# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1408631'
_audit_update_record             
;
2015-06-24 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C16 H8 F2 N2 O6 Pd) 2(C16 H36 N)'
_chemical_formula_sum            'C48 H80 F2 N4 O6 Pd'
_chemical_formula_weight         953.56

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'
F F 0.0171 0.0103 '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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.6448(7)
_cell_length_b                   16.3141(12)
_cell_length_c                   16.9067(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.808(3)
_cell_angle_gamma                90
_cell_volume                     2657.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9840
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.41

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.402
_shelx_estimated_absorpt_T_min   0.872
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8722
_exptl_absorpt_correction_T_max  0.9724
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34933
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.736
_diffrn_reflns_theta_max         26.746
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5622
_reflns_number_gt                4450
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0525P)²+0.5165P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5622
_refine_ls_number_parameters     281
_refine_ls_number_restraints     190
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.1008
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.090
_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
Pd1 Pd 0.5000 0.5000 0.0000 0.04195(9) Uani 1 2 d S . P . .
C1 C 0.3134(2) 0.61541(14) 0.05596(13) 0.0559(5) Uani 1 1 d . U . . .
C2 C 0.4412(2) 0.62335(14) 0.11286(13) 0.0584(5) Uani 1 1 d . U . . .
O1 O 0.32344(15) 0.56431(10) -0.00225(9) 0.0586(4) Uani 1 1 d . U . . .
O2 O 0.20994(19) 0.65746(13) 0.06495(11) 0.0797(5) Uani 1 1 d . U . . .
O3 O 0.4387(2) 0.67239(14) 0.16880(13) 0.1007(7) Uani 1 1 d . U . . .
N1 N 0.54689(18) 0.57526(10) 0.09398(9) 0.0483(4) Uani 1 1 d . U . . .
C3 C 0.6734(2) 0.57731(13) 0.14135(13) 0.0542(5) Uani 1 1 d . U . . .
C4 C 0.7980(3) 0.56819(15) 0.10474(17) 0.0672(6) Uani 1 1 d . U . . .
H4 H 0.7979 0.5622 0.0500 0.081 Uiso 1 1 calc R U . . .
C5 C 0.9248(3) 0.56786(17) 0.1498(2) 0.0870(8) Uani 1 1 d . U . . .
H5 H 1.0089 0.5625 0.1256 0.104 Uiso 1 1 calc R U . . .
C6 C 0.9205(4) 0.57558(18) 0.2301(2) 0.0932(9) Uani 1 1 d . U . . .
C7 C 0.8009(4) 0.58537(19) 0.2679(2) 0.0923(9) Uani 1 1 d . U . . .
H7 H 0.8026 0.5913 0.3227 0.111 Uiso 1 1 calc R U . . .
C8 C 0.6761(3) 0.58643(16) 0.22368(16) 0.0723(7) Uani 1 1 d . U . . .
H8 H 0.5934 0.5933 0.2490 0.087 Uiso 1 1 calc R U . . .
F1 F 1.0444(2) 0.57306(13) 0.27425(16) 0.1425(9) Uani 1 1 d . U . . .
N2 N 0.77405(18) 0.29777(11) 0.19371(10) 0.0508(4) Uani 1 1 d . . . . .
C9 C 0.6592(2) 0.36216(15) 0.19324(15) 0.0586(6) Uani 1 1 d . U . . .
H9A H 0.6988 0.4131 0.2134 0.070 Uiso 1 1 calc R U . . .
H9B H 0.6269 0.3717 0.1388 0.070 Uiso 1 1 calc R U . . .
C10 C 0.5341(3) 0.34120(18) 0.24111(16) 0.0740(7) Uani 1 1 d . U . . .
H10A H 0.4915 0.2911 0.2209 0.089 Uiso 1 1 calc R U . . .
H10B H 0.5642 0.3321 0.2960 0.089 Uiso 1 1 calc R U . . .
C11 C 0.4285(3) 0.4099(2) 0.2363(2) 0.1076(11) Uani 1 1 d . U . . .
H11A H 0.4005 0.4195 0.1812 0.129 Uiso 1 1 calc R U . . .
H11B H 0.4716 0.4597 0.2569 0.129 Uiso 1 1 calc R U . . .
C12 C 0.3002(3) 0.3917(3) 0.2821(3) 0.1318(16) Uani 1 1 d . U . . .
H12A H 0.2644 0.3388 0.2671 0.198 Uiso 1 1 calc R U . . .
H12B H 0.2309 0.4327 0.2702 0.198 Uiso 1 1 calc R U . . .
H12C H 0.3245 0.3922 0.3378 0.198 Uiso 1 1 calc R U . . .
C13 C 0.8366(2) 0.28246(14) 0.27756(12) 0.0573(5) Uani 1 1 d . U . . .
H13A H 0.7660 0.2575 0.3087 0.069 Uiso 1 1 calc R U . . .
H13B H 0.9117 0.2433 0.2743 0.069 Uiso 1 1 calc R U . . .
C14 C 0.8918(3) 0.35754(16) 0.32102(15) 0.0706(7) Uani 1 1 d . U . . .
H14A H 0.8154 0.3940 0.3316 0.085 Uiso 1 1 calc R U . . .
H14B H 0.9550 0.3867 0.2880 0.085 Uiso 1 1 calc R U . . .
C15 C 0.9671(4) 0.3338(2) 0.39829(17) 0.0923(9) Uani 1 1 d . U . . .
H15A H 1.0482 0.3014 0.3872 0.111 Uiso 1 1 calc R U . . .
H15B H 0.9065 0.3001 0.4289 0.111 Uiso 1 1 calc R U . . .
C16 C 1.0119(5) 0.4081(3) 0.4466(2) 0.1323(16) Uani 1 1 d . U . . .
H16A H 1.0732 0.4411 0.4168 0.198 Uiso 1 1 calc R U . . .
H16B H 1.0592 0.3907 0.4949 0.198 Uiso 1 1 calc R U . . .
H16C H 0.9317 0.4398 0.4586 0.198 Uiso 1 1 calc R U . . .
C17 C 0.7187(2) 0.21517(14) 0.16466(13) 0.0577(5) Uani 1 1 d . U . . .
H17A H 0.6515 0.1960 0.2013 0.069 Uiso 1 1 calc R U . . .
H17B H 0.7950 0.1764 0.1665 0.069 Uiso 1 1 calc R U . . .
C18 C 0.6505(3) 0.21410(16) 0.08146(14) 0.0689(6) Uani 1 1 d . U . . .
H18A H 0.5729 0.2520 0.0788 0.083 Uiso 1 1 calc R U . . .
H18B H 0.7169 0.2321 0.0438 0.083 Uiso 1 1 calc R U . . .
C19 C 0.5996(5) 0.1291(2) 0.0594(2) 0.1148(13) Uani 1 1 d . U . . .
H19A H 0.6769 0.0911 0.0646 0.138 Uiso 1 1 calc R U . . .
H19B H 0.5312 0.1122 0.0963 0.138 Uiso 1 1 calc R U . . .
C20 C 0.5367(6) 0.1238(4) -0.0226(3) 0.163(2) Uani 1 1 d . U . . .
