# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_compound_3a
_database_code_depnum_ccdc_archive 'CCDC 1054314'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C9 H8 Br2 Cl4 N4 Pd), C2 H3 N'
_chemical_formula_sum            'C29 H27 Br6 Cl12 N13 Pd3'
_chemical_formula_weight         1781.70

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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   19.767(5)
_cell_length_b                   15.478(10)
_cell_length_c                   34.001(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10403(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    198(2)
_cell_measurement_reflns_used    1000
_cell_measurement_theta_min      4.166
_cell_measurement_theta_max      20.899

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6752
_exptl_absorpt_coefficient_mu    6.292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1521
_exptl_absorpt_correction_T_max  0.4215
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      198(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            177002
_diffrn_reflns_av_R_equivalents  0.1558
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         23.25
_reflns_number_total             7462
_reflns_number_gt                5210
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1999)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 2012)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0689P)²+30.9607P] 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         7462
_refine_ls_number_parameters     575
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1297
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd3 Pd 1.25048(4) 0.41171(5) -0.15851(2) 0.0242(2) Uani 1 1 d . . .
Pd1 Pd 1.17710(4) 0.17588(5) -0.00742(2) 0.0195(2) Uani 1 1 d . . .
Pd2 Pd 1.35370(4) 0.07236(5) 0.14208(2) 0.0205(2) Uani 1 1 d . . .
Br3 Br 1.25801(5) 0.06722(7) 0.09564(3) 0.0270(3) Uani 1 1 d . . .
Br1 Br 1.07656(5) 0.13092(7) -0.04573(3) 0.0291(3) Uani 1 1 d . . .
Br2 Br 1.24085(6) 0.20423(7) -0.06841(3) 0.0317(3) Uani 1 1 d . . .
Br5 Br 1.15596(6) 0.48737(7) -0.19135(3) 0.0355(3) Uani 1 1 d . . .
Br6 Br 1.32204(6) 0.41694(8) -0.21860(3) 0.0401(3) Uani 1 1 d . . .
Br4 Br 1.42790(6) -0.01034(7) 0.09692(3) 0.0325(3) Uani 1 1 d . . .
Cl10 Cl 1.07066(15) 0.3957(2) -0.02497(8) 0.0431(8) Uani 1 1 d . . .
Cl5 Cl 1.29926(16) 0.35644(16) 0.24079(8) 0.0361(7) Uani 1 1 d . . .
Cl1 Cl 1.09101(16) 0.2416(2) 0.14753(7) 0.0449(8) Uani 1 1 d . . .
Cl9 Cl 1.23129(14) 0.46296(17) 0.00486(7) 0.0306(7) Uani 1 1 d . . .
Cl11 Cl 1.43521(14) 0.35301(17) -0.03483(7) 0.0314(7) Uani 1 1 d . . .
Cl4 Cl 1.42758(15) 0.2588(2) 0.07140(9) 0.0466(8) Uani 1 1 d . . .
Cl7 Cl 1.48884(16) 0.2370(2) 0.26524(9) 0.0544(10) Uani 1 1 d . . .
Cl3 Cl 1.29202(17) 0.35577(18) 0.12005(8) 0.0461(9) Uani 1 1 d . . .
Cl2 Cl 1.03319(16) 0.0330(2) 0.12391(8) 0.0499(9) Uani 1 1 d . . .
Cl12 Cl 1.44854(15) 0.17546(18) -0.09805(9) 0.0399(8) Uani 1 1 d . . .
Cl6 Cl 1.15544(15) 0.2263(2) 0.24424(8) 0.0420(8) Uani 1 1 d . . .
Cl8 Cl 1.52716(16) 0.0158(2) 0.27322(8) 0.0503(9) Uani 1 1 d . . .
N3 N 1.2348(5) 0.2753(5) 0.0576(2) 0.026(2) Uani 1 1 d . . .
N9 N 1.2414(4) 0.4423(5) -0.0744(2) 0.022(2) Uani 1 1 d . . .
N10 N 1.1434(4) 0.3974(5) -0.0926(2) 0.021(2) Uani 1 1 d . . .
C23 C 1.3139(5) 0.4614(6) -0.0764(3) 0.023(2) Uani 1 1 d . . .
H23A H 1.3215 0.5146 -0.0919 0.027 Uiso 1 1 calc R . .
H23B H 1.3320 0.4707 -0.0495 0.027 Uiso 1 1 calc R . .
N12 N 1.3576(4) 0.2795(5) -0.1338(2) 0.025(2) Uani 1 1 d . . .
N4 N 1.3184(4) 0.2118(5) 0.0281(2) 0.023(2) Uani 1 1 d . . .
C16 C 1.4729(5) 0.1546(7) 0.2339(3) 0.031(3) Uani 1 1 d . . .
N11 N 1.3482(4) 0.3886(5) -0.0949(2) 0.024(2) Uani 1 1 d . . .
N2 N 1.0957(4) 0.0875(5) 0.0580(2) 0.023(2) Uani 1 1 d . . .
N8 N 1.4574(4) 0.0284(5) 0.2053(2) 0.026(2) Uani 1 1 d . . .
C29 C 1.3447(8) 0.6400(10) -0.1643(4) 0.075(5) Uani 1 1 d . . .
H29A H 1.3193 0.6842 -0.1788 0.112 Uiso 1 1 calc R . .
H29B H 1.3333 0.6433 -0.1363 0.112 Uiso 1 1 calc R . .
H29C H 1.3329 0.5827 -0.1745 0.112 Uiso 1 1 calc R . .
C2 C 1.0956(5) 0.1845(7) 0.1049(3) 0.027(3) Uani 1 1 d . . .
C26 C 1.4009(5) 0.2659(7) -0.1016(3) 0.027(3) Uani 1 1 d . . .
N5 N 1.3272(4) 0.2217(5) 0.1925(2) 0.023(2) Uani 1 1 d . . .
C1 C 1.1285(5) 0.1556(6) 0.0426(3) 0.021(2) Uani 1 1 d . . .
C20 C 1.2018(6) 0.4371(6) -0.0406(3) 0.023(3) Uani 1 1 d . . .
C15 C 1.4238(5) 0.0864(7) 0.1827(3) 0.026(3) Uani 1 1 d . . .
