##############################################################################
###                                                                        ###
###           Full Paper (Acta Crystallographica Section C)                ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section C. It conforms to the editorial and technical    #
# requirements of Notes for Authors for Section C, and has been peer         #
# reviewed under the auspices of the IUCr Commission on Journals.            #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
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data_global
_audit_creation_method
;
  machine and manual editing
_atom_site_refinement_flags as well as
_atom_site_symmetry_multiplicity were edited manually.
;
_journal_date_recd_electronic     2004-05-06
_journal_date_accepted     2004-07-08
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2004
_journal_volume     60
_journal_issue      9
_journal_page_first     m426
_journal_page_last     m430
_journal_paper_category     FM
_publ_contact_author_name     'Jan Fabry'
_publ_contact_author_address
;
Institute of Physics
Czech Academy of Science
Na Slovance 2
162 53 Praha 6
Czech Republic
;
_publ_contact_author_email     fabry@fzu.cz
_publ_contact_author_fax     '(420)2 8689 0527'
_publ_contact_author_phone     '(420)2 6605 2695'
_publ_section_title
;
Two phases of bis(tetraethylammonium) di-μ-chloro-bis[dichloropalladium(II)]
;
loop_
    _publ_author_name
    _publ_author_address
    "Fábry, Jan"
;
Institute of Physics
Czech Academy of Sciences
Na Slovance 2
182 21 Praha 8
Czech Republic
;
    'Dušek, Michal'
;
Institute of Physics
Czech Academy of Sciences
Na Slovance 2
182 21 Praha 8
Czech Republic
;
    "Fejfarová, Karla"
;
Institute of Physics
Czech Academy of Sciences
Na Slovance 2
182 21 Praha 8
Czech Republic
;
    "Krupková, Radmila"
;
Institute of Physics
Czech Academy of Sciences
Na Slovance 2
182 21 Praha 8
Czech Republic
;
    'Vaněk, Přemysl'
;
Institute of Physics
Czech Academy of Sciences
Na Slovance 2
182 21 Praha 8
Czech Republic
;
    'Němec, Ivan'
;
Department of Inorganic Chemistry
Faculty of Science
Charles University
Hlavova 8
128 43 Praha 2
Czech Republic
;
data_I
_audit_creation_method
;
  machine and manual editing
;
_chemical_name_systematic
;
bis(tetraethylammonium) di-μ-chloro-bis[dichloropalladium(II)]
;
_chemical_name_common
;
;
_chemical_formula_moiety     '2C8 H20 N + , Cl6 Pd2 2-'
_chemical_formula_sum     'C16 H40 Cl6 N2 Pd2'
_chemical_formula_iupac     '(C8 H20 N)2 [Pd2 Cl6]'
_chemical_formula_weight     686.04
_chemical_melting_point     ?
