Multi-Ligand-Directed Synthesis of Chiral Silver Nanoclusters
Zou, Xuejuan; Jin, Shan; Du, Wenjun; Li, Yangfeng; Wang, Shuxin; li, peng; Zhu, Manzhou; Nanoscale  (2017) –; doi:10.1039/C7NR06338E

data_1547469
_publ_section_title
;
 Multi-Ligand-Directed Synthesis of Chiral Silver Nanoclusters
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C7NR06338E
_journal_year                    2017
_chemical_formula_moiety
'C255 H300 Ag32 Cl8 P10 S13, 2.99(F6 Sb), C H2 Cl2'
_chemical_formula_sum            'C256 H303 Ag32 Cl10 F17.96 P10 S13 Sb3'
_chemical_formula_weight         8619.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                102.6310(10)
_cell_angle_beta                 98.3050(10)
_cell_angle_gamma                100.3720(10)
_cell_formula_units_Z            4
_cell_length_a                   24.4964(3)
_cell_length_b                   36.3669(5)
_cell_length_c                   38.1702(5)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.76
_cell_measurement_theta_min      2.22
_cell_volume                     32035.0(8)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_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_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1011
_diffrn_reflns_av_unetI/netI     0.1425
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            340624
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         0.701
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.423
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0814 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.8565.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour
&#x00EF;&#x00BF;&#x00BD;&#x00EF;&#x00BF;&#x00BD;black&#x00EF;&#x00BF;&#x00BD;&#x00EF;&#x00BF;&#x00BD;
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_description       block
_exptl_crystal_F_000             16743
_refine_diff_density_max         8.879
_refine_diff_density_min         -4.678
_refine_diff_density_rms         0.368
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     5841
_refine_ls_number_reflns         116936
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1980
_refine_ls_R_factor_gt           0.1140
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1917P)^2^+528.6930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3027
_refine_ls_wR_factor_ref         0.3656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                58841
_reflns_number_total             116936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nr06338e2.cif
_cod_data_source_block           20170324a_1_0m
