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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_I3
_database_code_depnum_ccdc_archive 'CCDC 1441626'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H32 N6 O5 Pd2'
_chemical_formula_weight         865.50

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.7725(6)
_cell_length_b                   12.4247(9)
_cell_length_c                   16.5407(12)
_cell_angle_alpha                70.7900(10)
_cell_angle_beta                 84.1970(10)
_cell_angle_gamma                87.9410(10)
_cell_volume                     1693.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7252
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      28.54

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             868
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7234
_exptl_absorpt_correction_T_max  0.8593
_exptl_absorpt_process_details   SADABS

_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  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20743
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         28.59
_reflns_number_total             7942
_reflns_number_gt                7583
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0321P)²+1.1216P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Patterson
_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         7942
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0639
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.136
_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 -0.073271(15) 0.313169(11) 0.247205(8) 0.01183(4) Uani 1 1 d . . .
Pd2 Pd 0.120387(15) 0.404608(11) 0.338417(8) 0.01123(4) Uani 1 1 d . . .
O1 O 0.05846(15) 0.43100(11) 0.13724(8) 0.0151(3) Uani 1 1 d . . .
O2 O 0.28656(15) 0.29104(11) 0.30068(9) 0.0153(3) Uani 1 1 d . . .
O3 O -0.02617(16) 0.05649(12) 0.22889(9) 0.0191(3) Uani 1 1 d . . .
O4 O 0.25882(16) 0.66994(11) 0.25878(9) 0.0171(3) Uani 1 1 d . . .
N1 N 0.09548(18) 0.19404(13) 0.26631(10) 0.0140(3) Uani 1 1 d . . .
N2 N -0.24736(18) 0.42334(14) 0.22940(10) 0.0153(3) Uani 1 1 d . . .
N3 N -0.36282(17) 0.39678(14) 0.29422(10) 0.0150(3) Uani 1 1 d . . .
N4 N 0.15204(17) 0.52635(13) 0.22116(10) 0.0132(3) Uani 1 1 d . . .
N5 N 0.08277(18) 0.29376(14) 0.45802(10) 0.0149(3) Uani 1 1 d . . .
N6 N -0.03739(19) 0.32256(14) 0.50595(10) 0.0162(3) Uani 1 1 d . . .
C1 C -0.2096(2) 0.23219(16) 0.34981(12) 0.0140(3) Uani 1 1 d . . .
C2 C -0.1846(2) 0.13068(16) 0.41575(13) 0.0172(4) Uani 1 1 d . . .
H2 H -0.0943 0.0876 0.4114 0.021 Uiso 1 1 calc R . .
C3 C -0.2900(2) 0.09180(17) 0.48774(13) 0.0206(4) Uani 1 1 d . . .
H3 H -0.2703 0.0231 0.5322 0.025 Uiso 1 1 calc R . .
C4 C -0.4237(2) 0.15237(17) 0.49518(13) 0.0205(4) Uani 1 1 d . . .
H4 H -0.4957 0.1244 0.5441 0.025 Uiso 1 1 calc R . .
C5 C -0.4522(2) 0.25412(17) 0.43085(13) 0.0176(4) Uani 1 1 d . . .
H5 H -0.5434 0.2963 0.4351 0.021 Uiso 1 1 calc R . .
C6 C -0.3445(2) 0.29246(16) 0.36043(12) 0.0146(3) Uani 1 1 d . . .
C7 C -0.4685(2) 0.48127(17) 0.28016(13) 0.0181(4) Uani 1 1 d . . .
H7 H -0.5596 0.4830 0.3161 0.022 Uiso 1 1 calc R . .
C8 C -0.4197(2) 0.56439(18) 0.20407(14) 0.0218(4) Uani 1 1 d . . .
H8 H -0.4700 0.6342 0.1772 0.026 Uiso 1 1 calc R . .
C9 C -0.2807(2) 0.52469(17) 0.17462(13) 0.0191(4) Uani 1 1 d . . .
H9 H -0.2195 0.5642 0.1233 0.023 Uiso 1 1 calc R . .
C10 C 0.2407(2) 0.20980(15) 0.28172(11) 0.0136(3) Uani 1 1 d . . .
C11 C 0.3390(2) 0.11280(16) 0.27247(12) 0.0156(4) Uani 1 1 d . . .
C12 C 0.4938(2) 0.09082(17) 0.27808(13) 0.0185(4) Uani 1 1 d . . .
H12 H 0.5589 0.1411 0.2911 0.022 Uiso 1 1 calc R . .
C13 C 0.5503(2) -0.00888(18) 0.26368(14) 0.0223(4) Uani 1 1 d . . .
H13 H 0.6564 -0.0264 0.2665 0.027 Uiso 1 1 calc R . .
C14 C 0.4542(2) -0.08272(17) 0.24538(14) 0.0225(4) Uani 1 1 d . . .
H14 H 0.4955 -0.1503 0.2367 0.027 Uiso 1 1 calc R . .
C15 C 0.2980(2) -0.05924(16) 0.23948(13) 0.0189(4) Uani 1 1 d . . .
H15 H 0.2319 -0.1094 0.2270 0.023 Uiso 1 1 calc R . .
C16 C 0.2439(2) 0.03998(16) 0.25255(12) 0.0154(4) Uani 1 1 d . . .
C17 C 0.0877(2) 0.09261(16) 0.24722(12) 0.0152(4) Uani 1 1 d . . .
C18 C -0.0497(2) 0.48534(16) 0.38122(12) 0.0144(3) Uani 1 1 d . . .
C19 C -0.1228(2) 0.58563(17) 0.33726(13) 0.0177(4) Uani 1 1 d . . .
H19 H -0.0828 0.6292 0.2808 0.021 Uiso 1 1 calc R . .
C20 C -0.2546(2) 0.62293(18) 0.37529(14) 0.0221(4) Uani 1 1 d . . .
H20 H -0.3030 0.6918 0.3446 0.027 Uiso 1 1 calc R . .
C21 C -0.3150(2) 0.56053(19) 0.45716(15) 0.0230(4) Uani 1 1 d . . .
H21 H -0.4053 0.5864 0.4820 0.028 Uiso 1 1 calc R . .
C22 C -0.2447(2) 0.46028(18) 0.50333(13) 0.0203(4) Uani 1 1 d . . .
H22 H -0.2847 0.4173 0.5599 0.024 Uiso 1 1 calc R . .
C23 C -0.1140(2) 0.42498(17) 0.46417(12) 0.0161(4) Uani 1 1 d . . .
C24 C -0.0567(2) 0.24385(18) 0.58500(13) 0.0218(4) Uani 1 1 d . . .
H24 H -0.1326 0.2451 0.6299 0.026 Uiso 1 1 calc R . .
C25 C 0.0537(3) 0.16163(18) 0.58856(13) 0.0228(4) Uani 1 1 d . . .
H25 H 0.0696 0.0952 0.6359 0.027 Uiso 1 1 calc R . .
C26 C 0.1381(2) 0.19622(16) 0.50782(13) 0.0190(4) Uani 1 1 d . . .
H26 H 0.2226 0.1558 0.4911 0.023 Uiso 1 1 calc R . .
C27 C 0.1197(2) 0.51488(15) 0.14593(12) 0.0134(3) Uani 1 1 d . . .
C28 C 0.1660(2) 0.62033(16) 0.07327(12) 0.0150(4) Uani 1 1 d . . .
C29 C 0.1519(2) 0.65126(17) -0.01385(13) 0.0196(4) Uani 1 1 d . . .
H29 H 0.1074 0.6015 -0.0379 0.024 Uiso 1 1 calc R . .
C30 C 0.2062(2) 0.75922(18) -0.06522(13) 0.0225(4) Uani 1 1 d . . .
H30 H 0.1979 0.7838 -0.1254 0.027 Uiso 1 1 calc R . .
C31 C 0.2723(2) 0.83112(17) -0.02926(13) 0.0215(4) Uani 1 1 d . . .
H31 H 0.3101 0.9033 -0.0656 0.026 Uiso 1 1 calc R . .
C32 C 0.2841(2) 0.79918(16) 0.05907(13) 0.0188(4) Uani 1 1 d . . .
H32 H 0.3284 0.8485 0.0836 0.023 Uiso 1 1 calc R . .
C33 C 0.2290(2) 0.69317(16) 0.10932(12) 0.0144(3) Uani 1 1 d . . .
C34 C 0.2187(2) 0.63333(15) 0.20453(12) 0.0139(3) Uani 1 1 d . . .
O5 O -0.2781(2) 0.75437(14) 0.02799(11) 0.0330(4) Uani 1 1 d . . .
C38 C -0.3981(3) 0.6433(2) -0.04132(16) 0.0379(6) Uani 1 1 d . . .
H38A H -0.4233 0.6422 -0.0974 0.057 Uiso 1 1 calc R . .
H38B H -0.4926 0.6393 -0.0035 0.057 Uiso 1 1 calc R . .
H38C H -0.3327 0.5777 -0.0156 0.057 Uiso 1 1 calc R . .
C37 C -0.3151(3) 0.7510(2) -0.05267(15) 0.0371(6) Uani 1 1 d . . .
H37A H -0.2199 0.7555 -0.0913 0.044 Uiso 1 1 calc R . .
H37B H -0.3802 0.8174 -0.0795 0.044 Uiso 1 1 calc R . .
C36 C -0.2012(4) 0.8561(2) 0.0208(2) 0.0476(7) Uani 1 1 d . . .
H36A H -0.2696 0.9224 -0.0007 0.057 Uiso 1 1 calc R . .
H36B H -0.1090 0.8659 -0.0206 0.057 Uiso 1 1 calc R . .
C35 C -0.1554(3) 0.8499(2) 0.1078(2) 0.0452(7) Uani 1 1 d . . .
H35A H -0.1021 0.9201 0.1028 0.068 Uiso 1 1 calc R . .
H35B H -0.0871 0.7845 0.1287 0.068 Uiso 1 1 calc R . .
H35C H -0.2472 0.8412 0.1485 0.068 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.9686(18) . ?
Pd1 N2 1.9920(16) . ?
Pd1 N1 2.0277(15) . ?
Pd1 O1 2.1752(13) . ?
Pd1 Pd2 2.8702(2) . ?
Pd2 C18 1.9700(18) . ?
Pd2 N5 2.0067(16) . ?
Pd2 N4 2.0292(15) . ?
Pd2 O2 2.1802(13) . ?
O1 C27 1.245(2) . ?
O2 C10 1.242(2) . ?
O3 C17 1.214(2) . ?
O4 C34 1.216(2) . ?
N1 C10 1.357(2) . ?
N1 C17 1.402(2) . ?
N2 C9 1.330(2) . ?
N2 N3 1.362(2) . ?
N3 C7 1.352(2) . ?
N3 C6 1.411(2) . ?
N4 C27 1.357(2) . ?
N4 C34 1.403(2) . ?
N5 C26 1.328(2) . ?
N5 N6 1.363(2) . ?
N6 C24 1.349(3) . ?
N6 C23 1.415(3) . ?
C1 C2 1.397(3) . ?
C1 C6 1.404(3) . ?
C2 C3 1.392(3) . ?
C3 C4 1.387(3) . ?
C4 C5 1.393(3) . ?
C5 C6 1.386(3) . ?
C7 C8 1.379(3) . ?
C8 C9 1.401(3) . ?
C10 C11 1.496(2) . ?
C11 C12 1.382(3) . ?
C11 C16 1.389(3) . ?
C12 C13 1.401(3) . ?
C13 C14 1.391(3) . ?
C14 C15 1.397(3) . ?
C15 C16 1.380(3) . ?
C16 C17 1.495(3) . ?
C18 C19 1.390(3) . ?
C18 C23 1.400(3) . ?
C19 C20 1.398(3) . ?
C20 C21 1.382(3) . ?
C21 C22 1.389(3) . ?
C22 C23 1.388(3) . ?
C24 C25 1.374(3) . ?
C25 C26 1.400(3) . ?
C27 C28 1.493(3) . ?
C28 C29 1.381(3) . ?
C28 C33 1.392(3) . ?
C29 C30 1.401(3) . ?
C30 C31 1.395(3) . ?
C31 C32 1.396(3) . ?
C32 C33 1.380(3) . ?
C33 C34 1.499(3) . ?
O5 C37 1.418(3) . ?
O5 C36 1.418(3) . ?
C38 C37 1.495(4) . ?
C36 C35 1.511(5) . ?

