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_7714489
_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         '2(C70 H60 Ag2 O18 P2 Ti2)'
_chemical_formula_sum            'C140 H120 Ag4 O36 P4 Ti4'
_chemical_formula_weight         3125.326
_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_Int_Tables_number      2
_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                103.505(9)
_cell_angle_beta                 101.189(8)
_cell_angle_gamma                101.414(8)
_cell_formula_units_Z            1
_cell_length_a                   12.4087(19)
_cell_length_b                   14.508(3)
_cell_length_c                   20.709(4)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.951
_cell_measurement_theta_min      2.706
_cell_volume                     3438.6(11)
_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  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 VENTURE'
_diffrn_measured_fraction_theta_full 0.9850
_diffrn_measured_fraction_theta_max 0.9850
_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_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.9850
_diffrn_reflns_Laue_measured_fraction_max 0.9850
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50748
_diffrn_reflns_point_group_measured_fraction_full 0.9850
_diffrn_reflns_point_group_measured_fraction_max 0.9850
_diffrn_reflns_theta_full        25.0779
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.901
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1583.044
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.8763
_refine_diff_density_min         -0.6826
_refine_diff_density_rms         0.1410
_refine_ls_d_res_high            0.8384
_refine_ls_d_res_low             7.9635
_refine_ls_goodness_of_fit_ref   1.1873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    108
_refine_ls_number_parameters     903
_refine_ls_number_reflns         12042
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.1860
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+11.6384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1702
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8279
_reflns_number_total             12042
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt02387g2.cif
_cod_data_source_block           2277824
_cod_database_code               7714489
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Ag1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.03 within 2A
Ag2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.03 within 2A
Uanis(C61) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C64)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C10(H10), C11(H11), C23(H23), C30(H30), C31(H31), C32(H32),
 C34(H34), C36(H36), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47), C49(H49),
  C50(H50), C51(H51), C56(H56), C60(H60), C61(H61), C21(H21), C24(H24),
 C25(H25), C28(H28), C35(H35), C37(H37), C39(H39), C40(H40), C45(H45), C48(H48),
  C53(H53), C55(H55), C57(H57), C59(H59), C63(H63), C65(H65), C66(H66),
 C67(H67), C68(H68), C70(H70), C71(H71)
2.b Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C62(H62a,H62b,H62c), C64(H64a,H64b,H64c), C44(H44a,H44b,
 H44c), C52(H52a,H52b,H52c), C69(H69a,H69b,H69c)
;
_olex2_submission_special_instructions 'No special instructions were received'