_symmetry_cell_setting     'orthorhombic'
_symmetry_space_group_name_H-M     'I m m m'
_symmetry_space_group_name_Hall     '-I 2 2'
loop_
    _symmetry_equiv_pos_site_id
    _symmetry_equiv_pos_as_xyz
    1 x,y,z
    2 x,y,-z
    3 -x,y,z
    4 -x,y,-z
    5 -x,-y,-z
    6 -x,-y,z
    7 x,-y,-z
    8 x,-y,z
    9 1/2+x,1/2+y,1/2+z
    10 1/2+x,1/2+y,1/2-z
    11 1/2-x,1/2+y,1/2+z
    12 1/2-x,1/2+y,1/2-z
    13 1/2-x,1/2-y,1/2-z
    14 1/2-x,1/2-y,1/2+z
    15 1/2+x,1/2-y,1/2-z
    16 1/2+x,1/2-y,1/2+z
_cell_length_a     8.7922(12)
_cell_length_b     12.3094(16)
_cell_length_c     13.2806(19)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     1437.3(3)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     30
_cell_measurement_theta_min     5.70
_cell_measurement_theta_max     14.01
_cell_measurement_temperature     292(2)
_exptl_crystal_description     'plate with a trigonal base'
_exptl_crystal_colour     red
_exptl_crystal_size_max     0.240
_exptl_crystal_size_mid     0.180
_exptl_crystal_size_min     0.120
_exptl_crystal_density_diffrn     1.585
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     688
_exptl_absorpt_coefficient_mu     1.814
_exptl_absorpt_correction_type     'Gaussian'
_exptl_absorpt_process_details     'JANA2000 (Petříček & Dušek, 2000)'
_exptl_absorpt_correction_T_min     0.6756
_exptl_absorpt_correction_T_max     0.7370
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     292(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kuma XCalibur'
_diffrn_measurement_method     ω/2θ
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     6309
_diffrn_reflns_av_R_equivalents     0.0287
_diffrn_reflns_av_sigmaI/netI     0.0099
_diffrn_reflns_theta_min     2.26
_diffrn_reflns_theta_max     27.00
_diffrn_reflns_theta_full     27.00
_diffrn_measured_fraction_theta_max     1.000
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -11
_diffrn_reflns_limit_h_max     11
_diffrn_reflns_limit_k_min     -15
_diffrn_reflns_limit_k_max     15
_diffrn_reflns_limit_l_min     -16
_diffrn_reflns_limit_l_max     16
_diffrn_standards_number     3
_diffrn_standards_interval_count     100
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     2.8
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    -2 4 2
    2 4 -2
    4 0 0
_refine_special_details
;
Refinement of F² against ALL reflections.  The H atoms were restrained and
constrained.
;
_reflns_number_total     919
_reflns_number_gt     668
_reflns_threshold_expression     I>3σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0459
_refine_ls_R_factor_gt     0.0250
_refine_ls_wR_factor_gt     0.0642
_refine_ls_wR_factor_ref     0.0728
_refine_ls_goodness_of_fit_ref     1.61
_refine_ls_restrained_S_all     ?
_refine_ls_number_reflns     919
_refine_ls_number_parameters     43
_refine_ls_number_restraints     0
_refine_ls_number_constraints     22
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     sigma
_refine_ls_weighting_details     'w = 1/[σ²(I)+0.0009I²]'
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.0015
_refine_ls_shift/su_mean     0.0003
_refine_diff_density_max     0.40
_refine_diff_density_min     -0.24
_refine_ls_extinction_method     'none'
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    C 0.003 0.002 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.4'
    H 0.000 0.000 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.4'
    Cl 0.148 0.159 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.4'
    N 0.006 0.003 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.4'
    Pd -0.999 1.007 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.4'
_computing_data_collection     'KM4B8 (Gałdecki et al., 1997)'
_computing_cell_refinement     'KM4B8'
