Coordination of bis(pyrazol-1-yl)amine to palladium(II): influence of the co-ligands and counter-ions on the molecular and crystal structures
Mendoza, María de los Angeles; Bernès, Sylvain; Mendoza-Díaz, Guillermo; Acta Crystallographica Section E 71 (2015) 22–27; doi:10.1107/S205698901402595X

data_2240285
_publ_section_title
;
 Coordination of bis(pyrazol-1-yl)amine to palladium(II): influence of the
 co-ligands and counter-ions on the molecular and crystal structures
;
_journal_coeditor_code           WM5076
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              22
_journal_page_last               27
_journal_paper_doi               10.1107/S205698901402595X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Pd (N C S) (C14 H23 N5)]2 [Pd (N C S )4]'
_chemical_formula_moiety         '2(C15 H23 N6 Pd S +), C4 N4 Pd S4 2-'
_chemical_formula_sum            'C34 H46 N16 Pd3 S6'
_chemical_formula_weight         1190.43
_chemical_name_systematic
;
Bis[{bis[2-(3,5-dimethylpyrazol-1-yl-\k<i>N</i>^2^)ethyl]amine-\
\k<i>N</i>}(thiocyanato-\k<i>N</i>)palladium]
tetrakis(thiocyanato-\k<i>S</i>)palladate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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           SHELXL2014
_cell_angle_alpha                94.838(14)
_cell_angle_beta                 100.947(12)
_cell_angle_gamma                103.989(13)
_cell_formula_units_Z            1
_cell_length_a                   9.0286(17)
_cell_length_b                   10.532(2)
_cell_length_c                   13.066(3)
_cell_measurement_reflns_used    75
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.43
_cell_measurement_theta_min      4.69
_cell_volume                     1172.5(4)
_computing_cell_refinement
;
XSCANS (Siemens, 1996)
;
_computing_data_collection
;
XSCANS (Siemens, 1996)
;
_computing_data_reduction
;
XSCANS (Siemens, 1996)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298.0(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.012
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  0.378
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(XSCANS; Siemens, 1996)
;
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       Irregular_Plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.1014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                4874
_reflns_number_total             5367
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5076sup1.cif
_cod_data_source_block           5
_cod_database_code               2240285
_cod_database_fobs_code          2240285
_shelx_hkl_checksum              53398
_shelx_res_checksum              96904
_shelxl_version_number           2.014