H20A H 0.4516 0.1544 -0.0259 0.244 Uiso 1 1 calc R U . . .
H20B H 0.5179 0.0675 -0.0356 0.244 Uiso 1 1 calc R U . . .
H20C H 0.5999 0.1461 -0.0591 0.244 Uiso 1 1 calc R U . . .
C21 C 0.8829(2) 0.33155(14) 0.13970(13) 0.0564(5) Uani 1 1 d . U . . .
H21A H 0.8379 0.3421 0.0882 0.068 Uiso 1 1 calc R U . . .
H21B H 0.9149 0.3838 0.1610 0.068 Uiso 1 1 calc R U . . .
C22 C 1.0086(2) 0.27847(17) 0.12792(15) 0.0674(6) Uani 1 1 d . U . . .
H22A H 0.9799 0.2268 0.1038 0.081 Uiso 1 1 calc R U . . .
H22B H 1.0555 0.2668 0.1787 0.081 Uiso 1 1 calc R U . . .
C23 C 1.1073(3) 0.3228(2) 0.07476(17) 0.0847(9) Uani 1 1 d . U . . .
H23A H 1.0589 0.3342 0.0243 0.102 Uiso 1 1 calc R U . . .
H23B H 1.1333 0.3748 0.0989 0.102 Uiso 1 1 calc R U . . .
C24 C 1.2375(3) 0.2748(3) 0.0600(2) 0.1101(12) Uani 1 1 d . U . . .
H24A H 1.2836 0.2607 0.1098 0.165 Uiso 1 1 calc R U . . .
H24B H 1.2982 0.3076 0.0297 0.165 Uiso 1 1 calc R U . . .
H24C H 1.2134 0.2257 0.0313 0.165 Uiso 1 1 calc R 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
Pd1 O1 1.9989(14) . ?
Pd1 O1 1.9990(14) 3_665 ?
Pd1 N1 2.0411(16) . ?
Pd1 N1 2.0412(16) 3_665 ?
C1 O2 1.226(3) . ?
C1 O1 1.297(3) . ?
C1 C2 1.532(3) . ?
C2 O3 1.240(3) . ?
C2 N1 1.337(3) . ?
N1 C3 1.426(3) . ?
C3 C4 1.387(3) . ?
C3 C8 1.399(3) . ?
C4 C5 1.409(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.365(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.356(5) . ?
C6 F1 1.379(3) . ?
C7 C8 1.386(4) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
N2 C17 1.522(3) . ?
N2 C9 1.527(3) . ?
N2 C21 1.528(3) . ?
N2 C13 1.534(3) . ?
C9 C10 1.524(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.514(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.520(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.512(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.513(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.514(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.524(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.512(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.488(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.511(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.523(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.510(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

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
O1 Pd1 O1 180.0 . 3_665 ?
O1 Pd1 N1 81.67(6) . . ?
O1 Pd1 N1 98.33(6) 3_665 . ?
O1 Pd1 N1 98.33(6) . 3_665 ?
O1 Pd1 N1 81.67(6) 3_665 3_665 ?
N1 Pd1 N1 180.0 . 3_665 ?
O2 C1 O1 123.0(2) . . ?
O2 C1 C2 120.6(2) . . ?
O1 C1 C2 116.31(18) . . ?
O3 C2 N1 127.2(2) . . ?
O3 C2 C1 119.3(2) . . ?
N1 C2 C1 113.58(18) . . ?
C1 O1 Pd1 114.72(14) . . ?
C2 N1 C3 119.54(18) . . ?
C2 N1 Pd1 113.35(15) . . ?
C3 N1 Pd1 127.01(13) . . ?
C4 C3 C8 118.8(2) . . ?
C4 C3 N1 118.9(2) . . ?
C8 C3 N1 122.4(2) . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 118.0(3) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C7 C6 C5 123.2(3) . . ?
C7 C6 F1 118.9(4) . . ?
C5 C6 F1 117.9(4) . . ?
C6 C7 C8 118.9(3) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C7 C8 C3 120.6(3) . . ?
C7 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
C17 N2 C9 111.38(17) . . ?
C17 N2 C21 111.53(17) . . ?
C9 N2 C21 105.58(15) . . ?
C17 N2 C13 105.66(16) . . ?
C9 N2 C13 111.67(17) . . ?
C21 N2 C13 111.13(17) . . ?
C10 C9 N2 115.86(19) . . ?
C10 C9 H9A 108.3 . . ?
N2 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
N2 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C11 C10 C9 110.7(2) . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C10 C11 C12 113.0(3) . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N2 115.51(18) . . ?
C14 C13 H13A 108.4 . . ?
N2 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
N2 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C13 C14 C15 110.8(2) . . ?
C13 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C14 C15 C16 111.9(3) . . ?
C14 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 C18 115.90(19) . . ?
N2 C17 H17A 108.3 . . ?
C18 C17 H17A 108.3 . . ?
N2 C17 H17B 108.3 . . ?
C18 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C19 C18 C17 111.0(2) . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18B 109.4 . . ?
C17 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 113.3(3) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N2 116.83(18) . . ?
C22 C21 H21A 108.1 . . ?
N2 C21 H21A 108.1 . . ?
C22 C21 H21B 108.1 . . ?
N2 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
C21 C22 C23 109.5(2) . . ?
C21 C22 H22A 109.8 . . ?
C23 C22 H22A 109.8 . . ?
C21 C22 H22B 109.8 . . ?
C23 C22 H22B 109.8 . . ?
H22A C22 H22B 108.2 . . ?
C24 C23 C22 113.6(3) . . ?
C24 C23 H23A 108.8 . . ?
C22 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
C22 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_refine_diff_density_max         0.390
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.137

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1408632'
_audit_update_record             
;
2015-06-24 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H88 Cl2 N4 O10 Pd'
_chemical_formula_weight         1058.52

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   12.5224(9)
_cell_length_b                   15.6996(11)
_cell_length_c                   17.1433(13)
_cell_angle_alpha                63.551(3)
_cell_angle_beta                 69.815(4)
_cell_angle_gamma                82.697(4)
_cell_volume                     2830.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9951
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      21.6

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.475
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54404
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.403
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11951
_reflns_number_gt                8464
_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1025P)²+1.9766P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11951
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1878
_refine_ls_wR_factor_gt          0.1630
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Pd1 Pd 1.0000 0.0000 0.5000 0.04826(13) Uani 1 2 d S . P . .
Cl1 Cl 0.75107(19) -0.45957(11) 0.64495(18) 0.1424(8) Uani 1 1 d . . . . .
Cl2 Cl 0.7649(2) 0.47050(14) 0.9137(2) 0.1623(10) Uani 1 1 d . . . . .
O1 O 0.9159(2) 0.12211(18) 0.4682(2) 0.0621(7) Uani 1 1 d . . . . .
O2 O 0.7422(3) 0.1765(2) 0.4771(3) 0.0910(11) Uani 1 1 d . . . . .
O3 O 0.6641(2) -0.0033(2) 0.5283(3) 0.0741(9) Uani 1 1 d . . . . .
