#------------------------------------------------------------------------------
#$Date: 2019-12-26 22:14:25 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246160 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/19/2311900.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_2311900
loop_
_publ_author_name
'Jandl, C.'
'Stegbauer, S.'
'Pöthig, A'
_publ_section_title
;
 A halide-free pyridinium-substituted η³-cycloheptatrienide-Pd
 complex.
;
_journal_coeditor_code           EG3226
_journal_issue                   'Pt 9'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              754
_journal_page_last               759
_journal_paper_doi               10.1107/S2053229617012244
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Pd2 Br2 (C14 H16 N2)2] (B F4)2, 2C2 H3 N'
_chemical_formula_moiety
'C28 H32 Br2 N4 Pd2 2+, 2(B F4 -), 2(C2 H3 N)'
_chemical_formula_sum            'C32 H38 B2 Br2 F8 N6 Pd2'
_chemical_formula_weight         1052.90
_chemical_name_systematic
'Di-μ-bromido-bis({η³-[4-(dimethylamino)pyridinium-1-yl]cycloheptatrienido}palladium(II)) bis(tetrafluoroborate) acetonitrile disolvate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                116.3393(12)
_cell_angle_beta                 99.6342(14)
_cell_angle_gamma                98.3722(13)
_cell_formula_units_Z            1
_cell_length_a                   7.8161(2)
_cell_length_b                   11.3126(3)
_cell_length_c                   12.2248(3)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.3839
_cell_measurement_theta_min      2.7291
_cell_volume                     925.00(4)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae et al.,  2006)
;
_computing_publication_material
;
PLATON (Spek, 2009), enCIFer (Allen et al.,  2004) and
publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and
shelXle (Hübschle et al.,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'MONTEL optic'
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28005
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    3.206
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            'intense red'
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.814
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4416
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[Σ²(FO²)+(0.0292P)²+1.1587P] WHERE P=(FO²+2FC²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                4080
_reflns_number_total             4416
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            eg3226sup1.cif
_cod_data_source_block           compound_2
_cod_database_code               2311900
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
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_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd1 0.30067(2) 0.42089(2) 0.36673(2) 0.01910(10) Uani d . 1.000 . .
Br Br1 0.36109(3) 0.49481(2) 0.60127(2) 0.02190(10) Uani d . 1.000 . .
N N1 -0.1818(3) 0.19750(19) 0.34633(19) 0.0215(5) Uani d . 1.000 . .
F F1 0.0333(8) 0.3623(4) 0.7921(6) 0.1043(18) Uani d DUP 0.598(4) A 1
F F2 0.0730(5) 0.1444(4) 0.7054(3) 0.0616(11) Uani d DUP 0.598(4) A 1
N N2 -0.5447(3) 0.1651(2) 0.5480(2) 0.0293(6) Uani d . 1.000 . .
F F3 0.2297(5) 0.3099(4) 0.9049(4) 0.0473(11) Uani d DUP 0.598(4) A 1
F F4 -0.0695(6) 0.2183(5) 0.8542(5) 0.0874(16) Uani d DUP 0.598(4) A 1
C C1 0.0932(3) 0.3768(3) 0.2137(2) 0.0271(7) Uani d . 1.000 . .
C C2 0.2216(3) 0.3115(3) 0.1596(2) 0.0314(7) Uani d . 1.000 . .
C C3 0.2317(3) 0.1732(3) 0.1243(2) 0.0346(8) Uani d . 1.000 . .
C C4 0.1253(3) 0.0773(3) 0.1368(2) 0.0331(7) Uani d . 1.000 . .
C C5 -0.0102(3) 0.0908(3) 0.2036(2) 0.0279(7) Uani d . 1.000 . .
C C6 -0.0516(3) 0.2081(2) 0.2770(2) 0.0223(6) Uani d . 1.000 . .
C C7 0.0114(3) 0.3442(2) 0.2959(2) 0.0231(6) Uani d . 1.000 . .
C C8 -0.1313(3) 0.2607(2) 0.4752(2) 0.0237(6) Uani d . 1.000 . .
C C9 -0.2469(3) 0.2515(2) 0.5435(2) 0.0247(7) Uani d . 1.000 . .
C C10 -0.4280(3) 0.1748(2) 0.4822(2) 0.0247(7) Uani d . 1.000 . .
C C11 -0.4756(3) 0.1086(2) 0.3475(2) 0.0270(7) Uani d . 1.000 . .
C C12 -0.3535(3) 0.1220(2) 0.2845(2) 0.0265(7) Uani d . 1.000 . .