_computing_data_reduction     'JANA2000 (Petříček & Dušek, 2000)'
_computing_structure_solution     'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement     'JANA2000'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material     'JANA2000'
loop_
    _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
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Pd 0.5 0.36236(3) 0.5 0.06391(15) Uani d . 1 . . Pd
    N 0.5 0.0 0.7478(3) 0.0687(14) Uani d . 1 . . N
    C1 0.3631(5) 0.0 0.6782(4) 0.0956(18) Uani d . 1 . . C
    C2 0.5 0.0980(3) 0.8170(3) 0.0792(13) Uani d . 1 . . C
    C3 0.2123(6) 0.0 0.7272(5) 0.134(3) Uani d . 1 . . C
    C4 0.5 0.2067(3) 0.7671(4) 0.102(2) Uani d . 1 . . C
    Cl1 0.68081(16) 0.5 0.5 0.0823(5) Uani d . 1 . . Cl
    Cl2 0.31118(14) 0.23685(9) 0.5 0.0987(4) Uani d . 1 . . Cl
    H11 0.3699 -0.0604 0.6328 0.1147 Uiso d . 1 . . H
    H12 0.5846 0.0933 0.8625 0.0951 Uiso d . 1 . . H
    H13 0.1335 0.0 0.6761 0.1607 Uiso d . 1 . . H
    H23 0.2022 -0.0643 0.7688 0.1607 Uiso d . 1 . . H
    H14 0.5 0.2632 0.8179 0.123 Uiso d . 1 . . H
    H24 0.5901 0.2137 0.7254 0.123 Uiso d . 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    _atom_site_aniso_type_symbol
    Pd 0.0761(3) 0.0616(2) 0.0540(2) 0.0 0.0 0.0 Pd
    N 0.070(3) 0.064(2) 0.072(2) 0.0 0.0 0.0 N
    C1 0.107(4) 0.083(3) 0.096(3) 0.0 -0.028(3) 0.0 C
    C2 0.078(2) 0.081(2) 0.079(2) 0.0 0.0 -0.009(2) C
    C3 0.080(3) 0.145(5) 0.176(6) 0.0 -0.042(4) 0.0 C
    C4 0.117(4) 0.073(2) 0.118(4) 0.0 0.0 -0.014(3) C
    Cl1 0.0680(8) 0.0738(8) 0.1052(10) 0.0 0.0 0.0 Cl
    Cl2 0.1043(8) 0.0755(7) 0.1165(8) -0.0215(6) 0.0 0.0 Cl
_geom_special_details
;
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Pd Cl1 . . 2.3233(9) yes
    Pd Cl1 . 5_666 2.3233(9) no
    Pd Cl2 . . 2.2679(11) yes
    Pd Cl2 . 3_655 2.2679(11) no
    N C1 . . 1.518(5) yes
    N C1 . 6_655 1.518(5) no
    N C2 . . 1.517(4) yes
    N C2 . 6_655 1.517(4) no
    C1 C3 . . 1.473(7) yes
    C2 C4 . . 1.495(6) yes
    C1 H11 . . 0.960 no
    C1 H11 . 8_555 0.960 no
    C2 H12 . . 0.960 no
    C2 H12 . 3_655 0.960 no
    C3 H13 . . 0.970 no
    C3 H23 . . 0.970 no
    C3 H23 . 8_555 0.970 no
    C4 H14 . . 0.970 no
    C4 H24 . . 0.970 no
    C4 H24 . 3_655 0.970 no
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_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    Cl1 Pd Cl1 . . 5_666 86.35(4) no
    Cl1 Pd Cl2 . . . 176.12(4) no
    Cl1 Pd Cl2 . . 3_655 89.77(4) no
    Cl1 Pd Cl1 5_666 . . 86.35(4) no
    Cl1 Pd Cl2 5_666 . . 89.77(4) no
    Cl1 Pd Cl2 5_666 . 3_655 176.12(4) no
    Cl2 Pd Cl2 . . 3_655 94.12(4) no
    Cl2 Pd Cl2 3_655 . . 94.12(4) no
    C1 N C1 . . 6_655 105.0(3) no
    C1 N C2 . . . 111.66(11) no
    C1 N C2 . . 6_655 111.66(11) no
    C1 N C1 6_655 . . 105.0(3) no
    C1 N C2 6_655 . . 111.66(11) no
    C1 N C2 6_655 . 6_655 111.66(11) no
    C2 N C2 . . 6_655 105.3(3) no
    C2 N C2 6_655 . . 105.3(3) no
    N C1 C3 . . . 116.4(4) no
    N C2 C4 . . . 116.4(3) no
    H11 C1 H11 . . 8_555 101.5 no
    H12 C2 H12 . . 3_655 101.6 no
    H13 C3 H23 . . . 109.5 no
    H13 C3 H23 . . 8_555 109.5 no
    H23 C3 H23 . . 8_555 109.5 no
    H14 C4 H24 . . . 109.5 no
    H14 C4 H24 . . 3_655 109.5 no
    H24 C4 H24 . . 3_655 109.5 no
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
    _geom_hbond_publ_flag
    C1 H11 Cl2 7_556 0.96 2.84 3.783(3) 166 yes
    C2 H12 Cl1 13_656 0.96 2.98 3.903(3) 161 yes
    C2 H12 Cl2 15_556 0.96 3.42 4.186(3) 139 yes
    C3 H23 Cl1 9_445 0.97 3.18 3.636(7) 111 yes
    C4 H24 Cl2 3_655 0.97 3.13 3.935(5) 141 yes
data_II
_chemical_name_systematic
;
bis(tetraethylammonium) di-μ-chloro-bis[dichloropalladium(II)]
;
_chemical_name_common     ?
