#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:52:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179081 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/43/4304375.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_4304375
loop_
_publ_author_name
'José Ruiz'
'María Dolores Villa'
'Natalia Cutillas'
'Concepción de Haro'
'Delia Bautista'
'Virtudes Moreno'
'Laura Valencia'
_publ_section_title
;
Palladium(II) and Platinum(II) Organometallic Complexes with
4,7-dihydro-5-methyl-7-oxo[1,2,4]triazolo[1,5-a]pyrimidine. Antitumor
Activity of the Platinum Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4490
_journal_page_last               4505
_journal_paper_doi               10.1021/ic701873b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C30 H34 N10 O2 Pd2'
_chemical_formula_weight         779.47
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.253(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7961(8)
_cell_length_b                   27.5078(18)
_cell_length_c                   11.3078(8)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      4.71
_cell_volume                     3029.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       ω-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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6040
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.9077
_exptl_absorpt_correction_T_min  0.6380
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    'methyls rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0390P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                3980
_reflns_number_total             5333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701873b-file001_4.cif
_cod_data_source_block           md11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4304375
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.58824(3) 0.591815(12) 0.82104(3) 0.01851(9) Uani 1 1 d . . .
Pd2 Pd 0.48972(3) 0.682471(12) 0.67476(3) 0.01911(9) Uani 1 1 d . . .
O1 O 0.8591(3) 0.55124(12) 0.3544(3) 0.0323(8) Uani 1 1 d . . .
O2 O 1.0689(3) 0.72561(13) 1.0118(3) 0.0348(8) Uani 1 1 d . . .
N1 N 0.6718(3) 0.62871(13) 0.3779(3) 0.0201(8) Uani 1 1 d . . .
N3 N 0.5903(3) 0.64578(13) 0.5532(3) 0.0196(8) Uani 1 1 d . . .
N4 N 0.7126(4) 0.58434(13) 0.6741(3) 0.0213(8) Uani 1 1 d . . .
N5 N 0.4397(4) 0.54234(13) 0.7492(3) 0.0223(8) Uani 1 1 d . . .
N6 N 0.3771(4) 0.72195(14) 0.7875(3) 0.0262(9) Uani 1 1 d . . .
N8 N 0.7241(3) 0.59712(13) 0.4662(3) 0.0198(8) Uani 1 1 d . . .
N11 N 0.8698(4) 0.75001(14) 0.8200(3) 0.0270(9) Uani 1 1 d . . .
N13 N 0.6858(4) 0.70234(13) 0.7643(3) 0.0222(8) Uani 1 1 d . . .
N14 N 0.7386(4) 0.63704(13) 0.9049(3) 0.0228(8) Uani 1 1 d . . .
N18 N 0.8718(4) 0.70866(13) 0.8891(3) 0.0216(8) Uani 1 1 d . . .
C2 C 0.5945(2) 0.65677(8) 0.43632(19) 0.0212(10) Uani 1 1 d . . .
H2 H 0.5443 0.6832 0.3993 0.025 Uiso 1 1 calc R . .
C3A C 0.6761(2) 0.60800(8) 0.57252(19) 0.0193(9) Uani 1 1 d R . .
C5 C 0.8109(2) 0.54877(8) 0.66643(19) 0.0234(10) Uani 1 1 d R . .
C6 C 0.8614(2) 0.53660(8) 0.56294(19) 0.0249(10) Uani 1 1 d R . .
H6 H 0.9275 0.5112 0.5650 0.030 Uiso 1 1 calc R . .
C7 C 0.8211(4) 0.55965(16) 0.4518(4) 0.0230(10) Uani 1 1 d . . .
C8 C 0.8670(5) 0.52551(18) 0.7819(4) 0.0325(12) Uani 1 1 d . . .
H8A H 0.9270 0.4983 0.7658 0.039 Uiso 1 1 calc R . .
H8B H 0.7910 0.5134 0.8233 0.039 Uiso 1 1 calc R . .
H8C H 0.9197 0.5496 0.8319 0.039 Uiso 1 1 calc R . .
C12 C 0.7572(5) 0.74365(16) 0.7480(4) 0.0262(10) Uani 1 1 d . . .
H12 H 0.7272 0.7666 0.6879 0.031 Uiso 1 1 calc R . .
C13A C 0.7608(4) 0.67998(16) 0.8544(4) 0.0202(9) Uani 1 1 d . . .
