Facile Syntheses and Structures of New Metal-Maleonitrilediselenolates [K([2.2.2]-cryptand)]3[Ag(Se2C2(CN)2)(Se6)], [K([2.2.2]-cryptand)]2[Ni(Se2C2(CN)2)2], and Ni(dppp)(Se2C2(CN)2)
Craig C. McLauchlan; James A. Ibers; Inorganic Chemistry 39 (2000) 1046–1048; doi:10.1021/ic9901719

data_4300009
_publ_section_title
;
Facile Syntheses and Structures of New Metal-Maleonitrilediselenolates
[K([2.2.2]-cryptand)]3[Ag(Se2C2(CN)2)(Se6)],
[K([2.2.2]-cryptand)]2[Ni(Se2C2(CN)2)2], and Ni(dppp)(Se2C2(CN)2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1046
_journal_page_last               1048
_journal_paper_doi               10.1021/ic9901719
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         '(K C18 H36 O6 N2)2 (Ni Se4 C8 N4)'
_chemical_formula_sum            'C44 H72 K2 N8 Ni O12 Se4'
_chemical_formula_weight         1357.85
_chemical_name_common
;
bis(potassium-[2.2.2]-cryptand) bis(maleonitrilediselenolate)nickelate(ii)
;
_chemical_name_systematic
; 
bis(potassium-4,7,13,16,21,24-hexaoxa-1,10-diazobicyclo[8.8.8]hexacosane)
bis(cis-1,2-dicyano,1,2-diselenato-ethene-Se-Se')nickelate(ii)
;
_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                 107.644(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2196(11)
_cell_length_b                   15.8602(15)
_cell_length_c                   15.3055(14)
_cell_measurement_reflns_used    4989
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.75
_cell_volume                     2826.7(5)
_computing_cell_refinement       'SMART Version 5.101 (Bruker, 1997)'
_computing_data_collection       'SMART Version 5.101 (Bruker, 1997)'
_computing_data_reduction        'SAINT-Plus Version 5.101 (Bruker, 1997)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART-1000 CCD'
_diffrn_measurement_method       '/w scans'
_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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20947
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    3.128
_exptl_absorpt_correction_T_max  0.86330
_exptl_absorpt_correction_T_min  0.64423
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          .160
_exptl_crystal_size_mid          .140
_exptl_crystal_size_min          .082
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.006
_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          0.0814
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                3101
_reflns_number_total             4989
_reflns_threshold_expression     'I > 2sigma(I)'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4300009