C1 C 0.8085(4) 0.1124(3) 0.4846(3) 0.0606(10) Uani 1 1 d . . . . .
C2 C 0.7651(4) 0.0111(3) 0.5152(3) 0.0563(9) Uani 1 1 d . . . . .
O4 O 0.9147(3) -0.1081(2) 1.0130(2) 0.0697(8) Uani 1 1 d . . . . .
O5 O 0.7516(3) -0.1443(3) 1.0102(3) 0.0926(11) Uani 1 1 d . . . . .
O6 O 0.6845(2) 0.0401(3) 0.9756(2) 0.0742(9) Uani 1 1 d . . . . .
C3 C 0.8155(4) -0.0872(4) 1.0039(3) 0.0681(12) Uani 1 1 d . . . . .
C4 C 0.7789(3) 0.0146(3) 0.9843(3) 0.0610(10) Uani 1 1 d . . . . .
N1 N 0.8461(3) -0.0524(2) 0.5271(2) 0.0531(7) Uani 1 1 d . . . . .
N2 N 0.8579(3) 0.0687(3) 0.9797(2) 0.0625(9) Uani 1 1 d . . . . .
C5 C 0.8203(3) -0.1503(3) 0.5554(3) 0.0533(9) Uani 1 1 d . . . . .
C6 C 0.8345(4) -0.2184(3) 0.6363(3) 0.0730(12) Uani 1 1 d . . . . .
H6 H 0.8589 -0.2002 0.6723 0.088 Uiso 1 1 calc R U . . .
C7 C 0.8125(5) -0.3141(3) 0.6643(4) 0.0861(15) Uani 1 1 d . . . . .
H7 H 0.8225 -0.3601 0.7187 0.103 Uiso 1 1 calc R U . . .
C8 C 0.7761(4) -0.3398(3) 0.6113(4) 0.0810(15) Uani 1 1 d . . . . .
C9 C 0.7597(5) -0.2740(4) 0.5322(4) 0.0866(15) Uani 1 1 d . . . . .
H9 H 0.7333 -0.2928 0.4976 0.104 Uiso 1 1 calc R U . . .
C10 C 0.7824(4) -0.1779(3) 0.5031(3) 0.0687(11) Uani 1 1 d . . . . .
H10 H 0.7721 -0.1325 0.4486 0.082 Uiso 1 1 calc R U . . .
C11 C 0.8361(4) 0.1651(3) 0.9623(3) 0.0651(11) Uani 1 1 d . . . . .
C12 C 0.7930(5) 0.2260(4) 0.8921(4) 0.0871(15) Uani 1 1 d . . . . .
H12 H 0.7784 0.2034 0.8550 0.105 Uiso 1 1 calc R U . . .
C13 C 0.7718(6) 0.3191(5) 0.8772(5) 0.109(2) Uani 1 1 d . . . . .
H13 H 0.7418 0.3590 0.8310 0.131 Uiso 1 1 calc R U . . .
C14 C 0.7953(5) 0.3521(4) 0.9310(6) 0.103(2) Uani 1 1 d . . . . .
C15 C 0.8379(5) 0.2950(5) 0.9998(5) 0.0981(17) Uani 1 1 d . . . . .
H15 H 0.8528 0.3190 1.0359 0.118 Uiso 1 1 calc R U . . .
C16 C 0.8585(4) 0.2025(4) 1.0153(4) 0.0808(13) Uani 1 1 d . . . . .
H16 H 0.8881 0.1636 1.0621 0.097 Uiso 1 1 calc R U . . .
Pd2 Pd 1.0000 0.0000 1.0000 0.05555(14) Uani 1 2 d S . P . .
N4 N 1.1719(4) 0.5525(3) -0.3015(3) 0.0832(12) Uani 1 1 d . . . . .
N3 N 0.4284(3) 0.0025(3) 0.1990(2) 0.0610(8) Uani 1 1 d . . . . .
C17 C 0.4414(4) 0.0970(3) 0.1146(3) 0.0744(12) Uani 1 1 d . . . . .
H17A H 0.5199 0.1049 0.0746 0.089 Uiso 1 1 calc R U . . .
H17B H 0.3943 0.0938 0.0813 0.089 Uiso 1 1 calc R U . . .
C18 C 0.4111(7) 0.1833(4) 0.1322(5) 0.116(2) Uani 1 1 d . . . . .
H18A H 0.4541 0.1862 0.1684 0.139 Uiso 1 1 calc R U . . .
H18B H 0.3307 0.1803 0.1665 0.139 Uiso 1 1 calc R U . . .
C19 C 0.4385(10) 0.2722(6) 0.0397(6) 0.160(4) Uani 1 1 d . . . . .
H19A H 0.5193 0.2735 0.0071 0.191 Uiso 1 1 calc R U . . .
H19B H 0.3982 0.2655 0.0034 0.191 Uiso 1 1 calc R U . . .
C20 C 0.4140(16) 0.3543(9) 0.0424(11) 0.281(9) Uani 1 1 d . . . . .
H20A H 0.3398 0.3499 0.0862 0.422 Uiso 1 1 calc R U . . .
H20B H 0.4148 0.4018 -0.0174 0.422 Uiso 1 1 calc R U . . .
H20C H 0.4694 0.3717 0.0604 0.422 Uiso 1 1 calc R U . . .
C21 C 0.3069(4) -0.0155(4) 0.2650(3) 0.0705(12) Uani 1 1 d . . . . .
H21A H 0.3034 -0.0754 0.3185 0.085 Uiso 1 1 calc R U . . .
H21B H 0.2884 0.0343 0.2860 0.085 Uiso 1 1 calc R U . . .
C22 C 0.2173(4) -0.0192(4) 0.2261(4) 0.0838(14) Uani 1 1 d . . . . .
H22A H 0.2204 0.0403 0.1724 0.101 Uiso 1 1 calc R U . . .
H22B H 0.2339 -0.0699 0.2064 0.101 Uiso 1 1 calc R U . . .
C23 C 0.1003(5) -0.0354(6) 0.2939(4) 0.107(2) Uani 1 1 d . . . . .
H23A H 0.0977 -0.0948 0.3476 0.128 Uiso 1 1 calc R U . . .
H23B H 0.0842 0.0153 0.3136 0.128 Uiso 1 1 calc R U . . .
C24 C 0.0102(5) -0.0393(8) 0.2576(5) 0.140(3) Uani 1 1 d . . . . .
H24A H 0.0155 0.0173 0.2019 0.210 Uiso 1 1 calc R U . . .
H24B H -0.0632 -0.0437 0.3025 0.210 Uiso 1 1 calc R U . . .
H24C H 0.0199 -0.0940 0.2449 0.210 Uiso 1 1 calc R U . . .
C25 C 0.5039(3) 0.0000(3) 0.2542(3) 0.0690(12) Uani 1 1 d . . . . .
H25A H 0.4799 0.0490 0.2759 0.083 Uiso 1 1 calc R U . . .
H25B H 0.4913 -0.0609 0.3078 0.083 Uiso 1 1 calc R U . . .
C26 C 0.6297(4) 0.0145(4) 0.2015(4) 0.0826(14) Uani 1 1 d . . . . .
