# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2011


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Bluemel, Janet'
_publ_contact_author_email       bluemel@tamu.edu

_publ_section_title              
;
Immobilized Sonogashira Catalyst Systems:
New Insights by Multinuclear HRMAS NMR Studies
;
loop_
_publ_author_name
T.Posset
J.Guenther
J.Pope
T.Oeser
J.Blumel

# Attachment '- tp6.cif'

data_tp6
_database_code_depnum_ccdc_archive 'CCDC 795029'
#TrackingRef '- tp6.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Dichloro-palladium-complex
;
_chemical_name_common            Dichloro-palladium-complex
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H49 Cl6 N O3 P2 Pd Si'
_chemical_formula_weight         964.90

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'
Si Si 0.0817 0.0704 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   11.2996(7)
_cell_length_b                   13.4269(8)
_cell_length_c                   28.789(2)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     4367.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9710
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      28.23

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7494
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            46007
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.028
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         28.32
_reflns_number_total             10832
_reflns_number_gt                10292
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0374P)^2^+3.0318P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(18)
_refine_ls_number_reflns         10832
_refine_ls_number_parameters     489
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.771291(18) 0.104201(14) 0.978568(7) 0.01565(5) Uani 1 1 d . . .
Cl1 Cl 0.88543(6) 0.00195(5) 1.02708(3) 0.02429(14) Uani 1 1 d . . .
Cl2 Cl 0.94265(6) 0.15551(5) 0.93808(3) 0.02175(14) Uani 1 1 d . . .
Si1 Si 0.25056(8) 0.04739(7) 0.81110(3) 0.0296(2) Uani 1 1 d . A .
P1 P 0.61091(6) 0.03810(5) 1.01263(2) 0.01704(14) Uani 1 1 d . . .
P2 P 0.66341(6) 0.19430(5) 0.92831(3) 0.01673(14) Uani 1 1 d . . .
O1 O 0.2525(2) 0.1547(2) 0.78476(8) 0.0412(6) Uani 1 1 d D . .
O2 O 0.3080(2) -0.0307(2) 0.77446(9) 0.0433(7) Uani 1 1 d . . .
O3 O 0.1141(2) 0.01832(19) 0.82457(8) 0.0331(5) Uani 1 1 d . . .
N1 N 0.4467(2) 0.12489(17) 0.95564(9) 0.0191(5) Uani 1 1 d . . .
C1 C 0.4715(2) 0.1045(2) 1.00476(9) 0.0194(5) Uani 1 1 d . . .
H1A H 0.4062 0.0641 1.0179 0.023 Uiso 1 1 calc R . .
H1B H 0.4746 0.1682 1.0220 0.023 Uiso 1 1 calc R . .
C2 C 0.5062(2) 0.2162(2) 0.94142(10) 0.0197(5) Uani 1 1 d . . .
H2A H 0.4996 0.2662 0.9666 0.024 Uiso 1 1 calc R . .
H2B H 0.4665 0.2435 0.9135 0.024 Uiso 1 1 calc R . .
C3 C 0.3176(2) 0.1320(2) 0.94825(10) 0.0208(6) Uani 1 1 d . . .
H3A H 0.2878 0.1917 0.9647 0.025 Uiso 1 1 calc R . .
H3B H 0.2794 0.0731 0.9625 0.025 Uiso 1 1 calc R . .
C4 C 0.2805(3) 0.1381(2) 0.89773(10) 0.0225(6) Uani 1 1 d . A .
H4A H 0.3099 0.2016 0.8845 0.027 Uiso 1 1 calc R . .
H4B H 0.1930 0.1392 0.8961 0.027 Uiso 1 1 calc R . .
C5 C 0.3265(3) 0.0515(2) 0.86781(11) 0.0254(6) Uani 1 1 d . . .
H5A H 0.3135 -0.0121 0.8844 0.030 Uiso 1 1 calc R A .
H5B H 0.4127 0.0595 0.8628 0.030 Uiso 1 1 calc R . .
C11 C 0.6199(3) 0.0312(2) 1.07555(10) 0.0217(6) Uani 1 1 d . . .
C12 C 0.6302(3) 0.1202(2) 1.10033(11) 0.0276(7) Uani 1 1 d . . .
H12 H 0.6322 0.1819 1.0842 0.033 Uiso 1 1 calc R . .
C13 C 0.6376(3) 0.1187(3) 1.14847(12) 0.0350(8) Uani 1 1 d . . .
