First Palladium(II) and Platinum(II) Complexes from Employment of 2,6-Diacetylpyridine Dioxime: Synthesis, Structural and Spectroscopic Characterization, and Biological Evaluation
Evangelia S. Koumousi; Marianthi Zampakou; Catherine P. Raptopoulou; Vassilis Psycharis; Christine M. Beavers; Simon J. Teat; George Psomas; Theocharis C. Stamatatos; Inorganic Chemistry 51 (2012) 7699–7710; doi:10.1021/ic300739x

data_4329708
_publ_section_title
;
 First Palladium(II) and Platinum(II) Complexes from Employment of
 2,6-Diacetylpyridine Dioxime: Synthesis, Structural and Spectroscopic
 Characterization, and Biological Evaluation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7699
_journal_page_last               7710
_journal_paper_doi               10.1021/ic300739x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C9 H10 Cl N3 O2 Pd'
_chemical_formula_weight         334.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_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            4
_cell_length_a                   6.8389(4)
_cell_length_b                   13.8406(7)
_cell_length_c                   10.9849(6)
_cell_measurement_reflns_used    6619
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.59
_cell_measurement_theta_min      5.00
_cell_volume                     1039.77(10)
_computing_cell_refinement       'Bruker SAINT v7.60a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.60a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9175
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         33.60
_diffrn_reflns_theta_min         3.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.530
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_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_parameters     148
_refine_ls_number_reflns         3085
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                2986
_reflns_number_total             3085
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300739x_si_001.cif
_cod_data_source_block           xs49c
_cod_database_code               4329708