#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:21:35 +0100 (vie 25 de mar de 2016) $
#$Revision: 180074 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/20/7052019.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_7052019
loop_
_publ_author_name
'Budzisz, Elzbieta'
'Lorenz, Ingo-Peter'
'Mayer, Peter'
'Paneth, Piotr'
'Szatkowski, Lukasz'
'Krajewska, Urszula'
'Rozalski, Marek'
'Miernicka, Magdalena'
_publ_section_title
;
 Synthesis, crystal structure, theoretical calculation and cytotoxic
 effect of new Pt(ii), Pd(ii) and Cu(ii) complexes with
 pyridine-pyrazoles derivatives
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2238
_journal_paper_doi               10.1039/b808301k
_journal_volume                  32
_journal_year                    2008
_chemical_formula_moiety         'Pd, 2Cl, C16 H11 N3 O2'
_chemical_formula_sum            'C16 H11 Cl2 N3 O2 Pd'
_chemical_formula_weight         454.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Pd_Cl_C16H11N3O2_jn526_lorenz
_audit_creation_date             28-Dec-05
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             13-Jun-08
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1538(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5751(2)
_cell_length_b                   24.2068(4)
_cell_length_c                   7.00870(10)
_cell_measurement_reflns_used    3574
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     1568.01(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of Göttingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0493095
_diffrn_orient_matrix_UB_12      0.0383796
_diffrn_orient_matrix_UB_13      -0.0072731
_diffrn_orient_matrix_UB_21      0.0332178
_diffrn_orient_matrix_UB_22      -0.0100457
_diffrn_orient_matrix_UB_23      -0.0921905
_diffrn_orient_matrix_UB_31      -0.1353361
_diffrn_orient_matrix_UB_32      0.0115179
_diffrn_orient_matrix_UB_33      -0.0561715
_diffrn_radiation_collimation    0.20
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6706
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.34
_diffrn_source_current           45.00
_diffrn_source_power             2.250
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.92575(6)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0295
_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)+(0.0401P)²+0.0500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                2706
_reflns_number_total             3560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b808301k.txt
_cod_data_source_block           jn526
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7052019
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Pd Pd 0.43935(2) 0.251817(7) 0.47184(3) 0.02302(9) Uani 1 1 d . . .
Cl1 Cl 0.64984(7) 0.30013(3) 0.56937(11) 0.03674(19) Uani 1 1 d . . .
Cl2 Cl 0.31647(8) 0.33338(3) 0.42309(11) 0.03282(17) Uani 1 1 d . . .
O1 O 0.6423(2) 0.00124(7) 0.7694(3) 0.0366(5) Uani 1 1 d . . .
O2 O 0.8431(2) 0.04857(9) 0.7835(3) 0.0485(6) Uani 1 1 d . . .
N1 N 0.2562(2) 0.20571(8) 0.3798(3) 0.0236(5) Uani 1 1 d . . .
N2 N 0.4137(2) 0.13675(8) 0.5236(3) 0.0242(5) Uani 1 1 d . . .
N3 N 0.5252(2) 0.17422(9) 0.5227(3) 0.0260(5) Uani 1 1 d . . .
C1 C 0.1291(3) 0.22423(11) 0.2654(4) 0.0304(6) Uani 1 1 d . . .
H1 H 0.1135 0.2629 0.2486 0.037 Uiso 1 1 calc R . .
C2 C 0.0210(3) 0.18827(12) 0.1723(4) 0.0353(7) Uani 1 1 d . . .
H2 H -0.0699 0.2019 0.0974 0.042 Uiso 1 1 calc R . .
C3 C 0.0473(3) 0.13215(12) 0.1896(4) 0.0350(7) Uani 1 1 d . . .
H3 H -0.0241 0.1069 0.1205 0.042 Uiso 1 1 calc R . .
C4 C 0.1763(3) 0.11276(11) 0.3066(4) 0.0284(6) Uani 1 1 d . . .
H4 H 0.1960 0.0743 0.3197 0.034 Uiso 1 1 calc R . .
C5 C 0.2770(3) 0.15145(11) 0.4052(4) 0.0237(6) Uani 1 1 d . . .
C6 C 0.4693(3) 0.08943(10) 0.6175(4) 0.0255(6) Uani 1 1 d . . .
C7 C 0.4008(3) 0.04149(11) 0.6749(4) 0.0285(6) Uani 1 1 d . . .
C8 C 0.2553(3) 0.03604(11) 0.6799(4) 0.0338(7) Uani 1 1 d . . .
H8 H 0.1905 0.0662 0.6422 0.041 Uiso 1 1 calc R . .
