# Electronic Supplementary Material (ESI) for Chemical Science.
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# 
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#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
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#  as required by the journal to which it was submitted.
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data_s12103
_audit_creation_date             2013-04-16
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr  9 2013 14:10:59, GUI svn.r4458)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C42 H64 P2 Pd Si, C5 H12'
_chemical_formula_sum            'C47 H76 P2 Pd Si'
_chemical_formula_weight         837.51
_chemical_melting_point          ?
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'
P P 0.1023 0.0942 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   16.1665(11)
_cell_length_b                   10.3002(7)
_cell_length_c                   27.3994(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.802(7)
_cell_angle_gamma                90.00
_cell_volume                     4449.1(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21810
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.228
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   'Jacobson, R (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.1570
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37324
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         3.02
_diffrn_ambient_temperature      150
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 70.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: -0.0057
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 70.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 120.0000
	             XTD: 127.4000
	          2theta: -0.0057
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 70.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: -0.0057
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 70.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: -0.0057
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 70.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 240.0000
	             XTD: 127.4000
	          2theta: -0.0057
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 70.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 90.0000
	             XTD: 127.4000
	          2theta: -0.0057
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 70.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: -0.0057
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.010187
_diffrn_orient_matrix_UB_12      -0.083158
_diffrn_orient_matrix_UB_13      -0.016569
_diffrn_orient_matrix_UB_21      0.057330
_diffrn_orient_matrix_UB_22      -0.007000
_diffrn_orient_matrix_UB_23      0.022892
_diffrn_orient_matrix_UB_31      -0.025164
_diffrn_orient_matrix_UB_32      -0.049613
_diffrn_orient_matrix_UB_33      0.024541
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_number_gt                4558
_reflns_number_total             6808
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.645
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6808
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0628
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0611P)²+1.3362P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1453
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C44-C45 \\sim C45-C46
 with sigma of 0.02
 C45-C46 \\sim C46-C47
 with sigma of 0.02
 C45-C44 \\sim C44-C43
 with sigma of 0.02
 C43A-C44A \\sim C44A-C45A
 with sigma of 0.02
 C44A-C45A \\sim C45A-C46A
 with sigma of 0.02
 C45A-C46A \\sim C46A-C47A
 with sigma of 0.02
3. Rigid bond restraints
 C43, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43A, C44A, C45A, C46A, C47A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C46, C44, C47, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C47A \\sim C46A \\sim C45A \\sim C44A \\sim C43A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C43 \\sim C46 \\sim C44 \\sim C47 \\sim C45: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C43A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C43A) = Uanis(C44A) = Uanis(C45A)
Uanis(C47) = Uanis(C46)
5. Others
 1-1*Sof(C43)=1-1*Sof(H43D)=1-1*Sof(H43E)=1-1*Sof(H43F)=1-1*Sof(C46)=1-1*
 Sof(H46C)=1-1*Sof(H46D)=1-1*Sof(C44)=1-1*Sof(H44C)=1-1*Sof(H44D)=1-1*Sof(C47)=
 1-1*Sof(H47D)=1-1*Sof(H47E)=1-1*Sof(H47F)=1-1*Sof(C45)=1-1*Sof(H45C)=1-1*
 Sof(H45D)=1*Sof(C44A)=1*Sof(H44A)=1*Sof(H44B)=1*Sof(C47A)=1*Sof(H47A)=1*
 Sof(H47B)=1*Sof(H47C)=1*Sof(C46A)=1*Sof(H46A)=1*Sof(H46B)=1*Sof(C43A)=1*
 Sof(H43A)=1*Sof(H43B)=1*Sof(H43C)=1*Sof(C45A)=1*Sof(H45A)=1*Sof(H45B)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C6(H6), C37(H37), C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C17(H17A,H17B), C11(H11A,H11B), C14(H14A,H14B),
 C38(H38A,H38B), C13(H13A,H13B), C32(H32A,H32B), C39(H39A,H39B), C42(H42A,H42B),
  C9(H9A,H9B), C10(H10A,H10B), C8(H8A,H8B), C41(H41A,H41B), C34(H34A,H34B),
 C36(H36A,H36B), C33(H33A,H33B), C35(H35A,H35B), C15(H15A,H15B), C16(H16A,H16B),
  C40(H40A,H40B), C46(H46C,H46D), C44(H44C,H44D), C45(H45C,H45D), C44A(H44A,
 H44B), C46A(H46A,H46B), C45A(H45A,H45B)
6.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C19(H19), C29(H29), C28(H28), C26(H26), C22(H22), C27(H27), C2(H2),
 C20(H20)
6.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C43(H43D,H43E,H43F),
 C47(H47D,H47E,H47F), C47A(H47A,H47B,H47C), C43A(H43A,H43B,H43C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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 0.25261(3) 0.45664(4) 0.857904(18) 0.02706(17) Uani 1 1 d . . .
P2 P 0.25716(10) 0.47608(16) 0.77591(6) 0.0296(4) Uani 1 1 d . . .
Si2 Si 0.28736(11) 0.67645(16) 0.86062(7) 0.0294(4) Uani 1 1 d . . .
P1 P 0.20378(10) 0.50654(15) 0.92856(6) 0.0288(4) Uani 1 1 d . . .
C1 C 0.2457(4) 0.2421(6) 0.8581(2) 0.0374(16) Uani 1 1 d . . .
H1A H 0.1881 0.2128 0.8567 0.045 Uiso 1 1 calc R . .
H1B H 0.2653 0.2056 0.8301 0.045 Uiso 1 1 calc R . .
C12 C 0.0991(3) 0.4393(5) 0.9306(2) 0.0276(15) Uani 1 1 d . . .
H12 H 0.0798 0.4828 0.9579 0.033 Uiso 1 1 calc R . .
C6 C 0.2712(4) 0.4676(6) 0.9904(2) 0.0308(15) Uani 1 1 d . . .
H6 H 0.2801 0.3735 0.9907 0.037 Uiso 1 1 calc R . .
C18 C 0.1817(4) 0.6813(6) 0.9297(2) 0.0288(15) Uani 1 1 d . . .
C7 C 0.3593(4) 0.5295(7) 0.9956(3) 0.0458(18) Uani 1 1 d . . .
H7A H 0.3831 0.5031 0.9676 0.055 Uiso 1 1 calc R . .
H7B H 0.3537 0.6233 0.9947 0.055 Uiso 1 1 calc R . .
C17 C 0.0349(4) 0.4686(6) 0.8822(3) 0.0418(18) Uani 1 1 d . . .
H17A H 0.0532 0.4278 0.8545 0.050 Uiso 1 1 calc R . .
H17B H 0.0328 0.5616 0.8765 0.050 Uiso 1 1 calc R . .
C11 C 0.2356(4) 0.4989(7) 1.0365(2) 0.0396(17) Uani 1 1 d . . .
H11A H 0.1813 0.4562 1.0335 0.047 Uiso 1 1 calc R . .
H11B H 0.2266 0.5918 1.0381 0.047 Uiso 1 1 calc R . .
C21 C 0.1505(5) 0.9469(7) 0.9271(3) 0.051(2) Uani 1 1 d . . .
H21 H 0.1401 1.0357 0.9261 0.061 Uiso 1 1 calc R . .
C14 C 0.0121(4) 0.2445(6) 0.9429(3) 0.0414(18) Uani 1 1 d . . .
H14A H -0.0053 0.2841 0.9711 0.050 Uiso 1 1 calc R . .
H14B H 0.0142 0.1512 0.9480 0.050 Uiso 1 1 calc R . .
C38 C 0.0838(4) 0.5066(7) 0.7393(3) 0.0426(18) Uani 1 1 d . . .
H38A H 0.0950 0.5966 0.7326 0.051 Uiso 1 1 calc R . .
H38B H 0.0781 0.5008 0.7737 0.051 Uiso 1 1 calc R . .
C13 C 0.0996(4) 0.2932(6) 0.9406(2) 0.0357(16) Uani 1 1 d . . .
H13A H 0.1191 0.2478 0.9143 0.043 Uiso 1 1 calc R . .
H13B H 0.1389 0.2745 0.9721 0.043 Uiso 1 1 calc R . .
C37 C 0.1587(4) 0.4235(6) 0.7328(2) 0.0309(15) Uani 1 1 d . . .
H37 H 0.1660 0.4365 0.6986 0.037 Uiso 1 1 calc R . .
C19 C 0.1301(4) 0.7360(6) 0.9587(2) 0.0380(17) Uani 1 1 d . . .
H19 H 0.1068 0.6829 0.9796 0.046 Uiso 1 1 calc R . .
C25 C 0.2693(4) 0.7402(6) 0.7940(2) 0.0313(15) Uani 1 1 d . . .
C23 C 0.2191(4) 0.7601(6) 0.8988(2) 0.0281(15) Uani 1 1 d . . .
C29 C 0.2558(4) 0.6837(6) 0.7067(2) 0.0336(16) Uani 1 1 d . . .
H29 H 0.2502 0.6207 0.6819 0.040 Uiso 1 1 calc R . .
C32 C 0.4296(4) 0.4414(7) 0.7858(3) 0.0454(19) Uani 1 1 d . . .
H32A H 0.4303 0.4400 0.8213 0.054 Uiso 1 1 calc R . .
H32B H 0.4360 0.5309 0.7762 0.054 Uiso 1 1 calc R . .
C28 C 0.2571(4) 0.8133(6) 0.6943(2) 0.0372(17) Uani 1 1 d . . .
H28 H 0.2537 0.8376 0.6612 0.045 Uiso 1 1 calc R . .
C39 C 0.0006(4) 0.4645(7) 0.7045(3) 0.053(2) Uani 1 1 d . . .
H39A H -0.0456 0.5169 0.7111 0.063 Uiso 1 1 calc R . .
H39B H 0.0040 0.4789 0.6700 0.063 Uiso 1 1 calc R . .
C24 C 0.3991(4) 0.7276(6) 0.8887(2) 0.0384(17) Uani 1 1 d . . .
H24A H 0.4120 0.7095 0.9239 0.058 Uiso 1 1 calc R . .
H24B H 0.4051 0.8189 0.8835 0.058 Uiso 1 1 calc R . .
H24C H 0.4375 0.6804 0.8730 0.058 Uiso 1 1 calc R . .
C42 C 0.1393(4) 0.2800(6) 0.7386(3) 0.0420(18) Uani 1 1 d . . .
H42A H 0.1362 0.2631 0.7730 0.050 Uiso 1 1 calc R . .
H42B H 0.1851 0.2280 0.7312 0.050 Uiso 1 1 calc R . .
C26 C 0.2702(4) 0.8714(6) 0.7805(3) 0.0397(17) Uani 1 1 d . . .
H26 H 0.2754 0.9351 0.8051 0.048 Uiso 1 1 calc R . .
C30 C 0.2629(4) 0.6464(6) 0.7568(2) 0.0320(16) Uani 1 1 d . . .
C22 C 0.2036(4) 0.8939(6) 0.8989(3) 0.0410(17) Uani 1 1 d . . .
H22 H 0.2293 0.9483 0.8796 0.049 Uiso 1 1 calc R . .
C31 C 0.3445(4) 0.3893(7) 0.7566(2) 0.0385(17) Uani 1 1 d . . .
H31 H 0.3415 0.3000 0.7684 0.046 Uiso 1 1 calc R . .
C9 C 0.3827(5) 0.5159(7) 1.0895(3) 0.055(2) Uani 1 1 d . . .
H9A H 0.3777 0.6090 1.0935 0.066 Uiso 1 1 calc R . .
H9B H 0.4212 0.4827 1.1191 0.066 Uiso 1 1 calc R . .
C27 C 0.2636(4) 0.9073(7) 0.7312(3) 0.0426(18) Uani 1 1 d . . .
H27 H 0.2634 0.9947 0.7227 0.051 Uiso 1 1 calc R . .
C10 C 0.2966(4) 0.4539(7) 1.0847(2) 0.0477(19) Uani 1 1 d . . .
H10A H 0.2737 0.4773 1.1134 0.057 Uiso 1 1 calc R . .
H10B H 0.3022 0.3602 1.0843 0.057 Uiso 1 1 calc R . .
C3 C 0.3823(4) 0.1756(7) 0.9168(3) 0.0473(19) Uani 1 1 d . . .
C2 C 0.3008(4) 0.2068(6) 0.9047(3) 0.0413(18) Uani 1 1 d . . .
H2 H 0.2743 0.2056 0.9316 0.050 Uiso 1 1 calc R . .
C8 C 0.4187(4) 0.4890(8) 1.0443(3) 0.055(2) Uani 1 1 d . . .
H8A H 0.4305 0.3969 1.0429 0.066 Uiso 1 1 calc R . .
H8B H 0.4720 0.5352 1.0477 0.066 Uiso 1 1 calc R . .
C20 C 0.1128(4) 0.8673(7) 0.9571(3) 0.0476(19) Uani 1 1 d . . .
H20 H 0.0765 0.9021 0.9757 0.057 Uiso 1 1 calc R . .
C41 C 0.0551(4) 0.2393(7) 0.7035(3) 0.057(2) Uani 1 1 d . . .
H41A H 0.0600 0.2474 0.6690 0.068 Uiso 1 1 calc R . .
H41B H 0.0434 0.1491 0.7095 0.068 Uiso 1 1 calc R . .
C34 C 0.5025(4) 0.3473(9) 0.7226(3) 0.063(2) Uani 1 1 d . . .
H34A H 0.5480 0.2901 0.7183 0.076 Uiso 1 1 calc R . .
H34B H 0.5120 0.4315 0.7090 0.076 Uiso 1 1 calc R . .
C36 C 0.3443(4) 0.3772(8) 0.7025(3) 0.061(2) Uani 1 1 d . . .
H36A H 0.3483 0.4630 0.6886 0.073 Uiso 1 1 calc R . .
H36B H 0.2913 0.3385 0.6851 0.073 Uiso 1 1 calc R . .
C33 C 0.5047(4) 0.3609(9) 0.7761(3) 0.065(2) Uani 1 1 d . . .
H33A H 0.5574 0.4023 0.7925 0.078 Uiso 1 1 calc R . .
H33B H 0.5033 0.2753 0.7907 0.078 Uiso 1 1 calc R . .
C35 C 0.4188(4) 0.2934(8) 0.6942(3) 0.063(2) Uani 1 1 d . . .
H35A H 0.4121 0.2053 0.7052 0.075 Uiso 1 1 calc R . .
H35B H 0.4185 0.2907 0.6588 0.075 Uiso 1 1 calc R . .
C15 C -0.0527(4) 0.2761(7) 0.8950(3) 0.055(2) Uani 1 1 d . . .
H15A H -0.0389 0.2284 0.8673 0.066 Uiso 1 1 calc R . .
H15B H -0.1086 0.2489 0.8985 0.066 Uiso 1 1 calc R . .
C4 C 0.4347(5) 0.1641(8) 0.8778(3) 0.068(3) Uani 1 1 d . . .
H4A H 0.3981 0.1682 0.8451 0.103 Uiso 1 1 calc R . .
H4B H 0.4644 0.0828 0.8818 0.103 Uiso 1 1 calc R . .
H4C H 0.4748 0.2341 0.8818 0.103 Uiso 1 1 calc R . .
C16 C -0.0539(4) 0.4198(7) 0.8838(3) 0.058(2) Uani 1 1 d . . .
H16A H -0.0746 0.4668 0.9094 0.070 Uiso 1 1 calc R . .
H16B H -0.0923 0.4364 0.8519 0.070 Uiso 1 1 calc R . .
C40 C -0.0175(4) 0.3230(8) 0.7119(3) 0.067(3) Uani 1 1 d . . .
H40A H -0.0694 0.2979 0.6885 0.080 Uiso 1 1 calc R . .
H40B H -0.0255 0.3096 0.7456 0.080 Uiso 1 1 calc R . .
C5 C 0.4288(5) 0.1471(9) 0.9690(3) 0.084(3) Uani 1 1 d . . .
H5A H 0.4753 0.2066 0.9785 0.126 Uiso 1 1 calc R . .
H5B H 0.4501 0.0598 0.9708 0.126 Uiso 1 1 calc R . .
H5C H 0.3910 0.1565 0.9912 0.126 Uiso 1 1 calc R . .
C43 C 0.1274(11) 1.2103(16) 1.0841(6) 0.067(5) Uani 0.515(12) 1 d PDU A 1
H43D H 0.1536 1.2233 1.1188 0.100 Uiso 0.515(12) 1 calc PR A 1
H43E H 0.0700 1.2412 1.0776 0.100 Uiso 0.515(12) 1 calc PR A 1
H43F H 0.1585 1.2571 1.0637 0.100 Uiso 0.515(12) 1 calc PR A 1
C46 C 0.2419(13) 0.9740(16) 1.0888(7) 0.071(4) Uani 0.515(12) 1 d PDU A 1
H46C H 0.1945 0.9156 1.0879 0.085 Uiso 0.515(12) 1 calc PR A 1
H46D H 0.2647 0.9965 1.1235 0.085 Uiso 0.515(12) 1 calc PR A 1
C44 C 0.1277(15) 1.0760(19) 1.0727(10) 0.088(7) Uani 0.515(12) 1 d PDU A 1
H44C H 0.0849 1.0519 1.0433 0.105 Uiso 0.515(12) 1 calc PR A 1
H44D H 0.1245 1.0204 1.1007 0.105 Uiso 0.515(12) 1 calc PR A 1
C47 C 0.3056(12) 0.9057(18) 1.0707(7) 0.071(4) Uani 0.515(12) 1 d PDU A 1
H47D H 0.3260 0.9591 1.0471 0.106 Uiso 0.515(12) 1 calc PR A 1
H47E H 0.2819 0.8272 1.0545 0.106 Uiso 0.515(12) 1 calc PR A 1
H47F H 0.3517 0.8847 1.0982 0.106 Uiso 0.515(12) 1 calc PR A 1
C45 C 0.2116(12) 1.0850(16) 1.0634(7) 0.069(5) Uani 0.515(12) 1 d PDU A 1
H45C H 0.2118 1.0802 1.0281 0.083 Uiso 0.515(12) 1 calc PR A 1
H45D H 0.2416 1.1621 1.0781 0.083 Uiso 0.515(12) 1 calc PR A 1
C44A C 0.1956(11) 1.009(2) 1.0922(7) 0.068(4) Uani 0.485(12) 1 d PDU A 2
H44A H 0.2201 1.0015 1.1278 0.082 Uiso 0.485(12) 1 calc PR A 2
H44B H 0.1669 0.9285 1.0809 0.082 Uiso 0.485(12) 1 calc PR A 2
C47A C 0.3355(11) 0.8955(17) 1.0363(7) 0.073(6) Uani 0.485(12) 1 d PDU A 2
H47A H 0.3316 0.9598 1.0106 0.110 Uiso 0.485(12) 1 calc PR A 2
H47B H 0.2871 0.8392 1.0284 0.110 Uiso 0.485(12) 1 calc PR A 2
H47C H 0.3863 0.8455 1.0386 0.110 Uiso 0.485(12) 1 calc PR A 2
C46A C 0.3378(13) 0.958(3) 1.0829(9) 0.114(9) Uani 0.485(12) 1 d PDU A 2
H46A H 0.3871 1.0133 1.0932 0.137 Uiso 0.485(12) 1 calc PR A 2
H46B H 0.3346 0.8967 1.1094 0.137 Uiso 0.485(12) 1 calc PR A 2
C43A C 0.1337(16) 1.117(2) 1.0836(10) 0.068(4) Uani 0.485(12) 1 d PDU A 2
H43A H 0.1206 1.1394 1.0487 0.102 Uiso 0.485(12) 1 calc PR A 2
H43B H 0.1575 1.1909 1.1030 0.102 Uiso 0.485(12) 1 calc PR A 2
H43C H 0.0829 1.0903 1.0934 0.102 Uiso 0.485(12) 1 calc PR A 2
C45A C 0.2600(10) 1.031(2) 1.0666(7) 0.068(4) Uani 0.485(12) 1 d PDU A 2
H45A H 0.2742 1.1227 1.0692 0.082 Uiso 0.485(12) 1 calc PR A 2
H45B H 0.2376 1.0123 1.0315 0.082 Uiso 0.485(12) 1 calc PR A 2


_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 P2 2.2729(18) . ?
Pd1 Si2 2.3300(18) . ?
Pd1 P1 2.3048(17) . ?
Pd1 C1 2.213(6) . ?
P2 C37 1.841(6) . ?
P2 C30 1.839(6) . ?
P2 C31 1.846(6) . ?
Si2 C25 1.901(6) . ?
Si2 C23 1.889(6) . ?
Si2 C24 1.876(6) . ?
P1 C12 1.841(6) . ?
P1 C6 1.844(6) . ?
P1 C18 1.836(6) . ?
C1 C2 1.432(8) . ?
C12 C17 1.522(8) . ?
C12 C13 1.529(7) . ?
C6 C7 1.536(8) . ?
C6 C11 1.534(8) . ?
C18 C19 1.391(8) . ?
C18 C23 1.402(8) . ?
C7 C8 1.520(9) . ?
C17 C16 1.531(9) . ?
C11 C10 1.535(9) . ?
C21 C22 1.389(9) . ?
C21 C20 1.392(9) . ?
C14 C13 1.515(8) . ?
C14 C15 1.522(9) . ?
C38 C37 1.525(8) . ?
C38 C39 1.530(9) . ?
C37 C42 1.526(8) . ?
C19 C20 1.380(9) . ?
C25 C26 1.402(8) . ?
C25 C30 1.392(8) . ?
C23 C22 1.401(8) . ?
C29 C28 1.379(8) . ?
C29 C30 1.404(8) . ?
C32 C31 1.528(8) . ?
C32 C33 1.541(9) . ?
C28 C27 1.387(9) . ?
C39 C40 1.509(10) . ?
C42 C41 1.541(8) . ?
C26 C27 1.383(9) . ?
C31 C36 1.485(9) . ?
C9 C10 1.511(9) . ?
C9 C8 1.507(10) . ?
C3 C2 1.326(9) . ?
C3 C4 1.507(10) . ?
C3 C5 1.489(10) . ?
C41 C40 1.514(10) . ?
C34 C33 1.464(9) . ?
C34 C35 1.510(9) . ?
C36 C35 1.540(9) . ?
C15 C16 1.511(9) . ?
C43 C44 1.418(17) . ?
C46 C47 1.424(16) . ?
C46 C45 1.370(16) . ?
C44 C45 1.438(19) . ?
C44A C43A 1.476(19) . ?
C44A C45A 1.397(19) . ?
C47A C46A 1.422(19) . ?
C46A C45A 1.449(19) . ?

