#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:33:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180342 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/11/7201147.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_7201147
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(C16 H20 N), Cl4 Pd'
_chemical_formula_sum            'C32 H40 Cl4 N2 Pd'
_chemical_formula_weight         700.86
_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                63.85(3)
_cell_angle_beta                 82.50(3)
_cell_angle_gamma                65.19(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6420(17)
_cell_length_b                   10.201(2)
_cell_length_c                   10.998(2)
_cell_measurement_temperature    153(2)
_cell_volume                     788.2(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     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11388
_diffrn_reflns_theta_full        28.78
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.8037
_exptl_absorpt_correction_T_min  0.7504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo (Z. Otwinowski, 2003)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0380
_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)+(0.0218P)²+0.4361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                3483
_reflns_number_total             4087
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b905421a.txt
_cod_data_source_block           1b
_cod_original_cell_volume        788.3(3)
_cod_database_code               7201147
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 0.5000 0.5000 0.02042(8) Uani 1 2 d S . .
Cl2 Cl 1.19423(8) 0.23638(7) 0.57795(7) 0.02873(15) Uani 1 1 d . . .
Cl1 Cl 0.83225(8) 0.43826(8) 0.68070(7) 0.02923(15) Uani 1 1 d . . .
N1 N 0.6948(3) 0.1624(2) 0.5834(2) 0.0223(4) Uani 1 1 d . . .
C31 C 0.5944(3) 0.1849(3) 0.7039(3) 0.0252(5) Uani 1 1 d . . .
H31A H 0.5987 0.2773 0.7100 0.030 Uiso 1 1 calc R . .
H31B H 0.4732 0.2108 0.6862 0.030 Uiso 1 1 calc R . .
C12 C 0.8813(3) 0.1059(3) 0.6141(3) 0.0255(5) Uani 1 1 d . . .
H12A H 0.9237 -0.0015 0.6891 0.038 Uiso 1 1 calc R . .
H12B H 0.8993 0.1792 0.6398 0.038 Uiso 1 1 calc R . .
H12C H 0.9432 0.1028 0.5334 0.038 Uiso 1 1 calc R . .
C21 C 0.6283(3) 0.3265(3) 0.4622(3) 0.0258(5) Uani 1 1 d . . .
H21A H 0.5025 0.3671 0.4517 0.031 Uiso 1 1 calc R . .
H21B H 0.6541 0.4008 0.4827 0.031 Uiso 1 1 calc R . .
C22 C 0.7005(3) 0.3298(3) 0.3291(3) 0.0271(6) Uani 1 1 d . . .
C32 C 0.6595(3) 0.0418(3) 0.8377(3) 0.0255(5) Uani 1 1 d . . .
C11 C 0.6653(4) 0.0439(3) 0.5552(3) 0.0299(6) Uani 1 1 d . . .
H11A H 0.7236 0.0362 0.4744 0.045 Uiso 1 1 calc R . .
H11B H 0.5425 0.0788 0.5393 0.045 Uiso 1 1 calc R . .
H11C H 0.7104 -0.0609 0.6332 0.045 Uiso 1 1 calc R . .
C34 C 0.6704(4) -0.2145(3) 1.0044(3) 0.0332(6) Uani 1 1 d . . .
H34 H 0.6385 -0.3014 1.0310 0.040 Uiso 1 1 calc R . .
C37 C 0.7674(3) 0.0364(3) 0.9260(3) 0.0296(6) Uani 1 1 d . . .
H37 H 0.8011 0.1221 0.8995 0.036 Uiso 1 1 calc R . .
C36 C 0.8252(4) -0.0924(4) 1.0510(3) 0.0340(6) Uani 1 1 d . . .
H36 H 0.8973 -0.0943 1.1106 0.041 Uiso 1 1 calc R . .
C25 C 0.8274(4) 0.3415(3) 0.0795(3) 0.0407(7) Uani 1 1 d . . .
H25 H 0.8717 0.3440 -0.0049 0.049 Uiso 1 1 calc R . .
C35 C 0.7782(3) -0.2192(4) 1.0899(3) 0.0333(6) Uani 1 1 d . . .
H35 H 0.8200 -0.3089 1.1752 0.040 Uiso 1 1 calc R . .
C23 C 0.8512(4) 0.3510(3) 0.2897(3) 0.0306(6) Uani 1 1 d . . .
H23 H 0.9116 0.3618 0.3485 0.037 Uiso 1 1 calc R . .
C33 C 0.6083(3) -0.0839(3) 0.8799(3) 0.0294(6) Uani 1 1 d . . .
H33 H 0.5308 -0.0799 0.8232 0.035 Uiso 1 1 calc R . .
C24 C 0.9141(4) 0.3564(3) 0.1664(3) 0.0366(7) Uani 1 1 d . . .
H24 H 1.0174 0.3705 0.1412 0.044 Uiso 1 1 calc R . .
