# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_interlock-propanol
_database_code_depnum_ccdc_archive 'CCDC 1405236'
_audit_update_record             
;
2015-06-06 deposited with the CCDC.
2017-04-20 downloaded from the CCDC.
;

_audit_creation_date             2015-06-06T13:29:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C100 H76 N8 O20 Pd2)'
_chemical_formula_sum            'C200 H152 N16 O40 Pd4'
_chemical_formula_weight         3845.17

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'
_space_group_IT_number           126
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   18.9341(8)
_cell_length_b                   18.9341(8)
_cell_length_c                   38.159(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13679.9(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    4123
_cell_measurement_theta_min      1.521
_cell_measurement_theta_max      24.736

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_F_000             3935
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_probe          X-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_number            65225
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.521
_diffrn_reflns_theta_max         24.736
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.998
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_total             5869
_reflns_number_gt                3416
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1474P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5869
_refine_ls_number_parameters     306
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0741
_refine_ls_wR_factor_ref         0.2323
_refine_ls_wR_factor_gt          0.2021
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.349
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.094

#----------------------------------------------------------------------------#
#                   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 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.999 1.007 '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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0875(4) 0.0906(4) 0.35357(18) 0.126(3) Uani 1 1 d . . . . .
C2 C -0.0546(3) 0.1075(3) 0.31963(15) 0.0978(18) Uani 1 1 d . . . . .
C3 C 0.0146(2) 0.1309(2) 0.31636(13) 0.0729(13) Uani 1 1 d . . . . .
H3 H 0.0439 0.1319 0.3366 0.088 Uiso 1 1 calc R U . . .
C4 C 0.0415(2) 0.1521(2) 0.28538(12) 0.0654(12) Uani 1 1 d . . . . .
H4 H 0.0878 0.1712 0.2843 0.078 Uiso 1 1 calc R U . . .
C5 C 0.0018(3) 0.1463(2) 0.25536(12) 0.0687(12) Uani 1 1 d . . . . .
C6 C -0.0650(3) 0.1203(4) 0.25632(15) 0.118(2) Uani 1 1 d . . . . .
H6 H -0.0915 0.1147 0.2354 0.141 Uiso 1 1 calc R U . . .
C7 C -0.0945(3) 0.1017(4) 0.28905(17) 0.126(2) Uani 1 1 d . . . . .
C14 C -0.0053(3) 0.1642(3) 0.19364(14) 0.0858(15) Uani 1 1 d . . . . .
H14A H -0.0493 0.1922 0.1958 0.103 Uiso 1 1 calc R U . . .
H14B H -0.0186 0.1145 0.1891 0.103 Uiso 1 1 calc R U . . .
C15 C 0.1099(3) 0.0436(3) 0.49103(16) 0.0968(17) Uani 1 1 d . . . . .
H15A H 0.1465 0.0465 0.4726 0.116 Uiso 1 1 calc R U . . .
H15B H 0.0929 -0.0057 0.4924 0.116 Uiso 1 1 calc R U . . .
C16 C 0.1400(3) 0.0663(3) 0.52578(15) 0.0815(14) Uani 1 1 d . . . . .
C17 C 0.1347(3) 0.0274(3) 0.5548(2) 0.1023(19) Uani 1 1 d . . . . .
H17 H 0.1128 -0.0178 0.5542 0.123 Uiso 1 1 calc R U . . .
C18 C 0.1622(3) 0.0544(4) 0.58681(18) 0.119(2) Uani 1 1 d . . . . .
H18 H 0.1588 0.0276 0.6078 0.143 Uiso 1 1 calc R U . . .
C19 C 0.1928(3) 0.1178(3) 0.58694(15) 0.0896(16) Uani 1 1 d . . . . .
H19 H 0.2105 0.1359 0.6084 0.108 Uiso 1 1 calc R U . . .
C20 C 0.1721(3) 0.1319(3) 0.52886(14) 0.0814(14) Uani 1 1 d . . . . .
H20 H 0.1746 0.1607 0.5085 0.098 Uiso 1 1 calc R U . . .
