Silver(i) dithiocarboxylate complexes - clustering and aggregation.
Grote, Johanna; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6036–6040; doi:10.1039/c8dt00279g

data_7045855
_publ_section_title
;
 Silver(i) dithiocarboxylate complexes - clustering and aggregation.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6036
_journal_page_last               6040
_journal_paper_doi               10.1039/c8dt00279g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C55 H59 Ag4 N3 S8, 0.5(C5 H5 N)'
_chemical_formula_sum            'C57.5 H61.5 Ag4 N3.5 S8'
_chemical_formula_weight         1489.56
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-22 deposited with the CCDC.
2018-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3063(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.72625(5)
_cell_length_b                   21.79602(9)
_cell_length_c                   21.46037(9)
_cell_measurement_reflns_used    146204
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.8460
_cell_measurement_theta_min      3.4490
_cell_volume                     5916.69(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00  28.00   1.00    7.50    --  -42.33  58.00  73.00   97
  2  \w   -112.00 -15.00   1.00    7.50    --  -42.33 -58.00 -66.00   97
  3  \w     15.00 112.00   1.00    7.50    --   42.33  58.00  73.00   97
  4  \w     84.00 178.00   1.00   24.50    --  111.00  58.00  73.00   94
  5  \w     41.00 138.00   1.00   24.50    --  111.00 -58.00 -66.00   97
  6  \w   -115.00 -20.00   1.00    7.50    --  -42.33 -37.00 -30.00   95
  7  \w   -116.00 -11.00   1.00    7.50    --  -42.33 -77.00   0.00  105
  8  \w   -116.00 -11.00   1.00    7.50    --  -42.33 -77.00-150.00  105
  9  \w   -116.00 -11.00   1.00    7.50    --  -42.33 -77.00 120.00  105
 10  \w   -115.00 -20.00   1.00    7.50    --  -42.33 -37.00  60.00   95
 11  \w   -116.00 -11.00   1.00    7.50    --  -42.33 -77.00  60.00  105
 12  \w   -116.00 -11.00   1.00    7.50    --  -42.33 -77.00 -60.00  105
 13  \w      1.00  82.00   1.00    7.50    --   42.33 -99.00 150.00   81
 14  \w    -28.00  69.00   1.00    7.50    --   42.33 -58.00 -66.00   97
 15  \w     57.00 129.00   1.00    7.50    --   42.33 178.00 -30.00   72
 16  \w     83.00 178.00   1.00   24.50    --  111.00  61.00  30.00   95
 17  \w     30.00 109.00   1.00   24.50    --  111.00 -94.00 -60.00   79
 18  \w     81.00 178.00   1.00   24.50    --  111.00  71.00 106.96   97
 19  \w     37.00 142.00   1.00   24.50    --  111.00 -77.00  90.00  105
 20  \w     39.00 121.00   1.00   24.50    --  111.00-125.00 120.00   82
 21  \w     39.00 121.00   1.00   24.50    --  111.00-125.00 -60.00   82
 22  \w     80.00 178.00   1.00   24.50    --  111.00  77.00-150.00   98
 23  \w     83.00 178.00   1.00   24.50    --  111.00  61.00  60.00   95
 24  \w     80.00 178.00   1.00   24.50    --  111.00  77.00 -60.00   98
 25  \w     83.00 178.00   1.00   24.50    --  111.00  61.00 -90.00   95
 26  \w     80.00 178.00   1.00   24.50    --  111.00  77.00 -30.00   98
 27  \w     80.00 178.00   1.00   24.50    --  111.00  77.00 120.00   98
 28  \w     83.00 178.00   1.00   24.50    --  111.00  61.00 150.00   95
 29  \w     83.00 178.00   1.00   24.50    --  111.00  61.00-150.00   95
 30  \w     81.00 178.00   1.00   24.50    --  111.00  70.00  42.55   97
 31  \w     81.00 178.00   1.00   24.50    --  111.00  71.00 113.22   97
 32  \w     80.00 178.00   1.00   24.50    --  111.00  77.00 -90.00   98
 33  \w     80.00 178.00   1.00   24.50    --  111.00  75.00 -41.00   98
 34  \w     39.00 121.00   1.00   24.50    --  111.00-125.00 -90.00   82
 35  \w     80.00 178.00   1.00   24.50    --  111.00  77.00  60.00   98
 36  \w     83.00 178.00   1.00   24.50    --  111.00  61.00-180.00   95
 37  \w     39.00 121.00   1.00   24.50    --  111.00-125.00  60.00   82
 38  \w     83.00 178.00   1.00   24.50    --  111.00  61.00-120.00   95
 39  \w     80.00 178.00   1.00   24.50    --  111.00  77.00  90.00   98
 40  \w     83.00 178.00   1.00   24.50    --  111.00  61.00 -30.00   95
