#------------------------------------------------------------------------------
#$Date: 2018-05-23 00:12:19 +0300 (Wed, 23 May 2018) $
#$Revision: 207915 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/35/4033570.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_4033570
loop_
_publ_author_name
'Illán-Cabeza, Nuria A'
'García-García, Antonio R'
'Martínez-Martos, José M'
'Ramírez-Expósito, María J'
'Moreno-Carretero, Miguel N'
_publ_section_title
;
 Antiproliferative effects of palladium(II) complexes of
 5-nitrosopyrimidines and interactions with the proteolytic regulatory
 enzymes of the renin-angiotensin system in tumoral brain cells.
;
_journal_name_full               'Journal of inorganic biochemistry'
_journal_page_first              118
_journal_page_last               127
_journal_paper_doi               10.1016/j.jinorgbio.2013.06.005
_journal_volume                  126
_journal_year                    2013
_chemical_formula_moiety         '2(C8 H10 Cl N5 O3 Pd), O'
_chemical_formula_sum            'C16 H20 Cl2 N10 O7 Pd2'
_chemical_formula_weight         748.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.720(5)
_cell_angle_beta                 104.256(4)
_cell_angle_gamma                97.837(6)
_cell_formula_units_Z            2
_cell_length_a                   8.6817(6)
_cell_length_b                   11.5495(6)
_cell_length_c                   13.8579(6)
_cell_measurement_reflns_used    5746
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      4.03
_cell_volume                     1257.25(14)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31706
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.03
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  0.8349
_exptl_absorpt_correction_T_min  0.5794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2.10, 2003'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.369
_refine_diff_density_min         -2.081
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0607P)²+7.9044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                3856
_reflns_number_total             5746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            pddanu_871269.cif
_cod_data_source_block           import
_cod_original_cell_volume        1257.25(12)
_cod_database_code               4033570
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N1S' N 0.3301(6) 0.2451(4) 0.7287(3) 0.0202(10) Uani 1 1 d . . .
O5' O 0.2181(6) 0.4708(5) 0.8280(4) 0.0419(12) Uani 1 1 d . . .
N5' N 0.3668(7) 0.5054(5) 0.8628(4) 0.0274(11) Uani 1 1 d . . .
N3 N 0.5134(7) 0.8450(5) 0.5481(4) 0.0315(13) Uani 1 1 d . . .
C4 C 0.6329(8) 0.7833(6) 0.5228(5) 0.0288(14) Uani 1 1 d . . .
N1 N 0.2905(6) 0.6810(5) 0.4526(4) 0.0267(11) Uani 1 1 d . . .
C5 C 0.5640(8) 0.6543(6) 0.4585(5) 0.0251(12) Uani 1 1 d . . .
C5' C 0.4447(8) 0.6204(6) 0.9278(5) 0.0295(14) Uani 1 1 d . . .
C6' C 0.6195(9) 0.6385(6) 0.9590(5) 0.0297(14) Uani 1 1 d . . .
O2 O 0.2610(5) 0.8686(4) 0.5465(4) 0.0324(10) Uani 1 1 d . . .
C2 C 0.3505(8) 0.8037(6) 0.5199(5) 0.0270(13) Uani 1 1 d . . .
C3 C 0.5889(10) 0.9754(6) 0.6236(6) 0.0419(18) Uani 1 1 d . . .
H1A H 0.7072 0.9921 0.6366 0.063 Uiso 1 1 calc R . .
H1B H 0.5645 0.9844 0.6904 0.063 Uiso 1 1 calc R . .
H1C H 0.5438 1.0345 0.5927 0.063 Uiso 1 1 calc R . .
C1 C 0.1133(7) 0.6300(6) 0.4184(6) 0.0354(16) Uani 1 1 d . . .
H3A H 0.0593 0.6941 0.4491 0.053 Uiso 1 1 calc R . .
H3B H 0.0912 0.5591 0.4423 0.053 Uiso 1 1 calc R . .
