Syntheses and Characterization of the Metal Maleonitrilediselenolates [K([2.2.2]-cryptand)]2[M(Se2C2(CN)2)2] (M = Ni, Pd, Pt) and [Ni(dmf)5Cl]2[Ni(Se2C2(CN)2)2]
Craig C. McLauchlan; Scott D. Robowski; James A. Ibers; Inorganic Chemistry 40 (2001) 1372–1375; doi:10.1021/ic0008666

data_4319357
_publ_section_title
;
 Syntheses and Characterization of the Metal Maleonitrilediselenolates
 [K([2.2.2]-cryptand)]2[M(Se2C2(CN)2)2] (M = Ni, Pd, Pt) and
 [Ni(dmf)5Cl]2[Ni(Se2C2(CN)2)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1372
_journal_page_last               1375
_journal_paper_doi               10.1021/ic0008666
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '2(C18 H36 K N2 O6) (C8 N4 Pd Se4)'
_chemical_formula_sum            'C44 H72 K2 N8 O12 Pd Se4'
_chemical_formula_weight         1405.54
_chemical_melting_point          514.1(10)
_chemical_name_common
'Bis([2.2.2]-cryptand) Palladium-bis(maleonitrilediselenolate)'
_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                 108.554(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2906(8)
_cell_length_b                   15.6686(10)
_cell_length_c                   15.5476(10)
_cell_measurement_temperature    153(2)
_cell_volume                     2838.5(4)
_computing_cell_refinement       'SMART Version 5.054 (Bruker, 1997)'
_computing_data_collection       'SMART Version 5.054 (Bruker, 1997)'
_computing_data_reduction        'SAINT+ Version 6.0 (Bruker, 1997)'
_computing_molecular_graphics    'SHELX-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELX-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 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker-AXS SMART-1000 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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.1019
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25636
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    3.100
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_refine_diff_density_max         1.545
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.679
_refine_ls_shift/su_mean         0.044
_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          0.0850
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                3618
_reflns_number_total             6854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0008666_2.cif
_cod_data_source_block           pdmns2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '240-242 C' was changed to
'514.1(10)' - 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_original_cell_volume        2838.5(3)
_cod_database_code               4319357