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
P2 Pd1 Si2 83.43(6) . . ?
P2 Pd1 P1 154.52(6) . . ?
P1 Pd1 Si2 83.19(6) . . ?
C1 Pd1 P2 95.96(17) . . ?
C1 Pd1 Si2 169.23(18) . . ?
C1 Pd1 P1 101.14(17) . . ?
C37 P2 Pd1 113.3(2) . . ?
C37 P2 C31 106.3(3) . . ?
C30 P2 Pd1 112.4(2) . . ?
C30 P2 C37 100.9(3) . . ?
C30 P2 C31 106.9(3) . . ?
C31 P2 Pd1 115.8(2) . . ?
C25 Si2 Pd1 108.7(2) . . ?
C23 Si2 Pd1 107.1(2) . . ?
C23 Si2 C25 113.0(3) . . ?
C24 Si2 Pd1 119.3(2) . . ?
C24 Si2 C25 103.1(3) . . ?
C24 Si2 C23 105.8(3) . . ?
C12 P1 Pd1 115.5(2) . . ?
C12 P1 C6 104.5(3) . . ?
C6 P1 Pd1 118.7(2) . . ?
C18 P1 Pd1 109.7(2) . . ?
C18 P1 C12 100.6(3) . . ?
C18 P1 C6 106.0(3) . . ?
C2 C1 Pd1 103.5(4) . . ?
C17 C12 P1 110.6(4) . . ?
C17 C12 C13 109.1(5) . . ?
C13 C12 P1 114.1(4) . . ?
C7 C6 P1 110.0(4) . . ?
C11 C6 P1 117.2(4) . . ?
C11 C6 C7 110.2(5) . . ?
C19 C18 P1 123.4(5) . . ?
C19 C18 C23 120.2(6) . . ?
C23 C18 P1 116.4(5) . . ?
C8 C7 C6 111.1(6) . . ?
C12 C17 C16 111.9(6) . . ?
C6 C11 C10 111.0(5) . . ?
C22 C21 C20 120.2(7) . . ?
C13 C14 C15 111.4(5) . . ?
C37 C38 C39 112.3(6) . . ?
C14 C13 C12 111.5(5) . . ?
C38 C37 P2 110.8(4) . . ?
C38 C37 C42 110.2(5) . . ?
C42 C37 P2 112.8(4) . . ?
C20 C19 C18 121.5(6) . . ?
C26 C25 Si2 125.3(5) . . ?
C30 C25 Si2 115.7(5) . . ?
C30 C25 C26 118.7(6) . . ?
C18 C23 Si2 117.0(4) . . ?
C22 C23 Si2 125.1(5) . . ?
C22 C23 C18 117.9(6) . . ?
C28 C29 C30 120.2(6) . . ?
C31 C32 C33 111.9(5) . . ?
C29 C28 C27 119.9(6) . . ?
C40 C39 C38 111.2(6) . . ?
C37 C42 C41 111.9(5) . . ?
C27 C26 C25 120.8(7) . . ?
C25 C30 P2 117.0(5) . . ?
C25 C30 C29 120.2(6) . . ?
C29 C30 P2 122.7(5) . . ?
C21 C22 C23 121.3(6) . . ?
C32 C31 P2 109.7(4) . . ?
C36 C31 P2 119.6(5) . . ?
C36 C31 C32 110.8(5) . . ?
C8 C9 C10 111.6(6) . . ?
C26 C27 C28 120.2(6) . . ?
C9 C10 C11 110.5(6) . . ?
C2 C3 C4 121.7(7) . . ?
C2 C3 C5 123.3(7) . . ?
C5 C3 C4 114.9(7) . . ?
C3 C2 C1 132.2(7) . . ?
C9 C8 C7 112.7(6) . . ?
C19 C20 C21 118.9(7) . . ?
C40 C41 C42 111.0(6) . . ?
C33 C34 C35 111.8(6) . . ?
C31 C36 C35 111.4(6) . . ?
C34 C33 C32 112.3(6) . . ?
C34 C35 C36 111.0(6) . . ?
C16 C15 C14 111.1(6) . . ?
C15 C16 C17 111.0(6) . . ?
C39 C40 C41 110.5(6) . . ?
C45 C46 C47 116(2) . . ?
C43 C44 C45 91.5(17) . . ?
C46 C45 C44 96(2) . . ?
C45A C44A C43A 111(2) . . ?
C47A C46A C45A 96.3(18) . . ?
C44A C45A C46A 117(2) . . ?

_database_code_depnum_ccdc_archive 'CCDC 997342'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_00713008
_audit_creation_date             2013-01-24
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C42 H64 P2 Pd Si, C5 H12'
_chemical_formula_sum            'C23.50 H38 P Pd0.50 Si0.50'
_chemical_formula_weight         418.75
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.8954(3)
_cell_length_b                   18.9114(3)
_cell_length_c                   16.6032(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.453(7)
_cell_angle_gamma                90.00
_cell_volume                     4485.5(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    46969
_cell_measurement_temperature    93
_cell_measurement_theta_max      63.7
_cell_measurement_theta_min      2.3
_exptl_absorpt_coefficient_mu    4.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
'Rigaku MicroMax-007HF, Rigaku Saturn 944+ CCD'
;
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52296
_diffrn_reflns_theta_full        63.69
_diffrn_reflns_theta_max         63.69
_diffrn_reflns_theta_min         3.52
_diffrn_ambient_temperature      93
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -48.0000 - 132.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 50.0000
	          2theta: 42.0000
scan:
	Number of images: 360
	           Slice: -48.0000 - 132.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 15.0000
	             Phi: 180.0000
	             XTD: 50.0000
	          2theta: 42.0000
scan:
	Number of images: 344
	           Slice: -48.0000 - 124.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 30.0000
	             Phi: 90.0000
	             XTD: 50.0000
	          2theta: 42.0000
scan:
	Number of images: 348
	           Slice: -48.0000 - 126.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 45.0000
	             Phi: 180.0000
	             XTD: 50.0000
	          2theta: 42.0000
scan:
	Number of images: 270
	           Slice: -14.0000 - 121.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 45.0000
	             Phi: 0.0000
	             XTD: 50.0000
	          2theta: 42.0000
scan:
	Number of images: 360
	           Slice: -48.0000 - 132.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 45.0000
	             Phi: 90.0000
	             XTD: 50.0000
	          2theta: 42.0000
scan:
	Number of images: 240
	           Slice: -18.0000 - 102.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 180.0000
	             XTD: 50.0000
	          2theta: 42.0000
scan:
	Number of images: 360
	           Slice: 0.0000 - 180.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 15.0000
	             Phi: 90.0000
	             XTD: 50.0000
	          2theta: 90.0000
scan:
	Number of images: 360
	           Slice: 0.0000 - 180.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 15.0000
	             Phi: 0.0000
	             XTD: 50.0000
	          2theta: 90.0000
scan:
	Number of images: 360
	           Slice: 0.0000 - 180.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 50.0000
	          2theta: 90.0000
scan:
	Number of images: 360
	           Slice: 0.0000 - 180.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 15.0000
	             Phi: 180.0000
	             XTD: 50.0000
	          2theta: 90.0000
scan:
	Number of images: 360
	           Slice: 0.0000 - 180.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 45.0000
	             Phi: 0.0000
	             XTD: 50.0000
	          2theta: 90.0000
scan:
	Number of images: 360
	           Slice: 0.0000 - 180.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 30.0000
	             Phi: 180.0000
	             XTD: 50.0000
	          2theta: 90.0000
scan:
	Number of images: 360
	           Slice: 0.0000 - 180.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 30.0000
	             Phi: 90.0000
	             XTD: 50.0000
	          2theta: 90.0000
scan:
	Number of images: 328
	           Slice: 0.0000 - 164.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 45.0000
	             Phi: 180.0000
	             XTD: 50.0000
	          2theta: 90.0000
scan:
	Number of images: 360
	           Slice: 0.0000 - 180.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 45.0000
	             Phi: 90.0000
	             XTD: 50.0000
	          2theta: 90.0000
;
_diffrn_measurement_device       
;
AFC11 (Left): Eulerian 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       ω
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.030047
_diffrn_orient_matrix_UB_12      0.006508
_diffrn_orient_matrix_UB_13      -0.061526
_diffrn_orient_matrix_UB_21      0.041364
_diffrn_orient_matrix_UB_22      0.041642
_diffrn_orient_matrix_UB_23      -0.000038
_diffrn_orient_matrix_UB_31      0.047816
_diffrn_orient_matrix_UB_32      -0.031933
_diffrn_orient_matrix_UB_33      -0.012590
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_reflns_number_gt                6896
_reflns_number_total             7332
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7332
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0690P)²+5.4438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1077
_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.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H26 of C26, H11 of C11, {H42a,H42b} of C42, {H40a,H40b} of C40, {H2a,H2b}
  of C2, {H39a,H39b} of C39, H10 of C10, {H38a,H38b} of C38, {H32a,H32b} of C32,
   H8 of C8, H29 of C29, H31 of C31, H37 of C37, H27 of C27, H3 of C3, H9 of C9,
   {H18a,H18b} of C18, H28 of C28, {H21a,H21b} of C21, {H22a,H22b} of C22,
  {H16a,H16b} of C16, {H33a,H33b} of C33, {H17a,H17b} of C17, {H35a,H35b} of
  C35, {H34a,H34b} of C34, {H1Ba,H1Bb} of C1B, {H1Da,H1Db} of C1D, H19 of C19,
  {H20a,H20b} of C20, {H14a,H14b} of C14, {H41a,H41b} of C41, {H15a,H15b} of
  C15, {H24a,H24b} of C24, {H36a,H36b} of C36, H13 of C13, {H23a,H23b} of C23,
  {H1Wa,H1Wb} of C1W
 At 1.5 times of:
  {H5a,H5b,H5c} of C5, {H6a,H6b,H6c} of C6, {H1Aa,H1Ab,H1Ac} of C1A, {H1Ca,
  H1Cb,H1Cc} of C1C, {H1a,H1b,H1c} of C1
2. Restrained distances
 C1C-C1D ~ C1D-C1W
 with sigma of 0.02
 C1D-C1W ~ C1W-C1B
 with sigma of 0.02
 C1W-C1B ~ C1B-C1A
 with sigma of 0.02
3. Rigid bond restraints
 C1A, C1B, C1W, C1D, C1C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1A ~ C1B ~ C1W ~ C1D ~ C1C: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5.a Ternary CH refined with riding coordinates:
 C37(H37), C31(H31), C19(H19), C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C38(H38a,H38b), C42(H42a,H42b), C2(H2a,H2b), C39(H39a,H39b), C40(H40a,H40b),
 C32(H32a,H32b), C20(H20a,H20b), C14(H14a,H14b), C41(H41a,H41b), C15(H15a,H15b),
  C24(H24a,H24b), C36(H36a,H36b), C23(H23a,H23b), C18(H18a,H18b), C21(H21a,
 H21b), C22(H22a,H22b), C16(H16a,H16b), C33(H33a,H33b), C17(H17a,H17b),
 C35(H35a,H35b), C34(H34a,H34b), C1B(H1Ba,H1Bb), C1D(H1Da,H1Db), C1W(H1Wa,H1Wb)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C26(H26), C10(H10), C8(H8), C27(H27), C29(H29), C3(H3), C9(H9),
 C28(H28)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C1A(H1Aa,H1Ab,H1Ac),
 C1C(H1Ca,H1Cb,H1Cc)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.843417(14) 0.303580(11) 0.801886(12) 0.02170(9) Uani 1 1 d . . .
P1 P 0.68783(5) 0.27631(4) 0.75090(4) 0.02150(16) Uani 1 1 d . . .
P2 P 0.93266(5) 0.25990(4) 0.70978(4) 0.02295(17) Uani 1 1 d . . .
Si1 Si 0.80355(6) 0.34706(4) 0.91654(5) 0.02674(19) Uani 1 1 d . . .
C38 C 0.8920(2) 0.13375(16) 0.61762(18) 0.0283(6) Uani 1 1 d . . .
H38A H 0.8297 0.1362 0.6249 0.034 Uiso 1 1 calc R . .
H38B H 0.8916 0.1603 0.5675 0.034 Uiso 1 1 calc R . .
C12 C 0.6200(2) 0.30596(15) 0.82091(19) 0.0251(6) Uani 1 1 d . . .
C25 C 1.0277(2) 0.29566(15) 0.79366(19) 0.0260(7) Uani 1 1 d . . .
C11 C 0.5221(2) 0.30361(16) 0.7998(2) 0.0301(7) Uani 1 1 d . . .
H11 H 0.4880 0.2858 0.7479 0.036 Uiso 1 1 calc R . .
C26 C 1.1249(2) 0.29507(17) 0.8062(2) 0.0321(7) Uani 1 1 d . . .
H26 H 1.1507 0.2726 0.7682 0.039 Uiso 1 1 calc R . .
C42 C 0.9689(2) 0.12369(16) 0.77300(18) 0.0282(6) Uani 1 1 d . . .
H42A H 1.0158 0.1443 0.8201 0.034 Uiso 1 1 calc R . .
H42B H 0.9092 0.1251 0.7856 0.034 Uiso 1 1 calc R . .
C2 C 0.8670(3) 0.29998(19) 1.0173(2) 0.0395(8) Uani 1 1 d . . .
H2A H 0.9331 0.3114 1.0305 0.047 Uiso 1 1 calc R . .
H2B H 0.8442 0.3184 1.0624 0.047 Uiso 1 1 calc R . .
C39 C 0.9167(2) 0.05666(17) 0.60637(19) 0.0322(7) Uani 1 1 d . . .
H39A H 0.8687 0.0360 0.5602 0.039 Uiso 1 1 calc R . .
H39B H 0.9755 0.0547 0.5922 0.039 Uiso 1 1 calc R . .
C30 C 0.9854(2) 0.32719(16) 0.84967(18) 0.0264(6) Uani 1 1 d . . .
C40 C 0.9250(2) 0.01394(17) 0.68542(19) 0.0326(7) Uani 1 1 d . . .
H40A H 0.9451 -0.0337 0.6775 0.039 Uiso 1 1 calc R . .
H40B H 0.8641 0.0109 0.6955 0.039 Uiso 1 1 calc R . .
C10 C 0.4760(2) 0.32789(18) 0.8562(2) 0.0338(7) Uani 1 1 d . . .
H10 H 0.4110 0.3269 0.8420 0.041 Uiso 1 1 calc R . .
C8 C 0.6238(2) 0.35697(17) 0.95447(19) 0.0316(7) Uani 1 1 d . . .
H8 H 0.6573 0.3746 1.0066 0.038 Uiso 1 1 calc R . .
C7 C 0.6725(2) 0.33406(16) 0.89810(18) 0.0264(6) Uani 1 1 d . . .
C27 C 1.1815(2) 0.32863(18) 0.8765(2) 0.0352(7) Uani 1 1 d . . .
H27 H 1.2462 0.3284 0.8866 0.042 Uiso 1 1 calc R . .
C29 C 1.0451(2) 0.36215(17) 0.91921(19) 0.0302(7) Uani 1 1 d . . .
H29 H 1.0199 0.3852 0.9573 0.036 Uiso 1 1 calc R . .
C37 C 0.9625(2) 0.16721(16) 0.69399(17) 0.0249(6) Uani 1 1 d . . .
H37 H 1.0241 0.1667 0.6838 0.030 Uiso 1 1 calc R . .
C32 C 1.0204(2) 0.29262(17) 0.5818(2) 0.0325(7) Uani 1 1 d . . .
H32A H 1.0749 0.3109 0.6235 0.039 Uiso 1 1 calc R . .
H32B H 1.0295 0.2423 0.5760 0.039 Uiso 1 1 calc R . .
C31 C 0.9335(2) 0.30460(15) 0.61137(19) 0.0268(7) Uani 1 1 d . . .
H31 H 0.8802 0.2860 0.5673 0.032 Uiso 1 1 calc R . .
C19 C 0.6266(2) 0.31720(15) 0.64913(17) 0.0240(6) Uani 1 1 d . . .
H19 H 0.5600 0.3051 0.6360 0.029 Uiso 1 1 calc R . .
C20 C 0.6636(2) 0.28976(17) 0.57807(18) 0.0291(7) Uani 1 1 d . . .
H20A H 0.6514 0.2394 0.5710 0.035 Uiso 1 1 calc R . .
H20B H 0.7308 0.2967 0.5930 0.035 Uiso 1 1 calc R . .
C14 C 0.7068(2) 0.13889(16) 0.81677(19) 0.0291(7) Uani 1 1 d . . .
H14A H 0.7718 0.1520 0.8413 0.035 Uiso 1 1 calc R . .
H14B H 0.6726 0.1507 0.8567 0.035 Uiso 1 1 calc R . .
C41 C 0.9947(2) 0.04705(17) 0.76178(19) 0.0312(7) Uani 1 1 d . . .
H41A H 0.9952 0.0202 0.8117 0.037 Uiso 1 1 calc R . .
H41B H 1.0571 0.0452 0.7547 0.037 Uiso 1 1 calc R . .
C15 C 0.7001(2) 0.05954(17) 0.7998(2) 0.0351(7) Uani 1 1 d . . .
H15A H 0.7218 0.0345 0.8528 0.042 Uiso 1 1 calc R . .
H15B H 0.7412 0.0471 0.7659 0.042 Uiso 1 1 calc R . .
C24 C 0.6359(2) 0.39755(16) 0.65707(18) 0.0288(7) Uani 1 1 d . . .
H24A H 0.6077 0.4138 0.6998 0.035 Uiso 1 1 calc R . .
H24B H 0.7017 0.4102 0.6749 0.035 Uiso 1 1 calc R . .
C36 C 0.9163(2) 0.38411(16) 0.6178(2) 0.0309(7) Uani 1 1 d . . .
H36A H 0.8596 0.3912 0.6346 0.037 Uiso 1 1 calc R . .
H36B H 0.9680 0.4048 0.6606 0.037 Uiso 1 1 calc R . .
C1 C 0.8240(2) 0.44442(18) 0.9402(2) 0.0379(8) Uani 1 1 d . . .
H1A H 0.8897 0.4545 0.9527 0.057 Uiso 1 1 calc R . .
H1B H 0.8024 0.4566 0.9877 0.057 Uiso 1 1 calc R . .
H1C H 0.7904 0.4716 0.8923 0.057 Uiso 1 1 calc R . .
C13 C 0.6666(2) 0.18064(16) 0.73546(18) 0.0244(6) Uani 1 1 d . . .
H13 H 0.7016 0.1653 0.6967 0.029 Uiso 1 1 calc R . .
C23 C 0.5886(2) 0.43461(17) 0.57412(19) 0.0338(7) Uani 1 1 d . . .
H23A H 0.5217 0.4261 0.5591 0.041 Uiso 1 1 calc R . .
H23B H 0.5989 0.4852 0.5807 0.041 Uiso 1 1 calc R . .
C3 C 0.8569(2) 0.22194(19) 1.0157(2) 0.0344(7) Uani 1 1 d . . .
H3 H 0.8798 0.1986 0.9763 0.041 Uiso 1 1 calc R . .
C9 C 0.5274(2) 0.35381(17) 0.9340(2) 0.0348(7) Uani 1 1 d . . .
H9 H 0.4966 0.3690 0.9725 0.042 Uiso 1 1 calc R . .
C18 C 0.5645(2) 0.15776(17) 0.6955(2) 0.0364(8) Uani 1 1 d . . .
H18A H 0.5277 0.1682 0.7338 0.044 Uiso 1 1 calc R . .
H18B H 0.5384 0.1843 0.6442 0.044 Uiso 1 1 calc R . .
C28 C 1.1413(2) 0.36264(17) 0.9317(2) 0.0338(7) Uani 1 1 d . . .
H28 H 1.1795 0.3862 0.9779 0.041 Uiso 1 1 calc R . .
C21 C 0.6179(2) 0.32756(18) 0.49507(18) 0.0322(7) Uani 1 1 d . . .
H21A H 0.6471 0.3117 0.4529 0.039 Uiso 1 1 calc R . .
H21B H 0.5521 0.3151 0.4761 0.039 Uiso 1 1 calc R . .
C22 C 0.6275(2) 0.40767(17) 0.50425(19) 0.0344(7) Uani 1 1 d . . .
H22A H 0.6930 0.4206 0.5166 0.041 Uiso 1 1 calc R . .
H22B H 0.5942 0.4299 0.4517 0.041 Uiso 1 1 calc R . .
C16 C 0.6006(2) 0.03552(18) 0.7547(2) 0.0379(8) Uani 1 1 d . . .
H16A H 0.6014 -0.0140 0.7395 0.045 Uiso 1 1 calc R . .
H16B H 0.5615 0.0403 0.7922 0.045 Uiso 1 1 calc R . .
C33 C 1.0111(3) 0.32913(19) 0.4979(2) 0.0384(8) Uani 1 1 d . . .
H33A H 0.9603 0.3077 0.4549 0.046 Uiso 1 1 calc R . .
H33B H 1.0684 0.3226 0.4819 0.046 Uiso 1 1 calc R . .
C17 C 0.5593(2) 0.07906(18) 0.6760(2) 0.0401(8) Uani 1 1 d . . .
H17A H 0.4945 0.0656 0.6514 0.048 Uiso 1 1 calc R . .
H17B H 0.5932 0.0692 0.6353 0.048 Uiso 1 1 calc R . .
C35 C 0.9066(3) 0.42095(18) 0.5342(2) 0.0393(8) Uani 1 1 d . . .
H35A H 0.8511 0.4035 0.4928 0.047 Uiso 1 1 calc R . .
H35B H 0.8988 0.4714 0.5407 0.047 Uiso 1 1 calc R . .
C4 C 0.8198(2) 0.1807(2) 1.0626(2) 0.0479(10) Uani 1 1 d . . .
C34 C 0.9921(3) 0.40804(18) 0.5032(2) 0.0411(8) Uani 1 1 d . . .
H34A H 1.0462 0.4305 0.5412 0.049 Uiso 1 1 calc R . .
H34B H 0.9821 0.4293 0.4482 0.049 Uiso 1 1 calc R . .
C5 C 0.7816(3) 0.2104(3) 1.1308(3) 0.0772(17) Uani 1 1 d . . .
H5A H 0.8143 0.2532 1.1523 0.116 Uiso 1 1 calc R . .
H5B H 0.7902 0.1765 1.1754 0.116 Uiso 1 1 calc R . .
H5C H 0.7161 0.2204 1.1080 0.116 Uiso 1 1 calc R . .
C6 C 0.8106(4) 0.1022(3) 1.0495(3) 0.0776(16) Uani 1 1 d . . .
H6A H 0.7456 0.0894 1.0333 0.116 Uiso 1 1 calc R . .
H6B H 0.8422 0.0784 1.1007 0.116 Uiso 1 1 calc R . .
H6C H 0.8381 0.0886 1.0060 0.116 Uiso 1 1 calc R . .
C1A C 1.3048(4) 0.4932(3) 0.8570(3) 0.0719(13) Uani 1 1 d DU A 1
H1AA H 1.3166 0.5431 0.8632 0.108 Uiso 1 1 calc R A 1
H1AB H 1.3630 0.4680 0.8741 0.108 Uiso 1 1 calc R A 1
H1AC H 1.2659 0.4791 0.8915 0.108 Uiso 1 1 calc R A 1
C1B C 1.2559(4) 0.4767(3) 0.7665(3) 0.0743(13) Uani 1 1 d DU A 1
H1BA H 1.2939 0.4930 0.7316 0.089 Uiso 1 1 calc R A 1
H1BB H 1.2486 0.4259 0.7596 0.089 Uiso 1 1 calc R A 1
C1C C 1.2263(4) 0.6301(3) 0.7047(4) 0.0928(19) Uani 1 1 d DU A 1
H1CA H 1.2193 0.6105 0.6499 0.139 Uiso 1 1 calc R A 1
H1CB H 1.2900 0.6248 0.7382 0.139 Uiso 1 1 calc R A 1
H1CC H 1.2102 0.6794 0.6996 0.139 Uiso 1 1 calc R A 1
C1D C 1.1626(4) 0.5918(3) 0.7459(5) 0.107(2) Uani 1 1 d DU A 1
H1DA H 1.0992 0.6085 0.7212 0.128 Uiso 1 1 calc R A 1
H1DB H 1.1803 0.6045 0.8050 0.128 Uiso 1 1 calc R A 1
C1W C 1.1630(3) 0.5107(3) 0.7390(4) 0.0797(15) Uani 1 1 d DU A 1
H1WA H 1.1244 0.4915 0.7721 0.096 Uiso 1 1 calc R A 1
H1WB H 1.1338 0.4978 0.6809 0.096 Uiso 1 1 calc R A 1