H3C H 0.0717 0.6030 0.3412 0.053 Uiso 1 1 calc R . .
N1' N 0.7135(7) 0.7513(5) 1.0273(4) 0.0349(13) Uani 1 1 d . . .
O2' O 0.7293(7) 0.9479(4) 1.1308(4) 0.0447(13) Uani 1 1 d . . .
C2' C 0.6446(9) 0.8504(6) 1.0689(5) 0.0349(16) Uani 1 1 d . . .
N3' N 0.4732(7) 0.8254(5) 1.0344(4) 0.0277(12) Uani 1 1 d . . .
O4' O 0.2215(6) 0.7125(5) 0.9402(4) 0.0400(12) Uani 1 1 d . . .
C3' C 0.4001(10) 0.9328(6) 1.0803(6) 0.0430(18) Uani 1 1 d . . .
H1'1 H 0.4876 1.0032 1.1295 0.065 Uiso 1 1 calc R . .
H1'2 H 0.3274 0.9072 1.1181 0.065 Uiso 1 1 calc R . .
H1'3 H 0.3380 0.9574 1.0231 0.065 Uiso 1 1 calc R . .
C4' C 0.3679(9) 0.7203(6) 0.9649(5) 0.0330(15) Uani 1 1 d . . .
C1' C 0.8906(9) 0.7738(7) 1.0552(6) 0.0467(19) Uani 1 1 d . . .
H3'1 H 0.9381 0.8587 1.1039 0.070 Uiso 1 1 calc R . .
H3'2 H 0.9240 0.7627 0.9911 0.070 Uiso 1 1 calc R . .
H3'3 H 0.9287 0.7151 1.0892 0.070 Uiso 1 1 calc R . .
C2S C 0.9398(8) 0.2277(6) 0.2782(6) 0.0307(14) Uani 1 1 d . . .
C1S' C 0.2151(8) 0.1766(6) 0.6912(5) 0.0304(14) Uani 1 1 d . . .
C1S C 0.8008(8) 0.2834(6) 0.2914(5) 0.0282(14) Uani 1 1 d . . .
C2S' C 0.0628(9) 0.0821(7) 0.6396(6) 0.0378(16) Uani 1 1 d . . .
O4 O 0.7773(5) 0.8331(4) 0.5505(4) 0.0317(10) Uani 1 1 d . . .
O2W O -0.0001(12) 0.5026(9) 0.9554(7) 0.043(3) Uani 0.50 1 d P . .
O1W O 0.0596(12) 0.4478(9) 0.1742(8) 0.044(2) Uani 0.50 1 d P . .
H6' H 0.766(9) 0.543(7) 0.933(6) 0.03(2) Uiso 1 1 d . . .
H2S3 H 0.993(8) 0.266(6) 0.235(5) 0.035(19) Uiso 1 1 d . . .
H2S2 H 0.916(8) 0.142(6) 0.240(5) 0.026(17) Uiso 1 1 d . . .
H2S4 H -0.002(8) 0.077(6) 0.693(5) 0.027(17) Uiso 1 1 d . . .
H2S1 H 1.025(11) 0.251(8) 0.357(7) 0.07(3) Uiso 1 1 d . . .
H2S5 H -0.005(10) 0.111(7) 0.594(6) 0.05(2) Uiso 1 1 d . . .
H2S6 H 0.089(10) -0.002(8) 0.606(6) 0.06(3) Uiso 1 1 d . . .
H6 H 0.244(9) 0.460(6) 0.326(5) 0.029 Uiso 1 1 d . . .
Pd1 Pd 0.50825(5) 0.40445(4) 0.32544(3) 0.02320(15) Uani 1 1 d . . .
Pd2 Pd 0.51841(6) 0.39602(4) 0.82336(3) 0.02610(15) Uani 1 1 d . . .
Cl1 Cl 0.3247(2) 0.22275(14) 0.21572(13) 0.0311(4) Uani 1 1 d . . .
