Tetra-2,3-pyrazinoporphyrazines with Externally Appended Pyridine Rings. 5. Synthesis, Physicochemical and Theoretical Studies of a Novel Pentanuclear Palladium(II) Complex and Related Mononuclear Species
Maria Pia Donzello; Elisa Viola; Xiaohui Cai; Luisa Mannina; Corrado Rizzoli; Giampaolo Ricciardi; Claudio Ercolani; Karl M. Kadish; Angela Rosa; Inorganic Chemistry 47 (2008) 3903–3919; doi:10.1021/ic702430j

data_4304845
_publ_contact_author
;
 Prof. Corrado Rizzoli
 Universit\'a degli Studi di Parma
 Dipartimento di Chimica Generale ed Inorganica,
 Chimica Analitica, Chimica Fisica
 Viale G. P. Usberti 17/A
 I-43100 Parma"
 Italy
;
_publ_section_title
;
Tetra-2,3-pyrazinoporphyrazines with Externally Appended Pyridine Rings. 5.
Synthesis, Physicochemical and Theoretical Studies of a Novel Pentanuclear
Palladium(II) Complex and Related Mononuclear Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3903
_journal_page_last               3919
_journal_paper_doi               10.1021/ic702430j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C16 H8 Cl2 N6 Pd, 0.75(C2 H3 N)'
_chemical_formula_sum            'C17.5 H10.25 Cl2 N6.75 Pd'
_chemical_formula_weight         492.37
_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
_audit_creation_date             16/01/2007
_audit_creation_method           'ModiCIF v2.00'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.606(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.618(2)
_cell_length_b                   13.123(2)
_cell_length_c                   28.273(3)
_cell_measurement_reflns_used    2430
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.36
_cell_measurement_theta_min      3.20
_cell_volume                     4236.9(11)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELX97-L (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker SMART 1000 CCD'
_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  0.1626
_diffrn_reflns_av_sigmaI/netI    0.2843
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21207
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.743
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7841
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      0.736
_refine_ls_R_factor_all          0.2561
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                2094
_reflns_number_total             7841
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic702430j-file002.cif
_cod_data_source_block           er25
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C17.50 H10.25 Cl2 N6.75 Pd'
_cod_database_code               4304845