# 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_11081m
_database_code_depnum_ccdc_archive 'CCDC 1040521'
_audit_update_record             
;
2015-02-09 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         28 %     
RESPONSE: ...The crystal data is weak due to crystal quality.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C24 H24 N2 O3 Pd), 7(C H Cl3), H2 O '
_chemical_formula_sum            'C103 H105 Cl21 N8 O13 Pd4'
_chemical_formula_weight         2833.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2(1)/c

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

_cell_length_a                   27.533(6)
_cell_length_b                   19.525(4)
_cell_length_c                   23.435(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.63(3)
_cell_angle_gamma                90.00
_cell_volume                     11711(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    782
_cell_measurement_theta_min      2.221
_cell_measurement_theta_max      28.540

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5696
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.198
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   
;
absorption correction based on 0.1137 reflections(SADABS);Rint 0.1137 before
correction and 0.0687 after.
;


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

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22937
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.3482
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         0.80
_diffrn_reflns_theta_max         26.00
_reflns_number_total             22937
_reflns_number_gt                6367
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 

The crystal data was weak due to crystal quality.DELU and SIMU restraints were 
used for the whole structure. DFIX  distance restriants were also used fof
C20-C21, C20-C22, C20-C21A and C20-C22A bond distances. 


 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)+(0.0416P)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         22937
_refine_ls_number_parameters     1358
_refine_ls_number_restraints     1134
_refine_ls_R_factor_all          0.2822
_refine_ls_R_factor_gt           0.0958
_refine_ls_wR_factor_ref         0.1947
_refine_ls_wR_factor_gt          0.1419
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_restrained_S_all      0.808
_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 0.94597(4) 0.14200(5) -0.00933(4) 0.0342(3) Uani 1 1 d U . .
O1 O 0.9320(3) 0.1093(4) -0.0924(3) 0.043(2) Uani 1 1 d U . .
O2 O 0.9534(3) 0.2374(4) -0.0405(3) 0.038(2) Uani 1 1 d U . .
O3 O 1.0387(3) 0.2293(4) 0.0143(4) 0.046(2) Uani 1 1 d U . .
N1 N 0.9578(3) 0.1722(4) 0.0751(4) 0.027(2) Uani 1 1 d U . .
N2 N 0.9422(3) 0.0513(4) 0.0247(4) 0.029(2) Uani 1 1 d U . .
C1 C 0.9656(5) 0.2420(6) 0.0975(5) 0.035(3) Uani 1 1 d U . .
C2 C 0.9239(5) 0.2896(6) 0.0726(6) 0.051(4) Uani 1 1 d U . .
H2 H 0.8917 0.2758 0.0442 0.061 Uiso 1 1 calc R . .
C3 C 0.9327(6) 0.3564(7) 0.0916(6) 0.058(4) Uani 1 1 d U . .
H3 H 0.9054 0.3876 0.0763 0.070 Uiso 1 1 calc R . .
C4 C 0.9798(7) 0.3794(7) 0.1321(6) 0.060(4) Uani 1 1 d U . .
C5 C 1.0211(5) 0.3332(7) 0.1551(5) 0.053(4) Uani 1 1 d U . .
H5 H 1.0534 0.3475 0.1827 0.064 Uiso 1 1 calc R . .
C6 C 1.0126(5) 0.2643(6) 0.1357(5) 0.045(3) Uani 1 1 d U . .
H6 H 1.0403 0.2335 0.1495 0.054 Uiso 1 1 calc R . .
C7 C 0.9558(4) 0.1232(6) 0.1129(5) 0.034(3) Uani 1 1 d U . .
C8 C 0.9623(4) 0.1325(5) 0.1782(4) 0.042(3) Uani 1 1 d U . .
H8A H 0.9573 0.1799 0.1856 0.063 Uiso 1 1 calc R . .
H8B H 0.9968 0.1185 0.2042 0.063 Uiso 1 1 calc R . .
H8C H 0.9369 0.1051 0.1870 0.063 Uiso 1 1 calc R . .
C9 C 0.9500(4) 0.0529(6) 0.0860(5) 0.029(3) Uani 1 1 d U . .
C10 C 0.9549(4) -0.0044(6) 0.1207(6) 0.037(3) Uani 1 1 d U . .
H10 H 0.9603 -0.0015 0.1622 0.044 Uiso 1 1 calc R . .
C11 C 0.9517(5) -0.0664(6) 0.0925(6) 0.046(4) Uani 1 1 d U . .
H11 H 0.9560 -0.1066 0.1151 0.055 Uiso 1 1 calc R . .
C12 C 0.9423(5) -0.0696(6) 0.0315(6) 0.042(3) Uani 1 1 d U . .
H12 H 0.9395 -0.1124 0.0132 0.051 Uiso 1 1 calc R . .
C13 C 0.9367(4) -0.0105(6) -0.0056(5) 0.029(3) Uani 1 1 d U . .
C14 C 0.9270(5) -0.0125(6) -0.0716(5) 0.034(3) Uani 1 1 d U . .
C15 C 0.9228(5) 0.0451(6) -0.1082(6) 0.034(3) Uani 1 1 d U . .
C16 C 0.9108(5) 0.0336(6) -0.1715(6) 0.046(4) Uani 1 1 d U . .
H16 H 0.9100 0.0712 -0.1963 0.055 Uiso 1 1 calc R . .
C17 C 0.9004(5) -0.0306(6) -0.1986(6) 0.049(4) Uani 1 1 d U . .
H17 H 0.8904 -0.0356 -0.2408 0.059 Uiso 1 1 calc R . .
C18 C 0.9051(5) -0.0869(6) -0.1613(5) 0.041(3) Uani 1 1 d U . .
H18 H 0.9008 -0.1308 -0.1778 0.049 Uiso 1 1 calc R . .
C19 C 0.9163(4) -0.0776(6) -0.0994(5) 0.038(3) Uani 1 1 d U . .
H19 H 0.9169 -0.1156 -0.0752 0.046 Uiso 1 1 calc R . .
C20 C 0.9857(7) 0.4523(7) 0.1472(7) 0.087(5) Uani 1 1 d DU . .
H20 H 1.0263 0.4517 0.1807 0.104 Uiso 1 1 d R . .
C21 C 1.0017(6) 0.4998(6) 0.1073(6) 0.101(6) Uani 1 1 d DU . .
H21A H 1.0374 0.4910 0.1125 0.152 Uiso 1 1 calc R . .
H21B H 0.9982 0.5463 0.1186 0.152 Uiso 1 1 calc R . .
H21C H 0.9796 0.4925 0.0651 0.152 Uiso 1 1 calc R . .
C22 C 0.9741(7) 0.4750(7) 0.2010(6) 0.136(8) Uani 1 1 d DU . .
H22A H 0.9709 0.5240 0.2003 0.205 Uiso 1 1 calc R . .
H22B H 1.0020 0.4612 0.2380 0.205 Uiso 1 1 calc R . .
H22C H 0.9420 0.4547 0.1996 0.205 Uiso 1 1 calc R . .
C23 C 0.9990(6) 0.2622(7) -0.0141(6) 0.042(3) Uani 1 1 d U . .
C24 C 1.0028(5) 0.3402(6) -0.0223(5) 0.066(4) Uani 1 1 d U . .
H24A H 1.0250 0.3492 -0.0449 0.099 Uiso 1 1 calc R . .
H24B H 1.0172 0.3616 0.0173 0.099 Uiso 1 1 calc R . .
H24C H 0.9686 0.3584 -0.0443 0.099 Uiso 1 1 calc R . .
Pd1A Pd 0.81447(4) 0.13359(5) 1.04589(4) 0.0380(3) Uani 1 1 d U . .
O1A O 0.8324(3) 0.1042(4) 1.1297(3) 0.049(2) Uani 1 1 d U . .
O2A O 0.8203(3) 0.2316(4) 1.0771(4) 0.043(2) Uani 1 1 d U . .
O3A O 0.7399(4) 0.2362(4) 1.0779(4) 0.057(3) Uani 1 1 d U . .
N1A N 0.7985(4) 0.1610(5) 0.9595(4) 0.035(2) Uani 1 1 d U . .
N2A N 0.8121(3) 0.0411(4) 1.0110(4) 0.030(2) Uani 1 1 d U . .
C1A C 0.7921(5) 0.2307(6) 0.9378(6) 0.041(3) Uani 1 1 d U . .
C2A C 0.7482(5) 0.2659(6) 0.9371(5) 0.049(3) Uani 1 1 d U . .
H2A H 0.7230 0.2432 0.9476 0.058 Uiso 1 1 calc R . .
C3A C 0.7415(5) 0.3338(6) 0.9211(6) 0.057(4) Uani 1 1 d U . .
H3A H 0.7115 0.3568 0.9199 0.068 Uiso 1 1 calc R . .
C4A C 0.7805(6) 0.3686(8) 0.9065(6) 0.063(4) Uani 1 1 d U . .
C5A C 0.8232(6) 0.3310(7) 0.9074(6) 0.064(4) Uani 1 1 d U . .
H5A H 0.8491 0.3533 0.8979 0.077 Uiso 1 1 calc R . .
C6A C 0.8297(5) 0.2625(7) 0.9216(6) 0.059(4) Uani 1 1 d U . .
H6A H 0.8585 0.2385 0.9204 0.071 Uiso 1 1 calc R . .
C7A C 0.7970(5) 0.1092(6) 0.9244(6) 0.039(3) Uani 1 1 d U . .
C8A C 0.7877(5) 0.1169(6) 0.8577(5) 0.049(4) Uani 1 1 d U . .
H8A1 H 0.7822 0.1643 0.8464 0.074 Uiso 1 1 calc R . .
H8A2 H 0.7573 0.0910 0.8338 0.074 Uiso 1 1 calc R . .
H8A3 H 0.8175 0.1002 0.8499 0.074 Uiso 1 1 calc R . .
C9A C 0.8023(5) 0.0420(6) 0.9493(6) 0.038(3) Uani 1 1 d U . .
C10A C 0.7996(5) -0.0179(6) 0.9179(6) 0.046(3) Uani 1 1 d U . .
H10A H 0.7967 -0.0174 0.8771 0.055 Uiso 1 1 calc R . .
C11A C 0.8013(5) -0.0807(6) 0.9491(6) 0.044(4) Uani 1 1 d U . .
H11A H 0.7958 -0.1221 0.9280 0.053 Uiso 1 1 calc R . .
C12A C 0.8109(4) -0.0793(6) 1.0093(6) 0.035(3) Uani 1 1 d U . .
H12A H 0.8138 -0.1212 1.0292 0.042 Uiso 1 1 calc R . .
C13A C 0.8171(5) -0.0199(6) 1.0447(6) 0.037(3) Uani 1 1 d U . .
C14A C 0.8280(5) -0.0187(6) 1.1093(6) 0.036(3) Uani 1 1 d U . .
C15A C 0.8363(5) 0.0399(7) 1.1468(6) 0.043(3) Uani 1 1 d U . .
C16A C 0.8480(5) 0.0302(6) 1.2108(6) 0.048(4) Uani 1 1 d U . .
H16A H 0.8520 0.0685 1.2357 0.058 Uiso 1 1 calc R . .
C17A C 0.8535(5) -0.0338(7) 1.2372(6) 0.061(4) Uani 1 1 d U . .
H17A H 0.8627 -0.0383 1.2794 0.073 Uiso 1 1 calc R . .
C18A C 0.8451(5) -0.0911(7) 1.2002(6) 0.057(4) Uani 1 1 d U . .
H18A H 0.8472 -0.1345 1.2172 0.069 Uiso 1 1 calc R . .
C19A C 0.8337(5) -0.0840(6) 1.1385(6) 0.051(4) Uani 1 1 d U . .
H19A H 0.8296 -0.1233 1.1147 0.061 Uiso 1 1 calc R . .
C20A C 0.7772(7) 0.4433(8) 0.8957(6) 0.102(6) Uani 1 1 d DU . .
H20A H 0.8109 0.4458 0.8906 0.123 Uiso 1 1 calc R . .
C21A C 0.7947(7) 0.4873(7) 0.9523(7) 0.117(7) Uani 1 1 d DU . .
H21D H 0.7862 0.5343 0.9408 0.176 Uiso 1 1 calc R . .
H21E H 0.8318 0.4829 0.9732 0.176 Uiso 1 1 calc R . .
H21F H 0.7773 0.4730 0.9790 0.176 Uiso 1 1 calc R . .
C22A C 0.7470(9) 0.4635(8) 0.8320(7) 0.233(14) Uani 1 1 d DU . .
H22D H 0.7564 0.5092 0.8250 0.350 Uiso 1 1 calc R . .
H22E H 0.7103 0.4619 0.8249 0.350 Uiso 1 1 calc R . .
H22F H 0.7544 0.4325 0.8044 0.350 Uiso 1 1 calc R . .
C23A C 0.7813(6) 0.2608(7) 1.0845(6) 0.049(4) Uani 1 1 d U . .
C24A C 0.7946(5) 0.3369(6) 1.1048(6) 0.081(5) Uani 1 1 d U . .
H24D H 0.7822 0.3475 1.1371 0.122 Uiso 1 1 calc R . .
H24E H 0.7780 0.3667 1.0705 0.122 Uiso 1 1 calc R . .
H24F H 0.8317 0.3435 1.1194 0.122 Uiso 1 1 calc R . .
Pd1B Pd 0.69162(4) 0.86149(5) 0.02206(5) 0.0442(3) Uani 1 1 d U . .
N1B N 0.7024(4) 0.8359(5) 0.1076(5) 0.040(2) Uani 1 1 d U . .
N2B N 0.6942(4) 0.9551(5) 0.0559(5) 0.039(2) Uani 1 1 d U . .
O1B O 0.6784(3) 0.8900(4) -0.0621(3) 0.046(2) Uani 1 1 d U . .
O2B O 0.6927(3) 0.7641(4) -0.0062(4) 0.052(2) Uani 1 1 d U . .
O3B O 0.7796(3) 0.7653(4) 0.0406(4) 0.045(2) Uani 1 1 d U . .
C1B C 0.7094(5) 0.7655(6) 0.1296(6) 0.049(4) Uani 1 1 d U . .
C2B C 0.6652(5) 0.7244(6) 0.1129(6) 0.057(4) Uani 1 1 d U . .
H2B H 0.6321 0.7418 0.0907 0.069 Uiso 1 1 calc R . .
C3B C 0.6725(5) 0.6565(6) 0.1306(6) 0.060(4) Uani 1 1 d U . .
H3B H 0.6434 0.6279 0.1184 0.072 Uiso 1 1 calc R . .
C4B C 0.7194(6) 0.6290(7) 0.1647(6) 0.059(4) Uani 1 1 d U . .
C5B C 0.7615(5) 0.6735(6) 0.1813(5) 0.050(4) Uani 1 1 d U . .
H5B H 0.7945 0.6567 0.2047 0.060 Uiso 1 1 calc R . .
C6B C 0.7568(5) 0.7417(6) 0.1646(5) 0.041(3) Uani 1 1 d U . .
H6B H 0.7858 0.7705 0.1772 0.050 Uiso 1 1 calc R . .
C7B C 0.7069(5) 0.8871(6) 0.1445(6) 0.041(3) Uani 1 1 d U . .
C8B C 0.7156(5) 0.8813(6) 0.2120(5) 0.054(4) Uani 1 1 d U . .
H8B1 H 0.7037 0.8374 0.2199 0.081 Uiso 1 1 calc R . .
H8B2 H 0.6965 0.9168 0.2229 0.081 Uiso 1 1 calc R . .
H8B3 H 0.7522 0.8861 0.2360 0.081 Uiso 1 1 calc R . .
C9B C 0.7048(5) 0.9537(6) 0.1170(6) 0.037(3) Uani 1 1 d U . .
C10B C 0.7138(5) 1.0138(6) 0.1506(6) 0.052(4) Uani 1 1 d U . .
H10B H 0.7203 1.0129 0.1924 0.063 Uiso 1 1 calc R . .
C11B C 0.7130(5) 1.0752(7) 0.1209(7) 0.060(4) Uani 1 1 d U . .
H11B H 0.7199 1.1163 0.1426 0.072 Uiso 1 1 calc R . .
C12B C 0.7017(5) 1.0745(7) 0.0582(7) 0.058(4) Uani 1 1 d U . .
H12B H 0.7011 1.1159 0.0383 0.070 Uiso 1 1 calc R . .
C13B C 0.6912(5) 1.0144(7) 0.0238(7) 0.048(3) Uani 1 1 d U . .
C14B C 0.6793(5) 1.0149(7) -0.0423(7) 0.048(3) Uani 1 1 d U . .
C15B C 0.6734(5) 0.9559(7) -0.0805(7) 0.050(3) Uani 1 1 d U . .
C16B C 0.6628(5) 0.9647(7) -0.1441(6) 0.060(4) Uani 1 1 d U . .
H16B H 0.6605 0.9267 -0.1689 0.073 Uiso 1 1 calc R . .
C17B C 0.6560(5) 1.0291(7) -0.1689(7) 0.065(4) Uani 1 1 d U . .
H17B H 0.6476 1.0345 -0.2109 0.078 Uiso 1 1 calc R . .
C18B C 0.6612(6) 1.0854(7) -0.1330(7) 0.076(5) Uani 1 1 d U . .
H18B H 0.6580 1.1287 -0.1504 0.091 Uiso 1 1 calc R . .
C19B C 0.6712(5) 1.0790(7) -0.0722(7) 0.063(4) Uani 1 1 d U . .
H19B H 0.6728 1.1184 -0.0493 0.076 Uiso 1 1 calc R . .
C20B C 0.7248(7) 0.5522(7) 0.1819(7) 0.076(5) Uani 1 1 d U . .
H20B H 0.6904 0.5307 0.1637 0.092 Uiso 1 1 calc R . .
C21B C 0.7625(6) 0.5164(7) 0.1555(7) 0.111(6) Uani 1 1 d U . .
H21G H 0.7957 0.5393 0.1703 0.166 Uiso 1 1 calc R . .
H21H H 0.7479 0.5184 0.1115 0.166 Uiso 1 1 calc R . .
H21I H 0.7671 0.4695 0.1685 0.166 Uiso 1 1 calc R . .
C22B C 0.7441(7) 0.5406(7) 0.2464(7) 0.130(8) Uani 1 1 d U . .
H22G H 0.7804 0.5526 0.2638 0.195 Uiso 1 1 calc R . .
H22H H 0.7399 0.4931 0.2542 0.195 Uiso 1 1 calc R . .
H22I H 0.7248 0.5682 0.2646 0.195 Uiso 1 1 calc R . .
C23B C 0.7378(6) 0.7354(7) 0.0159(6) 0.044(4) Uani 1 1 d U . .
C24B C 0.7364(5) 0.6581(6) 0.0075(6) 0.077(5) Uani 1 1 d U . .
H24G H 0.7697 0.6426 0.0082 0.115 Uiso 1 1 calc R . .
H24H H 0.7098 0.6464 -0.0312 0.115 Uiso 1 1 calc R . .
H24I H 0.7289 0.6366 0.0401 0.115 Uiso 1 1 calc R . .
Pd1C Pd 0.55370(4) 0.85645(5) 1.01626(5) 0.0453(3) Uani 1 1 d U . .
O1C O 0.5659(3) 0.8788(4) 1.1008(4) 0.053(2) Uani 1 1 d U . .
O2C O 0.5439(3) 0.7582(4) 1.0375(4) 0.049(2) Uani 1 1 d U . .
O3C O 0.4570(3) 0.7701(4) 0.9984(4) 0.057(3) Uani 1 1 d U . .
N1C N 0.5420(4) 0.8366(5) 0.9302(5) 0.043(2) Uani 1 1 d U . .
N2C N 0.5605(4) 0.9523(5) 0.9893(6) 0.050(3) Uani 1 1 d U . .
C1C C 0.5329(5) 0.7699(7) 0.9037(6) 0.046(3) Uani 1 1 d U . .
C2C C 0.5706(5) 0.7193(6) 0.9245(6) 0.052(4) Uani 1 1 d U . .
H2C H 0.6030 0.7303 0.9540 0.062 Uiso 1 1 calc R . .
C3C C 0.5617(5) 0.6536(7) 0.9029(6) 0.062(4) Uani 1 1 d U . .
H3C H 0.5887 0.6217 0.9162 0.075 Uiso 1 1 calc R . .
C4C C 0.5131(6) 0.6339(7) 0.8614(6) 0.059(4) Uani 1 1 d U . .
C5C C 0.4759(5) 0.6836(7) 0.8414(6) 0.061(4) Uani 1 1 d U . .
H5C H 0.4434 0.6723 0.8124 0.074 Uiso 1 1 calc R . .
C6C C 0.4846(5) 0.7489(7) 0.8621(6) 0.059(4) Uani 1 1 d U . .
H6C H 0.4576 0.7806 0.8481 0.070 Uiso 1 1 calc R . .
C7C C 0.5422(5) 0.8897(7) 0.8967(7) 0.047(3) Uani 1 1 d U . .
C8C C 0.5339(5) 0.8882(6) 0.8292(5) 0.069(4) Uani 1 1 d U . .
H8C1 H 0.5358 0.8417 0.8167 0.103 Uiso 1 1 calc R . .
H8C2 H 0.5605 0.9149 0.8223 0.103 Uiso 1 1 calc R . .
H8C3 H 0.5002 0.9069 0.8057 0.103 Uiso 1 1 calc R . .
C9C C 0.5497(5) 0.9548(7) 0.9273(7) 0.052(3) Uani 1 1 d U . .
C10C C 0.5467(5) 1.0174(7) 0.8989(7) 0.064(4) Uani 1 1 d U . .
H10C H 0.5416 1.0199 0.8574 0.076 Uiso 1 1 calc R . .
C11C C 0.5516(5) 1.0770(7) 0.9336(8) 0.068(4) Uani 1 1 d U . .
H11C H 0.5479 1.1199 0.9152 0.081 Uiso 1 1 calc R . .
C12C C 0.5618(5) 1.0711(7) 0.9944(7) 0.060(4) Uani 1 1 d U . .
H12C H 0.5659 1.1114 1.0169 0.071 Uiso 1 1 calc R . .
C13C C 0.5666(5) 1.0087(7) 1.0264(8) 0.062(4) Uani 1 1 d U . .
C14C C 0.5783(5) 1.0014(7) 1.0921(7) 0.055(3) Uani 1 1 d U . .
C15C C 0.5776(5) 0.9408(7) 1.1245(7) 0.055(4) Uani 1 1 d U . .
C16C C 0.5891(5) 0.9454(7) 1.1880(7) 0.067(4) Uani 1 1 d U . .
H16C H 0.5877 0.9059 1.2096 0.081 Uiso 1 1 calc R . .
C17C C 0.6023(6) 1.0062(8) 1.2191(7) 0.076(4) Uani 1 1 d U . .
H17C H 0.6118 1.0075 1.2615 0.091 Uiso 1 1 calc R . .
C18C C 0.6013(6) 1.0663(8) 1.1863(8) 0.075(5) Uani 1 1 d U . .
H18C H 0.6087 1.1081 1.2066 0.090 Uiso 1 1 calc R . .
C19C C 0.5893(5) 1.0636(7) 1.1231(7) 0.072(4) Uani 1 1 d U . .
H19C H 0.5886 1.1038 1.1015 0.087 Uiso 1 1 calc R . .
C20C C 0.5037(6) 0.5617(7) 0.8386(7) 0.070(4) Uani 1 1 d U . .
H20C H 0.5362 0.5364 0.8595 0.084 Uiso 1 1 calc R . .
C21C C 0.4626(6) 0.5288(7) 0.8557(7) 0.109(6) Uani 1 1 d U . .
H21J H 0.4700 0.5359 0.8986 0.163 Uiso 1 1 calc R . .
H21K H 0.4619 0.4806 0.8474 0.163 Uiso 1 1 calc R . .
H21L H 0.4293 0.5486 0.8321 0.163 Uiso 1 1 calc R . .
C22C C 0.4915(7) 0.5550(7) 0.7718(6) 0.115(7) Uani 1 1 d U . .
H22J H 0.4590 0.5775 0.7497 0.172 Uiso 1 1 calc R . .
H22K H 0.4889 0.5074 0.7609 0.172 Uiso 1 1 calc R . .
H22L H 0.5189 0.5759 0.7616 0.172 Uiso 1 1 calc R . .
C23C C 0.4956(6) 0.7372(7) 1.0227(6) 0.051(4) Uani 1 1 d U . .
C24C C 0.4946(5) 0.6613(6) 1.0346(6) 0.075(5) Uani 1 1 d U . .
H24J H 0.4613 0.6492 1.0363 0.112 Uiso 1 1 calc R . .
H24K H 0.5218 0.6501 1.0729 0.112 Uiso 1 1 calc R . .
H24L H 0.4998 0.6363 1.0021 0.112 Uiso 1 1 calc R . .
C25 C 0.8815(5) 0.7961(6) 0.6286(5) 0.050(3) Uani 1 1 d U . .
H25 H 0.8449 0.7817 0.6090 0.060 Uiso 1 1 calc R . .
Cl1 Cl 0.91854(15) 0.7517(2) 0.59553(17) 0.0743(12) Uani 1 1 d U . .
Cl2 Cl 0.8851(2) 0.8833(2) 0.6181(2) 0.1216(19) Uani 1 1 d U . .
Cl3 Cl 0.90278(16) 0.7774(2) 0.70760(17) 0.0952(15) Uani 1 1 d U . .
C26 C 0.9210(5) 0.2353(6) 0.8073(6) 0.059(3) Uani 1 1 d U . .
H26 H 0.9333 0.2138 0.8479 0.071 Uiso 1 1 calc R . .
Cl4 Cl 0.95202(17) 0.19760(18) 0.76310(18) 0.0774(13) Uani 1 1 d U . .
Cl5 Cl 0.93669(19) 0.32330(19) 0.81539(17) 0.0957(16) Uani 1 1 d U . .
Cl6 Cl 0.85317(17) 0.2254(3) 0.7728(2) 0.1104(17) Uani 1 1 d U . .
C30 C 0.3761(9) 0.9531(11) 0.5043(12) 0.193(8) Uani 1 1 d U . .
H30 H 0.3983 0.9216 0.5356 0.231 Uiso 1 1 calc R . .
Cl7 Cl 0.3375(3) 0.9923(4) 0.5354(4) 0.250(4) Uani 1 1 d U . .
Cl8 Cl 0.4171(3) 1.0093(4) 0.4896(3) 0.213(3) Uani 1 1 d U . .
Cl9 Cl 0.3486(4) 0.9073(4) 0.4421(5) 0.397(7) Uani 1 1 d U . .
C31 C 0.6997(5) 0.2663(6) 0.1823(6) 0.058(4) Uani 1 1 d U . .
H31 H 0.7235 0.2606 0.1603 0.070 Uiso 1 1 calc R . .
Cl10 Cl 0.63746(14) 0.24548(19) 0.13292(17) 0.0716(12) Uani 1 1 d U . .
Cl11 Cl 0.70181(19) 0.3527(2) 0.20502(18) 0.1086(17) Uani 1 1 d U . .
Cl12 Cl 0.72179(16) 0.2152(2) 0.24771(18) 0.0833(14) Uani 1 1 d U . .
C32 C 0.6593(6) 0.7469(10) 0.3358(8) 0.130(6) Uani 1 1 d U . .
H32 H 0.6584 0.7256 0.3732 0.156 Uiso 1 1 calc R . .
Cl13 Cl 0.7082(2) 0.7148(3) 0.3108(3) 0.138(2) Uani 1 1 d U . .
Cl14 Cl 0.6016(2) 0.7453(3) 0.2749(3) 0.195(3) Uani 1 1 d U . .
Cl15 Cl 0.6759(2) 0.8415(3) 0.3428(2) 0.139(2) Uani 1 1 d U . .
C33 C 0.8619(5) 0.7984(6) 0.3975(5) 0.051(3) Uani 1 1 d U . .
H33 H 0.8976 0.7816 0.4183 0.061 Uiso 1 1 calc R . .
Cl16 Cl 0.83863(16) 0.7637(2) 0.32431(17) 0.0853(14) Uani 1 1 d U . .
Cl17 Cl 0.86516(19) 0.88794(19) 0.3941(2) 0.0987(16) Uani 1 1 d U . .
Cl18 Cl 0.82628(16) 0.7741(2) 0.44119(16) 0.0746(13) Uani 1 1 d U . .
C34 C 0.4191(6) 0.7107(7) 0.1526(6) 0.079(4) Uani 1 1 d U . .
H34 H 0.3975 0.7207 0.1097 0.095 Uiso 1 1 calc R . .
Cl19 Cl 0.38263(18) 0.7268(2) 0.19908(19) 0.0925(15) Uani 1 1 d U . .
Cl20 Cl 0.4348(2) 0.6214(2) 0.1600(2) 0.1185(19) Uani 1 1 d U . .
Cl21 Cl 0.47474(18) 0.7578(2) 0.1731(2) 0.1154(18) Uani 1 1 d U . .
O4 O 0.6368(3) 0.2486(5) 0.9821(4) 0.100(4) Uani 1 1 d . . .
H4A H 0.6620 0.2502 1.0207 0.120 Uiso 1 1 d R . .
H4B H 0.6130 0.2402 0.9957 0.120 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O1 1.947(7) . ?
Pd1 N2 1.961(9) . ?
Pd1 N1 1.972(9) . ?
Pd1 O2 2.038(8) . ?
O1 C15 1.306(12) . ?
O2 C23 1.274(14) . ?
O3 C23 1.232(14) . ?
N1 C7 1.319(12) . ?
N1 C1 1.449(13) . ?
N2 C9 1.373(12) . ?
N2 C13 1.379(12) . ?
C1 C6 1.347(14) . ?
C1 C2 1.424(15) . ?
C2 C3 1.371(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(17) . ?
C4 C20 1.461(16) . ?
C5 C6 1.412(14) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.484(13) . ?
C7 C9 1.495(14) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.360(14) . ?
C10 C11 1.368(14) . ?
C10 H10 0.9300 . ?
C11 C12 1.357(14) . ?
C11 H11 0.9300 . ?
C12 C13 1.418(14) . ?
C12 H12 0.9300 . ?
C13 C14 1.470(14) . ?
C14 C15 1.394(14) . ?
C14 C19 1.409(13) . ?
C15 C16 1.415(14) . ?
C16 C17 1.387(14) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(14) . ?
C17 H17 0.9300 . ?
C18 C19 1.379(14) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C22 1.478(9) . ?
C20 C21 1.493(9) . ?
C20 H20 1.1036 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.543(15) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
Pd1A O1A 1.928(8) . ?
Pd1A N2A 1.972(9) . ?
Pd1A N1A 1.980(9) . ?
Pd1A O2A 2.033(8) . ?
O1A C15A 1.310(13) . ?
O2A C23A 1.284(15) . ?
O3A C23A 1.193(15) . ?
N1A C7A 1.295(13) . ?
N1A C1A 1.440(13) . ?
N2A C9A 1.371(13) . ?
N2A C13A 1.409(13) . ?
C1A C6A 1.375(16) . ?
C1A C2A 1.386(15) . ?
C2A C3A 1.371(14) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.416(18) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.379(18) . ?
C4A C20A 1.479(18) . ?
C5A C6A 1.374(15) . ?
C5A H5A 0.9300 . ?
C6A H6A 0.9300 . ?
C7A C9A 1.422(15) . ?
C7A C8A 1.496(14) . ?
C8A H8A1 0.9600 . ?
C8A H8A2 0.9600 . ?
C8A H8A3 0.9600 . ?
C9A C10A 1.369(15) . ?
C10A C11A 1.420(14) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.336(14) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.400(14) . ?
C12A H12A 0.9300 . ?
C13A C14A 1.430(15) . ?
C14A C15A 1.410(15) . ?
C14A C19A 1.429(14) . ?
C15A C16A 1.425(14) . ?
C16A C17A 1.377(15) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.383(16) . ?
C17A H17A 0.9300 . ?
C18A C19A 1.369(15) . ?
C18A H18A 0.9300 . ?
C19A H19A 0.9300 . ?
C20A C22A 1.470(9) . ?
C20A C21A 1.503(9) . ?
C20A H20A 0.9800 . ?
C21A H21D 0.9600 . ?
C21A H21E 0.9600 . ?
C21A H21F 0.9600 . ?
C22A H22D 0.9600 . ?
C22A H22E 0.9600 . ?
C22A H22F 0.9600 . ?
C23A C24A 1.564(16) . ?
C24A H24D 0.9600 . ?
C24A H24E 0.9600 . ?
C24A H24F 0.9600 . ?
Pd1B O1B 1.951(8) . ?
Pd1B N2B 1.984(9) . ?
Pd1B N1B 1.978(10) . ?
Pd1B O2B 2.016(8) . ?
N1B C7B 1.298(14) . ?
N1B C1B 1.457(14) . ?
N2B C9B 1.351(13) . ?
N2B C13B 1.367(14) . ?
O1B C15B 1.347(13) . ?
O2B C23B 1.286(14) . ?
O3B C23B 1.228(13) . ?
C1B C6B 1.343(15) . ?
C1B C2B 1.388(15) . ?
C2B C3B 1.381(15) . ?
C2B H2B 0.9300 . ?
C3B C4B 1.353(16) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.385(16) . ?
C4B C20B 1.546(17) . ?
C5B C6B 1.380(14) . ?
C5B H5B 0.9300 . ?
C6B H6B 0.9300 . ?
C7B C9B 1.443(15) . ?
C7B C8B 1.515(15) . ?
C8B H8B1 0.9600 . ?
C8B H8B2 0.9600 . ?
C8B H8B3 0.9600 . ?
C9B C10B 1.383(15) . ?
C10B C11B 1.384(16) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.384(16) . ?
C11B H11B 0.9300 . ?
C12B C13B 1.393(16) . ?
C12B H12B 0.9300 . ?
C13B C14B 1.459(16) . ?
C14B C19B 1.412(15) . ?
C14B C15B 1.432(17) . ?
C15B C16B 1.420(16) . ?
C16B C17B 1.370(16) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.357(18) . ?
C17B H17B 0.9300 . ?
C18B C19B 1.354(17) . ?
C18B H18B 0.9300 . ?
C19B H19B 0.9300 . ?
C20B C22B 1.423(16) . ?
C20B C21B 1.553(19) . ?
C20B H20B 0.9800 . ?
C21B H21G 0.9600 . ?
C21B H21H 0.9600 . ?
C21B H21I 0.9600 . ?
C22B H22G 0.9600 . ?
C22B H22H 0.9600 . ?
C22B H22I 0.9600 . ?
C23B C24B 1.521(15) . ?
C24B H24G 0.9600 . ?
C24B H24H 0.9600 . ?
C24B H24I 0.9600 . ?
Pd1C O1C 1.934(8) . ?
Pd1C N1C 1.961(10) . ?
Pd1C N2C 2.005(10) . ?
Pd1C O2C 2.025(8) . ?
O1C C15C 1.321(14) . ?
O2C C23C 1.308(15) . ?
O3C C23C 1.193(14) . ?
N1C C7C 1.302(14) . ?
N1C C1C 1.424(14) . ?
N2C C9C 1.373(15) . ?
N2C C13C 1.376(15) . ?
C1C C6C 1.388(15) . ?
C1C C2C 1.387(15) . ?
C2C C3C 1.368(15) . ?
C2C H2C 0.9300 . ?
C3C C4C 1.388(16) . ?
C3C H3C 0.9300 . ?
C4C C5C 1.362(16) . ?
C4C C20C 1.496(17) . ?
C5C C6C 1.354(15) . ?
C5C H5C 0.9300 . ?
C6C H6C 0.9300 . ?
C7C C9C 1.436(17) . ?
C7C C8C 1.514(15) . ?
C8C H8C1 0.9600 . ?
C8C H8C2 0.9600 . ?
C8C H8C3 0.9600 . ?
C9C C10C 1.380(16) . ?
C10C C11C 1.398(17) . ?
C10C H10C 0.9300 . ?
C11C C12C 1.354(17) . ?
C11C H11C 0.9300 . ?
C12C C13C 1.411(17) . ?
C12C H12C 0.9300 . ?
C13C C14C 1.458(18) . ?
C14C C19C 1.391(16) . ?
C14C C15C 1.410(17) . ?
C15C C16C 1.405(17) . ?
C16C C17C 1.371(17) . ?
C16C H16C 0.9300 . ?
C17C C18C 1.398(18) . ?
C17C H17C 0.9300 . ?
C18C C19C 1.393(18) . ?
C18C H18C 0.9300 . ?
C19C H19C 0.9300 . ?
C20C C22C 1.481(16) . ?
C20C C21C 1.480(18) . ?
C20C H20C 0.9800 . ?
C21C H21J 0.9600 . ?
C21C H21K 0.9600 . ?
C21C H21L 0.9600 . ?
C22C H22J 0.9600 . ?
C22C H22K 0.9600 . ?
C22C H22L 0.9600 . ?
C23C C24C 1.510(15) . ?
C24C H24J 0.9600 . ?
C24C H24K 0.9600 . ?
C24C H24L 0.9600 . ?
C25 Cl2 1.727(12) . ?
C25 Cl1 1.726(12) . ?
C25 Cl3 1.761(12) . ?
C25 H25 0.9800 . ?
C26 Cl4 1.732(13) . ?
C26 Cl6 1.751(14) . ?
C26 Cl5 1.765(12) . ?
C26 H26 0.9800 . ?
C30 Cl9 1.64(2) . ?
C30 Cl7 1.68(2) . ?
C30 Cl8 1.70(2) . ?
C30 H30 0.9800 . ?
C31 Cl10 1.725(12) . ?
C31 Cl12 1.741(12) . ?
C31 Cl11 1.762(12) . ?
C31 H31 0.9800 . ?
C32 Cl14 1.700(17) . ?
C32 Cl13 1.768(18) . ?
C32 Cl15 1.895(17) . ?
C32 H32 0.9800 . ?
C33 Cl18 1.726(12) . ?
C33 Cl16 1.732(12) . ?
C33 Cl17 1.753(12) . ?
C33 H33 0.9800 . ?
C34 Cl21 1.697(14) . ?
C34 Cl19 1.762(15) . ?
C34 Cl20 1.790(14) . ?
C34 H34 0.9800 . ?
O4 H4A 0.9147 . ?
O4 H4B 0.8444 . ?

