#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:33:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180342 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/11/7201140.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_7201140
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 N), 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                107.93(3)
_cell_angle_beta                 105.75(3)
_cell_angle_gamma                109.92(3)
_cell_formula_units_Z            1
_cell_length_a                   10.332(2)
_cell_length_b                   10.381(2)
_cell_length_c                   11.125(2)
_cell_measurement_temperature    153(2)
_cell_volume                     968.3(6)
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14631
_diffrn_reflns_theta_full        28.72
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  0.8983
_exptl_absorpt_correction_T_min  0.7002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo (Z. Otwinowski, 2003)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0122P)²+0.6422P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                4040
_reflns_number_total             4975
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b905421a.txt
_cod_data_source_block           7
_cod_original_cell_volume        968.3(3)
_cod_database_code               7201140
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 0.39412(2) 0.94042(2) 0.82873(2) 0.02389(7) Uani 1 1 d . . .
Cl1 Cl 0.40821(8) 1.04738(8) 0.67937(8) 0.03131(17) Uani 1 1 d . . .
Cl2 Cl 0.18977(8) 0.71868(8) 0.65857(8) 0.03579(18) Uani 1 1 d . . .
Cl3 Cl 0.60345(8) 1.16089(8) 1.01149(8) 0.03599(19) Uani 1 1 d . . .
N1 N 0.8007(2) 0.3749(2) 0.7284(2) 0.0198(5) Uani 1 1 d . . .
C11 C 0.9492(3) 0.4872(3) 0.7456(3) 0.0259(6) Uani 1 1 d . . .
H11A H 0.9590 0.5904 0.7836 0.039 Uiso 1 1 calc R . .
H11B H 0.9538 0.4621 0.6549 0.039 Uiso 1 1 calc R . .
H11C H 1.0323 0.4828 0.8096 0.039 Uiso 1 1 calc R . .
C12 C 0.7881(3) 0.4196(3) 0.8638(3) 0.0237(6) Uani 1 1 d . . .
H12A H 0.8738 0.4258 0.9346 0.036 Uiso 1 1 calc R . .
H12B H 0.6929 0.3430 0.8532 0.036 Uiso 1 1 calc R . .
H12C H 0.7892 0.5193 0.8926 0.036 Uiso 1 1 calc R . .
C21 C 0.6698(3) 0.3684(3) 0.6175(3) 0.0236(6) Uani 1 1 d . . .
H21A H 0.6786 0.3347 0.5280 0.028 Uiso 1 1 calc R . .
H21B H 0.5731 0.2902 0.6053 0.028 Uiso 1 1 calc R . .
C22 C 0.6622(3) 0.5176(3) 0.6494(3) 0.0237(6) Uani 1 1 d . . .
C23 C 0.7482(3) 0.6208(3) 0.6110(3) 0.0307(7) Uani 1 1 d . . .
H23 H 0.8103 0.5962 0.5686 0.037 Uiso 1 1 calc R . .
C24 C 0.7445(4) 0.7581(4) 0.6338(4) 0.0393(8) Uani 1 1 d . . .
H24 H 0.8063 0.8286 0.6103 0.047 Uiso 1 1 calc R . .
C25 C 0.6504(3) 0.7913(4) 0.6906(3) 0.0387(8) Uani 1 1 d . . .
H25 H 0.6455 0.8843 0.7048 0.046 Uiso 1 1 calc R . .
C26 C 0.5637(3) 0.6903(3) 0.7267(3) 0.0351(7) Uani 1 1 d . . .
H26 H 0.4987 0.7144 0.7652 0.042 Uiso 1 1 calc R . .
C27 C 0.5682(3) 0.5531(3) 0.7087(3) 0.0279(6) Uani 1 1 d . . .
C28 C 0.4687(3) 0.4508(4) 0.7525(4) 0.0410(8) Uani 1 1 d . . .
H28A H 0.4369 0.3439 0.6928 0.061 Uiso 1 1 calc R . .
H28B H 0.3789 0.4666 0.7436 0.061 Uiso 1 1 calc R . .
H28C H 0.5254 0.4754 0.8496 0.061 Uiso 1 1 calc R . .
C31 C 0.7866(3) 0.2131(3) 0.6752(3) 0.0232(6) Uani 1 1 d . . .
H31A H 0.6894 0.1417 0.6683 0.028 Uiso 1 1 calc R . .
H31B H 0.7826 0.1817 0.5801 0.028 Uiso 1 1 calc R . .
C32 C 0.9141(3) 0.1975(3) 0.7650(3) 0.0242(6) Uani 1 1 d . . .
C33 C 0.9082(3) 0.1762(3) 0.8817(3) 0.0308(7) Uani 1 1 d . . .
H33 H 0.8259 0.1750 0.9048 0.037 Uiso 1 1 calc R . .
C34 C 1.0198(4) 0.1567(3) 0.9646(3) 0.0410(8) Uani 1 1 d . . .
H34 H 1.0155 0.1449 1.0450 0.049 Uiso 1 1 calc R . .
C35 C 1.1373(4) 0.1545(4) 0.9290(4) 0.0446(9) Uani 1 1 d . . .
H35 H 1.2149 0.1420 0.9856 0.053 Uiso 1 1 calc R . .
C36 C 1.1422(3) 0.1702(4) 0.8125(4) 0.0399(8) Uani 1 1 d . . .
H36 H 1.2230 0.1667 0.7888 0.048 Uiso 1 1 calc R . .