C21 C 0.0373(3) 0.1916(2) 0.16373(12) 0.0700(12) Uani 1 1 d . . . . .
C22 C 0.0050(3) 0.1996(2) 0.13155(14) 0.0733(13) Uani 1 1 d . . . . .
H22 H -0.0433 0.1877 0.1286 0.088 Uiso 1 1 calc R U . . .
C23 C 0.0428(3) 0.2247(3) 0.10429(14) 0.0796(14) Uani 1 1 d . . . . .
H23 H 0.0212 0.2304 0.082 0.095 Uiso 1 1 calc R U . . .
C24 C 0.1121(3) 0.2417(2) 0.10889(13) 0.0736(13) Uani 1 1 d . . . . .
H24 H 0.1379 0.2612 0.0898 0.088 Uiso 1 1 calc R U . . .
C25 C 0.1078(2) 0.2061(2) 0.16641(11) 0.0584(11) Uani 1 1 d . . . . .
H25 H 0.1311 0.1976 0.188 0.07 Uiso 1 1 calc R U . . .
N1 N 0.1995(2) 0.1567(2) 0.55807(10) 0.0707(10) Uani 1 1 d . . . . .
N2 N 0.1448(2) 0.2318(2) 0.13965(9) 0.0645(10) Uani 1 1 d . . . . .
O1 O 0.0542(2) 0.0889(2) 0.48325(11) 0.0963(11) Uani 1 1 d . . . . .
O3 O -0.1491(3) 0.0734(4) 0.35529(12) 0.164(2) Uani 1 1 d . . . . .
O4 O -0.1615(3) 0.0811(5) 0.28885(14) 0.202(3) Uani 1 1 d . . . . .
H4A H -0.1825 0.0984 0.3062 0.303 Uiso 1 1 calc R U . . .
O5 O 0.03368(15) 0.16858(15) 0.22537(8) 0.0713(8) Uani 1 1 d . . . . .
Pd1 Pd 0.25 0.25 0.55898(2) 0.0689(3) Uani 1 4 d S T P . .
Pd2 Pd 0.25 0.25 0.14197(2) 0.0602(3) Uani 1 4 d S T P . .
C8 C -0.0453(4) 0.0927(5) 0.38792(19) 0.103(2) Uani 1 1 d . . . . .
C9 C 0.0075(4) 0.0422(5) 0.39278(19) 0.0964(18) Uani 1 1 d . . . . .
C10 C 0.0427(3) 0.0396(4) 0.42546(18) 0.103(2) Uani 1 1 d . . . . .
H10 H 0.0787 0.0057 0.4297 0.124 Uiso 1 1 calc R U . . .
C11 C 0.0240(3) 0.0863(4) 0.45035(19) 0.0914(17) Uani 1 1 d . . . . .
C12 C -0.0285(4) 0.1352(4) 0.44407(19) 0.1021(18) Uani 1 1 d . . . . .
H12 H -0.0403 0.1679 0.462 0.123 Uiso 1 1 calc R U . . .
C13 C -0.0644(5) 0.1385(5) 0.4130(2) 0.117(2) Uani 1 1 d . . . . .
O2A O -0.1131(4) 0.1832(4) 0.4058(2) 0.118(3) Uani 0.556(10) 1 d . . P A 1
H2A H -0.1269 0.177 0.3851 0.177 Uiso 0.556(10) 1 calc R U P A 1
O2B O 0.0175(6) -0.0010(5) 0.3707(4) 0.121(4) Uani 0.444(10) 1 d . . P A 2
H2B H 0.0117 0.0173 0.3508 0.182 Uiso 0.444(10) 1 calc R U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 O3 1.212(7) . ?
C1 C2 1.472(7) . ?
C1 C8 1.536(9) . ?
C2 C3 1.389(6) . ?
C2 C7 1.394(7) . ?
C3 C4 1.348(6) . ?
C4 C5 1.374(6) . ?
C5 C6 1.358(7) . ?
C5 O5 1.361(5) . ?
