#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:03:01 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239829 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/02/4350295.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4350295
loop_
_publ_author_name
'Ruiz, José'
'Lorenzo, Julia'
'Sanglas, Laura'
'Cutillas, Natalia'
'Vicente, Consuelo'
'Villa, María Dolores'
'Avilés, Francesc X'
'López, Gregorio'
'Moreno, Virtudes'
'Pérez, José'
'Bautista, Delia'
_publ_section_title
;
 Palladium(II) and platinum(II) organometallic complexes with the model
 nucleobase anions of thymine, uracil, and cytosine: antitumor activity
 and interactions with DNA of the platinum compounds.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6347
_journal_page_last               6360
_journal_paper_doi               10.1021/ic060374e
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C30 H38 N6 O4 Pd2'
_chemical_formula_sum            'C30 H38 N6 O4 Pd2'
_chemical_formula_weight         759.46
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.19(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9003(2)
_cell_length_b                   19.3077(4)
_cell_length_c                   16.9681(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3114.9(2)
_computing_molecular_graphics    'CAMERON (D.J. Watkin and L.J. Pearce)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21088
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0328
_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/[σ²(Fo²)+(0.0366P)²+1.3619P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                6052
_reflns_number_total             7737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060374esi20060307_051734.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        3114.81(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4350295
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.95697(2) 0.191073(11) 0.797352(13) 0.03641(7) Uani 1 1 d .
Pd2 Pd 1.16995(2) 0.082161(11) 0.789257(13) 0.03604(7) Uani 1 1 d .
C1 C 1.0475(3) 0.27270(15) 0.8599(2) 0.0423(7) Uani 1 1 d .
C2 C 1.0731(4) 0.28592(18) 0.9428(2) 0.0563(9) Uani 1 1 d .
H2 H 1.0472 0.2532 0.9761 0.068 Uiso 1 1 calc R
C3 C 1.1364(5) 0.3469(2) 0.9774(3) 0.0738(12) Uani 1 1 d .
H3 H 1.1515 0.3548 1.0333 0.089 Uiso 1 1 calc R
C4 C 1.1768(5) 0.3956(2) 0.9300(3) 0.0814(13) Uani 1 1 d .
H4 H 1.2214 0.4359 0.9539 0.098 Uiso 1 1 calc R
C5 C 1.1516(4) 0.38498(19) 0.8473(3) 0.0717(12) Uani 1 1 d .
H5 H 1.1775 0.4185 0.8149 0.086 Uiso 1 1 calc R
C6 C 1.0870(4) 0.32376(17) 0.8114(2) 0.0513(8) Uani 1 1 d .
C7 C 1.0600(4) 0.30816(19) 0.7225(2) 0.0636(10) Uani 1 1 d .
H7A H 1.1452 0.2906 0.7120 0.076 Uiso 1 1 calc R
H7B H 1.0330 0.3503 0.6908 0.076 Uiso 1 1 calc R
N1 N 0.9457(3) 0.25580(14) 0.69665(16) 0.0502(7) Uani 1 1 d .
C8 C 0.9558(5) 0.2206(2) 0.6205(2) 0.0731(12) Uani 1 1 d .
H8A H 1.0458 0.1984 0.6306 0.110 Uiso 1 1 calc R
H8B H 0.9454 0.2541 0.5775 0.110 Uiso 1 1 calc R
H8C H 0.8826 0.1865 0.6044 0.110 Uiso 1 1 calc R
C9 C 0.8060(4) 0.2900(2) 0.6799(2) 0.0685(11) Uani 1 1 d .
H9A H 0.7332 0.2557 0.6638 0.103 Uiso 1 1 calc R
H9B H 0.7962 0.3231 0.6365 0.103 Uiso 1 1 calc R
H9C H 0.7985 0.3132 0.7285 0.103 Uiso 1 1 calc R
N2 N 0.9598(3) 0.13859(12) 0.90403(14) 0.0362(5) Uani 1 1 d .
C10 C 0.8533(3) 0.15808(15) 0.93700(18) 0.0403(6) Uani 1 1 d .
O1 O 0.7529(2) 0.19290(12) 0.89923(15) 0.0547(6) Uani 1 1 d .
C13 C 1.0788(3) 0.07824(14) 1.02919(17) 0.0367(6) Uani 1 1 d .
C14 C 1.2018(4) 0.03593(17) 1.07639(19) 0.0494(8) Uani 1 1 d .
H14A H 1.2628 0.0268 1.0425 0.074 Uiso 1 1 calc R
H14B H 1.1688 -0.0071 1.0926 0.074 Uiso 1 1 calc R
H14C H 1.2526 0.0610 1.1244 0.074 Uiso 1 1 calc R
C12 C 0.9766(4) 0.09856(16) 1.06086(18) 0.0452(7) Uani 1 1 d .