_chemical_formula_moiety     '2C8 H20 N + , Cl6 Pd2 2-'
_chemical_formula_sum     'C16 H40 Cl6 N2 Pd2'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac     '(C8 H20 N)2 [Pd2 Cl6]'
_chemical_formula_weight     686.04
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'I 2/m'
_symmetry_space_group_name_Hall     '-I 2y'
loop_
    _symmetry_equiv_pos_site_id
    _symmetry_equiv_pos_as_xyz
    1 x,y,z
    2 -x,y,-z
    3 -x,-y,-z
    4 x,-y,z
    5 1/2+x,1/2+y,1/2+z
    6 1/2-x,1/2+y,1/2-z
    7 1/2-x,1/2-y,1/2-z
    8 1/2+x,1/2-y,1/2+z
_cell_length_a     8.7249(12)
_cell_length_b     12.238(3)
_cell_length_c     13.062(2)
_cell_angle_alpha     90
_cell_angle_beta     91.973(17)
_cell_angle_gamma     90
_cell_volume     1393.8(4)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     39
_cell_measurement_theta_min     6.81
_cell_measurement_theta_max     12.83
_cell_measurement_temperature     130
_cell_special_details
;
The choice of the unit cell is non-standard to enable easier comparison with
the parent high-temperature phase. A unit-cell for the standard setting
C 1 2/m 1 can be obtained by a following transformation:
#_diffrn_reflns_transf_matrix_11  -1
#_diffrn_reflns_transf_matrix_12   0
#_diffrn_reflns_transf_matrix_13   1
#_diffrn_reflns_transf_matrix_14   0
#_diffrn_reflns_transf_matrix_15   1
#_diffrn_reflns_transf_matrix_16   0
#_diffrn_reflns_transf_matrix_17  -1
#_diffrn_reflns_transf_matrix_18   0
#_diffrn_reflns_transf_matrix_19   0
The corresponding standard unit-cell, compatible with C 1 2/m 1, is
#_cell_length_a                           15.4562(28)
#_cell_length_b                           12.2375(28)
#_cell_length_c                           8.7249(12)
#_cell_angle_alpha                        90
#_cell_angle_beta                         122.371(17)
#_cell_angle_gamma                        90
#_cell_volume                             1393.8(5)
#_cell_formula_units_Z                    2
and the space-group type is as follows:
#_symmetry_cell_setting                   monoclinic
#_symmetry_space_group_name_H-M           'C 1 2/m 1'
#_symmetry_space_group_name_Hall          '-C 2y'
#_space_group_IT_number                   12
The corresponding atomic parameters described in C 1 2/m 1 are :
