# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Dietrich Gudat'
_publ_contact_author_address     
;
Institut fur Anorganische Chemie
Universitat Stuttgart
Pfaffenwaldring 55
Stuttgart
70569
GERMANY
;
_publ_contact_author_email       GUDAT@IAC.UNI-STUTTGART.DE
loop_
_publ_author_name
_publ_author_address
S.Chikkali
;
Institut fur Anorganische Chemie
Universitat Stuttgart
Pfaffenwaldring 55
D-70569 Stuttgart
Germany
;
D.Gudat
;
Institut fur Anorganische Chemie
Universitat Stuttgart
Pfaffenwaldring 55
D-70569 Stuttgart
Germany
;
M.Niemeyer
;
Institut fur Anorganische Chemie
Universitat Stuttgart
Pfaffenwaldring 55
D-70569 Stuttgart
Germany
;

_publ_section_title              
;
Template controlled self-assembly of bidentate
phosphine complexes with hemilabile coordination behaviour
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 616084'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis(chloro-1-\k-Sn)-bis(3-(diphenyl-phosphinoylmethyl)-benzene-1,2-diolat
o)-1-\k^4^-O,2-\k^2^-P-tin(IV)-palladium(II)
;
_chemical_name_common            
;
bis(chloro-1-kappa-Sn)-bis(3-(diphenyl-phosphinoylmethyl)-
benzene-1,2-diolat o)-1-kappa$4!-O,2-kappa$2!-P-tin(IV)-palladium(ii)
;
_chemical_melting_point          '487 K (dec.)'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H30 Cl2 O4 P2 Pd Sn'
_chemical_formula_weight         908.56

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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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/c

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

_cell_length_a                   12.227(2)
_cell_length_b                   11.707(2)
_cell_length_c                   16.475(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.516(12)
_cell_angle_gamma                90.00
_cell_volume                     2302.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    48
_cell_measurement_theta_min      5.1
_cell_measurement_theta_max      12.5

_exptl_crystal_description       rod
_exptl_crystal_colour            orange-red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'Siemens P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 198
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <0.5%
_diffrn_reflns_number            6056
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         28.00
_reflns_number_total             5523
_reflns_number_gt                4516
_reflns_threshold_expression     >2sigma(I)

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

_publ_section_exptl_refinement   
;
In the asymmetric unit, 1.5 additional CH2Cl2 molecules were located in
solvent accessible cavities of the structure (total of six in the unit cell).
Since they were severely disordered their contribution was eliminated
from the reflection data, using the BYPASS method (van der Sluis, P.;
Spek, A. L. Acta Cryst. 1990, A46, 194) as implemented in the
SQUEEZE routine of the PLATON98 package.
;

_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.

Disorder and restraints:

;