H26A H 0.6434 0.0742 0.1463 0.099 Uiso 1 1 calc R U . . .
H26B H 0.6561 -0.0365 0.1829 0.099 Uiso 1 1 calc R U . . .
C27 C 0.6960(6) 0.0159(6) 0.2612(5) 0.113(2) Uani 1 1 d . . . . .
H27A H 0.6738 -0.0403 0.3195 0.135 Uiso 1 1 calc R U . . .
H27B H 0.7765 0.0122 0.2308 0.135 Uiso 1 1 calc R U . . .
C28 C 0.6789(7) 0.1006(7) 0.2798(6) 0.145(3) Uani 1 1 d . . . . .
H28A H 0.6987 0.1569 0.2225 0.217 Uiso 1 1 calc R U . . .
H28B H 0.7263 0.0978 0.3144 0.217 Uiso 1 1 calc R U . . .
H28C H 0.6005 0.1023 0.3144 0.217 Uiso 1 1 calc R U . . .
C29 C 0.4611(4) -0.0724(3) 0.1628(3) 0.0685(11) Uani 1 1 d . . . . .
H29A H 0.4130 -0.0664 0.1269 0.082 Uiso 1 1 calc R U . . .
H29B H 0.5389 -0.0589 0.1213 0.082 Uiso 1 1 calc R U . . .
C30 C 0.4522(5) -0.1740(4) 0.2343(4) 0.0872(15) Uani 1 1 d . . . . .
H30A H 0.5023 -0.1823 0.2693 0.105 Uiso 1 1 calc R U . . .
H30B H 0.3748 -0.1892 0.2766 0.105 Uiso 1 1 calc R U . . .
C31 C 0.4848(6) -0.2396(5) 0.1878(5) 0.113(2) Uani 1 1 d . . . . .
H31A H 0.5624 -0.2240 0.1459 0.135 Uiso 1 1 calc R U . . .
H31B H 0.4356 -0.2292 0.1515 0.135 Uiso 1 1 calc R U . . .
C32 C 0.4758(9) -0.3449(6) 0.2563(8) 0.171(4) Uani 1 1 d . . . . .
H32A H 0.5088 -0.3528 0.3020 0.257 Uiso 1 1 calc R U . . .
H32B H 0.5159 -0.3822 0.2241 0.257 Uiso 1 1 calc R U . . .
H32C H 0.3972 -0.3655 0.2857 0.257 Uiso 1 1 calc R U . . .
C33 C 1.1859(11) 0.5981(5) -0.3998(5) 0.162(5) Uani 1 1 d . . . . .
H33A H 1.2051 0.6638 -0.4184 0.195 Uiso 1 1 calc R U . . .
H33B H 1.2560 0.5722 -0.4265 0.195 Uiso 1 1 calc R U . . .
C34 C 1.1273(13) 0.6049(7) -0.4467(9) 0.208(6) Uani 1 1 d . . . . .
H34A H 1.0580 0.6345 -0.4245 0.250 Uiso 1 1 calc R U . . .
H34B H 1.1055 0.5402 -0.4294 0.250 Uiso 1 1 calc R U . . .
C35 C 1.1619(10) 0.6543(7) -0.5503(6) 0.157(3) Uani 1 1 d . . . . .
H35A H 1.1927 0.7172 -0.5708 0.188 Uiso 1 1 calc R U . . .
H35B H 1.2228 0.6192 -0.5749 0.188 Uiso 1 1 calc R U . . .
C36 C 1.0782(10) 0.6644(10) -0.5882(9) 0.207(5) Uani 1 1 d . . . . .
H36A H 1.0402 0.6039 -0.5629 0.310 Uiso 1 1 calc R U . . .
H36B H 1.1116 0.6872 -0.6537 0.310 Uiso 1 1 calc R U . . .
H36C H 1.0242 0.7091 -0.5744 0.310 Uiso 1 1 calc R U . . .
C37 C 1.0837(6) 0.6124(10) -0.2538(6) 0.205(6) Uani 1 1 d . . . . .
H37A H 1.1127 0.6777 -0.2906 0.247 Uiso 1 1 calc R U . . .
H37B H 1.0141 0.6103 -0.2657 0.247 Uiso 1 1 calc R U . . .
C38 C 1.0513(12) 0.6019(10) -0.1711(10) 0.219(5) Uiso 1 1 d . . . . .
H38A H 1.1180 0.6031 -0.1551 0.263 Uiso 1 1 calc R U . . .
H38B H 1.0144 0.5395 -0.1312 0.263 Uiso 1 1 calc R U . . .
C39 C 0.9725(8) 0.6736(7) -0.1519(7) 0.142(3) Uani 1 1 d . . . . .
H39A H 0.9082 0.6697 -0.1695 0.171 Uiso 1 1 calc R U . . .
H39B H 0.9447 0.6488 -0.0853 0.171 Uiso 1 1 calc R U . . .
C40 C 0.9923(11) 0.7712(9) -0.1839(8) 0.209(5) Uani 1 1 d . . . . .
H40A H 1.0727 0.7845 -0.2056 0.313 Uiso 1 1 calc R U . . .
H40B H 0.9558 0.7895 -0.1345 0.313 Uiso 1 1 calc R U . . .
H40C H 0.9618 0.8065 -0.2333 0.313 Uiso 1 1 calc R U . . .
C41 C 1.1382(13) 0.4515(6) -0.2633(7) 0.219(7) Uani 1 1 d . . . . .
H41A H 1.1435 0.4258 -0.2018 0.263 Uiso 1 1 calc R U . . .
H41B H 1.0573 0.4545 -0.2544 0.263 Uiso 1 1 calc R U . . .
C42 C 1.1654(14) 0.3855(6) -0.2831(7) 0.253(9) Uani 1 1 d . . . . .
H42A H 1.2452 0.3772 -0.2878 0.303 Uiso 1 1 calc R U . . .
H42B H 1.1638 0.4096 -0.3455 0.303 Uiso 1 1 calc R U . . .
C43 C 1.1168(9) 0.2895(6) -0.2369(7) 0.158(3) Uani 1 1 d . . . . .
H43A H 1.0958 0.2690 -0.1710 0.190 Uiso 1 1 calc R U . . .
H43B H 1.0472 0.2919 -0.2506 0.190 Uiso 1 1 calc R U . . .
C44 C 1.1826(11) 0.2223(8) -0.2578(8) 0.194(5) Uani 1 1 d . . . . .
H44A H 1.1492 0.2004 -0.2886 0.290 Uiso 1 1 calc R U . . .
H44B H 1.1878 0.1698 -0.2022 0.290 Uiso 1 1 calc R U . . .
H44C H 1.2573 0.2491 -0.2975 0.290 Uiso 1 1 calc R U . . .
C45 C 1.2801(7) 0.5600(9) -0.2853(11) 0.229(7) Uani 1 1 d . . . . .
H45A H 1.2772 0.5002 -0.2319 0.275 Uiso 1 1 calc R U . . .
H45B H 1.3369 0.5513 -0.3363 0.275 Uiso 1 1 calc R U . . .
C46 C 1.3301(8) 0.6100(12) -0.2741(10) 0.232(7) Uani 1 1 d . . . . .