H13 H 0.6457 0.1792 1.1653 0.042 Uiso 1 1 calc R . .
C14 C 0.6330(3) 0.0277(3) 1.17205(12) 0.0352(8) Uani 1 1 d . . .
H14 H 0.6381 0.0263 1.2050 0.042 Uiso 1 1 calc R . .
C15 C 0.6212(3) -0.0593(3) 1.14780(12) 0.0347(8) Uani 1 1 d . . .
H15 H 0.6164 -0.1206 1.1642 0.042 Uiso 1 1 calc R . .
C16 C 0.6161(3) -0.0595(2) 1.09940(12) 0.0278(7) Uani 1 1 d . . .
H16 H 0.6102 -0.1204 1.0828 0.033 Uiso 1 1 calc R . .
C21 C 0.5828(3) -0.0861(2) 0.99074(10) 0.0206(6) Uani 1 1 d . . .
C22 C 0.4717(3) -0.1323(2) 0.99762(13) 0.0290(7) Uani 1 1 d . . .
H22 H 0.4126 -0.0997 1.0155 0.035 Uiso 1 1 calc R . .
C23 C 0.4488(3) -0.2246(2) 0.97845(14) 0.0319(7) Uani 1 1 d . . .
H23 H 0.3742 -0.2554 0.9835 0.038 Uiso 1 1 calc R . .
C24 C 0.5333(3) -0.2722(2) 0.95216(13) 0.0310(7) Uani 1 1 d . . .
H24 H 0.5163 -0.3350 0.9385 0.037 Uiso 1 1 calc R . .
C25 C 0.6434(3) -0.2284(2) 0.94558(13) 0.0315(7) Uani 1 1 d . . .
H25 H 0.7018 -0.2614 0.9275 0.038 Uiso 1 1 calc R . .
C26 C 0.6680(3) -0.1362(2) 0.96542(11) 0.0263(7) Uani 1 1 d . . .
H26 H 0.7441 -0.1074 0.9615 0.032 Uiso 1 1 calc R . .
C31 C 0.6595(3) 0.1302(2) 0.87276(10) 0.0214(6) Uani 1 1 d . . .
C32 C 0.6962(3) 0.0322(3) 0.86997(12) 0.0344(8) Uani 1 1 d . . .
H32 H 0.7312 0.0009 0.8962 0.041 Uiso 1 1 calc R . .
C33 C 0.6817(4) -0.0210(3) 0.82859(14) 0.0473(10) Uani 1 1 d . . .
H33 H 0.7061 -0.0886 0.8268 0.057 Uiso 1 1 calc R . .
C34 C 0.6322(4) 0.0245(4) 0.79047(14) 0.0483(11) Uani 1 1 d . . .
H34 H 0.6217 -0.0118 0.7625 0.058 Uiso 1 1 calc R . .
C35 C 0.5980(3) 0.1228(3) 0.79297(13) 0.0420(10) Uani 1 1 d . . .
H35 H 0.5660 0.1546 0.7663 0.050 Uiso 1 1 calc R . .
C36 C 0.6100(3) 0.1755(3) 0.83398(11) 0.0315(7) Uani 1 1 d . . .
H36 H 0.5842 0.2428 0.8356 0.038 Uiso 1 1 calc R . .
C41 C 0.7142(2) 0.3207(2) 0.91703(10) 0.0194(5) Uani 1 1 d . . .
C42 C 0.7920(3) 0.3407(2) 0.88051(11) 0.0255(6) Uani 1 1 d . . .
H42 H 0.8208 0.2877 0.8618 0.031 Uiso 1 1 calc R . .
C43 C 0.8275(3) 0.4381(2) 0.87150(12) 0.0297(7) Uani 1 1 d . . .
H43 H 0.8798 0.4517 0.8465 0.036 Uiso 1 1 calc R . .
C44 C 0.7860(3) 0.5155(2) 0.89926(12) 0.0307(7) Uani 1 1 d . . .
H44 H 0.8098 0.5820 0.8931 0.037 Uiso 1 1 calc R . .
C45 C 0.7104(3) 0.4958(2) 0.93574(12) 0.0258(6) Uani 1 1 d . . .
H45 H 0.6827 0.5489 0.9546 0.031 Uiso 1 1 calc R . .
C46 C 0.6744(2) 0.3987(2) 0.94506(10) 0.0213(5) Uani 1 1 d . . .