C6 C7 1.412(7) . ?
C7 O4 1.328(7) . ?
C14 O5 1.421(5) . ?
C14 C21 1.491(7) . ?
C15 O1 1.391(7) . ?
C15 C16 1.506(7) . ?
C16 C17 1.336(8) . ?
C16 C20 1.387(7) . ?
C17 C18 1.422(8) . ?
C18 C19 1.333(7) . ?
C19 N1 1.331(6) . ?
C20 N1 1.316(6) . ?
C21 C25 1.366(6) . ?
C21 C22 1.380(6) . ?
C22 C23 1.349(7) . ?
C23 C24 1.363(7) . ?
C24 N2 1.340(6) . ?
C25 N2 1.331(5) . ?
N1 Pd1 2.009(4) . ?
N2 Pd2 2.023(4) . ?
O1 C11 1.381(7) . ?
Pd1 N1 2.009(4) 2 ?
Pd1 N1 2.009(4) 4 ?
Pd1 N1 2.009(4) 3 ?
Pd2 N2 2.023(4) 2 ?
Pd2 N2 2.023(4) 3 ?
Pd2 N2 2.023(4) 4 ?
C8 C13 1.341(9) . ?
C8 C9 1.396(9) . ?
C9 O2B 1.190(10) . ?
C9 C10 1.415(9) . ?
C10 C11 1.345(8) . ?
C11 C12 1.380(8) . ?
C12 C13 1.368(9) . ?
C13 O2A 1.281(9) . ?

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
O3 C1 C2 120.8(6) . . ?
O3 C1 C8 117.5(6) . . ?
C2 C1 C8 121.7(5) . . ?
C3 C2 C7 117.4(5) . . ?
C3 C2 C1 123.2(5) . . ?
C7 C2 C1 119.4(5) . . ?
C4 C3 C2 122.0(5) . . ?
C3 C4 C5 120.1(4) . . ?
C6 C5 O5 123.3(4) . . ?
C6 C5 C4 121.0(4) . . ?
O5 C5 C4 115.7(4) . . ?
C5 C6 C7 118.8(5) . . ?
O4 C7 C2 123.0(6) . . ?
O4 C7 C6 116.5(6) . . ?
C2 C7 C6 120.5(5) . . ?
O5 C14 C21 110.5(4) . . ?
O1 C15 C16 107.4(5) . . ?
C17 C16 C20 117.2(5) . . ?
C17 C16 C15 123.0(6) . . ?
C20 C16 C15 119.7(5) . . ?
C16 C17 C18 119.1(6) . . ?
C19 C18 C17 119.1(6) . . ?
N1 C19 C18 122.5(6) . . ?
N1 C20 C16 124.3(5) . . ?
C25 C21 C22 118.5(5) . . ?
C25 C21 C14 122.8(4) . . ?
C22 C21 C14 118.6(5) . . ?
C23 C22 C21 119.3(5) . . ?
C22 C23 C24 119.7(5) . . ?
N2 C24 C23 121.6(5) . . ?
N2 C25 C21 122.1(4) . . ?
C20 N1 C19 117.8(5) . . ?
C20 N1 Pd1 121.1(4) . . ?
C19 N1 Pd1 121.2(4) . . ?
C25 N2 C24 118.7(4) . . ?
C25 N2 Pd2 123.2(3) . . ?
C24 N2 Pd2 118.0(3) . . ?
C11 O1 C15 119.1(5) . . ?
C5 O5 C14 117.9(4) . . ?
N1 Pd1 N1 89.983(4) 2 4 ?
N1 Pd1 N1 89.983(4) 2 3 ?
N1 Pd1 N1 178.0(2) 4 3 ?
N1 Pd1 N1 178.0(2) 2 . ?
N1 Pd1 N1 89.983(5) 4 . ?
N1 Pd1 N1 89.983(4) 3 . ?
N2 Pd2 N2 175.0(2) . 2 ?
N2 Pd2 N2 89.891(9) . 3 ?
N2 Pd2 N2 89.890(9) 2 3 ?
