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_4319489
_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(C18 H36 N2 NA1 O6) (C16 N8 Ag4 Se8) 0.33 (C2 H3 N)'
_chemical_formula_sum            'C88.67 H145 Ag4 N16.33 Na4 O24 S8'
_chemical_formula_weight         2603.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.039(4)
_cell_length_b                   27.039(4)
_cell_length_c                   15.358(3)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.77
_cell_measurement_theta_min      2.727
_cell_volume                     11228(3)
_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 0.931
_diffrn_measured_fraction_theta_max 0.931
_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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            140127
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         1.06
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  .87317
_exptl_absorpt_correction_T_min  .74637
_exptl_absorpt_correction_type   mixed
_exptl_absorpt_process_details
;
Face-absorption corrected followed by SADABS
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5377
_exptl_crystal_size_max          .320
_exptl_crystal_size_mid          .166
_exptl_crystal_size_min          .164
_refine_diff_density_max         1.315
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.410(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.690
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1314
_refine_ls_number_reflns         27572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.690
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.255
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
1/[\s^2^(Fo^2^)+(0.0300Fo^2^)^2^] 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                22676
_reflns_number_total             27572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000868q_2.cif
_cod_data_source_block           all
_cod_original_cell_volume        11229(3)
_cod_database_code               4319489