C C13 -0.4925(4) 0.2370(3) 0.6865(3) 0.0335(8) Uani d . 1.000 . .
C C14 -0.7336(3) 0.0959(3) 0.4839(3) 0.0387(9) Uani d . 1.000 . .
F F1A 0.0162(9) 0.3804(6) 0.9288(6) 0.0832(17) Uani d DUP 0.402(4) A 2
F F2A 0.1006(6) 0.3335(5) 0.7472(4) 0.0322(12) Uani d DUP 0.402(4) A 2
F F3A 0.2110(7) 0.2531(7) 0.8787(7) 0.0484(18) Uani d DUP 0.402(4) A 2
F F4A -0.0811(7) 0.1740(5) 0.7718(7) 0.0658(17) Uani d DUP 0.402(4) A 2
B B1 0.0688(6) 0.2585(7) 0.8148(5) 0.0438(12) Uani d DUP 0.598(4) A 1
B B1A 0.0624(8) 0.2830(7) 0.8285(7) 0.0437(14) Uani d DUP 0.402(4) A 2
N N3 0.6250(4) 0.1381(3) -0.0006(3) 0.0444(9) Uani d . 1.000 . .
C C15 0.6394(3) 0.2440(3) 0.0099(2) 0.0295(7) Uani d . 1.000 . .
C C16 0.6568(4) 0.3804(3) 0.0246(3) 0.0402(9) Uani d . 1.000 . .
H H1 0.06570 0.45300 0.19900 0.0320 Uiso c RU 1.000 . .
H H2 0.28820 0.35510 0.11850 0.0380 Uiso c RU 1.000 . .
H H3 0.32650 0.14620 0.08730 0.0410 Uiso c RU 1.000 . .
H H4 0.14300 -0.01180 0.09520 0.0400 Uiso c RU 1.000 . .
H H5 -0.07820 0.00940 0.19580 0.0340 Uiso c RU 1.000 . .
H H7 -0.05690 0.41000 0.34200 0.0280 Uiso c RU 1.000 . .
H H8 -0.01130 0.31290 0.51820 0.0280 Uiso c RU 1.000 . .
H H9 -0.20700 0.29660 0.63320 0.0300 Uiso c RU 1.000 . .
H H11 -0.59400 0.05470 0.30150 0.0320 Uiso c RU 1.000 . .
H H12 -0.38850 0.07750 0.19470 0.0320 Uiso c RU 1.000 . .
H H13A -0.59080 0.21050 0.71780 0.0500 Uiso c RU 1.000 . .
H H13B -0.46600 0.33550 0.71720 0.0500 Uiso c RU 1.000 . .
H H13C -0.38580 0.21310 0.71720 0.0500 Uiso c RU 1.000 . .
H H14A -0.78490 0.14270 0.44060 0.0580 Uiso c RU 1.000 . .
H H14B -0.79860 0.09720 0.54620 0.0580 Uiso c RU 1.000 . .
H H14C -0.74370 0.00130 0.42180 0.0580 Uiso c RU 1.000 . .
H H16A 0.75500 0.40160 -0.00930 0.0600 Uiso c RU 1.000 . .
H H16B 0.68230 0.44650 0.11440 0.0600 Uiso c RU 1.000 . .
H H16C 0.54480 0.38490 -0.02160 0.0600 Uiso c RU 1.000 . .
