# Supplementary Material (ESI) for Chemical Communications

# This journal is © The Royal Society of Chemistry 2003



data_global



_journal_coden_Cambridge         182



loop_

_publ_author_name

'Genevieve Balme'

'Blandine Clique'

'Cedric Couturier'

'Charles-Henry Fabritius'

'Nuno Monteiro'



_publ_contact_author_name        'Dr Genevieve Balme'

_publ_contact_author_address     

;

Laboratoire de Chimie Organique 1

Universite Claude Bernard

CNRS UMR 5622

Lyon 1, CPE.43

bd du 11 Novembre 1918

69622 Villeurbanne

FRANCE

;



_publ_contact_author_email       BALME@UNIV-LYON1.FR



_publ_requested_journal          'Chemical Communications'



_publ_section_title              

;

Unexpected isolation and structural

characterization of a B-hydrogen-containing o-alkylpalladium halide

complex in the course of an intramolecular Heck reaction.  Synthesis of

polycyclic isoquinoline derivatives

;



_publ_section_references         

;

1.Ishibashi, H.; Ito, K.; Hirano, T.; Tabuchi, M.; Ikeda, M.; 

Tetrahedron 1993,49, 4173-4182.

2. Nonius B.V. Collect Software Nonius B.V., Delft, The Netherlands 1997

3. Otwinowski, Z. and Minor, W,: Methods in Enzymology, Academic Press 1997.

4. Sheldrick, G.M.; SHELXL97, Program for Crystal Structure Solution and

Refinement, University of Gottingen, Germany 1997.  

5. Spek A.L.; PLATON, a Multipurpose Crystallographic tool, 

Utrecht University, Utrecht

the Netherland, 1999 

;



data_cf41f2

_database_code_CSD               200107



_publ_section_abstract           

;

The study of the titled structure was undertaken to establish the 

tridimentional structure and bonding of the complex.

;

_publ_section_exptl_prep         

;

Source of material: The title complex was prepared from N-Allyl-2-(1-iodo-

naphtalen-2-yl)-3,3-dimethoxycarbonyl-4-methylenepyrrolidine by intramolecular

Heck reaction using conditions analogous to those reported in [1] .  

;

_publ_section_experimental       

;

Data measured at 273 K on a Nonius Kappa CCD Diffractometer.

detector-crystal distance of 30 mmm; omega rotation scans with 2 deg 

steps; exposure time 1 sec/degre; 149 images collected using Kappa CCD 

Server Software[2]; cell refinement and data reduction with DENZO [3] 

Structure solution and structure refinement with SHELXTL [4]



;

_publ_section_comment            

;

Two molecules of the title compound crystallize with one molecule of

dichloromethane. 

Figure 1 obtained from PLATON[5] shows the

conformation of the molecule .

;

_publ_section_figure_captions    

;

Figure 1 View of the molecule

;

_chemical_name_systematic        

; 

((9-methylene-5,6-dihydro-10,10-dimethoxycarbonyl-benzo(f)

pyrrolidino(2,1-a)isoquinoline-5-methyl)Pd(PPh3)I), C40H37NO4IPPd

;

_chemical_name_common            ?

_chemical_formula_moiety         '(C40 H37 I N O4 P Pd),1/2(C H2 Cl2)'

_chemical_formula_sum            'C40.50 H38 Cl I N O4 P Pd'

_chemical_formula_weight         902.44



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'

P P 0.1023 0.0942 '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'

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

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



_symmetry_cell_setting           Triclinic

_symmetry_space_group_name_H-M   P-1



loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

'-x, -y, -z'



_cell_length_a                   11.291(2)

_cell_length_b                   12.161(2)

_cell_length_c                   15.324(3)

_cell_angle_alpha                86.99(3)

_cell_angle_beta                 78.04(3)

_cell_angle_gamma                68.60(3)

_cell_volume                     1915.8(7)

_cell_formula_units_Z            2

_cell_measurement_temperature    273(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      1

_cell_measurement_theta_max      27.48



_exptl_crystal_description       rhombic

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.7

_exptl_crystal_size_mid          0.4

_exptl_crystal_size_min          0.1

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.564

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             902

_exptl_absorpt_coefficient_mu    1.442

_exptl_absorpt_correction_type   none

_exptl_absorpt_correction_T_min  ?