_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 2.2896(7) . ?
Pd1 P2 2.4370(7) . ?
Pd1 Si1 2.3007(8) . ?
Pd1 C30 2.085(3) . ?
P1 C12 1.831(3) . ?
P1 C19 1.847(3) . ?
P1 C13 1.842(3) . ?
P2 C25 1.813(3) . ?
P2 C37 1.845(3) . ?
P2 C31 1.843(3) . ?
Si1 C2 1.895(3) . ?
Si1 C7 1.905(3) . ?
Si1 C1 1.889(3) . ?
C38 C39 1.528(4) . ?
C38 C37 1.535(4) . ?
C12 C11 1.400(5) . ?
C12 C7 1.403(4) . ?
C25 C26 1.402(5) . ?
C25 C30 1.397(5) . ?
C11 C10 1.387(5) . ?
C26 C27 1.385(5) . ?
C42 C37 1.528(4) . ?
C42 C41 1.524(4) . ?
C2 C3 1.483(5) . ?
C39 C40 1.516(4) . ?
C30 C29 1.407(4) . ?
C40 C41 1.527(4) . ?
C10 C9 1.392(5) . ?
C8 C7 1.404(4) . ?
C8 C9 1.381(5) . ?
C27 C28 1.386(5) . ?
C29 C28 1.388(5) . ?
C32 C31 1.526(4) . ?
C32 C33 1.525(4) . ?
C31 C36 1.534(4) . ?
C19 C20 1.528(4) . ?
C19 C24 1.528(4) . ?
C20 C21 1.530(4) . ?
C14 C15 1.525(5) . ?
C14 C13 1.532(4) . ?
C15 C16 1.529(5) . ?
C24 C23 1.528(4) . ?
C36 C35 1.523(4) . ?
C13 C18 1.538(4) . ?
C23 C22 1.524(5) . ?
C3 C4 1.329(5) . ?
C18 C17 1.521(5) . ?
C21 C22 1.525(5) . ?
C16 C17 1.519(5) . ?
C33 C34 1.526(5) . ?
C35 C34 1.522(5) . ?
C4 C5 1.512(7) . ?
C4 C6 1.501(7) . ?
C1A C1B 1.505(6) . ?
C1B C1W 1.476(6) . ?
C1C C1D 1.504(8) . ?
C1D C1W 1.539(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
P1 Pd1 P2 111.50(3) . . ?
P1 Pd1 Si1 85.12(3) . . ?
Si1 Pd1 P2 162.71(3) . . ?
C30 Pd1 P1 179.13(8) . . ?
C30 Pd1 P2 68.71(9) . . ?
C30 Pd1 Si1 94.60(9) . . ?
C12 P1 Pd1 112.28(10) . . ?
C12 P1 C19 103.54(14) . . ?
C12 P1 C13 106.56(14) . . ?
C19 P1 Pd1 115.46(11) . . ?
C13 P1 Pd1 112.87(9) . . ?
C13 P1 C19 105.25(13) . . ?
C25 P2 Pd1 80.67(11) . . ?
C25 P2 C37 107.25(13) . . ?
C25 P2 C31 108.06(14) . . ?
C37 P2 Pd1 127.38(10) . . ?
C31 P2 Pd1 122.87(10) . . ?
C31 P2 C37 104.33(13) . . ?
C2 Si1 Pd1 112.42(12) . . ?
C2 Si1 C7 108.29(15) . . ?
C7 Si1 Pd1 108.29(9) . . ?
C1 Si1 Pd1 117.14(11) . . ?
C1 Si1 C2 105.28(15) . . ?
C1 Si1 C7 104.90(14) . . ?
C39 C38 C37 111.2(3) . . ?
C11 C12 P1 123.6(2) . . ?
C11 C12 C7 120.8(3) . . ?
C7 C12 P1 115.5(2) . . ?
C26 C25 P2 131.3(3) . . ?
C30 C25 P2 105.6(2) . . ?
C30 C25 C26 123.1(3) . . ?
C10 C11 C12 120.0(3) . . ?
C27 C26 C25 118.5(3) . . ?
C41 C42 C37 111.3(3) . . ?
C3 C2 Si1 115.4(2) . . ?
C40 C39 C38 111.5(3) . . ?
C25 C30 Pd1 104.8(2) . . ?
C25 C30 C29 116.5(3) . . ?
C29 C30 Pd1 138.6(2) . . ?
C39 C40 C41 111.7(3) . . ?
C11 C10 C9 119.8(3) . . ?
C9 C8 C7 121.3(3) . . ?
C12 C7 Si1 118.4(2) . . ?
C12 C7 C8 117.8(3) . . ?
C8 C7 Si1 123.5(2) . . ?
C26 C27 C28 119.7(3) . . ?
C28 C29 C30 120.8(3) . . ?
C38 C37 P2 111.9(2) . . ?
C42 C37 P2 110.4(2) . . ?
C42 C37 C38 110.4(2) . . ?
C33 C32 C31 111.1(3) . . ?
C32 C31 P2 115.9(2) . . ?
C32 C31 C36 110.0(3) . . ?
C36 C31 P2 110.1(2) . . ?
C20 C19 P1 111.8(2) . . ?
C20 C19 C24 111.1(3) . . ?
C24 C19 P1 109.2(2) . . ?
C19 C20 C21 111.8(3) . . ?
C15 C14 C13 110.8(3) . . ?
C42 C41 C40 110.8(3) . . ?
C14 C15 C16 112.7(3) . . ?
C23 C24 C19 111.8(2) . . ?
C35 C36 C31 111.0(3) . . ?
C14 C13 P1 112.0(2) . . ?
C14 C13 C18 109.1(3) . . ?
C18 C13 P1 116.5(2) . . ?
C22 C23 C24 110.8(3) . . ?
C4 C3 C2 129.1(4) . . ?
C8 C9 C10 120.2(3) . . ?
C17 C18 C13 110.6(3) . . ?
C27 C28 C29 121.2(3) . . ?
C22 C21 C20 111.6(3) . . ?
C23 C22 C21 111.3(3) . . ?
C17 C16 C15 111.1(3) . . ?
C32 C33 C34 111.1(3) . . ?
C16 C17 C18 111.3(3) . . ?
C34 C35 C36 111.2(3) . . ?
C3 C4 C5 121.9(4) . . ?
C3 C4 C6 122.1(4) . . ?
C6 C4 C5 116.0(4) . . ?
C35 C34 C33 111.3(3) . . ?
C1W C1B C1A 111.4(5) . . ?
C1C C1D C1W 115.5(6) . . ?
C1B C1W C1D 115.7(5) . . ?