N6 N 1.2386(4) 0.1419(5) 0.1941(2) 0.025(2) Uani 1 1 d . . .
N7 N 1.4365(4) 0.1647(5) 0.1997(2) 0.025(2) Uani 1 1 d . . .
C13 C 1.1944(5) 0.0658(7) 0.1927(3) 0.028(3) Uani 1 1 d . . .
H13A H 1.2157 0.0208 0.1767 0.043 Uiso 1 1 calc R . .
H13B H 1.1508 0.0819 0.1811 0.043 Uiso 1 1 calc R . .
H13C H 1.1871 0.0440 0.2194 0.043 Uiso 1 1 calc R . .
C8 C 1.3450(6) 0.2560(7) 0.0599(3) 0.028(3) Uani 1 1 d . . .
C4 C 1.0894(6) 0.0032(7) 0.0392(3) 0.032(3) Uani 1 1 d . . .
H4A H 1.1028 0.0077 0.0116 0.048 Uiso 1 1 calc R . .
H4B H 1.0423 -0.0165 0.0409 0.048 Uiso 1 1 calc R . .
H4C H 1.1188 -0.0384 0.0526 0.048 Uiso 1 1 calc R . .
C10 C 1.3001(5) 0.1470(6) 0.1782(3) 0.022(2) Uani 1 1 d . . .
C17 C 1.4876(5) 0.0712(8) 0.2370(3) 0.030(3) Uani 1 1 d . . .
N1 N 1.1273(4) 0.2172(5) 0.0714(2) 0.022(2) Uani 1 1 d . . .
C12 C 1.2274(6) 0.2136(7) 0.2181(3) 0.025(3) Uani 1 1 d . . .
C25 C 1.3954(5) 0.3319(7) -0.0779(3) 0.022(2) Uani 1 1 d . . .
C9 C 1.3601(5) 0.1523(6) 0.0043(3) 0.028(3) Uani 1 1 d . . .
H9A H 1.3724 0.1018 0.0201 0.042 Uiso 1 1 calc R . .
H9B H 1.4013 0.1821 -0.0043 0.042 Uiso 1 1 calc R . .
H9C H 1.3344 0.1335 -0.0188 0.042 Uiso 1 1 calc R . .
C21 C 1.1404(5) 0.4107(6) -0.0520(3) 0.025(3) Uani 1 1 d . . .
C27 C 1.3436(6) 0.2171(7) -0.1651(3) 0.038(3) Uani 1 1 d . . .
H27A H 1.3143 0.2437 -0.1849 0.057 Uiso 1 1 calc R . .
H27B H 1.3209 0.1664 -0.1539 0.057 Uiso 1 1 calc R . .
H27C H 1.3862 0.1993 -0.1774 0.057 Uiso 1 1 calc R . .
C7 C 1.2933(6) 0.2950(6) 0.0784(3) 0.028(3) Uani 1 1 d . . .
C5 C 1.1650(6) 0.2952(6) 0.0669(3) 0.030(3) Uani 1 1 d . . .
H5A H 1.1629 0.3292 0.0915 0.036 Uiso 1 1 calc R . .
H5B H 1.1451 0.3304 0.0455 0.036 Uiso 1 1 calc R . .
C18 C 1.4583(7) -0.0649(7) 0.1998(3) 0.045(3) Uani 1 1 d . . .
H18A H 1.4354 -0.0929 0.2219 0.067 Uiso 1 1 calc R . .
H18B H 1.5053 -0.0850 0.1984 0.067 Uiso 1 1 calc R . .
H18C H 1.4350 -0.0796 0.1753 0.067 Uiso 1 1 calc R . .
C6 C 1.2510(5) 0.2225(6) 0.0264(3) 0.021(2) Uani 1 1 d . . .
C11 C 1.2825(6) 0.2624(7) 0.2173(3) 0.025(3) Uani 1 1 d . . .
C19 C 1.2056(5) 0.4169(6) -0.1058(3) 0.020(2) Uani 1 1 d . . .
C3 C 1.0761(5) 0.1056(7) 0.0964(3) 0.028(3) Uani 1 1 d . . .
C14 C 1.3981(6) 0.2419(7) 0.1872(3) 0.034(3) Uani 1 1 d . . .
H14A H 1.4109 0.2925 0.2034 0.041 Uiso 1 1 calc R . .
H14B H 1.4076 0.2553 0.1593 0.041 Uiso 1 1 calc R . .
C22 C 1.0885(6) 0.3590(7) -0.1149(3) 0.038(3) Uani 1 1 d . . .
H22A H 1.1013 0.3554 -0.1427 0.056 Uiso 1 1 calc R . .
H22B H 1.0479 0.3948 -0.1123 0.056 Uiso 1 1 calc R . .
H22C H 1.0792 0.3009 -0.1048 0.056 Uiso 1 1 calc R . .
C24 C 1.3243(6) 0.3537(6) -0.1290(3) 0.026(3) Uani 1 1 d . . .
C28 C 1.4141(9) 0.6542(9) -0.1693(4) 0.056(4) Uani 1 1 d . . .
N13 N 1.4703(8) 0.6633(10) -0.1739(4) 0.104(6) 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
Pd3 C24 1.986(11) . ?
Pd3 C19 2.002(9) . ?
Pd3 Br5 2.4717(16) . ?
Pd3 Br6 2.4862(14) . ?
Pd1 C1 1.980(10) . ?
Pd1 C6 1.995(10) . ?
Pd1 Br2 2.4659(14) . ?
Pd1 Br1 2.4761(14) . ?
Pd2 C15 1.968(10) . ?
Pd2 C10 1.991(10) . ?
Pd2 Br3 2.4653(14) . ?
Pd2 Br4 2.4793(15) . ?
Cl10 C21 1.673(10) . ?
Cl5 C11 1.693(11) . ?
Cl1 C2 1.701(10) . ?
Cl9 C20 1.700(10) . ?
Cl11 C25 1.695(10) . ?
Cl4 C8 1.678(11) . ?
Cl7 C16 1.693(11) . ?
Cl3 C7 1.699(11) . ?
Cl2 C3 1.691(11) . ?
Cl12 C26 1.692(11) . ?
Cl6 C12 1.689(11) . ?
Cl8 C17 1.693(11) . ?
N3 C6 1.377(12) . ?
N3 C7 1.388(13) . ?
N3 C5 1.449(13) . ?
N9 C19 1.338(12) . ?
N9 C20 1.392(12) . ?
N9 C23 1.465(12) . ?
N10 C19 1.344(12) . ?
N10 C21 1.397(12) . ?
N10 C22 1.450(12) . ?
C23 N11 1.459(12) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
N12 C24 1.333(12) . ?
N12 C26 1.406(13) . ?
N12 C27 1.464(12) . ?
N4 C6 1.343(12) . ?
N4 C8 1.384(12) . ?
N4 C9 1.479(12) . ?
C16 C17 1.327(15) . ?
C16 N7 1.375(13) . ?
N11 C24 1.364(12) . ?
N11 C25 1.404(12) . ?
N2 C1 1.344(12) . ?
N2 C3 1.389(12) . ?
N2 C4 1.459(12) . ?
N8 C15 1.356(12) . ?
N8 C17 1.398(13) . ?
N8 C18 1.456(13) . ?
C29 C28 1.40(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C2 C3 1.312(14) . ?
C2 N1 1.394(12) . ?
C26 C25 1.306(13) . ?
N5 C10 1.365(12) . ?
N5 C11 1.374(13) . ?
N5 C14 1.447(13) . ?
C1 N1 1.366(12) . ?
C20 C21 1.339(14) . ?
C15 N7 1.366(12) . ?
N6 C10 1.333(12) . ?
N6 C12 1.394(13) . ?
N6 C13 1.467(12) . ?
N7 C14 1.479(13) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C8 C7 1.344(15) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N1 C5 1.428(13) . ?
C12 C11 1.325(15) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C28 N13 1.130(18) . ?