H46A H 1.2802 0.6106 -0.2167 0.279 Uiso 1 1 calc R U . . .
H46B H 1.3242 0.6725 -0.3215 0.279 Uiso 1 1 calc R U . . .
C47 C 1.4377(9) 0.6135(10) -0.2698(12) 0.215(6) Uani 1 1 d . . . . .
H47A H 1.4642 0.5491 -0.2543 0.258 Uiso 1 1 calc R U . . .
H47B H 1.4840 0.6512 -0.3329 0.258 Uiso 1 1 calc R U . . .
C48 C 1.466(2) 0.6389(16) -0.2263(17) 0.343(13) Uiso 1 1 d . . . . .
H48A H 1.4753 0.7070 -0.2563 0.514 Uiso 1 1 calc R U . . .
H48B H 1.5374 0.6111 -0.2200 0.514 Uiso 1 1 calc R U . . .
H48C H 1.4097 0.6197 -0.1665 0.514 Uiso 1 1 calc R U . . .
O1W O 0.4818(4) 0.1189(3) 0.4890(4) 0.1262(17) Uani 1 1 d . . . . .
O2W O 0.5168(4) 0.2449(4) 0.5426(4) 0.1241(15) Uani 1 1 d . . . . .
O3W O 0.4375(8) 0.4280(6) 0.5052(8) 0.239(4) Uani 1 1 d . . . . .
O4W O 0.8351(11) 0.6737(6) 0.0621(5) 0.260(5) 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
Pd1 O1 2.008(3) 2_756 ?
Pd1 O1 2.008(3) . ?
Pd1 N1 2.013(3) 2_756 ?
Pd1 N1 2.013(3) . ?
Cl1 C8 1.740(5) . ?
Cl2 C14 1.759(6) . ?
O1 C1 1.290(5) . ?
O2 C1 1.211(5) . ?
O3 C2 1.238(5) . ?
C1 C2 1.543(6) . ?
C2 N1 1.330(5) . ?
O4 C3 1.289(5) . ?
O4 Pd2 2.007(3) . ?
O5 C3 1.221(5) . ?
O6 C4 1.235(5) . ?
C3 C4 1.523(7) . ?
C4 N2 1.345(5) . ?
N1 C5 1.435(5) . ?
N2 C11 1.415(6) . ?
N2 Pd2 2.013(3) . ?
C5 C6 1.377(6) . ?
C5 C10 1.380(6) . ?
C6 C7 1.392(6) . ?
C7 C8 1.362(8) . ?
C8 C9 1.356(8) . ?
C9 C10 1.395(7) . ?
C11 C12 1.394(7) . ?
C11 C16 1.395(7) . ?
C12 C13 1.373(8) . ?
C13 C14 1.363(10) . ?
C14 C15 1.360(10) . ?
C15 C16 1.362(8) . ?
Pd2 O4 2.007(3) 2_757 ?
Pd2 N2 2.013(3) 2_757 ?
N4 C33 1.462(9) . ?
N4 C41 1.475(8) . ?
N4 C45 1.501(10) . ?
N4 C37 1.605(11) . ?
N3 C29 1.514(6) . ?
N3 C21 1.521(5) . ?
N3 C17 1.519(6) . ?
N3 C25 1.537(5) . ?
C17 C18 1.492(8) . ?
C18 C19 1.535(10) . ?
C19 C20 1.304(13) . ?
C21 C22 1.508(7) . ?
C22 C23 1.488(7) . ?
C23 C24 1.484(8) . ?
C25 C26 1.508(6) . ?
C26 C27 1.532(7) . ?
C27 C28 1.474(10) . ?
C29 C30 1.506(7) . ?
C30 C31 1.504(8) . ?
C31 C32 1.534(11) . ?
C33 C34 1.227(13) . ?
C34 C35 1.508(13) . ?
C35 C36 1.370(13) . ?
C37 C38 1.269(14) . ?
C38 C39 1.474(13) . ?
C39 C40 1.401(13) . ?
C41 C42 1.203(13) . ?
C42 C43 1.452(11) . ?
C43 C44 1.354(12) . ?
C45 C46 1.178(12) . ?
C46 C47 1.384(12) . ?
C47 C48 1.15(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
O1 Pd1 O1 180.0 2_756 . ?
O1 Pd1 N1 81.03(12) 2_756 2_756 ?
O1 Pd1 N1 98.97(12) . 2_756 ?
O1 Pd1 N1 98.97(12) 2_756 . ?
O1 Pd1 N1 81.03(12) . . ?
N1 Pd1 N1 180.0 2_756 . ?
C1 O1 Pd1 114.9(2) . . ?
O2 C1 O1 124.5(4) . . ?
O2 C1 C2 119.5(4) . . ?
O1 C1 C2 116.0(3) . . ?
O3 C2 N1 127.9(4) . . ?
O3 C2 C1 119.9(4) . . ?
N1 C2 C1 112.1(3) . . ?
C3 O4 Pd2 114.5(3) . . ?
O5 C3 O4 123.5(5) . . ?
O5 C3 C4 119.8(4) . . ?
O4 C3 C4 116.7(4) . . ?
O6 C4 N2 126.3(5) . . ?
O6 C4 C3 120.8(4) . . ?
N2 C4 C3 112.8(4) . . ?
C2 N1 C5 119.4(3) . . ?
C2 N1 Pd1 115.6(3) . . ?
C5 N1 Pd1 124.9(2) . . ?
C4 N2 C11 119.5(4) . . ?
C4 N2 Pd2 114.3(3) . . ?
C11 N2 Pd2 126.2(3) . . ?
C6 C5 C10 119.4(4) . . ?
C6 C5 N1 119.1(4) . . ?
C10 C5 N1 121.5(4) . . ?
C5 C6 C7 120.3(5) . . ?
C8 C7 C6 119.3(5) . . ?
C7 C8 C9 121.4(4) . . ?
C7 C8 Cl1 119.5(5) . . ?
C9 C8 Cl1 119.1(5) . . ?
C8 C9 C10 119.7(5) . . ?
C5 C10 C9 119.9(5) . . ?
C12 C11 C16 117.6(5) . . ?
C12 C11 N2 122.1(5) . . ?
C16 C11 N2 120.2(4) . . ?
C13 C12 C11 120.9(6) . . ?
C14 C13 C12 119.1(6) . . ?
C13 C14 C15 121.8(6) . . ?
C13 C14 Cl2 119.1(6) . . ?
C15 C14 Cl2 119.1(6) . . ?
C16 C15 C14 119.4(6) . . ?
C15 C16 C11 121.2(5) . . ?
O4 Pd2 O4 180.0 2_757 . ?
O4 Pd2 N2 98.40(14) 2_757 . ?
O4 Pd2 N2 81.60(14) . . ?
O4 Pd2 N2 81.61(14) 2_757 2_757 ?
O4 Pd2 N2 98.39(14) . 2_757 ?
N2 Pd2 N2 180.0(2) . 2_757 ?
C33 N4 C41 109.0(6) . . ?
C33 N4 C45 111.2(8) . . ?
