#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:33:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180342 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/11/7201139.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7201139
loop_
_publ_author_name
'Peuronen, Anssi'
'Lahtinen, Manu'
'Valkonen, Jussi'
_publ_section_title
;
 The conformational polymorphism and weak interactions in solid state
 structures of ten new monomeric and dimeric substituted
 dibenzyldimethylammonium chloridopalladate salts
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2344
_journal_paper_doi               10.1039/b905421a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         '2(C18 H24 N1), (Cl6 Pd2)'
_chemical_formula_sum            'C36 H48 Cl6 N2 Pd2'
_chemical_formula_weight         934.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.17(3)
_cell_angle_beta                 107.55(3)
_cell_angle_gamma                114.80(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5640(19)
_cell_length_b                   10.679(2)
_cell_length_c                   11.417(2)
_cell_measurement_temperature    153(2)
_cell_volume                     965.8(5)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Diamond 3.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Kappa APEX II'
_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  0.1110
_diffrn_reflns_av_sigmaI/netI    0.1527
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16403
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.9345
_exptl_absorpt_correction_T_min  0.8748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo (Z. Otwinowski, 2003)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0694
_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)+(0.0190P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                2941
_reflns_number_total             4979
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b905421a.txt
_cod_data_source_block           8a
_cod_original_cell_volume        965.7(3)
_cod_database_code               7201139
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.04883(5) 0.16310(5) -0.02925(4) 0.02145(15) Uani 1 1 d . . .
Cl1 Cl 1.07731(17) 0.24736(19) -0.19858(14) 0.0342(4) Uani 1 1 d . . .
Cl2 Cl 1.12449(17) 0.38491(18) 0.08981(15) 0.0341(4) Uani 1 1 d . . .
Cl3 Cl 1.02083(16) 0.06755(16) 0.13983(13) 0.0282(4) Uani 1 1 d . . .
N1 N 0.5774(5) 0.2910(5) 0.0803(4) 0.0184(10) Uani 1 1 d . . .
C11 C 0.7481(6) 0.3040(7) 0.1290(5) 0.0306(16) Uani 1 1 d . . .
H11A H 0.7803 0.3028 0.2187 0.046 Uiso 1 1 calc R . .
H11B H 0.8290 0.3948 0.1232 0.046 Uiso 1 1 calc R . .
H11C H 0.7469 0.2230 0.0770 0.046 Uiso 1 1 calc R . .
C12 C 0.4485(6) 0.1469(6) 0.0769(5) 0.0221(13) Uani 1 1 d . . .
H12A H 0.4453 0.0704 0.0172 0.033 Uiso 1 1 calc R . .
H12B H 0.3383 0.1418 0.0483 0.033 Uiso 1 1 calc R . .
H12C H 0.4778 0.1344 0.1630 0.033 Uiso 1 1 calc R . .
C21 C 0.5371(7) 0.3125(7) -0.0524(5) 0.0230(13) Uani 1 1 d . . .
H21A H 0.4338 0.3213 -0.0766 0.028 Uiso 1 1 calc R . .
H21B H 0.6290 0.4049 -0.0478 0.028 Uiso 1 1 calc R . .
C22 C 0.5125(6) 0.1947(6) -0.1572(5) 0.0213(13) Uani 1 1 d . . .
C23 C 0.6491(7) 0.2006(7) -0.1830(5) 0.0287(15) Uani 1 1 d . . .
H23 H 0.7593 0.2770 -0.1328 0.034 Uiso 1 1 calc R . .
C24 C 0.6207(7) 0.0937(7) -0.2828(5) 0.0283(15) Uani 1 1 d . . .
H24 H 0.7130 0.0963 -0.2999 0.034 Uiso 1 1 calc R . .
C25 C 0.4598(7) -0.0181(7) -0.3591(5) 0.0294(15) Uani 1 1 d . . .
H25 H 0.4441 -0.0909 -0.4265 0.035 Uiso 1 1 calc R . .
