Reactions of Pd(II) with Chelate-Tethered 2,6-Diaminopurine Derivatives: N3-Coordination and Reaction of the Purine System
Miguel A. Galindo; David Amantia; Alberto Martinez-Martinez; William Clegg; Ross W. Harrington; Virtudes Moreno Martinez; Andrew Houlton; Inorganic Chemistry 48 (2009) 11085–11091; doi:10.1021/ic901475y

data_4303699
_publ_section_title
;
Reactions of Pd(II) with Chelate-Tethered 2,6-Diaminopurine Derivatives:
N3-Coordination and Reaction of the Purine System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11085
_journal_page_last               11091
_journal_paper_doi               10.1021/ic901475y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C11 H19 N9 Pd 2+,2 Cl -,4 H2 O'
_chemical_formula_sum            'C11 H27 Cl2 N9 O4 Pd'
_chemical_formula_weight         526.72
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.503(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.082(2)
_cell_length_b                   12.740(4)
_cell_length_c                   21.772(8)
_cell_measurement_reflns_used    11328
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      2.43
_cell_volume                     1962.5(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'narrow-frame \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7020
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16994
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.067
_refine_diff_density_min         -1.772
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.0036(4)
_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   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5008
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+4.1598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                4442
_reflns_number_total             5008
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic901475y_si_001_2.cif
_cod_data_source_block           wc903_compound2
_cod_original_cell_volume        1962.6(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303699