A series of silver doped butterfly-like Ti<sub>8</sub>Ag<sub>2</sub> clusters with two Ag ions panelled on a Ti<sub>8</sub> surface.
Yu, You-Zhu; Guo, Yao; Zhang, Yan-Ru; Liu, Min-Min; Feng, Ya-Ru; Geng, Cui-Huan; Zhang, Xian-Ming; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13423–13429; doi:10.1039/c9dt02508a

data_7700767
_publ_section_title
;
 A series of silver doped butterfly-like Ti<sub>8</sub>Ag<sub>2</sub>
 clusters with two Ag ions panelled on a Ti<sub>8</sub> surface.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13423
_journal_page_last               13429
_journal_paper_doi               10.1039/c9dt02508a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C148 H128 Ag2 O52 P2 Ti8), 6(C2 H3 N)'
_chemical_formula_sum            'C308.2 H274.61 Ag4 N6 O104 P4 Ti16'
_chemical_formula_weight         7048.09
_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
_audit_creation_date             2019-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-17 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                92.6270(10)
_cell_angle_beta                 99.8580(10)
_cell_angle_gamma                109.6870(10)
_cell_formula_units_Z            1
_cell_length_a                   15.6045(2)
_cell_length_b                   17.2291(3)
_cell_length_c                   31.2468(5)
_cell_measurement_reflns_used    9397
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.65
_cell_measurement_theta_min      2.20
_cell_volume                     7744.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            100488
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.263
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             3598
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.632
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2081
_refine_ls_number_reflns         27262
_refine_ls_number_restraints     1390
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+10.3412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23681
_reflns_number_total             27262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02508a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7700762--7700767.cif.'
_cod_original_formula_sum        'C308.20 H274.61 Ag4 N6 O104 P4 Ti16'
_cod_database_code               7700767
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.786
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H) groups, All C(H,H,H) groups
2. Restrained distances
 N3-C153
 1.15 with sigma of 0.01
 C153-C154
 1.45 with sigma of 0.01
 O6-C16A = O6-C16
 1.48 with sigma of 0.01
 N3-C154
 2.65 with sigma of 0.01
 N3-C15B
 1.15 with sigma of 0.01
 C15B-C15A
 1.52 with sigma of 0.01
 N3-C15A
 2.65 with sigma of 0.01
 O52A-C14G = O52-C147
 1.45 with sigma of 0.01
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C16A,
 C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32,
  C33, C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47,
 C48, C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63,
  C64, C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78,
 C79, C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92, C93, C94,
  C95, C96, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, C107, C108,
  C109, C110, C111, C112, C113, C114, C115, C116, C117, C118, C119, C120, C121,
 C122, C123, C124, C125, C126, C127, C128, C129, C130, C131, C132, C133, C134,
 C135, C136, C137, C138, C139, C140, C141, C142, C143, C144, C145, C146, C14A,
 C14B, C14C, C14D, C14E, C14F, C148, C147, C14G, C149, C150, C151, C152, C153,
 C154, C15A, C15B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C16A \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23
\\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31
\\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39
\\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47
\\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55
\\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63
\\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71
\\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79
\\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87
\\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95
\\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim
C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim
C110 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim
C117 \\sim C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim
C124 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim C130 \\sim
C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135 \\sim C136 \\sim C137 \\sim
C138 \\sim C139 \\sim C140 \\sim C141 \\sim C142 \\sim C143 \\sim C144 \\sim
C145 \\sim C146 \\sim C14A \\sim C14B \\sim C14C \\sim C14D \\sim C14E \\sim
C14F \\sim C148 \\sim C147 \\sim C14G \\sim C149 \\sim C150 \\sim C151 \\sim
C152 \\sim C153 \\sim C154 \\sim C15A \\sim C15B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C144) \\sim Ueq, Uanis(C147)
\\sim Ueq, Uanis(C14G) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(C153) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O52A) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(O52) \\sim Ueq, Uanis(O38)
\\sim Ueq, Uanis(O29) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.001
5. Others
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C141)=Sof(C142)=Sof(H142)=
 Sof(C143)=Sof(H143)=Sof(C144)=Sof(C145)=Sof(H145)=Sof(C146)=Sof(H146)=
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C15B)=Sof(O52A)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C14A)=Sof(C14B)=Sof(H14D)=
 Sof(C14C)=Sof(H14E)=Sof(C14D)=Sof(C14E)=Sof(H14F)=Sof(C14F)=Sof(H14G)=
 Sof(C147)=Sof(H14H)=Sof(H14I)=Sof(H14J)=Sof(C14G)=Sof(H14K)=Sof(H14L)=
 Sof(H14M)=Sof(C153)=Sof(C154)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(O52)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15),
 C19(H19), C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C30(H30), C31(H31),
  C35(H35), C36(H36), C38(H38), C39(H39), C43(H43), C44(H44), C46(H46),
 C47(H47), C51(H51), C52(H52), C54(H54), C55(H55), 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), C86(H86),
 C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C95(H95), C96(H96), C98(H98),
  C99(H99), C103(H103), C104(H104), C106(H106), C107(H107), C111(H111),
 C112(H112), C114(H114), C115(H115), C119(H119), C120(H120), C122(H122),
 C123(H123), C127(H127), C128(H128), C130(H130), C131(H131), C135(H135),
 C136(H136), C138(H138), C139(H139), C142(H142), C143(H143), C145(H145),
 C146(H146), C14B(H14D), C14C(H14E), C14E(H14F), C14F(H14G)
6.b Fitted hexagon refined as free rotating group:
 C141(C142,C143,C144,C145,C146), C14A(C14B,C14C,C14D,C14E,C14F)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C56(H56A,
 H56B,H56C), C100(H10A,H10B,H10C), C108(H10D,H10E,H10F), C116(H11A,H11B,H11C),
 C124(H12A,H12B,H12C), C132(H13A,H13B,H13C), C140(H14A,H14B,H14C), C147(H14H,
 H14I,H14J), C14G(H14K,H14L,H14M), C149(H14N,H14O,H14P), C152(H15G,H15H,H15I),
 C154(H15A,H15B,H15C), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              5849
_olex2_submission_special_instructions 'No special instructions were received'