# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc180b
_database_code_depnum_ccdc_archive 'CCDC 1436834'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H44 P2 Pd Si'
_chemical_formula_weight         613.09

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   17.0258(7)
_cell_length_b                   18.6108(8)
_cell_length_c                   19.0877(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6048.2(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2560
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6519
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            135804
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0075
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5331
_reflns_number_gt                5118
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0131P)²+9.7522P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5331
_refine_ls_number_parameters     336
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0580
_refine_ls_wR_factor_gt          0.0574
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_restrained_S_all      1.194
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.766117(9) 0.173410(8) 0.608289(8) 0.01553(6) Uani 1 1 d . . .
C C 0.66150(12) 0.12101(11) 0.56822(11) 0.0155(4) Uani 1 1 d . . .
H1 H 0.8391(18) 0.2116(17) 0.6388(16) 0.051(9) Uiso 1 1 d . . .
P1 P 0.69098(3) 0.20226(3) 0.70009(3) 0.01658(12) Uani 1 1 d . . .
Si Si 0.64397(4) 0.18335(3) 0.49250(3) 0.01886(13) Uani 1 1 d . . .
P2 P 0.83150(3) 0.10459(3) 0.52793(3) 0.01580(12) Uani 1 1 d . . .
H2 H 0.6029(15) 0.2427(14) 0.5170(13) 0.029(7) Uiso 1 1 d . . .
C11 C 0.59369(12) 0.16927(11) 0.67716(11) 0.0160(4) Uani 1 1 d . . .
H3 H 0.7124(15) 0.2092(14) 0.4637(13) 0.026(7) Uiso 1 1 d . . .
C12 C 0.58896(13) 0.13009(11) 0.61458(11) 0.0169(4) Uani 1 1 d . . .
C13 C 0.51360(13) 0.10732(12) 0.59337(12) 0.0218(5) Uani 1 1 d . . .
H13 H 0.5079 0.0822 0.5503 0.026 Uiso 1 1 calc R . .
C14 C 0.44772(13) 0.12073(13) 0.63390(13) 0.0255(5) Uani 1 1 d . . .
H14 H 0.3978 0.1038 0.6189 0.031 Uiso 1 1 calc R . .
C15 C 0.45400(13) 0.15858(13) 0.69620(13) 0.0244(5) Uani 1 1 d . . .
H15 H 0.4088 0.1672 0.7241 0.029 Uiso 1 1 calc R . .
C16 C 0.52652(13) 0.18366(12) 0.71722(12) 0.0215(5) Uani 1 1 d . . .
H16 H 0.5310 0.2109 0.7591 0.026 Uiso 1 1 calc R . .
C31 C 0.58580(13) 0.14491(12) 0.41717(12) 0.0211(5) Uani 1 1 d . . .
C26 C 0.78074(13) -0.03744(12) 0.49826(12) 0.0209(5) Uani 1 1 d . . .
H26 H 0.8309 -0.0451 0.4777 0.025 Uiso 1 1 calc R . .
C25 C 0.72971(14) -0.09474(13) 0.50529(12) 0.0246(5) Uani 1 1 d . . .
H25 H 0.7442 -0.1413 0.4896 0.029 Uiso 1 1 calc R . .
C24 C 0.65711(14) -0.08276(13) 0.53572(13) 0.0251(5) Uani 1 1 d . . .
H24 H 0.6221 -0.1219 0.5424 0.030 Uiso 1 1 calc R . .
C23 C 0.63476(13) -0.01458(12) 0.55647(12) 0.0216(5) Uani 1 1 d . . .
H23 H 0.5844 -0.0080 0.5769 0.026 Uiso 1 1 calc R . .
C22 C 0.68426(13) 0.04528(11) 0.54831(10) 0.0154(4) Uani 1 1 d . . .
C21 C 0.76022(13) 0.03150(11) 0.52073(11) 0.0161(4) Uani 1 1 d . . .
C32 C 0.51744(14) 0.17858(14) 0.39327(13) 0.0276(5) Uani 1 1 d . . .
H32 H 0.4986 0.2200 0.4170 0.033 Uiso 1 1 calc R . .
C33 C 0.47649(15) 0.15286(16) 0.33562(14) 0.0365(7) Uani 1 1 d . . .
H33 H 0.4305 0.1769 0.3200 0.044 Uiso 1 1 calc R . .
C34 C 0.50274(17) 0.09242(16) 0.30113(14) 0.0386(7) Uani 1 1 d . . .
H34 H 0.4745 0.0745 0.2619 0.046 Uiso 1 1 calc R . .
C35 C 0.56994(18) 0.05792(14) 0.32339(13) 0.0352(6) Uani 1 1 d . . .
H35 H 0.5882 0.0165 0.2993 0.042 Uiso 1 1 calc R . .
C36 C 0.61091(16) 0.08389(13) 0.38100(12) 0.0281(5) Uani 1 1 d . . .
H36 H 0.6570 0.0596 0.3961 0.034 Uiso 1 1 calc R . .
C41 C 0.67668(16) 0.29557(13) 0.72833(14) 0.0327(6) Uani 1 1 d . . .
H41 H 0.6363 0.2962 0.7664 0.039 Uiso 1 1 calc R . .
C42 C 0.71978(14) 0.15152(15) 0.77919(12) 0.0295(6) Uani 1 1 d . . .
H42 H 0.7737 0.1678 0.7926 0.035 Uiso 1 1 calc R . .
C43 C 0.6452(3) 0.33882(15) 0.66632(18) 0.0632(11) Uani 1 1 d . . .
H43A H 0.6844 0.3392 0.6287 0.095 Uiso 1 1 calc R . .
H43B H 0.6346 0.3882 0.6813 0.095 Uiso 1 1 calc R . .
H43C H 0.5966 0.3168 0.6492 0.095 Uiso 1 1 calc R . .
C44 C 0.7531(2) 0.3265(2) 0.7575(2) 0.0722(14) Uani 1 1 d . . .
H44A H 0.7937 0.3250 0.7212 0.108 Uiso 1 1 calc R . .
H44B H 0.7700 0.2979 0.7979 0.108 Uiso 1 1 calc R . .
H44C H 0.7444 0.3764 0.7721 0.108 Uiso 1 1 calc R . .
C45 C 0.66651(18) 0.16416(19) 0.84214(13) 0.0441(8) Uani 1 1 d . . .
H45A H 0.6651 0.2156 0.8531 0.066 Uiso 1 1 calc R . .
H45B H 0.6869 0.1376 0.8826 0.066 Uiso 1 1 calc R . .
H45C H 0.6133 0.1474 0.8312 0.066 Uiso 1 1 calc R . .
C46 C 0.7247(2) 0.07146(16) 0.76240(16) 0.0480(8) Uani 1 1 d . . .
H46A H 0.6720 0.0530 0.7521 0.072 Uiso 1 1 calc R . .
H46B H 0.7466 0.0457 0.8027 0.072 Uiso 1 1 calc R . .
H46C H 0.7587 0.0642 0.7216 0.072 Uiso 1 1 calc R . .
C51 C 0.85360(16) 0.13393(13) 0.43714(12) 0.0274(5) Uani 1 1 d . . .
H51 H 0.8017 0.1374 0.4129 0.033 Uiso 1 1 calc R . .
C52 C 0.92070(13) 0.05978(12) 0.56145(12) 0.0221(5) Uani 1 1 d . . .
H52 H 0.9334 0.0181 0.5303 0.027 Uiso 1 1 calc R . .
C53 C 0.90241(19) 0.08115(16) 0.39383(14) 0.0416(7) Uani 1 1 d . . .
H53A H 0.8769 0.0340 0.3939 0.062 Uiso 1 1 calc R . .
H53B H 0.9550 0.0769 0.4142 0.062 Uiso 1 1 calc R . .
H53C H 0.9066 0.0987 0.3456 0.062 Uiso 1 1 calc R . .
C54 C 0.88819(17) 0.20995(14) 0.43551(15) 0.0379(7) Uani 1 1 d . . .
H54A H 0.8896 0.2273 0.3871 0.057 Uiso 1 1 calc R . .
H54B H 0.9416 0.2090 0.4546 0.057 Uiso 1 1 calc R . .
H54C H 0.8555 0.2421 0.4638 0.057 Uiso 1 1 calc R . .
C55 C 0.90424(15) 0.03167(14) 0.63509(13) 0.0310(6) Uani 1 1 d . . .
H55A H 0.8576 0.0008 0.6342 0.046 Uiso 1 1 calc R . .
H55B H 0.8950 0.0722 0.6668 0.046 Uiso 1 1 calc R . .