_database_code_depnum_ccdc_archive 'CCDC 997343'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_s12071
_audit_creation_date             2013-04-16
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr  9 2013 14:10:59, GUI svn.r4458)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C43 H64 O2 P2 Pd Si'
_chemical_formula_sum            'C43 H64 O2 P2 Pd Si'
_chemical_formula_weight         809.37
_chemical_melting_point          ?
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'
Pd Pd -0.9988 1.0072 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6994(16)
_cell_length_b                   25.260(3)
_cell_length_c                   13.3608(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.432(7)
_cell_angle_gamma                90.00
_cell_volume                     4131.5(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17181
_cell_measurement_temperature    93
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   'Jacobson, R (1998) Private Communication'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.1550
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            59463
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         3.05
_diffrn_ambient_temperature      93
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: 20.0000 - 200.0000
	     Image width: 1.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 45.0000
	             Phi: 270.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 165
	           Slice: 20.0000 - 185.0000
	     Image width: 1.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 30.0000
	             Phi: 270.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 116
	           Slice: 20.0000 - 136.0000
	     Image width: 1.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: 0.0000
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.010581
_diffrn_orient_matrix_UB_12      -0.039237
_diffrn_orient_matrix_UB_13      -0.004897
_diffrn_orient_matrix_UB_21      -0.043899
_diffrn_orient_matrix_UB_22      0.001782
_diffrn_orient_matrix_UB_23      0.051927
_diffrn_orient_matrix_UB_31      -0.068074
_diffrn_orient_matrix_UB_32      0.004949
_diffrn_orient_matrix_UB_33      -0.057519
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_number_gt                5442
_reflns_number_total             6568
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6568
_refine_ls_number_restraints     115
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0597
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0316P)²+6.1079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1191
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C2 \\sim C2-C3A
 with sigma of 0.02
 C3A-C2 \\sim C2-C3
 with sigma of 0.02
 C3-C2 \\sim C2-C4A
 with sigma of 0.02
 C5A-C2 \\sim C2-C5
 with sigma of 0.02
 C6A-C5A \\sim C5-C6
 with sigma of 0.02
3. Rigid bond restraints
 C6A, C5A, C4, C2, C3A, C3, C4A, C6, C5, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C6A \\sim C5A \\sim C4 \\sim C3A \\sim C2 \\sim C3 \\sim C4A \\sim C5 \\sim C6 \\sim C1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C3A) = Uanis(C2) = Uanis(C5A)
5. Others
 1*Sof(C6A)=1*Sof(H6AC)=1*Sof(H6AD)=1-1*Sof(C5)=1-1*Sof(H5A)=1-1*Sof(C3)=1-1*
 Sof(H3AA)=1-1*Sof(H3AB)=1-1*Sof(H3AC)=1-1*Sof(C6)=1-1*Sof(H6AA)=1-1*Sof(H6AB)=
 1-1*Sof(C4)=1-1*Sof(H4AA)=1-1*Sof(H4AB)=1-1*Sof(H4AC)=1*Sof(C3A)=1*Sof(H3AD)=1*
 Sof(H3AE)=1*Sof(H3AF)=1*Sof(C5A)=1*Sof(H5AA)=1*Sof(C4A)=1*Sof(H4AD)=1*
 Sof(H4AE)=1*Sof(H4AF)
6.a Ternary CH refined with riding coordinates:
 C38(H38), C14(H14), C32(H32), C8(H8)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C16(H16A,H16B), C18(H18A,H18B), C36(H36A,H36B), C11(H11A,
 H11B), C42(H42A,H42B), C39(H39A,H39B), C34(H34A,H34B), C13(H13A,H13B),
 C15(H15A,H15B), C43(H43A,H43B), C41(H41A,H41B), C9(H9A,H9B), C33(H33A,H33B),
 C37(H37A,H37B), C35(H35A,H35B), C19(H19A,H19B), C40(H40A,H40B), C17(H17A,H17B),
  C12(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C27(H27), C28(H28), C29(H29), C23(H23), C24(H24), C21(H21),
 C22(H22), C5(H5A), C5A(H5AA)
6.d X=CH2 refined with riding coordinates:
 C6A(H6AC,H6AD), C6(H6AA,H6AB)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C3(H3AA,H3AB,H3AC), C4(H4AA,H4AB,H4AC), C3A(H3AD,H3AE,H3AF),
 C4A(H4AD,H4AE,H4AF)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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 0.83635(3) 0.356961(13) 0.80283(3) 0.02644(13) Uani 1 1 d . . .
P1 P 0.97444(10) 0.29646(5) 0.86006(10) 0.0289(3) Uani 1 1 d . . .
P2 P 0.72796(10) 0.43031(5) 0.80412(9) 0.0271(3) Uani 1 1 d . . .
Si1 Si 0.79549(11) 0.33591(5) 0.95243(10) 0.0277(3) Uani 1 1 d . . .
C31 C 0.6969(3) 0.43675(17) 0.9296(3) 0.0264(11) Uani 1 1 d . . .
O2 O 0.7365(3) 0.34373(16) 0.5713(3) 0.0652(12) Uani 1 1 d . . .
O1 O 0.8933(3) 0.37405(13) 0.6663(2) 0.0382(8) Uani 1 1 d . . .
C38 C 0.5981(4) 0.42803(18) 0.7013(3) 0.0308(11) Uani 1 1 d . . .
H38 H 0.6187 0.4248 0.6358 0.037 Uiso 1 1 calc R . .
C30 C 0.6443(4) 0.48033(19) 0.9582(4) 0.0331(12) Uani 1 1 d . . .
H30 H 0.6214 0.5079 0.9114 0.040 Uiso 1 1 calc R . .
C26 C 0.7329(3) 0.39517(17) 1.0003(4) 0.0277(11) Uani 1 1 d . . .
C10 C 1.1944(4) 0.41448(19) 0.8403(4) 0.0449(14) Uani 1 1 d . . .
H10A H 1.2043 0.4495 0.8712 0.054 Uiso 1 1 calc R . .
H10B H 1.1692 0.4187 0.7655 0.054 Uiso 1 1 calc R . .
C27 C 0.7106(4) 0.39854(19) 1.0964(4) 0.0366(12) Uani 1 1 d . . .
H27 H 0.7311 0.3708 1.1432 0.044 Uiso 1 1 calc R . .
C16 C 0.9001(5) 0.13719(19) 0.7968(4) 0.0481(15) Uani 1 1 d . . .
H16A H 0.9709 0.1222 0.8309 0.058 Uiso 1 1 calc R . .
H16B H 0.8445 0.1152 0.8134 0.058 Uiso 1 1 calc R . .
C14 C 0.9762(4) 0.22955(17) 0.8085(4) 0.0315(11) Uani 1 1 d . . .
H14 H 1.0489 0.2147 0.8392 0.038 Uiso 1 1 calc R . .
C18 C 0.9660(5) 0.1740(2) 0.6499(5) 0.0529(16) Uani 1 1 d . . .
H18A H 0.9509 0.1749 0.5748 0.063 Uiso 1 1 calc R . .
H18B H 1.0394 0.1604 0.6778 0.063 Uiso 1 1 calc R . .
C32 C 0.7891(4) 0.49484(18) 0.7881(4) 0.0300(11) Uani 1 1 d . . .
H32 H 0.7348 0.5223 0.7885 0.036 Uiso 1 1 calc R . .
C36 C 0.8748(4) 0.54903(19) 0.6712(4) 0.0399(13) Uani 1 1 d . . .
H36A H 0.8251 0.5786 0.6674 0.048 Uiso 1 1 calc R . .
H36B H 0.8960 0.5477 0.6066 0.048 Uiso 1 1 calc R . .
C11 C 1.3038(4) 0.3852(2) 0.8680(4) 0.0427(13) Uani 1 1 d . . .
H11A H 1.3555 0.4040 0.8390 0.051 Uiso 1 1 calc R . .
H11B H 1.3330 0.3843 0.9429 0.051 Uiso 1 1 calc R . .
C28 C 0.6589(4) 0.4418(2) 1.1244(4) 0.0385(13) Uani 1 1 d . . .
H28 H 0.6461 0.4434 1.1898 0.046 Uiso 1 1 calc R . .
C42 C 0.4397(4) 0.3699(2) 0.6170(4) 0.0490(15) Uani 1 1 d . . .
H42A H 0.4659 0.3643 0.5560 0.059 Uiso 1 1 calc R . .
H42B H 0.3994 0.3386 0.6269 0.059 Uiso 1 1 calc R . .
C39 C 0.5218(4) 0.4759(2) 0.6878(4) 0.0411(13) Uani 1 1 d . . .
H39A H 0.5613 0.5077 0.6791 0.049 Uiso 1 1 calc R . .
H39B H 0.4956 0.4802 0.7491 0.049 Uiso 1 1 calc R . .
C34 C 0.9458(4) 0.55758(19) 0.8627(4) 0.0394(13) Uani 1 1 d . . .
H34A H 0.8971 0.5870 0.8638 0.047 Uiso 1 1 calc R . .
H34B H 1.0112 0.5625 0.9192 0.047 Uiso 1 1 calc R . .
C2 C 0.8677(4) 0.3734(2) 0.4826(4) 0.0425(12) Uani 1 1 d DU . .
C13 C 1.2029(4) 0.29900(19) 0.8621(5) 0.0428(14) Uani 1 1 d . . .
H13A H 1.1928 0.2644 0.8293 0.051 Uiso 1 1 calc R . .
H13B H 1.2268 0.2938 0.9367 0.051 Uiso 1 1 calc R . .
C25 C 0.9238(4) 0.31022(17) 1.0457(4) 0.0302(11) Uani 1 1 d . . .
C8 C 1.0952(4) 0.32884(17) 0.8343(4) 0.0316(11) Uani 1 1 d . . .
H8 H 1.0768 0.3334 0.7588 0.038 Uiso 1 1 calc R . .
C29 C 0.6261(4) 0.48293(19) 1.0550(4) 0.0375(12) Uani 1 1 d . . .
H29 H 0.5918 0.5124 1.0737 0.045 Uiso 1 1 calc R . .
C23 C 1.0340(4) 0.2803(2) 1.2116(4) 0.0441(14) Uani 1 1 d . . .
H23 H 1.0462 0.2791 1.2834 0.053 Uiso 1 1 calc R . .
C20 C 1.0009(4) 0.28804(17) 0.9993(3) 0.0302(11) Uani 1 1 d . . .
C24 C 0.9428(4) 0.30592(19) 1.1523(4) 0.0370(12) Uani 1 1 d . . .
H24 H 0.8931 0.3206 1.1844 0.044 Uiso 1 1 calc R . .
C15 C 0.8926(4) 0.19290(18) 0.8369(4) 0.0396(13) Uani 1 1 d . . .
H15A H 0.9055 0.1920 0.9118 0.047 Uiso 1 1 calc R . .
H15B H 0.8196 0.2067 0.8074 0.047 Uiso 1 1 calc R . .
C43 C 0.5367(4) 0.37719(19) 0.7110(4) 0.0392(13) Uani 1 1 d . . .
H43A H 0.5856 0.3472 0.7169 0.047 Uiso 1 1 calc R . .
H43B H 0.5115 0.3786 0.7734 0.047 Uiso 1 1 calc R . .
C41 C 0.3635(4) 0.4173(2) 0.5990(4) 0.0527(16) Uani 1 1 d . . .
H41A H 0.3065 0.4123 0.5350 0.063 Uiso 1 1 calc R . .
H41B H 0.3291 0.4200 0.6555 0.063 Uiso 1 1 calc R . .
C9 C 1.1091(4) 0.38473(19) 0.8785(4) 0.0400(13) Uani 1 1 d . . .
H9A H 1.0400 0.4034 0.8575 0.048 Uiso 1 1 calc R . .
H9B H 1.1313 0.3831 0.9538 0.048 Uiso 1 1 calc R . .
C33 C 0.8898(4) 0.50573(17) 0.8793(4) 0.0335(12) Uani 1 1 d . . .
H33A H 0.8676 0.5079 0.9432 0.040 Uiso 1 1 calc R . .
H33B H 0.9411 0.4767 0.8858 0.040 Uiso 1 1 calc R . .
C1 C 0.8264(4) 0.36234(18) 0.5807(4) 0.0349(12) Uani 1 1 d U A .
C37 C 0.8173(4) 0.49786(19) 0.6849(4) 0.0363(12) Uani 1 1 d . . .
H37A H 0.7508 0.4947 0.6292 0.044 Uiso 1 1 calc R . .
H37B H 0.8640 0.4682 0.6796 0.044 Uiso 1 1 calc R . .
C7 C 0.6920(4) 0.28247(18) 0.9485(4) 0.0368(12) Uani 1 1 d . . .
H7A H 0.6233 0.2927 0.9023 0.055 Uiso 1 1 calc R . .
H7B H 0.6831 0.2772 1.0170 0.055 Uiso 1 1 calc R . .
H7C H 0.7165 0.2502 0.9243 0.055 Uiso 1 1 calc R . .
C35 C 0.9759(4) 0.5575(2) 0.7613(4) 0.0430(13) Uani 1 1 d . . .
H35A H 1.0284 0.5296 0.7618 0.052 Uiso 1 1 calc R . .
H35B H 1.0097 0.5910 0.7526 0.052 Uiso 1 1 calc R . .
C21 C 1.0904(4) 0.25977(18) 1.0602(4) 0.0348(12) Uani 1 1 d . . .
H21 H 1.1385 0.2431 1.0287 0.042 Uiso 1 1 calc R . .
C19 C 0.9583(4) 0.23015(18) 0.6911(4) 0.0398(13) Uani 1 1 d . . .
H19A H 1.0129 0.2525 0.6735 0.048 Uiso 1 1 calc R . .
H19B H 0.8869 0.2449 0.6584 0.048 Uiso 1 1 calc R . .
C22 C 1.1074(4) 0.25655(18) 1.1659(4) 0.0365(13) Uani 1 1 d . . .
H22 H 1.1677 0.2385 1.2063 0.044 Uiso 1 1 calc R . .
C40 C 0.4248(4) 0.4677(2) 0.5921(4) 0.0487(15) Uani 1 1 d . . .
H40A H 0.3752 0.4975 0.5856 0.058 Uiso 1 1 calc R . .
H40B H 0.4512 0.4666 0.5304 0.058 Uiso 1 1 calc R . .
C17 C 0.8848(5) 0.1374(2) 0.6808(5) 0.0586(17) Uani 1 1 d . . .
H17A H 0.8111 0.1489 0.6465 0.070 Uiso 1 1 calc R . .
H17B H 0.8939 0.1017 0.6576 0.070 Uiso 1 1 calc R . .
C12 C 1.2900(4) 0.3297(2) 0.8264(5) 0.0480(14) Uani 1 1 d . . .
H12A H 1.3592 0.3111 0.8493 0.058 Uiso 1 1 calc R . .
H12B H 1.2700 0.3308 0.7511 0.058 Uiso 1 1 calc R . .
C6A C 1.0678(18) 0.3428(9) 0.5057(17) 0.072(6) Uani 0.305(7) 1 d PDU A 2
H6AC H 1.0466 0.3125 0.4658 0.086 Uiso 0.305(7) 1 calc PR A 2
H6AD H 1.1415 0.3497 0.5347 0.086 Uiso 0.305(7) 1 calc PR A 2
C5 C 0.8973(7) 0.4322(3) 0.4835(6) 0.039(2) Uani 0.695(7) 1 d PDU A 1
H5A H 0.9509 0.4438 0.5412 0.047 Uiso 0.695(7) 1 calc PR A 1
C3 C 0.7760(8) 0.3611(4) 0.3858(6) 0.071(3) Uani 0.695(7) 1 d PDU A 1
H3AA H 0.7548 0.3247 0.3874 0.106 Uiso 0.695(7) 1 calc PR A 1
H3AB H 0.8010 0.3673 0.3251 0.106 Uiso 0.695(7) 1 calc PR A 1
H3AC H 0.7145 0.3835 0.3841 0.106 Uiso 0.695(7) 1 calc PR A 1
C6 C 0.8575(7) 0.4674(3) 0.4147(7) 0.057(2) Uani 0.695(7) 1 d PDU A 1
H6AA H 0.8036 0.4582 0.3552 0.068 Uiso 0.695(7) 1 calc PR A 1
H6AB H 0.8825 0.5022 0.4243 0.068 Uiso 0.695(7) 1 calc PR A 1
C4 C 0.9671(9) 0.3407(4) 0.4866(8) 0.077(3) Uani 0.695(7) 1 d PDU A 1
H4AA H 1.0247 0.3507 0.5461 0.116 Uiso 0.695(7) 1 calc PR A 1
H4AB H 0.9902 0.3465 0.4247 0.116 Uiso 0.695(7) 1 calc PR A 1
H4AC H 0.9501 0.3039 0.4917 0.116 Uiso 0.695(7) 1 calc PR A 1
C3A C 0.8378(16) 0.3262(6) 0.4112(12) 0.0425(12) Uani 0.305(7) 1 d PDU A 2
H3AD H 0.8785 0.2959 0.4432 0.064 Uiso 0.305(7) 1 calc PR A 2
H3AE H 0.8548 0.3337 0.3468 0.064 Uiso 0.305(7) 1 calc PR A 2
H3AF H 0.7611 0.3192 0.3981 0.064 Uiso 0.305(7) 1 calc PR A 2
C5A C 0.9956(12) 0.3747(8) 0.5208(13) 0.0425(12) Uani 0.305(7) 1 d PDU A 2
H5AA H 1.0238 0.4039 0.5615 0.051 Uiso 0.305(7) 1 calc PR A 2
C4A C 0.827(2) 0.4249(7) 0.4358(16) 0.058(5) Uani 0.305(7) 1 d PDU A 2
H4AD H 0.7489 0.4249 0.4165 0.088 Uiso 0.305(7) 1 calc PR A 2
H4AE H 0.8529 0.4307 0.3753 0.088 Uiso 0.305(7) 1 calc PR A 2
H4AF H 0.8538 0.4526 0.4852 0.088 Uiso 0.305(7) 1 calc PR A 2


_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 2.2983(13) . ?
Pd1 P2 2.3110(13) . ?
Pd1 Si1 2.2581(14) . ?
Pd1 O1 2.177(3) . ?
P1 C14 1.828(4) . ?
P1 C8 1.849(5) . ?
P1 C20 1.814(5) . ?
P2 C31 1.829(5) . ?
P2 C38 1.845(4) . ?
P2 C32 1.842(4) . ?
Si1 C26 1.885(5) . ?
Si1 C25 1.884(5) . ?
Si1 C7 1.875(5) . ?
C31 C30 1.393(6) . ?
C31 C26 1.405(6) . ?
O2 C1 1.210(6) . ?
O1 C1 1.266(6) . ?
C38 C39 1.530(6) . ?
C38 C43 1.526(6) . ?
C30 C29 1.374(7) . ?
C26 C27 1.389(6) . ?
C10 C11 1.530(7) . ?
C10 C9 1.515(7) . ?
C27 C28 1.377(6) . ?
C16 C15 1.518(6) . ?
C16 C17 1.510(8) . ?
C14 C15 1.532(6) . ?
C14 C19 1.523(6) . ?
C18 C19 1.535(6) . ?
C18 C17 1.520(7) . ?
C32 C33 1.538(6) . ?
C32 C37 1.515(6) . ?
C36 C37 1.520(6) . ?
C36 C35 1.524(7) . ?
C11 C12 1.503(7) . ?
C28 C29 1.381(7) . ?
C42 C43 1.518(7) . ?
C42 C41 1.516(7) . ?
C39 C40 1.535(7) . ?
C34 C33 1.534(6) . ?
C34 C35 1.502(7) . ?
C2 C1 1.561(7) . ?
C2 C5 1.531(9) . ?
C2 C3 1.525(8) . ?
C2 C4 1.497(9) . ?
C2 C3A 1.510(12) . ?
C2 C5A 1.567(15) . ?
C2 C4A 1.475(13) . ?
C13 C8 1.519(6) . ?
C13 C12 1.527(7) . ?
C25 C20 1.406(6) . ?
C25 C24 1.384(6) . ?
C8 C9 1.523(6) . ?
C23 C24 1.377(7) . ?
C23 C22 1.381(7) . ?
C20 C21 1.404(6) . ?
C41 C40 1.508(7) . ?
C21 C22 1.373(7) . ?
C6A C5A 1.278(18) . ?
C5 C6 1.283(11) . ?

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 159.06(5) . . ?
Si1 Pd1 P1 83.32(5) . . ?
Si1 Pd1 P2 84.52(5) . . ?
O1 Pd1 P1 90.93(9) . . ?
O1 Pd1 P2 100.29(9) . . ?
O1 Pd1 Si1 173.83(9) . . ?
C14 P1 Pd1 125.06(16) . . ?
C14 P1 C8 104.2(2) . . ?
C8 P1 Pd1 103.95(15) . . ?
C20 P1 Pd1 109.62(16) . . ?
C20 P1 C14 105.1(2) . . ?
C20 P1 C8 107.9(2) . . ?
C31 P2 Pd1 110.62(15) . . ?
C31 P2 C38 108.5(2) . . ?
C31 P2 C32 103.2(2) . . ?
C38 P2 Pd1 112.66(15) . . ?
C32 P2 Pd1 115.98(16) . . ?
C32 P2 C38 105.2(2) . . ?
C26 Si1 Pd1 109.29(15) . . ?
C25 Si1 Pd1 107.71(16) . . ?
C25 Si1 C26 114.7(2) . . ?
C7 Si1 Pd1 117.99(16) . . ?
C7 Si1 C26 103.0(2) . . ?
C7 Si1 C25 104.3(2) . . ?
C30 C31 P2 123.9(4) . . ?
C30 C31 C26 120.0(4) . . ?
C26 C31 P2 116.0(3) . . ?
C1 O1 Pd1 114.7(3) . . ?
C39 C38 P2 118.4(3) . . ?
C43 C38 P2 109.8(3) . . ?
C43 C38 C39 110.7(4) . . ?
C29 C30 C31 120.6(5) . . ?
C31 C26 Si1 117.2(3) . . ?
C27 C26 Si1 124.8(4) . . ?
C27 C26 C31 117.8(4) . . ?
C9 C10 C11 111.3(4) . . ?
C28 C27 C26 121.9(5) . . ?
C17 C16 C15 110.8(4) . . ?
C15 C14 P1 112.7(3) . . ?
C19 C14 P1 111.4(3) . . ?
C19 C14 C15 109.7(4) . . ?
C17 C18 C19 110.6(4) . . ?
C33 C32 P2 110.7(3) . . ?
C37 C32 P2 111.1(3) . . ?
C37 C32 C33 111.3(4) . . ?
C37 C36 C35 110.8(4) . . ?
C12 C11 C10 110.6(4) . . ?
C27 C28 C29 119.6(5) . . ?
C41 C42 C43 112.3(4) . . ?
C38 C39 C40 109.5(4) . . ?
C35 C34 C33 111.6(4) . . ?
C1 C2 C5A 106.4(7) . . ?
C5 C2 C1 107.7(5) . . ?
C5 C2 C5A 75.3(8) . . ?
C3 C2 C1 108.9(5) . . ?
C3 C2 C5 109.6(6) . . ?
C3 C2 C5A 140.5(8) . . ?
C4 C2 C1 109.9(5) . . ?
C4 C2 C5 109.4(6) . . ?
C4 C2 C3 111.3(7) . . ?
C4 C2 C3A 69.8(9) . . ?
C4 C2 C5A 37.8(7) . . ?
C3A C2 C1 107.8(7) . . ?
C3A C2 C5 142.2(8) . . ?
C3A C2 C3 45.2(7) . . ?
C3A C2 C5A 106.7(11) . . ?
C4A C2 C1 110.9(8) . . ?
C4A C2 C5 37.3(10) . . ?
C4A C2 C3 73.7(11) . . ?
C4A C2 C4 134.2(10) . . ?
C4A C2 C3A 115.3(12) . . ?
C4A C2 C5A 109.4(13) . . ?
C8 C13 C12 110.6(4) . . ?
C20 C25 Si1 115.3(3) . . ?
C24 C25 Si1 126.2(4) . . ?
C24 C25 C20 118.1(4) . . ?
C13 C8 P1 118.2(3) . . ?
C13 C8 C9 111.1(4) . . ?
C9 C8 P1 110.8(3) . . ?
C30 C29 C28 120.0(5) . . ?
C24 C23 C22 120.8(5) . . ?
C25 C20 P1 116.4(3) . . ?
C21 C20 P1 123.7(4) . . ?
C21 C20 C25 119.9(4) . . ?
C23 C24 C25 121.3(5) . . ?
C16 C15 C14 111.1(4) . . ?
C42 C43 C38 110.6(4) . . ?
C40 C41 C42 111.0(4) . . ?
C10 C9 C8 110.4(4) . . ?
C34 C33 C32 111.0(4) . . ?
O2 C1 O1 124.9(5) . . ?
O2 C1 C2 120.2(5) . . ?
O1 C1 C2 114.9(4) . . ?
C32 C37 C36 113.0(4) . . ?
C34 C35 C36 110.5(4) . . ?
C22 C21 C20 120.5(5) . . ?
C14 C19 C18 110.7(4) . . ?
C21 C22 C23 119.3(5) . . ?
C41 C40 C39 112.1(4) . . ?
C16 C17 C18 111.7(5) . . ?
C11 C12 C13 112.4(4) . . ?
C6 C5 C2 128.2(8) . . ?
C6A C5A C2 131.3(19) . . ?

