# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1478616'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H16 Cl N3 O2'
_chemical_formula_weight         413.85

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   14.075(2)
_cell_length_b                   7.9884(11)
_cell_length_c                   17.570(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1975.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2234
_cell_measurement_theta_min      4.637
_cell_measurement_theta_max      40.186

_exptl_crystal_description       'irregular block'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_F_000             856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.065
_exptl_absorpt_coefficient_mu    0.220
_shelx_estimated_absorpt_T_min   0.931
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7821
_exptl_absorpt_correction_T_max  0.9869
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart 1k'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22683
_diffrn_reflns_av_unetI/netI     0.1278
_diffrn_reflns_av_R_equivalents  0.1501
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.318
_diffrn_reflns_theta_max         27.021
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4314
_reflns_number_gt                1927
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART V5.624'
_computing_cell_refinement       'Bruker SMART V5.624'
_computing_data_reduction        'SAINT V6.28A (Bruker)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP3, Chimera 1.10.2'
_computing_publication_material  'ORTEP3, Chimera 1.10.2'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1037P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 683 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4314
_refine_ls_number_parameters     271
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1968
_refine_ls_R_factor_gt           0.0676
_refine_ls_wR_factor_ref         0.2065
_refine_ls_wR_factor_gt          0.1519
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 -0.1567(6) 0.4881(11) 0.4976(6) 0.051(2) Uani 1 1 d . . . . .
H1 H -0.1836 0.4469 0.4530 0.062 Uiso 1 1 calc R U . . .
C2 C -0.0717(5) 0.5770(9) 0.4918(5) 0.039(2) Uani 1 1 d . . . . .
C3 C -0.0318(5) 0.6325(9) 0.5606(5) 0.0393(19) Uani 1 1 d . . . . .
C4 C -0.0770(5) 0.6014(10) 0.6298(5) 0.041(2) Uani 1 1 d . . . . .
C5 C -0.1632(6) 0.5128(10) 0.6269(6) 0.053(2) Uani 1 1 d . . . . .
H5 H -0.1949 0.4908 0.6722 0.064 Uiso 1 1 calc R U . . .
C6 C -0.0238(6) 0.6114(12) 0.4216(5) 0.047(2) Uani 1 1 d . . . . .
H6 H -0.0503 0.5728 0.3764 0.056 Uiso 1 1 calc R U . . .
C7 C 0.0598(6) 0.6995(10) 0.4188(5) 0.042(2) Uani 1 1 d . . . . .
H7 H 0.0901 0.7199 0.3727 0.051 Uiso 1 1 calc R U . . .
C8 C 0.0988(5) 0.7591(10) 0.4889(5) 0.0372(19) Uani 1 1 d . . . . .
C9 C 0.0559(5) 0.7244(9) 0.5579(5) 0.0347(18) Uani 1 1 d . . . . .
C10 C 0.0939(5) 0.7848(10) 0.6279(5) 0.041(2) Uani 1 1 d . . . . .
C11 C 0.0475(6) 0.7484(12) 0.6981(5) 0.047(2) Uani 1 1 d . . . . .
H11 H 0.0743 0.7836 0.7437 0.057 Uiso 1 1 calc R U . . .
C12 C -0.0364(6) 0.6617(12) 0.6985(5) 0.051(2) Uani 1 1 d . . . . .
H12 H -0.0673 0.6420 0.7444 0.061 Uiso 1 1 calc R U . . .
C13 C 0.1814(5) 0.8599(10) 0.4900(5) 0.041(2) Uani 1 1 d . . . . .
H13 H 0.2123 0.8865 0.4448 0.050 Uiso 1 1 calc R U . . .
C14 C 0.1766(5) 0.8800(10) 0.6236(5) 0.041(2) Uani 1 1 d . . . . .
H14 H 0.2052 0.9180 0.6680 0.049 Uiso 1 1 calc R U . . .
C15 C 0.2990(5) 1.0355(10) 0.5537(6) 0.046(2) Uani 1 1 d . . . . .
H15A H 0.2844 1.1270 0.5193 0.055 Uiso 1 1 calc R U . . .
H15B H 0.3096 1.0825 0.6039 0.055 Uiso 1 1 calc R U . . .
C16 C 0.3882(5) 0.9490(11) 0.5273(5) 0.041(2) Uani 1 1 d . . . . .
C17 C 0.4084(6) 0.9492(12) 0.4524(5) 0.052(2) Uani 1 1 d . . . . .
H17 H 0.3680 1.0037 0.4186 0.062 Uiso 1 1 calc R U . . .
C18 C 0.4917(6) 0.8662(13) 0.4242(6) 0.054(2) Uani 1 1 d . . . . .
H18 H 0.5037 0.8669 0.3722 0.065 Uiso 1 1 calc R U . . .
C19 C 0.4525(6) 0.8692(10) 0.5782(5) 0.041(2) Uani 1 1 d . . . . .
C20 C 0.4420(6) 0.8702(12) 0.6582(5) 0.051(2) Uani 1 1 d . . . . .
H20 H 0.3896 0.9210 0.6808 0.061 Uiso 1 1 calc R U . . .
C21 C 0.5097(7) 0.7958(13) 0.7014(6) 0.066(3) Uani 1 1 d . . . . .
H21 H 0.5030 0.7984 0.7541 0.079 Uiso 1 1 calc R U . . .
C22 C 0.5891(7) 0.7155(13) 0.6708(7) 0.068(3) Uani 1 1 d . . . . .
H22 H 0.6340 0.6653 0.7022 0.082 Uiso 1 1 calc R U . . .
C23 C 0.5993(6) 0.7127(11) 0.5930(6) 0.049(2) Uani 1 1 d . . . . .
H23 H 0.6511 0.6576 0.5718 0.059 Uiso 1 1 calc R U . . .
C24 C 0.5337(5) 0.7906(10) 0.5453(5) 0.040(2) Uani 1 1 d . . . . .
N1 N -0.2013(5) 0.4589(9) 0.5621(5) 0.0540(19) Uani 1 1 d . . . . .
N2 N 0.2151(4) 0.9170(7) 0.5568(4) 0.0376(15) Uani 1 1 d . . . . .
N3 N 0.5520(5) 0.7885(9) 0.4700(4) 0.0488(19) Uani 1 1 d . . . . .
Cl1 Cl 0.73018(17) 1.0267(3) 0.30098(17) 0.0738(8) Uani 1 1 d . . . . .
O1 O 0.6996(7) 0.6767(11) 0.3722(5) 0.122(4) Uani 1 1 d . . . . .
O2 O 0.7868(6) 0.4186(10) 0.2994(6) 0.114(3) Uani 1 1 d . . . . .


_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 N1 1.316(12) . ?
C1 C2 1.394(11) . ?
C1 H1 0.9300 . ?
C2 C3 1.405(11) . ?
C2 C6 1.433(12) . ?
C3 C4 1.394(12) . ?
C3 C9 1.438(10) . ?
C4 C5 1.406(12) . ?
C4 C12 1.418(12) . ?
C5 N1 1.330(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.372(12) . ?
C6 H6 0.9300 . ?
C7 C8 1.431(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.383(11) . ?
C8 C13 1.414(11) . ?
C9 C10 1.425(11) . ?
C10 C14 1.392(10) . ?
C10 C11 1.426(12) . ?
C11 C12 1.369(12) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 N2 1.346(11) . ?
C13 H13 0.9300 . ?
C14 N2 1.325(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.507(11) . ?
C15 N2 1.515(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.347(11) . ?
C16 C19 1.423(10) . ?
C17 C18 1.435(13) . ?
C17 H17 0.9300 . ?
C18 N3 1.325(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.414(11) . ?
C19 C24 1.426(11) . ?
C20 C21 1.356(13) . ?
C20 H20 0.9300 . ?
C21 C22 1.397(14) . ?
C21 H21 0.9300 . ?
C22 C23 1.374(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.395(12) . ?
C23 H23 0.9300 . ?
C24 N3 1.347(10) . ?

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 C1 C2 124.2(9) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C1 C2 C3 116.2(8) . . ?
C1 C2 C6 124.3(8) . . ?
C3 C2 C6 119.5(7) . . ?
C4 C3 C2 120.8(7) . . ?
C4 C3 C9 120.7(8) . . ?
C2 C3 C9 118.5(8) . . ?
C3 C4 C5 116.8(9) . . ?
C3 C4 C12 119.9(7) . . ?
C5 C4 C12 123.3(9) . . ?
N1 C5 C4 122.8(9) . . ?
N1 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
C7 C6 C2 122.2(8) . . ?
C7 C6 H6 118.9 . . ?
C2 C6 H6 118.9 . . ?
C6 C7 C8 118.0(8) . . ?
C6 C7 H7 121.0 . . ?
C8 C7 H7 121.0 . . ?
C9 C8 C13 117.5(7) . . ?
C9 C8 C7 121.4(7) . . ?
C13 C8 C7 121.1(8) . . ?
C8 C9 C10 121.7(7) . . ?
C8 C9 C3 120.4(7) . . ?
C10 C9 C3 117.8(7) . . ?
C14 C10 C9 116.8(8) . . ?
C14 C10 C11 122.8(8) . . ?
C9 C10 C11 120.3(7) . . ?
C12 C11 C10 120.2(8) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C4 121.0(8) . . ?
C11 C12 H12 119.5 . . ?
C4 C12 H12 119.5 . . ?
N2 C13 C8 119.6(8) . . ?
N2 C13 H13 120.2 . . ?
C8 C13 H13 120.2 . . ?
N2 C14 C10 120.8(8) . . ?
N2 C14 H14 119.6 . . ?
C10 C14 H14 119.6 . . ?
C16 C15 N2 112.0(6) . . ?
C16 C15 H15A 109.2 . . ?
N2 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
N2 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C19 118.7(8) . . ?
C17 C16 C15 118.5(8) . . ?
C19 C16 C15 122.8(7) . . ?
C16 C17 C18 120.6(9) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
N3 C18 C17 122.1(9) . . ?
N3 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
C20 C19 C16 123.8(8) . . ?
C20 C19 C24 119.3(8) . . ?
C16 C19 C24 116.9(7) . . ?
C21 C20 C19 118.8(10) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C20 C21 C22 123.2(11) . . ?
C20 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C23 C22 C21 118.4(10) . . ?
C23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
C22 C23 C24 121.5(9) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
N3 C24 C23 117.2(8) . . ?
N3 C24 C19 123.9(7) . . ?
C23 C24 C19 118.9(8) . . ?
C1 N1 C5 119.2(7) . . ?
C14 N2 C13 123.5(6) . . ?
C14 N2 C15 119.4(7) . . ?
C13 N2 C15 117.0(7) . . ?
C18 N3 C24 117.9(7) . . ?

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
N1 C1 C2 C3 2.0(12) . . . . ?
N1 C1 C2 C6 -178.9(9) . . . . ?
C1 C2 C3 C4 -1.2(10) . . . . ?
C6 C2 C3 C4 179.7(8) . . . . ?
C1 C2 C3 C9 179.9(7) . . . . ?
C6 C2 C3 C9 0.7(10) . . . . ?
C2 C3 C4 C5 0.1(11) . . . . ?
C9 C3 C4 C5 179.1(7) . . . . ?
C2 C3 C4 C12 -178.7(8) . . . . ?
C9 C3 C4 C12 0.3(11) . . . . ?
C3 C4 C5 N1 0.3(12) . . . . ?
C12 C4 C5 N1 179.0(8) . . . . ?
C1 C2 C6 C7 -180.0(8) . . . . ?
C3 C2 C6 C7 -0.9(13) . . . . ?
C2 C6 C7 C8 -0.5(13) . . . . ?
C6 C7 C8 C9 2.3(12) . . . . ?
C6 C7 C8 C13 -175.9(7) . . . . ?
C13 C8 C9 C10 -1.1(10) . . . . ?
C7 C8 C9 C10 -179.3(8) . . . . ?
C13 C8 C9 C3 175.7(7) . . . . ?
C7 C8 C9 C3 -2.5(10) . . . . ?
C4 C3 C9 C8 -178.0(7) . . . . ?
C2 C3 C9 C8 1.0(10) . . . . ?
C4 C3 C9 C10 -1.1(11) . . . . ?
C2 C3 C9 C10 177.9(7) . . . . ?
C8 C9 C10 C14 -0.3(10) . . . . ?
C3 C9 C10 C14 -177.1(7) . . . . ?
C8 C9 C10 C11 179.3(8) . . . . ?
C3 C9 C10 C11 2.4(10) . . . . ?
C14 C10 C11 C12 176.5(8) . . . . ?
C9 C10 C11 C12 -3.1(12) . . . . ?
C10 C11 C12 C4 2.2(14) . . . . ?
C3 C4 C12 C11 -0.9(12) . . . . ?
C5 C4 C12 C11 -179.6(8) . . . . ?
C9 C8 C13 N2 0.3(10) . . . . ?
C7 C8 C13 N2 178.5(7) . . . . ?
C9 C10 C14 N2 2.6(11) . . . . ?
C11 C10 C14 N2 -177.0(8) . . . . ?
N2 C15 C16 C17 91.6(10) . . . . ?
N2 C15 C16 C19 -89.3(10) . . . . ?
C19 C16 C17 C18 1.9(13) . . . . ?
C15 C16 C17 C18 -179.0(7) . . . . ?
C16 C17 C18 N3 -0.8(14) . . . . ?
C17 C16 C19 C20 175.8(9) . . . . ?
C15 C16 C19 C20 -3.3(13) . . . . ?
C17 C16 C19 C24 -1.5(12) . . . . ?
C15 C16 C19 C24 179.4(7) . . . . ?
C16 C19 C20 C21 -177.3(8) . . . . ?
C24 C19 C20 C21 -0.1(14) . . . . ?
C19 C20 C21 C22 -1.0(15) . . . . ?
C20 C21 C22 C23 0.4(15) . . . . ?
C21 C22 C23 C24 1.4(15) . . . . ?
C22 C23 C24 N3 176.7(9) . . . . ?
C22 C23 C24 C19 -2.4(13) . . . . ?
C20 C19 C24 N3 -177.3(9) . . . . ?
C16 C19 C24 N3 0.1(12) . . . . ?
C20 C19 C24 C23 1.7(12) . . . . ?
C16 C19 C24 C23 179.2(8) . . . . ?
C2 C1 N1 C5 -1.7(13) . . . . ?
C4 C5 N1 C1 0.5(12) . . . . ?
C10 C14 N2 C13 -3.7(11) . . . . ?
C10 C14 N2 C15 173.7(6) . . . . ?
C8 C13 N2 C14 2.2(10) . . . . ?
C8 C13 N2 C15 -175.2(6) . . . . ?
C16 C15 N2 C14 113.9(8) . . . . ?
C16 C15 N2 C13 -68.6(9) . . . . ?
C17 C18 N3 C24 -0.6(13) . . . . ?
C23 C24 N3 C18 -178.1(7) . . . . ?
C19 C24 N3 C18 1.0(12) . . . . ?

_refine_diff_density_max         0.304
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1478617'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H58 N16 O25 Pd2'
_chemical_formula_weight         1519.94

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7510(15)
_cell_length_b                   11.3294(18)
_cell_length_c                   14.580(2)
_cell_angle_alpha                80.294(3)
_cell_angle_beta                 89.934(3)
_cell_angle_gamma                83.204(3)
_cell_volume                     1576.2(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3126
_cell_measurement_theta_min      5.670
_cell_measurement_theta_max      41.973