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 N2 81.47(7) . . ?
C1 Pd1 N1 96.48(7) . . ?
N2 Pd1 N1 176.83(6) . . ?
C1 Pd1 O1 169.39(6) . . ?
N2 Pd1 O1 89.52(6) . . ?
N1 Pd1 O1 92.75(6) . . ?
C1 Pd1 Pd2 94.88(5) . . ?
N2 Pd1 Pd2 101.88(5) . . ?
N1 Pd1 Pd2 80.67(4) . . ?
O1 Pd1 Pd2 81.44(4) . . ?
C18 Pd2 N5 81.51(7) . . ?
C18 Pd2 N4 94.54(7) . . ?
N5 Pd2 N4 175.55(6) . . ?
C18 Pd2 O2 170.89(6) . . ?
N5 Pd2 O2 91.98(6) . . ?
N4 Pd2 O2 92.17(6) . . ?
C18 Pd2 Pd1 93.33(5) . . ?
N5 Pd2 Pd1 101.08(5) . . ?
N4 Pd2 Pd1 81.14(4) . . ?
O2 Pd2 Pd1 81.61(3) . . ?
C27 O1 Pd1 119.18(12) . . ?
C10 O2 Pd2 119.50(12) . . ?
C10 N1 C17 109.68(15) . . ?
C10 N1 Pd1 125.40(12) . . ?
C17 N1 Pd1 123.64(12) . . ?
C9 N2 N3 106.99(15) . . ?
C9 N2 Pd1 138.12(14) . . ?
N3 N2 Pd1 114.54(12) . . ?
C7 N3 N2 110.17(16) . . ?
C7 N3 C6 134.77(17) . . ?
N2 N3 C6 115.03(15) . . ?
C27 N4 C34 109.23(15) . . ?
C27 N4 Pd2 125.40(13) . . ?
C34 N4 Pd2 125.29(12) . . ?
C26 N5 N6 106.30(16) . . ?
C26 N5 Pd2 139.81(14) . . ?
N6 N5 Pd2 113.88(12) . . ?
C24 N6 N5 110.56(17) . . ?
C24 N6 C23 133.98(17) . . ?
N5 N6 C23 115.46(15) . . ?
C2 C1 C6 116.78(17) . . ?
C2 C1 Pd1 129.35(14) . . ?
C6 C1 Pd1 113.58(14) . . ?
C3 C2 C1 120.92(18) . . ?
C4 C3 C2 120.69(19) . . ?
C3 C4 C5 119.97(18) . . ?
C6 C5 C4 118.46(18) . . ?
C5 C6 C1 123.15(18) . . ?
C5 C6 N3 121.70(17) . . ?
C1 C6 N3 115.15(16) . . ?
N3 C7 C8 107.33(17) . . ?
C7 C8 C9 105.81(18) . . ?
N2 C9 C8 109.70(18) . . ?
O2 C10 N1 126.16(17) . . ?
O2 C10 C11 124.70(17) . . ?
N1 C10 C11 109.14(16) . . ?
C12 C11 C16 121.52(17) . . ?
C12 C11 C10 131.96(18) . . ?
C16 C11 C10 106.49(16) . . ?
C11 C12 C13 117.04(18) . . ?
C14 C13 C12 121.27(19) . . ?
C13 C14 C15 121.13(18) . . ?
C16 C15 C14 117.13(18) . . ?
C15 C16 C11 121.89(18) . . ?
C15 C16 C17 130.90(18) . . ?
C11 C16 C17 107.20(16) . . ?
O3 C17 N1 125.24(17) . . ?
O3 C17 C16 127.28(18) . . ?
N1 C17 C16 107.48(16) . . ?
C19 C18 C23 117.04(17) . . ?
C19 C18 Pd2 128.79(15) . . ?
C23 C18 Pd2 113.75(14) . . ?
C18 C19 C20 120.63(19) . . ?
C21 C20 C19 120.6(2) . . ?
C20 C21 C22 120.47(19) . . ?
C23 C22 C21 117.87(19) . . ?
C22 C23 C18 123.41(19) . . ?
C22 C23 N6 121.47(18) . . ?
C18 C23 N6 115.12(16) . . ?
N6 C24 C25 107.36(18) . . ?
C24 C25 C26 105.61(18) . . ?
N5 C26 C25 110.18(18) . . ?
O1 C27 N4 126.24(17) . . ?
O1 C27 C28 124.09(17) . . ?
N4 C27 C28 109.66(16) . . ?
C29 C28 C33 121.97(18) . . ?
C29 C28 C27 131.54(18) . . ?
C33 C28 C27 106.47(16) . . ?
C28 C29 C30 117.03(19) . . ?
C31 C30 C29 120.93(19) . . ?
C30 C31 C32 121.36(19) . . ?
C33 C32 C31 117.35(18) . . ?
C32 C33 C28 121.34(18) . . ?
C32 C33 C34 131.82(18) . . ?
C28 C33 C34 106.84(16) . . ?
O4 C34 N4 125.24(17) . . ?
O4 C34 C33 126.96(17) . . ?
N4 C34 C33 107.80(15) . . ?
C37 O5 C36 112.5(2) . . ?
O5 C37 C38 110.3(2) . . ?
O5 C36 C35 109.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.918
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.099
####################################################################### 
# 
# 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_I5
_database_code_depnum_ccdc_archive 'CCDC 1441627'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H16 Cl N3 O Pd'
_chemical_formula_sum            'C22 H16 Cl N3 O Pd'
_chemical_formula_weight         480.23