_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^)+(0.0844P)^2^] 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    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5523
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1248
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Pd Pd 1.0000 1.11482(3) 0.2500 0.01697(11) Uani 1 2 d S . .
P P 1.00818(8) 1.24003(7) 0.14772(6) 0.01988(19) Uani 1 1 d . . .
O1 O 0.9967(2) 0.97519(19) 0.17066(16) 0.0192(5) Uani 1 1 d . . .
O2 O 1.1573(2) 0.8217(2) 0.22806(18) 0.0261(6) Uani 1 1 d . . .
Sn Sn 1.0000 0.82656(3) 0.2500 0.01907(11) Uani 1 2 d S . .
Cl Cl 0.93165(9) 0.70126(8) 0.13573(6) 0.0291(2) Uani 1 1 d . . .
C1 C 1.0193(4) 1.1512(3) 0.0570(2) 0.0259(8) Uani 1 1 d . . .
H1A H 0.9443 1.1197 0.0324 0.043(11) Uiso 1 1 calc R . .
H1B H 1.0414 1.2010 0.0147 0.043(11) Uiso 1 1 calc R . .
C11 C 1.1011(3) 1.0537(3) 0.0751(2) 0.0239(7) Uani 1 1 d . . .
C12 C 1.0880(3) 0.9726(3) 0.1338(2) 0.0220(7) Uani 1 1 d . . .
C13 C 1.1687(3) 0.8872(3) 0.1617(2) 0.0232(7) Uani 1 1 d . . .
C14 C 1.2567(4) 0.8738(4) 0.1214(3) 0.0343(9) Uani 1 1 d . . .
H14A H 1.3086 0.8130 0.1360 0.046(4) Uiso 1 1 calc R . .
C15 C 1.2678(4) 0.9508(4) 0.0593(3) 0.0374(10) Uani 1 1 d . . .
H15A H 1.3276 0.9414 0.0315 0.046(4) Uiso 1 1 calc R . .
C16 C 1.1925(4) 1.0424(3) 0.0367(3) 0.0317(9) Uani 1 1 d . . .
H16A H 1.2034 1.0960 -0.0042 0.046(4) Uiso 1 1 calc R . .
C21 C 1.1271(3) 1.3368(3) 0.1677(2) 0.0230(7) Uani 1 1 d . . .
C22 C 1.2320(4) 1.2943(3) 0.1650(3) 0.0306(8) Uani 1 1 d . . .
H22A H 1.2401 1.2166 0.1506 0.046(4) Uiso 1 1 calc R . .
C23 C 1.3261(4) 1.3654(4) 0.1832(3) 0.0392(10) Uani 1 1 d . . .
H23A H 1.3977 1.3363 0.1804 0.046(4) Uiso 1 1 calc R . .
C24 C 1.3149(4) 1.4785(4) 0.2055(3) 0.0424(11) Uani 1 1 d . . .
H24A H 1.3790 1.5264 0.2188 0.046(4) Uiso 1 1 calc R . .
C25 C 1.2099(4) 1.5219(3) 0.2085(3) 0.0373(10) Uani 1 1 d . . .
H25A H 1.2023 1.5994 0.2233 0.046(4) Uiso 1 1 calc R . .
C26 C 1.1155(4) 1.4511(3) 0.1895(3) 0.0274(8) Uani 1 1 d . . .
H26A H 1.0437 1.4806 0.1913 0.046(4) Uiso 1 1 calc R . .
C31 C 0.8828(3) 1.3215(3) 0.1074(2) 0.0237(7) Uani 1 1 d . . .
C32 C 0.8844(4) 1.4116(4) 0.0511(3) 0.0349(9) Uani 1 1 d . . .
H32A H 0.9530 1.4343 0.0378 0.046(4) Uiso 1 1 calc R . .
C33 C 0.7857(5) 1.4671(4) 0.0152(3) 0.0467(13) Uani 1 1 d . . .
H33A H 0.7867 1.5284 -0.0225 0.046(4) Uiso 1 1 calc R . .
C34 C 0.6867(5) 1.4334(5) 0.0339(4) 0.0537(14) Uani 1 1 d . . .
H34A H 0.6192 1.4721 0.0097 0.046(4) Uiso 1 1 calc R . .
C35 C 0.6845(4) 1.3431(5) 0.0883(4) 0.0500(13) Uani 1 1 d . . .
H35A H 0.6151 1.3190 0.0996 0.046(4) Uiso 1 1 calc R . .
C36 C 0.7823(4) 1.2881(4) 0.1262(3) 0.0340(9) Uani 1 1 d . . .
H36A H 0.7806 1.2280 0.1646 0.046(4) Uiso 1 1 calc R . .

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
Pd 0.0240(2) 0.01186(16) 0.01501(18) 0.000 0.00420(14) 0.000
P 0.0273(5) 0.0152(4) 0.0166(4) 0.0002(3) 0.0036(4) -0.0016(3)
O1 0.0215(12) 0.0163(11) 0.0212(12) -0.0024(9) 0.0081(10) -0.0027(9)
O2 0.0179(13) 0.0289(13) 0.0319(15) 0.0039(11) 0.0063(11) 0.0035(10)
Sn 0.02227(19) 0.01324(16) 0.02108(18) 0.000 0.00334(14) 0.000
Cl 0.0376(5) 0.0216(4) 0.0271(5) -0.0056(3) 0.0051(4) -0.0038(4)
C1 0.042(2) 0.0208(16) 0.0162(16) -0.0027(13) 0.0085(15) -0.0024(15)
C11 0.033(2) 0.0191(15) 0.0200(16) -0.0064(13) 0.0074(15) -0.0061(14)
C12 0.0254(18) 0.0178(15) 0.0238(17) -0.0085(13) 0.0076(14) -0.0049(13)
C13 0.0226(18) 0.0217(16) 0.0247(18) -0.0002(13) 0.0040(15) -0.0011(13)
C14 0.028(2) 0.038(2) 0.038(2) -0.0060(18) 0.0094(19) 0.0025(17)
C15 0.033(2) 0.040(2) 0.044(3) -0.006(2) 0.020(2) -0.0048(18)
C16 0.041(2) 0.0294(19) 0.028(2) -0.0043(16) 0.0150(18) -0.0062(17)
C21 0.030(2) 0.0200(16) 0.0182(16) 0.0018(13) 0.0031(15) -0.0055(14)
C22 0.029(2) 0.0261(18) 0.036(2) -0.0040(16) 0.0050(17) 0.0015(15)
C23 0.026(2) 0.042(2) 0.050(3) -0.006(2) 0.007(2) 0.0003(18)
C24 0.040(3) 0.040(2) 0.045(3) -0.010(2) 0.006(2) -0.017(2)
C25 0.041(2) 0.0221(18) 0.048(3) -0.0078(17) 0.008(2) -0.0075(17)
C26 0.032(2) 0.0206(16) 0.0299(19) -0.0017(15) 0.0081(16) 0.0003(15)
C31 0.028(2) 0.0224(17) 0.0177(16) 0.0000(13) -0.0009(15) -0.0006(14)
C32 0.040(2) 0.0292(19) 0.034(2) 0.0086(17) 0.0039(19) -0.0019(18)
C33 0.051(3) 0.037(2) 0.044(3) 0.012(2) -0.008(2) 0.006(2)
C34 0.037(3) 0.061(3) 0.052(3) 0.005(3) -0.014(2) 0.012(2)
C35 0.023(2) 0.074(4) 0.048(3) 0.003(3) -0.003(2) -0.001(2)
C36 0.026(2) 0.043(2) 0.030(2) 0.0051(18) 0.0011(17) -0.0048(17)

