#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/87/2018704.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_2018704
loop_
_publ_author_name
'Vranec, Peter'
'Potočňák, Ivan'
'Repovský, Peter'
_publ_section_title
;
 Low-dimensional compounds containing bioactive ligands. IV. Unusual ionic
 forms of 5-chloroquinolin-8-ol
;
_journal_coeditor_code           FG3281
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m370
_journal_page_last               m376
_journal_paper_doi               10.1107/S0108270112047452
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C2 H8 N) [Pd Cl3]'
_chemical_formula_moiety         'C2 H8 N +, Pd Cl3 -'
_chemical_formula_sum            'C2 H8 Cl3 N Pd'
_chemical_formula_weight         258.84
_chemical_name_systematic
;
catena-Poly[dimethylammonium [[dichloridopalladate(II)]-μ-chlorido]]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.359(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7896(7)
_cell_length_b                   13.2070(11)
_cell_length_c                   7.1410(6)
_cell_measurement_reflns_used    545
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8506
_cell_measurement_theta_min      3.0786
_cell_volume                     734.44(11)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3438
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur (Sapphire2, large Be window)'
_diffrn_measurement_method       'ω 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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1387
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    3.508
_exptl_absorpt_correction_T_max  0.603
_exptl_absorpt_correction_T_min  0.214
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Oxford Diffraction, 2007), based on expressions derived
by
Clark & Reid (1995)]
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.9712
_exptl_crystal_size_mid          0.1924
_exptl_crystal_size_min          0.1834
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.678
_refine_ls_extinction_coef       0.0188(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0272
_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)+(0.0291P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                629
_reflns_number_total             762
_reflns_threshold_expression     I>2sigma(I)
_iucr_refine_instructions_details
;
TITL II
CELL  0.71073   7.7896  13.2070   7.1410   90.000   91.359   90.000
ZERR     4.00   0.0007   0.0011   0.0006    0.000    0.007    0.000
LATT   7
SYMM  - X,   Y, 1/2 - Z
SFAC  C    H    N    CL   PD
UNIT  8    32   4    12   4
MERG   2
OMIT    -2.00  53.00
FMAP   2
PLAN   10
ACTA
BOND   $H
EQIV $1 x, -y+1, z-1/2
HTAB N1 Cl2
HTAB N1 Cl2_$1
L.S.  15
WGHT    0.029100
EXTI    0.018796
FVAR       5.22269
PD1   5    0.500000    0.500000    0.500000    10.50000    0.02412    0.02538 =
         0.01850    0.00164    0.00107    0.00037
CL1   4    0.500000    0.610903    0.750000    10.50000    0.04712    0.02936 =
         0.02237    0.00000    0.00107    0.00000
CL2   4    0.749366    0.427232    0.614924    11.00000    0.03238    0.04407 =
         0.03654   -0.00050   -0.00512    0.01028
C1    1    0.919268    0.312040    0.100930    11.00000    0.03844    0.04433 =
         0.04322   -0.00635   -0.00710   -0.00580
AFIX  33
H1A   2    0.869167    0.355720    0.007107    11.00000   -1.50000
