Synthesis and Characterization of the Silver Maleonitrilediselenolates and Silver Maleonitriledithiolates [K([2.2.2]-cryptand)]4[Ag4(Se2C2(CN)2)4], [Na([2.2.2]-cryptand)]4[Ag4(S2C2(CN)2)4].0.33MeCN, [NBu4]4[Ag4(S2C2(CN)2)4], [K([2.2.2]-cryptand)]3[Ag(Se2C2(CN)2)2].2MeCN, and [Na([2.2.2]-cryptand)]3[Ag(S2C2(CN)2)2]
Craig C. McLauchlan; James A. Ibers; Inorganic Chemistry 40 (2001) 1809–1815; doi:10.1021/ic000868q

data_4319493
_publ_section_title
;
 Synthesis and Characterization of the Silver Maleonitrilediselenolates
 and Silver Maleonitriledithiolates
 [K([2.2.2]-cryptand)]4[Ag4(Se2C2(CN)2)4],
 [Na([2.2.2]-cryptand)]4[Ag4(S2C2(CN)2)4].0.33MeCN,
 [NBu4]4[Ag4(S2C2(CN)2)4], [K([2.2.2]-cryptand)]3[Ag(Se2C2(CN)2)2].2MeCN,
 and [Na([2.2.2]-cryptand)]3[Ag(S2C2(CN)2)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1809
_journal_page_last               1815
_journal_paper_doi               10.1021/ic000868q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '4 (C16 H36 N) (C16 Ag4 N8 S8)'
_chemical_formula_sum            'C80 H144 Ag4 N12 S8'
_chemical_formula_weight         1962.03
_chemical_melting_point          451(2)
_chemical_name_common            '136 C dec'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.511(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   15.689(3)
_cell_length_b                   51.924(11)
_cell_length_c                   17.393(4)
_cell_measurement_temperature    153(2)
_cell_volume                     14142(5)
_computing_cell_refinement       'SAINT+ Version 6.02 (Bruker-AXS, 1999)'
_computing_data_collection       'SMART Version 5 (Bruker-AXS, 1999)'
_computing_data_reduction        'SAINT+ Version 6.02 (Bruker-AXS, 1999)'
_computing_molecular_graphics    'SHELXTL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker AXS SMART-1000 with CCD'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       69
_diffrn_reflns_limit_k_min       -69
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            169792
_diffrn_reflns_theta_full        29.06
_diffrn_reflns_theta_max         29.06
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        '< 2%'
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_type   mixed
_exptl_absorpt_process_details
;
face absorption in SHELXTL followed by SADABS
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             6144
_refine_diff_density_max         2.331
_refine_diff_density_min         -2.069
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.739
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         35020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.739
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.613
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
1/[\s^2^(Fo^2^)+(0.0400Fo^2^)^2^]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                23094
_reflns_number_total             35020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000868q_6.cif
_cod_data_source_block           p21c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '176-180 C' was changed to '451(2)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_database_code               4319493