# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 922717'
_audit_update_record             
;
2013-01-31 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
#TrackingRef 'pg-sm-2-63.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H26 I2 N4 O Pd'
_chemical_formula_sum            'C21 H26 I2 N4 O Pd'
_chemical_formula_weight         710.66

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'
I I -0.4742 1.8119 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P bcn'
_symmetry_space_group_name_Hall  '-P 2n 2ab'

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

_cell_length_a                   18.784(5)
_cell_length_b                   16.650(5)
_cell_length_c                   15.453(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4833(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      31.4

_exptl_crystal_description       Block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2720
_exptl_absorpt_coefficient_mu    3.342
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_T_max  0.7759
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34165
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4243
_reflns_number_gt                4210
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

_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)+(0.0119P)²+8.6835P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4243
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0504
_refine_ls_wR_factor_gt          0.0502
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_restrained_S_all      1.247
_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 0.824722(13) 0.246773(16) 0.729519(17) 0.02294(7) Uani 1 1 d . . .
I1 I 0.746383(13) 0.210908(15) 0.863979(15) 0.02947(7) Uani 1 1 d . . .
I2 I 0.906490(14) 0.277368(16) 0.596709(17) 0.03659(8) Uani 1 1 d . . .
O1 O 0.66611(15) 0.13871(17) 0.50462(16) 0.0382(7) Uani 1 1 d . . .
H1W H 0.6914 0.1698 0.4749 0.057 Uiso 1 1 calc R . .
N1 N 0.84850(15) 0.35865(18) 0.78383(18) 0.0253(7) Uani 1 1 d . . .
N2 N 0.84207(15) 0.07638(18) 0.68217(19) 0.0266(7) Uani 1 1 d . . .
N3 N 0.81794(16) 0.01124(18) 0.64127(19) 0.0286(7) Uani 1 1 d . . .
N4 N 0.75712(17) 0.03652(18) 0.60803(19) 0.0293(7) Uani 1 1 d . . .
C1 C 0.91337(19) 0.3781(2) 0.8133(2) 0.0324(9) Uani 1 1 d . . .
H1 H 0.9502 0.3390 0.8111 0.039 Uiso 1 1 calc R . .
C2 C 0.9284(2) 0.4529(3) 0.8467(3) 0.0383(10) Uani 1 1 d . . .
H2 H 0.9749 0.4648 0.8672 0.046 Uiso 1 1 calc R . .
C3 C 0.8761(2) 0.5100(2) 0.8504(3) 0.0369(10) Uani 1 1 d . . .
H3 H 0.8857 0.5620 0.8729 0.044 Uiso 1 1 calc R . .
C4 C 0.8092(2) 0.4904(2) 0.8206(2) 0.0356(9) Uani 1 1 d . . .
H4 H 0.7718 0.5287 0.8221 0.043 Uiso 1 1 calc R . .
C5 C 0.7972(2) 0.4146(2) 0.7887(2) 0.0298(8) Uani 1 1 d . . .
H5 H 0.7507 0.4013 0.7692 0.036 Uiso 1 1 calc R . .
C6 C 0.79989(17) 0.1424(2) 0.6760(2) 0.0229(7) Uani 1 1 d . . .
C7 C 0.74297(19) 0.1150(2) 0.6256(2) 0.0239(8) Uani 1 1 d . . .
C8 C 0.91174(18) 0.0687(2) 0.7250(2) 0.0328(9) Uani 1 1 d . . .
H8A H 0.9303 0.1230 0.7381 0.039 Uiso 1 1 calc R . .
H8B H 0.9456 0.0424 0.6848 0.039 Uiso 1 1 calc R . .
C9 C 0.90784(18) 0.0209(2) 0.8071(2) 0.0291(8) Uani 1 1 d . . .
C10 C 0.9146(2) 0.0583(3) 0.8864(3) 0.0414(10) Uani 1 1 d . . .
H10 H 0.9212 0.1148 0.8893 0.050 Uiso 1 1 calc R . .
C11 C 0.9116(3) 0.0134(3) 0.9619(3) 0.0602(14) Uani 1 1 d . . .
H11 H 0.9170 0.0391 1.0164 0.072 Uiso 1 1 calc R . .
C12 C 0.9011(3) -0.0678(3) 0.9584(3) 0.0544(13) Uani 1 1 d . . .
H12 H 0.8987 -0.0981 1.0104 0.065 Uiso 1 1 calc R . .
C13 C 0.8939(2) -0.1053(3) 0.8809(3) 0.0459(11) Uani 1 1 d . . .
H13 H 0.8859 -0.1616 0.8788 0.055 Uiso 1 1 calc R . .
C14 C 0.8982(2) -0.0618(2) 0.8052(3) 0.0392(10) Uani 1 1 d . . .
H14 H 0.8945 -0.0886 0.7511 0.047 Uiso 1 1 calc R . .
C15 C 0.7172(2) -0.0235(2) 0.5573(3) 0.0452(11) Uani 1 1 d . . .
H15A H 0.7429 -0.0747 0.5580 0.068 Uiso 1 1 calc R . .
H15B H 0.7124 -0.0047 0.4975 0.068 Uiso 1 1 calc R . .
H15C H 0.6699 -0.0308 0.5827 0.068 Uiso 1 1 calc R . .
C16 C 0.67557(19) 0.1567(2) 0.5952(2) 0.0275(8) Uani 1 1 d . . .
C17 C 0.61099(19) 0.1231(2) 0.6428(3) 0.0373(10) Uani 1 1 d . . .
H17A H 0.6180 0.1298 0.7059 0.045 Uiso 1 1 calc R . .
H17B H 0.6069 0.0649 0.6307 0.045 Uiso 1 1 calc R . .
C18 C 0.5419(2) 0.1651(3) 0.6159(3) 0.0556(13) Uani 1 1 d . . .
H18A H 0.5318 0.1534 0.5542 0.067 Uiso 1 1 calc R . .
H18B H 0.5018 0.1441 0.6508 0.067 Uiso 1 1 calc R . .
C19 C 0.5479(2) 0.2548(3) 0.6286(4) 0.0595(14) Uani 1 1 d . . .
H19A H 0.5040 0.2811 0.6073 0.071 Uiso 1 1 calc R . .
H19B H 0.5525 0.2667 0.6911 0.071 Uiso 1 1 calc R . .
C20 C 0.6113(2) 0.2887(3) 0.5812(3) 0.0426(10) Uani 1 1 d . . .
H20A H 0.6150 0.3469 0.5933 0.051 Uiso 1 1 calc R . .
H20B H 0.6043 0.2818 0.5181 0.051 Uiso 1 1 calc R . .
C21 C 0.6801(2) 0.2471(2) 0.6085(2) 0.0315(9) Uani 1 1 d . . .
H21A H 0.7203 0.2689 0.5743 0.038 Uiso 1 1 calc R . .
H21B H 0.6896 0.2586 0.6703 0.038 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 C6 1.980(3) . ?
Pd1 N1 2.091(3) . ?
Pd1 I2 2.6135(6) . ?
Pd1 I1 2.6152(6) . ?
O1 C16 1.442(4) . ?
O1 H1W 0.8400 . ?
N1 C1 1.341(4) . ?
N1 C5 1.343(5) . ?
N2 N3 1.335(4) . ?
N2 C6 1.358(4) . ?
N2 C8 1.472(4) . ?
N3 N4 1.321(4) . ?
N4 C7 1.362(5) . ?
N4 C15 1.474(5) . ?
C1 C2 1.377(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.368(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.399(5) . ?
C7 C16 1.518(5) . ?
C8 C9 1.501(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.380(5) . ?
C9 C14 1.389(5) . ?
C10 C11 1.387(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.367(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.358(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.523(5) . ?
C16 C17 1.526(5) . ?
C17 C18 1.532(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.511(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.507(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.526(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?

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
C6 Pd1 N1 178.27(13) . . ?
C6 Pd1 I2 88.95(9) . . ?
N1 Pd1 I2 90.92(8) . . ?
C6 Pd1 I1 89.93(9) . . ?
N1 Pd1 I1 90.27(8) . . ?
I2 Pd1 I1 177.550(15) . . ?
C16 O1 H1W 109.5 . . ?
C1 N1 C5 117.7(3) . . ?
C1 N1 Pd1 123.1(3) . . ?
C5 N1 Pd1 119.2(2) . . ?
N3 N2 C6 115.2(3) . . ?
N3 N2 C8 116.4(3) . . ?
C6 N2 C8 128.3(3) . . ?
N4 N3 N2 102.6(3) . . ?
N3 N4 C7 113.4(3) . . ?
N3 N4 C15 115.5(3) . . ?
C7 N4 C15 131.1(3) . . ?
N1 C1 C2 122.1(4) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 118.4(4) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 122.7(4) . . ?
N1 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
N2 C6 C7 102.8(3) . . ?
N2 C6 Pd1 122.9(2) . . ?
C7 C6 Pd1 134.3(3) . . ?
N4 C7 C6 105.9(3) . . ?
N4 C7 C16 122.6(3) . . ?
C6 C7 C16 131.4(3) . . ?
N2 C8 C9 112.5(3) . . ?
N2 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N2 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C14 118.6(4) . . ?
C10 C9 C8 120.5(4) . . ?
C14 C9 C8 120.9(4) . . ?
C9 C10 C11 120.0(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.4(4) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C11 120.3(4) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 120.1(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 120.7(4) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O1 C16 C7 108.0(3) . . ?
O1 C16 C21 110.1(3) . . ?
C7 C16 C21 111.3(3) . . ?
O1 C16 C17 107.1(3) . . ?
C7 C16 C17 110.2(3) . . ?
C21 C16 C17 110.0(3) . . ?
C16 C17 C18 112.0(3) . . ?
C16 C17 H17A 109.2 . . ?
C18 C17 H17A 109.2 . . ?
C16 C17 H17B 109.2 . . ?
C18 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C19 C18 C17 110.7(4) . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 111.5(4) . . ?
C20 C19 H19A 109.3 . . ?
C18 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
C18 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 C21 111.4(3) . . ?
C19 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C16 C21 C20 111.3(3) . . ?
C16 C21 H21A 109.4 . . ?
C20 C21 H21A 109.4 . . ?
C16 C21 H21B 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?

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
C6 Pd1 N1 C1 -153(4) . . . . ?
I2 Pd1 N1 C1 -67.3(3) . . . . ?
I1 Pd1 N1 C1 110.5(3) . . . . ?
C6 Pd1 N1 C5 26(4) . . . . ?
I2 Pd1 N1 C5 111.7(3) . . . . ?
I1 Pd1 N1 C5 -70.5(3) . . . . ?
C6 N2 N3 N4 -0.6(4) . . . . ?
C8 N2 N3 N4 -178.2(3) . . . . ?
N2 N3 N4 C7 0.8(4) . . . . ?
N2 N3 N4 C15 179.6(3) . . . . ?
C5 N1 C1 C2 -0.8(5) . . . . ?
Pd1 N1 C1 C2 178.2(3) . . . . ?
N1 C1 C2 C3 -0.1(6) . . . . ?
C1 C2 C3 C4 0.4(6) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
C1 N1 C5 C4 1.4(5) . . . . ?
Pd1 N1 C5 C4 -177.7(3) . . . . ?
C3 C4 C5 N1 -1.1(6) . . . . ?
N3 N2 C6 C7 0.1(4) . . . . ?
C8 N2 C6 C7 177.4(3) . . . . ?
N3 N2 C6 Pd1 -179.0(2) . . . . ?
C8 N2 C6 Pd1 -1.7(5) . . . . ?
N1 Pd1 C6 N2 167(4) . . . . ?
I2 Pd1 C6 N2 81.8(3) . . . . ?
I1 Pd1 C6 N2 -96.1(3) . . . . ?
N1 Pd1 C6 C7 -11(4) . . . . ?
I2 Pd1 C6 C7 -97.1(3) . . . . ?
I1 Pd1 C6 C7 85.1(3) . . . . ?
N3 N4 C7 C6 -0.8(4) . . . . ?
C15 N4 C7 C6 -179.3(4) . . . . ?
N3 N4 C7 C16 -179.1(3) . . . . ?
C15 N4 C7 C16 2.4(6) . . . . ?
N2 C6 C7 N4 0.4(4) . . . . ?
Pd1 C6 C7 N4 179.4(3) . . . . ?
N2 C6 C7 C16 178.4(3) . . . . ?
Pd1 C6 C7 C16 -2.5(6) . . . . ?
N3 N2 C8 C9 -74.8(4) . . . . ?
C6 N2 C8 C9 107.9(4) . . . . ?
N2 C8 C9 C10 -108.1(4) . . . . ?
N2 C8 C9 C14 72.6(4) . . . . ?
C14 C9 C10 C11 0.0(6) . . . . ?
C8 C9 C10 C11 -179.3(4) . . . . ?
C9 C10 C11 C12 -0.9(7) . . . . ?
C10 C11 C12 C13 0.5(8) . . . . ?
C11 C12 C13 C14 0.9(7) . . . . ?
C12 C13 C14 C9 -1.8(6) . . . . ?
C10 C9 C14 C13 1.4(6) . . . . ?
C8 C9 C14 C13 -179.3(4) . . . . ?
N4 C7 C16 O1 -48.0(4) . . . . ?
C6 C7 C16 O1 134.2(4) . . . . ?
N4 C7 C16 C21 -169.0(3) . . . . ?
C6 C7 C16 C21 13.2(5) . . . . ?
N4 C7 C16 C17 68.7(4) . . . . ?
C6 C7 C16 C17 -109.1(4) . . . . ?
O1 C16 C17 C18 -64.3(4) . . . . ?
C7 C16 C17 C18 178.4(3) . . . . ?
C21 C16 C17 C18 55.4(4) . . . . ?
C16 C17 C18 C19 -55.5(5) . . . . ?
C17 C18 C19 C20 55.4(6) . . . . ?
C18 C19 C20 C21 -56.2(5) . . . . ?
O1 C16 C21 C20 62.5(4) . . . . ?
C7 C16 C21 C20 -177.8(3) . . . . ?
C17 C16 C21 C20 -55.3(4) . . . . ?
C19 C20 C21 C16 56.3(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.072