C41 N4 C45 109.8(8) . . ?
C33 N4 C37 108.2(6) . . ?
C41 N4 C37 114.7(8) . . ?
C45 N4 C37 103.9(5) . . ?
C29 N3 C21 110.5(3) . . ?
C29 N3 C17 105.5(3) . . ?
C21 N3 C17 111.4(4) . . ?
C29 N3 C25 111.5(3) . . ?
C21 N3 C25 106.2(3) . . ?
C17 N3 C25 111.8(3) . . ?
C18 C17 N3 116.2(4) . . ?
C17 C18 C19 109.1(6) . . ?
C20 C19 C18 117.2(11) . . ?
C22 C21 N3 115.5(4) . . ?
C23 C22 C21 112.7(4) . . ?
C24 C23 C22 113.9(5) . . ?
C26 C25 N3 114.9(3) . . ?
C25 C26 C27 110.5(5) . . ?
C28 C27 C26 114.6(6) . . ?
C30 C29 N3 116.0(4) . . ?
C31 C30 C29 109.6(5) . . ?
C30 C31 C32 112.8(7) . . ?
C34 C33 N4 135.5(12) . . ?
C33 C34 C35 126.3(13) . . ?
C36 C35 C34 116.6(11) . . ?
C38 C37 N4 129.9(11) . . ?
C37 C38 C39 115.4(13) . . ?
C40 C39 C38 129.3(11) . . ?
C42 C41 N4 138.4(13) . . ?
C41 C42 C43 130.2(14) . . ?
C44 C43 C42 117.2(11) . . ?
C46 C45 N4 142.1(11) . . ?
C45 C46 C47 136.2(14) . . ?
C48 C47 C46 129.7(18) . . ?

_refine_diff_density_max         0.947
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.117

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1408633'
_audit_update_record             
;
2015-06-24 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C16 H8 Br2 N2 O6 Pd), 2(C16 H36 N), 2(H2 O)'
_chemical_formula_sum            'C48 H88 Br2 N4 O10 Pd'
_chemical_formula_weight         1147.44

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'
Br Br -0.2901 2.4595 '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           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   14.827(4)
_cell_length_b                   14.635(4)
_cell_length_c                   15.017(4)
_cell_angle_alpha                90
_cell_angle_beta                 114.983(9)
_cell_angle_gamma                90
_cell_volume                     2953.8(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9643
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      26.07

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.718
_shelx_estimated_absorpt_T_min   0.673
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6175
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27339
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.043
_diffrn_reflns_theta_max         25.676
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5573
_reflns_number_gt                4607
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0700P)²+1.0415P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     DIRECT
_atom_sites_solution_secondary   DIFMAP
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5573
_refine_ls_number_parameters     309
_refine_ls_number_restraints     242
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1276
_refine_ls_wR_factor_gt          0.1189
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.063
_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
Pd1 Pd 0.5000 0.63531(2) 0.2500 0.04100(13) Uani 1 2 d S T P . .
Br1 Br 0.41422(5) 1.12772(3) 0.33372(5) 0.1099(2) Uani 1 1 d . . . . .
O1 O 0.40688(15) 0.53854(14) 0.25635(15) 0.0532(5) Uani 1 1 d . . . . .
O2 O 0.26587(16) 0.51873(17) 0.27106(17) 0.0639(6) Uani 1 1 d . . . . .
O3 O 0.24941(16) 0.70636(17) 0.27908(17) 0.0649(6) Uani 1 1 d . . . . .
C1 C 0.3299(2) 0.5688(2) 0.2653(2) 0.0507(7) Uani 1 1 d . . . . .
C2 C 0.3206(2) 0.6723(2) 0.2689(2) 0.0478(7) Uani 1 1 d . . . . .
N1 N 0.39774(17) 0.71764(17) 0.26476(17) 0.0456(5) Uani 1 1 d . . . . .
C3 C 0.4004(2) 0.8135(2) 0.2790(2) 0.0477(6) Uani 1 1 d . U . . .
C4 C 0.4814(3) 0.8530(2) 0.3539(3) 0.0583(8) Uani 1 1 d . U . . .
H4 H 0.5343 0.8164 0.3939 0.070 Uiso 1 1 calc R U . . .
C5 C 0.4856(3) 0.9461(3) 0.3707(3) 0.0697(9) Uani 1 1 d . U . . .
H5 H 0.5402 0.9720 0.4220 0.084 Uiso 1 1 calc R U . . .
C6 C 0.4080(3) 0.9998(3) 0.3105(3) 0.0702(9) Uani 1 1 d . U . . .
C7 C 0.3267(3) 0.9631(3) 0.2350(3) 0.0732(10) Uani 1 1 d . U . . .
H7 H 0.2746 1.0004 0.1950 0.088 Uiso 1 1 calc R U . . .
C8 C 0.3230(3) 0.8697(2) 0.2188(3) 0.0624(8) Uani 1 1 d . U . . .
H8 H 0.2683 0.8444 0.1672 0.075 Uiso 1 1 calc R U . . .
N2 N 0.24475(18) 0.67365(18) 0.54069(17) 0.0545(6) Uani 1 1 d D U . . .
C1S C 0.1954(2) 0.5919(2) 0.4754(2) 0.0575(7) Uani 1 1 d D U . . .
H1S1 H 0.1240 0.6017 0.4456 0.069 Uiso 1 1 calc R U . . .
H1S2 H 0.2170 0.5899 0.4228 0.069 Uiso 1 1 calc R U . . .
C2S C 0.2161(3) 0.5002(2) 0.5258(2) 0.0649(8) Uani 1 1 d D U . . .
H2S1 H 0.1939 0.5009 0.5780 0.078 Uiso 1 1 calc R U . . .
H2S2 H 0.2873 0.4891 0.5553 0.078 Uiso 1 1 calc R U . . .
C3S C 0.1638(3) 0.4233(2) 0.4545(3) 0.0714(9) Uani 1 1 d D U . . .
H3S1 H 0.0927 0.4348 0.4247 0.086 Uiso 1 1 calc R U . . .
H3S2 H 0.1863 0.4227 0.4025 0.086 Uiso 1 1 calc R U . . .
C4S C 0.1832(3) 0.3322(3) 0.5034(3) 0.0898(12) Uani 1 1 d D U . . .
H4S1 H 0.2536 0.3214 0.5348 0.135 Uiso 1 1 calc R U . . .
H4S2 H 0.1517 0.2856 0.4553 0.135 Uiso 1 1 calc R U . . .
H4S3 H 0.1567 0.3311 0.5518 0.135 Uiso 1 1 calc R U . . .
C5S C 0.3569(2) 0.6627(2) 0.5916(2) 0.0582(8) Uani 1 1 d D U . . .
H5S1 H 0.3842 0.7149 0.6345 0.070 Uiso 1 1 calc R U . . .
H5S2 H 0.3717 0.6088 0.6329 0.070 Uiso 1 1 calc R U . . .
C6S C 0.4104(2) 0.6543(3) 0.5258(3) 0.0656(9) Uani 1 1 d D U . . .
H6S1 H 0.4034 0.7104 0.4891 0.079 Uiso 1 1 calc R U . . .
