# 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_12103
_database_code_depnum_ccdc_archive 'CCDC 1043191'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H25 N3 O2 Pd, C H Cl3, H2 O'
_chemical_formula_sum            'C25 H28 Cl3 N3 O3 Pd'
_chemical_formula_weight         631.25

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.9770(16)
_cell_length_b                   12.184(3)
_cell_length_c                   15.543(4)
_cell_angle_alpha                87.923(4)
_cell_angle_beta                 84.029(5)
_cell_angle_gamma                84.203(5)
_cell_volume                     1307.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    622
_cell_measurement_theta_min      2.950
_cell_measurement_theta_max      23.135

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   
;
absorption correction based on 2095 reflections(SADABS);Rint 0.0918 before
correction and 0.0420 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10332
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_sigmaI/netI    0.2111
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5074
_reflns_number_gt                2886
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0174P)²+0.0000P] 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         5074
_refine_ls_number_parameters     319
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0683
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1067
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_restrained_S_all      0.877
_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
Pd1 Pd 0.67621(9) 0.59296(5) 0.64335(4) 0.02034(17) Uani 1 1 d . . .
O1 O 0.6364(7) 0.6419(4) 0.7683(3) 0.0236(13) Uani 1 1 d . . .
O2 O 0.9340(8) 0.6986(4) 0.7555(3) 0.0336(14) Uani 1 1 d . . .
N1 N 0.5725(9) 0.7405(5) 0.5957(4) 0.0220(15) Uani 1 1 d . . .
N2 N 0.7085(8) 0.5563(5) 0.5204(4) 0.0187(15) Uani 1 1 d . . .
N3 N 0.7628(9) 0.4451(5) 0.6812(4) 0.0267(16) Uani 1 1 d . . .
H3A H 0.7577 0.4327 0.7375 0.032 Uiso 1 1 calc R . .
C1 C 0.5036(12) 0.8301(6) 0.6507(5) 0.027(2) Uani 1 1 d . . .
C2 C 0.3153(12) 0.8358(6) 0.6891(5) 0.034(2) Uani 1 1 d . . .
H2 H 0.2296 0.7854 0.6741 0.040 Uiso 1 1 calc R . .
C3 C 0.2525(13) 0.9154(7) 0.7496(5) 0.041(2) Uani 1 1 d . . .
H3 H 0.1229 0.9189 0.7760 0.049 Uiso 1 1 calc R . .
C4 C 0.3749(17) 0.9906(7) 0.7730(6) 0.055(3) Uani 1 1 d U . .
C5 C 0.5587(15) 0.9833(7) 0.7340(5) 0.050(3) Uani 1 1 d . . .
H5 H 0.6447 1.0336 0.7490 0.060 Uiso 1 1 calc R . .
C6 C 0.6238(13) 0.9052(6) 0.6734(5) 0.038(2) Uani 1 1 d . . .
H6 H 0.7530 0.9028 0.6469 0.046 Uiso 1 1 calc R . .
C7 C 0.5702(11) 0.7446(6) 0.5130(5) 0.0260(19) Uani 1 1 d . . .
C8 C 0.4978(10) 0.8447(6) 0.4624(5) 0.0249(19) Uani 1 1 d . . .
H8A H 0.4437 0.9029 0.5023 0.037 Uiso 1 1 calc R . .
H8B H 0.3971 0.8256 0.4276 0.037 Uiso 1 1 calc R . .
H8C H 0.6053 0.8709 0.4241 0.037 Uiso 1 1 calc R . .
C9 C 0.6452(10) 0.6426(6) 0.4683(5) 0.0205(18) Uani 1 1 d . . .
C10 C 0.6595(11) 0.6360(6) 0.3802(5) 0.0236(19) Uani 1 1 d . . .
H10 H 0.6140 0.6969 0.3455 0.028 Uiso 1 1 calc R . .
C11 C 0.7416(11) 0.5386(6) 0.3426(5) 0.027(2) Uani 1 1 d . . .
H11 H 0.7519 0.5317 0.2816 0.032 Uiso 1 1 calc R . .
C12 C 0.8084(10) 0.4516(6) 0.3945(5) 0.0224(18) Uani 1 1 d . . .
H12 H 0.8756 0.3987 0.3687 0.027 Uiso 1 1 d R . .
C13 C 0.7863(10) 0.4592(6) 0.4850(5) 0.0210(18) Uani 1 1 d . . .
C14 C 0.8507(10) 0.3632(6) 0.5393(5) 0.0239(19) Uani 1 1 d . . .
C15 C 0.8302(11) 0.3590(6) 0.6310(5) 0.0238(19) Uani 1 1 d . . .
C16 C 0.8892(11) 0.2577(6) 0.6738(5) 0.030(2) Uani 1 1 d . . .
H16 H 0.8719 0.2536 0.7353 0.036 Uiso 1 1 calc R . .
C17 C 0.9701(11) 0.1658(6) 0.6299(5) 0.030(2) Uani 1 1 d . . .
H17 H 1.0070 0.0994 0.6605 0.037 Uiso 1 1 calc R . .
C18 C 0.9973(10) 0.1711(6) 0.5397(5) 0.0248(19) Uani 1 1 d . . .
H18 H 1.0539 0.1086 0.5082 0.030 Uiso 1 1 calc R . .
C19 C 0.9424(10) 0.2661(6) 0.4977(5) 0.0261(19) Uani 1 1 d . . .
H19 H 0.9662 0.2686 0.4364 0.031 Uiso 1 1 calc R . .
C20 C 0.2996(18) 1.0708(7) 0.8418(6) 0.075(3) Uani 1 1 d DU . .
H20 H 0.1581 1.0792 0.8345 0.090 Uiso 1 1 calc R . .
C21 C 0.299(2) 1.0241(9) 0.9284(6) 0.159(6) Uani 1 1 d DU . .
H21A H 0.4243 1.0301 0.9499 0.238 Uiso 1 1 calc R . .
H21B H 0.2752 0.9462 0.9278 0.238 Uiso 1 1 calc R . .
H21C H 0.1961 1.0641 0.9663 0.238 Uiso 1 1 calc R . .
C22 C 0.3481(15) 1.1848(6) 0.8265(6) 0.069(3) Uani 1 1 d DU . .
H22A H 0.2886 1.2302 0.8748 0.104 Uiso 1 1 calc R . .
H22B H 0.2991 1.2142 0.7726 0.104 Uiso 1 1 calc R . .
H22C H 0.4890 1.1861 0.8219 0.104 Uiso 1 1 calc R . .
C23 C 0.7767(12) 0.6876(6) 0.7964(5) 0.0246(19) Uani 1 1 d . . .
C24 C 0.7278(12) 0.7294(6) 0.8879(5) 0.038(2) Uani 1 1 d . . .
H24A H 0.8293 0.6999 0.9239 0.057 Uiso 1 1 calc R . .
H24B H 0.6033 0.7051 0.9121 0.057 Uiso 1 1 calc R . .
H24C H 0.7194 0.8102 0.8865 0.057 Uiso 1 1 calc R . .
C25 C 0.7794(12) 0.3717(6) 0.9541(5) 0.038(2) Uani 1 1 d . . .
H25 H 0.7635 0.3940 1.0159 0.046 Uiso 1 1 calc R . .
Cl1 Cl 0.8234(4) 0.2279(2) 0.95095(18) 0.0687(9) Uani 1 1 d . . .
Cl2 Cl 0.9739(3) 0.43491(19) 0.89966(14) 0.0466(6) Uani 1 1 d . . .
Cl3 Cl 0.5651(3) 0.41685(18) 0.90698(14) 0.0439(6) Uani 1 1 d . . .
O3 O 0.2588(7) 0.6107(4) 0.8449(3) 0.0382(15) Uani 1 1 d . . .
H1A H 0.1838 0.6436 0.8245 0.046 Uiso 1 1 d R . .
H1B H 0.3666 0.6206 0.8317 0.046 Uiso 1 1 d 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 N3 1.932(6) . ?
Pd1 N2 1.963(5) . ?
Pd1 N1 2.014(6) . ?
Pd1 O1 2.036(5) . ?
O1 C23 1.294(8) . ?
O2 C23 1.226(9) . ?
N1 C7 1.286(8) . ?
N1 C1 1.426(9) . ?
N2 C13 1.361(8) . ?
N2 C9 1.369(8) . ?
N3 C15 1.347(9) . ?
N3 H3A 0.8800 . ?
C1 C6 1.380(10) . ?
C1 C2 1.382(10) . ?
C2 C3 1.383(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.396(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.356(13) . ?
C4 C20 1.494(11) . ?
C5 C6 1.374(10) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C9 1.469(9) . ?
C7 C8 1.499(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.367(9) . ?
C10 C11 1.386(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.404(9) . ?
C12 H12 0.8448 . ?
C13 C14 1.478(10) . ?
C14 C15 1.417(10) . ?
C14 C19 1.429(9) . ?
C15 C16 1.425(10) . ?
C16 C17 1.374(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.395(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.349(9) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.441(8) . ?
C20 C22 1.468(8) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.522(9) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 Cl1 1.750(8) . ?
C25 Cl2 1.754(8) . ?
C25 Cl3 1.763(8) . ?
C25 H25 1.0000 . ?
O3 H1A 0.7201 . ?
O3 H1B 0.7794 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Pd1 N2 93.7(2) . . ?
N3 Pd1 N1 174.6(3) . . ?
N2 Pd1 N1 82.2(2) . . ?
N3 Pd1 O1 90.3(2) . . ?
N2 Pd1 O1 176.0(2) . . ?
N1 Pd1 O1 93.8(2) . . ?
C23 O1 Pd1 116.7(5) . . ?
C7 N1 C1 124.0(7) . . ?
C7 N1 Pd1 114.2(5) . . ?
C1 N1 Pd1 121.7(5) . . ?
C13 N2 C9 120.0(6) . . ?
C13 N2 Pd1 127.4(5) . . ?
C9 N2 Pd1 112.6(5) . . ?
C15 N3 Pd1 127.2(5) . . ?
C15 N3 H3A 116.4 . . ?
Pd1 N3 H3A 116.4 . . ?
C6 C1 C2 118.8(8) . . ?
C6 C1 N1 122.1(8) . . ?
C2 C1 N1 118.8(7) . . ?
C1 C2 C3 119.5(8) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C2 C3 C4 121.5(9) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C5 C4 C3 117.7(8) . . ?
C5 C4 C20 123.8(10) . . ?
C3 C4 C20 118.5(10) . . ?
C4 C5 C6 121.7(9) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 120.8(9) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
N1 C7 C9 115.5(7) . . ?
N1 C7 C8 124.3(7) . . ?
C9 C7 C8 120.2(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 122.3(7) . . ?
C10 C9 C7 122.1(7) . . ?
N2 C9 C7 115.5(7) . . ?
C9 C10 C11 118.7(7) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 120.7(7) . . ?
C11 C12 H12 116.1 . . ?
C13 C12 H12 122.7 . . ?
N2 C13 C12 118.7(7) . . ?
N2 C13 C14 121.6(7) . . ?
C12 C13 C14 119.7(7) . . ?
C15 C14 C19 116.2(7) . . ?
C15 C14 C13 125.2(7) . . ?
C19 C14 C13 118.7(7) . . ?
N3 C15 C14 124.6(7) . . ?
N3 C15 C16 117.1(7) . . ?
C14 C15 C16 118.2(7) . . ?
C17 C16 C15 122.7(8) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C16 C17 C18 119.1(7) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C19 C18 C17 119.3(7) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C14 124.3(7) . . ?
C18 C19 H19 117.8 . . ?
C14 C19 H19 117.8 . . ?
C21 C20 C22 118.6(9) . . ?
C21 C20 C4 113.8(8) . . ?
C22 C20 C4 116.6(8) . . ?
C21 C20 H20 101.2 . . ?
C22 C20 H20 101.2 . . ?
C4 C20 H20 101.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C23 O1 125.4(7) . . ?
O2 C23 C24 121.6(7) . . ?
O1 C23 C24 112.9(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 . . ?
Cl1 C25 Cl2 110.8(5) . . ?
Cl1 C25 Cl3 110.4(5) . . ?
Cl2 C25 Cl3 109.6(4) . . ?
Cl1 C25 H25 108.7 . . ?
Cl2 C25 H25 108.7 . . ?
Cl3 C25 H25 108.7 . . ?
H1A O3 H1B 119.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Pd1 O1 C23 95.7(5) . . . . ?
N1 Pd1 O1 C23 -87.8(5) . . . . ?
N2 Pd1 N1 C7 1.1(5) . . . . ?
O1 Pd1 N1 C7 -179.2(5) . . . . ?
N2 Pd1 N1 C1 179.4(6) . . . . ?
O1 Pd1 N1 C1 -0.9(6) . . . . ?
N3 Pd1 N2 C13 -5.7(6) . . . . ?
N1 Pd1 N2 C13 177.8(6) . . . . ?
N3 Pd1 N2 C9 175.3(5) . . . . ?
N1 Pd1 N2 C9 -1.1(5) . . . . ?
N2 Pd1 N3 C15 4.0(7) . . . . ?
O1 Pd1 N3 C15 -176.0(6) . . . . ?
C7 N1 C1 C6 -92.1(10) . . . . ?
Pd1 N1 C1 C6 89.7(8) . . . . ?
C7 N1 C1 C2 94.4(10) . . . . ?
Pd1 N1 C1 C2 -83.8(8) . . . . ?
C6 C1 C2 C3 -0.6(12) . . . . ?
N1 C1 C2 C3 173.2(7) . . . . ?
C1 C2 C3 C4 0.1(13) . . . . ?
C2 C3 C4 C5 0.2(14) . . . . ?
C2 C3 C4 C20 -177.2(8) . . . . ?
C3 C4 C5 C6 0.1(14) . . . . ?
C20 C4 C5 C6 177.3(8) . . . . ?
C4 C5 C6 C1 -0.6(14) . . . . ?
C2 C1 C6 C5 0.9(13) . . . . ?
N1 C1 C6 C5 -172.7(7) . . . . ?
C1 N1 C7 C9 -179.0(7) . . . . ?
Pd1 N1 C7 C9 -0.7(8) . . . . ?
C1 N1 C7 C8 1.0(12) . . . . ?
Pd1 N1 C7 C8 179.3(6) . . . . ?
C13 N2 C9 C10 -1.0(11) . . . . ?
Pd1 N2 C9 C10 178.0(6) . . . . ?
C13 N2 C9 C7 -177.9(6) . . . . ?
Pd1 N2 C9 C7 1.1(8) . . . . ?
N1 C7 C9 C10 -177.2(7) . . . . ?
C8 C7 C9 C10 2.8(11) . . . . ?
N1 C7 C9 N2 -0.2(10) . . . . ?
C8 C7 C9 N2 179.7(6) . . . . ?
N2 C9 C10 C11 -0.2(11) . . . . ?
C7 C9 C10 C11 176.5(7) . . . . ?
C9 C10 C11 C12 -0.7(11) . . . . ?
C10 C11 C12 C13 2.7(11) . . . . ?
C9 N2 C13 C12 3.0(10) . . . . ?
Pd1 N2 C13 C12 -175.8(5) . . . . ?
C9 N2 C13 C14 -178.1(6) . . . . ?
Pd1 N2 C13 C14 3.0(10) . . . . ?
C11 C12 C13 N2 -3.9(11) . . . . ?
C11 C12 C13 C14 177.2(7) . . . . ?
N2 C13 C14 C15 3.5(12) . . . . ?
C12 C13 C14 C15 -177.6(7) . . . . ?
N2 C13 C14 C19 -176.1(6) . . . . ?
C12 C13 C14 C19 2.8(10) . . . . ?
Pd1 N3 C15 C14 0.6(11) . . . . ?
Pd1 N3 C15 C16 178.9(5) . . . . ?
C19 C14 C15 N3 174.1(7) . . . . ?
C13 C14 C15 N3 -5.5(12) . . . . ?
C19 C14 C15 C16 -4.2(10) . . . . ?
C13 C14 C15 C16 176.2(7) . . . . ?
N3 C15 C16 C17 -176.4(7) . . . . ?
C14 C15 C16 C17 2.0(12) . . . . ?
C15 C16 C17 C18 0.4(12) . . . . ?
C16 C17 C18 C19 -0.5(12) . . . . ?
C17 C18 C19 C14 -2.0(12) . . . . ?
C15 C14 C19 C18 4.4(11) . . . . ?
C13 C14 C19 C18 -176.0(7) . . . . ?
C5 C4 C20 C21 -98.5(14) . . . . ?
C3 C4 C20 C21 78.6(14) . . . . ?
C5 C4 C20 C22 45.1(15) . . . . ?
C3 C4 C20 C22 -137.7(10) . . . . ?
Pd1 O1 C23 O2 -3.8(10) . . . . ?
Pd1 O1 C23 C24 175.5(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3A Cl3 0.88 2.84 3.652(6) 154.2 .
O3 H1A O2 0.72 2.18 2.877(7) 164.2 1_455
O3 H1B O1 0.78 2.07 2.833(7) 166.9 .

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.149

####################################################################### 
# 
# 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_10019
_database_code_depnum_ccdc_archive 'CCDC 1043192'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H31 N3 O2 Pd,C H Cl3'
_chemical_formula_sum            'C28 H32 Cl3 N3 O2 Pd'
_chemical_formula_weight         655.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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

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

_cell_length_a                   14.194(4)
_cell_length_b                   15.316(4)
_cell_length_c                   15.711(4)
_cell_angle_alpha                61.002(5)
_cell_angle_beta                 77.050(7)
_cell_angle_gamma                80.162(7)
_cell_volume                     2903.6(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    700
_cell_measurement_theta_min      2.198
_cell_measurement_theta_max      23.352

