Supplementary Material for CrystEngComm
This Journal is © The Royal Society of Chemistry 2003

data_global

# 1.SUBMISSION DETAILS
_publ_contact_author_name        'Neve, Francesco'
_publ_contact_author_address     
;
Dipartimento di Chimica
Universit\'a della Calabria
87030 Arcavacata di Rende (CS)
Italy
;
_publ_contact_author_email       f.neve@unical.it
_publ_contact_author_fax         0984492044
_publ_contact_author_phone       0984492060

_publ_requested_journal          CrystEngComm
_publ_requested_coeditor_name    ?
_publ_contact_letter             
;
?
;
_publ_requested_category         ?

# 2.PROCESSING SUMMARY

_journal_coden_Cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?

# 3.TITLE AND AUTHOR LIST
_publ_section_title              
;
N,N'-Dodecamethylene-bis(pyridinium) goes lamellar.
Role of C-H...I, C-H...M, and I...I interactions in
the crystal structure of its hexaiododipalladate(II)
derivative
;

_publ_section_title_footnote     
;
?
;

loop_
_publ_author_name
_publ_author_address
'Francesco Neve'
;
Dipartimento di Chimica
Universit\'a della Calabria
I-87030 Arcavacata di Rende (CS)
Italy
;
'Alessandra Crispini'
;
Dipartimento di Chimica
Universit\'a della Calabria
I-87030 Arcavacata di Rende (CS)
Italy
;

data_copmound
_database_code_CSD               211293

# 4.CHEMICAL INFORMATION
_chemical_formula_moiety         'C22 H34 I6 N2 Pd2'
_chemical_formula_sum            'C22 H34 I6 N2 Pd2'
_chemical_formula_weight         1300.71
_chemical_name_systematic        
;
?
;

# 5.UNIT CELL INFORMATION
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5038(10)
_cell_length_b                   8.8887(10)
_cell_length_c                   11.5366(13)
_cell_angle_alpha                93.953(2)
_cell_angle_beta                 107.892(2)
_cell_angle_gamma                92.848(2)
_cell_volume                     825.57(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)

# 6.CRYSTAL INFORMATION
_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    2.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             590
_exptl_absorpt_coefficient_mu    6.712
_exptl_absorpt_correction_type   'psi scan'
_exptl_absorpt_correction_T_min  0.1695
_exptl_absorpt_correction_T_max  0.6508

# 7.DATA COLLECTION INFORMATION
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Bruker Smart Apex'
_diffrn_measurement_method       \o/2\q

_diffrn_reflns_number            8322
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.957
_reflns_number_total             3935
_reflns_number_gt                2879
_reflns_threshold_expression     >2sigma(I)

# 8.COMPUTER PROGRAMS USED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

# 9.REFINEMENT INFORMATION
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w==1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3935
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1120
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_restrained_S_all      0.942
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.886
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.184

