Pd(II) Complexes with Polydentate Nitrogen Ligands. Molecular Recognition and Dynamic Behavior Involving Pd-N Bond Rupture. X-ray Molecular Structures of [{Pd(C~6~HF~4~)~2~}(bpzm)] and [{PdΜ^3^-(C~4~H~7~)}~2~(bpzm)]CF~3~SO~3~)~2~ [bpzpm = 4,6-Bis(pyrazol-1-yl)pyrimidine]
Felipe Gómez-de la Torre; Antonio de la Hoz; Félix A. Jalón; Blanca R. Manzano; Ana M. Rodríguez; José Elguero; Martín Martínez-Ripoll; Inorganic Chemistry 39 (2000) 1152–1162; doi:10.1021/ic990495x

data_4300034
_publ_section_title
;
Pd(II) Complexes with Polydentate Nitrogen Ligands. Molecular Recognition
and Dynamic Behavior Involving Pd-N Bond Rupture. X-ray Molecular Structures of
[{Pd(C~6~HF~4~)~2~}(bpzm)] and [{Pd\M^3^-(C~4~H~7~)}~2~(bpzm)]CF~3~SO~3~)~2~
[bpzpm = 4,6-Bis(pyrazol-1-yl)pyrimidine]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1152
_journal_page_last               1162
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C22 H10 F8 N6 Pd'
_chemical_formula_weight         616.76
_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           SHELXL-97
_cell_angle_alpha                88.45(2)
_cell_angle_beta                 74.36(3)
_cell_angle_gamma                89.32(2)
_cell_formula_units_Z            2
_cell_length_a                   8.845(6)
_cell_length_b                   12.6609(9)
_cell_length_c                   12.826(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1382.6(10)
_computing_cell_refinement       'Mach3 (Nonius)'
_computing_data_collection       'MACH3 (Nonius)'
_computing_data_reduction        'Xray80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6664
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.28
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6664
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1664P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2452
_refine_ls_wR_factor_ref         0.3077
_reflns_number_gt                3333
_reflns_number_total             6664
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4300034
_journal_paper_doi 10.1021/ic990495x