_exptl_absorpt_correction_T_max  ?

_exptl_absorpt_process_details   ?



_exptl_special_details           

; 

Data measured at 273 K on a Nonius Kappa CCD Diffractometer.

detector-crystal distance of 30 mmm; omega rotation scans with 2 deg 

steps; exposure time 1 sec/degre; 149 images collected.

The hydrogen atoms of the dichloromethane were not localized.

;

_diffrn_ambient_temperature      273(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  'Nonius Kappa CCD diffractometer'

_diffrn_measurement_method       'area detector'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            22340

_diffrn_reflns_av_R_equivalents  0.1260

_diffrn_reflns_av_sigmaI/netI    0.1044

_diffrn_reflns_limit_h_min       -14

_diffrn_reflns_limit_h_max       14

_diffrn_reflns_limit_k_min       -15

_diffrn_reflns_limit_k_max       14

_diffrn_reflns_limit_l_min       -19

_diffrn_reflns_limit_l_max       19

_diffrn_reflns_theta_min         1.36

_diffrn_reflns_theta_max         27.50

_reflns_number_total             8721

_reflns_number_gt                6175

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Kappa CCD Server Software (Nonius, 1997)'

_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'

_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'

_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'

_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'

_computing_molecular_graphics    'PLATON (Spek, 1999)'

_computing_publication_material  'SHELXTL (Sheldrick, 1997)'



_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)+(0.0884P)²+0.1549P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    mixed

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         8721

_refine_ls_number_parameters     451

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0873

_refine_ls_R_factor_gt           0.0572

_refine_ls_wR_factor_ref         0.1757

_refine_ls_wR_factor_gt          0.1506

_refine_ls_goodness_of_fit_ref   1.045

_refine_ls_restrained_S_all      1.045

_refine_ls_shift/su_max          0.026

_refine_ls_shift/su_mean         0.001



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 0.60411(3) 0.38000(3) 0.18018(2) 0.03190(13) Uani 1 1 d . . .

I1 I 0.77495(4) 0.44052(3) 0.25048(3) 0.04942(15) Uani 1 1 d . . .

P3 P 0.45045(13) 0.56058(12) 0.20248(9) 0.0364(3) Uani 1 1 d . . .

N1 N 0.7310(4) 0.1938(4) 0.1631(3) 0.0330(9) Uani 1 1 d . . .

O31 O 0.8615(4) 0.0618(4) 0.3882(3) 0.0550(11) Uani 1 1 d . . .

O35 O 1.0013(4) -0.1041(4) 0.3171(3) 0.0551(11) Uani 1 1 d . . .

O34 O 0.7560(5) -0.1282(4) 0.3087(3) 0.0608(12) Uani 1 1 d . . .

O32 O 0.8057(5) -0.1328(4) 0.1595(3) 0.0664(13) Uani 1 1 d . . .

C35 C 1.0672(7) -0.1332(7) 0.3908(5) 0.0689(19) Uani 1 1 d . . .

H35A H 1.1382 -0.2076 0.3784 0.103 Uiso 1 1 calc R . .

H35B H 1.0076 -0.1388 0.4439 0.103 Uiso 1 1 calc R . .

H35C H 1.0999 -0.0728 0.3993 0.103 Uiso 1 1 calc R . .

C4 C 0.7195(5) 0.1351(4) 0.2516(3) 0.0334(10) Uani 1 1 d . . .

H4 H 0.7322 0.1847 0.2945 0.040 Uiso 1 1 calc R . .