C9 C 0.2066(4) -0.01312(11) 0.7396(4) 0.0395(7) Uani 1 1 d . . .
H9 H 0.1082 -0.0167 0.7414 0.047 Uiso 1 1 calc R . .
C10 C 0.3004(4) -0.05697(12) 0.7967(4) 0.0413(8) Uani 1 1 d . . .
H10 H 0.2644 -0.0912 0.8305 0.050 Uiso 1 1 calc R . .
C11 C 0.4447(4) -0.05196(11) 0.8054(4) 0.0383(7) Uani 1 1 d . . .
H11 H 0.5094 -0.0818 0.8498 0.046 Uiso 1 1 calc R . .
C12 C 0.4947(3) -0.00230(10) 0.7480(4) 0.0303(7) Uani 1 1 d . . .
C13 C 0.7135(3) 0.04980(12) 0.7421(4) 0.0346(7) Uani 1 1 d . . .
C14 C 0.6176(3) 0.09486(11) 0.6630(4) 0.0280(6) Uani 1 1 d . . .
C15 C 0.6493(3) 0.14830(11) 0.6046(4) 0.0285(6) Uani 1 1 d . . .
C16 C 0.7926(3) 0.17379(12) 0.6217(4) 0.0371(7) Uani 1 1 d . . .
H16A H 0.7936 0.1912 0.4958 0.056 Uiso 1 1 calc R . .
H16B H 0.8677 0.1453 0.6543 0.056 Uiso 1 1 calc R . .
H16C H 0.8114 0.2018 0.7263 0.056 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'
Cl Cl 0.1484 0.1585 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.015000
0 -1 0 0.001000
1 0 -14 0.040000
-1 0 14 0.050000
10 4 -3 0.050000
-10 -4 3 0.060000
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
N1 Pd N3 79.93(8) . . ?
N1 Pd Cl1 177.28(6) . . ?
N3 Pd Cl1 97.81(6) . . ?
N1 Pd Cl2 93.40(6) . . ?
N3 Pd Cl2 172.33(6) . . ?
Cl1 Pd Cl2 88.96(3) . . ?
C12 O1 C13 123.9(2) . . ?
C5 N1 C1 119.1(2) . . ?
C5 N1 Pd 114.32(17) . . ?
C1 N1 Pd 125.14(17) . . ?
C6 N2 C5 133.5(2) . . ?
C6 N2 N3 110.2(2) . . ?
C5 N2 N3 115.3(2) . . ?
C15 N3 N2 106.7(2) . . ?
C15 N3 Pd 141.23(18) . . ?
N2 N3 Pd 108.87(15) . . ?
N1 C1 C2 121.4(2) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C1 C2 C3 118.9(3) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 117.7(2) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
N1 C5 C4 122.5(2) . . ?
N1 C5 N2 114.4(2) . . ?
C4 C5 N2 122.8(2) . . ?
N2 C6 C14 106.4(2) . . ?
N2 C6 C7 131.7(2) . . ?
C14 C6 C7 121.9(2) . . ?
C12 C7 C8 117.7(3) . . ?
C12 C7 C6 114.7(3) . . ?
C8 C7 C6 127.4(2) . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 120.3(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 118.8(3) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
O1 C12 C11 116.1(2) . . ?
O1 C12 C7 122.2(2) . . ?
C11 C12 C7 121.6(3) . . ?
O2 C13 O1 117.2(3) . . ?
O2 C13 C14 128.9(3) . . ?
O1 C13 C14 113.9(2) . . ?
C6 C14 C15 107.8(2) . . ?
C6 C14 C13 122.1(3) . . ?
C15 C14 C13 129.9(3) . . ?
N3 C15 C14 108.7(2) . . ?
N3 C15 C16 122.8(3) . . ?
C14 C15 C16 128.5(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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
Pd N1 2.036(2) . ?
Pd N3 2.044(2) . ?
Pd Cl1 2.2752(7) . ?
Pd Cl2 2.2780(7) . ?
O1 C12 1.384(3) . ?
O1 C13 1.397(4) . ?
O2 C13 1.199(3) . ?
N1 C5 1.333(3) . ?
N1 C1 1.348(3) . ?
N2 C6 1.358(3) . ?
N2 C5 1.400(3) . ?
N2 N3 1.402(3) . ?
N3 C15 1.334(3) . ?
C1 C2 1.379(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.381(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(4) . ?
C4 H4 0.9500 . ?
C6 C14 1.378(4) . ?
C6 C7 1.441(4) . ?
C7 C12 1.398(4) . ?
C7 C8 1.409(4) . ?
C8 C9 1.382(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.373(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(4) . ?
C11 H11 0.9500 . ?