####################################################################### 
# 
# 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_PG165
_database_code_depnum_ccdc_archive 'CCDC 926236'
_audit_update_record             
;
2013-02-24 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
#TrackingRef 'PG165_150K_22fev13_APEX_VD_archive.cif'


_audit_creation_date             2013-02-22T10:06:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C35 H38 I2 N3 O1 P1 Pd1'
_chemical_formula_sum            'C35 H38 I2 N3 O P Pd'
_chemical_formula_weight         907.85
_chemical_compound_source        'synthesis as described'

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.1205(3)
_cell_length_b                   16.2538(5)
_cell_length_c                   26.3092(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6893.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6962
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.34
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.26
_exptl_crystal_density_diffrn    1.75
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3552
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    2.408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
[Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_T_max  0.535


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

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_number            30914
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             7871
_reflns_number_gt                5833
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
WinGX publication routines (Farrugia, 2012),
CRYSCAL (T. Roisnel, local program)
;

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

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0188P)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_number_reflns         7871
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0644
_refine_ls_wR_factor_gt          0.0584
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.119


#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.15602(19) 0.0902(2) 0.55743(11) 0.0181(7) Uani 1 1 d . . .
C2 C 0.19329(19) 0.1380(2) 0.51957(11) 0.0234(8) Uani 1 1 d . . .
H2 H 0.1863 0.196 0.52 0.028 Uiso 1 1 calc R . .
C3 C 0.2401(2) 0.1020(2) 0.48168(12) 0.0258(9) Uani 1 1 d . . .
H3 H 0.2638 0.1351 0.4557 0.031 Uiso 1 1 calc R . .
C4 C 0.2524(2) 0.0178(3) 0.48169(13) 0.0305(9) Uani 1 1 d . . .
H4 H 0.2856 -0.007 0.4561 0.037 Uiso 1 1 calc R . .
C5 C 0.2163(2) -0.0304(2) 0.51912(12) 0.0285(9) Uani 1 1 d . . .
H5 H 0.2244 -0.0883 0.519 0.034 Uiso 1 1 calc R . .
C6 C 0.1684(2) 0.0056(2) 0.55676(12) 0.0234(8) Uani 1 1 d . . .
H6 H 0.1439 -0.0278 0.5823 0.028 Uiso 1 1 calc R . .
C11 C 0.03262(19) 0.0534(2) 0.62935(11) 0.0181(7) Uani 1 1 d . . .
C12 C -0.0392(2) 0.0204(3) 0.60867(13) 0.0290(9) Uani 1 1 d . . .
H12 H -0.0676 0.0489 0.5824 0.035 Uiso 1 1 calc R . .
C13 C -0.0698(2) -0.0546(3) 0.62643(14) 0.0393(11) Uani 1 1 d . . .
H13 H -0.1186 -0.0773 0.6119 0.047 Uiso 1 1 calc R . .
C14 C -0.0297(2) -0.0958(2) 0.66489(14) 0.0355(10) Uani 1 1 d . . .
H14 H -0.051 -0.1467 0.677 0.043 Uiso 1 1 calc R . .
C15 C 0.0414(2) -0.0632(3) 0.68590(13) 0.0323(9) Uani 1 1 d . . .
H15 H 0.0693 -0.092 0.7123 0.039 Uiso 1 1 calc R . .
C16 C 0.0720(2) 0.0106(2) 0.66886(12) 0.0253(9) Uani 1 1 d . . .
H16 H 0.1205 0.0329 0.684 0.03 Uiso 1 1 calc R . .
C21 C 0.01816(18) 0.1961(2) 0.56008(11) 0.0186(7) Uani 1 1 d . . .
C22 C -0.00670(19) 0.2760(2) 0.57150(13) 0.0248(8) Uani 1 1 d . . .
H22 H 0.0078 0.2995 0.6033 0.03 Uiso 1 1 calc R . .
C23 C -0.0523(2) 0.3214(3) 0.53704(13) 0.0318(9) Uani 1 1 d . . .
H23 H -0.0679 0.3764 0.5448 0.038 Uiso 1 1 calc R . .
C24 C -0.0753(2) 0.2866(3) 0.49103(13) 0.0314(10) Uani 1 1 d . . .
H24 H -0.107 0.3176 0.4673 0.038 Uiso 1 1 calc R . .
C25 C -0.0525(2) 0.2072(3) 0.47965(12) 0.0290(9) Uani 1 1 d . . .
H25 H -0.0689 0.1833 0.4483 0.035 Uiso 1 1 calc R . .
C26 C -0.00558(19) 0.1619(2) 0.51367(12) 0.0241(8) Uani 1 1 d . . .
H26 H 0.0105 0.1073 0.5054 0.029 Uiso 1 1 calc R . .
C31 C 0.1437(2) 0.1999(2) 0.84705(13) 0.0278(8) Uani 1 1 d . . .
H31 H 0.1007 0.2067 0.8227 0.033 Uiso 1 1 calc R . .
C32 C 0.1243(2) 0.1961(2) 0.89797(14) 0.0343(9) Uani 1 1 d . . .
H32 H 0.0683 0.2013 0.9087 0.041 Uiso 1 1 calc R . .
C33 C 0.1865(3) 0.1846(2) 0.93329(14) 0.0376(10) Uani 1 1 d . . .
H33 H 0.1732 0.18 0.9684 0.045 Uiso 1 1 calc R . .
C34 C 0.2677(2) 0.1799(3) 0.91772(13) 0.0366(10) Uani 1 1 d . . .
H34 H 0.3106 0.1735 0.9422 0.044 Uiso 1 1 calc R . .
C35 C 0.2875(2) 0.1844(2) 0.86692(12) 0.0279(9) Uani 1 1 d . . .
H35 H 0.3438 0.1809 0.8565 0.034 Uiso 1 1 calc R . .
C36 C 0.2255(2) 0.1938(2) 0.83094(12) 0.0213(8) Uani 1 1 d . . .
C37 C 0.2458(2) 0.2017(2) 0.77538(12) 0.0252(8) Uani 1 1 d . . .
H37A H 0.3047 0.1869 0.7696 0.03 Uiso 1 1 calc R . .
H37B H 0.2109 0.1635 0.7554 0.03 Uiso 1 1 calc R . .
N38 N 0.23113(16) 0.28645(18) 0.75842(9) 0.0202(6) Uani 1 1 d . . .
N39 N 0.26079(17) 0.34569(19) 0.78799(10) 0.0251(7) Uani 1 1 d . . .
N40 N 0.23868(16) 0.41399(18) 0.76440(9) 0.0206(6) Uani 1 1 d . . .
C41 C 0.19630(18) 0.3985(2) 0.71994(11) 0.0152(7) Uani 1 1 d . . .
C42 C 0.19122(18) 0.3134(2) 0.71600(11) 0.0156(7) Uani 1 1 d . . .
C43 C 0.2611(2) 0.4915(2) 0.78993(12) 0.0285(9) Uani 1 1 d . . .
H43A H 0.2101 0.5237 0.7966 0.034 Uiso 1 1 calc R . .
H43B H 0.297 0.5244 0.7671 0.034 Uiso 1 1 calc R . .
C44 C 0.3055(2) 0.4768(2) 0.83899(13) 0.0346(10) Uani 1 1 d . . .
H44A H 0.2693 0.4461 0.8622 0.052 Uiso 1 1 calc R . .
H44B H 0.3202 0.5297 0.8544 0.052 Uiso 1 1 calc R . .
H44C H 0.356 0.445 0.8325 0.052 Uiso 1 1 calc R . .
C45 C 0.16051(19) 0.4647(2) 0.68663(12) 0.0183(7) Uani 1 1 d . . .
C46 C 0.07526(19) 0.4914(2) 0.70693(12) 0.0236(8) Uani 1 1 d . . .
H46A H 0.04 0.442 0.7113 0.028 Uiso 1 1 calc R . .
H46B H 0.0825 0.5171 0.7407 0.028 Uiso 1 1 calc R . .
C47 C 0.0310(2) 0.5521(2) 0.67180(13) 0.0301(9) Uani 1 1 d . . .
H47A H -0.025 0.5642 0.6854 0.036 Uiso 1 1 calc R . .
H47B H 0.0625 0.6043 0.6705 0.036 Uiso 1 1 calc R . .
C48 C 0.0232(2) 0.5168(3) 0.61834(13) 0.0329(10) Uani 1 1 d . . .
H48A H -0.0038 0.5579 0.5959 0.039 Uiso 1 1 calc R . .
H48B H -0.0124 0.4672 0.6192 0.039 Uiso 1 1 calc R . .
C49 C 0.1080(2) 0.4944(2) 0.59669(12) 0.0267(9) Uani 1 1 d . . .
H49A H 0.1422 0.5446 0.5932 0.032 Uiso 1 1 calc R . .
H49B H 0.1011 0.4698 0.5625 0.032 Uiso 1 1 calc R . .
C50 C 0.15204(19) 0.4328(2) 0.63185(11) 0.0197(8) Uani 1 1 d . . .
H50A H 0.208 0.4211 0.6181 0.024 Uiso 1 1 calc R . .
H50B H 0.1205 0.3806 0.6322 0.024 Uiso 1 1 calc R . .
O51 O 0.21863(13) 0.53187(15) 0.68856(8) 0.0241(6) Uani 1 1 d . . .
H51 H 0.204 0.5686 0.668 0.036 Uiso 1 1 calc R . .
P1 P 0.08798(5) 0.14158(6) 0.60374(3) 0.01756(19) Uani 1 1 d . . .
Pd1 Pd 0.144632(14) 0.231830(17) 0.664363(8) 0.01513(7) Uani 1 1 d . . .
I1 I 0.004799(12) 0.233607(17) 0.715068(8) 0.02527(7) Uani 1 1 d . . .
I2 I 0.294669(12) 0.232679(16) 0.627936(8) 0.02328(7) Uani 1 1 d . . .





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

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.389(5) . ?
C1 C2 1.399(4) . ?
C1 P1 1.840(3) . ?
C2 C3 1.380(4) . ?
C2 H2 0.95 . ?
C3 C4 1.383(5) . ?
C3 H3 0.95 . ?
C4 C5 1.387(5) . ?
C4 H4 0.95 . ?
C5 C6 1.385(4) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C11 C12 1.387(4) . ?
C11 C16 1.403(4) . ?
C11 P1 1.818(3) . ?
C12 C13 1.396(5) . ?
C12 H12 0.95 . ?
C13 C14 1.375(5) . ?
C13 H13 0.95 . ?
C14 C15 1.378(5) . ?
C14 H14 0.95 . ?
C15 C16 1.373(5) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C21 C22 1.391(5) . ?
C21 C26 1.395(4) . ?
C21 P1 1.836(3) . ?
C22 C23 1.381(5) . ?
C22 H22 0.95 . ?
C23 C24 1.387(5) . ?
C23 H23 0.95 . ?
C24 C25 1.375(5) . ?
C24 H24 0.95 . ?
C25 C26 1.383(5) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C31 C32 1.377(5) . ?
C31 C36 1.388(4) . ?
C31 H31 0.95 . ?
C32 C33 1.379(5) . ?
C32 H32 0.95 . ?
C33 C34 1.374(5) . ?
C33 H33 0.95 . ?
C34 C35 1.376(4) . ?
C34 H34 0.95 . ?
C35 C36 1.386(4) . ?
C35 H35 0.95 . ?
C36 C37 1.504(4) . ?
C37 N38 1.467(4) . ?
C37 H37A 0.99 . ?
C37 H37B 0.99 . ?
N38 N39 1.327(4) . ?
N38 C42 1.361(4) . ?
N39 N40 1.321(4) . ?
N40 C41 1.378(4) . ?
N40 C43 1.473(4) . ?
C41 C42 1.389(4) . ?
C41 C45 1.503(4) . ?
C42 Pd1 2.042(3) . ?
C43 C44 1.495(4) . ?
C43 H43A 0.99 . ?
C43 H43B 0.99 . ?
C44 H44A 0.98 . ?
C44 H44B 0.98 . ?
C44 H44C 0.98 . ?
C45 O51 1.440(4) . ?
C45 C50 1.537(4) . ?
C45 C46 1.537(4) . ?
C46 C47 1.529(5) . ?
C46 H46A 0.99 . ?
C46 H46B 0.99 . ?
C47 C48 1.524(5) . ?
C47 H47A 0.99 . ?
C47 H47B 0.99 . ?
C48 C49 1.526(4) . ?
C48 H48A 0.99 . ?
C48 H48B 0.99 . ?
C49 C50 1.536(4) . ?
C49 H49A 0.99 . ?
C49 H49B 0.99 . ?
C50 H50A 0.99 . ?
C50 H50B 0.99 . ?
O51 H51 0.84 . ?
P1 Pd1 2.3515(9) . ?
Pd1 I2 2.6017(3) . ?
Pd1 I1 2.6195(3) . ?