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 3767 reflections(SADABS);Rint 0.1246 before
correction and 0.0819 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22854
_diffrn_reflns_av_R_equivalents  0.1479
_diffrn_reflns_av_sigmaI/netI    0.2493
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         26.00
_reflns_number_total             11293
_reflns_number_gt                4526
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0753P)²+0.0000P] 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         11293
_refine_ls_number_parameters     679
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1888
_refine_ls_R_factor_gt           0.0873
_refine_ls_wR_factor_ref         0.2173
_refine_ls_wR_factor_gt          0.1788
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_restrained_S_all      0.848
_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 0.17657(6) 0.56487(6) 0.76218(6) 0.0453(3) Uani 1 1 d . . .
O1 O 0.3003(6) 0.5338(6) 0.6867(6) 0.068(2) Uani 1 1 d . . .
O2 O 0.4153(6) 0.6177(7) 0.6894(7) 0.086(3) Uani 1 1 d . . .
N1 N 0.1000(7) 0.5126(5) 0.7048(5) 0.040(2) Uani 1 1 d . . .
N2 N 0.0474(7) 0.5865(6) 0.8306(6) 0.046(2) Uani 1 1 d . . .
N3 N 0.2372(7) 0.6213(7) 0.8201(7) 0.066(3) Uani 1 1 d . . .
H3B H 0.2995 0.6291 0.7980 0.079 Uiso 1 1 calc R . .
C1 C 0.1423(7) 0.4738(7) 0.6362(7) 0.038(2) Uani 1 1 d . . .
C2 C 0.1592(7) 0.5357(7) 0.5374(7) 0.038(2) Uani 1 1 d . . .
C3 C 0.2046(8) 0.4960(7) 0.4745(7) 0.045(3) Uani 1 1 d . . .
H3 H 0.2185 0.5390 0.4056 0.054 Uiso 1 1 calc R . .
C4 C 0.2299(8) 0.3937(7) 0.5111(8) 0.051(3) Uani 1 1 d . . .
H4 H 0.2583 0.3663 0.4676 0.062 Uiso 1 1 calc R . .
C5 C 0.2129(8) 0.3332(8) 0.6111(8) 0.054(3) Uani 1 1 d . . .
H5 H 0.2314 0.2638 0.6353 0.065 Uiso 1 1 calc R . .
C6 C 0.1713(8) 0.3665(7) 0.6776(8) 0.044(3) Uani 1 1 d . . .
C7 C 0.0082(8) 0.5196(7) 0.7334(7) 0.040(3) Uani 1 1 d . . .
C8 C -0.0665(8) 0.4888(8) 0.6985(8) 0.056(3) Uani 1 1 d . . .
H8A H -0.0333 0.4644 0.6515 0.084 Uiso 1 1 calc R . .
H8B H -0.1112 0.5466 0.6665 0.084 Uiso 1 1 calc R . .
H8C H -0.1029 0.4355 0.7553 0.084 Uiso 1 1 calc R . .
C9 C -0.0252(8) 0.5591(6) 0.8045(7) 0.038(3) Uani 1 1 d . . .
C10 C -0.1214(8) 0.5708(8) 0.8388(8) 0.051(3) Uani 1 1 d . . .
H10 H -0.1700 0.5528 0.8184 0.061 Uiso 1 1 calc R . .
C11 C -0.1453(10) 0.6102(9) 0.9047(9) 0.068(4) Uani 1 1 d . . .
H11 H -0.2111 0.6169 0.9326 0.081 Uiso 1 1 calc R . .
C12 C -0.0746(10) 0.6390(8) 0.9290(8) 0.059(3) Uani 1 1 d . . .
H12 H -0.0927 0.6699 0.9707 0.070 Uiso 1 1 calc R . .
C13 C 0.0256(8) 0.6250(7) 0.8946(7) 0.041(3) Uani 1 1 d . . .
C14 C 0.0994(10) 0.6532(7) 0.9265(7) 0.050(3) Uani 1 1 d . . .
C15 C 0.1998(9) 0.6501(7) 0.8880(8) 0.050(3) Uani 1 1 d . . .
C16 C 0.2637(10) 0.6836(8) 0.9240(9) 0.066(4) Uani 1 1 d . . .
H16 H 0.3308 0.6850 0.8971 0.080 Uiso 1 1 calc R . .
C17 C 0.2319(11) 0.7131(9) 0.9950(9) 0.070(4) Uani 1 1 d . . .
H17 H 0.2767 0.7329 1.0181 0.084 Uiso 1 1 calc R . .
C18 C 0.1352(13) 0.7144(8) 1.0332(9) 0.075(4) Uani 1 1 d . . .
H18 H 0.1132 0.7347 1.0831 0.091 Uiso 1 1 calc R . .
C19 C 0.0703(10) 0.6867(7) 1.0000(8) 0.060(3) Uani 1 1 d . . .
H19 H 0.0035 0.6897 1.0266 0.072 Uiso 1 1 calc R . .
C20 C 0.1553(9) 0.2984(8) 0.7867(8) 0.055(3) Uani 1 1 d . . .
H20 H 0.1278 0.3397 0.8212 0.065 Uiso 1 1 calc R . .
C21 C 0.0853(10) 0.2204(9) 0.8160(9) 0.090(5) Uani 1 1 d . . .
H21A H 0.0257 0.2534 0.7887 0.135 Uiso 1 1 calc R . .
H21B H 0.0697 0.1838 0.8881 0.135 Uiso 1 1 calc R . .
H21C H 0.1150 0.1735 0.7902 0.135 Uiso 1 1 calc R . .
C22 C 0.2492(11) 0.2474(12) 0.8194(10) 0.117(6) Uani 1 1 d . . .
H22A H 0.2743 0.2018 0.7910 0.176 Uiso 1 1 calc R . .
H22B H 0.2394 0.2093 0.8916 0.176 Uiso 1 1 calc R . .
H22C H 0.2958 0.2975 0.7972 0.176 Uiso 1 1 calc R . .
C23 C 0.1352(8) 0.6471(7) 0.4952(7) 0.044(3) Uani 1 1 d . . .
H23 H 0.1046 0.6627 0.5505 0.052 Uiso 1 1 calc R . .
C24 C 0.0624(8) 0.6823(7) 0.4225(8) 0.056(3) Uani 1 1 d . . .
H24A H 0.0912 0.6669 0.3680 0.084 Uiso 1 1 calc R . .
H24B H 0.0471 0.7547 0.3962 0.084 Uiso 1 1 calc R . .
H24C H 0.0028 0.6476 0.4572 0.084 Uiso 1 1 calc R . .
C25 C 0.2272(7) 0.7021(7) 0.4435(8) 0.051(3) Uani 1 1 d . . .
H25A H 0.2680 0.6872 0.4924 0.077 Uiso 1 1 calc R . .
H25B H 0.2102 0.7743 0.4098 0.077 Uiso 1 1 calc R . .
H25C H 0.2627 0.6802 0.3952 0.077 Uiso 1 1 calc R . .
C26 C 0.3832(10) 0.5596(10) 0.6678(9) 0.064(4) Uani 1 1 d . . .
C27 C 0.4582(9) 0.5077(10) 0.6157(10) 0.082(4) Uani 1 1 d . . .
H27A H 0.4703 0.4372 0.6628 0.122 Uiso 1 1 calc R . .
H27B H 0.5188 0.5410 0.5908 0.122 Uiso 1 1 calc R . .
H27C H 0.4330 0.5118 0.5606 0.122 Uiso 1 1 calc R . .
Pd1A Pd 0.19550(6) 1.01151(6) 0.30844(5) 0.0382(2) Uani 1 1 d . . .
O1A O 0.2935(5) 1.0884(7) 0.1891(5) 0.074(3) Uani 1 1 d . . .
O2A O 0.2107(6) 1.1700(6) 0.0662(6) 0.074(3) Uani 1 1 d . . .
N1A N 0.2986(5) 0.9661(5) 0.3943(5) 0.0325(19) Uani 1 1 d . . .
N2A N 0.1146(5) 0.9295(5) 0.4353(5) 0.0292(18) Uani 1 1 d . . .
N3A N 0.0880(6) 1.0522(6) 0.2383(6) 0.044(2) Uani 1 1 d . . .
H3C H 0.0992 1.0983 0.1764 0.053 Uiso 1 1 calc R . .
C1A C 0.3955(7) 1.0000(7) 0.3556(7) 0.036(2) Uani 1 1 d . . .
C2A C 0.4607(8) 0.9552(8) 0.3075(7) 0.045(3) Uani 1 1 d . . .
C3A C 0.5497(8) 0.9963(8) 0.2603(8) 0.052(3) Uani 1 1 d . . .
H3A H 0.5979 0.9638 0.2305 0.062 Uiso 1 1 calc R . .
C4A C 0.5689(8) 1.0840(8) 0.2563(7) 0.049(3) Uani 1 1 d . . .
H4A H 0.6284 1.1131 0.2202 0.058 Uiso 1 1 calc R . .
C5A C 0.5026(8) 1.1295(8) 0.3043(7) 0.045(3) Uani 1 1 d . . .
H5A H 0.5175 1.1885 0.3026 0.053 Uiso 1 1 calc R . .
C6A C 0.4132(7) 1.0889(8) 0.3555(7) 0.044(3) Uani 1 1 d . . .
C7A C 0.2679(7) 0.9107(7) 0.4875(7) 0.036(2) Uani 1 1 d . . .
C8A C 0.3306(7) 0.8726(7) 0.5649(7) 0.042(3) Uani 1 1 d . . .
H8A1 H 0.3954 0.8969 0.5341 0.063 Uiso 1 1 calc R . .
H8A2 H 0.3356 0.7992 0.5981 0.063 Uiso 1 1 calc R . .
H8A3 H 0.3021 0.8965 0.6134 0.063 Uiso 1 1 calc R . .
C9A C 0.1662(7) 0.8892(7) 0.5135(7) 0.033(2) Uani 1 1 d . . .
C10A C 0.1221(7) 0.8351(7) 0.6089(7) 0.037(2) Uani 1 1 d . . .
H10A H 0.1580 0.8073 0.6617 0.044 Uiso 1 1 calc R . .
C11A C 0.0249(7) 0.8219(7) 0.6268(7) 0.037(2) Uani 1 1 d . . .
H11A H -0.0075 0.7864 0.6925 0.044 Uiso 1 1 calc R . .
C12A C -0.0245(7) 0.8594(7) 0.5508(7) 0.039(3) Uani 1 1 d . . .
H12A H -0.0916 0.8496 0.5643 0.047 Uiso 1 1 calc R . .
C13A C 0.0211(7) 0.9136(6) 0.4503(7) 0.035(2) Uani 1 1 d . . .
C14A C -0.0356(7) 0.9518(6) 0.3699(7) 0.034(2) Uani 1 1 d . . .
C15A C -0.0005(8) 1.0209(7) 0.2700(7) 0.041(3) Uani 1 1 d . . .
C16A C -0.0671(8) 1.0573(8) 0.2028(7) 0.045(3) Uani 1 1 d . . .
H16A H -0.0476 1.1069 0.1371 0.054 Uiso 1 1 calc R . .
C17A C -0.1575(8) 1.0245(8) 0.2279(9) 0.054(3) Uani 1 1 d . . .
H17A H -0.1986 1.0504 0.1795 0.065 Uiso 1 1 calc R . .
C18A C -0.1892(8) 0.9551(8) 0.3213(8) 0.047(3) Uani 1 1 d . . .
H18A H -0.2523 0.9321 0.3393 0.057 Uiso 1 1 calc R . .
C19A C -0.1278(8) 0.9193(7) 0.3888(8) 0.045(3) Uani 1 1 d . . .
H19A H -0.1495 0.8686 0.4532 0.054 Uiso 1 1 calc R . .
C20A C 0.3406(7) 1.1406(7) 0.4046(8) 0.042(3) Uani 1 1 d . . .
H20A H 0.2927 1.0909 0.4526 0.051 Uiso 1 1 calc R . .
C21A C 0.3851(8) 1.1738(8) 0.4639(8) 0.061(3) Uani 1 1 d . . .
H21D H 0.4177 1.1156 0.5133 0.091 Uiso 1 1 calc R . .
H21E H 0.3338 1.2038 0.4970 0.091 Uiso 1 1 calc R . .
H21F H 0.4322 1.2232 0.4191 0.091 Uiso 1 1 calc R . .
C22A C 0.2849(8) 1.2270(8) 0.3299(8) 0.057(3) Uani 1 1 d . . .
H22D H 0.3289 1.2791 0.2834 0.086 Uiso 1 1 calc R . .
H22E H 0.2325 1.2548 0.3642 0.086 Uiso 1 1 calc R . .
H22F H 0.2574 1.2030 0.2938 0.086 Uiso 1 1 calc R . .
C23A C 0.4391(8) 0.8625(9) 0.3061(8) 0.054(3) Uani 1 1 d . . .
H23A H 0.3672 0.8586 0.3229 0.064 Uiso 1 1 calc R . .
C24A C 0.4840(9) 0.7673(8) 0.3846(9) 0.070(4) Uani 1 1 d . . .
H24D H 0.5546 0.7636 0.3648 0.104 Uiso 1 1 calc R . .
H24E H 0.4581 0.7086 0.3911 0.104 Uiso 1 1 calc R . .
H24F H 0.4682 0.7686 0.4479 0.104 Uiso 1 1 calc R . .
C25A C 0.4721(8) 0.8665(10) 0.2019(9) 0.071(4) Uani 1 1 d . . .
H25D H 0.4402 0.9258 0.1529 0.106 Uiso 1 1 calc R . .
H25E H 0.4540 0.8061 0.2045 0.106 Uiso 1 1 calc R . .
H25F H 0.5426 0.8699 0.1834 0.106 Uiso 1 1 calc R . .
C26A C 0.2857(9) 1.1515(9) 0.1016(9) 0.051(3) Uani 1 1 d . . .
C27A C 0.3770(10) 1.1960(12) 0.0399(9) 0.108(6) Uani 1 1 d . . .
H27D H 0.4049 1.1633 -0.0014 0.162 Uiso 1 1 calc R . .
H27E H 0.4229 1.1865 0.0825 0.162 Uiso 1 1 calc R . .
H27F H 0.3638 1.2677 -0.0022 0.162 Uiso 1 1 calc R . .
C28 C 0.2165(9) 0.9440(8) 0.0801(8) 0.066(4) Uani 1 1 d . . .
H28 H 0.2169 0.9948 0.1027 0.079 Uiso 1 1 calc R . .
Cl1 Cl 0.2238(3) 0.8222(3) 0.1835(3) 0.1096(15) Uani 1 1 d . . .
Cl2 Cl 0.1115(3) 0.9640(3) 0.0368(3) 0.0930(12) Uani 1 1 d . . .
Cl3 Cl 0.3192(3) 0.9542(3) -0.0077(2) 0.0910(12) Uani 1 1 d . . .
C29 C 0.4343(9) 0.4936(10) 0.1757(9) 0.078(4) Uani 1 1 d . . .
H29 H 0.4763 0.4435 0.2239 0.093 Uiso 1 1 calc R . .
Cl4 Cl 0.3236(3) 0.5168(3) 0.2410(3) 0.0991(13) Uani 1 1 d . . .
Cl5 Cl 0.4112(3) 0.4435(3) 0.1036(3) 0.1170(16) Uani 1 1 d . . .
Cl6 Cl 0.4921(4) 0.6027(4) 0.1041(4) 0.145(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 N3 1.920(9) . ?
Pd1 N2 1.970(9) . ?
Pd1 O1 2.011(8) . ?
Pd1 N1 2.017(8) . ?
O1 C26 1.232(14) . ?
O2 C26 1.272(14) . ?
N1 C7 1.285(12) . ?
N1 C1 1.444(11) . ?
N2 C13 1.352(11) . ?
N2 C9 1.382(12) . ?
N3 C15 1.316(12) . ?
N3 H3B 0.8800 . ?
C1 C2 1.360(12) . ?
C1 C6 1.464(13) . ?
C2 C3 1.388(12) . ?
C2 C23 1.506(12) . ?
C3 C4 1.393(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.371(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.355(13) . ?
C5 H5 0.9500 . ?
C6 C20 1.501(14) . ?
C7 C9 1.468(13) . ?
C7 C8 1.527(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.367(13) . ?
C10 C11 1.389(15) . ?
C10 H10 0.9500 . ?
C11 C12 1.354(15) . ?
C11 H11 0.9500 . ?
C12 C13 1.423(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.461(14) . ?
C14 C15 1.421(15) . ?
C14 C19 1.434(14) . ?
C15 C16 1.442(15) . ?
C16 C17 1.358(15) . ?
C16 H16 0.9500 . ?
C17 C18 1.370(17) . ?
C17 H17 0.9500 . ?
C18 C19 1.365(15) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.487(16) . ?
C20 C21 1.515(15) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.521(13) . ?
C23 C24 1.550(13) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.544(16) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
Pd1A N3A 1.922(8) . ?
Pd1A N2A 1.977(7) . ?
Pd1A N1A 2.019(8) . ?
Pd1A O1A 2.021(7) . ?
O1A C26A 1.257(12) . ?
O2A C26A 1.237(12) . ?
N1A C7A 1.300(11) . ?
N1A C1A 1.447(11) . ?
N2A C13A 1.338(11) . ?
N2A C9A 1.394(11) . ?
N3A C15A 1.323(12) . ?
N3A H3C 0.8800 . ?
C1A C2A 1.368(13) . ?
C1A C6A 1.427(13) . ?
C2A C3A 1.393(14) . ?
C2A C23A 1.512(14) . ?
C3A C4A 1.384(14) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.382(14) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.403(13) . ?
C5A H5A 0.9500 . ?
C6A C20A 1.497(14) . ?
C7A C9A 1.458(13) . ?
C7A C8A 1.494(12) . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A C10A 1.370(12) . ?
C10A C11A 1.375(12) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.348(13) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.433(12) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.472(13) . ?
C14A C19A 1.398(13) . ?
C14A C15A 1.433(13) . ?
C15A C16A 1.419(13) . ?
C16A C17A 1.363(13) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.357(14) . ?
C17A H17A 0.9500 . ?
C18A C19A 1.368(13) . ?
C18A H18A 0.9500 . ?
C19A H19A 0.9500 . ?
C20A C22A 1.519(13) . ?
C20A C21A 1.535(13) . ?
C20A H20A 1.0000 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C23A C24A 1.531(15) . ?
C23A C25A 1.574(14) . ?
C23A H23A 1.0000 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C26A C27A 1.478(15) . ?
C27A H27D 0.9800 . ?
C27A H27E 0.9800 . ?
C27A H27F 0.9800 . ?
C28 Cl2 1.696(13) . ?
C28 Cl3 1.738(12) . ?
C28 Cl1 1.789(12) . ?
C28 H28 1.0000 . ?
C29 Cl6 1.722(12) . ?
C29 Cl5 1.753(13) . ?
C29 Cl4 1.757(13) . ?
C29 H29 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Pd1 N2 91.6(4) . . ?
N3 Pd1 O1 95.5(4) . . ?
N2 Pd1 O1 172.9(3) . . ?
N3 Pd1 N1 174.2(4) . . ?
N2 Pd1 N1 82.9(3) . . ?
O1 Pd1 N1 90.1(3) . . ?
C26 O1 Pd1 132.3(9) . . ?
C7 N1 C1 122.5(9) . . ?
C7 N1 Pd1 113.1(6) . . ?
C1 N1 Pd1 124.4(7) . . ?
C13 N2 C9 120.5(9) . . ?
C13 N2 Pd1 127.5(8) . . ?
C9 N2 Pd1 112.0(6) . . ?
C15 N3 Pd1 129.8(9) . . ?
C15 N3 H3B 115.1 . . ?
Pd1 N3 H3B 115.1 . . ?
C2 C1 N1 120.9(8) . . ?
C2 C1 C6 121.6(9) . . ?
N1 C1 C6 117.4(9) . . ?
C1 C2 C3 119.0(9) . . ?
C1 C2 C23 121.7(8) . . ?
C3 C2 C23 119.2(9) . . ?
C2 C3 C4 120.8(9) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 118.8(10) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C6 C5 C4 124.0(10) . . ?
C6 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C5 C6 C1 115.7(9) . . ?
C5 C6 C20 122.5(9) . . ?
C1 C6 C20 121.8(9) . . ?
N1 C7 C9 117.1(9) . . ?
N1 C7 C8 123.8(9) . . ?
C9 C7 C8 119.1(10) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 123.2(9) . . ?
C10 C9 C7 121.8(10) . . ?
N2 C9 C7 115.0(9) . . ?
C9 C10 C11 117.2(11) . . ?
C9 C10 H10 121.4 . . ?
C11 C10 H10 121.4 . . ?
C12 C11 C10 119.9(12) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 122.7(11) . . ?
C11 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
N2 C13 C12 116.5(10) . . ?
N2 C13 C14 122.9(10) . . ?
C12 C13 C14 120.6(10) . . ?
C15 C14 C19 117.3(11) . . ?
C15 C14 C13 123.5(9) . . ?
C19 C14 C13 119.2(11) . . ?
N3 C15 C14 124.2(11) . . ?
N3 C15 C16 118.5(12) . . ?
C14 C15 C16 117.2(10) . . ?
C17 C16 C15 122.6(13) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C16 C17 C18 119.9(13) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 120.5(12) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C14 122.4(13) . . ?
C18 C19 H19 118.8 . . ?
C14 C19 H19 118.8 . . ?
C22 C20 C6 110.0(10) . . ?
C22 C20 C21 109.3(11) . . ?
C6 C20 C21 112.1(10) . . ?
C22 C20 H20 108.5 . . ?
C6 C20 H20 108.5 . . ?
C21 C20 H20 108.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C2 C23 C25 110.1(9) . . ?
C2 C23 C24 110.6(8) . . ?
C25 C23 C24 110.4(8) . . ?
C2 C23 H23 108.6 . . ?
C25 C23 H23 108.6 . . ?
C24 C23 H23 108.6 . . ?
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 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O1 C26 O2 129.3(13) . . ?
O1 C26 C27 113.7(12) . . ?
O2 C26 C27 116.8(12) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3A Pd1A N2A 92.2(3) . . ?
N3A Pd1A N1A 174.3(3) . . ?
N2A Pd1A N1A 82.6(3) . . ?
N3A Pd1A O1A 95.6(3) . . ?
N2A Pd1A O1A 172.2(3) . . ?
N1A Pd1A O1A 89.6(3) . . ?
C26A O1A Pd1A 132.7(8) . . ?
C7A N1A C1A 123.6(8) . . ?
C7A N1A Pd1A 114.0(6) . . ?
C1A N1A Pd1A 122.2(6) . . ?
C13A N2A C9A 121.1(8) . . ?
C13A N2A Pd1A 127.3(6) . . ?
C9A N2A Pd1A 111.6(6) . . ?
C15A N3A Pd1A 129.3(7) . . ?
C15A N3A H3C 115.4 . . ?
Pd1A N3A H3C 115.4 . . ?
C2A C1A C6A 122.8(9) . . ?
C2A C1A N1A 118.7(9) . . ?
C6A C1A N1A 117.7(9) . . ?
C1A C2A C3A 118.0(10) . . ?
C1A C2A C23A 121.8(9) . . ?
C3A C2A C23A 120.1(10) . . ?
C4A C3A C2A 121.0(11) . . ?
C4A C3A H3A 119.5 . . ?
C2A C3A H3A 119.5 . . ?
C5A C4A C3A 120.7(10) . . ?
C5A C4A H4A 119.6 . . ?
C3A C4A H4A 119.6 . . ?
C4A C5A C6A 120.2(10) . . ?
C4A C5A H5A 119.9 . . ?
C6A C5A H5A 119.9 . . ?
C5A C6A C1A 117.1(10) . . ?
C5A C6A C20A 119.9(10) . . ?
C1A C6A C20A 123.0(9) . . ?
N1A C7A C9A 115.8(8) . . ?
N1A C7A C8A 123.1(9) . . ?
C9A C7A C8A 121.1(9) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10A C9A N2A 121.2(9) . . ?
C10A C9A C7A 122.8(9) . . ?
N2A C9A C7A 116.0(8) . . ?
C9A C10A C11A 118.8(9) . . ?
C9A C10A H10A 120.6 . . ?
C11A C10A H10A 120.6 . . ?
C12A C11A C10A 119.9(9) . . ?
C12A C11A H11A 120.0 . . ?
C10A C11A H11A 120.0 . . ?
C11A C12A C13A 122.1(9) . . ?
C11A C12A H12A 119.0 . . ?
C13A C12A H12A 119.0 . . ?
N2A C13A C12A 116.8(9) . . ?
N2A C13A C14A 123.2(8) . . ?
C12A C13A C14A 120.0(9) . . ?
C19A C14A C15A 116.7(9) . . ?
C19A C14A C13A 120.1(9) . . ?
C15A C14A C13A 123.2(9) . . ?
N3A C15A C16A 119.5(9) . . ?
N3A C15A C14A 124.2(9) . . ?
C16A C15A C14A 116.3(9) . . ?
C17A C16A C15A 123.2(10) . . ?
C17A C16A H16A 118.4 . . ?
C15A C16A H16A 118.4 . . ?
C18A C17A C16A 120.5(10) . . ?
C18A C17A H17A 119.7 . . ?
C16A C17A H17A 119.7 . . ?
C17A C18A C19A 118.1(11) . . ?
C17A C18A H18A 121.0 . . ?
C19A C18A H18A 121.0 . . ?
C18A C19A C14A 124.9(10) . . ?
C18A C19A H19A 117.6 . . ?
C14A C19A H19A 117.6 . . ?
C6A C20A C22A 110.5(9) . . ?
C6A C20A C21A 113.2(9) . . ?
C22A C20A C21A 111.8(9) . . ?
C6A C20A H20A 107.0 . . ?
C22A C20A H20A 107.0 . . ?
C21A C20A H20A 107.0 . . ?
C20A C21A H21D 109.5 . . ?
C20A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C20A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C20A C22A H22D 109.5 . . ?
C20A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C20A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C2A C23A C24A 111.5(9) . . ?
C2A C23A C25A 112.9(9) . . ?
C24A C23A C25A 110.1(9) . . ?
C2A C23A H23A 107.3 . . ?
C24A C23A H23A 107.3 . . ?
C25A C23A H23A 107.3 . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C23A C25A H25D 109.5 . . ?
C23A C25A H25E 109.5 . . ?
H25D C25A H25E 109.5 . . ?
C23A C25A H25F 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
O2A C26A O1A 124.0(10) . . ?
O2A C26A C27A 121.5(11) . . ?
O1A C26A C27A 114.3(11) . . ?
C26A C27A H27D 109.5 . . ?
C26A C27A H27E 109.5 . . ?
H27D C27A H27E 109.5 . . ?
C26A C27A H27F 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
Cl2 C28 Cl3 113.4(7) . . ?
Cl2 C28 Cl1 110.2(6) . . ?
Cl3 C28 Cl1 108.3(7) . . ?
Cl2 C28 H28 108.3 . . ?
Cl3 C28 H28 108.3 . . ?
Cl1 C28 H28 108.3 . . ?
Cl6 C29 Cl5 111.5(7) . . ?
Cl6 C29 Cl4 109.8(8) . . ?
Cl5 C29 Cl4 108.7(7) . . ?
Cl6 C29 H29 109.0 . . ?
Cl5 C29 H29 109.0 . . ?
Cl4 C29 H29 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Pd1 O1 C26 -12.8(12) . . . . ?
N1 Pd1 O1 C26 165.4(12) . . . . ?
N2 Pd1 N1 C7 2.2(6) . . . . ?
O1 Pd1 N1 C7 -178.8(7) . . . . ?
N2 Pd1 N1 C1 -179.5(7) . . . . ?
O1 Pd1 N1 C1 -0.5(7) . . . . ?
N3 Pd1 N2 C13 -1.9(8) . . . . ?
N1 Pd1 N2 C13 -180.0(8) . . . . ?
N3 Pd1 N2 C9 176.7(6) . . . . ?
N1 Pd1 N2 C9 -1.4(6) . . . . ?
N2 Pd1 N3 C15 6.6(10) . . . . ?
O1 Pd1 N3 C15 -172.6(10) . . . . ?
C7 N1 C1 C2 91.3(12) . . . . ?
Pd1 N1 C1 C2 -86.8(10) . . . . ?
C7 N1 C1 C6 -92.2(11) . . . . ?
Pd1 N1 C1 C6 89.7(10) . . . . ?
N1 C1 C2 C3 176.7(9) . . . . ?
C6 C1 C2 C3 0.3(15) . . . . ?
N1 C1 C2 C23 0.2(15) . . . . ?
C6 C1 C2 C23 -176.1(9) . . . . ?
C1 C2 C3 C4 2.0(16) . . . . ?
C23 C2 C3 C4 178.6(10) . . . . ?
C2 C3 C4 C5 -2.7(17) . . . . ?
C3 C4 C5 C6 1.0(18) . . . . ?
C4 C5 C6 C1 1.2(17) . . . . ?
C4 C5 C6 C20 -179.0(11) . . . . ?
C2 C1 C6 C5 -1.9(15) . . . . ?
N1 C1 C6 C5 -178.4(9) . . . . ?
C2 C1 C6 C20 178.3(10) . . . . ?
N1 C1 C6 C20 1.8(15) . . . . ?
C1 N1 C7 C9 179.1(8) . . . . ?
Pd1 N1 C7 C9 -2.5(10) . . . . ?
C1 N1 C7 C8 -0.4(14) . . . . ?
Pd1 N1 C7 C8 177.9(7) . . . . ?
C13 N2 C9 C10 1.5(14) . . . . ?
Pd1 N2 C9 C10 -177.2(8) . . . . ?
C13 N2 C9 C7 179.2(8) . . . . ?
Pd1 N2 C9 C7 0.5(10) . . . . ?
N1 C7 C9 C10 179.2(9) . . . . ?
C8 C7 C9 C10 -1.3(14) . . . . ?
N1 C7 C9 N2 1.4(12) . . . . ?
C8 C7 C9 N2 -179.0(8) . . . . ?
N2 C9 C10 C11 -1.5(15) . . . . ?
C7 C9 C10 C11 -179.1(9) . . . . ?
C9 C10 C11 C12 2.8(17) . . . . ?
C10 C11 C12 C13 -4.1(18) . . . . ?
C9 N2 C13 C12 -2.5(13) . . . . ?
Pd1 N2 C13 C12 176.0(6) . . . . ?
C9 N2 C13 C14 178.6(8) . . . . ?
Pd1 N2 C13 C14 -2.9(13) . . . . ?
C11 C12 C13 N2 3.9(15) . . . . ?
C11 C12 C13 C14 -177.2(10) . . . . ?
N2 C13 C14 C15 4.9(15) . . . . ?
C12 C13 C14 C15 -173.9(9) . . . . ?
N2 C13 C14 C19 -175.5(8) . . . . ?
C12 C13 C14 C19 5.7(14) . . . . ?
Pd1 N3 C15 C14 -6.5(16) . . . . ?
Pd1 N3 C15 C16 175.5(7) . . . . ?
C19 C14 C15 N3 -179.8(9) . . . . ?
C13 C14 C15 N3 -0.2(16) . . . . ?
C19 C14 C15 C16 -1.8(14) . . . . ?
C13 C14 C15 C16 177.8(9) . . . . ?
N3 C15 C16 C17 -178.9(10) . . . . ?
C14 C15 C16 C17 2.9(16) . . . . ?
C15 C16 C17 C18 -1.8(18) . . . . ?
C16 C17 C18 C19 -0.4(18) . . . . ?
C17 C18 C19 C14 1.4(17) . . . . ?
C15 C14 C19 C18 -0.3(15) . . . . ?
C13 C14 C19 C18 -179.9(9) . . . . ?
C5 C6 C20 C22 57.9(15) . . . . ?
C1 C6 C20 C22 -122.3(12) . . . . ?
C5 C6 C20 C21 -63.9(15) . . . . ?
C1 C6 C20 C21 115.9(11) . . . . ?
C1 C2 C23 C25 116.6(11) . . . . ?
C3 C2 C23 C25 -59.9(13) . . . . ?
C1 C2 C23 C24 -121.1(11) . . . . ?
C3 C2 C23 C24 62.4(13) . . . . ?
Pd1 O1 C26 O2 -2(2) . . . . ?
Pd1 O1 C26 C27 174.0(8) . . . . ?
N3A Pd1A O1A C26A 8.2(12) . . . . ?
N1A Pd1A O1A C26A -169.6(11) . . . . ?
N2A Pd1A N1A C7A -2.2(6) . . . . ?
O1A Pd1A N1A C7A 178.5(7) . . . . ?
N2A Pd1A N1A C1A -177.1(7) . . . . ?
O1A Pd1A N1A C1A 3.6(7) . . . . ?
N3A Pd1A N2A C13A 2.9(8) . . . . ?
N1A Pd1A N2A C13A -179.4(8) . . . . ?
N3A Pd1A N2A C9A -175.3(6) . . . . ?
N1A Pd1A N2A C9A 2.4(6) . . . . ?
N2A Pd1A N3A C15A -7.3(9) . . . . ?
O1A Pd1A N3A C15A 172.3(9) . . . . ?
C7A N1A C1A C2A 105.1(11) . . . . ?
Pd1A N1A C1A C2A -80.5(10) . . . . ?
C7A N1A C1A C6A -84.8(11) . . . . ?
Pd1A N1A C1A C6A 89.6(9) . . . . ?
C6A C1A C2A C3A 2.8(15) . . . . ?
N1A C1A C2A C3A 172.4(9) . . . . ?
C6A C1A C2A C23A -178.2(9) . . . . ?
N1A C1A C2A C23A -8.6(15) . . . . ?
C1A C2A C3A C4A -4.4(15) . . . . ?
C23A C2A C3A C4A 176.6(10) . . . . ?
C2A C3A C4A C5A 4.1(16) . . . . ?
C3A C4A C5A C6A -1.9(15) . . . . ?
C4A C5A C6A C1A 0.3(14) . . . . ?
C4A C5A C6A C20A -178.1(9) . . . . ?
C2A C1A C6A C5A -0.8(15) . . . . ?
N1A C1A C6A C5A -170.5(8) . . . . ?
C2A C1A C6A C20A 177.5(9) . . . . ?
N1A C1A C6A C20A 7.9(14) . . . . ?
C1A N1A C7A C9A 176.3(8) . . . . ?
Pd1A N1A C7A C9A 1.4(10) . . . . ?
C1A N1A C7A C8A -2.4(14) . . . . ?
Pd1A N1A C7A C8A -177.3(7) . . . . ?
C13A N2A C9A C10A -2.6(13) . . . . ?
Pd1A N2A C9A C10A 175.8(7) . . . . ?
C13A N2A C9A C7A 179.2(8) . . . . ?
Pd1A N2A C9A C7A -2.4(10) . . . . ?
N1A C7A C9A C10A -177.5(9) . . . . ?
C8A C7A C9A C10A 1.2(14) . . . . ?
N1A C7A C9A N2A 0.7(12) . . . . ?
C8A C7A C9A N2A 179.4(8) . . . . ?
N2A C9A C10A C11A -0.6(13) . . . . ?
C7A C9A C10A C11A 177.4(9) . . . . ?
C9A C10A C11A C12A 1.9(14) . . . . ?
C10A C11A C12A C13A -0.1(14) . . . . ?
C9A N2A C13A C12A 4.2(12) . . . . ?
Pd1A N2A C13A C12A -173.8(6) . . . . ?
C9A N2A C13A C14A -177.9(8) . . . . ?
Pd1A N2A C13A C14A 4.0(13) . . . . ?
C11A C12A C13A N2A -3.0(13) . . . . ?
C11A C12A C13A C14A 179.1(9) . . . . ?
N2A C13A C14A C19A 169.7(9) . . . . ?
C12A C13A C14A C19A -12.5(14) . . . . ?
N2A C13A C14A C15A -9.1(14) . . . . ?
C12A C13A C14A C15A 168.7(9) . . . . ?
Pd1A N3A C15A C16A -176.0(7) . . . . ?
Pd1A N3A C15A C14A 4.6(15) . . . . ?
C19A C14A C15A N3A -174.1(10) . . . . ?
C13A C14A C15A N3A 4.8(15) . . . . ?
C19A C14A C15A C16A 6.4(13) . . . . ?
C13A C14A C15A C16A -174.7(9) . . . . ?
N3A C15A C16A C17A 176.0(10) . . . . ?
C14A C15A C16A C17A -4.5(15) . . . . ?
C15A C16A C17A C18A 1.3(17) . . . . ?
C16A C17A C18A C19A -0.2(16) . . . . ?
C17A C18A C19A C14A 2.7(16) . . . . ?
C15A C14A C19A C18A -5.9(15) . . . . ?
C13A C14A C19A C18A 175.1(9) . . . . ?
C5A C6A C20A C22A 80.8(11) . . . . ?
C1A C6A C20A C22A -97.6(11) . . . . ?
C5A C6A C20A C21A -45.6(13) . . . . ?
C1A C6A C20A C21A 136.1(10) . . . . ?
C1A C2A C23A C24A -97.7(12) . . . . ?
C3A C2A C23A C24A 81.2(13) . . . . ?
C1A C2A C23A C25A 137.7(10) . . . . ?
C3A C2A C23A C25A -43.4(14) . . . . ?
Pd1A O1A C26A O2A -11(2) . . . . ?
Pd1A O1A C26A C27A 174.8(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3B O2 0.88 2.14 2.890(13) 142.7 .
N3A H3C O2A 0.88 2.06 2.800(11) 141.5 .