C61 C 0.2951(5) 0.5830(4) 0.1717(4) 0.0405(12) Uani 1 1 d . . .

C12 C 0.6769(5) 0.1428(5) 0.1011(3) 0.0373(11) Uani 1 1 d . . .

H12A H 0.7114 0.0571 0.1020 0.045 Uiso 1 1 calc R . .

H12B H 0.6981 0.1674 0.0405 0.045 Uiso 1 1 calc R . .

C1 C 0.8733(5) 0.1596(5) 0.1333(4) 0.0430(12) Uani 1 1 d . . .

H1A H 0.9042 0.2105 0.1616 0.052 Uiso 1 1 calc R . .

H1B H 0.8959 0.1659 0.0691 0.052 Uiso 1 1 calc R . .

C5 C 0.5858(5) 0.1307(4) 0.2854(3) 0.0349(11) Uani 1 1 d . . .

C10 C 0.4976(5) 0.1563(4) 0.2303(4) 0.0358(11) Uani 1 1 d . . .

C9 C 0.3678(5) 0.1597(5) 0.2670(4) 0.0453(13) Uani 1 1 d . . .

C41 C 0.4901(6) 0.6824(5) 0.1466(4) 0.0438(13) Uani 1 1 d . . .

C31 C 0.8999(5) -0.0030(5) 0.3249(4) 0.0418(12) Uani 1 1 d . . .

C62 C 0.2892(6) 0.5923(5) 0.0817(4) 0.0510(14) Uani 1 1 d . . .

H62 H 0.3612 0.5930 0.0396 0.061 Uiso 1 1 calc R . .

C32 C 0.8002(5) -0.0916(5) 0.2299(4) 0.0459(13) Uani 1 1 d . . .

C11 C 0.5309(5) 0.1905(5) 0.1358(3) 0.0382(11) Uani 1 1 d . . .

H11 H 0.4904 0.1575 0.0986 0.046 Uiso 1 1 calc R . .

C2 C 0.9315(5) 0.0354(5) 0.1599(4) 0.0443(13) Uani 1 1 d . . .

C3 C 0.8384(5) 0.0156(4) 0.2423(4) 0.0378(11) Uani 1 1 d . . .

C66 C 0.1864(6) 0.5835(7) 0.2325(4) 0.0618(18) Uani 1 1 d . . .

H66 H 0.1878 0.5781 0.2931 0.074 Uiso 1 1 calc R . .

C6 C 0.5520(6) 0.1045(5) 0.3751(4) 0.0460(13) Uani 1 1 d . . .

H6 H 0.6132 0.0874 0.4110 0.055 Uiso 1 1 calc R . .

C7 C 0.4317(6) 0.1036(6) 0.4108(4) 0.0600(17) Uani 1 1 d . . .

H7 H 0.4121 0.0852 0.4704 0.072 Uiso 1 1 calc R . .

C51 C 0.4088(6) 0.5984(6) 0.3218(4) 0.0517(15) Uani 1 1 d . . .

C52 C 0.4061(7) 0.7037(7) 0.3553(4) 0.0652(19) Uani 1 1 d . . .

H52 H 0.4279 0.7575 0.3160 0.078 Uiso 1 1 calc R . .

C8 C 0.3363(6) 0.1303(6) 0.3584(5) 0.0584(16) Uani 1 1 d . . .

C43 C 0.6475(8) 0.7596(7) 0.0623(5) 0.067(2) Uani 1 1 d . . .

H43 H 0.7314 0.7466 0.0307 0.081 Uiso 1 1 calc R . .

C46 C 0.3970(8) 0.7961(5) 0.1522(5) 0.0633(18) Uani 1 1 d . . .

H46 H 0.3118 0.8090 0.1807 0.076 Uiso 1 1 calc R . .

C42 C 0.6154(7) 0.6656(5) 0.1011(4) 0.0496(14) Uani 1 1 d . . .

