Bis(tetra-<i>n</i>-butylammonium) bis(5,6-dicyanopyrazine-2,3-dithiolato-κ^2^<i>S</i>,<i>S</i>')palladium(II)
Tomura, Masaaki; Yamashita, Yoshiro; Acta Crystallographica Section E 68 (2012) m57–; doi:10.1107/S1600536811053402

data_2233198
_publ_section_title
;
 Bis(tetra-<i>n</i>-butylammonium)
 bis(5,6-dicyanopyrazine-2,3-dithiolato-\k^2^<i>S</i>,<i>S</i>')palladium(II)
;
_journal_coeditor_code           HY2494
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m57
_journal_paper_doi               10.1107/S1600536811053402
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C16 H36 N)2 [Pd (C6 N4 S2)2]'
_chemical_formula_moiety         '2(C16 H36 N +), C12 N8 Pd S4 2-'
_chemical_formula_sum            'C44 H72 N10 Pd S4'
_chemical_formula_weight         975.80
_chemical_melting_point          520.5
_chemical_name_systematic
;
Bis(tetra-<i>n</i>-butylammonium)
bis(5,6-dicyanopyrazine-2,3-dithiolato-\k^2^<i>S</i>,<i>S</i>')palladium(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                68.82(2)
_cell_angle_beta                 87.74(3)
_cell_angle_gamma                80.16(3)
_cell_formula_units_Z            1
_cell_length_a                   9.912(3)
_cell_length_b                   10.635(4)
_cell_length_c                   13.286(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      22.71
_cell_measurement_theta_min      20.07
_cell_volume                     1286.3(8)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1988)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation & Rigaku, 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_sigmaI/netI    0.2686
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5102
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0.994
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.413
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.2713
_refine_ls_R_factor_gt           0.0928
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.2218
_reflns_number_gt                1751
_reflns_number_total             4835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2494.cif
_cod_data_source_block           I
_cod_database_code               2233198
_cod_database_fobs_code          2233198