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_F_000             774
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.665
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6114
_exptl_absorpt_correction_T_max  0.9614
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21927
_diffrn_reflns_av_unetI/netI     0.1042
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.417
_diffrn_reflns_theta_max         28.462
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             7797
_reflns_number_gt                4887
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'SAINT V7.12A (Bruker)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP3, Chimera 1.10.2'
_computing_publication_material  'ORTEP3, Chimera 1.10.2'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1137P)²+0.3410P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7797
_refine_ls_number_parameters     506
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.2127
_refine_ls_wR_factor_gt          0.1710
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C11 C 0.1430(6) 0.2943(5) 0.5667(4) 0.0350(13) Uani 1 1 d . . . . .
H11 H 0.0529 0.2820 0.5881 0.042 Uiso 1 1 calc R U . . .
C12 C 0.1786(6) 0.2700(5) 0.4802(4) 0.0355(13) Uani 1 1 d . . . . .
H12 H 0.1141 0.2412 0.4431 0.043 Uiso 1 1 calc R U . . .
N2 N 0.9716(17) 0.0341(15) 0.4713(10) 0.066(4) Uani 0.5 1 d . . P A 1
C7 C 0.3095(6) 0.2878(5) 0.4471(4) 0.0320(12) Uani 1 1 d . . . . .
C8 C 0.3979(7) 0.3316(5) 0.5035(4) 0.0379(14) Uani 1 1 d . . . . .
H8 H 0.4875 0.3469 0.4828 0.045 Uiso 1 1 calc R U . . .
C9 C 0.3559(6) 0.3529(5) 0.5892(4) 0.0361(13) Uani 1 1 d . . . . .
H9 H 0.4187 0.3821 0.6272 0.043 Uiso 1 1 calc R U . . .
C6 C 0.3290(7) 0.1479(6) 0.2301(4) 0.0451(16) Uani 1 1 d . . . . .
H6 H 0.2803 0.0953 0.2017 0.054 Uiso 1 1 calc R U . . .
C5 C 0.2847(6) 0.1799(6) 0.3124(4) 0.0393(14) Uani 1 1 d . . . . .
H5 H 0.2054 0.1492 0.3406 0.047 Uiso 1 1 calc R U . . .
C7AA C 0.3536(6) 0.2564(5) 0.3554(4) 0.0343(13) Uani 1 1 d . . . . .
C3 C 0.4662(8) 0.3012(6) 0.3096(4) 0.0462(16) Uani 1 1 d . . . . .
H3 H 0.5152 0.3558 0.3356 0.055 Uiso 1 1 calc R U . . .
C2 C 0.5073(8) 0.2665(6) 0.2264(5) 0.0486(17) Uani 1 1 d . . . . .
H2 H 0.5845 0.2977 0.1955 0.058 Uiso 1 1 calc R U . . .
C17 C 0.4926(8) 0.1492(6) 0.1020(4) 0.0498(18) Uani 1 1 d . . . . .
H17A H 0.5544 0.2058 0.0702 0.060 Uiso 1 1 calc R U . . .
H17B H 0.4143 0.1476 0.0592 0.060 Uiso 1 1 calc R U . . .
C18 C 0.5708(7) 0.0242(5) 0.1268(4) 0.0388(15) Uani 1 1 d . . . . .
C19 C 0.7057(7) 0.0115(5) 0.1531(4) 0.0410(15) Uani 1 1 d . . . . .
H19 H 0.7513 0.0816 0.1505 0.049 Uiso 1 1 calc R U . . .
C20 C 0.7809(6) -0.1029(6) 0.1843(4) 0.0366(13) Uani 1 1 d . . . . .
C3AA C 0.9288(7) -0.1129(7) 0.2122(5) 0.0489(16) Uani 1 1 d . . . . .
H3AA H 0.9361 -0.1045 0.2777 0.073 Uiso 1 1 calc R U . . .
H3AB H 0.9728 -0.0490 0.1736 0.073 Uiso 1 1 calc R U . . .
H3AC H 0.9752 -0.1918 0.2036 0.073 Uiso 1 1 calc R U . . .
C22 C 0.5844(6) -0.1950(5) 0.1598(4) 0.0318(12) Uani 1 1 d . . . . .
C23 C 0.5202(7) -0.3015(5) 0.1616(4) 0.0377(14) Uani 1 1 d . . . . .
H23 H 0.5720 -0.3776 0.1831 0.045 Uiso 1 1 calc R U . . .
C24 C 0.3853(7) -0.2973(7) 0.1331(5) 0.0489(17) Uani 1 1 d . . . . .
H24 H 0.3452 -0.3701 0.1351 0.059 Uiso 1 1 calc R U . . .
C25 C 0.3068(8) -0.1869(7) 0.1013(5) 0.0507(18) Uani 1 1 d . . . . .
H25 H 0.2135 -0.1848 0.0819 0.061 Uiso 1 1 calc R U . . .
C26 C 0.3634(7) -0.0820(7) 0.0979(4) 0.0496(18) Uani 1 1 d . . . . .
H26 H 0.3085 -0.0077 0.0758 0.060 Uiso 1 1 calc R U . . .
C21 C 0.5044(7) -0.0809(5) 0.1269(4) 0.0372(14) Uani 1 1 d . . . . .
C15 C -0.0112(9) 0.4977(8) 0.8600(6) 0.076(3) Uani 1 1 d . . . . .
H15A H -0.0312 0.5367 0.9153 0.091 Uiso 1 1 calc R U . . .
H15B H -0.0917 0.4573 0.8467 0.091 Uiso 1 1 calc R U . . .
C14 C 0.0187(11) 0.5908(8) 0.7765(6) 0.082(3) Uani 1 1 d . . . . .
H14A H -0.0647 0.6489 0.7582 0.098 Uiso 1 1 calc R U . . .
H14B H 0.0940 0.6360 0.7920 0.098 Uiso 1 1 calc R U . . .
C0AA C 0.4109(16) -0.0353(12) 0.5005(10) 0.040(3) Uani 0.5 1 d . U P B -1
H0AA H 0.3315 -0.0727 0.4901 0.048 Uiso 0.5 1 calc R U P B -1
N10 N 0.2297(5) 0.3346(4) 0.6225(3) 0.0319(10) Uani 1 1 d . . . . .
O7AA O 0.9331(17) 0.1138(13) 0.4075(11) 0.104(6) Uani 0.5 1 d . . P A 1
N1 N 0.4402(6) 0.1900(4) 0.1890(3) 0.0409(13) Uani 1 1 d . . . . .
N21 N 0.7192(5) -0.2014(4) 0.1890(3) 0.0289(10) Uani 1 1 d . . . . .
N13 N 0.0605(6) 0.5242(5) 0.6988(4) 0.0451(13) Uani 1 1 d . . . . .
H13A H 0.1105 0.5696 0.6570 0.054 Uiso 1 1 calc R U . . .
H13B H -0.0160 0.5093 0.6690 0.054 Uiso 1 1 calc R U . . .
N16 N 0.1150(6) 0.4093(5) 0.8767(4) 0.0472(14) Uani 1 1 d . . . . .
H16A H 0.0966 0.3421 0.9163 0.057 Uiso 1 1 calc R U . . .
H16B H 0.1831 0.4420 0.9027 0.057 Uiso 1 1 calc R U . . .
N6 N 0.9566(8) 0.8031(6) 0.9372(5) 0.0631(17) Uani 1 1 d . . . . .
O2AA O 0.8445(6) 0.8150(5) 0.9738(4) 0.0759(19) Uani 1 1 d . . . . .
O3BA O 0.9687(9) 0.8545(7) 0.8551(5) 0.099(2) Uani 1 1 d . . . . .
O5AA O 1.0521(7) 0.7380(6) 0.9829(6) 0.095(2) Uani 1 1 d . . . . .
O7 O 0.704(4) 0.395(3) 0.085(2) 0.092(10) Uani 0.5 1 d . . P C 2
O3AA O 0.7671(8) 0.3365(6) 0.4234(6) 0.106(3) Uani 1 1 d . . . . .
O4AA O 0.5593(14) 0.1178(10) 0.6682(7) 0.061(3) Uani 0.5 1 d . U P B -1
H4AA H 0.6335 0.1489 0.6653 0.091 Uiso 0.5 1 calc R U P B -1
O13 O 0.9695(8) 0.0534(7) 0.5518(5) 0.092(2) Uani 1 1 d . . . A 1
Pd1 Pd 0.17588(5) 0.36591(4) 0.75208(3) 0.03328(17) Uani 1 1 d . . . . .
C1 C 0.6304(18) 0.0277(13) 0.4425(11) 0.044(3) Uani 0.5 1 d . U P B -1
H1 H 0.6986 0.0349 0.3960 0.053 Uiso 0.5 1 calc R U P B -1
C4 C 0.423(2) 0.0108(16) 0.5796(12) 0.042(3) Uani 0.5 1 d . U P B -1
H4 H 0.3547 0.0063 0.6262 0.050 Uiso 0.5 1 calc R U P B -1
C6AA C 0.521(2) -0.0278(15) 0.4300(11) 0.038(3) Uani 0.5 1 d . U P B -1
C1BA C 0.6453(18) 0.0745(13) 0.5218(10) 0.048(3) Uani 0.5 1 d . U P B -1
H1BA H 0.7246 0.1124 0.5316 0.057 Uiso 0.5 1 calc R U P B -1
O1AA O 0.5030(11) -0.0759(9) 0.3507(7) 0.047(2) Uani 0.5 1 d . U P B -1
H1AA H 0.4290 -0.1073 0.3539 0.071 Uiso 0.5 1 calc R U P B -1
C5AA C 0.5429(17) 0.0658(12) 0.5877(10) 0.041(3) Uani 0.5 1 d . U P B -1
N0AA N 0.5854(11) 0.4886(9) 0.0288(7) 0.036(2) Uani 0.5 1 d . . P D 1
O6 O 0.4671(12) 0.4537(9) 0.0365(6) 0.041(2) Uani 0.5 1 d . . P D 1
O1BA O 0.6117(13) 0.5763(8) -0.0284(7) 0.049(3) Uani 0.5 1 d . . P D 1
O8AA O 0.8994(17) 0.1527(11) 0.3250(9) 0.090(4) Uani 0.5 1 d . . P E 2
O6AA O 0.7559(13) 0.1366(11) 0.6744(8) 0.078(4) Uani 0.5 1 d . . P F 2
O0BA O 0.701(4) 0.428(2) 0.087(2) 0.057(6) Uani 0.5 1 d . . P D 1
O14 O -0.1423(7) 0.4249(7) 0.5869(7) 0.113(3) Uani 1 1 d . U . . .
N22 N -0.2388(10) 0.4119(11) 0.6467(9) 0.117(3) Uani 1 1 d . U . G 1
O15 O -0.2372(10) 0.4859(11) 0.7073(7) 0.145(4) Uani 1 1 d . U . G 1
O1 O -0.3406(10) 0.3888(12) 0.6241(8) 0.192(5) Uani 1 1 d . U . G 1


_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
C11 N10 1.343(8) . ?
C11 C12 1.371(8) . ?
C11 H11 0.9500 . ?
C12 C7 1.389(8) . ?
C12 H12 0.9500 . ?
N2 N2 1.13(3) 2_756 ?
N2 O13 1.184(17) 2_756 ?
N2 O7AA 1.208(17) . ?
N2 O13 1.229(16) . ?
C7 C8 1.381(9) . ?
C7 C7AA 1.490(8) . ?
C8 C9 1.365(8) . ?
C8 H8 0.9500 . ?
C9 N10 1.348(8) . ?
C9 H9 0.9500 . ?
C6 N1 1.336(9) . ?
C6 C5 1.368(8) . ?
C6 H6 0.9500 . ?
C5 C7AA 1.384(9) . ?
C5 H5 0.9500 . ?
C7AA C3 1.387(9) . ?
C3 C2 1.382(9) . ?
C3 H3 0.9500 . ?
C2 N1 1.332(9) . ?
C2 H2 0.9500 . ?
C17 N1 1.491(7) . ?
C17 C18 1.513(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.355(10) . ?
C18 C21 1.420(9) . ?
C19 C20 1.415(8) . ?
C19 H19 0.9500 . ?
C20 N21 1.321(8) . ?
C20 C3AA 1.485(9) . ?
C3AA H3AA 0.9800 . ?
C3AA H3AB 0.9800 . ?
C3AA H3AC 0.9800 . ?
C22 N21 1.371(7) . ?
C22 C23 1.420(9) . ?
C22 C21 1.436(8) . ?
C23 C24 1.373(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.395(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.361(11) . ?
C25 H25 0.9500 . ?
C26 C21 1.441(9) . ?
C26 H26 0.9500 . ?
C15 N16 1.484(9) . ?
C15 C14 1.523(12) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C14 N13 1.494(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C0AA C4 1.35(2) . ?
C0AA C6AA 1.49(2) . ?
C0AA H0AA 0.9500 . ?
N10 Pd1 2.038(5) . ?
N21 Pd1 2.066(4) 2_656 ?
N13 Pd1 2.035(5) . ?
N13 H13A 0.9100 . ?
N13 H13B 0.9100 . ?
N16 Pd1 2.031(5) . ?
N16 H16A 0.9100 . ?
N16 H16B 0.9100 . ?
N6 O2AA 1.219(9) . ?
N6 O5AA 1.237(9) . ?
N6 O3BA 1.252(9) . ?
O4AA C5AA 1.416(19) . ?
O4AA H4AA 0.8400 . ?
O13 N2 1.184(17) 2_756 ?
Pd1 N21 2.066(4) 2_656 ?
C1 C6AA 1.33(3) . ?
C1 C1BA 1.37(2) . ?
C1 H1 0.9500 . ?
C4 C5AA 1.40(3) . ?
C4 H4 0.9500 . ?
C6AA O1AA 1.38(2) . ?
C1BA C5AA 1.39(2) . ?
C1BA H1BA 0.9500 . ?
O1AA H1AA 0.8400 . ?
N0AA O6 1.143(13) 2_665 ?
N0AA O1BA 1.236(14) . ?
N0AA O6 1.262(15) . ?
N0AA O0BA 1.44(4) . ?
N0AA N0AA 1.84(2) 2_665 ?
O6 O1BA 0.892(12) 2_665 ?
O6 N0AA 1.143(13) 2_665 ?
O6 O6 1.56(2) 2_665 ?
O1BA O6 0.892(12) 2_665 ?
O14 N22 1.287(13) . ?
N22 O1 1.119(13) . ?
N22 O15 1.317(15) . ?

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
N10 C11 C12 123.0(6) . . ?
N10 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C11 C12 C7 119.6(6) . . ?
C11 C12 H12 120.2 . . ?
C7 C12 H12 120.2 . . ?
N2 N2 O13 64.0(17) 2_756 2_756 ?
N2 N2 O7AA 169(2) 2_756 . ?
O13 N2 O7AA 114.2(16) 2_756 . ?
N2 N2 O13 60.0(13) 2_756 . ?
O13 N2 O13 124.0(14) 2_756 . ?
O7AA N2 O13 120.6(18) . . ?
C8 C7 C12 117.5(5) . . ?
C8 C7 C7AA 121.6(6) . . ?
C12 C7 C7AA 120.8(5) . . ?
C9 C8 C7 119.7(6) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
N10 C9 C8 123.3(6) . . ?
N10 C9 H9 118.4 . . ?
C8 C9 H9 118.4 . . ?
N1 C6 C5 120.6(6) . . ?
N1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C5 C7AA 121.0(6) . . ?
C6 C5 H5 119.5 . . ?
C7AA C5 H5 119.5 . . ?
C5 C7AA C3 116.9(6) . . ?
C5 C7AA C7 121.3(6) . . ?
C3 C7AA C7 121.7(6) . . ?
C2 C3 C7AA 120.1(6) . . ?
C2 C3 H3 119.9 . . ?
C7AA C3 H3 119.9 . . ?
N1 C2 C3 120.8(6) . . ?
N1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
N1 C17 C18 109.0(5) . . ?
N1 C17 H17A 109.9 . . ?
C18 C17 H17A 109.9 . . ?
N1 C17 H17B 109.9 . . ?
C18 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
C19 C18 C21 118.9(5) . . ?
C19 C18 C17 119.6(6) . . ?
C21 C18 C17 121.4(6) . . ?
C18 C19 C20 122.1(6) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 H19 119.0 . . ?
N21 C20 C19 119.9(6) . . ?
N21 C20 C3AA 119.8(6) . . ?
C19 C20 C3AA 120.4(6) . . ?
C20 C3AA H3AA 109.5 . . ?
C20 C3AA H3AB 109.5 . . ?
H3AA C3AA H3AB 109.5 . . ?
C20 C3AA H3AC 109.5 . . ?
H3AA C3AA H3AC 109.5 . . ?
H3AB C3AA H3AC 109.5 . . ?
N21 C22 C23 120.7(5) . . ?
N21 C22 C21 121.1(5) . . ?
C23 C22 C21 118.2(5) . . ?
C24 C23 C22 121.7(6) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C25 120.4(7) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C26 C25 C24 120.3(7) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 121.8(6) . . ?
C25 C26 H26 119.1 . . ?
C21 C26 H26 119.1 . . ?
C18 C21 C22 117.0(6) . . ?
C18 C21 C26 125.4(6) . . ?
C22 C21 C26 117.6(6) . . ?
N16 C15 C14 106.1(7) . . ?
N16 C15 H15A 110.5 . . ?
C14 C15 H15A 110.5 . . ?
N16 C15 H15B 110.5 . . ?
C14 C15 H15B 110.5 . . ?
H15A C15 H15B 108.7 . . ?
N13 C14 C15 107.4(7) . . ?
N13 C14 H14A 110.2 . . ?
C15 C14 H14A 110.2 . . ?
N13 C14 H14B 110.2 . . ?
C15 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
C4 C0AA C6AA 120.5(16) . . ?
C4 C0AA H0AA 119.7 . . ?
C6AA C0AA H0AA 119.7 . . ?
C11 N10 C9 116.9(5) . . ?
C11 N10 Pd1 122.2(4) . . ?
C9 N10 Pd1 120.9(4) . . ?
C2 N1 C6 120.4(5) . . ?
C2 N1 C17 119.3(6) . . ?
C6 N1 C17 120.3(6) . . ?
C20 N21 C22 120.9(5) . . ?
C20 N21 Pd1 119.3(4) . 2_656 ?
C22 N21 Pd1 119.7(4) . 2_656 ?
C14 N13 Pd1 109.0(4) . . ?
C14 N13 H13A 109.9 . . ?
Pd1 N13 H13A 109.9 . . ?
C14 N13 H13B 109.9 . . ?
Pd1 N13 H13B 109.9 . . ?
H13A N13 H13B 108.3 . . ?
C15 N16 Pd1 107.8(4) . . ?
C15 N16 H16A 110.1 . . ?
Pd1 N16 H16A 110.1 . . ?
C15 N16 H16B 110.1 . . ?
Pd1 N16 H16B 110.1 . . ?
H16A N16 H16B 108.5 . . ?
O2AA N6 O5AA 117.8(8) . . ?
O2AA N6 O3BA 118.9(8) . . ?
O5AA N6 O3BA 123.3(9) . . ?
C5AA O4AA H4AA 109.5 . . ?
N2 O13 N2 56.0(14) 2_756 . ?
N16 Pd1 N13 84.0(2) . . ?
N16 Pd1 N10 175.70(19) . . ?
N13 Pd1 N10 91.7(2) . . ?
N16 Pd1 N21 93.71(19) . 2_656 ?
N13 Pd1 N21 176.0(2) . 2_656 ?
N10 Pd1 N21 90.59(17) . 2_656 ?
C6AA C1 C1BA 120.4(16) . . ?
C6AA C1 H1 119.8 . . ?
C1BA C1 H1 119.8 . . ?
C0AA C4 C5AA 115.4(17) . . ?
C0AA C4 H4 122.3 . . ?
C5AA C4 H4 122.3 . . ?
C1 C6AA O1AA 121.7(16) . . ?
C1 C6AA C0AA 120.2(15) . . ?
O1AA C6AA C0AA 118.1(17) . . ?
C1 C1BA C5AA 119.0(17) . . ?
C1 C1BA H1BA 120.5 . . ?
C5AA C1BA H1BA 120.5 . . ?
C6AA O1AA H1AA 109.5 . . ?
C1BA C5AA C4 124.5(17) . . ?
C1BA C5AA O4AA 117.8(16) . . ?
C4 C5AA O4AA 117.7(14) . . ?
O6 N0AA O1BA 43.8(7) 2_665 . ?
O6 N0AA O6 80.5(11) 2_665 . ?
O1BA N0AA O6 123.2(12) . . ?
O6 N0AA O0BA 155.3(18) 2_665 . ?
O1BA N0AA O0BA 114.6(16) . . ?
O6 N0AA O0BA 122.2(15) . . ?
O6 N0AA N0AA 42.6(7) 2_665 2_665 ?
O1BA N0AA N0AA 85.8(10) . 2_665 ?
O6 N0AA N0AA 37.9(6) . 2_665 ?
O0BA N0AA N0AA 158.6(15) . 2_665 ?
O1BA O6 N0AA 73.6(12) 2_665 2_665 ?
O1BA O6 N0AA 165.9(14) 2_665 . ?
N0AA O6 N0AA 99.5(11) 2_665 . ?
O1BA O6 O6 125.4(14) 2_665 2_665 ?
N0AA O6 O6 53.1(8) 2_665 2_665 ?
N0AA O6 O6 46.4(8) . 2_665 ?
O6 O1BA N0AA 62.5(10) 2_665 . ?
O1 N22 O14 119.1(15) . . ?
O1 N22 O15 118.9(15) . . ?
O14 N22 O15 112.1(11) . . ?