H1B   2    0.831435    0.270354    0.153012    11.00000   -1.50000
H1C   2    1.004436    0.269828    0.045237    11.00000   -1.50000
AFIX   0
N1    3    1.000000    0.373569    0.250000    10.50000    0.03504    0.03238 =
         0.03703    0.00000   -0.00504    0.00000
H1N1  2    0.918864    0.406327    0.303477    11.00000    0.08952
HKLF 4
REM  exp_341 in C2/c
REM R1 =  0.0272 for    629 Fo > 4sig(Fo)  and  0.0389 for all    762 data
REM     40 parameters refined using      0 restraints
END
WGHT      0.0288      0.0000
REM Highest difference peak  0.667,  deepest hole -0.678,  1-sigma level  0.132
Q1    1   0.5000  0.3927  0.7500  10.50000  0.05    0.67
Q2    1   0.5961  0.4965  0.7803  11.00000  0.05    0.65
Q3    1   0.7468  0.4299  0.1249  11.00000  0.05    0.60
Q4    1   0.5479  0.5513  0.3747  11.00000  0.05    0.47
Q5    1   0.6412  0.4461  0.6752  11.00000  0.05    0.42
Q6    1   0.6842  0.4190  0.7108  11.00000  0.05    0.41
Q7    1   0.6525  0.5169  0.4063  11.00000  0.05    0.38
Q8    1   0.4432  0.6654  0.8995  11.00000  0.05    0.37
Q9    1   0.8776  0.2328  0.1590  11.00000  0.05    0.37
Q10   1   0.7965  0.5029  0.5119  11.00000  0.05    0.37
;
_cod_data_source_file            fg3281.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2018704
_cod_database_fobs_code          2018704
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_symmetry_multiplicity
Pd Pd1 0.5000 0.5000 0.5000 0.0227(2) Uani d S 1 2
Cl Cl1 0.5000 0.61090(11) 0.7500 0.0329(4) Uani d S 1 2
Cl Cl2 0.74937(14) 0.42723(9) 0.61492(15) 0.0378(3) Uani d . 1 1
C C1 0.9193(6) 0.3120(4) 0.1009(6) 0.0421(11) Uani d . 1 1
H H1A 0.8692 0.3557 0.0071 0.063 Uiso calc R 1 1
H H1B 0.8314 0.2704 0.1530 0.063 Uiso calc R 1 1
H H1C 1.0044 0.2698 0.0452 0.063 Uiso calc R 1 1
N N1 1.0000 0.3736(4) 0.2500 0.0349(13) Uani d S 1 2
H H1N1 0.919(8) 0.406(4) 0.303(9) 0.09(2) Uiso d . 1 1
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
Pd1 0.0241(3) 0.0254(3) 0.0185(3) 0.0004(2) 0.00107(17) 0.00164(16)
Cl1 0.0471(10) 0.0294(8) 0.0224(7) 0.000 0.0011(6) 0.000
Cl2 0.0324(6) 0.0441(7) 0.0365(6) 0.0103(6) -0.0051(4) -0.0005(5)
C1 0.038(3) 0.044(3) 0.043(3) -0.006(2) -0.007(2) -0.006(2)
N1 0.035(3) 0.032(3) 0.037(3) 0.000 -0.005(3) 0.000
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'
N N 0.0061 0.0033 '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'
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
Cl2 Pd1 Cl2 5_666 . 180.0 yes
Cl2 Pd1 Cl1 5_666 . 89.73(3) yes
Cl2 Pd1 Cl1 . . 90.27(3) yes
Cl2 Pd1 Cl1 5_666 5_666 90.27(3) yes
Cl2 Pd1 Cl1 . 5_666 89.73(3) yes
Cl1 Pd1 Cl1 . 5_666 180.0 yes
Pd1 Cl1 Pd1 . 2_656 101.27(6) yes
N1 C1 H1A . . 109.5 ?
N1 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
N1 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
C1 N1 C1 . 2_755 112.8(5) ?
C1 N1 H1N1 . . 107(5) ?
C1 N1 H1N1 2_755 . 105(5) ?
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 Cl2 5_666 2.3010(10) yes
Pd1 Cl2 . 2.3010(10) yes
Pd1 Cl1 . 2.3092(9) yes
Pd1 Cl1 5_666 2.3092(9) yes
Cl1 Pd1 2_656 2.3092(9) yes
C1 N1 . 1.469(5) ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
N1 C1 2_755 1.469(5) ?
N1 H1N1 . 0.86(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
N1 H1N1 Cl2 . 0.86(5) 2.63(6) 3.3684(16) 145(6)
N1 H1N1 Cl2 6_565 0.86(5) 2.88(6) 3.402(5) 121(5)