 41  \w     85.00 178.00   1.00   24.50    --  111.00  55.00 -43.47   93
 42  \w     82.00 178.00   1.00   24.50    --  111.00  68.00 -27.51   96
 43  \w     82.00 178.00   1.00   24.50    --  111.00  68.00 158.34   96
 44  \w     87.00 178.00   1.00   24.50    --  111.00  45.00  30.00   91
 45  \w     87.00 178.00   1.00   24.50    --  111.00  45.00-150.00   91
 46  \w     39.00 121.00   1.00   24.50    --  111.00-125.00-180.00   82
 47  \w     80.00 178.00   1.00   24.50    --  111.00  77.00-180.00   98
 48  \w     80.00 178.00   1.00   24.50    --  111.00  77.00   0.00   98
 49  \w     83.00 178.00   1.00   24.50    --  111.00  62.00-103.34   95
 50  \w     82.00 178.00   1.00   24.50    --  111.00  69.00-122.34   96
 51  \w     83.00 178.00   1.00   24.50    --  111.00  61.00 -60.00   95
 52  \w     83.00 178.00   1.00   24.50    --  111.00  63.00  89.28   95
 53  \w     83.00 178.00   1.00   24.50    --  111.00  62.00  39.98   95
 54  \w     83.00 178.00   1.00   24.50    --  111.00  61.00   0.00   95
 55  \w   -116.00 -11.00   1.00    7.50    --  -42.33 -77.00-120.00  105
 56  \w   -121.00  -5.00   1.00    7.50    --  -42.33 -19.00 -60.00  116
 57  \w   -112.00 -16.00   1.00    7.50    --  -42.33 -57.00-180.00   96
 58  \w   -116.00 -11.00   1.00    7.50    --  -42.33 -77.00  90.00  105
 59  \w   -116.00 -52.00   1.00    7.50    --  -42.33 -77.00 150.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0038287000
_diffrn_orient_matrix_UB_12      0.0489069000
_diffrn_orient_matrix_UB_13      -0.0520353000
_diffrn_orient_matrix_UB_21      0.1216975000
_diffrn_orient_matrix_UB_22      0.0026604000
_diffrn_orient_matrix_UB_23      0.0073907000
_diffrn_orient_matrix_UB_31      0.0026789000
_diffrn_orient_matrix_UB_32      -0.0509449000
_diffrn_orient_matrix_UB_33      -0.0495549000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0086
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            202082
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.349
_diffrn_reflns_theta_min         2.899
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.411
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             2988
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         11688
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0171
_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^)+(0.0208P)^2^+5.6160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11636
_reflns_number_total             11688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00279g2.cif
_cod_data_source_block           glatthor23
_cod_depositor_comments
'Adding full bibliography for 7045852--7045856.cif.'
_cod_original_formula_sum        'C57.50 H61.50 Ag4 N3.50 S8'
_cod_database_code               7045855
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C59 H59 Ag4 N2 S8'
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.347
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     43.26
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7B) = Uanis(C7A)
Uanis(C10B) = Uanis(C10A)
Uanis(C6B) = Uanis(C6A)
Uanis(C5B) = Uanis(C5A)
Uanis(C9B) = Uanis(C9A)
Uanis(C4B) = Uanis(C4A)
Uiso(C56) = Uiso(C57) = Uiso(C58) = Uiso(C59) = Uiso(C60)
3. Same fragment restrains
{N1, C41, C42, C43, C44, C45} sigma for 1-2: 0.02, 1-3: 0.04
as
{N4, C56, C57, C58, C59, C60}
4. Others
 Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(C9B)=Sof(H9BA)=
 Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Fixed Sof: N4(0.5) C56(0.5) H56(0.5) C57(0.5) H57(0.5) C58(0.5) H58(0.5)
 C59(0.5) H59(0.5) C60(0.5) H60(0.5)
5.a Me refined with riding coordinates:
 C10A(H10A,H10B,H10C), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F)
5.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C4B(H4B), C6B(H6B), C14(H14), C16(H16), C24(H24),
 C26(H26), C34(H34), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9A(H9AA,H9AB,H9AC), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              81490
_olex2_date_sample_data_collection 2016-09-27
_olex2_date_sample_submission    1474408800
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.777