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
C24 Pd3 C19 83.7(4) . . ?
C24 Pd3 Br5 176.4(3) . . ?
C19 Pd3 Br5 92.9(3) . . ?
C24 Pd3 Br6 90.7(3) . . ?
C19 Pd3 Br6 170.6(3) . . ?
Br5 Pd3 Br6 92.49(5) . . ?
C1 Pd1 C6 85.2(4) . . ?
C1 Pd1 Br2 177.9(3) . . ?
C6 Pd1 Br2 92.7(3) . . ?
C1 Pd1 Br1 91.0(3) . . ?
C6 Pd1 Br1 173.2(3) . . ?
Br2 Pd1 Br1 91.02(5) . . ?
C15 Pd2 C10 83.0(4) . . ?
C15 Pd2 Br3 173.3(3) . . ?
C10 Pd2 Br3 90.3(3) . . ?
C15 Pd2 Br4 94.3(3) . . ?
C10 Pd2 Br4 175.0(3) . . ?
Br3 Pd2 Br4 92.32(5) . . ?
C6 N3 C7 109.2(9) . . ?
C6 N3 C5 121.0(9) . . ?
C7 N3 C5 129.5(9) . . ?
C19 N9 C20 110.1(8) . . ?
C19 N9 C23 122.7(8) . . ?
C20 N9 C23 126.8(8) . . ?
C19 N10 C21 109.5(8) . . ?
C19 N10 C22 127.1(8) . . ?
C21 N10 C22 123.0(9) . . ?
N11 C23 N9 108.6(8) . . ?
N11 C23 H23A 110.0 . . ?
N9 C23 H23A 110.0 . . ?
N11 C23 H23B 110.0 . . ?
N9 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
C24 N12 C26 109.5(8) . . ?
C24 N12 C27 124.4(9) . . ?
C26 N12 C27 125.6(9) . . ?
C6 N4 C8 110.4(9) . . ?
C6 N4 C9 127.4(8) . . ?
C8 N4 C9 121.5(9) . . ?
C17 C16 N7 107.0(9) . . ?
C17 C16 Cl7 129.9(9) . . ?
N7 C16 Cl7 122.9(9) . . ?
C24 N11 C25 109.4(8) . . ?
C24 N11 C23 120.8(9) . . ?
C25 N11 C23 127.9(8) . . ?
C1 N2 C3 110.0(8) . . ?
C1 N2 C4 124.9(8) . . ?
C3 N2 C4 124.6(9) . . ?
C15 N8 C17 109.4(8) . . ?
C15 N8 C18 126.1(8) . . ?
C17 N8 C18 124.3(9) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C3 C2 N1 106.9(8) . . ?
C3 C2 Cl1 131.0(8) . . ?
N1 C2 Cl1 122.1(9) . . ?
C25 C26 N12 108.2(9) . . ?
C25 C26 Cl12 130.5(9) . . ?
N12 C26 Cl12 121.3(7) . . ?
C10 N5 C11 110.8(9) . . ?
C10 N5 C14 121.2(9) . . ?
C11 N5 C14 126.9(9) . . ?
N2 C1 N1 105.1(8) . . ?
N2 C1 Pd1 133.9(7) . . ?
N1 C1 Pd1 120.9(7) . . ?
C21 C20 N9 106.7(8) . . ?
C21 C20 Cl9 130.3(8) . . ?
N9 C20 Cl9 123.0(8) . . ?
N8 C15 N7 104.9(8) . . ?
N8 C15 Pd2 132.0(7) . . ?
N7 C15 Pd2 121.6(7) . . ?
C10 N6 C12 109.6(9) . . ?
C10 N6 C13 125.2(9) . . ?
C12 N6 C13 124.3(9) . . ?
C15 N7 C16 110.7(8) . . ?
C15 N7 C14 120.1(8) . . ?
C16 N7 C14 127.2(9) . . ?
N6 C13 H13A 109.5 . . ?
N6 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N6 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C8 N4 107.3(9) . . ?
C7 C8 Cl4 128.3(9) . . ?
N4 C8 Cl4 124.4(9) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N6 C10 N5 105.2(8) . . ?
N6 C10 Pd2 134.6(8) . . ?
N5 C10 Pd2 120.2(8) . . ?
C16 C17 N8 107.8(9) . . ?
C16 C17 Cl8 130.7(9) . . ?
N8 C17 Cl8 121.2(9) . . ?
C1 N1 C2 109.8(8) . . ?
C1 N1 C5 120.3(8) . . ?
C2 N1 C5 129.0(8) . . ?
C11 C12 N6 108.2(9) . . ?
C11 C12 Cl6 129.5(9) . . ?
N6 C12 Cl6 122.3(9) . . ?
C26 C25 N11 106.9(9) . . ?
C26 C25 Cl11 130.2(9) . . ?
N11 C25 Cl11 122.9(8) . . ?
N4 C9 H9A 109.5 . . ?
N4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C20 C21 N10 107.1(9) . . ?
C20 C21 Cl10 129.0(8) . . ?
N10 C21 Cl10 123.9(8) . . ?
N12 C27 H27A 109.5 . . ?
N12 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N12 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C8 C7 N3 107.2(9) . . ?
C8 C7 Cl3 130.5(9) . . ?
N3 C7 Cl3 122.2(9) . . ?
N1 C5 N3 109.9(8) . . ?
N1 C5 H5A 109.7 . . ?
N3 C5 H5A 109.7 . . ?
N1 C5 H5B 109.7 . . ?
N3 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
N8 C18 H18A 109.5 . . ?
N8 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N8 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C6 N3 105.7(8) . . ?
N4 C6 Pd1 134.9(8) . . ?
N3 C6 Pd1 119.3(7) . . ?
C12 C11 N5 106.2(9) . . ?
C12 C11 Cl5 129.9(9) . . ?
N5 C11 Cl5 123.8(9) . . ?
N9 C19 N10 106.6(8) . . ?
N9 C19 Pd3 119.5(7) . . ?
N10 C19 Pd3 134.0(7) . . ?
C2 C3 N2 108.2(9) . . ?
C2 C3 Cl2 130.1(8) . . ?
N2 C3 Cl2 121.7(9) . . ?
N5 C14 N7 106.6(8) . . ?
N5 C14 H14A 110.4 . . ?
N7 C14 H14A 110.4 . . ?
N5 C14 H14B 110.4 . . ?
N7 C14 H14B 110.4 . . ?
H14A C14 H14B 108.6 . . ?
N10 C22 H22A 109.5 . . ?
N10 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N10 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N12 C24 N11 106.0(9) . . ?
N12 C24 Pd3 133.6(7) . . ?
N11 C24 Pd3 120.4(7) . . ?
N13 C28 C29 177.8(17) . . ?

