Design and oxidative desulfurization of Ag/Ti heterometallic clusters based on Hard-Soft Acid-Base principle.
Yang, Shuyi; Fu, Yaomei; Tian, Yiran; Zhao, Liang; Wang, Xinlong; Li, Baoli; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt02387g

data_7714488
_publ_section_title
;
 Design and oxidative desulfurization of Ag/Ti heterometallic clusters
 based on Hard-Soft Acid-Base principle.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02387g
_journal_year                    2023
_chemical_formula_moiety         'Ag2 C108 O42 P2 Ti12, 3[CH3CN]'
_chemical_formula_sum            'C120 H145 Ag2 N3 O42 P2 Ti12'
_chemical_formula_weight         3153.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-23 deposited with the CCDC.	2023-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.457(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6923(16)
_cell_length_b                   25.691(2)
_cell_length_c                   30.026(2)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_cell_volume                     14409.2(19)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      173.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 VENTURE'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '0.60\ % \ w and 0.6\ % \ f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1225
_diffrn_reflns_av_unetI/netI     0.1305
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            91182
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.170
_diffrn_reflns_theta_max         25.170
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.9
_diffrn_source_power             0.0405
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6440
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.636
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1687
_refine_ls_number_reflns         25596
_refine_ls_number_restraints     4281
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.2313
_refine_ls_R_factor_gt           0.1151
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1731P)^2^+174.6657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2945
_refine_ls_wR_factor_ref         0.3961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11245
_reflns_number_total             25596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02387g2.cif
_cod_data_source_block           2277825
_cod_original_cell_volume        14409(2)
_cod_database_code               7714488
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Restrained distances
 O41-C98 \\sim O41-C1C \\sim O39-C110 \\sim O39-C1E \\sim O13-C91 \\sim O4-C88
\\sim O11-C85A \\sim O11-
 C85B \\sim O35-C98B \\sim O35-C98A \\sim O5-C101 \\sim O5-C105 \\sim O17-C95B
\\sim O17-C95A \\sim O37-C94
 \\sim O37-C97 \\sim O31-C84
 with sigma of 0.02
 C85-C84 \\sim C86-C84 \\sim C91-C90 \\sim C92-C91 \\sim C112-C110 \\sim
C111-C110 \\sim C96A-C95A ~
 C95B-C94B \\sim C96B-C95B \\sim C95A-C94A \\sim C95-C94 \\sim C97-C1A \\sim
C96-C94 \\sim C97-C1B ~
 C88-C87 \\sim C89-C88 \\sim C1D-C1C \\sim C1C-C109 \\sim C98-C108 \\sim
C99-C98 \\sim C85B-C84B \\sim C85A-
 C84A \\sim C86A-C85A \\sim C86B-C85B \\sim C98B-C100 \\sim C99B-C98B \\sim
C99A-C98A \\sim C98A-C107 ~
 C1F-C1E \\sim C1E-C113 \\sim C102-C101 \\sim C103-C101 \\sim C106-C105 \\sim
C105-C104