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
N10 C11 C12 C7 -0.3(9) . . . . ?
C11 C12 C7 C8 -1.0(8) . . . . ?
C11 C12 C7 C7AA 176.9(5) . . . . ?
C12 C7 C8 C9 1.5(8) . . . . ?
C7AA C7 C8 C9 -176.4(5) . . . . ?
C7 C8 C9 N10 -0.8(9) . . . . ?
N1 C6 C5 C7AA -0.1(9) . . . . ?
C6 C5 C7AA C3 1.9(8) . . . . ?
C6 C5 C7AA C7 -177.5(5) . . . . ?
C8 C7 C7AA C5 159.9(5) . . . . ?
C12 C7 C7AA C5 -18.0(8) . . . . ?
C8 C7 C7AA C3 -19.4(8) . . . . ?
C12 C7 C7AA C3 162.7(6) . . . . ?
C5 C7AA C3 C2 -1.8(9) . . . . ?
C7 C7AA C3 C2 177.6(6) . . . . ?
C7AA C3 C2 N1 -0.1(10) . . . . ?
N1 C17 C18 C19 -84.7(7) . . . . ?
N1 C17 C18 C21 92.6(7) . . . . ?
C21 C18 C19 C20 -2.7(9) . . . . ?
C17 C18 C19 C20 174.7(5) . . . . ?
C18 C19 C20 N21 -0.5(9) . . . . ?
C18 C19 C20 C3AA 179.8(6) . . . . ?
N21 C22 C23 C24 179.7(6) . . . . ?
C21 C22 C23 C24 -0.1(9) . . . . ?
C22 C23 C24 C25 0.0(10) . . . . ?
C23 C24 C25 C26 0.2(10) . . . . ?
C24 C25 C26 C21 -0.2(10) . . . . ?
C19 C18 C21 C22 3.0(8) . . . . ?
C17 C18 C21 C22 -174.3(5) . . . . ?
C19 C18 C21 C26 -177.8(6) . . . . ?
C17 C18 C21 C26 4.9(9) . . . . ?
N21 C22 C21 C18 -0.5(8) . . . . ?
C23 C22 C21 C18 179.4(5) . . . . ?
N21 C22 C21 C26 -179.7(5) . . . . ?
C23 C22 C21 C26 0.1(8) . . . . ?
C25 C26 C21 C18 -179.1(6) . . . . ?
C25 C26 C21 C22 0.0(9) . . . . ?
N16 C15 C14 N13 55.0(10) . . . . ?
C12 C11 N10 C9 1.1(8) . . . . ?
C12 C11 N10 Pd1 -178.4(4) . . . . ?
C8 C9 N10 C11 -0.5(9) . . . . ?
C8 C9 N10 Pd1 179.0(4) . . . . ?
C3 C2 N1 C6 2.0(10) . . . . ?
C3 C2 N1 C17 -176.4(6) . . . . ?
C5 C6 N1 C2 -1.9(9) . . . . ?
C5 C6 N1 C17 176.5(5) . . . . ?
C18 C17 N1 C2 101.1(7) . . . . ?
C18 C17 N1 C6 -77.3(8) . . . . ?
C19 C20 N21 C22 3.2(8) . . . . ?
C3AA C20 N21 C22 -177.1(5) . . . . ?
C19 C20 N21 Pd1 -173.4(4) . . . 2_656 ?
C3AA C20 N21 Pd1 6.3(7) . . . 2_656 ?
C23 C22 N21 C20 177.5(5) . . . . ?
C21 C22 N21 C20 -2.6(8) . . . . ?
C23 C22 N21 Pd1 -5.9(7) . . . 2_656 ?
C21 C22 N21 Pd1 173.9(4) . . . 2_656 ?
C15 C14 N13 Pd1 -37.3(9) . . . . ?
C14 C15 N16 Pd1 -46.1(9) . . . . ?
O13 N2 O13 N2 0.001(5) 2_756 . . 2_756 ?
O7AA N2 O13 N2 -167(3) . . . 2_756 ?
C6AA C0AA C4 C5AA 1(2) . . . . ?
C1BA C1 C6AA O1AA -180.0(13) . . . . ?
C1BA C1 C6AA C0AA 2(2) . . . . ?
C4 C0AA C6AA C1 -2(2) . . . . ?
C4 C0AA C6AA O1AA -179.8(10) . . . . ?
C6AA C1 C1BA C5AA -2(2) . . . . ?
C1 C1BA C5AA C4 0(2) . . . . ?
C1 C1BA C5AA O4AA -178.4(11) . . . . ?
C0AA C4 C5AA C1BA 0(2) . . . . ?
C0AA C4 C5AA O4AA 178.7(12) . . . . ?
O6 N0AA O6 O1BA 60(5) 2_665 . . 2_665 ?
O1BA N0AA O6 O1BA 70(6) . . . 2_665 ?
O0BA N0AA O6 O1BA -110(6) . . . 2_665 ?
N0AA N0AA O6 O1BA 60(5) 2_665 . . 2_665 ?
O6 N0AA O6 N0AA 0.001(1) 2_665 . . 2_665 ?
O1BA N0AA O6 N0AA 10.5(12) . . . 2_665 ?
O0BA N0AA O6 N0AA -169.5(17) . . . 2_665 ?
O1BA N0AA O6 O6 10.5(12) . . . 2_665 ?
O0BA N0AA O6 O6 -169.5(17) . . . 2_665 ?
N0AA N0AA O6 O6 -0.001(1) 2_665 . . 2_665 ?
O6 N0AA O1BA O6 -15.0(17) . . . 2_665 ?
O0BA N0AA O1BA O6 165.0(17) . . . 2_665 ?
N0AA N0AA O1BA O6 -8.6(10) 2_665 . . 2_665 ?

_refine_diff_density_max         1.617
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.153

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1478618'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H63 N16 O31 Pd2'
_chemical_formula_weight         1620.98

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7594(2)
_cell_length_b                   18.3309(4)
_cell_length_c                   19.7117(4)
_cell_angle_alpha                97.4150(10)
_cell_angle_beta                 90.7800(10)
_cell_angle_gamma                102.7820(10)
_cell_volume                     3407.00(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    29288
_cell_measurement_theta_min      5.302
_cell_measurement_theta_max      58.715

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_F_000             1654
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.627
_shelx_estimated_absorpt_T_min   0.839
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80146
_exptl_absorpt_correction_T_max  0.9286
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            123471
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.043
_diffrn_reflns_theta_max         29.865
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             19223
_reflns_number_gt                14265
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART V5.624'
_computing_cell_refinement       'Bruker SMART V5.624'
_computing_data_reduction        'SAINT V7.12A (Bruker)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP3, Chimera 1.10.2'
_computing_publication_material  'ORTEP3, Chimera 1.10.2'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0898P)²+13.7043P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19223
_refine_ls_number_parameters     934
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_ref         0.1934
_refine_ls_wR_factor_gt          0.1722
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.6275(5) 0.1475(3) 0.0788(2) 0.0291(9) Uani 1 1 d . . . . .
H1 H 0.5406 0.1625 0.0766 0.035 Uiso 1 1 calc R U . . .
C2 C 0.6609(5) 0.1169(3) 0.1354(2) 0.0285(9) Uani 1 1 d . . . . .
H2 H 0.5980 0.1120 0.1718 0.034 Uiso 1 1 calc R U . . .
C3 C 0.7865(4) 0.0932(2) 0.13957(18) 0.0217(7) Uani 1 1 d . . . . .
C4 C 0.8721(5) 0.1007(3) 0.0843(2) 0.0313(9) Uani 1 1 d . . . . .
H4 H 0.9576 0.0840 0.0841 0.038 Uiso 1 1 calc R U . . .
C5 C 0.8328(5) 0.1326(3) 0.0294(2) 0.0326(9) Uani 1 1 d . . . . .
H5 H 0.8930 0.1375 -0.0080 0.039 Uiso 1 1 calc R U . . .
C6 C 0.7874(5) 0.0332(3) 0.3153(2) 0.0307(9) Uani 1 1 d . . . . .
H6 H 0.7277 0.0288 0.3530 0.037 Uiso 1 1 calc R U . . .
C7 C 0.7443(5) 0.0573(3) 0.2573(2) 0.0300(9) Uani 1 1 d . . . . .
H7 H 0.6547 0.0695 0.2552 0.036 Uiso 1 1 calc R U . . .
C8 C 0.8297(4) 0.0644(2) 0.20124(18) 0.0216(7) Uani 1 1 d . . . . .
C9 C 0.9592(5) 0.0456(3) 0.2078(2) 0.0329(10) Uani 1 1 d . . . . .
H9 H 1.0214 0.0498 0.1711 0.039 Uiso 1 1 calc R U . . .
C10 C 0.9984(5) 0.0211(3) 0.2662(2) 0.0368(11) Uani 1 1 d . . . . .
H10 H 1.0869 0.0079 0.2693 0.044 Uiso 1 1 calc R U . . .
C11 C 0.9595(5) -0.0101(2) 0.3827(2) 0.0278(8) Uani 1 1 d . . . . .
H11A H 1.0138 -0.0493 0.3705 0.033 Uiso 1 1 calc R U . . .
H11B H 0.8761 -0.0327 0.4071 0.033 Uiso 1 1 calc R U . . .
C12 C 1.0498(5) 0.0559(2) 0.42871(19) 0.0243(8) Uani 1 1 d . . . . .
C13 C 1.1914(5) 0.0716(2) 0.4229(2) 0.0273(8) Uani 1 1 d . . . . .
H13 H 1.2328 0.0380 0.3936 0.033 Uiso 1 1 calc R U . . .
C14 C 1.2780(4) 0.1366(2) 0.4595(2) 0.0258(8) Uani 1 1 d . . . . .
C15 C 1.4324(5) 0.1528(3) 0.4489(2) 0.0354(10) Uani 1 1 d . . . . .
H15A H 1.4515 0.1749 0.4064 0.053 Uiso 1 1 calc R U . . .
H15B H 1.4653 0.1058 0.4460 0.053 Uiso 1 1 calc R U . . .
H15C H 1.4819 0.1884 0.4876 0.053 Uiso 1 1 calc R U . . .
C16 C 1.0820(4) 0.1669(2) 0.51455(19) 0.0214(7) Uani 1 1 d . . . . .
C17 C 0.9902(4) 0.1031(2) 0.47738(18) 0.0224(7) Uani 1 1 d . . . . .
C18 C 0.8453(5) 0.0900(3) 0.4908(2) 0.0308(9) Uani 1 1 d . . . . .
H18 H 0.7814 0.0481 0.4659 0.037 Uiso 1 1 calc R U . . .
C19 C 0.7965(5) 0.1374(3) 0.5396(2) 0.0357(10) Uani 1 1 d . . . . .
H19 H 0.6991 0.1279 0.5483 0.043 Uiso 1 1 calc R U . . .
C20 C 0.8895(5) 0.1998(3) 0.5769(2) 0.0354(10) Uani 1 1 d . . . . .
H20 H 0.8544 0.2321 0.6105 0.042 Uiso 1 1 calc R U . . .
C21 C 1.0292(5) 0.2141(2) 0.5653(2) 0.0274(8) Uani 1 1 d . . . . .
H21 H 1.0915 0.2559 0.5912 0.033 Uiso 1 1 calc R U . . .
C22 C 1.1722(5) 0.3634(2) 0.4687(2) 0.0281(8) Uani 1 1 d . . . . .
H22 H 1.1205 0.3612 0.5092 0.034 Uiso 1 1 calc R U . . .
C23 C 1.1259(5) 0.3966(2) 0.4162(2) 0.0282(8) Uani 1 1 d . . . . .
H23 H 1.0455 0.4177 0.4211 0.034 Uiso 1 1 calc R U . . .
C24 C 1.1984(4) 0.3985(2) 0.3563(2) 0.0239(8) Uani 1 1 d . . . . .
C25 C 1.3189(5) 0.3686(3) 0.3529(2) 0.0326(9) Uani 1 1 d . . . . .
H25 H 1.3723 0.3698 0.3129 0.039 Uiso 1 1 calc R U . . .
C26 C 1.3594(5) 0.3376(3) 0.4076(2) 0.0330(10) Uani 1 1 d . . . . .
H26 H 1.4415 0.3178 0.4049 0.040 Uiso 1 1 calc R U . . .
C27 C 0.9622(5) 0.4621(2) 0.2339(2) 0.0259(8) Uani 1 1 d . . . . .
H27 H 0.8673 0.4662 0.2297 0.031 Uiso 1 1 calc R U . . .
C28 C 1.0071(4) 0.4340(2) 0.2899(2) 0.0255(8) Uani 1 1 d . . . . .
H28 H 0.9427 0.4182 0.3237 0.031 Uiso 1 1 calc R U . . .
C29 C 1.1477(4) 0.4287(2) 0.29690(19) 0.0223(7) Uani 1 1 d . . . . .
C30 C 1.2375(5) 0.4507(2) 0.2454(2) 0.0281(8) Uani 1 1 d . . . . .
H30 H 1.3329 0.4470 0.2482 0.034 Uiso 1 1 calc R U . . .
C31 C 1.1880(5) 0.4780(3) 0.1904(2) 0.0302(9) Uani 1 1 d . . . . .
H31 H 1.2499 0.4929 0.1554 0.036 Uiso 1 1 calc R U . . .
C32 C 0.9988(5) 0.5109(2) 0.1239(2) 0.0286(8) Uani 1 1 d . . . . .
H32A H 1.0783 0.5397 0.1008 0.034 Uiso 1 1 calc R U . . .
H32B H 0.9354 0.5448 0.1384 0.034 Uiso 1 1 calc R U . . .
C33 C 0.9203(4) 0.4441(2) 0.07540(19) 0.0247(8) Uani 1 1 d . . . . .
C34 C 0.7777(5) 0.4214(2) 0.0776(2) 0.0272(8) Uani 1 1 d . . . . .
H34 H 0.7274 0.4513 0.1060 0.033 Uiso 1 1 calc R U . . .
C35 C 0.7048(4) 0.3545(3) 0.0383(2) 0.0266(8) Uani 1 1 d . . . . .
C36 C 0.9925(4) 0.4009(2) 0.02875(19) 0.0223(7) Uani 1 1 d . . . . .
C37 C 0.9142(4) 0.3346(2) -0.00993(18) 0.0222(7) Uani 1 1 d . . . . .
C38 C 0.9813(5) 0.2908(3) -0.0571(2) 0.0288(8) Uani 1 1 d . . . . .
H38 H 0.9280 0.2462 -0.0834 0.035 Uiso 1 1 calc R U . . .
C39 C 1.1213(5) 0.3123(3) -0.0650(2) 0.0377(11) Uani 1 1 d . . . . .
H39 H 1.1659 0.2821 -0.0962 0.045 Uiso 1 1 calc R U . . .
C40 C 1.2016(5) 0.3788(3) -0.0273(2) 0.0378(11) Uani 1 1 d . . . . .
H40 H 1.2997 0.3934 -0.0337 0.045 Uiso 1 1 calc R U . . .
C41 C 1.1394(5) 0.4226(3) 0.0183(2) 0.0329(9) Uani 1 1 d . . . . .
H41 H 1.1943 0.4676 0.0431 0.039 Uiso 1 1 calc R U . . .
C42 C 0.5485(5) 0.3314(3) 0.0450(2) 0.0317(9) Uani 1 1 d . . . . .
H42A H 0.5064 0.2963 0.0045 0.047 Uiso 1 1 calc R U . . .
H42B H 0.5084 0.3762 0.0486 0.047 Uiso 1 1 calc R U . . .
H42C H 0.5288 0.3066 0.0861 0.047 Uiso 1 1 calc R U . . .
C43 C 0.4882(5) 0.1979(3) -0.1721(2) 0.0332(9) Uani 1 1 d . . . . .
H43A H 0.4755 0.2098 -0.2190 0.040 Uiso 1 1 calc R U . . .
H43B H 0.4012 0.2004 -0.1475 0.040 Uiso 1 1 calc R U . . .
C44 C 0.5168(5) 0.1199(3) -0.1748(2) 0.0353(10) Uani 1 1 d . . . . .
H44A H 0.4323 0.0812 -0.1931 0.042 Uiso 1 1 calc R U . . .
H44B H 0.5953 0.1150 -0.2051 0.042 Uiso 1 1 calc R U . . .
C45 C 1.5411(5) 0.2997(3) 0.6571(2) 0.0318(9) Uani 1 1 d . . . . .
H45A H 1.6214 0.2934 0.6286 0.038 Uiso 1 1 calc R U . . .
H45B H 1.5621 0.2903 0.7041 0.038 Uiso 1 1 calc R U . . .
C46 C 1.5169(5) 0.3786(3) 0.6583(2) 0.0315(9) Uani 1 1 d . . . . .
H46A H 1.4440 0.3867 0.6910 0.038 Uiso 1 1 calc R U . . .
H46B H 1.6049 0.4165 0.6728 0.038 Uiso 1 1 calc R U . . .
C47 C 1.0661(6) 0.2215(3) 0.2786(3) 0.0377(10) Uani 1 1 d . . . . .
C48 C 0.9650(5) 0.2490(2) 0.2466(2) 0.0307(9) Uani 1 1 d . . . . .
H48 H 0.8809 0.2535 0.2688 0.037 Uiso 1 1 calc R U . . .
C49 C 0.9874(5) 0.2701(3) 0.1818(2) 0.0349(10) Uani 1 1 d . . . . .
C50 C 1.1095(6) 0.2647(3) 0.1489(3) 0.0452(12) Uani 1 1 d . . . . .
H50 H 1.1245 0.2795 0.1047 0.054 Uiso 1 1 calc R U . . .
C51 C 1.2097(6) 0.2370(4) 0.1819(3) 0.0530(14) Uani 1 1 d . . . . .
H51 H 1.2942 0.2330 0.1598 0.064 Uiso 1 1 calc R U . . .
C52 C 1.1894(6) 0.2151(3) 0.2460(3) 0.0485(13) Uani 1 1 d . . . . .
H52 H 1.2588 0.1959 0.2677 0.058 Uiso 1 1 calc R U . . .
N1 N 0.7136(4) 0.15676(19) 0.02681(16) 0.0238(7) Uani 1 1 d . . . . .
N2 N 0.9136(4) 0.01563(18) 0.31924(16) 0.0233(7) Uani 1 1 d . . . . .
N3 N 1.2243(3) 0.18363(19) 0.50281(16) 0.0218(6) Uani 1 1 d . . . . .
N4 N 1.2865(4) 0.3345(2) 0.46496(18) 0.0261(7) Uani 1 1 d . . . . .
N5 N 1.0529(4) 0.48376(19) 0.18525(16) 0.0246(7) Uani 1 1 d . . . . .
N6 N 0.7707(4) 0.31137(19) -0.00316(16) 0.0228(6) Uani 1 1 d . . . . .
N7 N 0.6108(4) 0.2533(2) -0.13542(17) 0.0262(7) Uani 1 1 d . . . . .
H7A H 0.5870 0.2981 -0.1218 0.031 Uiso 1 1 calc R U . . .
H7B H 0.6842 0.2616 -0.1635 0.031 Uiso 1 1 calc R U . . .
N8 N 0.5542(4) 0.1093(2) -0.10404(18) 0.0285(7) Uani 1 1 d . . . . .
H8A H 0.6067 0.0738 -0.1055 0.034 Uiso 1 1 calc R U . . .
H8B H 0.4745 0.0927 -0.0818 0.034 Uiso 1 1 calc R U . . .
N9 N 1.4094(4) 0.2461(2) 0.62764(17) 0.0253(7) Uani 1 1 d . . . . .
H9A H 1.3418 0.2426 0.6591 0.030 Uiso 1 1 calc R U . . .
H9B H 1.4260 0.1994 0.6153 0.030 Uiso 1 1 calc R U . . .
N10 N 1.4702(4) 0.3864(2) 0.58781(19) 0.0282(7) Uani 1 1 d . . . . .
H10A H 1.5464 0.3991 0.5621 0.034 Uiso 1 1 calc R U . . .
H10B H 1.4215 0.4235 0.5896 0.034 Uiso 1 1 calc R U . . .
N11 N 0.0348(4) 0.5947(2) 0.3694(2) 0.0322(8) Uani 1 1 d . . . . .
N12 N 0.2322(5) 0.7418(3) 0.5887(3) 0.0530(12) Uani 1 1 d . . . . .
N13 N 0.5276(5) 0.4273(3) 0.8839(2) 0.0426(10) Uani 1 1 d . . . . .
N14 N 0.4924(4) 0.0731(2) 0.6281(2) 0.0375(9) Uani 1 1 d . . . . .
N15 N 0.1345(4) 0.2089(2) 0.7411(2) 0.0348(8) Uani 1 1 d . . . . .
N16 N 0.2381(5) 0.0801(3) 0.9758(3) 0.0496(12) Uani 1 1 d . . . . .
O1 O 1.0508(5) 0.2002(2) 0.34255(19) 0.0477(9) Uani 1 1 d . . . . .
H1A H 0.9699 0.2022 0.3556 0.072 Uiso 1 1 calc R U . . .
O2 O 0.8922(4) 0.2962(2) 0.14757(17) 0.0393(8) Uani 1 1 d . . . . .
H2A H 0.8224 0.2978 0.1717 0.059 Uiso 1 1 calc R U . . .
O3 O 0.0279(4) 0.5584(2) 0.41952(18) 0.0390(8) Uani 1 1 d . . . . .
O4 O -0.0750(4) 0.6085(2) 0.3467(2) 0.0448(9) Uani 1 1 d . . . . .
O5 O 0.1496(3) 0.61498(19) 0.34216(18) 0.0386(8) Uani 1 1 d . . . . .
O6 O 0.1247(8) 0.7148(4) 0.5546(6) 0.156(4) Uani 1 1 d . . . . .
O7 O 0.2422(6) 0.8013(3) 0.6275(3) 0.0741(15) Uani 1 1 d . . . . .
O8 O 0.3291(6) 0.7075(3) 0.5860(4) 0.104(2) Uani 1 1 d . . . . .
O9 O 0.5125(4) 0.4927(2) 0.8800(3) 0.0575(11) Uani 1 1 d . . . . .
O10 O 0.6366(4) 0.4175(2) 0.9102(2) 0.0456(9) Uani 1 1 d . . . . .
O11 O 0.4347(4) 0.3693(2) 0.8598(3) 0.0551(11) Uani 1 1 d . . . . .
O12 O 0.3916(4) 0.0785(2) 0.59084(19) 0.0411(8) Uani 1 1 d . . . . .
O13 O 0.5144(4) 0.0100(2) 0.6357(2) 0.0503(10) Uani 1 1 d . . . . .
O14 O 0.5737(4) 0.1336(2) 0.65820(19) 0.0404(8) Uani 1 1 d . . . . .
O15 O 0.1995(4) 0.2702(2) 0.7266(2) 0.0492(9) Uani 1 1 d . . . . .
O16 O 0.1756(4) 0.1508(2) 0.7235(2) 0.0520(10) Uani 1 1 d . . . . .
O17 O 0.0232(4) 0.2067(2) 0.7743(2) 0.0507(10) Uani 1 1 d . . . . .
O18 O 0.2425(4) 0.0966(2) 0.9161(2) 0.0532(10) Uani 1 1 d . . . . .
O19 O 0.3438(5) 0.0689(3) 1.0031(2) 0.0639(13) Uani 1 1 d . . . . .
O20 O 0.1257(6) 0.0710(4) 1.0046(3) 0.093(2) Uani 1 1 d . . . . .
O21 O 0.2980(4) 0.4976(2) 0.60117(18) 0.0395(8) Uani 1 1 d . . . . .
O22 O 0.2840(4) 0.5800(2) 0.4949(2) 0.0423(8) Uani 1 1 d . . . . .
O23 O 0.2433(4) 0.4271(2) 0.7874(2) 0.0394(8) Uani 1 1 d D . . . .
O24 O 0.4056(4) 0.5539(2) 0.73528(18) 0.0390(8) Uani 1 1 d . . . . .
O25 O 0.4772(5) 0.7969(3) 0.7155(2) 0.0660(12) Uani 1 1 d . . . . .
O26 O 0.3501(4) 0.6923(2) 0.7923(2) 0.0502(9) Uani 1 1 d . . . . .
O27 O 0.6112(4) 0.9427(2) 0.7518(2) 0.0523(10) Uani 1 1 d . . . . .
O28 O 0.8010(4) 0.0869(2) 0.7105(2) 0.0467(9) Uani 1 1 d . . . . .
O29 O 0.8517(4) 0.3140(3) 0.7804(2) 0.0481(9) Uani 1 1 d D . . . .
O30 O 0.9748(4) 0.1095(2) 0.8763(2) 0.0477(9) Uani 1 1 d . . . . .
O31 O 0.7360(5) 0.0014(2) 0.8780(2) 0.0545(10) Uani 1 1 d . . . . .
Pd1 Pd 0.66502(3) 0.20857(2) -0.05277(2) 0.02323(9) Uani 1 1 d . . . . .
Pd2 Pd 1.34575(3) 0.28649(2) 0.54476(2) 0.02242(9) Uani 1 1 d . . . . .
H22A H 0.284(4) 0.628(2) 0.521(2) 0.010(9) Uiso 1 1 d . . . . .
H129 H 0.910(6) 0.283(3) 0.763(3) 0.07(2) Uiso 1 1 d D . . . .
H22B H 0.204(6) 0.573(3) 0.465(3) 0.035(14) Uiso 1 1 d . . . . .
H123 H 0.213(8) 0.382(2) 0.755(3) 0.08(3) Uiso 1 1 d D . . . .
H124 H 0.298(12) 0.408(6) 0.810(6) 0.14(4) Uiso 1 1 d . . . . .