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.493
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.174

####################################################################### 
# 
# 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_11047
_database_code_depnum_ccdc_archive 'CCDC 1043193'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H22 Cl N3 Pd'
_chemical_formula_sum            'C22 H22 Cl N3 Pd'
_chemical_formula_weight         470.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   17.674(4)
_cell_length_b                   8.9111(19)
_cell_length_c                   24.267(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.133(5)
_cell_angle_gamma                90.00
_cell_volume                     3816.2(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    688
_cell_measurement_theta_min      2.435
_cell_measurement_theta_max      28.383

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   
;
absorption correction based on 5677 reflections(SADABS);Rint 0.0838 before
correction and 0.0561 after.
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28912
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_sigmaI/netI    0.1441
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         26.00
_reflns_number_total             7469
_reflns_number_gt                4098
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0248P)²+0.0000P] 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         7469
_refine_ls_number_parameters     493
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1078
_refine_ls_wR_factor_gt          0.0914
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_restrained_S_all      0.889
_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
Pd1 Pd 0.87136(3) 0.83002(6) 0.02279(2) 0.03692(16) Uani 1 1 d . . .
Cl1 Cl 0.75405(10) 0.9033(2) 0.04909(7) 0.0550(5) Uani 1 1 d . . .
N1 N 0.8943(3) 0.6861(5) 0.0859(2) 0.0388(14) Uani 1 1 d . . .
N2 N 0.9730(3) 0.7647(5) 0.0025(2) 0.0352(13) Uani 1 1 d . . .
N3 N 0.8600(3) 0.9685(6) -0.0385(2) 0.0419(14) Uani 1 1 d . . .
H3C H 0.8213 1.0307 -0.0382 0.050 Uiso 1 1 calc R . .
C1 C 0.8438(4) 0.6568(7) 0.1293(3) 0.0406(17) Uani 1 1 d . . .
C2 C 0.7795(4) 0.5754(8) 0.1181(3) 0.052(2) Uani 1 1 d . . .
H2 H 0.7691 0.5340 0.0824 0.063 Uiso 1 1 calc R . .
C3 C 0.7294(4) 0.5538(8) 0.1594(3) 0.054(2) Uani 1 1 d . . .
H3 H 0.6855 0.4941 0.1519 0.065 Uiso 1 1 calc R . .
C4 C 0.7418(4) 0.6170(8) 0.2109(3) 0.0450(19) Uani 1 1 d . . .
C5 C 0.8082(4) 0.6972(8) 0.2211(3) 0.0499(19) Uani 1 1 d . . .
H5 H 0.8188 0.7396 0.2566 0.060 Uiso 1 1 calc R . .
C6 C 0.8585(4) 0.7165(7) 0.1815(3) 0.0484(19) Uani 1 1 d . . .
H6 H 0.9040 0.7711 0.1896 0.058 Uiso 1 1 calc R . .
C7 C 0.9620(4) 0.6299(7) 0.0865(3) 0.0409(18) Uani 1 1 d . . .
C8 C 0.9938(4) 0.5270(7) 0.1311(3) 0.050(2) Uani 1 1 d . . .
H8A H 0.9533 0.4971 0.1549 0.075 Uiso 1 1 calc R . .
H8B H 1.0336 0.5793 0.1533 0.075 Uiso 1 1 calc R . .
H8C H 1.0151 0.4376 0.1143 0.075 Uiso 1 1 calc R . .
C9 C 1.0080(4) 0.6720(7) 0.0412(3) 0.0398(17) Uani 1 1 d . . .
C10 C 1.0813(4) 0.6239(7) 0.0374(3) 0.0483(19) Uani 1 1 d . . .
H10 H 1.1041 0.5578 0.0642 0.058 Uiso 1 1 calc R . .
C11 C 1.1213(4) 0.6744(8) -0.0065(3) 0.055(2) Uani 1 1 d . . .
H11 H 1.1726 0.6453 -0.0094 0.067 Uiso 1 1 calc R . .
C12 C 1.0874(4) 0.7651(7) -0.0456(3) 0.051(2) Uani 1 1 d . . .
H12 H 1.1154 0.7986 -0.0756 0.061 Uiso 1 1 calc R . .
C13 C 1.0100(4) 0.8111(7) -0.0421(3) 0.0423(18) Uani 1 1 d . . .
C14 C 0.9755(4) 0.9032(7) -0.0858(3) 0.0364(16) Uani 1 1 d . . .
C15 C 0.9042(4) 0.9803(7) -0.0811(3) 0.0402(18) Uani 1 1 d . . .
C16 C 0.8782(4) 1.0751(7) -0.1263(3) 0.0446(18) Uani 1 1 d . . .
H16 H 0.8325 1.1302 -0.1235 0.054 Uiso 1 1 calc R . .
C17 C 0.9171(4) 1.0882(7) -0.1730(3) 0.0496(19) Uani 1 1 d . . .
H17 H 0.8984 1.1510 -0.2023 0.059 Uiso 1 1 calc R . .
C18 C 0.9843(4) 1.0096(8) -0.1776(3) 0.058(2) Uani 1 1 d . . .
H18 H 1.0120 1.0183 -0.2099 0.070 Uiso 1 1 calc R . .
C19 C 1.0101(4) 0.9183(7) -0.1344(3) 0.050(2) Uani 1 1 d . . .
H19 H 1.0550 0.8622 -0.1390 0.060 Uiso 1 1 calc R . .
C20 C 0.6818(4) 0.6068(8) 0.2523(3) 0.0495(19) Uani 1 1 d . . .
H20 H 0.6507 0.5152 0.2435 0.059 Uiso 1 1 calc R . .
C21 C 0.7150(4) 0.5913(8) 0.3118(3) 0.060(2) Uani 1 1 d . . .
H21A H 0.7514 0.5081 0.3139 0.090 Uiso 1 1 calc R . .
H21B H 0.6741 0.5712 0.3365 0.090 Uiso 1 1 calc R . .
H21C H 0.7409 0.6846 0.3230 0.090 Uiso 1 1 calc R . .
C22 C 0.6294(4) 0.7420(8) 0.2473(3) 0.061(2) Uani 1 1 d . . .
H22A H 0.6581 0.8332 0.2570 0.092 Uiso 1 1 calc R . .
H22B H 0.5882 0.7301 0.2723 0.092 Uiso 1 1 calc R . .
H22C H 0.6082 0.7500 0.2092 0.092 Uiso 1 1 calc R . .
Pd1A Pd 0.35032(3) 0.60208(6) 0.01433(2) 0.04820(19) Uani 1 1 d . . .
Cl1A Cl 0.29151(11) 0.7717(2) 0.06874(8) 0.0618(6) Uani 1 1 d . . .
N1A N 0.3371(3) 0.4205(6) 0.0638(2) 0.0454(15) Uani 1 1 d . . .
N2A N 0.4082(3) 0.4558(7) -0.0283(2) 0.0480(16) Uani 1 1 d . . .
N3A N 0.3647(3) 0.7596(6) -0.0387(2) 0.0540(17) Uani 1 1 d . . .
H3B H 0.3435 0.8462 -0.0314 0.065 Uiso 1 1 calc R . .
C1A C 0.2926(4) 0.4162(7) 0.1107(3) 0.0457(19) Uani 1 1 d . . .
C2A C 0.3168(4) 0.4932(8) 0.1583(3) 0.056(2) Uani 1 1 d . . .
H2A H 0.3624 0.5499 0.1592 0.067 Uiso 1 1 calc R . .
C3A C 0.2748(4) 0.4866(8) 0.2037(3) 0.066(2) Uani 1 1 d . . .
H3A H 0.2924 0.5398 0.2358 0.079 Uiso 1 1 calc R . .
C4A C 0.2075(4) 0.4065(8) 0.2056(3) 0.053(2) Uani 1 1 d . . .
C5A C 0.1846(4) 0.3341(7) 0.1574(3) 0.055(2) Uani 1 1 d . . .
H5A H 0.1383 0.2797 0.1561 0.066 Uiso 1 1 calc R . .
C6A C 0.2259(4) 0.3371(7) 0.1110(3) 0.051(2) Uani 1 1 d . . .
H6A H 0.2081 0.2841 0.0789 0.061 Uiso 1 1 calc R . .
C7A C 0.3709(4) 0.3020(8) 0.0462(3) 0.053(2) Uani 1 1 d . . .
C8A C 0.3721(4) 0.1566(8) 0.0756(3) 0.067(2) Uani 1 1 d . . .
H8A1 H 0.4245 0.1219 0.0814 0.100 Uiso 1 1 calc R . .
H8A2 H 0.3427 0.0826 0.0536 0.100 Uiso 1 1 calc R . .
H8A3 H 0.3497 0.1691 0.1114 0.100 Uiso 1 1 calc R . .
C9A C 0.4116(4) 0.3165(9) -0.0038(3) 0.050(2) Uani 1 1 d . . .
C10A C 0.4514(4) 0.2004(8) -0.0246(3) 0.060(2) Uani 1 1 d . . .
H10A H 0.4532 0.1053 -0.0068 0.072 Uiso 1 1 calc R . .
C11A C 0.4889(4) 0.2251(9) -0.0723(4) 0.063(3) Uani 1 1 d . . .
H11A H 0.5173 0.1465 -0.0878 0.076 Uiso 1 1 calc R . .
C12A C 0.4852(4) 0.3587(9) -0.0965(3) 0.059(2) Uani 1 1 d . . .
H12A H 0.5075 0.3761 -0.1288 0.070 Uiso 1 1 d R . .
C13A C 0.4442(4) 0.4818(9) -0.0750(3) 0.049(2) Uani 1 1 d . . .
C14A C 0.4412(4) 0.6250(9) -0.1036(3) 0.049(2) Uani 1 1 d . . .
C15A C 0.4022(4) 0.7553(9) -0.0849(3) 0.047(2) Uani 1 1 d . . .
C16A C 0.4017(4) 0.8855(8) -0.1186(3) 0.053(2) Uani 1 1 d . . .
H16A H 0.3747 0.9710 -0.1068 0.063 Uiso 1 1 calc R . .
C17A C 0.4369(4) 0.8950(9) -0.1659(3) 0.061(2) Uani 1 1 d . . .
H17A H 0.4355 0.9851 -0.1869 0.073 Uiso 1 1 calc R . .
C18A C 0.4763(4) 0.7670(11) -0.1839(3) 0.067(2) Uani 1 1 d . . .
H18A H 0.5020 0.7706 -0.2173 0.081 Uiso 1 1 calc R . .
C19A C 0.4771(4) 0.6417(9) -0.1540(4) 0.065(2) Uani 1 1 d D . .
H19A H 0.4986 0.5647 -0.1651 0.078 Uiso 1 1 d RD . .
C20A C 0.1662(5) 0.4029(9) 0.2593(4) 0.077(3) Uani 1 1 d . . .
H20A H 0.2011 0.3516 0.2872 0.093 Uiso 1 1 calc R . .
C21A C 0.0923(4) 0.3111(8) 0.2560(3) 0.073(3) Uani 1 1 d . . .
H21D H 0.0674 0.3196 0.2909 0.109 Uiso 1 1 calc R . .
H21E H 0.1040 0.2055 0.2490 0.109 Uiso 1 1 calc R . .
H21F H 0.0586 0.3497 0.2259 0.109 Uiso 1 1 calc R . .
C22A C 0.1530(7) 0.5455(13) 0.2802(5) 0.183(7) Uani 1 1 d . . .
H22D H 0.2006 0.5875 0.2960 0.275 Uiso 1 1 calc R . .
H22E H 0.1162 0.5386 0.3090 0.275 Uiso 1 1 calc R . .
H22F H 0.1327 0.6106 0.2504 0.275 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 N3 1.934(5) . ?
Pd1 N2 1.976(5) . ?
Pd1 N1 2.022(5) . ?
Pd1 Cl1 2.2971(18) . ?
N1 C7 1.297(7) . ?
N1 C1 1.439(8) . ?
N2 C13 1.361(8) . ?
N2 C9 1.372(7) . ?
N3 C15 1.335(8) . ?
N3 H3C 0.8800 . ?
C1 C2 1.364(8) . ?
C1 C6 1.387(8) . ?
C2 C3 1.386(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(8) . ?
C4 C20 1.503(9) . ?
C5 C6 1.354(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C9 1.452(9) . ?
C7 C8 1.504(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.373(8) . ?
C10 C11 1.385(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.359(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.436(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.448(9) . ?
C14 C19 1.365(8) . ?
C14 C15 1.446(8) . ?
C15 C16 1.439(8) . ?
C16 C17 1.363(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(9) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.520(8) . ?
C20 C21 1.534(8) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Pd1A N3A 1.931(6) . ?
Pd1A N2A 1.984(5) . ?
Pd1A N1A 2.035(6) . ?
Pd1A Cl1A 2.2931(18) . ?
N1A C7A 1.298(7) . ?
N1A C1A 1.420(8) . ?
N2A C13A 1.349(9) . ?
N2A C9A 1.377(8) . ?
N3A C15A 1.334(8) . ?
N3A H3B 0.8800 . ?
C1A C6A 1.375(9) . ?
C1A C2A 1.391(8) . ?
C2A C3A 1.364(9) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.390(9) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.378(9) . ?
C4A C20A 1.527(10) . ?
C5A C6A 1.375(9) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C7A C9A 1.449(10) . ?
C7A C8A 1.479(9) . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A C10A 1.363(8) . ?
C10A C11A 1.385(10) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.328(9) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.429(9) . ?
C12A H12A 0.9095 . ?
C13A C14A 1.453(10) . ?
C14A C19A 1.416(10) . ?
C14A C15A 1.437(9) . ?
C15A C16A 1.418(9) . ?
C16A C17A 1.339(9) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.418(10) . ?
C17A H17A 0.9500 . ?
C18A C19A 1.332(10) . ?
C18A H18A 0.9500 . ?
C19A H19A 0.8351 . ?
C20A C22A 1.392(11) . ?
C20A C21A 1.540(9) . ?
C20A H20A 1.0000 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 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
N3 Pd1 N2 93.1(2) . . ?
N3 Pd1 N1 174.4(2) . . ?
N2 Pd1 N1 81.6(2) . . ?
N3 Pd1 Cl1 88.54(16) . . ?
N2 Pd1 Cl1 178.21(17) . . ?
N1 Pd1 Cl1 96.67(16) . . ?
C7 N1 C1 122.0(6) . . ?
C7 N1 Pd1 113.6(5) . . ?
C1 N1 Pd1 124.2(4) . . ?
C13 N2 C9 120.6(6) . . ?
C13 N2 Pd1 126.3(5) . . ?
C9 N2 Pd1 112.9(5) . . ?
C15 N3 Pd1 127.3(5) . . ?
C15 N3 H3C 116.4 . . ?
Pd1 N3 H3C 116.4 . . ?
C2 C1 C6 119.9(7) . . ?
C2 C1 N1 119.6(6) . . ?
C6 C1 N1 120.4(6) . . ?
C1 C2 C3 119.3(7) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 121.5(7) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 117.6(7) . . ?
C3 C4 C20 119.9(6) . . ?
C5 C4 C20 122.3(7) . . ?
C6 C5 C4 121.5(7) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C1 120.1(6) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
N1 C7 C9 116.5(6) . . ?
N1 C7 C8 123.4(7) . . ?
C9 C7 C8 120.0(6) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 122.3(7) . . ?
N2 C9 C7 115.0(6) . . ?
C10 C9 C7 122.7(7) . . ?
C9 C10 C11 118.2(7) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C12 C11 C10 120.4(7) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.9(7) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
N2 C13 C12 117.4(6) . . ?
N2 C13 C14 123.6(6) . . ?
C12 C13 C14 118.9(7) . . ?
C19 C14 C15 117.0(6) . . ?
C19 C14 C13 119.9(7) . . ?
C15 C14 C13 123.1(6) . . ?
N3 C15 C16 117.5(6) . . ?
N3 C15 C14 125.0(6) . . ?
C16 C15 C14 117.6(7) . . ?
C17 C16 C15 122.0(7) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C16 C17 C18 119.8(7) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 118.9(7) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C14 C19 C18 124.6(7) . . ?
C14 C19 H19 117.7 . . ?
C18 C19 H19 117.7 . . ?
C4 C20 C22 110.3(6) . . ?
C4 C20 C21 112.7(5) . . ?
C22 C20 C21 110.4(6) . . ?
C4 C20 H20 107.8 . . ?
C22 C20 H20 107.8 . . ?
C21 C20 H20 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3A Pd1A N2A 92.2(3) . . ?
N3A Pd1A N1A 174.0(2) . . ?
N2A Pd1A N1A 82.2(3) . . ?
N3A Pd1A Cl1A 89.14(17) . . ?
N2A Pd1A Cl1A 175.39(15) . . ?
N1A Pd1A Cl1A 96.57(17) . . ?
C7A N1A C1A 121.8(6) . . ?
C7A N1A Pd1A 112.5(6) . . ?
C1A N1A Pd1A 125.5(4) . . ?
C13A N2A C9A 120.4(6) . . ?
C13A N2A Pd1A 127.3(5) . . ?
C9A N2A Pd1A 112.2(5) . . ?
C15A N3A Pd1A 129.0(5) . . ?
C15A N3A H3B 115.5 . . ?
Pd1A N3A H3B 115.5 . . ?
C6A C1A C2A 118.3(7) . . ?
C6A C1A N1A 122.1(6) . . ?
C2A C1A N1A 119.6(7) . . ?
C3A C2A C1A 119.5(7) . . ?
C3A C2A H2A 120.2 . . ?
C1A C2A H2A 120.2 . . ?
C2A C3A C4A 123.7(7) . . ?
C2A C3A H3A 118.2 . . ?
C4A C3A H3A 118.2 . . ?
C5A C4A C3A 115.1(8) . . ?
C5A C4A C20A 125.7(7) . . ?
C3A C4A C20A 119.2(7) . . ?
C6A C5A C4A 122.9(7) . . ?
C6A C5A H5A 118.6 . . ?
C4A C5A H5A 118.6 . . ?
C1A C6A C5A 120.5(7) . . ?
C1A C6A H6A 119.7 . . ?
C5A C6A H6A 119.7 . . ?
N1A C7A C9A 117.5(7) . . ?
N1A C7A C8A 123.3(7) . . ?
C9A C7A C8A 119.2(6) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10A C9A N2A 122.4(8) . . ?
C10A C9A C7A 122.1(8) . . ?
N2A C9A C7A 115.5(6) . . ?
C9A C10A C11A 118.0(8) . . ?
C9A C10A H10A 121.0 . . ?
C11A C10A H10A 121.0 . . ?
C12A C11A C10A 119.9(7) . . ?
C12A C11A H11A 120.1 . . ?
C10A C11A H11A 120.1 . . ?
C11A C12A C13A 122.7(8) . . ?
C11A C12A H12A 121.4 . . ?
C13A C12A H12A 115.9 . . ?
N2A C13A C12A 116.6(8) . . ?
N2A C13A C14A 123.1(7) . . ?
C12A C13A C14A 120.3(8) . . ?
C19A C14A C15A 115.7(7) . . ?
C19A C14A C13A 119.9(7) . . ?
C15A C14A C13A 124.4(7) . . ?
N3A C15A C16A 118.2(7) . . ?
N3A C15A C14A 123.9(8) . . ?
C16A C15A C14A 117.9(7) . . ?
C17A C16A C15A 123.8(7) . . ?
C17A C16A H16A 118.1 . . ?
C15A C16A H16A 118.1 . . ?
C16A C17A C18A 118.2(8) . . ?
C16A C17A H17A 120.9 . . ?
C18A C17A H17A 120.9 . . ?
C19A C18A C17A 119.9(8) . . ?
C19A C18A H18A 120.1 . . ?
C17A C18A H18A 120.1 . . ?
C18A C19A C14A 124.5(8) . . ?
C18A C19A H19A 120.3 . . ?
C14A C19A H19A 115.1 . . ?
C22A C20A C4A 112.9(8) . . ?
C22A C20A C21A 110.2(8) . . ?
C4A C20A C21A 114.1(7) . . ?
C22A C20A H20A 106.3 . . ?
C4A C20A H20A 106.3 . . ?
C21A C20A H20A 106.3 . . ?
C20A C21A H21D 109.5 . . ?
C20A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C20A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C20A C22A H22D 109.5 . . ?
C20A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C20A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 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
N2 Pd1 N1 C7 4.6(4) . . . . ?
Cl1 Pd1 N1 C7 -174.8(4) . . . . ?
N2 Pd1 N1 C1 179.4(5) . . . . ?
Cl1 Pd1 N1 C1 0.0(5) . . . . ?
N3 Pd1 N2 C13 -2.3(5) . . . . ?
N1 Pd1 N2 C13 179.6(5) . . . . ?
N3 Pd1 N2 C9 173.0(4) . . . . ?
N1 Pd1 N2 C9 -5.1(4) . . . . ?
N2 Pd1 N3 C15 10.4(5) . . . . ?
Cl1 Pd1 N3 C15 -170.2(5) . . . . ?
C7 N1 C1 C2 -113.6(7) . . . . ?
Pd1 N1 C1 C2 72.0(7) . . . . ?
C7 N1 C1 C6 69.4(8) . . . . ?
Pd1 N1 C1 C6 -105.0(6) . . . . ?
C6 C1 C2 C3 0.1(10) . . . . ?
N1 C1 C2 C3 -176.9(6) . . . . ?
C1 C2 C3 C4 2.3(11) . . . . ?
C2 C3 C4 C5 -3.1(10) . . . . ?
C2 C3 C4 C20 172.6(6) . . . . ?
C3 C4 C5 C6 1.7(10) . . . . ?
C20 C4 C5 C6 -173.9(6) . . . . ?
C4 C5 C6 C1 0.7(11) . . . . ?
C2 C1 C6 C5 -1.6(10) . . . . ?
N1 C1 C6 C5 175.5(6) . . . . ?
C1 N1 C7 C9 -178.1(5) . . . . ?
Pd1 N1 C7 C9 -3.2(7) . . . . ?
C1 N1 C7 C8 1.5(9) . . . . ?
Pd1 N1 C7 C8 176.5(4) . . . . ?
C13 N2 C9 C10 1.0(9) . . . . ?
Pd1 N2 C9 C10 -174.5(5) . . . . ?
C13 N2 C9 C7 -179.5(5) . . . . ?
Pd1 N2 C9 C7 4.9(6) . . . . ?
N1 C7 C9 N2 -1.2(8) . . . . ?
C8 C7 C9 N2 179.2(5) . . . . ?
N1 C7 C9 C10 178.3(6) . . . . ?
C8 C7 C9 C10 -1.3(9) . . . . ?
N2 C9 C10 C11 1.5(9) . . . . ?
C7 C9 C10 C11 -177.9(6) . . . . ?
C9 C10 C11 C12 -2.1(10) . . . . ?
C10 C11 C12 C13 0.3(10) . . . . ?
C9 N2 C13 C12 -2.9(8) . . . . ?
Pd1 N2 C13 C12 172.1(4) . . . . ?
C9 N2 C13 C14 177.1(5) . . . . ?
Pd1 N2 C13 C14 -8.0(8) . . . . ?
C11 C12 C13 N2 2.2(9) . . . . ?
C11 C12 C13 C14 -177.7(6) . . . . ?
N2 C13 C14 C19 -165.9(6) . . . . ?
C12 C13 C14 C19 14.0(9) . . . . ?
N2 C13 C14 C15 13.0(9) . . . . ?
C12 C13 C14 C15 -167.0(6) . . . . ?
Pd1 N3 C15 C16 170.4(4) . . . . ?
Pd1 N3 C15 C14 -8.5(9) . . . . ?
C19 C14 C15 N3 174.5(6) . . . . ?
C13 C14 C15 N3 -4.5(10) . . . . ?
C19 C14 C15 C16 -4.5(8) . . . . ?
C13 C14 C15 C16 176.6(5) . . . . ?
N3 C15 C16 C17 -176.4(6) . . . . ?
C14 C15 C16 C17 2.6(9) . . . . ?
C15 C16 C17 C18 -0.6(10) . . . . ?
C16 C17 C18 C19 0.3(10) . . . . ?
C15 C14 C19 C18 4.6(10) . . . . ?
C13 C14 C19 C18 -176.4(6) . . . . ?
C17 C18 C19 C14 -2.5(11) . . . . ?
C3 C4 C20 C22 -90.8(8) . . . . ?
C5 C4 C20 C22 84.7(8) . . . . ?
C3 C4 C20 C21 145.4(6) . . . . ?
C5 C4 C20 C21 -39.1(9) . . . . ?
N2A Pd1A N1A C7A 0.7(4) . . . . ?
Cl1A Pd1A N1A C7A -174.8(4) . . . . ?
N2A Pd1A N1A C1A -175.7(5) . . . . ?
Cl1A Pd1A N1A C1A 8.8(5) . . . . ?
N3A Pd1A N2A C13A 3.3(5) . . . . ?
N1A Pd1A N2A C13A -179.1(6) . . . . ?
N3A Pd1A N2A C9A -179.1(4) . . . . ?
N1A Pd1A N2A C9A -1.5(4) . . . . ?
N2A Pd1A N3A C15A -0.8(6) . . . . ?
Cl1A Pd1A N3A C15A 174.8(6) . . . . ?
C7A N1A C1A C6A -66.7(9) . . . . ?
Pd1A N1A C1A C6A 109.3(6) . . . . ?
C7A N1A C1A C2A 112.9(7) . . . . ?
Pd1A N1A C1A C2A -71.1(7) . . . . ?
C6A C1A C2A C3A 0.8(11) . . . . ?
N1A C1A C2A C3A -178.8(7) . . . . ?
C1A C2A C3A C4A -0.2(12) . . . . ?
C2A C3A C4A C5A -1.0(11) . . . . ?
C2A C3A C4A C20A 178.1(8) . . . . ?
C3A C4A C5A C6A 1.6(10) . . . . ?
C20A C4A C5A C6A -177.5(7) . . . . ?
C2A C1A C6A C5A -0.3(10) . . . . ?
N1A C1A C6A C5A 179.3(6) . . . . ?
C4A C5A C6A C1A -1.0(11) . . . . ?
C1A N1A C7A C9A 176.7(6) . . . . ?
Pd1A N1A C7A C9A 0.2(7) . . . . ?
C1A N1A C7A C8A -5.5(10) . . . . ?
Pd1A N1A C7A C8A 178.0(5) . . . . ?
C13A N2A C9A C10A 0.8(10) . . . . ?
Pd1A N2A C9A C10A -177.0(5) . . . . ?
C13A N2A C9A C7A 179.8(6) . . . . ?
Pd1A N2A C9A C7A 2.0(7) . . . . ?
N1A C7A C9A C10A 177.5(6) . . . . ?
C8A C7A C9A C10A -0.4(10) . . . . ?
N1A C7A C9A N2A -1.5(9) . . . . ?
C8A C7A C9A N2A -179.4(6) . . . . ?
N2A C9A C10A C11A -0.5(10) . . . . ?
C7A C9A C10A C11A -179.5(6) . . . . ?
C9A C10A C11A C12A -0.2(11) . . . . ?
C10A C11A C12A C13A 0.8(11) . . . . ?
C9A N2A C13A C12A -0.3(9) . . . . ?
Pd1A N2A C13A C12A 177.1(4) . . . . ?
C9A N2A C13A C14A 178.3(6) . . . . ?
Pd1A N2A C13A C14A -4.3(9) . . . . ?
C11A C12A C13A N2A -0.5(10) . . . . ?
C11A C12A C13A C14A -179.1(6) . . . . ?
N2A C13A C14A C19A -176.6(6) . . . . ?
C12A C13A C14A C19A 1.8(9) . . . . ?
N2A C13A C14A C15A 2.2(10) . . . . ?
C12A C13A C14A C15A -179.3(6) . . . . ?
Pd1A N3A C15A C16A 177.2(4) . . . . ?
Pd1A N3A C15A C14A -0.7(10) . . . . ?
C19A C14A C15A N3A 179.3(6) . . . . ?
C13A C14A C15A N3A 0.5(10) . . . . ?
C19A C14A C15A C16A 1.4(9) . . . . ?
C13A C14A C15A C16A -177.4(6) . . . . ?
N3A C15A C16A C17A -179.7(7) . . . . ?
C14A C15A C16A C17A -1.7(10) . . . . ?
C15A C16A C17A C18A 0.8(11) . . . . ?
C16A C17A C18A C19A 0.3(11) . . . . ?
C17A C18A C19A C14A -0.5(12) . . . . ?
C15A C14A C19A C18A -0.4(11) . . . . ?
C13A C14A C19A C18A 178.5(7) . . . . ?
C5A C4A C20A C22A -128.1(10) . . . . ?
C3A C4A C20A C22A 52.9(12) . . . . ?
C5A C4A C20A C21A -1.3(11) . . . . ?
C3A C4A C20A C21A 179.7(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3A H3B Cl1 0.88 2.84 3.665(6) 157.0 3_675
N3 H3C Cl1A 0.88 2.73 3.585(5) 163.5 3_675