 with sigma of 0.02
 C86-C85 \\sim C86A-C84A \\sim C86B-C84B \\sim C99B-C100 \\sim C99A-C107 \\sim
C1F-C113 \\sim C112-
 C111 \\sim C92-C90 \\sim C106-C104 \\sim C103-C102 \\sim C99-C108 \\sim
C89-C87 \\sim C1D-C109 \\sim C96B-
 C94B \\sim C96A-C94A \\sim C96-C95 \\sim C1B-C1A
 with sigma of 0.02
 O31-C86 \\sim O31-C85 \\sim O11-C84B \\sim O11-C84A \\sim O11-C86B \\sim
O11-C86A \\sim O41-C108 ~
 O41-C99 \\sim O5-C103 \\sim O5-C102 \\sim O5-C106 \\sim O5-C104 \\sim O41-C1D
\\sim O41-C109 \\sim O37-C1B
 \\sim O37-C95 \\sim O37-C1A \\sim O37-C96 \\sim O17-C94B \\sim O17-C94A \\sim
O17-C96A \\sim O17-C96B ~
 O35-C99B \\sim O35-C107 \\sim O35-C100 \\sim O35-C99A \\sim O13-C90 \\sim
O13-C92 \\sim O4-C87 \\sim O4-
 C89 \\sim O39-C1F \\sim O39-C113 \\sim O39-C112 \\sim O39-C111
 with sigma of 0.02
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C45 \\sim C51 \\sim C46 \\sim C66 \\sim C59 \\sim C38 \\sim C82 \\sim C69 \\sim
C37 \\sim C47 \\sim C42 \\sim C31 \\sim C36 \\sim C35 \\sim C34 \\sim C33 \\sim
C32 \\sim C62 \\sim C63 \\sim C64 \\sim C93 \\sim C65 \\sim C61 \\sim C76 \\sim
C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C54 \\sim C40 \\sim C41 \\sim
C50 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C43 \\sim
C53 \\sim C39 \\sim C88 \\sim C89 \\sim C68 \\sim C44 \\sim C74 \\sim C87 \\sim
C58 \\sim C72 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C91
\\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C73 \\sim C70
\\sim C25 \\sim C48 \\sim C90 \\sim C30 \\sim C55 \\sim C85B \\sim C92 \\sim
C49 \\sim C56 \\sim C7 \\sim C12 \\sim C11 \\sim C10 \\sim C9 \\sim C8 \\sim
C29 \\sim C67 \\sim C71 \\sim C26 \\sim C75 \\sim C28 \\sim C57 \\sim C52 \\sim
C86B \\sim C83 \\sim C95B \\sim C27 \\sim C60 \\sim C84B \\sim C96B \\sim C94B
\\sim C85A \\sim C86A \\sim C84A \\sim C95A \\sim C94A \\sim C96A \\sim C86
\\sim C84 \\sim C85 \\sim C94 \\sim C96 \\sim C95 \\sim C97 \\sim C1A \\sim C1B
\\sim C98B \\sim C99B \\sim C100 \\sim C101 \\sim C103 \\sim C102 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C98A \\sim C99A \\sim C99 \\sim C98
\\sim C108 \\sim C109 \\sim C1C \\sim C1D \\sim C110 \\sim C111 \\sim C112
\\sim C113 \\sim C1E \\sim C1F: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.03 within 3A
Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C113) \\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(C1F) \\sim Ueq, Uanis(C109)
\\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C98) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(C99) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.03
Uanis(C91) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C99A) \\sim Ueq, Uanis(O41) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.03
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(C85B)=Sof(H85B)=Sof(C86B)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(C84B)=
 Sof(H84A)=Sof(H84B)=Sof(H84C)=1-FVAR(1)
 Sof(C85A)=Sof(H85A)=Sof(C86A)=Sof(H86D)=Sof(H86E)=Sof(H86F)=Sof(C84A)=
 Sof(H84D)=Sof(H84E)=Sof(H84F)=FVAR(1)
 Sof(C95B)=Sof(H95B)=Sof(C96B)=Sof(H96A)=Sof(H96B)=Sof(H96C)=Sof(C94B)=
 Sof(H94A)=Sof(H94B)=Sof(H94C)=1-FVAR(2)
 Sof(C95A)=Sof(H95A)=Sof(C94A)=Sof(H94D)=Sof(H94E)=Sof(H94F)=Sof(C96A)=
 Sof(H96D)=Sof(H96E)=Sof(H96F)=FVAR(2)