_cod_original_cell_volume        32035.0(7)
_cod_database_code               1547469
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Sb4-F101 = Sb4-F47 = Sb4-F69 = Sb4-F194 = Sb4-F63
 1.837 with sigma of 0.02
 Sb0A-F219
 1.837 with sigma of 0.02
 C9YA-C0ZA
 1.6 with sigma of 0.02
 Sb0A-F158
 1.85 with sigma of 0.02
 Sb0A-F190
 1.85 with sigma of 0.02
 Sb0A-F218
 1.85 with sigma of 0.02
 Sb0A-F152
 1.85 with sigma of 0.02
 Sb4-F55
 1.85 with sigma of 0.02
 Sb3-F9
 1.85 with sigma of 0.02
 F68-Sb2 = Sb2-F199
 1.85 with sigma of 0.02
 C9YA-C2ZA
 1.4 with sigma of 0.02
 C1ZA-C2ZA
 1.4 with sigma of 0.02
 C7WA-C6WA
 1.5 with sigma of 0.02
 C6XA-C7XA
 1.5 with sigma of 0.02
 C5XA-C6XA
 1.5 with sigma of 0.02
 C7XA-C6XA
 1.5 with sigma of 0.02
 C0XA-C1XA
 1.5 with sigma of 0.02
 C246-C0XA
 1.5 with sigma of 0.02
 C1PA-C2PA
 1.5 with sigma of 0.02
 C2PA-C3PA
 1.5 with sigma of 0.02
 C43-C1FA
 1.5 with sigma of 0.02
 C43-C174
 1.5 with sigma of 0.02
 C43-C4IA
 1.5 with sigma of 0.02
 C174-C6WA
 1.5 with sigma of 0.02
 C1FA-C2FA
 1.5 with sigma of 0.02
 C4IA-C204
 1.5 with sigma of 0.02
 C7WA-C204
 1.5 with sigma of 0.02
 C204-C8WA
 1.5 with sigma of 0.02
 C8WA-C2FA
 1.5 with sigma of 0.02
 C2FA-C173
 1.5 with sigma of 0.02
 C173-C6WA
 1.5 with sigma of 0.02
 C6WA-C7WA
 1.5 with sigma of 0.02
 P2V-C100
 1.72 with sigma of 0.02
 P33-C59
 1.78 with sigma of 0.02
 P2P-C59
 1.83 with sigma of 0.02
 C59-P33
 1.77 with sigma of 0.02
 P33-C5IA
 1.76 with sigma of 0.02
 C160-C3JA
 1.5 with sigma of 0.02
 C3JA-C7RA
 1.5 with sigma of 0.02
 F219-F152
 2.67 with sigma of 0.04
 F152-F276
 2.67 with sigma of 0.04
 F190-F219
 2.67 with sigma of 0.04
 C246-C1XA
 2.5 with sigma of 0.04
 C1PA-C3PA
 2.5 with sigma of 0.04
 C1FA-C174
 2.5 with sigma of 0.04
 C1FA-C4IA
 2.5 with sigma of 0.04
 C174-C4IA
 2.5 with sigma of 0.04
 C7WA-C8WA
 2.5 with sigma of 0.04
 C4IA-C174
 2.5 with sigma of 0.04
 C204-C6WA
 2.5 with sigma of 0.04
 C43-C2FA
 2.5 with sigma of 0.04
 C6WA-C2FA
 2.5 with sigma of 0.04
 C43-C204
 2.5 with sigma of 0.04
 C2FA-C204
 2.5 with sigma of 0.04
 C6WA-C43
 2.5 with sigma of 0.04
 C173-C7WA
 2.5 with sigma of 0.04
 H7WB-H234
 2 with sigma of 0.04
 C0EA-C280
 4.2 with sigma of 0.04
 C56-C2VA
 3.9 with sigma of 0.04
 C280-C0EA
 4 with sigma of 0.04
 C2EA-C0VA
 3.7 with sigma of 0.04
 H7WA-H234
 1.9 with sigma of 0.04
 C59-C98
 3.1 with sigma of 0.04
 C98-P2P
 2.7 with sigma of 0.04
 C0EA-C2VA
 4 with sigma of 0.04
 C56-C3VA
 3.6 with sigma of 0.04
 C1EA-C1VA
 3.8 with sigma of 0.04
 C8IA-C172
 3.2 with sigma of 0.04
3. Restrained planarity
 F152, F218, Sb0A, F190, F158
