#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:52:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179081 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/43/4304374.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_4304374
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            'C18 H25 F5 N6 O3 Pd'
_chemical_formula_weight         574.84
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.845(4)
_cell_angle_beta                 78.512(6)
_cell_angle_gamma                69.745(6)
_cell_formula_units_Z            2
_cell_length_a                   9.2868(8)
_cell_length_b                   10.5789(6)
_cell_length_c                   12.4126(7)
_cell_measurement_reflns_used    91
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.41
_cell_measurement_theta_min      5.46
_cell_volume                     1119.08(14)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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-scan
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7918
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.13
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.8689
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         3938
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0242
_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)+(0.0368P)²+0.1658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                3485
_reflns_number_total             3938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701873b-file001_3.cif
_cod_data_source_block           md107b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Psi-scan' changed to 'psi-scan'
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 
;
_cod_original_cell_volume        1119.08(13)
_cod_database_code               4304374
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
Pd1 Pd 0.86310(2) 0.727738(19) 0.794479(15) 0.01854(7) Uani 1 1 d . . .
F22 F 0.7489(2) 0.64268(19) 0.58902(13) 0.0421(4) Uani 1 1 d . . .
F23 F 0.6032(2) 0.4638(2) 0.58550(16) 0.0599(6) Uani 1 1 d . . .
F24 F 0.5427(2) 0.3113(2) 0.77023(19) 0.0576(6) Uani 1 1 d . . .
F25 F 0.6230(3) 0.3452(2) 0.96127(17) 0.0572(6) Uani 1 1 d . . .
F26 F 0.7595(2) 0.5277(2) 0.96776(13) 0.0455(5) Uani 1 1 d . . .
N5 N 1.0888(2) 0.5949(2) 0.75453(17) 0.0236(5) Uani 1 1 d . . .
N6 N 0.9724(3) 0.8593(2) 0.83115(18) 0.0245(5) Uani 1 1 d . . .
N8 N 0.4223(3) 1.0111(2) 0.79558(18) 0.0246(5) Uani 1 1 d . . .
N1 N 0.3914(3) 0.9500(2) 0.89894(19) 0.0294(5) Uani 1 1 d . . .
N3 N 0.6455(2) 0.8624(2) 0.82360(18) 0.0236(5) Uani 1 1 d . . .
N4 N 0.6392(2) 0.9969(2) 0.65173(18) 0.0242(5) Uani 1 1 d . . .
O1 O 0.1735(2) 1.1501(2) 0.78734(18) 0.0361(5) Uani 1 1 d . . .
C11 C 1.1960(3) 0.6582(3) 0.7834(2) 0.0289(6) Uani 1 1 d . . .
H11A H 1.2994 0.6242 0.7366 0.035 Uiso 1 1 calc R . .
H11B H 1.2094 0.6327 0.8612 0.035 Uiso 1 1 calc R . .
C12 C 1.1319(3) 0.8106(3) 0.7669(2) 0.0286(6) Uani 1 1 d . . .
H12A H 1.1996 0.8515 0.7920 0.034 Uiso 1 1 calc R . .
H12B H 1.1293 0.8372 0.6878 0.034 Uiso 1 1 calc R . .
C13 C 0.9009(3) 1.0059(3) 0.8031(3) 0.0328(6) Uani 1 1 d . . .
H13A H 0.8966 1.0204 0.7241 0.039 Uiso 1 1 calc R . .
H13B H 0.9638 1.0552 0.8216 0.039 Uiso 1 1 calc R . .
H13C H 0.7953 1.0387 0.8451 0.039 Uiso 1 1 calc R . .
C14 C 0.9754(4) 0.8409(3) 0.9514(2) 0.0338(7) Uani 1 1 d . . .
H14A H 1.0484 0.8809 0.9683 0.041 Uiso 1 1 calc R . .
H14B H 1.0089 0.7443 0.9736 0.041 Uiso 1 1 calc R . .
