\sim C652 \\sim C653 \\sim C654 \\sim C655 \\sim C656: within 2A with
sigma of 0.06 and sigma for terminal atoms of 0.12
C661 \\sim C662 \\sim C663 \\sim C664 \\sim C665 \\sim C666: within 2A with
sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(C211) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C221) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C231) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(C312) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.12
Uanis(C315) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(C321) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C322) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C331) \\sim Ueq, Uanis(C336) \\sim Ueq: with sigma of 0.07 and sigma for
terminal atoms of 0.14
Uanis(C341) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(C344) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C345) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(C411) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C421) \\sim Ueq, Uanis(C424) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C431) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(C511) \\sim Ueq, Uanis(C514) \\sim Ueq: with sigma of 0.07 and sigma for
terminal atoms of 0.14
Uanis(C521) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C531) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.12
Uanis(C536) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.12
Uanis(C611) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C613) \\sim Ueq, Uanis(C614) \\sim Ueq: with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C621) \\sim Ueq: with sigma of 0.12 and sigma for terminal atoms of 0.24
Uanis(C623) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C631) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.1
Uanis(C636) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.1
Uanis(C662) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C621) = Uanis(C651)
Uanis(C311) = Uanis(C341)
Uanis(C314) = Uanis(C344)
Uanis(C326) = Uanis(C356) = Uanis(C322) = Uanis(C352)
Uanis(C325) = Uanis(C355) = Uanis(C323) = Uanis(C353)
Uanis(C321) = Uanis(C351)
Uanis(C324) = Uanis(C354)
Uanis(C331) = Uanis(C361)
Uanis(C616) = Uanis(C646) = Uanis(C612) = Uanis(C642)
Uanis(C641) = Uanis(C611)
Uanis(C643) = Uanis(C613) = Uanis(C615) = Uanis(C645)
Uanis(C644) = Uanis(C614)
Uanis(C631) = Uanis(C661)
5. Others
 Fixed Sof: C311(0.5) C312(0.5) H312(0.5) C313(0.5) H313(0.5) C314(0.5)
 H314(0.5) C315(0.5) H315(0.5) C316(0.5) H316(0.5) C321(0.5) C322(0.5)
 H322(0.5) C323(0.5) H323(0.5) C324(0.5) H324(0.5) C325(0.5) H325(0.5)
 C326(0.5) H326(0.5) C331(0.5) C332(0.5) H332(0.5) C333(0.5) H333(0.5)
 C334(0.5) H334(0.5) C335(0.5) H335(0.5) C336(0.5) H336(0.5) C611(0.5)
 C612(0.5) H612(0.5) C613(0.5) H613(0.5) C614(0.5) H614(0.5) C615(0.5)
 H615(0.5) C616(0.5) H616(0.5) C621(0.5) C622(0.5) H622(0.5) C623(0.5)
 H623(0.5) C624(0.5) H624(0.5) C625(0.5) H625(0.5) C626(0.5) H626(0.5)
 C631(0.5) C632(0.5) H632(0.5) C633(0.5) H633(0.5) C634(0.5) H634(0.5)
 C635(0.5) H635(0.5) C636(0.5) H636(0.5) C341(0.5) C342(0.5) H342(0.5)
 C343(0.5) H343(0.5) C344(0.5) H344(0.5) C345(0.5) H345(0.5) C346(0.5)
 H346(0.5) C351(0.5) C352(0.5) H352(0.5) C353(0.5) H353(0.5) C354(0.5)
 H354(0.5) C355(0.5) H355(0.5) C356(0.5) H356(0.5) C361(0.5) C362(0.5)
 H362(0.5) C363(0.5) H363(0.5) C364(0.5) H364(0.5) C365(0.5) H365(0.5)
 C366(0.5) H366(0.5) C641(0.5) C642(0.5) H642(0.5) C643(0.5) H643(0.5)
 C644(0.5) H644(0.5) C645(0.5) H645(0.5) C646(0.5) H646(0.5) C651(0.5)
 C652(0.5) H652(0.5) C653(0.5) H653(0.5) C654(0.5) H654(0.5) C655(0.5)
 H655(0.5) C656(0.5) H656(0.5) C661(0.5) C662(0.5) H662(0.5) C663(0.5)
 H663(0.5) C664(0.5) H664(0.5) C665(0.5) H665(0.5) C666(0.5) H666(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C222(H222), C223(H223), C224(H224), C225(H225), C226(H226), C232(H232),
 C233(H233), C234(H234), C235(H235), C236(H236), C412(H412), C413(H413),
 C414(H414), C415(H415), C416(H416), C422(H422), C423(H423), C424(H424),
 C425(H425), C426(H426), C432(H432), C433(H433), C434(H434), C435(H435),
 C436(H436), C512(H512), C513(H513), C514(H514), C515(H515), C516(H516),
 C522(H522), C523(H523), C524(H524), C525(H525), C526(H526), C532(H532),
 C533(H533), C534(H534), C535(H535), C536(H536), C212(H212), C213(H213),
 C214(H214), C215(H215), C216(H216), C312(H312), C313(H313), C314(H314),
 C315(H315), C316(H316), C322(H322), C323(H323), C324(H324), C325(H325),
 C326(H326), C332(H332), C333(H333), C334(H334), C335(H335), C336(H336),
 C612(H612), C613(H613), C614(H614), C615(H615), C616(H616), C622(H622),
 C623(H623), C624(H624), C625(H625), C626(H626), C632(H632), C633(H633),
 C634(H634), C635(H635), C636(H636), C342(H342), C343(H343), C344(H344),
 C345(H345), C346(H346), C352(H352), C353(H353), C354(H354), C355(H355),
 C356(H356), C362(H362), C363(H363), C364(H364), C365(H365), C366(H366),
 C642(H642), C643(H643), C644(H644), C645(H645), C646(H646), C652(H652),
 C653(H653), C654(H654), C655(H655), C656(H656), C662(H662), C663(H663),
 C664(H664), C665(H665), C666(H666)
6.b Fitted hexagon refined as free rotating group:
 C221(C222,C223,C224,C225,C226), C231(C232,C233,C234,C235,C236), C411(C412,
 C413,C414,C415,C416), C421(C422,C423,C424,C425,C426), C431(C432,C433,C434,C435,
 C436), C511(C512,C513,C514,C515,C516), C521(C522,C523,C524,C525,C526),
 C531(C532,C533,C534,C535,C536), C211(C212,C213,C214,C215,C216), C311(C312,C313,
 C314,C315,C316), C321(C322,C323,C324,C325,C326), C331(C332,C333,C334,C335,
 C336), C611(C612,C613,C614,C615,C616), C621(C622,C623,C624,C625,C626),
 C631(C632,C633,C634,C635,C636), C341(C342,C343,C344,C345,C346), C351(C352,C353,
 C354,C355,C356), C361(C362,C363,C364,C365,C366), C641(C642,C643,C644,C645,
 C646), C651(C652,C653,C654,C655,C656), C661(C662,C663,C664,C665,C666)
;
_shelx_fab_checksum              39038
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'