Silver-Thioether Crown Complexes as Templates for the Synthesis of Extended Polyiodide Networks: Synthesis and X-ray Crystal Structures of [Ag2([15]aneS5)2]I12, [Ag([18]aneS6)]I7, [Ag([18]aneS6)]I3, and [Ag([9]aneS3)2]I5
Alexander J. Blake; Robert O. Gould; Wan-Sheung Li; Vito Lippolis; Simon Parsons; Christian Radek; Martin Schröder; Inorganic Chemistry 37 (1998) 5070–5077; doi:10.1021/ic980413p

data_4323073
_publ_section_title
;
 Silver-Thioether Crown Complexes as Templates for the Synthesis of
 Extended Polyiodide Networks: Synthesis and X-ray Crystal Structures of
 [Ag2([15]aneS5)2]I12, [Ag([18]aneS6)]I7, [Ag([18]aneS6)]I3, and
 [Ag([9]aneS3)2]I5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5070
_journal_page_last               5077
_journal_paper_doi               10.1021/ic980413p
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C12 H24 Ag S6 +, I5 -'
_chemical_formula_sum            'C12 H24 Ag I5 S6'
_chemical_formula_weight         1103.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   'initially placed in calculated positions'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 118.65(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1117(12)
_cell_length_b                   12.612(2)
_cell_length_c                   14.016(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      12.5
_cell_volume                     2654.5(12)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device       'Enraf Nonius FAST diffractometer'
_diffrn_measurement_method       'area detector scans'
_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  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5379
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.045
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.760
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.35
_refine_diff_density_min         -1.43
_refine_diff_density_rms         0.26
_refine_ls_extinction_coef       0.00382(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.118
_refine_ls_goodness_of_fit_obs   1.141
_refine_ls_hydrogen_treatment    'riding model with U(iso,H) = 1.2U(eq)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_obs          0.0368
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0877
_refine_ls_wR_factor_obs         0.0861
_reflns_number_observed          1863
_reflns_number_total             2003
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980413p_4.cif
_cod_data_source_block           AGS3I7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (5 times).

'_geom_angle_publ_flag' value 'Yes'
changed to 'yes' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (12
times).

'_geom_torsion_publ_flag' value 'Yes' changed to 'yes'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2654.5(6)
_cod_database_code               4323073