#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/78/4327861.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_4327861
loop_
_publ_author_name
'Lisa Brückmann'
'Wieland Tyrra'
'Stefan Stucky'
'Sanjay Mathur'
_publ_section_title
;
 Novel Air-Stable and Volatile Bis(pyridylalkenolato)palladium(II) and
 -platinum(II) Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              536
_journal_page_last               542
_journal_paper_doi               10.1021/ic201996r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C16 H10 F6 N2 O2 Pd'
_chemical_formula_sum            'C16 H10 F6 N2 O2 Pd'
_chemical_formula_weight         482.66
_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                100.258(18)
_cell_angle_beta                 92.229(19)
_cell_angle_gamma                94.336(17)
_cell_formula_units_Z            2
_cell_length_a                   5.0335(7)
_cell_length_b                   9.8636(14)
_cell_length_c                   16.915(3)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.62
_cell_volume                     822.8(2)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'IPDS II (Stoe & Cie)'
_diffrn_measurement_method       'ω and φ 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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9723
_diffrn_reflns_theta_full        28.09
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       plate
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0383
_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+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                2181
_reflns_number_total             3613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201996r_si_002_1.cif
_cod_data_source_block           shelxl
_cod_database_code               4327861
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
Pd2 Pd 1.0000 1.0000 2.0000 0.04240(17) Uani 1 2 d S
Pd1 Pd 0.5000 1.0000 1.5000 0.04233(17) Uani 1 2 d S
F83 F 0.2358(10) 1.4480(3) 1.6896(3) 0.1090(15) Uani 1 1 d .
F81 F 0.3308(12) 1.4579(4) 1.5709(2) 0.1240(19) Uani 1 1 d .
N1 N 0.2073(8) 0.9358(4) 1.5702(2) 0.0455(9) Uani 1 1 d .
N2 N 0.6872(8) 0.8952(4) 1.9268(2) 0.0474(9) Uani 1 1 d .
F83A F 0.7867(14) 1.4222(4) 1.9401(3) 0.138(2) Uani 1 1 d .
O1 O 0.5034(8) 1.1944(3) 1.5547(2) 0.0638(10) Uani 1 1 d .
F82 F 0.6317(9) 1.4367(4) 1.6573(3) 0.1122(15) Uani 1 1 d .
F81A F 0.6662(11) 1.3445(4) 1.8208(3) 0.1230(18) Uani 1 1 d .
C7 C 0.3399(11) 1.2398(5) 1.6078(3) 0.0534(13) Uani 1 1 d .
O2 O 0.9807(8) 1.1659(3) 1.9504(2) 0.0664(10) Uani 1 1 d .
C2A C 0.4170(13) 0.6816(5) 1.8849(4) 0.0763(18) Uani 1 1 d .
H2A H 0.3798 0.5899 1.8901 0.092 Uiso 1 1 calc R
C5A C 0.5393(11) 0.9538(5) 1.8752(3) 0.0470(12) Uani 1 1 d .
C2 C -0.0563(13) 0.7435(6) 1.6032(4) 0.0681(15) Uani 1 1 d .
H2 H -0.0965 0.6484 1.5954 0.082 Uiso 1 1 calc R
C5 C 0.0818(11) 1.0238(5) 1.6248(3) 0.0482(12) Uani 1 1 d .
F82A F 1.0628(11) 1.3552(5) 1.8560(4) 0.153(2) Uani 1 1 d .
C7A C 0.7964(12) 1.1822(5) 1.9004(3) 0.0547(13) Uani 1 1 d .
C4A C 0.3269(12) 0.8758(6) 1.8296(3) 0.0629(14) Uani 1 1 d .
H4A H 0.2223 0.9178 1.7960 0.076 Uiso 1 1 calc R
C6 C 0.1492(11) 1.1704(5) 1.6404(3) 0.0546(13) Uani 1 1 d .
H6 H 0.0485 1.2227 1.6774 0.066 Uiso 1 1 calc R
C8 C 0.3822(14) 1.3954(5) 1.6316(4) 0.0672(15) Uani 1 1 d .
C8A C 0.8238(14) 1.3269(6) 1.8800(4) 0.0716(17) Uani 1 1 d .
C4 C -0.1215(12) 0.9689(6) 1.6672(3) 0.0610(14) Uani 1 1 d .
H4 H -0.2120 1.0290 1.7032 0.073 Uiso 1 1 calc R
C6A C 0.5956(11) 1.0951(5) 1.8654(3) 0.0537(13) Uani 1 1 d .
H6A H 0.4787 1.1286 1.8310 0.064 Uiso 1 1 calc R
C3A C 0.2666(13) 0.7385(6) 1.8325(4) 0.0700(16) Uani 1 1 d .
H3A H 0.1285 0.6864 1.8000 0.084 Uiso 1 1 calc R
C1 C 0.1355(11) 0.7989(5) 1.5615(3) 0.0595(14) Uani 1 1 d .
H1 H 0.2232 0.7389 1.5246 0.071 Uiso 1 1 calc R
C1A C 0.6230(12) 0.7611(5) 1.9296(4) 0.0667(15) Uani 1 1 d .
H1A H 0.7254 0.7200 1.9642 0.080 Uiso 1 1 calc R
C3 C -0.1908(12) 0.8313(6) 1.6576(3) 0.0648(15) Uani 1 1 d .