C15 C 0.8336(5) 0.62339(17) 0.9979(4) 0.0255(10) Uani 1 1 d . . .
C16 C 0.9444(5) 0.65165(17) 1.0352(4) 0.0269(11) Uani 1 1 d . . .
H16 H 1.0061 0.6402 1.0998 0.032 Uiso 1 1 calc R . .
C17 C 0.9736(5) 0.69706(17) 0.9839(4) 0.0257(11) Uani 1 1 d . . .
C18 C 0.8138(5) 0.57646(17) 1.0596(4) 0.0313(11) Uani 1 1 d . . .
H18A H 0.8964 0.5564 1.0587 0.038 Uiso 1 1 calc R . .
H18B H 0.7348 0.5593 1.0186 0.038 Uiso 1 1 calc R . .
H18C H 0.7972 0.5829 1.1421 0.038 Uiso 1 1 calc R . .
C21 C 0.3027(4) 0.66737(16) 0.5951(4) 0.0249(10) Uani 1 1 d . . .
C22 C 0.1976(5) 0.67815(17) 0.6650(4) 0.0302(11) Uani 1 1 d . . .
C23 C 0.0604(5) 0.67163(19) 0.6212(6) 0.0431(14) Uani 1 1 d . . .
H23 H -0.0100 0.6790 0.6700 0.052 Uiso 1 1 calc R . .
C24 C 0.0265(5) 0.6545(2) 0.5068(6) 0.0475(16) Uani 1 1 d . . .
H24 H -0.0671 0.6509 0.4761 0.057 Uiso 1 1 calc R . .
C25 C 0.1280(5) 0.64264(19) 0.4380(5) 0.0398(13) Uani 1 1 d . . .
H25 H 0.1048 0.6298 0.3605 0.048 Uiso 1 1 calc R . .
C26 C 0.2652(5) 0.64937(17) 0.4811(4) 0.0303(11) Uani 1 1 d . . .
H26 H 0.3346 0.6415 0.4318 0.036 Uiso 1 1 calc R . .
C27 C 0.2431(5) 0.69655(18) 0.7887(5) 0.0360(13) Uani 1 1 d . . .
H27A H 0.1737 0.7193 0.8145 0.043 Uiso 1 1 calc R . .
H27B H 0.2529 0.6690 0.8454 0.043 Uiso 1 1 calc R . .
C28 C 0.4413(6) 0.72798(18) 0.9111(4) 0.0388(13) Uani 1 1 d . . .
H28A H 0.3759 0.7436 0.9589 0.047 Uiso 1 1 calc R . .
H28B H 0.5235 0.7483 0.9116 0.047 Uiso 1 1 calc R . .
H28C H 0.4672 0.6961 0.9449 0.047 Uiso 1 1 calc R . .
C29 C 0.3514(5) 0.77098(17) 0.7348(4) 0.0336(12) Uani 1 1 d . . .
H29C H 0.3002 0.7678 0.6558 0.040 Uiso 1 1 calc R . .
H29A H 0.4393 0.7872 0.7278 0.040 Uiso 1 1 calc R . .
H29B H 0.2978 0.7903 0.7861 0.040 Uiso 1 1 calc R . .
C31 C 0.4642(4) 0.59580(15) 0.9488(4) 0.0209(9) Uani 1 1 d . . .
C32 C 0.3340(5) 0.57433(16) 0.9184(4) 0.0245(10) Uani 1 1 d . . .
C33 C 0.2369(5) 0.57309(18) 0.9975(4) 0.0304(11) Uani 1 1 d . . .
H33 H 0.1502 0.5582 0.9759 0.036 Uiso 1 1 calc R . .
C34 C 0.2673(5) 0.59396(19) 1.1103(4) 0.0353(12) Uani 1 1 d . . .
H34 H 0.2014 0.5926 1.1660 0.042 Uiso 1 1 calc R . .
C35 C 0.3901(5) 0.61615(17) 1.1409(4) 0.0293(11) Uani 1 1 d . . .
H35 H 0.4078 0.6315 1.2163 0.035 Uiso 1 1 calc R . .
C36 C 0.4913(5) 0.61661(17) 1.0616(4) 0.0264(11) Uani 1 1 d . . .
H36 H 0.5781 0.6311 1.0849 0.032 Uiso 1 1 calc R . .
