#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:52:15 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301804 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/48/2214812.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214812
loop_
_publ_author_name
'Guang-Quan Mei'
'Ke-Long Huang'
_publ_section_title
;(Acetonitrile-κN)(2,2':6',2''-terpyridyl-κ³N)palladium(II)]
 bis(hexafluorophosphate)
;
_journal_coeditor_code           NG2287
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2029
_journal_page_last               m2029
_journal_paper_doi               10.1107/S160053680703070X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Pd (C15 H11 N3) (C2 H3 N)] (P F6)2'
_chemical_formula_moiety         'C17 H14 N4 Pd 2+, 2(P F6 -)'
_chemical_formula_sum            'C17 H14 F12 N4 P2 Pd'
_chemical_formula_weight         670.66
_chemical_name_systematic
;
(Acetonitrile-\kN)(2,2':6',2''-terpyridyl-κ³N)palladium(II)]
bis(hexafluorophosphate)
;
_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                90.00
_cell_angle_beta                 97.8100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1073(3)
_cell_length_b                   11.8840(3)
_cell_length_c                   14.6085(4)
_cell_measurement_reflns_used    8518
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.22
_cell_volume                     2254.42(10)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16715
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.7972
_exptl_absorpt_correction_T_min  0.7379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.610
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0448
_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)+(0.0789P)²+2.9852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                4503
_reflns_number_total             5449
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2287.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2214812
_cod_database_fobs_code          2214812
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Pd Pd1 0.76117(2) 0.28974(2) 0.599820(18) 0.04089(12) Uani d . 1
N N1 0.6996(2) 0.3828(3) 0.6946(2) 0.0479(7) Uani d . 1
N N2 0.7149(2) 0.1693(3) 0.6726(2) 0.0426(6) Uani d . 1
N N3 0.8072(2) 0.1568(3) 0.5289(2) 0.0444(6) Uani d . 1
N N4 0.8108(3) 0.4156(3) 0.5235(2) 0.0527(8) Uani d . 1
C C1 0.6934(3) 0.4957(4) 0.6996(3) 0.0570(10) Uani d . 1
H H1 0.7211 0.5393 0.6562 0.068 Uiso calc R 1
C C2 0.6472(4) 0.5483(5) 0.7672(4) 0.0691(12) Uani d . 1
H H2 0.6433 0.6263 0.7692 0.083 Uiso calc R 1
C C3 0.6070(4) 0.4841(5) 0.8313(3) 0.0695(13) Uani d . 1
H H3 0.5765 0.5187 0.8779 0.083 Uiso calc R 1
C C4 0.6115(3) 0.3684(5) 0.8272(3) 0.0617(11) Uani d . 1
H H4 0.5833 0.3241 0.8699 0.074 Uiso calc R 1
C C5 0.6589(3) 0.3196(4) 0.7584(3) 0.0498(8) Uani d . 1