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 N2 95.2(3) . . ?
O1 Pd1 N1 177.5(4) . . ?
N2 Pd1 N1 82.9(4) . . ?
O1 Pd1 O2 87.1(3) . . ?
N2 Pd1 O2 176.9(3) . . ?
N1 Pd1 O2 94.9(3) . . ?
C15 O1 Pd1 123.0(7) . . ?
C23 O2 Pd1 112.7(8) . . ?
C7 N1 C1 118.4(10) . . ?
C7 N1 Pd1 115.2(8) . . ?
C1 N1 Pd1 126.4(7) . . ?
C9 N2 C13 120.3(10) . . ?
C9 N2 Pd1 113.2(7) . . ?
C13 N2 Pd1 126.4(8) . . ?
C6 C1 C2 119.6(12) . . ?
C6 C1 N1 121.5(12) . . ?
C2 C1 N1 118.4(10) . . ?
C3 C2 C1 117.9(13) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 123.0(14) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C5 119.0(13) . . ?
C3 C4 C20 118.6(15) . . ?
C5 C4 C20 122.3(15) . . ?
C4 C5 C6 118.5(12) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C1 C6 C5 121.7(13) . . ?
C1 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
N1 C7 C8 125.9(10) . . ?
N1 C7 C9 114.0(11) . . ?
C8 C7 C9 120.0(10) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 123.4(11) . . ?
C10 C9 C7 122.1(11) . . ?
N2 C9 C7 114.4(10) . . ?
C11 C10 C9 117.7(12) . . ?
C11 C10 H10 121.2 . . ?
C9 C10 H10 121.2 . . ?
C12 C11 C10 120.2(12) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 122.9(12) . . ?
C11 C12 H12 118.5 . . ?
C13 C12 H12 118.5 . . ?
N2 C13 C12 115.5(11) . . ?
N2 C13 C14 120.5(10) . . ?
C12 C13 C14 124.0(11) . . ?
C15 C14 C19 119.2(11) . . ?
C15 C14 C13 124.6(11) . . ?
C19 C14 C13 115.9(11) . . ?
O1 C15 C14 129.6(12) . . ?
O1 C15 C16 113.3(11) . . ?
C14 C15 C16 116.9(11) . . ?
C17 C16 C15 123.5(12) . . ?
C17 C16 H16 118.2 . . ?
C15 C16 H16 118.2 . . ?
C18 C17 C16 118.3(12) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
C17 C18 C19 119.6(11) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C14 122.1(11) . . ?
C18 C19 H19 118.9 . . ?
C14 C19 H19 118.9 . . ?
C22 C20 C21 123.6(13) . . ?
C22 C20 C4 117.4(11) . . ?
C21 C20 C4 119.0(11) . . ?
C22 C20 H20 82.9 . . ?
C21 C20 H20 89.8 . . ?
C4 C20 H20 98.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 O2 125.7(12) . . ?
O3 C23 C24 119.7(13) . . ?
O2 C23 C24 114.5(12) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1A Pd1A N2A 96.1(4) . . ?
O1A Pd1A N1A 177.5(4) . . ?
N2A Pd1A N1A 82.2(4) . . ?
O1A Pd1A O2A 87.6(3) . . ?
N2A Pd1A O2A 175.0(4) . . ?
N1A Pd1A O2A 94.1(4) . . ?
C15A O1A Pd1A 124.0(8) . . ?
C23A O2A Pd1A 120.5(9) . . ?
C7A N1A C1A 122.8(11) . . ?
C7A N1A Pd1A 112.4(8) . . ?
C1A N1A Pd1A 124.7(8) . . ?
C9A N2A C13A 122.8(10) . . ?
C9A N2A Pd1A 112.9(8) . . ?
C13A N2A Pd1A 124.2(8) . . ?
C6A C1A C2A 121.0(13) . . ?
C6A C1A N1A 121.2(12) . . ?
C2A C1A N1A 117.7(12) . . ?
C3A C2A C1A 120.8(14) . . ?
C3A C2A H2A 119.6 . . ?
C1A C2A H2A 119.6 . . ?
C2A C3A C4A 119.4(14) . . ?
C2A C3A H3A 120.3 . . ?
C4A C3A H3A 120.3 . . ?
C5A C4A C3A 117.4(14) . . ?
C5A C4A C20A 121.7(16) . . ?
C3A C4A C20A 120.7(15) . . ?
C6A C5A C4A 123.7(15) . . ?
C6A C5A H5A 118.1 . . ?
C4A C5A H5A 118.1 . . ?
C5A C6A C1A 117.6(14) . . ?
C5A C6A H6A 121.2 . . ?
C1A C6A H6A 121.2 . . ?
N1A C7A C9A 119.1(12) . . ?
N1A C7A C8A 122.6(11) . . ?
C9A C7A C8A 118.3(11) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10A C9A N2A 120.5(11) . . ?
C10A C9A C7A 126.2(13) . . ?
N2A C9A C7A 113.3(11) . . ?
C9A C10A C11A 118.5(12) . . ?
C9A C10A H10A 120.8 . . ?
C11A C10A H10A 120.8 . . ?
C12A C11A C10A 118.8(12) . . ?
C12A C11A H11A 120.6 . . ?
C10A C11A H11A 120.6 . . ?
C11A C12A C13A 125.2(12) . . ?
C11A C12A H12A 117.4 . . ?
C13A C12A H12A 117.4 . . ?
N2A C13A C12A 113.8(11) . . ?
N2A C13A C14A 121.1(11) . . ?
C12A C13A C14A 125.0(11) . . ?
C15A C14A C19A 117.5(12) . . ?
C15A C14A C13A 126.7(11) . . ?
C19A C14A C13A 115.8(12) . . ?
O1A C15A C14A 127.6(12) . . ?
O1A C15A C16A 114.3(12) . . ?
C14A C15A C16A 118.1(12) . . ?
C17A C16A C15A 122.6(13) . . ?
C17A C16A H16A 118.7 . . ?
C15A C16A H16A 118.7 . . ?
C18A C17A C16A 119.1(13) . . ?
C18A C17A H17A 120.5 . . ?
C16A C17A H17A 120.5 . . ?
C19A C18A C17A 120.1(13) . . ?
C19A C18A H18A 119.9 . . ?
C17A C18A H18A 119.9 . . ?
C18A C19A C14A 122.6(13) . . ?
C18A C19A H19A 118.7 . . ?
C14A C19A H19A 118.7 . . ?
C22A C20A C21A 128.4(16) . . ?
C22A C20A C4A 114.5(12) . . ?
C21A C20A C4A 115.7(12) . . ?
C22A C20A H20A 94.0 . . ?
C21A C20A H20A 94.0 . . ?
C4A C20A H20A 94.0 . . ?
C20A C21A H21D 109.5 . . ?
C20A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C20A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C20A C22A H22D 109.5 . . ?
C20A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C20A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3A C23A O2A 127.7(14) . . ?
O3A C23A C24A 121.8(15) . . ?
O2A C23A C24A 110.5(13) . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
O1B Pd1B N2B 96.2(4) . . ?
O1B Pd1B N1B 177.2(4) . . ?
N2B Pd1B N1B 81.8(4) . . ?
O1B Pd1B O2B 87.6(3) . . ?
N2B Pd1B O2B 175.8(4) . . ?
N1B Pd1B O2B 94.5(4) . . ?
C7B N1B C1B 121.5(11) . . ?
C7B N1B Pd1B 115.0(9) . . ?
C1B N1B Pd1B 123.3(8) . . ?
C9B N2B C13B 123.1(11) . . ?
C9B N2B Pd1B 111.5(8) . . ?
C13B N2B Pd1B 125.0(10) . . ?
C15B O1B Pd1B 123.7(8) . . ?
C23B O2B Pd1B 114.1(8) . . ?
C6B C1B C2B 121.8(13) . . ?
C6B C1B N1B 121.0(12) . . ?
C2B C1B N1B 117.3(12) . . ?
C3B C2B C1B 117.0(13) . . ?
C3B C2B H2B 121.5 . . ?
C1B C2B H2B 121.5 . . ?
C4B C3B C2B 124.0(13) . . ?
C4B C3B H3B 118.0 . . ?
C2B C3B H3B 118.0 . . ?
C3B C4B C5B 115.8(13) . . ?
C3B C4B C20B 121.2(13) . . ?
C5B C4B C20B 123.0(13) . . ?
C6B C5B C4B 123.0(13) . . ?
C6B C5B H5B 118.5 . . ?
C4B C5B H5B 118.5 . . ?
C1B C6B C5B 118.4(13) . . ?
C1B C6B H6B 120.8 . . ?
C5B C6B H6B 120.8 . . ?
N1B C7B C9B 114.7(12) . . ?
N1B C7B C8B 125.4(11) . . ?
C9B C7B C8B 119.9(12) . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
N2B C9B C10B 120.6(12) . . ?
N2B C9B C7B 116.6(11) . . ?
C10B C9B C7B 122.7(13) . . ?
C11B C10B C9B 118.8(14) . . ?
C11B C10B H10B 120.6 . . ?
C9B C10B H10B 120.6 . . ?
C12B C11B C10B 118.7(14) . . ?
C12B C11B H11B 120.6 . . ?
C10B C11B H11B 120.6 . . ?
C11B C12B C13B 122.8(14) . . ?
C11B C12B H12B 118.6 . . ?
C13B C12B H12B 118.6 . . ?
N2B C13B C12B 115.8(13) . . ?
N2B C13B C14B 122.3(12) . . ?
C12B C13B C14B 121.8(13) . . ?
C19B C14B C15B 116.2(14) . . ?
C19B C14B C13B 117.7(13) . . ?
C15B C14B C13B 126.0(12) . . ?
O1B C15B C16B 114.1(13) . . ?
O1B C15B C14B 126.4(13) . . ?
C16B C15B C14B 119.5(13) . . ?
C17B C16B C15B 119.9(14) . . ?
C17B C16B H16B 120.0 . . ?
C15B C16B H16B 120.0 . . ?
C18B C17B C16B 120.9(15) . . ?
C18B C17B H17B 119.5 . . ?
C16B C17B H17B 119.5 . . ?
C19B C18B C17B 120.8(14) . . ?
C19B C18B H18B 119.6 . . ?
C17B C18B H18B 119.6 . . ?
C18B C19B C14B 122.5(15) . . ?
C18B C19B H19B 118.7 . . ?
C14B C19B H19B 118.7 . . ?
C22B C20B C4B 113.2(12) . . ?
C22B C20B C21B 108.0(15) . . ?
C4B C20B C21B 110.3(13) . . ?
C22B C20B H20B 108.4 . . ?
C4B C20B H20B 108.4 . . ?
C21B C20B H20B 108.4 . . ?
C20B C21B H21G 109.5 . . ?
C20B C21B H21H 109.5 . . ?
H21G C21B H21H 109.5 . . ?
C20B C21B H21I 109.5 . . ?
H21G C21B H21I 109.5 . . ?
H21H C21B H21I 109.5 . . ?
C20B C22B H22G 109.5 . . ?
C20B C22B H22H 109.5 . . ?
H22G C22B H22H 109.5 . . ?
C20B C22B H22I 109.5 . . ?
H22G C22B H22I 109.5 . . ?
H22H C22B H22I 109.5 . . ?
O3B C23B O2B 125.5(13) . . ?
O3B C23B C24B 120.5(13) . . ?
O2B C23B C24B 114.0(12) . . ?
C23B C24B H24G 109.5 . . ?
C23B C24B H24H 109.5 . . ?
H24G C24B H24H 109.5 . . ?
C23B C24B H24I 109.5 . . ?
H24G C24B H24I 109.5 . . ?
H24H C24B H24I 109.5 . . ?
O1C Pd1C N1C 178.2(4) . . ?
O1C Pd1C N2C 96.4(4) . . ?
N1C Pd1C N2C 81.9(4) . . ?
O1C Pd1C O2C 87.2(3) . . ?
N1C Pd1C O2C 94.6(4) . . ?
N2C Pd1C O2C 176.1(4) . . ?
C15C O1C Pd1C 124.1(9) . . ?
C23C O2C Pd1C 116.5(8) . . ?
C7C N1C C1C 120.4(12) . . ?
C7C N1C Pd1C 115.3(10) . . ?
C1C N1C Pd1C 124.3(8) . . ?
C9C N2C C13C 124.6(13) . . ?
C9C N2C Pd1C 111.0(9) . . ?
C13C N2C Pd1C 123.6(11) . . ?
C6C C1C C2C 115.8(13) . . ?
C6C C1C N1C 123.1(12) . . ?
C2C C1C N1C 120.6(12) . . ?
C3C C2C C1C 122.0(13) . . ?
C3C C2C H2C 119.0 . . ?
C1C C2C H2C 119.0 . . ?
C2C C3C C4C 120.9(13) . . ?
C2C C3C H3C 119.6 . . ?
C4C C3C H3C 119.6 . . ?
C5C C4C C3C 116.9(14) . . ?
C5C C4C C20C 122.7(14) . . ?
C3C C4C C20C 120.4(14) . . ?
C4C C5C C6C 122.4(14) . . ?
C4C C5C H5C 118.8 . . ?
C6C C5C H5C 118.8 . . ?
C5C C6C C1C 121.8(13) . . ?
C5C C6C H6C 119.1 . . ?
C1C C6C H6C 119.1 . . ?
N1C C7C C9C 115.9(14) . . ?
N1C C7C C8C 125.5(13) . . ?
C9C C7C C8C 118.6(13) . . ?
C7C C8C H8C1 109.5 . . ?
C7C C8C H8C2 109.5 . . ?
H8C1 C8C H8C2 109.5 . . ?
C7C C8C H8C3 109.5 . . ?
H8C1 C8C H8C3 109.5 . . ?
H8C2 C8C H8C3 109.5 . . ?
N2C C9C C10C 119.6(14) . . ?
N2C C9C C7C 115.6(12) . . ?
C10C C9C C7C 124.8(16) . . ?
C9C C10C C11C 118.7(16) . . ?
C9C C10C H10C 120.6 . . ?
C11C C10C H10C 120.6 . . ?
C12C C11C C10C 118.7(15) . . ?
C12C C11C H11C 120.6 . . ?
C10C C11C H11C 120.6 . . ?
C11C C12C C13C 125.2(15) . . ?
C11C C12C H12C 117.4 . . ?
C13C C12C H12C 117.4 . . ?
N2C C13C C12C 113.0(15) . . ?
N2C C13C C14C 121.1(13) . . ?
C12C C13C C14C 125.9(14) . . ?
C19C C14C C15C 119.6(16) . . ?
C19C C14C C13C 112.8(14) . . ?
C15C C14C C13C 127.6(14) . . ?
O1C C15C C16C 115.4(14) . . ?
O1C C15C C14C 126.3(14) . . ?
C16C C15C C14C 118.3(14) . . ?
C17C C16C C15C 122.0(16) . . ?
C17C C16C H16C 119.0 . . ?
C15C C16C H16C 119.0 . . ?
C16C C17C C18C 119.1(16) . . ?
C16C C17C H17C 120.4 . . ?
C18C C17C H17C 120.4 . . ?
C19C C18C C17C 120.1(15) . . ?
C19C C18C H18C 119.9 . . ?
C17C C18C H18C 119.9 . . ?
C18C C19C C14C 120.6(16) . . ?
C18C C19C H19C 119.7 . . ?
C14C C19C H19C 119.7 . . ?
C22C C20C C21C 110.5(14) . . ?
C22C C20C C4C 113.8(13) . . ?
C21C C20C C4C 111.2(14) . . ?
C22C C20C H20C 107.0 . . ?
C21C C20C H20C 107.0 . . ?
C4C C20C H20C 107.0 . . ?
C20C C21C H21J 109.5 . . ?
C20C C21C H21K 109.5 . . ?
H21J C21C H21K 109.5 . . ?
C20C C21C H21L 109.5 . . ?
H21J C21C H21L 109.5 . . ?
H21K C21C H21L 109.5 . . ?
C20C C22C H22J 109.5 . . ?
C20C C22C H22K 109.5 . . ?
H22J C22C H22K 109.5 . . ?
C20C C22C H22L 109.5 . . ?
H22J C22C H22L 109.5 . . ?
H22K C22C H22L 109.5 . . ?
O3C C23C O2C 126.7(13) . . ?
O3C C23C C24C 122.8(14) . . ?
O2C C23C C24C 110.3(13) . . ?
C23C C24C H24J 109.5 . . ?
C23C C24C H24K 109.5 . . ?
H24J C24C H24K 109.5 . . ?
C23C C24C H24L 109.5 . . ?
H24J C24C H24L 109.5 . . ?
H24K C24C H24L 109.5 . . ?
Cl2 C25 Cl1 110.8(7) . . ?
Cl2 C25 Cl3 109.9(6) . . ?
Cl1 C25 Cl3 110.2(7) . . ?
Cl2 C25 H25 108.6 . . ?
Cl1 C25 H25 108.6 . . ?
Cl3 C25 H25 108.6 . . ?
Cl4 C26 Cl6 110.8(7) . . ?
Cl4 C26 Cl5 108.8(7) . . ?
Cl6 C26 Cl5 109.5(7) . . ?
Cl4 C26 H26 109.2 . . ?
Cl6 C26 H26 109.2 . . ?
Cl5 C26 H26 109.2 . . ?
Cl9 C30 Cl7 118.5(15) . . ?
Cl9 C30 Cl8 107.2(18) . . ?
Cl7 C30 Cl8 111.6(13) . . ?
Cl9 C30 H30 106.3 . . ?
Cl7 C30 H30 106.3 . . ?
Cl8 C30 H30 106.3 . . ?
Cl10 C31 Cl12 113.2(7) . . ?
Cl10 C31 Cl11 110.0(8) . . ?
Cl12 C31 Cl11 108.7(7) . . ?
Cl10 C31 H31 108.3 . . ?
Cl12 C31 H31 108.3 . . ?
Cl11 C31 H31 108.3 . . ?
Cl14 C32 Cl13 107.8(10) . . ?
Cl14 C32 Cl15 102.2(11) . . ?
Cl13 C32 Cl15 100.7(8) . . ?
Cl14 C32 H32 114.8 . . ?
Cl13 C32 H32 114.8 . . ?
Cl15 C32 H32 114.8 . . ?
Cl18 C33 Cl16 113.3(8) . . ?
Cl18 C33 Cl17 110.5(7) . . ?
Cl16 C33 Cl17 110.7(7) . . ?
Cl18 C33 H33 107.4 . . ?
Cl16 C33 H33 107.4 . . ?
Cl17 C33 H33 107.4 . . ?
Cl21 C34 Cl19 112.9(8) . . ?
Cl21 C34 Cl20 109.9(9) . . ?
Cl19 C34 Cl20 106.6(7) . . ?
Cl21 C34 H34 109.1 . . ?
Cl19 C34 H34 109.1 . . ?
Cl20 C34 H34 109.1 . . ?
H4A O4 H4B 92.6 . . ?