H46 H 0.6230 0.3854 0.9704 0.026 Uiso 1 1 calc R . .
C51 C 0.3012(4) 0.1823(4) 0.74113(16) 0.0433(11) Uani 0.85 1 d PD A 1
H51A H 0.3538 0.1284 0.7299 0.052 Uiso 0.85 1 calc PR A 1
H51B H 0.3496 0.2432 0.7450 0.052 Uiso 0.85 1 calc PR A 1
C52 C 0.2072(6) 0.2011(5) 0.70587(18) 0.0609(16) Uani 0.85 1 d PD A 1
H52A H 0.1646 0.1390 0.6995 0.091 Uiso 0.85 1 calc PR A 1
H52B H 0.2435 0.2256 0.6771 0.091 Uiso 0.85 1 calc PR A 1
H52C H 0.1518 0.2510 0.7178 0.091 Uiso 0.85 1 calc PR A 1
C51A C 0.257(3) 0.136(2) 0.7351(6) 0.053(8) Uiso 0.15 1 d PD A 2
H51C H 0.1837 0.1045 0.7237 0.063 Uiso 0.15 1 calc PR A 2
H51D H 0.3259 0.0936 0.7268 0.063 Uiso 0.15 1 calc PR A 2
C52A C 0.271(4) 0.238(2) 0.7170(13) 0.069(9) Uiso 0.15 1 d PD A 2
H52D H 0.1950 0.2730 0.7189 0.103 Uiso 0.15 1 calc PR A 2
H52E H 0.2969 0.2352 0.6845 0.103 Uiso 0.15 1 calc PR A 2
H52F H 0.3302 0.2738 0.7354 0.103 Uiso 0.15 1 calc PR A 2
C53 C 0.3278(5) -0.1322(3) 0.78462(18) 0.0588(13) Uani 1 1 d . A .
H53A H 0.3452 -0.1395 0.8182 0.071 Uiso 1 1 calc R . .
H53B H 0.3978 -0.1558 0.7671 0.071 Uiso 1 1 calc R . .
C54 C 0.2254(6) -0.1942(4) 0.7727(2) 0.0769(16) Uani 1 1 d . . .
H54A H 0.1598 -0.1791 0.7938 0.115 Uiso 1 1 calc R A .
H54B H 0.2467 -0.2647 0.7756 0.115 Uiso 1 1 calc R . .
H54C H 0.2011 -0.1804 0.7406 0.115 Uiso 1 1 calc R . .
C55 C 0.0176(3) 0.0233(3) 0.79286(14) 0.0399(9) Uani 1 1 d . A .
H55A H -0.0371 -0.0329 0.7986 0.048 Uiso 1 1 calc R . .
H55B H 0.0475 0.0175 0.7607 0.048 Uiso 1 1 calc R . .
C56 C -0.0486(4) 0.1211(3) 0.79840(16) 0.0493(11) Uani 1 1 d . . .
H56A H -0.0708 0.1302 0.8310 0.074 Uiso 1 1 calc R A .
H56B H -0.1202 0.1200 0.7791 0.074 Uiso 1 1 calc R . .
H56C H 0.0023 0.1763 0.7886 0.074 Uiso 1 1 calc R . .
Cl61 Cl -0.05818(9) 0.82137(8) 0.88973(4) 0.0445(2) Uani 1 1 d . . .
Cl62 Cl 0.17039(8) 0.84463(7) 0.93537(4) 0.0441(2) Uani 1 1 d . . .
C60 C 0.0356(3) 0.9037(3) 0.92080(12) 0.0324(7) Uani 1 1 d . . .
H60A H 0.0520 0.9632 0.9016 0.039 Uiso 1 1 calc R . .
H60B H -0.0047 0.9258 0.9495 0.039 Uiso 1 1 calc R . .