C C6 0.6679(3) 0.1969(4) 0.7459(3) 0.0489(9) Uani d . 1
C C7 0.6330(4) 0.1121(4) 0.7987(3) 0.0622(11) Uani d . 1
H H7 0.5998 0.1286 0.8494 0.075 Uiso calc R 1
C C8 0.6495(4) 0.0009(4) 0.7734(3) 0.0691(13) Uani d . 1
H H8 0.6265 -0.0574 0.8079 0.083 Uiso calc R 1
C C9 0.6985(4) -0.0243(4) 0.6990(3) 0.0615(11) Uani d . 1
H H9 0.7095 -0.0988 0.6832 0.074 Uiso calc R 1
C C10 0.7317(3) 0.0635(3) 0.6473(3) 0.0475(8) Uani d . 1
C C11 0.7857(3) 0.0558(3) 0.5664(3) 0.0468(8) Uani d . 1
C C12 0.8143(4) -0.0446(4) 0.5296(3) 0.0594(10) Uani d . 1
H H12 0.8001 -0.1127 0.5567 0.071 Uiso calc R 1
C C13 0.8644(4) -0.0430(4) 0.4523(4) 0.0664(12) Uani d . 1
H H13 0.8837 -0.1098 0.4263 0.080 Uiso calc R 1
C C14 0.8852(4) 0.0591(4) 0.4143(3) 0.0648(11) Uani d . 1
H H14 0.9185 0.0619 0.3621 0.078 Uiso calc R 1
C C15 0.8562(3) 0.1575(4) 0.4544(3) 0.0533(9) Uani d . 1
H H15 0.8713 0.2261 0.4287 0.064 Uiso calc R 1
C C16 0.8393(3) 0.4869(4) 0.4829(3) 0.0554(9) Uani d . 1
C C17 0.8762(4) 0.5793(4) 0.4315(4) 0.0729(13) Uani d . 1
H H17A 0.8209 0.6312 0.4137 0.109 Uiso calc R 1
H H17B 0.9011 0.5506 0.3772 0.109 Uiso calc R 1
H H17C 0.9310 0.6174 0.4695 0.109 Uiso calc R 1
P P1 0.42931(10) 0.28021(9) 0.51579(8) 0.0546(3) Uani d . 1
F F1 0.3845(4) 0.4019(3) 0.5203(3) 0.1248(16) Uani d . 1
F F2 0.4705(4) 0.2847(4) 0.6212(3) 0.1263(17) Uani d . 1
F F3 0.4664(6) 0.1569(4) 0.5074(4) 0.177(3) Uani d . 1
F F4 0.3944(6) 0.2746(5) 0.4096(3) 0.158(3) Uani d . 1
F F5 0.5332(4) 0.3245(6) 0.4898(4) 0.158(2) Uani d . 1
F F6 0.3290(4) 0.2329(6) 0.5489(5) 0.160(2) Uani d . 1
P P2 0.02951(11) 0.19057(12) 0.77715(10) 0.0668(3) Uani d . 1
F F7 0.1387(4) 0.2137(5) 0.7471(4) 0.142(2) Uani d . 1
F F8 0.0705(5) 0.0699(4) 0.8046(5) 0.169(2) Uani d . 1
F F9 -0.0789(4) 0.1664(6) 0.8057(4) 0.162(2) Uani d . 1
F F10 -0.0074(9) 0.3078(6) 0.7566(6) 0.237(5) Uani d . 1
F F11 0.0641(5) 0.2300(6) 0.8785(4) 0.156(2) Uani d . 1
F F12 -0.0095(4) 0.1471(8) 0.6798(4) 0.222(4) Uani d . 1
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_publ_flag
N2 Pd1 N1 81.00(10) y
N2 Pd1 N4 179.60(10) y
N1 Pd1 N4 99.20(10) ?
N2 Pd1 N3 80.90(10) y
N1 Pd1 N3 161.90(10) y
N4 Pd1 N3 98.90(10) ?
C1 N1 C5 118.7(4) ?
C1 N1 Pd1 127.9(3) ?
C5 N1 Pd1 113.4(3) ?
C10 N2 C6 123.9(3) ?
C10 N2 Pd1 118.0(2) ?
C6 N2 Pd1 118.0(3) ?
C15 N3 C11 118.7(3) ?
C15 N3 Pd1 128.4(3) ?
C11 N3 Pd1 112.9(2) ?
C16 N4 Pd1 178.3(4) ?
N1 C1 C2 121.8(4) ?
N1 C1 H1 119.1 ?
C2 C1 H1 119.1 ?
C3 C2 C1 119.1(5) ?
C3 C2 H2 120.4 ?
C1 C2 H2 120.4 ?
C2 C3 C4 120.2(4) ?
C2 C3 H3 119.9 ?
C4 C3 H3 119.9 ?
C3 C4 C5 118.5(5) ?
C3 C4 H4 120.7 ?
C5 C4 H4 120.7 ?
N1 C5 C4 121.6(4) ?
N1 C5 C6 114.5(3) ?
C4 C5 C6 123.8(4) ?
N2 C6 C7 119.2(4) ?
N2 C6 C5 113.1(3) ?
C7 C6 C5 127.7(4) ?
C6 C7 C8 117.8(4) ?
C6 C7 H7 121.1 ?
C8 C7 H7 121.1 ?