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
N2 Pd1 O1 C15 1.9(9) . . . . ?
O2 Pd1 O1 C15 179.7(9) . . . . ?
O1 Pd1 O2 C23 -117.5(9) . . . . ?
N1 Pd1 O2 C23 64.0(9) . . . . ?
N2 Pd1 N1 C7 -2.7(8) . . . . ?
O2 Pd1 N1 C7 179.5(8) . . . . ?
N2 Pd1 N1 C1 -179.3(9) . . . . ?
O2 Pd1 N1 C1 2.9(9) . . . . ?
O1 Pd1 N2 C9 -179.4(7) . . . . ?
N1 Pd1 N2 C9 -1.0(8) . . . . ?
O1 Pd1 N2 C13 5.6(9) . . . . ?
N1 Pd1 N2 C13 -176.0(9) . . . . ?
C7 N1 C1 C6 75.2(15) . . . . ?
Pd1 N1 C1 C6 -108.3(12) . . . . ?
C7 N1 C1 C2 -112.5(13) . . . . ?
Pd1 N1 C1 C2 64.0(14) . . . . ?
C6 C1 C2 C3 -3.9(19) . . . . ?
N1 C1 C2 C3 -176.4(11) . . . . ?
C1 C2 C3 C4 2(2) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C2 C3 C4 C20 177.2(12) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C20 C4 C5 C6 -176.8(11) . . . . ?
C2 C1 C6 C5 4.4(19) . . . . ?
N1 C1 C6 C5 176.6(10) . . . . ?
C4 C5 C6 C1 -2(2) . . . . ?
C1 N1 C7 C8 -1.7(17) . . . . ?
Pd1 N1 C7 C8 -178.6(9) . . . . ?
C1 N1 C7 C9 -177.6(10) . . . . ?
Pd1 N1 C7 C9 5.6(13) . . . . ?
C13 N2 C9 C10 2.9(17) . . . . ?
Pd1 N2 C9 C10 -172.4(9) . . . . ?
C13 N2 C9 C7 179.4(10) . . . . ?
Pd1 N2 C9 C7 4.1(12) . . . . ?
N1 C7 C9 C10 170.1(11) . . . . ?
C8 C7 C9 C10 -6.0(17) . . . . ?
N1 C7 C9 N2 -6.4(15) . . . . ?
C8 C7 C9 N2 177.5(10) . . . . ?
N2 C9 C10 C11 -0.3(18) . . . . ?
C7 C9 C10 C11 -176.5(11) . . . . ?
C9 C10 C11 C12 -1.9(19) . . . . ?
C10 C11 C12 C13 2(2) . . . . ?
C9 N2 C13 C12 -3.1(16) . . . . ?
Pd1 N2 C13 C12 171.5(8) . . . . ?
C9 N2 C13 C14 178.4(10) . . . . ?
Pd1 N2 C13 C14 -7.0(15) . . . . ?
C11 C12 C13 N2 1.0(18) . . . . ?
C11 C12 C13 C14 179.5(12) . . . . ?
N2 C13 C14 C15 0.2(18) . . . . ?
C12 C13 C14 C15 -178.1(12) . . . . ?
N2 C13 C14 C19 -173.4(11) . . . . ?
C12 C13 C14 C19 8.2(18) . . . . ?
Pd1 O1 C15 C14 -8.9(18) . . . . ?
Pd1 O1 C15 C16 176.7(8) . . . . ?
C19 C14 C15 O1 -177.9(12) . . . . ?
C13 C14 C15 O1 9(2) . . . . ?
C19 C14 C15 C16 -3.7(18) . . . . ?
C13 C14 C15 C16 -177.1(11) . . . . ?
O1 C15 C16 C17 179.1(12) . . . . ?
C14 C15 C16 C17 4(2) . . . . ?
C15 C16 C17 C18 -4(2) . . . . ?
C16 C17 C18 C19 5(2) . . . . ?
C17 C18 C19 C14 -5(2) . . . . ?
C15 C14 C19 C18 4.3(19) . . . . ?
C13 C14 C19 C18 178.3(11) . . . . ?
C3 C4 C20 C22 92(2) . . . . ?
C5 C4 C20 C22 -91(2) . . . . ?
C3 C4 C20 C21 -87(2) . . . . ?
C5 C4 C20 C21 90(2) . . . . ?
Pd1 O2 C23 O3 18.8(17) . . . . ?
Pd1 O2 C23 C24 -163.8(8) . . . . ?
N2A Pd1A O1A C15A -3.6(10) . . . . ?
O2A Pd1A O1A C15A 179.7(10) . . . . ?
O1A Pd1A O2A C23A -85.2(10) . . . . ?
N1A Pd1A O2A C23A 96.7(10) . . . . ?
N2A Pd1A N1A C7A -3.4(9) . . . . ?
O2A Pd1A N1A C7A 173.4(9) . . . . ?
N2A Pd1A N1A C1A -179.9(10) . . . . ?
O2A Pd1A N1A C1A -3.2(10) . . . . ?
O1A Pd1A N2A C9A -176.9(8) . . . . ?
N1A Pd1A N2A C9A 1.2(8) . . . . ?
O1A Pd1A N2A C13A 6.1(9) . . . . ?
N1A Pd1A N2A C13A -175.7(9) . . . . ?
C7A N1A C1A C6A -69.5(17) . . . . ?
Pd1A N1A C1A C6A 106.7(13) . . . . ?
C7A N1A C1A C2A 114.3(14) . . . . ?
Pd1A N1A C1A C2A -69.5(14) . . . . ?
C6A C1A C2A C3A -1(2) . . . . ?
N1A C1A C2A C3A 175.4(11) . . . . ?
C1A C2A C3A C4A -1(2) . . . . ?
C2A C3A C4A C5A 2(2) . . . . ?
C2A C3A C4A C20A -173.3(12) . . . . ?
C3A C4A C5A C6A 0(2) . . . . ?
C20A C4A C5A C6A 175.1(13) . . . . ?
C4A C5A C6A C1A -2(2) . . . . ?
C2A C1A C6A C5A 3(2) . . . . ?
N1A C1A C6A C5A -173.4(11) . . . . ?
C1A N1A C7A C9A -178.3(11) . . . . ?
Pd1A N1A C7A C9A 5.0(15) . . . . ?
C1A N1A C7A C8A -1.1(19) . . . . ?
Pd1A N1A C7A C8A -177.7(9) . . . . ?
C13A N2A C9A C10A -3.3(18) . . . . ?
Pd1A N2A C9A C10A 179.7(10) . . . . ?
C13A N2A C9A C7A 178.0(11) . . . . ?
Pd1A N2A C9A C7A 1.0(13) . . . . ?
N1A C7A C9A C10A 177.2(13) . . . . ?
C8A C7A C9A C10A 0(2) . . . . ?
N1A C7A C9A N2A -4.1(18) . . . . ?
C8A C7A C9A N2A 178.5(10) . . . . ?
N2A C9A C10A C11A 6.8(19) . . . . ?
C7A C9A C10A C11A -174.6(12) . . . . ?
C9A C10A C11A C12A -6.9(19) . . . . ?
C10A C11A C12A C13A 4(2) . . . . ?
C9A N2A C13A C12A -0.3(16) . . . . ?
Pd1A N2A C13A C12A 176.3(8) . . . . ?
C9A N2A C13A C14A 179.1(11) . . . . ?
Pd1A N2A C13A C14A -4.3(16) . . . . ?
C11A C12A C13A N2A 0.1(18) . . . . ?
C11A C12A C13A C14A -179.3(12) . . . . ?
N2A C13A C14A C15A -2(2) . . . . ?
C12A C13A C14A C15A 177.4(12) . . . . ?
N2A C13A C14A C19A -178.1(11) . . . . ?
C12A C13A C14A C19A 1.2(19) . . . . ?
Pd1A O1A C15A C14A -1(2) . . . . ?
Pd1A O1A C15A C16A -177.6(8) . . . . ?
C19A C14A C15A O1A -178.9(12) . . . . ?
C13A C14A C15A O1A 5(2) . . . . ?
C19A C14A C15A C16A -2.3(18) . . . . ?
C13A C14A C15A C16A -178.5(12) . . . . ?
O1A C15A C16A C17A 179.8(12) . . . . ?
C14A C15A C16A C17A 3(2) . . . . ?
C15A C16A C17A C18A -3(2) . . . . ?
C16A C17A C18A C19A 3(2) . . . . ?
C17A C18A C19A C14A -2(2) . . . . ?
C15A C14A C19A C18A 2(2) . . . . ?
C13A C14A C19A C18A 178.9(12) . . . . ?
C5A C4A C20A C22A 98(2) . . . . ?
C3A C4A C20A C22A -87(2) . . . . ?
C5A C4A C20A C21A -95.1(19) . . . . ?
C3A C4A C20A C21A 80(2) . . . . ?
Pd1A O2A C23A O3A 4(2) . . . . ?
Pd1A O2A C23A C24A -176.5(7) . . . . ?
N2B Pd1B N1B C7B -1.1(9) . . . . ?
O2B Pd1B N1B C7B 176.7(9) . . . . ?
N2B Pd1B N1B C1B -176.0(10) . . . . ?
O2B Pd1B N1B C1B 1.8(10) . . . . ?
O1B Pd1B N2B C9B -178.2(8) . . . . ?
N1B Pd1B N2B C9B 3.9(8) . . . . ?
O1B Pd1B N2B C13B -4.7(10) . . . . ?
N1B Pd1B N2B C13B 177.3(10) . . . . ?
N2B Pd1B O1B C15B -0.8(10) . . . . ?
O2B Pd1B O1B C15B -178.7(9) . . . . ?
O1B Pd1B O2B C23B 112.0(9) . . . . ?
N1B Pd1B O2B C23B -70.0(9) . . . . ?
C7B N1B C1B C6B -70.7(18) . . . . ?
Pd1B N1B C1B C6B 103.9(13) . . . . ?
C7B N1B C1B C2B 109.5(15) . . . . ?
Pd1B N1B C1B C2B -76.0(15) . . . . ?
C6B C1B C2B C3B -4(2) . . . . ?
N1B C1B C2B C3B 176.0(12) . . . . ?
C1B C2B C3B C4B 2(2) . . . . ?
C2B C3B C4B C5B -1(2) . . . . ?
C2B C3B C4B C20B -178.9(13) . . . . ?
C3B C4B C5B C6B 0(2) . . . . ?
C20B C4B C5B C6B 178.3(12) . . . . ?
C2B C1B C6B C5B 3(2) . . . . ?
N1B C1B C6B C5B -176.4(11) . . . . ?
C4B C5B C6B C1B -1(2) . . . . ?
C1B N1B C7B C9B 173.3(10) . . . . ?
Pd1B N1B C7B C9B -1.7(14) . . . . ?
C1B N1B C7B C8B -4.7(19) . . . . ?
Pd1B N1B C7B C8B -179.7(9) . . . . ?
C13B N2B C9B C10B -0.6(19) . . . . ?
Pd1B N2B C9B C10B 173.0(10) . . . . ?
C13B N2B C9B C7B -179.6(11) . . . . ?
Pd1B N2B C9B C7B -5.9(14) . . . . ?
N1B C7B C9B N2B 5.2(17) . . . . ?
C8B C7B C9B N2B -176.7(11) . . . . ?
N1B C7B C9B C10B -173.7(12) . . . . ?
C8B C7B C9B C10B 4.4(19) . . . . ?
N2B C9B C10B C11B -1.5(19) . . . . ?
C7B C9B C10B C11B 177.4(12) . . . . ?
C9B C10B C11B C12B 2(2) . . . . ?
C10B C11B C12B C13B 0(2) . . . . ?
C9B N2B C13B C12B 2.1(18) . . . . ?
Pd1B N2B C13B C12B -170.6(9) . . . . ?
C9B N2B C13B C14B -179.4(12) . . . . ?
Pd1B N2B C13B C14B 7.8(18) . . . . ?
C11B C12B C13B N2B -2(2) . . . . ?
C11B C12B C13B C14B 179.8(13) . . . . ?
N2B C13B C14B C19B 172.8(12) . . . . ?
C12B C13B C14B C19B -9(2) . . . . ?
N2B C13B C14B C15B -5(2) . . . . ?
C12B C13B C14B C15B 173.1(13) . . . . ?
Pd1B O1B C15B C16B -178.7(8) . . . . ?
Pd1B O1B C15B C14B 3.3(18) . . . . ?
C19B C14B C15B O1B -178.9(12) . . . . ?
C13B C14B C15B O1B -1(2) . . . . ?
C19B C14B C15B C16B 3.3(19) . . . . ?
C13B C14B C15B C16B -178.7(13) . . . . ?
O1B C15B C16B C17B 179.0(12) . . . . ?
C14B C15B C16B C17B -3(2) . . . . ?
C15B C16B C17B C18B 3(2) . . . . ?
C16B C17B C18B C19B -3(3) . . . . ?
C17B C18B C19B C14B 3(2) . . . . ?
C15B C14B C19B C18B -3(2) . . . . ?
C13B C14B C19B C18B 178.3(14) . . . . ?
C3B C4B C20B C22B -119.4(18) . . . . ?
C5B C4B C20B C22B 62(2) . . . . ?
C3B C4B C20B C21B 119.5(16) . . . . ?
C5B C4B C20B C21B -58.8(19) . . . . ?
Pd1B O2B C23B O3B -15.8(18) . . . . ?
Pd1B O2B C23B C24B 166.1(8) . . . . ?
N2C Pd1C O1C C15C -3.4(10) . . . . ?
O2C Pd1C O1C C15C 178.2(10) . . . . ?
O1C Pd1C O2C C23C 99.1(10) . . . . ?
N1C Pd1C O2C C23C -81.3(10) . . . . ?
N2C Pd1C N1C C7C -1.9(9) . . . . ?
O2C Pd1C N1C C7C 176.4(9) . . . . ?
N2C Pd1C N1C C1C 179.2(10) . . . . ?
O2C Pd1C N1C C1C -2.4(10) . . . . ?
O1C Pd1C N2C C9C -175.5(9) . . . . ?
N1C Pd1C N2C C9C 4.9(9) . . . . ?
O1C Pd1C N2C C13C -5.4(11) . . . . ?
N1C Pd1C N2C C13C 175.0(11) . . . . ?
C7C N1C C1C C6C -69.9(18) . . . . ?
Pd1C N1C C1C C6C 108.9(13) . . . . ?
C7C N1C C1C C2C 118.4(14) . . . . ?
Pd1C N1C C1C C2C -62.8(16) . . . . ?
C6C C1C C2C C3C 3(2) . . . . ?
N1C C1C C2C C3C 175.6(12) . . . . ?
C1C C2C C3C C4C -4(2) . . . . ?
C2C C3C C4C C5C 3(2) . . . . ?
C2C C3C C4C C20C -179.4(13) . . . . ?
C3C C4C C5C C6C -2(2) . . . . ?
C20C C4C C5C C6C -179.9(14) . . . . ?
C4C C5C C6C C1C 2(2) . . . . ?
C2C C1C C6C C5C -3(2) . . . . ?
N1C C1C C6C C5C -174.7(13) . . . . ?
C1C N1C C7C C9C 177.5(11) . . . . ?
Pd1C N1C C7C C9C -1.4(15) . . . . ?
C1C N1C C7C C8C -0.8(19) . . . . ?
Pd1C N1C C7C C8C -179.7(9) . . . . ?
C13C N2C C9C C10C 3(2) . . . . ?
Pd1C N2C C9C C10C 173.0(10) . . . . ?
C13C N2C C9C C7C -177.0(12) . . . . ?
Pd1C N2C C9C C7C -7.0(14) . . . . ?
N1C C7C C9C N2C 5.7(18) . . . . ?
C8C C7C C9C N2C -175.8(11) . . . . ?
N1C C7C C9C C10C -174.2(13) . . . . ?
C8C C7C C9C C10C 4(2) . . . . ?
N2C C9C C10C C11C -4(2) . . . . ?
C7C C9C C10C C11C 176.0(13) . . . . ?
C9C C10C C11C C12C 3(2) . . . . ?
C10C C11C C12C C13C -2(2) . . . . ?
C9C N2C C13C C12C -1.2(19) . . . . ?
Pd1C N2C C13C C12C -170.0(9) . . . . ?
C9C N2C C13C C14C -179.7(13) . . . . ?
Pd1C N2C C13C C14C 11.5(18) . . . . ?
C11C C12C C13C N2C 1(2) . . . . ?
C11C C12C C13C C14C 179.1(15) . . . . ?
N2C C13C C14C C19C 172.7(13) . . . . ?
C12C C13C C14C C19C -6(2) . . . . ?
N2C C13C C14C C15C -10(2) . . . . ?
C12C C13C C14C C15C 172.1(14) . . . . ?
Pd1C O1C C15C C16C -175.2(9) . . . . ?
Pd1C O1C C15C C14C 6.3(19) . . . . ?
C19C C14C C15C O1C 177.4(13) . . . . ?
C13C C14C C15C O1C 0(2) . . . . ?
C19C C14C C15C C16C -1(2) . . . . ?
C13C C14C C15C C16C -178.6(14) . . . . ?
O1C C15C C16C C17C 179.4(13) . . . . ?
C14C C15C C16C C17C -2(2) . . . . ?
C15C C16C C17C C18C 4(2) . . . . ?
C16C C17C C18C C19C -3(2) . . . . ?
C17C C18C C19C C14C 0(2) . . . . ?
C15C C14C C19C C18C 2(2) . . . . ?
C13C C14C C19C C18C -180.0(14) . . . . ?
C5C C4C C20C C22C 61(2) . . . . ?
C3C C4C C20C C22C -115.9(16) . . . . ?
C5C C4C C20C C21C -64.0(19) . . . . ?
C3C C4C C20C C21C 118.7(16) . . . . ?
Pd1C O2C C23C O3C -1(2) . . . . ?
Pd1C O2C C23C C24C 173.4(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4A O3A 0.91 2.09 2.907(12) 148.8 .
O4 H4B Cl10 0.84 3.03 3.528(9) 119.5 1_556
O4 H4B O3C 0.84 1.99 2.807(12) 162.1 3_667

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.140
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.122

####################################################################### 
# 
# 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_11004
_database_code_depnum_ccdc_archive 'CCDC 1040522'
_audit_update_record             
;
2015-02-09 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: ...Due to SQUEEZE option in PLATON.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H30 N2 O3 Pd,0.75 C6 H14'
_chemical_formula_sum            'C31.50 H40.50 N2 O3 Pd'
_chemical_formula_weight         601.56

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   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                   26.910(8)
_cell_length_b                   14.159(4)
_cell_length_c                   15.463(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.788(6)
_cell_angle_gamma                90.00
_cell_volume                     5508(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    847
_cell_measurement_theta_min      2.349
_cell_measurement_theta_max      28.322

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2508
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   
;
absorption correction based on 7716 reflections(SADABS);Rint 0.0758 before
correction and 0.0515 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21197
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5402
_reflns_number_gt                3979
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 

Disordered C6H14 was omitted using the SQUEEZE option of PLATON.The solvent
accessible voids are 954.4 Å3 with an estimated 316e/cell to be added.Six
solvent C6H14 molecules/unit cell accounting for 300e were included in the
formula, FWt, (000) and density calculations. PLATON Reference:
Spek, A.L. (1990), Acta Cryst. A46, C-34. 

