#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/78/4327862.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_4327862
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         'C18 H10 F10 N2 O2 Pd'
_chemical_formula_sum            'C18 H10 F10 N2 O2 Pd'
_chemical_formula_weight         582.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 96.453(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   11.411(5)
_cell_length_b                   5.940(5)
_cell_length_c                   14.471(5)
_cell_measurement_reflns_used    9269
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      3.18
_cell_volume                     974.6(10)
_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 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Stoe IPDS I'
_diffrn_measurement_method       '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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8789
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_description       needle
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0380P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                1432
_reflns_number_total             2165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201996r_si_002_2.cif
_cod_data_source_block           shelxl
_cod_database_code               4327862
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
Pd1 Pd 1.0000 0.0000 1.0000 0.03537(11) Uani 1 2 d S
F81 F 1.3692(2) -0.1949(6) 0.98199(17) 0.0921(9) Uani 1 1 d .
O1 O 1.16952(17) -0.0564(4) 1.04015(17) 0.0517(7) Uani 1 1 d .
F82 F 1.3732(2) -0.4938(5) 1.0656(2) 0.0934(8) Uani 1 1 d .
F92 F 1.52837(19) -0.1846(6) 1.1333(2) 0.1135(11) Uani 1 1 d .
F93 F 1.3941(2) -0.2418(7) 1.2212(2) 0.1264(14) Uani 1 1 d .
C4 C 0.9796(3) -0.5977(7) 1.1645(2) 0.0481(8) Uani 1 1 d .
H4 H 1.0289 -0.7174 1.1838 0.058 Uiso 1 1 calc R
N1 N 0.9509(2) -0.2495(5) 1.08480(16) 0.0383(6) Uani 1 1 d .
F91 F 1.3907(3) 0.0551(6) 1.1422(3) 0.1348(16) Uani 1 1 d .
C6 C 1.1455(3) -0.4264(6) 1.0980(2) 0.0430(8) Uani 1 1 d .
H6 H 1.1861 -0.5605 1.1109 0.052 Uiso 1 1 calc R
C8 C 1.3395(3) -0.2778(8) 1.0630(3) 0.0594(10) Uani 1 1 d .
C5 C 1.0231(3) -0.4233(6) 1.1143(2) 0.0380(8) Uani 1 1 d .
C3 C 0.8668(3) -0.5978(7) 1.1862(2) 0.0569(10) Uani 1 1 d .
H3 H 0.8382 -0.7170 1.2188 0.068 Uiso 1 1 calc R
C7 C 1.2064(3) -0.2561(6) 1.0663(2) 0.0445(8) Uani 1 1 d .
C2 C 0.7955(3) -0.4160(7) 1.1585(3) 0.0593(11) Uani 1 1 d .
H2 H 0.7187 -0.4081 1.1740 0.071 Uiso 1 1 calc R
C1 C 0.8399(3) -0.2493(7) 1.1083(2) 0.0502(9) Uani 1 1 d .
H1 H 0.7910 -0.1288 1.0891 0.060 Uiso 1 1 calc R
C9 C 1.4139(3) -0.1555(10) 1.1408(4) 0.0817(15) 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
O1 Pd1 O1 179.999(1) 3_757 .
O1 Pd1 N1 88.53(10) 3_757 .
O1 Pd1 N1 91.48(9) . .
O1 Pd1 N1 91.47(9) 3_757 3_757
O1 Pd1 N1 88.53(10) . 3_757
N1 Pd1 N1 179.999(1) . 3_757
C7 O1 Pd1 120.8(2) . .
C3 C4 C5 121.7(3) . .
C3 C4 H4 119.2 . .
C5 C4 H4 119.2 . .
C1 N1 C5 118.3(3) . .
C1 N1 Pd1 118.7(2) . .
C5 N1 Pd1 122.9(2) . .
C7 C6 C5 126.6(3) . .
C7 C6 H6 116.7 . .
C5 C6 H6 116.7 . .
F82 C8 F81 106.0(3) . .
F82 C8 C9 107.7(3) . .
F81 C8 C9 107.3(4) . .
F82 C8 C7 111.2(3) . .
F81 C8 C7 110.0(3) . .
C9 C8 C7 114.3(3) . .
N1 C5 C4 119.4(3) . .
N1 C5 C6 121.5(3) . .
C4 C5 C6 119.1(3) . .
C4 C3 C2 118.3(4) . .
C4 C3 H3 120.9 . .
C2 C3 H3 120.9 . .
O1 C7 C6 128.7(3) . .
O1 C7 C8 111.0(3) . .
C6 C7 C8 120.2(3) . .
C1 C2 C3 118.8(3) . .
C1 C2 H2 120.6 . .
C3 C2 H2 120.6 . .
N1 C1 C2 123.4(3) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
F91 C9 F93 108.2(5) . .
F91 C9 F92 109.5(5) . .
F93 C9 F92 106.8(4) . .
F91 C9 C8 112.4(4) . .
F93 C9 C8 109.5(4) . .
F92 C9 C8 110.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O1 1.985(2) 3_757
Pd1 O1 1.985(2) .
Pd1 N1 2.042(3) .
Pd1 N1 2.042(3) 3_757
F81 C8 1.349(4) .
O1 C7 1.301(4) .
F82 C8 1.338(5) .
F92 C9 1.334(4) .
F93 C9 1.313(5) .
C4 C3 1.359(5) .
C4 C5 1.389(5) .
C4 H4 0.9300 .
N1 C1 1.348(4) .
N1 C5 1.359(4) .
F91 C9 1.279(6) .
C6 C7 1.338(5) .
C6 C5 1.442(4) .
C6 H6 0.9300 .
C8 C9 1.517(6) .
C8 C7 1.530(4) .
C3 C2 1.383(6) .
C3 H3 0.9300 .
C2 C1 1.359(5) .
C2 H2 0.9300 .
C1 H1 0.9300 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139136786