_database_code_depnum_ccdc_archive 'CCDC 997344'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_s13061
_audit_creation_date             2013-09-11
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C39 H60 P2 Pd Si'
_chemical_formula_sum            'C39 H60 P2 Pd Si'
_chemical_formula_weight         725.30
_chemical_melting_point          ?
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'
P P 0.1023 0.0942 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   9.374(4)
_cell_length_b                   17.3855(7)
_cell_length_c                   23.3068(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.572(13)
_cell_angle_gamma                90.00
_cell_volume                     3721.3(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    48806
_cell_measurement_temperature    153
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      3.1
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   'Jacobson, R (1998) Private Communication'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.1585
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            105636
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.11
_diffrn_ambient_temperature      153
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: -0.0267
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 120.0000
	             XTD: 127.4000
	          2theta: -0.0267
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: -0.0267
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 0.0000
	             XTD: 127.4000
	          2theta: -0.0267
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 240.0000
	             XTD: 127.4000
	          2theta: -0.0267
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 90.0000
	             XTD: 127.4000
	          2theta: -0.0267
scan:
	Number of images: 90
	           Slice: 20.0000 - 200.0000
	     Image width: 2.0000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: -0.0267
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.005042
_diffrn_orient_matrix_UB_12      0.035236
_diffrn_orient_matrix_UB_13      0.029214
_diffrn_orient_matrix_UB_21      0.108795
_diffrn_orient_matrix_UB_22      0.001769
_diffrn_orient_matrix_UB_23      0.101466
_diffrn_orient_matrix_UB_31      -0.000325
_diffrn_orient_matrix_UB_32      0.045428
_diffrn_orient_matrix_UB_33      -0.026610
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_number_gt                5295
_reflns_number_total             6343
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0629
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0258P)²+10.6936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1101
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C34(H34), C1(H1), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C8(H8A,H8B), C20(H20A,H20B), C10(H10A,H10B), C11(H11A,H11B),
 C37(H37A,H37B), C33(H33A,H33B), C29(H29A,H29B), C9(H9A,H9B), C31(H31A,H31B),
 C39(H39A,H39B), C2(H2A,H2B), C6(H6A,H6B), C12(H12A,H12B), C32(H32A,H32B),
 C30(H30A,H30B), C38(H38A,H38B), C36(H36A,H36B), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C24(H24), C26(H26), C17(H17), C16(H16), C14(H14), C23(H23), C15(H15)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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 0.73193(4) 0.28943(2) 0.861814(15) 0.02490(12) Uani 1 1 d . . .
P1 P 0.57467(13) 0.24633(7) 0.77104(5) 0.0270(3) Uani 1 1 d . . .
P2 P 0.74724(13) 0.20315(7) 0.93775(5) 0.0275(3) Uani 1 1 d . . .
Si1 Si 0.87225(16) 0.36905(8) 0.92952(6) 0.0333(3) Uani 1 1 d . . .
C27 C 0.8675(5) 0.2389(3) 1.0043(2) 0.0289(11) Uani 1 1 d . . .
C7 C 0.3753(5) 0.2586(3) 0.7588(2) 0.0289(11) Uani 1 1 d . . .
H7 H 0.3371 0.2635 0.7157 0.035 Uiso 1 1 calc R . .
C22 C 0.9206(5) 0.3133(3) 1.0012(2) 0.0306(12) Uani 1 1 d . . .
C35 C 0.5750(6) 0.1220(3) 1.0086(2) 0.0405(13) Uani 1 1 d . . .
H35A H 0.6226 0.0739 0.9997 0.049 Uiso 1 1 calc R . .
H35B H 0.6325 0.1434 1.0455 0.049 Uiso 1 1 calc R . .
C8 C 0.3359(5) 0.3320(3) 0.7886(2) 0.0332(12) Uani 1 1 d . . .
H8A H 0.3791 0.3299 0.8310 0.040 Uiso 1 1 calc R . .
H8B H 0.3769 0.3772 0.7718 0.040 Uiso 1 1 calc R . .
C21 C 1.0567(6) 0.4029(3) 0.9165(2) 0.0484(15) Uani 1 1 d . . .
H21A H 1.1191 0.3582 0.9143 0.073 Uiso 1 1 calc R . .
H21B H 1.1027 0.4362 0.9489 0.073 Uiso 1 1 calc R . .
H21C H 1.0430 0.4316 0.8796 0.073 Uiso 1 1 calc R . .
C20 C 0.7761(7) 0.4581(3) 0.9463(2) 0.0468(15) Uani 1 1 d . . .
H20A H 0.8414 0.4860 0.9783 0.056 Uiso 1 1 calc R . .
H20B H 0.7607 0.4917 0.9113 0.056 Uiso 1 1 calc R . .
C34 C 0.5721(5) 0.1799(3) 0.9587(2) 0.0304(11) Uani 1 1 d . . .
H34 H 0.5098 0.1561 0.9232 0.037 Uiso 1 1 calc R . .
C1 C 0.6034(5) 0.1655(3) 0.7237(2) 0.0326(12) Uani 1 1 d . . .
H1 H 0.5713 0.1181 0.7418 0.039 Uiso 1 1 calc R . .
C25 C 1.0033(6) 0.2256(3) 1.1033(2) 0.0418(14) Uani 1 1 d . . .
H25 H 1.0311 0.1959 1.1380 0.050 Uiso 1 1 calc R . .
C13 C 0.6416(5) 0.3348(3) 0.7448(2) 0.0281(11) Uani 1 1 d . . .
C24 C 1.0559(6) 0.2994(3) 1.1010(2) 0.0438(14) Uani 1 1 d . . .
H24 H 1.1201 0.3206 1.1339 0.053 Uiso 1 1 calc R . .
C26 C 0.9103(5) 0.1951(3) 1.0554(2) 0.0356(12) Uani 1 1 d . . .
H26 H 0.8750 0.1441 1.0570 0.043 Uiso 1 1 calc R . .
C10 C 0.1024(6) 0.2705(3) 0.8026(2) 0.0379(13) Uani 1 1 d . . .
H10A H 0.1367 0.2665 0.8455 0.045 Uiso 1 1 calc R . .
H10B H -0.0048 0.2768 0.7946 0.045 Uiso 1 1 calc R . .
C11 C 0.1407(5) 0.1973(3) 0.7736(2) 0.0368(12) Uani 1 1 d . . .
H11A H 0.0955 0.1985 0.7314 0.044 Uiso 1 1 calc R . .
H11B H 0.1007 0.1525 0.7914 0.044 Uiso 1 1 calc R . .
C37 C 0.3395(6) 0.1764(4) 1.0281(2) 0.0512(16) Uani 1 1 d . . .
H37A H 0.3863 0.1986 1.0663 0.061 Uiso 1 1 calc R . .
H37B H 0.2379 0.1630 1.0299 0.061 Uiso 1 1 calc R . .
C33 C 0.7308(6) 0.0599(3) 0.8800(2) 0.0365(13) Uani 1 1 d . . .
H33A H 0.7076 0.0894 0.8430 0.044 Uiso 1 1 calc R . .
H33B H 0.6382 0.0487 0.8926 0.044 Uiso 1 1 calc R . .
C18 C 0.7273(5) 0.3681(3) 0.7947(2) 0.0281(11) Uani 1 1 d . . .
C29 C 0.9776(5) 0.1205(3) 0.9113(2) 0.0352(12) Uani 1 1 d . . .
H29A H 0.9671 0.1526 0.8756 0.042 Uiso 1 1 calc R . .
H29B H 1.0413 0.1483 0.9436 0.042 Uiso 1 1 calc R . .
C9 C 0.1710(5) 0.3406(3) 0.7801(2) 0.0372(13) Uani 1 1 d . . .
H9A H 0.1479 0.3869 0.8011 0.045 Uiso 1 1 calc R . .
H9B H 0.1291 0.3477 0.7379 0.045 Uiso 1 1 calc R . .
C28 C 0.8272(5) 0.1086(3) 0.9266(2) 0.0297(11) Uani 1 1 d . . .
H28 H 0.8414 0.0799 0.9645 0.036 Uiso 1 1 calc R . .
C31 C 0.9516(6) -0.0028(3) 0.8535(2) 0.0433(14) Uani 1 1 d . . .
H31A H 0.9392 0.0245 0.8156 0.052 Uiso 1 1 calc R . .
H31B H 0.9981 -0.0531 0.8493 0.052 Uiso 1 1 calc R . .
C39 C 0.4933(5) 0.2528(3) 0.9709(2) 0.0392(13) Uani 1 1 d . . .
H39A H 0.4877 0.2888 0.9376 0.047 Uiso 1 1 calc R . .
H39B H 0.5497 0.2782 1.0064 0.047 Uiso 1 1 calc R . .
C17 C 0.7858(6) 0.4411(3) 0.7858(2) 0.0347(12) Uani 1 1 d . . .
H17 H 0.8431 0.4673 0.8182 0.042 Uiso 1 1 calc R . .
C2 C 0.7661(5) 0.1554(3) 0.7243(2) 0.0368(13) Uani 1 1 d . . .
H2A H 0.8027 0.2011 0.7064 0.044 Uiso 1 1 calc R . .
H2B H 0.8201 0.1514 0.7653 0.044 Uiso 1 1 calc R . .
C16 C 0.7615(6) 0.4753(3) 0.7312(2) 0.0422(14) Uani 1 1 d . . .
H16 H 0.8048 0.5237 0.7266 0.051 Uiso 1 1 calc R . .
C6 C 0.5176(6) 0.1677(3) 0.6602(2) 0.0445(14) Uani 1 1 d . . .
H6A H 0.4123 0.1719 0.6602 0.053 Uiso 1 1 calc R . .
H6B H 0.5467 0.2137 0.6403 0.053 Uiso 1 1 calc R . .
C14 C 0.6141(6) 0.3696(3) 0.6898(2) 0.0439(14) Uani 1 1 d . . .
H14 H 0.5539 0.3450 0.6573 0.053 Uiso 1 1 calc R . .
C23 C 1.0149(6) 0.3422(3) 1.0507(2) 0.0403(13) Uani 1 1 d . . .
H23 H 1.0519 0.3929 1.0495 0.048 Uiso 1 1 calc R . .
C12 C 0.3052(5) 0.1882(3) 0.7807(2) 0.0349(12) Uani 1 1 d . . .
H12A H 0.3487 0.1798 0.8226 0.042 Uiso 1 1 calc R . .
H12B H 0.3262 0.1423 0.7587 0.042 Uiso 1 1 calc R . .
C32 C 0.8037(6) -0.0157(3) 0.8691(3) 0.0445(14) Uani 1 1 d . . .
H32A H 0.8156 -0.0481 0.9047 0.053 Uiso 1 1 calc R . .
H32B H 0.7401 -0.0437 0.8368 0.053 Uiso 1 1 calc R . .
C15 C 0.6756(6) 0.4404(3) 0.6832(2) 0.0460(14) Uani 1 1 d . . .
H15 H 0.6590 0.4649 0.6460 0.055 Uiso 1 1 calc R . .
C30 C 1.0487(6) 0.0442(3) 0.9009(2) 0.0434(14) Uani 1 1 d . . .
H30A H 1.1428 0.0543 0.8892 0.052 Uiso 1 1 calc R . .
H30B H 1.0688 0.0144 0.9379 0.052 Uiso 1 1 calc R . .
C38 C 0.3391(6) 0.2358(4) 0.9802(3) 0.0539(16) Uani 1 1 d . . .
H38A H 0.2945 0.2840 0.9908 0.065 Uiso 1 1 calc R . .
H38B H 0.2791 0.2167 0.9431 0.065 Uiso 1 1 calc R . .
C36 C 0.4204(6) 0.1043(4) 1.0167(3) 0.0502(15) Uani 1 1 d . . .
H36A H 0.3661 0.0785 0.9811 0.060 Uiso 1 1 calc R . .
H36B H 0.4252 0.0684 1.0500 0.060 Uiso 1 1 calc R . .
C3 C 0.7935(6) 0.0836(4) 0.6907(3) 0.0534(16) Uani 1 1 d . . .
H3A H 0.8987 0.0796 0.6903 0.064 Uiso 1 1 calc R . .
H3B H 0.7652 0.0375 0.7107 0.064 Uiso 1 1 calc R . .
C4 C 0.7076(7) 0.0858(4) 0.6282(3) 0.0610(18) Uani 1 1 d . . .
H4A H 0.7233 0.0373 0.6080 0.073 Uiso 1 1 calc R . .
H4B H 0.7428 0.1288 0.6069 0.073 Uiso 1 1 calc R . .
C5 C 0.5451(6) 0.0960(4) 0.6269(3) 0.0571(17) Uani 1 1 d . . .
H5A H 0.4920 0.1001 0.5857 0.069 Uiso 1 1 calc R . .
H5B H 0.5077 0.0504 0.6446 0.069 Uiso 1 1 calc R . .
C19 C 0.6347(8) 0.4471(4) 0.9636(3) 0.070(2) Uani 1 1 d . . .
H19A H 0.5631 0.4282 0.9300 0.105 Uiso 1 1 calc R . .
H19B H 0.6014 0.4962 0.9769 0.105 Uiso 1 1 calc R . .
H19C H 0.6454 0.4095 0.9955 0.105 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 P1 2.4411(14) . ?
Pd1 P2 2.3024(13) . ?
Pd1 Si1 2.3030(15) . ?
Pd1 C18 2.073(5) . ?
P1 C7 1.845(5) . ?
P1 C1 1.839(5) . ?
P1 C13 1.813(5) . ?
P2 C27 1.834(5) . ?
P2 C34 1.849(5) . ?
P2 C28 1.846(5) . ?
Si1 C22 1.906(5) . ?
Si1 C21 1.907(6) . ?
Si1 C20 1.872(5) . ?
C27 C22 1.393(7) . ?
C27 C26 1.402(7) . ?
C7 C8 1.533(6) . ?
C7 C12 1.526(6) . ?
C22 C23 1.398(7) . ?
C35 C34 1.536(7) . ?
C35 C36 1.529(7) . ?
C8 C9 1.526(7) . ?
C20 C19 1.474(8) . ?
C34 C39 1.524(7) . ?
C1 C2 1.533(7) . ?
C1 C6 1.536(7) . ?
C25 C24 1.380(7) . ?
C25 C26 1.377(7) . ?
C13 C18 1.400(6) . ?
C13 C14 1.394(7) . ?
C24 C23 1.376(7) . ?
C10 C11 1.516(7) . ?
C10 C9 1.519(7) . ?
C11 C12 1.527(7) . ?
C37 C38 1.520(8) . ?
C37 C36 1.516(8) . ?
C33 C28 1.522(7) . ?
C33 C32 1.526(7) . ?
C18 C17 1.414(7) . ?
C29 C28 1.536(7) . ?
C29 C30 1.525(7) . ?
C31 C32 1.518(7) . ?
C31 C30 1.522(7) . ?
C39 C38 1.532(7) . ?
C17 C16 1.381(7) . ?
C2 C3 1.523(7) . ?
C16 C15 1.382(7) . ?
C6 C5 1.518(7) . ?
C14 C15 1.381(7) . ?
C3 C4 1.517(8) . ?
C4 C5 1.528(8) . ?

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
P2 Pd1 P1 113.58(5) . . ?
P2 Pd1 Si1 85.75(5) . . ?
Si1 Pd1 P1 160.21(5) . . ?
C18 Pd1 P1 68.33(13) . . ?
C18 Pd1 P2 177.61(13) . . ?
C18 Pd1 Si1 92.47(13) . . ?
C7 P1 Pd1 121.00(16) . . ?
C1 P1 Pd1 128.23(16) . . ?
C1 P1 C7 105.2(2) . . ?
C13 P1 Pd1 80.96(15) . . ?
C13 P1 C7 104.9(2) . . ?
C13 P1 C1 110.1(2) . . ?
C27 P2 Pd1 111.27(16) . . ?
C27 P2 C34 106.2(2) . . ?
C27 P2 C28 102.9(2) . . ?
C34 P2 Pd1 115.05(16) . . ?
C28 P2 Pd1 115.84(16) . . ?
C28 P2 C34 104.4(2) . . ?
C22 Si1 Pd1 107.31(16) . . ?
C22 Si1 C21 103.5(2) . . ?
C21 Si1 Pd1 119.20(17) . . ?
C20 Si1 Pd1 114.1(2) . . ?
C20 Si1 C22 106.1(2) . . ?
C20 Si1 C21 105.5(3) . . ?
C22 C27 P2 115.8(4) . . ?
C22 C27 C26 120.2(4) . . ?
C26 C27 P2 123.9(4) . . ?
C8 C7 P1 110.8(3) . . ?
C12 C7 P1 110.3(3) . . ?
C12 C7 C8 110.9(4) . . ?
C27 C22 Si1 119.6(4) . . ?
C27 C22 C23 117.7(5) . . ?
C23 C22 Si1 122.7(4) . . ?
C36 C35 C34 110.6(4) . . ?
C9 C8 C7 110.6(4) . . ?
C19 C20 Si1 116.5(4) . . ?
C35 C34 P2 117.5(4) . . ?
C39 C34 P2 110.9(3) . . ?
C39 C34 C35 109.8(4) . . ?
C2 C1 P1 110.4(3) . . ?
C2 C1 C6 109.8(4) . . ?
C6 C1 P1 116.6(4) . . ?
C26 C25 C24 119.9(5) . . ?
C18 C13 P1 104.5(3) . . ?
C14 C13 P1 131.8(4) . . ?
C14 C13 C18 123.6(5) . . ?
C23 C24 C25 119.7(5) . . ?
C25 C26 C27 120.5(5) . . ?
C11 C10 C9 111.4(4) . . ?
C10 C11 C12 111.3(4) . . ?
C36 C37 C38 111.2(5) . . ?
C28 C33 C32 112.1(4) . . ?
C13 C18 Pd1 106.0(3) . . ?
C13 C18 C17 115.2(4) . . ?
C17 C18 Pd1 138.8(4) . . ?
C30 C29 C28 111.8(4) . . ?
C10 C9 C8 111.4(4) . . ?
C33 C28 P2 113.4(3) . . ?
C33 C28 C29 110.5(4) . . ?
C29 C28 P2 109.3(3) . . ?
C32 C31 C30 110.4(4) . . ?
C34 C39 C38 111.8(5) . . ?
C16 C17 C18 121.5(5) . . ?
C3 C2 C1 111.1(4) . . ?
C17 C16 C15 121.4(5) . . ?
C5 C6 C1 111.3(5) . . ?
C15 C14 C13 119.1(5) . . ?
C24 C23 C22 122.0(5) . . ?
C7 C12 C11 112.0(4) . . ?
C31 C32 C33 111.9(4) . . ?
C14 C15 C16 119.3(5) . . ?
C31 C30 C29 111.4(4) . . ?
C37 C38 C39 111.8(5) . . ?
C37 C36 C35 112.0(5) . . ?
C4 C3 C2 111.2(5) . . ?
C3 C4 C5 110.9(5) . . ?
C6 C5 C4 110.9(5) . . ?