H14C H 0.8710 0.8853 0.9916 0.041 Uiso 1 1 calc R . .
C15 C 1.1232(3) 0.5765(3) 0.6343(2) 0.0331(7) Uani 1 1 d . . .
H15A H 1.2316 0.5190 0.6139 0.040 Uiso 1 1 calc R . .
H15B H 1.1069 0.6646 0.5938 0.040 Uiso 1 1 calc R . .
H15C H 1.0537 0.5337 0.6158 0.040 Uiso 1 1 calc R . .
C16 C 1.1174(3) 0.4595(3) 0.8128(2) 0.0307(6) Uani 1 1 d . . .
H16A H 1.2279 0.4061 0.7949 0.037 Uiso 1 1 calc R . .
H16B H 1.0544 0.4136 0.7896 0.037 Uiso 1 1 calc R . .
H16C H 1.0889 0.4692 0.8925 0.037 Uiso 1 1 calc R . .
C2 C 0.5287(3) 0.8630(3) 0.9097(2) 0.0275(6) Uani 1 1 d . . .
H2 H 0.5458 0.8040 0.9736 0.033 Uiso 1 1 calc R . .
C3A C 0.5760(3) 0.9576(2) 0.7497(2) 0.0224(5) Uani 1 1 d . . .
C5 C 0.5383(3) 1.0982(3) 0.5980(2) 0.0258(6) Uani 1 1 d . . .
C6 C 0.3821(3) 1.1538(3) 0.6381(2) 0.0284(6) Uani 1 1 d . . .
H6 H 0.3191 1.2232 0.5946 0.034 Uiso 1 1 calc R . .
C7 C 0.3115(3) 1.1115(3) 0.7419(2) 0.0277(6) Uani 1 1 d . . .
C8 C 0.6092(4) 1.1497(3) 0.4892(2) 0.0344(7) Uani 1 1 d . . .
H8A H 0.6730 1.0732 0.4446 0.041 Uiso 1 1 calc R . .
H8B H 0.6746 1.2001 0.5018 0.041 Uiso 1 1 calc R . .
H8C H 0.5262 1.2092 0.4503 0.041 Uiso 1 1 calc R . .
C21 C 0.7622(3) 0.5922(2) 0.7781(2) 0.0209(5) Uani 1 1 d D . .
C22 C 0.7180(3) 0.5719(3) 0.6841(2) 0.0264(6) Uani 1 1 d D . .
C23 C 0.6436(3) 0.4797(3) 0.6803(2) 0.0347(7) Uani 1 1 d D . .
C24 C 0.6129(3) 0.4026(3) 0.7728(3) 0.0367(7) Uani 1 1 d D . .
C25 C 0.6533(4) 0.4191(3) 0.8688(3) 0.0340(7) Uani 1 1 d D . .
C26 C 0.7249(3) 0.5133(3) 0.8693(2) 0.0271(6) Uani 1 1 d D . .
O2 O -0.0147(3) 0.2828(3) 0.6308(2) 0.0614(7) Uani 1 1 d . . .
O3 O 0.0502(3) 0.1081(2) 0.46546(19) 0.0478(6) 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'
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'
F F 0.0171 0.0103 '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
C21 Pd1 N3 86.75(9) . . ?
C21 Pd1 N5 94.12(9) . . ?
N3 Pd1 N5 176.37(8) . . ?
C21 Pd1 N6 173.04(9) . . ?
N3 Pd1 N6 94.58(9) . . ?
N5 Pd1 N6 84.99(9) . . ?
C16 N5 C15 107.9(2) . . ?
C16 N5 C11 108.6(2) . . ?
C15 N5 C11 109.7(2) . . ?
C16 N5 Pd1 114.49(17) . . ?
C15 N5 Pd1 108.95(16) . . ?
C11 N5 Pd1 107.15(16) . . ?
C12 N6 C14 111.1(2) . . ?