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
C19 N9 C23 N11 -51.5(12) . . . . ?
C20 N9 C23 N11 120.3(10) . . . . ?
N9 C23 N11 C24 48.1(11) . . . . ?
N9 C23 N11 C25 -114.4(10) . . . . ?
C24 N12 C26 C25 -1.6(12) . . . . ?
C27 N12 C26 C25 -173.5(9) . . . . ?
C24 N12 C26 Cl12 177.8(7) . . . . ?
C27 N12 C26 Cl12 5.9(14) . . . . ?
C3 N2 C1 N1 -1.8(11) . . . . ?
C4 N2 C1 N1 -174.3(8) . . . . ?
C3 N2 C1 Pd1 174.1(8) . . . . ?
C4 N2 C1 Pd1 1.6(15) . . . . ?
C6 Pd1 C1 N2 -130.9(10) . . . . ?
Br1 Pd1 C1 N2 54.7(9) . . . . ?
C6 Pd1 C1 N1 44.4(8) . . . . ?
Br1 Pd1 C1 N1 -129.9(7) . . . . ?
C19 N9 C20 C21 -1.9(11) . . . . ?
C23 N9 C20 C21 -174.5(9) . . . . ?
C19 N9 C20 Cl9 179.0(7) . . . . ?
C23 N9 C20 Cl9 6.4(13) . . . . ?
C17 N8 C15 N7 2.7(11) . . . . ?
C18 N8 C15 N7 178.4(10) . . . . ?
C17 N8 C15 Pd2 -163.2(8) . . . . ?
C18 N8 C15 Pd2 12.6(16) . . . . ?
C10 Pd2 C15 N8 120.6(10) . . . . ?
Br4 Pd2 C15 N8 -63.6(10) . . . . ?
C10 Pd2 C15 N7 -43.3(8) . . . . ?
Br4 Pd2 C15 N7 132.5(8) . . . . ?
N8 C15 N7 C16 -4.4(12) . . . . ?
Pd2 C15 N7 C16 163.3(7) . . . . ?
N8 C15 N7 C14 -169.1(9) . . . . ?
Pd2 C15 N7 C14 -1.3(13) . . . . ?
C17 C16 N7 C15 4.5(12) . . . . ?
Cl7 C16 N7 C15 -172.2(8) . . . . ?
C17 C16 N7 C14 167.8(10) . . . . ?
Cl7 C16 N7 C14 -8.9(15) . . . . ?
C6 N4 C8 C7 -0.1(11) . . . . ?
C9 N4 C8 C7 -171.8(8) . . . . ?
C6 N4 C8 Cl4 -179.4(7) . . . . ?
C9 N4 C8 Cl4 8.9(13) . . . . ?
C12 N6 C10 N5 0.4(10) . . . . ?
C13 N6 C10 N5 -169.3(8) . . . . ?
C12 N6 C10 Pd2 179.3(8) . . . . ?
C13 N6 C10 Pd2 9.5(15) . . . . ?
C11 N5 C10 N6 0.2(10) . . . . ?
C14 N5 C10 N6 169.1(8) . . . . ?
C11 N5 C10 Pd2 -178.9(6) . . . . ?
C14 N5 C10 Pd2 -10.0(12) . . . . ?
C15 Pd2 C10 N6 -129.4(10) . . . . ?
Br3 Pd2 C10 N6 51.4(9) . . . . ?
C15 Pd2 C10 N5 49.4(8) . . . . ?
Br3 Pd2 C10 N5 -129.9(7) . . . . ?
N7 C16 C17 N8 -2.6(12) . . . . ?
Cl7 C16 C17 N8 173.7(8) . . . . ?
N7 C16 C17 Cl8 -176.0(9) . . . . ?
Cl7 C16 C17 Cl8 0.4(18) . . . . ?
C15 N8 C17 C16 0.0(12) . . . . ?
C18 N8 C17 C16 -175.9(10) . . . . ?
C15 N8 C17 Cl8 174.1(8) . . . . ?
C18 N8 C17 Cl8 -1.8(15) . . . . ?
N2 C1 N1 C2 2.2(11) . . . . ?
Pd1 C1 N1 C2 -174.4(7) . . . . ?
N2 C1 N1 C5 172.4(8) . . . . ?
Pd1 C1 N1 C5 -4.2(12) . . . . ?
C3 C2 N1 C1 -1.7(12) . . . . ?
Cl1 C2 N1 C1 175.1(7) . . . . ?
C3 C2 N1 C5 -170.8(10) . . . . ?
Cl1 C2 N1 C5 6.0(15) . . . . ?
C10 N6 C12 C11 -0.9(11) . . . . ?
C13 N6 C12 C11 169.0(9) . . . . ?
C10 N6 C12 Cl6 -177.8(7) . . . . ?
C13 N6 C12 Cl6 -7.9(13) . . . . ?
N12 C26 C25 N11 0.0(11) . . . . ?
Cl12 C26 C25 N11 -179.4(8) . . . . ?
N12 C26 C25 Cl11 -179.2(8) . . . . ?
Cl12 C26 C25 Cl11 1.4(17) . . . . ?
C24 N11 C25 C26 1.5(11) . . . . ?
C23 N11 C25 C26 165.6(9) . . . . ?
C24 N11 C25 Cl11 -179.1(7) . . . . ?
C23 N11 C25 Cl11 -15.1(14) . . . . ?
N9 C20 C21 N10 1.7(11) . . . . ?
Cl9 C20 C21 N10 -179.3(8) . . . . ?
N9 C20 C21 Cl10 -177.8(8) . . . . ?
Cl9 C20 C21 Cl10 1.2(16) . . . . ?
C19 N10 C21 C20 -1.0(11) . . . . ?
C22 N10 C21 C20 172.7(9) . . . . ?
C19 N10 C21 Cl10 178.6(7) . . . . ?
C22 N10 C21 Cl10 -7.7(14) . . . . ?
N4 C8 C7 N3 -0.5(11) . . . . ?
Cl4 C8 C7 N3 178.7(8) . . . . ?
N4 C8 C7 Cl3 177.7(7) . . . . ?
Cl4 C8 C7 Cl3 -3.0(16) . . . . ?
C6 N3 C7 C8 1.0(11) . . . . ?
C5 N3 C7 C8 174.4(9) . . . . ?
C6 N3 C7 Cl3 -177.5(7) . . . . ?
C5 N3 C7 Cl3 -4.1(14) . . . . ?
C1 N1 C5 N3 -52.7(11) . . . . ?
C2 N1 C5 N3 115.4(11) . . . . ?
C6 N3 C5 N1 54.0(11) . . . . ?
C7 N3 C5 N1 -118.7(10) . . . . ?
C8 N4 C6 N3 0.7(10) . . . . ?
C9 N4 C6 N3 171.8(8) . . . . ?
C8 N4 C6 Pd1 -175.6(8) . . . . ?
C9 N4 C6 Pd1 -4.5(15) . . . . ?
C7 N3 C6 N4 -1.0(10) . . . . ?
C5 N3 C6 N4 -175.1(8) . . . . ?
C7 N3 C6 Pd1 176.0(6) . . . . ?
C5 N3 C6 Pd1 1.9(12) . . . . ?
C1 Pd1 C6 N4 133.4(10) . . . . ?
Br2 Pd1 C6 N4 -47.0(9) . . . . ?
C1 Pd1 C6 N3 -42.5(7) . . . . ?
Br2 Pd1 C6 N3 137.1(7) . . . . ?
N6 C12 C11 N5 0.9(11) . . . . ?
Cl6 C12 C11 N5 177.5(8) . . . . ?
N6 C12 C11 Cl5 -179.2(7) . . . . ?
Cl6 C12 C11 Cl5 -2.6(16) . . . . ?
C10 N5 C11 C12 -0.7(11) . . . . ?
C14 N5 C11 C12 -168.8(9) . . . . ?
C10 N5 C11 Cl5 179.4(7) . . . . ?
C14 N5 C11 Cl5 11.3(14) . . . . ?
C20 N9 C19 N10 1.3(11) . . . . ?
C23 N9 C19 N10 174.3(8) . . . . ?
C20 N9 C19 Pd3 -177.1(6) . . . . ?
C23 N9 C19 Pd3 -4.1(12) . . . . ?
C21 N10 C19 N9 -0.2(11) . . . . ?
C22 N10 C19 N9 -173.6(9) . . . . ?
C21 N10 C19 Pd3 177.8(8) . . . . ?
C22 N10 C19 Pd3 4.4(16) . . . . ?
C24 Pd3 C19 N9 45.7(8) . . . . ?
Br5 Pd3 C19 N9 -133.2(7) . . . . ?
C24 Pd3 C19 N10 -132.1(10) . . . . ?
Br5 Pd3 C19 N10 49.0(10) . . . . ?
N1 C2 C3 N2 0.6(12) . . . . ?
Cl1 C2 C3 N2 -175.9(8) . . . . ?
N1 C2 C3 Cl2 -178.2(8) . . . . ?
Cl1 C2 C3 Cl2 5.4(18) . . . . ?
C1 N2 C3 C2 0.8(12) . . . . ?
C4 N2 C3 C2 173.3(9) . . . . ?
C1 N2 C3 Cl2 179.6(7) . . . . ?
C4 N2 C3 Cl2 -7.9(14) . . . . ?
C10 N5 C14 N7 -49.7(11) . . . . ?
C11 N5 C14 N7 117.3(10) . . . . ?
C15 N7 C14 N5 56.4(12) . . . . ?
C16 N7 C14 N5 -105.5(11) . . . . ?
C26 N12 C24 N11 2.5(11) . . . . ?
C27 N12 C24 N11 174.6(9) . . . . ?
C26 N12 C24 Pd3 -174.1(8) . . . . ?
C27 N12 C24 Pd3 -2.1(15) . . . . ?
C25 N11 C24 N12 -2.5(11) . . . . ?
C23 N11 C24 N12 -167.9(8) . . . . ?
C25 N11 C24 Pd3 174.7(6) . . . . ?
C23 N11 C24 Pd3 9.3(12) . . . . ?
C19 Pd3 C24 N12 127.7(10) . . . . ?
Br6 Pd3 C24 N12 -59.8(10) . . . . ?
C19 Pd3 C24 N11 -48.5(8) . . . . ?
Br6 Pd3 C24 N11 123.9(8) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        23.25
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.353

