Cis-thiolate bridged heterobimetallic complexes as efficient catalysts for glycosyl triazole synthesis
Shrivastav, Akash; Tiwari, Raman Kumar; Yadav, Mangal S.; Bhattacharya, Subrato; Catalysis Science & Technology 16 (2026) 1595–1609; doi:10.1039/D5CY01152C

data_1576832
_publ_section_title
;
 Cis-thiolate bridged heterobimetallic complexes as efficient catalysts
 for glycosyl triazole synthesis
;
_journal_issue                   5
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1595
_journal_page_last               1609
_journal_paper_doi               10.1039/D5CY01152C
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety
'C62 H52 Ag N8 Ni P2 S2, 2(C3 H7 N O), 1[C3H7NO], 1[NO3-]'
_chemical_formula_sum            'C71 H73 Ag N12 Ni O6 P2 S2'
_chemical_formula_weight         1483.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-11 deposited with the CCDC.	2025-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                102.5080(10)
_cell_angle_beta                 102.5660(10)
_cell_angle_gamma                102.8790(10)
_cell_formula_units_Z            2
_cell_length_a                   13.47670(10)
_cell_length_b                   16.1583(2)
_cell_length_c                   17.9322(3)
_cell_measurement_reflns_used    38108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9230
_cell_measurement_theta_min      2.6210
_cell_volume                     3568.42(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61301
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.157
_diffrn_reflns_theta_min         2.921
_exptl_absorpt_coefficient_mu    3.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         12931
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.2912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11433
_reflns_number_total             12931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy01152c2.cif
_cod_data_source_block           acr-33_sq
_cod_original_cell_volume        3568.41(8)
_cod_database_code               1576832
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.587
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N11-C64 \\sim N10-C64
 with sigma of 0.02
 N11-C67 \\sim N10-C69
 with sigma of 0.02
 N11-C68 \\sim N10-C70
 with sigma of 0.02
 C64-C67 \\sim C64-C69
 with sigma of 0.04
 C64-C68 \\sim C64-C70
 with sigma of 0.04
 C67-C68 \\sim C69-C70
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N10) = Uanis(C70) = Uanis(C69)
Uanis(C67) = Uanis(N11) = Uanis(C68)
4. Rigid body (RIGU) restrains
 N11, C67, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10, C69, C70
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H64A)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(N10)=Sof(C70)=Sof(H70A)=
 Sof(H70B)=Sof(H70C)=1-FVAR(1)
 Sof(N11)=Sof(H64)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C68)=Sof(H68A)=
 Sof(H68B)=Sof(H68C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N8(H8), C3(H3), C5(H5), C12(H12), C13(H13), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64A),
 C64(H64), C66(H66)
6.b Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 152 electrons were 
found in a volume of 564\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C3H7NO], 1[NO3-] per Formula Unit 
which account for 142 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9716
_shelx_fab_checksum              38407
_olex2_submission_special_instructions 'No special instructions were received'