#=======================================================================
## 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
#
#loop_
# _atom_site_label
# _atom_site_type_symbol
# _atom_site_fract_x
# _atom_site_fract_y
# _atom_site_fract_z
# _atom_site_adp_type
# _atom_site_U_iso_or_equiv
# _atom_site_symmetry_multiplicity
# _atom_site_occupancy
# _atom_site_calc_flag
# _atom_site_refinement_flags
# _atom_site_disorder_assembly
# _atom_site_disorder_group
#  Pd Pd 0.5 0.36120(4) 1 Uani 0.0288(2) 4 1 d . . .
#  N N 0.2525(3) 0.0 0.7286(6) Uani 0.030(2) 4 1 d . . .
#  C1 C 0.3164(4) 0.0 0.6459(8) Uani 0.036(3) 4 1 d . . .
#  C2 C 0.1826(3) 0.0990(3) 0.6700(5) Uani 0.0318(19) 8 1 d . . .
#  C3 C 0.2594(5) 0.0 0.4407(8) Uani 0.048(4) 4 1 d . . .
#  C4 C 0.2347(3) 0.2089(3) 0.7198(6) Uani 0.042(2) 8 1 d . . .
#  C5 C 0.3285(5) 0.0 0.9308(8) Uani 0.039(3) 4 1 d . . .
#  C6 C 0.2845(5) 0.0 1.0475(9) Uani 0.054(4) 4 1 d . . .
#  Cl1 Cl 0.49074(11) 0.5 1.17223(18) Uani 0.0343(7) 4 1 d . . .
#  Cl2 Cl 0.50676(9) 0.23448(9) 0.81494(15) Uani 0.0413(6) 8 1 d . . .
#  H11 H 0.3632 -0.0605 0.6929 Uiso 0.0437 8 1 d . . .
#  H12 H 0.1388 0.0931 0.7165 Uiso 0.0382 8 1 d . . .
#  H22 H 0.1341 0.096 0.5414 Uiso 0.0382 8 1 d . . .
#  H13 H 0.3083 0.0 0.4033 Uiso 0.0573 4 1 d . . .
#  H23 H 0.2168 -0.0647 0.3937 Uiso 0.0573 8 1 d . . .
#  H14 H 0.1835 0.2661 0.6792 Uiso 0.0499 8 1 d . . .
#  H24 H 0.281 0.2133 0.8504 Uiso 0.0499 8 1 d . . .
#  H34 H 0.2731 0.218 0.6618 Uiso 0.0499 8 1 d . . .
#  H15 H 0.3743 0.0608 0.9631 Uiso 0.0467 8 1 d . . .
#  H16 H 0.3397 0.0 1.1743 Uiso 0.0643 4 1 d . . .
#  H26 H 0.2427 0.0647 1.022 Uiso 0.0643 8 1 d . . .
#
#loop_
# _atom_site_aniso_label
# _atom_site_aniso_type_symbol
# _atom_site_aniso_U_11
# _atom_site_aniso_U_22
# _atom_site_aniso_U_33
# _atom_site_aniso_U_12
# _atom_site_aniso_U_13
# _atom_site_aniso_U_23
# Pd Pd 0.0268(2) 0.0275(2) 0.0301(3) 0.0 0.01399(19) 0.0
# N N 0.031(3) 0.030(3) 0.030(3) 0.0 0.017(2) 0.0
# C1 C 0.033(3) 0.032(3) 0.053(4) 0.0 0.029(3) 0.0
# C2 C 0.031(2) 0.0321(19) 0.034(2) 0.0061(16) 0.0191(19) 0.0033(16)
# C3 C 0.066(4) 0.051(4) 0.048(4) 0.0 0.046(4) 0.0
# C4 C 0.043(3) 0.033(2) 0.048(3) 0.0040(18) 0.023(2) 0.003(2)
# C5 C 0.042(3) 0.035(3) 0.032(4) 0.0 0.014(3) 0.0
# C6 C 0.054(4) 0.064(5) 0.028(4) 0.0 0.012(4) 0.0
# Cl1 Cl 0.0441(8) 0.0337(8) 0.0339(9) 0.0 0.0267(7) 0.0
# Cl2 Cl 0.0505(7) 0.0336(6) 0.0416(8) 0.0007(4) 0.0258(6) -0.0054(4)
#
#=======================================================================
;
_exptl_crystal_description     'prism'
_exptl_crystal_colour     red
_exptl_crystal_size_max     0.25
_exptl_crystal_size_mid     0.14
_exptl_crystal_size_min     0.12
_exptl_crystal_size_rad     ?