C12 N6 C13 109.0(2) . . ?
C14 N6 C13 108.0(2) . . ?
C12 N6 Pd1 104.03(16) . . ?
C14 N6 Pd1 107.24(16) . . ?
C13 N6 Pd1 117.36(17) . . ?
C3A N8 N1 111.2(2) . . ?
C3A N8 C7 123.6(2) . . ?
N1 N8 C7 125.2(2) . . ?
C2 N1 N8 101.6(2) . . ?
C3A N3 C2 104.4(2) . . ?
C3A N3 Pd1 125.58(18) . . ?
C2 N3 Pd1 128.92(18) . . ?
C3A N4 C5 114.3(2) . . ?
N5 C11 C12 110.8(2) . . ?
N6 C12 C11 108.9(2) . . ?
N1 C2 N3 115.9(2) . . ?
N4 C3A N3 128.5(2) . . ?
N4 C3A N8 124.6(2) . . ?
N3 C3A N8 106.9(2) . . ?
N4 C5 C6 124.1(2) . . ?
N4 C5 C8 115.3(2) . . ?
C6 C5 C8 120.7(2) . . ?
C5 C6 C7 122.5(3) . . ?
O1 C7 N8 119.4(3) . . ?
O1 C7 C6 129.7(3) . . ?
N8 C7 C6 110.9(2) . . ?
C22 C21 C26 114.1(2) . . ?
C22 C21 Pd1 126.6(2) . . ?
C26 C21 Pd1 119.21(19) . . ?
F22 C22 C21 119.7(2) . . ?
F22 C22 C23 117.0(2) . . ?
C21 C22 C23 123.3(3) . . ?
F23 C23 C24 119.5(3) . . ?
F23 C23 C22 120.7(3) . . ?
C24 C23 C22 119.8(3) . . ?
F24 C24 C23 120.6(3) . . ?
F24 C24 C25 119.9(3) . . ?
C23 C24 C25 119.5(3) . . ?
F25 C25 C24 120.6(3) . . ?
F25 C25 C26 120.6(3) . . ?
C24 C25 C26 118.8(3) . . ?
F26 C26 C25 116.4(2) . . ?
F26 C26 C21 119.1(2) . . ?
C25 C26 C21 124.5(3) . . ?
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 C21 2.013(2) . ?
Pd1 N3 2.022(2) . ?
Pd1 N5 2.082(2) . ?
Pd1 N6 2.120(2) . ?
F22 C22 1.353(3) . ?
F23 C23 1.350(3) . ?
F24 C24 1.345(3) . ?
F25 C25 1.344(3) . ?
F26 C26 1.363(3) . ?
N5 C16 1.484(3) . ?
N5 C15 1.486(3) . ?
N5 C11 1.494(3) . ?
N6 C12 1.483(3) . ?
N6 C14 1.486(3) . ?
N6 C13 1.487(3) . ?
N8 C3A 1.371(3) . ?
N8 N1 1.386(3) . ?
N8 C7 1.404(4) . ?
N1 C2 1.310(4) . ?
N3 C3A 1.352(3) . ?
N3 C2 1.362(3) . ?
N4 C3A 1.325(3) . ?
N4 C5 1.359(3) . ?
O1 C7 1.239(3) . ?
C11 C12 1.516(4) . ?
C5 C6 1.375(4) . ?
C5 C8 1.505(4) . ?
C6 C7 1.419(4) . ?
C21 C22 1.376(4) . ?
C21 C26 1.381(4) . ?
C22 C23 1.386(4) . ?
C23 C24 1.365(4) . ?
C24 C25 1.366(4) . ?
C25 C26 1.377(4) . ?
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
C15 H15B O3 0.98 2.45 3.362(4) 154.5 2_666
C13 H13B O1 0.98 2.43 3.343(3) 155.1 1_655
C11 H11B F26 0.99 2.54 3.465(3) 154.6 2_767