C70 C 0.4435(7) 0.5173(8) 0.8608(3) 0.0355(18) Uani 0.50 1 d P B 1
H70A H 0.4906 0.5135 0.8897 0.043 Uiso 0.50 1 calc PR B 1
H70B H 0.3625 0.4932 0.8676 0.043 Uiso 0.50 1 calc PR B 1
Cl71 Cl 0.4383(5) 0.6410(3) 0.84074(19) 0.0594(10) Uani 0.50 1 d P B 1
Cl72 Cl 0.5084(3) 0.4435(3) 0.81765(12) 0.0791(8) Uiso 0.50 1 d P B 1
Cl73 Cl 0.4303(2) 0.3876(2) 0.82014(7) 0.0627(7) Uani 0.50 1 d P C 2
Cl74 Cl 0.4505(7) 0.5987(4) 0.8360(2) 0.0820(17) Uani 0.50 1 d P C 2
C70A C 0.4402(18) 0.4727(12) 0.8582(7) 0.098(7) Uiso 0.50 1 d P C 2
H70C H 0.5109 0.4595 0.8775 0.117 Uiso 0.50 1 calc PR C 2
H70D H 0.3701 0.4685 0.8787 0.117 Uiso 0.50 1 calc PR C 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01357(8) 0.01334(8) 0.02004(9) 0.00018(8) -0.00046(8) -0.00006(7)
Cl1 0.0187(3) 0.0244(3) 0.0298(4) 0.0058(3) -0.0038(3) 0.0039(3)
Cl2 0.0167(3) 0.0192(3) 0.0294(4) 0.0002(3) 0.0036(3) -0.0008(2)
Si1 0.0254(5) 0.0401(5) 0.0234(4) -0.0048(4) -0.0006(3) -0.0019(4)
P1 0.0155(3) 0.0139(3) 0.0217(4) 0.0020(3) 0.0003(3) -0.0003(2)
P2 0.0141(3) 0.0163(3) 0.0197(3) 0.0011(3) 0.0003(3) -0.0007(3)
O1 0.0423(16) 0.0526(15) 0.0287(12) 0.0049(11) -0.0010(11) -0.0047(12)
O2 0.0379(15) 0.0543(17) 0.0378(15) -0.0163(12) 0.0048(11) -0.0004(13)
O3 0.0226(11) 0.0481(15) 0.0287(12) -0.0023(11) -0.0050(9) -0.0040(11)
N1 0.0141(11) 0.0183(12) 0.0249(12) 0.0049(9) -0.0021(9) 0.0004(9)
C1 0.0161(12) 0.0195(12) 0.0227(13) 0.0029(12) 0.0016(10) 0.0041(11)
C2 0.0149(13) 0.0176(13) 0.0267(15) 0.0035(11) 0.0015(11) 0.0010(10)
C3 0.0136(12) 0.0243(14) 0.0245(14) -0.0014(11) -0.0006(11) -0.0011(10)
C4 0.0168(13) 0.0246(13) 0.0261(14) -0.0004(11) -0.0017(12) 0.0008(12)
C5 0.0211(15) 0.0302(16) 0.0249(15) -0.0026(12) 0.0008(12) 0.0014(12)
C11 0.0171(13) 0.0263(14) 0.0219(14) 0.0025(11) 0.0002(11) 0.0001(11)
C12 0.0280(16) 0.0253(16) 0.0297(16) 0.0048(12) -0.0017(12) -0.0035(12)
C13 0.0360(19) 0.038(2) 0.0305(17) -0.0028(15) 0.0001(14) -0.0030(15)
C14 0.0287(18) 0.050(2) 0.0266(17) 0.0101(15) -0.0019(14) -0.0025(16)
C15 0.0320(17) 0.0404(19) 0.0317(18) 0.0188(15) -0.0028(14) -0.0019(15)
C16 0.0228(15) 0.0267(15) 0.0340(17) 0.0071(13) -0.0007(13) 0.0005(12)
C21 0.0212(13) 0.0147(13) 0.0259(14) 0.0030(10) -0.0016(11) -0.0010(10)
C22 0.0223(15) 0.0205(14) 0.0443(19) -0.0015(13) 0.0028(13) -0.0002(11)
C23 0.0220(14) 0.0222(14) 0.051(2) 0.0054(15) 0.0000(16) -0.0039(11)
C24 0.0334(18) 0.0160(13) 0.044(2) -0.0022(13) -0.0048(15) -0.0040(12)
C25 0.0348(18) 0.0177(14) 0.0419(19) -0.0051(13) 0.0063(15) 0.0000(12)
C26 0.0233(15) 0.0205(13) 0.0349(17) 0.0032(12) 0.0043(12) -0.0035(11)
C31 0.0196(14) 0.0227(14) 0.0219(14) -0.0022(11) 0.0015(11) -0.0065(11)
C32 0.044(2) 0.0310(17) 0.0282(17) -0.0060(14) -0.0055(14) -0.0004(15)
C33 0.066(3) 0.040(2) 0.037(2) -0.0149(17) -0.0016(19) -0.0024(19)
C34 0.052(3) 0.065(3) 0.0273(19) -0.0170(19) -0.0035(18) -0.014(2)
C35 0.036(2) 0.064(3) 0.0253(17) 0.0038(17) -0.0055(14) -0.0111(18)
C36 0.0314(17) 0.0364(18) 0.0267(16) 0.0043(14) -0.0017(14) -0.0026(14)
C41 0.0133(13) 0.0202(13) 0.0247(14) 0.0044(10) -0.0031(11) 0.0007(11)