C37 C 0.3062(4) 0.55650(17) 0.7926(4) 0.0248(10) Uani 1 1 d . . .
H37A H 0.2437 0.5281 0.7892 0.030 Uiso 1 1 calc R . .
H37B H 0.2616 0.5825 0.7414 0.030 Uiso 1 1 calc R . .
C38 C 0.4196(5) 0.53987(17) 0.6173(4) 0.0259(10) Uani 1 1 d . . .
H38C H 0.3425 0.5182 0.5921 0.031 Uiso 1 1 calc R . .
H38B H 0.5032 0.5273 0.5878 0.031 Uiso 1 1 calc R . .
H38A H 0.3999 0.5725 0.5849 0.031 Uiso 1 1 calc R . .
C39 C 0.4782(5) 0.49299(16) 0.7953(4) 0.0297(11) Uani 1 1 d . . .
H39B H 0.4061 0.4698 0.7669 0.036 Uiso 1 1 calc R . .
H39C H 0.4889 0.4935 0.8825 0.036 Uiso 1 1 calc R . .
H39A H 0.5651 0.4832 0.7668 0.036 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C31 Pd1 N14 95.42(16) . . ?
C31 Pd1 N5 82.17(16) . . ?
N14 Pd1 N5 175.11(14) . . ?
C31 Pd1 N4 175.90(16) . . ?
N14 Pd1 N4 88.68(14) . . ?
N5 Pd1 N4 93.76(14) . . ?
C31 Pd1 Pd2 99.47(12) . . ?
N14 Pd1 Pd2 85.73(10) . . ?
N5 Pd1 Pd2 98.85(10) . . ?
N4 Pd1 Pd2 80.52(9) . . ?
C21 Pd2 N3 94.57(17) . . ?
C21 Pd2 N6 82.13(17) . . ?
N3 Pd2 N6 175.52(14) . . ?
C21 Pd2 N13 176.75(17) . . ?
N3 Pd2 N13 88.33(14) . . ?
N6 Pd2 N13 94.89(15) . . ?
C21 Pd2 Pd1 106.96(13) . . ?
N3 Pd2 Pd1 79.40(10) . . ?
N6 Pd2 Pd1 104.42(10) . . ?
N13 Pd2 Pd1 74.99(10) . . ?
C2 N1 N8 101.3(3) . . ?
C3A N3 C2 104.2(3) . . ?
C3A N3 Pd2 127.8(2) . . ?
C2 N3 Pd2 127.7(2) . . ?
C3A N4 C5 114.5(3) . . ?
C3A N4 Pd1 119.4(2) . . ?
C5 N4 Pd1 124.5(2) . . ?
C38 N5 C39 108.1(3) . . ?
C38 N5 C37 108.4(3) . . ?
C39 N5 C37 108.7(3) . . ?
C38 N5 Pd1 115.5(3) . . ?
C39 N5 Pd1 108.6(3) . . ?
C37 N5 Pd1 107.4(3) . . ?
C28 N6 C29 108.3(4) . . ?
C28 N6 C27 109.2(4) . . ?
C29 N6 C27 108.6(4) . . ?
C28 N6 Pd2 116.0(3) . . ?
C29 N6 Pd2 107.8(3) . . ?
C27 N6 Pd2 106.7(3) . . ?
C3A N8 N1 111.2(3) . . ?
C3A N8 C7 123.8(3) . . ?
N1 N8 C7 124.9(3) . . ?
C12 N11 N18 101.6(4) . . ?
C13A N13 C12 103.9(4) . . ?
C13A N13 Pd2 129.2(3) . . ?
C12 N13 Pd2 126.7(3) . . ?
C13A N14 C15 116.0(4) . . ?
C13A N14 Pd1 118.3(3) . . ?
C15 N14 Pd1 124.9(3) . . ?
C13A N18 N11 110.6(3) . . ?
C13A N18 C17 124.0(4) . . ?
N11 N18 C17 125.4(4) . . ?
N1 C2 N3 116.0(3) . . ?
N4 C3A N3 128.6(3) . . ?
N4 C3A N8 124.2(3) . . ?
N3 C3A N8 107.2(3) . . ?
C6 C5 N4 123.31(17) . . ?
C6 C5 C8 120.6(2) . . ?
N4 C5 C8 116.0(3) . . ?
C5 C6 C7 123.9(2) . . ?