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.3070(6)
_cell_length_b                   10.4711(7)
_cell_length_c                   10.4887(7)
_cell_angle_alpha                93.918(2)
_cell_angle_beta                 102.381(2)
_cell_angle_gamma                108.576(2)
_cell_volume                     936.02(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9946
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      29.42

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8282
_exptl_absorpt_correction_T_max  0.9446
_exptl_absorpt_process_details   SADABS

_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  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29136
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         29.45
_reflns_number_total             5189
_reflns_number_gt                4638
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0408P)²+1.1530P] 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         5189
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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 0.543124(19) 0.953867(17) 0.721074(17) 0.01721(6) Uani 1 1 d . . .
O1 O 0.6492(2) 0.81855(17) 0.76950(18) 0.0225(3) Uani 1 1 d . . .
N1 N 0.4172(2) 1.0700(2) 0.6497(2) 0.0208(4) Uani 1 1 d . . .
N3 N 0.7333(2) 1.10518(19) 0.85170(19) 0.0176(4) Uani 1 1 d . . .
C1 C 0.3652(3) 0.8120(2) 0.5948(2) 0.0213(5) Uani 1 1 d . . .
C12 C 1.0729(3) 1.0063(3) 0.8380(2) 0.0200(4) Uani 1 1 d . . .
H12 H 1.1468 1.0956 0.8675 0.024 Uiso 1 1 calc R . .
N2 N 0.2822(2) 1.0005(2) 0.5551(2) 0.0216(4) Uani 1 1 d . . .
C11 C 0.9123(3) 0.9839(2) 0.8286(2) 0.0180(4) Uani 1 1 d . . .
C17 C 0.7187(3) 1.2238(2) 0.9159(2) 0.0175(4) Uani 1 1 d . . .
C18 C 0.6101(3) 1.2078(2) 0.9918(2) 0.0194(4) Uani 1 1 d . . .
H18 H 0.5418 1.1192 0.9948 0.023 Uiso 1 1 calc R . .
C6 C 0.2507(3) 0.8585(3) 0.5254(2) 0.0229(5) Uani 1 1 d . . .
C2 C 0.3394(3) 0.6734(3) 0.5693(3) 0.0241(5) Uani 1 1 d . . .
H2 H 0.4144 0.6371 0.6137 0.029 Uiso 1 1 calc R . .
C15 C 0.8594(3) 0.7437(3) 0.7614(2) 0.0226(5) Uani 1 1 d . . .
H15 H 0.7890 0.6524 0.7390 0.027 Uiso 1 1 calc R . .
C16 C 0.8009(3) 0.8500(2) 0.7862(2) 0.0187(4) Uani 1 1 d . . .
C8 C 0.2977(3) 1.2152(3) 0.5742(3) 0.0264(5) Uani 1 1 d . . .
H8 H 0.2773 1.2976 0.5632 0.032 Uiso 1 1 calc R . .
C3 C 0.2045(3) 0.5876(3) 0.4791(3) 0.0251(5) Uani 1 1 d . . .
H3 H 0.1884 0.4931 0.4628 0.030 Uiso 1 1 calc R . .
C13 C 1.1245(3) 0.9024(3) 0.8059(2) 0.0231(5) Uani 1 1 d . . .
H13 H 1.2318 0.9199 0.8085 0.028 Uiso 1 1 calc R . .
C7 C 0.2070(3) 1.0870(3) 0.5083(2) 0.0251(5) Uani 1 1 d . . .
H7 H 0.1110 1.0632 0.4430 0.030 Uiso 1 1 calc R . .
C10 C 0.8725(3) 1.0977(2) 0.8734(2) 0.0180(4) Uani 1 1 d . . .
H10 H 0.9562 1.1749 0.9237 0.022 Uiso 1 1 calc R . .
C14 C 1.0157(3) 0.7696(3) 0.7690(2) 0.0247(5) Uani 1 1 d . . .
H14 H 1.0505 0.6964 0.7489 0.030 Uiso 1 1 calc R . .
C22 C 0.8102(3) 1.3538(2) 0.9033(2) 0.0210(5) Uani 1 1 d . . .
H22 H 0.8802 1.3650 0.8477 0.025 Uiso 1 1 calc R . .
C9 C 0.4260(3) 1.1996(3) 0.6605(2) 0.0238(5) Uani 1 1 d . . .
H9 H 0.5084 1.2719 0.7190 0.029 Uiso 1 1 calc R . .
C4 C 0.0923(3) 0.6382(3) 0.4123(3) 0.0279(5) Uani 1 1 d . . .
H4 H 0.0003 0.5779 0.3517 0.033 Uiso 1 1 calc R . .
C5 C 0.1147(3) 0.7752(3) 0.4341(2) 0.0254(5) Uani 1 1 d . . .
H5 H 0.0403 0.8115 0.3886 0.031 Uiso 1 1 calc R . .
C21 C 0.7998(3) 1.4674(2) 0.9720(3) 0.0223(5) Uani 1 1 d . . .
H21 H 0.8615 1.5565 0.9631 0.027 Uiso 1 1 calc R . .
C20 C 0.6983(3) 1.4489(2) 1.0532(2) 0.0201(4) Uani 1 1 d . . .
C19 C 0.6008(3) 1.3204(2) 1.0634(2) 0.0211(5) Uani 1 1 d . . .
H19 H 0.5296 1.3098 1.1178 0.025 Uiso 1 1 calc R . .
Cl1 Cl 0.69316(8) 1.59130(6) 1.14612(7) 0.02844(14) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.982(2) . ?
Pd1 O1 2.0039(18) . ?
Pd1 N1 2.017(2) . ?
Pd1 N3 2.097(2) . ?
O1 C16 1.312(3) . ?
N1 C9 1.329(3) . ?
N1 N2 1.370(3) . ?
N3 C10 1.295(3) . ?
N3 C17 1.431(3) . ?
C1 C2 1.391(4) . ?
C1 C6 1.396(4) . ?
C12 C13 1.371(3) . ?
C12 C11 1.418(3) . ?
N2 C7 1.367(3) . ?
N2 C6 1.419(3) . ?
C11 C16 1.424(3) . ?
C11 C10 1.435(3) . ?
C17 C22 1.389(3) . ?
C17 C18 1.392(3) . ?
C18 C19 1.390(3) . ?
C6 C5 1.394(3) . ?
C2 C3 1.390(4) . ?
C15 C14 1.375(4) . ?
C15 C16 1.418(3) . ?
C8 C7 1.376(4) . ?
C8 C9 1.398(4) . ?
C3 C4 1.397(4) . ?
C13 C14 1.404(4) . ?
C22 C21 1.389(3) . ?
C4 C5 1.378(4) . ?
C21 C20 1.381(3) . ?
C20 C19 1.389(3) . ?
C20 Cl1 1.744(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 O1 91.43(9) . . ?
C1 Pd1 N1 80.66(10) . . ?
O1 Pd1 N1 171.79(8) . . ?
C1 Pd1 N3 178.91(8) . . ?
O1 Pd1 N3 88.71(7) . . ?
N1 Pd1 N3 99.15(8) . . ?
C16 O1 Pd1 121.26(15) . . ?
C9 N1 N2 105.8(2) . . ?
C9 N1 Pd1 139.74(17) . . ?
N2 N1 Pd1 114.38(16) . . ?
C10 N3 C17 116.70(19) . . ?
C10 N3 Pd1 120.72(16) . . ?
C17 N3 Pd1 122.52(15) . . ?
C2 C1 C6 116.8(2) . . ?
C2 C1 Pd1 128.3(2) . . ?
C6 C1 Pd1 114.93(18) . . ?
C13 C12 C11 121.7(2) . . ?
C7 N2 N1 110.8(2) . . ?
C7 N2 C6 133.8(2) . . ?
N1 N2 C6 115.4(2) . . ?
C12 C11 C16 119.6(2) . . ?
C12 C11 C10 117.1(2) . . ?
C16 C11 C10 123.1(2) . . ?
C22 C17 C18 119.8(2) . . ?
C22 C17 N3 121.2(2) . . ?
C18 C17 N3 119.0(2) . . ?
C19 C18 C17 120.5(2) . . ?
C5 C6 C1 124.1(2) . . ?
C5 C6 N2 121.2(2) . . ?
C1 C6 N2 114.6(2) . . ?
C3 C2 C1 120.4(2) . . ?
C14 C15 C16 121.6(2) . . ?
O1 C16 C15 118.1(2) . . ?
O1 C16 C11 124.7(2) . . ?
C15 C16 C11 117.2(2) . . ?
C7 C8 C9 106.1(2) . . ?
C2 C3 C4 121.1(2) . . ?
C12 C13 C14 118.7(2) . . ?
N2 C7 C8 106.6(2) . . ?
N3 C10 C11 126.1(2) . . ?
C15 C14 C13 121.1(2) . . ?
C17 C22 C21 120.2(2) . . ?
N1 C9 C8 110.8(2) . . ?
C5 C4 C3 120.2(2) . . ?
C4 C5 C6 117.5(3) . . ?
C20 C21 C22 119.0(2) . . ?
C21 C20 C19 121.9(2) . . ?
C21 C20 Cl1 118.93(19) . . ?
C19 C20 Cl1 119.12(18) . . ?
C20 C19 C18 118.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.106
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_II3
_database_code_depnum_ccdc_archive 'CCDC 1441628'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H28 N4 O4 Pd2, C H2 Cl2'
_chemical_formula_sum            'C43 H30 Cl2 N4 O4 Pd2'
_chemical_formula_weight         950.41