N2 Pd2 N2 89.889(9) . 4 ?
N2 Pd2 N2 89.890(9) 2 4 ?
N2 Pd2 N2 175.0(2) 3 4 ?
C13 C8 C9 122.8(8) . . ?
C13 C8 C1 119.0(8) . . ?
C9 C8 C1 117.9(8) . . ?
O2B C9 C8 119.4(9) . . ?
O2B C9 C10 121.8(10) . . ?
C8 C9 C10 118.6(8) . . ?
C11 C10 C9 118.4(7) . . ?
C10 C11 C12 120.6(7) . . ?
C10 C11 O1 123.8(7) . . ?
C12 C11 O1 115.7(7) . . ?
C13 C12 C11 122.6(8) . . ?
O2A C13 C8 117.9(9) . . ?
O2A C13 C12 124.9(9) . . ?
C8 C13 C12 117.1(9) . . ?

# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_interlock-dioxane
_database_code_depnum_ccdc_archive 'CCDC 1405237'
_audit_update_record             
;
2015-06-06 deposited with the CCDC.
2017-04-20 downloaded from the CCDC.
;

_audit_creation_date             2015-06-06T13:53:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C100 H80 N8 O20 Pd2)'
_chemical_formula_sum            'C200 H160 N16 O40 Pd4'
_chemical_formula_weight         3853.03

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'
_space_group_IT_number           126
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   18.9525(12)
_cell_length_b                   18.9525(12)
_cell_length_c                   38.292(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13754(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    3011
_cell_measurement_theta_min      1.519
_cell_measurement_theta_max      20.87

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    0.93
_exptl_crystal_F_000             3952
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_probe          X-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_number            45364
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.519
_diffrn_reflns_theta_max         20.874
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.583
_diffrn_measured_fraction_theta_max 0.998
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_number_total             3643
_reflns_number_gt                2030
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.2000P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3643
_refine_ls_number_parameters     230
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.099
_refine_ls_wR_factor_ref         0.3174
_refine_ls_wR_factor_gt          0.2835
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.102

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   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 0 '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 0.006 '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'
S S 0.1246 0.1234 '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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3933(6) 0.2064(5) 0.8341(2) 0.101(3) Uani 1 1 d . . . . .
H1 H 0.3702 0.1954 0.8127 0.121 Uiso 1 1 calc R U . . .
C2 C 0.3898(6) 0.2469(5) 0.8910(2) 0.113(3) Uani 1 1 d . . . . .
H2 H 0.3648 0.2685 0.9096 0.135 Uiso 1 1 calc R U . . .
C3 C 0.4557(7) 0.2293(6) 0.8956(2) 0.130(4) Uani 1 1 d . . . . .
H3 H 0.4769 0.2351 0.9179 0.156 Uiso 1 1 calc R U . . .
C4 C 0.4947(5) 0.2024(4) 0.8682(2) 0.107(3) Uani 1 1 d . . . . .
H4 H 0.5431 0.1911 0.8714 0.128 Uiso 1 1 calc R U . . .
C5 C 0.4640(6) 0.1921(5) 0.8369(2) 0.102(3) Uani 1 1 d . . . . .
C6 C 0.3272(6) 0.1323(8) 0.4720(2) 0.126(4) Uani 1 1 d . . . . .
H6 H 0.3177 0.1571 0.493 0.152 Uiso 1 1 calc R U . . .
C7 C 0.3166(6) 0.1197(8) 0.4134(3) 0.144(4) Uani 1 1 d . . . . .
H7 H 0.3006 0.1365 0.3914 0.172 Uiso 1 1 calc R U . . .
C8 C 0.3494(7) 0.0569(8) 0.4144(4) 0.166(5) Uani 1 1 d . . . . .
H8 H 0.3575 0.0306 0.3936 0.199 Uiso 1 1 calc R U . . .
C9 C 0.3710(7) 0.0316(7) 0.4468(4) 0.171(5) Uani 1 1 d . . . . .
H9 H 0.3916 -0.014 0.4481 0.206 Uiso 1 1 calc R U . . .