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'
B B 0.0013 0.0007 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 ' 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'
N N 0.0061 0.0033 ' 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br1 Pd1 C1 . . 140.47(7) no
Br1 Pd1 C2 . . 166.85(9) no
Br1 Pd1 C7 . . 104.30(6) no
Br1 Pd1 Br1 . 2_666 88.930(9) yes
C1 Pd1 C2 . . 38.57(9) no
C1 Pd1 C7 . . 39.12(10) no
Br1 Pd1 C1 2_666 . 127.67(8) no
C2 Pd1 C7 . . 69.33(9) no
Br1 Pd1 C2 2_666 . 98.10(7) no
Br1 Pd1 C7 2_666 . 166.63(6) no
Pd1 Br1 Pd1 . 2_666 91.070(9) yes
C6 N1 C8 . . 119.9(2) no
C6 N1 C12 . . 121.02(19) no
C8 N1 C12 . . 119.1(2) no
C10 N2 C13 . . 121.1(2) no
C10 N2 C14 . . 120.6(2) no
C13 N2 C14 . . 117.9(2) no
Pd1 C1 C2 . . 75.20(14) no
Pd1 C1 C7 . . 74.21(14) no
C2 C1 C7 . . 122.0(3) yes
Pd1 C2 C1 . . 66.23(12) no
Pd1 C2 C3 . . 105.53(17) no
C1 C2 C3 . . 127.4(3) no
C2 C3 C4 . . 128.9(2) no
C3 C4 C5 . . 129.1(3) no
C4 C5 C6 . . 126.5(3) no
N1 C6 C5 . . 116.2(2) no
N1 C6 C7 . . 113.9(2) no
C5 C6 C7 . . 129.9(2) no
Pd1 C7 C1 . . 66.67(13) no
Pd1 C7 C6 . . 113.26(16) no
C1 C7 C6 . . 125.2(2) no
N1 C8 C9 . . 122.0(2) no
C8 C9 C10 . . 120.6(2) no
N2 C10 C9 . . 121.5(2) no
N2 C10 C11 . . 122.5(2) no
C9 C10 C11 . . 116.0(2) no
C10 C11 C12 . . 120.6(2) no
N1 C12 C11 . . 121.8(2) no
Pd1 C1 H1 . . 119.00 no
C2 C1 H1 . . 119.00 no
C7 C1 H1 . . 119.00 no
Pd1 C2 H2 . . 115.00 no
C1 C2 H2 . . 115.00 no
C3 C2 H2 . . 115.00 no
C2 C3 H3 . . 115.00 no
C4 C3 H3 . . 116.00 no
C3 C4 H4 . . 115.00 no
C5 C4 H4 . . 115.00 no
C4 C5 H5 . . 117.00 no
C6 C5 H5 . . 117.00 no
Pd1 C7 H7 . . 114.00 no
C1 C7 H7 . . 114.00 no
C6 C7 H7 . . 114.00 no
N1 C8 H8 . . 119.00 no
C9 C8 H8 . . 119.00 no
C8 C9 H9 . . 120.00 no
C10 C9 H9 . . 120.00 no
C10 C11 H11 . . 120.00 no
C12 C11 H11 . . 120.00 no
N1 C12 H12 . . 119.00 no
C11 C12 H12 . . 119.00 no
N2 C13 H13A . . 109.00 no
N2 C13 H13B . . 109.00 no
N2 C13 H13C . . 109.00 no
H13A C13 H13B . . 109.00 no
H13A C13 H13C . . 109.00 no
H13B C13 H13C . . 110.00 no
N2 C14 H14A . . 109.00 no
N2 C14 H14B . . 109.00 no
N2 C14 H14C . . 109.00 no
H14A C14 H14B . . 110.00 no
H14A C14 H14C . . 109.00 no
H14B C14 H14C . . 109.00 no
F1 B1 F2 . . 112.5(5) no
F1 B1 F3 . . 107.1(6) no
F1 B1 F4 . . 106.7(5) no
F2 B1 F3 . . 111.3(5) no
F2 B1 F4 . . 106.4(6) no
F3 B1 F4 . . 112.9(5) no
F1A B1A F2A . . 110.0(7) no
F1A B1A F3A . . 107.1(6) no
F1A B1A F4A . . 105.2(6) no
F2A B1A F3A . . 110.7(6) no
F2A B1A F4A . . 112.4(6) no
F3A B1A F4A . . 111.2(7) no
N3 C15 C16 . . 179.3(3) no
C15 C16 H16A . . 109.00 no
C15 C16 H16B . . 110.00 no
C15 C16 H16C . . 109.00 no
H16A C16 H16B . . 109.00 no
H16A C16 H16C . . 109.00 no
H16B C16 H16C . . 109.00 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 Br1 . 2.5392(3) yes
Pd1 C1 . 2.074(2) yes
Pd1 C2 . 2.190(2) yes
Pd1 C7 . 2.173(2) yes
Pd1 Br1 2_666 2.5769(3) yes
N1 C6 . 1.453(3) no