C42 0.0221(16) 0.0213(14) 0.0331(16) 0.0036(12) 0.0030(12) -0.0005(11)
C43 0.0276(16) 0.0277(16) 0.0339(18) 0.0085(13) 0.0017(14) -0.0063(13)
C44 0.0269(16) 0.0208(14) 0.0443(19) 0.0089(13) -0.0043(14) -0.0035(12)
C45 0.0222(15) 0.0179(13) 0.0373(17) -0.0012(12) -0.0062(13) 0.0008(11)
C46 0.0168(12) 0.0209(13) 0.0264(14) 0.0021(12) -0.0039(10) 0.0007(12)
C51 0.039(3) 0.052(3) 0.039(2) 0.015(2) 0.0026(19) -0.008(2)
C52 0.082(4) 0.064(3) 0.037(3) 0.015(2) -0.015(3) -0.017(3)
C53 0.064(3) 0.055(3) 0.058(3) -0.024(2) 0.006(2) 0.005(2)
C54 0.071(3) 0.055(3) 0.105(5) -0.012(3) 0.017(4) -0.008(3)
C55 0.0274(17) 0.052(2) 0.040(2) -0.0056(17) -0.0129(15) -0.0037(16)
C56 0.033(2) 0.058(3) 0.057(3) 0.003(2) -0.0041(18) 0.0061(19)
Cl61 0.0354(5) 0.0450(5) 0.0533(6) -0.0031(4) -0.0046(4) -0.0051(4)
Cl62 0.0297(4) 0.0401(5) 0.0627(6) 0.0138(5) -0.0039(4) -0.0013(4)
C60 0.0327(17) 0.0248(15) 0.0396(18) -0.0019(14) 0.0010(14) 0.0040(14)
C70 0.024(3) 0.063(6) 0.019(3) 0.001(3) 0.003(3) 0.007(4)
Cl71 0.0628(17) 0.070(3) 0.0459(19) 0.012(2) -0.0003(14) -0.007(2)
Cl73 0.0680(15) 0.0807(17) 0.0394(10) 0.0155(11) 0.0015(10) 0.0496(14)
Cl74 0.106(4) 0.096(4) 0.0440(17) 0.004(3) -0.0001(19) -0.042(3)

_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 P1 2.2436(7) . ?
Pd1 P2 2.2457(7) . ?
Pd1 Cl1 2.3449(7) . ?
Pd1 Cl2 2.3628(7) . ?
Si1 O2 1.623(3) . ?
Si1 O1 1.628(3) . ?
Si1 O3 1.637(3) . ?
Si1 C5 1.845(3) . ?
P1 C21 1.810(3) . ?
P1 C11 1.817(3) . ?
P1 C1 1.824(3) . ?
P2 C31 1.817(3) . ?
P2 C41 1.821(3) . ?
P2 C2 1.840(3) . ?
O1 C51 1.420(5) . ?
O1 C51A 1.452(17) . ?
O2 C53 1.411(6) . ?
O3 C55 1.424(4) . ?
N1 C2 1.456(3) . ?
N1 C1 1.467(3) . ?
N1 C3 1.477(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.516(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.537(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C11 C12 1.397(4) . ?
C11 C16 1.398(4) . ?
C12 C13 1.388(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.399(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.367(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.395(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.383(4) . ?
C21 C22 1.414(4) . ?
C22 C23 1.381(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.376(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.392(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.382(5) . ?
C31 C36 1.389(4) . ?
C32 C33 1.398(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.375(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.395(4) . ?
C41 C42 1.397(4) . ?
C42 C43 1.392(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.393(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.379(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.392(4) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C52 1.491(7) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C51A C52A 1.475(19) . ?
C51A H51C 0.9900 . ?
C51A H51D 0.9900 . ?
C52A H52D 0.9800 . ?
C52A H52E 0.9800 . ?
C52A H52F 0.9800 . ?
C53 C54 1.467(7) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.520(6) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
Cl61 C60 1.773(4) . ?