 with sigma of 0.1
 F219, F152, Sb0A, F190, F276
 with sigma of 0.1
 F219, Sb0A, F276, F218, F158
 with sigma of 0.1
 C174, C6WA, C204, C4IA
 with sigma of 0.1
 C7WA, C8WA, C2FA, C6WA
 with sigma of 0.1
 C100, C8EA, C7IA, C122, C63, C172, P2V
 with sigma of 0.1
 F218, F219, F158, F276, Sb0A
 with sigma of 0.1
 P2L, C9EA, C8IA, C0FA, C4VA, C0JA, C9IA
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C81(H81), C84(H84), C96(H96), C101(H101), C107(H107), C127(H127), C1AA(H1AA),
 C165(H165), C175(H175), C177(H177), C178(H178), C182(H182), C193(H193),
 C196(H196), C7AA(H7AA), C5CA(H5CA), C2AA(H2AA), C4AA(H4AA), C3CA(H3CA),
 C4GA(H4GA), C1GA(H1GA), C5AA(H5AA), C9CA(H9CA), C164(H164), C171(H171),
 C2BA(H2BA), C179(H179), C2FA(H2FA), C62(H62), C80(H80), C4NA(H4NA), C7NA(H7NA),
  C1MA(H1MA), C9KA(H9KA), C1LA(H1LA), C3MA(H3MA), C128(H128), C4OA(H4OA),
 C1IA(H1IA), C2LA(H2LA), C149(H149), C9GA(H9GA), C7MA(H7MA), C9WA(H9WA),
 C3JA(H3JA), C1HA(H1HA), C3PA(H3PA), C5TA(H5TA), C1PA(H1PA), C6QA(H6QA),
 C6WA(H6WA), C1WA(H1WA), C9B(H9B), C6OA(H6OA), C7QA(H7QA), C1UA(H1UA),
 C5PA(H5PA), C4UA(H4UA), C202(H202), C204(H204), C211(H211), C217(H217),
 C218(H218), C222(H222), C237(H237), C246(H246), C257(H257), C258(H258),
 C273(H273), C282(H282), C4BB(H4BB), C6BB(H6BB), C7XA(H7XA), C9YA(H9YA),
 C1ZA(H1ZA), C1XA(H1XA), C5XA(H5XA), C209(H209)
5.b Secondary CH2 refined with riding coordinates:
 C146(H14A,H14B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B), C45(H45A,
 H45B), C3HA(H3HA,H3HB), C58(H58A,H58B), C59(H59A,H59B), C66(H66A,H66B),
 C71(H71A,H71B), C6HA(H6HA,H6HB), C83(H83A,H83B), C85(H85A,H85B), C8HA(H8HA,
 H8HB), C89(H89A,H89B), C9HA(H9HA,H9HB), C99(H99A,H99B), C102(H10A,H10B),
 C106(H10C,H10D), C108(H10E,H10F), C114(H11A,H11B), C116(H11C,H11D), C117(H11E,
 H11F), C120(H12A,H12B), C123(H12E,H12F), C124(H12C,H12D), C0AA(H0AA,H0AB),
 C138(H13C,H13D), C139(H13A,H13B), C145(H14C,H14D), C147(H14E,H14F), C151(H15A,
 H15B), C152(H15C,H15D), C154(H15E,H15F), C155(H15G,H15H), C163(H16A,H16B),
 C176(H17A,H17B), C185(H18A,H18B), C186(H18C,H18D), C188(H18E,H18F), C190(H19A,
 H19B), C48(H48A,H48B), C8AA(H8AA,H8AB), C6AA(H6AA,H6AB), C67(H67A,H67B),
 C9FA(H9FA,H9FB), C8FA(H8FA,H8FB), C95(H95A,H95B), C7GA(H7GA,H7GB), C110(H11G,
 H11H), C113(H11I,H11J), C3GA(H3GA,H3GB), C3AA(H3AA,H3AB), C7EA(H7EA,H7EB),
 C7FA(H7FA,H7FB), C4CA(H4CA,H4CB), C0GA(H0GA,H0GB), C5GA(H5GA,H5GB), C6EA(H6EA,
 H6EB), C9BA(H9BA,H9BB), C169(H16C,H16D), C1FA(H1FA,H1FB), C6CA(H6CA,H6CB),
 C0DA(H0DA,H0DB), C189(H18G,H18H), C200(H20A,H20B), C7LA(H7LA,H7LB), C52(H52A,