H55C H 0.9495 0.0039 0.6516 0.046 Uiso 1 1 calc R . .
C56 C 0.99116(14) 0.11027(15) 0.56324(16) 0.0360(6) Uani 1 1 d . . .
H56A H 1.0040 0.1255 0.5154 0.054 Uiso 1 1 calc R . .
H56B H 1.0363 0.0852 0.5837 0.054 Uiso 1 1 calc R . .
H56C H 0.9785 0.1525 0.5917 0.054 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
Pd C 2.170(2) . ?
Pd P1 2.2350(6) . ?
Pd P2 2.2876(6) . ?
Pd Si 3.0404(6) . ?
Pd H1 1.54(3) . ?
C C22 1.510(3) . ?
C C12 1.529(3) . ?
C Si 1.877(2) . ?
P1 C11 1.820(2) . ?
P1 C41 1.835(2) . ?
P1 C42 1.847(2) . ?
Si C31 1.887(2) . ?
Si H2 1.39(3) . ?
Si H3 1.37(3) . ?
P2 C21 1.828(2) . ?
P2 C52 1.847(2) . ?
P2 C51 1.855(2) . ?
C11 C16 1.402(3) . ?
C11 C12 1.402(3) . ?
C12 C13 1.411(3) . ?
C13 C14 1.385(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.380(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C31 C36 1.396(3) . ?
C31 C32 1.398(3) . ?
C26 C25 1.382(3) . ?
C26 C21 1.397(3) . ?
C26 H26 0.9500 . ?
C25 C24 1.384(3) . ?
C25 H25 0.9500 . ?
C24 C23 1.383(3) . ?
C24 H24 0.9500 . ?
C23 C22 1.406(3) . ?
C23 H23 0.9500 . ?
C22 C21 1.420(3) . ?
C32 C33 1.388(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.378(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.389(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C44 1.527(4) . ?
C41 C43 1.528(4) . ?
C41 H41 1.0000 . ?
C42 C45 1.524(3) . ?
C42 C46 1.526(4) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C53 1.529(3) . ?
C51 C54 1.533(4) . ?
C51 H51 1.0000 . ?
C52 C56 1.524(3) . ?
C52 C55 1.526(3) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C Pd P1 85.10(6) . . ?
C Pd P2 84.92(6) . . ?
P1 Pd P2 159.85(2) . . ?
C Pd Si 37.78(6) . . ?
P1 Pd Si 99.43(2) . . ?
P2 Pd Si 83.079(19) . . ?
C Pd H1 178.2(12) . . ?
P1 Pd H1 93.1(12) . . ?
P2 Pd H1 96.8(12) . . ?
Si Pd H1 142.8(12) . . ?
C22 C C12 117.14(18) . . ?
C22 C Si 115.08(14) . . ?
C12 C Si 104.41(14) . . ?
C22 C Pd 107.30(14) . . ?
C12 C Pd 114.17(14) . . ?
Si C Pd 97.13(9) . . ?
C11 P1 C41 105.62(11) . . ?
C11 P1 C42 105.41(11) . . ?
C41 P1 C42 106.20(13) . . ?
C11 P1 Pd 104.55(7) . . ?
C41 P1 Pd 122.25(8) . . ?
C42 P1 Pd 111.48(8) . . ?
C Si C31 115.84(10) . . ?
C Si Pd 45.09(6) . . ?
C31 Si Pd 152.86(8) . . ?
C Si H2 108.2(11) . . ?
C31 Si H2 107.1(10) . . ?
Pd Si H2 98.5(10) . . ?
C Si H3 112.9(11) . . ?
C31 Si H3 105.8(10) . . ?
Pd Si H3 74.5(10) . . ?
H2 Si H3 106.5(15) . . ?
C21 P2 C52 103.65(10) . . ?
C21 P2 C51 106.46(11) . . ?
C52 P2 C51 106.84(11) . . ?
C21 P2 Pd 98.28(7) . . ?
C52 P2 Pd 114.87(8) . . ?
C51 P2 Pd 124.07(8) . . ?
C16 C11 C12 121.2(2) . . ?
C16 C11 P1 123.15(17) . . ?
C12 C11 P1 115.64(16) . . ?
C11 C12 C13 116.9(2) . . ?
C11 C12 C 120.29(19) . . ?
C13 C12 C 122.38(19) . . ?
C14 C13 C12 121.5(2) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 C15 120.5(2) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C16 C15 C14 119.4(2) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C11 120.5(2) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C36 C31 C32 117.3(2) . . ?
C36 C31 Si 121.63(18) . . ?
C32 C31 Si 121.04(19) . . ?
C25 C26 C21 121.4(2) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
C26 C25 C24 118.6(2) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C23 C24 C25 120.9(2) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C23 C22 122.0(2) . . ?
C24 C23 H23 119.0 . . ?
C22 C23 H23 119.0 . . ?
C23 C22 C21 116.37(19) . . ?
C23 C22 C 123.91(19) . . ?
C21 C22 C 119.71(19) . . ?
C26 C21 C22 120.5(2) . . ?
C26 C21 P2 122.71(17) . . ?
C22 C21 P2 116.26(16) . . ?
C33 C32 C31 121.5(3) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C34 C33 C32 119.8(2) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 120.1(2) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 119.9(3) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C31 121.4(2) . . ?
C35 C36 H36 119.3 . . ?
C31 C36 H36 119.3 . . ?
C44 C41 C43 112.5(3) . . ?
C44 C41 P1 110.5(2) . . ?
C43 C41 P1 108.51(19) . . ?
C44 C41 H41 108.4 . . ?
C43 C41 H41 108.4 . . ?
P1 C41 H41 108.4 . . ?
C45 C42 C46 110.4(2) . . ?
C45 C42 P1 114.06(18) . . ?
C46 C42 P1 109.99(18) . . ?
C45 C42 H42 107.4 . . ?
C46 C42 H42 107.4 . . ?
P1 C42 H42 107.4 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C53 C51 C54 111.9(2) . . ?
C53 C51 P2 115.21(17) . . ?
C54 C51 P2 111.62(18) . . ?
C53 C51 H51 105.8 . . ?
C54 C51 H51 105.8 . . ?
P2 C51 H51 105.8 . . ?
C56 C52 C55 109.6(2) . . ?
C56 C52 P2 112.12(17) . . ?
C55 C52 P2 108.84(16) . . ?
C56 C52 H52 108.7 . . ?
C55 C52 H52 108.7 . . ?
P2 C52 H52 108.7 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 C56 H56A 109.5 . . ?
C52 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C52 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.054
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc170b
_database_code_depnum_ccdc_archive 'CCDC 1436835'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H48 P2 Pd Si'
_chemical_formula_weight         689.18

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   9.402(3)
_cell_length_b                   19.186(5)
_cell_length_c                   19.053(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.284(5)
_cell_angle_gamma                90.00
_cell_volume                     3431.3(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6944
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37894
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6047
_reflns_number_gt                4806
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0304P)²+1.6562P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6047
_refine_ls_number_parameters     386
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.26540(2) 0.847627(11) 0.224275(11) 0.01230(7) Uani 1 1 d . . .
P1 P 0.28267(8) 0.80114(4) 0.33229(4) 0.01460(17) Uani 1 1 d . . .
P2 P 0.16878(8) 0.86909(4) 0.11370(4) 0.01378(17) Uani 1 1 d . . .
C C 0.0811(3) 0.90247(14) 0.26035(14) 0.0130(6) Uani 1 1 d . . .
C11 C 0.1538(3) 0.85018(15) 0.37998(14) 0.0161(6) Uani 1 1 d . . .
C12 C 0.0582(3) 0.89195(14) 0.33844(14) 0.0140(6) Uani 1 1 d . . .
C13 C -0.0467(3) 0.92831(15) 0.37303(15) 0.0190(7) Uani 1 1 d . . .
H13 H -0.1137 0.9559 0.3462 0.023 Uiso 1 1 calc R . .
C14 C -0.0552(3) 0.92503(16) 0.44530(16) 0.0254(7) Uani 1 1 d . . .
H14 H -0.1273 0.9502 0.4673 0.030 Uiso 1 1 calc R . .
C15 C 0.0412(4) 0.88512(16) 0.48549(16) 0.0270(8) Uani 1 1 d . . .
H15 H 0.0362 0.8834 0.5351 0.032 Uiso 1 1 calc R . .
C16 C 0.1444(3) 0.84799(16) 0.45323(15) 0.0238(7) Uani 1 1 d . . .
H16 H 0.2102 0.8205 0.4809 0.029 Uiso 1 1 calc R . .
