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_4300008
_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         '(C27 H26 P2) Ni (Se2 C2 N4)'
_chemical_formula_sum            'C31 H26 N2 Ni P2 Se2'
_chemical_formula_weight         705.11
_chemical_name_common
;
1,3-bis(diphenylphosphino)propane maleneonitrilediselenolate nickel(ii)
;
_chemical_name_systematic
;
1,3-bis(diphenylphosphino)propane
cis-1,2-dicyano,1,2-diselenato-ethene-Se-Se-nickel(ii)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   12.4004(7)
_cell_length_b                   15.4068(9)
_cell_length_c                   15.4512(9)
_cell_measurement_reflns_used    3738
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      56.50
_cell_volume                     2952.0(3)
_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_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25662
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    3.255
_exptl_absorpt_correction_T_max  0.73524
_exptl_absorpt_correction_T_min  0.39552
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (Sheldrick, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.2625
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_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          0.0593
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                2913
_reflns_number_total             3738
_reflns_threshold_expression     'I > 2sigma(I)'
_cod_database_code               4300008