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   9.7804(10)
_cell_length_b                   17.4573(18)
_cell_length_c                   22.148(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.068(3)
_cell_angle_gamma                90.00
_cell_volume                     3752.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9598
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      29.87

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8196
_exptl_absorpt_correction_T_max  0.9663
_exptl_absorpt_process_details   SADABS

_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  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            54211
_diffrn_reflns_av_R_equivalents  0.1224
_diffrn_reflns_av_sigmaI/netI    0.1632
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         29.95
_reflns_number_total             10701
_reflns_number_gt                5834
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0295P)²+40.2191P] 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         10701
_refine_ls_number_parameters     481
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_ref         0.1602
_refine_ls_wR_factor_gt          0.1244
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.21718(5) 0.79260(3) 0.34734(2) 0.01462(13) Uani 1 1 d . . .
Pd2 Pd 0.43620(6) 0.91065(3) 0.36127(2) 0.01598(13) Uani 1 1 d . . .
N1 N 0.2769(6) 0.7388(3) 0.2722(2) 0.0191(13) Uani 1 1 d . . .
N2 N 0.1671(6) 0.8385(3) 0.4256(2) 0.0168(12) Uani 1 1 d . . .
N3 N 0.5930(6) 0.8515(3) 0.4112(2) 0.0193(13) Uani 1 1 d . . .
N4 N 0.2964(6) 0.9695(3) 0.3049(2) 0.0173(12) Uani 1 1 d . . .
O1 O 0.3251(5) 0.9380(3) 0.4370(2) 0.0195(10) Uani 1 1 d . . .
O2 O -0.0173(5) 0.7609(3) 0.4421(2) 0.0228(11) Uani 1 1 d . . .
O3 O 0.1086(5) 0.8872(2) 0.3001(2) 0.0171(10) Uani 1 1 d . . .
O4 O 0.4292(5) 1.0747(3) 0.2841(2) 0.0281(12) Uani 1 1 d . . .
C1 C 0.3178(7) 0.7055(4) 0.3878(3) 0.0158(14) Uani 1 1 d . . .
C2 C 0.3260(7) 0.6836(4) 0.4484(3) 0.0218(15) Uani 1 1 d . . .
H2 H 0.2794 0.7124 0.4760 0.026 Uiso 1 1 calc R . .
C3 C 0.4032(8) 0.6190(4) 0.4689(3) 0.0261(17) Uani 1 1 d . . .
H3 H 0.4067 0.6037 0.5102 0.031 Uiso 1 1 calc R . .
C4 C 0.4745(8) 0.5773(4) 0.4299(3) 0.0264(17) Uani 1 1 d . . .
H4 H 0.5273 0.5340 0.4445 0.032 Uiso 1 1 calc R . .
C5 C 0.4688(8) 0.5985(4) 0.3697(3) 0.0259(17) Uani 1 1 d . . .
H5 H 0.5184 0.5704 0.3428 0.031 Uiso 1 1 calc R . .
C6 C 0.3892(8) 0.6617(4) 0.3486(3) 0.0219(16) Uani 1 1 d . . .
C7 C 0.3612(8) 0.6824(4) 0.2852(3) 0.0251(16) Uani 1 1 d . . .
H7 H 0.4026 0.6560 0.2547 0.030 Uiso 1 1 calc R . .
C8 C 0.2385(7) 0.7599(4) 0.2103(3) 0.0179(14) Uani 1 1 d . . .
C9 C 0.3319(8) 0.7564(4) 0.1683(3) 0.0248(16) Uani 1 1 d . . .
H9 H 0.4239 0.7402 0.1806 0.030 Uiso 1 1 calc R . .
C10 C 0.2910(8) 0.7766(5) 0.1085(3) 0.0301(18) Uani 1 1 d . . .
H10 H 0.3557 0.7757 0.0799 0.036 Uiso 1 1 calc R . .
C11 C 0.1556(8) 0.7982(5) 0.0899(3) 0.0316(18) Uani 1 1 d . . .
H11 H 0.1271 0.8103 0.0485 0.038 Uiso 1 1 calc R . .
C12 C 0.0624(9) 0.8020(5) 0.1320(3) 0.036(2) Uani 1 1 d . . .
H12 H -0.0297 0.8180 0.1197 0.043 Uiso 1 1 calc R . .
C13 C 0.1038(8) 0.7822(4) 0.1927(3) 0.0286(18) Uani 1 1 d . . .
H13 H 0.0398 0.7841 0.2216 0.034 Uiso 1 1 calc R . .
C14 C 0.2272(7) 0.9011(4) 0.4541(3) 0.0177(14) Uani 1 1 d . . .
C15 C 0.1590(7) 0.9199(4) 0.5081(3) 0.0210(15) Uani 1 1 d . . .
C16 C 0.1829(9) 0.9755(4) 0.5521(3) 0.0317(19) Uani 1 1 d . . .
H16 H 0.2559 1.0114 0.5514 0.038 Uiso 1 1 calc R . .
C17 C 0.0964(10) 0.9777(5) 0.5978(4) 0.041(2) Uani 1 1 d . . .
H17 H 0.1116 1.0149 0.6292 0.049 Uiso 1 1 calc R . .
C18 C -0.0118(9) 0.9259(5) 0.5980(4) 0.038(2) Uani 1 1 d . . .
H18 H -0.0708 0.9290 0.6289 0.046 Uiso 1 1 calc R . .
C19 C -0.0346(8) 0.8695(4) 0.5533(3) 0.0307(18) Uani 1 1 d . . .
H19 H -0.1072 0.8333 0.5535 0.037 Uiso 1 1 calc R . .
C20 C 0.0517(7) 0.8681(4) 0.5090(3) 0.0196(15) Uani 1 1 d . . .