####################################################################### 
# 
# 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_compound_3b
_database_code_depnum_ccdc_archive 'CCDC 1054315'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H12 Br2 Cl4 N4 Pd, 2 C3 H7 N O'
_chemical_formula_sum            'C17 H26 Br2 Cl4 N6 O2 Pd'
_chemical_formula_weight         754.46

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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0460(14)
_cell_length_b                   11.574(2)
_cell_length_c                   15.7320(13)
_cell_angle_alpha                72.144(9)
_cell_angle_beta                 89.760(14)
_cell_angle_gamma                74.103(15)
_cell_volume                     1336.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    198(2)
_cell_measurement_reflns_used    917
_cell_measurement_theta_min      4.056
_cell_measurement_theta_max      25.023

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.38
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             740
_exptl_absorpt_coefficient_mu    4.112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1525
_exptl_absorpt_correction_T_max  0.3055
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'

_exptl_special_details           
;
 The crystal was fixed on the top of a glas fiber with
 perfluorinated ether and transferred to the diffractometer.
;

_diffrn_ambient_temperature      198(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method       'phi- and omega-rotation'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13850
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         26.40
_reflns_number_total             4963
_reflns_number_gt                3821
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1999)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  
'SHELXL-97 (Sheldrick, 2008), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0249P)²+2.9314P] 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         4963
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0809
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.159
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.70087(4) -0.08190(3) 0.27281(2) 0.02293(10) Uani 1 1 d . . .
O1 O 1.0573(10) 0.2317(5) 0.1993(3) 0.125(3) Uani 1 1 d . . .
C1 C 0.7781(5) 0.0248(4) 0.3318(3) 0.0242(10) Uani 1 1 d . . .
Br1 Br 0.61020(7) -0.20058(5) 0.41674(3) 0.04010(15) Uani 1 1 d . . .
Br2 Br 0.60523(7) -0.19846(6) 0.18342(4) 0.04303(16) Uani 1 1 d . . .
O2 O 0.3132(6) 0.4919(4) 0.2162(3) 0.0700(13) Uani 1 1 d . . .
Cl4 Cl 0.72029(17) 0.30329(12) -0.05077(8) 0.0400(3) Uani 1 1 d . . .
C4 C 0.4897(6) 0.1768(5) 0.3326(4) 0.0390(13) Uani 1 1 d . . .
H4A H 0.4438 0.1149 0.3173 0.058 Uiso 1 1 calc R . .
H4B H 0.4558 0.2574 0.2836 0.058 Uiso 1 1 calc R . .
H4C H 0.4427 0.1898 0.3876 0.058 Uiso 1 1 calc R . .
Cl1 Cl 1.12658(15) 0.12777(13) 0.43273(8) 0.0387(3) Uani 1 1 d . . .
Cl2 Cl 0.70426(17) 0.31843(13) 0.40815(9) 0.0442(3) Uani 1 1 d . . .
Cl3 Cl 1.13997(15) 0.11309(13) 0.01722(8) 0.0372(3) Uani 1 1 d . . .
N1 N 0.9421(4) 0.0141(3) 0.3579(2) 0.0227(8) Uani 1 1 d . . .
C9 C 0.9553(6) 0.1006(4) 0.0670(3) 0.0251(10) Uani 1 1 d . . .
C10 C 0.7939(6) 0.1735(5) 0.0399(3) 0.0298(11) Uani 1 1 d . . .
C5 C 1.0916(6) -0.0913(5) 0.3577(3) 0.0303(11) Uani 1 1 d . . .
H5A H 1.0533 -0.1687 0.3698 0.036 Uiso 1 1 calc R . .
H5B H 1.1777 -0.1058 0.4074 0.036 Uiso 1 1 calc R . .
N5 N 0.8924(6) 0.4314(4) 0.1355(3) 0.0443(11) Uani 1 1 d . . .
C6 C 1.1807(5) -0.0722(5) 0.2704(3) 0.0301(11) Uani 1 1 d . . .
H6A H 1.1870 0.0163 0.2491 0.036 Uiso 1 1 calc R . .
H6B H 1.3012 -0.1283 0.2840 0.036 Uiso 1 1 calc R . .
N6 N 0.2289(8) 0.5289(5) 0.3461(3) 0.0623(15) Uani 1 1 d . . .
C3 C 0.7829(6) 0.1835(4) 0.3825(3) 0.0257(10) Uani 1 1 d . . .
C2 C 0.9448(6) 0.1114(5) 0.3892(3) 0.0264(10) Uani 1 1 d . . .
C16 C 0.0910(13) 0.4753(9) 0.3522(6) 0.104(3) Uani 1 1 d . . .
H16A H 0.0558 0.4751 0.2927 0.156 Uiso 1 1 calc R . .
H16B H -0.0072 0.5253 0.3749 0.156 Uiso 1 1 calc R . .
H16C H 0.1280 0.3882 0.3932 0.156 Uiso 1 1 calc R . .
C15 C 0.3310(10) 0.5333(6) 0.2774(5) 0.070(2) Uani 1 1 d . . .
H15 H 0.4223 0.5709 0.2765 0.084 Uiso 1 1 calc R . .
C14 C 0.8998(11) 0.5572(7) 0.0892(6) 0.099(3) Uani 1 1 d . . .
H14A H 1.0210 0.5568 0.0824 0.149 Uiso 1 1 calc R . .
H14B H 0.8472 0.6135 0.1237 0.149 Uiso 1 1 calc R . .
H14C H 0.8361 0.5875 0.0299 0.149 Uiso 1 1 calc R . .
C13 C 0.7279(11) 0.4133(9) 0.1538(5) 0.095(3) Uani 1 1 d . . .
H13A H 0.7374 0.3227 0.1710 0.142 Uiso 1 1 calc R . .
H13B H 0.6468 0.4590 0.1001 0.142 Uiso 1 1 calc R . .
H13C H 0.6853 0.4455 0.2030 0.142 Uiso 1 1 calc R . .
C12 C 1.0361(11) 0.3356(7) 0.1628(5) 0.075(2) Uani 1 1 d . . .
H12 H 1.1400 0.3588 0.1490 0.090 Uiso 1 1 calc R . .
N4 N 0.6872(4) 0.1226(4) 0.1003(2) 0.0276(9) Uani 1 1 d . . .
N3 N 0.9484(4) 0.0056(3) 0.1441(2) 0.0242(8) Uani 1 1 d . . .
N2 N 0.6793(4) 0.1295(4) 0.3466(2) 0.0258(9) Uani 1 1 d . . .
C8 C 0.7827(5) 0.0196(4) 0.1643(3) 0.0252(10) Uani 1 1 d . . .
C17 C 0.2754(13) 0.5663(7) 0.4192(6) 0.110(3) Uani 1 1 d . . .
H17A H 0.3629 0.6118 0.4019 0.165 Uiso 1 1 calc R . .
H17B H 0.3229 0.4908 0.4713 0.165 Uiso 1 1 calc R . .
H17C H 0.1723 0.6218 0.4345 0.165 Uiso 1 1 calc R . .
C7 C 1.0964(6) -0.0970(4) 0.1946(3) 0.0301(11) Uani 1 1 d . . .
H7A H 1.1848 -0.1147 0.1528 0.036 Uiso 1 1 calc R . .
H7B H 1.0583 -0.1742 0.2198 0.036 Uiso 1 1 calc R . .
C11 C 0.4990(6) 0.1718(5) 0.0933(4) 0.0426(14) Uani 1 1 d . . .
H11A H 0.4511 0.1099 0.1356 0.064 Uiso 1 1 calc R . .
H11B H 0.4523 0.1871 0.0322 0.064 Uiso 1 1 calc R . .
H11C H 0.4669 0.2514 0.1075 0.064 Uiso 1 1 calc R . .


_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 C1 1.974(4) . ?
Pd1 C8 1.978(4) . ?
Pd1 Br2 2.4761(7) . ?
Pd1 Br1 2.4846(7) . ?
O1 C12 1.127(8) . ?
C1 N2 1.342(6) . ?
C1 N1 1.345(5) . ?
O2 C15 1.224(8) . ?
Cl4 C10 1.688(5) . ?
C4 N2 1.465(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
Cl1 C2 1.698(4) . ?
Cl2 C3 1.687(5) . ?
Cl3 C9 1.697(4) . ?
N1 C2 1.366(6) . ?
N1 C5 1.461(6) . ?
C9 C10 1.328(6) . ?
C9 N3 1.377(6) . ?
C10 N4 1.383(5) . ?
C5 C6 1.530(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N5 C12 1.327(9) . ?
N5 C13 1.411(8) . ?
N5 C14 1.432(8) . ?
C6 C7 1.513(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
N6 C15 1.352(9) . ?
N6 C16 1.401(9) . ?
N6 C17 1.431(9) . ?
C3 C2 1.325(6) . ?
C3 N2 1.382(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C15 H15 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C12 H12 0.9500 . ?
N4 C8 1.339(6) . ?
N4 C11 1.456(6) . ?
N3 C8 1.347(5) . ?
N3 C7 1.455(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

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
C1 Pd1 C8 84.36(17) . . ?
C1 Pd1 Br2 173.87(12) . . ?
C8 Pd1 Br2 89.76(13) . . ?
C1 Pd1 Br1 90.69(12) . . ?
C8 Pd1 Br1 174.99(13) . . ?
Br2 Pd1 Br1 95.20(2) . . ?
N2 C1 N1 105.9(4) . . ?
N2 C1 Pd1 126.8(3) . . ?
N1 C1 Pd1 127.1(3) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 N1 C2 109.9(4) . . ?
C1 N1 C5 124.1(4) . . ?
C2 N1 C5 125.9(4) . . ?
C10 C9 N3 107.3(4) . . ?
C10 C9 Cl3 128.5(4) . . ?
N3 C9 Cl3 124.2(3) . . ?
C9 C10 N4 107.2(4) . . ?
C9 C10 Cl4 129.2(4) . . ?
N4 C10 Cl4 123.6(4) . . ?
N1 C5 C6 114.8(4) . . ?
N1 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
N1 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.5 . . ?
C12 N5 C13 121.0(7) . . ?
C12 N5 C14 121.0(6) . . ?
C13 N5 C14 117.9(6) . . ?
C7 C6 C5 116.4(4) . . ?
C7 C6 H6A 108.2 . . ?
C5 C6 H6A 108.2 . . ?
C7 C6 H6B 108.2 . . ?
C5 C6 H6B 108.2 . . ?
H6A C6 H6B 107.3 . . ?
C15 N6 C16 121.5(6) . . ?
C15 N6 C17 118.9(7) . . ?
C16 N6 C17 119.2(7) . . ?
C2 C3 N2 107.0(4) . . ?
C2 C3 Cl2 129.9(4) . . ?
N2 C3 Cl2 123.1(3) . . ?
C3 C2 N1 107.7(4) . . ?
C3 C2 Cl1 128.1(4) . . ?
N1 C2 Cl1 124.2(3) . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O2 C15 N6 124.2(7) . . ?
O2 C15 H15 117.9 . . ?
N6 C15 H15 117.9 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C12 N5 131.6(9) . . ?
O1 C12 H12 114.2 . . ?
N5 C12 H12 114.2 . . ?
C8 N4 C10 109.8(4) . . ?
C8 N4 C11 125.4(4) . . ?
C10 N4 C11 124.8(4) . . ?
C8 N3 C9 109.8(4) . . ?
C8 N3 C7 124.8(4) . . ?
C9 N3 C7 125.4(4) . . ?
C1 N2 C3 109.6(4) . . ?
C1 N2 C4 126.0(4) . . ?
C3 N2 C4 124.3(4) . . ?
N4 C8 N3 106.0(4) . . ?
N4 C8 Pd1 127.1(3) . . ?
N3 C8 Pd1 126.7(3) . . ?
N6 C17 H17A 109.5 . . ?
N6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C7 C6 115.0(4) . . ?
N3 C7 H7A 108.5 . . ?
C6 C7 H7A 108.5 . . ?
N3 C7 H7B 108.5 . . ?
C6 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