_database_code_depnum_ccdc_archive 'CCDC 997345'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_s14022
_audit_creation_date             2014-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4773)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C44 H71 Al O2 P2 Pd Si'
_chemical_formula_sum            'C44 H71 Al O2 P2 Pd Si'
_chemical_formula_weight         855.41
_chemical_melting_point          ?
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'
Al Al 0.0645 0.0514 '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'
Pd Pd -0.9988 1.0072 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.632(3)
_cell_length_b                   23.5987(7)
_cell_length_c                   19.2983(14)
_cell_angle_alpha                90
_cell_angle_beta                 105.726(11)
_cell_angle_gamma                90
_cell_volume                     4660.9(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    67582
_cell_measurement_temperature    93
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1205
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            127755
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.689
_diffrn_reflns_theta_min         3.054
_diffrn_ambient_temperature      93
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       
;
Crystal Goniometer
;
_diffrn_measurement_device_type  
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Loop
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.000564
_diffrn_orient_matrix_UB_12      -0.009468
_diffrn_orient_matrix_UB_13      -0.049907
_diffrn_orient_matrix_UB_21      0.010181
_diffrn_orient_matrix_UB_22      0.041086
_diffrn_orient_matrix_UB_23      -0.002838
_diffrn_orient_matrix_UB_31      0.097415
_diffrn_orient_matrix_UB_32      -0.004239
_diffrn_orient_matrix_UB_33      0.083954
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5919
_reflns_number_total             7904
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         3.406
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.0076(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7904
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0902
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1890P)²+18.6753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2489
_refine_ls_wR_factor_ref         0.2734
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C40
 1.7 with sigma of 0.01
 C39-C40 \\sim C44-C43 \\sim C42-C41
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C40 \\sim C39 \\sim C42 \\sim C41 \\sim C43 \\sim C44: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C40) = Uanis(C39)
4. Rigid body (RIGU) restrains
 C40, C39, C42, C41, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C7(H7), C26(H26), C32(H32), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C27(H27A,H27B), C12(H12A,H12B), C37(H37A,H37B), C36(H36A,
 H36B), C28(H28A,H28B), C8(H8A,H8B), C10(H10A,H10B), C2(H2A,H2B), C33(H33A,
 H33B), C9(H9A,H9B), C6(H6A,H6B), C30(H30A,H30B), C3(H3A,H3B), C35(H35A,H35B),
 C31(H31A,H31B), C39(H39A,H39B), C29(H29A,H29B), C34(H34A,H34B), C43(H43A,H43B),
  C41(H41A,H41B), C5(H5A,H5B), C4(H4A,H4B)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C21(H21), C15(H15), C17(H17), C22(H22), C24(H24), C23(H23),
 C16(H16), C38(H38)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C40(H40A,H40B,
 H40C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.34027(5) 0.32997(2) 0.87161(3) 0.0357(3) Uani 1 1 d . . . . .
Si1 Si 0.5225(2) 0.33486(8) 0.83215(11) 0.0378(5) Uani 1 1 d . . . . .
P1 P 0.48682(18) 0.30629(8) 0.97988(10) 0.0389(5) Uani 1 1 d . . . . .
P2 P 0.24711(18) 0.38414(8) 0.77095(10) 0.0379(5) Uani 1 1 d . . . . .
Al1 Al -0.0156(3) 0.19373(12) 0.79075(14) 0.0547(7) Uani 1 1 d . . . . .
O1 O 0.1635(5) 0.3202(2) 0.9125(3) 0.0431(12) Uani 1 1 d . . . . .
O2 O 0.1006(5) 0.2482(2) 0.8369(3) 0.0500(13) Uani 1 1 d . . . . .
C14 C 0.7569(8) 0.3302(3) 1.0428(4) 0.0423(18) Uani 1 1 d . . . . .
H14 H 0.7452 0.3187 1.0867 0.051 Uiso 1 1 calc R . . . .
C13 C 0.6494(7) 0.3296(3) 0.9798(4) 0.0382(16) Uani 1 1 d . . . . .
C21 C 0.6018(8) 0.4148(4) 0.7366(4) 0.0492(19) Uani 1 1 d . . . . .
H21 H 0.6850 0.3991 0.7517 0.059 Uiso 1 1 calc R . . . .
C25 C 0.3759(7) 0.4166(3) 0.7374(4) 0.0368(16) Uani 1 1 d . . . . .
C15 C 0.8772(7) 0.3479(3) 1.0386(4) 0.0441(18) Uani 1 1 d . . . . .
H15 H 0.9468 0.3489 1.0800 0.053 Uiso 1 1 calc R . . . .
C20 C 0.5020(7) 0.3937(3) 0.7641(4) 0.0388(16) Uani 1 1 d . . . . .
C11 C 0.6033(9) 0.1369(4) 1.0026(6) 0.061(2) Uani 1 1 d . . . . .
H11A H 0.6528 0.1148 0.9767 0.073 Uiso 1 1 calc R . . . .
H11B H 0.6528 0.1380 1.0528 0.073 Uiso 1 1 calc R . . . .
C27 C 0.2067(7) 0.2947(3) 0.6722(4) 0.0433(17) Uani 1 1 d . . . . .
H27A H 0.2777 0.3081 0.6538 0.052 Uiso 1 1 calc R . . . .
H27B H 0.2439 0.2712 0.7139 0.052 Uiso 1 1 calc R . . . .
C18 C 0.6679(7) 0.3453(3) 0.9136(4) 0.0380(16) Uani 1 1 d . . . . .
C17 C 0.7929(7) 0.3626(3) 0.9118(4) 0.0449(18) Uani 1 1 d . . . . .
H17 H 0.8073 0.3732 0.8682 0.054 Uiso 1 1 calc R . . . .
C7 C 0.5084(7) 0.2323(3) 1.0133(4) 0.0403(17) Uani 1 1 d . . . . .
H7 H 0.5581 0.2333 1.0641 0.048 Uiso 1 1 calc R . . . .
C19 C 0.5506(7) 0.2674(4) 0.7872(4) 0.0491(19) Uani 1 1 d . . . . .
H19A H 0.5324 0.2356 0.8140 0.074 Uiso 1 1 calc GR . . . .
H19B H 0.6399 0.2657 0.7855 0.074 Uiso 1 1 calc GR . . . .
H19C H 0.4938 0.2662 0.7392 0.074 Uiso 1 1 calc GR . . . .
C12 C 0.5868(9) 0.1978(4) 0.9724(5) 0.059(2) Uani 1 1 d . . . . .
H12A H 0.6718 0.2150 0.9781 0.071 Uiso 1 1 calc R . . . .
H12B H 0.5414 0.1970 0.9215 0.071 Uiso 1 1 calc R . . . .
C22 C 0.5784(8) 0.4589(4) 0.6870(4) 0.052(2) Uani 1 1 d . . . . .
H22 H 0.6462 0.4723 0.6696 0.063 Uiso 1 1 calc R . . . .
C37 C 0.0181(7) 0.4285(3) 0.7993(5) 0.0455(18) Uani 1 1 d . . . . .
H37A H -0.0337 0.4116 0.7549 0.055 Uiso 1 1 calc R . . . .
H37B H 0.0283 0.4006 0.8373 0.055 Uiso 1 1 calc R . . . .
C36 C -0.0522(8) 0.4800(4) 0.8170(5) 0.056(2) Uani 1 1 d . . . . .
H36A H -0.0701 0.5060 0.7766 0.067 Uiso 1 1 calc R . . . .
H36B H -0.1352 0.4682 0.8241 0.067 Uiso 1 1 calc R . . . .
C24 C 0.3525(8) 0.4615(3) 0.6874(4) 0.0466(18) Uani 1 1 d . . . . .
H24 H 0.2691 0.4766 0.6706 0.056 Uiso 1 1 calc R . . . .
C26 C 0.1384(7) 0.3458(3) 0.6953(4) 0.0406(16) Uani 1 1 d . . . . .
H26 H 0.0681 0.3302 0.7136 0.049 Uiso 1 1 calc R . . . .
C28 C 0.1147(8) 0.2594(3) 0.6151(4) 0.0490(19) Uani 1 1 d . . . . .
H28A H 0.0512 0.2415 0.6358 0.059 Uiso 1 1 calc R . . . .
H28B H 0.1639 0.2298 0.5995 0.059 Uiso 1 1 calc R . . . .
C32 C 0.1540(7) 0.4448(3) 0.7908(4) 0.0430(17) Uani 1 1 d . . . . .
H32 H 0.1411 0.4717 0.7508 0.052 Uiso 1 1 calc R . . . .
C8 C 0.3782(8) 0.2048(3) 1.0085(5) 0.0491(19) Uani 1 1 d . . . . .
H8A H 0.3257 0.2049 0.9588 0.059 Uiso 1 1 calc R . . . .
H8B H 0.3321 0.2265 1.0366 0.059 Uiso 1 1 calc R . . . .
C23 C 0.4559(8) 0.4831(4) 0.6632(4) 0.052(2) Uani 1 1 d . . . . .
H23 H 0.4421 0.5135 0.6313 0.062 Uiso 1 1 calc R . . . .
C10 C 0.4749(8) 0.1083(3) 0.9964(5) 0.054(2) Uani 1 1 d . . . . .
H10A H 0.4895 0.0707 1.0173 0.064 Uiso 1 1 calc R . . . .
H10B H 0.4270 0.1046 0.9462 0.064 Uiso 1 1 calc R . . . .
C2 C 0.4576(9) 0.4122(3) 1.0369(5) 0.056(2) Uani 1 1 d . . . . .
H2A H 0.5508 0.4196 1.0496 0.068 Uiso 1 1 calc R . . . .
H2B H 0.4214 0.4219 0.9866 0.068 Uiso 1 1 calc R . . . .
C33 C 0.2333(8) 0.4744(3) 0.8589(5) 0.051(2) Uani 1 1 d . . . . .
H33A H 0.3166 0.4863 0.8523 0.062 Uiso 1 1 calc R . . . .
H33B H 0.2505 0.4479 0.8988 0.062 Uiso 1 1 calc R . . . .
C9 C 0.3960(9) 0.1439(4) 1.0363(5) 0.058(2) Uani 1 1 d . . . . .
H9A H 0.3109 0.1267 1.0303 0.070 Uiso 1 1 calc R . . . .
H9B H 0.4406 0.1442 1.0873 0.070 Uiso 1 1 calc R . . . .
C6 C 0.4803(11) 0.3316(4) 1.1257(5) 0.063(2) Uani 1 1 d . . . . .
H6A H 0.5743 0.3361 1.1428 0.075 Uiso 1 1 calc R . . . .
H6B H 0.4596 0.2920 1.1308 0.075 Uiso 1 1 calc R . . . .
C30 C -0.0246(8) 0.3456(4) 0.5727(4) 0.0505(19) Uani 1 1 d . . . . .
H30A H -0.0948 0.3326 0.5920 0.061 Uiso 1 1 calc R . . . .
H30B H -0.0626 0.3688 0.5307 0.061 Uiso 1 1 calc R . . . .
C3 C 0.3948(12) 0.4483(4) 1.0826(6) 0.075(3) Uani 1 1 d . . . . .
H3A H 0.4188 0.4876 1.0787 0.090 Uiso 1 1 calc R . . . .
H3B H 0.3006 0.4454 1.0645 0.090 Uiso 1 1 calc R . . . .
C1 C 0.4343(9) 0.3486(4) 1.0478(5) 0.052(2) Uani 1 1 d . . . . .
H1 H 0.3391 0.3444 1.0351 0.063 Uiso 1 1 calc R . . . .
C35 C 0.0261(9) 0.5103(4) 0.8835(5) 0.061(2) Uani 1 1 d . . . . .
H35A H 0.0350 0.4860 0.9251 0.074 Uiso 1 1 calc R . . . .
H35B H -0.0199 0.5443 0.8907 0.074 Uiso 1 1 calc R . . . .
C31 C 0.0711(8) 0.3816(3) 0.6295(4) 0.0501(19) Uani 1 1 d . . . . .
H31A H 0.1366 0.3977 0.6087 0.060 Uiso 1 1 calc R . . . .
H31B H 0.0243 0.4125 0.6443 0.060 Uiso 1 1 calc R . . . .
C39 C -0.1245(7) 0.2301(4) 0.7151(5) 0.078(3) Uani 1 1 d D . . A 1
H39A H -0.0828 0.2332 0.6764 0.094 Uiso 1 1 calc R . . A 1
H39B H -0.2037 0.2080 0.6976 0.094 Uiso 1 1 calc R . . A 1
C16 C 0.8962(7) 0.3641(3) 0.9741(4) 0.0457(18) Uani 1 1 d . . . . .
H16 H 0.9783 0.3762 0.9720 0.055 Uiso 1 1 calc R . . . .
C29 C 0.0430(8) 0.2944(4) 0.5501(4) 0.052(2) Uani 1 1 d . . . . .
H29A H -0.0217 0.2709 0.5176 0.062 Uiso 1 1 calc R . . . .
H29B H 0.1047 0.3073 0.5246 0.062 Uiso 1 1 calc R . . . .
C34 C 0.1609(8) 0.5261(4) 0.8770(6) 0.062(2) Uani 1 1 d . . . . .
H34A H 0.2115 0.5426 0.9220 0.074 Uiso 1 1 calc R . . . .
H34B H 0.1524 0.5545 0.8396 0.074 Uiso 1 1 calc R . . . .
C43 C 0.0889(11) 0.1405(5) 0.7546(6) 0.081(3) Uani 1 1 d . . . . .
H43A H 0.0378 0.1065 0.7391 0.097 Uiso 1 1 calc R . . . .
H43B H 0.1092 0.1568 0.7128 0.097 Uiso 1 1 calc R . . . .
C41 C -0.1229(10) 0.1695(4) 0.8535(5) 0.067(3) Uani 1 1 d . . . . .
H41A H -0.0676 0.1514 0.8960 0.080 Uiso 1 1 calc R . . . .
H41B H -0.1623 0.2026 0.8690 0.080 Uiso 1 1 calc R . . . .
C5 C 0.4134(12) 0.3686(4) 1.1714(5) 0.071(3) Uani 1 1 d . . . . .
H5A H 0.3206 0.3605 1.1585 0.085 Uiso 1 1 calc R . . . .
H5B H 0.4492 0.3596 1.2220 0.085 Uiso 1 1 calc R . . . .
C4 C 0.4345(12) 0.4313(5) 1.1593(6) 0.082(3) Uani 1 1 d . . . . .
H4A H 0.3852 0.4535 1.1852 0.099 Uiso 1 1 calc R . . . .
H4B H 0.5263 0.4402 1.1793 0.099 Uiso 1 1 calc R . . . .
C44 C 0.2209(11) 0.1234(6) 0.8112(6) 0.094(4) Uani 1 1 d . . . . .
H44A H 0.2651 0.0952 0.7906 0.141 Uiso 1 1 calc GR . . . .
H44B H 0.2022 0.1083 0.8535 0.141 Uiso 1 1 calc GR . . . .
H44C H 0.2755 0.1562 0.8239 0.141 Uiso 1 1 calc GR . . . .
C42 C -0.2346(12) 0.1268(5) 0.8141(6) 0.093(4) Uani 1 1 d . . . . .
H42A H -0.2868 0.1438 0.7706 0.140 Uiso 1 1 calc GR . . . .
H42B H -0.2888 0.1182 0.8452 0.140 Uiso 1 1 calc GR . . . .
H42C H -0.1959 0.0926 0.8026 0.140 Uiso 1 1 calc GR . . . .
C38 C 0.0873(7) 0.2826(3) 0.8854(4) 0.0436(18) Uani 1 1 d . . . . .
H38 H 0.0129 0.2786 0.9015 0.052 Uiso 1 1 calc R . . . .
C40 C -0.1652(7) 0.2973(4) 0.7384(5) 0.078(3) Uani 1 1 d D . . . .
H40A H -0.2535 0.3059 0.7121 0.117 Uiso 1 1 calc GR . . A .
H40B H -0.1071 0.3246 0.7269 0.117 Uiso 1 1 calc GR . . A .
H40C H -0.1574 0.2985 0.7891 0.117 Uiso 1 1 calc GR . . A .


_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 Si1 2.269(2) . ?
Pd1 P1 2.3111(19) . ?
Pd1 P2 2.3121(19) . ?
Pd1 O1 2.239(5) . ?
Si1 C20 1.881(7) . ?
Si1 C18 1.898(7) . ?
Si1 C19 1.876(8) . ?
P1 C13 1.815(8) . ?
P1 C7 1.854(7) . ?
P1 C1 1.850(9) . ?
P2 C25 1.833(7) . ?
P2 C26 1.836(7) . ?
P2 C32 1.839(8) . ?
Al1 O2 1.837(6) . ?
Al1 C39 1.815(8) . ?
Al1 C43 1.929(11) . ?
Al1 C41 1.960(11) . ?
O1 C38 1.221(9) . ?
O2 C38 1.274(9) . ?
C14 C13 1.425(10) . ?
C14 C15 1.369(11) . ?
C13 C18 1.393(10) . ?
C21 C20 1.401(10) . ?
C21 C22 1.389(11) . ?
C25 C20 1.408(10) . ?
C25 C24 1.409(10) . ?
C15 C16 1.367(11) . ?
C11 C12 1.542(12) . ?
C11 C10 1.498(12) . ?
C27 C26 1.535(10) . ?
C27 C28 1.510(11) . ?
C18 C17 1.400(10) . ?
C17 C16 1.392(11) . ?
C7 C12 1.529(11) . ?
C7 C8 1.509(11) . ?
C22 C23 1.382(12) . ?
C37 C36 1.513(11) . ?
C37 C32 1.546(10) . ?
C36 C35 1.507(12) . ?
C24 C23 1.402(11) . ?
C26 C31 1.531(11) . ?
C28 C29 1.522(11) . ?
C32 C33 1.525(11) . ?
C8 C9 1.527(12) . ?
C10 C9 1.534(12) . ?
C2 C3 1.507(12) . ?
C2 C1 1.544(11) . ?
C33 C34 1.533(11) . ?
C6 C1 1.504(12) . ?
C6 C5 1.545(13) . ?
C30 C31 1.534(11) . ?
C30 C29 1.528(12) . ?
C3 C4 1.480(14) . ?
C35 C34 1.520(12) . ?
C39 C40 1.733(8) . ?
C43 C44 1.578(12) . ?
C41 C42 1.586(11) . ?
C5 C4 1.524(15) . ?

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
Si1 Pd1 P1 83.56(7) . . ?
Si1 Pd1 P2 84.28(7) . . ?
P1 Pd1 P2 157.46(7) . . ?
O1 Pd1 Si1 176.80(14) . . ?
O1 Pd1 P1 94.64(14) . . ?
O1 Pd1 P2 98.28(14) . . ?
C20 Si1 Pd1 108.9(2) . . ?
C20 Si1 C18 113.4(3) . . ?
C18 Si1 Pd1 107.8(2) . . ?
C19 Si1 Pd1 111.7(3) . . ?
C19 Si1 C20 107.9(4) . . ?
C19 Si1 C18 107.3(3) . . ?
C13 P1 Pd1 109.6(3) . . ?
C13 P1 C7 104.9(3) . . ?
C13 P1 C1 107.9(4) . . ?
C7 P1 Pd1 122.1(2) . . ?
C1 P1 Pd1 104.6(3) . . ?
C1 P1 C7 107.1(4) . . ?
C25 P2 Pd1 109.7(2) . . ?
C25 P2 C26 107.1(3) . . ?
C25 P2 C32 104.1(3) . . ?
C26 P2 Pd1 115.5(3) . . ?
C26 P2 C32 106.9(3) . . ?
C32 P2 Pd1 112.8(3) . . ?
O2 Al1 C43 104.7(4) . . ?
O2 Al1 C41 109.4(3) . . ?
C39 Al1 O2 104.9(4) . . ?
C39 Al1 C43 108.8(5) . . ?
C39 Al1 C41 106.4(4) . . ?
C43 Al1 C41 121.5(5) . . ?
C38 O1 Pd1 116.6(5) . . ?
C38 O2 Al1 127.4(5) . . ?
C15 C14 C13 119.9(7) . . ?
C14 C13 P1 123.1(6) . . ?
C18 C13 P1 116.9(5) . . ?
C18 C13 C14 120.0(7) . . ?
C22 C21 C20 121.1(7) . . ?
C20 C25 P2 116.0(5) . . ?
C20 C25 C24 120.9(7) . . ?
C24 C25 P2 123.1(6) . . ?
C14 C15 C16 120.7(7) . . ?
C21 C20 Si1 124.8(6) . . ?
C21 C20 C25 117.9(7) . . ?
C25 C20 Si1 117.3(5) . . ?
C10 C11 C12 112.5(7) . . ?
C28 C27 C26 112.4(6) . . ?
C13 C18 Si1 116.1(5) . . ?
C13 C18 C17 118.1(7) . . ?
C17 C18 Si1 125.6(6) . . ?
C16 C17 C18 121.2(7) . . ?
C12 C7 P1 110.8(5) . . ?
C8 C7 P1 111.0(5) . . ?
C8 C7 C12 111.0(7) . . ?
C7 C12 C11 108.9(7) . . ?
C23 C22 C21 121.0(7) . . ?
C36 C37 C32 110.9(6) . . ?
C35 C36 C37 112.4(7) . . ?
C23 C24 C25 119.6(8) . . ?
C27 C26 P2 111.9(5) . . ?
C31 C26 P2 116.1(5) . . ?
C31 C26 C27 110.1(6) . . ?
C27 C28 C29 112.5(7) . . ?
C37 C32 P2 113.6(5) . . ?
C33 C32 P2 109.5(5) . . ?
C33 C32 C37 109.7(6) . . ?
C7 C8 C9 111.0(6) . . ?
C22 C23 C24 119.4(8) . . ?
C11 C10 C9 108.9(7) . . ?
C3 C2 C1 110.9(8) . . ?
C32 C33 C34 111.5(7) . . ?
C8 C9 C10 111.8(7) . . ?
C1 C6 C5 110.2(8) . . ?
C29 C30 C31 111.7(7) . . ?
C4 C3 C2 112.4(9) . . ?
C2 C1 P1 109.7(6) . . ?
C6 C1 P1 119.1(6) . . ?
C6 C1 C2 112.0(8) . . ?
C36 C35 C34 111.2(7) . . ?
C26 C31 C30 111.0(7) . . ?
C40 C39 Al1 112.0(6) . . ?
C15 C16 C17 120.2(7) . . ?
C28 C29 C30 111.2(7) . . ?
C35 C34 C33 111.4(7) . . ?
C44 C43 Al1 114.0(7) . . ?
C42 C41 Al1 112.0(7) . . ?
C4 C5 C6 110.6(8) . . ?
C3 C4 C5 113.7(9) . . ?
O1 C38 O2 125.8(7) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 216.4 2.4 ?
2 0.000 0.500 0.500 216.4 2.4 ?

