Unexpected formation and crystal structure of tetrakis(1<i>H</i>-pyrazole-κ<i>N</i>^2^)palladium(II) dichloride
Wagner, Thomas; Christiansen, Nena; Hrib, Cristian G.; Kaufmann, Dieter E.; Edelmann, Frank T.; Acta Crystallographica Section E 70 (2014) 486–488; doi:10.1107/S160053681402460X

data_2240197
_publ_section_title
;
 Unexpected formation and crystal structure of
 tetrakis(1<i>H</i>-pyrazole-\k<i>N</i>^2^)palladium(II) dichloride
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              486
_journal_page_last               488
_journal_paper_doi               10.1107/S160053681402460X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Pd (C12 H16 N8)] Cl2'
_chemical_formula_moiety         'C12 H16 N8 Pd 2+, 2(Cl -)'
_chemical_formula_sum            'C12 H16 Cl2 N8 Pd'
_chemical_formula_weight         449.63
_chemical_name_systematic
;
Tetrakis(1<i>H</i>-pyrazole-\k<i>N</i>^2^)palladium(II) dichloride
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 117.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.797(3)
_cell_length_b                   9.6560(19)
_cell_length_c                   14.174(3)
_cell_measurement_reflns_used    15423
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.69
_cell_volume                     1670.4(8)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-RED32 (Stoe, 2008)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       \w-scans
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7700
_diffrn_reflns_theta_full        29.17
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  0.7502
_exptl_absorpt_correction_T_min  0.5619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.785
_refine_diff_density_min         -1.734
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2253
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0490P)^2^+4.2172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                2030
_reflns_number_total             2253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            wm5084sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1670.4(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2240197
_cod_database_fobs_code          2240197