H12 H 0.9818 0.0865 1.1147 0.054 Uiso 1 1 calc R
N3 N 0.8640(3) 0.13667(14) 1.01695(15) 0.0461(6) Uani 1 1 d .
C11 C 0.7509(4) 0.1557(2) 1.0536(2) 0.0682(11) Uani 1 1 d .
H11A H 0.6805 0.1820 1.0148 0.102 Uiso 1 1 calc R
H11B H 0.7891 0.1831 1.1019 0.102 Uiso 1 1 calc R
H11C H 0.7093 0.1145 1.0682 0.102 Uiso 1 1 calc R
C15 C 1.0665(3) 0.09689(14) 0.94514(17) 0.0342(6) Uani 1 1 d .
O2 O 1.1570(2) 0.07378(11) 0.91228(12) 0.0461(5) Uani 1 1 d .
O3 O 0.8352(2) 0.11175(11) 0.72058(13) 0.0500(5) Uani 1 1 d .
N5 N 0.9929(3) 0.02303(12) 0.74283(14) 0.0381(5) Uani 1 1 d .
O4 O 1.1399(3) -0.07000(12) 0.76595(15) 0.0567(6) Uani 1 1 d .
N4 N 0.9080(3) -0.09032(13) 0.70064(17) 0.0523(7) Uani 1 1 d .
C16 C 0.8616(3) 0.04872(15) 0.71554(16) 0.0377(6) Uani 1 1 d .
C21 C 1.0215(4) -0.04653(15) 0.73825(18) 0.0416(7) Uani 1 1 d .
C17 C 0.7472(3) 0.00304(16) 0.67982(17) 0.0401(6) Uani 1 1 d .
C19 C 0.7761(4) -0.06463(17) 0.67390(19) 0.0479(8) Uani 1 1 d .
H19 H 0.7026 -0.0948 0.6505 0.057 Uiso 1 1 calc R
C18 C 0.6013(4) 0.0309(2) 0.6511(3) 0.0702(11) Uani 1 1 d .
H18A H 0.6028 0.0800 0.6607 0.105 Uiso 1 1 calc R
H18B H 0.5435 0.0088 0.6807 0.105 Uiso 1 1 calc R
H18C H 0.5636 0.0220 0.5935 0.105 Uiso 1 1 calc R
C20 C 0.9391(5) -0.16397(18) 0.6914(3) 0.0716(12) Uani 1 1 d .
H20A H 1.0381 -0.1720 0.7139 0.107 Uiso 1 1 calc R
H20B H 0.9117 -0.1760 0.6342 0.107 Uiso 1 1 calc R
H20C H 0.8878 -0.1919 0.7199 0.107 Uiso 1 1 calc R
N6 N 1.3647(3) 0.12974(14) 0.83102(16) 0.0449(6) Uani 1 1 d .
C22 C 1.2066(3) 0.09334(15) 0.68184(18) 0.0391(6) Uani 1 1 d .
C27 C 1.3153(3) 0.13950(16) 0.6825(2) 0.0461(7) Uani 1 1 d .
C23 C 1.1348(4) 0.06461(17) 0.6065(2) 0.0513(8) Uani 1 1 d .
H23 H 1.0631 0.0328 0.6040 0.062 Uiso 1 1 calc R
C29 C 1.3843(4) 0.1745(2) 0.9044(2) 0.0623(10) Uani 1 1 d .
H29A H 1.3176 0.2118 0.8920 0.093 Uiso 1 1 calc R
H29B H 1.4780 0.1930 0.9196 0.093 Uiso 1 1 calc R
H29C H 1.3699 0.1476 0.9490 0.093 Uiso 1 1 calc R
C28 C 1.3883(4) 0.17221(18) 0.7629(2) 0.0529(8) Uani 1 1 d .
H28A H 1.4883 0.1756 0.7685 0.064 Uiso 1 1 calc R
H28B H 1.3521 0.2186 0.7653 0.064 Uiso 1 1 calc R
C26 C 1.3490(4) 0.1569(2) 0.6107(2) 0.0629(10) Uani 1 1 d .
H26 H 1.4222 0.1876 0.6126 0.076 Uiso 1 1 calc R
C24 C 1.1688(5) 0.0828(2) 0.5351(2) 0.0682(11) Uani 1 1 d .
H24 H 1.1188 0.0634 0.4854 0.082 Uiso 1 1 calc R
C25 C 1.2744(5) 0.1288(2) 0.5369(3) 0.0714(11) Uani 1 1 d .
H25 H 1.2957 0.1409 0.4887 0.086 Uiso 1 1 calc R
C30 C 1.4683(4) 0.07233(19) 0.8506(2) 0.0587(9) Uani 1 1 d .
