#------------------------------------------------------------------------------
#$Date: 2018-09-01 02:18:24 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210276 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/83/4308392.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_4308392
loop_
_publ_author_name
'Bacchi, Alessia'
'Bosetti, Elsa'
'Carcelli, Mauro'
'Pelagatti, Paolo'
'Rogolino, Dominga'
'Pelizzi, Giancarlo'
_publ_section_title
;
 "Venetian Blinds" Mechanism of Solvation/Desolvation in Palladium(II)
 Wheel-and-Axle Organic--Inorganic Diols
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              431
_journal_page_last               442
_journal_paper_doi               10.1021/ic048896m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C36 H30 Cl2 N2 O2 Pd'
_chemical_formula_weight         699.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.584(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.736(2)
_cell_length_b                   17.410(2)
_cell_length_c                   16.933(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3150.0(8)
_computing_cell_refinement
;
SAINT: SAX, Area Detector Integration, Siemens Analytical instruments
INC., Madison, Wisconsin, USA. 
;
_computing_data_collection
;
SAINT: SAX, Area Detector Integration, Siemens Analytical instruments
 INC., Madison, Wisconsin, USA. 
;
_computing_data_reduction
;
SAINT: SAX, Area Detector Integration, Siemens Analytical instruments
 INC., Madison, Wisconsin, USA. 
SADABS: Siemens Area Detector Absorption Correction Software, 
Sheldrick G., 1996, University of Goettingen, Germany.
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'PARST -  M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS CCD diffractometer'
_diffrn_measurement_method       'ω scan'
_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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15478
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.625294
_exptl_absorpt_correction_type   'symmetry-related measurements'
_exptl_absorpt_process_details   'as implemented in SAINT+/SADABS package'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         4523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0355P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                2977
_reflns_number_total             4523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048896msi20040811_044420_01.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'mmonoclinic' was replaced with
'monoclinic' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4308392
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Pd Pd 0.47987(3) 0.09345(2) 0.13599(2) 0.04072(13) Uani 1 1 d . . .
Cl1 Cl 0.58151(12) 0.20798(7) 0.13562(13) 0.0978(7) Uani 1 1 d . . .
Cl2 Cl 0.37615(11) -0.02117(7) 0.13655(10) 0.0732(5) Uani 1 1 d . . .
N1 N 0.6437(3) 0.03667(19) 0.1359(2) 0.0362(9) Uani 1 1 d . . .
N2 N 0.3171(3) 0.15014(19) 0.1423(2) 0.0393(9) Uani 1 1 d . . .
O1 O 1.0802(3) -0.01565(19) 0.1086(2) 0.0483(10) Uani 1 1 d . . .
O2 O -0.1256(3) 0.1966(2) 0.1310(3) 0.0632(12) Uani 1 1 d . . .
C1 C 1.0144(4) -0.0651(2) 0.1575(3) 0.0348(11) Uani 1 1 d . . .
C2 C 0.8795(4) -0.0324(2) 0.1473(3) 0.0343(11) Uani 1 1 d . . .
C3 C 0.8352(4) 0.0089(3) 0.0819(3) 0.0411(12) Uani 1 1 d . . .
C4 C 0.7186(4) 0.0417(3) 0.0777(3) 0.0453(13) Uani 1 1 d . . .
C5 C 0.6834(5) -0.0067(3) 0.1980(3) 0.0468(13) Uani 1 1 d . . .
C6 C 0.7999(4) -0.0403(3) 0.2066(3) 0.0490(14) Uani 1 1 d . . .
C7 C 1.0654(4) -0.0582(2) 0.2449(3) 0.0363(11) Uani 1 1 d . . .
C8 C 1.1056(6) 0.0119(3) 0.2759(4) 0.0627(18) Uani 1 1 d . . .
C9 C 1.1443(6) 0.0208(4) 0.3543(5) 0.081(2) Uani 1 1 d . . .
C10 C 1.1427(7) -0.0402(5) 0.4044(4) 0.089(2) Uani 1 1 d . . .
C11 C 1.1044(7) -0.1098(4) 0.3753(4) 0.080(2) Uani 1 1 d . . .
C12 C 1.0669(5) -0.1178(3) 0.2969(3) 0.0549(15) Uani 1 1 d . . .