#10.ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.05322(4) 0.62007(4) 0.65170(3) 0.04968(14) Uani 1 1 d . . .
I1 I 0.09043(4) 0.64669(4) 0.43817(3) 0.06218(14) Uani 1 1 d . . .
I2 I 0.19970(5) 0.88782(5) 0.72800(4) 0.08162(16) Uani 1 1 d . . .
I3 I -0.00164(5) 0.57608(5) 0.85524(3) 0.07126(15) Uani 1 1 d . . .
N1 N 0.6834(5) 0.8759(5) 0.7095(3) 0.0533(9) Uani 1 1 d . . .
C2 C 0.7731(7) 1.0016(7) 0.7086(5) 0.0686(14) Uani 1 1 d . . .
H2 H 0.7975 1.0225 0.6379 0.082 Uiso 1 1 calc R . .
C3 C 0.8304(8) 1.1014(7) 0.8113(5) 0.0823(17) Uani 1 1 d . . .
H3 H 0.8918 1.1902 0.8092 0.099 Uiso 1 1 calc R . .
C4 C 0.7979(7) 1.0714(8) 0.9158(5) 0.0768(15) Uani 1 1 d . . .
H4 H 0.8359 1.1382 0.9859 0.092 Uiso 1 1 calc R . .
C5 C 0.7094(8) 0.9423(8) 0.9145(5) 0.0812(17) Uani 1 1 d . . .
H5 H 0.6861 0.9187 0.9851 0.097 Uiso 1 1 calc R . .
C6 C 0.6531(8) 0.8455(7) 0.8126(5) 0.0765(15) Uani 1 1 d . . .
H6 H 0.5922 0.7563 0.8144 0.092 Uiso 1 1 calc R . .
C7 C 0.6195(7) 0.7620(6) 0.6014(4) 0.0647(13) Uani 1 1 d . . .
H7A H 0.6741 0.6697 0.6220 0.078 Uiso 1 1 calc R . .
H7B H 0.5023 0.7391 0.5883 0.078 Uiso 1 1 calc R . .
C8 C 0.6400(6) 0.8032(6) 0.4835(5) 0.0591(12) Uani 1 1 d . . .
H8A H 0.7566 0.8249 0.4936 0.071 Uiso 1 1 calc R . .
H8B H 0.5829 0.8932 0.4590 0.071 Uiso 1 1 calc R . .
C9 C 0.5688(6) 0.6726(6) 0.3850(4) 0.0620(12) Uani 1 1 d . . .
H9A H 0.6240 0.5828 0.4129 0.074 Uiso 1 1 calc R . .
H9B H 0.4523 0.6530 0.3763 0.074 Uiso 1 1 calc R . .
C10 C 0.5844(6) 0.6967(6) 0.2603(4) 0.0583(12) Uani 1 1 d . . .
H10A H 0.6999 0.7215 0.2683 0.070 Uiso 1 1 calc R . .
H10B H 0.5225 0.7817 0.2286 0.070 Uiso 1 1 calc R . .
C11 C 0.5201(6) 0.5571(6) 0.1699(4) 0.0604(12) Uani 1 1 d . . .
H11A H 0.5838 0.4733 0.2021 0.073 Uiso 1 1 calc R . .
H11B H 0.4059 0.5313 0.1650 0.073 Uiso 1 1 calc R . .
C12 C 0.5274(6) 0.5733(6) 0.0417(4) 0.0600(12) Uani 1 1 d . . .
H12A H 0.6400 0.6052 0.0462 0.072 Uiso 1 1 calc R . .
H12B H 0.4569 0.6516 0.0063 0.072 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0595(2) 0.0504(3) 0.0410(2) 0.00042(16) 0.02059(15) -0.00633(17)
I1 0.0853(2) 0.0575(3) 0.0481(2) 0.00001(16) 0.03198(16) -0.01916(18)
I2 0.1107(3) 0.0610(3) 0.0719(3) -0.0134(2) 0.0356(2) -0.0252(2)
I3 0.0942(3) 0.0793(3) 0.0436(2) -0.00209(17) 0.03118(17) -0.0151(2)
N1 0.066(2) 0.043(2) 0.046(2) 0.0004(17) 0.0125(16) -0.0050(17)
C2 0.085(3) 0.066(4) 0.053(3) 0.004(3) 0.023(2) -0.017(3)
C3 0.113(4) 0.056(4) 0.068(3) -0.021(3) 0.026(3) -0.031(3)
C4 0.100(4) 0.071(4) 0.055(3) -0.011(3) 0.023(3) -0.006(3)
C5 0.120(5) 0.070(4) 0.053(3) -0.002(3) 0.030(3) -0.004(4)
C6 0.110(4) 0.061(4) 0.060(3) 0.001(3) 0.033(3) -0.018(3)
C7 0.081(3) 0.056(3) 0.053(3) -0.004(2) 0.020(2) -0.010(3)
C8 0.073(3) 0.047(3) 0.053(3) -0.002(2) 0.016(2) -0.002(2)
C9 0.072(3) 0.057(3) 0.052(3) -0.007(2) 0.017(2) -0.010(2)
C10 0.068(3) 0.051(3) 0.051(3) -0.005(2) 0.014(2) -0.002(2)
C11 0.070(3) 0.055(3) 0.053(3) -0.003(2) 0.019(2) -0.008(2)
C12 0.070(3) 0.057(3) 0.050(3) -0.004(2) 0.017(2) -0.004(2)

#11.MOLECULAR GEOMETRY
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 I3 2.5819(5) . ?
Pd1 I2 2.5949(5) . ?
Pd1 I1 2.6031(5) . ?
Pd1 I1 2.6047(5) 2_566 ?
I1 Pd1 2.6047(5) 2_566 ?
N1 C2 1.324(7) . ?
N1 C6 1.334(6) . ?
N1 C7 1.493(6) . ?
C2 C3 1.373(8) . ?
C3 C4 1.358(8) . ?
C4 C5 1.337(8) . ?
C5 C6 1.351(8) . ?
C7 C8 1.491(7) . ?
C8 C9 1.527(7) . ?
C9 C10 1.513(7) . ?
C10 C11 1.526(7) . ?
C11 C12 1.516(7) . ?
C12 C12 1.527(10) 2_665 ?

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
I3 Pd1 I2 94.273(16) . . ?
I3 Pd1 I1 175.373(17) . . ?
I2 Pd1 I1 90.139(15) . . ?
I3 Pd1 I1 89.386(15) . 2_566 ?
I2 Pd1 I1 176.341(16) . 2_566 ?
I1 Pd1 I1 86.204(14) . 2_566 ?
Pd1 I1 Pd1 93.796(14) . 2_566 ?
C2 N1 C6 119.0(5) . . ?
C2 N1 C7 123.1(4) . . ?
C6 N1 C7 117.8(4) . . ?
N1 C2 C3 120.6(5) . . ?
C4 C3 C2 120.4(6) . . ?
C5 C4 C3 117.7(6) . . ?
C4 C5 C6 121.2(6) . . ?
N1 C6 C5 121.1(5) . . ?
C8 C7 N1 117.4(4) . . ?
C7 C8 C9 109.6(4) . . ?
C10 C9 C8 115.7(4) . . ?
C9 C10 C11 112.1(4) . . ?
C12 C11 C10 115.4(4) . . ?
C11 C12 C12 112.8(5) . 2_665 ?
#          END of CIF