#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:33:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180342 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/11/7201141.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_7201141
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), Cl4 Pd'
_chemical_formula_sum            'C36 H48 Cl4 N2 Pd'
_chemical_formula_weight         756.96
_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                67.60(3)
_cell_angle_beta                 75.21(3)
_cell_angle_gamma                79.37(3)
_cell_formula_units_Z            1
_cell_length_a                   8.5340(17)
_cell_length_b                   10.496(2)
_cell_length_c                   10.809(2)
_cell_measurement_temperature    153(2)
_cell_volume                     861.4(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14759
_diffrn_reflns_theta_full        28.81
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.8441
_exptl_absorpt_correction_T_min  0.7788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo (Z. Otwinowski, 2003)'
_exptl_crystal_colour            'Dark Orange'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0340
_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)+(0.0218P)²+0.5530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                4038
_reflns_number_total             4477
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b905421a.txt
_cod_data_source_block           5
_cod_original_cell_volume        861.4(3)
_cod_database_code               7201141
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 1.0000 0.0000 1.0000 0.01569(7) Uani 1 2 d S . .
Cl2 Cl 1.15540(7) 0.11569(6) 1.05919(6) 0.02972(13) Uani 1 1 d . . .
Cl1 Cl 1.10838(6) 0.11108(6) 0.77346(5) 0.02432(12) Uani 1 1 d . . .
N1 N 0.5684(2) 0.30834(17) 0.79011(18) 0.0174(3) Uani 1 1 d . . .
C35 C 0.9158(3) 0.6909(2) 0.7228(3) 0.0267(5) Uani 1 1 d . . .
H35 H 0.9491 0.7749 0.7168 0.032 Uiso 1 1 calc R . .
C21 C 0.5016(3) 0.3076(2) 0.9336(2) 0.0219(4) Uani 1 1 d . . .
H21A H 0.3824 0.3027 0.9542 0.026 Uiso 1 1 calc R . .
H21B H 0.5194 0.3968 0.9367 0.026 Uiso 1 1 calc R . .
C43 C 0.4776(3) 0.2069(2) 0.5534(2) 0.0213(4) Uani 1 1 d . . .
H43 H 0.3733 0.2511 0.5787 0.026 Uiso 1 1 calc R . .
C32 C 0.8093(2) 0.4468(2) 0.7431(2) 0.0206(4) Uani 1 1 d . . .
C11 C 0.4867(2) 0.4336(2) 0.6929(2) 0.0209(4) Uani 1 1 d . . .
H11A H 0.5237 0.4295 0.5998 0.025 Uiso 1 1 calc R . .
H11B H 0.5249 0.5178 0.6913 0.025 Uiso 1 1 calc R . .
C47 C 0.7356(3) 0.0927(2) 0.6048(2) 0.0222(4) Uani 1 1 d . . .
H47 H 0.8095 0.0587 0.6653 0.027 Uiso 1 1 calc R . .
C42 C 0.5852(2) 0.1610(2) 0.6426(2) 0.0196(4) Uani 1 1 d . . .
C44 C 0.5210(3) 0.1890(2) 0.4283(2) 0.0242(5) Uani 1 1 d . . .
H44 H 0.4473 0.2222 0.3677 0.029 Uiso 1 1 calc R . .
C31 C 0.7530(2) 0.3163(2) 0.7490(2) 0.0209(4) Uani 1 1 d . . .
H31A H 0.8053 0.2362 0.8149 0.025 Uiso 1 1 calc R . .
H31B H 0.7918 0.3072 0.6580 0.025 Uiso 1 1 calc R . .
C45 C 0.6716(3) 0.1226(2) 0.3915(2) 0.0244(5) Uani 1 1 d . . .
H45 H 0.7018 0.1104 0.3056 0.029 Uiso 1 1 calc R . .
C36 C 0.8858(3) 0.5848(2) 0.8475(3) 0.0272(5) Uani 1 1 d . . .