C21 C -0.0169(3) 0.87844(14) 0.13588(15) 0.0159(6) Uani 1 1 d . . .
C22 C -0.0419(3) 0.88591(14) 0.20847(14) 0.0141(6) Uani 1 1 d . . .
C23 C -0.1835(3) 0.87702(15) 0.22702(16) 0.0210(7) Uani 1 1 d . . .
H23 H -0.2036 0.8785 0.2753 0.025 Uiso 1 1 calc R . .
C24 C -0.2947(3) 0.86612(16) 0.17730(17) 0.0274(8) Uani 1 1 d . . .
H24 H -0.3889 0.8602 0.1919 0.033 Uiso 1 1 calc R . .
C25 C -0.2693(4) 0.86384(17) 0.10647(18) 0.0305(8) Uani 1 1 d . . .
H25 H -0.3457 0.8585 0.0721 0.037 Uiso 1 1 calc R . .
C26 C -0.1310(3) 0.86945(17) 0.08682(17) 0.0271(8) Uani 1 1 d . . .
H26 H -0.1129 0.8671 0.0383 0.033 Uiso 1 1 calc R . .
C31 C 0.4488(3) 0.79580(15) 0.38836(15) 0.0196(7) Uani 1 1 d . . .
H31 H 0.4261 0.7794 0.4363 0.023 Uiso 1 1 calc R . .
C32 C 0.2126(3) 0.71068(15) 0.32865(16) 0.0224(7) Uani 1 1 d . . .
H32 H 0.2746 0.6834 0.2977 0.027 Uiso 1 1 calc R . .
C33 C 0.5176(3) 0.86714(16) 0.39439(18) 0.0278(8) Uani 1 1 d . . .
H33A H 0.5386 0.8838 0.3475 0.042 Uiso 1 1 calc R . .
H33B H 0.6064 0.8640 0.4238 0.042 Uiso 1 1 calc R . .
H33C H 0.4525 0.8997 0.4158 0.042 Uiso 1 1 calc R . .
H2 H 0.196(3) 1.0058(14) 0.1866(15) 0.020(8) Uiso 1 1 d . . .
H1 H 0.390(3) 0.8037(15) 0.2010(15) 0.024(8) Uiso 1 1 d . . .
Si Si 0.14726(8) 0.99462(4) 0.25230(4) 0.01316(17) Uani 1 1 d . . .
C34 C 0.5514(3) 0.74417(16) 0.35678(17) 0.0271(8) Uani 1 1 d . . .
H34A H 0.5709 0.7590 0.3090 0.041 Uiso 1 1 calc R . .
H34B H 0.5083 0.6976 0.3552 0.041 Uiso 1 1 calc R . .
H34C H 0.6407 0.7428 0.3859 0.041 Uiso 1 1 calc R . .
C35 C 0.2147(4) 0.67306(17) 0.39917(19) 0.0414(10) Uani 1 1 d . . .
H35A H 0.1740 0.6263 0.3925 0.062 Uiso 1 1 calc R . .
H35B H 0.1583 0.6995 0.4317 0.062 Uiso 1 1 calc R . .
H35C H 0.3132 0.6692 0.4186 0.062 Uiso 1 1 calc R . .
C36 C 0.0627(3) 0.71033(16) 0.29339(18) 0.0289(8) Uani 1 1 d . . .
H36A H 0.0624 0.7365 0.2492 0.043 Uiso 1 1 calc R . .
H36B H -0.0035 0.7321 0.3247 0.043 Uiso 1 1 calc R . .
H36C H 0.0330 0.6622 0.2836 0.043 Uiso 1 1 calc R . .
C41 C 0.2078(3) 0.94387(15) 0.05609(15) 0.0184(7) Uani 1 1 d . . .
H41 H 0.1580 0.9849 0.0758 0.022 Uiso 1 1 calc R . .
C42 C 0.1680(3) 0.79170(15) 0.05613(16) 0.0223(7) Uani 1 1 d . . .
H42 H 0.1035 0.8014 0.0137 0.027 Uiso 1 1 calc R . .
C43 C 0.1510(4) 0.93784(17) -0.02069(15) 0.0309(8) Uani 1 1 d . . .
H43A H 0.1707 0.9812 -0.0456 0.046 Uiso 1 1 calc R . .
H43B H 0.0480 0.9296 -0.0224 0.046 Uiso 1 1 calc R . .
H43C H 0.1981 0.8989 -0.0432 0.046 Uiso 1 1 calc R . .
C44 C 0.3671(3) 0.96207(17) 0.06112(17) 0.0305(8) Uani 1 1 d . . .
H44A H 0.4206 0.9254 0.0385 0.046 Uiso 1 1 calc R . .
H44B H 0.4003 0.9658 0.1107 0.046 Uiso 1 1 calc R . .
H44C H 0.3819 1.0066 0.0374 0.046 Uiso 1 1 calc R . .
C45 C 0.3166(4) 0.77619(17) 0.03171(17) 0.0321(8) Uani 1 1 d . . .
H45A H 0.3147 0.7323 0.0053 0.048 Uiso 1 1 calc R . .
H45B H 0.3840 0.7721 0.0727 0.048 Uiso 1 1 calc R . .
H45C H 0.3466 0.8141 0.0014 0.048 Uiso 1 1 calc R . .
C46 C 0.1101(4) 0.72806(16) 0.09406(18) 0.0371(9) Uani 1 1 d . . .
H46A H 0.1070 0.6879 0.0623 0.056 Uiso 1 1 calc R . .
H46B H 0.0138 0.7381 0.1084 0.056 Uiso 1 1 calc R . .
H46C H 0.1723 0.7175 0.1357 0.056 Uiso 1 1 calc R . .
C51 C 0.0044(3) 1.06303(14) 0.26150(15) 0.0162(6) Uani 1 1 d . . .
C52 C 0.0134(3) 1.11776(15) 0.31060(15) 0.0200(7) Uani 1 1 d . . .
H52 H 0.0957 1.1213 0.3418 0.024 Uiso 1 1 calc R . .
C53 C -0.0938(3) 1.16647(15) 0.31482(16) 0.0221(7) Uani 1 1 d . . .
H53 H -0.0854 1.2023 0.3492 0.027 Uiso 1 1 calc R . .
C54 C -0.2137(3) 1.16330(15) 0.26908(16) 0.0235(7) Uani 1 1 d . . .
H54 H -0.2875 1.1968 0.2718 0.028 Uiso 1 1 calc R . .
C55 C -0.2246(3) 1.11057(16) 0.21922(16) 0.0232(7) Uani 1 1 d . . .
H55 H -0.3058 1.1083 0.1872 0.028 Uiso 1 1 calc R . .
C56 C -0.1178(3) 1.06115(15) 0.21592(15) 0.0199(7) Uani 1 1 d . . .
H56 H -0.1276 1.0251 0.1819 0.024 Uiso 1 1 calc R . .
C61 C 0.3008(3) 1.01432(14) 0.31671(15) 0.0154(6) Uani 1 1 d . . .
C62 C 0.4381(3) 1.02243(15) 0.29368(16) 0.0230(7) Uani 1 1 d . . .
H62 H 0.4538 1.0155 0.2454 0.028 Uiso 1 1 calc R . .
C63 C 0.5525(3) 1.04038(16) 0.33945(18) 0.0299(8) Uani 1 1 d . . .
H63 H 0.6450 1.0454 0.3224 0.036 Uiso 1 1 calc R . .
C64 C 0.5316(4) 1.05087(16) 0.40946(19) 0.0314(9) Uani 1 1 d . . .
H64 H 0.6093 1.0639 0.4408 0.038 Uiso 1 1 calc R . .
C65 C 0.3973(4) 1.04246(15) 0.43418(17) 0.0255(8) Uani 1 1 d . . .
H65 H 0.3829 1.0493 0.4826 0.031 Uiso 1 1 calc R . .
C66 C 0.2840(3) 1.02418(14) 0.38859(15) 0.0189(7) Uani 1 1 d . . .
H66 H 0.1925 1.0181 0.4064 0.023 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
Pd C 2.173(3) . ?
Pd P1 2.2402(9) . ?
Pd P2 2.2834(9) . ?
Pd H1 1.53(3) . ?
P1 C11 1.818(3) . ?
P1 C31 1.844(3) . ?
P1 C32 1.856(3) . ?
P2 C21 1.828(3) . ?
P2 C42 1.846(3) . ?
P2 C41 1.856(3) . ?
C C22 1.511(4) . ?
C C12 1.529(4) . ?
C Si 1.884(3) . ?
C11 C16 1.404(4) . ?
C11 C12 1.412(4) . ?