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
C8 Pd1 C1 N2 96.4(4) . . . . ?
Br1 Pd1 C1 N2 -84.4(4) . . . . ?
C8 Pd1 C1 N1 -77.1(4) . . . . ?
Br1 Pd1 C1 N1 102.1(4) . . . . ?
N2 C1 N1 C2 0.3(5) . . . . ?
Pd1 C1 N1 C2 174.9(3) . . . . ?
N2 C1 N1 C5 176.6(4) . . . . ?
Pd1 C1 N1 C5 -8.7(6) . . . . ?
N3 C9 C10 N4 -0.4(5) . . . . ?
Cl3 C9 C10 N4 177.4(3) . . . . ?
N3 C9 C10 Cl4 -179.3(4) . . . . ?
Cl3 C9 C10 Cl4 -1.5(7) . . . . ?
C1 N1 C5 C6 90.0(5) . . . . ?
C2 N1 C5 C6 -94.3(5) . . . . ?
N1 C5 C6 C7 -80.4(5) . . . . ?
N2 C3 C2 N1 0.1(5) . . . . ?
Cl2 C3 C2 N1 -178.6(3) . . . . ?
N2 C3 C2 Cl1 -177.2(3) . . . . ?
Cl2 C3 C2 Cl1 4.2(7) . . . . ?
C1 N1 C2 C3 -0.2(5) . . . . ?
C5 N1 C2 C3 -176.5(4) . . . . ?
C1 N1 C2 Cl1 177.2(3) . . . . ?
C5 N1 C2 Cl1 0.9(6) . . . . ?
C16 N6 C15 O2 -0.2(10) . . . . ?
C17 N6 C15 O2 172.4(6) . . . . ?
C13 N5 C12 O1 2.4(11) . . . . ?
C14 N5 C12 O1 -179.7(8) . . . . ?
C9 C10 N4 C8 0.4(5) . . . . ?
Cl4 C10 N4 C8 179.3(3) . . . . ?
C9 C10 N4 C11 -177.8(4) . . . . ?
Cl4 C10 N4 C11 1.1(7) . . . . ?
C10 C9 N3 C8 0.3(5) . . . . ?
Cl3 C9 N3 C8 -177.6(3) . . . . ?
C10 C9 N3 C7 178.4(4) . . . . ?
Cl3 C9 N3 C7 0.5(6) . . . . ?
N1 C1 N2 C3 -0.2(5) . . . . ?
Pd1 C1 N2 C3 -174.9(3) . . . . ?
N1 C1 N2 C4 -176.8(4) . . . . ?
Pd1 C1 N2 C4 8.6(6) . . . . ?
C2 C3 N2 C1 0.1(5) . . . . ?
Cl2 C3 N2 C1 178.9(3) . . . . ?
C2 C3 N2 C4 176.7(4) . . . . ?
Cl2 C3 N2 C4 -4.5(6) . . . . ?
C10 N4 C8 N3 -0.2(5) . . . . ?
C11 N4 C8 N3 178.0(4) . . . . ?
C10 N4 C8 Pd1 174.4(3) . . . . ?
C11 N4 C8 Pd1 -7.4(7) . . . . ?
C9 N3 C8 N4 -0.1(5) . . . . ?
C7 N3 C8 N4 -178.1(4) . . . . ?
C9 N3 C8 Pd1 -174.7(3) . . . . ?
C7 N3 C8 Pd1 7.2(6) . . . . ?
C1 Pd1 C8 N4 -95.5(4) . . . . ?
Br2 Pd1 C8 N4 82.8(4) . . . . ?
C1 Pd1 C8 N3 78.1(4) . . . . ?
Br2 Pd1 C8 N3 -103.7(4) . . . . ?
C8 N3 C7 C6 -89.2(5) . . . . ?
C9 N3 C7 C6 93.0(5) . . . . ?
C5 C6 C7 N3 80.2(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.907
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.106

####################################################################### 
# 
# 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_compound_3c
_database_code_depnum_ccdc_archive 'CCDC 1054316'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H14 Br2 Cl4 N4 Pd'
_chemical_formula_sum            'C16 H14 Br2 Cl4 N4 Pd'
_chemical_formula_weight         670.33

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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   13.430(3)
_cell_length_b                   18.758(2)
_cell_length_c                   8.310(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2093.5(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    198(2)
_cell_measurement_reflns_used    867
_cell_measurement_theta_min      4.081
_cell_measurement_theta_max      23.854

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_absorpt_coefficient_mu    5.225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1672
_exptl_absorpt_correction_T_max  0.3621
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      198(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43521
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         26.37
_reflns_number_total             2215
_reflns_number_gt                1773
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1999)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 2012)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0281P)²+3.7009P] 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         2215
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0659
_refine_ls_wR_factor_gt          0.0608
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.36706(3) 0.2500 0.42741(4) 0.01837(11) Uani 1 2 d S . .
Br1 Br 0.31326(3) 0.15435(2) 0.24190(5) 0.03547(13) Uani 1 1 d . . .
Cl1 Cl 0.37869(10) 0.03012(7) 0.90249(14) 0.0580(4) Uani 1 1 d . . .
Cl2 Cl 0.58733(8) 0.01301(5) 0.66317(13) 0.0374(2) Uani 1 1 d . . .
N1 N 0.3665(2) 0.14305(17) 0.6980(4) 0.0283(7) Uani 1 1 d . . .
N2 N 0.4961(2) 0.13270(15) 0.5474(3) 0.0237(7) Uani 1 1 d . . .
C1 C 0.4141(3) 0.17300(19) 0.5723(4) 0.0229(7) Uani 1 1 d . . .
C2 C 0.4181(3) 0.0834(2) 0.7506(4) 0.0295(9) Uani 1 1 d . . .
C3 C 0.4987(3) 0.07702(19) 0.6570(4) 0.0261(8) Uani 1 1 d . . .
C4 C 0.5679(3) 0.1438(2) 0.4196(5) 0.0374(10) Uani 1 1 d . . .
H4A H 0.5341 0.1636 0.3252 0.056 Uiso 1 1 calc R . .
H4B H 0.5988 0.0982 0.3912 0.056 Uiso 1 1 calc R . .
H4C H 0.6193 0.1771 0.4562 0.056 Uiso 1 1 calc R . .
C5 C 0.2772(4) 0.1700(3) 0.7821(6) 0.0679(18) Uani 1 1 d . . .
H5A H 0.2991 0.1997 0.8739 0.081 Uiso 1 1 calc R . .
H5B H 0.2404 0.1287 0.8268 0.081 Uiso 1 1 calc R . .
C6 C 0.2071(3) 0.2128(2) 0.6817(4) 0.0295(9) Uani 1 1 d . . .
C7 C 0.1347(4) 0.1778(3) 0.5938(5) 0.0534(14) Uani 1 1 d . . .
H7 H 0.1345 0.1272 0.5910 0.064 Uiso 1 1 calc R . .
C8 C 0.0634(3) 0.2145(3) 0.5106(6) 0.079(2) Uani 1 1 d . . .
H8 H 0.0136 0.1892 0.4526 0.094 Uiso 1 1 calc R . .


_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 C1 1.984(4) 8_565 ?
Pd1 C1 1.984(4) . ?
Pd1 Br1 2.4734(8) . ?
Pd1 Br1 2.4734(8) 8_565 ?
Cl1 C2 1.694(4) . ?
Cl2 C3 1.692(4) . ?
N1 C1 1.347(5) . ?
N1 C2 1.387(5) . ?
N1 C5 1.477(6) . ?
N2 C1 1.353(4) . ?
N2 C3 1.386(5) . ?
N2 C4 1.449(5) . ?
C2 C3 1.338(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.492(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.382(6) . ?
C6 C6 1.397(8) 8_565 ?
C7 C8 1.367(7) . ?
C7 H7 0.9500 . ?
C8 C8 1.333(13) 8_565 ?
C8 H8 0.9500 . ?