C37 C 1.0326(3) 0.1912(3) 0.7277(3) 0.0306(7) Uani 1 1 d . . .
C38 C 1.0430(4) 0.2020(4) 0.5983(4) 0.0402(8) Uani 1 1 d . . .
H38A H 1.0757 0.3079 0.6123 0.060 Uiso 1 1 calc R . .
H38B H 0.9432 0.1359 0.5193 0.060 Uiso 1 1 calc R . .
H38C H 1.1167 0.1693 0.5793 0.060 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
Cl1 Pd1 Cl2 92.36(4) . . ?
Cl1 Pd1 Cl3 176.34(3) . 2_677 ?
Cl2 Pd1 Cl3 90.60(4) . 2_677 ?
Cl1 Pd1 Cl3 90.89(4) . . ?
Cl2 Pd1 Cl3 176.74(3) . . ?
Cl3 Pd1 Cl3 86.14(4) 2_677 . ?
Pd1 Cl3 Pd1 93.86(4) 2_677 . ?
C12 N1 C11 109.7(2) . . ?
C12 N1 C21 110.1(2) . . ?
C11 N1 C21 110.1(2) . . ?
C12 N1 C31 110.5(2) . . ?
C11 N1 C31 110.20(19) . . ?
C21 N1 C31 106.14(19) . . ?
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 115.0(2) . . ?
C22 C21 H21A 108.5 . . ?
N1 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
N1 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C27 C22 C23 119.0(3) . . ?
C27 C22 C21 123.0(2) . . ?
C23 C22 C21 117.9(2) . . ?
C24 C23 C22 121.3(3) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C25 C24 C23 119.4(3) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C26 C25 C24 120.0(3) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 122.0(3) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
C26 C27 C22 118.4(3) . . ?
C26 C27 C28 117.5(3) . . ?
C22 C27 C28 124.1(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 C31 N1 114.7(2) . . ?
C32 C31 H31A 108.6 . . ?
N1 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
N1 C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
C33 C32 C37 118.8(3) . . ?
C33 C32 C31 119.3(2) . . ?
C37 C32 C31 121.6(3) . . ?
C34 C33 C32 121.4(3) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C35 C34 C33 119.3(3) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C36 C35 C34 120.1(3) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C37 122.1(3) . . ?
C35 C36 H36 118.9 . . ?
C37 C36 H36 118.9 . . ?
C36 C37 C32 118.3(3) . . ?
C36 C37 C38 118.9(3) . . ?
C32 C37 C38 122.9(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 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 Cl1 2.2743(9) . ?
Pd1 Cl2 2.2750(18) . ?
Pd1 Cl3 2.3261(9) 2_677 ?
Pd1 Cl3 2.3291(19) . ?
Cl3 Pd1 2.3261(9) 2_677 ?
N1 C12 1.490(3) . ?
N1 C11 1.495(3) . ?
N1 C21 1.529(3) . ?
N1 C31 1.538(3) . ?
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 1.513(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.399(4) . ?
C22 C23 1.399(4) . ?
C23 C24 1.385(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.375(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.371(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.395(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.506(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C31 C32 1.513(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.396(4) . ?
C32 C37 1.411(4) . ?
C33 C34 1.384(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.367(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.391(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.506(4) . ?
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
Cl1 Pd1 Cl3 Pd1 -177.86(3) . . . 2_677 ?
Cl2 Pd1 Cl3 Pd1 -2.8(5) . . . 2_677 ?
Cl3 Pd1 Cl3 Pd1 0.0 2_677 . . 2_677 ?
C12 N1 C21 C22 60.4(3) . . . . ?
C11 N1 C21 C22 -60.7(3) . . . . ?
C31 N1 C21 C22 -180.0(2) . . . . ?
N1 C21 C22 C27 -97.1(3) . . . . ?
N1 C21 C22 C23 86.1(3) . . . . ?
C27 C22 C23 C24 1.5(4) . . . . ?
C21 C22 C23 C24 178.5(3) . . . . ?
C22 C23 C24 C25 -2.3(5) . . . . ?
C23 C24 C25 C26 1.3(5) . . . . ?
C24 C25 C26 C27 0.5(5) . . . . ?
C25 C26 C27 C22 -1.3(5) . . . . ?
C25 C26 C27 C28 179.8(3) . . . . ?
C23 C22 C27 C26 0.3(4) . . . . ?
C21 C22 C27 C26 -176.5(3) . . . . ?
C23 C22 C27 C28 179.1(3) . . . . ?
C21 C22 C27 C28 2.3(4) . . . . ?
C12 N1 C31 C32 -65.3(3) . . . . ?
C11 N1 C31 C32 56.1(3) . . . . ?
C21 N1 C31 C32 175.3(2) . . . . ?
N1 C31 C32 C33 83.2(3) . . . . ?
N1 C31 C32 C37 -102.1(3) . . . . ?
C37 C32 C33 C34 3.2(4) . . . . ?
C31 C32 C33 C34 178.0(3) . . . . ?
C32 C33 C34 C35 -1.6(4) . . . . ?
C33 C34 C35 C36 -0.5(5) . . . . ?
C34 C35 C36 C37 1.1(5) . . . . ?
C35 C36 C37 C32 0.5(5) . . . . ?
C35 C36 C37 C38 -177.8(3) . . . . ?
C33 C32 C37 C36 -2.6(4) . . . . ?
C31 C32 C37 C36 -177.3(3) . . . . ?
C33 C32 C37 C38 175.7(3) . . . . ?
C31 C32 C37 C38 1.0(4) . . . . ?