N1 C8 . 1.364(3) no
N1 C12 . 1.362(3) no
F1 B1 . 1.375(10) no
N2 C13 . 1.465(4) no
N2 C14 . 1.462(4) no
F2 B1 . 1.397(7) no
N2 C10 . 1.336(3) no
F3 B1 . 1.374(7) no
F4 B1 . 1.354(8) no
C1 C7 . 1.425(4) yes
C1 C2 . 1.412(4) yes
C2 C3 . 1.445(5) no
C3 C4 . 1.349(5) no
C4 C5 . 1.428(3) no
C5 C6 . 1.355(4) no
C6 C7 . 1.446(4) no
C8 C9 . 1.352(3) no
C9 C10 . 1.424(3) no
C10 C11 . 1.425(3) no
C11 C12 . 1.354(3) no
C1 H1 . 1.0000 no
F1A B1A . 1.383(10) no
C2 H2 . 1.0000 no
F2A B1A . 1.399(10) no
C3 H3 . 0.9500 no
F3A B1A . 1.378(10) no
C4 H4 . 0.9500 no
F4A B1A . 1.356(10) no
C5 H5 . 0.9500 no
C7 H7 . 1.0000 no
C8 H8 . 0.9500 no
C9 H9 . 0.9500 no
C11 H11 . 0.9500 no
C12 H12 . 0.9500 no
C13 H13B . 0.9800 no
C13 H13C . 0.9800 no
C13 H13A . 0.9800 no
C14 H14B . 0.9800 no
C14 H14C . 0.9800 no
C14 H14A . 0.9800 no
N3 C15 . 1.133(5) no
C15 C16 . 1.455(5) no
C16 H16A . 0.9800 no
C16 H16B . 0.9800 no
C16 H16C . 0.9800 no
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_site_symmetry_1
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 Pd1 Br1 Pd1 . . 2_666 -159.65(15) no
C7 Pd1 Br1 Pd1 . . 2_666 -178.04(7) no
Br1 Pd1 Br1 Pd1 2_666 . 2_666 0.00(3) no
Br1 Pd1 C1 C2 . . . -159.12(15) no
Br1 Pd1 C1 C7 . . . -29.0(2) no
C2 Pd1 C1 C7 . . . 130.2(3) no
C7 Pd1 C1 C2 . . . -130.2(3) no
Br1 Pd1 C1 C2 2_666 . . 46.9(2) no
Br1 Pd1 C1 C7 2_666 . . 177.08(11) no
C1 Pd1 C2 C3 . . . -124.4(3) no
C7 Pd1 C2 C1 . . . 31.03(19) no
C7 Pd1 C2 C3 . . . -93.41(18) no
Br1 Pd1 C2 C1 2_666 . . -144.26(18) no
Br1 Pd1 C2 C3 2_666 . . 91.30(16) no
Br1 Pd1 C7 C1 . . . 161.45(15) no
Br1 Pd1 C7 C6 . . . -78.71(15) no
C1 Pd1 C7 C6 . . . 119.9(2) no
C2 Pd1 C7 C1 . . . -30.62(18) no
C2 Pd1 C7 C6 . . . 89.23(18) no
Br1 Pd1 Br1 Pd1 . 2_666 2_666 0.00(3) no
C1 Pd1 Br1 Pd1 . 2_666 2_666 163.76(11) no
C2 Pd1 Br1 Pd1 . 2_666 2_666 -168.85(9) no
C12 N1 C6 C7 . . . 115.3(3) no
C6 N1 C12 C11 . . . 178.6(2) no
C8 N1 C12 C11 . . . 0.4(4) no
C12 N1 C8 C9 . . . -0.5(4) no
C8 N1 C6 C7 . . . -66.5(3) no
C6 N1 C8 C9 . . . -178.7(2) no
C8 N1 C6 C5 . . . 114.7(3) yes
C12 N1 C6 C5 . . . -63.5(3) no
C14 N2 C10 C11 . . . -6.1(4) no
C13 N2 C10 C9 . . . 2.1(4) no
C14 N2 C10 C9 . . . 174.6(3) no
C13 N2 C10 C11 . . . -178.6(3) no
C7 C1 C2 C3 . . . 31.7(4) no
Pd1 C1 C7 C6 . . . -102.8(2) no
Pd1 C1 C2 C3 . . . 91.8(2) no
C2 C1 C7 C6 . . . -42.2(4) no
C2 C1 C7 Pd1 . . . 60.7(2) no
C7 C1 C2 Pd1 . . . -60.2(2) no
Pd1 C2 C3 C4 . . . 70.3(3) no
C1 C2 C3 C4 . . . -1.4(4) no
C2 C3 C4 C5 . . . -9.7(4) no
C3 C4 C5 C6 . . . -5.0(4) no
C4 C5 C6 C7 . . . 7.9(4) no
C4 C5 C6 N1 . . . -173.5(2) no
C5 C6 C7 C1 . . . 18.8(4) no
N1 C6 C7 Pd1 . . . 123.18(18) no
N1 C6 C7 C1 . . . -159.8(2) no
C5 C6 C7 Pd1 . . . -58.2(3) no
N1 C8 C9 C10 . . . -0.2(4) no
C8 C9 C10 N2 . . . -179.6(2) no
C8 C9 C10 C11 . . . 1.1(4) no
N2 C10 C11 C12 . . . 179.5(3) no
C9 C10 C11 C12 . . . -1.2(4) no
C10 C11 C12 N1 . . . 0.5(4) no
