#------------------------------------------------------------------------------
#$Date: 2018-09-01 02:18:24 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210276 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/83/4308395.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_4308395
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            'C44 H46 Cl2 N2 O4 Pd'
_chemical_formula_weight         844.13
_space_group_IT_number           2
_symmetry_cell_setting           tericlinic
_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                100.534(2)
_cell_angle_beta                 96.889(2)
_cell_angle_gamma                98.944(2)
_cell_formula_units_Z            1
_cell_length_a                   7.9754(7)
_cell_length_b                   11.2200(10)
_cell_length_c                   11.5430(10)
_cell_measurement_temperature    293(2)
_cell_volume                     991.38(15)
_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 0.898
_diffrn_measured_fraction_theta_max 0.898
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13589
_diffrn_reflns_theta_full        30.19
_diffrn_reflns_theta_max         30.19
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.774150
_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    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0250
_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)+(0.0413P)²+0.2164P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                5009
_reflns_number_total             5280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048896msi20040811_044420_04.cif
_cod_data_source_block           5
_cod_database_code               4308395
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 0.0000 0.0000 0.03329(6) Uani 1 2 d S . .
Cl1 Cl 0.11693(5) -0.03146(4) -0.17301(4) 0.04743(9) Uani 1 1 d . . .
N1 N -0.15586(15) 0.10095(11) -0.07492(11) 0.0348(2) Uani 1 1 d . . .
O1 O -0.63901(15) 0.30133(12) -0.18098(11) 0.0450(3) Uani 1 1 d . . .
C1 C -0.49998(18) 0.30022(13) -0.24795(12) 0.0348(3) Uani 1 1 d . . .
C2 C -0.37496(18) 0.23345(13) -0.18379(12) 0.0336(3) Uani 1 1 d . . .
C3 C -0.43889(19) 0.13791(15) -0.13091(15) 0.0420(3) Uani 1 1 d . . .
C4 C -0.32619(19) 0.07548(15) -0.07684(15) 0.0424(3) Uani 1 1 d . . .
C5 C -0.09368(19) 0.19212(14) -0.12743(14) 0.0388(3) Uani 1 1 d . . .
C6 C -0.19890(19) 0.25991(14) -0.18116(14) 0.0390(3) Uani 1 1 d . . .
C7 C -0.41782(18) 0.43443(13) -0.24395(12) 0.0346(3) Uani 1 1 d . . .
C8 C -0.3739(2) 0.51370(16) -0.13264(14) 0.0463(3) Uani 1 1 d . . .
C9 C -0.3060(3) 0.63695(18) -0.12111(17) 0.0552(4) Uani 1 1 d . . .
C10 C -0.2791(3) 0.68429(16) -0.22141(19) 0.0542(4) Uani 1 1 d . . .
C11 C -0.3236(3) 0.60752(16) -0.33219(17) 0.0509(4) Uani 1 1 d . . .
C12 C -0.3932(2) 0.48350(14) -0.34405(14) 0.0419(3) Uani 1 1 d . . .
C13 C -0.5609(2) 0.22354(13) -0.37484(14) 0.0404(3) Uani 1 1 d . . .
C14 C -0.7350(3) 0.17877(19) -0.41438(19) 0.0575(5) Uani 1 1 d . . .
C15 C -0.7903(4) 0.1101(2) -0.5303(2) 0.0751(7) Uani 1 1 d . . .
C16 C -0.6747(4) 0.08441(19) -0.6049(2) 0.0735(7) Uani 1 1 d . . .
C17 C -0.5022(4) 0.12618(19) -0.56689(18) 0.0658(6) Uani 1 1 d . . .
C18 C -0.4450(3) 0.19572(16) -0.45169(16) 0.0501(4) Uani 1 1 d . . .
O100 O -0.8668(2) 0.44799(15) -0.24411(14) 0.0635(4) Uani 1 1 d . . .
C100 C -0.7807(5) 0.6577(3) -0.2033(5) 0.1369(19) Uani 1 1 d . . .
H10I H -0.8239 0.7318 -0.1737 0.164 Uiso 1 1 calc R . .
H10J H -0.6569 0.6731 -0.1805 0.164 Uiso 1 1 calc R . .
C101 C -0.8625(5) 0.5523(4) -0.1567(2) 0.1052(12) Uani 1 1 d . . .
H10K H -0.7960 0.5468 -0.0824 0.126 Uiso 1 1 calc R . .
H10L H -0.9778 0.5614 -0.1427 0.126 Uiso 1 1 calc R . .
C102 C -0.8281(5) 0.6191(3) -0.3327(4) 0.1087(12) Uani 1 1 d . . .
H10M H -0.7300 0.6387 -0.3725 0.130 Uiso 1 1 calc R . .
H10N H -0.9192 0.6593 -0.3614 0.130 Uiso 1 1 calc R . .
C103 C -0.8868(4) 0.4848(3) -0.3537(2) 0.0781(7) Uani 1 1 d . . .
H10O H -1.0065 0.4637 -0.3901 0.094 Uiso 1 1 calc R . .
H10P H -0.8197 0.4429 -0.4073 0.094 Uiso 1 1 calc R . .
H11 H 0.028(3) 0.2050(17) -0.1277(16) 0.040(5) Uiso 1 1 d . . .
H7 H -0.423(3) 0.4339(19) -0.4184(19) 0.048(5) Uiso 1 1 d . . .