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_10012
_database_code_depnum_ccdc_archive 'CCDC 1043194'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H28 Cl N3 Pd, C H Cl3'
_chemical_formula_sum            'C26 H29 Cl4 N3 Pd'
_chemical_formula_weight         631.72

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'
Pd Pd -0.9988 1.0072 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.410(8)
_cell_length_b                   17.663(13)
_cell_length_c                   12.991(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.182(13)
_cell_angle_gamma                90.00
_cell_volume                     2611(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    936
_cell_measurement_theta_min      2.294
_cell_measurement_theta_max      25.767

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 9749 reflections(SADABS);Rint 0.1508 before
correction and 0.0573 after.
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19939
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5116
_reflns_number_gt                4146
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0403P)²+0.0000P] 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         5116
_refine_ls_number_parameters     312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0904
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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 0.91850(2) 0.102569(15) 0.78027(2) 0.01880(10) Uani 1 1 d . . .
Cl1 Cl 0.86114(9) 0.22334(5) 0.72980(8) 0.0289(2) Uani 1 1 d . . .
N1 N 0.7940(3) 0.04492(17) 0.6932(2) 0.0197(7) Uani 1 1 d . . .
N2 N 0.9682(3) -0.00154(16) 0.8218(2) 0.0183(7) Uani 1 1 d . . .
N3 N 1.0398(3) 0.14721(18) 0.8719(3) 0.0286(8) Uani 1 1 d . . .
H3A H 1.0335 0.1962 0.8821 0.034 Uiso 1 1 calc R . .
C1 C 0.7079(3) 0.0785(2) 0.6196(3) 0.0209(8) Uani 1 1 d . . .
C2 C 0.7382(3) 0.0898(2) 0.5185(3) 0.0275(9) Uani 1 1 d . . .
C3 C 0.6566(4) 0.1243(2) 0.4498(3) 0.0303(10) Uani 1 1 d . . .
H3 H 0.6755 0.1331 0.3808 0.036 Uiso 1 1 calc R . .
C4 C 0.5477(4) 0.1464(2) 0.4798(3) 0.0301(10) Uani 1 1 d . . .
H4 H 0.4928 0.1703 0.4318 0.036 Uiso 1 1 calc R . .
C5 C 0.5196(4) 0.1335(2) 0.5796(3) 0.0257(9) Uani 1 1 d . . .
H5 H 0.4445 0.1483 0.5997 0.031 Uiso 1 1 calc R . .
C6 C 0.5987(3) 0.0993(2) 0.6515(3) 0.0242(9) Uani 1 1 d . . .
C7 C 0.7960(3) -0.0271(2) 0.7096(3) 0.0214(8) Uani 1 1 d . . .
C8 C 0.7086(4) -0.0810(2) 0.6590(3) 0.0328(10) Uani 1 1 d . . .
H8A H 0.6540 -0.0532 0.6110 0.049 Uiso 1 1 calc R . .
H8B H 0.6647 -0.1056 0.7118 0.049 Uiso 1 1 calc R . .
H8C H 0.7498 -0.1195 0.6211 0.049 Uiso 1 1 calc R . .
C9 C 0.8909(3) -0.0551(2) 0.7811(3) 0.0200(8) Uani 1 1 d . . .
C10 C 0.9051(3) -0.1307(2) 0.8026(3) 0.0250(9) Uani 1 1 d . . .
H10 H 0.8516 -0.1672 0.7728 0.030 Uiso 1 1 calc R . .
C11 C 0.9997(4) -0.1523(2) 0.8689(3) 0.0315(10) Uani 1 1 d . . .
H11 H 1.0110 -0.2041 0.8863 0.038 Uiso 1 1 calc R . .
C12 C 1.0768(3) -0.0992(2) 0.9094(3) 0.0275(9) Uani 1 1 d . . .
H12 H 1.1309 -0.1174 0.9586 0.033 Uiso 1 1 d R . .
C13 C 1.0620(3) -0.0217(2) 0.8856(3) 0.0213(8) Uani 1 1 d . . .
C14 C 1.1469(3) 0.0338(2) 0.9305(3) 0.0214(8) Uani 1 1 d . . .
C15 C 1.1321(3) 0.1136(2) 0.9220(3) 0.0224(8) Uani 1 1 d . . .
C16 C 1.2198(3) 0.1611(2) 0.9731(3) 0.0280(9) Uani 1 1 d . . .
H16 H 1.2099 0.2144 0.9697 0.034 Uiso 1 1 calc R . .
C17 C 1.3168(4) 0.1325(2) 1.0264(3) 0.0288(9) Uani 1 1 d . . .
H17 H 1.3730 0.1658 1.0594 0.035 Uiso 1 1 calc R . .
C18 C 1.3343(3) 0.0544(2) 1.0328(3) 0.0293(10) Uani 1 1 d . . .
H18 H 1.4032 0.0342 1.0679 0.035 Uiso 1 1 calc R . .
C19 C 1.2498(3) 0.0076(2) 0.9873(3) 0.0259(9) Uani 1 1 d . . .
H19 H 1.2645 -0.0486 0.9936 0.031 Uiso 1 1 d R . .
C20 C 0.8553(4) 0.0654(3) 0.4824(3) 0.0403(12) Uani 1 1 d . . .
H20 H 0.9008 0.0413 0.5423 0.048 Uiso 1 1 calc R . .
C21 C 0.8409(5) 0.0066(3) 0.3967(4) 0.0592(15) Uani 1 1 d . . .
H21A H 0.7937 -0.0357 0.4193 0.089 Uiso 1 1 calc R . .
H21B H 0.9185 -0.0119 0.3806 0.089 Uiso 1 1 calc R . .
H21C H 0.8014 0.0297 0.3349 0.089 Uiso 1 1 calc R . .
C22 C 0.9268(5) 0.1330(4) 0.4483(5) 0.0681(17) Uani 1 1 d . . .
H22A H 0.8858 0.1569 0.3878 0.102 Uiso 1 1 calc R . .
H22B H 1.0044 0.1156 0.4306 0.102 Uiso 1 1 calc R . .
H22C H 0.9361 0.1699 0.5047 0.102 Uiso 1 1 calc R . .
C23 C 0.5652(4) 0.0858(2) 0.7605(3) 0.0315(10) Uani 1 1 d . . .
H23 H 0.6280 0.0542 0.7969 0.038 Uiso 1 1 calc R . .
C24 C 0.5581(4) 0.1604(3) 0.8188(4) 0.0514(14) Uani 1 1 d . . .
H24A H 0.6347 0.1858 0.8215 0.077 Uiso 1 1 calc R . .
H24B H 0.5366 0.1504 0.8892 0.077 Uiso 1 1 calc R . .
H24C H 0.4986 0.1930 0.7833 0.077 Uiso 1 1 calc R . .
C25 C 0.4485(4) 0.0425(3) 0.7613(4) 0.0395(11) Uani 1 1 d . . .
H25A H 0.3852 0.0731 0.7275 0.059 Uiso 1 1 calc R . .
H25B H 0.4312 0.0323 0.8328 0.059 Uiso 1 1 calc R . .
H25C H 0.4547 -0.0054 0.7242 0.059 Uiso 1 1 calc R . .
C26 C 0.6517(4) 0.2437(2) 0.1397(3) 0.0338(10) Uani 1 1 d . . .
H26 H 0.5781 0.2740 0.1430 0.041 Uiso 1 1 calc R . .
Cl2 Cl 0.61813(10) 0.14752(6) 0.15192(9) 0.0403(3) Uani 1 1 d . . .
Cl3 Cl 0.71100(12) 0.26047(7) 0.02009(10) 0.0529(3) Uani 1 1 d . . .
Cl4 Cl 0.75258(12) 0.27219(8) 0.23912(10) 0.0545(4) 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 N3 1.927(3) . ?
Pd1 N2 1.987(3) . ?
Pd1 N1 2.025(3) . ?
Pd1 Cl1 2.3123(17) . ?
N1 C7 1.289(5) . ?
N1 C1 1.447(4) . ?
N2 C13 1.353(5) . ?
N2 C9 1.373(5) . ?
N3 C15 1.336(5) . ?
N3 H3A 0.8800 . ?
C1 C6 1.390(5) . ?
C1 C2 1.397(5) . ?
C2 C3 1.385(5) . ?
C2 C20 1.510(6) . ?
C3 C4 1.384(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(5) . ?
C5 H5 0.9500 . ?
C6 C23 1.512(6) . ?
C7 C9 1.461(5) . ?
C7 C8 1.496(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.371(5) . ?
C10 C11 1.385(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.365(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.410(5) . ?
C12 H12 0.9140 . ?
C13 C14 1.469(5) . ?
C14 C19 1.418(5) . ?
C14 C15 1.424(5) . ?
C15 C16 1.431(5) . ?
C16 C17 1.359(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.372(5) . ?
C18 H18 0.9500 . ?
C19 H19 1.0083 . ?
C20 C21 1.523(7) . ?
C20 C22 1.530(7) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.526(6) . ?
C23 C25 1.536(6) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 Cl4 1.741(5) . ?
C26 Cl2 1.751(4) . ?
C26 Cl3 1.764(5) . ?
C26 H26 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Pd1 N2 91.91(13) . . ?
N3 Pd1 N1 173.63(13) . . ?
N2 Pd1 N1 82.01(13) . . ?
N3 Pd1 Cl1 88.47(10) . . ?
N2 Pd1 Cl1 179.27(9) . . ?
N1 Pd1 Cl1 97.63(10) . . ?
C7 N1 C1 121.1(3) . . ?
C7 N1 Pd1 113.6(3) . . ?
C1 N1 Pd1 125.3(2) . . ?
C13 N2 C9 120.7(3) . . ?
C13 N2 Pd1 127.4(3) . . ?
C9 N2 Pd1 111.8(2) . . ?
C15 N3 Pd1 128.6(3) . . ?
C15 N3 H3A 115.7 . . ?
Pd1 N3 H3A 115.7 . . ?
C6 C1 C2 122.1(4) . . ?
C6 C1 N1 119.4(3) . . ?
C2 C1 N1 118.4(3) . . ?
C3 C2 C1 117.9(4) . . ?
C3 C2 C20 119.6(4) . . ?
C1 C2 C20 122.5(4) . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 117.8(4) . . ?
C5 C6 C23 120.1(3) . . ?
C1 C6 C23 122.1(3) . . ?
N1 C7 C9 116.3(3) . . ?
N1 C7 C8 123.5(3) . . ?
C9 C7 C8 120.2(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 122.0(3) . . ?
C10 C9 C7 122.1(3) . . ?
N2 C9 C7 115.9(3) . . ?
C9 C10 C11 118.0(4) . . ?
C9 C10 H10 121.0 . . ?
C11 C10 H10 121.0 . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 121.2(4) . . ?
C11 C12 H12 114.2 . . ?
C13 C12 H12 124.0 . . ?
N2 C13 C12 117.9(3) . . ?
N2 C13 C14 122.4(3) . . ?
C12 C13 C14 119.7(4) . . ?
C19 C14 C15 116.9(3) . . ?
C19 C14 C13 119.0(3) . . ?
C15 C14 C13 124.0(3) . . ?
N3 C15 C14 124.2(3) . . ?
N3 C15 C16 117.8(3) . . ?
C14 C15 C16 118.0(3) . . ?
C17 C16 C15 122.3(4) . . ?
C17 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C16 C17 C18 120.4(4) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 118.5(4) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C18 C19 C14 123.8(4) . . ?
C18 C19 H19 116.8 . . ?
C14 C19 H19 119.4 . . ?
C2 C20 C21 111.8(4) . . ?
C2 C20 C22 111.7(4) . . ?
C21 C20 C22 110.6(4) . . ?
C2 C20 H20 107.5 . . ?
C21 C20 H20 107.5 . . ?
C22 C20 H20 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C6 C23 C24 110.8(4) . . ?
C6 C23 C25 111.3(4) . . ?
C24 C23 C25 110.4(3) . . ?
C6 C23 H23 108.1 . . ?
C24 C23 H23 108.1 . . ?
C25 C23 H23 108.1 . . ?
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 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Cl4 C26 Cl2 110.5(2) . . ?
Cl4 C26 Cl3 109.2(2) . . ?
Cl2 C26 Cl3 110.1(2) . . ?
Cl4 C26 H26 109.0 . . ?
Cl2 C26 H26 109.0 . . ?
Cl3 C26 H26 109.0 . . ?