_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 N1 1.337(5) . ?
C1 C2 1.378(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.393(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(5) . ?
C3 C8 1.478(5) . ?
C4 C5 1.382(6) . ?
C4 H4 0.9500 . ?
C5 N1 1.336(6) . ?
C5 H5 0.9500 . ?
C6 N2 1.343(6) . ?
C6 C7 1.373(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.395(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.391(6) . ?
C9 C10 1.367(6) . ?
C9 H9 0.9500 . ?
C10 N2 1.343(5) . ?
C10 H10 0.9500 . ?
C11 N2 1.489(5) . ?
C11 C12 1.512(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.357(6) . ?
C12 C17 1.427(5) . ?
C13 C14 1.403(6) . ?
C13 H13 0.9500 . ?
C14 N3 1.330(5) . ?
C14 C15 1.493(6) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N3 1.384(5) . ?
C16 C21 1.415(5) . ?
C16 C17 1.415(6) . ?
C17 C18 1.415(6) . ?
C18 C19 1.374(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.406(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.359(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 N4 1.337(5) . ?
C22 C23 1.385(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.402(6) . ?
C24 C29 1.481(5) . ?
C25 C26 1.375(6) . ?
C25 H25 0.9500 . ?
C26 N4 1.344(5) . ?
C26 H26 0.9500 . ?
C27 N5 1.352(5) . ?
C27 C28 1.381(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.403(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.391(5) . ?
C30 C31 1.375(6) . ?
C30 H30 0.9500 . ?
C31 N5 1.349(6) . ?
C31 H31 0.9500 . ?
C32 N5 1.497(5) . ?
C32 C33 1.506(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.364(6) . ?
C33 C36 1.430(5) . ?
C34 C35 1.402(6) . ?
C34 H34 0.9500 . ?
C35 N6 1.333(5) . ?
C35 C42 1.502(6) . ?
C36 C37 1.407(6) . ?
C36 C41 1.426(6) . ?
C37 N6 1.384(5) . ?
C37 C38 1.412(6) . ?
C38 C39 1.353(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.408(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.365(7) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N7 1.495(6) . ?
C43 C44 1.511(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N8 1.485(5) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N9 1.493(5) . ?
C45 C46 1.513(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 N10 1.490(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O1 1.368(6) . ?
C47 C48 1.382(7) . ?
C47 C52 1.392(8) . ?
C48 C49 1.388(6) . ?
C48 H48 0.9500 . ?
C49 O2 1.346(6) . ?
C49 C50 1.380(7) . ?
C50 C51 1.388(9) . ?
C50 H50 0.9500 . ?
C51 C52 1.378(8) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
N1 Pd1 2.037(3) . ?
N3 Pd2 2.056(3) . ?
N4 Pd2 2.035(3) . ?
N6 Pd1 2.051(3) . ?
N7 Pd1 2.030(3) . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N8 Pd1 2.032(4) . ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N9 Pd2 2.022(3) . ?
N9 H9A 0.9100 . ?
N9 H9B 0.9100 . ?
N10 Pd2 2.033(4) . ?
N10 H10A 0.9100 . ?
N10 H10B 0.9100 . ?
N11 O4 1.245(5) . ?
N11 O5 1.252(5) . ?
N11 O3 1.255(5) . ?
N12 O6 1.209(8) . ?
N12 O7 1.232(7) . ?
N12 O8 1.245(7) . ?
N13 O10 1.236(6) . ?
N13 O9 1.251(6) . ?
N13 O11 1.270(6) . ?
N14 O12 1.249(5) . ?
N14 O13 1.249(5) . ?
N14 O14 1.281(6) . ?
N15 O16 1.231(5) . ?
N15 O15 1.233(5) . ?
N15 O17 1.272(5) . ?
N16 O19 1.226(7) . ?
N16 O20 1.230(6) . ?
N16 O18 1.252(6) . ?
O1 H1A 0.8400 . ?
O2 H2A 0.8400 . ?
O22 H22A 0.96(4) . ?
O22 H22B 0.95(6) . ?
O23 H123 0.957(5) . ?
O23 H124 0.84(11) . ?
O29 H129 0.92(2) . ?

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 C1 C2 122.1(4) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 120.3(4) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 C2 116.9(4) . . ?
C4 C3 C8 121.3(4) . . ?
C2 C3 C8 121.8(3) . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 122.7(4) . . ?
N1 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
N2 C6 C7 120.3(4) . . ?
N2 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C8 121.1(4) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C9 C8 C7 116.3(4) . . ?
C9 C8 C3 122.1(3) . . ?
C7 C8 C3 121.5(4) . . ?
C10 C9 C8 121.0(4) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
N2 C10 C9 120.9(4) . . ?
N2 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
N2 C11 C12 110.0(3) . . ?
N2 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
N2 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C13 C12 C17 118.8(4) . . ?
C13 C12 C11 119.4(4) . . ?
C17 C12 C11 121.8(4) . . ?
C12 C13 C14 121.3(4) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
N3 C14 C13 121.0(4) . . ?
N3 C14 C15 120.0(4) . . ?
C13 C14 C15 119.0(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 C21 118.9(4) . . ?
N3 C16 C17 121.0(3) . . ?
C21 C16 C17 120.1(4) . . ?
C18 C17 C16 118.2(4) . . ?
C18 C17 C12 124.0(4) . . ?
C16 C17 C12 117.8(4) . . ?
C19 C18 C17 120.5(4) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 120.6(4) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C21 C20 C19 120.5(4) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C16 120.0(4) . . ?
C20 C21 H21 120.0 . . ?
C16 C21 H21 120.0 . . ?
N4 C22 C23 122.8(4) . . ?
N4 C22 H22 118.6 . . ?
C23 C22 H22 118.6 . . ?
C22 C23 C24 119.1(4) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C23 C24 C25 117.8(4) . . ?
C23 C24 C29 121.1(4) . . ?
C25 C24 C29 121.0(4) . . ?
C26 C25 C24 119.7(4) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
N4 C26 C25 122.1(4) . . ?
N4 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
N5 C27 C28 120.3(4) . . ?
N5 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C27 C28 C29 120.1(4) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 118.0(4) . . ?
C30 C29 C24 120.8(4) . . ?
C28 C29 C24 121.2(3) . . ?
C31 C30 C29 119.9(4) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
N5 C31 C30 121.1(4) . . ?
N5 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
N5 C32 C33 109.2(3) . . ?
N5 C32 H32A 109.8 . . ?
C33 C32 H32A 109.8 . . ?
N5 C32 H32B 109.8 . . ?
C33 C32 H32B 109.8 . . ?
H32A C32 H32B 108.3 . . ?
C34 C33 C36 118.6(4) . . ?
C34 C33 C32 119.9(4) . . ?
C36 C33 C32 121.4(4) . . ?
C33 C34 C35 120.6(4) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
N6 C35 C34 121.8(4) . . ?
N6 C35 C42 120.3(4) . . ?
C34 C35 C42 117.9(4) . . ?
C37 C36 C41 118.2(4) . . ?
C37 C36 C33 118.4(4) . . ?
C41 C36 C33 123.4(4) . . ?
N6 C37 C36 121.0(4) . . ?
N6 C37 C38 118.8(4) . . ?
C36 C37 C38 120.1(4) . . ?
C39 C38 C37 120.1(4) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C38 C39 C40 120.8(4) . . ?
C38 C39 H39 119.6 . . ?
C40 C39 H39 119.6 . . ?
C41 C40 C39 120.4(4) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C40 C41 C36 120.4(4) . . ?
C40 C41 H41 119.8 . . ?
C36 C41 H41 119.8 . . ?
C35 C42 H42A 109.5 . . ?
C35 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C35 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N7 C43 C44 108.1(4) . . ?
N7 C43 H43A 110.1 . . ?
C44 C43 H43A 110.1 . . ?
N7 C43 H43B 110.1 . . ?
C44 C43 H43B 110.1 . . ?
H43A C43 H43B 108.4 . . ?
N8 C44 C43 107.7(4) . . ?
N8 C44 H44A 110.2 . . ?
C43 C44 H44A 110.2 . . ?
N8 C44 H44B 110.2 . . ?
C43 C44 H44B 110.2 . . ?
H44A C44 H44B 108.5 . . ?
N9 C45 C46 107.0(3) . . ?
N9 C45 H45A 110.3 . . ?
C46 C45 H45A 110.3 . . ?
N9 C45 H45B 110.3 . . ?
C46 C45 H45B 110.3 . . ?
H45A C45 H45B 108.6 . . ?
N10 C46 C45 107.8(4) . . ?
N10 C46 H46A 110.1 . . ?
C45 C46 H46A 110.1 . . ?
N10 C46 H46B 110.1 . . ?
C45 C46 H46B 110.1 . . ?
H46A C46 H46B 108.5 . . ?
O1 C47 C48 122.3(5) . . ?
O1 C47 C52 117.5(5) . . ?
C48 C47 C52 120.1(5) . . ?
C47 C48 C49 119.5(5) . . ?
C47 C48 H48 120.3 . . ?
C49 C48 H48 120.3 . . ?
O2 C49 C50 116.6(4) . . ?
O2 C49 C48 122.3(4) . . ?
C50 C49 C48 121.2(5) . . ?
C49 C50 C51 118.5(5) . . ?
C49 C50 H50 120.8 . . ?
C51 C50 H50 120.8 . . ?
C52 C51 C50 121.4(5) . . ?
C52 C51 H51 119.3 . . ?
C50 C51 H51 119.3 . . ?
C51 C52 C47 119.3(5) . . ?
C51 C52 H52 120.3 . . ?
C47 C52 H52 120.3 . . ?
C5 N1 C1 118.2(3) . . ?
C5 N1 Pd1 121.3(3) . . ?
C1 N1 Pd1 120.5(3) . . ?
C10 N2 C6 120.3(4) . . ?
C10 N2 C11 119.9(4) . . ?
C6 N2 C11 119.8(3) . . ?
C14 N3 C16 119.9(4) . . ?
C14 N3 Pd2 120.7(3) . . ?
C16 N3 Pd2 119.1(3) . . ?
C22 N4 C26 118.5(4) . . ?
C22 N4 Pd2 119.9(3) . . ?
C26 N4 Pd2 121.6(3) . . ?
C31 N5 C27 120.7(3) . . ?
C31 N5 C32 120.6(3) . . ?
C27 N5 C32 118.6(4) . . ?
C35 N6 C37 119.4(4) . . ?
C35 N6 Pd1 121.1(3) . . ?
C37 N6 Pd1 119.4(3) . . ?
C43 N7 Pd1 107.4(2) . . ?
C43 N7 H7A 110.2 . . ?
Pd1 N7 H7A 110.2 . . ?
C43 N7 H7B 110.2 . . ?
Pd1 N7 H7B 110.2 . . ?
H7A N7 H7B 108.5 . . ?
C44 N8 Pd1 109.8(3) . . ?
C44 N8 H8A 109.7 . . ?
Pd1 N8 H8A 109.7 . . ?
C44 N8 H8B 109.7 . . ?
Pd1 N8 H8B 109.7 . . ?
H8A N8 H8B 108.2 . . ?
C45 N9 Pd2 107.6(2) . . ?
C45 N9 H9A 110.2 . . ?
Pd2 N9 H9A 110.2 . . ?
C45 N9 H9B 110.2 . . ?
Pd2 N9 H9B 110.2 . . ?
H9A N9 H9B 108.5 . . ?
C46 N10 Pd2 109.0(3) . . ?
C46 N10 H10A 109.9 . . ?
Pd2 N10 H10A 109.9 . . ?
C46 N10 H10B 109.9 . . ?
Pd2 N10 H10B 109.9 . . ?
H10A N10 H10B 108.3 . . ?
O4 N11 O5 121.0(4) . . ?
O4 N11 O3 118.7(4) . . ?
O5 N11 O3 120.3(4) . . ?
O6 N12 O7 119.7(7) . . ?
O6 N12 O8 119.3(7) . . ?
O7 N12 O8 120.9(6) . . ?
O10 N13 O9 120.3(5) . . ?
O10 N13 O11 117.8(5) . . ?
O9 N13 O11 121.9(5) . . ?
O12 N14 O13 120.9(5) . . ?
O12 N14 O14 118.8(4) . . ?
O13 N14 O14 120.4(4) . . ?
O16 N15 O15 120.9(4) . . ?
O16 N15 O17 120.4(4) . . ?
O15 N15 O17 118.7(4) . . ?
O19 N16 O20 121.1(5) . . ?
O19 N16 O18 119.5(5) . . ?
O20 N16 O18 119.3(6) . . ?
C47 O1 H1A 109.5 . . ?
C49 O2 H2A 109.5 . . ?
H22A O22 H22B 102(4) . . ?
H123 O23 H124 94(8) . . ?
N7 Pd1 N8 84.41(14) . . ?
N7 Pd1 N1 176.22(14) . . ?
N8 Pd1 N1 91.82(14) . . ?
N7 Pd1 N6 93.25(13) . . ?
N8 Pd1 N6 177.29(14) . . ?
N1 Pd1 N6 90.52(13) . . ?
N9 Pd2 N10 84.49(14) . . ?
N9 Pd2 N4 175.99(14) . . ?
N10 Pd2 N4 91.66(14) . . ?
N9 Pd2 N3 93.80(13) . . ?
N10 Pd2 N3 178.06(13) . . ?
N4 Pd2 N3 90.06(14) . . ?