C12 C13 1.403(4) . ?
C13 C14 1.385(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.377(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.392(4) . ?
C21 C22 1.423(4) . ?
C22 C23 1.407(4) . ?
C23 C24 1.386(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.378(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C33 1.515(4) . ?
C31 C34 1.530(4) . ?
C31 H31 1.0000 . ?
C32 C35 1.524(4) . ?
C32 C36 1.526(4) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
Si C61 1.879(3) . ?
Si C51 1.893(3) . ?
Si H2 1.38(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 C43 1.533(4) . ?
C41 C44 1.535(4) . ?
C41 H41 1.0000 . ?
C42 C45 1.527(5) . ?
C42 C46 1.535(4) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C56 1.400(4) . ?
C51 C52 1.406(4) . ?
C52 C53 1.380(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.386(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.388(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.386(4) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C62 1.396(4) . ?
C61 C66 1.400(4) . ?
C62 C63 1.388(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.374(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.382(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.380(4) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?

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
C Pd P1 85.37(7) . . ?
C Pd P2 85.53(7) . . ?
P1 Pd P2 157.43(3) . . ?
C Pd H1 175.5(11) . . ?
P1 Pd H1 91.8(10) . . ?
P2 Pd H1 95.9(10) . . ?
C11 P1 C31 107.81(13) . . ?
C11 P1 C32 104.91(14) . . ?
C31 P1 C32 104.88(13) . . ?
C11 P1 Pd 103.76(9) . . ?
C31 P1 Pd 124.66(11) . . ?
C32 P1 Pd 109.33(10) . . ?
C21 P2 C42 104.19(14) . . ?
C21 P2 C41 106.54(13) . . ?
C42 P2 C41 105.34(14) . . ?
C21 P2 Pd 98.00(9) . . ?
C42 P2 Pd 113.02(10) . . ?
C41 P2 Pd 127.11(10) . . ?
C22 C C12 117.6(2) . . ?
C22 C Si 112.83(18) . . ?
C12 C Si 105.58(18) . . ?
C22 C Pd 106.61(18) . . ?
C12 C Pd 113.77(18) . . ?
Si C Pd 98.94(12) . . ?
C16 C11 C12 120.0(3) . . ?
C16 C11 P1 124.3(2) . . ?
C12 C11 P1 115.8(2) . . ?
C13 C12 C11 117.5(3) . . ?
C13 C12 C 122.2(3) . . ?
C11 C12 C 120.0(2) . . ?
C14 C13 C12 121.8(3) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 119.7(3) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C11 121.0(3) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C26 C21 C22 120.1(3) . . ?
C26 C21 P2 122.8(2) . . ?
C22 C21 P2 116.6(2) . . ?
C23 C22 C21 116.3(3) . . ?
C23 C22 C 124.1(3) . . ?
C21 C22 C 119.6(2) . . ?
C24 C23 C22 122.3(3) . . ?
C24 C23 H23 118.9 . . ?
C22 C23 H23 118.9 . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C26 C25 C24 118.7(3) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
C25 C26 C21 122.0(3) . . ?
C25 C26 H26 119.0 . . ?
C21 C26 H26 119.0 . . ?
C33 C31 C34 109.8(3) . . ?
C33 C31 P1 109.7(2) . . ?
C34 C31 P1 109.9(2) . . ?
C33 C31 H31 109.1 . . ?
C34 C31 H31 109.1 . . ?
P1 C31 H31 109.1 . . ?
C35 C32 C36 110.6(3) . . ?
C35 C32 P1 115.0(2) . . ?
C36 C32 P1 109.7(2) . . ?
C35 C32 H32 107.0 . . ?
C36 C32 H32 107.0 . . ?
P1 C32 H32 107.0 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C61 Si C 112.39(12) . . ?
C61 Si C51 108.82(13) . . ?
C Si C51 113.80(13) . . ?
C61 Si H2 106.1(12) . . ?
C Si H2 110.5(11) . . ?
C51 Si H2 104.7(11) . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C43 C41 C44 111.2(3) . . ?
C43 C41 P2 115.9(2) . . ?
C44 C41 P2 111.4(2) . . ?
C43 C41 H41 105.9 . . ?
C44 C41 H41 105.9 . . ?
P2 C41 H41 105.9 . . ?
C45 C42 C46 110.1(3) . . ?
C45 C42 P2 111.4(2) . . ?
C46 C42 P2 110.5(2) . . ?
C45 C42 H42 108.2 . . ?
C46 C42 H42 108.2 . . ?
P2 C42 H42 108.2 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C56 C51 C52 116.6(3) . . ?
C56 C51 Si 119.1(2) . . ?
C52 C51 Si 124.3(2) . . ?
C53 C52 C51 121.9(3) . . ?
C53 C52 H52 119.1 . . ?
C51 C52 H52 119.1 . . ?
C52 C53 C54 120.3(3) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C53 C54 C55 119.2(3) . . ?
C53 C54 H54 120.4 . . ?
C55 C54 H54 120.4 . . ?
C56 C55 C54 120.3(3) . . ?
C56 C55 H55 119.9 . . ?
C54 C55 H55 119.9 . . ?
C55 C56 C51 121.7(3) . . ?
C55 C56 H56 119.1 . . ?
C51 C56 H56 119.1 . . ?
C62 C61 C66 116.8(3) . . ?
C62 C61 Si 120.5(2) . . ?
C66 C61 Si 122.7(2) . . ?
C63 C62 C61 121.8(3) . . ?
C63 C62 H62 119.1 . . ?
C61 C62 H62 119.1 . . ?
C64 C63 C62 119.8(3) . . ?
C64 C63 H63 120.1 . . ?
C62 C63 H63 120.1 . . ?
C63 C64 C65 119.9(3) . . ?
C63 C64 H64 120.1 . . ?
C65 C64 H64 120.1 . . ?
C66 C65 C64 120.1(3) . . ?
C66 C65 H65 119.9 . . ?
C64 C65 H65 119.9 . . ?
C65 C66 C61 121.6(3) . . ?
C65 C66 H66 119.2 . . ?
C61 C66 H66 119.2 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.075
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc231
_database_code_depnum_ccdc_archive 'CCDC 1436836'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 P2 Pd Si'
_chemical_formula_weight         765.28

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5894(6)
_cell_length_b                   10.6642(7)
_cell_length_c                   19.5486(13)
_cell_angle_alpha                78.851(3)
_cell_angle_beta                 76.192(3)
_cell_angle_gamma                76.697(2)
_cell_volume                     1868.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6829
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56344
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         28.45
_reflns_number_total             9370
_reflns_number_gt                7945
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0337P)²+1.6702P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9370
_refine_ls_number_parameters     435
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0772
_refine_ls_wR_factor_gt          0.0732
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.261153(17) 0.076114(15) 0.322116(9) 0.01217(5) Uani 1 1 d . . .
P1 P 0.31475(6) 0.27875(5) 0.28653(3) 0.01175(11) Uani 1 1 d . . .
C21 C 0.5405(2) -0.1405(2) 0.30667(11) 0.0126(4) Uani 1 1 d . . .
C22 C 0.4397(2) -0.2145(2) 0.35149(11) 0.0138(4) Uani 1 1 d . . .
C23 C 0.4836(3) -0.3474(2) 0.37531(12) 0.0197(5) Uani 1 1 d . . .
H23 H 0.4130 -0.3961 0.4033 0.024 Uiso 1 1 calc R . .
C24 C 0.6285(3) -0.4082(2) 0.35847(13) 0.0222(5) Uani 1 1 d . . .
H24 H 0.6585 -0.4974 0.3762 0.027 Uiso 1 1 calc R . .
C25 C 0.7295(3) -0.3374(2) 0.31549(13) 0.0208(5) Uani 1 1 d . . .
H25 H 0.8296 -0.3780 0.3043 0.025 Uiso 1 1 calc R . .
C26 C 0.6856(2) -0.2079(2) 0.28869(12) 0.0165(4) Uani 1 1 d . . .
H26 H 0.7560 -0.1629 0.2570 0.020 Uiso 1 1 calc R . .
C31 C 0.2590(2) 0.3873(2) 0.35633(11) 0.0166(4) Uani 1 1 d . . .
H31 H 0.2974 0.4693 0.3363 0.020 Uiso 1 1 calc R . .
C32 C 0.2741(2) 0.3816(2) 0.20287(12) 0.0161(4) Uani 1 1 d . . .
H32 H 0.3144 0.3244 0.1650 0.019 Uiso 1 1 calc R . .
C33 C 0.3237(3) 0.3232(3) 0.42174(13) 0.0267(5) Uani 1 1 d . . .
