A triclinic polymorph of <i>cyclo</i>-tetra-μ-thiosaccharinato-κ^8^<i>S</i>:<i>S</i>-tetrakis[(triphenylphosphane-κ<i>P</i>)silver(I)]
Dennehy, Mariana; Freire, Eleonora; Baggio, Ricardo; Acta Crystallographica Section C 68 (2012) m17–m20; doi:10.1107/S0108270111053674

data_2018340
_publ_section_title
;
 A triclinic polymorph of
 <i>cyclo</i>-tetra-\m-thiosaccharinato-\k^8^<i>S</i>:<i>S</i>-tetrakis[(triphenylphosphane-\k<i>P</i>)silver(I)]
;
_journal_coeditor_code           BI3030
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m17
_journal_page_last               m20
_journal_paper_doi               10.1107/S0108270111053674
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ag4 (C7 H4 N O2 S2)4 (C18 H15 P)4]'
_chemical_formula_moiety         'C100 H76 Ag4 N4 O8 P4 S8'
_chemical_formula_sum            'C100 H76 Ag4 N4 O8 P4 S8'
_chemical_formula_weight         2273.49
_chemical_name_systematic
;
<i>cyclo</i>-tetrakis(\m-1,1-dioxo-1\l^6^,2-benzothiazole-3-thiolato-
\k^2^<i>S</i>:<i>S</i>)tetrakis[(triphenylphosphane-\k<i>P</i>)silver(I)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                77.771(4)
_cell_angle_beta                 123.880(3)
_cell_angle_gamma                86.4650(10)
_cell_formula_units_Z            1
_cell_length_a                   15.3566(10)
_cell_length_b                   14.1309(7)
_cell_length_c                   14.0768(6)
_cell_measurement_reflns_used    4175
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.88
_cell_measurement_theta_min      3.50
_cell_volume                     2416.9(3)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Oxford Gemini CCD S Ultra'
_diffrn_measurement_method       '\w scans, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20631
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         3.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.700
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         11017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                5568
_reflns_number_total             11017
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi3030.cif
_cod_data_source_block           I
_cod_original_cell_volume        2416.9(2)
_cod_database_code               2018340
_cod_database_fobs_code          2018340