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
C1 Pd1 C1 93.4(2) 8_565 . ?
C1 Pd1 Br1 178.24(11) 8_565 . ?
C1 Pd1 Br1 86.75(10) . . ?
C1 Pd1 Br1 86.75(10) 8_565 8_565 ?
C1 Pd1 Br1 178.23(11) . 8_565 ?
Br1 Pd1 Br1 93.00(4) . 8_565 ?
C1 N1 C2 110.1(3) . . ?
C1 N1 C5 127.6(3) . . ?
C2 N1 C5 122.2(3) . . ?
C1 N2 C3 109.9(3) . . ?
C1 N2 C4 125.0(3) . . ?
C3 N2 C4 125.0(3) . . ?
N1 C1 N2 105.8(3) . . ?
N1 C1 Pd1 128.6(3) . . ?
N2 C1 Pd1 125.0(3) . . ?
C3 C2 N1 107.0(3) . . ?
C3 C2 Cl1 129.3(3) . . ?
N1 C2 Cl1 123.7(3) . . ?
C2 C3 N2 107.2(3) . . ?
C2 C3 Cl2 127.9(3) . . ?
N2 C3 Cl2 124.9(3) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 115.6(3) . . ?
N1 C5 H5A 108.4 . . ?
C6 C5 H5A 108.4 . . ?
N1 C5 H5B 108.4 . . ?
C6 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
C7 C6 C6 118.3(3) . 8_565 ?
C7 C6 C5 119.0(5) . . ?
C6 C6 C5 122.6(3) 8_565 . ?
C8 C7 C6 121.5(5) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C8 C8 C7 120.2(3) 8_565 . ?
C8 C8 H8 119.9 8_565 . ?
C7 C8 H8 119.9 . . ?

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
C2 N1 C1 N2 -0.8(4) . . . . ?
C5 N1 C1 N2 174.4(4) . . . . ?
C2 N1 C1 Pd1 170.2(3) . . . . ?
C5 N1 C1 Pd1 -14.6(6) . . . . ?
C3 N2 C1 N1 0.8(4) . . . . ?
C4 N2 C1 N1 177.6(3) . . . . ?
C3 N2 C1 Pd1 -170.6(2) . . . . ?
C4 N2 C1 Pd1 6.3(5) . . . . ?
C1 Pd1 C1 N1 86.1(3) 8_565 . . . ?
Br1 Pd1 C1 N1 -95.7(3) . . . . ?
C1 Pd1 C1 N2 -104.6(3) 8_565 . . . ?
Br1 Pd1 C1 N2 73.7(3) . . . . ?
C1 N1 C2 C3 0.5(4) . . . . ?
C5 N1 C2 C3 -175.0(4) . . . . ?
C1 N1 C2 Cl1 -177.8(3) . . . . ?
C5 N1 C2 Cl1 6.7(6) . . . . ?
N1 C2 C3 N2 -0.1(4) . . . . ?
Cl1 C2 C3 N2 178.1(3) . . . . ?
N1 C2 C3 Cl2 -178.6(3) . . . . ?
Cl1 C2 C3 Cl2 -0.4(6) . . . . ?
C1 N2 C3 C2 -0.4(4) . . . . ?
C4 N2 C3 C2 -177.3(3) . . . . ?
C1 N2 C3 Cl2 178.2(3) . . . . ?
C4 N2 C3 Cl2 1.3(5) . . . . ?
C1 N1 C5 C6 29.6(8) . . . . ?
C2 N1 C5 C6 -155.6(4) . . . . ?
N1 C5 C6 C7 86.4(6) . . . . ?
N1 C5 C6 C6 -98.3(5) . . . 8_565 ?
C6 C6 C7 C8 -1.1(5) 8_565 . . . ?
C5 C6 C7 C8 174.4(4) . . . . ?
C6 C7 C8 C8 1.2(5) . . . 8_565 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.109

####################################################################### 
# 
# 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_compound_3e
_database_code_depnum_ccdc_archive 'CCDC 1054317'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 Br2 N8 Pd'
_chemical_formula_sum            'C15 H12 Br2 N8 Pd'
_chemical_formula_weight         570.55

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'
Br Br -0.2901 2.4595 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41cd
_symmetry_space_group_name_Hall  'I 4bw -2c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'-x, y, z+1/2'
'x, -y, z+1/2'
'y+1/2, x, z+1/4'
'-y+1/2, -x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'y+1, x+1/2, z+3/4'
'-y+1, -x+1/2, z+3/4'

_cell_length_a                   23.9130(3)
_cell_length_b                   23.9130(3)
_cell_length_c                   13.699(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7833.5(16)
_cell_formula_units_Z            16
_cell_measurement_temperature    198(2)
_cell_measurement_reflns_used    1000
_cell_measurement_theta_min      4.088
_cell_measurement_theta_max      21.166

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4384
_exptl_absorpt_coefficient_mu    5.044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3653
_exptl_absorpt_correction_T_max  0.4019
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'

_exptl_special_details           
; 
  The crystal was fixed on the top of a glas fiber with
 perfluorinated ether and transferred to the diffractometer.
;

_diffrn_ambient_temperature      198(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method       'phi- and omega-rotation'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            72663
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         25.20
_reflns_number_total             3514
_reflns_number_gt                3204
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1999)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  
'SHELXLE-97 (Sheldrick, 2008), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0365P)²+26.3781P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.128(10)
_refine_ls_number_reflns         3514
_refine_ls_number_parameters     237
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.201574(17) 0.489631(15) 0.91218(3) 0.03159(12) Uani 1 1 d . . .
Br1 Br 0.24722(3) 0.55918(3) 0.80752(5) 0.05181(19) Uani 1 1 d . . .
N1 N 0.2365(2) 0.5641(2) 1.0732(4) 0.0343(11) Uani 1 1 d . . .
C1 C 0.2462(2) 0.5184(2) 1.0215(4) 0.0326(13) Uani 1 1 d . . .
Br2 Br 0.14047(3) 0.45238(3) 0.78361(5) 0.05031(19) Uani 1 1 d . . .
N2 N 0.29073(19) 0.4933(2) 1.0631(4) 0.0375(12) Uani 1 1 d . . .
C2 C 0.2741(3) 0.5685(3) 1.1465(4) 0.0400(14) Uani 1 1 d . . .
N3 N 0.1209(2) 0.4517(2) 1.0618(4) 0.0397(12) Uani 1 1 d . . .
C3 C 0.3083(2) 0.5251(3) 1.1411(5) 0.0448(16) Uani 1 1 d . . .
N4 N 0.1900(2) 0.3950(2) 1.0521(4) 0.0395(11) Uani 1 1 d . . .
C4 C 0.1934(3) 0.6056(3) 1.0508(5) 0.0458(15) Uani 1 1 d . . .
H4A H 0.1634 0.6033 1.0995 0.069 Uiso 1 1 calc R . .
H4B H 0.1779 0.5982 0.9858 0.069 Uiso 1 1 calc R . .
H4C H 0.2098 0.6432 1.0522 0.069 Uiso 1 1 calc R . .
N5 N 0.2723(3) 0.6459(3) 1.2738(6) 0.085(2) Uani 1 1 d . . .
C5 C 0.3188(3) 0.4422(3) 1.0274(5) 0.0457(16) Uani 1 1 d . . .
H5A H 0.3587 0.4440 1.0466 0.055 Uiso 1 1 calc R . .
H5B H 0.3174 0.4423 0.9551 0.055 Uiso 1 1 calc R . .
N6 N 0.3907(3) 0.5032(4) 1.2521(6) 0.087(2) Uani 1 1 d . . .
C6 C 0.2945(3) 0.3869(3) 1.0639(5) 0.0427(15) Uani 1 1 d . . .
H6A H 0.3233 0.3576 1.0549 0.051 Uiso 1 1 calc R . .
H6B H 0.2879 0.3905 1.1349 0.051 Uiso 1 1 calc R . .
N7 N 0.0353(3) 0.4153(3) 1.2592(6) 0.092(3) Uani 1 1 d . . .
C7 C 0.2409(3) 0.3663(3) 1.0174(5) 0.0470(16) Uani 1 1 d . . .
H7A H 0.2437 0.3712 0.9458 0.056 Uiso 1 1 calc R . .
H7B H 0.2370 0.3258 1.0305 0.056 Uiso 1 1 calc R . .
N8 N 0.1839(4) 0.2967(3) 1.2405(6) 0.096(3) Uani 1 1 d . . .
C8 C 0.1674(2) 0.4396(3) 1.0097(4) 0.0358(14) Uani 1 1 d . . .
C9 C 0.1147(3) 0.4135(3) 1.1347(5) 0.0465(16) Uani 1 1 d . . .
C10 C 0.1578(3) 0.3782(3) 1.1294(4) 0.0464(17) Uani 1 1 d . . .
C11 C 0.0821(2) 0.4970(3) 1.0400(5) 0.0507(16) Uani 1 1 d . . .
H11A H 0.0853 0.5261 1.0901 0.076 Uiso 1 1 calc R . .
H11B H 0.0438 0.4824 1.0392 0.076 Uiso 1 1 calc R . .
H11C H 0.0911 0.5130 0.9760 0.076 Uiso 1 1 calc R . .
C12 C 0.2740(3) 0.6124(3) 1.2162(5) 0.0542(18) Uani 1 1 d . . .
C13 C 0.3546(3) 0.5109(3) 1.2026(5) 0.0561(19) Uani 1 1 d . . .
C14 C 0.0695(3) 0.4139(3) 1.2027(6) 0.061(2) Uani 1 1 d . . .
C15 C 0.1727(3) 0.3320(3) 1.1910(6) 0.062(2) 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 C1 1.964(6) . ?
Pd1 C8 1.971(6) . ?
Pd1 Br1 2.4521(8) . ?
Pd1 Br2 2.4557(8) . ?
N1 C1 1.323(8) . ?
N1 C2 1.351(8) . ?
N1 C4 1.465(8) . ?
C1 N2 1.349(7) . ?
N2 C3 1.377(9) . ?
N2 C5 1.477(8) . ?
C2 C3 1.323(9) . ?
C2 C12 1.419(10) . ?
N3 C8 1.351(8) . ?
N3 C9 1.361(8) . ?
N3 C11 1.458(8) . ?
C3 C13 1.433(9) . ?
N4 C8 1.330(8) . ?
N4 C10 1.369(8) . ?
N4 C7 1.476(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N5 C12 1.126(9) . ?
C5 C6 1.531(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N6 C13 1.112(9) . ?
C6 C7 1.513(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
N7 C14 1.126(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N8 C15 1.116(10) . ?
C9 C10 1.335(9) . ?
C9 C14 1.428(10) . ?
C10 C15 1.434(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