H30A H 1.4560 0.0431 0.8033 0.088 Uiso 1 1 calc R
H30B H 1.4541 0.0456 0.8953 0.088 Uiso 1 1 calc R
H30C H 1.5618 0.0911 0.8658 0.088 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 Pd1 N2 91.58(11)
C1 Pd1 N1 82.81(12)
N2 Pd1 N1 172.36(10)
C1 Pd1 O3 172.01(11)
N2 Pd1 O3 92.85(9)
N1 Pd1 O3 92.15(10)
C22 Pd2 N5 93.64(11)
C22 Pd2 N6 82.76(12)
N5 Pd2 N6 171.47(10)
C22 Pd2 O2 172.82(11)
N5 Pd2 O2 93.18(9)
N6 Pd2 O2 90.17(10)
C2 C1 C6 117.7(3)
C2 C1 Pd1 128.5(2)
C6 C1 Pd1 113.8(2)
C1 C2 C3 121.4(4)
C4 C3 C2 120.5(4)
C3 C4 C5 120.0(4)
C4 C5 C6 120.1(4)
C5 C6 C1 120.3(4)
C5 C6 C7 122.9(3)
C1 C6 C7 116.8(3)
C6 C7 N1 110.0(3)
C8 N1 C9 108.7(3)
C8 N1 C7 109.7(3)
C9 N1 C7 110.2(3)
C8 N1 Pd1 115.8(2)
C9 N1 Pd1 104.9(2)
C7 N1 Pd1 107.6(2)
C15 N2 C10 121.9(2)
C15 N2 Pd1 124.04(19)
C10 N2 Pd1 113.37(19)
O1 C10 N2 122.7(3)
O1 C10 N3 120.2(3)
N2 C10 N3 117.1(3)
C12 C13 C15 117.5(3)
C12 C13 C14 122.7(3)
C15 C13 C14 119.7(3)
C13 C12 N3 122.3(3)
C12 N3 C10 121.2(3)
C12 N3 C11 120.3(3)
C10 N3 C11 118.5(3)
O2 C15 N2 122.0(3)
O2 C15 C13 118.3(3)
N2 C15 C13 119.7(3)
C15 O2 Pd2 130.51(19)
C16 O3 Pd1 129.9(2)
C16 N5 C21 122.2(3)
C16 N5 Pd2 124.4(2)
C21 N5 Pd2 113.3(2)
C19 N4 C21 120.4(3)
C19 N4 C20 122.0(3)
C21 N4 C20 117.6(3)
O3 C16 N5 122.3(3)
O3 C16 C17 118.2(3)
N5 C16 C17 119.5(3)
O4 C21 N5 122.0(3)
O4 C21 N4 120.7(3)
N5 C21 N4 117.4(3)
C19 C17 C16 118.1(3)
C19 C17 C18 122.2(3)
C16 C17 C18 119.8(3)
C17 C19 N4 122.4(3)
C29 N6 C30 109.1(3)
C29 N6 C28 108.6(3)
C30 N6 C28 109.7(3)
C29 N6 Pd2 115.8(2)
C30 N6 Pd2 105.3(2)
C28 N6 Pd2 108.12(19)
C23 C22 C27 117.2(3)
C23 C22 Pd2 128.9(2)
C27 C22 Pd2 113.8(2)
C26 C27 C22 121.3(3)
C26 C27 C28 121.7(3)
C22 C27 C28 117.0(3)
C22 C23 C24 120.9(3)
N6 C28 C27 109.6(3)
C25 C26 C27 120.2(4)
C25 C24 C23 121.0(4)
C24 C25 C26 119.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C1 1.970(3)
Pd1 N2 2.068(2)
Pd1 N1 2.095(2)
Pd1 O3 2.150(2)
Pd2 C22 1.967(3)
Pd2 N5 2.056(2)
Pd2 N6 2.074(3)
Pd2 O2 2.133(2)
C1 C2 1.382(5)
C1 C6 1.408(4)
C2 C3 1.386(5)
C3 C4 1.367(6)
C4 C5 1.372(6)
C5 C6 1.400(5)
C6 C7 1.488(5)
C7 N1 1.489(5)
N1 C8 1.487(4)
N1 C9 1.486(4)
N2 C15 1.356(4)
N2 C10 1.377(4)
C10 O1 1.223(4)
C10 N3 1.394(4)
C13 C12 1.331(4)
C13 C15 1.443(4)
C13 C14 1.499(4)
C12 N3 1.370(4)
N3 C11 1.472(4)
C15 O2 1.262(3)
O3 C16 1.253(4)
N5 C16 1.347(4)
N5 C21 1.379(4)
O4 C21 1.222(4)
N4 C19 1.351(5)
N4 C21 1.409(4)
N4 C20 1.473(4)
C16 C17 1.430(4)
C17 C19 1.347(4)
C17 C18 1.491(5)
N6 C29 1.483(4)
N6 C30 1.483(4)
N6 C28 1.487(4)
C22 C23 1.393(4)
C22 C27 1.395(4)
C27 C26 1.391(5)
C27 C28 1.494(5)
C23 C24 1.390(5)
C26 C25 1.376(6)
C24 C25 1.365(6)
