#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:33:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180342 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/11/7201148.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_7201148
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                107.25(3)
_cell_angle_beta                 105.75(3)
_cell_angle_gamma                103.75(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2770(17)
_cell_length_b                   10.612(2)
_cell_length_c                   11.527(2)
_cell_measurement_temperature    153(2)
_cell_volume                     873.1(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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0422
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13580
_diffrn_reflns_theta_full        28.72
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  0.9033
_exptl_absorpt_correction_T_min  0.8598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo (Z. Otwinowski, 2003)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0323
_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)+(0.0200P)²+0.5521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                4042
_reflns_number_total             4511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905421a.txt
_cod_data_source_block           2
_cod_original_cell_volume        873.1(3)
_cod_database_code               7201148
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 0.0000 0.5000 0.0000 0.02577(7) Uani 1 2 d S . .
Cl2 Cl 0.00368(7) 0.44485(6) 0.18000(5) 0.03519(13) Uani 1 1 d . . .
Cl1 Cl 0.16368(8) 0.35675(6) -0.04777(6) 0.03823(13) Uani 1 1 d . . .
N1 N -0.4325(2) 0.39349(16) 0.26967(15) 0.0214(3) Uani 1 1 d . B .
C11 C -0.5976(3) 0.3645(2) 0.3019(2) 0.0277(4) Uani 1 1 d . . .
H11A H -0.6190 0.2775 0.3181 0.042 Uiso 1 1 calc R . .
H11B H -0.7003 0.3542 0.2286 0.042 Uiso 1 1 calc R . .
H11C H -0.5815 0.4428 0.3803 0.042 Uiso 1 1 calc R . .
C12 C -0.2772(3) 0.4095(2) 0.38164(19) 0.0252(4) Uani 1 1 d . . .
H12A H -0.2576 0.4910 0.4585 0.038 Uiso 1 1 calc R . .
H12B H -0.1700 0.4234 0.3592 0.038 Uiso 1 1 calc R . .
H12C H -0.3015 0.3245 0.4010 0.038 Uiso 1 1 calc R . .
C21 C -0.3980(3) 0.52675(19) 0.2390(2) 0.0253(4) Uani 1 1 d . . .
H21A H -0.2897 0.5413 0.2164 0.030 Uiso 1 1 calc R . .
H21B H -0.5000 0.5113 0.1611 0.030 Uiso 1 1 calc R . .
C22 C -0.3730(3) 0.6586(2) 0.3487(2) 0.0246(4) Uani 1 1 d . . .
C28 C -0.0327(3) 0.7430(2) 0.4164(3) 0.0403(5) Uani 1 1 d . . .
H28A H -0.0153 0.6612 0.4337 0.060 Uiso 1 1 calc R . .
H28B H 0.0685 0.8280 0.4785 0.060 Uiso 1 1 calc R . .
H28C H -0.0404 0.7304 0.3271 0.060 Uiso 1 1 calc R . .
C23 C -0.5256(3) 0.6865(2) 0.3623(2) 0.0337(5) Uani 1 1 d . . .
H23 H -0.6407 0.6215 0.3037 0.040 Uiso 1 1 calc R . .
C26 C -0.1939(3) 0.8780(2) 0.5294(2) 0.0372(5) Uani 1 1 d . . .
H26 H -0.0797 0.9452 0.5874 0.045 Uiso 1 1 calc R . .
C27 C -0.2037(3) 0.7575(2) 0.4317(2) 0.0291(4) Uani 1 1 d . . .
C25 C -0.3452(4) 0.9020(3) 0.5439(2) 0.0419(6) Uani 1 1 d . . .
H25 H -0.3346 0.9840 0.6121 0.050 Uiso 1 1 calc R . .
C24 C -0.5116(4) 0.8067(3) 0.4593(3) 0.0406(6) Uani 1 1 d . . .
H24 H -0.6164 0.8236 0.4677 0.049 Uiso 1 1 calc R . .
C31 C -0.4579(3) 0.27278(19) 0.14544(19) 0.0250(4) Uani 1 1 d . . .