 H52B), C69(H69A,H69B), C5NA(H5NA,H5NB), C0MA(H0MA,H0MB), C86(H86A,H86B),
 C97(H97A,H97B), C9LA(H9LA,H9LB), C0IA(H0IA,H0IB), C105(H10G,H10H), C3LA(H3LA,
 H3LB), C6NA(H6NA,H6NB), C3OA(H3OA,H3OB), C8NA(H8NA,H8NB), C4LA(H4LA,H4LB),
 C0A(H0AC,H0AD), C134(H13E,H13F), C2HA(H2HA,H2HB), C9MA(H9MA,H9MB), C0HA(H0HA,
 H0HB), C160(H16E,H16F), C0LA(H0LA,H0LB), C2JA(H2JA,H2JB), C173(H17C,H17D),
 C174(H17E,H17F), C5OA(H5OA,H5OB), C2MA(H2MA,H2MB), C1A(H1AB,H1AC), C8MA(H8MA,
 H8MB), C191(H19C,H19D), C197(H19E,H19F), C6MA(H6MA,H6MB), C4IA(H4IA,H4IB),
 C6VA(H6VA,H6VB), C9TA(H9TA,H9TB), C7VA(H7VA,H7VB), C8QA(H8QA,H8QB), C4PA(H4PA,
 H4PB), C92(H92A,H92B), C0WA(H0WA,H0WB), C2UA(H2UA,H2UB), C3UA(H3UA,H3UB),
 C7UA(H7UA,H7UB), C7TA(H7TA,H7TB), C8RA(H8RA,H8RB), C6RA(H6RA,H6RB), C9OA(H9OA,
 H9OB), C4RA(H4RA,H4RB), C7RA(H7RA,H7RB), C4TA(H4TA,H4TB), C0PA(H0PA,H0PB),
 C7WA(H7WA,H7WB), C3RA(H3RA,H3RB), C3TA(H3TA,H3TB), C8OA(H8OA,H8OB), C9VA(H9VA,
 H9VB), C2RA(H2RA,H2RB), C6TA(H6TA,H6TB), C(HA,HB), C0UA(H0UA,H0UB), C8VA(H8VA,
 H8VB), C2WA(H2WA,H2WB), C8WA(H8WA,H8WB), C206(H20C,H20D), C212(H21A,H21B),
 C7C(H7CB,H7CC), C8C(H8CB,H8CC), C242(H24C,H24D), C247(H24A,H24B), C250(H25A,
 H25B), C262(H26A,H26B), C265(H26C,H26D), C268(H26E,H26F), C271(H27A,H27B),
 C275(H27E,H27F), C277(H27C,H27D), C284(H28A,H28B), C286(H28C,H28D), C298(H29A,
 H29B), C1AB(H1AD,H1AE), C7BB(H7BB,H7BC), C2XA(H2XA,H2XB), C5BB(H5BB,H5BC),
 C2ZA(H2ZA,H2ZB), C2AB(H2AB,H2AC), C2BB(H2BB,H2BC), C0ZA(H0ZA,H0ZB), C6XA(H6XA,
 H6XB), C3XA(H3XA,H3XB), C4XA(H4XA,H4XB), C0XA(H0XA,H0XB), C8YA(H8YA,H8YB),
 C3ZA(H3ZA,H3ZB), C9XA(H9XA,H9XB), C8XA(H8XA,H8XB), C9BB(H9BC,H9BD), C2CB(H2CB,
 H2CC), C344(H34A,H34B)
5.c Aromatic/amide H refined with riding coordinates:
 C136(H136), C33(H33), C46(H46), C79(H79), C0NA(H0NA), C8BA(H8BA), C7BA(H7BA),
 C6BA(H6BA), C61(H61), C4HA(H4HA), C129(H129), C199(H199), C135(H135),
 C5BA(H5BA), C75(H75), C68(H68), C98(H98), C153(H153), C4EA(H4EA), C3EA(H3EA),
 C42(H42), C78(H78), C7HA(H7HA), C162(H162), C8CA(H8CA), C142(H142), C143(H143),
  C7CA(H7CA), C7IA(H7IA), C122(H122), C63(H63), C172(H172), C103(H103),
 C111(H111), C115(H115), C119(H119), C130(H130), C131(H131), C56(H56),
 C0EA(H0EA), C1EA(H1EA), C2EA(H2EA), C132(H132), C150(H150), C9PA(H9PA),
 C9DA(H9DA), C166(H166), C158(H158), C278(H278), C7PA(H7PA), C8PA(H8PA),
 C1CB(H1CB), C276(H276), C49(H49), C50(H50), C2CA(H2CA), C3BA(H3BA), C1BA(H1BA),
  C1CA(H1CA), C76(H76), C77(H77), C87(H87), C94(H94), C8DA(H8DA), C9AA(H9AA),
 C0BA(H0BA), C125(H125), C126(H126), C4BA(H4BA), C6IA(H6IA), C9UA(H9UA),
 C234(H234), C248(H248), C8UA(H8UA), C5FA(H5FA), C2KA(H2KA), C9QA(H9QA),