C21 C 0.0589(7) 0.8156(4) 0.4560(3) 0.0181(14) Uani 1 1 d . . .
C22 C 0.5481(7) 0.8877(4) 0.2953(3) 0.0195(15) Uani 1 1 d . . .
C23 C 0.5226(8) 0.9050(4) 0.2339(3) 0.0224(15) Uani 1 1 d . . .
H23 H 0.4408 0.9315 0.2186 0.027 Uiso 1 1 calc R . .
C24 C 0.6165(8) 0.8838(4) 0.1946(3) 0.0266(17) Uani 1 1 d . . .
H24 H 0.5977 0.8957 0.1525 0.032 Uiso 1 1 calc R . .
C25 C 0.7366(8) 0.8457(4) 0.2157(3) 0.0262(17) Uani 1 1 d . . .
H25 H 0.7997 0.8315 0.1883 0.031 Uiso 1 1 calc R . .
C26 C 0.7647(8) 0.8284(4) 0.2762(3) 0.0256(17) Uani 1 1 d . . .
H26 H 0.8480 0.8031 0.2911 0.031 Uiso 1 1 calc R . .
C27 C 0.6699(7) 0.8483(4) 0.3158(3) 0.0206(15) Uani 1 1 d . . .
C28 C 0.6884(7) 0.8289(4) 0.3794(3) 0.0219(15) Uani 1 1 d . . .
H28 H 0.7664 0.8009 0.3972 0.026 Uiso 1 1 calc R . .
C29 C 0.6046(7) 0.8334(4) 0.4746(3) 0.0191(15) Uani 1 1 d . . .
C30 C 0.6420(8) 0.7602(4) 0.4953(3) 0.0257(17) Uani 1 1 d . . .
H30 H 0.6578 0.7210 0.4672 0.031 Uiso 1 1 calc R . .
C31 C 0.6560(8) 0.7449(4) 0.5573(3) 0.0264(17) Uani 1 1 d . . .
H31 H 0.6820 0.6951 0.5717 0.032 Uiso 1 1 calc R . .
C32 C 0.6323(8) 0.8017(4) 0.5980(3) 0.0280(18) Uani 1 1 d . . .
H32 H 0.6437 0.7911 0.6404 0.034 Uiso 1 1 calc R . .
C33 C 0.5918(8) 0.8742(4) 0.5774(3) 0.0271(17) Uani 1 1 d . . .
H33 H 0.5733 0.9131 0.6053 0.033 Uiso 1 1 calc R . .
C34 C 0.5786(7) 0.8894(4) 0.5154(3) 0.0220(15) Uani 1 1 d . . .
H34 H 0.5513 0.9391 0.5010 0.026 Uiso 1 1 calc R . .
C35 C 0.1643(7) 0.9475(4) 0.2867(3) 0.0196(15) Uani 1 1 d . . .
C36 C 0.0938(7) 1.0068(4) 0.2451(3) 0.0205(15) Uani 1 1 d . . .
C37 C -0.0367(8) 1.0101(4) 0.2139(3) 0.0297(18) Uani 1 1 d . . .
H37 H -0.1026 0.9709 0.2176 0.036 Uiso 1 1 calc R . .
C38 C -0.0677(9) 1.0731(5) 0.1767(4) 0.037(2) Uani 1 1 d . . .
H38 H -0.1569 1.0773 0.1545 0.045 Uiso 1 1 calc R . .
C39 C 0.0291(9) 1.1306(5) 0.1712(4) 0.038(2) Uani 1 1 d . . .
H39 H 0.0048 1.1733 0.1454 0.046 Uiso 1 1 calc R . .
C40 C 0.1603(8) 1.1261(4) 0.2028(3) 0.0297(18) Uani 1 1 d . . .
H40 H 0.2266 1.1652 0.1995 0.036 Uiso 1 1 calc R . .
C41 C 0.1909(8) 1.0637(4) 0.2389(3) 0.0229(16) Uani 1 1 d . . .
C42 C 0.3201(7) 1.0400(4) 0.2779(3) 0.0203(15) Uani 1 1 d . . .
C43 C 0.1372(13) 1.0688(7) 0.0386(5) 0.072(3) Uiso 1 1 d . . .
H43A H 0.0366 1.0765 0.0373 0.087 Uiso 1 1 calc R . .
H43B H 0.1841 1.1150 0.0571 0.087 Uiso 1 1 calc R . .
Cl1 Cl 0.1882(3) 0.98732(16) 0.08418(13) 0.0642(7) Uiso 1 1 d . . .
Cl2 Cl 0.1776(3) 1.05778(17) -0.03397(14) 0.0719(8) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.966(6) . ?
Pd1 N2 2.023(5) . ?
Pd1 N1 2.058(5) . ?
Pd1 O3 2.163(4) . ?
Pd1 Pd2 2.9611(8) . ?
Pd2 C22 1.971(7) . ?
Pd2 N4 2.016(5) . ?
Pd2 N3 2.055(6) . ?
Pd2 O1 2.162(5) . ?
N1 C7 1.295(9) . ?
N1 C8 1.424(8) . ?
N2 C14 1.358(8) . ?
N2 C21 1.382(9) . ?
N3 C28 1.298(9) . ?
N3 C29 1.429(8) . ?
N4 C35 1.361(9) . ?
N4 C42 1.400(9) . ?
O1 C14 1.250(8) . ?
O2 C21 1.227(8) . ?
O3 C35 1.238(8) . ?
O4 C42 1.220(8) . ?
C1 C2 1.388(9) . ?
C1 C6 1.405(9) . ?
C2 C3 1.401(9) . ?
C3 C4 1.382(10) . ?
C4 C5 1.378(10) . ?
C5 C6 1.398(10) . ?
C6 C7 1.441(10) . ?
C8 C9 1.382(10) . ?
C8 C13 1.384(10) . ?
C9 C10 1.382(10) . ?
C10 C11 1.389(11) . ?
C11 C12 1.384(11) . ?
C12 C13 1.398(10) . ?
C14 C15 1.478(9) . ?
C15 C16 1.375(10) . ?
C15 C20 1.387(9) . ?
C16 C17 1.398(11) . ?
C17 C18 1.392(11) . ?
C18 C19 1.395(10) . ?
C19 C20 1.372(10) . ?
C20 C21 1.497(9) . ?
C22 C23 1.385(9) . ?
C22 C27 1.403(10) . ?
C23 C24 1.392(10) . ?
C24 C25 1.381(10) . ?
C25 C26 1.367(10) . ?
C26 C27 1.396(10) . ?
C27 C28 1.438(9) . ?
C29 C34 1.376(9) . ?
C29 C30 1.392(10) . ?
C30 C31 1.389(10) . ?
C31 C32 1.380(11) . ?
C32 C33 1.387(11) . ?
C33 C34 1.389(10) . ?
C35 C36 1.496(9) . ?
C36 C37 1.376(10) . ?
C36 C41 1.393(10) . ?
C37 C38 1.385(10) . ?
C38 C39 1.395(12) . ?
C39 C40 1.387(11) . ?
C40 C41 1.363(10) . ?
C41 C42 1.498(10) . ?
C43 Cl2 1.712(12) . ?
C43 Cl1 1.780(12) . ?