C13 C 1.0202(4) -0.1483(2) 0.1267(3) 0.0385(12) Uani 1 1 d . . .
C14 C 1.1292(5) -0.1742(3) 0.1000(3) 0.0517(15) Uani 1 1 d . . .
C15 C 1.1416(7) -0.2486(4) 0.0746(4) 0.0670(19) Uani 1 1 d . . .
C16 C 1.0456(6) -0.2997(3) 0.0760(4) 0.0692(17) Uani 1 1 d . . .
C17 C 0.9379(7) -0.2745(4) 0.1036(4) 0.075(2) Uani 1 1 d . . .
C18 C 0.9243(5) -0.1999(3) 0.1280(4) 0.0557(16) Uani 1 1 d . . .
C19 C -0.0441(4) 0.2477(2) 0.1769(3) 0.0413(12) Uani 1 1 d . . .
C20 C 0.0871(4) 0.2168(2) 0.1641(3) 0.0370(11) Uani 1 1 d . . .
C21 C 0.1088(5) 0.1810(3) 0.0950(3) 0.0463(14) Uani 1 1 d . . .
C22 C 0.2232(5) 0.1486(3) 0.0863(3) 0.0473(13) Uani 1 1 d . . .
C23 C 0.2998(5) 0.1880(3) 0.2097(4) 0.0488(14) Uani 1 1 d . . .
C24 C 0.1861(4) 0.2209(3) 0.2212(3) 0.0487(14) Uani 1 1 d . . .
C25 C -0.0639(4) 0.2431(3) 0.2649(3) 0.0475(13) Uani 1 1 d . . .
C26 C -0.0401(5) 0.3037(4) 0.3154(4) 0.0578(15) Uani 1 1 d . . .
C27 C -0.0485(6) 0.2971(5) 0.3958(4) 0.080(2) Uani 1 1 d . . .
C28 C -0.0808(8) 0.2302(6) 0.4263(6) 0.109(3) Uani 1 1 d . . .
C29 C -0.1073(8) 0.1687(5) 0.3782(7) 0.114(4) Uani 1 1 d . . .
C30 C -0.0987(6) 0.1741(4) 0.2971(6) 0.082(2) Uani 1 1 d . . .
C31 C -0.0633(4) 0.3302(3) 0.1444(3) 0.0389(11) Uani 1 1 d . . .
C32 C 0.0320(5) 0.3817(3) 0.1407(4) 0.0582(15) Uani 1 1 d . . .
C33 C 0.0090(7) 0.4555(4) 0.1133(4) 0.0672(18) Uani 1 1 d . . .
C34 C -0.1076(6) 0.4783(4) 0.0883(4) 0.0646(17) Uani 1 1 d . . .
C35 C -0.2040(6) 0.4287(3) 0.0908(4) 0.0635(17) Uani 1 1 d . . .
C36 C -0.1815(5) 0.3552(3) 0.1192(3) 0.0490(14) Uani 1 1 d . . .
H1O H 1.145(4) -0.022(2) 0.120(2) 0.022(14) Uiso 1 1 d . . .
H2O H -0.188(4) 0.205(3) 0.142(3) 0.048(17) Uiso 1 1 d . . .
H3 H 0.878(3) 0.0154(19) 0.041(2) 0.027(11) Uiso 1 1 d . . .
H4 H 0.690(3) 0.0717(18) 0.037(2) 0.021(11) Uiso 1 1 d . . .
H5 H 0.630(5) -0.010(3) 0.232(3) 0.070(17) Uiso 1 1 d . . .
H6 H 0.819(3) -0.069(2) 0.249(2) 0.029(12) Uiso 1 1 d . . .
H8 H 1.107(4) 0.045(2) 0.248(3) 0.030(15) Uiso 1 1 d . . .
H9 H 1.164(5) 0.064(3) 0.369(3) 0.058(18) Uiso 1 1 d . . .
H10 H 1.159(5) -0.038(3) 0.454(3) 0.069(19) Uiso 1 1 d . . .
H11 H 1.098(6) -0.152(3) 0.404(4) 0.11(3) Uiso 1 1 d . . .
H12 H 1.048(4) -0.163(2) 0.281(2) 0.037(14) Uiso 1 1 d . . .
H14 H 1.186(3) -0.147(2) 0.095(2) 0.017(12) Uiso 1 1 d . . .