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
C6 C1 C2 118.6(3) . . ?
C6 C1 P1 122.9(2) . . ?
C2 C1 P1 118.4(3) . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H4 120 . . ?
C5 C4 H4 120 . . ?
C6 C5 C4 120.2(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 120.5(3) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C12 C11 C16 118.4(3) . . ?
C12 C11 P1 124.7(3) . . ?
C16 C11 P1 116.3(2) . . ?
C11 C12 C13 120.1(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 120.4(4) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 120.0(4) . . ?
C13 C14 H14 120 . . ?
C15 C14 H14 120 . . ?
C16 C15 C14 120.3(4) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C11 120.8(3) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
C22 C21 C26 118.8(3) . . ?
C22 C21 P1 119.5(2) . . ?
C26 C21 P1 121.6(3) . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 119.8(4) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 120.1(3) . . ?
C25 C24 H24 120 . . ?
C23 C24 H24 120 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 120.3(3) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
C32 C31 C36 120.6(3) . . ?
C32 C31 H31 119.7 . . ?
C36 C31 H31 119.7 . . ?
C31 C32 C33 119.8(3) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 119.9(3) . . ?
C34 C33 H33 120 . . ?
C32 C33 H33 120 . . ?
C33 C34 C35 120.5(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C36 120.1(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 119.0(3) . . ?
C35 C36 C37 121.1(3) . . ?
C31 C36 C37 119.9(3) . . ?
N38 C37 C36 109.9(3) . . ?
N38 C37 H37A 109.7 . . ?
C36 C37 H37A 109.7 . . ?
N38 C37 H37B 109.7 . . ?
C36 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
N39 N38 C42 114.7(3) . . ?
N39 N38 C37 116.4(2) . . ?
C42 N38 C37 128.9(3) . . ?
N40 N39 N38 103.7(2) . . ?
N39 N40 C41 112.3(3) . . ?
N39 N40 C43 116.0(3) . . ?
C41 N40 C43 131.7(3) . . ?
N40 C41 C42 105.9(3) . . ?
N40 C41 C45 123.7(3) . . ?
C42 C41 C45 130.3(3) . . ?
N38 C42 C41 103.4(3) . . ?
N38 C42 Pd1 120.7(2) . . ?
C41 C42 Pd1 135.9(2) . . ?
N40 C43 C44 112.0(3) . . ?
N40 C43 H43A 109.2 . . ?
C44 C43 H43A 109.2 . . ?
N40 C43 H43B 109.2 . . ?
C44 C43 H43B 109.2 . . ?
H43A C43 H43B 107.9 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O51 C45 C41 105.8(2) . . ?
O51 C45 C50 110.2(3) . . ?
C41 C45 C50 109.9(3) . . ?
O51 C45 C46 110.8(3) . . ?
C41 C45 C46 110.0(3) . . ?
C50 C45 C46 110.0(3) . . ?
C47 C46 C45 112.9(3) . . ?
C47 C46 H46A 109 . . ?
C45 C46 H46A 109 . . ?
C47 C46 H46B 109 . . ?
C45 C46 H46B 109 . . ?
H46A C46 H46B 107.8 . . ?
C48 C47 C46 110.7(3) . . ?
C48 C47 H47A 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 108.1 . . ?
C47 C48 C49 111.1(3) . . ?
C47 C48 H48A 109.4 . . ?
C49 C48 H48A 109.4 . . ?
C47 C48 H48B 109.4 . . ?
C49 C48 H48B 109.4 . . ?
H48A C48 H48B 108 . . ?
C48 C49 C50 110.2(3) . . ?
C48 C49 H49A 109.6 . . ?
C50 C49 H49A 109.6 . . ?
C48 C49 H49B 109.6 . . ?
C50 C49 H49B 109.6 . . ?
H49A C49 H49B 108.1 . . ?
C49 C50 C45 112.7(3) . . ?
C49 C50 H50A 109 . . ?
C45 C50 H50A 109 . . ?
C49 C50 H50B 109 . . ?
C45 C50 H50B 109 . . ?
H50A C50 H50B 107.8 . . ?
C45 O51 H51 109.5 . . ?
C11 P1 C21 108.15(15) . . ?
C11 P1 C1 100.37(15) . . ?
C21 P1 C1 99.81(14) . . ?
C11 P1 Pd1 115.54(10) . . ?
C21 P1 Pd1 111.17(12) . . ?
C1 P1 Pd1 120.06(10) . . ?
C42 Pd1 P1 177.97(9) . . ?
C42 Pd1 I2 84.24(8) . . ?
P1 Pd1 I2 96.58(2) . . ?
C42 Pd1 I1 88.31(8) . . ?
P1 Pd1 I1 91.04(2) . . ?
I2 Pd1 I1 170.950(12) . . ?


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
C6 C1 C2 C3 1.3(5) . . . . ?
P1 C1 C2 C3 -175.3(2) . . . . ?
C1 C2 C3 C4 -1.7(5) . . . . ?
C2 C3 C4 C5 1.3(5) . . . . ?
C3 C4 C5 C6 -0.5(5) . . . . ?
C4 C5 C6 C1 0.0(5) . . . . ?
C2 C1 C6 C5 -0.4(5) . . . . ?
P1 C1 C6 C5 176.0(3) . . . . ?
C16 C11 C12 C13 -1.3(5) . . . . ?
P1 C11 C12 C13 170.1(3) . . . . ?
C11 C12 C13 C14 0.8(6) . . . . ?
C12 C13 C14 C15 -0.4(6) . . . . ?
C13 C14 C15 C16 0.5(6) . . . . ?
C14 C15 C16 C11 -1.1(5) . . . . ?
C12 C11 C16 C15 1.5(5) . . . . ?
P1 C11 C16 C15 -170.7(3) . . . . ?
C26 C21 C22 C23 -1.6(5) . . . . ?
P1 C21 C22 C23 173.5(3) . . . . ?
C21 C22 C23 C24 1.5(5) . . . . ?
C22 C23 C24 C25 -0.3(5) . . . . ?
C23 C24 C25 C26 -0.8(5) . . . . ?
C24 C25 C26 C21 0.7(5) . . . . ?
C22 C21 C26 C25 0.5(5) . . . . ?
P1 C21 C26 C25 -174.5(3) . . . . ?
C36 C31 C32 C33 -1.1(6) . . . . ?
C31 C32 C33 C34 2.2(6) . . . . ?
C32 C33 C34 C35 -1.7(6) . . . . ?
C33 C34 C35 C36 0.1(6) . . . . ?
C34 C35 C36 C31 0.9(6) . . . . ?
C34 C35 C36 C37 177.9(4) . . . . ?
C32 C31 C36 C35 -0.4(6) . . . . ?
C32 C31 C36 C37 -177.4(4) . . . . ?
C35 C36 C37 N38 -108.3(4) . . . . ?
C31 C36 C37 N38 68.6(4) . . . . ?
C36 C37 N38 N39 46.4(4) . . . . ?
C36 C37 N38 C42 -134.0(3) . . . . ?
C42 N38 N39 N40 0.7(3) . . . . ?
C37 N38 N39 N40 -179.6(3) . . . . ?
N38 N39 N40 C41 -0.8(3) . . . . ?
N38 N39 N40 C43 177.9(3) . . . . ?
N39 N40 C41 C42 0.5(3) . . . . ?
C43 N40 C41 C42 -177.8(3) . . . . ?
N39 N40 C41 C45 177.2(3) . . . . ?
C43 N40 C41 C45 -1.2(5) . . . . ?
N39 N38 C42 C41 -0.4(3) . . . . ?
C37 N38 C42 C41 179.9(3) . . . . ?
N39 N38 C42 Pd1 177.9(2) . . . . ?
C37 N38 C42 Pd1 -1.8(4) . . . . ?
N40 C41 C42 N38 -0.1(3) . . . . ?
C45 C41 C42 N38 -176.4(3) . . . . ?
N40 C41 C42 Pd1 -178.0(2) . . . . ?
C45 C41 C42 Pd1 5.7(5) . . . . ?
N39 N40 C43 C44 -0.2(4) . . . . ?
C41 N40 C43 C44 178.1(3) . . . . ?
N40 C41 C45 O51 36.6(4) . . . . ?
C42 C41 C45 O51 -147.6(3) . . . . ?
N40 C41 C45 C50 155.6(3) . . . . ?
C42 C41 C45 C50 -28.6(4) . . . . ?
N40 C41 C45 C46 -83.1(4) . . . . ?
C42 C41 C45 C46 92.6(4) . . . . ?
O51 C45 C46 C47 69.4(3) . . . . ?
C41 C45 C46 C47 -173.9(3) . . . . ?
C50 C45 C46 C47 -52.8(4) . . . . ?
C45 C46 C47 C48 55.3(4) . . . . ?
C46 C47 C48 C49 -57.0(4) . . . . ?
C47 C48 C49 C50 57.2(4) . . . . ?
C48 C49 C50 C45 -55.9(4) . . . . ?
O51 C45 C50 C49 -69.3(3) . . . . ?
C41 C45 C50 C49 174.4(3) . . . . ?
C46 C45 C50 C49 53.1(4) . . . . ?
C12 C11 P1 C21 16.9(3) . . . . ?
C16 C11 P1 C21 -171.5(2) . . . . ?
C12 C11 P1 C1 -87.2(3) . . . . ?
C16 C11 P1 C1 84.5(3) . . . . ?
C12 C11 P1 Pd1 142.2(3) . . . . ?
C16 C11 P1 Pd1 -46.2(3) . . . . ?
C22 C21 P1 C11 115.9(3) . . . . ?
C26 C21 P1 C11 -69.2(3) . . . . ?
C22 C21 P1 C1 -139.7(3) . . . . ?
C26 C21 P1 C1 35.2(3) . . . . ?
C22 C21 P1 Pd1 -12.0(3) . . . . ?
C26 C21 P1 Pd1 162.9(2) . . . . ?
C6 C1 P1 C11 -13.6(3) . . . . ?
C2 C1 P1 C11 162.9(2) . . . . ?
C6 C1 P1 C21 -124.2(3) . . . . ?
C2 C1 P1 C21 52.2(3) . . . . ?
C6 C1 P1 Pd1 114.2(3) . . . . ?
C2 C1 P1 Pd1 -69.4(3) . . . . ?
N38 C42 Pd1 I2 -84.3(2) . . . . ?
C41 C42 Pd1 I2 93.3(3) . . . . ?
N38 C42 Pd1 I1 90.5(2) . . . . ?
C41 C42 Pd1 I1 -91.9(3) . . . . ?
C11 P1 Pd1 C42 -119(2) . . . . ?
C21 P1 Pd1 C42 5(2) . . . . ?
C1 P1 Pd1 C42 121(2) . . . . ?
C11 P1 Pd1 I2 127.67(12) . . . . ?
C21 P1 Pd1 I2 -108.60(10) . . . . ?
C1 P1 Pd1 I2 7.20(13) . . . . ?
C11 P1 Pd1 I1 -47.43(12) . . . . ?
C21 P1 Pd1 I1 76.30(10) . . . . ?
C1 P1 Pd1 I1 -167.89(13) . . . . ?
####################################################################### 
# 
# 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_pg112
_database_code_depnum_ccdc_archive 'CCDC 926965'
_audit_update_record             
;
2013-02-28 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
#TrackingRef 'PG112.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H28 I2 N4 O Pd'
_chemical_formula_sum            'C22 H28 I2 N4 O Pd'
_chemical_formula_weight         724.68


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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C c'

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

_cell_length_a                   18.443(10)
_cell_length_b                   17.780(11)
_cell_length_c                   8.017(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.425(7)
_cell_angle_gamma                90.00
_cell_volume                     2463(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3570
_cell_measurement_theta_min      3.51
_cell_measurement_theta_max      25.360

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    3.280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_T_max  0.394
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Rigaku CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7282
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         25.36
_reflns_number_total             4514
_reflns_number_gt                3570
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku CrystalClear'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Rigaku SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Rigaku SHELXTL (Sheldrick, 2008)'

