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_7714487
_publ_section_title
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 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         'C110 H92 Ag2 O58 Ti11, 6[CH3OH]'
_chemical_formula_sum            'C116 H116 Ag2 O64 Ti11'
_chemical_formula_weight         3276.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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
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2023-10-23 deposited with the CCDC.	2023-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.036(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.292(5)
_cell_length_b                   39.754(9)
_cell_length_c                   16.628(4)
_cell_measurement_reflns_used    8965
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     14066(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'mirror optics'
_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  0.1440
_diffrn_reflns_av_unetI/netI     0.0933
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            67489
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.062
_diffrn_reflns_theta_max         25.062
_diffrn_reflns_theta_min         2.451
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.952
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6640
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         12423
_refine_ls_number_restraints     1072
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0743P)^2^+19.6845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7249
_reflns_number_total             12423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02387g2.cif
_cod_data_source_block           2277823
_cod_database_code               7714487
_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
 O28-C54B = O28-C54A
 1.4 with sigma of 0.02
 C52B-C30B = C52A-C30A
 1.5 with sigma of 0.01
 O26-C46B = O26-C46A
 1.4 with sigma of 0.02
 O29A-C22A
 1.325 with sigma of 0.01
 O23A-C30A
 1.25 with sigma of 0.01
2. Restrained planarity
 C52A, C30A, C53A, C48A, C51A, C50A, C49A
 with sigma of 0.001
 C21, C23, O29A, C22A, C27A, C26A, C25A, C24A
 with sigma of 0.01
 C53A, O25A, C52A, C48A, C49A, C50A, C51A, C30A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O23B \\sim C30A \\sim O24B \\sim C30B \\sim C52A \\sim C52B \\sim C53A \\sim
C53B \\sim C48A \\sim C48B \\sim C49B \\sim C49A \\sim C50B \\sim C50A \\sim
C51B \\sim C51A \\sim O25B: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.03 within 3.8A
C54A \\sim C54B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.03 within 2A
O28: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.03 within 2A
C46B \\sim C46A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.03 within 2A
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim O29 \\sim C22A
\\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim O29A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.03 within 2A
O23A \\sim O23B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.03 within 2A
O25A \\sim O25B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.03 within 2A
O28 \\sim C54B \\sim C54A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.03 within 2A
Uanis(O25B) \\sim Ueq, Uanis(C53B) \\sim Ueq, Uanis(C53A) \\sim Ueq,
Uanis(C48B) \\sim Ueq, Uanis(C48A) \\sim Ueq, Uanis(C49B) \\sim Ueq,
Uanis(C49A) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C50B) \\sim Ueq,
Uanis(C52B) \\sim Ueq, Uanis(C52A) \\sim Ueq, Uanis(C51B) \\sim Ueq,
Uanis(C51A) \\sim Ueq, Uanis(C30B) \\sim Ueq, Uanis(O23B) \\sim Ueq,
Uanis(O24B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C54B) \\sim Ueq, Uanis(C54A) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(O24A) \\sim Ueq, Uanis(O25A) \\sim Ueq, Uanis(C46B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(O25B)=Sof(C30B)=Sof(C53B)=Sof(C48B)=Sof(H48B)=Sof(C49B)=Sof(H49B)=
 Sof(C50B)=Sof(H50B)=Sof(C51B)=Sof(H51B)=Sof(C52B)=1-FVAR(1)
 Sof(C30A)=Sof(C53A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=
 Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(O25A)=FVAR(1)
 Sof(C46B)=Sof(H46A)=Sof(H46B)=Sof(H46C)=1-FVAR(2)
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=FVAR(2)
 Sof(C54B)=Sof(H54A)=Sof(H54B)=Sof(H54C)=1-FVAR(3)
 Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=FVAR(3)
 Sof(C22A)=Sof(C27A)=Sof(H27A)=Sof(C26A)=Sof(H26A)=Sof(C25A)=Sof(H25A)=
 Sof(C24A)=Sof(H24A)=Sof(O29A)=1-FVAR(4)
 Sof(C22)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=
 Sof(H27)=Sof(O29)=FVAR(4)
 Fixed Sof: O23B(0.5) O24B(0.5) O23A(0.5) O24A(0.5)
5.a Riding coordinates:
 C54B(H54A,H54B,H54C)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17),
 C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C40(H40), C41(H41), C42(H42),
 C45(H45), C48B(H48B), C49B(H49B), C50B(H50B), C51B(H51B), C48A(H48A),
 C49A(H49A), C50A(H50A), C51A(H51A), C27A(H27A), C26A(H26A), C25A(H25A),
 C24A(H24A)
5.c Fitted hexagon refined as free rotating group:
 C6(C7,C8,C9,C10,C11), C13(C14,C15,C16,C17,C18), C32(C33,C34,C35,C36,C37),
 C40(C41,C42,C43,C44,C45), C53B(C48B,C49B,C50B,C51B,C52B), C53A(C48A,C49A,C50A,
 C51A,C52A), C22A(C27A,C26A,C25A,C24A,C23)
5.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C39(H39A,H39B,H39C), C46B(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C55(H55A,H55B,H55C), C46A(H46D,H46E,H46F), C54A(H54D,H54E,H54F)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 434 electrons were 
found in a volume of 2916\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
3[CH3OH]per Asymmetric Unit 
which account for 432 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80735
_shelx_fab_checksum              32726
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'