Cl62 C60 1.767(3) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C70 Cl72 1.750(9) . ?
C70 Cl71 1.760(11) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
Cl73 C70A 1.588(18) . ?
Cl74 C70A 1.812(18) . ?
C70A H70C 0.9900 . ?
C70A H70D 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
P1 Pd1 P2 93.23(3) . . ?
P1 Pd1 Cl1 87.27(3) . . ?
P2 Pd1 Cl1 176.11(3) . . ?
P1 Pd1 Cl2 173.19(3) . . ?
P2 Pd1 Cl2 88.27(3) . . ?
Cl1 Pd1 Cl2 90.79(3) . . ?
O2 Si1 O1 105.30(15) . . ?
O2 Si1 O3 112.13(14) . . ?
O1 Si1 O3 109.50(15) . . ?
O2 Si1 C5 114.10(15) . . ?
O1 Si1 C5 112.29(15) . . ?
O3 Si1 C5 103.62(14) . . ?
C21 P1 C11 108.05(14) . . ?
C21 P1 C1 104.76(14) . . ?
C11 P1 C1 101.36(13) . . ?
C21 P1 Pd1 110.74(10) . . ?
C11 P1 Pd1 114.26(10) . . ?
C1 P1 Pd1 116.76(10) . . ?
C31 P2 C41 107.01(13) . . ?
C31 P2 C2 103.47(14) . . ?
C41 P2 C2 101.06(13) . . ?
C31 P2 Pd1 108.96(10) . . ?
C41 P2 Pd1 116.50(9) . . ?
C2 P2 Pd1 118.55(10) . . ?
C51 O1 C51A 32.9(12) . . ?
C51 O1 Si1 130.4(3) . . ?
C51A O1 Si1 107.8(11) . . ?
C53 O2 Si1 123.5(3) . . ?
C55 O3 Si1 123.9(2) . . ?
C2 N1 C1 109.9(2) . . ?
C2 N1 C3 111.1(2) . . ?
C1 N1 C3 109.8(2) . . ?
N1 C1 P1 112.05(18) . . ?
N1 C1 H1A 109.2 . . ?
P1 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
P1 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N1 C2 P2 111.64(19) . . ?
N1 C2 H2A 109.3 . . ?
P2 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
P2 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C4 114.5(2) . . ?
N1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 C5 113.8(2) . . ?
C3 C4 H4A 108.8 . . ?
C5 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C4 C5 Si1 111.2(2) . . ?
C4 C5 H5A 109.4 . . ?
Si1 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
Si1 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C12 C11 C16 119.8(3) . . ?
C12 C11 P1 118.1(2) . . ?
C16 C11 P1 122.2(2) . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 119.7(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 121.0(3) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C11 119.2(3) . . ?
C15 C16 H16 120.4 . . ?
C11 C16 H16 120.4 . . ?
C26 C21 C22 118.6(3) . . ?
C26 C21 P1 120.6(2) . . ?
C22 C21 P1 120.8(2) . . ?
C23 C22 C21 120.3(3) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 120.0(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 119.9(3) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 120.7(3) . . ?
C21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C32 C31 C36 119.4(3) . . ?
C32 C31 P2 119.7(2) . . ?
C36 C31 P2 120.6(2) . . ?
C31 C32 C33 120.0(4) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 120.1(4) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 119.9(4) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C36 120.5(4) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 120.1(3) . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
C46 C41 C42 119.6(3) . . ?
C46 C41 P2 119.6(2) . . ?
C42 C41 P2 120.7(2) . . ?
C43 C42 C41 120.1(3) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C42 C43 C44 119.8(3) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C45 C44 C43 120.2(3) . . ?
C45 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C44 C45 C46 120.4(3) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C45 C46 C41 119.8(3) . . ?
C45 C46 H46 120.1 . . ?
C41 C46 H46 120.1 . . ?
O1 C51 C52 111.7(4) . . ?
O1 C51 H51A 109.3 . . ?
C52 C51 H51A 109.3 . . ?
O1 C51 H51B 109.3 . . ?
C52 C51 H51B 109.3 . . ?
H51A C51 H51B 107.9 . . ?
O1 C51A C52A 101(2) . . ?
O1 C51A H51C 111.6 . . ?
C52A C51A H51C 111.6 . . ?
O1 C51A H51D 111.6 . . ?
C52A C51A H51D 111.6 . . ?
H51C C51A H51D 109.4 . . ?
C51A C52A H52D 109.5 . . ?