H31A H -0.5670 0.2607 0.0746 0.030 Uiso 1 1 calc R A 1
H31B H -0.3551 0.3004 0.1189 0.030 Uiso 1 1 calc R A 1
C32A C -0.4743(6) 0.1328(4) 0.1573(6) 0.0267(17) Uani 0.50 1 d PG B 1
C37A C -0.6351(6) 0.0298(4) 0.1287(5) 0.0366(14) Uani 0.50 1 d PG B 1
C36A C -0.6363(7) -0.0991(4) 0.1352(5) 0.0481(18) Uani 0.50 1 d PG B 1
H36A H -0.7462 -0.1695 0.1156 0.058 Uiso 0.50 1 calc PR B 1
C35A C -0.4768(7) -0.1250(4) 0.1704(5) 0.054(2) Uani 0.50 1 d PG B 1
H35A H -0.4776 -0.2131 0.1749 0.065 Uiso 0.50 1 calc PR B 1
C34A C -0.3160(7) -0.0219(4) 0.1991(4) 0.0551(16) Uani 0.50 1 d PG B 1
H34A H -0.2069 -0.0396 0.2231 0.066 Uiso 0.50 1 calc PR B 1
C33A C -0.3147(6) 0.1070(4) 0.1925(5) 0.0356(13) Uani 0.50 1 d PG B 1
H33A H -0.2048 0.1774 0.2121 0.043 Uiso 0.50 1 calc PR B 1
C38A C -0.8168(7) 0.0444(6) 0.0800(6) 0.0585(16) Uani 0.50 1 d P B 1
H38A H -0.8501 0.0838 0.1546 0.088 Uiso 0.50 1 calc PR B 1
H38B H -0.9064 -0.0482 0.0215 0.088 Uiso 0.50 1 calc PR B 1
H38C H -0.8112 0.1072 0.0326 0.088 Uiso 0.50 1 calc PR B 1
C32B C -0.5075(6) 0.1269(4) 0.1488(6) 0.0309(18) Uani 0.50 1 d PG B 2
C33B C -0.6905(6) 0.0539(4) 0.1066(5) 0.0371(14) Uani 0.50 1 d PG B 2
H33B H -0.7745 0.0970 0.0805 0.045 Uiso 0.50 1 calc PR B 2
C34B C -0.7500(6) -0.0824(4) 0.1029(4) 0.0496(14) Uani 0.50 1 d PG B 2
H34B H -0.8745 -0.1321 0.0743 0.059 Uiso 0.50 1 calc PR B 2
C35B C -0.6265(7) -0.1458(4) 0.1413(5) 0.0528(19) Uani 0.50 1 d PG B 2
H35B H -0.6669 -0.2385 0.1388 0.063 Uiso 0.50 1 calc PR B 2
C36B C -0.4434(7) -0.0728(4) 0.1835(5) 0.0479(18) Uani 0.50 1 d PG B 2
H36B H -0.3594 -0.1159 0.2096 0.058 Uiso 0.50 1 calc PR B 2
C37B C -0.3839(6) 0.0636(4) 0.1872(5) 0.0341(13) Uani 0.50 1 d PG B 2
C38B C -0.1882(8) 0.1293(5) 0.2240(5) 0.0438(12) Uani 0.50 1 d P B 2
H38D H -0.1330 0.1865 0.3180 0.066 Uiso 0.50 1 calc PR B 2
H38E H -0.1664 0.1892 0.1755 0.066 Uiso 0.50 1 calc PR B 2
H38F H -0.1362 0.0556 0.2029 0.066 Uiso 0.50 1 calc PR B 2
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 Cl1 180.0 . 2_565 ?
Cl1 Pd1 Cl2 90.74(3) . 2_565 ?
Cl1 Pd1 Cl2 89.26(3) 2_565 2_565 ?
Cl1 Pd1 Cl2 89.26(3) . . ?
Cl1 Pd1 Cl2 90.74(3) 2_565 . ?