_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)+(0.1184P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_number_reflns         3685
_refine_ls_number_parameters     272
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1490
_refine_ls_wR_factor_gt          0.1481
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.066
_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
I1 I 0.48486(3) 0.59073(4) 0.69879(7) 0.0278(2) Uani 1 1 d . . .
I2 I 0.44957(4) 0.78192(3) 0.18004(8) 0.0228(2) Uani 1 1 d . . .
Pd1 Pd 0.46789(5) 0.68554(4) 0.44028(11) 0.0177(2) Uani 1 1 d . . .
O1 O 0.3433(5) 0.8558(4) 0.7463(10) 0.0224(16) Uani 1 1 d . . .
H1A H 0.2951 0.8617 0.7040 0.034 Uiso 1 1 calc R . .
N1 N 0.2998(6) 0.6658(5) 0.3666(12) 0.0193(18) Uani 1 1 d . . .
N2 N 0.2341(6) 0.6953(5) 0.3726(12) 0.0187(19) Uani 1 1 d . . .
N3 N 0.2550(5) 0.7599(5) 0.4533(12) 0.0205(18) Uani 1 1 d . . .
N4 N 0.5784(6) 0.6609(5) 0.4435(13) 0.0235(19) Uani 1 1 d . . .
C1B C 0.3343(7) 0.7725(5) 0.5035(15) 0.018(2) Uani 1 1 d . . .
C2B C 0.3623(6) 0.7106(6) 0.4386(14) 0.019(2) Uani 1 1 d . . .
C3B C 0.6360(7) 0.7124(5) 0.4955(15) 0.021(2) Uani 1 1 d . . .
H3BA H 0.6240 0.7620 0.5212 0.025 Uiso 1 1 calc R . .
C4B C 0.7116(8) 0.6957(7) 0.5130(18) 0.033(3) Uani 1 1 d . . .
H4BA H 0.7505 0.7333 0.5509 0.040 Uiso 1 1 calc R . .
C5B C 0.7305(8) 0.6235(7) 0.4747(17) 0.032(3) Uani 1 1 d . . .
H5BA H 0.7819 0.6105 0.4854 0.039 Uiso 1 1 calc R . .
C6B C 0.6719(9) 0.5723(8) 0.421(2) 0.046(4) Uani 1 1 d . . .
H6BA H 0.6827 0.5223 0.3952 0.055 Uiso 1 1 calc R . .
C7B C 0.5977(10) 0.5914(7) 0.404(3) 0.049(4) Uani 1 1 d . . .
H7BA H 0.5582 0.5545 0.3629 0.059 Uiso 1 1 calc R . .
C8B C 0.3187(7) 0.5987(5) -0.0007(17) 0.024(2) Uani 1 1 d . . .
H8BA H 0.3727 0.6012 0.0643 0.029 Uiso 1 1 calc R . .
C9B C 0.2923(7) 0.6025(6) -0.1842(17) 0.030(3) Uani 1 1 d . . .
H9BA H 0.3279 0.6088 -0.2448 0.036 Uiso 1 1 calc R . .
C10B C 0.2118(8) 0.5971(6) -0.2821(16) 0.030(2) Uani 1 1 d . . .
H10A H 0.1927 0.5985 -0.4085 0.036 Uiso 1 1 calc R . .
C11B C 0.1619(8) 0.5897(6) -0.1880(18) 0.030(3) Uani 1 1 d . . .
H11A H 0.1080 0.5858 -0.2519 0.036 Uiso 1 1 calc R . .
C12B C 0.1878(8) 0.5878(6) -0.0061(18) 0.028(3) Uani 1 1 d . . .
H12A H 0.1522 0.5840 0.0552 0.033 Uiso 1 1 calc R . .
C13B C 0.2676(7) 0.5915(5) 0.0889(16) 0.022(2) Uani 1 1 d . . .
C14A C 0.2953(7) 0.5899(5) 0.2876(16) 0.026(2) Uani 1 1 d . . .
H14A H 0.2598 0.5584 0.3262 0.031 Uiso 1 1 calc R . .
H14B H 0.3472 0.5663 0.3329 0.031 Uiso 1 1 calc R . .
C15A C 0.3543(6) 0.9104(5) 0.4823(14) 0.020(2) Uani 1 1 d . . .
H15A H 0.3726 0.9008 0.3820 0.024 Uiso 1 1 calc R . .
H15B H 0.2977 0.9184 0.4324 0.024 Uiso 1 1 calc R . .
C16A C 0.3933(7) 0.9819(5) 0.5803(14) 0.020(2) Uani 1 1 d . . .
H16A H 0.3830 1.0240 0.4945 0.024 Uiso 1 1 calc R . .
H16B H 0.3705 0.9950 0.6715 0.024 Uiso 1 1 calc R . .
C17A C 0.4803(8) 0.9718(6) 0.6697(17) 0.028(3) Uani 1 1 d . . .
H17A H 0.5020 1.0163 0.7450 0.033 Uiso 1 1 calc R . .
H17B H 0.5044 0.9688 0.5773 0.033 Uiso 1 1 calc R . .
C18A C 0.5001(8) 0.9009(6) 0.7847(15) 0.028(2) Uani 1 1 d . . .
H18A H 0.5569 0.8937 0.8284 0.034 Uiso 1 1 calc R . .
H18B H 0.4845 0.9084 0.8898 0.034 Uiso 1 1 calc R . .
C19A C 0.4626(6) 0.8319(5) 0.6908(15) 0.021(2) Uani 1 1 d . . .
H19A H 0.4749 0.7893 0.7757 0.026 Uiso 1 1 calc R . .
H19B H 0.4836 0.8199 0.5959 0.026 Uiso 1 1 calc R . .
C20A C 0.3718(6) 0.8412(5) 0.6055(13) 0.019(2) Uani 1 1 d . . .
C21A C 0.1930(6) 0.8110(6) 0.4698(15) 0.024(2) Uani 1 1 d . . .
H21A H 0.1655 0.8347 0.3530 0.029 Uiso 1 1 calc R . .
H21B H 0.2172 0.8514 0.5561 0.029 Uiso 1 1 calc R . .
C22A C 0.1355(8) 0.7688(7) 0.5306(18) 0.032(3) Uani 1 1 d . . .
H22A H 0.0962 0.8038 0.5404 0.048 Uiso 1 1 calc R . .
H22B H 0.1625 0.7458 0.6468 0.048 Uiso 1 1 calc R . .
H22C H 0.1106 0.7295 0.4439 0.048 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
I1 Pd1 2.6041(15) . ?
I2 Pd1 2.6290(15) . ?
Pd1 C2B 1.993(11) . ?
Pd1 N4 2.077(10) . ?
O1 C20A 1.425(11) . ?
O1 H1A 0.8400 . ?
N1 N2 1.337(13) . ?
N1 C2B 1.353(14) . ?
N1 C14A 1.480(12) . ?
N2 N3 1.308(13) . ?
N3 C1B 1.393(15) . ?
N3 C21A 1.502(13) . ?
N4 C7B 1.352(15) . ?
N4 C3B 1.353(15) . ?
C1B C2B 1.393(15) . ?
C1B C20A 1.498(14) . ?
C3B C4B 1.384(17) . ?
C3B H3BA 0.9500 . ?
C4B C5B 1.391(17) . ?
C4B H4BA 0.9500 . ?
C5B C6B 1.36(2) . ?
C5B H5BA 0.9500 . ?
C6B C7B 1.37(2) . ?
C6B H6BA 0.9500 . ?
C7B H7BA 0.9500 . ?
C8B C13B 1.375(15) . ?
C8B C9B 1.380(18) . ?
C8B H8BA 0.9500 . ?
C9B C10B 1.420(19) . ?
C9B H9BA 0.9500 . ?
C10B C11B 1.384(18) . ?
C10B H10A 0.9500 . ?
C11B C12B 1.367(18) . ?
C11B H11A 0.9500 . ?
C12B C13B 1.404(19) . ?
C12B H12A 0.9500 . ?
C13B C14A 1.494(17) . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C15A C16A 1.533(13) . ?
C15A C20A 1.540(12) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C16A C17A 1.523(19) . ?
C16A H16A 0.9900 . ?
C16A H16B 0.9900 . ?
C17A C18A 1.529(15) . ?
C17A H17A 0.9900 . ?
C17A H17B 0.9900 . ?
C18A C19A 1.479(14) . ?
C18A H18A 0.9900 . ?
C18A H18B 0.9900 . ?
C19A C20A 1.582(15) . ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
C21A C22A 1.511(15) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 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
C2B Pd1 N4 179.2(4) . . ?
C2B Pd1 I1 89.8(3) . . ?
N4 Pd1 I1 90.5(3) . . ?
C2B Pd1 I2 89.7(3) . . ?
N4 Pd1 I2 90.1(3) . . ?
I1 Pd1 I2 179.41(4) . . ?
C20A O1 H1A 109.5 . . ?
N2 N1 C2B 113.7(9) . . ?
N2 N1 C14A 117.2(9) . . ?
C2B N1 C14A 129.1(9) . . ?
N3 N2 N1 104.4(9) . . ?
N2 N3 C1B 112.5(8) . . ?
N2 N3 C21A 118.2(9) . . ?
C1B N3 C21A 129.2(8) . . ?
C7B N4 C3B 116.6(11) . . ?
C7B N4 Pd1 121.8(9) . . ?
C3B N4 Pd1 121.5(7) . . ?
N3 C1B C2B 104.7(9) . . ?
N3 C1B C20A 121.8(9) . . ?
C2B C1B C20A 133.5(10) . . ?
N1 C2B C1B 104.6(9) . . ?
N1 C2B Pd1 123.8(7) . . ?
C1B C2B Pd1 131.6(8) . . ?
N4 C3B C4B 122.7(10) . . ?
N4 C3B H3BA 118.6 . . ?
C4B C3B H3BA 118.6 . . ?
C3B C4B C5B 119.7(12) . . ?
C3B C4B H4BA 120.1 . . ?
C5B C4B H4BA 120.1 . . ?
C6B C5B C4B 117.0(12) . . ?
C6B C5B H5BA 121.5 . . ?
C4B C5B H5BA 121.5 . . ?
C5B C6B C7B 121.3(13) . . ?
C5B C6B H6BA 119.3 . . ?
C7B C6B H6BA 119.3 . . ?
N4 C7B C6B 122.6(14) . . ?
N4 C7B H7BA 118.7 . . ?
C6B C7B H7BA 118.7 . . ?
C13B C8B C9B 120.6(11) . . ?
C13B C8B H8BA 119.7 . . ?
C9B C8B H8BA 119.7 . . ?
C8B C9B C10B 119.9(10) . . ?
C8B C9B H9BA 120.1 . . ?
C10B C9B H9BA 120.1 . . ?
C11B C10B C9B 118.1(11) . . ?
C11B C10B H10A 121.0 . . ?
C9B C10B H10A 121.0 . . ?
C12B C11B C10B 122.2(12) . . ?
C12B C11B H11A 118.9 . . ?
C10B C11B H11A 118.9 . . ?
C11B C12B C13B 119.1(11) . . ?
C11B C12B H12A 120.4 . . ?
C13B C12B H12A 120.4 . . ?
C8B C13B C12B 120.1(11) . . ?
C8B C13B C14A 121.1(11) . . ?
C12B C13B C14A 118.7(10) . . ?
N1 C14A C13B 112.7(8) . . ?
N1 C14A H14A 109.0 . . ?
C13B C14A H14A 109.0 . . ?
N1 C14A H14B 109.0 . . ?
C13B C14A H14B 109.0 . . ?
H14A C14A H14B 107.8 . . ?
C16A C15A C20A 112.2(9) . . ?
C16A C15A H15A 109.2 . . ?
C20A C15A H15A 109.2 . . ?
C16A C15A H15B 109.2 . . ?
C20A C15A H15B 109.2 . . ?
H15A C15A H15B 107.9 . . ?
C17A C16A C15A 111.9(8) . . ?
C17A C16A H16A 109.2 . . ?
C15A C16A H16A 109.2 . . ?
C17A C16A H16B 109.2 . . ?
C15A C16A H16B 109.2 . . ?
H16A C16A H16B 107.9 . . ?
C16A C17A C18A 111.8(9) . . ?
C16A C17A H17A 109.3 . . ?
C18A C17A H17A 109.3 . . ?
C16A C17A H17B 109.3 . . ?
C18A C17A H17B 109.3 . . ?
H17A C17A H17B 107.9 . . ?
C19A C18A C17A 114.0(10) . . ?
C19A C18A H18A 108.8 . . ?
C17A C18A H18A 108.8 . . ?
C19A C18A H18B 108.8 . . ?
C17A C18A H18B 108.8 . . ?
H18A C18A H18B 107.7 . . ?
C18A C19A C20A 111.7(8) . . ?
C18A C19A H19A 109.3 . . ?
C20A C19A H19A 109.3 . . ?
C18A C19A H19B 109.3 . . ?
C20A C19A H19B 109.3 . . ?
H19A C19A H19B 107.9 . . ?
O1 C20A C1B 110.7(8) . . ?
O1 C20A C15A 108.1(7) . . ?
C1B C20A C15A 110.4(8) . . ?
O1 C20A C19A 107.7(8) . . ?
C1B C20A C19A 111.6(8) . . ?
C15A C20A C19A 108.3(8) . . ?
N3 C21A C22A 111.7(8) . . ?
N3 C21A H21A 109.3 . . ?
C22A C21A H21A 109.3 . . ?
N3 C21A H21B 109.3 . . ?
C22A C21A H21B 109.3 . . ?
H21A C21A H21B 107.9 . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 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
C2B N1 N2 N3 -1.3(11) . . . . ?
C14A N1 N2 N3 177.6(8) . . . . ?
N1 N2 N3 C1B -1.0(11) . . . . ?
N1 N2 N3 C21A 175.4(8) . . . . ?
C2B Pd1 N4 C7B 173(100) . . . . ?
I1 Pd1 N4 C7B 63.6(12) . . . . ?
I2 Pd1 N4 C7B -116.6(12) . . . . ?
C2B Pd1 N4 C3B -3(34) . . . . ?
I1 Pd1 N4 C3B -112.3(8) . . . . ?
I2 Pd1 N4 C3B 67.5(8) . . . . ?
N2 N3 C1B C2B 2.8(12) . . . . ?
C21A N3 C1B C2B -173.1(10) . . . . ?
N2 N3 C1B C20A -177.1(9) . . . . ?
C21A N3 C1B C20A 7.0(16) . . . . ?
N2 N1 C2B C1B 3.0(12) . . . . ?
C14A N1 C2B C1B -175.8(10) . . . . ?
N2 N1 C2B Pd1 -176.9(7) . . . . ?
C14A N1 C2B Pd1 4.4(15) . . . . ?
N3 C1B C2B N1 -3.3(11) . . . . ?
C20A C1B C2B N1 176.6(11) . . . . ?
N3 C1B C2B Pd1 176.5(8) . . . . ?
C20A C1B C2B Pd1 -3.5(19) . . . . ?
N4 Pd1 C2B N1 174(100) . . . . ?
I1 Pd1 C2B N1 -76.7(8) . . . . ?
I2 Pd1 C2B N1 103.5(8) . . . . ?
N4 Pd1 C2B C1B -6(35) . . . . ?
I1 Pd1 C2B C1B 103.5(10) . . . . ?
I2 Pd1 C2B C1B -76.3(10) . . . . ?
C7B N4 C3B C4B -1.6(18) . . . . ?
Pd1 N4 C3B C4B 174.6(9) . . . . ?
N4 C3B C4B C5B 0.5(19) . . . . ?
C3B C4B C5B C6B -0.1(19) . . . . ?
C4B C5B C6B C7B 1(2) . . . . ?
C3B N4 C7B C6B 2(2) . . . . ?
Pd1 N4 C7B C6B -173.9(13) . . . . ?
C5B C6B C7B N4 -2(3) . . . . ?
C13B C8B C9B C10B -1.5(15) . . . . ?
C8B C9B C10B C11B 1.4(16) . . . . ?
C9B C10B C11B C12B 0.2(16) . . . . ?
C10B C11B C12B C13B -1.7(16) . . . . ?
C9B C8B C13B C12B 0.1(14) . . . . ?
C9B C8B C13B C14A -177.9(9) . . . . ?
C11B C12B C13B C8B 1.5(15) . . . . ?
C11B C12B C13B C14A 179.6(9) . . . . ?
N2 N1 C14A C13B 81.4(12) . . . . ?
C2B N1 C14A C13B -99.9(13) . . . . ?
C8B C13B C14A N1 89.4(12) . . . . ?
C12B C13B C14A N1 -88.6(12) . . . . ?
C20A C15A C16A C17A 55.5(11) . . . . ?
C15A C16A C17A C18A -51.0(12) . . . . ?
C16A C17A C18A C19A 52.0(13) . . . . ?
C17A C18A C19A C20A -54.6(13) . . . . ?
N3 C1B C20A O1 44.4(13) . . . . ?
C2B C1B C20A O1 -135.5(12) . . . . ?
N3 C1B C20A C15A -75.2(12) . . . . ?
C2B C1B C20A C15A 104.9(13) . . . . ?
N3 C1B C20A C19A 164.3(9) . . . . ?
C2B C1B C20A C19A -15.6(16) . . . . ?
C16A C15A C20A O1 60.2(11) . . . . ?
C16A C15A C20A C1B -178.6(8) . . . . ?
C16A C15A C20A C19A -56.2(10) . . . . ?
C18A C19A C20A O1 -60.9(11) . . . . ?
C18A C19A C20A C1B 177.4(9) . . . . ?
C18A C19A C20A C15A 55.7(11) . . . . ?
N2 N3 C21A C22A 46.0(14) . . . . ?
C1B N3 C21A C22A -138.2(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.36
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         2.147
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.261