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
C1 Pd1 C8 85.5(2) . . ?
C1 Pd1 Br1 88.08(15) . . ?
C8 Pd1 Br1 173.03(17) . . ?
C1 Pd1 Br2 175.99(15) . . ?
C8 Pd1 Br2 91.11(17) . . ?
Br1 Pd1 Br2 95.25(3) . . ?
C1 N1 C2 110.2(5) . . ?
C1 N1 C4 124.8(5) . . ?
C2 N1 C4 124.9(5) . . ?
N1 C1 N2 106.3(5) . . ?
N1 C1 Pd1 127.1(4) . . ?
N2 C1 Pd1 126.5(5) . . ?
C1 N2 C3 108.7(5) . . ?
C1 N2 C5 126.0(6) . . ?
C3 N2 C5 125.2(5) . . ?
C3 C2 N1 107.9(6) . . ?
C3 C2 C12 128.3(7) . . ?
N1 C2 C12 123.8(6) . . ?
C8 N3 C9 109.5(5) . . ?
C8 N3 C11 125.0(5) . . ?
C9 N3 C11 125.4(5) . . ?
C2 C3 N2 106.8(5) . . ?
C2 C3 C13 129.1(7) . . ?
N2 C3 C13 124.1(7) . . ?
C8 N4 C10 110.2(5) . . ?
C8 N4 C7 124.6(5) . . ?
C10 N4 C7 125.2(5) . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 115.7(5) . . ?
N2 C5 H5A 108.4 . . ?
C6 C5 H5A 108.4 . . ?
N2 C5 H5B 108.4 . . ?
C6 C5 H5B 108.4 . . ?
H5A C5 H5B 107.4 . . ?
C7 C6 C5 117.8(5) . . ?
C7 C6 H6A 107.9 . . ?
C5 C6 H6A 107.9 . . ?
C7 C6 H6B 107.9 . . ?
C5 C6 H6B 107.9 . . ?
H6A C6 H6B 107.2 . . ?
N4 C7 C6 114.3(5) . . ?
N4 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N4 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N4 C8 N3 106.0(5) . . ?
N4 C8 Pd1 127.9(4) . . ?
N3 C8 Pd1 124.7(5) . . ?
C10 C9 N3 107.5(5) . . ?
C10 C9 C14 128.6(7) . . ?
N3 C9 C14 123.9(7) . . ?
C9 C10 N4 106.9(6) . . ?
C9 C10 C15 130.3(6) . . ?
N4 C10 C15 122.8(7) . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 C2 177.0(8) . . ?
N6 C13 C3 175.6(10) . . ?
N7 C14 C9 177.0(9) . . ?
N8 C15 C10 178.6(10) . . ?

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
C2 N1 C1 N2 0.2(6) . . . . ?
C4 N1 C1 N2 176.9(5) . . . . ?
C2 N1 C1 Pd1 176.1(4) . . . . ?
C4 N1 C1 Pd1 -7.2(8) . . . . ?
C8 Pd1 C1 N1 -98.2(5) . . . . ?
Br1 Pd1 C1 N1 79.2(5) . . . . ?
C8 Pd1 C1 N2 76.8(5) . . . . ?
Br1 Pd1 C1 N2 -105.7(5) . . . . ?
N1 C1 N2 C3 -0.5(6) . . . . ?
Pd1 C1 N2 C3 -176.4(4) . . . . ?
N1 C1 N2 C5 -176.4(5) . . . . ?
Pd1 C1 N2 C5 7.6(8) . . . . ?
C1 N1 C2 C3 0.2(7) . . . . ?
C4 N1 C2 C3 -176.6(5) . . . . ?
C1 N1 C2 C12 -178.5(6) . . . . ?
C4 N1 C2 C12 4.8(9) . . . . ?
N1 C2 C3 N2 -0.5(7) . . . . ?
C12 C2 C3 N2 178.1(6) . . . . ?
N1 C2 C3 C13 -179.6(6) . . . . ?
C12 C2 C3 C13 -1.0(12) . . . . ?
C1 N2 C3 C2 0.6(7) . . . . ?
C5 N2 C3 C2 176.6(5) . . . . ?
C1 N2 C3 C13 179.7(6) . . . . ?
C5 N2 C3 C13 -4.2(10) . . . . ?
C1 N2 C5 C6 -87.6(7) . . . . ?
C3 N2 C5 C6 97.1(7) . . . . ?
N2 C5 C6 C7 77.0(8) . . . . ?
C8 N4 C7 C6 92.5(7) . . . . ?
C10 N4 C7 C6 -90.7(7) . . . . ?
C5 C6 C7 N4 -77.5(7) . . . . ?
C10 N4 C8 N3 1.0(7) . . . . ?
C7 N4 C8 N3 178.2(5) . . . . ?
C10 N4 C8 Pd1 167.8(4) . . . . ?
C7 N4 C8 Pd1 -15.0(9) . . . . ?
C9 N3 C8 N4 -1.4(7) . . . . ?
C11 N3 C8 N4 -178.5(6) . . . . ?
C9 N3 C8 Pd1 -168.6(4) . . . . ?
C11 N3 C8 Pd1 14.2(9) . . . . ?
C1 Pd1 C8 N4 -73.4(6) . . . . ?
Br2 Pd1 C8 N4 108.6(5) . . . . ?
C1 Pd1 C8 N3 91.0(5) . . . . ?
Br2 Pd1 C8 N3 -86.9(5) . . . . ?
C8 N3 C9 C10 1.2(7) . . . . ?
C11 N3 C9 C10 178.3(6) . . . . ?
C8 N3 C9 C14 -179.4(6) . . . . ?
C11 N3 C9 C14 -2.3(10) . . . . ?
N3 C9 C10 N4 -0.5(7) . . . . ?
C14 C9 C10 N4 -179.9(7) . . . . ?
N3 C9 C10 C15 176.9(7) . . . . ?
C14 C9 C10 C15 -2.5(13) . . . . ?
C8 N4 C10 C9 -0.4(7) . . . . ?
C7 N4 C10 C9 -177.5(6) . . . . ?
C8 N4 C10 C15 -178.0(6) . . . . ?
C7 N4 C10 C15 4.9(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.092