H33A H 0.2816 0.2461 0.4442 0.040 Uiso 1 1 calc R . .
H33B H 0.3010 0.3851 0.4558 0.040 Uiso 1 1 calc R . .
H33C H 0.4301 0.2971 0.4072 0.040 Uiso 1 1 calc R . .
H H 0.065(3) 0.132(3) 0.3851(16) 0.040 Uiso 1 1 d . . .
C34 C 0.0922(3) 0.4234(3) 0.37895(14) 0.0277(5) Uani 1 1 d . . .
H34A H 0.0515 0.4764 0.3388 0.042 Uiso 1 1 calc R . .
H34B H 0.0669 0.4731 0.4189 0.042 Uiso 1 1 calc R . .
H34C H 0.0515 0.3437 0.3936 0.042 Uiso 1 1 calc R . .
C35 C 0.1100(3) 0.4228(3) 0.20342(15) 0.0301(6) Uani 1 1 d . . .
H35A H 0.0948 0.4435 0.1543 0.045 Uiso 1 1 calc R . .
H35B H 0.0699 0.4999 0.2274 0.045 Uiso 1 1 calc R . .
H35C H 0.0604 0.3515 0.2289 0.045 Uiso 1 1 calc R . .
C36 C 0.3494(3) 0.4988(2) 0.17817(13) 0.0262(5) Uani 1 1 d . . .
H36A H 0.3157 0.5507 0.1359 0.039 Uiso 1 1 calc R . .
H36B H 0.4556 0.4685 0.1663 0.039 Uiso 1 1 calc R . .
H36C H 0.3253 0.5525 0.2163 0.039 Uiso 1 1 calc R . .
C41 C 0.1272(2) -0.2233(2) 0.37531(12) 0.0168(4) Uani 1 1 d . . .
H41 H 0.1609 -0.3154 0.3964 0.020 Uiso 1 1 calc R . .
C42 C 0.2432(3) -0.1316(2) 0.47842(11) 0.0170(4) Uani 1 1 d . . .
H42 H 0.1460 -0.0782 0.4971 0.020 Uiso 1 1 calc R . .
C43 C 0.1262(3) -0.2204(2) 0.29691(13) 0.0256(5) Uani 1 1 d . . .
H43A H 0.0895 -0.1312 0.2760 0.038 Uiso 1 1 calc R . .
H43B H 0.0626 -0.2777 0.2932 0.038 Uiso 1 1 calc R . .
H43C H 0.2259 -0.2505 0.2713 0.038 Uiso 1 1 calc R . .
C44 C -0.0266(3) -0.1733(2) 0.41666(13) 0.0236(5) Uani 1 1 d . . .
H44A H -0.0581 -0.0811 0.3988 0.035 Uiso 1 1 calc R . .
H44B H -0.0250 -0.1831 0.4674 0.035 Uiso 1 1 calc R . .
H44C H -0.0949 -0.2236 0.4102 0.035 Uiso 1 1 calc R . .
C45 C 0.2502(3) -0.2675(2) 0.52236(12) 0.0240(5) Uani 1 1 d . . .
H45A H 0.1802 -0.3109 0.5114 0.036 Uiso 1 1 calc R . .
H45B H 0.2255 -0.2598 0.5732 0.036 Uiso 1 1 calc R . .
H45C H 0.3492 -0.3189 0.5107 0.036 Uiso 1 1 calc R . .
C46 C 0.3602(3) -0.0665(2) 0.49020(13) 0.0240(5) Uani 1 1 d . . .
H46A H 0.4573 -0.1195 0.4756 0.036 Uiso 1 1 calc R . .
H46B H 0.3438 -0.0585 0.5407 0.036 Uiso 1 1 calc R . .
H46C H 0.3546 0.0203 0.4618 0.036 Uiso 1 1 calc R . .
C51 C 0.3137(2) -0.0127(2) 0.15517(11) 0.0156(4) Uani 1 1 d . . .
C52 C 0.1877(2) 0.0811(2) 0.17219(12) 0.0175(4) Uani 1 1 d . . .
H52 H 0.1911 0.1469 0.1979 0.021 Uiso 1 1 calc R . .
C53 C 0.0574(2) 0.0812(2) 0.15265(12) 0.0203(5) Uani 1 1 d . . .
H53 H -0.0258 0.1475 0.1640 0.024 Uiso 1 1 calc R . .
C54 C 0.0496(3) -0.0159(3) 0.11656(14) 0.0261(5) Uani 1 1 d . . .
H54 H -0.0396 -0.0176 0.1039 0.031 Uiso 1 1 calc R . .
C55 C 0.1723(3) -0.1102(3) 0.09901(15) 0.0296(6) Uani 1 1 d . . .
H55 H 0.1675 -0.1770 0.0743 0.036 Uiso 1 1 calc R . .
C56 C 0.3026(3) -0.1073(2) 0.11742(13) 0.0227(5) Uani 1 1 d . . .
H56 H 0.3866 -0.1715 0.1039 0.027 Uiso 1 1 calc R . .
C61 C 0.5537(2) 0.1468(2) 0.11557(11) 0.0141(4) Uani 1 1 d . . .
C62 C 0.6791(2) 0.1878(2) 0.12060(11) 0.0150(4) Uani 1 1 d . . .
H62 H 0.7307 0.1440 0.1570 0.018 Uiso 1 1 calc R . .
C63 C 0.7299(3) 0.2908(2) 0.07377(12) 0.0193(5) Uani 1 1 d . . .
H63 H 0.8157 0.3162 0.0782 0.023 Uiso 1 1 calc R . .
C64 C 0.6559(3) 0.3564(2) 0.02083(12) 0.0226(5) Uani 1 1 d . . .
H64 H 0.6890 0.4285 -0.0104 0.027 Uiso 1 1 calc R . .
C65 C 0.5332(3) 0.3167(2) 0.01336(12) 0.0219(5) Uani 1 1 d . . .
H65 H 0.4832 0.3607 -0.0236 0.026 Uiso 1 1 calc R . .
C66 C 0.4832(2) 0.2124(2) 0.05997(12) 0.0178(4) Uani 1 1 d . . .
H66 H 0.3997 0.1853 0.0540 0.021 Uiso 1 1 calc R . .
C71 C 0.6274(2) -0.1450(2) 0.13600(11) 0.0149(4) Uani 1 1 d . . .
C72 C 0.6159(2) -0.2754(2) 0.16224(12) 0.0188(4) Uani 1 1 d . . .
H72 H 0.5408 -0.2937 0.2021 0.023 Uiso 1 1 calc R . .
C73 C 0.7111(3) -0.3782(2) 0.13158(13) 0.0227(5) Uani 1 1 d . . .
H73 H 0.7013 -0.4654 0.1508 0.027 Uiso 1 1 calc R . .
C74 C 0.8205(3) -0.3538(2) 0.07291(14) 0.0268(5) Uani 1 1 d . . .
H74 H 0.8865 -0.4241 0.0522 0.032 Uiso 1 1 calc R . .
C76 C 0.8332(3) -0.2267(2) 0.04468(14) 0.0266(5) Uani 1 1 d . . .
H76 H 0.9072 -0.2094 0.0040 0.032 Uiso 1 1 calc R . .
C77 C 0.7376(2) -0.1239(2) 0.07577(12) 0.0194(5) Uani 1 1 d . . .
H77 H 0.7473 -0.0371 0.0556 0.023 Uiso 1 1 calc R . .
P2 P 0.25695(6) -0.12495(5) 0.38185(3) 0.01260(11) Uani 1 1 d . . .
Si Si 0.49393(6) -0.00202(5) 0.17528(3) 0.01224(12) Uani 1 1 d . . .
C C 0.4899(2) 0.00090(19) 0.27439(11) 0.0120(4) Uani 1 1 d . . .
C11 C 0.5743(2) 0.0987(2) 0.28454(10) 0.0114(4) Uani 1 1 d . . .
C12 C 0.5124(2) 0.2344(2) 0.27727(11) 0.0124(4) Uani 1 1 d . . .
C13 C 0.5959(2) 0.3270(2) 0.27533(11) 0.0157(4) Uani 1 1 d . . .
H13 H 0.5534 0.4170 0.2677 0.019 Uiso 1 1 calc R . .
C14 C 0.7391(2) 0.2901(2) 0.28428(12) 0.0174(4) Uani 1 1 d . . .
H14 H 0.7973 0.3534 0.2800 0.021 Uiso 1 1 calc R . .
C15 C 0.7958(2) 0.1584(2) 0.29963(11) 0.0176(4) Uani 1 1 d . . .