_database_code_depnum_ccdc_archive 'CCDC 997346'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_m13025
_audit_creation_date             2013-12-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38 H55 F3 O3 P2 Pd S Si'
_chemical_formula_sum            'C38 H55 F3 O3 P2 Pd S Si'
_chemical_formula_weight         845.31
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   23.517(18)
_cell_length_b                   21.766(18)
_cell_length_c                   14.710(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7530(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    223
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method Pentane
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24546
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.049
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Mini
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5066
_reflns_number_total             7105
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.319
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0634
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0476P)²+21.3540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1433
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C26(H26), C1(H1), C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C27(H27A,H27B), C28(H28A,H28B), C8(H8A,H8B), C12(H12A,H12B),
 C29(H29A,H29B), C30(H30A,H30B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C33(H33A,H33B), C2(H2A,H2B), C37(H37A,H37B), C6(H6A,H6B), C34(H34A,H34B),
 C5(H5A,H5B), C36(H36A,H36B), C3(H3A,H3B), C4(H4A,H4B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C16(H16), C24(H24), C14(H14), C22(H22), C15(H15), C17(H17), C23(H23)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.36690(2) 0.06283(2) 0.25821(3) 0.03057(14) Uani 1 1 d . . . . .
P1 P 0.41321(6) -0.02648(6) 0.24804(9) 0.0324(3) Uani 1 1 d . . . . .
Si1 Si 0.31896(6) 0.01776(7) 0.36964(10) 0.0330(4) Uani 1 1 d . . . . .
P2 P 0.34039(6) 0.14968(6) 0.33009(10) 0.0338(3) Uani 1 1 d . . . . .
C18 C 0.3520(2) -0.0564(2) 0.3966(4) 0.0342(13) Uani 1 1 d . . . . .
C13 C 0.3933(2) -0.0767(2) 0.3386(4) 0.0359(13) Uani 1 1 d . . . . .
C20 C 0.3172(2) 0.0712(2) 0.4672(4) 0.0335(12) Uani 1 1 d . . . . .
C21 C 0.3073(2) 0.0556(3) 0.5573(4) 0.0458(15) Uani 1 1 d . . . . .
H21 H 0.2994 0.0144 0.5722 0.055 Uiso 1 1 calc R U . . .
C7 C 0.4882(2) -0.0170(3) 0.2669(4) 0.0349(13) Uani 1 1 d . . . . .
H7 H 0.5068 -0.0570 0.2545 0.042 Uiso 1 1 calc R U . . .
C16 C 0.3612(3) -0.1478(3) 0.4800(5) 0.061(2) Uani 1 1 d . . . . .
H16 H 0.3500 -0.1728 0.5288 0.073 Uiso 1 1 calc R U . . .
C26 C 0.2831(2) 0.1950(3) 0.2857(4) 0.0378(13) Uani 1 1 d . . . . .
H26 H 0.2966 0.2109 0.2265 0.045 Uiso 1 1 calc R U . . .
C24 C 0.3258(2) 0.1737(3) 0.5152(4) 0.0467(15) Uani 1 1 d . . . . .
H24 H 0.3309 0.2154 0.5009 0.056 Uiso 1 1 calc R U . . .
C25 C 0.3258(2) 0.1314(3) 0.4477(4) 0.0349(13) Uani 1 1 d . . . . .
C31 C 0.2323(2) 0.1576(3) 0.2650(4) 0.0445(15) Uani 1 1 d . . . . .
H31A H 0.2164 0.1413 0.3216 0.053 Uiso 1 1 calc R U . . .
H31B H 0.2433 0.1227 0.2267 0.053 Uiso 1 1 calc R U . . .
C14 C 0.4193(3) -0.1311(3) 0.3525(4) 0.0458(15) Uani 1 1 d . . . . .
H14 H 0.4484 -0.1442 0.3132 0.055 Uiso 1 1 calc R U . . .
C27 C 0.2676(2) 0.2501(3) 0.3403(5) 0.0523(17) Uani 1 1 d . . . . .
H27A H 0.3015 0.2754 0.3503 0.063 Uiso 1 1 calc R U . . .
H27B H 0.2531 0.2372 0.3997 0.063 Uiso 1 1 calc R U . . .
C28 C 0.2235(3) 0.2870(3) 0.2920(5) 0.0575(18) Uani 1 1 d . . . . .
H28A H 0.2122 0.3217 0.3303 0.069 Uiso 1 1 calc R U . . .
H28B H 0.2397 0.3035 0.2357 0.069 Uiso 1 1 calc R U . . .
C8 C 0.5004(2) -0.0005(3) 0.3643(4) 0.0474(15) Uani 1 1 d . . . . .
H8A H 0.4809 0.0380 0.3794 0.057 Uiso 1 1 calc R U . . .
H8B H 0.4855 -0.0327 0.4042 0.057 Uiso 1 1 calc R U . . .
C12 C 0.5132(2) 0.0293(3) 0.2031(4) 0.0503(16) Uani 1 1 d . . . . .
H12A H 0.4941 0.0689 0.2113 0.060 Uiso 1 1 calc R U . . .
H12B H 0.5072 0.0160 0.1402 0.060 Uiso 1 1 calc R U . . .
C22 C 0.3089(3) 0.0981(3) 0.6239(4) 0.0543(17) Uani 1 1 d . . . . .
H22 H 0.3031 0.0863 0.6846 0.065 Uiso 1 1 calc R U . . .
C29 C 0.1733(3) 0.2497(3) 0.2704(5) 0.0572(18) Uani 1 1 d . . . . .
H29A H 0.1462 0.2747 0.2358 0.069 Uiso 1 1 calc R U . . .
H29B H 0.1547 0.2370 0.3270 0.069 Uiso 1 1 calc R U . . .
C15 C 0.4033(3) -0.1667(3) 0.4236(4) 0.0569(18) Uani 1 1 d . . . . .
H15 H 0.4214 -0.2046 0.4339 0.068 Uiso 1 1 calc R U . . .
C30 C 0.1884(3) 0.1948(3) 0.2172(5) 0.0603(19) Uani 1 1 d . . . . .
H30A H 0.2030 0.2074 0.1576 0.072 Uiso 1 1 calc R U . . .
H30B H 0.1544 0.1697 0.2074 0.072 Uiso 1 1 calc R U . . .
C17 C 0.3357(3) -0.0939(3) 0.4665(4) 0.0482(16) Uani 1 1 d . . . . .
H17 H 0.3062 -0.0815 0.5055 0.058 Uiso 1 1 calc R U . . .
C9 C 0.5627(3) 0.0069(3) 0.3806(5) 0.0602(19) Uani 1 1 d . . . . .
H9A H 0.5691 0.0203 0.4434 0.072 Uiso 1 1 calc R U . . .
H9B H 0.5817 -0.0328 0.3723 0.072 Uiso 1 1 calc R U . . .
C10 C 0.5871(3) 0.0521(3) 0.3178(5) 0.063(2) Uani 1 1 d . . . . .
H10A H 0.6283 0.0543 0.3275 0.076 Uiso 1 1 calc R U . . .
H10B H 0.5711 0.0927 0.3312 0.076 Uiso 1 1 calc R U . . .
C23 C 0.3184(3) 0.1566(4) 0.6038(4) 0.0595(19) Uani 1 1 d . . . . .
H23 H 0.3201 0.1862 0.6503 0.071 Uiso 1 1 calc R U . . .
C11 C 0.5758(3) 0.0367(4) 0.2204(5) 0.066(2) Uani 1 1 d . . . . .
H11A H 0.5954 -0.0016 0.2048 0.079 Uiso 1 1 calc R U . . .
H11B H 0.5908 0.0694 0.1815 0.079 Uiso 1 1 calc R U . . .
S1 S 0.34666(9) 0.11337(10) 0.05788(13) 0.0685(6) Uani 1 1 d . . . . .
O1 O 0.39280(19) 0.0996(2) 0.1216(3) 0.0572(12) Uani 1 1 d . . . . .
C33 C 0.4150(3) 0.2249(3) 0.2439(5) 0.0625(19) Uani 1 1 d . . . . .
H33A H 0.4220 0.1902 0.2030 0.075 Uiso 1 1 calc R U . . .
H33B H 0.3829 0.2484 0.2195 0.075 Uiso 1 1 calc R U . . .
C1 C 0.4060(2) -0.0645(3) 0.1399(4) 0.0433(14) Uani 1 1 d . . . . .
H1 H 0.4143 -0.0323 0.0943 0.052 Uiso 1 1 calc R U . . .
C32 C 0.3999(2) 0.2011(3) 0.3364(4) 0.0422(14) Uani 1 1 d . . . . .
H32 H 0.3896 0.2362 0.3758 0.051 Uiso 1 1 calc R U . . .
C2 C 0.3445(3) -0.0816(3) 0.1235(4) 0.0521(17) Uani 1 1 d . . . . .
H2A H 0.3203 -0.0454 0.1324 0.063 Uiso 1 1 calc R U . . .
H2B H 0.3328 -0.1132 0.1670 0.063 Uiso 1 1 calc R U . . .
C37 C 0.4499(2) 0.1694(3) 0.3763(5) 0.0524(17) Uani 1 1 d . . . . .
H37A H 0.4580 0.1322 0.3411 0.063 Uiso 1 1 calc R U . . .
H37B H 0.4409 0.1569 0.4387 0.063 Uiso 1 1 calc R U . . .
O2 O 0.3053(2) 0.0670(3) 0.0486(5) 0.111(2) Uani 1 1 d . . . . .
C6 C 0.4433(3) -0.1139(4) 0.1173(5) 0.074(2) Uani 1 1 d . . . . .
H6A H 0.4360 -0.1486 0.1580 0.088 Uiso 1 1 calc R U . . .
H6B H 0.4827 -0.1008 0.1260 0.088 Uiso 1 1 calc R U . . .
F1 F 0.3488(3) 0.1208(3) -0.1144(3) 0.1132(19) Uani 1 1 d . . . . .
F3 F 0.4082(3) 0.0603(3) -0.0563(4) 0.155(3) Uani 1 1 d . . . . .
C19 C 0.2470(2) 0.0005(3) 0.3331(5) 0.0533(17) Uani 1 1 d . . . . .
H19A H 0.2281 0.0382 0.3149 0.080 Uiso 1 1 calc R U . . .
H19B H 0.2262 -0.0182 0.3828 0.080 Uiso 1 1 calc R U . . .
H19C H 0.2482 -0.0276 0.2820 0.080 Uiso 1 1 calc R U . . .
O3 O 0.3250(3) 0.1719(3) 0.0633(4) 0.104(2) Uani 1 1 d . . . . .
C34 C 0.4661(3) 0.2646(4) 0.2462(6) 0.079(2) Uani 1 1 d . . . . .
H34A H 0.4750 0.2786 0.1845 0.095 Uiso 1 1 calc R U . . .
H34B H 0.4584 0.3009 0.2837 0.095 Uiso 1 1 calc R U . . .
F2 F 0.4216(3) 0.1552(3) -0.0444(5) 0.154(3) Uani 1 1 d . . . . .
C5 C 0.4348(3) -0.1344(4) 0.0186(5) 0.074(2) Uani 1 1 d . . . . .
H5A H 0.4455 -0.1009 -0.0224 0.089 Uiso 1 1 calc R U . . .
H5B H 0.4595 -0.1696 0.0058 0.089 Uiso 1 1 calc R U . . .
C36 C 0.5016(3) 0.2095(4) 0.3772(6) 0.077(2) Uani 1 1 d . . . . .
H36A H 0.4950 0.2449 0.4170 0.093 Uiso 1 1 calc R U . . .
H36B H 0.5340 0.1863 0.4013 0.093 Uiso 1 1 calc R U . . .
C3 C 0.3374(3) -0.1056(4) 0.0269(6) 0.089(3) Uani 1 1 d . . . . .
H3A H 0.2985 -0.1212 0.0202 0.107 Uiso 1 1 calc R U . . .
H3B H 0.3418 -0.0712 -0.0154 0.107 Uiso 1 1 calc R U . . .
C4 C 0.3749(3) -0.1517(4) 0.0021(6) 0.093(3) Uani 1 1 d . . . . .
H4A H 0.3699 -0.1610 -0.0626 0.112 Uiso 1 1 calc R U . . .
H4B H 0.3661 -0.1890 0.0365 0.112 Uiso 1 1 calc R U . . .
C35 C 0.5148(3) 0.2312(4) 0.2837(7) 0.086(3) Uani 1 1 d . . . . .
H35A H 0.5481 0.2582 0.2852 0.103 Uiso 1 1 calc R U . . .
H35B H 0.5237 0.1959 0.2447 0.103 Uiso 1 1 calc R U . . .
C38 C 0.3829(5) 0.1111(5) -0.0448(6) 0.096(3) 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 P1 2.233(2) . ?
Pd1 Si1 2.2183(18) . ?
Pd1 P2 2.254(2) . ?
Pd1 O1 2.247(4) . ?
P1 C13 1.786(6) . ?
P1 C7 1.798(5) . ?
P1 C1 1.801(6) . ?
Si1 C18 1.834(6) . ?
Si1 C20 1.848(5) . ?
Si1 C19 1.815(6) . ?
P2 C26 1.794(6) . ?
P2 C25 1.808(6) . ?
P2 C32 1.794(6) . ?
C18 C13 1.365(8) . ?
C18 C17 1.369(8) . ?
C13 C14 1.348(7) . ?
C20 C21 1.389(8) . ?
C20 C25 1.354(7) . ?
C21 C22 1.348(8) . ?
C7 C8 1.504(8) . ?
C7 C12 1.499(8) . ?
C16 C15 1.354(10) . ?
C16 C17 1.332(9) . ?
C26 C31 1.477(8) . ?
C26 C27 1.488(8) . ?
C24 C25 1.355(7) . ?
C24 C23 1.366(9) . ?
C31 C30 1.490(8) . ?
C14 C15 1.355(8) . ?
C27 C28 1.491(8) . ?
C28 C29 1.468(9) . ?
C8 C9 1.493(8) . ?
C12 C11 1.501(8) . ?
C22 C23 1.327(9) . ?
C29 C30 1.473(9) . ?
C9 C10 1.468(9) . ?
C10 C11 1.495(9) . ?
S1 O1 1.465(5) . ?
S1 O2 1.408(5) . ?
S1 O3 1.374(5) . ?
S1 C38 1.735(10) . ?
C33 C32 1.500(9) . ?
C33 C34 1.479(9) . ?
C1 C2 1.512(8) . ?
C1 C6 1.426(8) . ?
C32 C37 1.484(8) . ?
C2 C3 1.523(9) . ?
C37 C36 1.496(9) . ?
C6 C5 1.532(9) . ?
F1 C38 1.317(10) . ?
F3 C38 1.266(10) . ?
C34 C35 1.464(10) . ?
F2 C38 1.323(12) . ?
C5 C4 1.478(10) . ?
C36 C35 1.487(11) . ?
C3 C4 1.386(10) . ?

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 153.69(6) . . ?
P1 Pd1 O1 96.78(12) . . ?
Si1 Pd1 P1 84.97(7) . . ?
Si1 Pd1 P2 83.32(7) . . ?
Si1 Pd1 O1 162.96(13) . . ?
O1 Pd1 P2 101.29(13) . . ?
C13 P1 Pd1 110.8(2) . . ?
C13 P1 C7 102.3(3) . . ?
C13 P1 C1 110.6(3) . . ?
C7 P1 Pd1 111.62(19) . . ?
C7 P1 C1 106.4(3) . . ?
C1 P1 Pd1 114.4(2) . . ?
C18 Si1 Pd1 109.45(18) . . ?
C18 Si1 C20 113.3(2) . . ?
C20 Si1 Pd1 107.83(19) . . ?
C19 Si1 Pd1 110.3(2) . . ?
C19 Si1 C18 106.1(3) . . ?
C19 Si1 C20 109.9(3) . . ?
C26 P2 Pd1 119.9(2) . . ?
C26 P2 C25 109.1(3) . . ?
C25 P2 Pd1 108.45(19) . . ?
C32 P2 Pd1 109.4(2) . . ?
C32 P2 C26 105.2(3) . . ?
C32 P2 C25 103.6(3) . . ?
C13 C18 Si1 116.9(4) . . ?
C13 C18 C17 118.4(5) . . ?
C17 C18 Si1 124.6(5) . . ?
C18 C13 P1 117.0(4) . . ?
C14 C13 P1 122.1(5) . . ?
C14 C13 C18 120.9(5) . . ?
C21 C20 Si1 126.2(5) . . ?
C25 C20 Si1 116.2(4) . . ?
C25 C20 C21 117.7(5) . . ?
C22 C21 C20 121.4(6) . . ?
C8 C7 P1 111.2(4) . . ?
C12 C7 P1 111.4(4) . . ?
C12 C7 C8 111.2(5) . . ?
C17 C16 C15 120.4(6) . . ?
C31 C26 P2 112.2(4) . . ?
C31 C26 C27 111.1(5) . . ?
C27 C26 P2 115.5(4) . . ?
C25 C24 C23 121.0(6) . . ?
C20 C25 P2 116.4(4) . . ?
C20 C25 C24 120.1(5) . . ?
C24 C25 P2 123.5(5) . . ?
C26 C31 C30 110.9(5) . . ?
C13 C14 C15 119.5(6) . . ?
C26 C27 C28 110.3(6) . . ?
C29 C28 C27 111.4(5) . . ?
C9 C8 C7 111.5(5) . . ?
C7 C12 C11 110.5(5) . . ?
C23 C22 C21 120.2(6) . . ?
C28 C29 C30 111.7(5) . . ?
C16 C15 C14 120.1(6) . . ?
C29 C30 C31 111.0(6) . . ?
C16 C17 C18 120.7(6) . . ?
C10 C9 C8 110.7(6) . . ?
C9 C10 C11 112.5(6) . . ?
C22 C23 C24 119.6(6) . . ?
C10 C11 C12 111.2(6) . . ?
O1 S1 C38 100.8(4) . . ?
O2 S1 O1 115.3(3) . . ?
O2 S1 C38 103.5(5) . . ?
O3 S1 O1 115.3(4) . . ?
O3 S1 O2 114.5(4) . . ?
O3 S1 C38 105.0(4) . . ?
S1 O1 Pd1 116.4(3) . . ?
C34 C33 C32 112.0(6) . . ?
C2 C1 P1 110.2(4) . . ?
C6 C1 P1 119.6(5) . . ?
C6 C1 C2 111.4(5) . . ?
C33 C32 P2 110.7(4) . . ?
C37 C32 P2 110.4(4) . . ?
C37 C32 C33 109.4(5) . . ?
C1 C2 C3 109.9(5) . . ?
C32 C37 C36 112.1(6) . . ?
C1 C6 C5 111.2(6) . . ?
C35 C34 C33 110.7(6) . . ?
C4 C5 C6 110.7(7) . . ?
C35 C36 C37 110.3(6) . . ?
C4 C3 C2 115.2(7) . . ?
C3 C4 C5 112.3(7) . . ?
C34 C35 C36 110.0(7) . . ?
F1 C38 S1 111.9(8) . . ?
F1 C38 F2 107.9(8) . . ?
F3 C38 S1 111.8(7) . . ?
F3 C38 F1 108.9(9) . . ?
F3 C38 F2 108.1(10) . . ?
F2 C38 S1 108.3(7) . . ?