 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)+(0.0476P)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         5402
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1084
_refine_ls_wR_factor_gt          0.1019
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.959
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.146 470 158 ' '
2 0.000 0.500 0.746 470 158 ' '
_platon_squeeze_details          
;
Disordered C6H14 was omitted using the SQUEEZE option of PLATON.The solvent
accessible voids are 954.4 Å3 with an estimated 316e/cell to be added.Six
solvent C6H14 molecules/unit cell accounting for 300e were included in the
formula, FWt, (000) and density calculations. PLATON Reference:
Spek, A.L. (1990), Acta Cryst. A46, C-34.  
;

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 0.146478(12) 0.05874(2) 0.14034(2) 0.02649(11) Uani 1 1 d . . .
O2 O 0.18548(11) 0.1569(2) 0.09212(19) 0.0356(7) Uani 1 1 d . . .
O3 O 0.11927(16) 0.2577(3) 0.0513(3) 0.0836(14) Uani 1 1 d . . .
O1 O 0.11130(11) 0.0117(2) 0.01458(19) 0.0347(7) Uani 1 1 d . . .
N1 N 0.18444(13) 0.0942(2) 0.2731(2) 0.0271(8) Uani 1 1 d . . .
N2 N 0.11804(12) -0.0415(2) 0.1980(2) 0.0261(7) Uani 1 1 d . . .
C1 C 0.21499(16) 0.1798(3) 0.3002(3) 0.0291(9) Uani 1 1 d . . .
C2 C 0.18986(16) 0.2580(3) 0.3203(3) 0.0315(10) Uani 1 1 d . . .
C3 C 0.21952(18) 0.3416(3) 0.3431(3) 0.0380(11) Uani 1 1 d . . .
H3 H 0.2038 0.3967 0.3574 0.046 Uiso 1 1 calc R . .
C4 C 0.27076(18) 0.3452(3) 0.3452(3) 0.0393(11) Uani 1 1 d . . .
H4 H 0.2902 0.4025 0.3615 0.047 Uiso 1 1 calc R . .
C5 C 0.29431(18) 0.2668(3) 0.3240(3) 0.0418(11) Uani 1 1 d . . .
H5 H 0.3297 0.2709 0.3249 0.050 Uiso 1 1 calc R . .
C6 C 0.26695(17) 0.1811(3) 0.3013(3) 0.0323(10) Uani 1 1 d . . .
C7 C 0.17970(16) 0.0326(3) 0.3315(3) 0.0301(10) Uani 1 1 d . . .
C8 C 0.20783(18) 0.0396(3) 0.4347(3) 0.0372(11) Uani 1 1 d . . .
H8A H 0.2319 0.0941 0.4490 0.056 Uiso 1 1 calc R . .
H8B H 0.2284 -0.0182 0.4576 0.056 Uiso 1 1 calc R . .
H8C H 0.1816 0.0474 0.4647 0.056 Uiso 1 1 calc R . .
C9 C 0.14298(15) -0.0453(3) 0.2924(3) 0.0260(9) Uani 1 1 d . . .
C10 C 0.13160(17) -0.1134(3) 0.3447(3) 0.0346(10) Uani 1 1 d . . .
H10 H 0.1489 -0.1142 0.4100 0.042 Uiso 1 1 calc R . .
C11 C 0.09396(18) -0.1820(3) 0.3006(3) 0.0404(11) Uani 1 1 d . . .
H11 H 0.0855 -0.2309 0.3351 0.048 Uiso 1 1 calc R . .
C12 C 0.06949(17) -0.1777(3) 0.2069(3) 0.0390(11) Uani 1 1 d . . .
H12 H 0.0440 -0.2246 0.1766 0.047 Uiso 1 1 calc R . .
C13 C 0.08081(15) -0.1056(3) 0.1533(3) 0.0295(9) Uani 1 1 d . . .
C14 C 0.05348(16) -0.1006(3) 0.0529(3) 0.0313(10) Uani 1 1 d . . .
C15 C 0.06968(16) -0.0447(3) -0.0088(3) 0.0314(10) Uani 1 1 d . . .
C16 C 0.03939(17) -0.0499(3) -0.1045(3) 0.0381(11) Uani 1 1 d . . .
H16 H 0.0501 -0.0134 -0.1464 0.046 Uiso 1 1 calc R . .
C17 C -0.00430(18) -0.1051(4) -0.1387(3) 0.0440(12) Uani 1 1 d . . .
H17 H -0.0232 -0.1073 -0.2035 0.053 Uiso 1 1 calc R . .
C18 C -0.02133(18) -0.1575(3) -0.0805(3) 0.0446(12) Uani 1 1 d . . .
H18 H -0.0523 -0.1954 -0.1045 0.054 Uiso 1 1 calc R . .
C19 C 0.00661(17) -0.1551(3) 0.0130(3) 0.0412(11) Uani 1 1 d . . .
H19 H -0.0059 -0.1915 0.0527 0.049 Uiso 1 1 calc R . .
C20 C 0.29379(18) 0.0948(3) 0.2791(3) 0.0418(11) Uani 1 1 d . . .
H20 H 0.2662 0.0444 0.2559 0.050 Uiso 1 1 calc R . .
C21 C 0.3164(2) 0.1138(4) 0.2044(4) 0.0579(14) Uani 1 1 d . . .
H21A H 0.2878 0.1336 0.1477 0.087 Uiso 1 1 calc R . .
H21B H 0.3330 0.0562 0.1922 0.087 Uiso 1 1 calc R . .
H21C H 0.3431 0.1640 0.2247 0.087 Uiso 1 1 calc R . .
C22 C 0.3369(3) 0.0573(4) 0.3666(4) 0.0753(18) Uani 1 1 d . . .
H22A H 0.3526 -0.0001 0.3516 0.113 Uiso 1 1 calc R . .
H22B H 0.3211 0.0426 0.4132 0.113 Uiso 1 1 calc R . .
H22C H 0.3646 0.1053 0.3910 0.113 Uiso 1 1 calc R . .
C23 C 0.13279(18) 0.2572(3) 0.3185(3) 0.0432(12) Uani 1 1 d . . .
H23 H 0.1165 0.1958 0.2907 0.052 Uiso 1 1 calc R . .
C24 C 0.09976(19) 0.3351(4) 0.2589(4) 0.0572(14) Uani 1 1 d . . .
H24A H 0.1140 0.3965 0.2857 0.086 Uiso 1 1 calc R . .
H24B H 0.0629 0.3292 0.2559 0.086 Uiso 1 1 calc R . .
H24C H 0.1009 0.3304 0.1965 0.086 Uiso 1 1 calc R . .
C25 C 0.1311(2) 0.2619(4) 0.4162(4) 0.0679(16) Uani 1 1 d . . .
H25A H 0.1441 0.3236 0.4435 0.102 Uiso 1 1 calc R . .
H25B H 0.1536 0.2120 0.4543 0.102 Uiso 1 1 calc R . .
H25C H 0.0944 0.2530 0.4134 0.102 Uiso 1 1 calc R . .
C26 C 0.1656(2) 0.2369(3) 0.0665(3) 0.0403(11) Uani 1 1 d . . .
C27 C 0.2025(2) 0.3114(4) 0.0544(4) 0.0625(15) Uani 1 1 d . . .
H27A H 0.1824 0.3557 0.0059 0.094 Uiso 1 1 calc R . .
H27B H 0.2303 0.2813 0.0367 0.094 Uiso 1 1 calc R . .
H27C H 0.2189 0.3456 0.1127 0.094 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O1 1.953(3) . ?
Pd1 N2 1.969(3) . ?
Pd1 N1 2.006(3) . ?
Pd1 O2 2.036(3) . ?
O2 C26 1.257(5) . ?
O3 C26 1.219(5) . ?
O1 C15 1.317(5) . ?
N1 C7 1.292(5) . ?
N1 C1 1.441(5) . ?
N2 C13 1.347(5) . ?
N2 C9 1.374(5) . ?
C1 C2 1.389(5) . ?
C1 C6 1.393(6) . ?
C2 C3 1.401(5) . ?
C2 C23 1.526(6) . ?
C3 C4 1.369(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(6) . ?
C5 H5 0.9500 . ?
C6 C20 1.518(6) . ?
C7 C9 1.462(5) . ?
C7 C8 1.509(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.361(5) . ?
C10 C11 1.394(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.364(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.414(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.464(6) . ?
C14 C19 1.420(6) . ?
C14 C15 1.422(6) . ?
C15 C16 1.416(5) . ?
C16 C17 1.353(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.366(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.373(6) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.509(6) . ?
C20 C22 1.532(7) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.508(6) . ?
C23 C25 1.530(7) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.506(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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
O1 Pd1 N2 94.35(12) . . ?
O1 Pd1 N1 174.49(12) . . ?
N2 Pd1 N1 81.68(13) . . ?
O1 Pd1 O2 89.93(11) . . ?
N2 Pd1 O2 172.47(12) . . ?
N1 Pd1 O2 93.61(12) . . ?
C26 O2 Pd1 120.9(3) . . ?
C15 O1 Pd1 123.0(3) . . ?
C7 N1 C1 123.5(3) . . ?
C7 N1 Pd1 113.9(3) . . ?
C1 N1 Pd1 122.6(2) . . ?
C13 N2 C9 120.8(3) . . ?
C13 N2 Pd1 126.2(3) . . ?
C9 N2 Pd1 112.8(2) . . ?
C2 C1 C6 123.6(4) . . ?
C2 C1 N1 117.6(4) . . ?
C6 C1 N1 118.8(4) . . ?
C1 C2 C3 116.8(4) . . ?
C1 C2 C23 123.9(4) . . ?
C3 C2 C23 119.3(4) . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.7(4) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 121.0(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 116.8(4) . . ?
C1 C6 C20 122.9(4) . . ?
C5 C6 C20 120.3(4) . . ?
N1 C7 C9 116.1(4) . . ?
N1 C7 C8 123.9(4) . . ?
C9 C7 C8 119.9(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 122.1(4) . . ?
C10 C9 C7 123.4(4) . . ?
N2 C9 C7 114.4(3) . . ?
C9 C10 C11 118.6(4) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 118.8(4) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
C11 C12 C13 122.1(4) . . ?
C11 C12 H12 118.9 . . ?
C13 C12 H12 118.9 . . ?
N2 C13 C12 117.5(4) . . ?
N2 C13 C14 120.9(4) . . ?
C12 C13 C14 121.6(4) . . ?
C19 C14 C15 116.6(4) . . ?
C19 C14 C13 118.0(4) . . ?
C15 C14 C13 125.4(4) . . ?
O1 C15 C16 115.9(4) . . ?
O1 C15 C14 125.9(4) . . ?
C16 C15 C14 118.2(4) . . ?
C17 C16 C15 122.4(4) . . ?
C17 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C16 C17 C18 120.3(4) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C14 122.8(4) . . ?
C18 C19 H19 118.6 . . ?
C14 C19 H19 118.6 . . ?
C21 C20 C6 112.5(4) . . ?
C21 C20 C22 110.7(4) . . ?
C6 C20 C22 110.6(4) . . ?
C21 C20 H20 107.6 . . ?
C6 C20 H20 107.6 . . ?
C22 C20 H20 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C2 112.2(4) . . ?
C24 C23 C25 110.7(4) . . ?
C2 C23 C25 111.4(4) . . ?
C24 C23 H23 107.4 . . ?
C2 C23 H23 107.4 . . ?
C25 C23 H23 107.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O3 C26 O2 124.7(5) . . ?
O3 C26 C27 118.9(5) . . ?
O2 C26 C27 116.4(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

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
O1 Pd1 O2 C26 89.5(3) . . . . ?
N2 Pd1 O2 C26 -145.7(9) . . . . ?
N1 Pd1 O2 C26 -94.7(3) . . . . ?
N2 Pd1 O1 C15 20.6(3) . . . . ?
N1 Pd1 O1 C15 64.3(14) . . . . ?
O2 Pd1 O1 C15 -165.6(3) . . . . ?
O1 Pd1 N1 C7 -35.1(14) . . . . ?
N2 Pd1 N1 C7 9.0(3) . . . . ?
O2 Pd1 N1 C7 -165.1(3) . . . . ?
O1 Pd1 N1 C1 143.7(12) . . . . ?
N2 Pd1 N1 C1 -172.2(3) . . . . ?
O2 Pd1 N1 C1 13.7(3) . . . . ?
O1 Pd1 N2 C13 -8.6(3) . . . . ?
N1 Pd1 N2 C13 175.2(3) . . . . ?
O2 Pd1 N2 C13 -133.1(8) . . . . ?
O1 Pd1 N2 C9 167.1(3) . . . . ?
N1 Pd1 N2 C9 -9.1(3) . . . . ?
O2 Pd1 N2 C9 42.5(10) . . . . ?
C7 N1 C1 C2 -86.2(5) . . . . ?
Pd1 N1 C1 C2 95.2(4) . . . . ?
C7 N1 C1 C6 96.5(5) . . . . ?
Pd1 N1 C1 C6 -82.2(4) . . . . ?
C6 C1 C2 C3 -0.4(6) . . . . ?
N1 C1 C2 C3 -177.7(4) . . . . ?
C6 C1 C2 C23 179.5(4) . . . . ?
N1 C1 C2 C23 2.2(6) . . . . ?
C1 C2 C3 C4 0.1(6) . . . . ?
C23 C2 C3 C4 -179.8(4) . . . . ?
C2 C3 C4 C5 0.6(7) . . . . ?
C3 C4 C5 C6 -1.1(7) . . . . ?
C2 C1 C6 C5 0.0(6) . . . . ?
N1 C1 C6 C5 177.2(4) . . . . ?
C2 C1 C6 C20 -179.9(4) . . . . ?
N1 C1 C6 C20 -2.7(6) . . . . ?
C4 C5 C6 C1 0.7(6) . . . . ?
C4 C5 C6 C20 -179.3(4) . . . . ?
C1 N1 C7 C9 174.1(3) . . . . ?
Pd1 N1 C7 C9 -7.1(5) . . . . ?
C1 N1 C7 C8 -3.5(6) . . . . ?
Pd1 N1 C7 C8 175.3(3) . . . . ?
C13 N2 C9 C10 0.2(6) . . . . ?
Pd1 N2 C9 C10 -175.7(3) . . . . ?
C13 N2 C9 C7 -176.1(3) . . . . ?
Pd1 N2 C9 C7 8.0(4) . . . . ?
N1 C7 C9 C10 -176.8(4) . . . . ?
C8 C7 C9 C10 0.9(6) . . . . ?
N1 C7 C9 N2 -0.6(5) . . . . ?
C8 C7 C9 N2 177.1(3) . . . . ?
N2 C9 C10 C11 1.0(6) . . . . ?
C7 C9 C10 C11 176.9(4) . . . . ?
C9 C10 C11 C12 -0.8(6) . . . . ?
C10 C11 C12 C13 -0.5(7) . . . . ?
C9 N2 C13 C12 -1.4(5) . . . . ?
Pd1 N2 C13 C12 173.9(3) . . . . ?
C9 N2 C13 C14 178.9(3) . . . . ?
Pd1 N2 C13 C14 -5.8(5) . . . . ?
C11 C12 C13 N2 1.6(6) . . . . ?
C11 C12 C13 C14 -178.7(4) . . . . ?
N2 C13 C14 C19 -165.3(4) . . . . ?
C12 C13 C14 C19 15.0(6) . . . . ?
N2 C13 C14 C15 14.1(6) . . . . ?
C12 C13 C14 C15 -165.6(4) . . . . ?
Pd1 O1 C15 C16 161.8(3) . . . . ?
Pd1 O1 C15 C14 -19.2(5) . . . . ?
C19 C14 C15 O1 178.8(4) . . . . ?
C13 C14 C15 O1 -0.6(6) . . . . ?
C19 C14 C15 C16 -2.2(6) . . . . ?
C13 C14 C15 C16 178.4(4) . . . . ?
O1 C15 C16 C17 179.8(4) . . . . ?
C14 C15 C16 C17 0.7(6) . . . . ?
C15 C16 C17 C18 0.9(7) . . . . ?
C16 C17 C18 C19 -1.0(7) . . . . ?
C17 C18 C19 C14 -0.6(7) . . . . ?
C15 C14 C19 C18 2.2(6) . . . . ?
C13 C14 C19 C18 -178.3(4) . . . . ?
C1 C6 C20 C21 126.5(4) . . . . ?
C5 C6 C20 C21 -53.4(6) . . . . ?
C1 C6 C20 C22 -109.1(5) . . . . ?
C5 C6 C20 C22 70.9(6) . . . . ?
C1 C2 C23 C24 -127.2(4) . . . . ?
C3 C2 C23 C24 52.7(6) . . . . ?
C1 C2 C23 C25 108.0(5) . . . . ?
C3 C2 C23 C25 -72.1(5) . . . . ?
Pd1 O2 C26 O3 -14.3(6) . . . . ?
Pd1 O2 C26 C27 165.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.110

####################################################################### 
# 
# 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_13083
_database_code_depnum_ccdc_archive 'CCDC 1040523'
_audit_update_record             
;
2015-02-09 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: ...Due to SQUEEZE option in PLATON.see_platon_squeeze_details
;

_vrf_PLAT051_I                   
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      38.97 %    
RESPONSE: ...Due to SQUEEZE option in PLATON. see_platon_squeeze_details
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H28 N2 O3 Pd, 1.5 C H Cl3'
_chemical_formula_sum            'C26.50 H29.50 Cl4.50 N2 O3 Pd'
_chemical_formula_weight         689.95

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   P2(1)/c

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

_cell_length_a                   16.155(4)
_cell_length_b                   13.910(3)
_cell_length_c                   13.360(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.643(5)
_cell_angle_gamma                90.00
_cell_volume                     2827.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    681
_cell_measurement_theta_min      2.929
_cell_measurement_theta_max      23.568

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1396
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 2191 reflections(SADABS);Rint 0.0830 before
correction and 0.0505 after.
;


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

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22017
_diffrn_reflns_av_R_equivalents  0.1884
_diffrn_reflns_av_sigmaI/netI    0.3022
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5551
_reflns_number_gt                1647
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 

The crystal data was weak due to crystal quality and the restraints
DELU and SIMU were used for the whole structure,also a a single DFIX 
restraint for C21-C23 bond distance was used in the refinement.

 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)+(0.0673P)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         5551
_refine_ls_number_parameters     285
_refine_ls_number_restraints     277
_refine_ls_R_factor_all          0.1940
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.1815
_refine_ls_wR_factor_gt          0.1575
_refine_ls_goodness_of_fit_ref   0.725
_refine_ls_restrained_S_all      0.714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 1.000 0.296 0.170 864 385 ' '
_platon_squeeze_details          
;
Disordered CHCl3 was omitted using the SQUEEZE option of PLATON.The solvent
accessible voids are 864.5 Å3 with an estimated 385e/cell to be added.Six solvent 
CHCl3 molecules/unit cell accounting for 348e were included in the formula, FWt, 
(000) and density calculations. PLATON Reference: Spek, A.L. (1990),
Acta Cryst. A46, C-34.   
;