H15 H 0.8912 0.1314 0.3098 0.021 Uiso 1 1 calc R . .
C16 C 0.7150(2) 0.0658(2) 0.30034(11) 0.0146(4) Uani 1 1 d . . .
H16 H 0.7563 -0.0236 0.3120 0.018 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
Pd C 2.198(2) . ?
Pd P2 2.2386(5) . ?
Pd P1 2.2753(5) . ?
Pd H 2.02(3) . ?
P1 C12 1.819(2) . ?
P1 C32 1.856(2) . ?
P1 C31 1.862(2) . ?
C21 C26 1.407(3) . ?
C21 C22 1.416(3) . ?
C21 C 1.533(3) . ?
C22 C23 1.402(3) . ?
C22 P2 1.813(2) . ?
C23 C24 1.382(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C33 1.528(3) . ?
C31 C34 1.532(3) . ?
C31 H31 1.0000 . ?
C32 C36 1.528(3) . ?
C32 C35 1.531(3) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 C43 1.529(3) . ?
C41 C44 1.532(3) . ?
C41 P2 1.842(2) . ?
C41 H41 1.0000 . ?
C42 C46 1.529(3) . ?
C42 C45 1.531(3) . ?
C42 P2 1.849(2) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C56 1.395(3) . ?
C51 C52 1.397(3) . ?
C51 Si 1.894(2) . ?
C52 C53 1.390(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.385(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.382(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.388(3) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C62 1.401(3) . ?
C61 C66 1.403(3) . ?
C61 Si 1.895(2) . ?
C62 C63 1.388(3) . ?
C62 H62 0.9500 . ?
C63 C64 1.380(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.385(3) . ?
C64 H64 0.9500 . ?
C65 C66 1.394(3) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C77 1.402(3) . ?
C71 C72 1.407(3) . ?
C71 Si 1.907(2) . ?
C72 C73 1.388(3) . ?
C72 H72 0.9500 . ?
C73 C74 1.385(4) . ?
C73 H73 0.9500 . ?
C74 C76 1.383(4) . ?
C74 H74 0.9500 . ?
C76 C77 1.393(3) . ?
C76 H76 0.9500 . ?
C77 H77 0.9500 . ?
Si C 1.935(2) . ?
C C11 1.526(3) . ?
C11 C16 1.406(3) . ?
C11 C12 1.425(3) . ?
C12 C13 1.397(3) . ?
C13 C14 1.383(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

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
C Pd P2 86.58(5) . . ?
C Pd P1 86.80(5) . . ?
P2 Pd P1 160.92(2) . . ?
C Pd H 168.1(8) . . ?
P2 Pd H 87.0(8) . . ?
P1 Pd H 96.2(8) . . ?
C12 P1 C32 108.19(10) . . ?
C12 P1 C31 103.15(10) . . ?
C32 P1 C31 106.59(10) . . ?
C12 P1 Pd 98.55(7) . . ?
C32 P1 Pd 122.63(7) . . ?
C31 P1 Pd 115.44(7) . . ?
C26 C21 C22 116.06(19) . . ?
C26 C21 C 122.45(18) . . ?
C22 C21 C 121.24(18) . . ?
C23 C22 C21 121.2(2) . . ?
C23 C22 P2 122.42(17) . . ?
C21 C22 P2 116.21(15) . . ?
C24 C23 C22 120.7(2) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 119.2(2) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C24 C25 C26 120.5(2) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 122.3(2) . . ?
C25 C26 H26 118.8 . . ?
C21 C26 H26 118.8 . . ?
C33 C31 C34 109.20(19) . . ?
C33 C31 P1 110.90(16) . . ?
C34 C31 P1 111.67(16) . . ?
C33 C31 H31 108.3 . . ?
C34 C31 H31 108.3 . . ?
P1 C31 H31 108.3 . . ?
C36 C32 C35 110.7(2) . . ?
C36 C32 P1 115.37(16) . . ?
C35 C32 P1 113.18(16) . . ?
C36 C32 H32 105.5 . . ?
C35 C32 H32 105.5 . . ?
P1 C32 H32 105.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C43 C41 C44 110.9(2) . . ?
C43 C41 P2 109.36(15) . . ?
C44 C41 P2 110.79(15) . . ?
C43 C41 H41 108.6 . . ?
C44 C41 H41 108.6 . . ?
P2 C41 H41 108.6 . . ?
C46 C42 C45 110.32(19) . . ?
C46 C42 P2 109.55(15) . . ?
C45 C42 P2 115.53(15) . . ?
C46 C42 H42 107.0 . . ?
C45 C42 H42 107.0 . . ?
P2 C42 H42 107.0 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C56 C51 C52 116.6(2) . . ?
C56 C51 Si 122.00(17) . . ?
C52 C51 Si 121.18(16) . . ?
C53 C52 C51 122.1(2) . . ?
C53 C52 H52 118.9 . . ?
C51 C52 H52 118.9 . . ?
C54 C53 C52 119.7(2) . . ?
C54 C53 H53 120.2 . . ?
C52 C53 H53 120.2 . . ?
C55 C54 C53 119.6(2) . . ?
C55 C54 H54 120.2 . . ?
C53 C54 H54 120.2 . . ?
C54 C55 C56 120.1(2) . . ?
C54 C55 H55 120.0 . . ?
C56 C55 H55 120.0 . . ?
C55 C56 C51 121.9(2) . . ?
C55 C56 H56 119.0 . . ?
C51 C56 H56 119.0 . . ?
C62 C61 C66 117.07(19) . . ?
C62 C61 Si 121.21(16) . . ?
C66 C61 Si 121.42(16) . . ?
C63 C62 C61 121.7(2) . . ?
C63 C62 H62 119.2 . . ?
C61 C62 H62 119.2 . . ?
C64 C63 C62 120.1(2) . . ?
C64 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
C63 C64 C65 119.8(2) . . ?
C63 C64 H64 120.1 . . ?
C65 C64 H64 120.1 . . ?
C64 C65 C66 120.1(2) . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C65 C66 C61 121.2(2) . . ?
C65 C66 H66 119.4 . . ?
C61 C66 H66 119.4 . . ?
C77 C71 C72 116.4(2) . . ?
C77 C71 Si 120.82(16) . . ?
C72 C71 Si 122.65(17) . . ?
C73 C72 C71 121.9(2) . . ?
C73 C72 H72 119.0 . . ?
C71 C72 H72 119.0 . . ?
C74 C73 C72 120.1(2) . . ?
C74 C73 H73 120.0 . . ?
C72 C73 H73 120.0 . . ?
C76 C74 C73 119.7(2) . . ?
C76 C74 H74 120.2 . . ?
C73 C74 H74 120.2 . . ?
C74 C76 C77 120.0(2) . . ?
C74 C76 H76 120.0 . . ?
C77 C76 H76 120.0 . . ?
C76 C77 C71 121.9(2) . . ?
C76 C77 H77 119.1 . . ?
C71 C77 H77 119.1 . . ?
C22 P2 C41 107.16(10) . . ?
C22 P2 C42 104.08(10) . . ?
C41 P2 C42 105.11(10) . . ?
C22 P2 Pd 103.58(7) . . ?
C41 P2 Pd 122.97(7) . . ?
C42 P2 Pd 112.35(7) . . ?
C51 Si C61 106.62(9) . . ?
C51 Si C71 103.35(9) . . ?
C61 Si C71 104.03(9) . . ?
C51 Si C 115.04(9) . . ?
C61 Si C 112.12(9) . . ?
C71 Si C 114.64(9) . . ?
C11 C C21 115.47(17) . . ?
C11 C Si 112.86(13) . . ?
C21 C Si 106.28(13) . . ?
C11 C Pd 104.43(13) . . ?
C21 C Pd 111.43(13) . . ?
Si C Pd 106.06(9) . . ?
C16 C11 C12 115.08(18) . . ?
C16 C11 C 124.56(18) . . ?
C12 C11 C 120.36(18) . . ?
C13 C12 C11 121.19(19) . . ?
C13 C12 P1 121.23(16) . . ?
C11 C12 P1 116.71(15) . . ?
C14 C13 C12 121.2(2) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 118.3(2) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C16 C15 C14 120.8(2) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C11 122.6(2) . . ?
C15 C16 H16 118.7 . . ?
C11 C16 H16 118.7 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.083
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc243
_database_code_depnum_ccdc_archive 'CCDC 1436837'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H64 P2 Pd Si'
_chemical_formula_weight         837.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.401(2)
_cell_length_b                   12.592(2)
_cell_length_c                   30.423(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.666(3)
_cell_angle_gamma                90.00
_cell_volume                     4328.5(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1768
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6854
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            126183
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         28.37
_reflns_number_total             10820
_reflns_number_gt                8147
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0388P)²+5.1335P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10820
_refine_ls_number_parameters     527
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.0983
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 1.0992(2) 0.6051(2) 0.39512(9) 0.0195(6) Uani 1 1 d . . .