####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 934458'
_audit_update_record             
;
2013-04-17 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
#TrackingRef 'pg-sm-2-28.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H20 I2 N4 Pd'
_chemical_formula_sum            'C21 H20 I2 N4 Pd'
_chemical_formula_weight         688.61

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'
I I -0.4742 1.8119 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.668(3)
_cell_length_b                   10.097(4)
_cell_length_c                   13.798(5)
_cell_angle_alpha                110.578(3)
_cell_angle_beta                 90.704(2)
_cell_angle_gamma                115.409(5)
_cell_volume                     1117.6(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1848
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      25.3

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             652
_exptl_absorpt_coefficient_mu    3.606
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.7144
_exptl_absorpt_correction_T_max  0.9314
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8354
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3875
_reflns_number_gt                3367
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

_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)+(0.0125P)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         3875
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0376
_refine_ls_wR_factor_gt          0.0366
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.86192(2) 0.22797(3) 0.321707(16) 0.01559(6) Uani 1 1 d . . .
I1 I 0.94601(2) 0.22038(2) 0.142611(15) 0.02303(6) Uani 1 1 d . . .
I2 I 0.76690(2) 0.25046(2) 0.500377(15) 0.02346(6) Uani 1 1 d . . .
N1 N 1.0581(2) 0.2118(3) 0.37253(17) 0.0178(5) Uani 1 1 d . . .
N2 N 0.6722(2) 0.3708(3) 0.27341(17) 0.0162(5) Uani 1 1 d . . .
N3 N 0.5375(2) 0.3459(3) 0.22484(18) 0.0193(5) Uani 1 1 d . . .
N4 N 0.4549(2) 0.1893(3) 0.18661(17) 0.0171(5) Uani 1 1 d . . .
C1 C 1.0410(3) 0.0850(4) 0.3911(2) 0.0284(7) Uani 1 1 d . . .
H1 H 0.9383 0.0060 0.3854 0.034 Uiso 1 1 calc R . .
C2 C 1.1640(4) 0.0629(4) 0.4179(3) 0.0399(9) Uani 1 1 d . . .
H2 H 1.1461 -0.0305 0.4289 0.048 Uiso 1 1 calc R . .
C3 C 1.3126(4) 0.1766(5) 0.4286(2) 0.0437(10) Uani 1 1 d . . .
H3 H 1.4000 0.1653 0.4487 0.052 Uiso 1 1 calc R . .
C4 C 1.3325(3) 0.3075(4) 0.4096(2) 0.0356(9) Uani 1 1 d . . .
H4 H 1.4346 0.3883 0.4163 0.043 Uiso 1 1 calc R . .
C5 C 1.2038(3) 0.3218(4) 0.3807(2) 0.0256(7) Uani 1 1 d . . .
H5 H 1.2190 0.4119 0.3663 0.031 Uiso 1 1 calc R . .
C6 C 0.6774(3) 0.2354(3) 0.2675(2) 0.0153(6) Uani 1 1 d . . .
C7 C 0.5316(3) 0.1149(3) 0.2099(2) 0.0154(6) Uani 1 1 d . . .
C8 C 0.7941(3) 0.5382(3) 0.3281(2) 0.0197(6) Uani 1 1 d . . .
H8A H 0.8900 0.5395 0.3555 0.024 Uiso 1 1 calc R . .
H8B H 0.7582 0.5931 0.3891 0.024 Uiso 1 1 calc R . .
C9 C 0.8321(3) 0.6280(3) 0.2569(2) 0.0180(6) Uani 1 1 d . . .
C10 C 0.9588(3) 0.6435(3) 0.2069(2) 0.0249(7) Uani 1 1 d . . .
H10 H 1.0242 0.6006 0.2195 0.030 Uiso 1 1 calc R . .
C11 C 0.9897(3) 0.7216(4) 0.1386(2) 0.0284(8) Uani 1 1 d . . .
H11 H 1.0756 0.7309 0.1039 0.034 Uiso 1 1 calc R . .
C12 C 0.8963(3) 0.7857(4) 0.1208(2) 0.0260(7) Uani 1 1 d . . .
H12 H 0.9183 0.8397 0.0744 0.031 Uiso 1 1 calc R . .
C13 C 0.7696(3) 0.7711(4) 0.1709(2) 0.0288(8) Uani 1 1 d . . .
H13 H 0.7050 0.8151 0.1589 0.035 Uiso 1 1 calc R . .
C14 C 0.7387(3) 0.6925(3) 0.2382(2) 0.0229(7) Uani 1 1 d . . .
H14 H 0.6521 0.6824 0.2722 0.027 Uiso 1 1 calc R . .
C15 C 0.2945(3) 0.1196(4) 0.1306(2) 0.0281(7) Uani 1 1 d . . .
H15A H 0.2736 0.2046 0.1266 0.042 Uiso 1 1 calc R . .
H15B H 0.2215 0.0644 0.1685 0.042 Uiso 1 1 calc R . .
H15C H 0.2813 0.0434 0.0591 0.042 Uiso 1 1 calc R . .
C16 C 0.4617(3) -0.0595(3) 0.1759(2) 0.0176(6) Uani 1 1 d . . .
C17 C 0.4118(3) -0.1617(4) 0.0694(2) 0.0234(7) Uani 1 1 d . . .
H17 H 0.4225 -0.1183 0.0174 0.028 Uiso 1 1 calc R . .
C18 C 0.3474(3) -0.3245(4) 0.0387(2) 0.0308(8) Uani 1 1 d . . .
H18 H 0.3157 -0.3927 -0.0342 0.037 Uiso 1 1 calc R . .
C19 C 0.3287(3) -0.3892(4) 0.1148(2) 0.0288(8) Uani 1 1 d . . .
H19 H 0.2841 -0.5015 0.0940 0.035 Uiso 1 1 calc R . .
C20 C 0.3752(3) -0.2898(4) 0.2200(2) 0.0254(7) Uani 1 1 d . . .
H20 H 0.3609 -0.3341 0.2717 0.031 Uiso 1 1 calc R . .
C21 C 0.4433(3) -0.1245(3) 0.2517(2) 0.0219(7) Uani 1 1 d . . .
H21 H 0.4769 -0.0566 0.3245 0.026 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 C6 1.967(3) . ?
Pd1 N1 2.104(2) . ?
Pd1 I1 2.5968(9) . ?
Pd1 I2 2.6104(9) . ?
N1 C1 1.335(3) . ?
N1 C5 1.340(3) . ?
N2 N3 1.337(3) . ?
N2 C6 1.363(3) . ?
N2 C8 1.479(3) . ?
N3 N4 1.317(3) . ?
N4 C7 1.365(3) . ?
N4 C15 1.466(3) . ?
C1 C2 1.369(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.366(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.371(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.385(3) . ?
C7 C16 1.472(4) . ?
C8 C9 1.508(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.387(4) . ?
C9 C10 1.390(4) . ?
C10 C11 1.388(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.379(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.393(3) . ?
C16 C17 1.395(4) . ?
C17 C18 1.377(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.396(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.374(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.396(4) . ?
C20 H20 0.9500 . ?
C21 H21 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
C6 Pd1 N1 177.24(10) . . ?
C6 Pd1 I1 86.56(7) . . ?
N1 Pd1 I1 91.38(6) . . ?
C6 Pd1 I2 89.39(7) . . ?
N1 Pd1 I2 92.75(6) . . ?
I1 Pd1 I2 175.183(10) . . ?
C1 N1 C5 117.5(2) . . ?
C1 N1 Pd1 120.64(18) . . ?
C5 N1 Pd1 121.72(19) . . ?
N3 N2 C6 114.5(2) . . ?
N3 N2 C8 117.3(2) . . ?
C6 N2 C8 128.2(2) . . ?
N4 N3 N2 102.7(2) . . ?
N3 N4 C7 113.6(2) . . ?
N3 N4 C15 117.4(2) . . ?
C7 N4 C15 129.0(2) . . ?
N1 C1 C2 123.4(3) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 118.3(3) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 121.7(3) . . ?
N1 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
N2 C6 C7 103.5(2) . . ?
N2 C6 Pd1 124.95(19) . . ?
C7 C6 Pd1 131.4(2) . . ?
N4 C7 C6 105.7(2) . . ?
N4 C7 C16 123.0(2) . . ?
C6 C7 C16 131.2(2) . . ?
N2 C8 C9 112.5(2) . . ?
N2 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N2 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C14 C9 C10 119.1(2) . . ?
C14 C9 C8 120.5(2) . . ?
C10 C9 C8 120.4(2) . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 119.9(3) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 119.5(3) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C9 121.1(2) . . ?
C13 C14 H14 119.5 . . ?
C9 C14 H14 119.5 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 119.1(3) . . ?
C21 C16 C7 119.4(3) . . ?
C17 C16 C7 121.5(2) . . ?
C18 C17 C16 120.9(3) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C19 119.8(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 119.7(3) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.7(3) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C16 C21 C20 119.7(3) . . ?
C16 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?

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
C6 Pd1 N1 C1 -74.1(18) . . . . ?
I1 Pd1 N1 C1 -115.8(2) . . . . ?
I2 Pd1 N1 C1 66.7(2) . . . . ?
C6 Pd1 N1 C5 101.4(18) . . . . ?
I1 Pd1 N1 C5 59.7(2) . . . . ?
I2 Pd1 N1 C5 -117.8(2) . . . . ?
C6 N2 N3 N4 -0.2(3) . . . . ?
C8 N2 N3 N4 -178.8(2) . . . . ?
N2 N3 N4 C7 0.5(3) . . . . ?
N2 N3 N4 C15 177.7(2) . . . . ?
C5 N1 C1 C2 0.1(4) . . . . ?
Pd1 N1 C1 C2 175.8(2) . . . . ?
N1 C1 C2 C3 1.4(5) . . . . ?
C1 C2 C3 C4 -1.5(5) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C1 N1 C5 C4 -1.5(4) . . . . ?
Pd1 N1 C5 C4 -177.1(2) . . . . ?
C3 C4 C5 N1 1.3(5) . . . . ?
N3 N2 C6 C7 -0.2(3) . . . . ?
C8 N2 C6 C7 178.3(2) . . . . ?
N3 N2 C6 Pd1 175.63(17) . . . . ?
C8 N2 C6 Pd1 -5.9(4) . . . . ?
N1 Pd1 C6 N2 -127.0(17) . . . . ?
I1 Pd1 C6 N2 -85.3(2) . . . . ?
I2 Pd1 C6 N2 92.1(2) . . . . ?
N1 Pd1 C6 C7 47.6(18) . . . . ?
I1 Pd1 C6 C7 89.3(2) . . . . ?
I2 Pd1 C6 C7 -93.3(2) . . . . ?
N3 N4 C7 C6 -0.7(3) . . . . ?
C15 N4 C7 C6 -177.5(2) . . . . ?
N3 N4 C7 C16 179.6(2) . . . . ?
C15 N4 C7 C16 2.8(4) . . . . ?
N2 C6 C7 N4 0.5(3) . . . . ?
Pd1 C6 C7 N4 -174.95(18) . . . . ?
N2 C6 C7 C16 -179.8(3) . . . . ?
Pd1 C6 C7 C16 4.7(4) . . . . ?
N3 N2 C8 C9 -54.3(3) . . . . ?
C6 N2 C8 C9 127.3(3) . . . . ?
N2 C8 C9 C14 81.6(3) . . . . ?
N2 C8 C9 C10 -96.6(3) . . . . ?
C14 C9 C10 C11 -0.5(4) . . . . ?
C8 C9 C10 C11 177.7(3) . . . . ?
C9 C10 C11 C12 0.7(5) . . . . ?
C10 C11 C12 C13 -0.5(5) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C12 C13 C14 C9 0.2(5) . . . . ?
C10 C9 C14 C13 0.1(4) . . . . ?
C8 C9 C14 C13 -178.2(3) . . . . ?
N4 C7 C16 C21 -119.4(3) . . . . ?
C6 C7 C16 C21 61.0(4) . . . . ?
N4 C7 C16 C17 60.0(4) . . . . ?
C6 C7 C16 C17 -119.7(3) . . . . ?
C21 C16 C17 C18 -1.0(4) . . . . ?
C7 C16 C17 C18 179.6(2) . . . . ?
C16 C17 C18 C19 1.2(4) . . . . ?
C17 C18 C19 C20 -0.2(4) . . . . ?
C18 C19 C20 C21 -1.0(4) . . . . ?
C17 C16 C21 C20 -0.2(4) . . . . ?
C7 C16 C21 C20 179.2(2) . . . . ?
C19 C20 C21 C16 1.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.080
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 934462'
_audit_update_record             
;
2013-04-17 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
#TrackingRef 'pg-sm-3-69-1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 I2 N3 P Pd'
_chemical_formula_sum            'C34 H30 I2 N3 P Pd'
_chemical_formula_weight         871.78