 Sof(C97)=Sof(H97)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(H1BC)=1-FVAR(3)
 Sof(C94)=Sof(H94)=Sof(C96)=Sof(H96G)=Sof(H96H)=Sof(H96I)=Sof(C95)=Sof(H95C)=
 Sof(H95D)=Sof(H95E)=FVAR(3)
 Sof(C101)=Sof(H101)=Sof(C103)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C102)=
 Sof(H10G)=Sof(H10H)=Sof(H10I)=1-FVAR(4)
 Sof(C104)=Sof(H10J)=Sof(H10K)=Sof(H10L)=Sof(C105)=Sof(H105)=Sof(C106)=
 Sof(H10M)=Sof(H10N)=Sof(H10O)=FVAR(4)
 Sof(C98B)=Sof(H98B)=Sof(C99B)=Sof(H99A)=Sof(H99B)=Sof(H99C)=Sof(C100)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=1-FVAR(5)
 Sof(C107)=Sof(H10P)=Sof(H10Q)=Sof(H10R)=Sof(C98A)=Sof(H98A)=Sof(C99A)=
 Sof(H99D)=Sof(H99E)=Sof(H99F)=FVAR(5)
 Sof(C109)=Sof(H10V)=Sof(H10W)=Sof(H10X)=Sof(C1C)=Sof(H1C)=Sof(C1D)=Sof(H1DA)=
 Sof(H1DB)=Sof(H1DC)=1-FVAR(6)
 Sof(C99)=Sof(H99G)=Sof(H99H)=Sof(H99I)=Sof(C98)=Sof(H98)=Sof(C108)=Sof(H10S)=
 Sof(H10T)=Sof(H10U)=FVAR(6)
 Sof(C113)=Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C1E)=Sof(H1E)=Sof(C1F)=Sof(H1FA)=
 Sof(H1FB)=Sof(H1FC)=1-FVAR(7)
 Sof(C110)=Sof(H110)=Sof(C111)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C112)=
 Sof(H11D)=Sof(H11E)=Sof(H11F)=FVAR(7)
5.a Riding coordinates:
 C84A(H84D,H84E,H84F), C95(H95C,H95D,H95E), C104(H10J,H10K,H10L), C106(H10M,
 H10N,H10O), C107(H10P,H10Q,H10R), C99A(H99D,H99E,H99F), C99(H99G,H99H,H99I),
 C108(H10S,H10T,H10U), C109(H10V,H10W,H10X), C1D(H1DA,H1DB,H1DC), C111(H11A,
 H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C1F(H1FA,H1FB,H1FC)
5.b Ternary CH refined with riding coordinates:
 C88(H88), C91(H91), C85B(H85B), C95B(H95B), C85A(H85A), C95A(H95A), C84(H84),
 C94(H94), C97(H97), C98B(H98B), C101(H101), C105(H105), C98A(H98A), C98(H98),
 C1C(H1C), C110(H110), C1E(H1E)
5.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C42(H42), C36(H36), C35(H35), C34(H34), C33(H33), C32(H32),
 C63(H63), C64(H64), C65(H65), C78(H78), C79(H79), C81(H81), C40(H40), C50(H50),
  C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C39(H39), C58(H58), C2(H2),
 C3(H3), C4(H4), C5(H5), C6(H6), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C73(H73), C70(H70), C48(H48), C30(H30), C55(H55), C56(H56), C12(H12),
  C11(H11), C10(H10), C9(H9), C8(H8), C29(H29), C71(H71), C26(H26), C28(H28),
 C27(H27)
5.d Fitted hexagon refined as free rotating group:
 C31(C36,C35,C34,C33,C32), C62(C63,C64,C93,C65,C61), C76(C77,C78,C79,C80,C81),
 C13(C14,C15,C16,C17,C18), C1(C2,C3,C4,C5,C6), C19(C20,C21,C22,C23,C24), C7(C12,
 C11,C10,C9,C8)
5.e Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C44(H44A,H44B,H44C), C87(H87A,H87B,H87C), C90(H90A,H90B,
 H90C), C92(H92A,H92B,H92C), C67(H67A,H67B,H67C), C75(H75A,H75B,H75C), C52(H52A,
 H52B,H52C), C86B(H86A,H86B,H86C), C83(H83A,H83B,H83C), C60(H60A,H60B,H60C),
 C84B(H84A,H84B,H84C), C96B(H96A,H96B,H96C), C94B(H94A,H94B,H94C), C86A(H86D,
 H86E,H86F), C94A(H94D,H94E,H94F), C96A(H96D,H96E,H96F), C86(H86G,H86H,H86I),
 C85(H85C,H85D,H85E), C96(H96G,H96H,H96I), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,
 H1BC), C99B(H99A,H99B,H99C), C100(H10A,H10B,H10C), C103(H10D,H10E,H10F),
 C102(H10G,H10H,H10I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80297
_shelx_fab_checksum              70658
_olex2_submission_special_instructions 'No special instructions were received'