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 N2 94.4(2) . . ?
C1 Pd1 N1 80.8(2) . . ?
N2 Pd1 N1 175.2(2) . . ?
C1 Pd1 O3 178.2(2) . . ?
N2 Pd1 O3 87.42(19) . . ?
N1 Pd1 O3 97.4(2) . . ?
C1 Pd1 Pd2 100.13(19) . . ?
N2 Pd1 Pd2 83.30(16) . . ?
N1 Pd1 Pd2 97.36(16) . . ?
O3 Pd1 Pd2 79.91(12) . . ?
C22 Pd2 N4 92.3(3) . . ?
C22 Pd2 N3 81.4(3) . . ?
N4 Pd2 N3 173.6(2) . . ?
C22 Pd2 O1 176.4(2) . . ?
N4 Pd2 O1 90.0(2) . . ?
N3 Pd2 O1 96.1(2) . . ?
C22 Pd2 Pd1 104.00(19) . . ?
N4 Pd2 Pd1 82.16(16) . . ?
N3 Pd2 Pd1 100.87(15) . . ?
O1 Pd2 Pd1 78.95(12) . . ?
C7 N1 C8 119.8(6) . . ?
C7 N1 Pd1 113.7(5) . . ?
C8 N1 Pd1 126.4(4) . . ?
C14 N2 C21 108.7(5) . . ?
C14 N2 Pd1 125.4(4) . . ?
C21 N2 Pd1 125.7(4) . . ?
C28 N3 C29 119.4(6) . . ?
C28 N3 Pd2 113.5(5) . . ?
C29 N3 Pd2 127.1(5) . . ?
C35 N4 C42 108.8(5) . . ?
C35 N4 Pd2 125.9(4) . . ?
C42 N4 Pd2 125.3(5) . . ?
C14 O1 Pd2 126.6(4) . . ?
C35 O3 Pd1 124.1(4) . . ?
C2 C1 C6 118.3(6) . . ?
C2 C1 Pd1 128.3(5) . . ?
C6 C1 Pd1 113.4(4) . . ?
C1 C2 C3 119.9(7) . . ?
C4 C3 C2 121.0(7) . . ?
C5 C4 C3 120.0(7) . . ?
C4 C5 C6 119.3(7) . . ?
C5 C6 C1 121.4(6) . . ?
C5 C6 C7 123.7(6) . . ?
C1 C6 C7 114.6(6) . . ?
N1 C7 C6 116.6(6) . . ?
C9 C8 C13 120.6(6) . . ?
C9 C8 N1 121.2(6) . . ?
C13 C8 N1 118.2(6) . . ?
C8 C9 C10 119.7(7) . . ?
C9 C10 C11 120.4(7) . . ?
C12 C11 C10 119.8(7) . . ?
C11 C12 C13 119.9(7) . . ?
C8 C13 C12 119.6(7) . . ?
O1 C14 N2 125.3(6) . . ?
O1 C14 C15 124.6(6) . . ?
N2 C14 C15 110.0(6) . . ?
C16 C15 C20 121.0(7) . . ?
C16 C15 C14 132.6(7) . . ?
C20 C15 C14 106.5(6) . . ?
C15 C16 C17 117.8(7) . . ?
C18 C17 C16 120.9(7) . . ?
C17 C18 C19 120.8(7) . . ?
C20 C19 C18 117.5(7) . . ?
C19 C20 C15 122.1(6) . . ?
C19 C20 C21 131.6(7) . . ?
C15 C20 C21 106.3(6) . . ?
O2 C21 N2 125.5(6) . . ?
O2 C21 C20 126.1(6) . . ?
N2 C21 C20 108.5(6) . . ?
C23 C22 C27 117.9(7) . . ?
C23 C22 Pd2 129.4(5) . . ?
C27 C22 Pd2 112.8(5) . . ?
C24 C23 C22 120.3(7) . . ?
C25 C24 C23 121.0(7) . . ?
C26 C25 C24 119.9(7) . . ?
C25 C26 C27 119.5(7) . . ?
C26 C27 C22 121.5(6) . . ?
C26 C27 C28 122.9(7) . . ?
C22 C27 C28 115.6(6) . . ?
N3 C28 C27 116.6(6) . . ?
C34 C29 C30 119.9(6) . . ?
C34 C29 N3 119.3(6) . . ?
C30 C29 N3 120.8(6) . . ?
C31 C30 C29 119.5(7) . . ?
C32 C31 C30 120.3(7) . . ?
C31 C32 C33 120.3(7) . . ?
C34 C33 C32 119.2(7) . . ?
C29 C34 C33 120.8(7) . . ?
O3 C35 N4 126.8(6) . . ?
O3 C35 C36 123.5(6) . . ?
N4 C35 C36 109.6(6) . . ?
C37 C36 C41 121.5(6) . . ?
C37 C36 C35 131.9(7) . . ?
C41 C36 C35 106.6(6) . . ?
C36 C37 C38 117.0(7) . . ?
C37 C38 C39 121.5(8) . . ?
C40 C39 C38 120.7(7) . . ?
C41 C40 C39 117.6(7) . . ?
C40 C41 C36 121.7(7) . . ?
C40 C41 C42 131.8(7) . . ?
C36 C41 C42 106.5(6) . . ?
O4 C42 N4 125.2(6) . . ?
O4 C42 C41 126.3(6) . . ?
N4 C42 C41 108.5(6) . . ?
Cl2 C43 Cl1 111.2(7) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         1.761
_refine_diff_density_min         -2.490
_refine_diff_density_rms         0.254
####################################################################### 
# 
# 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_II4
_database_code_depnum_ccdc_archive 'CCDC 1441629'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 N6 Pd2 S2'
_chemical_formula_sum            'C34 H30 N6 Pd2 S2'
_chemical_formula_weight         799.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/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'
'-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                   23.5263(19)
_cell_length_b                   10.5734(8)
_cell_length_c                   13.8590(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.96
_cell_angle_gamma                90.00
_cell_volume                     3072.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6838
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      28.62

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6810
_exptl_absorpt_correction_T_max  0.8775
_exptl_absorpt_process_details   SADABS