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 0.37235(5) 0.29743(5) 0.77660(6) 0.0591(3) Uani 1 1 d U . .
O1 O 0.4785(4) 0.3146(4) 0.8996(5) 0.0658(17) Uani 1 1 d U . .
O2 O 0.3287(4) 0.4218(4) 0.8168(5) 0.0636(17) Uani 1 1 d U . .
O3 O 0.2423(4) 0.4652(5) 0.6570(6) 0.089(2) Uani 1 1 d U . .
N1 N 0.2626(4) 0.2696(5) 0.6463(5) 0.0582(18) Uani 1 1 d U . .
H1 H 0.2376 0.3280 0.6177 0.070 Uiso 1 1 calc R . .
N2 N 0.4138(5) 0.1774(5) 0.7288(6) 0.0602(19) Uani 1 1 d U . .
C1 C 0.1999(6) 0.2182(8) 0.6867(7) 0.069(3) Uani 1 1 d U . .
C2 C 0.1221(6) 0.2723(8) 0.6792(8) 0.084(3) Uani 1 1 d U . .
H2 H 0.1124 0.3350 0.6493 0.101 Uiso 1 1 calc R . .
C3 C 0.0625(7) 0.2282(8) 0.7176(9) 0.092(3) Uani 1 1 d U . .
H3 H 0.0107 0.2622 0.7145 0.111 Uiso 1 1 calc R . .
C4 C 0.0747(7) 0.1358(9) 0.7608(9) 0.091(3) Uani 1 1 d U . .
C5 C 0.1489(7) 0.0844(8) 0.7624(9) 0.097(4) Uani 1 1 d U . .
H5 H 0.1574 0.0203 0.7885 0.117 Uiso 1 1 calc R . .
C6 C 0.2093(7) 0.1267(7) 0.7261(9) 0.084(3) Uani 1 1 d U . .
H6 H 0.2600 0.0912 0.7282 0.101 Uiso 1 1 calc R . .
C7 C 0.2956(6) 0.2222(7) 0.5691(8) 0.068(2) Uani 1 1 d U . .
C8 C 0.2192(6) 0.1729(7) 0.4858(7) 0.085(3) Uani 1 1 d U . .
H8A H 0.1939 0.1242 0.5200 0.128 Uiso 1 1 calc R . .
H8B H 0.2402 0.1421 0.4328 0.128 Uiso 1 1 calc R . .
H8C H 0.1742 0.2207 0.4507 0.128 Uiso 1 1 calc R . .
C9 C 0.3330(6) 0.3049(6) 0.5183(6) 0.072(3) Uani 1 1 d U . .
H9A H 0.2862 0.3511 0.4843 0.109 Uiso 1 1 calc R . .
H9B H 0.3559 0.2782 0.4650 0.109 Uiso 1 1 calc R . .
H9C H 0.3805 0.3375 0.5737 0.109 Uiso 1 1 calc R . .
C10 C 0.3692(6) 0.1566(6) 0.6271(8) 0.060(2) Uani 1 1 d U . .
C11 C 0.3956(6) 0.0795(7) 0.5836(9) 0.076(3) Uani 1 1 d U . .
H11 H 0.3640 0.0616 0.5123 0.091 Uiso 1 1 calc R . .
C12 C 0.4682(7) 0.0267(8) 0.6424(9) 0.080(3) Uani 1 1 d U . .
H12 H 0.4880 -0.0251 0.6099 0.095 Uiso 1 1 calc R . .
C13 C 0.5100(7) 0.0471(7) 0.7421(9) 0.071(3) Uani 1 1 d U . .
H13 H 0.5594 0.0097 0.7814 0.085 Uiso 1 1 calc R . .
C14 C 0.4822(6) 0.1250(7) 0.7928(8) 0.064(2) Uani 1 1 d U . .
C15 C 0.5242(6) 0.1523(7) 0.9046(8) 0.064(2) Uani 1 1 d U . .
C16 C 0.5203(6) 0.2390(7) 0.9521(9) 0.067(3) Uani 1 1 d U . .
C17 C 0.5624(7) 0.2490(8) 1.0581(9) 0.091(3) Uani 1 1 d U . .
H17 H 0.5612 0.3098 1.0901 0.109 Uiso 1 1 calc R . .
C18 C 0.6072(7) 0.1733(8) 1.1218(10) 0.107(4) Uani 1 1 d U . .
H18 H 0.6348 0.1849 1.1956 0.129 Uiso 1 1 calc R . .
C19 C 0.6136(7) 0.0846(8) 1.0845(9) 0.101(4) Uani 1 1 d U . .
H19 H 0.6435 0.0328 1.1283 0.121 Uiso 1 1 calc R . .
C20 C 0.5701(6) 0.0765(7) 0.9706(9) 0.086(3) Uani 1 1 d U . .
H20 H 0.5726 0.0163 0.9382 0.103 Uiso 1 1 calc R . .
C21 C 0.0069(8) 0.0894(10) 0.8031(10) 0.121(4) Uani 1 1 d DU . .
H21 H -0.0484 0.1270 0.7705 0.145 Uiso 1 1 calc R . .
C22 C -0.0141(9) -0.0065(9) 0.7645(13) 0.177(6) Uani 1 1 d U . .
H22A H -0.0129 -0.0107 0.6917 0.265 Uiso 1 1 calc R . .
H22B H -0.0729 -0.0233 0.7649 0.265 Uiso 1 1 calc R . .
H22C H 0.0292 -0.0511 0.8103 0.265 Uiso 1 1 calc R . .
C23 C 0.0332(9) 0.1078(13) 0.9204(10) 0.203(7) Uani 1 1 d DU . .
H23A H 0.0122 0.0550 0.9542 0.304 Uiso 1 1 calc R . .
H23B H 0.0072 0.1684 0.9326 0.304 Uiso 1 1 calc R . .
H23C H 0.0974 0.1119 0.9509 0.304 Uiso 1 1 calc R . .
C24 C 0.2767(7) 0.4798(7) 0.7545(10) 0.067(3) Uani 1 1 d U . .
C25 C 0.2577(6) 0.5726(7) 0.8031(8) 0.090(3) Uani 1 1 d U . .
H25A H 0.3077 0.6164 0.8165 0.135 Uiso 1 1 calc R . .
H25B H 0.2483 0.5581 0.8703 0.135 Uiso 1 1 calc R . .
H25C H 0.2049 0.6028 0.7540 0.135 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 1.951(6) . ?
Pd1 N2 1.983(7) . ?
Pd1 O2 2.008(6) . ?
Pd1 N1 2.061(6) . ?
O1 C16 1.317(10) . ?
O2 C24 1.257(10) . ?
O3 C24 1.249(10) . ?
N1 C7 1.467(10) . ?
N1 C1 1.482(10) . ?
N1 H1 0.9300 . ?
N2 C10 1.337(10) . ?
N2 C14 1.360(10) . ?
C1 C6 1.366(12) . ?
C1 C2 1.440(12) . ?
C2 C3 1.378(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(13) . ?
C4 C21 1.534(14) . ?
C5 C6 1.360(12) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C10 1.493(12) . ?
C7 C8 1.519(11) . ?
C7 C9 1.557(11) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.355(11) . ?
C11 C12 1.384(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.306(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.428(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.467(12) . ?
C15 C16 1.374(12) . ?
C15 C20 1.415(12) . ?
C16 C17 1.356(12) . ?
C17 C18 1.394(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.347(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.450(13) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.428(15) . ?
C21 C23 1.501(8) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.522(12) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pd1 N2 94.5(3) . . ?
O1 Pd1 O2 87.6(2) . . ?
N2 Pd1 O2 176.8(3) . . ?
O1 Pd1 N1 176.1(3) . . ?
N2 Pd1 N1 81.8(3) . . ?
O2 Pd1 N1 96.2(3) . . ?
C16 O1 Pd1 120.0(6) . . ?
C24 O2 Pd1 126.3(7) . . ?
C7 N1 C1 119.6(7) . . ?
C7 N1 Pd1 105.4(5) . . ?
C1 N1 Pd1 106.4(5) . . ?
C7 N1 H1 108.3 . . ?
C1 N1 H1 108.3 . . ?
Pd1 N1 H1 108.3 . . ?
C10 N2 C14 124.7(8) . . ?
C10 N2 Pd1 112.6(6) . . ?
C14 N2 Pd1 122.6(7) . . ?
C6 C1 C2 119.7(10) . . ?
C6 C1 N1 126.1(9) . . ?
C2 C1 N1 114.2(9) . . ?
C3 C2 C1 116.4(10) . . ?
C3 C2 H2 121.8 . . ?
C1 C2 H2 121.8 . . ?
C2 C3 C4 123.1(11) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C5 C4 C3 118.8(11) . . ?
C5 C4 C21 119.8(12) . . ?
C3 C4 C21 121.5(12) . . ?
C6 C5 C4 119.3(11) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C1 122.8(11) . . ?
C5 C6 H6 118.6 . . ?
C1 C6 H6 118.6 . . ?
N1 C7 C10 108.9(8) . . ?
N1 C7 C8 108.7(7) . . ?
C10 C7 C8 114.4(8) . . ?
N1 C7 C9 105.1(7) . . ?
C10 C7 C9 108.7(7) . . ?
C8 C7 C9 110.7(8) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 117.9(9) . . ?
N2 C10 C7 117.2(8) . . ?
C11 C10 C7 124.8(10) . . ?
C10 C11 C12 120.3(11) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 120.9(11) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 120.8(11) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
N2 C14 C13 115.3(10) . . ?
N2 C14 C15 120.1(9) . . ?
C13 C14 C15 124.6(10) . . ?
C16 C15 C20 117.5(10) . . ?
C16 C15 C14 128.4(9) . . ?
C20 C15 C14 114.1(9) . . ?
O1 C16 C17 117.5(10) . . ?
O1 C16 C15 123.3(10) . . ?
C17 C16 C15 119.2(10) . . ?
C16 C17 C18 122.3(11) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C19 C18 C17 123.8(11) . . ?
C19 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
C18 C19 C20 112.8(11) . . ?
C18 C19 H19 123.6 . . ?
C20 C19 H19 123.6 . . ?
C15 C20 C19 124.4(10) . . ?
C15 C20 H20 117.8 . . ?
C19 C20 H20 117.8 . . ?
C22 C21 C23 119.1(15) . . ?
C22 C21 C4 111.9(12) . . ?
C23 C21 C4 109.0(10) . . ?
C22 C21 H21 105.2 . . ?
C23 C21 H21 105.2 . . ?
C4 C21 H21 105.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O3 C24 O2 123.4(10) . . ?
O3 C24 C25 120.0(10) . . ?
O2 C24 C25 116.5(10) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Pd1 O1 C16 -35.0(7) . . . . ?
O2 Pd1 O1 C16 147.4(7) . . . . ?
O1 Pd1 O2 C24 151.5(8) . . . . ?
N1 Pd1 O2 C24 -29.5(8) . . . . ?
N2 Pd1 N1 C7 -32.1(5) . . . . ?
O2 Pd1 N1 C7 145.4(5) . . . . ?
N2 Pd1 N1 C1 95.9(6) . . . . ?
O2 Pd1 N1 C1 -86.6(6) . . . . ?
O1 Pd1 N2 C10 -161.5(6) . . . . ?
N1 Pd1 N2 C10 19.7(6) . . . . ?
O1 Pd1 N2 C14 16.4(7) . . . . ?
N1 Pd1 N2 C14 -162.4(7) . . . . ?
C7 N1 C1 C6 49.3(13) . . . . ?
Pd1 N1 C1 C6 -69.7(10) . . . . ?
C7 N1 C1 C2 -128.9(9) . . . . ?
Pd1 N1 C1 C2 112.0(7) . . . . ?
C6 C1 C2 C3 2.8(15) . . . . ?
N1 C1 C2 C3 -178.9(8) . . . . ?
C1 C2 C3 C4 -0.7(16) . . . . ?
C2 C3 C4 C5 -2.1(18) . . . . ?
C2 C3 C4 C21 179.8(10) . . . . ?
C3 C4 C5 C6 2.8(17) . . . . ?
C21 C4 C5 C6 -179.1(10) . . . . ?
C4 C5 C6 C1 -0.7(17) . . . . ?
C2 C1 C6 C5 -2.2(16) . . . . ?
N1 C1 C6 C5 179.7(9) . . . . ?
C1 N1 C7 C10 -81.5(9) . . . . ?
Pd1 N1 C7 C10 38.1(8) . . . . ?
C1 N1 C7 C8 43.7(11) . . . . ?
Pd1 N1 C7 C8 163.3(6) . . . . ?
C1 N1 C7 C9 162.2(7) . . . . ?
Pd1 N1 C7 C9 -78.2(7) . . . . ?
C14 N2 C10 C11 -2.2(13) . . . . ?
Pd1 N2 C10 C11 175.7(6) . . . . ?
C14 N2 C10 C7 179.8(8) . . . . ?
Pd1 N2 C10 C7 -2.3(10) . . . . ?
N1 C7 C10 N2 -25.3(11) . . . . ?
C8 C7 C10 N2 -147.1(8) . . . . ?
C9 C7 C10 N2 88.6(9) . . . . ?
N1 C7 C10 C11 156.8(8) . . . . ?
C8 C7 C10 C11 35.0(13) . . . . ?
C9 C7 C10 C11 -89.3(11) . . . . ?
N2 C10 C11 C12 -2.1(14) . . . . ?
C7 C10 C11 C12 175.8(9) . . . . ?
C10 C11 C12 C13 3.4(15) . . . . ?
C11 C12 C13 C14 -0.5(16) . . . . ?
C10 N2 C14 C13 4.8(12) . . . . ?
Pd1 N2 C14 C13 -172.9(6) . . . . ?
C10 N2 C14 C15 -177.6(8) . . . . ?
Pd1 N2 C14 C15 4.8(11) . . . . ?
C12 C13 C14 N2 -3.3(13) . . . . ?
C12 C13 C14 C15 179.2(9) . . . . ?
N2 C14 C15 C16 -18.2(15) . . . . ?
C13 C14 C15 C16 159.2(9) . . . . ?
N2 C14 C15 C20 158.0(8) . . . . ?
C13 C14 C15 C20 -24.6(13) . . . . ?
Pd1 O1 C16 C17 -148.0(8) . . . . ?
Pd1 O1 C16 C15 33.0(12) . . . . ?
C20 C15 C16 O1 -178.9(9) . . . . ?
C14 C15 C16 O1 -2.8(16) . . . . ?
C20 C15 C16 C17 2.1(15) . . . . ?
C14 C15 C16 C17 178.2(10) . . . . ?
O1 C16 C17 C18 178.7(10) . . . . ?
C15 C16 C17 C18 -2.2(17) . . . . ?
C16 C17 C18 C19 1(2) . . . . ?
C17 C18 C19 C20 1.0(18) . . . . ?
C16 C15 C20 C19 -0.5(16) . . . . ?
C14 C15 C20 C19 -177.2(9) . . . . ?
C18 C19 C20 C15 -1.0(17) . . . . ?
C5 C4 C21 C22 -45.9(17) . . . . ?
C3 C4 C21 C22 132.3(14) . . . . ?
C5 C4 C21 C23 87.9(15) . . . . ?
C3 C4 C21 C23 -94.0(15) . . . . ?
Pd1 O2 C24 O3 2.6(14) . . . . ?
Pd1 O2 C24 C25 -176.3(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O3 0.93 1.97 2.750(9) 139.7 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.112

####################################################################### 
# 
# 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_12020
_database_code_depnum_ccdc_archive 'CCDC 1040524'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H34 N2 O3 Pd, C H2 Cl2'
_chemical_formula_sum            'C29 H36 Cl2 N2 O3 Pd'
_chemical_formula_weight         637.90

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   P2(1)/c

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

_cell_length_a                   16.640(6)
_cell_length_b                   10.960(4)
_cell_length_c                   17.137(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.252(5)
_cell_angle_gamma                90.00
_cell_volume                     2803.1(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    981
_cell_measurement_theta_min      2.305
_cell_measurement_theta_max      26.653

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 981 reflections(SADABS);Rint 0.1144 before
correction and 0.0344 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21332
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5505
_reflns_number_gt                4829
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0530P)²+0.7350P] 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         5505
_refine_ls_number_parameters     341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0966
_refine_ls_wR_factor_gt          0.0935
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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 0.342032(13) 0.894065(18) 0.267371(13) 0.01976(9) Uani 1 1 d . . .
O1 O 0.41962(13) 0.76614(18) 0.34245(13) 0.0288(5) Uani 1 1 d . . .
O2 O 0.35510(13) 0.97499(18) 0.37916(12) 0.0262(4) Uani 1 1 d . . .
O3 O 0.39988(15) 1.1436(2) 0.33701(14) 0.0357(5) Uani 1 1 d . . .
N1 N 0.25963(15) 1.0260(2) 0.18758(15) 0.0219(5) Uani 1 1 d . . .
H1 H 0.2863 1.0804 0.2099 0.026 Uiso 1 1 d R . .
N2 N 0.33747(14) 0.8258(2) 0.15899(14) 0.0203(5) Uani 1 1 d . . .
C1 C 0.17081(18) 1.0407(3) 0.18493(18) 0.0243(6) Uani 1 1 d . . .
C2 C 0.11083(19) 0.9422(3) 0.16309(19) 0.0273(6) Uani 1 1 d . . .
C3 C 0.0300(2) 0.9589(3) 0.1676(2) 0.0360(8) Uani 1 1 d . . .
H3 H -0.0104 0.8923 0.1541 0.043 Uiso 1 1 calc R . .
C4 C 0.0068(2) 1.0684(4) 0.1908(2) 0.0434(9) Uani 1 1 d . . .
H4 H -0.0487 1.0775 0.1935 0.052 Uiso 1 1 calc R . .
C5 C 0.0655(2) 1.1648(3) 0.2101(2) 0.0400(8) Uani 1 1 d . . .
H5 H 0.0492 1.2409 0.2256 0.048 Uiso 1 1 calc R . .
C6 C 0.1480(2) 1.1552(3) 0.2078(2) 0.0311(7) Uani 1 1 d . . .
C7 C 0.26910(19) 1.0274(3) 0.10306(18) 0.0240(6) Uani 1 1 d . . .
C8 C 0.3395(2) 1.1249(3) 0.1142(2) 0.0332(7) Uani 1 1 d . . .
H8A H 0.3162 1.2055 0.1185 0.050 Uiso 1 1 calc R . .
H8B H 0.3528 1.1231 0.0640 0.050 Uiso 1 1 calc R . .
H8C H 0.3943 1.1083 0.1674 0.050 Uiso 1 1 calc R . .
C9 C 0.1803(2) 1.0580(3) 0.0250(2) 0.0352(7) Uani 1 1 d . . .
H9A H 0.1365 0.9938 0.0174 0.053 Uiso 1 1 calc R . .
H9B H 0.1896 1.0635 -0.0275 0.053 Uiso 1 1 calc R . .
H9C H 0.1580 1.1362 0.0350 0.053 Uiso 1 1 calc R . .
C10 C 0.30590(19) 0.9048(2) 0.09093(19) 0.0233(6) Uani 1 1 d . . .
C11 C 0.3103(2) 0.8775(3) 0.0147(2) 0.0300(7) Uani 1 1 d . . .
H11 H 0.2860 0.9317 -0.0335 0.036 Uiso 1 1 calc R . .
C12 C 0.3508(2) 0.7693(3) 0.0092(2) 0.0320(7) Uani 1 1 d . . .
H12 H 0.3569 0.7504 -0.0420 0.038 Uiso 1 1 calc R . .
C13 C 0.3816(2) 0.6904(3) 0.0776(2) 0.0289(7) Uani 1 1 d . . .
H13 H 0.4097 0.6166 0.0738 0.035 Uiso 1 1 calc R . .
C14 C 0.37277(18) 0.7161(3) 0.15365(19) 0.0239(6) Uani 1 1 d . . .
C15 C 0.39941(19) 0.6271(3) 0.2245(2) 0.0254(6) Uani 1 1 d . . .
C16 C 0.41947(18) 0.6556(3) 0.31173(19) 0.0243(6) Uani 1 1 d . . .
C17 C 0.4444(2) 0.5595(3) 0.3734(2) 0.0291(7) Uani 1 1 d . . .
H17 H 0.4576 0.5778 0.4320 0.035 Uiso 1 1 calc R . .
C18 C 0.4499(2) 0.4412(3) 0.3508(2) 0.0338(7) Uani 1 1 d . . .
H18 H 0.4667 0.3786 0.3935 0.041 Uiso 1 1 calc R . .
C19 C 0.4309(2) 0.4128(3) 0.2658(2) 0.0361(8) Uani 1 1 d . . .
H19 H 0.4346 0.3308 0.2498 0.043 Uiso 1 1 calc R . .
C20 C 0.4070(2) 0.5026(3) 0.2056(2) 0.0332(7) Uani 1 1 d . . .
H20 H 0.3946 0.4814 0.1476 0.040 Uiso 1 1 calc R . .
C21 C 0.2043(2) 1.2703(3) 0.2274(2) 0.0390(8) Uani 1 1 d . . .
H21 H 0.2635 1.2475 0.2297 0.047 Uiso 1 1 calc R . .
C22 C 0.1602(3) 1.3623(4) 0.1537(3) 0.0610(12) Uani 1 1 d . . .
H22A H 0.1496 1.3240 0.0983 0.091 Uiso 1 1 calc R . .
H22B H 0.1998 1.4329 0.1641 0.091 Uiso 1 1 calc R . .
H22C H 0.1030 1.3890 0.1514 0.091 Uiso 1 1 calc R . .
C23 C 0.2222(3) 1.3280(4) 0.3140(3) 0.0567(11) Uani 1 1 d . . .
H23A H 0.1668 1.3647 0.3102 0.085 Uiso 1 1 calc R . .
H23B H 0.2682 1.3912 0.3284 0.085 Uiso 1 1 calc R . .
H23C H 0.2430 1.2653 0.3595 0.085 Uiso 1 1 calc R . .
C24 C 0.1283(2) 0.8164(3) 0.1371(2) 0.0346(7) Uani 1 1 d . . .
H24 H 0.1804 0.8229 0.1230 0.042 Uiso 1 1 calc R . .
C25 C 0.1536(3) 0.7260(4) 0.2122(3) 0.0552(11) Uani 1 1 d . . .
H25A H 0.2059 0.7566 0.2632 0.083 Uiso 1 1 calc R . .
H25B H 0.1679 0.6468 0.1950 0.083 Uiso 1 1 calc R . .
H25C H 0.1031 0.7165 0.2267 0.083 Uiso 1 1 calc R . .
C26 C 0.0483(2) 0.7679(4) 0.0561(3) 0.0553(11) Uani 1 1 d . . .
H26A H -0.0027 0.7554 0.0693 0.083 Uiso 1 1 calc R . .
H26B H 0.0645 0.6902 0.0386 0.083 Uiso 1 1 calc R . .
H26C H 0.0320 0.8271 0.0087 0.083 Uiso 1 1 calc R . .
C27 C 0.3890(2) 1.0836(3) 0.3917(2) 0.0264(6) Uani 1 1 d . . .
C28 C 0.4161(2) 1.1344(3) 0.4819(2) 0.0381(8) Uani 1 1 d . . .
H28A H 0.4763 1.1055 0.5210 0.057 Uiso 1 1 calc R . .
H28B H 0.3735 1.1069 0.5035 0.057 Uiso 1 1 calc R . .
H28C H 0.4160 1.2238 0.4797 0.057 Uiso 1 1 calc R . .
C29 C 0.1795(3) 0.9688(4) 0.3997(3) 0.0597(11) Uani 1 1 d . . .
H29A H 0.2420 0.9437 0.4160 0.072 Uiso 1 1 calc R . .
H29B H 0.1531 0.9963 0.3384 0.072 Uiso 1 1 calc R . .
Cl1 Cl 0.12018(11) 0.8421(2) 0.40657(12) 0.1219(7) Uani 1 1 d . . .
Cl2 Cl 0.18112(17) 1.0893(2) 0.46340(17) 0.1723(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O1 1.9541(19) . ?
Pd1 N2 1.972(2) . ?
Pd1 O2 2.034(2) . ?
Pd1 N1 2.045(2) . ?
O1 C16 1.321(3) . ?
O2 C27 1.294(3) . ?
O3 C27 1.223(4) . ?
N1 C1 1.467(3) . ?
N1 C7 1.525(4) . ?
N1 H1 0.7407 . ?
N2 C10 1.358(4) . ?
N2 C14 1.360(3) . ?
C1 C2 1.404(4) . ?
C1 C6 1.415(4) . ?
C2 C3 1.393(4) . ?
C2 C24 1.516(4) . ?
C3 C4 1.373(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(4) . ?
C5 H5 0.9500 . ?
C6 C21 1.517(5) . ?
C7 C9 1.529(4) . ?
C7 C10 1.529(4) . ?
C7 C8 1.533(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.374(4) . ?
C11 C12 1.388(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.362(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.403(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.465(4) . ?
C15 C16 1.415(4) . ?
C15 C20 1.420(4) . ?
C16 C17 1.417(4) . ?
C17 C18 1.368(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.352(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C23 1.517(5) . ?
C21 C22 1.526(5) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.528(5) . ?
C24 C26 1.531(5) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.511(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 Cl2 1.706(5) . ?
C29 Cl1 1.737(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 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
O1 Pd1 N2 94.99(9) . . ?
O1 Pd1 O2 85.90(8) . . ?
N2 Pd1 O2 174.90(8) . . ?
O1 Pd1 N1 179.16(9) . . ?
N2 Pd1 N1 84.46(9) . . ?
O2 Pd1 N1 94.71(9) . . ?
C16 O1 Pd1 120.77(17) . . ?
C27 O2 Pd1 114.56(19) . . ?
C1 N1 C7 119.7(2) . . ?
C1 N1 Pd1 117.82(17) . . ?
C7 N1 Pd1 108.77(16) . . ?
C1 N1 H1 107.0 . . ?
C7 N1 H1 101.2 . . ?
Pd1 N1 H1 98.8 . . ?
C10 N2 C14 121.4(2) . . ?
C10 N2 Pd1 113.97(18) . . ?
C14 N2 Pd1 124.14(19) . . ?
C2 C1 C6 120.7(3) . . ?
C2 C1 N1 120.7(3) . . ?
C6 C1 N1 118.6(3) . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 C24 116.8(3) . . ?
C1 C2 C24 124.9(3) . . ?
C4 C3 C2 122.2(3) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 118.7(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C6 122.5(3) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C1 117.5(3) . . ?
C5 C6 C21 116.7(3) . . ?
C1 C6 C21 125.8(3) . . ?
N1 C7 C9 111.6(2) . . ?
N1 C7 C10 109.7(2) . . ?
C9 C7 C10 111.3(2) . . ?
N1 C7 C8 106.4(2) . . ?
C9 C7 C8 110.2(3) . . ?
C10 C7 C8 107.5(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 121.0(3) . . ?
N2 C10 C7 118.0(2) . . ?
C11 C10 C7 120.9(3) . . ?
C10 C11 C12 118.8(3) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 121.2(3) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
N2 C14 C13 117.8(3) . . ?
N2 C14 C15 121.0(3) . . ?
C13 C14 C15 121.2(3) . . ?
C16 C15 C20 116.8(3) . . ?
C16 C15 C14 124.9(3) . . ?
C20 C15 C14 118.4(3) . . ?
O1 C16 C15 125.6(3) . . ?
O1 C16 C17 115.9(3) . . ?
C15 C16 C17 118.5(3) . . ?
C18 C17 C16 121.9(3) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C15 123.4(3) . . ?
C19 C20 H20 118.3 . . ?
C15 C20 H20 118.3 . . ?
C6 C21 C23 113.5(3) . . ?
C6 C21 C22 110.0(3) . . ?
C23 C21 C22 110.4(3) . . ?
C6 C21 H21 107.6 . . ?
C23 C21 H21 107.6 . . ?
C22 C21 H21 107.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C2 C24 C25 111.1(3) . . ?
C2 C24 C26 112.3(3) . . ?
C25 C24 C26 110.1(3) . . ?
C2 C24 H24 107.7 . . ?
C25 C24 H24 107.7 . . ?
C26 C24 H24 107.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O3 C27 O2 124.6(3) . . ?
O3 C27 C28 120.5(3) . . ?
O2 C27 C28 114.9(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Cl2 C29 Cl1 115.1(3) . . ?
Cl2 C29 H29A 108.5 . . ?
Cl1 C29 H29A 108.5 . . ?
Cl2 C29 H29B 108.5 . . ?
Cl1 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Pd1 O1 C16 -27.3(2) . . . . ?
O2 Pd1 O1 C16 157.7(2) . . . . ?
O1 Pd1 O2 C27 121.1(2) . . . . ?
N1 Pd1 O2 C27 -59.5(2) . . . . ?
N2 Pd1 N1 C1 119.9(2) . . . . ?
N2 Pd1 N1 C7 -20.52(17) . . . . ?
O2 Pd1 N1 C7 154.43(17) . . . . ?
O1 Pd1 N2 C10 -165.09(19) . . . . ?
N1 Pd1 N2 C10 15.55(19) . . . . ?
O1 Pd1 N2 C14 6.8(2) . . . . ?
N1 Pd1 N2 C14 -172.5(2) . . . . ?
C7 N1 C1 C2 79.3(3) . . . . ?
Pd1 N1 C1 C2 -56.7(3) . . . . ?
C7 N1 C1 C6 -102.9(3) . . . . ?
Pd1 N1 C1 C6 121.1(3) . . . . ?
C6 C1 C2 C3 -2.3(4) . . . . ?
N1 C1 C2 C3 175.5(3) . . . . ?
C6 C1 C2 C24 179.6(3) . . . . ?
N1 C1 C2 C24 -2.6(5) . . . . ?
C1 C2 C3 C4 1.3(5) . . . . ?
C24 C2 C3 C4 179.6(3) . . . . ?
C2 C3 C4 C5 0.1(5) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C4 C5 C6 C1 -0.4(5) . . . . ?
C4 C5 C6 C21 177.8(3) . . . . ?
C2 C1 C6 C5 1.8(5) . . . . ?
N1 C1 C6 C5 -176.0(3) . . . . ?
C2 C1 C6 C21 -176.2(3) . . . . ?
N1 C1 C6 C21 6.0(5) . . . . ?
C1 N1 C7 C9 5.8(4) . . . . ?
Pd1 N1 C7 C9 145.4(2) . . . . ?
C1 N1 C7 C10 -118.0(3) . . . . ?
Pd1 N1 C7 C10 21.5(3) . . . . ?
C1 N1 C7 C8 126.1(3) . . . . ?
Pd1 N1 C7 C8 -94.4(2) . . . . ?
C14 N2 C10 C11 -1.4(4) . . . . ?
Pd1 N2 C10 C11 170.8(2) . . . . ?
C14 N2 C10 C7 -178.7(2) . . . . ?
Pd1 N2 C10 C7 -6.6(3) . . . . ?
N1 C7 C10 N2 -10.7(3) . . . . ?
C9 C7 C10 N2 -134.7(3) . . . . ?
C8 C7 C10 N2 104.6(3) . . . . ?
N1 C7 C10 C11 172.0(3) . . . . ?
C9 C7 C10 C11 48.0(4) . . . . ?
C8 C7 C10 C11 -72.8(3) . . . . ?
N2 C10 C11 C12 -2.4(4) . . . . ?
C7 C10 C11 C12 174.9(3) . . . . ?
C10 C11 C12 C13 2.8(5) . . . . ?
C11 C12 C13 C14 0.4(5) . . . . ?
C10 N2 C14 C13 4.6(4) . . . . ?
Pd1 N2 C14 C13 -166.8(2) . . . . ?
C10 N2 C14 C15 -174.6(2) . . . . ?
Pd1 N2 C14 C15 14.1(4) . . . . ?
C12 C13 C14 N2 -4.1(4) . . . . ?
C12 C13 C14 C15 175.1(3) . . . . ?
N2 C14 C15 C16 -21.6(4) . . . . ?
C13 C14 C15 C16 159.3(3) . . . . ?
N2 C14 C15 C20 159.2(3) . . . . ?
C13 C14 C15 C20 -19.9(4) . . . . ?
Pd1 O1 C16 C15 28.7(4) . . . . ?
Pd1 O1 C16 C17 -153.3(2) . . . . ?
C20 C15 C16 O1 177.2(3) . . . . ?
C14 C15 C16 O1 -2.0(5) . . . . ?
C20 C15 C16 C17 -0.7(4) . . . . ?
C14 C15 C16 C17 -180.0(3) . . . . ?
O1 C16 C17 C18 -177.8(3) . . . . ?
C15 C16 C17 C18 0.3(4) . . . . ?
C16 C17 C18 C19 0.0(5) . . . . ?
C17 C18 C19 C20 0.0(5) . . . . ?
C18 C19 C20 C15 -0.4(5) . . . . ?
C16 C15 C20 C19 0.8(5) . . . . ?
C14 C15 C20 C19 -179.9(3) . . . . ?
C5 C6 C21 C23 55.1(4) . . . . ?
C1 C6 C21 C23 -126.9(3) . . . . ?
C5 C6 C21 C22 -69.2(4) . . . . ?
C1 C6 C21 C22 108.8(4) . . . . ?
C3 C2 C24 C25 -75.4(4) . . . . ?
C1 C2 C24 C25 102.8(4) . . . . ?
C3 C2 C24 C26 48.4(4) . . . . ?
C1 C2 C24 C26 -133.4(3) . . . . ?
Pd1 O2 C27 O3 11.3(4) . . . . ?
Pd1 O2 C27 C28 -168.3(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O3 0.74 2.27 2.895(3) 142.7 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_11076
_database_code_depnum_ccdc_archive 'CCDC 1040525'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H21 Cl N2 O Pd, C H Cl3'
_chemical_formula_sum            'C23 H22 Cl4 N2 O Pd'
_chemical_formula_weight         590.63