C13 C14 1.440(4) . ?
C14 C15 1.414(4) . ?
C15 C16 1.481(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
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
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Pd N1 C5 3.38(18) . . . . ?
Cl1 Pd N1 C5 37.0(14) . . . . ?
Cl2 Pd N1 C5 -172.81(17) . . . . ?
N3 Pd N1 C1 -162.9(2) . . . . ?
Cl1 Pd N1 C1 -129.3(12) . . . . ?
Cl2 Pd N1 C1 20.9(2) . . . . ?
C6 N2 N3 C15 4.0(3) . . . . ?
C5 N2 N3 C15 -166.4(2) . . . . ?
C6 N2 N3 Pd -160.38(17) . . . . ?
C5 N2 N3 Pd 29.2(2) . . . . ?
N1 Pd N3 C15 -172.8(3) . . . . ?
Cl1 Pd N3 C15 8.7(3) . . . . ?
Cl2 Pd N3 C15 -142.9(4) . . . . ?
N1 Pd N3 N2 -17.12(15) . . . . ?
Cl1 Pd N3 N2 164.40(14) . . . . ?
Cl2 Pd N3 N2 12.7(6) . . . . ?
C5 N1 C1 C2 -0.9(4) . . . . ?
Pd N1 C1 C2 164.8(2) . . . . ?
N1 C1 C2 C3 -3.2(4) . . . . ?
C1 C2 C3 C4 3.4(4) . . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C1 N1 C5 C4 4.8(4) . . . . ?
Pd N1 C5 C4 -162.4(2) . . . . ?
C1 N1 C5 N2 178.9(2) . . . . ?
Pd N1 C5 N2 11.7(3) . . . . ?
C3 C4 C5 N1 -4.4(4) . . . . ?
C3 C4 C5 N2 -178.0(2) . . . . ?
C6 N2 C5 N1 164.6(3) . . . . ?
N3 N2 C5 N1 -27.9(3) . . . . ?
C6 N2 C5 C4 -21.3(4) . . . . ?
N3 N2 C5 C4 146.2(2) . . . . ?
C5 N2 C6 C14 163.3(3) . . . . ?
N3 N2 C6 C14 -4.7(3) . . . . ?
C5 N2 C6 C7 -19.3(5) . . . . ?
N3 N2 C6 C7 172.7(3) . . . . ?
N2 C6 C7 C12 172.4(3) . . . . ?
C14 C6 C7 C12 -10.6(4) . . . . ?
N2 C6 C7 C8 -13.1(5) . . . . ?
C14 C6 C7 C8 163.9(3) . . . . ?
C12 C7 C8 C9 -5.5(4) . . . . ?
C6 C7 C8 C9 -179.8(3) . . . . ?
C7 C8 C9 C10 0.7(4) . . . . ?
C8 C9 C10 C11 3.4(5) . . . . ?
C9 C10 C11 C12 -2.5(4) . . . . ?
C13 O1 C12 C11 -172.0(2) . . . . ?
C13 O1 C12 C7 7.4(4) . . . . ?
C10 C11 C12 O1 176.9(2) . . . . ?
C10 C11 C12 C7 -2.5(4) . . . . ?
C8 C7 C12 O1 -172.9(2) . . . . ?
C6 C7 C12 O1 2.1(4) . . . . ?
C8 C7 C12 C11 6.4(4) . . . . ?
C6 C7 C12 C11 -178.5(2) . . . . ?
C12 O1 C13 O2 173.0(2) . . . . ?
C12 O1 C13 C14 -8.0(4) . . . . ?
N2 C6 C14 C15 3.6(3) . . . . ?
C7 C6 C14 C15 -174.1(2) . . . . ?
N2 C6 C14 C13 -172.2(2) . . . . ?
C7 C6 C14 C13 10.1(4) . . . . ?
O2 C13 C14 C6 178.1(3) . . . . ?
O1 C13 C14 C6 -0.6(4) . . . . ?
O2 C13 C14 C15 3.3(5) . . . . ?
O1 C13 C14 C15 -175.4(3) . . . . ?
N2 N3 C15 C14 -1.6(3) . . . . ?
Pd N3 C15 C14 154.4(2) . . . . ?
N2 N3 C15 C16 177.1(2) . . . . ?
Pd N3 C15 C16 -27.0(5) . . . . ?
C6 C14 C15 N3 -1.2(3) . . . . ?
C13 C14 C15 N3 174.1(3) . . . . ?
C6 C14 C15 C16 -179.8(3) . . . . ?
C13 C14 C15 C16 -4.5(5) . . . . ?
loop_
_reflns_scale_group_code
_reflns_scale_meas_F
1 1.0