H H 1.1415 0.5466 0.4130 0.023 Uiso 1 1 calc R . .
Pd Pd 0.930309(18) 0.538248(16) 0.367939(7) 0.01569(6) Uani 1 1 d . . .
Si Si 0.75463(7) 0.42896(6) 0.35192(2) 0.01697(15) Uani 1 1 d . . .
C21 C 1.0950(3) 0.6955(2) 0.42711(10) 0.0231(6) Uani 1 1 d . . .
C22 C 0.9875(2) 0.7440(2) 0.43210(9) 0.0184(5) Uani 1 1 d . . .
C23 C 0.9867(3) 0.8354(2) 0.45866(10) 0.0273(7) Uani 1 1 d . . .
H23 H 0.9142 0.8709 0.4608 0.033 Uiso 1 1 calc R . .
C24 C 1.0902(3) 0.8736(3) 0.48146(10) 0.0322(7) Uani 1 1 d . . .
H24 H 1.0896 0.9367 0.4985 0.039 Uiso 1 1 calc R . .
C25 C 1.1954(3) 0.8201(3) 0.47963(10) 0.0311(7) Uani 1 1 d . . .
H25 H 1.2659 0.8437 0.4971 0.037 Uiso 1 1 calc R . .
C26 C 1.1982(3) 0.7332(3) 0.45269(10) 0.0290(7) Uani 1 1 d . . .
H26 H 1.2712 0.6979 0.4513 0.035 Uiso 1 1 calc R . .
C31 C 1.0080(2) 0.4418(2) 0.26257(9) 0.0200(6) Uani 1 1 d . . .
H31 H 1.0807 0.4237 0.2490 0.024 Uiso 1 1 calc R . .
C32 C 1.1178(2) 0.3217(2) 0.34024(9) 0.0212(6) Uani 1 1 d . . .
H32 H 1.0522 0.2685 0.3376 0.025 Uiso 1 1 calc R . .
C33 C 0.9184(3) 0.3548(2) 0.24965(10) 0.0251(6) Uani 1 1 d . . .
H33A H 0.8438 0.3725 0.2606 0.038 Uiso 1 1 calc R . .
H33B H 0.9486 0.2874 0.2627 0.038 Uiso 1 1 calc R . .
H33C H 0.9048 0.3482 0.2173 0.038 Uiso 1 1 calc R . .
C81 C 0.2131(10) 0.0087(9) 0.3894(4) 0.055(3) Uani 0.523(10) 1 d PU A 2
H81A H 0.1949 0.0818 0.3797 0.083 Uiso 0.523(10) 1 calc PR A 2
H81B H 0.1851 -0.0033 0.4181 0.083 Uiso 0.523(10) 1 calc PR A 2
H81C H 0.1737 -0.0410 0.3675 0.083 Uiso 0.523(10) 1 calc PR A 2
C83 C 0.3965(11) 0.0651(10) 0.4316(4) 0.085(4) Uani 0.523(10) 1 d PU A 2
H83A H 0.3527 0.0530 0.4572 0.102 Uiso 0.523(10) 1 calc PR A 2
H83B H 0.3831 0.1395 0.4217 0.102 Uiso 0.523(10) 1 calc PR A 2
C85 C 0.6173(10) 0.0540(10) 0.4139(4) 0.077(3) Uani 0.523(10) 1 d PU A 2
H85A H 0.6974 0.0503 0.4301 0.116 Uiso 0.523(10) 1 calc PR A 2
H85B H 0.6073 0.1214 0.3977 0.116 Uiso 0.523(10) 1 calc PR A 2
H85C H 0.6053 -0.0051 0.3928 0.116 Uiso 0.523(10) 1 calc PR A 2
C84 C 0.5284(9) 0.0470(9) 0.4459(4) 0.078(3) Uani 0.523(10) 1 d PU A 2
H84A H 0.5535 0.0985 0.4700 0.093 Uiso 0.523(10) 1 calc PR A 2
H84B H 0.5366 -0.0245 0.4595 0.093 Uiso 0.523(10) 1 calc PR A 2
C82 C 0.3512(7) -0.0094(7) 0.3944(3) 0.048(2) Uani 0.523(10) 1 d PU A 2
H82A H 0.3718 -0.0840 0.4022 0.058 Uiso 0.523(10) 1 calc PR A 2
H82B H 0.3833 0.0093 0.3667 0.058 Uiso 0.523(10) 1 calc PR A 2
C91 C 0.2253(9) 0.0030(8) 0.3774(3) 0.038(2) Uani 0.477(10) 1 d PU A 1
H91A H 0.1702 -0.0437 0.3903 0.057 Uiso 0.477(10) 1 calc PR A 1
H91B H 0.2498 -0.0308 0.3511 0.057 Uiso 0.477(10) 1 calc PR A 1
H91C H 0.1861 0.0707 0.3690 0.057 Uiso 0.477(10) 1 calc PR A 1
C92 C 0.3348(15) 0.0233(14) 0.4117(6) 0.105(5) Uani 0.477(10) 1 d PU A 1
H92A H 0.3055 0.0497 0.4389 0.126 Uiso 0.477(10) 1 calc PR A 1
H92B H 0.3717 -0.0467 0.4192 0.126 Uiso 0.477(10) 1 calc PR A 1
C93 C 0.4256(10) 0.0919(10) 0.4032(4) 0.077(4) Uani 0.477(10) 1 d PU A 1
H93A H 0.3987 0.1613 0.4134 0.092 Uiso 0.477(10) 1 calc PR A 1
H93B H 0.4139 0.0964 0.3704 0.092 Uiso 0.477(10) 1 calc PR A 1
C94 C 0.5526(14) 0.0989(13) 0.4138(5) 0.104(5) Uani 0.477(10) 1 d PU A 1
H94A H 0.5718 0.1570 0.4356 0.125 Uiso 0.477(10) 1 calc PR A 1
H94B H 0.5866 0.1179 0.3866 0.125 Uiso 0.477(10) 1 calc PR A 1
C95 C 0.6095(10) -0.0002(9) 0.4324(4) 0.064(3) Uani 0.477(10) 1 d PU A 1
H95A H 0.6019 -0.0554 0.4095 0.076 Uiso 0.477(10) 1 calc PR A 1
H95B H 0.5708 -0.0239 0.4576 0.076 Uiso 0.477(10) 1 calc PR A 1
H95C H 0.6935 0.0132 0.4424 0.076 Uiso 0.477(10) 1 calc PR A 1
C34 C 0.9649(3) 0.5501(2) 0.24422(10) 0.0263(6) Uani 1 1 d . . .
H34A H 1.0294 0.6018 0.2497 0.039 Uiso 1 1 calc R . .
H34B H 0.8980 0.5735 0.2590 0.039 Uiso 1 1 calc R . .
H34C H 0.9396 0.5442 0.2122 0.039 Uiso 1 1 calc R . .
C35 C 1.1716(3) 0.3263(2) 0.38907(10) 0.0276(7) Uani 1 1 d . . .
H35A H 1.1948 0.2547 0.3994 0.041 Uiso 1 1 calc R . .
H35B H 1.1130 0.3547 0.4068 0.041 Uiso 1 1 calc R . .
H35C H 1.2414 0.3725 0.3923 0.041 Uiso 1 1 calc R . .
C36 C 1.2105(3) 0.2825(2) 0.31182(11) 0.0307(7) Uani 1 1 d . . .
H36A H 1.2378 0.2116 0.3218 0.046 Uiso 1 1 calc R . .
H36B H 1.2778 0.3317 0.3148 0.046 Uiso 1 1 calc R . .
H36C H 1.1751 0.2792 0.2807 0.046 Uiso 1 1 calc R . .
C41 C 0.7763(2) 0.6379(2) 0.45357(9) 0.0193(6) Uani 1 1 d . . .
H41 H 0.7040 0.5978 0.4408 0.023 Uiso 1 1 calc R . .
C42 C 0.7718(3) 0.7746(2) 0.37395(10) 0.0227(6) Uani 1 1 d . . .
H42 H 0.7734 0.8404 0.3924 0.027 Uiso 1 1 calc R . .
C43 C 0.8521(3) 0.5611(2) 0.48422(10) 0.0276(7) Uani 1 1 d . . .
H43A H 0.8069 0.5362 0.5074 0.041 Uiso 1 1 calc R . .