H42 H 0.6790 0.5903 0.0964 0.059 Uiso 1 1 calc R . .

C56 C 0.3808(8) 0.5176(8) 0.3814(4) 0.078(2) Uani 1 1 d . . .

H56 H 0.3849 0.4454 0.3609 0.094 Uiso 1 1 calc R . .

C63 C 0.1772(7) 0.6003(6) 0.0542(5) 0.0583(16) Uani 1 1 d . . .

H63 H 0.1752 0.6052 -0.0063 0.070 Uiso 1 1 calc R . .

C45 C 0.4298(11) 0.8903(6) 0.1158(6) 0.083(3) Uani 1 1 d . . .

H45 H 0.3680 0.9665 0.1213 0.100 Uiso 1 1 calc R . .

C44 C 0.5578(11) 0.8688(7) 0.0706(6) 0.082(3) Uani 1 1 d . . .

H44 H 0.5807 0.9316 0.0460 0.099 Uiso 1 1 calc R . .

C64 C 0.0704(8) 0.6012(7) 0.1142(6) 0.079(2) Uani 1 1 d . . .

H64 H -0.0051 0.6079 0.0954 0.095 Uiso 1 1 calc R . .

C15 C 0.2688(6) 0.1938(6) 0.2170(5) 0.0607(17) Uani 1 1 d . . .

H15 H 0.2868 0.2136 0.1576 0.073 Uiso 1 1 calc R . .

C34 C 0.6995(9) -0.2173(7) 0.3077(6) 0.087(3) Uani 1 1 d . . .

H34A H 0.6708 -0.2370 0.3679 0.131 Uiso 1 1 calc R . .

H34B H 0.7635 -0.2867 0.2761 0.131 Uiso 1 1 calc R . .

H34C H 0.6269 -0.1875 0.2786 0.131 Uiso 1 1 calc R . .

C54 C 0.3406(9) 0.6534(11) 0.5011(6) 0.098(3) Uani 1 1 d . . .

H54 H 0.3137 0.6734 0.5616 0.117 Uiso 1 1 calc R . .

C55 C 0.3464(9) 0.5454(11) 0.4726(5) 0.098(3) Uani 1 1 d . . .

H55 H 0.3276 0.4919 0.5136 0.117 Uiso 1 1 calc R . .

C16 C 0.1463(7) 0.1979(8) 0.2557(7) 0.082(3) Uani 1 1 d . . .

H16 H 0.0814 0.2225 0.2224 0.099 Uiso 1 1 calc R . .

C17 C 0.1178(8) 0.1664(9) 0.3425(8) 0.094(3) Uani 1 1 d . . .

H17 H 0.0345 0.1680 0.3668 0.113 Uiso 1 1 calc R . .

C18 C 0.2088(7) 0.1333(8) 0.3929(6) 0.084(2) Uani 1 1 d . . .

H18 H 0.1876 0.1119 0.4516 0.101 Uiso 1 1 calc R . .

C53 C 0.3722(8) 0.7294(9) 0.4447(5) 0.085(3) Uani 1 1 d . . .

H53 H 0.3712 0.8000 0.4660 0.103 Uiso 1 1 calc R . .

C65 C 0.0749(7) 0.5919(9) 0.2039(6) 0.088(3) Uani 1 1 d . . .

H65 H 0.0022 0.5914 0.2454 0.105 Uiso 1 1 calc R . .

C110 C 0.4807(5) 0.3247(4) 0.1277(4) 0.0409(12) Uani 1 1 d . . .

H11A H 0.3922 0.3597 0.1610 0.049 Uiso 1 1 calc R . .

H11B H 0.4827 0.3464 0.0657 0.049 Uiso 1 1 calc R . .

C20 C 1.0403(7) -0.0437(7) 0.1191(5) 0.0650(18) Uani 1 1 d . . .