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
N1 C1 C2 C3 -1.1(7) . . . . ?
C1 C2 C3 C4 -1.1(6) . . . . ?
C1 C2 C3 C8 176.2(4) . . . . ?
C2 C3 C4 C5 1.8(7) . . . . ?
C8 C3 C4 C5 -175.6(4) . . . . ?
C3 C4 C5 N1 -0.3(8) . . . . ?
N2 C6 C7 C8 -0.1(7) . . . . ?
C6 C7 C8 C9 0.1(7) . . . . ?
C6 C7 C8 C3 -177.6(4) . . . . ?
C4 C3 C8 C9 1.9(6) . . . . ?
C2 C3 C8 C9 -175.4(4) . . . . ?
C4 C3 C8 C7 179.4(4) . . . . ?
C2 C3 C8 C7 2.2(6) . . . . ?
C7 C8 C9 C10 0.4(7) . . . . ?
C3 C8 C9 C10 178.1(4) . . . . ?
C8 C9 C10 N2 -0.9(8) . . . . ?
N2 C11 C12 C13 -91.4(4) . . . . ?
N2 C11 C12 C17 87.4(4) . . . . ?
C17 C12 C13 C14 -5.4(6) . . . . ?
C11 C12 C13 C14 173.4(4) . . . . ?
C12 C13 C14 N3 2.3(6) . . . . ?
C12 C13 C14 C15 -177.5(4) . . . . ?
N3 C16 C17 C18 -178.7(3) . . . . ?
C21 C16 C17 C18 2.1(5) . . . . ?
N3 C16 C17 C12 1.5(5) . . . . ?
C21 C16 C17 C12 -177.6(3) . . . . ?
C13 C12 C17 C18 -176.3(4) . . . . ?
C11 C12 C17 C18 4.9(6) . . . . ?
C13 C12 C17 C16 3.5(5) . . . . ?
C11 C12 C17 C16 -175.3(3) . . . . ?
C16 C17 C18 C19 -1.2(6) . . . . ?
C12 C17 C18 C19 178.6(4) . . . . ?
C17 C18 C19 C20 0.2(7) . . . . ?
C18 C19 C20 C21 -0.1(7) . . . . ?
C19 C20 C21 C16 1.0(7) . . . . ?
N3 C16 C21 C20 178.8(4) . . . . ?
C17 C16 C21 C20 -2.1(6) . . . . ?
N4 C22 C23 C24 1.6(7) . . . . ?
C22 C23 C24 C25 -2.1(6) . . . . ?
C22 C23 C24 C29 175.9(4) . . . . ?
C23 C24 C25 C26 1.1(7) . . . . ?
C29 C24 C25 C26 -176.8(4) . . . . ?
C24 C25 C26 N4 0.4(8) . . . . ?
N5 C27 C28 C29 0.8(6) . . . . ?
C27 C28 C29 C30 -1.5(6) . . . . ?
C27 C28 C29 C24 -179.8(4) . . . . ?
C23 C24 C29 C30 161.4(4) . . . . ?
C25 C24 C29 C30 -20.7(6) . . . . ?
C23 C24 C29 C28 -20.4(6) . . . . ?
C25 C24 C29 C28 157.5(4) . . . . ?
C28 C29 C30 C31 1.1(6) . . . . ?
C24 C29 C30 C31 179.4(4) . . . . ?
C29 C30 C31 N5 0.0(7) . . . . ?
N5 C32 C33 C34 95.3(4) . . . . ?
N5 C32 C33 C36 -81.6(4) . . . . ?
C36 C33 C34 C35 4.2(6) . . . . ?
C32 C33 C34 C35 -172.8(3) . . . . ?
C33 C34 C35 N6 -1.0(6) . . . . ?
C33 C34 C35 C42 177.9(4) . . . . ?
C34 C33 C36 C37 -3.7(5) . . . . ?
C32 C33 C36 C37 173.3(3) . . . . ?
C34 C33 C36 C41 174.9(4) . . . . ?
C32 C33 C36 C41 -8.1(6) . . . . ?
C41 C36 C37 N6 -178.6(3) . . . . ?
C33 C36 C37 N6 0.0(5) . . . . ?
C41 C36 C37 C38 0.6(5) . . . . ?
C33 C36 C37 C38 179.3(4) . . . . ?
N6 C37 C38 C39 179.8(4) . . . . ?
C36 C37 C38 C39 0.5(6) . . . . ?
C37 C38 C39 C40 -1.1(7) . . . . ?
C38 C39 C40 C41 0.6(7) . . . . ?
C39 C40 C41 C36 0.6(7) . . . . ?
C37 C36 C41 C40 -1.1(6) . . . . ?
C33 C36 C41 C40 -179.7(4) . . . . ?
N7 C43 C44 N8 52.1(5) . . . . ?
N9 C45 C46 N10 -53.7(5) . . . . ?
O1 C47 C48 C49 179.7(4) . . . . ?
C52 C47 C48 C49 0.1(7) . . . . ?
C47 C48 C49 O2 179.0(4) . . . . ?
C47 C48 C49 C50 -0.6(7) . . . . ?
O2 C49 C50 C51 -179.1(5) . . . . ?
C48 C49 C50 C51 0.5(8) . . . . ?
C49 C50 C51 C52 0.1(9) . . . . ?
C50 C51 C52 C47 -0.5(9) . . . . ?
O1 C47 C52 C51 -179.1(5) . . . . ?
C48 C47 C52 C51 0.5(8) . . . . ?
C4 C5 N1 C1 -2.0(7) . . . . ?
C4 C5 N1 Pd1 176.6(4) . . . . ?
C2 C1 N1 C5 2.6(7) . . . . ?
C2 C1 N1 Pd1 -176.0(3) . . . . ?
C9 C10 N2 C6 0.9(7) . . . . ?
C9 C10 N2 C11 -179.2(4) . . . . ?
C7 C6 N2 C10 -0.4(7) . . . . ?
C7 C6 N2 C11 179.7(4) . . . . ?
C12 C11 N2 C10 84.4(5) . . . . ?
C12 C11 N2 C6 -95.7(5) . . . . ?
C13 C14 N3 C16 2.8(6) . . . . ?
C15 C14 N3 C16 -177.4(4) . . . . ?
C13 C14 N3 Pd2 -170.5(3) . . . . ?
C15 C14 N3 Pd2 9.3(5) . . . . ?
C21 C16 N3 C14 174.5(4) . . . . ?
C17 C16 N3 C14 -4.7(5) . . . . ?
C21 C16 N3 Pd2 -12.1(5) . . . . ?
C17 C16 N3 Pd2 168.8(3) . . . . ?
C23 C22 N4 C26 -0.1(7) . . . . ?
C23 C22 N4 Pd2 -179.7(3) . . . . ?
C25 C26 N4 C22 -0.9(7) . . . . ?
C25 C26 N4 Pd2 178.7(4) . . . . ?
C30 C31 N5 C27 -0.7(7) . . . . ?
C30 C31 N5 C32 -177.9(4) . . . . ?
C28 C27 N5 C31 0.3(6) . . . . ?
C28 C27 N5 C32 177.5(4) . . . . ?
C33 C32 N5 C31 99.6(5) . . . . ?
C33 C32 N5 C27 -77.6(5) . . . . ?
C34 C35 N6 C37 -2.7(5) . . . . ?
C42 C35 N6 C37 178.4(3) . . . . ?
C34 C35 N6 Pd1 173.8(3) . . . . ?
C42 C35 N6 Pd1 -5.1(5) . . . . ?
C36 C37 N6 C35 3.2(5) . . . . ?
C38 C37 N6 C35 -176.1(4) . . . . ?
C36 C37 N6 Pd1 -173.4(3) . . . . ?
C38 C37 N6 Pd1 7.3(5) . . . . ?
C44 C43 N7 Pd1 -43.3(4) . . . . ?
C43 C44 N8 Pd1 -35.3(4) . . . . ?
C46 C45 N9 Pd2 44.7(4) . . . . ?
C45 C46 N10 Pd2 36.4(4) . . . . ?

_refine_diff_density_max         7.315
_refine_diff_density_min         -1.840
_refine_diff_density_rms         0.152


# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Residual Density  0.76A From Pd1 5.60 eA-3  
RESPONSE: The residual density is near a heavy atom and, taking
into account that no similar problems nor disorder are observed
for other atoms (all of which have reasonably small ellipsoids),
it should correspond to Fourier truncation ripples rather to
actual electron density corresponding to an atom in that
position.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1478619'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H76 N16 O36 Pd2'
_chemical_formula_weight         1858.20

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4048(12)
_cell_length_b                   13.2527(13)
_cell_length_c                   13.3614(13)
_cell_angle_alpha                66.448(2)
_cell_angle_beta                 80.549(2)
_cell_angle_gamma                83.081(2)
_cell_volume                     1982.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12362
_cell_measurement_theta_min      4.874
_cell_measurement_theta_max      56.449

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.217
_exptl_absorpt_coefficient_mu    0.554
_shelx_estimated_absorpt_T_min   0.795
_shelx_estimated_absorpt_T_max   0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6177
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart 1K'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26214
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.679
_diffrn_reflns_theta_max         28.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9786
_reflns_number_gt                7989
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART V5.624'
_computing_cell_refinement       'Bruker SMART V5.624'
_computing_data_reduction        'SAINT V6.28A (Bruker)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP3, Chimera 1.10.2'
_computing_publication_material  'ORTEP3, Chimera 1.10.2'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1171P)²+5.0089P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9786
_refine_ls_number_parameters     533
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.1947
_refine_ls_wR_factor_gt          0.1827
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.3213(4) 0.2051(4) 0.9945(4) 0.0341(10) Uani 1 1 d . . . . .
H1 H 0.3510 0.1330 1.0033 0.041 Uiso 1 1 calc R U . . .
C2 C 0.3629(4) 0.2939(4) 0.9037(4) 0.0328(9) Uani 1 1 d . . . . .
H2 H 0.4196 0.2823 0.8515 0.039 Uiso 1 1 calc R U . . .
C3 C 0.3205(3) 0.4012(3) 0.8894(3) 0.0248(8) Uani 1 1 d . . . . .
C4 C 0.2377(4) 0.4122(3) 0.9683(4) 0.0283(8) Uani 1 1 d . . . . .
H4 H 0.2069 0.4834 0.9620 0.034 Uiso 1 1 calc R U . . .
C5 C 0.1998(3) 0.3194(4) 1.0567(4) 0.0288(8) Uani 1 1 d . . . . .
H5 H 0.1425 0.3286 1.1096 0.035 Uiso 1 1 calc R U . . .
C6 C 0.5082(4) 0.5848(4) 0.6515(4) 0.0304(9) Uani 1 1 d . . . . .
H6 H 0.5777 0.5799 0.6109 0.036 Uiso 1 1 calc R U . . .
C7 C 0.4668(4) 0.4922(3) 0.7344(3) 0.0282(8) Uani 1 1 d . . . . .
H7 H 0.5074 0.4232 0.7503 0.034 Uiso 1 1 calc R U . . .
C8 C 0.3653(3) 0.4983(3) 0.7956(3) 0.0249(8) Uani 1 1 d . . . . .
C9 C 0.3079(4) 0.6015(4) 0.7667(4) 0.0320(9) Uani 1 1 d . . . . .
H9 H 0.2381 0.6089 0.8056 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3523(4) 0.6924(4) 0.6821(4) 0.0337(9) Uani 1 1 d . . . . .
H10 H 0.3128 0.7622 0.6626 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5011(4) 0.7836(4) 0.5410(4) 0.0329(10) Uani 1 1 d . . . . .
H11A H 0.4429 0.8410 0.5108 0.040 Uiso 1 1 calc R U . . .
H11B H 0.5430 0.7655 0.4800 0.040 Uiso 1 1 calc R U . . .
C12 C 0.7551(4) 0.8199(3) 0.6481(4) 0.0307(9) Uani 1 1 d . . . . .
C13 C 0.6839(4) 0.7896(4) 0.5920(4) 0.0327(9) Uani 1 1 d . . . . .
H13 H 0.7120 0.7429 0.5540 0.039 Uiso 1 1 calc R U . . .
C14 C 0.5769(4) 0.8263(3) 0.5920(3) 0.0298(9) Uani 1 1 d . . . . .
C15 C 0.5374(4) 0.9018(3) 0.6432(3) 0.0290(9) Uani 1 1 d . . . . .
C16 C 0.4287(4) 0.9518(4) 0.6424(4) 0.0345(10) Uani 1 1 d . . . . .
H16 H 0.3788 0.9358 0.6046 0.041 Uiso 1 1 calc R U . . .
C17 C 0.3947(4) 1.0225(4) 0.6952(4) 0.0368(10) Uani 1 1 d . . . . .
H17 H 0.3218 1.0541 0.6949 0.044 Uiso 1 1 calc R U . . .
C18 C 0.4692(4) 1.0476(4) 0.7499(4) 0.0364(10) Uani 1 1 d . . . . .
H18 H 0.4461 1.0967 0.7862 0.044 Uiso 1 1 calc R U . . .
C19 C 0.5747(4) 1.0022(4) 0.7513(4) 0.0309(9) Uani 1 1 d . . . . .
H19 H 0.6237 1.0204 0.7884 0.037 Uiso 1 1 calc R U . . .
C20 C 0.6111(4) 0.9291(3) 0.6987(3) 0.0274(8) Uani 1 1 d . . . . .
C21 C 0.8710(4) 0.7760(5) 0.6475(5) 0.0421(11) Uani 1 1 d . . . . .
H21A H 0.9138 0.8198 0.6691 0.063 Uiso 1 1 calc R U . . .
H21B H 0.9008 0.7803 0.5734 0.063 Uiso 1 1 calc R U . . .
H21C H 0.8750 0.6990 0.6996 0.063 Uiso 1 1 calc R U . . .
C22 C 0.0258(6) -0.0505(6) 1.1881(5) 0.068(2) Uani 1 1 d . . . . .
H22A H -0.0459 -0.0202 1.2123 0.082 Uiso 1 1 calc R U . . .
H22B H 0.0123 -0.0953 1.1477 0.082 Uiso 1 1 calc R U . . .
C23 C 0.0772(6) -0.1190(5) 1.2819(5) 0.0558(16) Uani 1 1 d . . . . .
H23A H 0.1362 -0.1668 1.2607 0.067 Uiso 1 1 calc R U . . .
H23B H 0.0229 -0.1672 1.3381 0.067 Uiso 1 1 calc R U . . .
C24 C 0.5395(3) 0.5202(4) -0.0472(3) 0.0262(8) Uani 1 1 d . . . . .
C25 C 0.5380(4) 0.6347(4) -0.1145(3) 0.0298(9) Uani 1 1 d . . . . .
H25 H 0.5914 0.6617 -0.1771 0.036 Uiso 1 1 calc R U . . .
C26 C 0.4605(4) 0.7053(4) -0.0897(4) 0.0324(9) Uani 1 1 d . . . . .
H26 H 0.4599 0.7816 -0.1357 0.039 Uiso 1 1 calc R U . . .
C27 C 0.3808(4) 0.6675(4) 0.0033(4) 0.0330(9) Uani 1 1 d . . . . .
H27 H 0.3270 0.7183 0.0191 0.040 Uiso 1 1 calc R U . . .
C28 C 0.3808(4) 0.5578(4) 0.0708(3) 0.0283(8) Uani 1 1 d . . . . .
C29 C 0.2332(4) 0.5908(4) 0.1949(4) 0.0393(11) Uani 1 1 d . . . . .
H29A H 0.1817 0.6246 0.1394 0.047 Uiso 1 1 calc R U . . .
H29B H 0.2737 0.6503 0.1958 0.047 Uiso 1 1 calc R U . . .
C30 C 0.1703(4) 0.5345(5) 0.3061(4) 0.0419(11) Uani 1 1 d . . . . .
H30A H 0.1106 0.5856 0.3204 0.050 Uiso 1 1 calc R U . . .
H30B H 0.1371 0.4693 0.3081 0.050 Uiso 1 1 calc R U . . .
C31 C 0.1829(5) 0.4703(6) 0.4988(5) 0.0531(14) Uani 1 1 d . . . . .
H31A H 0.1409 0.4050 0.5170 0.064 Uiso 1 1 calc R U . . .
H31B H 0.1306 0.5319 0.5023 0.064 Uiso 1 1 calc R U . . .
C32 C 0.2632(6) 0.4449(6) 0.5799(5) 0.0554(15) Uani 1 1 d . . . . .
H32A H 0.3133 0.5056 0.5536 0.067 Uiso 1 1 calc R U . . .
H32B H 0.2229 0.4408 0.6517 0.067 Uiso 1 1 calc R U . . .
N1 N 0.2414(3) 0.2164(3) 1.0701(3) 0.0264(7) Uani 1 1 d . . . . .
N2 N 0.4509(3) 0.6828(3) 0.6274(3) 0.0288(8) Uani 1 1 d . . . . .
N3 N 0.7183(3) 0.8850(3) 0.7013(3) 0.0256(7) Uani 1 1 d . . . . .
N4 N 0.0938(3) 0.0419(3) 1.1131(3) 0.0318(8) Uani 1 1 d . . . . .
H4A H 0.0499 0.1012 1.0768 0.038 Uiso 1 1 calc R U . . .
H4B H 0.1384 0.0213 1.0623 0.038 Uiso 1 1 calc R U . . .
N5 N 0.1242(3) -0.0532(3) 1.3297(3) 0.0327(8) Uani 1 1 d . . . . .
H5A H 0.1784 -0.0940 1.3696 0.039 Uiso 1 1 calc R U . . .
H5B H 0.0715 -0.0326 1.3750 0.039 Uiso 1 1 calc R U . . .
N6 N 0.1522(4) 0.9561(5) 0.5754(4) 0.0535(12) Uani 1 1 d . U . . .
N7 N 0.6227(4) 0.2767(4) 0.6508(5) 0.0507(12) Uani 1 1 d . . . . .
N8 N 0.1141(7) -0.2488(7) 0.9015(6) 0.088(2) Uani 1 1 d . U . . .
O1 O 0.2296(3) 0.9205(3) 0.5254(3) 0.0481(9) Uani 1 1 d . U . . .
O2 O 0.1567(4) 1.0372(4) 0.6008(4) 0.0612(11) Uani 1 1 d . U . . .
O3 O 0.0646(6) 0.9251(10) 0.5836(11) 0.198(6) Uani 1 1 d . U . . .
O4 O 0.5566(5) 0.3486(5) 0.5894(5) 0.0783(16) Uani 1 1 d . . . . .
O5 O 0.6998(5) 0.2414(4) 0.6030(5) 0.0866(19) Uani 1 1 d . . . . .
O6 O 0.6000(5) 0.2503(4) 0.7512(4) 0.0727(15) Uani 1 1 d . . . . .
O7 O 0.1718(11) -0.1995(7) 0.8121(7) 0.181(5) Uani 1 1 d . U . . .
O8 O 0.0940(4) -0.1992(4) 0.9672(5) 0.0729(14) Uani 1 1 d . U . . .
O9 O 0.0819(4) -0.3485(5) 0.9296(5) 0.0785(15) Uani 1 1 d . U . . .
O10 O 0.3090(3) 0.5133(3) 0.1651(3) 0.0325(7) Uani 1 1 d . . . . .
O11 O 0.2423(3) 0.5004(4) 0.3897(3) 0.0461(9) Uani 1 1 d . . . . .
O12 O 0.3246(4) 0.3458(4) 0.5943(4) 0.0699(14) Uani 1 1 d . . . . .
H12 H 0.2824 0.2940 0.6173 0.105 Uiso 1 1 calc R U . . .
O13 O 0.1183(4) 0.7037(4) 0.5694(4) 0.0684(13) Uani 1 1 d . . . . .
O14 O 0.0410(5) 0.5534(5) 0.7823(5) 0.0852(17) Uani 1 1 d . . . . .
O15 O 0.0488(5) 0.3251(5) 0.8421(5) 0.0852(17) Uani 1 1 d . . . . .
O16 O 0.2030(4) 0.1911(4) 0.7779(4) 0.0660(13) Uani 1 1 d . . . . .
O17 O 0.2213(3) -0.0202(3) 0.9402(3) 0.0476(9) Uani 1 1 d . . . . .
O18 O 0.4134(3) -0.0726(3) 1.0339(4) 0.0491(9) Uani 1 1 d . . . . .
Pd1 Pd 0.18565(3) 0.08270(3) 1.20318(3) 0.02551(12) Uani 1 1 d . . . . .


