Mercury(II), silver(I) and gold(I) thioether crown chemistry: synthesis, electrochemistry and structures of [(HgBr2)2([24]aneS8)], [{Ag2([24]aneS8)(CF3SO3)2(MeCN)2}∞], [Ag2([28]aneS8)][NO3]2 and [Au2([28]aneS8)][PF6]2 ([24]aneS8 = 1,4,7,10,13,16,19,22-octathiacyclotetracosane; [28]aneS8 = 1,4,8,11,15,18,22,25-octathiacyclooctacosane)
Blake, Alexander J.; Li, Wan-Sheung; Lippolis, Vito; Taylor, Anne; Schröder, Martin; Journal of the Chemical Society, Dalton Transactions  (1998) 2931–; doi:10.1039/a803358g

data_7028121
_publ_section_title
;
 Mercury(II), silver(I) and gold(I) thioether crown chemistry: synthesis,
 electrochemistry and structures of [(HgBr2)2([24]aneS8)],
 [{Ag2([24]aneS8)(CF3SO3)2(MeCN)2}\\infty ], [Ag2([28]aneS8)][NO3]2 and
 [Au2([28]aneS8)][PF6]2
 ([24]aneS8&#x2005;=&#x2005;1,4,7,10,13,16,19,22-octathiacyclotetracosane;
 [28]aneS8&#x2005;=&#x2005;1,4,8,11,15,18,22,25-octathiacyclooctacosane)
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2931
_journal_paper_doi               10.1039/a803358g
_journal_year                    1998
_chemical_formula_moiety
'C16 H32 Ag2 S8 2+, 2(C1 F3 O3 S1 -), 2(C2 H3 N1)'
_chemical_formula_sum            'C22 H38 Ag2 F6 N2 O6 S10'
_chemical_formula_weight         1076.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'introduced at calculated positions'
_atom_sites_solution_primary     'direct methods (Ag)'
_atom_sites_solution_secondary   'difference Fourier synthesis'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.752(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.285(2)
_cell_length_b                   6.3340(10)
_cell_length_c                   22.547(3)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      13
_cell_volume                     1890.7(5)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1995a)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1995a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1995b)'
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1995)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device
;
Stoe Stadi-4 four-circle diffractometer with Oxford Cryosystems
open-flow cryostat
;
_diffrn_measurement_method       'omega-theta 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3344
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_obs          0.0431
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+0.399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0779
_refine_ls_wR_factor_obs         0.0653
_reflns_number_observed          2255
_reflns_number_total             3344
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            G803358sup1.cif
_cod_data_source_block           24s8ag
_cod_depositor_comments
;
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^)+(0.0252P)^2^+0.399P] 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^)+(0.0252P)^2^+0.399P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P2(1)/c (No. 14)'
_cod_database_code               7028121