C10 C 0.3642(6) 0.0679(8) 0.4749(3) 0.133(4) Uani 1 1 d . . . . .
C11 C 0.5060(5) 0.1622(5) 0.8072(2) 0.118(3) Uani 1 1 d . . . . .
H11A H 0.5517 0.1873 0.8054 0.141 Uiso 1 1 calc R U . . .
H11B H 0.5158 0.1117 0.8116 0.141 Uiso 1 1 calc R U . . .
N1 N 0.3046(5) 0.1614(5) 0.4425(2) 0.140(3) Uani 1 1 d . . . . .
N2 N 0.3554(4) 0.2348(4) 0.85973(18) 0.105(2) Uani 1 1 d . . . . .
O1 O 0.4670(3) 0.1701(3) 0.77538(12) 0.0969(16) Uani 1 1 d . . . . .
Pd1 Pd 0.25 0.25 0.44143(3) 0.1191(8) Uani 1 4 d S T P . .
Pd2 Pd 0.25 0.25 0.85770(3) 0.0963(7) Uani 1 4 d S T P . .
C12A C 0.3856(11) 0.0396(12) 0.5084(5) 0.105(7) Uiso 0.520(11) 1 d . U P A 1
H12A H 0.3472 0.0457 0.5257 0.125 Uiso 0.520(11) 1 calc R U P A 1
H12B H 0.3958 -0.0115 0.5062 0.125 Uiso 0.520(11) 1 calc R U P A 1
C13A C 0.4932(7) 0.1351(8) 0.7476(3) 0.088(6) Uiso 0.520(11) 1 d G U P A 1
C14A C 0.4583(5) 0.1472(8) 0.7163(4) 0.076(6) Uiso 0.520(11) 1 d G U P A 1
H14A H 0.4167 0.1751 0.7159 0.091 Uiso 0.520(11) 1 calc R U P A 1
C15A C 0.4844(6) 0.1185(8) 0.6855(3) 0.096(7) Uiso 0.520(11) 1 d G U P A 1
H15A H 0.4606 0.1267 0.664 0.115 Uiso 0.520(11) 1 calc R U P A 1
C16A C 0.5453(7) 0.0776(8) 0.6860(3) 0.101(5) Uiso 0.520(11) 1 d G U P A 1
C17A C 0.5801(6) 0.0655(8) 0.7174(4) 0.139(7) Uiso 0.520(11) 1 d G . P A 1
C18A C 0.5541(7) 0.0943(8) 0.7482(3) 0.110(6) Uiso 0.520(11) 1 d G U P A 1
H18A H 0.5779 0.086 0.7697 0.132 Uiso 0.520(11) 1 calc R U P A 1
C19A C 0.4704(7) 0.0701(9) 0.5531(3) 0.096(5) Uiso 0.520(11) 1 d G U P A 1
C20A C 0.5253(7) 0.1158(8) 0.5612(3) 0.104(5) Uiso 0.520(11) 1 d G U P A 1
H20A H 0.5414 0.1489 0.5444 0.125 Uiso 0.520(11) 1 calc R U P A 1
C21A C 0.5568(7) 0.1131(8) 0.5940(4) 0.142(7) Uiso 0.520(11) 1 d G U P A 1
C22A C 0.5333(8) 0.0646(9) 0.6186(3) 0.098(5) Uiso 0.520(11) 1 d G U P A 1
C23A C 0.4784(7) 0.0189(8) 0.6105(3) 0.118(6) Uiso 0.520(11) 1 d G U P A 1
H23A H 0.4623 -0.0143 0.6273 0.142 Uiso 0.520(11) 1 calc R U P A 1
C24A C 0.4469(6) 0.0216(8) 0.5777(4) 0.123(6) Uiso 0.520(11) 1 d G U P A 1
H24A H 0.4094 -0.0097 0.5722 0.147 Uiso 0.520(11) 1 calc R U P A 1
C25A C 0.5674(16) 0.0567(17) 0.6541(7) 0.176(11) Uiso 0.520(11) 1 d . . P A 1
O2A O 0.4450(11) 0.0748(10) 0.5194(5) 0.129(7) Uiso 0.520(11) 1 d . U P A 1
O3A O 0.6374(10) 0.0367(10) 0.6523(4) 0.173(7) Uiso 0.520(11) 1 d . . P A 1