Cl2 Cl 0.7121(2) 0.28394(14) 0.78440(13) 0.0327(4) Uani 1 1 d . . .
N1S N 0.6966(6) 0.3238(5) 0.3020(4) 0.0241(11) Uani 1 1 d . . .
N6' N 0.6823(7) 0.5488(5) 0.9214(4) 0.0263(12) Uani 1 1 d . . .
N6 N 0.3359(6) 0.4941(5) 0.3559(4) 0.0227(11) Uani 1 1 d . . .
N5 N 0.6488(6) 0.5689(5) 0.4247(4) 0.0254(11) Uani 1 1 d . . .
O5 O 0.7989(5) 0.5923(4) 0.4542(4) 0.0341(11) Uani 1 1 d . . .
C6 C 0.3890(7) 0.6049(5) 0.4192(4) 0.0215(12) Uani 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1S' N1S' Pd2 166.2(5) . .
O5' N5' C5' 123.8(6) . .
O5' N5' Pd2 122.9(4) . .
C5' N5' Pd2 113.3(4) . .
C2 N3 C4 130.1(6) . .
C2 N3 C3 118.8(5) . .
C4 N3 C3 111.0(6) . .
O4 C4 N3 123.7(6) . .
O4 C4 C5 124.6(6) . .
N3 C4 C5 111.7(6) . .
C6 N1 C2 123.1(5) . .
C6 N1 C1 118.6(5) . .
C2 N1 C1 118.3(5) . .
N5 C5 C4 126.0(6) . .
N5 C5 C6 112.6(5) . .
C4 C5 C6 121.4(5) . .
N5' C5' C6' 113.6(6) . .
N5' C5' C4' 125.6(6) . .
C6' C5' C4' 120.8(6) . .
N6' C6' N1' 121.9(7) . .
N6' C6' C5' 118.7(6) . .
N1' C6' C5' 119.4(6) . .
O2 C2 N3 122.9(6) . .
O2 C2 N1 121.5(6) . .
N3 C2 N1 115.4(5) . .
N3 C3 H1A 109.5 . .
N3 C3 H1B 109.5 . .
H1A C3 H1B 109.5 . .
N3 C3 H1C 109.5 . .
H1A C3 H1C 109.5 . .
H1B C3 H1C 109.5 . .
N1 C1 H3A 109.5 . .
N1 C1 H3B 109.5 . .
H3A C1 H3B 109.5 . .
N1 C1 H3C 109.5 . .
H3A C1 H3C 109.5 . .
H3B C1 H3C 109.5 . .
C6' N1' C2' 122.1(6) . .
C6' N1' C1' 120.3(6) . .
C2' N1' C1' 117.6(6) . .
O2' C2' N1' 121.1(7) . .
O2' C2' N3' 123.9(6) . .
N1' C2' N3' 115.1(6) . .
C4' N3' C2' 128.4(6) . .
C4' N3' C3' 116.9(6) . .
C2' N3' C3' 114.6(6) . .
N3' C3' H1'1 109.5 . .
N3' C3' H1'2 109.5 . .
H1'1 C3' H1'2 109.5 . .
N3' C3' H1'3 109.5 . .
H1'1 C3' H1'3 109.5 . .
H1'2 C3' H1'3 109.5 . .
O4' C4' N3' 121.5(6) . .
O4' C4' C5' 124.4(6) . .
N3' C4' C5' 114.1(6) . .
N1' C1' H3'1 109.5 . .
N1' C1' H3'2 109.5 . .
H3'1 C1' H3'2 109.5 . .
N1' C1' H3'3 109.5 . .
H3'1 C1' H3'3 109.5 . .
H3'2 C1' H3'3 109.5 . .
C1S C2S H2S3 108(4) . .
C1S C2S H2S2 117(4) . .
H2S3 C2S H2S2 104(5) . .
C1S C2S H2S1 107(5) . .
H2S3 C2S H2S1 110(6) . .
H2S2 C2S H2S1 112(6) . .