Cl2 Pd1 Cl2 180.000(1) 2_565 . ?
C12 N1 C11 109.18(15) . . ?
C12 N1 C31 110.49(14) . . ?
C11 N1 C31 109.88(15) . . ?
C12 N1 C21 110.28(15) . . ?
C11 N1 C21 111.00(14) . . ?
C31 N1 C21 105.98(14) . . ?
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 114.58(15) . . ?
C22 C21 H21A 108.6 . . ?
N1 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
N1 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C27 C22 C23 119.23(19) . . ?
C27 C22 C21 122.22(17) . . ?
C23 C22 C21 118.43(19) . . ?
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 . . ?
C24 C23 C22 121.2(2) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C25 C26 C27 121.9(2) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C26 C27 C22 118.1(2) . . ?
C26 C27 C28 118.8(2) . . ?
C22 C27 C28 122.98(19) . . ?
C24 C25 C26 119.7(2) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C24 C23 119.7(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C32A C31 C32B 9.5(3) . . ?
C32A C31 N1 115.5(3) . . ?
C32B C31 N1 115.7(3) . . ?
C32A C31 H31A 108.4 . . ?
C32B C31 H31A 100.0 . . ?
N1 C31 H31A 108.4 . . ?
C32A C31 H31B 108.4 . . ?
C32B C31 H31B 116.0 . . ?
N1 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C37A C32A C33A 120.0 . . ?
C37A C32A C31 124.6(3) . . ?
C33A C32A C31 115.3(3) . . ?
C36A C37A C32A 120.0 . . ?
C36A C37A C38A 116.1(3) . . ?
C32A C37A C38A 123.7(3) . . ?
C37A C36A C35A 120.0 . . ?
C37A C36A H36A 120.0 . . ?
C35A C36A H36A 120.0 . . ?
C36A C35A C34A 120.0 . . ?
C36A C35A H35A 120.0 . . ?
C34A C35A H35A 120.0 . . ?
C33A C34A C35A 120.0 . . ?
C33A C34A H34A 120.0 . . ?
C35A C34A H34A 120.0 . . ?
C34A C33A C32A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C33B C32B C37B 120.0 . . ?
C33B C32B C31 115.6(3) . . ?
C37B C32B C31 124.4(3) . . ?
C32B C33B C34B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C34B C33B H33B 120.0 . . ?
C35B C34B C33B 120.0 . . ?
C35B C34B H34B 120.0 . . ?
C33B C34B H34B 120.0 . . ?
C34B C35B C36B 120.0 . . ?
C34B C35B H35B 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C37B C36B C35B 120.0 . . ?
C37B C36B H36B 120.0 . . ?
C35B C36B H36B 120.0 . . ?
C36B C37B C32B 120.0 . . ?
C36B C37B C38B 116.3(3) . . ?
C32B C37B C38B 123.5(3) . . ?
C37B C38B H38D 109.5 . . ?
C37B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C37B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 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 2.3102(8) . ?
Pd1 Cl1 2.3102(8) 2_565 ?
Pd1 Cl2 2.3114(7) 2_565 ?
Pd1 Cl2 2.3114(7) . ?
N1 C12 1.488(2) . ?
N1 C11 1.498(2) . ?
N1 C31 1.535(3) . ?
N1 C21 1.538(2) . ?
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 1.507(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.400(3) . ?
C22 C23 1.401(3) . ?
C28 C27 1.510(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C23 C24 1.380(3) . ?
C23 H23 0.9500 . ?
C26 C25 1.379(3) . ?
C26 C27 1.399(3) . ?
C26 H26 0.9500 . ?
C25 C24 1.377(4) . ?
C25 H25 0.9500 . ?
C24 H24 0.9500 . ?
C31 C32A 1.509(4) . ?
C31 C32B 1.519(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32A C37A 1.390(2) . ?
C32A C33A 1.390(2) . ?
C37A C36A 1.390(2) . ?
C37A C38A 1.519(7) . ?
C36A C35A 1.390(2) . ?
C36A H36A 0.9500 . ?