O4A O 0.6153(7) 0.1747(7) 0.5993(3) 0.151(6) Uiso 0.520(11) 1 d . . P A 1
H4A H 0.6333 0.1711 0.6192 0.226 Uiso 0.520(11) 1 calc R U P A 1
O6A O 0.6397(8) 0.0359(9) 0.7193(4) 0.168(6) Uiso 0.520(11) 1 d . . P A 1
H6A H 0.6509 0.0202 0.6995 0.252 Uiso 0.520(11) 1 calc R U P A 1
C12B C 0.3986(15) 0.0672(14) 0.5114(6) 0.108(8) Uiso 0.480(11) 1 d . U P A 2
H12C H 0.3609 0.0805 0.528 0.13 Uiso 0.480(11) 1 calc R U P A 2
H12D H 0.4101 0.0172 0.5163 0.13 Uiso 0.480(11) 1 calc R U P A 2
C13B C 0.5006(7) 0.1531(8) 0.7454(3) 0.084(6) Uiso 0.480(11) 1 d G U P A 2
C14B C 0.4595(6) 0.1592(8) 0.7155(4) 0.114(10) Uiso 0.480(11) 1 d G U P A 2
H14B H 0.4131 0.1779 0.717 0.137 Uiso 0.480(11) 1 calc R U P A 2
C15B C 0.4863(6) 0.1378(8) 0.6834(3) 0.084(6) Uiso 0.480(11) 1 d G U P A 2
H15B H 0.4582 0.1419 0.6629 0.1 Uiso 0.480(11) 1 calc R U P A 2
C16B C 0.5542(6) 0.1104(7) 0.6812(2) 0.075(5) Uiso 0.480(11) 1 d G U P A 2
C17B C 0.5953(5) 0.1044(7) 0.7111(3) 0.083(5) Uiso 0.480(11) 1 d G . P A 2
C18B C 0.5685(7) 0.1258(7) 0.7432(2) 0.086(5) Uiso 0.480(11) 1 d G U P A 2
H18B H 0.5967 0.1217 0.7636 0.103 Uiso 0.480(11) 1 calc R U P A 2
C19B C 0.4787(7) 0.0975(8) 0.5500(3) 0.083(5) Uiso 0.480(11) 1 d G U P A 2
C20B C 0.4576(6) 0.0503(7) 0.5758(3) 0.106(6) Uiso 0.480(11) 1 d G U P A 2
H20B H 0.4196 0.0188 0.5715 0.127 Uiso 0.480(11) 1 calc R U P A 2
C21B C 0.4921(7) 0.0492(7) 0.6078(3) 0.076(4) Uiso 0.480(11) 1 d G U P A 2
C22B C 0.5477(7) 0.0953(8) 0.6141(3) 0.094(5) Uiso 0.480(11) 1 d G U P A 2
C23B C 0.5688(6) 0.1425(8) 0.5884(4) 0.122(6) Uiso 0.480(11) 1 d G U P A 2
H23B H 0.6068 0.174 0.5927 0.146 Uiso 0.480(11) 1 calc R U P A 2
C24B C 0.5343(7) 0.1436(8) 0.5563(3) 0.117(7) Uiso 0.480(11) 1 d G U P A 2
H24B H 0.5488 0.1758 0.5387 0.14 Uiso 0.480(11) 1 calc R U P A 2
C25B C 0.5917(10) 0.0931(10) 0.6473(4) 0.084(5) Uiso 0.480(11) 1 d . . P A 2
O2B O 0.4489(8) 0.1001(9) 0.5197(4) 0.104(6) Uiso 0.480(11) 1 d . U P A 2
O3B O 0.6526(8) 0.0787(8) 0.6449(3) 0.116(5) Uiso 0.480(11) 1 d . . P A 2
O4B O 0.4785(13) -0.0047(14) 0.6316(7) 0.243(11) Uiso 0.480(11) 1 d . . P A 2
H4B H 0.5031 0.0014 0.6496 0.365 Uiso 0.480(11) 1 calc R U P A 2
O6B O 0.6624(6) 0.0842(7) 0.7119(3) 0.116(5) Uiso 0.480(11) 1 d . . P A 2
H6B H 0.6751 0.0718 0.6918 0.174 Uiso 0.480(11) 1 calc R U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 N2 1.330(11) . ?