C9 C8 C7 121.5(4) ?
C9 C8 H8 119.2 ?
C7 C8 H8 119.2 ?
C8 C9 C10 118.8(4) ?
C8 C9 H9 120.6 ?
C10 C9 H9 120.6 ?
N2 C10 C9 118.7(4) ?
N2 C10 C11 113.5(3) ?
C9 C10 C11 127.8(4) ?
N3 C11 C12 121.5(4) ?
N3 C11 C10 114.8(3) ?
C12 C11 C10 123.8(4) ?
C11 C12 C13 119.4(4) ?
C11 C12 H12 120.3 ?
C13 C12 H12 120.3 ?
C14 C13 C12 118.9(4) ?
C14 C13 H13 120.5 ?
C12 C13 H13 120.5 ?
C13 C14 C15 119.6(4) ?
C13 C14 H14 120.2 ?
C15 C14 H14 120.2 ?
N3 C15 C14 122.0(4) ?
N3 C15 H15 119.0 ?
C14 C15 H15 119.0 ?
N4 C16 C17 179.5(5) ?
C16 C17 H17A 109.5 ?
C16 C17 H17B 109.5 ?
H17A C17 H17B 109.5 ?
C16 C17 H17C 109.5 ?
H17A C17 H17C 109.5 ?
H17B C17 H17C 109.5 ?
F3 P1 F5 90.3(4) ?
F3 P1 F4 86.2(3) ?
F5 P1 F4 85.4(4) ?
F3 P1 F2 92.3(3) ?
F5 P1 F2 91.8(3) ?
F4 P1 F2 176.8(4) ?
F3 P1 F6 88.3(4) ?
F5 P1 F6 175.8(4) ?
F4 P1 F6 98.5(4) ?
F2 P1 F6 84.3(3) ?
F3 P1 F1 176.0(4) ?
F5 P1 F1 92.5(3) ?
F4 P1 F1 91.2(3) ?
F2 P1 F1 90.5(3) ?
F6 P1 F1 89.0(3) ?
F10 P2 F12 94.0(5) ?
F10 P2 F9 86.8(5) ?
F12 P2 F9 89.1(3) ?
F10 P2 F11 87.4(5) ?
F12 P2 F11 176.4(5) ?
F9 P2 F11 87.7(3) ?
F10 P2 F8 176.7(5) ?
F12 P2 F8 89.3(4) ?
F9 P2 F8 93.2(4) ?
F11 P2 F8 89.2(4) ?
F10 P2 F7 93.6(5) ?
F12 P2 F7 90.1(4) ?
F9 P2 F7 179.1(3) ?
F11 P2 F7 93.1(3) ?
F8 P2 F7 86.4(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N1 2.023(3) y
Pd1 N2 1.929(3) y
Pd1 N3 2.026(3) y
Pd1 N4 2.025(3) y
N1 C1 1.346(5) ?
N1 C5 1.362(5) ?
N2 C10 1.338(5) ?
N2 C6 1.346(5) ?
N3 C15 1.337(5) ?
N3 C11 1.365(5) ?
N4 C16 1.126(5) ?
C1 C2 1.377(6) ?
C1 H1 0.9300 ?
C2 C3 1.367(8) ?
C2 H2 0.9300 ?
C3 C4 1.379(7) ?
C3 H3 0.9300 ?
C4 C5 1.379(6) ?
C4 H4 0.9300 ?
C5 C6 1.477(6) ?
C6 C7 1.384(6) ?
C7 C8 1.397(7) ?
C7 H7 0.9300 ?
C8 C9 1.369(7) ?
C8 H8 0.9300 ?
C9 C10 1.391(5) ?
C9 H9 0.9300 ?
C10 C11 1.461(6) ?
C11 C12 1.381(6) ?
C12 C13 1.381(7) ?
C12 H12 0.9300 ?
C13 C14 1.377(7) ?
C13 H13 0.9300 ?
C14 C15 1.383(6) ?
C14 H14 0.9300 ?
C15 H15 0.9300 ?
C16 C17 1.451(6) ?
C17 H17A 0.9600 ?
C17 H17B 0.9600 ?