_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 N1 1.335(6) . ?
C1 C2 1.387(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.404(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(6) . ?
C3 C8 1.480(6) . ?
C4 C5 1.387(6) . ?
C4 H4 0.9500 . ?
C5 N1 1.351(6) . ?
C5 H5 0.9500 . ?
C6 N2 1.346(6) . ?
C6 C7 1.369(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.400(6) . ?
C9 C10 1.378(6) . ?
C9 H9 0.9500 . ?
C10 N2 1.338(6) . ?
C10 H10 0.9500 . ?
C11 N2 1.496(5) . ?
C11 C14 1.522(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N3 1.322(6) . ?
C12 C13 1.430(6) . ?
C12 C21 1.485(7) . ?
C13 C14 1.358(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.423(6) . ?
C15 C20 1.426(6) . ?
C15 C16 1.429(7) . ?
C16 C17 1.374(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.410(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.373(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.404(6) . ?
C19 H19 0.9500 . ?
C20 N3 1.386(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.420(9) . ?
C22 N4 1.485(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N5 1.482(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.420(6) . ?
C24 C24 1.421(8) 2_665 ?
C24 C28 1.435(6) 2_665 ?
C25 C26 1.355(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.411(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.371(6) . ?
C27 H27 0.9500 . ?
C28 O10 1.376(5) . ?
C28 C24 1.435(6) 2_665 ?
C29 O10 1.438(6) . ?
C29 C30 1.499(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 O11 1.441(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 O11 1.443(7) . ?
C31 C32 1.503(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 O12 1.395(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
N1 Pd1 2.038(4) . ?
N3 Pd1 2.072(3) 2_667 ?
N4 Pd1 2.040(4) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N5 Pd1 2.039(4) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N6 O3 1.181(8) . ?
N6 O1 1.234(6) . ?
N6 O2 1.259(7) . ?
N7 O5 1.213(7) . ?
N7 O6 1.236(7) . ?
N7 O4 1.290(7) . ?
N8 O7 1.255(10) . ?
N8 O8 1.272(9) . ?
N8 O9 1.315(10) . ?
O12 H12 0.8400 . ?
Pd1 N3 2.072(3) 2_667 ?

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 C1 C2 123.0(4) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 119.4(4) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 117.3(4) . . ?
C4 C3 C8 121.7(4) . . ?
C2 C3 C8 121.0(4) . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 122.4(4) . . ?
N1 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
N2 C6 C7 120.3(4) . . ?
N2 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C8 120.5(4) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C9 117.3(4) . . ?
C7 C8 C3 122.0(4) . . ?
C9 C8 C3 120.7(4) . . ?
C10 C9 C8 120.3(4) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
N2 C10 C9 120.2(4) . . ?
N2 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
N2 C11 C14 109.1(3) . . ?
N2 C11 H11A 109.9 . . ?
C14 C11 H11A 109.9 . . ?
N2 C11 H11B 109.9 . . ?
C14 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N3 C12 C13 120.7(4) . . ?
N3 C12 C21 120.0(4) . . ?
C13 C12 C21 119.3(4) . . ?
C14 C13 C12 121.2(4) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 118.9(4) . . ?
C13 C14 C11 119.7(4) . . ?
C15 C14 C11 121.4(4) . . ?
C14 C15 C20 117.8(4) . . ?
C14 C15 C16 124.2(4) . . ?
C20 C15 C16 118.0(4) . . ?
C17 C16 C15 121.4(4) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 119.3(5) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 120.9(4) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 120.8(4) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
N3 C20 C19 119.4(4) . . ?
N3 C20 C15 121.2(4) . . ?
C19 C20 C15 119.5(4) . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N4 111.8(5) . . ?
C23 C22 H22A 109.3 . . ?
N4 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
N4 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
C22 C23 N5 111.6(5) . . ?
C22 C23 H23A 109.3 . . ?
N5 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
N5 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
C25 C24 C24 120.0(5) . 2_665 ?
C25 C24 C28 122.1(4) . 2_665 ?
C24 C24 C28 117.8(5) 2_665 2_665 ?
C26 C25 C24 120.2(4) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C27 121.1(4) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C28 C27 C26 120.2(4) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 O10 124.7(4) . . ?
C27 C28 C24 120.6(4) . 2_665 ?
O10 C28 C24 114.7(4) . 2_665 ?
O10 C29 C30 110.5(4) . . ?
O10 C29 H29A 109.5 . . ?
C30 C29 H29A 109.5 . . ?
O10 C29 H29B 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
O11 C30 C29 109.9(4) . . ?
O11 C30 H30A 109.7 . . ?
C29 C30 H30A 109.7 . . ?
O11 C30 H30B 109.7 . . ?
C29 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
O11 C31 C32 108.8(5) . . ?
O11 C31 H31A 109.9 . . ?
C32 C31 H31A 109.9 . . ?
O11 C31 H31B 109.9 . . ?
C32 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
O12 C32 C31 112.2(6) . . ?
O12 C32 H32A 109.2 . . ?
C31 C32 H32A 109.2 . . ?
O12 C32 H32B 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C1 N1 C5 118.0(4) . . ?
C1 N1 Pd1 121.0(3) . . ?
C5 N1 Pd1 121.0(3) . . ?
C10 N2 C6 121.4(4) . . ?
C10 N2 C11 119.4(4) . . ?
C6 N2 C11 119.1(4) . . ?
C12 N3 C20 120.1(4) . . ?
C12 N3 Pd1 121.7(3) . 2_667 ?
C20 N3 Pd1 118.2(3) . 2_667 ?
C22 N4 Pd1 109.1(3) . . ?
C22 N4 H4A 109.9 . . ?
Pd1 N4 H4A 109.9 . . ?
C22 N4 H4B 109.9 . . ?
Pd1 N4 H4B 109.9 . . ?
H4A N4 H4B 108.3 . . ?
C23 N5 Pd1 108.0(3) . . ?
C23 N5 H5A 110.1 . . ?
Pd1 N5 H5A 110.1 . . ?
C23 N5 H5B 110.1 . . ?
Pd1 N5 H5B 110.1 . . ?
H5A N5 H5B 108.4 . . ?
O3 N6 O1 118.0(6) . . ?
O3 N6 O2 117.0(6) . . ?
O1 N6 O2 123.7(5) . . ?
O5 N7 O6 127.3(7) . . ?
O5 N7 O4 115.9(6) . . ?
O6 N7 O4 116.8(6) . . ?
O7 N8 O8 115.7(9) . . ?
O7 N8 O9 122.8(8) . . ?
O8 N8 O9 121.3(7) . . ?
C28 O10 C29 115.8(4) . . ?
C30 O11 C31 112.2(4) . . ?
C32 O12 H12 109.5 . . ?
N1 Pd1 N5 176.21(14) . . ?
N1 Pd1 N4 92.30(15) . . ?
N5 Pd1 N4 83.91(15) . . ?
N1 Pd1 N3 90.01(14) . 2_667 ?
N5 Pd1 N3 93.77(14) . 2_667 ?
N4 Pd1 N3 176.80(14) . 2_667 ?

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
N1 C1 C2 C3 0.3(8) . . . . ?
C1 C2 C3 C4 -0.2(7) . . . . ?
C1 C2 C3 C8 177.9(4) . . . . ?
C2 C3 C4 C5 -0.3(6) . . . . ?
C8 C3 C4 C5 -178.3(4) . . . . ?
C3 C4 C5 N1 0.6(7) . . . . ?
N2 C6 C7 C8 -0.7(6) . . . . ?
C6 C7 C8 C9 1.5(6) . . . . ?
C6 C7 C8 C3 -176.8(4) . . . . ?
C4 C3 C8 C7 161.3(4) . . . . ?
C2 C3 C8 C7 -16.7(6) . . . . ?
C4 C3 C8 C9 -16.9(6) . . . . ?
C2 C3 C8 C9 165.1(4) . . . . ?
C7 C8 C9 C10 -1.0(6) . . . . ?
C3 C8 C9 C10 177.3(4) . . . . ?
C8 C9 C10 N2 -0.4(7) . . . . ?
N3 C12 C13 C14 -0.2(6) . . . . ?
C21 C12 C13 C14 178.9(4) . . . . ?
C12 C13 C14 C15 3.9(6) . . . . ?
C12 C13 C14 C11 -174.1(4) . . . . ?
N2 C11 C14 C13 89.9(5) . . . . ?
N2 C11 C14 C15 -88.1(5) . . . . ?
C13 C14 C15 C20 -4.2(6) . . . . ?
C11 C14 C15 C20 173.8(4) . . . . ?
C13 C14 C15 C16 175.8(4) . . . . ?
C11 C14 C15 C16 -6.2(6) . . . . ?
C14 C15 C16 C17 178.7(4) . . . . ?
C20 C15 C16 C17 -1.3(6) . . . . ?
C15 C16 C17 C18 1.0(7) . . . . ?
C16 C17 C18 C19 -0.2(7) . . . . ?
C17 C18 C19 C20 -0.3(7) . . . . ?
C18 C19 C20 N3 179.7(4) . . . . ?
C18 C19 C20 C15 0.0(7) . . . . ?
C14 C15 C20 N3 1.0(6) . . . . ?
C16 C15 C20 N3 -179.0(4) . . . . ?
C14 C15 C20 C19 -179.2(4) . . . . ?
C16 C15 C20 C19 0.8(6) . . . . ?
N4 C22 C23 N5 44.7(9) . . . . ?
C24 C24 C25 C26 -0.8(7) 2_665 . . . ?
C28 C24 C25 C26 179.4(4) 2_665 . . . ?
C24 C25 C26 C27 0.6(6) . . . . ?
C25 C26 C27 C28 0.3(7) . . . . ?
C26 C27 C28 O10 177.8(4) . . . . ?
C26 C27 C28 C24 -0.9(6) . . . 2_665 ?
O10 C29 C30 O11 68.3(5) . . . . ?
O11 C31 C32 O12 -71.5(7) . . . . ?
C2 C1 N1 C5 0.0(7) . . . . ?
C2 C1 N1 Pd1 -178.9(4) . . . . ?
C4 C5 N1 C1 -0.5(6) . . . . ?
C4 C5 N1 Pd1 178.5(3) . . . . ?
C9 C10 N2 C6 1.3(7) . . . . ?
C9 C10 N2 C11 -175.9(4) . . . . ?
C7 C6 N2 C10 -0.7(6) . . . . ?
C7 C6 N2 C11 176.4(4) . . . . ?
C14 C11 N2 C10 95.0(5) . . . . ?
C14 C11 N2 C6 -82.3(5) . . . . ?
C13 C12 N3 C20 -3.1(6) . . . . ?
C21 C12 N3 C20 177.8(4) . . . . ?
C13 C12 N3 Pd1 173.5(3) . . . 2_667 ?
C21 C12 N3 Pd1 -5.7(6) . . . 2_667 ?
C19 C20 N3 C12 -177.1(4) . . . . ?
C15 C20 N3 C12 2.7(6) . . . . ?
C19 C20 N3 Pd1 6.3(5) . . . 2_667 ?
C15 C20 N3 Pd1 -174.0(3) . . . 2_667 ?
C23 C22 N4 Pd1 -29.7(8) . . . . ?
C22 C23 N5 Pd1 -36.9(7) . . . . ?
C27 C28 O10 C29 -3.1(6) . . . . ?
C24 C28 O10 C29 175.8(4) 2_665 . . . ?
C30 C29 O10 C28 -172.3(4) . . . . ?
C29 C30 O11 C31 165.9(5) . . . . ?
C32 C31 O11 C30 -175.4(5) . . . . ?

_refine_diff_density_max         2.202
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.145

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1478620'
_audit_update_record             
;
2016-08-12 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C92 H80 N16 O34 Pd2'
_chemical_formula_weight         2166.52

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.126(5)
_cell_length_b                   20.379(5)
_cell_length_c                   25.002(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.801(5)
_cell_angle_gamma                90
_cell_volume                     9503(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6101
_cell_measurement_theta_min      5.921
_cell_measurement_theta_max      43.101

