Silver dithiocarbamates derived from amino acid esters.
Behling, Vreni; Heinrich, Jakob; Díaz, Dolores; Brohmer, Elias H. P.; Heinrich, Julian; Schlörer, Nils; Kupfer, Stephan; Kulak, Nora; Köhler, Phil; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12772–12783; doi:10.1039/d5dt01476j

data_7719230
_publ_section_title
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 Silver dithiocarbamates derived from amino acid esters.
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_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12772
_journal_page_last               12783
_journal_paper_doi               10.1039/d5dt01476j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C9 H14 Ag N O4 S2'
_chemical_formula_sum            'C9 H14 Ag N O4 S2'
_chemical_formula_weight         372.20
_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     dual
_audit_creation_date             2025-05-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-06-11 deposited with the CCDC.	2025-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                66.891(4)
_cell_angle_beta                 82.622(5)
_cell_angle_gamma                81.844(5)
_cell_formula_units_Z            8
_cell_length_a                   13.065(3)
_cell_length_b                   14.645(3)
_cell_length_c                   14.967(3)
_cell_measurement_reflns_used    6313
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.875
_cell_measurement_theta_min      2.479
_cell_volume                     2599.0(10)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Diamond 4 (Brandenburg, 1997)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker APEX II'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33882
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.484
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_T_max  0.8014
_exptl_absorpt_correction_T_min  0.7070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0989 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.8822.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         11426
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0228P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7604
_reflns_number_total             11426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01476j2.cif
_cod_data_source_block           bn01007
_cod_depositor_comments
'Adding full bibliography for 7719229--7719231.cif.'
_cod_original_cell_volume        2599.0(9)
_cod_database_code               7719230
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C27A \\sim C26-C27B
 with sigma of 0.02
 O16A-C32 \\sim O16B-C32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C26, C27A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, O16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, O16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=FVAR(1)
 Sof(O16B)=1-FVAR(2)
 Sof(O16A)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C11(H11A,H11B), C13(H13A,
 H13B), C15(H15A,H15B), C17(H17A,H17B), C20(H20A,H20B), C22(H22A,H22B),
 C24(H24A,H24B), C26(H26A,H26B), C26(H26C,H26D), C29(H29A,H29B), C31(H31A,H31B),
  C33(H33A,H33B), C35(H35A,H35B)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
 C25(H25A,H25B,H25C), C27B(H27A,H27B,H27C), C27A(H27D,H27E,H27F), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              97784
_shelx_hkl_checksum              70994
_olex2_date_sample_data_collection 2025-05-14
_olex2_date_sample_submission    2025-04-25
_olex2_submission_special_instructions 'No special instructions were received'