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
N2 Pd1 N1 C7 5.6(3) . . . . ?
Cl1 Pd1 N1 C7 -175.0(2) . . . . ?
N2 Pd1 N1 C1 -175.3(3) . . . . ?
Cl1 Pd1 N1 C1 4.1(3) . . . . ?
N3 Pd1 N2 C13 -4.8(3) . . . . ?
N1 Pd1 N2 C13 177.1(3) . . . . ?
N3 Pd1 N2 C9 172.3(2) . . . . ?
N1 Pd1 N2 C9 -5.8(2) . . . . ?
N2 Pd1 N3 C15 12.3(4) . . . . ?
Cl1 Pd1 N3 C15 -167.1(3) . . . . ?
C7 N1 C1 C6 87.1(4) . . . . ?
Pd1 N1 C1 C6 -92.0(4) . . . . ?
C7 N1 C1 C2 -93.6(4) . . . . ?
Pd1 N1 C1 C2 87.4(4) . . . . ?
C6 C1 C2 C3 1.5(6) . . . . ?
N1 C1 C2 C3 -177.8(3) . . . . ?
C6 C1 C2 C20 -178.2(4) . . . . ?
N1 C1 C2 C20 2.5(6) . . . . ?
C1 C2 C3 C4 -0.7(6) . . . . ?
C20 C2 C3 C4 179.1(4) . . . . ?
C2 C3 C4 C5 -0.3(6) . . . . ?
C3 C4 C5 C6 0.6(6) . . . . ?
C4 C5 C6 C1 0.2(6) . . . . ?
C4 C5 C6 C23 -180.0(4) . . . . ?
C2 C1 C6 C5 -1.3(6) . . . . ?
N1 C1 C6 C5 178.0(3) . . . . ?
C2 C1 C6 C23 178.9(4) . . . . ?
N1 C1 C6 C23 -1.8(5) . . . . ?
C1 N1 C7 C9 176.7(3) . . . . ?
Pd1 N1 C7 C9 -4.2(4) . . . . ?
C1 N1 C7 C8 -2.7(5) . . . . ?
Pd1 N1 C7 C8 176.4(3) . . . . ?
C13 N2 C9 C10 -0.3(5) . . . . ?
Pd1 N2 C9 C10 -177.6(3) . . . . ?
C13 N2 C9 C7 -177.3(3) . . . . ?
Pd1 N2 C9 C7 5.4(4) . . . . ?
N1 C7 C9 C10 -177.9(3) . . . . ?
C8 C7 C9 C10 1.6(5) . . . . ?
N1 C7 C9 N2 -0.8(5) . . . . ?
C8 C7 C9 N2 178.6(3) . . . . ?
N2 C9 C10 C11 1.2(6) . . . . ?
C7 C9 C10 C11 178.0(3) . . . . ?
C9 C10 C11 C12 -1.2(6) . . . . ?
C10 C11 C12 C13 0.4(6) . . . . ?
C9 N2 C13 C12 -0.5(5) . . . . ?
Pd1 N2 C13 C12 176.3(3) . . . . ?
C9 N2 C13 C14 179.8(3) . . . . ?
Pd1 N2 C13 C14 -3.4(5) . . . . ?
C11 C12 C13 N2 0.5(6) . . . . ?
C11 C12 C13 C14 -179.8(3) . . . . ?
N2 C13 C14 C19 -173.1(3) . . . . ?
C12 C13 C14 C19 7.2(5) . . . . ?
N2 C13 C14 C15 8.0(6) . . . . ?
C12 C13 C14 C15 -171.7(4) . . . . ?
Pd1 N3 C15 C14 -11.5(6) . . . . ?
Pd1 N3 C15 C16 170.5(3) . . . . ?
C19 C14 C15 N3 -179.4(3) . . . . ?
C13 C14 C15 N3 -0.4(6) . . . . ?
C19 C14 C15 C16 -1.5(5) . . . . ?
C13 C14 C15 C16 177.5(3) . . . . ?
N3 C15 C16 C17 179.8(4) . . . . ?
C14 C15 C16 C17 1.7(6) . . . . ?
C15 C16 C17 C18 0.1(6) . . . . ?
C16 C17 C18 C19 -2.2(6) . . . . ?
C17 C18 C19 C14 2.4(6) . . . . ?
C15 C14 C19 C18 -0.6(6) . . . . ?
C13 C14 C19 C18 -179.6(4) . . . . ?
C3 C2 C20 C21 -61.5(6) . . . . ?
C1 C2 C20 C21 118.2(5) . . . . ?
C3 C2 C20 C22 63.1(5) . . . . ?
C1 C2 C20 C22 -117.2(5) . . . . ?
C5 C6 C23 C24 -70.0(5) . . . . ?
C1 C6 C23 C24 109.8(4) . . . . ?
C5 C6 C23 C25 53.3(5) . . . . ?
C1 C6 C23 C25 -126.9(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.551
_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_11054
_database_code_depnum_ccdc_archive 'CCDC 1043195'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H27 N3 Pd'
_chemical_formula_sum            'C28 H27 N3 Pd'
_chemical_formula_weight         511.93

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   17.244(11)
_cell_length_b                   11.142(8)
_cell_length_c                   12.238(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.925(14)
_cell_angle_gamma                90.00
_cell_volume                     2261(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    743
_cell_measurement_theta_min      2.514
_cell_measurement_theta_max      28.551

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   
;
absorption correction based on 2521 reflections(SADABS);Rint 0.1195 before
correction and 0.0605 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17292
_diffrn_reflns_av_R_equivalents  0.2311
_diffrn_reflns_av_sigmaI/netI    0.2269
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4444
_reflns_number_gt                2190
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0306P)²+0.0000P] 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         4444
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1615
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.1450
_refine_ls_wR_factor_gt          0.1210
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_restrained_S_all      0.867
_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 0.13239(4) 0.47249(6) 0.21394(5) 0.0290(2) Uani 1 1 d . . .
N1 N 0.2079(4) 0.3929(5) 0.1308(5) 0.0251(16) Uani 1 1 d . . .
N2 N 0.0478(4) 0.3756(5) 0.0942(5) 0.0257(16) Uani 1 1 d . . .
N3 N 0.0500(3) 0.5372(6) 0.2775(5) 0.0315(16) Uani 1 1 d . . .
H3A H 0.0663 0.5928 0.3299 0.038 Uiso 1 1 calc R . .
C1 C 0.2918(5) 0.4127(7) 0.1592(7) 0.031(2) Uani 1 1 d . . .
C2 C 0.3379(5) 0.3736(8) 0.2644(7) 0.038(2) Uani 1 1 d . . .
H2 H 0.3138 0.3287 0.3124 0.045 Uiso 1 1 calc R . .
C3 C 0.4186(6) 0.3999(8) 0.2989(7) 0.042(2) Uani 1 1 d . . .
H3 H 0.4500 0.3708 0.3704 0.051 Uiso 1 1 calc R . .
C4 C 0.4563(5) 0.4686(8) 0.2321(8) 0.040(2) Uani 1 1 d . . .
C5 C 0.4080(5) 0.5034(7) 0.1252(7) 0.043(3) Uani 1 1 d . . .
H5 H 0.4320 0.5457 0.0754 0.052 Uiso 1 1 calc R . .
C6 C 0.3280(5) 0.4784(8) 0.0907(7) 0.035(2) Uani 1 1 d . . .
H6 H 0.2965 0.5062 0.0188 0.043 Uiso 1 1 calc R . .
C7 C 0.1683(5) 0.3346(7) 0.0405(6) 0.032(2) Uani 1 1 d . . .
C8 C 0.2117(5) 0.2713(7) -0.0339(7) 0.038(2) Uani 1 1 d . . .
H8A H 0.2694 0.2672 0.0053 0.058 Uiso 1 1 calc R . .
H8B H 0.2039 0.3155 -0.1053 0.058 Uiso 1 1 calc R . .
H8C H 0.1902 0.1898 -0.0501 0.058 Uiso 1 1 calc R . .
C9 C 0.0817(5) 0.3197(7) 0.0185(6) 0.027(2) Uani 1 1 d . . .
C10 C 0.0346(6) 0.2575(7) -0.0731(7) 0.034(2) Uani 1 1 d . . .
H10 H 0.0585 0.2217 -0.1264 0.041 Uiso 1 1 calc R . .
C11 C -0.0472(5) 0.2473(7) -0.0874(6) 0.034(2) Uani 1 1 d . . .
H11 H -0.0803 0.2021 -0.1483 0.040 Uiso 1 1 calc R . .
C12 C -0.0784(5) 0.3037(7) -0.0118(7) 0.033(2) Uani 1 1 d . . .
H12 H -0.1350 0.3001 -0.0222 0.040 Uiso 1 1 calc R . .
C13 C -0.0306(5) 0.3681(6) 0.0826(7) 0.0246(19) Uani 1 1 d . . .
C14 C -0.0693(5) 0.4281(6) 0.1631(6) 0.0226(19) Uani 1 1 d . . .
C15 C -0.0276(5) 0.5094(7) 0.2531(6) 0.028(2) Uani 1 1 d . . .
C16 C -0.0771(5) 0.5649(7) 0.3156(6) 0.036(2) Uani 1 1 d . . .
H16 H -0.0526 0.6222 0.3720 0.043 Uiso 1 1 calc R . .
C17 C -0.1554(5) 0.5413(8) 0.2998(6) 0.035(2) Uani 1 1 d . . .
H17 H -0.1850 0.5824 0.3432 0.042 Uiso 1 1 calc R . .
C18 C -0.1932(5) 0.4563(8) 0.2196(7) 0.036(2) Uani 1 1 d . . .
H18 H -0.2481 0.4360 0.2108 0.043 Uiso 1 1 calc R . .
C19 C -0.1516(5) 0.4031(7) 0.1546(6) 0.030(2) Uani 1 1 d . . .
H19 H -0.1787 0.3457 0.1000 0.036 Uiso 1 1 calc R . .
C20 C 0.5431(6) 0.5045(9) 0.2794(8) 0.059(3) Uani 1 1 d . . .
H20 H 0.5730 0.4329 0.3190 0.071 Uiso 1 1 calc R . .
C21 C 0.5847(6) 0.5449(10) 0.1897(9) 0.078(4) Uani 1 1 d . . .
H21A H 0.5813 0.4805 0.1340 0.118 Uiso 1 1 calc R . .
H21B H 0.6414 0.5630 0.2267 0.118 Uiso 1 1 calc R . .
H21C H 0.5578 0.6168 0.1511 0.118 Uiso 1 1 calc R . .
C22 C 0.5522(6) 0.6034(11) 0.3663(9) 0.098(5) Uani 1 1 d . . .
H22A H 0.5283 0.6775 0.3285 0.147 Uiso 1 1 calc R . .
H22B H 0.6096 0.6166 0.4035 0.147 Uiso 1 1 calc R . .
H22C H 0.5247 0.5804 0.4233 0.147 Uiso 1 1 calc R . .
C23 C 0.2142(5) 0.5709(7) 0.3282(7) 0.027(2) Uani 1 1 d . . .
C24 C 0.2169(5) 0.5706(7) 0.4405(7) 0.038(2) Uani 1 1 d . . .
H24 H 0.1786 0.5249 0.4657 0.045 Uiso 1 1 calc R . .
C25 C 0.2762(6) 0.6374(8) 0.5199(8) 0.050(3) Uani 1 1 d . . .
H25 H 0.2778 0.6343 0.5981 0.060 Uiso 1 1 calc R . .
C26 C 0.3309(6) 0.7061(9) 0.4872(9) 0.051(3) Uani 1 1 d . . .
H26 H 0.3701 0.7515 0.5412 0.061 Uiso 1 1 calc R . .
C27 C 0.3283(5) 0.7082(8) 0.3760(10) 0.052(3) Uani 1 1 d . . .
H27 H 0.3663 0.7552 0.3514 0.063 Uiso 1 1 calc R . .
C28 C 0.2700(5) 0.6416(7) 0.2963(8) 0.043(3) Uani 1 1 d . . .
H28 H 0.2690 0.6454 0.2184 0.052 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 N3 1.937(6) . ?
Pd1 C23 2.016(8) . ?
Pd1 N1 2.060(6) . ?
Pd1 N2 2.066(6) . ?
N1 C7 1.302(9) . ?
N1 C1 1.409(9) . ?
N2 C13 1.324(9) . ?
N2 C9 1.372(9) . ?
N3 C15 1.326(9) . ?
N3 H3A 0.8800 . ?
C1 C6 1.383(10) . ?
C1 C2 1.386(10) . ?
C2 C3 1.370(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.402(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(11) . ?
C4 C20 1.505(11) . ?
C5 C6 1.357(10) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C9 1.452(10) . ?
C7 C8 1.504(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.377(10) . ?
C10 C11 1.378(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.347(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.416(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.491(10) . ?
C14 C19 1.422(10) . ?
C14 C15 1.455(10) . ?
C15 C16 1.433(10) . ?
C16 C17 1.336(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.347(10) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.509(13) . ?
C20 C21 1.534(12) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.362(11) . ?
C23 C28 1.381(10) . ?
C24 C25 1.414(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.358(12) . ?
C25 H25 0.9500 . ?
C26 C27 1.349(13) . ?
C26 H26 0.9500 . ?
C27 C28 1.405(11) . ?
C27 H27 0.9500 . ?
C28 H28 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
N3 Pd1 C23 88.2(3) . . ?
N3 Pd1 N1 172.5(3) . . ?
C23 Pd1 N1 99.2(3) . . ?
N3 Pd1 N2 91.5(3) . . ?
C23 Pd1 N2 178.5(3) . . ?
N1 Pd1 N2 81.0(3) . . ?
C7 N1 C1 123.5(7) . . ?
C7 N1 Pd1 112.3(5) . . ?
C1 N1 Pd1 123.8(5) . . ?
C13 N2 C9 120.7(7) . . ?
C13 N2 Pd1 127.6(5) . . ?
C9 N2 Pd1 111.6(5) . . ?
C15 N3 Pd1 129.0(5) . . ?
C15 N3 H3A 115.5 . . ?
Pd1 N3 H3A 115.5 . . ?
C6 C1 C2 119.3(8) . . ?
C6 C1 N1 122.5(7) . . ?
C2 C1 N1 118.0(8) . . ?
C3 C2 C1 119.7(8) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 122.0(8) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C5 C4 C3 116.4(8) . . ?
C5 C4 C20 124.0(9) . . ?
C3 C4 C20 119.5(8) . . ?
C6 C5 C4 121.8(8) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C1 120.6(8) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
N1 C7 C9 119.2(7) . . ?
N1 C7 C8 121.0(8) . . ?
C9 C7 C8 119.5(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 120.9(8) . . ?
N2 C9 C7 115.4(7) . . ?
C10 C9 C7 123.7(8) . . ?
C9 C10 C11 119.9(8) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 117.6(8) . . ?
C12 C11 H11 121.2 . . ?
C10 C11 H11 121.2 . . ?
C11 C12 C13 122.9(8) . . ?
C11 C12 H12 118.5 . . ?
C13 C12 H12 118.5 . . ?
N2 C13 C12 117.9(7) . . ?
N2 C13 C14 122.1(7) . . ?
C12 C13 C14 120.0(7) . . ?
C19 C14 C15 116.9(7) . . ?
C19 C14 C13 118.9(7) . . ?
C15 C14 C13 124.2(7) . . ?
N3 C15 C16 119.4(7) . . ?
N3 C15 C14 125.1(7) . . ?
C16 C15 C14 115.5(7) . . ?
C17 C16 C15 124.3(8) . . ?
C17 C16 H16 117.9 . . ?
C15 C16 H16 117.9 . . ?
C16 C17 C18 119.8(8) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 119.6(8) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C18 C19 C14 123.6(8) . . ?
C18 C19 H19 118.2 . . ?
C14 C19 H19 118.2 . . ?
C4 C20 C22 111.4(8) . . ?
C4 C20 C21 114.5(8) . . ?
C22 C20 C21 108.1(8) . . ?
C4 C20 H20 107.5 . . ?
C22 C20 H20 107.5 . . ?
C21 C20 H20 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 116.9(8) . . ?
C24 C23 Pd1 121.5(6) . . ?
C28 C23 Pd1 121.6(6) . . ?
C23 C24 C25 120.7(9) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 121.6(9) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C27 C26 C25 118.3(9) . . ?
C27 C26 H26 120.9 . . ?
C25 C26 H26 120.9 . . ?
C26 C27 C28 120.7(10) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C23 C28 C27 121.8(9) . . ?
C23 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?

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
C23 Pd1 N1 C7 -171.5(5) . . . . ?
N2 Pd1 N1 C7 7.0(5) . . . . ?
C23 Pd1 N1 C1 0.4(6) . . . . ?
N2 Pd1 N1 C1 178.9(6) . . . . ?
N3 Pd1 N2 C13 -2.6(6) . . . . ?
N1 Pd1 N2 C13 177.8(6) . . . . ?
N3 Pd1 N2 C9 174.4(5) . . . . ?
N1 Pd1 N2 C9 -5.1(5) . . . . ?
C23 Pd1 N3 C15 -174.6(7) . . . . ?
N2 Pd1 N3 C15 6.9(7) . . . . ?
C7 N1 C1 C6 62.3(11) . . . . ?
Pd1 N1 C1 C6 -108.7(8) . . . . ?
C7 N1 C1 C2 -123.5(8) . . . . ?
Pd1 N1 C1 C2 65.5(9) . . . . ?
C6 C1 C2 C3 -0.2(12) . . . . ?
N1 C1 C2 C3 -174.6(7) . . . . ?
C1 C2 C3 C4 1.7(13) . . . . ?
C2 C3 C4 C5 -3.4(13) . . . . ?
C2 C3 C4 C20 174.2(8) . . . . ?
C3 C4 C5 C6 3.9(13) . . . . ?
C20 C4 C5 C6 -173.6(8) . . . . ?
C4 C5 C6 C1 -2.6(13) . . . . ?
C2 C1 C6 C5 0.7(12) . . . . ?
N1 C1 C6 C5 174.8(7) . . . . ?
C1 N1 C7 C9 -179.7(7) . . . . ?
Pd1 N1 C7 C9 -7.7(9) . . . . ?
C1 N1 C7 C8 7.2(11) . . . . ?
Pd1 N1 C7 C8 179.1(6) . . . . ?
C13 N2 C9 C10 2.0(11) . . . . ?
Pd1 N2 C9 C10 -175.3(6) . . . . ?
C13 N2 C9 C7 -179.9(7) . . . . ?
Pd1 N2 C9 C7 2.8(8) . . . . ?
N1 C7 C9 N2 3.4(11) . . . . ?
C8 C7 C9 N2 176.7(7) . . . . ?
N1 C7 C9 C10 -178.6(7) . . . . ?
C8 C7 C9 C10 -5.3(12) . . . . ?
N2 C9 C10 C11 -2.4(11) . . . . ?
C7 C9 C10 C11 179.8(7) . . . . ?
C9 C10 C11 C12 2.6(11) . . . . ?
C10 C11 C12 C13 -2.5(12) . . . . ?
C9 N2 C13 C12 -1.8(10) . . . . ?
Pd1 N2 C13 C12 175.0(5) . . . . ?
C9 N2 C13 C14 -179.8(6) . . . . ?
Pd1 N2 C13 C14 -3.0(10) . . . . ?
C11 C12 C13 N2 2.1(11) . . . . ?
C11 C12 C13 C14 -179.8(7) . . . . ?
N2 C13 C14 C19 -171.7(7) . . . . ?
C12 C13 C14 C19 10.4(10) . . . . ?
N2 C13 C14 C15 6.6(11) . . . . ?
C12 C13 C14 C15 -171.3(7) . . . . ?
Pd1 N3 C15 C16 176.8(5) . . . . ?
Pd1 N3 C15 C14 -5.6(11) . . . . ?
C19 C14 C15 N3 175.9(7) . . . . ?
C13 C14 C15 N3 -2.4(11) . . . . ?
C19 C14 C15 C16 -6.3(10) . . . . ?
C13 C14 C15 C16 175.4(7) . . . . ?
N3 C15 C16 C17 -178.4(8) . . . . ?
C14 C15 C16 C17 3.7(11) . . . . ?
C15 C16 C17 C18 1.2(13) . . . . ?
C16 C17 C18 C19 -3.4(12) . . . . ?
C17 C18 C19 C14 0.4(12) . . . . ?
C15 C14 C19 C18 4.6(11) . . . . ?
C13 C14 C19 C18 -177.0(7) . . . . ?
C5 C4 C20 C22 102.9(10) . . . . ?
C3 C4 C20 C22 -74.5(11) . . . . ?
C5 C4 C20 C21 -20.1(13) . . . . ?
C3 C4 C20 C21 162.5(9) . . . . ?
N3 Pd1 C23 C24 48.7(7) . . . . ?
N1 Pd1 C23 C24 -131.9(7) . . . . ?
N3 Pd1 C23 C28 -131.3(7) . . . . ?
N1 Pd1 C23 C28 48.1(7) . . . . ?
C28 C23 C24 C25 -1.8(12) . . . . ?
Pd1 C23 C24 C25 178.2(6) . . . . ?
C23 C24 C25 C26 1.5(14) . . . . ?
C24 C25 C26 C27 -0.8(15) . . . . ?
C25 C26 C27 C28 0.4(15) . . . . ?
C24 C23 C28 C27 1.4(12) . . . . ?
Pd1 C23 C28 C27 -178.5(6) . . . . ?
C26 C27 C28 C23 -0.8(14) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.321
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.138

####################################################################### 
# 
# 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_11015
_database_code_depnum_ccdc_archive 'CCDC 1043196'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H33 N3 Pd'
_chemical_formula_sum            'C31 H33 N3 Pd'
_chemical_formula_weight         554.00

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'
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

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

_cell_length_a                   12.118(3)
_cell_length_b                   10.844(3)
_cell_length_c                   40.250(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5289(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    945
_cell_measurement_theta_min      2.571
_cell_measurement_theta_max      28.345

