Anion-templated nanosized silver clusters protected by mixed thiolate and diphosphine.
Li, Xiao-Yu; Wang, Zhi; Su, Hai-Feng; Feng, Sheng; Kurmoo, Mohamedally; Tung, Chen-Ho; Sun, Di; Zheng, Lan-Sun; Nanoscale 9 (2017) 3601–3608; doi:10.1039/c6nr09632h

data_1545292
_publ_section_title
;
 Anion-templated nanosized silver clusters protected by mixed thiolate and
 diphosphine.
;
_journal_issue                   10
_journal_name_full               Nanoscale
_journal_page_first              3601
_journal_page_last               3608
_journal_paper_doi               10.1039/c6nr09632h
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'C288 H252 Ag24 Fe6 Mo5 O20 P12 S12, C2 H3 N'
_chemical_formula_sum            'C290 H255 Ag24 Fe6 Mo5 N O20 P12 S12'
_chemical_formula_weight         8233.99
_chemical_name_systematic
;
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-04 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                69.6918(7)
_cell_angle_beta                 88.7509(8)
_cell_angle_gamma                84.3460(8)
_cell_formula_units_Z            2
_cell_length_a                   22.7887(18)
_cell_length_b                   27.962(2)
_cell_length_c                   33.377(3)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.27
_cell_volume                     19848(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXH-1997 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.1102
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            97197
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.669
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0722 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.7748.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8056
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.980
_refine_diff_density_min         -1.911
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3337
_refine_ls_number_reflns         68124
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1178P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.2048
_reflns_number_gt                40743
_reflns_number_total             68124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nr09632h2.cif
_cod_data_source_block           4
_cod_depositor_comments          'Adding full bibliography for 1545292.cif.'
_cod_database_code               1545292
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim C217: within 1.7A with
sigma of 0.008 and sigma for terminal atoms of 0.08
C136 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.08
C211 \\sim C208 \\sim C207 \\sim C209 \\sim C210 \\sim C206: within 1.7A with
sigma of 0.002 and sigma for terminal atoms of 0.08
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C32) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C226) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C75) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(C137) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C212) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.2
Uanis(C136) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.2
Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
: with sigma of 0.002 and sigma for terminal atoms of 0.1
: with sigma of 0.005 and sigma for terminal atoms of 0.1
3.a Ternary CH refined with riding coordinates:
 C53(H53), C115(H115), C151(H151)
3.b Me refined with riding coordinates:
 C267(H26D,H26E,H26F), C292(H29A,H29B,H29C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
  C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39),
  C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
 C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59),
  C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67),
 C68(H68), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77),
  C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C84(H84), C85(H85),
 C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95),
  C96(H96), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104),
 C105(H105), C106(H106), C107(H107), C108(H108), C110(H110), C111(H111),
 C112(H112), C113(H113), C114(H114), C117(H117), C118(H118), C119(H119),
 C120(H120), C121(H121), C123(H123), C124(H124), C126(H126), C127(H127),
 C128(H128), C129(H129), C130(H130), C132(H132), C133(H133), C134(H134),
 C135(H135), C136(H136), C138(H138), C139(H139), C140(H140), C141(H141),
 C142(H142), C144(H144), C145(H145), C146(H146), C147(H147), C148(H148),
 C150(H150), C152(H152), C153(H153), C154(H154), C156(H156), C157(H157),
 C158(H158), C160(H160), C161(H161), C162(H162), C163(H163), C164(H164),
 C166(H166), C167(H167), C168(H168), C169(H169), C170(H170), C172(H172),
 C173(H173), C174(H174), C175(H175), C176(H176), C178(H178), C179(H179),
 C180(H180), C181(H181), C182(H182), C183(H183), C185(H185), C186(H186),
 C187(H187), C189(H189), C190(H190), C191(H191), C192(H192), C194(H194),
 C195(H195), C196(H196), C197(H197), C198(H198), C200(H200), C201(H201),
 C202(H202), C203(H203), C204(H204), C206(H206), C207(H207), C209(H209),
 C210(H210), C213(H213), C214(H214), C216(H216), C217(H217), C220(H220),
 C221(H221), C223(H223), C224(H224), C227(H227), C228(H228), C230(H230),
 C231(H231), C234(H234), C235(H235), C237(H237), C238(H238), C241(H241),
 C242(H242), C244(H244), C245(H245), C248(H248), C249(H249), C251(H251),
 C252(H252), C255(H255), C256(H256), C258(H258), C259(H259), C262(H262),
 C263(H263), C265(H265), C266(H266), C269(H269), C270(H270), C272(H272),
 C273(H273), C276(H276), C277(H277), C279(H279), C280(H280), C283(H283),
 C284(H284), C286(H286), C287(H287)
3.d Idealised Me refined as rotating group:
 C211(H21A,H21B,H21C), C218(H21D,H21E,H21F), C225(H22A,H22B,H22C), C232(H23A,
 H23B,H23C), C239(H23D,H23E,H23F), C246(H24A,H24B,H24C), C253(H25A,H25B,H25C),
 C260(H26A,H26B,H26C), C274(H27A,H27B,H27C), C281(H28A,H28B,H28C), C288(H28D,
 H28E,H28F)
;
_olex2_submission_special_instructions 'No special instructions were received'