C1 C5 1.370(11) . ?
C2 C3 1.305(12) . ?
C2 N2 1.381(11) . ?
C3 C4 1.382(12) . ?
C4 C5 1.346(11) . ?
C5 C11 1.499(12) . ?
C6 N1 1.326(12) . ?
C6 C10 1.412(14) . ?
C7 C8 1.343(13) . ?
C7 N1 1.385(13) . ?
C8 C9 1.391(14) . ?
C9 C10 1.284(13) . ?
C10 C12A 1.45(2) . ?
C10 C12B 1.54(3) . ?
C11 O1 1.434(8) . ?
N1 Pd1 1.974(10) . ?
N2 Pd2 2.020(9) . ?
O1 C13A 1.346(10) . ?
O1 C13B 1.353(10) . ?
Pd1 N1 1.974(10) 3 ?
Pd1 N1 1.974(10) 4 ?
Pd1 N1 1.974(10) 2 ?
Pd2 N2 2.020(9) 3 ?
Pd2 N2 2.020(9) 4 ?
Pd2 N2 2.020(9) 2 ?
C12A O2A 1.37(3) . ?
C13A C14A 1.39 . ?
C13A C18A 1.39 . ?
C14A C15A 1.39 . ?
C15A C16A 1.39 . ?
C16A C25A 1.35(3) . ?
C16A C17A 1.39 . ?
C17A O6A 1.263(16) . ?
C17A C18A 1.39 . ?
C19A O2A 1.38(2) . ?
C19A C20A 1.39 . ?
C19A C24A 1.39 . ?
C20A C21A 1.39 . ?
C21A C22A 1.39 . ?
C21A O4A 1.623(18) . ?
C22A C23A 1.39 . ?
C22A C25A 1.51(3) . ?
C23A C24A 1.39 . ?
C25A O3A 1.38(3) . ?
C12B O2B 1.18(3) . ?
C13B C14B 1.39 . ?
C13B C18B 1.39 . ?
C14B C15B 1.39 . ?
C15B C16B 1.39 . ?
C16B C17B 1.39 . ?
C16B C25B 1.515(18) . ?
C17B O6B 1.329(13) . ?
C17B C18B 1.39 . ?
C19B O2B 1.294(18) . ?
C19B C20B 1.39 . ?
C19B C24B 1.39 . ?
C20B C21B 1.39 . ?
C21B C22B 1.39 . ?
C21B O4B 1.39(3) . ?
C22B C23B 1.39 . ?
C22B C25B 1.521(18) . ?
C23B C24B 1.39 . ?
C25B O3B 1.190(19) . ?

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
N2 C1 C5 123.3(8) . . ?
C3 C2 N2 121.8(9) . . ?
C2 C3 C4 120.2(9) . . ?
C5 C4 C3 119.8(10) . . ?
C4 C5 C1 117.7(9) . . ?
C4 C5 C11 119.9(10) . . ?
C1 C5 C11 122.3(8) . . ?
N1 C6 C10 125.9(10) . . ?
C8 C7 N1 124.0(10) . . ?
C7 C8 C9 117.8(11) . . ?
C10 C9 C8 122.3(12) . . ?
C9 C10 C6 116.5(10) . . ?
C9 C10 C12A 121.1(15) . . ?
C6 C10 C12A 122.0(13) . . ?
C9 C10 C12B 135.4(15) . . ?
C6 C10 C12B 106.8(14) . . ?