C35A C34A 1.390(2) . ?
C35A H35A 0.9500 . ?
C34A C33A 1.390(2) . ?
C34A H34A 0.9500 . ?
C33A H33A 0.9500 . ?
C38A H38A 0.9800 . ?
C38A H38B 0.9800 . ?
C38A H38C 0.9800 . ?
C32B C33B 1.397(2) . ?
C32B C37B 1.397(2) . ?
C33B C34B 1.397(2) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.397(2) . ?
C34B H34B 0.9500 . ?
C35B C36B 1.397(2) . ?
C35B H35B 0.9500 . ?
C36B C37B 1.397(2) . ?
C36B H36B 0.9500 . ?
C37B C38B 1.484(7) . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 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
C12 N1 C21 C22 -61.6(2) . . . . ?
C11 N1 C21 C22 59.5(2) . . . . ?
C31 N1 C21 C22 178.78(16) . . . . ?
N1 C21 C22 C27 100.2(2) . . . . ?
N1 C21 C22 C23 -83.7(2) . . . . ?
C27 C22 C23 C24 -2.7(3) . . . . ?
C21 C22 C23 C24 -178.84(18) . . . . ?
C25 C26 C27 C22 -1.0(3) . . . . ?
C25 C26 C27 C28 176.1(2) . . . . ?
C23 C22 C27 C26 2.9(3) . . . . ?
C21 C22 C27 C26 178.88(17) . . . . ?
C23 C22 C27 C28 -174.18(19) . . . . ?
C21 C22 C27 C28 1.8(3) . . . . ?
C27 C26 C25 C24 -1.1(3) . . . . ?
C26 C25 C24 C23 1.3(3) . . . . ?
C22 C23 C24 C25 0.5(3) . . . . ?
C12 N1 C31 C32A 54.3(3) . . . . ?
C11 N1 C31 C32A -66.3(3) . . . . ?
C21 N1 C31 C32A 173.7(2) . . . . ?
C12 N1 C31 C32B 64.8(3) . . . . ?
C11 N1 C31 C32B -55.8(3) . . . . ?
C21 N1 C31 C32B -175.8(2) . . . . ?
C32B C31 C32A C37A -2(3) . . . . ?
N1 C31 C32A C37A 91.7(4) . . . . ?
C32B C31 C32A C33A 174(3) . . . . ?
N1 C31 C32A C33A -92.1(3) . . . . ?
C33A C32A C37A C36A 0.0 . . . . ?
C31 C32A C37A C36A 176.0(5) . . . . ?
C33A C32A C37A C38A -175.5(5) . . . . ?
C31 C32A C37A C38A 0.6(5) . . . . ?
C32A C37A C36A C35A 0.0 . . . . ?
C38A C37A C36A C35A 175.8(4) . . . . ?
C37A C36A C35A C34A 0.0 . . . . ?
C36A C35A C34A C33A 0.0 . . . . ?
C35A C34A C33A C32A 0.0 . . . . ?
C37A C32A C33A C34A 0.0 . . . . ?
C31 C32A C33A C34A -176.4(5) . . . . ?
C32A C31 C32B C33B 180(3) . . . . ?
N1 C31 C32B C33B 89.1(3) . . . . ?
C32A C31 C32B C37B -2(3) . . . . ?
N1 C31 C32B C37B -92.5(4) . . . . ?
C37B C32B C33B C34B 0.0 . . . . ?
C31 C32B C33B C34B 178.4(5) . . . . ?
C32B C33B C34B C35B 0.0 . . . . ?
C33B C34B C35B C36B 0.0 . . . . ?
C34B C35B C36B C37B 0.0 . . . . ?
C35B C36B C37B C32B 0.0 . . . . ?
C35B C36B C37B C38B -175.7(4) . . . . ?
C33B C32B C37B C36B 0.0 . . . . ?
C31 C32B C37B C36B -178.3(5) . . . . ?
C33B C32B C37B C38B 175.4(5) . . . . ?
C31 C32B C37B C38B -2.9(5) . . . . ?
