A facile route to 'naked' Ag<sup>+</sup> ions enabling the coordination of the weak Lewis base Ni(CO)<sub>4</sub>.
Berg, Willi R.; Moshtaha, Amina L.; Sievers, Robin; Reimann, Marc; Streit, Tim-Niclas; Rupf, Susanne M.; Kaupp, Martin; Malischewski, Moritz; Chemical science 17 (2026) 406–411; doi:10.1039/d5sc05589j

data_1576234
_publ_section_title
;
 A facile route to 'naked' Ag<sup>+</sup> ions enabling the coordination
 of the weak Lewis base Ni(CO)<sub>4</sub>.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              406
_journal_page_last               411
_journal_paper_doi               10.1039/d5sc05589j
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety
'0.9(C6 H4 Ag Cl4 Ni O4), B2 C37 F30 N, 0.1(C2 H4 Ag Cl4), 0.1(C H2 Cl2), 1[CH2Cl2]'
_chemical_formula_sum            'C43.7 H6.2 Ag B2 Cl6.2 F30 N Ni0.9 O3.6'
_chemical_formula_weight         1574.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-10-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-10 deposited with the CCDC.	2025-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2880(5)
_cell_length_b                   28.0807(10)
_cell_length_c                   13.7219(4)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.23
_cell_volume                     5118.1(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            64186
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.372
_diffrn_reflns_theta_min         2.076
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.194
_exptl_absorpt_correction_T_max  0.2394
_exptl_absorpt_correction_T_min  0.1634
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1351 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.6825.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_description       block
_exptl_crystal_F_000             3047
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         9383
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0423P)^2^+15.1622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7579
_reflns_number_total             9383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05589j2.cif
_cod_data_source_block           p21_c_num_smr
_cod_depositor_comments
'Adding full bibliography for 1576233--1576234.cif.'
_cod_original_formula_sum        'C43.70 H6.20 Ag B2 Cl6.20 F30 N Ni0.90 O3.60'
_cod_database_code               1576234
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.890
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Shared sites
{N014, C39}
{C016, N1}
3. Restrained distances
 Cl5-C37
 1.78 with sigma of 0.02
 C37-Cl6
 1.78 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C02G) = Uanis(C37)
Uanis(N014) = Uanis(C39)
Uanis(C016) = Uanis(N1)
Uanis(C40) = Uanis(C02D)
Uanis(Cl4) = Uanis(Cl5)
Uanis(Cl1) = Uanis(Cl10)
Uanis(Cl3) = Uanis(Cl9)
5. Others
 Fixed Sof: Ag1(0.9) Ni01(0.9) Cl1(0.9) Cl2(0.9) Cl3(0.9) Cl4(0.9) N014(0.5)
 O1(0.9) C016(0.5) C1(0.9) O2(0.9) O4(0.9) C3(0.9) C02D(0.9) H02A(0.9)
 H02B(0.9) C02G(0.9) H02C(0.9) H02D(0.9) C2(0.9) C4(0.9) O3(0.9) Ag2(0.1)
 Cl5(0.1) Cl6(0.1) C37(0.1) H37A(0.1) H37B(0.1) Cl7(0.1) Cl8(0.1) C38(0.1)
 H38A(0.1) H38B(0.1) C39(0.5) N1(0.5) Cl9(0.1) Cl10(0.1) C40(0.1) H40A(0.1)
 H40B(0.1)
6.a Secondary CH2 refined with riding coordinates:
 C02D(H02A,H02B), C02G(H02C,H02D), C37(H37A,H37B), C38(H38A,H38B), C40(H40A,
 H40B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              510
_shelx_fab_checksum              76575
_olex2_submission_special_instructions 'No special instructions were received'