C27 C 0.6117(4) 0.3174(4) 0.2393(3) 0.0367(7) Uani 1 1 d . . .
H27 H 0.5073 0.3052 0.2633 0.044 Uiso 1 1 calc R . .
C26 C 0.6760(4) 0.3228(4) 0.1157(3) 0.0422(8) Uani 1 1 d . . .
H26 H 0.6158 0.3137 0.0556 0.051 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 180.0 2_766 . ?
Cl2 Pd1 Cl1 88.24(4) 2_766 . ?
Cl2 Pd1 Cl1 91.76(4) . . ?
Cl2 Pd1 Cl1 91.76(4) 2_766 2_766 ?
Cl2 Pd1 Cl1 88.24(4) . 2_766 ?
Cl1 Pd1 Cl1 180.000(1) . 2_766 ?
C11 N1 C12 109.67(19) . . ?
C11 N1 C21 110.54(19) . . ?
C12 N1 C21 110.2(2) . . ?
C11 N1 C31 110.35(19) . . ?
C12 N1 C31 109.90(19) . . ?
C21 N1 C31 106.15(18) . . ?
C32 C31 N1 114.1(2) . . ?
C32 C31 H31A 108.7 . . ?
N1 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
N1 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
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 115.22(19) . . ?
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 . . ?
C23 C22 C27 118.5(3) . . ?
C23 C22 C21 121.7(2) . . ?
C27 C22 C21 119.8(3) . . ?
C33 C32 C37 118.8(3) . . ?
C33 C32 C31 121.4(2) . . ?
C37 C32 C31 119.7(2) . . ?
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 . . ?
C35 C34 C33 120.5(3) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C36 C37 C32 120.6(3) . . ?
C36 C37 H37 119.7 . . ?
C32 C37 H37 119.7 . . ?
C37 C36 C35 120.1(3) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C24 C25 C26 119.8(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C34 C35 C36 119.8(3) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C24 C23 C22 120.9(3) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C34 C33 C32 120.1(3) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C27 C22 120.1(3) . . ?
C26 C27 H27 119.9 . . ?
C22 C27 H27 119.9 . . ?
C25 C26 C27 120.4(3) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
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 2.3108(13) 2_766 ?
Pd1 Cl2 2.3108(13) . ?
Pd1 Cl1 2.3150(10) . ?
Pd1 Cl1 2.3150(10) 2_766 ?
N1 C11 1.494(3) . ?
N1 C12 1.494(3) . ?
N1 C21 1.528(3) . ?
N1 C31 1.537(3) . ?
C31 C32 1.499(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.507(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.391(4) . ?
C22 C27 1.404(4) . ?
C32 C33 1.398(4) . ?
C32 C37 1.400(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C34 C35 1.381(4) . ?
C34 C33 1.386(4) . ?
C34 H34 0.9500 . ?
C37 C36 1.379(4) . ?
C37 H37 0.9500 . ?
C36 C35 1.389(4) . ?
C36 H36 0.9500 . ?
C25 C24 1.381(4) . ?
C25 C26 1.383(4) . ?
C25 H25 0.9500 . ?
C35 H35 0.9500 . ?
C23 C24 1.380(4) . ?
C23 H23 0.9500 . ?
C33 H33 0.9500 . ?
C24 H24 0.9500 . ?
C27 C26 1.386(4) . ?
C27 H27 0.9500 . ?
C26 H26 0.9500 . ?
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 C31 C32 68.7(3) . . . . ?
C12 N1 C31 C32 -52.3(3) . . . . ?
C21 N1 C31 C32 -171.5(2) . . . . ?
C11 N1 C21 C22 -55.9(3) . . . . ?
C12 N1 C21 C22 65.5(3) . . . . ?
C31 N1 C21 C22 -175.6(2) . . . . ?
N1 C21 C22 C23 -87.8(3) . . . . ?
N1 C21 C22 C27 94.6(3) . . . . ?
N1 C31 C32 C33 -84.5(3) . . . . ?
N1 C31 C32 C37 98.7(3) . . . . ?
C33 C32 C37 C36 1.5(4) . . . . ?
C31 C32 C37 C36 178.3(2) . . . . ?
C32 C37 C36 C35 0.7(4) . . . . ?
C33 C34 C35 C36 -0.2(4) . . . . ?
C37 C36 C35 C34 -1.4(4) . . . . ?
C27 C22 C23 C24 -1.3(4) . . . . ?
C21 C22 C23 C24 -178.9(2) . . . . ?
C35 C34 C33 C32 2.4(4) . . . . ?
C37 C32 C33 C34 -3.0(4) . . . . ?
C31 C32 C33 C34 -179.8(2) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C26 C25 C24 C23 0.7(5) . . . . ?
C23 C22 C27 C26 1.3(4) . . . . ?
C21 C22 C27 C26 179.0(3) . . . . ?
C24 C25 C26 C27 -0.7(5) . . . . ?
C22 C27 C26 C25 -0.4(5) . . . . ?