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_F_000             4432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.085
_exptl_absorpt_coefficient_mu    0.473
_shelx_estimated_absorpt_T_min   0.869
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46176
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.480
_diffrn_reflns_theta_max         28.307
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11712
_reflns_number_gt                7215
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Apex2 V.1.0-27 (Bruker, 2005)'
_computing_cell_refinement       'SAINT V7.12A (Bruker 2004) in Apex2 suite.'
_computing_data_reduction        
'SAINT and XPREP 6.14 COPYRIGHT(c) 2003 Bruker-AXS'
_computing_structure_solution    'Sir92 (Altomare, et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP3, Chimera 1.10.2'
_computing_publication_material  'ORTEP3, Chimera 1.10.2'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1944P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11712
_refine_ls_number_parameters     657
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_ref         0.2962
_refine_ls_wR_factor_gt          0.2475
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.7010(3) 0.0337(2) 0.0582(2) 0.0440(12) Uani 1 1 d . . . . .
H1 H 0.6575 0.0105 0.0450 0.053 Uiso 1 1 calc R U . . .
C2 C 0.7422(3) 0.0503(3) 0.0220(2) 0.0429(12) Uani 1 1 d . . . . .
C3 C 0.8053(3) 0.0852(2) 0.0418(2) 0.0359(11) Uani 1 1 d . . . . .
C4 C 0.8264(3) 0.1004(3) 0.0982(2) 0.0399(12) Uani 1 1 d . . . . .
C5 C 0.7814(3) 0.0806(3) 0.1312(2) 0.0447(13) Uani 1 1 d . . . . .
H5 H 0.7946 0.0899 0.1693 0.054 Uiso 1 1 calc R U . . .
C7 C 0.7222(5) 0.0338(3) -0.0363(3) 0.0647(19) Uani 1 1 d . . . . .
H7 H 0.6814 0.0070 -0.0496 0.078 Uiso 1 1 calc R U . . .
C8 C 0.7614(4) 0.0562(3) -0.0717(2) 0.0522(15) Uani 1 1 d . . . . .
H8 H 0.7464 0.0473 -0.1098 0.063 Uiso 1 1 calc R U . . .
C9 C 0.8267(3) 0.0941(2) -0.0510(2) 0.0403(12) Uani 1 1 d . . . . .
C10 C 0.8482(3) 0.1083(2) 0.0055(2) 0.0370(11) Uani 1 1 d . . . . .
C11 C 0.9106(3) 0.1453(2) 0.0256(2) 0.0384(11) Uani 1 1 d . . . . .
C12 C 0.9313(3) 0.1608(3) 0.0839(2) 0.0441(12) Uani 1 1 d . . . . .
H12 H 0.9721 0.1874 0.0976 0.053 Uiso 1 1 calc R U . . .
C13 C 0.8919(3) 0.1369(3) 0.1182(3) 0.0536(15) Uani 1 1 d . . . . .
H13 H 0.9077 0.1443 0.1565 0.064 Uiso 1 1 calc R U . . .
C14 C 0.9425(3) 0.3678(3) -0.1061(3) 0.0475(13) Uani 1 1 d . . . . .
H14 H 0.9639 0.4040 -0.0847 0.057 Uiso 1 1 calc R U . . .
C15 C 0.9698(3) 0.3035(3) -0.0914(3) 0.0484(13) Uani 1 1 d . . . . .
H15 H 1.0083 0.2973 -0.0605 0.058 Uiso 1 1 calc R U . . .
C16 C 0.9398(3) 0.2510(3) -0.1220(2) 0.0415(12) Uani 1 1 d . . . . .
C17 C 0.8839(3) 0.2612(2) -0.1677(2) 0.0398(12) Uani 1 1 d . . . . .
C18 C 0.8506(3) 0.2116(3) -0.2035(3) 0.0487(14) Uani 1 1 d . . . . .
H18 H 0.8665 0.1676 -0.1968 0.058 Uiso 1 1 calc R U . . .
C19 C 0.7954(4) 0.2250(3) -0.2479(3) 0.0564(15) Uani 1 1 d . . . . .
H19 H 0.7729 0.1904 -0.2708 0.068 Uiso 1 1 calc R U . . .
C20 C 0.7724(3) 0.2905(3) -0.2592(3) 0.0564(15) Uani 1 1 d . . . . .
H20 H 0.7348 0.2994 -0.2901 0.068 Uiso 1 1 calc R U . . .
C21 C 0.8029(3) 0.3410(3) -0.2269(3) 0.0466(13) Uani 1 1 d . . . . .
H21 H 0.7869 0.3847 -0.2352 0.056 Uiso 1 1 calc R U . . .
C22 C 0.8592(3) 0.3278(2) -0.1804(2) 0.0412(12) Uani 1 1 d . . . . .
C23 C 0.9672(3) 0.1833(3) -0.1040(3) 0.0468(13) Uani 1 1 d . . . . .
H23A H 0.9619 0.1544 -0.1365 0.056 Uiso 1 1 calc R U . . .
H23B H 1.0189 0.1858 -0.0863 0.056 Uiso 1 1 calc R U . . .
C24 C 0.9492(3) 0.1681(2) -0.0116(2) 0.0417(12) Uani 1 1 d . . . . .
H24 H 0.9913 0.1934 0.0012 0.050 Uiso 1 1 calc R U . . .
C25 C 0.8684(3) 0.1181(2) -0.0849(2) 0.0435(12) Uani 1 1 d . . . . .
H25 H 0.8554 0.1087 -0.1231 0.052 Uiso 1 1 calc R U . . .
C26 C 0.0000 0.2246(7) 0.2500 0.102(5) Uani 1 2 d S T P . .
C27 C 0.0000 0.1547(6) 0.2500 0.085(4) Uani 1 2 d S T P . .
C28 C -0.0470(5) 0.1187(4) 0.2789(4) 0.084(2) Uani 1 1 d . . . . .
H28 H -0.0497 0.0721 0.2776 0.101 Uiso 1 1 calc R U . . .
C29 C -0.0866(5) 0.1541(5) 0.3075(4) 0.087(3) Uani 1 1 d . . . . .
C30 C -0.0837(5) 0.2235(5) 0.3113(5) 0.097(3) Uani 1 1 d . . . . .
H30 H -0.1095 0.2470 0.3336 0.117 Uiso 1 1 calc R U . . .
C31 C -0.0384(6) 0.2577(5) 0.2789(6) 0.133(5) Uani 1 1 d . . . . .
H31 H -0.0370 0.3043 0.2788 0.160 Uiso 1 1 calc R U . . .
C32 C 0.0805(5) 0.9500(4) 0.5338(3) 0.069(2) Uani 1 1 d . . . . .
H32 H 0.1026 0.9341 0.5692 0.083 Uiso 1 1 calc R U . A 1
C33 C 0.0157(4) 0.9897(3) 0.5264(3) 0.0550(16) Uani 1 1 d . . . . .
C34 C -0.0155(4) 1.0054(4) 0.5705(3) 0.0649(19) Uani 1 1 d . . . . .
H34 H 0.0064 0.9904 0.6063 0.078 Uiso 1 1 calc R U . B 1
C35 C -0.0759(5) 1.0411(3) 0.5632(3) 0.067(2) Uani 0.5 1 d . . P C 1
C36 C 0.1091(4) 0.9358(3) 0.4902(4) 0.070(2) Uani 0.5 1 d . . P D 1
C45 C -0.0759(5) 1.0411(3) 0.5632(3) 0.067(2) Uani 0.5 1 d . . P C 2
H45 H -0.0965 1.0511 0.5935 0.081 Uiso 0.5 1 calc R U P C 2
C46 C 0.1091(4) 0.9358(3) 0.4902(4) 0.070(2) Uani 0.5 1 d . . P D 2
H46 H 0.1516 0.9102 0.4953 0.084 Uiso 0.5 1 calc R U P D 2
C63 C 0.5519(7) 0.2269(6) 0.2929(6) 0.125(5) Uani 1 1 d . . . . .
H63 H 0.5904 0.2245 0.3243 0.150 Uiso 1 1 calc R U . E 3
C64 C 0.5308(7) 0.2864(6) 0.2760(5) 0.120(5) Uani 1 1 d . . . . .
C65 C 0.5551(10) 0.3445(7) 0.2946(6) 0.171(8) Uani 1 1 d . . . . .
H65 H 0.5943 0.3444 0.3255 0.205 Uiso 1 1 calc R U . F 3
C50 C 0.5280(7) 0.1738(5) 0.2733(7) 0.136(7) Uani 0.5 1 d . . P G 3
C56 C 0.5315(12) 0.4033(6) 0.2753(5) 0.168(8) Uani 0.5 1 d . . P H 3
O6 O 0.5430(12) 0.4632(6) 0.2921(7) 0.130(7) Uani 0.5 1 d . . P H 3
H6 H 0.5717 0.4635 0.3228 0.195 Uiso 0.5 1 calc R U P H 3
O5 O 0.5445(9) 0.1068(8) 0.2855(7) 0.125(5) Uani 0.5 1 d . . P G 3
H5A H 0.5172 0.0830 0.2625 0.187 Uiso 0.5 1 calc R U P G 3
C60 C 0.5280(7) 0.1738(5) 0.2733(7) 0.136(7) Uani 0.5 1 d . . P G 4
H60 H 0.5474 0.1337 0.2894 0.163 Uiso 0.5 1 calc R U P G 4
C66 C 0.5315(12) 0.4033(6) 0.2753(5) 0.168(8) Uani 0.5 1 d . . P H 4
H66 H 0.5522 0.4428 0.2918 0.202 Uiso 0.5 1 calc R U P H 4
C43 C 0.6026(5) -0.0604(4) 0.2356(4) 0.088(3) Uani 1 1 d . . . . .
H43A H 0.5600 -0.0826 0.2436 0.106 Uiso 1 1 calc R U . . .
H43B H 0.6378 -0.0534 0.2707 0.106 Uiso 1 1 calc R U . . .
C42 C 0.6352(5) -0.1020(4) 0.1981(5) 0.094(3) Uani 1 1 d . . . . .
H42A H 0.6591 -0.1404 0.2186 0.112 Uiso 1 1 calc R U . . .
H42B H 0.5968 -0.1184 0.1677 0.112 Uiso 1 1 calc R U . . .
C80 C 0.8114(3) 0.7124(3) 0.52727(19) 0.0635(18) Uani 0.5 1 d G . P I 5
C81 C 0.8709(3) 0.6766(3) 0.5539(3) 0.087(6) Uani 0.5 1 d DG . P I 5
H81 H 0.9020 0.6576 0.5335 0.104 Uiso 0.5 1 calc R U P I 5
C82 C 0.8847(4) 0.6687(4) 0.6105(4) 0.102(6) Uani 0.5 1 d DG U P I 5
C83 C 0.8392(4) 0.6966(4) 0.6405(2) 0.097(7) Uani 0.5 1 d DG . P I 5
H83 H 0.8486 0.6912 0.6791 0.116 Uiso 0.5 1 calc R U P I 5
C84 C 0.7797(3) 0.7324(3) 0.61380(17) 0.089(2) Uani 0.5 1 d G . P I 5
H84 H 0.7486 0.7514 0.6343 0.106 Uiso 0.5 1 calc R U P I 5
C85 C 0.7659(2) 0.7403(2) 0.55721(17) 0.0563(17) Uani 0.5 1 d G . P I 5
C98 C 0.7935(4) 0.7241(3) 0.4690(3) 0.0632(19) Uani 0.5 1 d . . P I 5
H98 H 0.8241 0.7063 0.4475 0.076 Uiso 0.5 1 calc R U P I 5
C70 C 0.8114(3) 0.7124(3) 0.52727(19) 0.0635(18) Uani 0.5 1 d . . P J 6
H70 H 0.8520 0.6871 0.5442 0.076 Uiso 0.5 1 calc R U P J 6
O84 O 0.7797(3) 0.7324(3) 0.61380(17) 0.089(2) Uani 0.5 1 d . . P J 6
H94 H 0.8168 0.7095 0.6241 0.133 Uiso 0.5 1 calc R U P J 6
C75 C 0.7659(2) 0.7403(2) 0.55721(17) 0.0563(17) Uani 0.5 1 d . . P J 6
C78 C 0.7935(4) 0.7241(3) 0.4690(3) 0.0632(19) Uani 0.5 1 d . . P J 6
H78 H 0.8241 0.7063 0.4475 0.076 Uiso 0.5 1 calc R U P J 6
N1 N 0.5819(3) 0.0026(3) 0.2090(3) 0.0614(15) Uani 1 1 d . . . . .
H1A H 0.5824 0.0340 0.2349 0.074 Uiso 1 1 calc R U . . .
H1B H 0.5365 -0.0003 0.1881 0.074 Uiso 1 1 calc R U . . .
N2 N 0.6877(3) -0.0649(2) 0.1754(2) 0.0516(12) Uani 1 1 d . . . . .
H2A H 0.6934 -0.0838 0.1436 0.062 Uiso 1 1 calc R U . . .
H2B H 0.7309 -0.0645 0.1996 0.062 Uiso 1 1 calc R U . . .
N3 N 0.7195(3) 0.0487(2) 0.11137(19) 0.0405(10) Uani 1 1 d . . . . .
N4 N 0.9277(2) 0.15489(19) -0.06516(19) 0.0389(10) Uani 1 1 d . . . . .
N5 N 0.8899(2) 0.3785(2) -0.14749(19) 0.0419(10) Uani 1 1 d . . . . .
N6 N 0.8219(4) 0.9814(3) 0.2862(3) 0.080(2) Uani 1 1 d . . . . .
N8 N 0.2385(10) 0.8225(7) 0.4058(7) 0.236(5) Uani 1 1 d D U . . .
O1 O 0.8684(6) 0.9920(6) 0.3269(4) 0.200(6) Uani 1 1 d . . . . .
O2 O 0.8037(4) 1.0234(3) 0.2515(3) 0.099(2) Uani 1 1 d . . . . .
O3 O 0.7915(4) 0.9311(3) 0.2844(3) 0.100(2) Uani 1 1 d . . . . .
O4 O -0.1279(5) 0.1244(4) 0.3381(3) 0.117(2) Uani 1 1 d . . . . .
H4 H -0.1240 0.0835 0.3358 0.176 Uiso 1 1 calc R U . . .
O7 O 0.1677(6) 0.8997(5) 0.4926(6) 0.090(3) Uani 0.5 1 d . . P . .
H7A H 0.1837 0.8872 0.5250 0.135 Uiso 0.5 1 calc R U P D 1
O8 O -0.1132(7) 1.0557(6) 0.6045(5) 0.085(3) Uani 0.5 1 d . . P . .
H8A H -0.1496 1.0783 0.5912 0.127 Uiso 0.5 1 calc R U P C 1
O12 O 0.2010(11) 0.7665(7) 0.4175(8) 0.295(7) Uani 1 1 d D U . . .
O25 O 0.9388(8) 0.6307(7) 0.6378(5) 0.128(6) Uani 0.5 1 d D . P . .
H25A H 0.9627 0.6166 0.6158 0.191 Uiso 0.5 1 calc R U P I 5
O69 O 0.2363(5) 0.8829(5) 0.4086(4) 0.151(3) Uani 1 1 d D U . . .
O70 O 0.2942(10) 0.8015(9) 0.3839(8) 0.302(7) Uani 1 1 d D U . . .
Pd1 Pd 0.65044(2) 0.02834(2) 0.16072(2) 0.04351(19) Uani 1 1 d . . . . .
O52 O -0.1141(6) 0.2408(5) 0.5016(6) 0.212(6) Uani 1 1 d . . . . .
O50 O 0.2825(10) 0.6580(10) 0.4080(8) 0.082(6) Uani 0.355(17) 1 d . U P K 7
O54 O 0.1396(11) 0.6079(7) 0.3859(13) 0.142(12) Uani 0.355(17) 1 d . U P K 7
O40 O 0.321(2) 0.704(2) 0.4022(15) 0.344(19) Uani 0.645(17) 1 d . U P K 8
O44 O 0.232(2) 0.6356(18) 0.3986(12) 0.37(2) Uani 0.645(17) 1 d . U P K 8
O51 O 0.3819(13) 0.8774(8) 0.5004(10) 0.421(18) Uani 1 1 d . U . . .


_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 N3 1.333(7) . ?
C1 C2 1.369(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.393(8) . ?
C2 C7 1.464(9) . ?
C3 C4 1.412(7) . ?
C3 C10 1.433(7) . ?
C4 C5 1.377(8) . ?
C4 C13 1.448(9) . ?
C5 N3 1.346(8) . ?
C5 H5 0.9500 . ?
C7 C8 1.359(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.462(8) . ?
C8 H8 0.9500 . ?
C9 C25 1.376(8) . ?
C9 C10 1.410(7) . ?
C10 C11 1.407(8) . ?
C11 C24 1.388(7) . ?
C11 C12 1.457(8) . ?
C12 C13 1.351(8) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 N5 1.292(8) . ?
C14 C15 1.428(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.366(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.396(8) . ?
C16 C23 1.509(7) . ?
C17 C18 1.405(8) . ?
C17 C22 1.448(7) . ?
C18 C19 1.379(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.415(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.357(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.423(8) . ?
C21 H21 0.9500 . ?
C22 N5 1.371(7) . ?
C23 N4 1.475(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N4 1.339(7) . ?
C24 H24 0.9500 . ?
C25 N4 1.358(7) . ?
C25 H25 0.9500 . ?
C26 C31 1.324(14) 2 ?
C26 C31 1.324(14) . ?
C26 C27 1.424(18) . ?
C27 C28 1.469(11) . ?
C27 C28 1.469(11) 2 ?
C28 C29 1.359(13) . ?
C28 H28 0.9500 . ?
C29 O4 1.357(12) . ?
C29 C30 1.419(13) . ?
C30 C31 1.485(18) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C46 1.355(11) . ?
C32 C36 1.355(11) . ?
C32 C33 1.456(11) . ?
C32 H32 0.9500 . ?
C33 C33 1.387(14) 5_576 ?
C33 C34 1.404(10) . ?
C34 C45 1.344(12) . ?
C34 C35 1.344(12) . ?
C34 H34 0.9500 . ?
C35 O8 1.412(13) . ?
C35 C36 1.425(12) 5_576 ?
C35 C45 16.546(16) 2 ?
C36 O7 1.332(13) . ?
C36 C35 1.425(12) 5_576 ?
C36 C46 11.811(17) 2 ?
C45 C46 1.425(12) 5_576 ?
C45 H45 0.9500 . ?
C46 C45 1.425(12) 5_576 ?
C46 H46 0.9500 . ?
C63 C60 1.233(16) . ?
C63 C50 1.233(16) . ?
C63 C64 1.318(15) . ?
C63 H63 0.9500 . ?
C64 C65 1.318(18) . ?
C64 C64 1.55(3) 2_655 ?
C65 C66 1.332(17) . ?
C65 C56 1.332(17) . ?
C65 H65 0.9500 . ?
C50 C50 1.40(3) 2_655 ?
C50 O5 1.420(19) . ?
C56 O6 1.296(16) . ?
C56 C56 1.54(4) 2_655 ?
O6 H6 0.8400 . ?
O5 H5A 0.8400 . ?
C60 C60 1.40(3) 2_655 ?
C60 C50 19.97(2) 2 ?
C60 H60 0.9500 . ?
C66 C66 1.54(4) 2_655 ?
C66 C56 20.09(4) 2 ?
C66 H66 0.9500 . ?
C43 N1 1.459(9) . ?
C43 C42 1.499(13) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C42 N2 1.468(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C80 C81 1.3900 . ?
C80 C85 1.3900 . ?
C80 C98 1.439(9) . ?
C81 C82 1.3900 . ?
C81 H81 0.9500 . ?
C82 O25 1.349(12) . ?
C82 C83 1.3900 . ?
C83 C84 1.3900 . ?
C83 H83 0.9500 . ?
C84 C85 1.3900 . ?
C84 H84 0.9500 . ?
C85 C98 1.385(9) 7_666 ?
C85 C78 29.814(11) 2 ?
C98 C85 1.385(13) 7_666 ?
C98 C75 29.814(15) 2 ?
C98 H98 0.9500 . ?
C70 C75 1.3900 . ?
C70 C78 1.439(9) . ?
C70 H70 0.9500 . ?
O84 C75 1.3900 . ?
O84 H94 0.8400 . ?
C75 C78 1.385(9) 7_666 ?
C75 C78 29.814(11) 2 ?
C78 C75 1.385(13) 7_666 ?
C78 C85 29.814(15) 2 ?
C78 H78 0.9500 . ?
N1 Pd1 2.037(5) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 Pd1 2.033(5) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N3 Pd1 2.040(5) . ?
N5 Pd1 2.048(4) 7_655 ?
N6 O3 1.173(8) . ?
N6 O1 1.213(10) . ?
N6 O2 1.214(8) . ?
N8 O69 1.235(13) . ?
N8 O70 1.369(15) . ?
N8 O12 1.413(15) . ?
O4 H4 0.8400 . ?
O7 H7A 0.8400 . ?
O8 H8A 0.8400 . ?
O25 H25A 0.8400 . ?
Pd1 N5 2.048(4) 7_655 ?

