#------------------------------------------------------------------------------
#$Date: 2018-05-31 19:12:25 +0300 (Thu, 31 May 2018) $
#$Revision: 208078 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/94/1549494.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_1549494
loop_
_publ_author_name
'Oberley, Alan J.'
'Kadel, Lava R.'
'Senaratne, Nilmini K.'
'Eichhorn, David M.'
_publ_section_title
;
 Tetraethylammonium (acetonitrile)trichloridopalladate(II)
;
_journal_coeditor_code           BT4069
_journal_issue                   5
_journal_name_full               IUCrData
_journal_page_first              x180750
_journal_paper_doi               10.1107/S2414314618007502
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac          '(C8 H20 N) [Pd Cl3 (C2 H3 N)]'
_chemical_formula_moiety         'C8 H20 N +, C2 H3 Cl3 N Pd -'
_chemical_formula_sum            'C10 H23 Cl3 N2 Pd'
_chemical_formula_weight         384.05
_chemical_name_systematic
;
Tetraethylammonium (acetonitrile)trichloridopalladate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.769(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.286(2)
_cell_length_b                   17.379(5)
_cell_length_c                   12.950(3)
_cell_measurement_reflns_used    8735
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.220
_cell_measurement_theta_min      3.186
_cell_volume                     1599.2(7)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR2004 (Burla et al.,  2007)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            54175
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.147
_diffrn_reflns_theta_min         3.704
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.641
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5892
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       irregular
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.628
_exptl_crystal_size_mid          0.569
_exptl_crystal_size_min          0.312
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.613
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         3516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0519P)²+0.4406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                2804
_reflns_number_total             3516
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            bt4069sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1599.3(8)
_cod_database_code               1549494
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           .2013
loop_
_space_group_symop_operation_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_occupancy
Pd Pd1 0.25580(3) 0.43656(2) 0.67953(2) 0.03879(10) Uani d 1
Cl Cl1 0.32497(12) 0.30742(5) 0.70147(6) 0.0518(2) Uani d 1
Cl Cl2 0.19617(13) 0.44208(4) 0.84354(7) 0.0518(2) Uani d 1
Cl Cl3 0.19872(15) 0.56612(5) 0.65811(9) 0.0645(3) Uani d 1
N N1 0.2950(4) 0.43234(17) 0.5297(2) 0.0567(8) Uani d 1
C C1 0.2887(7) 0.4325(3) 0.3309(3) 0.0967(19) Uani d 1
H H1A 0.1600 0.4424 0.2911 0.145 Uiso calc 1
H H1B 0.3308 0.3824 0.3100 0.145 Uiso calc 1
H H1C 0.3725 0.4729 0.3154 0.145 Uiso calc 1
C C2 0.2927(5) 0.4320(2) 0.4438(3) 0.0649(10) Uani d 1
N N2 0.2491(3) 0.80441(13) 0.48732(17) 0.0363(5) Uani d 1
C C3 0.5222(5) 0.8575(2) 0.4139(3) 0.0559(8) Uani d 1
H H3A 0.4597 0.8401 0.3428 0.084 Uiso calc 1
H H3B 0.6589 0.8538 0.4223 0.084 Uiso calc 1
H H3C 0.4874 0.9110 0.4235 0.084 Uiso calc 1
C C4 0.4611(4) 0.80727(18) 0.4959(2) 0.0450(7) Uani d 1
H H4A 0.5222 0.8264 0.5672 0.054 Uiso calc 1
H H4B 0.5069 0.7543 0.4894 0.054 Uiso calc 1
C C5 0.0118(4) 0.74911(19) 0.5853(3) 0.0529(8) Uani d 1
H H5A -0.0551 0.7241 0.5200 0.079 Uiso calc 1
H H5B -0.0451 0.7994 0.5920 0.079 Uiso calc 1
H H5C 0.0030 0.7170 0.6462 0.079 Uiso calc 1
C C6 0.2159(4) 0.75965(17) 0.5818(2) 0.0441(7) Uani d 1
H H6A 0.2744 0.7082 0.5818 0.053 Uiso calc 1
H H6B 0.2806 0.7865 0.6472 0.053 Uiso calc 1
C C7 0.2554(5) 0.93366(18) 0.5807(3) 0.0600(9) Uani d 1
H H7A 0.1960 0.9846 0.5739 0.090 Uiso calc 1
H H7B 0.3905 0.9393 0.5844 0.090 Uiso calc 1
H H7C 0.2362 0.9087 0.6454 0.090 Uiso calc 1
C C8 0.1677(4) 0.88483(17) 0.4855(3) 0.0499(8) Uani d 1
H H8A 0.0308 0.8807 0.4815 0.060 Uiso calc 1
H H8B 0.1846 0.9114 0.4206 0.060 Uiso calc 1
C C9 0.1992(5) 0.6812(2) 0.3746(3) 0.0612(9) Uani d 1
H H9A 0.1275 0.6610 0.3070 0.092 Uiso calc 1
H H9B 0.1670 0.6521 0.4330 0.092 Uiso calc 1
H H9C 0.3341 0.6760 0.3774 0.092 Uiso calc 1
C C10 0.1512(5) 0.7654(2) 0.3845(2) 0.0532(8) Uani d 1
H H10A 0.0135 0.7698 0.3775 0.064 Uiso calc 1
H H10B 0.1834 0.7938 0.3247 0.064 Uiso calc 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
Cl2 Pd1 Cl1 90.44(3) y
Cl2 Pd1 Cl3 90.26(3) y
N1 Pd1 Cl1 90.55(9) y
N1 Pd1 Cl3 88.84(9) y
Cl3 Pd1 Cl1 177.84(3) y
N1 Pd1 Cl2 177.08(8) y
C2 N1 Pd1 171.1(3) y
H1A C1 H1B 109.5 ?