H36 H 0.9004 0.5956 0.9270 0.033 Uiso 1 1 calc R . .
C37 C 0.8348(3) 0.4629(2) 0.8577(2) 0.0253(5) Uani 1 1 d . . .
H37 H 0.8172 0.3898 0.9437 0.030 Uiso 1 1 calc R . .
C41 C 0.5347(3) 0.1729(2) 0.7820(2) 0.0196(4) Uani 1 1 d . . .
H41A H 0.5920 0.0944 0.8455 0.023 Uiso 1 1 calc R . .
H41B H 0.4166 0.1633 0.8146 0.023 Uiso 1 1 calc R . .
C46 C 0.7779(3) 0.0742(2) 0.4809(2) 0.0251(5) Uani 1 1 d . . .
H46 H 0.8809 0.0277 0.4563 0.030 Uiso 1 1 calc R . .
C22 C 0.5726(3) 0.1917(2) 1.0450(2) 0.0292(5) Uani 1 1 d . . .
H22A H 0.5547 0.1024 1.0444 0.044 Uiso 1 1 calc R . .
H22B H 0.5194 0.1998 1.1339 0.044 Uiso 1 1 calc R . .
H22C H 0.6897 0.1979 1.0291 0.044 Uiso 1 1 calc R . .
C34 C 0.8971(3) 0.6741(2) 0.6075(3) 0.0270(5) Uani 1 1 d . . .
H34 H 0.9205 0.7457 0.5210 0.032 Uiso 1 1 calc R . .
C33 C 0.8441(2) 0.5528(2) 0.6172(2) 0.0219(4) Uani 1 1 d . . .
H33 H 0.8313 0.5419 0.5371 0.026 Uiso 1 1 calc R . .
C12 C 0.3018(3) 0.4490(2) 0.7254(3) 0.0282(5) Uani 1 1 d . . .
H12A H 0.2617 0.3616 0.7399 0.042 Uiso 1 1 calc R . .
H12B H 0.2615 0.5228 0.6490 0.042 Uiso 1 1 calc R . .
H12C H 0.2627 0.4724 0.8084 0.042 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 Cl2 180.00(2) 2_757 . ?
Cl2 Pd1 Cl1 90.45(3) 2_757 . ?
Cl2 Pd1 Cl1 89.55(3) . . ?
Cl2 Pd1 Cl1 89.55(3) 2_757 2_757 ?
Cl2 Pd1 Cl1 90.45(3) . 2_757 ?
Cl1 Pd1 Cl1 180.0 . 2_757 ?
C21 N1 C11 108.44(16) . . ?
C21 N1 C31 111.89(17) . . ?
C11 N1 C31 108.82(16) . . ?
C21 N1 C41 108.87(16) . . ?
C11 N1 C41 111.21(16) . . ?
C31 N1 C41 107.63(15) . . ?
C34 C35 C36 119.6(2) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
N1 C21 C22 116.10(18) . . ?
N1 C21 H21A 108.3 . . ?
C22 C21 H21A 108.3 . . ?
N1 C21 H21B 108.3 . . ?
C22 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C44 C43 C42 120.7(2) . . ?
C44 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
C37 C32 C33 118.6(2) . . ?
C37 C32 C31 122.4(2) . . ?
C33 C32 C31 119.0(2) . . ?
N1 C11 C12 116.06(18) . . ?
N1 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
N1 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C46 C47 C42 120.6(2) . . ?
C46 C47 H47 119.7 . . ?
C42 C47 H47 119.7 . . ?
C43 C42 C47 118.5(2) . . ?
C43 C42 C41 120.81(19) . . ?
C47 C42 C41 120.4(2) . . ?
C43 C44 C45 120.1(2) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C32 C31 N1 115.40(17) . . ?
C32 C31 H31A 108.4 . . ?
N1 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
N1 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C44 C45 C46 119.5(2) . . ?
C44 C45 H45 120.2 . . ?
C46 C45 H45 120.2 . . ?