H6S2 H 0.3819 0.6048 0.4794 0.079 Uiso 1 1 calc R U . . .
C7S C 0.5195(3) 0.6354(3) 0.5890(3) 0.0694(9) Uani 1 1 d D U . . .
H7S1 H 0.5456 0.6835 0.6377 0.083 Uiso 1 1 calc R U . . .
H7S2 H 0.5251 0.5783 0.6237 0.083 Uiso 1 1 calc R U . . .
C8S C 0.5814(4) 0.6297(4) 0.5344(4) 0.1062(18) Uani 1 1 d D U . . .
H8S1 H 0.5546 0.5842 0.4838 0.159 Uiso 1 1 calc R U . . .
H8S2 H 0.6481 0.6132 0.5785 0.159 Uiso 1 1 calc R U . . .
H8S3 H 0.5819 0.6879 0.5051 0.159 Uiso 1 1 calc R U . . .
C9S C 0.2130(2) 0.6822(3) 0.6242(2) 0.0634(8) Uani 1 1 d D U . . .
H9S1 H 0.2383 0.6296 0.6670 0.076 Uiso 1 1 calc R U . . .
H9S2 H 0.2445 0.7361 0.6623 0.076 Uiso 1 1 calc R U . . .
C10S C 0.1031(3) 0.6888(3) 0.5948(3) 0.0816(12) Uani 1 1 d D U . . .
H10A H 0.0716 0.6307 0.5684 0.098 Uiso 1 1 calc R U . . .
H10B H 0.0743 0.7349 0.5442 0.098 Uiso 1 1 calc R U . . .
C11S C 0.0848(4) 0.7142(4) 0.6848(3) 0.0992(15) Uani 1 1 d D U . . .
H11A H 0.0154 0.7033 0.6698 0.119 Uiso 1 1 calc R U . . .
H11B H 0.1243 0.6741 0.7387 0.119 Uiso 1 1 calc R U . . .
C12S C 0.1092(5) 0.8093(4) 0.7169(6) 0.169(3) Uani 1 1 d D U . . .
H12A H 0.1799 0.8179 0.7432 0.253 Uiso 1 1 calc R U . . .
H12B H 0.0865 0.8229 0.7666 0.253 Uiso 1 1 calc R U . . .
H12C H 0.0770 0.8494 0.6618 0.253 Uiso 1 1 calc R U . . .
C13S C 0.2151(3) 0.7565(2) 0.4738(2) 0.0610(8) Uani 1 1 d D U . . .
H13A H 0.2376 0.7469 0.4225 0.073 Uiso 1 1 calc R U . . .
H13B H 0.1430 0.7594 0.4424 0.073 Uiso 1 1 calc R U . . .
C14S C 0.2537(4) 0.8481(3) 0.5207(3) 0.0867(12) Uani 1 1 d D U . . .
H14A H 0.3256 0.8461 0.5556 0.104 Uiso 1 1 calc R U . . .
H14B H 0.2266 0.8624 0.5676 0.104 Uiso 1 1 calc R U . . .
C15S C 0.2235(5) 0.9213(4) 0.4419(5) 0.134(2) Uani 1 1 d D U . . .
H15A H 0.2675 0.9735 0.4667 0.161 Uiso 0.636(9) 1 calc R U P A 1
H15B H 0.2316 0.8977 0.3853 0.161 Uiso 0.636(9) 1 calc R U P A 1
H15C H 0.2676 0.9154 0.4094 0.161 Uiso 0.364(9) 1 calc R U P A 2
H15D H 0.1573 0.9058 0.3935 0.161 Uiso 0.364(9) 1 calc R U P A 2
C16A C 0.1225(7) 0.9509(8) 0.4114(10) 0.209(6) Uani 0.636(9) 1 d D U P A 1
H16A H 0.1094 1.0018 0.3674 0.314 Uiso 0.636(9) 1 calc R U P A 1
H16B H 0.1123 0.9689 0.4679 0.314 Uiso 0.636(9) 1 calc R U P A 1
H16C H 0.0781 0.9016 0.3785 0.314 Uiso 0.636(9) 1 calc R U P A 1
C16B C 0.2217(15) 1.0157(6) 0.4644(13) 0.153(7) Uani 0.364(9) 1 d D U P A 2
H16D H 0.2099 1.0517 0.4071 0.229 Uiso 0.364(9) 1 calc R U P A 2
H16E H 0.2844 1.0326 0.5163 0.229 Uiso 0.364(9) 1 calc R U P A 2
H16F H 0.1695 1.0264 0.4850 0.229 Uiso 0.364(9) 1 calc R U P A 2
O1W O 0.0577(2) 0.5511(3) 0.1928(2) 0.1060(11) Uani 1 1 d . . . . .
O2W O 0.0447(2) 0.7461(3) 0.1830(2) 0.1221(13) 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
Pd1 O1 2.008(2) 2_655 ?
Pd1 O1 2.008(2) . ?
Pd1 N1 2.021(2) . ?
Pd1 N1 2.021(2) 2_655 ?
Br1 C6 1.899(4) . ?
O1 C1 1.283(4) . ?
O2 C1 1.232(4) . ?
O3 C2 1.234(3) . ?
C1 C2 1.524(5) . ?
C2 N1 1.345(4) . ?
N1 C3 1.417(4) . ?
C3 C4 1.379(5) . ?
C3 C8 1.391(4) . ?
C4 C5 1.382(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.371(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.368(5) . ?
C7 C8 1.385(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
N2 C13S 1.516(4) . ?
N2 C5S 1.517(4) . ?
N2 C9S 1.519(3) . ?
N2 C1S 1.523(4) . ?
C1S C2S 1.507(4) . ?
C1S H1S1 0.9700 . ?
C1S H1S2 0.9700 . ?
C2S C3S 1.521(4) . ?
C2S H2S1 0.9700 . ?
C2S H2S2 0.9700 . ?
C3S C4S 1.491(5) . ?
C3S H3S1 0.9700 . ?
C3S H3S2 0.9700 . ?
C4S H4S1 0.9600 . ?
C4S H4S2 0.9600 . ?
C4S H4S3 0.9600 . ?
C5S C6S 1.511(4) . ?
C5S H5S1 0.9700 . ?
C5S H5S2 0.9700 . ?
C6S C7S 1.515(4) . ?
C6S H6S1 0.9700 . ?
C6S H6S2 0.9700 . ?
C7S C8S 1.468(5) . ?
C7S H7S1 0.9700 . ?
C7S H7S2 0.9700 . ?
C8S H8S1 0.9600 . ?
C8S H8S2 0.9600 . ?
C8S H8S3 0.9600 . ?
C9S C10S 1.501(4) . ?
C9S H9S1 0.9700 . ?
C9S H9S2 0.9700 . ?
C10S C11S 1.533(4) . ?
C10S H10A 0.9700 . ?
C10S H10B 0.9700 . ?
C11S C12S 1.468(6) . ?
C11S H11A 0.9700 . ?
C11S H11B 0.9700 . ?
C12S H12A 0.9600 . ?
C12S H12B 0.9600 . ?
C12S H12C 0.9600 . ?