H20A H 1.0889 -0.0239 0.0682 0.078 Uiso 1 1 calc R . .

H20B H 1.0692 -0.1197 0.1409 0.078 Uiso 1 1 calc R . .

Cl1S Cl -0.0606(6) 0.6050(5) 0.4562(4) 0.210(2) Uani 1 1 d . . .

C1S C 0.021(4) 0.446(2) 0.4493(14) 0.161(13) Uani 0.50 1 d P . .






_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 C110 2.061(5) . ?

Pd1 N1 2.188(4) . ?

Pd1 P3 2.2365(16) . ?

Pd1 I1 2.7210(8) . ?

P3 C41 1.822(6) . ?

P3 C51 1.829(5) . ?

P3 C61 1.832(6) . ?

N1 C1 1.479(6) . ?

N1 C12 1.497(6) . ?

N1 C4 1.504(6) . ?

O31 C31 1.187(6) . ?

O35 C31 1.330(7) . ?

O35 C35 1.438(7) . ?

O34 C32 1.326(7) . ?

O34 C34 1.447(7) . ?

O32 C32 1.194(7) . ?

C4 C5 1.511(7) . ?

C4 C3 1.566(7) . ?

C61 C66 1.377(8) . ?

C61 C62 1.392(8) . ?

C12 C11 1.519(7) . ?

C1 C2 1.485(8) . ?

C5 C10 1.377(7) . ?

C5 C6 1.400(7) . ?

C10 C9 1.444(7) . ?

C10 C11 1.496(7) . ?

C9 C15 1.411(9) . ?

C9 C8 1.432(9) . ?

C41 C42 1.388(9) . ?

C41 C46 1.392(8) . ?

C31 C3 1.533(8) . ?

C62 C63 1.383(9) . ?

C32 C3 1.547(7) . ?

C11 C110 1.527(7) . ?

C2 C20 1.307(8) . ?

C2 C3 1.536(8) . ?

C66 C65 1.385(10) . ?

C6 C7 1.359(8) . ?

C7 C8 1.409(10) . ?

C51 C56 1.383(10) . ?

C51 C52 1.393(10) . ?

C52 C53 1.365(9) . ?

C8 C18 1.414(9) . ?

C43 C44 1.337(12) . ?

C43 C42 1.390(9) . ?

C46 C45 1.385(11) . ?

C56 C55 1.395(10) . ?

C63 C64 1.353(11) . ?

C45 C44 1.401(13) . ?

C64 C65 1.383(11) . ?

C15 C16 1.372(10) . ?

C54 C53 1.325(14) . ?

C54 C55 1.381(15) . ?

C16 C17 1.370(12) . ?

C17 C18 1.346(12) . ?

Cl1S C1S 1.63(3) 2_566 ?

Cl1S C1S 1.81(3) . ?

C1S Cl1S 1.63(3) 2_566 ?

C1S C1S 1.96(4) 2_566 ?



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

C110 Pd1 N1 83.91(18) . . ?

C110 Pd1 P3 89.25(15) . . ?

N1 Pd1 P3 171.63(11) . . ?

C110 Pd1 I1 176.89(15) . . ?

N1 Pd1 I1 93.05(11) . . ?

P3 Pd1 I1 93.73(5) . . ?

C41 P3 C51 105.7(3) . . ?

C41 P3 C61 101.4(3) . . ?

C51 P3 C61 104.8(3) . . ?

C41 P3 Pd1 117.4(2) . . ?

C51 P3 Pd1 108.7(2) . . ?

C61 P3 Pd1 117.61(17) . . ?

C1 N1 C12 110.7(4) . . ?

C1 N1 C4 102.4(4) . . ?

C12 N1 C4 108.9(4) . . ?

C1 N1 Pd1 120.8(3) . . ?

C12 N1 Pd1 104.7(3) . . ?

C4 N1 Pd1 108.9(3) . . ?

C31 O35 C35 116.4(5) . . ?