H1A C1 H1C 109.5 ?
H1B C1 H1C 109.5 ?
C2 C1 H1A 109.5 ?
C2 C1 H1B 109.5 ?
C2 C1 H1C 109.5 ?
N1 C2 C1 179.3(5) ?
C6 N2 C4 107.4(2) ?
C6 N2 C8 110.8(2) ?
C6 N2 C10 110.5(2) ?
C8 N2 C4 111.0(2) ?
C8 N2 C10 106.9(2) ?
C10 N2 C4 110.5(2) ?
H3A C3 H3B 109.5 ?
H3A C3 H3C 109.5 ?
H3B C3 H3C 109.5 ?
C4 C3 H3A 109.5 ?
C4 C3 H3B 109.5 ?
C4 C3 H3C 109.5 ?
N2 C4 H4A 108.6 ?
N2 C4 H4B 108.6 ?
C3 C4 N2 114.7(2) ?
C3 C4 H4A 108.6 ?
C3 C4 H4B 108.6 ?
H4A C4 H4B 107.6 ?
H5A C5 H5B 109.5 ?
H5A C5 H5C 109.5 ?
H5B C5 H5C 109.5 ?
C6 C5 H5A 109.5 ?
C6 C5 H5B 109.5 ?
C6 C5 H5C 109.5 ?
N2 C6 H6A 108.5 ?
N2 C6 H6B 108.5 ?
C5 C6 N2 114.9(2) ?
C5 C6 H6A 108.5 ?
C5 C6 H6B 108.5 ?
H6A C6 H6B 107.5 ?
H7A C7 H7B 109.5 ?
H7A C7 H7C 109.5 ?
H7B C7 H7C 109.5 ?
C8 C7 H7A 109.5 ?
C8 C7 H7B 109.5 ?
C8 C7 H7C 109.5 ?
N2 C8 C7 114.2(3) ?
N2 C8 H8A 108.7 ?
N2 C8 H8B 108.7 ?
C7 C8 H8A 108.7 ?
C7 C8 H8B 108.7 ?
H8A C8 H8B 107.6 ?
H9A C9 H9B 109.5 ?
H9A C9 H9C 109.5 ?
H9B C9 H9C 109.5 ?
C10 C9 H9A 109.5 ?
C10 C9 H9B 109.5 ?
C10 C9 H9C 109.5 ?
N2 C10 H10A 108.4 ?
N2 C10 H10B 108.4 ?
C9 C10 N2 115.6(3) ?
C9 C10 H10A 108.4 ?
C9 C10 H10B 108.4 ?
H10A C10 H10B 107.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 Cl1 2.3040(11) y
Pd1 Cl2 2.2621(10) y
Pd1 Cl3 2.2953(11) y
Pd1 N1 2.024(3) y
N1 C2 1.108(5) y
C1 H1A 0.9800 ?
C1 H1B 0.9800 ?
C1 H1C 0.9800 ?
C1 C2 1.457(5) ?
N2 C4 1.524(4) ?
N2 C6 1.514(3) ?
N2 C8 1.516(4) ?
N2 C10 1.524(4) ?
C3 H3A 0.9800 ?
C3 H3B 0.9800 ?
C3 H3C 0.9800 ?
C3 C4 1.515(4) ?
C4 H4A 0.9900 ?
C4 H4B 0.9900 ?
C5 H5A 0.9800 ?
C5 H5B 0.9800 ?
C5 H5C 0.9800 ?
C5 C6 1.509(4) ?
C6 H6A 0.9900 ?
C6 H6B 0.9900 ?
C7 H7A 0.9800 ?
C7 H7B 0.9800 ?
C7 H7C 0.9800 ?
C7 C8 1.517(5) ?
C8 H8A 0.9900 ?
C8 H8B 0.9900 ?
C9 H9A 0.9800 ?
C9 H9B 0.9800 ?
C9 H9C 0.9800 ?
C9 C10 1.517(5) ?
C10 H10A 0.9900 ?
C10 H10B 0.9900 ?
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
C4 N2 C6 C5 -178.5(3)
C4 N2 C8 C7 -57.2(3)
C4 N2 C10 C9 64.6(3)
C6 N2 C4 C3 -173.7(3)
C6 N2 C8 C7 61.9(3)
C6 N2 C10 C9 -54.0(3)
C8 N2 C4 C3 -52.5(3)
C8 N2 C6 C5 60.2(3)
C8 N2 C10 C9 -174.6(3)
C10 N2 C4 C3 65.8(3)
C10 N2 C6 C5 -58.0(3)
C10 N2 C8 C7 -177.7(3)

_cod_database_fobs_code 1549494