N1S' C1S' C2S' 178.5(7) . .
N1S C1S C2S 179.0(7) . .
C1S' C2S' H2S4 111(4) . .
C1S' C2S' H2S5 107(5) . .
H2S4 C2S' H2S5 102(6) . .
C1S' C2S' H2S6 109(5) . .
H2S4 C2S' H2S6 111(6) . .
H2S5 C2S' H2S6 115(7) . .
N6 Pd1 N5 80.2(2) . .
N6 Pd1 N1S 175.8(2) . .
N5 Pd1 N1S 95.6(2) . .
N6 Pd1 Cl1 94.01(16) . .
N5 Pd1 Cl1 174.19(15) . .
N1S Pd1 Cl1 90.12(16) . .
N6' Pd2 N5' 80.7(2) . .
N6' Pd2 N1S' 173.9(2) . .
N5' Pd2 N1S' 93.5(2) . .
N6' Pd2 Cl2 94.60(17) . .
N5' Pd2 Cl2 175.17(16) . .
N1S' Pd2 Cl2 91.28(15) . .
C1S N1S Pd1 178.0(6) . .
C6' N6' Pd2 113.7(5) . .
C6' N6' H6' 131(6) . .
Pd2 N6' H6' 115(6) . .
C6 N6 Pd1 114.8(4) . .
C6 N6 H6 127(5) . .
Pd1 N6 H6 118(5) . .
O5 N5 C5 121.7(5) . .
O5 N5 Pd1 124.2(4) . .
C5 N5 Pd1 114.1(4) . .
N6 C6 N1 123.8(6) . .
N6 C6 C5 118.3(5) . .
N1 C6 C5 117.9(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1S' C1S' 1.088(8) .
N1S' Pd2 2.070(5) .
O5' N5' 1.225(7) .
N5' C5' 1.341(8) .
N5' Pd2 2.009(5) .
N3 C2 1.348(8) .
N3 C4 1.394(8) .
N3 C3 1.510(9) .
C4 O4 1.220(8) .
C4 C5 1.450(9) .
N1 C6 1.373(7) .
N1 C2 1.396(8) .
N1 C1 1.473(8) .
C5 N5 1.355(8) .
C5 C6 1.452(9) .
C5' C6' 1.439(10) .
C5' C4' 1.442(9) .
C6' N6' 1.275(8) .
C6' N1' 1.371(8) .
O2 C2 1.200(7) .
C3 H1A 0.9800 .
C3 H1B 0.9800 .
C3 H1C 0.9800 .
C1 H3A 0.9800 .
C1 H3B 0.9800 .
C1 H3C 0.9800 .
N1' C2' 1.406(9) .
N1' C1' 1.456(9) .
O2' C2' 1.205(8) .
C2' N3' 1.407(9) .
N3' C4' 1.352(9) .
N3' C3' 1.519(8) .
O4' C4' 1.216(9) .
C3' H1'1 0.9800 .
C3' H1'2 0.9800 .
C3' H1'3 0.9800 .
C1' H3'1 0.9800 .
C1' H3'2 0.9800 .
C1' H3'3 0.9800 .
C2S C1S 1.469(9) .
C2S H2S3 1.00(7) .
C2S H2S2 0.94(7) .
C2S H2S1 1.09(9) .
C1S' C2S' 1.464(10) .
C1S N1S 1.094(8) .
C2S' H2S4 1.04(7) .
C2S' H2S5 0.92(8) .
C2S' H2S6 1.03(9) .
O2W O2W 1.255(19) 2_567
Pd1 N6 1.993(5) .
Pd1 N5 2.006(5) .
Pd1 N1S 2.037(5) .
Pd1 Cl1 2.3051(17) .
Pd2 N6' 1.992(6) .
Pd2 Cl2 2.3312(17) .
N6' H6' 0.73(7) .
N6 C6 1.269(8) .
N6 H6 0.79(7) .
N5 O5 1.232(6) .