C17 H17C 0.9600 ?
P1 F3 1.554(4) ?
P1 F5 1.555(4) ?
P1 F4 1.558(5) ?
P1 F2 1.561(4) ?
P1 F6 1.566(5) ?
P1 F1 1.566(4) ?
P2 F10 1.491(6) ?
P2 F12 1.533(5) ?
P2 F9 1.561(5) ?
P2 F11 1.561(5) ?
P2 F8 1.565(5) ?
P2 F7 1.578(5) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C15 H15 F9 4_665 0.93 2.37 3.213(6) 151
C14 H14 F10 4_665 0.93 2.47 3.268(9) 143
C13 H13 F12 3_656 0.93 2.45 3.142(7) 131
C7 H7 F5 4_566 0.93 2.40 3.326(7) 173
C3 H3 F3 2_656 0.93 2.47 3.363(7) 162
P1 F2 Cg1 . ? 2.95 3.062(5) 122.3(3)
P2 F12 Cg2 1_455 ? 2.97 3.075(6) 121.7(3)
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
N2 Pd1 N1 C1 -178.6(4)
N4 Pd1 N1 C1 1.7(4)
N3 Pd1 N1 C1 -178.3(4)
N2 Pd1 N1 C5 0.0(3)
N4 Pd1 N1 C5 -179.7(3)
N3 Pd1 N1 C5 0.3(6)
N1 Pd1 N2 C10 179.9(3)
N3 Pd1 N2 C10 0.0(3)
N1 Pd1 N2 C6 -0.1(3)
N3 Pd1 N2 C6 180.0(3)
N2 Pd1 N3 C15 -179.3(4)
N1 Pd1 N3 C15 -179.7(4)
N4 Pd1 N3 C15 0.3(4)
N2 Pd1 N3 C11 -1.0(3)
N1 Pd1 N3 C11 -1.3(6)
N4 Pd1 N3 C11 178.7(3)
C5 N1 C1 C2 0.0(7)
Pd1 N1 C1 C2 178.6(3)
N1 C1 C2 C3 0.4(8)
C1 C2 C3 C4 -1.0(8)
C2 C3 C4 C5 1.2(8)
C1 N1 C5 C4 0.2(6)
Pd1 N1 C5 C4 -178.6(3)
C1 N1 C5 C6 178.9(4)
Pd1 N1 C5 C6 0.2(4)
C3 C4 C5 N1 -0.8(7)
C3 C4 C5 C6 -179.4(4)
C10 N2 C6 C7 -0.7(6)
Pd1 N2 C6 C7 179.4(3)
C10 N2 C6 C5 -179.8(3)
Pd1 N2 C6 C5 0.3(4)
N1 C5 C6 N2 -0.3(5)
C4 C5 C6 N2 178.4(4)
N1 C5 C6 C7 -179.3(4)
C4 C5 C6 C7 -0.6(7)
N2 C6 C7 C8 0.5(7)
C5 C6 C7 C8 179.5(4)
C6 C7 C8 C9 0.1(8)
C7 C8 C9 C10 -0.6(8)
C6 N2 C10 C9 0.2(6)
Pd1 N2 C10 C9 -179.8(3)
C6 N2 C10 C11 -179.1(3)
Pd1 N2 C10 C11 0.9(5)
C8 C9 C10 N2 0.4(7)
C8 C9 C10 C11 179.6(4)
C15 N3 C11 C12 0.8(6)
Pd1 N3 C11 C12 -177.7(3)
C15 N3 C11 C10 -179.8(4)
Pd1 N3 C11 C10 1.7(4)
N2 C10 C11 N3 -1.7(5)
C9 C10 C11 N3 179.1(4)
N2 C10 C11 C12 177.7(4)
C9 C10 C11 C12 -1.5(7)
N3 C11 C12 C13 -1.2(7)
C10 C11 C12 C13 179.4(4)
C11 C12 C13 C14 0.6(8)
C12 C13 C14 C15 0.3(8)
C11 N3 C15 C14 0.2(6)
Pd1 N3 C15 C14 178.4(3)
C13 C14 C15 N3 -0.7(7)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139072773