C13S C14S 1.510(5) . ?
C13S H13A 0.9700 . ?
C13S H13B 0.9700 . ?
C14S C15S 1.517(5) . ?
C14S H14A 0.9700 . ?
C14S H14B 0.9700 . ?
C15S C16B 1.425(8) . ?
C15S C16A 1.436(7) . ?
C15S H15A 0.9700 . ?
C15S H15B 0.9700 . ?
C15S H15C 0.9700 . ?
C15S H15D 0.9700 . ?
C16A H16A 0.9600 . ?
C16A H16B 0.9600 . ?
C16A H16C 0.9600 . ?
C16B H16D 0.9600 . ?
C16B H16E 0.9600 . ?
C16B H16F 0.9600 . ?

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
O1 Pd1 O1 90.30(12) 2_655 . ?
O1 Pd1 N1 171.30(9) 2_655 . ?
O1 Pd1 N1 81.52(10) . . ?
O1 Pd1 N1 81.52(10) 2_655 2_655 ?
O1 Pd1 N1 171.30(9) . 2_655 ?
N1 Pd1 N1 106.80(14) . 2_655 ?
C1 O1 Pd1 114.9(2) . . ?
O2 C1 O1 123.2(3) . . ?
O2 C1 C2 120.4(3) . . ?
O1 C1 C2 116.4(2) . . ?
O3 C2 N1 126.5(3) . . ?
O3 C2 C1 120.0(3) . . ?
N1 C2 C1 113.4(2) . . ?
C2 N1 C3 116.8(2) . . ?
C2 N1 Pd1 113.8(2) . . ?
C3 N1 Pd1 129.20(18) . . ?
C4 C3 C8 118.5(3) . . ?
C4 C3 N1 119.9(3) . . ?
C8 C3 N1 121.6(3) . . ?
C3 C4 C5 121.3(3) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 119.0(3) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C7 C6 C5 121.4(3) . . ?
C7 C6 Br1 119.8(3) . . ?
C5 C6 Br1 118.8(3) . . ?
C6 C7 C8 119.3(3) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C3 120.6(3) . . ?
C7 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
C13S N2 C5S 111.6(2) . . ?
C13S N2 C9S 112.2(3) . . ?
C5S N2 C9S 104.4(2) . . ?
C13S N2 C1S 106.0(2) . . ?
C5S N2 C1S 111.6(2) . . ?
C9S N2 C1S 111.3(2) . . ?
C2S C1S N2 115.8(2) . . ?
C2S C1S H1S1 108.3 . . ?
N2 C1S H1S1 108.3 . . ?
C2S C1S H1S2 108.3 . . ?
N2 C1S H1S2 108.3 . . ?
H1S1 C1S H1S2 107.4 . . ?
C1S C2S C3S 111.7(3) . . ?
C1S C2S H2S1 109.3 . . ?
C3S C2S H2S1 109.3 . . ?
C1S C2S H2S2 109.3 . . ?
C3S C2S H2S2 109.3 . . ?
H2S1 C2S H2S2 107.9 . . ?
C4S C3S C2S 112.3(3) . . ?
C4S C3S H3S1 109.1 . . ?
C2S C3S H3S1 109.1 . . ?
C4S C3S H3S2 109.1 . . ?
C2S C3S H3S2 109.1 . . ?
H3S1 C3S H3S2 107.9 . . ?
C3S C4S H4S1 109.5 . . ?
C3S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
C3S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
C6S C5S N2 116.5(3) . . ?
C6S C5S H5S1 108.2 . . ?
N2 C5S H5S1 108.2 . . ?
C6S C5S H5S2 108.2 . . ?
N2 C5S H5S2 108.2 . . ?
H5S1 C5S H5S2 107.3 . . ?
C5S C6S C7S 108.8(3) . . ?
C5S C6S H6S1 109.9 . . ?
C7S C6S H6S1 109.9 . . ?
C5S C6S H6S2 109.9 . . ?
C7S C6S H6S2 109.9 . . ?
H6S1 C6S H6S2 108.3 . . ?
C8S C7S C6S 114.5(3) . . ?
C8S C7S H7S1 108.6 . . ?
C6S C7S H7S1 108.6 . . ?
C8S C7S H7S2 108.6 . . ?
C6S C7S H7S2 108.6 . . ?
H7S1 C7S H7S2 107.6 . . ?
C7S C8S H8S1 109.5 . . ?
C7S C8S H8S2 109.5 . . ?
H8S1 C8S H8S2 109.5 . . ?
C7S C8S H8S3 109.5 . . ?
H8S1 C8S H8S3 109.5 . . ?
H8S2 C8S H8S3 109.5 . . ?
C10S C9S N2 116.0(3) . . ?
C10S C9S H9S1 108.3 . . ?
N2 C9S H9S1 108.3 . . ?
C10S C9S H9S2 108.3 . . ?
N2 C9S H9S2 108.3 . . ?
H9S1 C9S H9S2 107.4 . . ?
C9S C10S C11S 109.3(3) . . ?
C9S C10S H10A 109.8 . . ?
C11S C10S H10A 109.8 . . ?
C9S C10S H10B 109.8 . . ?
C11S C10S H10B 109.8 . . ?
H10A C10S H10B 108.3 . . ?
C12S C11S C10S 114.1(4) . . ?
C12S C11S H11A 108.7 . . ?
C10S C11S H11A 108.7 . . ?
C12S C11S H11B 108.7 . . ?
C10S C11S H11B 108.7 . . ?
H11A C11S H11B 107.6 . . ?
C11S C12S H12A 109.5 . . ?
C11S C12S H12B 109.5 . . ?
H12A C12S H12B 109.5 . . ?
C11S C12S H12C 109.5 . . ?
H12A C12S H12C 109.5 . . ?
H12B C12S H12C 109.5 . . ?
C14S C13S N2 117.0(3) . . ?
C14S C13S H13A 108.0 . . ?
N2 C13S H13A 108.0 . . ?
C14S C13S H13B 108.0 . . ?
N2 C13S H13B 108.0 . . ?
H13A C13S H13B 107.3 . . ?
C13S C14S C15S 109.6(4) . . ?
C13S C14S H14A 109.8 . . ?
C15S C14S H14A 109.8 . . ?
C13S C14S H14B 109.8 . . ?
C15S C14S H14B 109.8 . . ?
H14A C14S H14B 108.2 . . ?
C16B C15S C14S 121.9(8) . . ?
C16A C15S C14S 112.7(6) . . ?
C16A C15S H15A 109.1 . . ?
C14S C15S H15A 109.1 . . ?
C16A C15S H15B 109.1 . . ?
C14S C15S H15B 109.1 . . ?
H15A C15S H15B 107.8 . . ?
C16B C15S H15C 106.9 . . ?
C14S C15S H15C 106.9 . . ?
C16B C15S H15D 106.9 . . ?
C14S C15S H15D 106.9 . . ?
H15C C15S H15D 106.7 . . ?
C15S C16A H16A 109.5 . . ?
C15S C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C15S C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C15S C16B H16D 109.5 . . ?
C15S C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C15S C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?

_refine_diff_density_max         0.867
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.067

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
