#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:53:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179904 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/00/7020006.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_7020006
loop_
_publ_author_name
'Gao, Enjun'
'Lin, Lin'
'Liu, Lei'
'Zhu, Mingchang'
'Wang, Bo'
'Gao, Xianan'
_publ_section_title
;
 Two new palladium(ii) complexes: synthesis, characterization and their
 interaction with HeLa cells.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11187
_journal_page_last               11194
_journal_paper_doi               10.1039/c2dt30990d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C8 H14 N4 O6 Pd'
_chemical_formula_weight         368.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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                 96.499(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.283(2)
_cell_length_b                   13.376(3)
_cell_length_c                   11.202(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1233.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6693
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.536
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0198
_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)+(0.0294P)²+0.5349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0530
_reflns_number_gt                2291
_reflns_number_total             2399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30990d.txt
_cod_data_source_block           sa20
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7020006
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 0.237467(18) 0.975591(11) 0.357288(13) 0.02235(7) Uani 1 1 d .
C1 C 0.2524(3) 1.01765(14) 0.6057(2) 0.0238(4) Uani 1 1 d .
C2 C 0.3337(3) 1.10512(16) 0.55039(19) 0.0289(4) Uani 1 1 d .
C3 C 0.2356(2) 1.00877(16) 0.72697(19) 0.0235(4) Uani 1 1 d .
C4 C 0.2873(2) 1.08671(16) 0.82222(18) 0.0268(4) Uani 1 1 d .
C5 C 0.1127(3) 0.85700(17) 0.6912(2) 0.0340(5) Uani 1 1 d .
H5 H 0.0643 0.8002 0.7192 0.041 Uiso 1 1 calc R
C6 C 0.1250(3) 0.86489(15) 0.56912(19) 0.0294(4) Uani 1 1 d .
H6 H 0.0835 0.8149 0.5167 0.035 Uiso 1 1 calc R
C7 C 0.2085(3) 0.84166(16) 0.15693(19) 0.0302(5) Uani 1 1 d .
H7A H 0.1448 0.7935 0.1069 0.036 Uiso 1 1 calc R
H7B H 0.3214 0.8209 0.1650 0.036 Uiso 1 1 calc R
C8 C 0.1907(3) 0.94429(17) 0.10209(19) 0.0305(5) Uani 1 1 d .
H8A H 0.2358 0.9458 0.0259 0.037 Uiso 1 1 calc R
H8B H 0.0769 0.9630 0.0884 0.037 Uiso 1 1 calc R
N1 N 0.1972(2) 0.94496(13) 0.52761(15) 0.0239(3) Uani 1 1 d .
N2 N 0.1665(2) 0.92648(14) 0.76953(16) 0.0316(4) Uani 1 1 d .
N3 N 0.1491(2) 0.84833(13) 0.27677(15) 0.0260(4) Uani 1 1 d .
H3A H 0.1832 0.7950 0.3217 0.031 Uiso 1 1 calc R
H3B H 0.0397 0.8492 0.2687 0.031 Uiso 1 1 calc R
N4 N 0.2809(2) 1.01405(13) 0.18921(17) 0.0275(4) Uani 1 1 d .
H4A H 0.2480 1.0773 0.1733 0.033 Uiso 1 1 calc R
H4B H 0.3881 1.0104 0.1829 0.033 Uiso 1 1 calc R
O1 O 0.3360(2) 1.10054(12) 0.43609(13) 0.0374(4) Uani 1 1 d .
O2 O 0.3916(2) 1.17293(13) 0.61485(15) 0.0472(5) Uani 1 1 d .
O3 O 0.18272(19) 1.15113(12) 0.83827(14) 0.0361(4) Uani 1 1 d .
O4 O 0.42299(19) 1.07524(14) 0.87995(15) 0.0408(4) Uani 1 1 d .
O5 O 0.6489(2) 0.29840(13) 0.57623(16) 0.0352(4) Uani 1 1 d .
O6 O 0.5273(3) 0.18405(16) 0.0901(2) 0.0509(5) Uani 1 1 d .
H5B H 0.571(4) 0.267(2) 0.576(3) 0.061 Uiso 1 1 d .
H6B H 0.506(4) 0.146(2) 0.025(3) 0.061 Uiso 1 1 d .
H5A H 0.662(4) 0.309(3) 0.514(3) 0.061 Uiso 1 1 d .
H6A H 0.612(4) 0.180(3) 0.105(3) 0.061 Uiso 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'
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
N1 Pd1 O1 81.74(7)
N1 Pd1 N4 176.88(7)
O1 Pd1 N4 95.21(7)
N1 Pd1 N3 99.24(7)
O1 Pd1 N3 177.35(7)
N4 Pd1 N3 83.83(7)
N1 C1 C3 120.53(18)
N1 C1 C2 115.08(19)
C3 C1 C2 124.39(19)
O2 C2 O1 125.09(19)
O2 C2 C1 119.57(19)
O1 C2 C1 115.33(18)
N2 C3 C1 120.59(19)
N2 C3 C4 114.09(18)
C1 C3 C4 125.32(18)
O4 C4 O3 127.7(2)
O4 C4 C3 116.62(19)
O3 C4 C3 115.44(18)
N2 C5 C6 123.0(2)
N1 C6 C5 119.36(19)
N3 C7 C8 106.69(16)
N4 C8 C7 106.58(17)
C6 N1 C1 118.90(18)
C6 N1 Pd1 128.40(15)
C1 N1 Pd1 112.70(14)
C5 N2 C3 117.60(18)
C7 N3 Pd1 108.25(13)
C8 N4 Pd1 108.77(13)
C2 O1 Pd1 115.12(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 N1 2.0157(17)
Pd1 O1 2.0189(16)
Pd1 N4 2.0229(19)
Pd1 N3 2.0243(17)
C1 N1 1.352(3)
C1 C3 1.387(3)
C1 C2 1.516(3)
C2 O2 1.223(3)
C2 O1 1.284(3)
C3 N2 1.352(3)
C3 C4 1.518(3)
C4 O4 1.241(3)
C4 O3 1.249(3)
C5 N2 1.320(3)
C5 C6 1.387(3)
C6 N1 1.335(3)
C7 N3 1.484(3)
C7 C8 1.504(3)
C8 N4 1.489(3)