_audit_update_record             
;
????
;
_database_code_depnum_ccdc_archive 'CCDC 997347'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_007140
_audit_creation_date             2014-05-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38.73 H59.32 Cl0.14 P2 Pd Si'
_chemical_formula_sum            'C39 H60 P2 Pd Si'
_chemical_formula_weight         725.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9946(4)
_cell_length_b                   14.2318(4)
_cell_length_c                   20.8681(15)
_cell_angle_alpha                90
_cell_angle_beta                 100.188(7)
_cell_angle_gamma                90
_cell_volume                     3798.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    56378
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.030
_diffrn_ambient_temperature      223
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       
;
SCXMini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.076975
_diffrn_orient_matrix_UB_12      0.007285
_diffrn_orient_matrix_UB_13      0.015262
_diffrn_orient_matrix_UB_21      -0.002319
_diffrn_orient_matrix_UB_22      0.062780
_diffrn_orient_matrix_UB_23      -0.021730
_diffrn_orient_matrix_UB_31      -0.013522
_diffrn_orient_matrix_UB_32      0.030704
_diffrn_orient_matrix_UB_33      0.040809
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7534
_reflns_number_total             8675
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8675
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²+2.6381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0827
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C9(H9), C34(H34), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C4(H4A,H4B), C33(H33A,H33B), C14(H14A,H14B), C10(H10A,H10B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C8(H8A,H8B), C11(H11A,H11B),
 C5(H5A,H5B), C35(H35A,H35B), C7(H7A,H7B), C6(H6A,H6B), C39(H39A,H39B),
 C12(H12A,H12B), C13(H13A,H13B), C36(H36A,H36B), C38(H38A,H38B), C37(H37A,H37B),
  C1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C16(H16), C26(H26), C19(H19), C25(H25), C17(H17), C24(H24), C18(H18)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.31642(2) 0.79977(2) 0.81726(2) 0.02958(6) Uani 1 1 d . . . . .
P1 P 0.18978(5) 0.89688(4) 0.84407(3) 0.03073(14) Uani 1 1 d . . . . .
P2 P 0.40053(5) 0.66304(4) 0.79824(3) 0.03086(14) Uani 1 1 d . . . . .
Si1 Si 0.29350(5) 0.72047(5) 0.91089(3) 0.03126(15) Uani 1 1 d . . . . .
C27 C 0.12187(19) 0.84226(18) 0.90538(12) 0.0344(5) Uani 1 1 d . . . . .
C22 C 0.16275(19) 0.75690(18) 0.93185(12) 0.0367(6) Uani 1 1 d . . . . .
C3 C 0.3452(2) 0.62490(18) 0.71449(12) 0.0348(5) Uani 1 1 d . . . . .
H3 H 0.3615 0.6754 0.6859 0.042 Uiso 1 1 calc R . . . .
C23 C 0.1089(2) 0.7102(2) 0.97515(15) 0.0534(8) Uani 1 1 d . . . . .
H23 H 0.1352 0.6538 0.9938 0.064 Uiso 1 1 calc R . . . .
C29 C 0.1681(2) 1.08074(17) 0.89925(13) 0.0385(6) Uani 1 1 d . . . . .
H29A H 0.1415 1.0536 0.9357 0.046 Uiso 1 1 calc R . . . .
H29B H 0.1092 1.0923 0.8645 0.046 Uiso 1 1 calc R . . . .
C20 C 0.3149(2) 0.59011(17) 0.90051(13) 0.0359(6) Uani 1 1 d . . . . .
C15 C 0.37334(19) 0.56690(17) 0.85213(12) 0.0338(5) Uani 1 1 d . . . . .
C16 C 0.4119(2) 0.47572(19) 0.84860(14) 0.0439(6) Uani 1 1 d . . . . .
H16 H 0.4522 0.4612 0.8173 0.053 Uiso 1 1 calc R . . . .
C4 C 0.2258(2) 0.6210(2) 0.70489(15) 0.0526(8) Uani 1 1 d . . . . .
H4A H 0.2047 0.5694 0.7300 0.063 Uiso 1 1 calc R . . . .
H4B H 0.1996 0.6789 0.7206 0.063 Uiso 1 1 calc R . . . .
C33 C 0.3407(2) 0.99684(18) 0.92756(14) 0.0418(6) Uani 1 1 d . . . . .
H33A H 0.3212 0.9657 0.9650 0.050 Uiso 1 1 calc R . . . .
H33B H 0.3894 0.9564 0.9103 0.050 Uiso 1 1 calc R . . . .
C9 C 0.54429(19) 0.65741(18) 0.80370(12) 0.0357(5) Uani 1 1 d . . . . .
H9 H 0.5623 0.5934 0.7924 0.043 Uiso 1 1 calc R . . . .
C34 C 0.0772(2) 0.9262(2) 0.77883(13) 0.0412(6) Uani 1 1 d . . . . .
H34 H 0.0223 0.9526 0.8002 0.049 Uiso 1 1 calc R . . . .
C26 C 0.0311(2) 0.8792(2) 0.92295(14) 0.0425(6) Uani 1 1 d . . . . .
H26 H 0.0052 0.9368 0.9061 0.051 Uiso 1 1 calc R . . . .
C14 C 0.5992(2) 0.6768(3) 0.87385(15) 0.0550(8) Uani 1 1 d . . . . .
H14A H 0.5769 0.6309 0.9029 0.066 Uiso 1 1 calc R . . . .
H14B H 0.5796 0.7387 0.8871 0.066 Uiso 1 1 calc R . . . .
C28 C 0.24319(18) 1.01164(16) 0.87565(12) 0.0310(5) Uani 1 1 d . . . . .
H28 H 0.2675 1.0427 0.8391 0.037 Uiso 1 1 calc R . . . .
C10 C 0.5826(2) 0.7245(2) 0.75628(16) 0.0499(7) Uani 1 1 d . . . . .
H10A H 0.5612 0.7880 0.7646 0.060 Uiso 1 1 calc R . . . .
H10B H 0.5506 0.7080 0.7121 0.060 Uiso 1 1 calc R . . . .
C19 C 0.2958(3) 0.5190(2) 0.94335(15) 0.0506(7) Uani 1 1 d . . . . .
H19 H 0.2576 0.5330 0.9759 0.061 Uiso 1 1 calc R . . . .
C30 C 0.2233(2) 1.17394(18) 0.92024(13) 0.0398(6) Uani 1 1 d . . . . .
H30A H 0.2432 1.2042 0.8826 0.048 Uiso 1 1 calc R . . . .
H30B H 0.1753 1.2153 0.9373 0.048 Uiso 1 1 calc R . . . .
C25 C -0.0204(2) 0.8308(2) 0.96508(15) 0.0505(7) Uani 1 1 d . . . . .
H25 H -0.0811 0.8555 0.9762 0.061 Uiso 1 1 calc R . . . .
C21 C 0.3897(2) 0.7460(2) 0.98788(14) 0.0468(7) Uani 1 1 d . . . . .
H21A H 0.4592 0.7320 0.9811 0.070 Uiso 1 1 calc GR . . . .
H21B H 0.3734 0.7079 1.0227 0.070 Uiso 1 1 calc GR . . . .
H21C H 0.3854 0.8112 0.9990 0.070 Uiso 1 1 calc GR . . . .
C31 C 0.3196(2) 1.15880(19) 0.97154(14) 0.0455(7) Uani 1 1 d . . . . .
H31A H 0.3549 1.2184 0.9817 0.055 Uiso 1 1 calc R . . . .
H31B H 0.2988 1.1353 1.0110 0.055 Uiso 1 1 calc R . . . .
C32 C 0.3940(2) 1.08992(19) 0.94898(16) 0.0494(7) Uani 1 1 d . . . . .
H32A H 0.4522 1.0785 0.9842 0.059 Uiso 1 1 calc R . . . .
H32B H 0.4217 1.1170 0.9129 0.059 Uiso 1 1 calc R . . . .
C8 C 0.3872(2) 0.5349(2) 0.68858(14) 0.0458(7) Uani 1 1 d . . . . .
H8A H 0.3695 0.4814 0.7133 0.055 Uiso 1 1 calc R . . . .
H8B H 0.4628 0.5384 0.6937 0.055 Uiso 1 1 calc R . . . .
C17 C 0.3908(3) 0.4071(2) 0.89105(15) 0.0532(8) Uani 1 1 d . . . . .
H17 H 0.4158 0.3464 0.8878 0.064 Uiso 1 1 calc R . . . .
C24 C 0.0175(3) 0.7462(2) 0.99063(16) 0.0583(8) Uani 1 1 d . . . . .
H24 H -0.0181 0.7132 1.0183 0.070 Uiso 1 1 calc R . . . .
C11 C 0.7011(2) 0.7212(3) 0.76247(17) 0.0584(8) Uani 1 1 d . . . . .
H11A H 0.7216 0.6601 0.7485 0.070 Uiso 1 1 calc R . . . .
H11B H 0.7230 0.7681 0.7339 0.070 Uiso 1 1 calc R . . . .
C5 C 0.1787(3) 0.6077(3) 0.63319(17) 0.0642(9) Uani 1 1 d . . . . .
H5A H 0.1033 0.6022 0.6286 0.077 Uiso 1 1 calc R . . . .
H5B H 0.1939 0.6624 0.6088 0.077 Uiso 1 1 calc R . . . .
C35 C 0.1016(2) 0.9995(3) 0.73003(15) 0.0572(8) Uani 1 1 d . . . . .
H35A H 0.1598 0.9779 0.7106 0.069 Uiso 1 1 calc R . . . .
H35B H 0.1221 1.0580 0.7527 0.069 Uiso 1 1 calc R . . . .
C18 C 0.3324(3) 0.4285(2) 0.93834(16) 0.0579(8) Uani 1 1 d . . . . .
H18 H 0.3176 0.3821 0.9668 0.070 Uiso 1 1 calc R . . . .
C7 C 0.3400(3) 0.5219(3) 0.61640(15) 0.0606(9) Uani 1 1 d . . . . .
H7A H 0.3635 0.5725 0.5913 0.073 Uiso 1 1 calc R . . . .
H7B H 0.3645 0.4631 0.6010 0.073 Uiso 1 1 calc R . . . .
C6 C 0.2213(3) 0.5214(2) 0.60537(16) 0.0607(9) Uani 1 1 d . . . . .
H6A H 0.1943 0.5182 0.5590 0.073 Uiso 1 1 calc R . . . .
H6B H 0.1976 0.4659 0.6255 0.073 Uiso 1 1 calc R . . . .
C39 C 0.0339(3) 0.8358(3) 0.74495(19) 0.0715(10) Uani 1 1 d . . . . .
H39A H 0.0884 0.8048 0.7265 0.086 Uiso 1 1 calc R . . . .
H39B H 0.0124 0.7937 0.7767 0.086 Uiso 1 1 calc R . . . .
C12 C 0.7562(3) 0.7391(3) 0.83163(19) 0.0686(10) Uani 1 1 d . . . . .
H12A H 0.7432 0.8033 0.8437 0.082 Uiso 1 1 calc R . . . .
H12B H 0.8310 0.7316 0.8340 0.082 Uiso 1 1 calc R . . . .
C13 C 0.7186(2) 0.6719(3) 0.87920(17) 0.0685(10) Uani 1 1 d . . . . .
H13A H 0.7518 0.6877 0.9232 0.082 Uiso 1 1 calc R . . . .
H13B H 0.7388 0.6083 0.8702 0.082 Uiso 1 1 calc R . . . .
C36 C 0.0068(3) 1.0172(3) 0.67636(19) 0.0794(12) Uani 1 1 d . . . . .
H36A H -0.0491 1.0451 0.6952 0.095 Uiso 1 1 calc R . . . .
H36B H 0.0257 1.0610 0.6448 0.095 Uiso 1 1 calc R . . . .
C38 C -0.0589(4) 0.8554(4) 0.6912(3) 0.1078(17) Uani 1 1 d . . . . .
H38A H -0.1167 0.8792 0.7103 0.129 Uiso 1 1 calc R . . . .
H38B H -0.0813 0.7973 0.6687 0.129 Uiso 1 1 calc R . . . .
C37 C -0.0310(4) 0.9268(4) 0.6427(2) 0.1082(18) Uani 1 1 d . . . . .
H37A H 0.0232 0.9012 0.6212 0.130 Uiso 1 1 calc R . . . .
H37B H -0.0920 0.9393 0.6097 0.130 Uiso 1 1 calc R . . . .
C2 C 0.3218(4) 0.8718(3) 0.6664(3) 0.0653(13) Uani 0.863(8) 1 d . U P A 1
H2A H 0.3333 0.9257 0.6410 0.098 Uiso 0.863(8) 1 calc GR . P A 1
H2B H 0.2488 0.8561 0.6583 0.098 Uiso 0.863(8) 1 calc GR . P A 1
H2C H 0.3615 0.8196 0.6547 0.098 Uiso 0.863(8) 1 calc GR . P A 1
C1 C 0.3566(7) 0.8939(6) 0.7387(4) 0.0386(13) Uani 0.863(8) 1 d . U P A 1
H1A H 0.3296 0.9558 0.7460 0.046 Uiso 0.863(8) 1 calc R . P A 1
H1B H 0.4322 0.8993 0.7462 0.046 Uiso 0.863(8) 1 calc R . P A 1
Cl1 Cl 0.3490(16) 0.8799(15) 0.7240(11) 0.104(12) Uani 0.137(8) 1 d . . P A 2


_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 2.2929(6) . ?
Pd1 P2 2.3004(6) . ?
Pd1 Si1 2.3207(7) . ?
Pd1 C1 2.249(6) . ?
Pd1 Cl1 2.36(2) . ?
P1 C27 1.849(3) . ?
P1 C34 1.861(3) . ?
P1 C28 1.850(2) . ?
P2 C3 1.850(3) . ?
P2 C15 1.845(3) . ?
P2 C9 1.853(3) . ?
Si1 C22 1.900(3) . ?
Si1 C20 1.894(3) . ?
Si1 C21 1.888(3) . ?
C27 C22 1.400(4) . ?
C27 C26 1.399(3) . ?
C22 C23 1.404(4) . ?
C3 C4 1.530(4) . ?
C3 C8 1.528(4) . ?
C23 C24 1.383(4) . ?
C29 C28 1.527(3) . ?
C29 C30 1.535(4) . ?
C20 C15 1.405(3) . ?
C20 C19 1.402(4) . ?
C15 C16 1.398(3) . ?
C16 C17 1.378(4) . ?
C4 C5 1.525(4) . ?
C33 C28 1.529(3) . ?
C33 C32 1.525(4) . ?
C9 C14 1.536(4) . ?
C9 C10 1.521(4) . ?
C34 C35 1.530(4) . ?
C34 C39 1.527(4) . ?
C26 C25 1.380(4) . ?
C14 C13 1.537(4) . ?
C10 C11 1.523(4) . ?
C19 C18 1.383(4) . ?
C30 C31 1.511(4) . ?
C25 C24 1.372(4) . ?
C31 C32 1.510(4) . ?
C8 C7 1.534(4) . ?
C17 C18 1.381(4) . ?
C11 C12 1.515(5) . ?
C5 C6 1.505(5) . ?
C35 C36 1.532(4) . ?
C7 C6 1.519(5) . ?
C39 C38 1.520(5) . ?
C12 C13 1.520(5) . ?
C36 C37 1.505(6) . ?
C38 C37 1.523(7) . ?
C2 C1 1.529(9) . ?

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 159.30(2) . . ?
P1 Pd1 Si1 83.29(2) . . ?
P1 Pd1 Cl1 98.7(5) . . ?
P2 Pd1 Si1 82.51(2) . . ?
P2 Pd1 Cl1 96.1(5) . . ?
Si1 Pd1 Cl1 177.1(5) . . ?
C1 Pd1 P1 95.1(2) . . ?
C1 Pd1 P2 101.5(2) . . ?
C1 Pd1 Si1 169.8(3) . . ?
C27 P1 Pd1 111.49(8) . . ?
C27 P1 C34 101.01(12) . . ?
C27 P1 C28 108.64(11) . . ?
C34 P1 Pd1 117.52(9) . . ?
C28 P1 Pd1 112.26(8) . . ?
C28 P1 C34 105.03(12) . . ?
C3 P2 Pd1 107.10(8) . . ?
C3 P2 C9 105.34(11) . . ?
C15 P2 Pd1 111.97(8) . . ?
C15 P2 C3 105.90(12) . . ?
C15 P2 C9 103.31(12) . . ?
C9 P2 Pd1 122.04(9) . . ?
C22 Si1 Pd1 108.32(8) . . ?
C20 Si1 Pd1 109.67(8) . . ?
C20 Si1 C22 116.69(12) . . ?
C21 Si1 Pd1 117.29(10) . . ?
C21 Si1 C22 103.64(12) . . ?
C21 Si1 C20 101.39(12) . . ?
C22 C27 P1 116.34(18) . . ?
C26 C27 P1 123.5(2) . . ?
C26 C27 C22 120.1(2) . . ?
C27 C22 Si1 116.00(18) . . ?
C27 C22 C23 117.9(2) . . ?
C23 C22 Si1 125.9(2) . . ?
C4 C3 P2 110.49(18) . . ?
C8 C3 P2 118.47(19) . . ?
C8 C3 C4 109.9(2) . . ?
C24 C23 C22 121.4(3) . . ?
C28 C29 C30 110.8(2) . . ?
C15 C20 Si1 114.92(18) . . ?
C19 C20 Si1 126.0(2) . . ?
C19 C20 C15 117.9(2) . . ?
C20 C15 P2 116.72(18) . . ?
C16 C15 P2 123.2(2) . . ?
C16 C15 C20 120.0(2) . . ?
C17 C16 C15 120.7(3) . . ?
C5 C4 C3 110.8(3) . . ?
C32 C33 C28 111.4(2) . . ?
C14 C9 P2 110.15(18) . . ?
C10 C9 P2 112.04(19) . . ?
C10 C9 C14 110.9(2) . . ?
C35 C34 P1 114.28(19) . . ?
C39 C34 P1 109.1(2) . . ?
C39 C34 C35 111.7(3) . . ?
C25 C26 C27 120.4(3) . . ?
C9 C14 C13 110.7(2) . . ?
C29 C28 P1 117.54(17) . . ?
C29 C28 C33 110.9(2) . . ?
C33 C28 P1 110.03(16) . . ?
C9 C10 C11 111.6(3) . . ?
C18 C19 C20 121.5(3) . . ?
C31 C30 C29 111.5(2) . . ?
C24 C25 C26 120.3(3) . . ?
C32 C31 C30 111.6(2) . . ?
C31 C32 C33 111.8(2) . . ?
C3 C8 C7 110.0(2) . . ?
C16 C17 C18 120.0(3) . . ?
C25 C24 C23 119.9(3) . . ?
C12 C11 C10 112.1(3) . . ?
C6 C5 C4 111.6(3) . . ?
C34 C35 C36 111.3(3) . . ?
C17 C18 C19 119.9(3) . . ?
C6 C7 C8 111.7(3) . . ?
C5 C6 C7 111.7(3) . . ?
C38 C39 C34 111.5(3) . . ?
C11 C12 C13 111.3(3) . . ?
C12 C13 C14 111.1(3) . . ?
C37 C36 C35 110.8(3) . . ?
C39 C38 C37 111.2(4) . . ?
C36 C37 C38 110.9(4) . . ?
C2 C1 Pd1 122.0(5) . . ?

_database_code_depnum_ccdc_archive 'CCDC 1001292'