H10 H -0.151(3) 0.3198(18) -0.2149(18) 0.045(5) Uiso 1 1 d . . .
H12 H -0.368(3) 0.013(2) -0.0427(19) 0.052(5) Uiso 1 1 d . . .
H8 H -0.556(3) 0.114(2) -0.1343(19) 0.055(6) Uiso 1 1 d . . .
H14 H -0.812(3) 0.204(2) -0.365(2) 0.064(7) Uiso 1 1 d . . .
H6 H -0.311(3) 0.640(2) -0.399(2) 0.065(7) Uiso 1 1 d . . .
H5 H -0.232(3) 0.766(2) -0.214(2) 0.063(6) Uiso 1 1 d . . .
H3 H -0.388(3) 0.480(2) -0.066(2) 0.058(6) Uiso 1 1 d . . .
H1O H -0.696(3) 0.344(2) -0.204(2) 0.055(6) Uiso 1 1 d . . .
H18 H -0.327(3) 0.2224(19) -0.4288(18) 0.049(5) Uiso 1 1 d . . .
H4 H -0.281(3) 0.685(2) -0.049(2) 0.073(7) Uiso 1 1 d . . .
H17 H -0.419(3) 0.109(2) -0.615(2) 0.066(7) Uiso 1 1 d . . .
H15 H -0.903(4) 0.081(3) -0.554(3) 0.103(10) Uiso 1 1 d . . .
H16 H -0.730(4) 0.035(3) -0.680(3) 0.082(8) 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 Pd1 N1 180.00(8) 2 . ?
N1 Pd1 Cl1 91.14(4) 2 . ?
N1 Pd1 Cl1 88.86(4) . . ?
N1 Pd1 Cl1 88.86(4) 2 2 ?
N1 Pd1 Cl1 91.14(4) . 2 ?
Cl1 Pd1 Cl1 180.00(3) . 2 ?
C4 N1 C5 117.81(12) . . ?
C4 N1 Pd1 120.58(9) . . ?
C5 N1 Pd1 121.57(10) . . ?
O1 C1 C7 108.12(12) . . ?
O1 C1 C13 110.76(12) . . ?
C7 C1 C13 113.79(11) . . ?
O1 C1 C2 104.89(11) . . ?
C7 C1 C2 111.34(11) . . ?
C13 C1 C2 107.60(12) . . ?
C6 C2 C3 117.46(12) . . ?
C6 C2 C1 122.81(12) . . ?
C3 C2 C1 119.64(12) . . ?
C4 C3 C2 119.38(14) . . ?
N1 C4 C3 123.00(13) . . ?
N1 C5 C6 122.19(13) . . ?
C5 C6 C2 120.13(13) . . ?
C12 C7 C8 117.92(14) . . ?
C12 C7 C1 124.39(13) . . ?
C8 C7 C1 117.59(13) . . ?
C9 C8 C7 121.49(16) . . ?
C8 C9 C10 120.06(17) . . ?
C11 C10 C9 119.20(17) . . ?
C10 C11 C12 120.83(17) . . ?
C7 C12 C11 120.49(15) . . ?
C18 C13 C14 118.54(17) . . ?
C18 C13 C1 121.26(15) . . ?
C14 C13 C1 120.19(16) . . ?
C13 C14 C15 120.1(2) . . ?
C16 C15 C14 120.6(2) . . ?
C15 C16 C17 120.2(2) . . ?
C16 C17 C18 120.0(2) . . ?
C13 C18 C17 120.6(2) . . ?
C101 O100 C103 106.5(2) . . ?
C102 C100 C101 104.2(3) . . ?
O100 C101 C100 105.8(3) . . ?
C100 C102 C103 104.7(3) . . ?
O100 C103 C102 108.5(3) . . ?
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 N1 2.0283(11) 2 ?
Pd1 N1 2.0283(11) . ?
Pd1 Cl1 2.2964(4) . ?
Pd1 Cl1 2.2964(4) 2 ?
N1 C4 1.3406(19) . ?
N1 C5 1.3419(18) . ?
O1 C1 1.4260(18) . ?
C1 C7 1.536(2) . ?
C1 C13 1.536(2) . ?
C1 C2 1.5369(18) . ?
C2 C6 1.385(2) . ?
C2 C3 1.388(2) . ?
C3 C4 1.382(2) . ?
C5 C6 1.3833(19) . ?
C7 C12 1.389(2) . ?
C7 C8 1.394(2) . ?
C8 C9 1.380(3) . ?
C9 C10 1.385(3) . ?
C10 C11 1.377(3) . ?
C11 C12 1.391(2) . ?
C13 C18 1.387(3) . ?
C13 C14 1.392(3) . ?
C14 C15 1.398(3) . ?
C15 C16 1.363(4) . ?
C16 C17 1.373(4) . ?
C17 C18 1.396(3) . ?
O100 C101 1.392(3) . ?
O100 C103 1.400(3) . ?
C100 C102 1.463(6) . ?
C100 C101 1.479(6) . ?
C102 C103 1.472(4) . ?
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 O100 0.77(2) 1.99(2) 2.7548(18) 171(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 N1 C5 -2.3(2) . . 2 2 ?
O1 C1 C2 C3 34.49(18) . . . . ?
O1 C1 C1 O1 180.0 . . 2 2 ?
C3 C2 C1 O1 34.49(18) . . . . ?
C8 C7 C1 O1 50.51(17) . . . . ?
C14 C13 C1 O1 7.42(19) . . . . ?