C51A C52A H52E 109.5 . . ?
H52D C52A H52E 109.5 . . ?
C51A C52A H52F 109.5 . . ?
H52D C52A H52F 109.5 . . ?
H52E C52A H52F 109.5 . . ?
O2 C53 C54 112.0(5) . . ?
O2 C53 H53A 109.2 . . ?
C54 C53 H53A 109.2 . . ?
O2 C53 H53B 109.2 . . ?
C54 C53 H53B 109.2 . . ?
H53A C53 H53B 107.9 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O3 C55 C56 110.5(3) . . ?
O3 C55 H55A 109.5 . . ?
C56 C55 H55A 109.5 . . ?
O3 C55 H55B 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
Cl62 C60 Cl61 110.81(19) . . ?
Cl62 C60 H60A 109.5 . . ?
Cl61 C60 H60A 109.5 . . ?
Cl62 C60 H60B 109.5 . . ?
Cl61 C60 H60B 109.5 . . ?
H60A C60 H60B 108.1 . . ?
Cl72 C70 Cl71 108.4(5) . . ?
Cl72 C70 H70A 110.0 . . ?
Cl71 C70 H70A 110.0 . . ?
Cl72 C70 H70B 110.0 . . ?
Cl71 C70 H70B 110.0 . . ?
H70A C70 H70B 108.4 . . ?
Cl73 C70A Cl74 115.7(11) . . ?
Cl73 C70A H70C 108.4 . . ?
Cl74 C70A H70C 108.4 . . ?
Cl73 C70A H70D 108.4 . . ?
Cl74 C70A H70D 108.4 . . ?
H70C C70A H70D 107.4 . . ?

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
P2 Pd1 P1 C21 99.65(10) . . . . ?
Cl1 Pd1 P1 C21 -76.49(10) . . . . ?
Cl2 Pd1 P1 C21 -2.9(3) . . . . ?
P2 Pd1 P1 C11 -138.07(11) . . . . ?
Cl1 Pd1 P1 C11 45.80(11) . . . . ?
Cl2 Pd1 P1 C11 119.4(2) . . . . ?
P2 Pd1 P1 C1 -20.09(11) . . . . ?
Cl1 Pd1 P1 C1 163.78(11) . . . . ?
Cl2 Pd1 P1 C1 -122.6(2) . . . . ?
P1 Pd1 P2 C31 -99.72(10) . . . . ?
Cl1 Pd1 P2 C31 -2.5(4) . . . . ?
Cl2 Pd1 P2 C31 73.63(10) . . . . ?
P1 Pd1 P2 C41 139.15(11) . . . . ?
Cl1 Pd1 P2 C41 -123.6(4) . . . . ?
Cl2 Pd1 P2 C41 -47.50(11) . . . . ?
P1 Pd1 P2 C2 18.14(11) . . . . ?
Cl1 Pd1 P2 C2 115.3(4) . . . . ?
Cl2 Pd1 P2 C2 -168.51(11) . . . . ?
O2 Si1 O1 C51 -5.1(4) . . . . ?
O3 Si1 O1 C51 -125.8(3) . . . . ?
C5 Si1 O1 C51 119.6(3) . . . . ?
O2 Si1 O1 C51A 22.7(15) . . . . ?
O3 Si1 O1 C51A -98.1(15) . . . . ?
C5 Si1 O1 C51A 147.4(15) . . . . ?
O1 Si1 O2 C53 177.0(3) . . . . ?
O3 Si1 O2 C53 -64.0(4) . . . . ?
C5 Si1 O2 C53 53.4(4) . . . . ?
O2 Si1 O3 C55 -67.8(3) . . . . ?
O1 Si1 O3 C55 48.7(3) . . . . ?
C5 Si1 O3 C55 168.6(3) . . . . ?
C2 N1 C1 P1 -84.7(2) . . . . ?
C3 N1 C1 P1 152.7(2) . . . . ?
C21 P1 C1 N1 -71.0(2) . . . . ?
C11 P1 C1 N1 176.7(2) . . . . ?
Pd1 P1 C1 N1 51.9(2) . . . . ?
C1 N1 C2 P2 80.7(2) . . . . ?
C3 N1 C2 P2 -157.6(2) . . . . ?
C31 P2 C2 N1 74.1(2) . . . . ?
C41 P2 C2 N1 -175.3(2) . . . . ?
Pd1 P2 C2 N1 -46.7(2) . . . . ?