_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
Pd O1 2.088(2) . ?
Pd O1 2.088(2) 2_755 ?
Pd P 2.2519(10) 2_755 ?
Pd P 2.2519(10) . ?
P C31 1.805(4) . ?
P C21 1.816(4) . ?
P C1 1.850(4) . ?
O1 C12 1.381(5) . ?
O1 Sn 2.171(2) . ?
O2 C13 1.368(5) . ?
O2 Sn 2.033(3) . ?
Sn O2 2.033(3) 2_755 ?
Sn O1 2.171(2) 2_755 ?
Sn Cl 2.3901(10) . ?
Sn Cl 2.3901(10) 2_755 ?
C1 C11 1.504(6) . ?
C11 C12 1.389(5) . ?
C11 C16 1.404(6) . ?
C12 C13 1.410(5) . ?
C13 C14 1.390(6) . ?
C14 C15 1.391(7) . ?
C15 C16 1.410(7) . ?
C21 C22 1.386(6) . ?
C21 C26 1.401(5) . ?
C22 C23 1.398(6) . ?
C23 C24 1.390(7) . ?
C24 C25 1.391(7) . ?
C25 C26 1.400(6) . ?
C31 C36 1.387(6) . ?
C31 C32 1.408(5) . ?
C32 C33 1.385(7) . ?
C33 C34 1.371(9) . ?
C34 C35 1.390(8) . ?
C35 C36 1.382(7) . ?

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 Pd O1 76.95(14) . 2_755 ?
O1 Pd P 168.55(7) . 2_755 ?
O1 Pd P 92.24(7) 2_755 2_755 ?
O1 Pd P 92.24(7) . . ?
O1 Pd P 168.55(7) 2_755 . ?
P Pd P 98.78(5) 2_755 . ?
C31 P C21 108.67(17) . . ?
C31 P C1 101.83(18) . . ?
C21 P C1 107.51(19) . . ?
C31 P Pd 116.57(14) . . ?
C21 P Pd 115.70(12) . . ?
C1 P Pd 105.17(12) . . ?
C12 O1 Pd 112.59(19) . . ?
C12 O1 Sn 109.6(2) . . ?
Pd O1 Sn 104.78(11) . . ?
C13 O2 Sn 113.0(2) . . ?
O2 Sn O2 176.76(15) . 2_755 ?
O2 Sn O1 103.58(11) . 2_755 ?
O2 Sn O1 79.07(10) 2_755 2_755 ?
O2 Sn O1 79.07(10) . . ?
O2 Sn O1 103.58(11) 2_755 . ?
O1 Sn O1 73.49(13) 2_755 . ?
O2 Sn Cl 91.46(9) . . ?
O2 Sn Cl 86.56(8) 2_755 . ?
O1 Sn Cl 157.47(7) 2_755 . ?
O1 Sn Cl 93.43(7) . . ?
O2 Sn Cl 86.56(8) . 2_755 ?
O2 Sn Cl 91.45(9) 2_755 2_755 ?
O1 Sn Cl 93.43(7) 2_755 2_755 ?
O1 Sn Cl 157.47(7) . 2_755 ?
Cl Sn Cl 104.28(5) . 2_755 ?
C11 C1 P 115.4(3) . . ?
C12 C11 C16 118.2(4) . . ?
C12 C11 C1 119.0(3) . . ?
C16 C11 C1 122.8(4) . . ?
O1 C12 C11 121.2(3) . . ?
O1 C12 C13 116.6(3) . . ?
C11 C12 C13 122.2(4) . . ?
O2 C13 C14 122.8(4) . . ?
O2 C13 C12 118.2(3) . . ?
C14 C13 C12 119.0(4) . . ?
C13 C14 C15 119.1(4) . . ?
C14 C15 C16 121.6(4) . . ?
C11 C16 C15 119.3(4) . . ?
C22 C21 C26 119.8(4) . . ?
C22 C21 P 118.7(3) . . ?
C26 C21 P 121.4(3) . . ?
C21 C22 C23 120.2(4) . . ?
C24 C23 C22 120.1(4) . . ?
C23 C24 C25 120.1(4) . . ?
C24 C25 C26 119.9(4) . . ?
C25 C26 C21 119.9(4) . . ?
C36 C31 C32 119.8(4) . . ?
C36 C31 P 119.5(3) . . ?
C32 C31 P 120.4(3) . . ?
C33 C32 C31 119.9(5) . . ?
C34 C33 C32 119.9(5) . . ?
C33 C34 C35 120.4(5) . . ?
C36 C35 C34 120.6(5) . . ?
C35 C36 C31 119.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.138