Palladium(II) saccharinate (sac) and thiosaccharinate (tsac) complexes with 2-aminopyridine (2-ampy), 2-acetylaminopyridine (2-aampy) and 2-acetylaminopyrimidine (2-aampym) co-ligands: X-ray crystal structures of trans-[Pd(sac)2(ampy)2] and solvatomorphs trans-[Pd(sac)2(2-aampy)2].S (S = CHCl3, thf)
Subhi A. Al-Jibori; Qusay K.A. Al-Jibori; Harry Schmidt; Kurt Merzweiler; Christoph Wagner; Graeme Hogarth; Inorganica Chimica Acta 402 (2013) 69–74; doi:

data_1517150
_publ_section_title
;
 Palladium(II) saccharinate (sac) and thiosaccharinate (tsac) complexes
 with 2-aminopyridine (2-ampy), 2-acetylaminopyridine (2-aampy) and
 2-acetylaminopyrimidine (2-aampym) co-ligands: X-ray crystal structures
 of trans-[Pd(sac)2(ampy)2] and solvatomorphs trans-[Pd(sac)2(2-aampy)2].S
 (S = CHCl3, thf)
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              69
_journal_page_last               74
_journal_volume                  402
_journal_year                    2013
_chemical_formula_moiety         'C28 H24 N6 O8 Pd S2, C H Cl3'
_chemical_formula_sum            'C29 H25 Cl3 N6 O8 Pd S2'
_chemical_formula_weight         862.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 111.332(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3994(4)
_cell_length_b                   24.8507(8)
_cell_length_c                   12.8085(5)
_cell_measurement_reflns_used    13221
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      2.08
_cell_volume                     3379.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20267
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.09
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  0.9401
_exptl_absorpt_correction_T_min  0.8956
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(IPDS Software; Stoe & Cie, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0031(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0592P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                4752
_reflns_number_total             6622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-402-69-74-2.cif
_cod_data_source_block           z:\i2t0335
_cod_original_sg_symbol_Hall     '-P 2ybc  '
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1517150