O1 C11 C5 109.3(7) . . ?
C6 N1 C7 113.2(11) . . ?
C6 N1 Pd1 122.7(8) . . ?
C7 N1 Pd1 123.7(8) . . ?
C1 N2 C2 116.8(9) . . ?
C1 N2 Pd2 124.3(7) . . ?
C2 N2 Pd2 118.4(7) . . ?
C13A O1 C11 115.5(8) . . ?
C13B O1 C11 117.1(8) . . ?
N1 Pd1 N1 89.976(11) . 3 ?
N1 Pd1 N1 89.974(11) . 4 ?
N1 Pd1 N1 177.6(5) 3 4 ?
N1 Pd1 N1 177.6(5) . 2 ?
N1 Pd1 N1 89.975(11) 3 2 ?
N1 Pd1 N1 89.975(11) 4 2 ?
N2 Pd2 N2 89.917(18) . 3 ?
N2 Pd2 N2 89.914(16) . 4 ?
N2 Pd2 N2 175.6(4) 3 4 ?
N2 Pd2 N2 175.6(4) . 2 ?
N2 Pd2 N2 89.915(16) 3 2 ?
N2 Pd2 N2 89.915(17) 4 2 ?
O2A C12A C10 108.7(16) . . ?
O1 C13A C14A 115.2(10) . . ?
O1 C13A C18A 124.5(10) . . ?
C14A C13A C18A 120 . . ?
C15A C14A C13A 120 . . ?
C14A C15A C16A 120 . . ?
C25A C16A C15A 114.0(17) . . ?
C25A C16A C17A 125.9(17) . . ?
C15A C16A C17A 120 . . ?
O6A C17A C18A 116.4(12) . . ?
O6A C17A C16A 123.1(13) . . ?
C18A C17A C16A 120 . . ?
C17A C18A C13A 120 . . ?
O2A C19A C20A 115.5(13) . . ?
O2A C19A C24A 124.5(13) . . ?
C20A C19A C24A 120 . . ?
C21A C20A C19A 120 . . ?
C20A C21A C22A 120 . . ?
C20A C21A O4A 112.2(10) . . ?
C22A C21A O4A 127.6(10) . . ?
C23A C22A C21A 120 . . ?
C23A C22A C25A 117.3(15) . . ?
C21A C22A C25A 122.6(15) . . ?
C22A C23A C24A 120 . . ?
C23A C24A C19A 120 . . ?
C16A C25A O3A 115(2) . . ?
C16A C25A C22A 131(2) . . ?
O3A C25A C22A 113(2) . . ?
C12A O2A C19A 122.6(17) . . ?
O2B C12B C10 125(2) . . ?
O1 C13B C14B 114.6(10) . . ?
O1 C13B C18B 125.2(10) . . ?
C14B C13B C18B 120 . . ?
C15B C14B C13B 120 . . ?
C14B C15B C16B 120 . . ?
C17B C16B C15B 120 . . ?
C17B C16B C25B 115.1(11) . . ?
C15B C16B C25B 124.6(11) . . ?
O6B C17B C16B 125.5(10) . . ?
O6B C17B C18B 114.3(10) . . ?
C16B C17B C18B 120 . . ?
C17B C18B C13B 120 . . ?
O2B C19B C20B 122.5(12) . . ?
O2B C19B C24B 117.5(12) . . ?
C20B C19B C24B 120 . . ?
C19B C20B C21B 120 . . ?
C22B C21B C20B 120 . . ?
C22B C21B O4B 119.2(14) . . ?
C20B C21B O4B 120.0(14) . . ?
C21B C22B C23B 120 . . ?
C21B C22B C25B 122.9(12) . . ?
C23B C22B C25B 116.9(12) . . ?
C24B C23B C22B 120 . . ?
C23B C24B C19B 120 . . ?
O3B C25B C16B 124.9(15) . . ?
O3B C25B C22B 118.3(15) . . ?
C16B C25B C22B 116.9(14) . . ?
C12B O2B C19B 124.9(18) . . ?

# END of CIF
