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_4323072
_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_sum            'C12 H24 Ag I3 S6'
_chemical_formula_weight         849.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.634(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.5767(11)
_cell_length_b                   11.9188(7)
_cell_length_c                   5.2714(5)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      14.5
_cell_volume                     1161.51(15)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measurement_device_type  'Stoe Stadi4 four-circle'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_av_sigmaI/netI    0.014
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_limit_l_min       -1
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_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.42
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
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_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.428
_exptl_crystal_density_meas      ?
_exptl_crystal_description       column
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_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.58
_refine_diff_density_rms         0.07
_refine_ls_extinction_coef       0.0057(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    'riding model'
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_refine_ls_number_parameters     58
_refine_ls_number_reflns         1071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_obs          0.0181
_refine_ls_shift/esd_max         0.25
_refine_ls_shift/esd_mean        0.06
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.018P)^2^+2.04P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0422
_refine_ls_wR_factor_obs         0.0403
_reflns_number_observed          988
_reflns_number_total             1074
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980413p_3.cif
_cod_data_source_block           18S6I4
_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 (3 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 (3
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 (4 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.018P)^2^+2.04P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.018P)^2^+2.04P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1161.5(2)
_cod_original_formula_sum        'C12 H24 Ag1 I3 S6'
_cod_database_code               4323072