C2 N1 C3 C4 66.6(3) . . . . ?
C1 N1 C3 C4 -171.6(2) . . . . ?
N1 C3 C4 C5 55.7(3) . . . . ?
C3 C4 C5 Si1 166.7(2) . . . . ?
O2 Si1 C5 C4 170.9(2) . . . . ?
O1 Si1 C5 C4 51.2(3) . . . . ?
O3 Si1 C5 C4 -66.9(2) . . . . ?
C21 P1 C11 C12 -174.1(2) . . . . ?
C1 P1 C11 C12 -64.3(3) . . . . ?
Pd1 P1 C11 C12 62.1(3) . . . . ?
C21 P1 C11 C16 5.5(3) . . . . ?
C1 P1 C11 C16 115.3(3) . . . . ?
Pd1 P1 C11 C16 -118.2(2) . . . . ?
C16 C11 C12 C13 0.5(5) . . . . ?
P1 C11 C12 C13 -179.9(3) . . . . ?
C11 C12 C13 C14 -0.9(5) . . . . ?
C12 C13 C14 C15 -0.1(5) . . . . ?
C13 C14 C15 C16 1.4(5) . . . . ?
C14 C15 C16 C11 -1.8(5) . . . . ?
C12 C11 C16 C15 0.9(5) . . . . ?
P1 C11 C16 C15 -178.8(3) . . . . ?
C11 P1 C21 C26 -111.8(3) . . . . ?
C1 P1 C21 C26 140.7(2) . . . . ?
Pd1 P1 C21 C26 14.0(3) . . . . ?
C11 P1 C21 C22 70.6(3) . . . . ?
C1 P1 C21 C22 -36.8(3) . . . . ?
Pd1 P1 C21 C22 -163.5(2) . . . . ?
C26 C21 C22 C23 -1.4(5) . . . . ?
P1 C21 C22 C23 176.2(3) . . . . ?
C21 C22 C23 C24 -0.6(5) . . . . ?
C22 C23 C24 C25 1.4(6) . . . . ?
C23 C24 C25 C26 -0.3(5) . . . . ?
C22 C21 C26 C25 2.5(5) . . . . ?
P1 C21 C26 C25 -175.1(3) . . . . ?
C24 C25 C26 C21 -1.7(5) . . . . ?
C41 P2 C31 C32 140.2(3) . . . . ?
C2 P2 C31 C32 -113.6(3) . . . . ?
Pd1 P2 C31 C32 13.4(3) . . . . ?
C41 P2 C31 C36 -45.8(3) . . . . ?
C2 P2 C31 C36 60.4(3) . . . . ?
Pd1 P2 C31 C36 -172.6(2) . . . . ?
C36 C31 C32 C33 -0.9(5) . . . . ?
P2 C31 C32 C33 173.2(3) . . . . ?
C31 C32 C33 C34 0.7(7) . . . . ?
C32 C33 C34 C35 0.6(7) . . . . ?
C33 C34 C35 C36 -1.8(6) . . . . ?
C34 C35 C36 C31 1.6(6) . . . . ?
C32 C31 C36 C35 -0.3(5) . . . . ?
P2 C31 C36 C35 -174.3(3) . . . . ?
C31 P2 C41 C46 148.9(2) . . . . ?
C2 P2 C41 C46 41.0(3) . . . . ?
Pd1 P2 C41 C46 -88.9(2) . . . . ?
C31 P2 C41 C42 -30.8(3) . . . . ?
C2 P2 C41 C42 -138.7(2) . . . . ?
Pd1 P2 C41 C42 91.4(2) . . . . ?
C46 C41 C42 C43 -1.5(5) . . . . ?
P2 C41 C42 C43 178.2(3) . . . . ?
C41 C42 C43 C44 0.6(5) . . . . ?
C42 C43 C44 C45 0.3(5) . . . . ?
C43 C44 C45 C46 -0.3(5) . . . . ?
C44 C45 C46 C41 -0.7(4) . . . . ?
C42 C41 C46 C45 1.5(4) . . . . ?
P2 C41 C46 C45 -178.2(2) . . . . ?
C51A O1 C51 C52 53(2) . . . . ?
Si1 O1 C51 C52 107.9(5) . . . . ?
C51 O1 C51A C52A -35(2) . . . . ?
Si1 O1 C51A C52A -174(2) . . . . ?
Si1 O2 C53 C54 89.7(5) . . . . ?
Si1 O3 C55 C56 -96.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.080