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'
I I -0.4742 1.8119 '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'
P P 0.1023 0.0942 '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   'P bca'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   17.887(6)
_cell_length_b                   18.351(7)
_cell_length_c                   19.356(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6353(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6964
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      25.3

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3376
_exptl_absorpt_coefficient_mu    2.606
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.9029
_exptl_absorpt_correction_T_max  0.9497
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            45356
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5586
_reflns_number_gt                5265
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

_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)+(0.0064P)²+31.9157P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5586
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_restrained_S_all      1.273
_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 0.15460(2) 0.08819(2) 0.64202(3) 0.01666(12) Uani 1 1 d . . .
I1 I 0.27825(2) 0.08848(2) 0.56617(3) 0.02932(13) Uani 1 1 d . . .
I2 I 0.14240(3) -0.05441(2) 0.62796(3) 0.03081(13) Uani 1 1 d . . .
P1 P 0.05306(8) 0.09234(9) 0.71315(9) 0.0171(4) Uani 1 1 d . . .
N1 N 0.2146(3) 0.2365(3) 0.6808(3) 0.0219(12) Uani 1 1 d . . .
N2 N 0.2103(3) 0.3085(3) 0.6718(3) 0.0287(14) Uani 1 1 d . . .
N3 N 0.1548(3) 0.3157(3) 0.6269(3) 0.0224(13) Uani 1 1 d . . .
C1 C -0.0295(3) 0.0455(3) 0.6793(4) 0.0193(14) Uani 1 1 d . . .
C2 C -0.0409(4) 0.0429(4) 0.6086(4) 0.0275(16) Uani 1 1 d . . .
H2 H -0.0056 0.0645 0.5781 0.033 Uiso 1 1 calc R . .
C3 C -0.1038(4) 0.0089(4) 0.5823(4) 0.040(2) Uani 1 1 d . . .
H3 H -0.1121 0.0083 0.5338 0.048 Uiso 1 1 calc R . .
C4 C -0.1537(4) -0.0236(3) 0.6248(5) 0.037(2) Uani 1 1 d . . .
H4 H -0.1960 -0.0478 0.6060 0.044 Uiso 1 1 calc R . .
C5 C -0.1434(4) -0.0217(4) 0.6958(4) 0.038(2) Uani 1 1 d . . .
H5 H -0.1788 -0.0442 0.7256 0.046 Uiso 1 1 calc R . .
C6 C -0.0815(3) 0.0130(3) 0.7232(4) 0.0293(17) Uani 1 1 d . . .
H6 H -0.0744 0.0147 0.7718 0.035 Uiso 1 1 calc R . .
C7 C 0.0682(3) 0.0551(3) 0.7995(3) 0.0210(14) Uani 1 1 d . . .
C8 C 0.0262(4) 0.0792(4) 0.8557(4) 0.0311(17) Uani 1 1 d . . .
H8 H -0.0102 0.1163 0.8490 0.037 Uiso 1 1 calc R . .
C9 C 0.0365(4) 0.0507(4) 0.9199(4) 0.0372(19) Uani 1 1 d . . .
H9 H 0.0076 0.0685 0.9575 0.045 Uiso 1 1 calc R . .
C10 C 0.0880(4) -0.0035(4) 0.9311(4) 0.0375(19) Uani 1 1 d . . .
H10 H 0.0944 -0.0237 0.9759 0.045 Uiso 1 1 calc R . .
C11 C 0.1301(4) -0.0280(4) 0.8768(4) 0.0347(18) Uani 1 1 d . . .
H11 H 0.1660 -0.0653 0.8842 0.042 Uiso 1 1 calc R . .
C12 C 0.1211(3) 0.0006(3) 0.8112(4) 0.0256(16) Uani 1 1 d . . .
H12 H 0.1510 -0.0168 0.7742 0.031 Uiso 1 1 calc R . .
C13 C 0.0210(3) 0.1848(3) 0.7322(3) 0.0185(14) Uani 1 1 d . . .
C14 C -0.0409(3) 0.2150(3) 0.6998(4) 0.0254(16) Uani 1 1 d . . .
H14 H -0.0714 0.1862 0.6704 0.030 Uiso 1 1 calc R . .
C15 C -0.0577(4) 0.2882(3) 0.7110(4) 0.0296(17) Uani 1 1 d . . .
H15 H -0.1005 0.3090 0.6896 0.036 Uiso 1 1 calc R . .
C16 C -0.0134(4) 0.3307(3) 0.7524(4) 0.0327(19) Uani 1 1 d . . .
H16 H -0.0245 0.3809 0.7586 0.039 Uiso 1 1 calc R . .
C17 C 0.0477(4) 0.3000(3) 0.7851(4) 0.0313(18) Uani 1 1 d . . .
H17 H 0.0778 0.3291 0.8146 0.038 Uiso 1 1 calc R . .
C18 C 0.0652(3) 0.2279(3) 0.7752(3) 0.0227(15) Uani 1 1 d . . .
H18 H 0.1075 0.2073 0.7976 0.027 Uiso 1 1 calc R . .
C19 C 0.1638(3) 0.1971(3) 0.6432(3) 0.0173(14) Uani 1 1 d . . .
C20 C 0.1250(3) 0.2503(3) 0.6076(3) 0.0166(14) Uani 1 1 d . . .
C21 C 0.2752(3) 0.2089(4) 0.7251(4) 0.0292(17) Uani 1 1 d . . .
H21A H 0.3209 0.2378 0.7160 0.035 Uiso 1 1 calc R . .
H21B H 0.2859 0.1578 0.7121 0.035 Uiso 1 1 calc R . .
C22 C 0.2586(3) 0.2116(4) 0.8013(4) 0.0273(17) Uani 1 1 d . . .
C23 C 0.2576(4) 0.1484(4) 0.8398(4) 0.0328(18) Uani 1 1 d . . .
H23 H 0.2645 0.1029 0.8173 0.039 Uiso 1 1 calc R . .
C24 C 0.2469(4) 0.1500(5) 0.9103(4) 0.045(2) Uani 1 1 d . . .
H24 H 0.2459 0.1060 0.9360 0.054 Uiso 1 1 calc R . .
C25 C 0.2375(4) 0.2162(4) 0.9431(4) 0.044(2) Uani 1 1 d . . .
H25 H 0.2312 0.2179 0.9918 0.053 Uiso 1 1 calc R . .
C26 C 0.2373(4) 0.2798(4) 0.9050(4) 0.041(2) Uani 1 1 d . . .
H26 H 0.2298 0.3252 0.9276 0.049 Uiso 1 1 calc R . .
C27 C 0.2478(4) 0.2780(4) 0.8342(4) 0.0311(17) Uani 1 1 d . . .
H27 H 0.2477 0.3220 0.8083 0.037 Uiso 1 1 calc R . .
C28 C 0.1387(4) 0.3906(3) 0.6039(4) 0.039(2) Uani 1 1 d . . .
H28A H 0.1707 0.4248 0.6292 0.059 Uiso 1 1 calc R . .
H28B H 0.0861 0.4020 0.6130 0.059 Uiso 1 1 calc R . .
H28C H 0.1487 0.3948 0.5543 0.059 Uiso 1 1 calc R . .
C29 C 0.0656(3) 0.2429(3) 0.5559(3) 0.0192(14) Uani 1 1 d . . .
C30 C 0.0052(4) 0.2917(4) 0.5508(4) 0.0296(17) Uani 1 1 d . . .
H30 H 0.0029 0.3326 0.5808 0.036 Uiso 1 1 calc R . .
C31 C -0.0505(4) 0.2812(4) 0.5032(4) 0.038(2) Uani 1 1 d . . .
H31 H -0.0903 0.3153 0.5000 0.045 Uiso 1 1 calc R . .
C32 C -0.0491(4) 0.2218(4) 0.4601(4) 0.0351(19) Uani 1 1 d . . .
H32 H -0.0886 0.2140 0.4281 0.042 Uiso 1 1 calc R . .
C33 C 0.0103(4) 0.1733(4) 0.4635(4) 0.0339(18) Uani 1 1 d . . .
H33 H 0.0119 0.1325 0.4333 0.041 Uiso 1 1 calc R . .
C34 C 0.0668(3) 0.1841(3) 0.5104(3) 0.0227(15) Uani 1 1 d . . .
H34 H 0.1075 0.1508 0.5119 0.027 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 C19 2.006(6) . ?
Pd1 P1 2.2804(17) . ?
Pd1 I2 2.6399(12) . ?
Pd1 I1 2.6546(9) . ?
P1 C7 1.826(7) . ?
P1 C13 1.829(6) . ?
P1 C1 1.829(6) . ?
N1 N2 1.335(7) . ?
N1 C19 1.370(7) . ?
N1 C21 1.472(8) . ?
N2 N3 1.326(7) . ?
N3 C20 1.366(7) . ?
N3 C28 1.472(8) . ?
C1 C2 1.385(9) . ?
C1 C6 1.395(9) . ?
C2 C3 1.385(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.353(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.393(9) . ?
C7 C12 1.395(9) . ?
C8 C9 1.361(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.388(9) . ?
C13 C18 1.393(9) . ?
C14 C15 1.394(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.370(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.374(9) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.382(8) . ?
C20 C29 1.466(8) . ?
C21 C22 1.504(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.378(9) . ?
C22 C27 1.389(9) . ?
C23 C24 1.378(10) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.382(10) . ?
C25 H25 0.9500 . ?
C26 C27 1.383(10) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C34 1.392(9) . ?
C29 C30 1.408(8) . ?
C30 C31 1.369(10) . ?
C30 H30 0.9500 . ?
C31 C32 1.374(10) . ?
C31 H31 0.9500 . ?
C32 C33 1.388(10) . ?
C32 H32 0.9500 . ?
C33 C34 1.373(9) . ?
C33 H33 0.9500 . ?
C34 H34 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
C19 Pd1 P1 91.41(17) . . ?
C19 Pd1 I2 174.76(18) . . ?
P1 Pd1 I2 91.69(4) . . ?
C19 Pd1 I1 86.36(16) . . ?
P1 Pd1 I1 175.88(5) . . ?
I2 Pd1 I1 90.79(2) . . ?
C7 P1 C13 102.1(3) . . ?
C7 P1 C1 105.8(3) . . ?
C13 P1 C1 104.8(3) . . ?
C7 P1 Pd1 115.0(2) . . ?
C13 P1 Pd1 113.7(2) . . ?
C1 P1 Pd1 114.2(2) . . ?
N2 N1 C19 114.5(5) . . ?
N2 N1 C21 117.3(5) . . ?
C19 N1 C21 128.0(5) . . ?
N3 N2 N1 103.1(5) . . ?
N2 N3 C20 112.6(5) . . ?
N2 N3 C28 115.9(5) . . ?
C20 N3 C28 131.4(6) . . ?
C2 C1 C6 119.3(6) . . ?
C2 C1 P1 119.3(5) . . ?
C6 C1 P1 121.4(5) . . ?
C1 C2 C3 119.9(7) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 120.8(8) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.3(7) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 119.8(7) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 119.9(7) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
C8 C7 C12 117.8(6) . . ?
C8 C7 P1 121.0(5) . . ?
C12 C7 P1 121.2(5) . . ?
C9 C8 C7 121.2(6) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 120.8(7) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 119.1(7) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 121.1(7) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C7 120.0(7) . . ?
C11 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
C14 C13 C18 119.8(6) . . ?
C14 C13 P1 122.0(5) . . ?
C18 C13 P1 117.9(5) . . ?
C13 C14 C15 119.1(6) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 121.0(7) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 119.5(6) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 120.6(7) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C13 120.0(6) . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
N1 C19 C20 103.0(5) . . ?
N1 C19 Pd1 125.9(4) . . ?
C20 C19 Pd1 131.1(5) . . ?
N3 C20 C19 106.7(5) . . ?
N3 C20 C29 123.5(5) . . ?
C19 C20 C29 129.7(5) . . ?
N1 C21 C22 114.5(5) . . ?
N1 C21 H21A 108.6 . . ?
C22 C21 H21A 108.6 . . ?
N1 C21 H21B 108.6 . . ?
C22 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C23 C22 C27 119.2(7) . . ?
C23 C22 C21 120.3(6) . . ?
C27 C22 C21 120.4(6) . . ?
C24 C23 C22 121.3(7) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C25 119.5(7) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C26 C25 C24 119.9(8) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 120.5(7) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C22 119.7(7) . . ?
C26 C27 H27 120.2 . . ?
C22 C27 H27 120.2 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C34 C29 C30 117.5(6) . . ?
C34 C29 C20 119.5(5) . . ?
C30 C29 C20 123.0(6) . . ?
C31 C30 C29 121.0(7) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C30 C31 C32 120.5(7) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C33 119.5(7) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C34 C33 C32 120.2(7) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C29 121.2(6) . . ?
C33 C34 H34 119.4 . . ?
C29 C34 H34 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
C19 Pd1 P1 C7 -112.0(3) . . . . ?
I2 Pd1 P1 C7 72.2(2) . . . . ?
I1 Pd1 P1 C7 -54.8(7) . . . . ?
C19 Pd1 P1 C13 5.2(3) . . . . ?
I2 Pd1 P1 C13 -170.6(2) . . . . ?
I1 Pd1 P1 C13 62.4(7) . . . . ?
C19 Pd1 P1 C1 125.4(3) . . . . ?
I2 Pd1 P1 C1 -50.4(2) . . . . ?
I1 Pd1 P1 C1 -177.4(6) . . . . ?
C19 N1 N2 N3 -0.1(7) . . . . ?
C21 N1 N2 N3 176.0(5) . . . . ?
N1 N2 N3 C20 -0.3(7) . . . . ?
N1 N2 N3 C28 -177.2(6) . . . . ?
C7 P1 C1 C2 -158.5(5) . . . . ?
C13 P1 C1 C2 94.1(5) . . . . ?
Pd1 P1 C1 C2 -31.0(6) . . . . ?
C7 P1 C1 C6 22.1(6) . . . . ?
C13 P1 C1 C6 -85.3(5) . . . . ?
Pd1 P1 C1 C6 149.6(5) . . . . ?
C6 C1 C2 C3 0.6(10) . . . . ?
P1 C1 C2 C3 -178.8(5) . . . . ?
C1 C2 C3 C4 -1.6(10) . . . . ?
C2 C3 C4 C5 1.5(11) . . . . ?
C3 C4 C5 C6 -0.5(11) . . . . ?
C4 C5 C6 C1 -0.4(10) . . . . ?
C2 C1 C6 C5 0.4(10) . . . . ?
P1 C1 C6 C5 179.7(5) . . . . ?
C13 P1 C7 C8 29.5(6) . . . . ?
C1 P1 C7 C8 -79.8(6) . . . . ?
Pd1 P1 C7 C8 153.2(5) . . . . ?
C13 P1 C7 C12 -151.6(5) . . . . ?
C1 P1 C7 C12 99.0(5) . . . . ?
Pd1 P1 C7 C12 -28.0(6) . . . . ?
C12 C7 C8 C9 0.0(10) . . . . ?
P1 C7 C8 C9 178.9(6) . . . . ?
C7 C8 C9 C10 -0.8(11) . . . . ?
C8 C9 C10 C11 0.9(11) . . . . ?
C9 C10 C11 C12 -0.3(11) . . . . ?
C10 C11 C12 C7 -0.4(10) . . . . ?
C8 C7 C12 C11 0.6(9) . . . . ?
P1 C7 C12 C11 -178.3(5) . . . . ?
C7 P1 C13 C14 -133.5(5) . . . . ?
C1 P1 C13 C14 -23.4(6) . . . . ?
Pd1 P1 C13 C14 102.1(5) . . . . ?
C7 P1 C13 C18 53.3(5) . . . . ?
C1 P1 C13 C18 163.4(5) . . . . ?
Pd1 P1 C13 C18 -71.1(5) . . . . ?
C18 C13 C14 C15 0.0(10) . . . . ?
P1 C13 C14 C15 -173.1(5) . . . . ?
C13 C14 C15 C16 1.1(10) . . . . ?
C14 C15 C16 C17 -1.8(11) . . . . ?
C15 C16 C17 C18 1.4(11) . . . . ?
C16 C17 C18 C13 -0.4(10) . . . . ?
C14 C13 C18 C17 -0.3(10) . . . . ?
P1 C13 C18 C17 173.1(5) . . . . ?
N2 N1 C19 C20 0.4(7) . . . . ?
C21 N1 C19 C20 -175.2(6) . . . . ?
N2 N1 C19 Pd1 178.8(4) . . . . ?
C21 N1 C19 Pd1 3.3(9) . . . . ?
P1 Pd1 C19 N1 102.6(5) . . . . ?
I2 Pd1 C19 N1 -131.1(16) . . . . ?
I1 Pd1 C19 N1 -74.0(5) . . . . ?
P1 Pd1 C19 C20 -79.5(6) . . . . ?
I2 Pd1 C19 C20 47(2) . . . . ?
I1 Pd1 C19 C20 104.0(6) . . . . ?
N2 N3 C20 C19 0.5(7) . . . . ?
C28 N3 C20 C19 176.9(7) . . . . ?
N2 N3 C20 C29 -176.8(6) . . . . ?
C28 N3 C20 C29 -0.4(11) . . . . ?
N1 C19 C20 N3 -0.5(6) . . . . ?
Pd1 C19 C20 N3 -178.8(4) . . . . ?
N1 C19 C20 C29 176.6(6) . . . . ?
Pd1 C19 C20 C29 -1.8(10) . . . . ?
N2 N1 C21 C22 82.4(7) . . . . ?
C19 N1 C21 C22 -102.1(7) . . . . ?
N1 C21 C22 C23 119.5(7) . . . . ?
N1 C21 C22 C27 -63.8(8) . . . . ?
C27 C22 C23 C24 -0.6(10) . . . . ?
C21 C22 C23 C24 176.2(6) . . . . ?
C22 C23 C24 C25 -0.6(12) . . . . ?
C23 C24 C25 C26 1.5(12) . . . . ?
C24 C25 C26 C27 -1.3(12) . . . . ?
C25 C26 C27 C22 0.1(11) . . . . ?
C23 C22 C27 C26 0.8(10) . . . . ?
C21 C22 C27 C26 -176.0(6) . . . . ?
N3 C20 C29 C34 142.5(6) . . . . ?
C19 C20 C29 C34 -34.1(10) . . . . ?
N3 C20 C29 C30 -39.4(9) . . . . ?
C19 C20 C29 C30 144.0(7) . . . . ?
C34 C29 C30 C31 0.5(10) . . . . ?
C20 C29 C30 C31 -177.7(6) . . . . ?
C29 C30 C31 C32 1.2(12) . . . . ?
C30 C31 C32 C33 -1.9(12) . . . . ?
C31 C32 C33 C34 0.9(11) . . . . ?
C32 C33 C34 C29 0.7(11) . . . . ?
C30 C29 C34 C33 -1.4(10) . . . . ?
C20 C29 C34 C33 176.8(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.121