O1 C7 N8 120.9(4) . . ?
O1 C7 C6 128.9(4) . . ?
N8 C7 C6 110.2(3) . . ?
N11 C12 N13 116.0(4) . . ?
N13 C13A N14 128.9(4) . . ?
N13 C13A N18 107.9(4) . . ?
N14 C13A N18 123.2(4) . . ?
C16 C15 N14 121.9(4) . . ?
C16 C15 C18 119.3(4) . . ?
N14 C15 C18 118.8(4) . . ?
C15 C16 C17 124.4(4) . . ?
O2 C17 C16 129.5(4) . . ?
O2 C17 N18 120.0(4) . . ?
C16 C17 N18 110.5(4) . . ?
C26 C21 C22 117.6(4) . . ?
C26 C21 Pd2 129.0(4) . . ?
C22 C21 Pd2 113.4(4) . . ?
C23 C22 C21 120.9(5) . . ?
C23 C22 C27 123.3(5) . . ?
C21 C22 C27 115.8(4) . . ?
C24 C23 C22 120.0(5) . . ?
C25 C24 C23 119.9(5) . . ?
C24 C25 C26 120.2(5) . . ?
C25 C26 C21 121.3(5) . . ?
N6 C27 C22 108.7(4) . . ?
C36 C31 C32 118.0(4) . . ?
C36 C31 Pd1 128.0(3) . . ?
C32 C31 Pd1 114.0(3) . . ?
C33 C32 C31 121.4(4) . . ?
C33 C32 C37 122.8(4) . . ?
C31 C32 C37 115.7(4) . . ?
C32 C33 C34 119.3(5) . . ?
C35 C34 C33 120.6(4) . . ?
C34 C35 C36 120.5(5) . . ?
C31 C36 C35 120.1(4) . . ?
N5 C37 C32 108.7(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C31 1.989(4) . ?
Pd1 N14 2.077(4) . ?
Pd1 N5 2.091(4) . ?
Pd1 N4 2.175(3) . ?
Pd1 Pd2 3.0885(5) . ?
Pd2 C21 1.996(4) . ?
Pd2 N3 2.043(3) . ?
Pd2 N6 2.080(4) . ?
Pd2 N13 2.142(4) . ?
O1 C7 1.222(5) . ?
O2 C17 1.235(5) . ?
N1 C2 1.309(4) . ?
N1 N8 1.379(5) . ?
N3 C3A 1.339(4) . ?
N3 C2 1.361(4) . ?
N4 C3A 1.334(4) . ?
N4 C5 1.382(4) . ?
N5 C38 1.485(5) . ?
N5 C39 1.488(5) . ?
N5 C37 1.497(5) . ?
N6 C28 1.479(6) . ?
N6 C29 1.485(6) . ?
N6 C27 1.489(6) . ?
N8 C3A 1.371(4) . ?
N8 C7 1.424(5) . ?
N11 C12 1.310(6) . ?
N11 N18 1.379(5) . ?
N13 C13A 1.339(5) . ?
N13 C12 1.357(5) . ?
N14 C13A 1.340(5) . ?
N14 C15 1.379(5) . ?
N18 C13A 1.365(5) . ?
N18 C17 1.419(6) . ?
C5 C6 1.3614 . ?
C5 C8 1.503(5) . ?
C6 C7 1.425(5) . ?
C15 C16 1.363(6) . ?
C15 C18 1.490(6) . ?
C16 C17 1.419(6) . ?
C21 C26 1.393(6) . ?
C21 C22 1.397(6) . ?
C22 C23 1.393(7) . ?
C22 C27 1.508(7) . ?
C23 C24 1.383(8) . ?
C24 C25 1.367(8) . ?
C25 C26 1.390(6) . ?
C31 C36 1.397(6) . ?
C31 C32 1.414(6) . ?
C32 C33 1.376(6) . ?
C32 C37 1.501(6) . ?
C33 C34 1.401(7) . ?
C34 C35 1.360(7) . ?
C35 C36 1.406(6) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C24 H24 N8 0.95 2.52 3.344(6) 145.5 1_455
C12 H12 O2 0.95 2.40 3.190(6) 140.8 4_575
C2 H2 N11 0.95 2.60 3.538(4) 169.2 4_575
C18 H18C O1 0.98 2.56 3.386(6) 141.6 1_556