C26 C 0.3209(7) -0.0241(7) -0.3371(5) 0.0234(13) Uani 1 1 d . . .
C27 C 0.3521(7) 0.0843(6) -0.2349(5) 0.0232(13) Uani 1 1 d . . .
H27 H 0.2601 0.0825 -0.2179 0.028 Uiso 1 1 calc R . .
C28 C 0.1470(7) -0.1376(7) -0.4217(5) 0.0366(17) Uani 1 1 d . . .
H28A H 0.0786 -0.1623 -0.3707 0.055 Uiso 1 1 calc R . .
H28B H 0.1489 -0.2236 -0.4610 0.055 Uiso 1 1 calc R . .
H28C H 0.0990 -0.1016 -0.4892 0.055 Uiso 1 1 calc R . .
C31 C 0.5764(7) 0.4125(6) 0.1662(5) 0.0211(13) Uani 1 1 d . . .
H31A H 0.6617 0.5058 0.1659 0.025 Uiso 1 1 calc R . .
H31B H 0.4658 0.4075 0.1281 0.025 Uiso 1 1 calc R . .
C32 C 0.6097(6) 0.4109(6) 0.3028(5) 0.0224(13) Uani 1 1 d . . .
C33 C 0.7730(7) 0.4873(7) 0.3965(5) 0.0272(14) Uani 1 1 d . . .
H33 H 0.8644 0.5386 0.3738 0.033 Uiso 1 1 calc R . .
C34 C 0.8001(7) 0.4874(7) 0.5215(6) 0.0367(17) Uani 1 1 d . . .
H34 H 0.9106 0.5414 0.5858 0.044 Uiso 1 1 calc R . .
C35 C 0.6689(8) 0.4101(7) 0.5549(5) 0.0330(16) Uani 1 1 d . . .
H35 H 0.6909 0.4077 0.6413 0.040 Uiso 1 1 calc R . .
C36 C 0.5057(7) 0.3358(7) 0.4647(5) 0.0265(14) Uani 1 1 d . . .
C37 C 0.4779(7) 0.3367(6) 0.3380(5) 0.0205(13) Uani 1 1 d . . .
H37 H 0.3668 0.2856 0.2745 0.025 Uiso 1 1 calc R . .
C38 C 0.3603(8) 0.2530(7) 0.4998(6) 0.0354(17) Uani 1 1 d . . .
H38A H 0.2742 0.2815 0.4678 0.053 Uiso 1 1 calc R . .
H38B H 0.3991 0.2741 0.5933 0.053 Uiso 1 1 calc R . .
H38C H 0.3131 0.1495 0.4610 0.053 Uiso 1 1 calc R . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Pd1 Cl1 91.26(7) . . ?
Cl2 Pd1 Cl3 91.31(6) . . ?
Cl1 Pd1 Cl3 177.26(6) . . ?
Cl2 Pd1 Cl3 176.40(6) . 2_755 ?
Cl1 Pd1 Cl3 91.75(6) . 2_755 ?
Cl3 Pd1 Cl3 85.65(6) . 2_755 ?
Pd1 Cl3 Pd1 94.35(6) . 2_755 ?
C11 N1 C12 110.6(4) . . ?
C11 N1 C21 109.4(4) . . ?
C12 N1 C21 110.7(4) . . ?
C11 N1 C31 109.6(4) . . ?
C12 N1 C31 110.3(4) . . ?
C21 N1 C31 106.1(4) . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C22 C21 N1 115.4(5) . . ?
C22 C21 H21A 108.4 . . ?
N1 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
N1 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C27 C22 C23 119.3(5) . . ?
C27 C22 C21 120.0(4) . . ?
C23 C22 C21 120.6(5) . . ?
C24 C23 C22 118.9(5) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C23 C24 C25 121.5(5) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C24 C25 C26 120.6(5) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C27 C26 C25 117.1(5) . . ?