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
N3 C1 C2 122.5(6) . . ?
N3 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C1 C2 C3 118.2(5) . . ?
C1 C2 C7 122.7(6) . . ?
C3 C2 C7 119.1(5) . . ?
C2 C3 C4 120.0(5) . . ?
C2 C3 C10 121.1(5) . . ?
C4 C3 C10 118.9(5) . . ?
C5 C4 C3 117.1(5) . . ?
C5 C4 C13 123.5(5) . . ?
C3 C4 C13 119.4(5) . . ?
N3 C5 C4 122.5(5) . . ?
N3 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C8 C7 C2 120.7(6) . . ?
C8 C7 H7 119.7 . . ?
C2 C7 H7 119.7 . . ?
C7 C8 C9 120.0(6) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C25 C9 C10 117.6(5) . . ?
C25 C9 C8 122.4(5) . . ?
C10 C9 C8 120.0(5) . . ?
C11 C10 C9 120.3(5) . . ?
C11 C10 C3 120.6(5) . . ?
C9 C10 C3 119.1(5) . . ?
C24 C11 C10 118.3(5) . . ?
C24 C11 C12 122.1(5) . . ?
C10 C11 C12 119.6(5) . . ?
C13 C12 C11 119.5(5) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C4 121.8(5) . . ?
C12 C13 H13 119.1 . . ?
C4 C13 H13 119.1 . . ?
N5 C14 C15 122.6(6) . . ?
N5 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C16 C15 C14 119.3(6) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 119.5(5) . . ?
C15 C16 C23 118.3(5) . . ?
C17 C16 C23 122.2(5) . . ?
C16 C17 C18 124.8(5) . . ?
C16 C17 C22 118.2(5) . . ?
C18 C17 C22 117.0(5) . . ?
C19 C18 C17 121.9(5) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 119.7(6) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 121.5(6) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C22 119.4(5) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
N5 C22 C21 119.6(5) . . ?
N5 C22 C17 120.0(5) . . ?
C21 C22 C17 120.5(5) . . ?
N4 C23 C16 111.1(4) . . ?
N4 C23 H23A 109.4 . . ?
C16 C23 H23A 109.4 . . ?
N4 C23 H23B 109.4 . . ?
C16 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
N4 C24 C11 120.8(5) . . ?
N4 C24 H24 119.6 . . ?
C11 C24 H24 119.6 . . ?
N4 C25 C9 121.5(5) . . ?
N4 C25 H25 119.3 . . ?
C9 C25 H25 119.3 . . ?
C31 C26 C31 118.7(17) 2 . ?
C31 C26 C27 120.7(9) 2 . ?
C31 C26 C27 120.7(9) . . ?
C26 C27 C28 120.0(6) . . ?
C26 C27 C28 120.0(6) . 2 ?
C28 C27 C28 120.0(12) . 2 ?
C29 C28 C27 117.9(9) . . ?
C29 C28 H28 121.1 . . ?
C27 C28 H28 121.1 . . ?
O4 C29 C28 121.4(9) . . ?
O4 C29 C30 115.2(10) . . ?
C28 C29 C30 123.2(10) . . ?
C29 C30 C31 116.7(10) . . ?
C29 C30 H30 121.6 . . ?
C31 C30 H30 121.6 . . ?
C26 C31 C30 121.4(10) . . ?
C26 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C46 C32 C33 120.0(7) . . ?
C36 C32 C33 120.0(7) . . ?
C36 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C33 C33 C34 120.5(9) 5_576 . ?
C33 C33 C32 117.8(8) 5_576 . ?
C34 C33 C32 121.6(7) . . ?
C45 C34 C33 121.2(8) . . ?
C35 C34 C33 121.2(8) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C34 C35 O8 124.8(9) . . ?
C34 C35 C36 119.9(7) . 5_576 ?
O8 C35 C36 115.2(9) . 5_576 ?
C34 C35 C45 78.7(5) . 2 ?
O8 C35 C45 156.4(7) . 2 ?
O7 C36 C32 124.7(10) . . ?
O7 C36 C35 114.8(9) . 5_576 ?
C32 C36 C35 120.5(8) . 5_576 ?
O7 C36 C46 98.6(7) . 2 ?
C32 C36 C46 134.7(6) . 2 ?
C34 C45 C46 119.9(7) . 5_576 ?
C34 C45 H45 120.0 . . ?
C46 C45 H45 120.0 5_576 . ?
C32 C46 C45 120.5(8) . 5_576 ?
C32 C46 H46 119.8 . . ?
C45 C46 H46 119.8 5_576 . ?
C60 C63 C64 128.2(17) . . ?
C50 C63 C64 128.2(17) . . ?
C50 C63 H63 115.9 . . ?
C64 C63 H63 115.9 . . ?
C63 C64 C65 130.9(16) . . ?
C63 C64 C64 113.1(9) . 2_655 ?
C65 C64 C64 116.0(10) . 2_655 ?
C64 C65 C66 128(2) . . ?
C64 C65 C56 128(2) . . ?
C64 C65 H65 116.0 . . ?
C56 C65 H65 116.0 . . ?
C63 C50 C50 118.7(10) . 2_655 ?
C63 C50 O5 135.4(17) . . ?
C50 C50 O5 105.8(10) 2_655 . ?
O6 C56 C65 135.4(19) . . ?
O6 C56 C56 108.2(13) . 2_655 ?
C65 C56 C56 115.9(12) . 2_655 ?
C56 O6 H6 109.5 . . ?
C50 O5 H5A 109.5 . . ?
C63 C60 C60 118.7(10) . 2_655 ?
C63 C60 C50 107.7(7) . 2 ?
C63 C60 H60 120.6 . . ?
C60 C60 H60 120.6 2_655 . ?
C65 C66 C66 115.9(12) . 2_655 ?
C65 C66 C56 106.3(11) . 2 ?
C65 C66 H66 122.0 . . ?
C66 C66 H66 122.0 2_655 . ?
N1 C43 C42 108.6(6) . . ?
N1 C43 H43A 110.0 . . ?
C42 C43 H43A 110.0 . . ?
N1 C43 H43B 110.0 . . ?
C42 C43 H43B 110.0 . . ?
H43A C43 H43B 108.3 . . ?
N2 C42 C43 111.4(7) . . ?
N2 C42 H42A 109.3 . . ?
C43 C42 H42A 109.3 . . ?
N2 C42 H42B 109.3 . . ?
C43 C42 H42B 109.3 . . ?
H42A C42 H42B 108.0 . . ?
C81 C80 C85 120.0 . . ?
C81 C80 C98 123.9(5) . . ?
C85 C80 C98 116.1(5) . . ?
C80 C81 C82 120.0 . . ?
C80 C81 H81 120.0 . . ?
C82 C81 H81 120.0 . . ?
O25 C82 C83 117.6(9) . . ?
O25 C82 C81 122.2(9) . . ?
C83 C82 C81 120.0 . . ?
C82 C83 C84 120.0 . . ?
C82 C83 H83 120.0 . . ?
C84 C83 H83 120.0 . . ?
C83 C84 C85 120.0 . . ?
C83 C84 H84 120.0 . . ?
C85 C84 H84 120.0 . . ?
C98 C85 C84 119.6(5) 7_666 . ?
C98 C85 C80 120.4(5) 7_666 . ?
C84 C85 C80 120.0 . . ?
C85 C98 C80 123.5(6) 7_666 . ?
C85 C98 H98 118.2 7_666 . ?
C80 C98 H98 118.2 . . ?
C75 C70 C78 116.1(5) . . ?
C75 C70 H70 121.9 . . ?
C78 C70 H70 121.9 . . ?
C75 O84 H94 109.5 . . ?
C78 C75 O84 119.6(5) 7_666 . ?
C78 C75 C70 120.4(5) 7_666 . ?
O84 C75 C70 120.0 . . ?
C78 C75 C78 33.0(3) 7_666 2 ?
O84 C75 C78 113.2(2) . 2 ?
C70 C75 C78 116.3(2) . 2 ?
C75 C78 C70 123.5(6) 7_666 . ?
C75 C78 H78 118.2 7_666 . ?
C70 C78 H78 118.2 . . ?
C43 N1 Pd1 110.6(4) . . ?
C43 N1 H1A 109.5 . . ?
Pd1 N1 H1A 109.5 . . ?
C43 N1 H1B 109.5 . . ?
Pd1 N1 H1B 109.5 . . ?
H1A N1 H1B 108.1 . . ?
C42 N2 Pd1 108.0(4) . . ?
C42 N2 H2A 110.1 . . ?
Pd1 N2 H2A 110.1 . . ?
C42 N2 H2B 110.1 . . ?
Pd1 N2 H2B 110.1 . . ?
H2A N2 H2B 108.4 . . ?
C1 N3 C5 119.7(5) . . ?
C1 N3 Pd1 119.4(4) . . ?
C5 N3 Pd1 120.7(4) . . ?
C24 N4 C25 121.5(4) . . ?
C24 N4 C23 119.4(5) . . ?
C25 N4 C23 119.1(5) . . ?
C14 N5 C22 120.4(5) . . ?
C14 N5 Pd1 119.1(4) . 7_655 ?
C22 N5 Pd1 120.4(4) . 7_655 ?
O3 N6 O1 116.9(7) . . ?
O3 N6 O2 121.8(8) . . ?
O1 N6 O2 121.0(8) . . ?
O69 N8 O70 112.0(16) . . ?
O69 N8 O12 140.2(17) . . ?
O70 N8 O12 107.8(15) . . ?
C29 O4 H4 109.5 . . ?
C36 O7 H7A 109.5 . . ?
C35 O8 H8A 109.5 . . ?
C82 O25 H25A 109.5 . . ?
N2 Pd1 N1 84.2(2) . . ?
N2 Pd1 N3 92.94(18) . . ?
N1 Pd1 N3 176.8(2) . . ?
N2 Pd1 N5 177.91(18) . 7_655 ?
N1 Pd1 N5 93.76(19) . 7_655 ?
N3 Pd1 N5 89.13(17) . 7_655 ?

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
N3 C1 C2 C3 -1.0(8) . . . . ?
N3 C1 C2 C7 179.8(6) . . . . ?
C1 C2 C3 C4 2.3(7) . . . . ?
C7 C2 C3 C4 -178.5(5) . . . . ?
C1 C2 C3 C10 -175.4(4) . . . . ?
C7 C2 C3 C10 3.7(8) . . . . ?
C2 C3 C4 C5 -1.5(7) . . . . ?
C10 C3 C4 C5 176.2(4) . . . . ?
C2 C3 C4 C13 -179.8(5) . . . . ?
C10 C3 C4 C13 -2.0(7) . . . . ?
C3 C4 C5 N3 -0.6(8) . . . . ?
C13 C4 C5 N3 177.6(5) . . . . ?
C1 C2 C7 C8 174.2(6) . . . . ?
C3 C2 C7 C8 -5.0(10) . . . . ?
C2 C7 C8 C9 3.6(10) . . . . ?
C7 C8 C9 C25 -179.9(6) . . . . ?
C7 C8 C9 C10 -1.1(9) . . . . ?
C25 C9 C10 C11 -0.6(7) . . . . ?
C8 C9 C10 C11 -179.4(5) . . . . ?
C25 C9 C10 C3 178.7(4) . . . . ?
C8 C9 C10 C3 -0.1(7) . . . . ?
C2 C3 C10 C11 178.0(4) . . . . ?
C4 C3 C10 C11 0.2(7) . . . . ?
C2 C3 C10 C9 -1.3(7) . . . . ?
C4 C3 C10 C9 -179.1(4) . . . . ?
C9 C10 C11 C24 1.1(7) . . . . ?
C3 C10 C11 C24 -178.1(4) . . . . ?
C9 C10 C11 C12 178.7(4) . . . . ?
C3 C10 C11 C12 -0.6(7) . . . . ?
C24 C11 C12 C13 -179.7(5) . . . . ?
C10 C11 C12 C13 2.9(8) . . . . ?
C11 C12 C13 C4 -4.8(9) . . . . ?
C5 C4 C13 C12 -173.7(6) . . . . ?
C3 C4 C13 C12 4.4(9) . . . . ?
N5 C14 C15 C16 0.4(9) . . . . ?
C14 C15 C16 C17 1.0(8) . . . . ?
C14 C15 C16 C23 -177.2(5) . . . . ?
C15 C16 C17 C18 177.7(5) . . . . ?
C23 C16 C17 C18 -4.2(8) . . . . ?
C15 C16 C17 C22 -0.8(7) . . . . ?
C23 C16 C17 C22 177.3(5) . . . . ?
C16 C17 C18 C19 179.8(5) . . . . ?
C22 C17 C18 C19 -1.7(8) . . . . ?
C17 C18 C19 C20 1.8(9) . . . . ?
C18 C19 C20 C21 -0.8(10) . . . . ?
C19 C20 C21 C22 -0.2(9) . . . . ?
C20 C21 C22 N5 -179.7(5) . . . . ?
C20 C21 C22 C17 0.2(8) . . . . ?
C16 C17 C22 N5 -0.8(7) . . . . ?
C18 C17 C22 N5 -179.4(5) . . . . ?
C16 C17 C22 C21 179.3(5) . . . . ?
C18 C17 C22 C21 0.7(7) . . . . ?
C15 C16 C23 N4 88.6(6) . . . . ?
C17 C16 C23 N4 -89.6(6) . . . . ?
C10 C11 C24 N4 -0.4(7) . . . . ?
C12 C11 C24 N4 -177.9(4) . . . . ?
C10 C9 C25 N4 -0.8(7) . . . . ?
C8 C9 C25 N4 178.0(5) . . . . ?
C31 C26 C27 C28 -175.4(7) 2 . . . ?
C31 C26 C27 C28 4.6(7) . . . . ?
C31 C26 C27 C28 4.6(7) 2 . . 2 ?
C31 C26 C27 C28 -175.4(7) . . . 2 ?
C26 C27 C28 C29 -3.5(9) . . . . ?
C28 C27 C28 C29 176.5(9) 2 . . . ?
C27 C28 C29 O4 -175.8(7) . . . . ?
C27 C28 C29 C30 -1.0(13) . . . . ?
O4 C29 C30 C31 179.4(9) . . . . ?
C28 C29 C30 C31 4.2(14) . . . . ?
C31 C26 C31 C30 178.9(13) 2 . . . ?
C27 C26 C31 C30 -1.1(13) . . . . ?
C29 C30 C31 C26 -3.2(15) . . . . ?
C46 C32 C33 C33 1.7(10) . . . 5_576 ?
C36 C32 C33 C33 1.7(10) . . . 5_576 ?
C46 C32 C33 C34 179.9(6) . . . . ?
C36 C32 C33 C34 179.9(6) . . . . ?
C33 C33 C34 C45 -0.9(10) 5_576 . . . ?
C32 C33 C34 C45 -178.9(6) . . . . ?
C33 C33 C34 C35 -0.9(10) 5_576 . . . ?
C32 C33 C34 C35 -178.9(6) . . . . ?
C33 C34 C35 O8 176.0(7) . . . . ?
C33 C34 C35 C36 -0.3(10) . . . 5_576 ?
C33 C32 C36 O7 -179.6(8) . . . . ?
C33 C32 C36 C35 -0.6(10) . . . 5_576 ?
C33 C34 C45 C46 -0.3(10) . . . 5_576 ?
C33 C32 C46 C45 -0.6(10) . . . 5_576 ?
C60 C63 C64 C65 -178.4(12) . . . . ?
C50 C63 C64 C65 -178.4(12) . . . . ?
C60 C63 C64 C64 -1.4(17) . . . 2_655 ?
C50 C63 C64 C64 -1.4(17) . . . 2_655 ?
C63 C64 C65 C66 179.6(12) . . . . ?
C64 C64 C65 C66 2.7(18) 2_655 . . . ?
C63 C64 C65 C56 179.6(12) . . . . ?
C64 C64 C65 C56 2.7(18) 2_655 . . . ?
C64 C63 C50 C50 1(2) . . . 2_655 ?
C64 C63 C50 O5 179.0(13) . . . . ?
C64 C65 C56 O6 170(2) . . . . ?
C64 C65 C56 C56 -1(2) . . . 2_655 ?
C64 C63 C60 C60 1(2) . . . 2_655 ?
C64 C65 C66 C66 -1(2) . . . 2_655 ?
N1 C43 C42 N2 46.6(11) . . . . ?
C85 C80 C81 C82 0.0 . . . . ?
C98 C80 C81 C82 178.9(5) . . . . ?
C80 C81 C82 O25 175.3(11) . . . . ?
C80 C81 C82 C83 0.0 . . . . ?
O25 C82 C83 C84 -175.5(10) . . . . ?
C81 C82 C83 C84 0.0 . . . . ?
C82 C83 C84 C85 0.0 . . . . ?
C83 C84 C85 C98 180.0(5) . . . 7_666 ?
C83 C84 C85 C80 0.0 . . . . ?
C81 C80 C85 C98 -180.0(5) . . . 7_666 ?
C98 C80 C85 C98 1.0(6) . . . 7_666 ?
C81 C80 C85 C84 0.0 . . . . ?
C98 C80 C85 C84 -179.0(5) . . . . ?
C81 C80 C98 C85 180.0(9) . . . 7_666 ?
C85 C80 C98 C85 -1.1(8) . . . 7_666 ?
C78 C70 C75 C78 1.0(6) . . . 7_666 ?
C78 C70 C75 O84 -179.0(5) . . . . ?
C78 C70 C75 C78 38.5(4) . . . 2 ?
C75 C70 C78 C75 -1.1(8) . . . 7_666 ?
C42 C43 N1 Pd1 -32.5(9) . . . . ?
C43 C42 N2 Pd1 -37.1(9) . . . . ?
C2 C1 N3 C5 -1.0(8) . . . . ?
C2 C1 N3 Pd1 175.0(4) . . . . ?
C4 C5 N3 C1 1.9(8) . . . . ?
C4 C5 N3 Pd1 -174.2(4) . . . . ?
C11 C24 N4 C25 -1.0(7) . . . . ?
C11 C24 N4 C23 176.2(4) . . . . ?
C9 C25 N4 C24 1.6(7) . . . . ?
C9 C25 N4 C23 -175.6(4) . . . . ?
C16 C23 N4 C24 -86.3(6) . . . . ?
C16 C23 N4 C25 91.0(6) . . . . ?
C15 C14 N5 C22 -2.1(8) . . . . ?
C15 C14 N5 Pd1 174.6(4) . . . 7_655 ?
C21 C22 N5 C14 -177.8(5) . . . . ?
C17 C22 N5 C14 2.2(7) . . . . ?
C21 C22 N5 Pd1 5.5(6) . . . 7_655 ?
C17 C22 N5 Pd1 -174.4(4) . . . 7_655 ?

_refine_diff_density_max         1.507
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.166



loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 151 55 ' '
2 0.000 0.500 0.500 151 55 ' '
3 0.200 0.447 0.837 15 6 ' '
4 0.200 0.553 0.337 14 5 ' '
5 0.305 0.051 0.162 15 5 ' '
6 0.305 0.949 0.662 15 5 ' '
7 0.501 0.000 -0.001 149 54 ' '
8 0.501 0.000 0.499 150 55 ' '
9 0.700 0.053 0.337 14 5 ' '
10 0.700 0.947 0.837 15 6 ' '
11 0.800 0.447 0.663 14 5 ' '
12 0.800 0.553 0.163 13 4 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
One of the nitrate counterions in the assymmetric
unit is disordered and could not be modelled adequately
by assigning specific positions to those atoms.
These 8 nitrate anions in the unit cell have been 
treated as a diffuse contribution 
to the overall scattering by SQUEEZE/PLATON.
;

# start Validation Reply Form
_vrf_CHEMW03_shelx               
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: One of the nitrate counterions in the assymmetric
unit is disordered and could not be modelled adequately
by assigning specific positions to those atoms.
These 8 nitrate anions in the unit cell have been 
treated as a diffuse contribution 
to the overall scattering by SQUEEZE/PLATON, and they were
introduced in the chemical formula.
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact  O50B   ..  O70     ..       2.18 Ang.  
RESPONSE: These alerts correspond to short contacts between different
O atoms of water molecules or a water molecule and a nitrate anion, 
likely involved in hydrogen bonding. 
;
# end Validation Reply Form