_exptl_crystal_density_diffrn     1.6341
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     688
_exptl_absorpt_coefficient_mu     1.871
_exptl_absorpt_correction_type     'Gaussian'
_exptl_absorpt_process_details     'JANA2000 (Petříček & Dušek, 2000)'
_exptl_absorpt_correction_T_min     0.7405
_exptl_absorpt_correction_T_max     0.8202
_exptl_special_details
;
Prior to data collection, the twinning matrix was determined and it was tested
how to achieve separation of reflections stemming from the domains of both
domain states.
;
_diffrn_ambient_temperature     230.0(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kuma XCalibur'
_diffrn_measurement_method     ω/2θ
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     7138
_diffrn_reflns_av_R_equivalents     0.1129
_diffrn_reflns_av_sigmaI/netI     0.0550
_diffrn_reflns_theta_min     2.28
_diffrn_reflns_theta_max     26.99
_diffrn_reflns_theta_full     26.99
_diffrn_measured_fraction_theta_max     1.0
_diffrn_measured_fraction_theta_full     1.0
_diffrn_reflns_limit_h_min     -11
_diffrn_reflns_limit_h_max     11
_diffrn_reflns_limit_k_min     -15
_diffrn_reflns_limit_k_max     15
_diffrn_reflns_limit_l_min     -16
_diffrn_reflns_limit_l_max     16
_diffrn_reflns_reduction_process     ?
_diffrn_standards_number     3
_diffrn_standards_interval_count     100
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     1.8
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    0 0 6
    2 4 0
    4 0 0
_refine_special_details
;
The refinement of the low-temperature data was performed on a data set composed
of two merged sets of reflections corresponding to the respective domain
states. The exactly superimposed reflections of both domains are 0 k l.
The orientation matrix relating the respective domain states of the
low-temperature phase was determined experimentally and corresponds well with
an idealized twinning matrix:
$
\left(\matrix{h_{2} & k_{2} & l_{2} \cr}\right) =
\left (\matrix{h_{1} & k_{1} & l_{1} \cr} \right)
\pmatrix{
-1 & 0 & -(2c/a)\cos(β) \cr
0 & -1  & 0 \cr
0 & 0 & 1 \cr~$
The respective reflections refer to the first and second domain states.
The refinement program JANA2000 (Pet\v r\'ι\v cek & Du\v sek, 2000) accounts
for the systematic superposition of the reflections that occurs in accordance
with the twinning matrix. The refined domain-state fraction resulted in a value
of 0.5008(9). The H atoms were clearly discernible on a difference Fourier map
and they were refined as constrained.
The extinction correction turned out to be insignificant.
From the refinement of the low-temperature phase, 115 unmatched reflections
were omitted for which |Fₒ-Fc| > 3σ(Fₒ).
The Fourier synthesis was calculated with weighted intensities.
;
_reflns_number_total     2101
_reflns_number_gt     1326
_reflns_threshold_expression     I>3σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_R_factor_all     0.0850
_refine_ls_R_factor_gt     0.0289
_refine_ls_wR_factor_gt     0.0606
_refine_ls_wR_factor_ref     0.0751
_refine_ls_goodness_of_fit_ref     1.15
_refine_ls_restrained_S_all     ?