C27 C26 C28 121.2(5) . . ?
C25 C26 C28 121.6(5) . . ?
C22 C27 C26 122.5(5) . . ?
C22 C27 H27 118.7 . . ?
C26 C27 H27 118.7 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 C31 N1 115.6(4) . . ?
C32 C31 H31A 108.4 . . ?
N1 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
N1 C31 H31B 108.4 . . ?
H31A C31 H31B 107.4 . . ?
C37 C32 C33 119.4(5) . . ?
C37 C32 C31 120.1(5) . . ?
C33 C32 C31 120.5(5) . . ?
C34 C33 C32 119.5(6) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C35 120.7(5) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C34 C35 C36 121.0(5) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C37 118.2(5) . . ?
C35 C36 C38 121.9(5) . . ?
C37 C36 C38 119.9(5) . . ?
C32 C37 C36 121.1(5) . . ?
C32 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl2 2.2687(19) . ?
Pd1 Cl1 2.2733(17) . ?
Pd1 Cl3 2.3267(16) . ?
Pd1 Cl3 2.3333(18) 2_755 ?
Cl3 Pd1 2.3333(18) 2_755 ?
N1 C11 1.495(6) . ?
N1 C12 1.501(7) . ?
N1 C21 1.518(6) . ?
N1 C31 1.531(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.509(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.390(7) . ?
C22 C23 1.402(7) . ?
C23 C24 1.379(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.394(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.402(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.398(7) . ?
C26 C28 1.489(8) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C31 C32 1.498(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C37 1.388(7) . ?
C32 C33 1.398(7) . ?
C33 C34 1.370(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.392(7) . ?
C36 C38 1.506(8) . ?
C37 H37 0.9500 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 Pd1 Cl3 Pd1 -178.07(5) . . . 2_755 ?
Cl1 Pd1 Cl3 Pd1 -18.3(12) . . . 2_755 ?
Cl3 Pd1 Cl3 Pd1 0.0 2_755 . . 2_755 ?
C11 N1 C21 C22 68.3(6) . . . . ?
C12 N1 C21 C22 -53.8(5) . . . . ?
C31 N1 C21 C22 -173.5(4) . . . . ?
N1 C21 C22 C27 95.9(6) . . . . ?
N1 C21 C22 C23 -88.6(6) . . . . ?
C27 C22 C23 C24 -2.0(8) . . . . ?
C21 C22 C23 C24 -177.6(5) . . . . ?
C22 C23 C24 C25 1.0(9) . . . . ?
C23 C24 C25 C26 0.7(9) . . . . ?
C24 C25 C26 C27 -1.3(8) . . . . ?
C24 C25 C26 C28 176.5(6) . . . . ?
C23 C22 C27 C26 1.5(9) . . . . ?
C21 C22 C27 C26 177.0(5) . . . . ?
C25 C26 C27 C22 0.2(8) . . . . ?
C28 C26 C27 C22 -177.6(6) . . . . ?
C11 N1 C31 C32 -63.3(6) . . . . ?
C12 N1 C31 C32 58.7(6) . . . . ?
C21 N1 C31 C32 178.7(4) . . . . ?
N1 C31 C32 C37 -90.2(6) . . . . ?
N1 C31 C32 C33 91.6(6) . . . . ?
C37 C32 C33 C34 0.1(9) . . . . ?
C31 C32 C33 C34 178.3(6) . . . . ?
C32 C33 C34 C35 1.7(9) . . . . ?
C33 C34 C35 C36 -3.1(10) . . . . ?
C34 C35 C36 C37 2.5(9) . . . . ?
C34 C35 C36 C38 -178.9(5) . . . . ?
C33 C32 C37 C36 -0.7(8) . . . . ?
C31 C32 C37 C36 -178.9(5) . . . . ?
C35 C36 C37 C32 -0.6(8) . . . . ?
C38 C36 C37 C32 -179.3(5) . . . . ?