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2288
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 16794 reflections(SADABS);Rint 0.0676 before
correction and 0.0363 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41613
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5763
_reflns_number_gt                4754
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0385P)²+2.6022P] 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         5763
_refine_ls_number_parameters     321
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0906
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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
Pd1 Pd 0.478573(19) 0.40663(2) 0.142734(5) 0.01863(8) Uani 1 1 d . . .
N1 N 0.40154(19) 0.5587(2) 0.12384(6) 0.0196(5) Uani 1 1 d . . .
N2 N 0.3659(2) 0.4411(2) 0.18023(6) 0.0200(5) Uani 1 1 d . . .
N3 N 0.5381(2) 0.2641(2) 0.16669(6) 0.0267(6) Uani 1 1 d . . .
H3A H 0.5974 0.2252 0.1578 0.032 Uiso 1 1 d R . .
C1 C 0.4366(3) 0.6272(3) 0.09513(7) 0.0211(6) Uani 1 1 d . . .
C2 C 0.5058(2) 0.7292(3) 0.09935(8) 0.0243(7) Uani 1 1 d . . .
C3 C 0.5416(3) 0.7891(3) 0.07105(8) 0.0325(8) Uani 1 1 d . . .
H3 H 0.5894 0.8581 0.0731 0.039 Uiso 1 1 calc R . .
C4 C 0.5092(3) 0.7504(3) 0.03987(9) 0.0366(9) Uani 1 1 d . . .
H4 H 0.5344 0.7930 0.0207 0.044 Uiso 1 1 calc R . .
C5 C 0.4403(3) 0.6501(3) 0.03649(8) 0.0330(8) Uani 1 1 d . . .
H5 H 0.4183 0.6246 0.0149 0.040 Uiso 1 1 calc R . .
C6 C 0.4024(3) 0.5857(3) 0.06391(7) 0.0262(7) Uani 1 1 d . . .
C7 C 0.3177(3) 0.5966(3) 0.14076(7) 0.0229(6) Uani 1 1 d . . .
C8 C 0.2536(3) 0.7111(3) 0.13263(8) 0.0318(8) Uani 1 1 d . . .
H8A H 0.2708 0.7373 0.1099 0.048 Uiso 1 1 calc R . .
H8B H 0.2738 0.7769 0.1482 0.048 Uiso 1 1 calc R . .
H8C H 0.1745 0.6940 0.1345 0.048 Uiso 1 1 calc R . .
C9 C 0.2876(2) 0.5237(3) 0.17024(7) 0.0219(6) Uani 1 1 d . . .
C10 C 0.1867(3) 0.5325(3) 0.18560(8) 0.0298(7) Uani 1 1 d . . .
H10 H 0.1339 0.5921 0.1787 0.036 Uiso 1 1 calc R . .
C11 C 0.1642(3) 0.4519(3) 0.21147(8) 0.0351(8) Uani 1 1 d . . .
H11 H 0.0940 0.4535 0.2220 0.042 Uiso 1 1 calc R . .
C12 C 0.2425(3) 0.3706(3) 0.22181(8) 0.0315(8) Uani 1 1 d . . .
H12 H 0.2264 0.3156 0.2395 0.038 Uiso 1 1 calc R . .
C13 C 0.3478(3) 0.3669(3) 0.20647(7) 0.0238(7) Uani 1 1 d . . .
C14 C 0.4349(3) 0.2851(3) 0.21898(7) 0.0269(7) Uani 1 1 d . . .
C15 C 0.5242(3) 0.2400(3) 0.19928(8) 0.0257(7) Uani 1 1 d . . .
C16 C 0.5989(3) 0.1571(3) 0.21490(8) 0.0321(8) Uani 1 1 d . . .
H16 H 0.6589 0.1251 0.2024 0.039 Uiso 1 1 calc R . .
C17 C 0.5870(3) 0.1219(3) 0.24730(9) 0.0390(9) Uani 1 1 d . . .
H17 H 0.6384 0.0659 0.2568 0.047 Uiso 1 1 calc R . .
C18 C 0.5011(3) 0.1669(3) 0.26655(9) 0.0411(10) Uani 1 1 d . . .
H18 H 0.4934 0.1425 0.2891 0.049 Uiso 1 1 calc R . .
C19 C 0.4277(3) 0.2470(3) 0.25244(8) 0.0354(8) Uani 1 1 d . . .
H19 H 0.3693 0.2784 0.2657 0.042 Uiso 1 1 calc R . .
C20 C 0.3249(3) 0.4774(3) 0.06016(8) 0.0322(8) Uani 1 1 d . . .
H20 H 0.3256 0.4307 0.0816 0.039 Uiso 1 1 calc R . .
C21 C 0.3602(3) 0.3889(3) 0.03285(9) 0.0408(9) Uani 1 1 d . . .
H21A H 0.3548 0.4302 0.0113 0.061 Uiso 1 1 calc R . .
H21B H 0.3119 0.3164 0.0330 0.061 Uiso 1 1 calc R . .
H21C H 0.4366 0.3629 0.0367 0.061 Uiso 1 1 calc R . .
C22 C 0.2068(3) 0.5211(4) 0.05416(13) 0.0629(13) Uani 1 1 d . . .
H22A H 0.1841 0.5758 0.0723 0.094 Uiso 1 1 calc R . .
H22B H 0.1574 0.4497 0.0533 0.094 Uiso 1 1 calc R . .
H22C H 0.2032 0.5660 0.0331 0.094 Uiso 1 1 calc R . .
C23 C 0.5431(3) 0.7714(3) 0.13385(8) 0.0274(7) Uani 1 1 d . . .
H23 H 0.4870 0.7430 0.1504 0.033 Uiso 1 1 calc R . .
C24 C 0.6543(3) 0.7116(4) 0.14284(9) 0.0480(10) Uani 1 1 d . . .
H24A H 0.6456 0.6219 0.1438 0.072 Uiso 1 1 calc R . .
H24B H 0.6788 0.7421 0.1645 0.072 Uiso 1 1 calc R . .
H24C H 0.7093 0.7328 0.1259 0.072 Uiso 1 1 calc R . .
C25 C 0.5519(4) 0.9113(3) 0.13634(10) 0.0517(11) Uani 1 1 d . . .
H25A H 0.6121 0.9403 0.1221 0.078 Uiso 1 1 calc R . .
H25B H 0.5668 0.9347 0.1594 0.078 Uiso 1 1 calc R . .
H25C H 0.4823 0.9487 0.1291 0.078 Uiso 1 1 calc R . .
C26 C 0.5664(3) 0.3549(3) 0.10264(7) 0.0226(6) Uani 1 1 d . . .
C27 C 0.5565(3) 0.2329(3) 0.09218(8) 0.0299(7) Uani 1 1 d . . .
H27 H 0.5120 0.1776 0.1047 0.036 Uiso 1 1 calc R . .
C28 C 0.6102(3) 0.1903(3) 0.06390(8) 0.0375(9) Uani 1 1 d . . .
H28 H 0.6018 0.1067 0.0573 0.045 Uiso 1 1 calc R . .
C29 C 0.6758(3) 0.2687(4) 0.04537(8) 0.0387(9) Uani 1 1 d . . .
H29 H 0.7128 0.2398 0.0261 0.046 Uiso 1 1 calc R . .
C30 C 0.6864(3) 0.3894(3) 0.05536(8) 0.0333(8) Uani 1 1 d . . .
H30 H 0.7312 0.4441 0.0428 0.040 Uiso 1 1 calc R . .
C31 C 0.6325(3) 0.4324(3) 0.08365(7) 0.0259(7) Uani 1 1 d . . .
H31 H 0.6411 0.5162 0.0901 0.031 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 N3 1.959(3) . ?
Pd1 C26 2.013(3) . ?
Pd1 N1 2.041(2) . ?
Pd1 N2 2.069(2) . ?
N1 C7 1.291(4) . ?
N1 C1 1.438(4) . ?
N2 C13 1.345(4) . ?
N2 C9 1.366(4) . ?
N3 C15 1.348(4) . ?
N3 H3A 0.9068 . ?
C1 C6 1.398(4) . ?
C1 C2 1.399(4) . ?
C2 C3 1.381(4) . ?
C2 C23 1.530(4) . ?
C3 C4 1.380(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(4) . ?
C5 H5 0.9500 . ?
C6 C20 1.511(4) . ?
C7 C9 1.472(4) . ?
C7 C8 1.500(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.374(4) . ?
C10 C11 1.386(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.361(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.418(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.468(4) . ?
C14 C19 1.411(4) . ?
C14 C15 1.427(5) . ?
C15 C16 1.423(4) . ?
C16 C17 1.366(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.367(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.520(5) . ?
C20 C22 1.527(5) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.524(5) . ?
C23 C24 1.538(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C31 1.390(4) . ?
C26 C27 1.393(4) . ?
C27 C28 1.390(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.383(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.393(4) . ?
C30 H30 0.9500 . ?
C31 H31 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
N3 Pd1 C26 88.85(11) . . ?
N3 Pd1 N1 171.38(10) . . ?
C26 Pd1 N1 99.68(11) . . ?
N3 Pd1 N2 91.51(10) . . ?
C26 Pd1 N2 169.73(11) . . ?
N1 Pd1 N2 79.88(10) . . ?
C7 N1 C1 119.4(2) . . ?
C7 N1 Pd1 114.9(2) . . ?
C1 N1 Pd1 125.58(18) . . ?
C13 N2 C9 120.7(3) . . ?
C13 N2 Pd1 124.9(2) . . ?
C9 N2 Pd1 111.23(18) . . ?
C15 N3 Pd1 125.8(2) . . ?
C15 N3 H3A 113.2 . . ?
Pd1 N3 H3A 117.7 . . ?
C6 C1 C2 122.8(3) . . ?
C6 C1 N1 117.9(3) . . ?
C2 C1 N1 119.2(3) . . ?
C3 C2 C1 117.4(3) . . ?
C3 C2 C23 121.0(3) . . ?
C1 C2 C23 121.6(3) . . ?
C4 C3 C2 121.2(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.3(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 117.1(3) . . ?
C5 C6 C20 121.2(3) . . ?
C1 C6 C20 121.6(3) . . ?
N1 C7 C9 116.7(3) . . ?
N1 C7 C8 123.8(3) . . ?
C9 C7 C8 119.5(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 122.1(3) . . ?
N2 C9 C7 114.7(3) . . ?
C10 C9 C7 123.1(3) . . ?
C9 C10 C11 118.0(3) . . ?
C9 C10 H10 121.0 . . ?
C11 C10 H10 121.0 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
N2 C13 C12 118.2(3) . . ?
N2 C13 C14 120.9(3) . . ?
C12 C13 C14 121.0(3) . . ?
C19 C14 C15 118.5(3) . . ?
C19 C14 C13 117.4(3) . . ?
C15 C14 C13 124.2(3) . . ?
N3 C15 C16 118.2(3) . . ?
N3 C15 C14 124.7(3) . . ?
C16 C15 C14 117.0(3) . . ?
C17 C16 C15 122.1(3) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C16 C17 C18 121.0(3) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 118.7(3) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C18 C19 C14 122.8(4) . . ?
C18 C19 H19 118.6 . . ?
C14 C19 H19 118.6 . . ?
C6 C20 C21 112.8(3) . . ?
C6 C20 C22 110.9(3) . . ?
C21 C20 C22 110.2(3) . . ?
C6 C20 H20 107.6 . . ?
C21 C20 H20 107.6 . . ?
C22 C20 H20 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C2 112.2(3) . . ?
C25 C23 C24 110.1(3) . . ?
C2 C23 C24 110.3(3) . . ?
C25 C23 H23 108.1 . . ?
C2 C23 H23 108.1 . . ?
C24 C23 H23 108.1 . . ?
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 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C31 C26 C27 117.2(3) . . ?
C31 C26 Pd1 125.2(2) . . ?
C27 C26 Pd1 117.5(2) . . ?
C28 C27 C26 121.5(3) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C29 C28 C27 120.4(3) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C30 C29 C28 118.8(3) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
C29 C30 C31 120.9(3) . . ?
C29 C30 H30 119.5 . . ?
C31 C30 H30 119.5 . . ?
C26 C31 C30 121.1(3) . . ?
C26 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?

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
C26 Pd1 N1 C7 163.5(2) . . . . ?
N2 Pd1 N1 C7 -6.1(2) . . . . ?
C26 Pd1 N1 C1 -19.9(2) . . . . ?
N2 Pd1 N1 C1 170.6(2) . . . . ?
N3 Pd1 N2 C13 -7.5(2) . . . . ?
C26 Pd1 N2 C13 84.4(6) . . . . ?
N1 Pd1 N2 C13 172.9(2) . . . . ?
N3 Pd1 N2 C9 -167.2(2) . . . . ?
C26 Pd1 N2 C9 -75.3(6) . . . . ?
N1 Pd1 N2 C9 13.13(19) . . . . ?
C26 Pd1 N3 C15 172.8(3) . . . . ?
N2 Pd1 N3 C15 -17.5(3) . . . . ?
C7 N1 C1 C6 -98.5(3) . . . . ?
Pd1 N1 C1 C6 85.0(3) . . . . ?
C7 N1 C1 C2 83.7(4) . . . . ?
Pd1 N1 C1 C2 -92.8(3) . . . . ?
C6 C1 C2 C3 -0.6(5) . . . . ?
N1 C1 C2 C3 177.1(3) . . . . ?
C6 C1 C2 C23 -179.1(3) . . . . ?
N1 C1 C2 C23 -1.4(4) . . . . ?
C1 C2 C3 C4 0.7(5) . . . . ?
C23 C2 C3 C4 179.2(3) . . . . ?
C2 C3 C4 C5 -0.3(5) . . . . ?
C3 C4 C5 C6 -0.3(5) . . . . ?
C4 C5 C6 C1 0.4(5) . . . . ?
C4 C5 C6 C20 178.7(3) . . . . ?
C2 C1 C6 C5 0.1(5) . . . . ?
N1 C1 C6 C5 -177.7(3) . . . . ?
C2 C1 C6 C20 -178.2(3) . . . . ?
N1 C1 C6 C20 4.0(4) . . . . ?
C1 N1 C7 C9 -178.8(3) . . . . ?
Pd1 N1 C7 C9 -1.9(3) . . . . ?
C1 N1 C7 C8 -0.9(4) . . . . ?
Pd1 N1 C7 C8 175.9(2) . . . . ?
C13 N2 C9 C10 -2.0(4) . . . . ?
Pd1 N2 C9 C10 158.7(2) . . . . ?
C13 N2 C9 C7 -178.7(2) . . . . ?
Pd1 N2 C9 C7 -17.9(3) . . . . ?
N1 C7 C9 N2 13.7(4) . . . . ?
C8 C7 C9 N2 -164.2(3) . . . . ?
N1 C7 C9 C10 -162.9(3) . . . . ?
C8 C7 C9 C10 19.2(4) . . . . ?
N2 C9 C10 C11 -1.7(5) . . . . ?
C7 C9 C10 C11 174.7(3) . . . . ?
C9 C10 C11 C12 2.6(5) . . . . ?
C10 C11 C12 C13 0.1(5) . . . . ?
C9 N2 C13 C12 4.6(4) . . . . ?
Pd1 N2 C13 C12 -153.4(2) . . . . ?
C9 N2 C13 C14 -175.0(3) . . . . ?
Pd1 N2 C13 C14 27.0(4) . . . . ?
C11 C12 C13 N2 -3.7(5) . . . . ?
C11 C12 C13 C14 175.9(3) . . . . ?
N2 C13 C14 C19 156.4(3) . . . . ?
C12 C13 C14 C19 -23.2(4) . . . . ?
N2 C13 C14 C15 -25.2(4) . . . . ?
C12 C13 C14 C15 155.2(3) . . . . ?
Pd1 N3 C15 C16 -160.6(2) . . . . ?
Pd1 N3 C15 C14 24.0(4) . . . . ?
C19 C14 C15 N3 176.7(3) . . . . ?
C13 C14 C15 N3 -1.8(5) . . . . ?
C19 C14 C15 C16 1.2(4) . . . . ?
C13 C14 C15 C16 -177.3(3) . . . . ?
N3 C15 C16 C17 -176.1(3) . . . . ?
C14 C15 C16 C17 -0.3(5) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
C16 C17 C18 C19 0.3(5) . . . . ?
C17 C18 C19 C14 0.7(5) . . . . ?
C15 C14 C19 C18 -1.4(5) . . . . ?
C13 C14 C19 C18 177.2(3) . . . . ?
C5 C6 C20 C21 45.5(4) . . . . ?
C1 C6 C20 C21 -136.2(3) . . . . ?
C5 C6 C20 C22 -78.6(4) . . . . ?
C1 C6 C20 C22 99.6(4) . . . . ?
C3 C2 C23 C25 37.4(4) . . . . ?
C1 C2 C23 C25 -144.1(3) . . . . ?
C3 C2 C23 C24 -85.6(4) . . . . ?
C1 C2 C23 C24 92.8(4) . . . . ?
N3 Pd1 C26 C31 -132.0(3) . . . . ?
N1 Pd1 C26 C31 49.2(3) . . . . ?
N2 Pd1 C26 C31 135.8(5) . . . . ?
N3 Pd1 C26 C27 50.9(2) . . . . ?
N1 Pd1 C26 C27 -127.9(2) . . . . ?
N2 Pd1 C26 C27 -41.2(7) . . . . ?
C31 C26 C27 C28 -0.1(5) . . . . ?
Pd1 C26 C27 C28 177.2(3) . . . . ?
C26 C27 C28 C29 0.3(5) . . . . ?
C27 C28 C29 C30 -0.2(5) . . . . ?
C28 C29 C30 C31 0.1(5) . . . . ?
C27 C26 C31 C30 0.0(4) . . . . ?
Pd1 C26 C31 C30 -177.1(2) . . . . ?
C29 C30 C31 C26 0.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_13102
_database_code_depnum_ccdc_archive 'CCDC 1043197'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;
_vrf_RINTA01_I                   
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: ...The crystal data was weak due to crystal quality.
;
_vrf_PLAT020_I                   
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.265       
RESPONSE: ...The crystal data was weak due to crystal quality.
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         28 %     
RESPONSE: ...The crystal data was weak due to crystal quality.
;
_vrf_PLAT213_I                   
;
PROBLEM: Atom C15A            has ADP max/min Ratio .....        9.6 oblate
RESPONSE: ...The crystal data was not the best.
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn     H21L   ..  H22F    ..       1.59 Ang.  
RESPONSE: ...There is disorder in the structure which has been modelled.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H26 N4 Pd, C F3 O3 S, 2(C H Cl3)'
_chemical_formula_sum            'C30 H28 Cl6 F3 N4 O3 Pd S'
_chemical_formula_weight         900.72

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   14.155(7)
_cell_length_b                   16.226(8)
_cell_length_c                   17.503(8)
_cell_angle_alpha                89.109(9)
_cell_angle_beta                 76.364(11)
_cell_angle_gamma                70.267(10)
_cell_volume                     3668(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    967
_cell_measurement_theta_min      2.203
_cell_measurement_theta_max      28,620

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1804
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.139
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 2952 reflections(SADABS);Rint 0.1763 before
correction and 0.0930 after.
;

_exptl_special_details           
; 
 The crystal data was weak due to crystal quality. 
;