H15 H 1.202(4) -0.265(3) 0.064(3) 0.043(16) Uiso 1 1 d . . .
H16 H 1.058(4) -0.352(3) 0.058(3) 0.071(16) Uiso 1 1 d . . .
H17 H 0.878(5) -0.302(3) 0.103(3) 0.07(2) Uiso 1 1 d . . .
H18 H 0.862(4) -0.183(3) 0.145(3) 0.060(18) Uiso 1 1 d . . .
H21 H 0.054(3) 0.1749(19) 0.060(2) 0.016(11) Uiso 1 1 d . . .
H22 H 0.238(4) 0.124(2) 0.042(2) 0.041(13) Uiso 1 1 d . . .
H23 H 0.361(5) 0.188(3) 0.242(3) 0.071(19) Uiso 1 1 d . . .
H24 H 0.184(4) 0.245(2) 0.266(3) 0.039(14) Uiso 1 1 d . . .
H26 H -0.019(4) 0.348(2) 0.296(2) 0.040(14) Uiso 1 1 d . . .
H27 H -0.027(4) 0.336(3) 0.429(3) 0.056(18) Uiso 1 1 d . . .
H28 H -0.080(6) 0.224(3) 0.478(4) 0.11(3) Uiso 1 1 d . . .
H29 H -0.120(5) 0.126(3) 0.397(3) 0.08(2) Uiso 1 1 d . . .
H30 H -0.118(4) 0.136(3) 0.264(3) 0.056(18) Uiso 1 1 d . . .
H32 H 0.107(4) 0.374(2) 0.167(2) 0.033(13) Uiso 1 1 d . . .
H33 H 0.065(5) 0.488(3) 0.115(3) 0.08(2) Uiso 1 1 d . . .
H34 H -0.124(4) 0.524(3) 0.072(3) 0.051(15) Uiso 1 1 d . . .
H35 H -0.281(5) 0.444(3) 0.075(3) 0.067(17) Uiso 1 1 d . . .
H36 H -0.240(4) 0.324(2) 0.116(3) 0.045(15) Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 '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
N1 Pd N2 177.03(16) . . ?
N1 Pd Cl1 90.63(10) . . ?
N2 Pd Cl1 89.40(10) . . ?
N1 Pd Cl2 89.85(10) . . ?
N2 Pd Cl2 90.12(10) . . ?
Cl1 Pd Cl2 179.51(5) . . ?
C5 N1 C4 116.9(4) . . ?
C5 N1 Pd 119.3(3) . . ?
C4 N1 Pd 123.8(3) . . ?
C22 N2 C23 117.5(4) . . ?
C22 N2 Pd 124.0(3) . . ?
C23 N2 Pd 118.4(3) . . ?
O1 C1 C7 111.2(4) . . ?
O1 C1 C13 109.4(3) . . ?
C7 C1 C13 112.2(3) . . ?
O1 C1 C2 102.9(3) . . ?
C7 C1 C2 108.7(3) . . ?
C13 C1 C2 112.1(3) . . ?
C3 C2 C6 116.7(4) . . ?
C3 C2 C1 122.1(4) . . ?
C6 C2 C1 121.1(4) . . ?
C2 C3 C4 120.4(4) . . ?
N1 C4 C3 123.1(5) . . ?
N1 C5 C6 122.9(4) . . ?
C5 C6 C2 119.9(5) . . ?
C12 C7 C8 116.4(5) . . ?
C12 C7 C1 123.1(4) . . ?
C8 C7 C1 120.4(5) . . ?
C9 C8 C7 121.7(6) . . ?
C10 C9 C8 119.9(7) . . ?
C11 C10 C9 119.6(7) . . ?
C12 C11 C10 119.8(7) . . ?
C11 C12 C7 122.6(6) . . ?
C18 C13 C14 117.2(5) . . ?
C18 C13 C1 123.7(4) . . ?
C14 C13 C1 119.0(4) . . ?
C13 C14 C15 121.7(6) . . ?
C16 C15 C14 120.8(6) . . ?
C17 C16 C15 117.7(6) . . ?
C16 C17 C18 121.7(6) . . ?
C13 C18 C17 120.9(6) . . ?
O2 C19 C25 111.3(4) . . ?
O2 C19 C20 103.1(4) . . ?