_refine_ls_number_reflns     1986
_refine_ls_number_parameters     70
_refine_ls_number_restraints     0
_refine_ls_number_constraints     42
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     sigma
_refine_ls_weighting_details     'w = 1/[σ²(I)+0.0009I²]'
_refine_ls_shift/su_max     0.0003
_refine_ls_shift/su_mean     0.0000
_refine_diff_density_max     0.43
_refine_diff_density_min     -0.40
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    C 0.003 0.002 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.1'
    H 0.000 0.000 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.1'
    Cl 0.148 0.159 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.1'
    N 0.006 0.003 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.1'
    Pd -0.999 1.007 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.1'
    O 0.011 0.006 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.1'
_computing_data_collection     'KM4B8 (Gałdecki et al., 1997)'
_computing_cell_refinement     'KM4B8'
_computing_data_reduction     'JANA2000 (Petříček & Dušek, 2000)'
_computing_structure_solution     'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement     'JANA2000'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material     'JANA2000'
loop_
    _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
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Pd 0.5 0.36120(4) 0.5 0.02878(14) Uani d . 1 . . Pd
    N 0.4761(5) 0.0 0.7475(3) 0.0302(15) Uani d . 1 . . N
    C1 0.3295(6) 0.0 0.6836(4) 0.0364(18) Uani d . 1 . . C
    C2 0.4874(4) 0.0990(3) 0.8174(3) 0.0318(12) Uani d . 1 . . C
    C3 0.1813(6) 0.0 0.7406(5) 0.048(2) Uani d . 1 . . C
    C4 0.4851(5) 0.2089(3) 0.7653(3) 0.0416(15) Uani d . 1 . . C
    C5 0.6023(6) 0.0 0.6715(5) 0.039(2) Uani d . 1 . . C
    C6 0.7630(7) 0.0 0.7155(5) 0.054(2) Uani d . 1 . . C
    Cl1 0.68149(15) 0.5 0.50926(11) 0.0343(5) Uani d . 1 . . Cl
    Cl2 0.30818(13) 0.23448(9) 0.49324(9) 0.0413(4) Uani d . 1 . . Cl
    H11 0.3297 -0.0605 0.6368 0.0437 Uiso d . 1 . . H
    H12 0.5777 0.0931 0.8612 0.0382 Uiso d . 1 . . H
    H22 0.4073 0.096 0.8659 0.0382 Uiso d . 1 . . H
    H15 0.5887 0.0608 0.6257 0.0467 Uiso d . 1 . . H
    H13 0.095 0.0 0.6917 0.0573 Uiso d . 1 . . H
    H23 0.1769 -0.0647 0.7832 0.0573 Uiso d . 1 . . H
    H16 0.8346 0.0 0.6603 0.0643 Uiso d . 1 . . H
    H26 0.7793 0.0647 0.7573 0.0643 Uiso d . 1 . . H
    H14 0.4956 0.2661 0.8165 0.0499 Uiso d . 1 . . H
    H24 0.5694 0.2133 0.719 0.0499 Uiso d . 1 . . H
    H34 0.3888 0.218 0.7269 0.0499 Uiso d . 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    _atom_site_aniso_type_symbol
    Pd 0.0320(3) 0.0275(2) 0.0268(2) 0.0 0.00138(17) 0.0 Pd
    N 0.029(3) 0.030(3) 0.031(3) 0.0 0.0006(19) 0.0 N
    C1 0.043(3) 0.032(3) 0.033(3) 0.0 -0.012(3) 0.0 C
    C2 0.032(2) 0.0321(19) 0.031(2) -0.0002(16) -0.0018(17) -0.0061(16) C
