Bis(tetra-<i>n</i>-butylammonium) bis(1,2-dicyanoethylene-1,2-dithiolato-κ^2^<i>S</i>,<i>S</i>')palladate(II)
Xu, Hong-Wu; Yuan, Wen-Bing; Li, Jin-Xia; Liu, Min; Acta Crystallographica Section E 63 (2007) m1237–m1238; doi:10.1107/S1600536807015541

data_2213126
_publ_section_title
;
 Bis(tetra-<i>n</i>-butylammonium)
 bis(1,2-dicyanoethylene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>')palladate(II)
;
_journal_coeditor_code           BH2096
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1237
_journal_page_last               m1238
_journal_paper_doi               10.1107/S1600536807015541
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C16 H36 N2)2 [Pd (C4 N2 S2)2]'
_chemical_formula_moiety         '2(C16 H36 N), C8 N4 Pd S4'
_chemical_formula_sum            'C40 H72 N6 Pd S4'
_chemical_formula_weight         871.74
_chemical_name_systematic
;
Bis(Tetra-n-butylammonium)
bis(1,2-dicyanoethylene-1,2-dithiolato-\k^2^S,S')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
_audit_creation_method           SHELXL97
_cell_angle_alpha                85.631(2)
_cell_angle_beta                 87.964(2)
_cell_angle_gamma                65.476(2)
_cell_formula_units_Z            1
_cell_length_a                   9.7986(11)
_cell_length_b                   10.8084(12)
_cell_length_c                   12.4030(13)
_cell_measurement_reflns_used    2635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      1.65
_cell_volume                     1191.6(2)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'XPREP (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Siemens, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6213
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.639
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0377P)^2^+2.3236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                3178
_reflns_number_total             4181
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2096.cif
_cod_data_source_block           I
_cod_database_code               2213126
_cod_database_fobs_code          2213126