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_4319491
_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         '3 [C18 H36 Na N2 O6] [C8 N4 Ag S4]'
_chemical_formula_sum            'C62 H108 Ag N10 Na3 O18 S4'
_chemical_formula_weight         1586.66
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 91.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.547(2)
_cell_length_b                   11.766(2)
_cell_length_c                   27.774(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3771.5(12)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS SMART-1000 with CCD'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            26049
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  .96710
_exptl_absorpt_correction_T_min  .90707
_exptl_absorpt_correction_type   mixed
_exptl_absorpt_process_details
;
    face absorption in SHELXTL followed by SADABS
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          .232
_exptl_crystal_size_mid          .163
_exptl_crystal_size_min          .072
_refine_diff_density_max         2.526
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.538
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.538
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.206
_refine_ls_shift/su_mean         0.002
_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          0.1591
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                4003
_reflns_number_total             6638
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000868q_4.cif
_cod_data_source_block           agmnt2
_cod_original_cell_volume        3771.5(13)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               4319491