C35 C36 C37 120.7(2) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 H36 119.7 . . ?
C36 C37 C32 120.3(2) . . ?
C36 C37 H37 119.8 . . ?
C32 C37 H37 119.8 . . ?
C42 C41 N1 115.59(16) . . ?
C42 C41 H41A 108.4 . . ?
N1 C41 H41A 108.4 . . ?
C42 C41 H41B 108.4 . . ?
N1 C41 H41B 108.4 . . ?
H41A C41 H41B 107.4 . . ?
C47 C46 C45 120.6(2) . . ?
C47 C46 H46 119.7 . . ?
C45 C46 H46 119.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C35 C34 C33 120.1(2) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C33 C32 120.7(2) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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 2.2939(8) 2_757 ?
Pd1 Cl2 2.2939(8) . ?
Pd1 Cl1 2.2971(10) . ?
Pd1 Cl1 2.2971(10) 2_757 ?
N1 C21 1.507(3) . ?
N1 C11 1.517(3) . ?
N1 C31 1.533(3) . ?
N1 C41 1.539(3) . ?
C35 C34 1.374(3) . ?
C35 C36 1.381(3) . ?
C35 H35 0.9500 . ?
C21 C22 1.510(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C43 C44 1.383(3) . ?
C43 C42 1.392(3) . ?
C43 H43 0.9500 . ?
C32 C37 1.386(3) . ?
C32 C33 1.393(3) . ?
C32 C31 1.507(3) . ?
C11 C12 1.519(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C47 C46 1.374(3) . ?
C47 C42 1.395(3) . ?
C47 H47 0.9500 . ?
C42 C41 1.505(3) . ?
C44 C45 1.384(3) . ?
C44 H44 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C45 C46 1.385(3) . ?
C45 H45 0.9500 . ?
C36 C37 1.382(3) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C46 H46 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C34 C33 1.388(3) . ?
C34 H34 0.9500 . ?
C33 H33 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
C11 N1 C21 C22 -178.32(18) . . . . ?
C31 N1 C21 C22 -58.3(2) . . . . ?
C41 N1 C21 C22 60.5(2) . . . . ?
C21 N1 C11 C12 -53.3(2) . . . . ?
C31 N1 C11 C12 -175.19(19) . . . . ?
C41 N1 C11 C12 66.4(2) . . . . ?
C44 C43 C42 C47 -1.9(3) . . . . ?
C44 C43 C42 C41 -176.39(19) . . . . ?
C46 C47 C42 C43 1.5(3) . . . . ?
C46 C47 C42 C41 175.96(19) . . . . ?
C42 C43 C44 C45 1.1(3) . . . . ?
C37 C32 C31 N1 84.9(3) . . . . ?
C33 C32 C31 N1 -98.0(2) . . . . ?
C21 N1 C31 C32 -63.7(2) . . . . ?
C11 N1 C31 C32 56.1(2) . . . . ?
C41 N1 C31 C32 176.72(18) . . . . ?
C43 C44 C45 C46 0.2(3) . . . . ?
C34 C35 C36 C37 -1.0(3) . . . . ?
C35 C36 C37 C32 -1.5(3) . . . . ?
C33 C32 C37 C36 3.2(3) . . . . ?
C31 C32 C37 C36 -179.7(2) . . . . ?
C43 C42 C41 N1 -90.0(2) . . . . ?
C47 C42 C41 N1 95.6(2) . . . . ?
C21 N1 C41 C42 176.44(17) . . . . ?
C11 N1 C41 C42 57.0(2) . . . . ?
C31 N1 C41 C42 -62.1(2) . . . . ?
C42 C47 C46 C45 -0.2(3) . . . . ?
C44 C45 C46 C47 -0.7(3) . . . . ?
C36 C35 C34 C33 1.8(3) . . . . ?
C35 C34 C33 C32 0.0(3) . . . . ?
C37 C32 C33 C34 -2.4(3) . . . . ?
C31 C32 C33 C34 -179.63(19) . . . . ?