C32 O34 C34 116.5(6) . . ?

N1 C4 C5 112.5(4) . . ?

N1 C4 C3 106.6(4) . . ?

C5 C4 C3 117.7(4) . . ?

C66 C61 C62 118.4(6) . . ?

C66 C61 P3 123.3(5) . . ?

C62 C61 P3 118.2(4) . . ?

N1 C12 C11 105.2(4) . . ?

N1 C1 C2 106.2(4) . . ?

C10 C5 C6 120.8(5) . . ?

C10 C5 C4 120.8(4) . . ?

C6 C5 C4 118.3(5) . . ?

C5 C10 C9 119.0(5) . . ?

C5 C10 C11 121.0(4) . . ?

C9 C10 C11 119.8(5) . . ?

C15 C9 C8 118.2(5) . . ?

C15 C9 C10 122.7(6) . . ?

C8 C9 C10 119.1(5) . . ?

C42 C41 C46 118.1(6) . . ?

C42 C41 P3 120.9(4) . . ?

C46 C41 P3 120.9(5) . . ?

O31 C31 O35 124.0(5) . . ?

O31 C31 C3 125.3(5) . . ?

O35 C31 C3 110.7(4) . . ?

C63 C62 C61 120.6(6) . . ?

O32 C32 O34 125.0(5) . . ?

O32 C32 C3 124.8(6) . . ?

O34 C32 C3 110.1(5) . . ?

C10 C11 C12 111.0(4) . . ?

C10 C11 C110 110.9(4) . . ?

C12 C11 C110 108.5(4) . . ?

C20 C2 C1 126.2(6) . . ?

C20 C2 C3 126.3(6) . . ?

C1 C2 C3 107.5(4) . . ?

C31 C3 C2 110.4(4) . . ?

C31 C3 C32 108.8(5) . . ?

C2 C3 C32 112.5(4) . . ?

C31 C3 C4 110.4(4) . . ?

C2 C3 C4 102.3(4) . . ?

C32 C3 C4 112.2(4) . . ?

C61 C66 C65 120.3(7) . . ?

C7 C6 C5 121.4(6) . . ?

C6 C7 C8 120.7(6) . . ?

C56 C51 C52 118.6(6) . . ?

C56 C51 P3 118.4(6) . . ?

C52 C51 P3 123.1(5) . . ?

C53 C52 C51 121.1(8) . . ?

C7 C8 C18 122.8(7) . . ?

C7 C8 C9 118.9(5) . . ?

C18 C8 C9 118.3(7) . . ?

C44 C43 C42 120.0(8) . . ?

C45 C46 C41 120.8(8) . . ?

C41 C42 C43 121.1(7) . . ?

C51 C56 C55 119.4(9) . . ?

C64 C63 C62 120.9(6) . . ?

C46 C45 C44 118.9(8) . . ?

C43 C44 C45 121.1(7) . . ?

C63 C64 C65 119.2(7) . . ?

C16 C15 C9 120.3(7) . . ?

C53 C54 C55 121.9(8) . . ?

C54 C55 C56 119.0(9) . . ?

C17 C16 C15 121.2(8) . . ?

C18 C17 C16 120.8(7) . . ?

C17 C18 C8 121.2(8) . . ?

C54 C53 C52 119.8(9) . . ?

C64 C65 C66 120.7(7) . . ?

C11 C110 Pd1 105.3(3) . . ?

C1S Cl1S C1S 69.1(11) 2_566 . ?

Cl1S C1S Cl1S 110.9(11) 2_566 . ?

Cl1S C1S C1S 60.0(14) 2_566 2_566 ?

Cl1S C1S C1S 51.0(12) . 2_566 ?



_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        27.50

_diffrn_measured_fraction_theta_full 0.992

_refine_diff_density_max         1.412

_refine_diff_density_min         -1.143

_refine_diff_density_rms         0.160