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   17.785(4)
_cell_length_b                   8.6156(19)
_cell_length_c                   16.469(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.168(4)
_cell_angle_gamma                90.00
_cell_volume                     2368.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    748
_cell_measurement_theta_min      2.635
_cell_measurement_theta_max      23.187

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   
;
absorption correction based on 4126 reflections(SADABS);Rint 0.0892 before
correction and 0.0552 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18002
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4659
_reflns_number_gt                2937
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0187P)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         4659
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.0938
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_restrained_S_all      0.897
_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 0.55526(2) 0.78110(5) 0.45000(3) 0.02802(13) Uani 1 1 d . . .
Cl1 Cl 0.64576(8) 0.80914(16) 0.37910(9) 0.0355(4) Uani 1 1 d . . .
O1 O 0.4818(2) 0.9154(4) 0.3619(2) 0.0359(10) Uani 1 1 d . . .
N1 N 0.6264(2) 0.6525(5) 0.5485(3) 0.0290(11) Uani 1 1 d . . .
N2 N 0.4809(2) 0.7546(5) 0.5143(3) 0.0262(11) Uani 1 1 d . . .
C1 C 0.7079(3) 0.6083(6) 0.5606(3) 0.0283(13) Uani 1 1 d . . .
C2 C 0.7682(3) 0.6561(7) 0.6337(4) 0.0451(17) Uani 1 1 d . . .
H2 H 0.7565 0.7201 0.6748 0.054 Uiso 1 1 calc R . .
C3 C 0.8465(4) 0.6104(7) 0.6475(4) 0.0521(19) Uani 1 1 d . . .
H3 H 0.8881 0.6457 0.6977 0.062 Uiso 1 1 calc R . .
C4 C 0.8652(3) 0.5148(7) 0.5900(4) 0.0373(15) Uani 1 1 d . . .
C5 C 0.8040(3) 0.4701(6) 0.5170(4) 0.0368(15) Uani 1 1 d . . .
H5 H 0.8157 0.4054 0.4762 0.044 Uiso 1 1 calc R . .
C6 C 0.7252(3) 0.5165(6) 0.5008(3) 0.0318(14) Uani 1 1 d . . .
H6 H 0.6839 0.4853 0.4493 0.038 Uiso 1 1 calc R . .
C7 C 0.5945(3) 0.6149(6) 0.6060(3) 0.0303(14) Uani 1 1 d . . .
C8 C 0.6307(3) 0.5077(6) 0.6809(3) 0.0451(17) Uani 1 1 d . . .
H8A H 0.6784 0.4581 0.6755 0.068 Uiso 1 1 calc R . .
H8B H 0.5916 0.4280 0.6813 0.068 Uiso 1 1 calc R . .
H8C H 0.6460 0.5670 0.7350 0.068 Uiso 1 1 calc R . .
C9 C 0.5163(3) 0.6847(6) 0.5937(3) 0.0277(13) Uani 1 1 d . . .
C10 C 0.4816(3) 0.6849(6) 0.6559(4) 0.0353(14) Uani 1 1 d . . .
H10 H 0.5066 0.6345 0.7099 0.042 Uiso 1 1 calc R . .
C11 C 0.4088(3) 0.7607(6) 0.6381(4) 0.0355(14) Uani 1 1 d . . .
H11 H 0.3851 0.7696 0.6815 0.043 Uiso 1 1 calc R . .
C12 C 0.3713(3) 0.8226(6) 0.5574(4) 0.0330(14) Uani 1 1 d . . .
H12 H 0.3205 0.8708 0.5446 0.040 Uiso 1 1 calc R . .
C13 C 0.4070(3) 0.8157(6) 0.4934(4) 0.0293(13) Uani 1 1 d . . .
C14 C 0.3658(3) 0.8774(6) 0.4063(4) 0.0286(13) Uani 1 1 d . . .
C15 C 0.4049(3) 0.9257(6) 0.3503(4) 0.0290(13) Uani 1 1 d . . .
C16 C 0.3573(3) 0.9961(6) 0.2709(4) 0.0361(15) Uani 1 1 d . . .
H16 H 0.3832 1.0384 0.2342 0.043 Uiso 1 1 calc R . .
C17 C 0.2755(4) 1.0048(6) 0.2456(4) 0.0420(16) Uani 1 1 d . . .
H17 H 0.2458 1.0518 0.1919 0.050 Uiso 1 1 calc R . .
C18 C 0.2359(4) 0.9453(7) 0.2980(4) 0.0448(17) Uani 1 1 d . . .
H18 H 0.1790 0.9458 0.2794 0.054 Uiso 1 1 calc R . .
C19 C 0.2810(3) 0.8850(6) 0.3784(4) 0.0409(16) Uani 1 1 d . . .
H19 H 0.2543 0.8479 0.4156 0.049 Uiso 1 1 calc R . .
C20 C 0.9502(4) 0.4589(8) 0.6091(4) 0.0490(17) Uani 1 1 d . . .
H20 H 0.9498 0.3851 0.5621 0.059 Uiso 1 1 calc R . .
C21 C 1.0069(3) 0.5912(8) 0.6087(4) 0.059(2) Uani 1 1 d . . .
H21A H 0.9854 0.6490 0.5543 0.089 Uiso 1 1 calc R . .
H21B H 1.0596 0.5489 0.6143 0.089 Uiso 1 1 calc R . .
H21C H 1.0122 0.6610 0.6574 0.089 Uiso 1 1 calc R . .
C22 C 0.9797(4) 0.3708(8) 0.6939(4) 0.074(2) Uani 1 1 d . . .
H22A H 0.9785 0.4392 0.7410 0.112 Uiso 1 1 calc R . .
H22B H 1.0346 0.3351 0.7049 0.112 Uiso 1 1 calc R . .
H22C H 0.9448 0.2811 0.6906 0.112 Uiso 1 1 calc R . .
C23 C 0.8354(3) 0.9582(7) 0.4341(4) 0.0531(18) Uani 1 1 d . . .
H23 H 0.7850 0.9133 0.4381 0.064 Uiso 1 1 calc R . .
Cl2 Cl 0.89630(12) 1.0154(2) 0.53738(12) 0.0817(6) Uani 1 1 d . . .
Cl3 Cl 0.88282(11) 0.8157(2) 0.39323(12) 0.0702(6) Uani 1 1 d . . .
Cl4 Cl 0.81021(11) 1.1185(2) 0.36413(12) 0.0689(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O1 1.961(3) . ?
Pd1 N2 1.972(4) . ?
Pd1 N1 2.011(4) . ?
Pd1 Cl1 2.3039(14) . ?
O1 C15 1.317(6) . ?
N1 C7 1.301(6) . ?
N1 C1 1.445(6) . ?
N2 C13 1.346(6) . ?
N2 C9 1.378(6) . ?
C1 C2 1.371(7) . ?
C1 C6 1.377(6) . ?
C2 C3 1.388(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.370(7) . ?
C4 C20 1.513(7) . ?
C5 C6 1.392(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C9 1.464(7) . ?
C7 C8 1.497(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.366(7) . ?
C10 C11 1.388(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.373(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.406(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.468(7) . ?
C14 C15 1.396(7) . ?
C14 C19 1.418(7) . ?
C15 C16 1.425(7) . ?
C16 C17 1.371(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(7) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.516(8) . ?
C20 C21 1.523(8) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 Cl2 1.742(6) . ?
C23 Cl3 1.750(6) . ?
C23 Cl4 1.755(6) . ?
C23 H23 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pd1 N2 93.84(16) . . ?
O1 Pd1 N1 174.56(16) . . ?
N2 Pd1 N1 81.65(17) . . ?
O1 Pd1 Cl1 88.09(11) . . ?
N2 Pd1 Cl1 177.97(13) . . ?
N1 Pd1 Cl1 96.40(13) . . ?
C15 O1 Pd1 122.7(3) . . ?
C7 N1 C1 120.2(5) . . ?
C7 N1 Pd1 114.4(4) . . ?
C1 N1 Pd1 125.3(3) . . ?
C13 N2 C9 120.0(4) . . ?
C13 N2 Pd1 126.4(4) . . ?
C9 N2 Pd1 112.8(3) . . ?
C2 C1 C6 120.1(5) . . ?
C2 C1 N1 119.0(5) . . ?
C6 C1 N1 120.9(5) . . ?
C1 C2 C3 119.6(5) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 121.6(6) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C5 C4 C3 117.6(5) . . ?
C5 C4 C20 121.8(5) . . ?
C3 C4 C20 120.5(6) . . ?
C4 C5 C6 122.0(5) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C5 119.1(5) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
N1 C7 C9 115.4(5) . . ?
N1 C7 C8 125.6(5) . . ?
C9 C7 C8 119.0(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 122.3(5) . . ?
C10 C9 C7 123.4(5) . . ?
N2 C9 C7 114.3(5) . . ?
C9 C10 C11 118.1(5) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C12 C11 C10 119.6(5) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 121.0(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
N2 C13 C12 118.6(5) . . ?
N2 C13 C14 120.4(5) . . ?
C12 C13 C14 120.9(5) . . ?
C15 C14 C19 119.2(5) . . ?
C15 C14 C13 124.0(5) . . ?
C19 C14 C13 116.8(5) . . ?
O1 C15 C14 127.9(5) . . ?
O1 C15 C16 114.8(5) . . ?
C14 C15 C16 117.4(5) . . ?
C17 C16 C15 122.3(5) . . ?
C17 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C17 C18 120.3(6) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C19 118.7(5) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C18 C19 C14 121.8(6) . . ?
C18 C19 H19 119.1 . . ?
C14 C19 H19 119.1 . . ?
C4 C20 C22 110.7(5) . . ?
C4 C20 C21 112.1(5) . . ?
C22 C20 C21 111.1(5) . . ?
C4 C20 H20 107.6 . . ?
C22 C20 H20 107.6 . . ?
C21 C20 H20 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Cl2 C23 Cl3 110.8(3) . . ?
Cl2 C23 Cl4 110.5(3) . . ?
Cl3 C23 Cl4 110.3(4) . . ?
Cl2 C23 H23 108.4 . . ?
Cl3 C23 H23 108.4 . . ?
Cl4 C23 H23 108.4 . . ?

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
N2 Pd1 O1 C15 -16.3(4) . . . . ?
Cl1 Pd1 O1 C15 164.3(4) . . . . ?
N2 Pd1 N1 C7 -0.9(4) . . . . ?
Cl1 Pd1 N1 C7 178.6(3) . . . . ?
N2 Pd1 N1 C1 -177.8(4) . . . . ?
Cl1 Pd1 N1 C1 1.7(4) . . . . ?
O1 Pd1 N2 C13 0.9(4) . . . . ?
N1 Pd1 N2 C13 177.8(4) . . . . ?
O1 Pd1 N2 C9 -169.4(3) . . . . ?
N1 Pd1 N2 C9 7.6(3) . . . . ?
C7 N1 C1 C2 -57.6(7) . . . . ?
Pd1 N1 C1 C2 119.1(5) . . . . ?
C7 N1 C1 C6 120.8(6) . . . . ?
Pd1 N1 C1 C6 -62.5(6) . . . . ?
C6 C1 C2 C3 -0.5(9) . . . . ?
N1 C1 C2 C3 177.9(5) . . . . ?
C1 C2 C3 C4 -1.4(10) . . . . ?
C2 C3 C4 C5 2.0(10) . . . . ?
C2 C3 C4 C20 -176.4(6) . . . . ?
C3 C4 C5 C6 -0.8(9) . . . . ?
C20 C4 C5 C6 177.5(5) . . . . ?
C2 C1 C6 C5 1.6(8) . . . . ?
N1 C1 C6 C5 -176.8(5) . . . . ?
C4 C5 C6 C1 -1.0(8) . . . . ?
C1 N1 C7 C9 171.4(4) . . . . ?
Pd1 N1 C7 C9 -5.7(6) . . . . ?
C1 N1 C7 C8 -9.2(8) . . . . ?
Pd1 N1 C7 C8 173.7(4) . . . . ?
C13 N2 C9 C10 -5.2(7) . . . . ?
Pd1 N2 C9 C10 165.8(4) . . . . ?
C13 N2 C9 C7 176.5(4) . . . . ?
Pd1 N2 C9 C7 -12.6(5) . . . . ?
N1 C7 C9 C10 -166.1(5) . . . . ?
C8 C7 C9 C10 14.4(8) . . . . ?
N1 C7 C9 N2 12.2(7) . . . . ?
C8 C7 C9 N2 -167.2(4) . . . . ?
N2 C9 C10 C11 -1.0(8) . . . . ?
C7 C9 C10 C11 177.2(5) . . . . ?
C9 C10 C11 C12 4.7(8) . . . . ?
C10 C11 C12 C13 -2.5(8) . . . . ?
C9 N2 C13 C12 7.4(7) . . . . ?
Pd1 N2 C13 C12 -162.3(4) . . . . ?
C9 N2 C13 C14 -174.3(4) . . . . ?
Pd1 N2 C13 C14 16.1(7) . . . . ?
C11 C12 C13 N2 -3.6(7) . . . . ?
C11 C12 C13 C14 178.0(5) . . . . ?
N2 C13 C14 C15 -22.0(8) . . . . ?
C12 C13 C14 C15 156.3(5) . . . . ?
N2 C13 C14 C19 156.9(5) . . . . ?
C12 C13 C14 C19 -24.8(7) . . . . ?
Pd1 O1 C15 C14 15.8(7) . . . . ?
Pd1 O1 C15 C16 -164.8(3) . . . . ?
C19 C14 C15 O1 -173.9(5) . . . . ?
C13 C14 C15 O1 5.0(9) . . . . ?
C19 C14 C15 C16 6.6(7) . . . . ?
C13 C14 C15 C16 -174.4(5) . . . . ?
O1 C15 C16 C17 174.8(5) . . . . ?
C14 C15 C16 C17 -5.7(8) . . . . ?
C15 C16 C17 C18 0.6(9) . . . . ?
C16 C17 C18 C19 3.6(9) . . . . ?
C17 C18 C19 C14 -2.5(9) . . . . ?
C15 C14 C19 C18 -2.8(8) . . . . ?
C13 C14 C19 C18 178.2(5) . . . . ?
C5 C4 C20 C22 -120.1(6) . . . . ?
C3 C4 C20 C22 58.2(8) . . . . ?
C5 C4 C20 C21 115.2(6) . . . . ?
C3 C4 C20 C21 -66.5(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_13015
_database_code_depnum_ccdc_archive 'CCDC 1040526'
_audit_update_record             
;
2015-02-09 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H24 N3 O Pd, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C27 H27 F3 N4 O4 Pd S'
_chemical_formula_weight         666.99

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'
S S 0.1246 0.1234 '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'
F F 0.0171 0.0103 '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                   13.264(11)
_cell_length_b                   13.822(11)
_cell_length_c                   17.160(14)
_cell_angle_alpha                80.989(15)
_cell_angle_beta                 78.907(15)
_cell_angle_gamma                64.369(13)
_cell_volume                     2774(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1000
_cell_measurement_theta_min      2.240
_cell_measurement_theta_max      28.231

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1352
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
absorption correction based on 6715 reflections(SADABS);Rint 0.1370 before
correction and 0.0694 after.
;

_exptl_special_details           
; 
 One of the CF3SO3- anions is highly disordered.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21653
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_sigmaI/netI    0.1559
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         26.00
_reflns_number_total             10758
_reflns_number_gt                6520
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 

The restraints DELU, SIMU and DFIX have been used in the refinement of the 
structure.
 