 C1KA(H1KA), C4FA(H4FA), C148(H148), C5DA(H5DA), C1DA(H1DA), C2DA(H2DA),
 C3DA(H3DA), C4DA(H4DA), C9SA(H9SA), C0TA(H0TA), C1TA(H1TA), C2TA(H2TA),
 C6FA(H6FA), C7DA(H7DA), C198(H198), C118(H118), C4QA(H4QA), C5QA(H5QA),
 C4JA(H4JA), C195(H195), C0VA(H0VA), C1VA(H1VA), C280(H280), C2VA(H2VA),
 C3NA(H3NA), C4KA(H4KA), C5KA(H5KA), C9IA(H9IA), C0JA(H0JA), C4VA(H4VA),
 C0FA(H0FA), C6KA(H6KA), C3KA(H3KA), C7JA(H7JA), C5LA(H5LA), C3WA(H3WA),
 C274(H274), C264(H264), C213(H213), C57(H57), C2IA(H2IA), C5WA(H5WA),
 C4WA(H4WA), C168(H168), C0OA(H0OA), C7KA(H7KA), C2NA(H2NA), C281(H281),
 C7YA(H7YA), C6YA(H6YA), C5YA(H5YA), C4YA(H4YA), C4MA(H4MA), C109(H109),
 C1RA(H1RA), C214(H214), C137(H137), C6JA(H6JA), C8JA(H8JA), C9JA(H9JA),
 C1OA(H1OA), C181(H181), C1NA(H1NA), C8KA(H8KA), C0KA(H0KA), C5ZA(H5ZA),
 C6ZA(H6ZA), C201(H201), C7ZA(H7ZA), C4ZA(H4ZA), C5MA(H5MA), C0QA(H0QA),
 C2QA(H2QA), C82(H82), C5SA(H5SA), C1QA(H1QA), C1SA(H1SA), C208(H208),
 C253(H253), C3SA(H3SA), C4AB(H4AB), C3AB(H3AC), C3QA(H3QA), C9RA(H9RA),
 C220(H220), C5AB(H5AB), C6AB(H6AC), C283(H283), C7SA(H7SA), C2PA(H2PA),
 C8AB(H8AC), C9AB(H9AB), C0BB(H0BB), C1BB(H1BB), C7AB(H7AB), C4SA(H4SA),
 C5UA(H5UA), C0RA(H0RA), C5RA(H5RA), C6UA(H6UA), C0SA(H0SA), C203(H203),
 C219(H219), C232(H232), C0YA(H0YA), C3YA(H3YA), C1YA(H1YA), C2YA(H2YA),
 C263(H263), C245(H245), C259(H259), C225(H225), C9ZA(H9ZA), C249(H249),
 C0AB(H0AE), C8ZA(H8ZA), C289(H289), C300(H300), C184(H184), C210(H210),
 C291(H291), C112(H112), C3BB(H3BB)
5.d Fitted hexagon refined as free rotating group:
 C51(C79,C0NA,C8BA,C7BA,C6BA), C65(C129,C199,C135,C5BA,C75), C70(C98,C153,C4EA,
 C3EA,C42), C91(C162,C8CA,C142,C143,C7CA), C100(C8EA,C7IA,C122,C63,C172),
 C131(C60,C56,C0EA,C1EA,C2EA), C150(C9PA,C9DA,C166,C180,C5HA), C2GA(C278,C7PA,
 C8PA,C1CB,C276), C5EA(C6IA,C9UA,C234,C248,C8UA), C3FA(C5FA,C2KA,C9QA,C1KA,
 C4FA), C157(C5DA,C1DA,C2DA,C3DA,C4DA), C170(C9SA,C0TA,C1TA,C2TA,C6FA),
 C183(C198,C118,C4QA,C5QA,C4JA), C5IA(C0VA,C1VA,C280,C2VA,C3VA), C8IA(C9EA,C9IA,
 C0JA,C4VA,C0FA), C3IA(C5LA,C3WA,C274,C264,C213), C121(C57,C2IA,C5WA,C4WA,C168),
  C6LA(C281,C7YA,C6YA,C5YA,C4YA), C5JA(C109,C1RA,C214,C137,C6JA), C1JA(C5ZA,
 C6ZA,C201,C7ZA,C4ZA), C2SA(C208,C253,C3SA,C4AB,C3AB), C6SA(C220,C5AB,C6AB,C283,
 C7SA), C8SA(C8AB,C9AB,C0BB,C1BB,C7AB), C243(C0YA,C3YA,C1YA,C2YA,C263),
 C285(C225,C9ZA,C249,C0AB,C8ZA), C290(C289,C300,C184,C210,C291)
;
_shelx_res_checksum              82261
_shelx_hkl_checksum              13111
_shelx_fab_checksum              1464
_olex2_submission_special_instructions 'No special instructions were received'