####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 935843'
_audit_update_record             
;
2013-04-24 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
#TrackingRef 'pg-sm-3-73-1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 I2 N3 O P Pd'
_chemical_formula_sum            'C34 H36 I2 N3 O P Pd'
_chemical_formula_weight         893.83

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'
I I -0.4742 1.8119 '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'
P P 0.1023 0.0942 '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   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   15.928(4)
_cell_length_b                   16.099(4)
_cell_length_c                   26.191(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6716(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9851
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      25.3

_exptl_crystal_description       Block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3488
_exptl_absorpt_coefficient_mu    2.470
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.8269
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49512
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         25.39
_reflns_number_total             6138
_reflns_number_gt                6034
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

_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)+(0.0275P)²+9.9391P] 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         6138
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.0915
_refine_ls_wR_factor_gt          0.0911
_refine_ls_goodness_of_fit_ref   1.409
_refine_ls_restrained_S_all      1.409
_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 0.34842(2) 0.23344(2) 0.333937(14) 0.02055(11) Uani 1 1 d . . .
I1 I 0.19642(2) 0.23950(2) 0.369915(14) 0.02962(11) Uani 1 1 d . . .
I2 I 0.49093(2) 0.23017(2) 0.284448(13) 0.02997(11) Uani 1 1 d . . .
P1 P 0.40260(8) 0.14067(8) 0.39528(5) 0.0227(3) Uani 1 1 d . . .
O17 O 0.2923(2) 0.5392(2) 0.31121(14) 0.0340(9) Uani 1 1 d . . .
H17 H 0.3110 0.5774 0.3299 0.051 Uiso 1 1 calc R . .
N7 N 0.2680(3) 0.4243(3) 0.23429(16) 0.0307(10) Uani 1 1 d . . .
N8 N 0.2651(3) 0.2958(2) 0.23907(15) 0.0239(9) Uani 1 1 d . . .
N12 N 0.2406(3) 0.3585(3) 0.20914(15) 0.0302(10) Uani 1 1 d . . .
C1 C 0.3064(3) 0.3186(3) 0.28185(18) 0.0219(10) Uani 1 1 d . . .
C2 C 0.3083(3) 0.4048(3) 0.27866(18) 0.0227(10) Uani 1 1 d . . .
C3 C 0.3487(3) 0.4684(3) 0.3132(2) 0.0284(12) Uani 1 1 d . . .
C4 C 0.3544(3) 0.4353(3) 0.36750(19) 0.0312(12) Uani 1 1 d . . .
H4A H 0.3819 0.3801 0.3668 0.037 Uiso 1 1 calc R . .
H4B H 0.2970 0.4277 0.3812 0.037 Uiso 1 1 calc R . .
C5 C 0.4032(4) 0.4923(3) 0.4031(2) 0.0420(15) Uani 1 1 d . . .
H5A H 0.3723 0.5452 0.4073 0.050 Uiso 1 1 calc R . .
H5B H 0.4083 0.4659 0.4371 0.050 Uiso 1 1 calc R . .
C6 C 0.4904(4) 0.5101(4) 0.3821(3) 0.0466(16) Uani 1 1 d . . .
H6A H 0.5232 0.4579 0.3804 0.056 Uiso 1 1 calc R . .
H6B H 0.5202 0.5491 0.4051 0.056 Uiso 1 1 calc R . .
C7 C 0.4834(4) 0.5484(4) 0.3283(2) 0.0435(15) Uani 1 1 d . . .
H7A H 0.4542 0.6026 0.3305 0.052 Uiso 1 1 calc R . .
H7B H 0.5403 0.5583 0.3144 0.052 Uiso 1 1 calc R . .
C8 C 0.4354(3) 0.4913(3) 0.2927(2) 0.0335(13) Uani 1 1 d . . .
H8A H 0.4683 0.4399 0.2874 0.040 Uiso 1 1 calc R . .
H8B H 0.4289 0.5189 0.2592 0.040 Uiso 1 1 calc R . .
C9 C 0.2515(4) 0.5046(3) 0.2096(2) 0.0421(15) Uani 1 1 d . . .
H9A H 0.2203 0.4955 0.1778 0.063 Uiso 1 1 calc R . .
H9B H 0.3048 0.5322 0.2020 0.063 Uiso 1 1 calc R . .
H9C H 0.2182 0.5396 0.2326 0.063 Uiso 1 1 calc R . .
C10 C 0.2441(3) 0.2118(3) 0.22155(18) 0.0278(11) Uani 1 1 d . . .
H10A H 0.1829 0.2024 0.2251 0.033 Uiso 1 1 calc R . .
H10B H 0.2736 0.1703 0.2429 0.033 Uiso 1 1 calc R . .
C11 C 0.2693(3) 0.2011(3) 0.16678(19) 0.0255(11) Uani 1 1 d . . .
C12 C 0.3538(4) 0.2005(3) 0.1537(2) 0.0334(13) Uani 1 1 d . . .
H12 H 0.3952 0.2041 0.1798 0.040 Uiso 1 1 calc R . .
C13 C 0.3781(4) 0.1947(3) 0.1034(2) 0.0398(14) Uani 1 1 d . . .
H13 H 0.4360 0.1958 0.0948 0.048 Uiso 1 1 calc R . .
C14 C 0.3187(4) 0.1874(3) 0.0656(2) 0.0441(16) Uani 1 1 d . . .
H14 H 0.3353 0.1829 0.0309 0.053 Uiso 1 1 calc R . .
C15 C 0.2343(4) 0.1867(4) 0.0786(2) 0.0441(15) Uani 1 1 d . . .
H15 H 0.1931 0.1814 0.0525 0.053 Uiso 1 1 calc R . .
C16 C 0.2093(4) 0.1937(3) 0.1289(2) 0.0357(13) Uani 1 1 d . . .
H16 H 0.1513 0.1935 0.1374 0.043 Uiso 1 1 calc R . .
C17 C 0.4593(3) 0.0517(3) 0.36964(19) 0.0257(11) Uani 1 1 d . . .
C18 C 0.4193(3) 0.0059(3) 0.33184(19) 0.0305(12) Uani 1 1 d . . .
H18 H 0.3684 0.0260 0.3174 0.037 Uiso 1 1 calc R . .
C19 C 0.4524(4) -0.0680(3) 0.3151(2) 0.0384(14) Uani 1 1 d . . .
H19 H 0.4234 -0.0995 0.2900 0.046 Uiso 1 1 calc R . .
C20 C 0.5278(4) -0.0968(4) 0.3346(2) 0.0437(15) Uani 1 1 d . . .
H20 H 0.5511 -0.1476 0.3227 0.052 Uiso 1 1 calc R . .
C21 C 0.5689(4) -0.0510(4) 0.3715(2) 0.0423(15) Uani 1 1 d . . .
H21 H 0.6207 -0.0704 0.3849 0.051 Uiso 1 1 calc R . .
C22 C 0.5353(3) 0.0232(3) 0.3892(2) 0.0342(13) Uani 1 1 d . . .
H22 H 0.5641 0.0544 0.4145 0.041 Uiso 1 1 calc R . .
C23 C 0.3332(3) 0.0895(3) 0.44152(18) 0.0227(11) Uani 1 1 d . . .
C24 C 0.3227(3) 0.0044(3) 0.4437(2) 0.0323(12) Uani 1 1 d . . .
H24 H 0.3479 -0.0299 0.4184 0.039 Uiso 1 1 calc R . .
C25 C 0.2759(4) -0.0312(4) 0.4823(2) 0.0408(14) Uani 1 1 d . . .
H25 H 0.2679 -0.0897 0.4827 0.049 Uiso 1 1 calc R . .
C26 C 0.2407(4) 0.0169(3) 0.5201(2) 0.0398(14) Uani 1 1 d . . .
H26 H 0.2098 -0.0084 0.5470 0.048 Uiso 1 1 calc R . .
C27 C 0.2503(3) 0.1015(3) 0.5188(2) 0.0356(13) Uani 1 1 d . . .
H27 H 0.2259 0.1352 0.5446 0.043 Uiso 1 1 calc R . .
C28 C 0.2962(3) 0.1374(3) 0.47951(19) 0.0289(12) Uani 1 1 d . . .
H28 H 0.3025 0.1961 0.4786 0.035 Uiso 1 1 calc R . .
C29 C 0.4731(3) 0.1935(3) 0.43942(19) 0.0259(11) Uani 1 1 d . . .
C30 C 0.4966(3) 0.1579(3) 0.4861(2) 0.0302(12) Uani 1 1 d . . .
H30 H 0.4798 0.1026 0.4937 0.036 Uiso 1 1 calc R . .
C31 C 0.5436(3) 0.2012(3) 0.5212(2) 0.0323(12) Uani 1 1 d . . .
H31 H 0.5592 0.1759 0.5526 0.039 Uiso 1 1 calc R . .
C32 C 0.5681(3) 0.2820(4) 0.5106(2) 0.0369(14) Uani 1 1 d . . .
H32 H 0.6006 0.3122 0.5348 0.044 Uiso 1 1 calc R . .
C33 C 0.5452(3) 0.3189(3) 0.4650(2) 0.0356(13) Uani 1 1 d . . .
H33 H 0.5611 0.3747 0.4580 0.043 Uiso 1 1 calc R . .
C34 C 0.4990(3) 0.2745(3) 0.4293(2) 0.0319(12) Uani 1 1 d . . .
H34 H 0.4849 0.2995 0.3976 0.038 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.047(5) . ?
Pd1 P1 2.3571(13) . ?
Pd1 I1 2.5998(7) . ?
Pd1 I2 2.6145(7) . ?
P1 C17 1.821(5) . ?
P1 C29 1.822(5) . ?
P1 C23 1.835(5) . ?
O17 C3 1.451(6) . ?
O17 H17 0.8400 . ?
N7 N12 1.322(6) . ?
N7 C2 1.364(6) . ?
N7 C9 1.468(6) . ?
N8 N12 1.336(5) . ?
N8 C1 1.350(6) . ?
N8 C10 1.468(6) . ?
C1 C2 1.390(7) . ?
C2 C3 1.510(7) . ?
C3 C4 1.521(7) . ?
C3 C8 1.528(7) . ?
C4 C5 1.522(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.521(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.543(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.515(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.500(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C16 1.383(7) . ?
C11 C12 1.387(7) . ?
C12 C13 1.376(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.375(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.380(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.389(7) . ?
C17 C22 1.393(7) . ?