 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)+(0.1366P)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         10758
_refine_ls_number_parameters     740
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.0999
_refine_ls_wR_factor_ref         0.2619
_refine_ls_wR_factor_gt          0.2351
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.038
_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 0.45216(6) 0.17003(6) 0.40941(4) 0.0308(2) Uani 1 1 d . . .
O1 O 0.6138(6) 0.0759(6) 0.4020(4) 0.0407(17) Uani 1 1 d . . .
N1 N 0.2835(7) 0.2571(6) 0.4242(5) 0.036(2) Uani 1 1 d . . .
N2 N 0.4267(7) 0.1586(6) 0.5258(5) 0.0277(17) Uani 1 1 d . . .
N3 N 0.4718(7) 0.1807(7) 0.2899(6) 0.038(2) Uani 1 1 d . . .
C1 C 0.2193(8) 0.3115(7) 0.3586(6) 0.031(2) Uani 1 1 d . . .
C2 C 0.1907(11) 0.2529(9) 0.3152(7) 0.052(3) Uani 1 1 d . . .
H2 H 0.2094 0.1785 0.3294 0.063 Uiso 1 1 calc R . .
C3 C 0.1343(10) 0.3052(10) 0.2506(7) 0.052(3) Uani 1 1 d . . .
H3 H 0.1136 0.2662 0.2206 0.063 Uiso 1 1 calc R . .
C4 C 0.1073(9) 0.4133(8) 0.2288(6) 0.039(2) Uani 1 1 d . . .
C5 C 0.1384(8) 0.4668(8) 0.2715(6) 0.036(2) Uani 1 1 d . . .
H5 H 0.1215 0.5406 0.2560 0.044 Uiso 1 1 calc R . .
C6 C 0.1946(8) 0.4182(8) 0.3375(7) 0.040(3) Uani 1 1 d . . .
H6 H 0.2151 0.4580 0.3670 0.048 Uiso 1 1 calc R . .
C7 C 0.2335(8) 0.2551(8) 0.4955(6) 0.035(2) Uani 1 1 d . . .
C8 C 0.1112(8) 0.3040(9) 0.5231(7) 0.048(3) Uani 1 1 d . . .
H8A H 0.0708 0.3424 0.4777 0.071 Uiso 1 1 calc R . .
H8B H 0.0951 0.3547 0.5627 0.071 Uiso 1 1 calc R . .
H8C H 0.0864 0.2474 0.5473 0.071 Uiso 1 1 calc R . .
C9 C 0.3129(8) 0.1987(7) 0.5571(6) 0.033(2) Uani 1 1 d . . .
C10 C 0.2782(9) 0.1861(8) 0.6350(6) 0.039(3) Uani 1 1 d . . .
H10 H 0.1999 0.2121 0.6548 0.047 Uiso 1 1 calc R . .
C11 C 0.3595(10) 0.1338(8) 0.6870(7) 0.047(3) Uani 1 1 d . . .
H11 H 0.3365 0.1261 0.7427 0.056 Uiso 1 1 calc R . .
C12 C 0.4724(9) 0.0939(8) 0.6571(6) 0.039(2) Uani 1 1 d . . .
H12 H 0.5270 0.0565 0.6922 0.047 Uiso 1 1 calc R . .
C13 C 0.5078(9) 0.1075(7) 0.5761(6) 0.034(2) Uani 1 1 d . . .
C14 C 0.6286(8) 0.0692(7) 0.5437(6) 0.031(2) Uani 1 1 d . . .
C15 C 0.6722(9) 0.0507(8) 0.4614(6) 0.037(2) Uani 1 1 d . . .
C16 C 0.7895(9) -0.0009(8) 0.4423(7) 0.044(3) Uani 1 1 d . . .
H16 H 0.8192 -0.0179 0.3888 0.053 Uiso 1 1 calc R . .
C17 C 0.8639(9) -0.0284(8) 0.4947(7) 0.044(3) Uani 1 1 d . . .
H17 H 0.9430 -0.0622 0.4780 0.052 Uiso 1 1 calc R . .
C18 C 0.8205(9) -0.0053(8) 0.5755(7) 0.043(3) Uani 1 1 d . . .
H18 H 0.8697 -0.0211 0.6137 0.052 Uiso 1 1 calc R . .
C19 C 0.7071(9) 0.0398(8) 0.5963(6) 0.038(2) Uani 1 1 d . . .
H19 H 0.6789 0.0523 0.6507 0.045 Uiso 1 1 calc R . .
C20 C 0.0453(10) 0.4738(11) 0.1572(7) 0.058(3) Uani 1 1 d . . .
H20 H -0.0215 0.5397 0.1757 0.070 Uiso 1 1 calc R . .
C21 C 0.1208(14) 0.5083(19) 0.0933(9) 0.123(8) Uani 1 1 d . . .
H21A H 0.1908 0.4455 0.0787 0.184 Uiso 1 1 calc R . .
H21B H 0.1386 0.5610 0.1133 0.184 Uiso 1 1 calc R . .
H21C H 0.0821 0.5411 0.0464 0.184 Uiso 1 1 calc R . .
C22 C 0.0034(17) 0.4067(14) 0.1198(11) 0.114(7) Uani 1 1 d . . .
H22A H -0.0465 0.4530 0.0810 0.171 Uiso 1 1 calc R . .
H22B H -0.0381 0.3756 0.1616 0.171 Uiso 1 1 calc R . .
H22C H 0.0682 0.3488 0.0929 0.171 Uiso 1 1 calc R . .
C23 C 0.4817(10) 0.1859(10) 0.2223(7) 0.051(3) Uani 1 1 d . . .
C24 C 0.4938(13) 0.1933(13) 0.1353(8) 0.077(4) Uani 1 1 d . . .
H24A H 0.5501 0.1245 0.1160 0.116 Uiso 1 1 calc R . .
H24B H 0.5183 0.2506 0.1130 0.116 Uiso 1 1 calc R . .
H24C H 0.4210 0.2097 0.1187 0.116 Uiso 1 1 calc R . .
Pd1A Pd 0.50531(6) 0.38587(6) 0.39441(5) 0.0313(2) Uani 1 1 d . . .
O1A O 0.3473(6) 0.4661(6) 0.4427(4) 0.0445(18) Uani 1 1 d . . .
N1A N 0.6678(6) 0.3104(6) 0.3499(5) 0.0291(18) Uani 1 1 d . . .
N2A N 0.5661(7) 0.3427(6) 0.4954(5) 0.0313(19) Uani 1 1 d . . .
N3A N 0.4528(7) 0.4362(7) 0.2880(6) 0.042(2) Uani 1 1 d . . .
C1A C 0.7083(8) 0.2886(9) 0.2689(7) 0.040(3) Uani 1 1 d . . .
C2A C 0.7113(9) 0.3710(9) 0.2139(7) 0.046(3) Uani 1 1 d . . .
H2A H 0.6890 0.4405 0.2308 0.055 Uiso 1 1 calc R . .
C3A C 0.7460(10) 0.3543(10) 0.1349(7) 0.053(3) Uani 1 1 d . . .
H3A H 0.7478 0.4122 0.0975 0.063 Uiso 1 1 calc R . .
C4A C 0.7792(10) 0.2519(11) 0.1083(7) 0.051(3) Uani 1 1 d . . .
C5A C 0.7710(10) 0.1726(11) 0.1628(8) 0.058(3) Uani 1 1 d . . .
H5A H 0.7895 0.1041 0.1457 0.070 Uiso 1 1 calc R . .
C6A C 0.7362(9) 0.1891(9) 0.2436(7) 0.046(3) Uani 1 1 d . . .
H6A H 0.7317 0.1321 0.2810 0.055 Uiso 1 1 calc R . .
C7A C 0.7359(9) 0.2771(7) 0.4030(7) 0.038(3) Uani 1 1 d . . .
C8A C 0.8627(8) 0.2250(8) 0.3847(7) 0.042(3) Uani 1 1 d . . .
H8A1 H 0.8850 0.2220 0.3269 0.064 Uiso 1 1 calc R . .
H8A2 H 0.8912 0.1518 0.4108 0.064 Uiso 1 1 calc R . .
H8A3 H 0.8945 0.2672 0.4043 0.064 Uiso 1 1 calc R . .
C9A C 0.6830(8) 0.2970(7) 0.4861(6) 0.035(2) Uani 1 1 d . . .
C10A C 0.7405(9) 0.2721(8) 0.5500(7) 0.043(3) Uani 1 1 d . . .
H10A H 0.8207 0.2403 0.5428 0.052 Uiso 1 1 calc R . .
C11A C 0.6807(10) 0.2938(8) 0.6246(7) 0.044(3) Uani 1 1 d . . .
H11A H 0.7196 0.2796 0.6691 0.053 Uiso 1 1 calc R . .
C12A C 0.5648(11) 0.3359(9) 0.6353(7) 0.046(3) Uani 1 1 d . . .
H12A H 0.5236 0.3482 0.6872 0.056 Uiso 1 1 calc R . .
C13A C 0.5071(9) 0.3609(7) 0.5690(7) 0.039(3) Uani 1 1 d . . .
C14A C 0.3809(8) 0.4082(7) 0.5815(6) 0.033(2) Uani 1 1 d . . .
C15A C 0.3129(8) 0.4590(8) 0.5188(6) 0.033(2) Uani 1 1 d . . .
C16A C 0.1956(9) 0.5105(8) 0.5387(8) 0.048(3) Uani 1 1 d . . .
H16A H 0.1506 0.5472 0.4975 0.058 Uiso 1 1 calc R . .
C17A C 0.1445(11) 0.5098(10) 0.6147(8) 0.053(3) Uani 1 1 d . . .
H17A H 0.0646 0.5446 0.6265 0.064 Uiso 1 1 calc R . .
C18A C 0.2117(12) 0.4559(9) 0.6776(8) 0.060(4) Uani 1 1 d . . .
H18A H 0.1770 0.4537 0.7313 0.072 Uiso 1 1 calc R . .
C19A C 0.3245(10) 0.4087(8) 0.6592(7) 0.043(3) Uani 1 1 d . . .
H19A H 0.3683 0.3738 0.7013 0.052 Uiso 1 1 calc R . .
C20A C 0.8158(12) 0.2352(14) 0.0185(9) 0.080(5) Uani 1 1 d . . .
H20A H 0.8094 0.3079 -0.0058 0.096 Uiso 1 1 calc R . .
C21A C 0.7402(14) 0.2160(16) -0.0205(9) 0.099(6) Uani 1 1 d . . .
H21D H 0.7648 0.2175 -0.0781 0.148 Uiso 1 1 calc R . .
H21E H 0.6635 0.2721 -0.0093 0.148 Uiso 1 1 calc R . .
H21F H 0.7405 0.1454 -0.0006 0.148 Uiso 1 1 calc R . .
C22A C 0.9404(13) 0.1672(15) 0.0050(9) 0.098(6) Uani 1 1 d . . .
H22D H 0.9561 0.0940 0.0293 0.148 Uiso 1 1 calc R . .
H22E H 0.9797 0.1982 0.0292 0.148 Uiso 1 1 calc R . .
H22F H 0.9668 0.1650 -0.0524 0.148 Uiso 1 1 calc R . .
C23A C 0.4234(9) 0.4756(9) 0.2258(8) 0.044(3) Uani 1 1 d . . .
C24A C 0.3927(11) 0.5200(11) 0.1469(7) 0.061(3) Uani 1 1 d . . .
H24D H 0.4545 0.5344 0.1138 0.092 Uiso 1 1 calc R . .
H24E H 0.3242 0.5872 0.1513 0.092 Uiso 1 1 calc R . .
H24F H 0.3788 0.4683 0.1224 0.092 Uiso 1 1 calc R . .
S1 S 0.0505(3) 0.8023(3) 0.2747(2) 0.0575(9) Uani 1 1 d . . .
O2 O 0.1447(9) 0.7236(7) 0.2310(6) 0.088(3) Uani 1 1 d . . .
O3 O -0.0595(10) 0.8271(13) 0.2562(7) 0.124(5) Uani 1 1 d . . .
O4 O 0.0542(7) 0.7958(8) 0.3573(5) 0.068(3) Uani 1 1 d . . .
C25 C 0.0682(11) 0.9265(11) 0.2360(9) 0.063(4) Uani 1 1 d . . .
F1 F 0.1723(7) 0.9130(6) 0.2450(5) 0.076(2) Uani 1 1 d . . .
F2 F 0.0575(8) 0.9510(7) 0.1612(5) 0.093(3) Uani 1 1 d . . .
F3 F -0.0034(9) 1.0074(7) 0.2777(6) 0.112(4) Uani 1 1 d . . .
S2 S 0.6245(4) 0.6712(3) 0.0710(3) 0.0935(14) Uani 1 1 d DU A .
O5 O 0.6816(14) 0.7270(12) 0.0145(8) 0.149(5) Uani 1 1 d DU . .
O6 O 0.5801(9) 0.6202(8) 0.0299(6) 0.075(3) Uani 1 1 d . . .
O7 O 0.6964(12) 0.6100(9) 0.1302(8) 0.120(5) Uani 1 1 d . . .
C26 C 0.5068(14) 0.7838(12) 0.1180(9) 0.141(7) Uani 1 1 d DU . .
F4 F 0.5516(10) 0.8351(10) 0.1528(8) 0.146(5) Uani 1 1 d . A .
F5 F 0.4569(12) 0.8539(10) 0.0593(8) 0.159(6) Uani 1 1 d D A .
F6B F 0.424(2) 0.766(2) 0.1657(15) 0.148(8) Uani 0.50 1 d PDU A 1
F6C F 0.512(3) 0.6901(19) 0.1609(17) 0.170(8) Uani 0.50 1 d PDU A 2
N4 N 0.7352(14) 0.9558(12) 0.1069(9) 0.104(5) Uani 1 1 d . . .
C27 C 0.7858(14) 0.8674(13) 0.1155(8) 0.069(4) Uani 1 1 d . . .
C28 C 0.8524(17) 0.7528(12) 0.1266(10) 0.103(6) Uani 1 1 d . . .
H28A H 0.8916 0.7250 0.0750 0.154 Uiso 1 1 calc R . .
H28B H 0.8028 0.7170 0.1506 0.154 Uiso 1 1 calc R . .
H28C H 0.9081 0.7387 0.1619 0.154 Uiso 1 1 calc R . .
N5 N 0.3446(12) 0.0429(10) 0.2064(8) 0.080(4) Uani 1 1 d . . .
C29 C 0.2989(16) 0.0601(12) 0.1522(10) 0.082(5) Uani 1 1 d . . .
C30 C 0.244(2) 0.0765(17) 0.0821(12) 0.140(9) Uani 1 1 d . . .
H30A H 0.2844 0.0137 0.0509 0.210 Uiso 1 1 calc R . .
H30B H 0.2449 0.1409 0.0493 0.210 Uiso 1 1 calc R . .
H30C H 0.1656 0.0859 0.0991 0.210 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 N2 1.953(8) . ?
Pd1 O1 1.959(7) . ?
Pd1 N3 2.007(9) . ?
Pd1 N1 2.017(8) . ?
O1 C15 1.312(12) . ?
N1 C7 1.277(13) . ?
N1 C1 1.452(12) . ?
N2 C13 1.382(12) . ?
N2 C9 1.389(12) . ?
N3 C23 1.138(13) . ?
C1 C6 1.369(13) . ?
C1 C2 1.385(15) . ?
C2 C3 1.383(15) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.342(15) . ?
C4 C20 1.536(15) . ?
C5 C6 1.394(14) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.472(14) . ?
C7 C9 1.515(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.337(14) . ?
C10 C11 1.405(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(15) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(14) . ?
C12 H12 0.9500 . ?
C13 C14 1.474(14) . ?
C14 C19 1.394(14) . ?
C14 C15 1.437(14) . ?
C15 C16 1.398(14) . ?
C16 C17 1.355(15) . ?
C16 H16 0.9500 . ?
C17 C18 1.424(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.353(15) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.503(18) . ?
C20 C22 1.532(19) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.462(17) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
Pd1A N2A 1.951(8) . ?
Pd1A O1A 1.979(7) . ?
Pd1A N3A 1.994(10) . ?
Pd1A N1A 1.997(8) . ?
O1A C15A 1.301(12) . ?
N1A C7A 1.297(13) . ?
N1A C1A 1.420(13) . ?
N2A C13A 1.349(13) . ?
N2A C9A 1.385(12) . ?
N3A C23A 1.176(14) . ?
C1A C2A 1.371(14) . ?
C1A C6A 1.379(15) . ?
C2A C3A 1.367(16) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.411(17) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.353(17) . ?
C4A C20A 1.545(18) . ?
C5A C6A 1.396(16) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C7A C9A 1.473(15) . ?
C7A C8A 1.506(14) . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A C10A 1.372(14) . ?
C10A C11A 1.371(15) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.374(16) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.407(15) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.495(14) . ?
C14A C19A 1.399(14) . ?
C14A C15A 1.433(14) . ?
C15A C16A 1.399(14) . ?
C16A C17A 1.350(16) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.435(18) . ?
C17A H17A 0.9500 . ?
C18A C19A 1.342(16) . ?
C18A H18A 0.9500 . ?
C19A H19A 0.9500 . ?
C20A C21A 1.44(2) . ?
C20A C22A 1.50(2) . ?
C20A H20A 1.0000 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C23A C24A 1.454(17) . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
S1 O4 1.416(9) . ?
S1 O2 1.423(10) . ?
S1 O3 1.434(11) . ?
S1 C25 1.838(14) . ?
C25 F2 1.294(15) . ?
C25 F3 1.317(14) . ?
C25 F1 1.348(15) . ?
S2 O6 1.419(10) . ?
S2 O7 1.436(11) . ?
S2 O5 1.448(8) . ?
S2 C26 1.821(10) . ?
C26 F6B 1.326(10) . ?
C26 F5 1.337(10) . ?
C26 F4 1.36(2) . ?
C26 F6C 1.366(10) . ?
N4 C27 1.112(18) . ?
C27 C28 1.44(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N5 C29 1.145(19) . ?
C29 C30 1.46(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
N2 Pd1 O1 94.5(3) . . ?
N2 Pd1 N3 177.3(3) . . ?
O1 Pd1 N3 87.4(3) . . ?
N2 Pd1 N1 82.0(3) . . ?
O1 Pd1 N1 175.0(3) . . ?
N3 Pd1 N1 95.9(3) . . ?
C15 O1 Pd1 123.7(6) . . ?
C7 N1 C1 120.7(9) . . ?
C7 N1 Pd1 115.6(7) . . ?
C1 N1 Pd1 123.4(6) . . ?
C13 N2 C9 119.8(8) . . ?
C13 N2 Pd1 126.8(7) . . ?
C9 N2 Pd1 113.1(6) . . ?
C23 N3 Pd1 178.8(10) . . ?
C6 C1 C2 121.1(10) . . ?
C6 C1 N1 119.4(9) . . ?
C2 C1 N1 119.4(9) . . ?
C3 C2 C1 118.4(10) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 121.4(11) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 118.4(10) . . ?
C5 C4 C20 118.8(10) . . ?
C3 C4 C20 122.7(10) . . ?
C4 C5 C6 122.5(9) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C1 C6 C5 118.1(10) . . ?
C1 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
N1 C7 C8 127.6(10) . . ?
N1 C7 C9 114.0(9) . . ?
C8 C7 C9 118.4(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 122.1(10) . . ?
C10 C9 C7 123.7(10) . . ?
N2 C9 C7 114.2(8) . . ?
C9 C10 C11 118.9(10) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C10 119.8(10) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.9(10) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
N2 C13 C12 118.4(10) . . ?
N2 C13 C14 120.1(9) . . ?
C12 C13 C14 121.4(9) . . ?
C19 C14 C15 117.1(10) . . ?
C19 C14 C13 118.8(9) . . ?
C15 C14 C13 123.8(9) . . ?
O1 C15 C16 116.1(10) . . ?
O1 C15 C14 127.1(10) . . ?
C16 C15 C14 116.8(10) . . ?
C17 C16 C15 124.7(11) . . ?
C17 C16 H16 117.7 . . ?
C15 C16 H16 117.7 . . ?
C16 C17 C18 118.2(10) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C19 C18 C17 118.2(10) . . ?
C19 C18 H18 120.9 . . ?
C17 C18 H18 120.9 . . ?
C18 C19 C14 124.8(10) . . ?
C18 C19 H19 117.6 . . ?
C14 C19 H19 117.6 . . ?
C21 C20 C22 107.9(14) . . ?
C21 C20 C4 110.7(10) . . ?
C22 C20 C4 113.2(11) . . ?
C21 C20 H20 108.3 . . ?
C22 C20 H20 108.3 . . ?
C4 C20 H20 108.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 C24 179.6(17) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2A Pd1A O1A 95.0(3) . . ?
N2A Pd1A N3A 174.9(3) . . ?
O1A Pd1A N3A 87.8(3) . . ?
N2A Pd1A N1A 82.5(3) . . ?
O1A Pd1A N1A 176.1(3) . . ?
N3A Pd1A N1A 94.5(3) . . ?
C15A O1A Pd1A 123.3(7) . . ?
C7A N1A C1A 121.3(8) . . ?
C7A N1A Pd1A 113.8(7) . . ?
C1A N1A Pd1A 124.8(6) . . ?
C13A N2A C9A 119.5(9) . . ?
C13A N2A Pd1A 127.0(7) . . ?
C9A N2A Pd1A 113.2(6) . . ?
C23A N3A Pd1A 172.8(9) . . ?
C2A C1A C6A 119.4(11) . . ?
C2A C1A N1A 118.8(10) . . ?
C6A C1A N1A 121.6(10) . . ?
C3A C2A C1A 120.7(11) . . ?
C3A C2A H2A 119.7 . . ?
C1A C2A H2A 119.7 . . ?
C2A C3A C4A 120.7(11) . . ?
C2A C3A H3A 119.7 . . ?
C4A C3A H3A 119.7 . . ?
C5A C4A C3A 117.9(11) . . ?
C5A C4A C20A 122.1(13) . . ?
C3A C4A C20A 119.9(12) . . ?
C4A C5A C6A 121.6(12) . . ?
C4A C5A H5A 119.2 . . ?
C6A C5A H5A 119.2 . . ?
C1A C6A C5A 119.6(11) . . ?
C1A C6A H6A 120.2 . . ?
C5A C6A H6A 120.2 . . ?
N1A C7A C9A 116.3(9) . . ?
N1A C7A C8A 124.6(10) . . ?
C9A C7A C8A 119.1(10) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10A C9A N2A 121.4(10) . . ?
C10A C9A C7A 125.1(10) . . ?
N2A C9A C7A 113.5(9) . . ?
C11A C10A C9A 119.2(10) . . ?
C11A C10A H10A 120.4 . . ?
C9A C10A H10A 120.4 . . ?
C10A C11A C12A 120.2(11) . . ?
C10A C11A H11A 119.9 . . ?
C12A C11A H11A 119.9 . . ?
C11A C12A C13A 119.9(11) . . ?
C11A C12A H12A 120.1 . . ?
C13A C12A H12A 120.1 . . ?
N2A C13A C12A 119.8(10) . . ?
N2A C13A C14A 121.0(10) . . ?
C12A C13A C14A 119.2(10) . . ?
C19A C14A C15A 117.2(9) . . ?
C19A C14A C13A 118.7(10) . . ?
C15A C14A C13A 124.1(9) . . ?
O1A C15A C16A 113.7(10) . . ?
O1A C15A C14A 127.4(9) . . ?
C16A C15A C14A 118.8(9) . . ?
C17A C16A C15A 122.0(12) . . ?
C17A C16A H16A 119.0 . . ?
C15A C16A H16A 119.0 . . ?
C16A C17A C18A 119.5(12) . . ?
C16A C17A H17A 120.3 . . ?
C18A C17A H17A 120.3 . . ?
C19A C18A C17A 118.9(12) . . ?
C19A C18A H18A 120.6 . . ?
C17A C18A H18A 120.6 . . ?
C18A C19A C14A 123.5(12) . . ?
C18A C19A H19A 118.2 . . ?
C14A C19A H19A 118.2 . . ?
C21A C20A C22A 120.5(14) . . ?
C21A C20A C4A 116.0(12) . . ?
C22A C20A C4A 108.6(13) . . ?
C21A C20A H20A 103.0 . . ?
C22A C20A H20A 103.0 . . ?
C4A C20A H20A 103.0 . . ?
C20A C21A H21D 109.5 . . ?
C20A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C20A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C20A C22A H22D 109.5 . . ?
C20A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C20A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
N3A C23A C24A 176.9(12) . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
O4 S1 O2 115.6(6) . . ?
O4 S1 O3 113.5(6) . . ?
O2 S1 O3 117.4(8) . . ?
O4 S1 C25 103.5(6) . . ?
O2 S1 C25 101.9(6) . . ?
O3 S1 C25 101.8(8) . . ?
F2 C25 F3 110.1(11) . . ?
F2 C25 F1 108.2(11) . . ?
F3 C25 F1 106.3(13) . . ?
F2 C25 S1 112.4(11) . . ?
F3 C25 S1 110.8(10) . . ?
F1 C25 S1 108.8(9) . . ?
O6 S2 O7 120.0(7) . . ?
O6 S2 O5 110.0(8) . . ?
O7 S2 O5 108.3(10) . . ?
O6 S2 C26 108.2(9) . . ?
O7 S2 C26 107.5(8) . . ?
O5 S2 C26 101.0(10) . . ?
F6B C26 F5 105(2) . . ?
F6B C26 F4 112.9(18) . . ?
F5 C26 F4 105.2(15) . . ?
F6B C26 F6C 52.2(17) . . ?
F5 C26 F6C 142(3) . . ?
F4 C26 F6C 112(2) . . ?
F6B C26 S2 118.9(17) . . ?
F5 C26 S2 106.8(10) . . ?
F4 C26 S2 107.1(12) . . ?
F6C C26 S2 71.0(15) . . ?
N4 C27 C28 179(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C29 C30 177.2(19) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Pd1 O1 C15 -16.5(8) . . . . ?
N3 Pd1 O1 C15 165.4(8) . . . . ?
N1 Pd1 O1 C15 -64(4) . . . . ?
N2 Pd1 N1 C7 -9.1(7) . . . . ?
N3 Pd1 N1 C7 169.1(7) . . . . ?
N2 Pd1 N1 C1 176.1(8) . . . . ?
N3 Pd1 N1 C1 -5.7(8) . . . . ?
O1 Pd1 N2 C13 5.9(7) . . . . ?
N1 Pd1 N2 C13 -177.8(8) . . . . ?
O1 Pd1 N2 C9 -167.7(6) . . . . ?
N1 Pd1 N2 C9 8.6(6) . . . . ?
C7 N1 C1 C6 89.7(12) . . . . ?
Pd1 N1 C1 C6 -95.8(10) . . . . ?
C7 N1 C1 C2 -94.5(12) . . . . ?
Pd1 N1 C1 C2 80.0(11) . . . . ?
C6 C1 C2 C3 -1.3(17) . . . . ?
N1 C1 C2 C3 -177.0(10) . . . . ?
C1 C2 C3 C4 0.5(18) . . . . ?
C2 C3 C4 C5 0.7(17) . . . . ?
C2 C3 C4 C20 179.7(11) . . . . ?
C3 C4 C5 C6 -1.3(16) . . . . ?
C20 C4 C5 C6 179.7(10) . . . . ?
C2 C1 C6 C5 0.7(15) . . . . ?
N1 C1 C6 C5 176.5(9) . . . . ?
C4 C5 C6 C1 0.6(15) . . . . ?
C1 N1 C7 C8 -0.3(16) . . . . ?
Pd1 N1 C7 C8 -175.2(9) . . . . ?
C1 N1 C7 C9 -177.8(8) . . . . ?
Pd1 N1 C7 C9 7.3(11) . . . . ?
C13 N2 C9 C10 -2.5(13) . . . . ?
Pd1 N2 C9 C10 171.5(8) . . . . ?
C13 N2 C9 C7 178.6(8) . . . . ?
Pd1 N2 C9 C7 -7.4(10) . . . . ?
N1 C7 C9 C10 -178.9(9) . . . . ?
C8 C7 C9 C10 3.4(15) . . . . ?
N1 C7 C9 N2 0.0(12) . . . . ?
C8 C7 C9 N2 -177.7(9) . . . . ?
N2 C9 C10 C11 2.2(15) . . . . ?
C7 C9 C10 C11 -179.1(9) . . . . ?
C9 C10 C11 C12 -2.0(16) . . . . ?
C10 C11 C12 C13 2.1(16) . . . . ?
C9 N2 C13 C12 2.6(13) . . . . ?
Pd1 N2 C13 C12 -170.6(7) . . . . ?
C9 N2 C13 C14 -177.2(8) . . . . ?
Pd1 N2 C13 C14 9.7(12) . . . . ?
C11 C12 C13 N2 -2.4(15) . . . . ?
C11 C12 C13 C14 177.3(9) . . . . ?
N2 C13 C14 C19 166.1(8) . . . . ?
C12 C13 C14 C19 -13.6(13) . . . . ?
N2 C13 C14 C15 -19.9(13) . . . . ?
C12 C13 C14 C15 160.4(9) . . . . ?
Pd1 O1 C15 C16 -168.9(7) . . . . ?
Pd1 O1 C15 C14 12.0(13) . . . . ?
C19 C14 C15 O1 -177.2(9) . . . . ?
C13 C14 C15 O1 8.6(15) . . . . ?
C19 C14 C15 C16 3.6(13) . . . . ?
C13 C14 C15 C16 -170.5(9) . . . . ?
O1 C15 C16 C17 176.6(10) . . . . ?
C14 C15 C16 C17 -4.1(15) . . . . ?
C15 C16 C17 C18 1.2(16) . . . . ?
C16 C17 C18 C19 2.1(15) . . . . ?
C17 C18 C19 C14 -2.4(15) . . . . ?
C15 C14 C19 C18 -0.5(14) . . . . ?
C13 C14 C19 C18 173.9(9) . . . . ?
C5 C4 C20 C21 65.1(17) . . . . ?
C3 C4 C20 C21 -113.8(15) . . . . ?
C5 C4 C20 C22 -173.6(13) . . . . ?
C3 C4 C20 C22 7.5(18) . . . . ?
N2A Pd1A O1A C15A -12.9(8) . . . . ?
N3A Pd1A O1A C15A 171.4(8) . . . . ?
N2A Pd1A N1A C7A -4.9(7) . . . . ?
N3A Pd1A N1A C7A 170.9(7) . . . . ?
N2A Pd1A N1A C1A 172.0(8) . . . . ?
N3A Pd1A N1A C1A -12.2(8) . . . . ?
O1A Pd1A N2A C13A 4.4(8) . . . . ?
N1A Pd1A N2A C13A -178.6(8) . . . . ?
O1A Pd1A N2A C9A -170.0(6) . . . . ?
N1A Pd1A N2A C9A 7.1(6) . . . . ?
C7A N1A C1A C2A -107.2(11) . . . . ?
Pd1A N1A C1A C2A 76.2(11) . . . . ?
C7A N1A C1A C6A 78.0(13) . . . . ?
Pd1A N1A C1A C6A -98.7(10) . . . . ?
C6A C1A C2A C3A -2.7(17) . . . . ?
N1A C1A C2A C3A -177.7(10) . . . . ?
C1A C2A C3A C4A 0.2(18) . . . . ?
C2A C3A C4A C5A 2.7(18) . . . . ?
C2A C3A C4A C20A 178.7(11) . . . . ?
C3A C4A C5A C6A -3.0(18) . . . . ?
C20A C4A C5A C6A -179.0(11) . . . . ?
C2A C1A C6A C5A 2.4(16) . . . . ?
N1A C1A C6A C5A 177.2(10) . . . . ?
C4A C5A C6A C1A 0.5(18) . . . . ?
C1A N1A C7A C9A -175.1(8) . . . . ?
Pd1A N1A C7A C9A 1.9(10) . . . . ?
C1A N1A C7A C8A 7.5(14) . . . . ?
Pd1A N1A C7A C8A -175.5(7) . . . . ?
C13A N2A C9A C10A -1.7(13) . . . . ?
Pd1A N2A C9A C10A 173.1(7) . . . . ?
C13A N2A C9A C7A 177.2(8) . . . . ?
Pd1A N2A C9A C7A -8.0(9) . . . . ?
N1A C7A C9A C10A -177.1(9) . . . . ?
C8A C7A C9A C10A 0.4(14) . . . . ?
N1A C7A C9A N2A 4.0(12) . . . . ?
C8A C7A C9A N2A -178.5(8) . . . . ?
N2A C9A C10A C11A -0.4(14) . . . . ?
C7A C9A C10A C11A -179.2(9) . . . . ?
C9A C10A C11A C12A 2.5(15) . . . . ?
C10A C11A C12A C13A -2.5(16) . . . . ?
C9A N2A C13A C12A 1.7(13) . . . . ?
Pd1A N2A C13A C12A -172.3(7) . . . . ?
C9A N2A C13A C14A -178.8(8) . . . . ?
Pd1A N2A C13A C14A 7.1(12) . . . . ?
C11A C12A C13A N2A 0.3(15) . . . . ?
C11A C12A C13A C14A -179.1(9) . . . . ?
N2A C13A C14A C19A 169.4(9) . . . . ?
C12A C13A C14A C19A -11.1(13) . . . . ?
N2A C13A C14A C15A -14.3(14) . . . . ?
C12A C13A C14A C15A 165.2(9) . . . . ?
Pd1A O1A C15A C16A -171.6(7) . . . . ?
Pd1A O1A C15A C14A 10.1(14) . . . . ?
C19A C14A C15A O1A -178.6(9) . . . . ?
C13A C14A C15A O1A 5.0(16) . . . . ?
C19A C14A C15A C16A 3.2(14) . . . . ?
C13A C14A C15A C16A -173.2(9) . . . . ?
O1A C15A C16A C17A 178.7(10) . . . . ?
C14A C15A C16A C17A -2.9(15) . . . . ?
C15A C16A C17A C18A 0.9(17) . . . . ?
C16A C17A C18A C19A 0.9(17) . . . . ?
C17A C18A C19A C14A -0.5(16) . . . . ?
C15A C14A C19A C18A -1.5(15) . . . . ?
C13A C14A C19A C18A 175.0(9) . . . . ?
C5A C4A C20A C21A 65(2) . . . . ?
C3A C4A C20A C21A -110.7(17) . . . . ?
C5A C4A C20A C22A -74.3(16) . . . . ?
C3A C4A C20A C22A 109.9(16) . . . . ?
O4 S1 C25 F2 -174.6(9) . . . . ?
O2 S1 C25 F2 65.1(11) . . . . ?
O3 S1 C25 F2 -56.6(11) . . . . ?
O4 S1 C25 F3 -50.9(12) . . . . ?
O2 S1 C25 F3 -171.3(11) . . . . ?
O3 S1 C25 F3 67.0(12) . . . . ?
O4 S1 C25 F1 65.6(10) . . . . ?
O2 S1 C25 F1 -54.8(11) . . . . ?
O3 S1 C25 F1 -176.5(10) . . . . ?
O6 S2 C26 F6B 54(2) . . . . ?
O7 S2 C26 F6B -77(2) . . . . ?
O5 S2 C26 F6B 170(2) . . . . ?
O6 S2 C26 F5 -64.2(17) . . . . ?
O7 S2 C26 F5 164.8(14) . . . . ?
O5 S2 C26 F5 51.4(17) . . . . ?
O6 S2 C26 F4 -176.4(11) . . . . ?
O7 S2 C26 F4 52.6(14) . . . . ?
O5 S2 C26 F4 -60.9(14) . . . . ?
O6 S2 C26 F6C 75.7(18) . . . . ?
O7 S2 C26 F6C -55.3(19) . . . . ?
O5 S2 C26 F6C -168.7(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.806
_refine_diff_density_min         -2.301
_refine_diff_density_rms         0.177