_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  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18269
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         28.65
_reflns_number_total             3749
_reflns_number_gt                3662
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0247P)²+5.0887P] 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         3749
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0201
_refine_ls_wR_factor_ref         0.0511
_refine_ls_wR_factor_gt          0.0506
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.003
_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 0.508507(5) 0.313578(11) 0.862141(9) 0.01199(5) Uani 1 1 d . . .
S1 S 0.605428(18) 0.40745(4) 0.90564(3) 0.01632(8) Uani 1 1 d . . .
N1 N 0.45768(6) 0.48579(13) 0.80674(11) 0.0141(3) Uani 1 1 d . . .
N2 N 0.42679(7) 0.21014(13) 0.83614(11) 0.0150(3) Uani 1 1 d . . .
N3 N 0.37432(6) 0.60246(13) 0.70365(11) 0.0167(3) Uani 1 1 d . . .
C1 C 0.54769(8) 0.14186(15) 0.90235(12) 0.0152(3) Uani 1 1 d . . .
C2 C 0.61072(8) 0.10179(17) 0.94115(14) 0.0208(3) Uani 1 1 d . . .
H2 H 0.6438 0.1628 0.9608 0.025 Uiso 1 1 calc R . .
C3 C 0.62590(9) -0.02679(18) 0.95152(15) 0.0251(4) Uani 1 1 d . . .
H3 H 0.6692 -0.0516 0.9785 0.030 Uiso 1 1 calc R . .
C4 C 0.57931(9) -0.11908(17) 0.92339(15) 0.0243(4) Uani 1 1 d . . .
H4 H 0.5904 -0.2061 0.9289 0.029 Uiso 1 1 calc R . .
C5 C 0.51648(9) -0.08263(17) 0.88711(15) 0.0218(3) Uani 1 1 d . . .
H5 H 0.4839 -0.1445 0.8690 0.026 Uiso 1 1 calc R . .
C6 C 0.50120(8) 0.04642(16) 0.87733(13) 0.0168(3) Uani 1 1 d . . .
C7 C 0.43683(8) 0.08923(16) 0.84377(14) 0.0188(3) Uani 1 1 d . . .
C8 C 0.36369(8) 0.25738(15) 0.80202(13) 0.0165(3) Uani 1 1 d . . .
C9 C 0.35497(8) 0.35981(16) 0.85712(14) 0.0180(3) Uani 1 1 d . . .
H9 H 0.3901 0.3936 0.9189 0.022 Uiso 1 1 calc R . .
C10 C 0.29468(8) 0.41227(16) 0.82135(15) 0.0212(3) Uani 1 1 d . . .
H10 H 0.2887 0.4822 0.8588 0.025 Uiso 1 1 calc R . .
C11 C 0.24296(8) 0.36310(18) 0.73094(16) 0.0242(4) Uani 1 1 d . . .
H11 H 0.2020 0.4009 0.7054 0.029 Uiso 1 1 calc R . .
C12 C 0.25158(9) 0.25823(18) 0.67822(15) 0.0248(4) Uani 1 1 d . . .
H12 H 0.2162 0.2226 0.6179 0.030 Uiso 1 1 calc R . .
C13 C 0.31185(8) 0.20559(17) 0.71358(15) 0.0208(3) Uani 1 1 d . . .
H13 H 0.3177 0.1342 0.6774 0.025 Uiso 1 1 calc R . .
C14 C 0.45212(8) 0.58390(15) 0.86806(13) 0.0166(3) Uani 1 1 d . . .
C15 C 0.40033(8) 0.65494(17) 0.80616(14) 0.0188(3) Uani 1 1 d . . .
C16 C 0.41024(7) 0.50028(15) 0.70644(13) 0.0143(3) Uani 1 1 d . . .
C17 C 0.31500(8) 0.64105(18) 0.61205(15) 0.0240(4) Uani 1 1 d . . .
H17A H 0.2988 0.7176 0.6310 0.036 Uiso 1 1 calc R . .
H17B H 0.2835 0.5731 0.5938 0.036 Uiso 1 1 calc R . .
H17C H 0.3228 0.6585 0.5496 0.036 Uiso 1 1 calc R . .
H7 H 0.4024(10) 0.032(2) 0.8295(17) 0.022(5) Uiso 1 1 d . . .
H14 H 0.4801(11) 0.596(2) 0.9415(19) 0.027(6) Uiso 1 1 d . . .
H15 H 0.3821(10) 0.726(2) 0.8221(18) 0.021(5) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.9977(16) . ?
Pd1 N2 2.0962(14) . ?
Pd1 N1 2.1219(13) . ?
Pd1 S1 2.3025(4) . ?
Pd1 Pd1 2.9485(3) 2_656 ?
S1 C16 1.7300(17) 2_656 ?
N1 C16 1.340(2) . ?
N1 C14 1.384(2) . ?
N2 C7 1.296(2) . ?
N2 C8 1.429(2) . ?
N3 C16 1.361(2) . ?
N3 C15 1.383(2) . ?
N3 C17 1.456(2) . ?
C1 C2 1.395(2) . ?
C1 C6 1.411(2) . ?
C2 C3 1.396(3) . ?
C3 C4 1.385(3) . ?
C4 C5 1.383(3) . ?
C5 C6 1.402(2) . ?
C6 C7 1.441(2) . ?
C8 C13 1.391(2) . ?
C8 C9 1.393(2) . ?
C9 C10 1.389(2) . ?
C10 C11 1.392(3) . ?
C11 C12 1.392(3) . ?
C12 C13 1.389(3) . ?
C14 C15 1.355(2) . ?
C16 S1 1.7300(16) 2_656 ?

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 N2 81.08(6) . . ?
C1 Pd1 N1 173.67(6) . . ?
N2 Pd1 N1 93.61(5) . . ?
C1 Pd1 S1 92.40(5) . . ?
N2 Pd1 S1 172.82(4) . . ?
N1 Pd1 S1 93.07(4) . . ?
C1 Pd1 Pd1 96.84(4) . 2_656 ?
N2 Pd1 Pd1 98.23(4) . 2_656 ?
N1 Pd1 Pd1 80.42(4) . 2_656 ?
S1 Pd1 Pd1 85.474(11) . 2_656 ?
C16 S1 Pd1 103.11(5) 2_656 . ?
C16 N1 C14 106.57(13) . . ?
C16 N1 Pd1 122.77(11) . . ?
C14 N1 Pd1 127.99(11) . . ?
C7 N2 C8 119.72(14) . . ?
C7 N2 Pd1 112.44(11) . . ?
C8 N2 Pd1 127.51(11) . . ?
C16 N3 C15 108.02(14) . . ?
C16 N3 C17 125.76(15) . . ?
C15 N3 C17 125.90(14) . . ?
C2 C1 C6 116.60(15) . . ?
C2 C1 Pd1 131.24(13) . . ?
C6 C1 Pd1 111.91(12) . . ?
C1 C2 C3 120.87(17) . . ?
C4 C3 C2 121.61(17) . . ?
C5 C4 C3 119.02(17) . . ?
C4 C5 C6 119.43(17) . . ?
C5 C6 C1 122.42(16) . . ?
C5 C6 C7 121.53(16) . . ?
C1 C6 C7 116.03(15) . . ?
N2 C7 C6 117.54(15) . . ?
C13 C8 C9 120.08(15) . . ?
C13 C8 N2 121.23(15) . . ?
C9 C8 N2 118.66(15) . . ?
C10 C9 C8 119.69(16) . . ?
C9 C10 C11 120.45(17) . . ?
C10 C11 C12 119.59(16) . . ?
C13 C12 C11 120.13(17) . . ?
C12 C13 C8 120.01(17) . . ?
C15 C14 N1 109.56(15) . . ?
C14 C15 N3 106.27(15) . . ?
N1 C16 N3 109.55(14) . . ?
N1 C16 S1 127.23(12) . 2_656 ?
N3 C16 S1 123.23(12) . 2_656 ?

_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.105
####################################################################### 
# 
# 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_II5
_database_code_depnum_ccdc_archive 'CCDC 1441630'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H19 Cl N2 O Pd'
_chemical_formula_sum            'C26 H19 Cl N2 O Pd'
_chemical_formula_weight         517.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P212121

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'

_cell_length_a                   9.3779(8)
_cell_length_b                   10.1838(9)
_cell_length_c                   22.3045(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2130.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9479
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      30.31

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7778
_exptl_absorpt_correction_T_max  0.9509
_exptl_absorpt_process_details   SADABS