C18 C19 1.374(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.380(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(8) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.382(7) . ?
C23 C28 1.390(7) . ?
C24 C25 1.380(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.378(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.371(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(7) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.392(7) . ?
C29 C30 1.403(7) . ?
C30 C31 1.375(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.385(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(7) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 P1 176.80(14) . . ?
C1 Pd1 I1 84.96(13) . . ?
P1 Pd1 I1 96.76(4) . . ?
C1 Pd1 I2 88.10(13) . . ?
P1 Pd1 I2 90.42(4) . . ?
I1 Pd1 I2 171.484(19) . . ?
C17 P1 C29 107.2(2) . . ?
C17 P1 C23 100.9(2) . . ?
C29 P1 C23 99.3(2) . . ?
C17 P1 Pd1 115.36(17) . . ?
C29 P1 Pd1 111.23(17) . . ?
C23 P1 Pd1 120.89(16) . . ?
C3 O17 H17 109.5 . . ?
N12 N7 C2 113.3(4) . . ?
N12 N7 C9 115.2(4) . . ?
C2 N7 C9 131.5(4) . . ?
N12 N8 C1 115.1(4) . . ?
N12 N8 C10 116.5(4) . . ?
C1 N8 C10 128.4(4) . . ?
N7 N12 N8 102.5(4) . . ?
N8 C1 C2 103.4(4) . . ?
N8 C1 Pd1 122.0(3) . . ?
C2 C1 Pd1 134.6(4) . . ?
N7 C2 C1 105.7(4) . . ?
N7 C2 C3 123.7(4) . . ?
C1 C2 C3 130.5(4) . . ?
O17 C3 C2 104.3(4) . . ?
O17 C3 C4 110.3(4) . . ?
C2 C3 C4 110.4(4) . . ?
O17 C3 C8 110.9(4) . . ?
C2 C3 C8 109.7(4) . . ?
C4 C3 C8 111.0(4) . . ?
C3 C4 C5 113.0(4) . . ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 C4 111.1(5) . . ?
C6 C5 H5A 109.4 . . ?
C4 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 C7 109.8(5) . . ?
C5 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C8 C7 C6 110.9(5) . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 C3 112.7(5) . . ?
C7 C8 H8A 109.1 . . ?
C3 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
C3 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
N7 C9 H9A 109.5 . . ?
N7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N8 C10 C11 110.1(4) . . ?
N8 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
N8 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.2 . . ?
C16 C11 C12 119.5(5) . . ?
C16 C11 C10 120.7(5) . . ?
C12 C11 C10 119.8(5) . . ?
C13 C12 C11 120.6(5) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 120.2(6) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 119.4(6) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 120.8(5) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C11 119.5(5) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
C18 C17 C22 119.1(5) . . ?
C18 C17 P1 116.9(4) . . ?
C22 C17 P1 123.7(4) . . ?
C19 C18 C17 120.7(5) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.3(5) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C21 C20 C19 119.3(5) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C22 120.7(5) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C17 119.8(5) . . ?
C21 C22 H22 120.1 . . ?
C17 C22 H22 120.1 . . ?
C24 C23 C28 118.1(5) . . ?
C24 C23 P1 123.0(4) . . ?
C28 C23 P1 118.6(4) . . ?
C25 C24 C23 120.4(5) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C26 C25 C24 120.9(5) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C27 C26 C25 119.7(5) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C26 C27 C28 119.4(5) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C27 C28 C23 121.5(5) . . ?
C27 C28 H28 119.3 . . ?
C23 C28 H28 119.3 . . ?
C34 C29 C30 118.1(5) . . ?
C34 C29 P1 119.9(4) . . ?
C30 C29 P1 121.8(4) . . ?
C31 C30 C29 121.4(5) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C30 C31 C32 119.7(5) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C33 C32 C31 120.1(5) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.0(5) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C29 120.7(5) . . ?
C33 C34 H34 119.6 . . ?
C29 C34 H34 119.6 . . ?

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
C1 Pd1 P1 C17 -108(2) . . . . ?
I1 Pd1 P1 C17 129.80(18) . . . . ?
I2 Pd1 P1 C17 -45.61(18) . . . . ?
C1 Pd1 P1 C29 14(2) . . . . ?
I1 Pd1 P1 C29 -107.84(18) . . . . ?
I2 Pd1 P1 C29 76.76(18) . . . . ?
C1 Pd1 P1 C23 130(2) . . . . ?
I1 Pd1 P1 C23 7.96(18) . . . . ?
I2 Pd1 P1 C23 -167.45(18) . . . . ?
C2 N7 N12 N8 -0.2(5) . . . . ?
C9 N7 N12 N8 178.8(4) . . . . ?
C1 N8 N12 N7 0.2(5) . . . . ?
C10 N8 N12 N7 -179.8(4) . . . . ?
N12 N8 C1 C2 -0.1(5) . . . . ?
C10 N8 C1 C2 179.9(5) . . . . ?
N12 N8 C1 Pd1 179.1(3) . . . . ?
C10 N8 C1 Pd1 -0.9(7) . . . . ?
P1 Pd1 C1 N8 154(2) . . . . ?
I1 Pd1 C1 N8 -83.5(4) . . . . ?
I2 Pd1 C1 N8 91.6(4) . . . . ?
P1 Pd1 C1 C2 -27(3) . . . . ?
I1 Pd1 C1 C2 95.3(5) . . . . ?
I2 Pd1 C1 C2 -89.6(5) . . . . ?
N12 N7 C2 C1 0.2(6) . . . . ?
C9 N7 C2 C1 -178.6(5) . . . . ?
N12 N7 C2 C3 177.3(4) . . . . ?
C9 N7 C2 C3 -1.5(8) . . . . ?
N8 C1 C2 N7 -0.1(5) . . . . ?
Pd1 C1 C2 N7 -179.0(4) . . . . ?
N8 C1 C2 C3 -177.0(5) . . . . ?
Pd1 C1 C2 C3 4.1(8) . . . . ?
N7 C2 C3 O17 37.5(6) . . . . ?
C1 C2 C3 O17 -146.1(5) . . . . ?
N7 C2 C3 C4 155.9(5) . . . . ?
C1 C2 C3 C4 -27.7(7) . . . . ?
N7 C2 C3 C8 -81.4(6) . . . . ?
C1 C2 C3 C8 95.0(6) . . . . ?
O17 C3 C4 C5 -71.7(6) . . . . ?
C2 C3 C4 C5 173.6(4) . . . . ?
C8 C3 C4 C5 51.7(6) . . . . ?
C3 C4 C5 C6 -55.3(6) . . . . ?
C4 C5 C6 C7 57.1(6) . . . . ?
C5 C6 C7 C8 -57.4(7) . . . . ?
C6 C7 C8 C3 55.4(6) . . . . ?
O17 C3 C8 C7 71.1(6) . . . . ?
C2 C3 C8 C7 -174.2(4) . . . . ?
C4 C3 C8 C7 -52.0(6) . . . . ?
N12 N8 C10 C11 49.2(6) . . . . ?
C1 N8 C10 C11 -130.8(5) . . . . ?
N8 C10 C11 C16 -110.7(5) . . . . ?
N8 C10 C11 C12 67.7(6) . . . . ?
C16 C11 C12 C13 1.6(8) . . . . ?
C10 C11 C12 C13 -176.8(5) . . . . ?
C11 C12 C13 C14 -1.6(8) . . . . ?
C12 C13 C14 C15 0.6(9) . . . . ?
C13 C14 C15 C16 0.3(9) . . . . ?
C14 C15 C16 C11 -0.3(9) . . . . ?
C12 C11 C16 C15 -0.6(8) . . . . ?
C10 C11 C16 C15 177.8(5) . . . . ?
C29 P1 C17 C18 -175.1(4) . . . . ?
C23 P1 C17 C18 81.4(4) . . . . ?
Pd1 P1 C17 C18 -50.6(4) . . . . ?
C29 P1 C17 C22 11.4(5) . . . . ?
C23 P1 C17 C22 -92.0(5) . . . . ?
Pd1 P1 C17 C22 135.9(4) . . . . ?
C22 C17 C18 C19 2.3(8) . . . . ?
P1 C17 C18 C19 -171.5(4) . . . . ?
C17 C18 C19 C20 -2.0(8) . . . . ?
C18 C19 C20 C21 0.7(9) . . . . ?
C19 C20 C21 C22 0.2(9) . . . . ?
C20 C21 C22 C17 0.2(9) . . . . ?
C18 C17 C22 C21 -1.4(8) . . . . ?
P1 C17 C22 C21 172.0(4) . . . . ?
C17 P1 C23 C24 -11.1(5) . . . . ?
C29 P1 C23 C24 -120.7(4) . . . . ?
Pd1 P1 C23 C24 117.5(4) . . . . ?
C17 P1 C23 C28 162.0(4) . . . . ?
C29 P1 C23 C28 52.3(4) . . . . ?
Pd1 P1 C23 C28 -69.5(4) . . . . ?
C28 C23 C24 C25 0.8(8) . . . . ?
P1 C23 C24 C25 173.8(4) . . . . ?
C23 C24 C25 C26 -1.8(9) . . . . ?
C24 C25 C26 C27 1.6(9) . . . . ?
C25 C26 C27 C28 -0.5(9) . . . . ?
C26 C27 C28 C23 -0.4(8) . . . . ?
C24 C23 C28 C27 0.3(8) . . . . ?
P1 C23 C28 C27 -173.1(4) . . . . ?
C17 P1 C29 C34 116.6(4) . . . . ?
C23 P1 C29 C34 -138.8(4) . . . . ?
Pd1 P1 C29 C34 -10.4(5) . . . . ?
C17 P1 C29 C30 -69.2(5) . . . . ?
C23 P1 C29 C30 35.4(5) . . . . ?
Pd1 P1 C29 C30 163.9(4) . . . . ?
C34 C29 C30 C31 0.3(8) . . . . ?
P1 C29 C30 C31 -174.0(4) . . . . ?
C29 C30 C31 C32 0.4(8) . . . . ?
C30 C31 C32 C33 0.0(8) . . . . ?
C31 C32 C33 C34 -1.1(9) . . . . ?
C32 C33 C34 C29 1.8(8) . . . . ?
C30 C29 C34 C33 -1.4(8) . . . . ?
P1 C29 C34 C33 173.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.39
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.101


