New cyclometallated precursors of unsubstituted N-phenylpyrazole [{Pd(phpz)(μ-X)}2] (X = AcO or OH) and study of their reactivity towards selected ligands.
Serrano, José Luis; García, Luis; Pérez, José; Pérez, Eduardo; Galiana, José Miguel; García, Joaquín; Martínez, Marina; Sánchez, Gregorio; da Silva, Ivan; Dalton transactions (Cambridge, England : 2003) 40 (2011) 156–168; doi:10.1039/c0dt00814a

data_7021864
_publ_section_title
;
 New cyclometallated precursors of unsubstituted N-phenylpyrazole
 [{Pd(phpz)(\m-X)}2] (X = AcO or OH) and study of their reactivity towards
 selected ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              156
_journal_page_last               168
_journal_paper_doi               10.1039/c0dt00814a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C26 H24 N8 PD2 S2'
_chemical_formula_sum            'C26 H24 N8 Pd2 S2'
_chemical_formula_weight         725.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.1797(5)
_cell_length_b                   17.5215(7)
_cell_length_c                   26.8062(11)
_cell_measurement_temperature    100(2)
_cell_volume                     5250.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.967
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            57537
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    1.562
_exptl_absorpt_correction_T_max  0.9121
_exptl_absorpt_correction_T_min  0.7556
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+15.2285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                5927
_reflns_number_total             6240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00814a.txt
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7021861--7021866.cif.'
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7021864