_diffrn_ambient_temperature      150(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 Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26756
_diffrn_reflns_av_R_equivalents  0.2649
_diffrn_reflns_av_sigmaI/netI    0.3929
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12826
_reflns_number_gt                3593
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0904P)²+0.0000P] 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         12826
_refine_ls_number_parameters     889
_refine_ls_number_restraints     749
_refine_ls_R_factor_all          0.2711
_refine_ls_R_factor_gt           0.1055
_refine_ls_wR_factor_ref         0.2821
_refine_ls_wR_factor_gt          0.2112
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_restrained_S_all      0.809
_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
Pd1 Pd 0.43790(9) 0.91453(8) 0.36399(6) 0.0457(4) Uani 1 1 d U . .
N1 N 0.4728(9) 0.7833(8) 0.3801(7) 0.049(3) Uani 1 1 d U . .
N2 N 0.3992(8) 0.9251(8) 0.4814(7) 0.046(3) Uani 1 1 d U . .
N3 N 0.4045(9) 1.0401(7) 0.3577(7) 0.052(3) Uani 1 1 d U . .
H3B H 0.4107 1.0592 0.3101 0.062 Uiso 1 1 calc R . .
N4 N 0.4797(9) 0.8962(7) 0.2458(7) 0.047(3) Uani 1 1 d U . .
C1 C 0.5159(12) 0.7159(10) 0.3176(9) 0.055(4) Uani 1 1 d U . .
C2 C 0.4564(12) 0.6726(10) 0.2959(9) 0.057(4) Uani 1 1 d U . .
H2 H 0.3880 0.6822 0.3262 0.068 Uiso 1 1 calc R . .
C3 C 0.4966(13) 0.6165(10) 0.2311(9) 0.059(4) Uani 1 1 d U . .
H3 H 0.4555 0.5867 0.2165 0.070 Uiso 1 1 calc R . .
C4 C 0.5988(13) 0.6004(10) 0.1838(9) 0.054(4) Uani 1 1 d U A .
C5 C 0.6559(12) 0.6446(9) 0.2083(9) 0.057(4) Uani 1 1 d U . .
H5 H 0.7245 0.6355 0.1787 0.068 Uiso 1 1 calc R . .
C6 C 0.6153(11) 0.7015(9) 0.2747(8) 0.051(4) Uani 1 1 d U . .
H6 H 0.6560 0.7307 0.2909 0.061 Uiso 1 1 calc R . .
C7 C 0.4516(11) 0.7704(9) 0.4533(9) 0.050(4) Uani 1 1 d U . .
C8 C 0.4717(12) 0.6770(9) 0.4825(8) 0.061(5) Uani 1 1 d U . .
H8A H 0.5074 0.6335 0.4375 0.092 Uiso 1 1 calc R . .
H8B H 0.4056 0.6701 0.5081 0.092 Uiso 1 1 calc R . .
H8C H 0.5149 0.6681 0.5203 0.092 Uiso 1 1 calc R . .
C9 C 0.4136(10) 0.8435(9) 0.5128(9) 0.043(3) Uani 1 1 d U . .
C10 C 0.3962(11) 0.8353(10) 0.5904(9) 0.053(4) Uani 1 1 d U . .
H10 H 0.4050 0.7790 0.6100 0.063 Uiso 1 1 calc R . .
C11 C 0.3661(11) 0.9069(10) 0.6420(9) 0.057(4) Uani 1 1 d U . .
H11 H 0.3549 0.9007 0.6972 0.068 Uiso 1 1 calc R . .
C12 C 0.3517(11) 0.9906(10) 0.6120(9) 0.054(4) Uani 1 1 d U . .
H12 H 0.3288 1.0415 0.6470 0.064 Uiso 1 1 calc R . .
C13 C 0.3723(10) 0.9983(10) 0.5274(9) 0.043(3) Uani 1 1 d U . .
C14 C 0.3534(10) 1.0876(9) 0.4977(9) 0.044(3) Uani 1 1 d U . .
C15 C 0.3732(11) 1.1009(10) 0.4176(9) 0.053(4) Uani 1 1 d U . .
C16 C 0.3548(11) 1.1889(10) 0.3972(9) 0.054(4) Uani 1 1 d U . .
H16 H 0.3621 1.2005 0.3431 0.065 Uiso 1 1 calc R . .
C17 C 0.3271(12) 1.2573(11) 0.4511(9) 0.062(4) Uani 1 1 d U . .
H17 H 0.3216 1.3142 0.4338 0.074 Uiso 1 1 calc R . .
C18 C 0.3060(13) 1.2449(11) 0.5340(10) 0.070(5) Uani 1 1 d U . .
H18 H 0.2818 1.2923 0.5730 0.084 Uiso 1 1 calc R . .
C19 C 0.3231(11) 1.1615(10) 0.5522(9) 0.055(4) Uani 1 1 d U . .
H19 H 0.3142 1.1506 0.6064 0.066 Uiso 1 1 calc R . .
C20 C 0.6434(15) 0.5424(11) 0.1061(9) 0.073(5) Uani 1 1 d DU . .
C21B C 0.732(4) 0.459(3) 0.102(3) 0.22(3) Uani 0.50 1 d PDU A 1
H21A H 0.7913 0.4730 0.1107 0.330 Uiso 0.50 1 calc PR A 1
H21B H 0.7504 0.4282 0.0506 0.330 Uiso 0.50 1 calc PR A 1
H21C H 0.7119 0.4225 0.1435 0.330 Uiso 0.50 1 calc PR A 1
C21C C 0.607(3) 0.469(2) 0.1055(16) 0.075(10) Uani 0.50 1 d PU A 2
H21D H 0.6489 0.4279 0.0597 0.112 Uiso 0.50 1 calc PR A 2
H21E H 0.5342 0.4903 0.1025 0.112 Uiso 0.50 1 calc PR A 2
H21F H 0.6123 0.4382 0.1539 0.112 Uiso 0.50 1 calc PR A 2
C22 C 0.6168(18) 0.5945(13) 0.0349(9) 0.119(8) Uani 1 1 d U A .
H22A H 0.6482 0.5555 -0.0134 0.178 Uiso 1 1 calc R . .
H22B H 0.6437 0.6431 0.0305 0.178 Uiso 1 1 calc R . .
H22C H 0.5414 0.6178 0.0423 0.178 Uiso 1 1 calc R . .
C23 C 0.4378(11) 0.8536(9) 0.2071(9) 0.050(4) Uani 1 1 d U . .
H23 H 0.3806 0.8388 0.2359 0.061 Uiso 1 1 calc R . .
C24 C 0.4729(12) 0.8297(10) 0.1269(9) 0.057(4) Uani 1 1 d U . .
H24 H 0.4394 0.8001 0.1019 0.068 Uiso 1 1 calc R . .
C25 C 0.5560(14) 0.8491(10) 0.0840(9) 0.063(4) Uani 1 1 d U . .
H25 H 0.5818 0.8328 0.0291 0.075 Uiso 1 1 calc R . .
C26 C 0.6011(13) 0.8931(10) 0.1228(9) 0.069(5) Uani 1 1 d U . .
H26 H 0.6593 0.9069 0.0945 0.082 Uiso 1 1 calc R . .
C27 C 0.5617(11) 0.9177(9) 0.2037(8) 0.049(4) Uani 1 1 d U . .
H27 H 0.5922 0.9494 0.2294 0.058 Uiso 1 1 calc R . .
S1 S 0.1700(3) 0.7387(3) 0.2119(2) 0.0580(12) Uani 1 1 d U . .
O1 O 0.2476(7) 0.7719(6) 0.2247(6) 0.061(3) Uani 1 1 d U . .
O2 O 0.0780(8) 0.8043(7) 0.2001(6) 0.070(3) Uani 1 1 d U . .
O3 O 0.1502(8) 0.6736(7) 0.2683(6) 0.069(3) Uani 1 1 d U . .
C28 C 0.2302(18) 0.6759(15) 0.1214(11) 0.085(4) Uani 1 1 d U . .
F1 F 0.3143(9) 0.6103(8) 0.1197(7) 0.135(4) Uani 1 1 d U . .
F2 F 0.2526(10) 0.7244(8) 0.0623(6) 0.131(4) Uani 1 1 d U . .
F3 F 0.1677(9) 0.6399(7) 0.0965(6) 0.115(4) Uani 1 1 d U . .
Pd1A Pd 0.15815(9) 0.04341(8) 0.34471(7) 0.0462(4) Uani 1 1 d U . .
N1A N 0.1232(8) 0.1748(8) 0.3345(7) 0.046(3) Uani 1 1 d U . .
N2A N 0.1197(8) 0.0801(8) 0.4568(7) 0.049(3) Uani 1 1 d U . .
N3A N 0.1822(8) -0.0808(7) 0.3633(6) 0.046(3) Uani 1 1 d U . .
H3C H 0.2043 -0.1179 0.3215 0.055 Uiso 1 1 calc R . .
N4A N 0.1992(9) 0.0142(7) 0.2274(7) 0.047(3) Uani 1 1 d U . .
C1A C 0.1167(12) 0.2173(10) 0.2624(9) 0.055(3) Uani 1 1 d U . .
C2A C 0.1894(13) 0.2554(10) 0.2264(10) 0.072(4) Uani 1 1 d U . .
H2A H 0.2394 0.2604 0.2522 0.087 Uiso 1 1 calc R . .
C3A C 0.1869(15) 0.2854(13) 0.1529(11) 0.095(5) Uani 1 1 d U . .
H3A H 0.2371 0.3104 0.1281 0.115 Uiso 1 1 calc R . .
C4A C 0.1140(16) 0.2810(13) 0.1128(11) 0.095(5) Uani 1 1 d U B .
C5A C 0.0412(13) 0.2431(10) 0.1509(10) 0.071(4) Uani 1 1 d U . .
H5A H -0.0109 0.2399 0.1265 0.086 Uiso 1 1 calc R . .
C6A C 0.0458(11) 0.2096(10) 0.2257(9) 0.057(4) Uani 1 1 d U . .
H6A H -0.0014 0.1816 0.2503 0.068 Uiso 1 1 calc R . .
C7A C 0.0924(11) 0.2184(10) 0.4013(10) 0.058(4) Uani 1 1 d U . .
C8A C 0.0568(13) 0.3182(10) 0.4120(10) 0.085(6) Uani 1 1 d U . .
H8A1 H 0.0916 0.3349 0.4482 0.128 Uiso 1 1 calc R . .
H8A2 H -0.0183 0.3417 0.4339 0.128 Uiso 1 1 calc R . .
H8A3 H 0.0742 0.3420 0.3609 0.128 Uiso 1 1 calc R . .
C9A C 0.0947(10) 0.1666(10) 0.4735(9) 0.046(3) Uani 1 1 d U . .
C10A C 0.0676(11) 0.2065(11) 0.5473(9) 0.060(4) Uani 1 1 d U . .
H10A H 0.0503 0.2682 0.5546 0.072 Uiso 1 1 calc R . .
C11A C 0.0658(11) 0.1542(12) 0.6129(10) 0.066(4) Uani 1 1 d U . .
H11A H 0.0475 0.1797 0.6652 0.079 Uiso 1 1 calc R . .
C12A C 0.0909(11) 0.0673(11) 0.5988(9) 0.061(4) Uani 1 1 d U . .
H12A H 0.0910 0.0315 0.6423 0.074 Uiso 1 1 calc R . .
C13A C 0.1180(10) 0.0257(11) 0.5201(9) 0.052(3) Uani 1 1 d U . .
C14A C 0.1405(11) -0.0675(11) 0.5089(9) 0.051(3) Uani 1 1 d U . .
C15A C 0.1683(10) -0.1135(10) 0.4326(9) 0.048(3) Uani 1 1 d U . .
C16A C 0.1895(11) -0.2085(10) 0.4303(8) 0.056(4) Uani 1 1 d U . .
H16A H 0.2067 -0.2393 0.3805 0.067 Uiso 1 1 calc R . .
C17A C 0.1857(11) -0.2551(12) 0.4964(8) 0.062(4) Uani 1 1 d U . .
H17A H 0.2011 -0.3168 0.4919 0.075 Uiso 1 1 calc R . .
C18A C 0.1585(13) -0.2098(13) 0.5716(10) 0.076(5) Uani 1 1 d U . .
H18A H 0.1558 -0.2417 0.6176 0.091 Uiso 1 1 calc R . .
C19A C 0.1358(12) -0.1193(12) 0.5788(10) 0.071(4) Uani 1 1 d U . .
H19A H 0.1170 -0.0905 0.6298 0.086 Uiso 1 1 calc R . .
C20A C 0.119(2) 0.3136(18) 0.0333(16) 0.143(8) Uani 1 1 d DU . .
C21D C 0.056(3) 0.402(2) 0.015(3) 0.151(17) Uani 0.50 1 d PDU B 1
H21G H 0.0709 0.4059 -0.0425 0.227 Uiso 0.50 1 calc PR B 1
H21H H 0.0735 0.4470 0.0392 0.227 Uiso 0.50 1 calc PR B 1
H21I H -0.0175 0.4109 0.0354 0.227 Uiso 0.50 1 calc PR B 1
C21E C 0.008(2) 0.368(2) 0.039(3) 0.116(14) Uani 0.50 1 d PDU B 2
H21J H 0.0039 0.4117 0.0000 0.174 Uiso 0.50 1 calc PR B 2
H21K H -0.0236 0.3974 0.0921 0.174 Uiso 0.50 1 calc PR B 2
H21L H -0.0295 0.3295 0.0296 0.174 Uiso 0.50 1 calc PR B 2
C22A C 0.127(2) 0.2522(16) -0.0270(11) 0.175(13) Uani 1 1 d U B .
H22D H 0.1746 0.1943 -0.0196 0.263 Uiso 1 1 calc R . .
H22E H 0.1535 0.2711 -0.0785 0.263 Uiso 1 1 calc R . .
H22F H 0.0586 0.2487 -0.0242 0.263 Uiso 1 1 calc R . .
C23A C 0.2754(10) 0.0423(9) 0.1806(9) 0.053(4) Uani 1 1 d U . .
H23A H 0.3091 0.0723 0.2048 0.063 Uiso 1 1 calc R . .
C24A C 0.3027(12) 0.0273(10) 0.0998(10) 0.064(4) Uani 1 1 d U . .
H24A H 0.3553 0.0465 0.0691 0.077 Uiso 1 1 calc R . .
C25A C 0.2539(13) -0.0157(11) 0.0624(10) 0.069(4) Uani 1 1 d U . .
H25A H 0.2724 -0.0263 0.0067 0.082 Uiso 1 1 calc R . .
C26A C 0.1772(11) -0.0428(10) 0.1092(9) 0.057(4) Uani 1 1 d U . .
H26A H 0.1413 -0.0717 0.0863 0.069 Uiso 1 1 calc R . .
C27A C 0.1544(11) -0.0266(9) 0.1898(8) 0.047(4) Uani 1 1 d U . .
H27A H 0.1025 -0.0462 0.2209 0.056 Uiso 1 1 calc R . .
S1A S 0.5267(3) 0.1347(3) 0.1432(2) 0.0550(11) Uani 1 1 d U . .
O1A O 0.4405(8) 0.1369(7) 0.2063(6) 0.067(3) Uani 1 1 d U . .
O2A O 0.6250(8) 0.0852(7) 0.1589(6) 0.071(3) Uani 1 1 d U . .
O3A O 0.5174(10) 0.1199(9) 0.0657(6) 0.102(4) Uani 1 1 d U . .
C28A C 0.5246(17) 0.2464(14) 0.1446(14) 0.092(5) Uani 1 1 d U . .
F1A F 0.5282(11) 0.2715(8) 0.2184(8) 0.138(4) Uani 1 1 d U . .
F2A F 0.6052(9) 0.2548(8) 0.0964(9) 0.151(5) Uani 1 1 d U . .
F3A F 0.4398(9) 0.3014(7) 0.1316(7) 0.126(4) Uani 1 1 d U . .
C29 C 0.7587(16) 0.4857(11) 0.6464(11) 0.099(5) Uani 1 1 d U . .
H29 H 0.7826 0.4261 0.6666 0.119 Uiso 1 1 calc R . .
Cl1 Cl 0.7541(7) 0.5615(4) 0.7159(4) 0.179(3) Uani 1 1 d U . .
Cl2 Cl 0.8495(4) 0.4886(4) 0.5602(4) 0.114(2) Uani 1 1 d U . .
Cl3 Cl 0.6407(5) 0.5025(4) 0.6259(4) 0.127(2) Uani 1 1 d U . .
C30 C 0.2995(14) 0.5452(12) 0.6780(10) 0.088(4) Uani 1 1 d U . .
H30 H 0.3269 0.4878 0.7010 0.105 Uiso 1 1 calc R . .
Cl4 Cl 0.1712(5) 0.6012(4) 0.7321(4) 0.130(2) Uani 1 1 d U . .
Cl5 Cl 0.3037(5) 0.5263(4) 0.5827(3) 0.123(2) Uani 1 1 d U . .
Cl6 Cl 0.3737(5) 0.6103(4) 0.6885(4) 0.134(2) Uani 1 1 d U . .
C31 C 0.8396(12) 0.0857(11) 0.1412(9) 0.072(4) Uani 1 1 d U . .
H31 H 0.7731 0.0886 0.1288 0.086 Uiso 1 1 calc R . .
Cl7 Cl 0.8969(4) -0.0185(4) 0.1686(4) 0.128(2) Uani 1 1 d U . .
Cl8 Cl 0.9205(4) 0.1079(4) 0.0549(3) 0.1035(18) Uani 1 1 d U . .
Cl9 Cl 0.8114(4) 0.1674(4) 0.2161(3) 0.1032(18) Uani 1 1 d U . .
C32 C 0.0255(14) 0.3998(13) 0.7343(13) 0.126(6) Uani 1 1 d U . .
H32 H -0.0396 0.3894 0.7325 0.151 Uiso 1 1 calc R . .
Cl10 Cl 0.1190(5) 0.2979(5) 0.7557(3) 0.139(2) Uani 1 1 d U . .
Cl11 Cl 0.0793(5) 0.4266(4) 0.6437(4) 0.141(2) Uani 1 1 d U . .
Cl12 Cl -0.0004(7) 0.4752(6) 0.8103(5) 0.226(5) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N3 1.937(11) . ?
Pd1 N2 1.992(11) . ?
Pd1 N4 2.010(11) . ?
Pd1 N1 2.049(12) . ?
N1 C7 1.276(16) . ?
N1 C1 1.428(17) . ?
N2 C13 1.336(15) . ?
N2 C9 1.395(16) . ?
N3 C15 1.336(16) . ?
N3 H3B 0.8800 . ?
N4 C23 1.330(16) . ?
N4 C27 1.370(16) . ?
C1 C6 1.372(18) . ?
C1 C2 1.38(2) . ?
C2 C3 1.347(18) . ?
C2 H2 0.9500 . ?
C3 C4 1.43(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.39(2) . ?
C4 C20 1.54(2) . ?
C5 C6 1.375(17) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C9 1.457(18) . ?
C7 C8 1.546(18) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.335(17) . ?
C10 C11 1.365(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.416(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.452(18) . ?
C12 H12 0.9500 . ?
C13 C14 1.491(18) . ?
C14 C15 1.391(18) . ?
C14 C19 1.424(17) . ?
C15 C16 1.418(19) . ?
C16 C17 1.358(18) . ?
C16 H16 0.9500 . ?
C17 C18 1.436(19) . ?
C17 H17 0.9500 . ?
C18 C19 1.339(19) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21C 1.46(3) . ?
C20 C21B 1.486(10) . ?
C20 C22 1.54(2) . ?
C21B H21A 0.9800 . ?
C21B H21B 0.9800 . ?
C21B H21C 0.9800 . ?
C21C H21D 0.9800 . ?
C21C H21E 0.9800 . ?
C21C H21F 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.387(17) . ?
C23 H23 0.9500 . ?
C24 C25 1.37(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.38(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.404(18) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
S1 O2 1.435(11) . ?
S1 O1 1.437(10) . ?
S1 O3 1.485(10) . ?
S1 C28 1.762(19) . ?
C28 F1 1.30(2) . ?
C28 F2 1.33(2) . ?
C28 F3 1.36(2) . ?
Pd1A N2A 1.952(11) . ?
Pd1A N3A 1.962(11) . ?
Pd1A N4A 2.015(11) . ?
Pd1A N1A 2.034(12) . ?
N1A C7A 1.279(16) . ?
N1A C1A 1.436(17) . ?
N2A C9A 1.345(16) . ?
N2A C13A 1.407(18) . ?
N3A C15A 1.316(16) . ?
N3A H3C 0.8800 . ?
N4A C27A 1.329(16) . ?
N4A C23A 1.395(16) . ?
C1A C6A 1.351(19) . ?
C1A C2A 1.396(19) . ?
C2A C3A 1.37(2) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.40(2) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.41(2) . ?
C4A C20A 1.48(3) . ?
C5A C6A 1.418(19) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C7A C9A 1.51(2) . ?
C7A C8A 1.524(19) . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A C10A 1.364(17) . ?
C10A C11A 1.42(2) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.34(2) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.450(18) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.443(19) . ?
C14A C15A 1.442(18) . ?
C14A C19A 1.476(19) . ?
C15A C16A 1.466(19) . ?
C16A C17A 1.372(18) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.42(2) . ?
C17A H17A 0.9500 . ?
C18A C19A 1.39(2) . ?
C18A H18A 0.9500 . ?
C19A H19A 0.9500 . ?
C20A C22A 1.42(3) . ?
C20A C21D 1.486(10) . ?
C20A C21E 1.502(10) . ?
C21D H21G 0.9800 . ?
C21D H21H 0.9800 . ?
C21D H21I 0.9800 . ?
C21E H21J 0.9800 . ?
C21E H21K 0.9800 . ?
C21E H21L 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C23A C24A 1.378(18) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.40(2) . ?
C24A H24A 0.9500 . ?
C25A C26A 1.390(19) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.378(17) . ?
C26A H26A 0.9500 . ?
C27A H27A 0.9500 . ?
S1A O3A 1.424(11) . ?
S1A O1A 1.430(9) . ?
S1A O2A 1.441(11) . ?
S1A C28A 1.80(2) . ?
C28A F2A 1.30(2) . ?
C28A F3A 1.30(2) . ?
C28A F1A 1.38(2) . ?
C29 Cl1 1.719(18) . ?
C29 Cl3 1.72(2) . ?
C29 Cl2 1.75(2) . ?
C29 H29 1.0000 . ?
C30 Cl5 1.683(18) . ?
C30 Cl6 1.761(19) . ?
C30 Cl4 1.766(18) . ?
C30 H30 1.0000 . ?
C31 Cl7 1.727(17) . ?
C31 Cl9 1.757(16) . ?
C31 Cl8 1.780(16) . ?
C31 H31 1.0000 . ?
C32 Cl11 1.71(2) . ?
C32 Cl12 1.707(19) . ?
C32 Cl10 1.83(2) . ?
C32 H32 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Pd1 N2 92.6(5) . . ?
N3 Pd1 N4 90.8(5) . . ?
N2 Pd1 N4 176.6(5) . . ?
N3 Pd1 N1 175.3(5) . . ?
N2 Pd1 N1 82.9(5) . . ?
N4 Pd1 N1 93.7(5) . . ?
C7 N1 C1 125.0(13) . . ?
C7 N1 Pd1 110.7(10) . . ?
C1 N1 Pd1 124.2(10) . . ?
C13 N2 C9 121.5(13) . . ?
C13 N2 Pd1 126.3(10) . . ?
C9 N2 Pd1 111.9(9) . . ?
C15 N3 Pd1 127.2(11) . . ?
C15 N3 H3B 116.4 . . ?
Pd1 N3 H3B 116.4 . . ?
C23 N4 C27 117.8(13) . . ?
C23 N4 Pd1 121.6(10) . . ?
C27 N4 Pd1 120.1(11) . . ?
C6 C1 C2 120.8(16) . . ?
C6 C1 N1 117.8(15) . . ?
C2 C1 N1 121.1(14) . . ?
C3 C2 C1 119.2(15) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 122.2(16) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 116.6(15) . . ?
C5 C4 C20 120.1(15) . . ?
C3 C4 C20 123.2(16) . . ?
C6 C5 C4 121.3(15) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C1 C6 C5 119.9(16) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
N1 C7 C9 120.7(14) . . ?
N1 C7 C8 121.7(13) . . ?
C9 C7 C8 117.5(13) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 121.6(14) . . ?
C10 C9 C7 124.6(15) . . ?
N2 C9 C7 113.7(13) . . ?
C9 C10 C11 120.9(15) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C12 118.9(15) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C11 C12 C13 119.6(14) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
N2 C13 C12 117.4(13) . . ?
N2 C13 C14 124.1(13) . . ?
C12 C13 C14 118.3(13) . . ?
C15 C14 C19 118.2(14) . . ?
C15 C14 C13 122.2(13) . . ?
C19 C14 C13 119.4(14) . . ?
N3 C15 C14 127.2(15) . . ?
N3 C15 C16 116.3(14) . . ?
C14 C15 C16 116.5(14) . . ?
C17 C16 C15 123.2(16) . . ?
C17 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
C16 C17 C18 120.9(16) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C19 C18 C17 114.9(16) . . ?
C19 C18 H18 122.5 . . ?
C17 C18 H18 122.5 . . ?
C18 C19 C14 126.0(16) . . ?
C18 C19 H19 117.0 . . ?
C14 C19 H19 117.0 . . ?
C21C C20 C21B 71(3) . . ?
C21C C20 C4 114.0(17) . . ?
C21B C20 C4 118(2) . . ?
C21C C20 C22 106(2) . . ?
C21B C20 C22 126(2) . . ?
C4 C20 C22 112.2(14) . . ?
C20 C21B H21A 109.5 . . ?
C20 C21B H21B 109.5 . . ?
C20 C21B H21C 109.5 . . ?
C20 C21C H21D 109.5 . . ?
C20 C21C H21E 109.5 . . ?
H21D C21C H21E 109.5 . . ?
C20 C21C H21F 109.5 . . ?
H21D C21C H21F 109.5 . . ?
H21E C21C H21F 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 C24 123.7(14) . . ?
N4 C23 H23 118.2 . . ?
C24 C23 H23 118.2 . . ?
C25 C24 C23 119.5(16) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 118.0(16) . . ?
C24 C25 H25 121.0 . . ?
C26 C25 H25 121.0 . . ?
C25 C26 C27 120.5(16) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
N4 C27 C26 120.4(14) . . ?
N4 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
O2 S1 O1 114.8(7) . . ?
O2 S1 O3 114.1(6) . . ?
O1 S1 O3 113.6(7) . . ?
O2 S1 C28 105.8(9) . . ?
O1 S1 C28 103.1(9) . . ?
O3 S1 C28 103.7(9) . . ?
F1 C28 F2 106.9(18) . . ?
F1 C28 F3 104.7(18) . . ?
F2 C28 F3 102.8(16) . . ?
F1 C28 S1 116.1(15) . . ?
F2 C28 S1 112.4(15) . . ?
F3 C28 S1 112.9(15) . . ?
N2A Pd1A N3A 93.8(5) . . ?
N2A Pd1A N4A 175.7(5) . . ?
N3A Pd1A N4A 90.3(4) . . ?
N2A Pd1A N1A 82.0(5) . . ?
N3A Pd1A N1A 174.9(4) . . ?
N4A Pd1A N1A 94.0(5) . . ?
C7A N1A C1A 121.8(14) . . ?
C7A N1A Pd1A 112.7(11) . . ?
C1A N1A Pd1A 124.8(10) . . ?
C9A N2A C13A 117.9(13) . . ?
C9A N2A Pd1A 115.1(10) . . ?
C13A N2A Pd1A 127.0(10) . . ?
C15A N3A Pd1A 125.8(10) . . ?
C15A N3A H3C 117.1 . . ?
Pd1A N3A H3C 117.1 . . ?
C27A N4A C23A 116.4(13) . . ?
C27A N4A Pd1A 124.4(10) . . ?
C23A N4A Pd1A 119.1(10) . . ?
C6A C1A C2A 121.0(16) . . ?
C6A C1A N1A 117.4(14) . . ?
C2A C1A N1A 121.1(15) . . ?
C3A C2A C1A 118.5(17) . . ?
C3A C2A H2A 120.8 . . ?
C1A C2A H2A 120.8 . . ?
C2A C3A C4A 123.1(18) . . ?
C2A C3A H3A 118.4 . . ?
C4A C3A H3A 118.4 . . ?
C3A C4A C5A 117.1(18) . . ?
C3A C4A C20A 118.9(19) . . ?
C5A C4A C20A 124.0(19) . . ?
C4A C5A C6A 119.7(17) . . ?
C4A C5A H5A 120.1 . . ?
C6A C5A H5A 120.1 . . ?
C1A C6A C5A 120.6(15) . . ?
C1A C6A H6A 119.7 . . ?
C5A C6A H6A 119.7 . . ?
N1A C7A C9A 117.0(15) . . ?
N1A C7A C8A 124.3(16) . . ?
C9A C7A C8A 118.6(14) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
N2A C9A C10A 125.3(15) . . ?
N2A C9A C7A 112.8(13) . . ?
C10A C9A C7A 121.7(15) . . ?
C9A C10A C11A 118.7(16) . . ?
C9A C10A H10A 120.6 . . ?
C11A C10A H10A 120.6 . . ?
C12A C11A C10A 117.8(16) . . ?
C12A C11A H11A 121.1 . . ?
C10A C11A H11A 121.1 . . ?
C11A C12A C13A 123.0(17) . . ?
C11A C12A H12A 118.5 . . ?
C13A C12A H12A 118.5 . . ?
N2A C13A C14A 122.3(14) . . ?
N2A C13A C12A 117.3(15) . . ?
C14A C13A C12A 120.4(15) . . ?
C15A C14A C13A 123.6(14) . . ?
C15A C14A C19A 117.7(15) . . ?
C13A C14A C19A 118.7(15) . . ?
N3A C15A C14A 127.3(15) . . ?
N3A C15A C16A 115.1(13) . . ?
C14A C15A C16A 117.5(14) . . ?
C17A C16A C15A 123.5(15) . . ?
C17A C16A H16A 118.2 . . ?
C15A C16A H16A 118.2 . . ?
C16A C17A C18A 119.0(17) . . ?
C16A C17A H17A 120.5 . . ?
C18A C17A H17A 120.5 . . ?
C19A C18A C17A 121.0(16) . . ?
C19A C18A H18A 119.5 . . ?
C17A C18A H18A 119.5 . . ?
C18A C19A C14A 121.3(16) . . ?
C18A C19A H19A 119.4 . . ?
C14A C19A H19A 119.4 . . ?
C22A C20A C4A 115(2) . . ?
C22A C20A C21D 108(3) . . ?
C4A C20A C21D 125(3) . . ?
C22A C20A C21E 96(3) . . ?
C4A C20A C21E 102(2) . . ?
C21D C20A C21E 40(2) . . ?
C20A C21D H21G 109.5 . . ?
C20A C21D H21H 109.5 . . ?
C20A C21D H21I 109.5 . . ?
C20A C21E H21J 109.5 . . ?
C20A C21E H21K 109.5 . . ?
H21J C21E H21K 109.5 . . ?
C20A C21E H21L 109.5 . . ?
H21J C21E H21L 109.5 . . ?
H21K C21E H21L 109.5 . . ?
C20A C22A H22D 109.5 . . ?
C20A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C20A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C24A C23A N4A 121.1(14) . . ?
C24A C23A H23A 119.4 . . ?
N4A C23A H23A 119.4 . . ?
C23A C24A C25A 120.8(15) . . ?
C23A C24A H24A 119.6 . . ?
C25A C24A H24A 119.6 . . ?
C26A C25A C24A 117.9(16) . . ?
C26A C25A H25A 121.0 . . ?
C24A C25A H25A 121.0 . . ?
C27A C26A C25A 118.4(16) . . ?
C27A C26A H26A 120.8 . . ?
C25A C26A H26A 120.8 . . ?
N4A C27A C26A 125.4(14) . . ?
N4A C27A H27A 117.3 . . ?
C26A C27A H27A 117.3 . . ?
O3A S1A O1A 116.2(8) . . ?
O3A S1A O2A 115.3(7) . . ?
O1A S1A O2A 113.0(7) . . ?
O3A S1A C28A 102.9(10) . . ?
O1A S1A C28A 103.5(8) . . ?
O2A S1A C28A 103.6(9) . . ?
F2A C28A F3A 111.0(18) . . ?
F2A C28A F1A 106(2) . . ?
F3A C28A F1A 106.0(19) . . ?
F2A C28A S1A 112.1(16) . . ?
F3A C28A S1A 112.3(16) . . ?
F1A C28A S1A 109.4(14) . . ?
Cl1 C29 Cl3 113.2(10) . . ?
Cl1 C29 Cl2 108.8(13) . . ?
Cl3 C29 Cl2 109.9(11) . . ?
Cl1 C29 H29 108.3 . . ?
Cl3 C29 H29 108.3 . . ?
Cl2 C29 H29 108.3 . . ?
Cl5 C30 Cl6 111.7(9) . . ?
Cl5 C30 Cl4 110.9(11) . . ?
Cl6 C30 Cl4 107.3(10) . . ?
Cl5 C30 H30 109.0 . . ?
Cl6 C30 H30 109.0 . . ?
Cl4 C30 H30 109.0 . . ?
Cl7 C31 Cl9 112.5(9) . . ?
Cl7 C31 Cl8 110.5(9) . . ?
Cl9 C31 Cl8 109.1(9) . . ?
Cl7 C31 H31 108.2 . . ?
Cl9 C31 H31 108.2 . . ?
Cl8 C31 H31 108.2 . . ?
Cl11 C32 Cl12 115.2(12) . . ?
Cl11 C32 Cl10 107.1(9) . . ?
Cl12 C32 Cl10 106.7(15) . . ?
Cl11 C32 H32 109.2 . . ?
Cl12 C32 H32 109.2 . . ?
Cl10 C32 H32 109.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Pd1 N1 C7 16(6) . . . . ?
N2 Pd1 N1 C7 2.0(10) . . . . ?
N4 Pd1 N1 C7 -178.1(10) . . . . ?
N3 Pd1 N1 C1 -163(5) . . . . ?
N2 Pd1 N1 C1 -177.4(12) . . . . ?
N4 Pd1 N1 C1 2.4(12) . . . . ?
N3 Pd1 N2 C13 -5.8(12) . . . . ?
N4 Pd1 N2 C13 170(7) . . . . ?
N1 Pd1 N2 C13 173.1(12) . . . . ?
N3 Pd1 N2 C9 -179.3(9) . . . . ?
N4 Pd1 N2 C9 -3(8) . . . . ?
N1 Pd1 N2 C9 -0.5(9) . . . . ?
N2 Pd1 N3 C15 3.0(13) . . . . ?
N4 Pd1 N3 C15 -176.7(13) . . . . ?
N1 Pd1 N3 C15 -11(6) . . . . ?
N3 Pd1 N4 C23 -125.0(11) . . . . ?
N2 Pd1 N4 C23 59(8) . . . . ?
N1 Pd1 N4 C23 56.2(11) . . . . ?
N3 Pd1 N4 C27 63.2(11) . . . . ?
N2 Pd1 N4 C27 -113(8) . . . . ?
N1 Pd1 N4 C27 -115.6(11) . . . . ?
C7 N1 C1 C6 -111.6(17) . . . . ?
Pd1 N1 C1 C6 67.8(17) . . . . ?
C7 N1 C1 C2 75(2) . . . . ?
Pd1 N1 C1 C2 -106.0(14) . . . . ?
C6 C1 C2 C3 -1(2) . . . . ?
N1 C1 C2 C3 172.7(13) . . . . ?
C1 C2 C3 C4 0(2) . . . . ?
C2 C3 C4 C5 1(2) . . . . ?
C2 C3 C4 C20 -175.0(14) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C20 C4 C5 C6 175.6(13) . . . . ?
C2 C1 C6 C5 1(2) . . . . ?
N1 C1 C6 C5 -172.4(13) . . . . ?
C4 C5 C6 C1 -1(2) . . . . ?
C1 N1 C7 C9 176.2(13) . . . . ?
Pd1 N1 C7 C9 -3.3(17) . . . . ?
C1 N1 C7 C8 0(2) . . . . ?
Pd1 N1 C7 C8 -179.1(11) . . . . ?
C13 N2 C9 C10 3(2) . . . . ?
Pd1 N2 C9 C10 177.3(11) . . . . ?
C13 N2 C9 C7 -174.9(12) . . . . ?
Pd1 N2 C9 C7 -1.0(14) . . . . ?
N1 C7 C9 C10 -175.2(14) . . . . ?
C8 C7 C9 C10 1(2) . . . . ?
N1 C7 C9 N2 3.0(19) . . . . ?
C8 C7 C9 N2 179.0(12) . . . . ?
N2 C9 C10 C11 -2(2) . . . . ?
C7 C9 C10 C11 176.4(14) . . . . ?
C9 C10 C11 C12 1(2) . . . . ?
C10 C11 C12 C13 -2(2) . . . . ?
C9 N2 C13 C12 -4.0(19) . . . . ?
Pd1 N2 C13 C12 -177.0(9) . . . . ?
C9 N2 C13 C14 -178.6(12) . . . . ?
Pd1 N2 C13 C14 8.4(19) . . . . ?
C11 C12 C13 N2 3(2) . . . . ?
C11 C12 C13 C14 178.2(13) . . . . ?
N2 C13 C14 C15 -7(2) . . . . ?
C12 C13 C14 C15 178.5(13) . . . . ?
N2 C13 C14 C19 178.8(12) . . . . ?
C12 C13 C14 C19 4.3(19) . . . . ?
Pd1 N3 C15 C14 -3(2) . . . . ?
Pd1 N3 C15 C16 179.3(10) . . . . ?
C19 C14 C15 N3 178.4(14) . . . . ?
C13 C14 C15 N3 4(2) . . . . ?
C19 C14 C15 C16 -4(2) . . . . ?
C13 C14 C15 C16 -178.2(13) . . . . ?
N3 C15 C16 C17 -177.0(14) . . . . ?
C14 C15 C16 C17 5(2) . . . . ?
C15 C16 C17 C18 -5(2) . . . . ?
C16 C17 C18 C19 5(2) . . . . ?
C17 C18 C19 C14 -4(2) . . . . ?
C15 C14 C19 C18 4(2) . . . . ?
C13 C14 C19 C18 178.3(15) . . . . ?
C5 C4 C20 C21C 150(2) . . . . ?
C3 C4 C20 C21C -34(3) . . . . ?
C5 C4 C20 C21B 70(4) . . . . ?
C3 C4 C20 C21B -115(4) . . . . ?
C5 C4 C20 C22 -89.2(19) . . . . ?
C3 C4 C20 C22 87(2) . . . . ?
C27 N4 C23 C24 0(2) . . . . ?
Pd1 N4 C23 C24 -171.6(11) . . . . ?
N4 C23 C24 C25 1(2) . . . . ?
C23 C24 C25 C26 -1(2) . . . . ?
C24 C25 C26 C27 -1(2) . . . . ?
C23 N4 C27 C26 -2(2) . . . . ?
Pd1 N4 C27 C26 170.4(11) . . . . ?
C25 C26 C27 N4 2(2) . . . . ?
O2 S1 C28 F1 -178.0(16) . . . . ?
O1 S1 C28 F1 61.1(19) . . . . ?
O3 S1 C28 F1 -57.6(19) . . . . ?
O2 S1 C28 F2 58.6(17) . . . . ?
O1 S1 C28 F2 -62.3(17) . . . . ?
O3 S1 C28 F2 179.0(15) . . . . ?
O2 S1 C28 F3 -57.1(17) . . . . ?
O1 S1 C28 F3 -178.0(15) . . . . ?
O3 S1 C28 F3 63.3(17) . . . . ?
N2A Pd1A N1A C7A -1.1(10) . . . . ?
N3A Pd1A N1A C7A 32(6) . . . . ?
N4A Pd1A N1A C7A -179.7(10) . . . . ?
N2A Pd1A N1A C1A -171.6(11) . . . . ?
N3A Pd1A N1A C1A -138(5) . . . . ?
N4A Pd1A N1A C1A 9.8(11) . . . . ?
N3A Pd1A N2A C9A -179.7(10) . . . . ?
N4A Pd1A N2A C9A 17(7) . . . . ?
N1A Pd1A N2A C9A -2.5(9) . . . . ?
N3A Pd1A N2A C13A 1.7(11) . . . . ?
N4A Pd1A N2A C13A -162(6) . . . . ?
N1A Pd1A N2A C13A 178.9(12) . . . . ?
N2A Pd1A N3A C15A 2.3(12) . . . . ?
N4A Pd1A N3A C15A -178.9(12) . . . . ?
N1A Pd1A N3A C15A -31(6) . . . . ?
N2A Pd1A N4A C27A -140(6) . . . . ?
N3A Pd1A N4A C27A 56.7(12) . . . . ?
N1A Pd1A N4A C27A -120.6(12) . . . . ?
N2A Pd1A N4A C23A 36(7) . . . . ?
N3A Pd1A N4A C23A -127.2(11) . . . . ?
N1A Pd1A N4A C23A 55.5(11) . . . . ?
C7A N1A C1A C6A -108.9(17) . . . . ?
Pd1A N1A C1A C6A 60.7(17) . . . . ?
C7A N1A C1A C2A 79.0(19) . . . . ?
Pd1A N1A C1A C2A -111.4(15) . . . . ?
C6A C1A C2A C3A 0(3) . . . . ?
N1A C1A C2A C3A 172.1(16) . . . . ?
C1A C2A C3A C4A 1(3) . . . . ?
C2A C3A C4A C5A 0(3) . . . . ?
C2A C3A C4A C20A -179(2) . . . . ?
C3A C4A C5A C6A -2(3) . . . . ?
C20A C4A C5A C6A 177(2) . . . . ?
C2A C1A C6A C5A -2(2) . . . . ?
N1A C1A C6A C5A -174.4(14) . . . . ?
C4A C5A C6A C1A 3(3) . . . . ?
C1A N1A C7A C9A 175.0(12) . . . . ?
Pd1A N1A C7A C9A 4.3(16) . . . . ?
C1A N1A C7A C8A -7(2) . . . . ?
Pd1A N1A C7A C8A -177.5(12) . . . . ?
C13A N2A C9A C10A 0(2) . . . . ?
Pd1A N2A C9A C10A -178.6(11) . . . . ?
C13A N2A C9A C7A -176.1(11) . . . . ?
Pd1A N2A C9A C7A 5.2(14) . . . . ?
N1A C7A C9A N2A -6.4(18) . . . . ?
C8A C7A C9A N2A 175.2(12) . . . . ?
N1A C7A C9A C10A 177.2(13) . . . . ?
C8A C7A C9A C10A -1(2) . . . . ?
N2A C9A C10A C11A 1(2) . . . . ?
C7A C9A C10A C11A 176.4(13) . . . . ?
C9A C10A C11A C12A 0(2) . . . . ?
C10A C11A C12A C13A -1(2) . . . . ?
C9A N2A C13A C14A 178.1(12) . . . . ?
Pd1A N2A C13A C14A -3.4(19) . . . . ?
C9A N2A C13A C12A -1.1(18) . . . . ?
Pd1A N2A C13A C12A 177.4(9) . . . . ?
C11A C12A C13A N2A 2(2) . . . . ?
C11A C12A C13A C14A -177.7(15) . . . . ?
N2A C13A C14A C15A 1(2) . . . . ?
C12A C13A C14A C15A -179.7(13) . . . . ?
N2A C13A C14A C19A -179.5(12) . . . . ?
C12A C13A C14A C19A 0(2) . . . . ?
Pd1A N3A C15A C14A -5(2) . . . . ?
Pd1A N3A C15A C16A 178.5(9) . . . . ?
C13A C14A C15A N3A 3(2) . . . . ?
C19A C14A C15A N3A -176.1(14) . . . . ?
C13A C14A C15A C16A 179.7(13) . . . . ?
C19A C14A C15A C16A 0.3(19) . . . . ?
N3A C15A C16A C17A 175.7(14) . . . . ?
C14A C15A C16A C17A -1(2) . . . . ?
C15A C16A C17A C18A 1(2) . . . . ?
C16A C17A C18A C19A 0(2) . . . . ?
C17A C18A C19A C14A -1(3) . . . . ?
C15A C14A C19A C18A 1(2) . . . . ?
C13A C14A C19A C18A -178.9(15) . . . . ?
C3A C4A C20A C22A 124(3) . . . . ?
C5A C4A C20A C22A -54(3) . . . . ?
C3A C4A C20A C21D -98(4) . . . . ?
C5A C4A C20A C21D 84(4) . . . . ?
C3A C4A C20A C21E -134(3) . . . . ?
C5A C4A C20A C21E 48(4) . . . . ?
C27A N4A C23A C24A -1(2) . . . . ?
Pd1A N4A C23A C24A -177.1(11) . . . . ?
N4A C23A C24A C25A 1(2) . . . . ?
C23A C24A C25A C26A 0(2) . . . . ?
C24A C25A C26A C27A -1(2) . . . . ?
C23A N4A C27A C26A 0(2) . . . . ?
Pd1A N4A C27A C26A 176.1(11) . . . . ?
C25A C26A C27A N4A 1(2) . . . . ?
O3A S1A C28A F2A -65.9(19) . . . . ?
O1A S1A C28A F2A 172.7(17) . . . . ?
O2A S1A C28A F2A 54.6(19) . . . . ?
O3A S1A C28A F3A 59.8(18) . . . . ?
O1A S1A C28A F3A -61.5(18) . . . . ?
O2A S1A C28A F3A -179.7(15) . . . . ?
O3A S1A C28A F1A 177.2(14) . . . . ?
O1A S1A C28A F1A 55.8(16) . . . . ?
O2A S1A C28A F1A -62.3(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3A H3C O1 0.88 2.30 3.175(14) 170.6 1_545
N3 H3B O1A 0.88 2.23 3.086(15) 162.7 1_565