_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  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31348
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         31.07
_reflns_number_total             6520
_reflns_number_gt                5271
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0465P)²+2.5940P] 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   0.97(3)
_refine_ls_number_reflns         6520
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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 0.97372(3) 0.65021(3) 0.209428(12) 0.01383(8) Uani 1 1 d . . .
Cl1 Cl 1.14858(13) 0.82473(13) 0.50311(5) 0.0322(3) Uani 1 1 d . . .
N1 N 1.1723(3) 0.6610(4) 0.24576(14) 0.0147(7) Uani 1 1 d . . .
N2 N 0.8497(3) 0.6289(3) 0.28761(16) 0.0151(6) Uani 1 1 d . . .
O1 O 0.8009(3) 0.6258(3) 0.15836(12) 0.0192(7) Uani 1 1 d . . .
C1 C 1.0845(5) 0.7028(4) 0.13613(18) 0.0180(8) Uani 1 1 d . . .
C2 C 1.0349(6) 0.7212(4) 0.07912(18) 0.0244(9) Uani 1 1 d . . .
H2 H 0.9395 0.6982 0.0694 0.029 Uiso 1 1 calc R . .
C3 C 1.1239(6) 0.7735(5) 0.03536(19) 0.0272(11) Uani 1 1 d . . .
H3 H 1.0886 0.7846 -0.0042 0.033 Uiso 1 1 calc R . .
C4 C 1.2651(6) 0.8103(5) 0.0485(2) 0.0302(11) Uani 1 1 d . . .
H4 H 1.3240 0.8483 0.0184 0.036 Uiso 1 1 calc R . .
C5 C 1.3168(5) 0.7903(4) 0.10591(18) 0.0195(9) Uani 1 1 d . . .
H5 H 1.4125 0.8121 0.1156 0.023 Uiso 1 1 calc R . .
C6 C 1.2264(5) 0.7378(4) 0.14911(17) 0.0140(8) Uani 1 1 d . . .
C7 C 1.2690(4) 0.7066(4) 0.2098(2) 0.0172(8) Uani 1 1 d . . .
H7 H 1.3644 0.7192 0.2229 0.021 Uiso 1 1 calc R . .
C8 C 1.2217(4) 0.6134(4) 0.30236(16) 0.0145(9) Uani 1 1 d . . .
C9 C 1.3065(5) 0.6916(4) 0.33919(19) 0.0184(9) Uani 1 1 d . . .
H9 H 1.3251 0.7801 0.3283 0.022 Uiso 1 1 calc R . .
C10 C 1.3639(4) 0.6413(5) 0.39149(17) 0.0221(9) Uani 1 1 d . . .
H10 H 1.4211 0.6954 0.4165 0.026 Uiso 1 1 calc R . .
C11 C 1.3379(5) 0.5123(4) 0.40731(18) 0.0209(9) Uani 1 1 d . . .
H11 H 1.3791 0.4772 0.4428 0.025 Uiso 1 1 calc R . .
C12 C 1.2512(5) 0.4334(4) 0.37141(18) 0.0202(9) Uani 1 1 d . . .
H12 H 1.2324 0.3452 0.3827 0.024 Uiso 1 1 calc R . .
C13 C 1.1922(5) 0.4843(4) 0.31895(18) 0.0178(8) Uani 1 1 d . . .
H13 H 1.1322 0.4312 0.2947 0.021 Uiso 1 1 calc R . .
C14 C 0.7228(4) 0.5795(4) 0.2877(2) 0.0158(8) Uani 1 1 d . . .
H14 H 0.6768 0.5709 0.3255 0.019 Uiso 1 1 calc R . .
C15 C 0.6454(4) 0.5366(4) 0.23605(18) 0.0164(8) Uani 1 1 d . . .
C16 C 0.5152(5) 0.4695(4) 0.24612(17) 0.0168(8) Uani 1 1 d . . .
H16 H 0.4872 0.4520 0.2863 0.020 Uiso 1 1 calc R . .
C17 C 0.4284(5) 0.4291(4) 0.2008(2) 0.0234(9) Uani 1 1 d . . .
H17 H 0.3436 0.3815 0.2092 0.028 Uiso 1 1 calc R . .
C18 C 0.4664(6) 0.4588(4) 0.14133(19) 0.0243(9) Uani 1 1 d . . .
H18 H 0.4058 0.4328 0.1093 0.029 Uiso 1 1 calc R . .
C19 C 0.5885(5) 0.5242(4) 0.12946(19) 0.0222(9) Uani 1 1 d . . .
H19 H 0.6103 0.5447 0.0889 0.027 Uiso 1 1 calc R . .
C20 C 0.6854(4) 0.5635(4) 0.17461(19) 0.0175(9) Uani 1 1 d . . .
C21 C 0.9062(4) 0.6775(4) 0.34362(17) 0.0135(8) Uani 1 1 d . . .
C22 C 0.9536(4) 0.8073(4) 0.34522(17) 0.0171(8) Uani 1 1 d . . .
H22 H 0.9386 0.8629 0.3116 0.021 Uiso 1 1 calc R . .
C23 C 1.0224(5) 0.8556(4) 0.39561(16) 0.0202(7) Uani 1 1 d . . .
H23 H 1.0539 0.9442 0.3973 0.024 Uiso 1 1 calc R . .
C24 C 1.0441(5) 0.7714(4) 0.44340(17) 0.0213(9) Uani 1 1 d . . .
C25 C 0.9934(4) 0.6445(4) 0.44311(16) 0.0206(9) Uani 1 1 d . . .
H25 H 1.0058 0.5897 0.4772 0.025 Uiso 1 1 calc R . .
C26 C 0.9240(5) 0.5976(4) 0.39258(18) 0.0187(9) Uani 1 1 d . . .
H26 H 0.8888 0.5101 0.3918 0.022 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 O1 1.996(3) . ?
Pd1 C1 2.010(4) . ?
Pd1 N1 2.034(3) . ?
Pd1 N2 2.107(4) . ?
Cl1 C24 1.741(4) . ?
N1 C7 1.297(5) . ?
N1 C8 1.430(5) . ?
N2 C14 1.293(5) . ?
N2 C21 1.445(5) . ?
O1 C20 1.306(5) . ?
C1 C2 1.367(6) . ?
C1 C6 1.407(6) . ?
C2 C3 1.390(7) . ?
C3 C4 1.407(7) . ?
C4 C5 1.385(6) . ?
C5 C6 1.390(6) . ?
C6 C7 1.447(6) . ?
C8 C13 1.394(6) . ?
C8 C9 1.394(6) . ?
C9 C10 1.383(6) . ?
C10 C11 1.382(7) . ?
C11 C12 1.395(6) . ?
C12 C13 1.394(6) . ?
C14 C15 1.430(6) . ?
C15 C16 1.417(6) . ?
C15 C20 1.447(6) . ?
C16 C17 1.362(6) . ?
C17 C18 1.406(6) . ?
C18 C19 1.351(7) . ?
C19 C20 1.415(6) . ?
C21 C26 1.372(6) . ?
C21 C22 1.395(6) . ?
C22 C23 1.387(5) . ?
C23 C24 1.383(6) . ?
C24 C25 1.376(6) . ?
C25 C26 1.387(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pd1 C1 89.35(15) . . ?
O1 Pd1 N1 167.78(12) . . ?
C1 Pd1 N1 80.59(16) . . ?
O1 Pd1 N2 90.65(13) . . ?
C1 Pd1 N2 170.36(14) . . ?
N1 Pd1 N2 100.44(12) . . ?
C7 N1 C8 116.2(3) . . ?
C7 N1 Pd1 114.4(3) . . ?
C8 N1 Pd1 129.1(3) . . ?
C14 N2 C21 118.0(4) . . ?
C14 N2 Pd1 123.4(3) . . ?
C21 N2 Pd1 118.6(2) . . ?
C20 O1 Pd1 125.1(3) . . ?
C2 C1 C6 118.6(4) . . ?
C2 C1 Pd1 128.1(4) . . ?
C6 C1 Pd1 112.9(3) . . ?
C1 C2 C3 120.1(5) . . ?
C2 C3 C4 121.4(4) . . ?
C5 C4 C3 118.8(4) . . ?
C4 C5 C6 119.0(4) . . ?
C5 C6 C1 122.1(4) . . ?
C5 C6 C7 124.4(4) . . ?
C1 C6 C7 113.5(4) . . ?
N1 C7 C6 117.6(4) . . ?
C13 C8 C9 119.7(4) . . ?
C13 C8 N1 119.4(4) . . ?
C9 C8 N1 120.8(4) . . ?
C10 C9 C8 120.5(4) . . ?
C11 C10 C9 119.9(4) . . ?
C10 C11 C12 120.2(4) . . ?
C13 C12 C11 119.9(4) . . ?
C12 C13 C8 119.6(4) . . ?
N2 C14 C15 125.8(4) . . ?
C16 C15 C14 117.2(4) . . ?
C16 C15 C20 117.7(4) . . ?
C14 C15 C20 125.0(4) . . ?
C17 C16 C15 122.9(4) . . ?
C16 C17 C18 118.9(4) . . ?
C19 C18 C17 120.3(4) . . ?
C18 C19 C20 123.0(4) . . ?
O1 C20 C19 118.2(4) . . ?
O1 C20 C15 124.7(4) . . ?
C19 C20 C15 117.0(4) . . ?
C26 C21 C22 120.2(4) . . ?
C26 C21 N2 122.0(4) . . ?
C22 C21 N2 117.6(3) . . ?
C23 C22 C21 120.3(4) . . ?
C24 C23 C22 118.2(4) . . ?
C25 C24 C23 121.9(4) . . ?
C25 C24 Cl1 119.4(3) . . ?
C23 C24 Cl1 118.6(3) . . ?
C24 C25 C26 119.3(4) . . ?
C21 C26 C25 119.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         2.770
_refine_diff_density_min         -1.646
_refine_diff_density_rms         0.143