####################################################################### 
# 
# 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_13087
_database_code_depnum_ccdc_archive 'CCDC 1040527'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H22 N2 O'
_chemical_formula_sum            'C22 H22 N2 O'
_chemical_formula_weight         330.42

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   7.6425(19)
_cell_length_b                   11.027(3)
_cell_length_c                   20.590(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.528(5)
_cell_angle_gamma                90.00
_cell_volume                     1731.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    779
_cell_measurement_theta_min      3.248
_cell_measurement_theta_max      23.467

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   
;
absorption correction based on 4761 reflections(SADABS);Rint 0.1061 before
correction and 0.0393 after.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13311
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.99
_reflns_number_total             3410
_reflns_number_gt                2503
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0533P)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         3410
_refine_ls_number_parameters     229
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1147
_refine_ls_wR_factor_gt          0.1054
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_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
O1 O 0.62667(15) 0.40140(10) 1.08619(6) 0.0366(3) Uani 1 1 d . . .
H1 H 0.5423 0.3580 1.0721 0.055 Uiso 1 1 calc R . .
N1 N 0.46304(17) 0.20729(12) 1.05053(6) 0.0266(3) Uani 1 1 d . . .
N2 N 0.08286(17) 0.17660(12) 0.94895(6) 0.0295(3) Uani 1 1 d . . .
C1 C 0.7592(2) 0.32999(15) 1.10917(7) 0.0299(4) Uani 1 1 d . . .
C2 C 0.9100(2) 0.38479(17) 1.13461(8) 0.0373(4) Uani 1 1 d . . .
H2 H 0.9154 0.4707 1.1375 0.045 Uiso 1 1 calc R . .
C3 C 1.0521(2) 0.31710(18) 1.15580(8) 0.0399(5) Uani 1 1 d . . .
H3 H 1.1549 0.3560 1.1737 0.048 Uiso 1 1 calc R . .
C4 C 1.0465(2) 0.19269(18) 1.15118(8) 0.0405(5) Uani 1 1 d . . .
H4 H 1.1462 0.1454 1.1645 0.049 Uiso 1 1 calc R . .
C5 C 0.8954(2) 0.13777(17) 1.12712(8) 0.0359(4) Uani 1 1 d . . .
H5 H 0.8922 0.0518 1.1241 0.043 Uiso 1 1 calc R . .
C6 C 0.7468(2) 0.20319(15) 1.10707(7) 0.0281(4) Uani 1 1 d . . .
C7 C 0.5843(2) 0.14122(15) 1.08487(7) 0.0264(4) Uani 1 1 d . . .
C8 C 0.5520(2) 0.02067(15) 1.09861(8) 0.0312(4) Uani 1 1 d . . .
H8 H 0.6369 -0.0257 1.1234 0.037 Uiso 1 1 calc R . .
C9 C 0.3976(2) -0.03121(15) 1.07634(8) 0.0313(4) Uani 1 1 d . . .
H9 H 0.3735 -0.1134 1.0864 0.038 Uiso 1 1 calc R . .
C10 C 0.2772(2) 0.03571(14) 1.03939(8) 0.0292(4) Uani 1 1 d . . .
H10 H 0.1704 0.0003 1.0227 0.035 Uiso 1 1 calc R . .
C11 C 0.3149(2) 0.15543(14) 1.02710(7) 0.0266(4) Uani 1 1 d . . .
C12 C 0.1931(2) 0.23272(15) 0.98652(7) 0.0278(4) Uani 1 1 d . . .
C13 C 0.2170(2) 0.36662(15) 0.99182(8) 0.0341(4) Uani 1 1 d . . .
H13A H 0.1330 0.4073 0.9612 0.051 Uiso 1 1 calc R . .
H13B H 0.3366 0.3879 0.9815 0.051 Uiso 1 1 calc R . .
H13C H 0.1969 0.3927 1.0363 0.051 Uiso 1 1 calc R . .
C14 C -0.0448(2) 0.23601(14) 0.90826(8) 0.0278(4) Uani 1 1 d . . .
C15 C -0.0605(2) 0.20383(15) 0.84330(8) 0.0316(4) Uani 1 1 d . . .
H15 H 0.0221 0.1494 0.8266 0.038 Uiso 1 1 calc R . .
C16 C -0.1930(2) 0.24898(15) 0.80259(8) 0.0317(4) Uani 1 1 d . . .
H16 H -0.1985 0.2271 0.7579 0.038 Uiso 1 1 calc R . .
C17 C -0.3187(2) 0.32553(14) 0.82498(7) 0.0282(4) Uani 1 1 d . . .
C18 C -0.3018(2) 0.35814(15) 0.89012(7) 0.0300(4) Uani 1 1 d . . .
H18 H -0.3850 0.4121 0.9068 0.036 Uiso 1 1 calc R . .
C19 C -0.1679(2) 0.31454(14) 0.93126(8) 0.0298(4) Uani 1 1 d . . .
H19 H -0.1599 0.3384 0.9757 0.036 Uiso 1 1 calc R . .
C20 C -0.4705(2) 0.36755(16) 0.78075(8) 0.0348(4) Uani 1 1 d . . .
H20 H -0.4617 0.3258 0.7380 0.042 Uiso 1 1 calc R . .
C21 C -0.6438(2) 0.33080(18) 0.80722(9) 0.0445(5) Uani 1 1 d . . .
H21A H -0.6457 0.2428 0.8136 0.067 Uiso 1 1 calc R . .
H21B H -0.7402 0.3543 0.7762 0.067 Uiso 1 1 calc R . .
H21C H -0.6573 0.3716 0.8489 0.067 Uiso 1 1 calc R . .
C22 C -0.4637(3) 0.50303(16) 0.76841(9) 0.0431(5) Uani 1 1 d . . .
H22A H -0.4737 0.5466 0.8095 0.065 Uiso 1 1 calc R . .
H22B H -0.5610 0.5263 0.7377 0.065 Uiso 1 1 calc R . .
H22C H -0.3522 0.5237 0.7501 0.065 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
O1 C1 1.3455(19) . ?
O1 H1 0.8400 . ?
N1 C11 1.3318(19) . ?
N1 C7 1.3448(19) . ?
N2 C12 1.2692(19) . ?
N2 C14 1.4080(19) . ?
C1 C2 1.376(2) . ?
C1 C6 1.402(2) . ?
C2 C3 1.367(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.370(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.466(2) . ?
C7 C8 1.384(2) . ?
C8 C9 1.365(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.482(2) . ?
C12 C13 1.491(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.382(2) . ?
C14 C19 1.384(2) . ?
C15 C16 1.368(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(2) . ?
C17 C20 1.503(2) . ?
C18 C19 1.374(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.517(2) . ?
C20 C21 1.518(2) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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 O1 H1 109.5 . . ?
C11 N1 C7 120.03(14) . . ?
C12 N2 C14 123.06(15) . . ?
O1 C1 C2 118.13(16) . . ?
O1 C1 C6 121.67(14) . . ?
C2 C1 C6 120.19(15) . . ?
C3 C2 C1 120.80(18) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C2 C3 C4 120.11(17) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.22(17) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 122.31(18) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C1 117.22(15) . . ?
C5 C6 C7 120.86(16) . . ?
C1 C6 C7 121.91(14) . . ?
N1 C7 C8 120.13(15) . . ?
N1 C7 C6 117.04(14) . . ?
C8 C7 C6 122.83(14) . . ?
C9 C8 C7 119.68(15) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 119.79(16) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C11 118.45(15) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
N1 C11 C10 121.84(15) . . ?
N1 C11 C12 116.61(14) . . ?
C10 C11 C12 121.55(14) . . ?
N2 C12 C11 115.71(15) . . ?
N2 C12 C13 126.95(15) . . ?
C11 C12 C13 117.29(14) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 118.14(15) . . ?
C15 C14 N2 118.17(15) . . ?
C19 C14 N2 123.27(15) . . ?
C16 C15 C14 121.10(16) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 121.49(15) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C16 C17 C18 117.16(15) . . ?
C16 C17 C20 120.91(14) . . ?
C18 C17 C20 121.90(15) . . ?
C19 C18 C17 121.80(16) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C14 120.27(15) . . ?
C18 C19 H19 119.9 . . ?
C14 C19 H19 119.9 . . ?
C17 C20 C22 111.84(14) . . ?
C17 C20 C21 110.99(14) . . ?
C22 C20 C21 111.25(16) . . ?
C17 C20 H20 107.5 . . ?
C22 C20 H20 107.5 . . ?
C21 C20 H20 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

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
O1 C1 C2 C3 -176.82(15) . . . . ?
C6 C1 C2 C3 2.6(2) . . . . ?
C1 C2 C3 C4 0.8(3) . . . . ?
C2 C3 C4 C5 -2.1(3) . . . . ?
C3 C4 C5 C6 0.0(3) . . . . ?
C4 C5 C6 C1 3.2(2) . . . . ?
C4 C5 C6 C7 -176.65(15) . . . . ?
O1 C1 C6 C5 174.93(14) . . . . ?
C2 C1 C6 C5 -4.4(2) . . . . ?
O1 C1 C6 C7 -5.2(2) . . . . ?
C2 C1 C6 C7 175.39(15) . . . . ?
C11 N1 C7 C8 -3.1(2) . . . . ?
C11 N1 C7 C6 177.78(14) . . . . ?
C5 C6 C7 N1 -162.77(14) . . . . ?
C1 C6 C7 N1 17.4(2) . . . . ?
C5 C6 C7 C8 18.1(2) . . . . ?
C1 C6 C7 C8 -161.73(15) . . . . ?
N1 C7 C8 C9 0.9(2) . . . . ?
C6 C7 C8 C9 -179.99(15) . . . . ?
C7 C8 C9 C10 1.4(2) . . . . ?
C8 C9 C10 C11 -1.5(2) . . . . ?
C7 N1 C11 C10 3.0(2) . . . . ?
C7 N1 C11 C12 -176.47(13) . . . . ?
C9 C10 C11 N1 -0.6(2) . . . . ?
C9 C10 C11 C12 178.76(14) . . . . ?
C14 N2 C12 C11 178.49(14) . . . . ?
C14 N2 C12 C13 -4.3(3) . . . . ?
N1 C11 C12 N2 159.24(14) . . . . ?
C10 C11 C12 N2 -20.2(2) . . . . ?
N1 C11 C12 C13 -18.3(2) . . . . ?
C10 C11 C12 C13 162.29(15) . . . . ?
C12 N2 C14 C15 129.75(17) . . . . ?
C12 N2 C14 C19 -57.8(2) . . . . ?
C19 C14 C15 C16 0.6(2) . . . . ?
N2 C14 C15 C16 173.38(15) . . . . ?
C14 C15 C16 C17 -1.8(3) . . . . ?
C15 C16 C17 C18 2.1(2) . . . . ?
C15 C16 C17 C20 -175.71(15) . . . . ?
C16 C17 C18 C19 -1.3(2) . . . . ?
C20 C17 C18 C19 176.53(15) . . . . ?
C17 C18 C19 C14 0.1(2) . . . . ?
C15 C14 C19 C18 0.3(2) . . . . ?
N2 C14 C19 C18 -172.14(15) . . . . ?
C16 C17 C20 C22 -114.01(18) . . . . ?
C18 C17 C20 C22 68.2(2) . . . . ?
C16 C17 C20 C21 121.10(18) . . . . ?
C18 C17 C20 C21 -56.6(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N1 0.84 1.81 2.5634(17) 147.5 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.043

####################################################################### 
# 
# 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_12010
_database_code_depnum_ccdc_archive 'CCDC 1040528'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H26 N2 O'
_chemical_formula_sum            'C23 H26 N2 O'
_chemical_formula_weight         346.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.166(6)
_cell_length_b                   16.955(11)
_cell_length_c                   13.033(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.965(11)
_cell_angle_gamma                90.00
_cell_volume                     1974(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    866
_cell_measurement_theta_min      2.403
_cell_measurement_theta_max      28.190

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_process_details   
;
absorption correction based on 6079 reflections(SADABS);Rint 0.0701 before
correction and 0.0320 after.
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13931
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3471
_reflns_number_gt                2725
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0689P)²+0.2751P] 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         3471
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1385
_refine_ls_wR_factor_gt          0.1289
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
O1 O 0.96824(15) 0.08165(8) 0.89502(11) 0.0512(4) Uani 1 1 d . . .
H1 H 0.9228 0.1162 0.8537 0.077 Uiso 1 1 calc R . .
N1 N 0.93250(15) 0.18930(8) 0.75630(11) 0.0344(4) Uani 1 1 d . . .
N2 N 0.59234(17) 0.29836(9) 0.66509(13) 0.0460(4) Uani 1 1 d . . .
H2A H 0.5527 0.3439 0.6713 0.055 Uiso 1 1 d R . .
C1 C 1.1013(2) 0.06569(10) 0.87088(14) 0.0383(4) Uani 1 1 d . . .
C2 C 1.1913(2) 0.00932(11) 0.93203(16) 0.0472(5) Uani 1 1 d . . .
H2 H 1.1570 -0.0170 0.9865 0.057 Uiso 1 1 calc R . .
C3 C 1.3289(2) -0.00834(12) 0.91419(17) 0.0529(5) Uani 1 1 d . . .
H3 H 1.3902 -0.0467 0.9565 0.064 Uiso 1 1 calc R . .
C4 C 1.3791(2) 0.02932(12) 0.83486(18) 0.0563(6) Uani 1 1 d . . .
H4 H 1.4751 0.0172 0.8229 0.068 Uiso 1 1 calc R . .
C5 C 1.2901(2) 0.08452(12) 0.77296(16) 0.0478(5) Uani 1 1 d . . .
H5 H 1.3258 0.1097 0.7182 0.057 Uiso 1 1 calc R . .
C6 C 1.14866(19) 0.10455(10) 0.78853(13) 0.0356(4) Uani 1 1 d . . .
C7 C 1.05723(18) 0.16680(10) 0.72499(13) 0.0344(4) Uani 1 1 d . . .
C8 C 1.0964(2) 0.20388(12) 0.64018(15) 0.0456(5) Uani 1 1 d . . .
H8 H 1.1829 0.1877 0.6171 0.055 Uiso 1 1 calc R . .
C9 C 1.0088(2) 0.26419(13) 0.58998(15) 0.0526(5) Uani 1 1 d . . .
H9 H 1.0351 0.2901 0.5321 0.063 Uiso 1 1 calc R . .
C10 C 0.8834(2) 0.28717(12) 0.62320(15) 0.0471(5) Uani 1 1 d . . .
H10 H 0.8227 0.3291 0.5891 0.057 Uiso 1 1 calc R . .
C11 C 0.84722(19) 0.24799(10) 0.70733(13) 0.0371(4) Uani 1 1 d . . .
C12 C 0.7140(2) 0.27391(11) 0.75201(14) 0.0433(5) Uani 1 1 d . . .
C13 C 0.7635(2) 0.34797(13) 0.81876(17) 0.0582(6) Uani 1 1 d . . .
H13A H 0.7923 0.3892 0.7744 0.087 Uiso 1 1 calc R . .
H13B H 0.8492 0.3350 0.8761 0.087 Uiso 1 1 calc R . .
H13C H 0.6805 0.3669 0.8483 0.087 Uiso 1 1 calc R . .
C14 C 0.50985(18) 0.24905(11) 0.58868(14) 0.0374(4) Uani 1 1 d . . .
C15 C 0.38228(19) 0.27873(11) 0.52046(14) 0.0410(5) Uani 1 1 d . . .
H15 H 0.3559 0.3325 0.5258 0.049 Uiso 1 1 calc R . .
C16 C 0.2942(2) 0.23175(12) 0.44580(14) 0.0441(5) Uani 1 1 d . . .
H16 H 0.2081 0.2542 0.4009 0.053 Uiso 1 1 calc R . .
C17 C 0.3256(2) 0.15338(12) 0.43335(14) 0.0447(5) Uani 1 1 d . . .
C18 C 0.4567(2) 0.12476(12) 0.49780(16) 0.0501(5) Uani 1 1 d . . .
H18 H 0.4848 0.0716 0.4895 0.060 Uiso 1 1 calc R . .
C19 C 0.5479(2) 0.17097(11) 0.57379(15) 0.0457(5) Uani 1 1 d . . .
H19 H 0.6369 0.1493 0.6160 0.055 Uiso 1 1 calc R . .
C20 C 0.2207(2) 0.10157(14) 0.35445(17) 0.0595(6) Uani 1 1 d . . .
H20 H 0.1343 0.1355 0.3199 0.071 Uiso 1 1 calc R . .
C21 C 0.1565(3) 0.03432(15) 0.4075(2) 0.0795(8) Uani 1 1 d . . .
H21A H 0.2375 -0.0012 0.4411 0.119 Uiso 1 1 calc R . .
H21B H 0.0834 0.0051 0.3548 0.119 Uiso 1 1 calc R . .
H21C H 0.1072 0.0557 0.4609 0.119 Uiso 1 1 calc R . .
C22 C 0.2913(3) 0.0720(2) 0.2688(3) 0.1113(12) Uani 1 1 d . . .
H22A H 0.3237 0.1169 0.2321 0.167 Uiso 1 1 calc R . .
H22B H 0.2183 0.0406 0.2188 0.167 Uiso 1 1 calc R . .
H22C H 0.3781 0.0392 0.2995 0.167 Uiso 1 1 calc R . .
C23 C 0.6645(2) 0.21153(13) 0.82228(16) 0.0548(6) Uani 1 1 d . . .
H23A H 0.5745 0.2299 0.8439 0.082 Uiso 1 1 calc R . .
H23B H 0.7449 0.2027 0.8848 0.082 Uiso 1 1 calc R . .
H23C H 0.6423 0.1620 0.7830 0.082 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
O1 C1 1.353(2) . ?
O1 H1 0.8400 . ?
N1 C11 1.336(2) . ?
N1 C7 1.352(2) . ?
N2 C14 1.387(2) . ?
N2 C12 1.460(2) . ?
N2 H2A 0.8648 . ?
C1 C2 1.391(3) . ?
C1 C6 1.409(3) . ?
C2 C3 1.366(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.480(2) . ?
C7 C8 1.387(3) . ?
C8 C9 1.372(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.373(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.530(3) . ?
C12 C23 1.533(3) . ?
C12 C13 1.537(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.394(3) . ?
C14 C15 1.394(2) . ?
C15 C16 1.371(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(3) . ?
C17 C20 1.520(3) . ?
C18 C19 1.386(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.496(4) . ?
C20 C21 1.519(3) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1 109.5 . . ?
C11 N1 C7 120.64(15) . . ?
C14 N2 C12 125.76(15) . . ?
C14 N2 H2A 115.6 . . ?
C12 N2 H2A 116.4 . . ?
O1 C1 C2 117.02(17) . . ?
O1 C1 C6 122.12(16) . . ?
C2 C1 C6 120.86(18) . . ?
C3 C2 C1 120.35(19) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 120.12(19) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 120.05(19) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 121.77(19) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 116.83(17) . . ?
C5 C6 C7 121.27(16) . . ?
C1 C6 C7 121.82(16) . . ?
N1 C7 C8 120.00(16) . . ?
N1 C7 C6 116.31(15) . . ?
C8 C7 C6 123.64(16) . . ?
C9 C8 C7 119.33(18) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 120.18(18) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 118.70(18) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
N1 C11 C10 121.14(17) . . ?
N1 C11 C12 117.61(15) . . ?
C10 C11 C12 121.13(16) . . ?
N2 C12 C11 108.79(15) . . ?
N2 C12 C23 112.47(16) . . ?
C11 C12 C23 113.43(16) . . ?
N2 C12 C13 106.52(16) . . ?
C11 C12 C13 106.90(15) . . ?
C23 C12 C13 108.35(17) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 C19 124.02(16) . . ?
N2 C14 C15 118.97(17) . . ?
C19 C14 C15 117.00(17) . . ?
C16 C15 C14 121.26(18) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 122.61(17) . . ?
C15 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C16 C17 C18 116.15(18) . . ?
C16 C17 C20 121.36(18) . . ?
C18 C17 C20 122.5(2) . . ?
C19 C18 C17 122.37(19) . . ?
C19 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
C18 C19 C14 120.46(17) . . ?
C18 C19 H19 119.8 . . ?
C14 C19 H19 119.8 . . ?
C22 C20 C21 111.4(2) . . ?
C22 C20 C17 112.60(19) . . ?
C21 C20 C17 112.12(19) . . ?
C22 C20 H20 106.8 . . ?
C21 C20 H20 106.8 . . ?
C17 C20 H20 106.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C12 C23 H23A 109.5 . . ?
C12 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C12 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 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
O1 C1 C2 C3 -178.21(17) . . . . ?
C6 C1 C2 C3 1.1(3) . . . . ?
C1 C2 C3 C4 -0.4(3) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
C4 C5 C6 C1 0.1(3) . . . . ?
C4 C5 C6 C7 176.92(18) . . . . ?
O1 C1 C6 C5 178.33(16) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
O1 C1 C6 C7 1.6(3) . . . . ?
C2 C1 C6 C7 -177.71(16) . . . . ?
C11 N1 C7 C8 -1.1(2) . . . . ?
C11 N1 C7 C6 176.40(14) . . . . ?
C5 C6 C7 N1 -170.84(16) . . . . ?
C1 C6 C7 N1 5.8(2) . . . . ?
C5 C6 C7 C8 6.5(3) . . . . ?
C1 C6 C7 C8 -176.86(17) . . . . ?
N1 C7 C8 C9 1.1(3) . . . . ?
C6 C7 C8 C9 -176.16(17) . . . . ?
C7 C8 C9 C10 -0.4(3) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C7 N1 C11 C10 0.3(3) . . . . ?
C7 N1 C11 C12 -175.84(15) . . . . ?
C9 C10 C11 N1 0.5(3) . . . . ?
C9 C10 C11 C12 176.47(18) . . . . ?
C14 N2 C12 C11 68.5(2) . . . . ?
C14 N2 C12 C23 -58.0(2) . . . . ?
C14 N2 C12 C13 -176.58(17) . . . . ?
N1 C11 C12 N2 -146.06(15) . . . . ?
C10 C11 C12 N2 37.8(2) . . . . ?
N1 C11 C12 C23 -20.1(2) . . . . ?
C10 C11 C12 C23 163.82(17) . . . . ?
N1 C11 C12 C13 99.28(19) . . . . ?
C10 C11 C12 C13 -76.8(2) . . . . ?
C12 N2 C14 C19 -11.2(3) . . . . ?
C12 N2 C14 C15 170.09(17) . . . . ?
N2 C14 C15 C16 -177.87(16) . . . . ?
C19 C14 C15 C16 3.3(3) . . . . ?
C14 C15 C16 C17 -0.1(3) . . . . ?
C15 C16 C17 C18 -3.0(3) . . . . ?
C15 C16 C17 C20 176.20(17) . . . . ?
C16 C17 C18 C19 2.8(3) . . . . ?
C20 C17 C18 C19 -176.31(18) . . . . ?
C17 C18 C19 C14 0.3(3) . . . . ?
N2 C14 C19 C18 177.86(18) . . . . ?
C15 C14 C19 C18 -3.4(3) . . . . ?
C16 C17 C20 C22 116.2(3) . . . . ?
C18 C17 C20 C22 -64.7(3) . . . . ?
C16 C17 C20 C21 -117.3(2) . . . . ?
C18 C17 C20 C21 61.8(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N1 0.84 1.79 2.538(2) 147.2 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.037