C25 C19 C20 109.5(4) . . ?
O2 C19 C31 109.5(4) . . ?
C25 C19 C31 111.7(3) . . ?
C20 C19 C31 111.5(3) . . ?
C21 C20 C24 116.3(4) . . ?
C21 C20 C19 120.9(4) . . ?
C24 C20 C19 122.7(4) . . ?
C20 C21 C22 120.6(5) . . ?
N2 C22 C21 123.1(5) . . ?
N2 C23 C24 121.4(5) . . ?
C20 C24 C23 121.1(5) . . ?
C26 C25 C30 117.7(6) . . ?
C26 C25 C19 122.3(4) . . ?
C30 C25 C19 119.9(5) . . ?
C25 C26 C27 121.8(6) . . ?
C28 C27 C26 120.0(8) . . ?
C27 C28 C29 120.2(8) . . ?
C28 C29 C30 120.6(8) . . ?
C25 C30 C29 119.7(8) . . ?
C32 C31 C36 116.9(5) . . ?
C32 C31 C19 123.5(4) . . ?
C36 C31 C19 119.5(4) . . ?
C31 C32 C33 121.1(6) . . ?
C34 C33 C32 120.8(6) . . ?
C33 C34 C35 119.6(6) . . ?
C34 C35 C36 119.7(6) . . ?
C31 C36 C35 121.8(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
Pd N1 2.018(3) . ?
Pd N2 2.019(3) . ?
Pd Cl1 2.2733(13) . ?
Pd Cl2 2.2856(13) . ?
N1 C5 1.330(6) . ?
N1 C4 1.334(5) . ?
N2 C22 1.315(6) . ?
N2 C23 1.347(6) . ?
O1 C1 1.429(5) . ?
O2 C19 1.423(5) . ?
C1 C7 1.532(6) . ?
C1 C13 1.543(6) . ?
C1 C2 1.551(5) . ?
C2 C3 1.367(6) . ?
C2 C6 1.386(6) . ?
C3 C4 1.371(6) . ?
C5 C6 1.376(6) . ?
C7 C12 1.360(6) . ?
C7 C8 1.380(7) . ?
C8 C9 1.362(9) . ?
C9 C10 1.360(9) . ?
C10 C11 1.356(9) . ?
C11 C12 1.357(8) . ?
C13 C18 1.367(6) . ?
C13 C14 1.371(6) . ?
C14 C15 1.374(7) . ?
C15 C16 1.363(8) . ?
C16 C17 1.361(8) . ?
C17 C18 1.375(8) . ?
C19 C25 1.527(7) . ?
C19 C20 1.543(6) . ?
C19 C31 1.546(6) . ?
C20 C21 1.365(6) . ?
C20 C24 1.368(6) . ?
C21 C22 1.373(6) . ?
C23 C24 1.379(7) . ?
C25 C26 1.367(7) . ?
C25 C30 1.385(7) . ?
C26 C27 1.377(8) . ?
C27 C28 1.334(10) . ?
C28 C29 1.359(11) . ?
C29 C30 1.389(11) . ?
C31 C32 1.367(6) . ?
C31 C36 1.370(6) . ?
C32 C33 1.379(8) . ?
C33 C34 1.342(8) . ?
C34 C35 1.352(8) . ?
C35 C36 1.381(7) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O Cl2 0.71(4) 2.47(4) 3.168(4) 166(4) 1_655
O2 H2O Cl1 0.73(4) 2.46(5) 3.159(4) 160(5) 1_455
C12 H12 Cl1 0.85(4) 3.06(4) 3.660(6) 130(3) 2_645
C26 H26 Cl2 0.87(4) 2.92(4) 3.574(6) 133(3) 2
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
C4 N1 N2 C22 54.4(5) . . . . ?
O1 C1 C2 C3 24.3(6) . . . . ?
O2 C19 C20 C21 30.3(6) . . . . ?
O1 C1 C19 O2 109.6(4) . . . . ?
C3 C2 C1 O1 24.3(6) . . . . ?
C8 C7 C1 O1 36.1(5) . . . . ?
C14 C13 C1 O1 39.2(6) . . . . ?
C21 C20 C19 O2 30.3(6) . . . . ?
C36 C31 C19 O2 39.1(6) . . . . ?
C30 C25 C19 O2 32.4(6) . . . . ?