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.065
_refine_diff_density_min         -1.955
_refine_diff_density_rms         0.165

####################################################################### 
# 
# 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_10002
_database_code_depnum_ccdc_archive 'CCDC 1043198'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H29 N3'
_chemical_formula_sum            'C25 H29 N3'
_chemical_formula_weight         371.51

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   12.906(10)
_cell_length_b                   8.308(6)
_cell_length_c                   39.43(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4228(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    570
_cell_measurement_theta_min      2.600
_cell_measurement_theta_max      23.260

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9836
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_process_details   
;
absorption correction based on 3051 reflections(SADABS);Rint 0.1675 before
correction and 0.0928 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28600
_diffrn_reflns_av_R_equivalents  0.2201
_diffrn_reflns_av_sigmaI/netI    0.1300
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3715
_reflns_number_gt                1816
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0431P)²+0.0000P] 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         3715
_refine_ls_number_parameters     258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.1377
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_restrained_S_all      0.871
_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
N1 N 0.43909(17) 0.1358(3) 0.14261(6) 0.0378(6) Uani 1 1 d . . .
N2 N 0.41944(17) 0.1220(3) 0.05335(5) 0.0363(6) Uani 1 1 d . . .
N3 N 0.5141(2) 0.3056(3) 0.00701(6) 0.0732(9) Uani 1 1 d . . .
H3A H 0.5574 0.3808 0.0002 0.088 Uiso 1 1 calc R . .
H3B H 0.5141 0.2744 0.0283 0.088 Uiso 1 1 calc R . .
C1 C 0.4905(2) 0.2094(3) 0.17054(6) 0.0347(7) Uani 1 1 d . . .
C2 C 0.4503(2) 0.3519(3) 0.18468(7) 0.0378(7) Uani 1 1 d . . .
C3 C 0.4996(2) 0.4163(4) 0.21271(7) 0.0449(8) Uani 1 1 d . . .
H3 H 0.4744 0.5133 0.2224 0.054 Uiso 1 1 calc R . .
C4 C 0.5850(2) 0.3417(4) 0.22680(7) 0.0462(8) Uani 1 1 d . . .
H4 H 0.6189 0.3886 0.2458 0.055 Uiso 1 1 calc R . .
C5 C 0.6212(2) 0.1986(4) 0.21329(7) 0.0442(8) Uani 1 1 d . . .
H5 H 0.6790 0.1470 0.2235 0.053 Uiso 1 1 calc R . .
C6 C 0.5749(2) 0.1288(4) 0.18514(7) 0.0408(8) Uani 1 1 d . . .
C7 C 0.4675(2) 0.1591(3) 0.11196(7) 0.0354(7) Uani 1 1 d . . .
C8 C 0.5540(2) 0.2684(4) 0.10091(7) 0.0505(9) Uani 1 1 d . . .
H8A H 0.5257 0.3561 0.0871 0.076 Uiso 1 1 calc R . .
H8B H 0.6042 0.2070 0.0875 0.076 Uiso 1 1 calc R . .
H8C H 0.5885 0.3133 0.1209 0.076 Uiso 1 1 calc R . .
C9 C 0.4089(2) 0.0708(3) 0.08552(7) 0.0343(7) Uani 1 1 d . . .
C10 C 0.3462(2) -0.0575(4) 0.09402(8) 0.0509(9) Uani 1 1 d . . .
H10 H 0.3405 -0.0932 0.1168 0.061 Uiso 1 1 calc R . .
C11 C 0.2925(3) -0.1318(4) 0.06848(8) 0.0734(12) Uani 1 1 d . . .
H11 H 0.2492 -0.2211 0.0735 0.088 Uiso 1 1 calc R . .
C12 C 0.3006(3) -0.0786(4) 0.03574(8) 0.0666(11) Uani 1 1 d . . .
H12 H 0.2625 -0.1300 0.0182 0.080 Uiso 1 1 calc R . .
C13 C 0.3653(2) 0.0517(4) 0.02825(7) 0.0424(8) Uani 1 1 d . . .
C14 C 0.3743(2) 0.1170(4) -0.00648(7) 0.0443(8) Uani 1 1 d . . .
C15 C 0.4469(3) 0.2373(4) -0.01555(7) 0.0518(9) Uani 1 1 d . . .
C16 C 0.4495(3) 0.2910(4) -0.04944(8) 0.0693(11) Uani 1 1 d . . .
H16 H 0.4981 0.3717 -0.0557 0.083 Uiso 1 1 calc R . .
C17 C 0.3843(3) 0.2303(5) -0.07366(9) 0.0729(12) Uani 1 1 d . . .
H17 H 0.3881 0.2678 -0.0964 0.087 Uiso 1 1 calc R . .
C18 C 0.3128(3) 0.1137(5) -0.06471(9) 0.0694(11) Uani 1 1 d . . .
H18 H 0.2665 0.0712 -0.0812 0.083 Uiso 1 1 calc R . .
C19 C 0.3093(2) 0.0601(4) -0.03191(8) 0.0578(10) Uani 1 1 d . . .
H19 H 0.2599 -0.0202 -0.0262 0.069 Uiso 1 1 calc R . .
C20 C 0.6127(2) -0.0315(4) 0.17196(8) 0.0492(9) Uani 1 1 d . . .
H20 H 0.5675 -0.0610 0.1523 0.059 Uiso 1 1 calc R . .
C21 C 0.6006(3) -0.1636(4) 0.19837(8) 0.0695(11) Uani 1 1 d . . .
H21A H 0.6442 -0.1390 0.2180 0.104 Uiso 1 1 calc R . .
H21B H 0.6219 -0.2668 0.1886 0.104 Uiso 1 1 calc R . .
H21C H 0.5280 -0.1699 0.2055 0.104 Uiso 1 1 calc R . .
C22 C 0.7235(2) -0.0246(4) 0.15884(7) 0.0544(9) Uani 1 1 d . . .
H22A H 0.7287 0.0574 0.1411 0.082 Uiso 1 1 calc R . .
H22B H 0.7428 -0.1297 0.1495 0.082 Uiso 1 1 calc R . .
H22C H 0.7704 0.0029 0.1775 0.082 Uiso 1 1 calc R . .
C23 C 0.3542(2) 0.4304(3) 0.16975(7) 0.0422(8) Uani 1 1 d . . .
H23 H 0.3208 0.3497 0.1544 0.051 Uiso 1 1 calc R . .
C24 C 0.2756(3) 0.4740(5) 0.19692(8) 0.0768(12) Uani 1 1 d . . .
H24A H 0.2599 0.3786 0.2106 0.115 Uiso 1 1 calc R . .
H24B H 0.2120 0.5132 0.1862 0.115 Uiso 1 1 calc R . .
H24C H 0.3043 0.5584 0.2115 0.115 Uiso 1 1 calc R . .
C25 C 0.3804(3) 0.5774(4) 0.14823(9) 0.0713(11) Uani 1 1 d . . .
H25A H 0.4150 0.6582 0.1624 0.107 Uiso 1 1 calc R . .
H25B H 0.3165 0.6230 0.1388 0.107 Uiso 1 1 calc R . .
H25C H 0.4265 0.5455 0.1297 0.107 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
N1 C7 1.277(3) . ?
N1 C1 1.423(3) . ?
N2 C9 1.345(3) . ?
N2 C13 1.345(3) . ?
N3 C15 1.366(4) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
C1 C6 1.402(4) . ?
C1 C2 1.408(4) . ?
C2 C3 1.383(4) . ?
C2 C23 1.519(4) . ?
C3 C4 1.380(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(4) . ?
C5 H5 0.9500 . ?
C6 C20 1.510(4) . ?
C7 C9 1.482(4) . ?
C7 C8 1.504(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.380(4) . ?
C10 C11 1.370(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.368(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.399(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.477(4) . ?
C14 C19 1.390(4) . ?
C14 C15 1.417(4) . ?
C15 C16 1.409(4) . ?
C16 C17 1.370(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.368(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.520(4) . ?
C20 C22 1.522(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.519(4) . ?
C23 C25 1.524(4) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 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
C7 N1 C1 122.2(2) . . ?
C9 N2 C13 120.3(3) . . ?
C15 N3 H3A 120.0 . . ?
C15 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C6 C1 C2 121.7(3) . . ?
C6 C1 N1 118.3(3) . . ?
C2 C1 N1 119.7(3) . . ?
C3 C2 C1 118.2(3) . . ?
C3 C2 C23 121.3(3) . . ?
C1 C2 C23 120.6(3) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 121.4(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 117.6(3) . . ?
C5 C6 C20 120.3(3) . . ?
C1 C6 C20 122.0(3) . . ?
N1 C7 C9 116.4(3) . . ?
N1 C7 C8 125.3(2) . . ?
C9 C7 C8 118.3(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 122.2(3) . . ?
N2 C9 C7 117.1(3) . . ?
C10 C9 C7 120.7(3) . . ?
C11 C10 C9 117.8(3) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.6(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
N2 C13 C12 119.4(3) . . ?
N2 C13 C14 118.8(3) . . ?
C12 C13 C14 121.8(3) . . ?
C19 C14 C15 117.2(3) . . ?
C19 C14 C13 119.8(3) . . ?
C15 C14 C13 123.0(3) . . ?
N3 C15 C16 118.1(3) . . ?
N3 C15 C14 123.3(3) . . ?
C16 C15 C14 118.6(3) . . ?
C17 C16 C15 122.0(4) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C16 C17 C18 119.3(4) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 119.4(3) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C14 123.5(3) . . ?
C18 C19 H19 118.3 . . ?
C14 C19 H19 118.3 . . ?
C6 C20 C21 111.6(3) . . ?
C6 C20 C22 112.8(3) . . ?
C21 C20 C22 110.9(2) . . ?
C6 C20 H20 107.1 . . ?
C21 C20 H20 107.1 . . ?
C22 C20 H20 107.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C2 C23 C24 112.0(2) . . ?
C2 C23 C25 112.3(2) . . ?
C24 C23 C25 110.4(3) . . ?
C2 C23 H23 107.3 . . ?
C24 C23 H23 107.3 . . ?
C25 C23 H23 107.3 . . ?
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 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 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
C7 N1 C1 C6 -88.8(3) . . . . ?
C7 N1 C1 C2 96.9(3) . . . . ?
C6 C1 C2 C3 3.2(4) . . . . ?
N1 C1 C2 C3 177.3(2) . . . . ?
C6 C1 C2 C23 -175.8(3) . . . . ?
N1 C1 C2 C23 -1.8(4) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
C23 C2 C3 C4 178.0(3) . . . . ?
C2 C3 C4 C5 -1.3(4) . . . . ?
C3 C4 C5 C6 1.4(4) . . . . ?
C4 C5 C6 C1 0.7(4) . . . . ?
C4 C5 C6 C20 -177.0(3) . . . . ?
C2 C1 C6 C5 -3.0(4) . . . . ?
N1 C1 C6 C5 -177.2(2) . . . . ?
C2 C1 C6 C20 174.6(3) . . . . ?
N1 C1 C6 C20 0.5(4) . . . . ?
C1 N1 C7 C9 178.2(2) . . . . ?
C1 N1 C7 C8 -2.2(4) . . . . ?
C13 N2 C9 C10 2.4(4) . . . . ?
C13 N2 C9 C7 -177.2(2) . . . . ?
N1 C7 C9 N2 164.1(2) . . . . ?
C8 C7 C9 N2 -15.6(4) . . . . ?
N1 C7 C9 C10 -15.6(4) . . . . ?
C8 C7 C9 C10 164.7(3) . . . . ?
N2 C9 C10 C11 -1.0(5) . . . . ?
C7 C9 C10 C11 178.6(3) . . . . ?
C9 C10 C11 C12 -0.5(5) . . . . ?
C10 C11 C12 C13 0.7(6) . . . . ?
C9 N2 C13 C12 -2.2(4) . . . . ?
C9 N2 C13 C14 176.6(2) . . . . ?
C11 C12 C13 N2 0.6(5) . . . . ?
C11 C12 C13 C14 -178.1(3) . . . . ?
N2 C13 C14 C19 -171.8(3) . . . . ?
C12 C13 C14 C19 7.0(4) . . . . ?
N2 C13 C14 C15 8.1(4) . . . . ?
C12 C13 C14 C15 -173.2(3) . . . . ?
C19 C14 C15 N3 178.9(3) . . . . ?
C13 C14 C15 N3 -1.0(5) . . . . ?
C19 C14 C15 C16 -0.4(4) . . . . ?
C13 C14 C15 C16 179.7(3) . . . . ?
N3 C15 C16 C17 -179.4(3) . . . . ?
C14 C15 C16 C17 0.0(5) . . . . ?
C15 C16 C17 C18 0.6(5) . . . . ?
C16 C17 C18 C19 -0.7(5) . . . . ?
C17 C18 C19 C14 0.2(5) . . . . ?
C15 C14 C19 C18 0.3(5) . . . . ?
C13 C14 C19 C18 -179.8(3) . . . . ?
C5 C6 C20 C21 61.1(4) . . . . ?
C1 C6 C20 C21 -116.4(3) . . . . ?
C5 C6 C20 C22 -64.4(4) . . . . ?
C1 C6 C20 C22 118.0(3) . . . . ?
C3 C2 C23 C24 -46.9(4) . . . . ?
C1 C2 C23 C24 132.1(3) . . . . ?
C3 C2 C23 C25 78.0(3) . . . . ?
C1 C2 C23 C25 -103.0(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3B N2 0.88 2.02 2.675(4) 130.7 .

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.042