H3 H -0.3249 0.7970 1.6867 0.078 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'
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
O2 Pd2 O2 179.999(5) 2_779 .
O2 Pd2 N2 92.29(15) 2_779 2_779
O2 Pd2 N2 87.71(15) . 2_779
O2 Pd2 N2 87.71(15) 2_779 .
O2 Pd2 N2 92.29(15) . .
N2 Pd2 N2 179.999(2) 2_779 .
O1 Pd1 O1 180.00(8) . 2_678
O1 Pd1 N1 87.54(15) . 2_678
O1 Pd1 N1 92.46(15) 2_678 2_678
O1 Pd1 N1 92.46(15) . .
O1 Pd1 N1 87.54(15) 2_678 .
N1 Pd1 N1 180.000(2) 2_678 .
C1 N1 C5 118.1(4) . .
C1 N1 Pd1 118.4(3) . .
C5 N1 Pd1 123.5(3) . .
C1A N2 C5A 117.5(4) . .
C1A N2 Pd2 118.9(4) . .
C5A N2 Pd2 123.5(3) . .
C7 O1 Pd1 124.7(3) . .
O1 C7 C6 129.4(5) . .
O1 C7 C8 110.8(5) . .
C6 C7 C8 119.8(5) . .
C7A O2 Pd2 124.4(3) . .
C3A C2A C1A 119.2(6) . .
C3A C2A H2A 120.4 . .
C1A C2A H2A 120.4 . .
N2 C5A C4A 119.5(5) . .
N2 C5A C6A 122.2(5) . .
C4A C5A C6A 118.2(5) . .
C1 C2 C3 118.7(5) . .
C1 C2 H2 120.7 . .
C3 C2 H2 120.7 . .
N1 C5 C4 118.6(5) . .
N1 C5 C6 122.5(5) . .
C4 C5 C6 118.9(5) . .
O2 C7A C6A 130.2(5) . .
O2 C7A C8A 111.5(5) . .
C6A C7A C8A 118.3(5) . .
C3A C4A C5A 122.1(6) . .
C3A C4A H4A 119.0 . .
C5A C4A H4A 119.0 . .
C7 C6 C5 127.2(5) . .
C7 C6 H6 116.4 . .
C5 C6 H6 116.4 . .
F83 C8 F81 106.3(5) . .
F83 C8 F82 105.4(5) . .
F81 C8 F82 106.4(6) . .
F83 C8 C7 114.2(5) . .
F81 C8 C7 112.0(5) . .
F82 C8 C7 111.9(5) . .
F83A C8A F81A 107.0(6) . .
F83A C8A F82A 106.9(6) . .
F81A C8A F82A 103.6(6) . .
F83A C8A C7A 113.1(5) . .
F81A C8A C7A 114.7(5) . .
F82A C8A C7A 110.8(5) . .
C3 C4 C5 122.4(5) . .
C3 C4 H4 118.8 . .
C5 C4 H4 118.8 . .
C7A C6A C5A 126.7(5) . .
C7A C6A H6A 116.7 . .
C5A C6A H6A 116.7 . .
C2A C3A C4A 117.5(6) . .
C2A C3A H3A 121.3 . .
C4A C3A H3A 121.3 . .
N1 C1 C2 124.2(5) . .
N1 C1 H1 117.9 . .
C2 C1 H1 117.9 . .
N2 C1A C2A 124.2(5) . .
N2 C1A H1A 117.9 . .
C2A C1A H1A 117.9 . .
C4 C3 C2 118.1(6) . .
C4 C3 H3 121.0 . .
C2 C3 H3 121.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd2 O2 1.975(3) 2_779
Pd2 O2 1.975(3) .
Pd2 N2 2.056(4) 2_779
Pd2 N2 2.056(4) .
Pd1 O1 1.974(3) .
Pd1 O1 1.974(3) 2_678
Pd1 N1 2.060(4) 2_678
Pd1 N1 2.060(4) .
F83 C8 1.307(7) .
F81 C8 1.315(7) .
N1 C1 1.352(6) .
N1 C5 1.359(6) .
N2 C1A 1.347(6) .
N2 C5A 1.357(6) .
F83A C8A 1.285(7) .
O1 C7 1.286(6) .
F82 C8 1.323(8) .
F81A C8A 1.298(7) .
C7 C6 1.330(7) .
C7 C8 1.512(7) .
O2 C7A 1.270(6) .
C2A C3A 1.365(8) .
C2A C1A 1.367(8) .
C2A H2A 0.9300 .
C5A C4A 1.390(7) .
C5A C6A 1.442(7) .
C2 C1 1.356(8) .
C2 C3 1.381(8) .
C2 H2 0.9300 .
C5 C4 1.403(7) .
C5 C6 1.435(7) .
F82A C8A 1.311(8) .
C7A C6A 1.323(7) .
C7A C8A 1.524(7) .
C4A C3A 1.375(8) .
C4A H4A 0.9300 .
C6 H6 0.9300 .
C4 C3 1.354(8) .
C4 H4 0.9300 .
C6A H6A 0.9300 .
C3A H3A 0.9300 .
C1 H1 0.9300 .
C1A H1A 0.9300 .
C3 H3 0.9300 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139136785