    C3 0.025(3) 0.051(4) 0.066(4) 0.0 -0.010(3) 0.0 C
    C4 0.049(3) 0.033(2) 0.043(3) 0.001(2) 0.001(2) -0.0040(18) C
    C5 0.041(4) 0.035(3) 0.042(3) 0.0 0.011(3) 0.0 C
    C6 0.045(4) 0.064(5) 0.054(4) 0.0 0.022(3) 0.0 C
    Cl1 0.0249(8) 0.0337(8) 0.0441(8) 0.0 -0.0021(7) 0.0 Cl
    Cl2 0.0399(7) 0.0336(6) 0.0505(7) -0.0069(4) 0.0032(6) -0.0007(4) Cl
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Pd Cl1 . . 2.3225(9) yes
    Pd Cl1 . 3_666 2.3225(9) no
    Pd Cl2 . . 2.2811(11) yes
    Pd Cl2 . 2_656 2.2811(11) no
    N C1 . . 1.504(7) yes
    N C2 . . 1.518(4) yes
    N C2 . 4_555 1.518(4) no
    N C5 . . 1.508(7) yes
    C1 C3 . . 1.514(8) yes
    C2 C4 . . 1.507(5) yes
    C5 C6 . . 1.497(8) yes
    C1 H11 . . 0.960 no
    C1 H11 . 4_555 0.960 no
    C2 H12 . . 0.960 no
    C2 H22 . . 0.960 no
    C3 H13 . . 0.970 no
    C3 H23 . . 0.970 no
    C3 H23 . 4_555 0.970 no
    C4 H14 . . 0.970 no
    C4 H24 . . 0.970 no
    C4 H34 . . 0.970 no
    C5 H15 . . 0.960 no
    C5 H15 . 4_555 0.960 no
    C6 H16 . . 0.970 no
    C6 H26 . . 0.970 no
    C6 H26 . 4_555 0.970 no
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_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    Cl1 Pd Cl1 . . 3_666 86.00(4) no
    Cl1 Pd Cl2 . . . 175.72(4) no
    Cl1 Pd Cl2 . . 2_656 89.84(4) no
    Cl1 Pd Cl1 3_666 . . 86.00(4) no
    Cl1 Pd Cl2 3_666 . . 89.84(4) no
    Cl1 Pd Cl2 3_666 . 2_656 175.72(4) no
    Cl2 Pd Cl2 . . 2_656 94.34(4) no
    Cl2 Pd Cl2 2_656 . . 94.34(4) no
    C1 N C2 . . . 111.7(3) no
    C1 N C2 . . 4_555 111.7(3) no
    C1 N C5 . . . 105.1(4) no
    C2 N C2 . . 4_555 105.9(3) no
    C2 N C5 . . . 111.3(3) no
    C2 N C2 4_555 . . 105.9(3) no
    C2 N C5 4_555 . . 111.3(3) no
    N C1 C3 . . . 116.8(5) no
    N C2 C4 . . . 116.2(3) no
    N C5 C6 . . . 116.2(5) no
    H11 C1 H11 . . 4_555 100.9 no
    H11 C1 H11 4_555 . . 100.9 no
    H12 C2 H22 . . . 101.8 no
    H13 C3 H23 . . . 109.5 no
    H13 C3 H23 . . 4_555 109.5 no
    H23 C3 H23 . . 4_555 109.5 no
    H23 C3 H23 4_555 . . 109.5 no
    H14 C4 H24 . . . 109.5 no
    H14 C4 H34 . . . 109.5 no
    H24 C4 H34 . . . 109.5 no
    H15 C5 H15 . . 4_555 101.7 no
    H15 C5 H15 4_555 . . 101.7 no
    H16 C6 H26 . . . 109.5 no
    H16 C6 H26 . . 4_555 109.5 no
    H26 C6 H26 . . 4_555 109.5 no
    H26 C6 H26 4_555 . . 109.5 no
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
    _geom_hbond_publ_flag
    C1 H11 Cl2 4_555 0.96 2.84 3.797(4) 176 yes
    C2 H12 Cl1 7_656 0.96 2.89 3.806(4) 161 yes
    C2 H12 Cl2 8_555 0.96 3.35 4.101(4) 137 yes
    C2 H22 Cl1 5_445 0.96 3.00 3.915(4) 159 yes
    C2 H22 Cl2 7_556 0.96 3.39 4.167(4) 140 yes
    C3 H23 Cl1 5_445 0.97 3.06 3.510(7) 110 yes
    C4 H24 Cl2 2_656 0.97 3.02 3.895(4) 152 yes
    C4 H34 Cl2 1_555 0.97 3.12 3.838(4) 133 yes
    C5 H15 Cl2 2_656 0.96 2.80 3.686(4) 154 yes
    C6 H26 Cl1 7_656 0.97 3.16 3.612(7) 110 yes