H43B H 0.9237 0.5976 0.4979 0.041 Uiso 1 1 calc R . .
H43C H 0.8743 0.5003 0.4670 0.041 Uiso 1 1 calc R . .
C44 C 0.7339(3) 0.7310(3) 0.47981(10) 0.0296(7) Uani 1 1 d . . .
H44A H 0.8019 0.7638 0.4979 0.044 Uiso 1 1 calc R . .
H44B H 0.6780 0.7049 0.4992 0.044 Uiso 1 1 calc R . .
H44C H 0.6946 0.7837 0.4592 0.044 Uiso 1 1 calc R . .
C45 C 0.6423(3) 0.7437(2) 0.36029(10) 0.0283(7) Uani 1 1 d . . .
H45A H 0.6048 0.7296 0.3869 0.042 Uiso 1 1 calc R . .
H45B H 0.6384 0.6798 0.3418 0.042 Uiso 1 1 calc R . .
H45C H 0.6008 0.8020 0.3435 0.042 Uiso 1 1 calc R . .
C46 C 0.8332(3) 0.7994(3) 0.33322(10) 0.0306(7) Uani 1 1 d . . .
H46A H 0.9160 0.8183 0.3428 0.046 Uiso 1 1 calc R . .
H46B H 0.7929 0.8590 0.3169 0.046 Uiso 1 1 calc R . .
H46C H 0.8298 0.7368 0.3140 0.046 Uiso 1 1 calc R . .
C51 C 0.8078(2) 0.2854(2) 0.35759(9) 0.0190(6) Uani 1 1 d . . .
C52 C 0.8829(2) 0.2563(2) 0.39621(10) 0.0226(6) Uani 1 1 d . . .
H52 H 0.9034 0.3081 0.4186 0.027 Uiso 1 1 calc R . .
C53 C 0.9278(3) 0.1545(2) 0.40246(10) 0.0282(7) Uani 1 1 d . . .
H53 H 0.9780 0.1374 0.4290 0.034 Uiso 1 1 calc R . .
C54 C 0.9000(3) 0.0775(2) 0.37038(11) 0.0301(7) Uani 1 1 d . . .
H54 H 0.9305 0.0076 0.3747 0.036 Uiso 1 1 calc R . .
C55 C 0.8274(3) 0.1038(2) 0.33195(11) 0.0296(7) Uani 1 1 d . . .
H55 H 0.8082 0.0518 0.3095 0.036 Uiso 1 1 calc R . .
C56 C 0.7821(3) 0.2062(2) 0.32586(9) 0.0231(6) Uani 1 1 d . . .
H56 H 0.7321 0.2225 0.2992 0.028 Uiso 1 1 calc R . .
C61 C 0.6518(2) 0.4422(2) 0.29727(9) 0.0205(6) Uani 1 1 d . . .
C62 C 0.5595(2) 0.3703(2) 0.28566(9) 0.0234(6) Uani 1 1 d . . .
H62 H 0.5513 0.3114 0.3045 0.028 Uiso 1 1 calc R . .
C63 C 0.4796(3) 0.3825(3) 0.24755(10) 0.0267(7) Uani 1 1 d . . .
H63 H 0.4187 0.3316 0.2402 0.032 Uiso 1 1 calc R . .
C64 C 0.4884(3) 0.4688(3) 0.22012(10) 0.0300(7) Uani 1 1 d . . .
H64 H 0.4334 0.4775 0.1940 0.036 Uiso 1 1 calc R . .
C65 C 0.5774(3) 0.5420(3) 0.23074(10) 0.0279(6) Uani 1 1 d . . .
H65 H 0.5837 0.6016 0.2121 0.034 Uiso 1 1 calc R . .
C66 C 0.6578(3) 0.5285(2) 0.26888(9) 0.0230(6) Uani 1 1 d . . .
H66 H 0.7188 0.5797 0.2758 0.028 Uiso 1 1 calc R . .
C71 C 0.6376(2) 0.4325(2) 0.39180(9) 0.0183(5) Uani 1 1 d . . .
C72 C 0.6472(3) 0.3766(2) 0.43181(9) 0.0232(6) Uani 1 1 d . . .
H72 H 0.7148 0.3332 0.4401 0.028 Uiso 1 1 calc R . .
C73 C 0.5607(3) 0.3829(3) 0.45988(10) 0.0303(7) Uani 1 1 d . . .
H73 H 0.5692 0.3433 0.4867 0.036 Uiso 1 1 calc R . .
C74 C 0.4626(3) 0.4464(3) 0.44901(10) 0.0291(7) Uani 1 1 d . . .
H74 H 0.4045 0.4520 0.4686 0.035 Uiso 1 1 calc R . .
C75 C 0.4495(3) 0.5017(2) 0.40955(10) 0.0241(6) Uani 1 1 d . . .
H75 H 0.3819 0.5453 0.4017 0.029 Uiso 1 1 calc R . .
C76 C 0.5349(2) 0.4937(2) 0.38133(9) 0.0207(6) Uani 1 1 d . . .
H76 H 0.5235 0.5309 0.3539 0.025 Uiso 1 1 calc R . .
P1 P 1.05226(6) 0.45229(6) 0.32326(2) 0.01644(14) Uani 1 1 d . . .
P2 P 0.85747(6) 0.67189(6) 0.40682(2) 0.01621(14) Uani 1 1 d . . .
C11 C 1.1729(2) 0.6267(2) 0.35802(9) 0.0199(6) Uani 1 1 d . . .
C12 C 1.1744(2) 0.5472(2) 0.32543(9) 0.0185(5) Uani 1 1 d . . .
C13 C 1.2555(2) 0.5515(2) 0.29512(9) 0.0218(6) Uani 1 1 d . . .
H13 H 1.2604 0.4943 0.2751 0.026 Uiso 1 1 calc R . .
C14 C 1.3296(3) 0.6392(3) 0.29408(10) 0.0265(7) Uani 1 1 d . . .
H14 H 1.3859 0.6418 0.2737 0.032 Uiso 1 1 calc R . .
C15 C 1.3200(3) 0.7223(2) 0.32294(10) 0.0260(7) Uani 1 1 d . . .
H15 H 1.3661 0.7846 0.3210 0.031 Uiso 1 1 calc R . .
C16 C 1.2441(2) 0.7159(2) 0.35478(10) 0.0242(6) Uani 1 1 d . . .
H16 H 1.2404 0.7733 0.3748 0.029 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
C C21 1.502(4) . ?
C C11 1.519(4) . ?
C Pd 2.162(3) . ?
C H 1.0000 . ?
Pd P2 2.2765(7) . ?
Pd P1 2.3360(7) . ?
Pd Si 2.4253(8) . ?
Si C51 1.907(3) . ?
Si C61 1.910(3) . ?
Si C71 1.920(3) . ?
C21 C22 1.396(4) . ?
C21 C26 1.404(4) . ?
C22 C23 1.407(4) . ?
C22 P2 1.820(3) . ?
C23 C24 1.373(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.370(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C33 1.514(4) . ?
C31 C34 1.529(4) . ?
C31 P1 1.853(3) . ?
C31 H31 1.0000 . ?
C32 C35 1.531(4) . ?
C32 C36 1.534(4) . ?
C32 P1 1.851(3) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C81 C82 1.577(14) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C83 C82 1.510(16) . ?
C83 C84 1.526(15) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C85 C84 1.500(17) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C91 C92 1.538(19) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 C93 1.399(19) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 C94 1.443(17) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C94 C95 1.48(2) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 C43 1.528(4) . ?
C41 C44 1.532(4) . ?
C41 P2 1.848(3) . ?
C41 H41 1.0000 . ?
C42 C45 1.529(4) . ?
C42 C46 1.534(4) . ?
C42 P2 1.834(3) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C56 1.392(4) . ?
C51 C52 1.407(4) . ?
C52 C53 1.384(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.382(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.380(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.392(4) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C66 1.396(4) . ?
C61 C62 1.397(4) . ?
C62 C63 1.384(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.381(4) . ?
C63 H63 0.9500 . ?
C64 C65 1.377(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.390(4) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C72 1.397(4) . ?
C71 C76 1.403(4) . ?
C72 C73 1.391(4) . ?
C72 H72 0.9500 . ?
C73 C74 1.378(4) . ?
C73 H73 0.9500 . ?
C74 C75 1.379(4) . ?
C74 H74 0.9500 . ?
C75 C76 1.385(4) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
P1 C12 1.829(3) . ?
C11 C16 1.397(4) . ?
C11 C12 1.411(4) . ?
C12 C13 1.392(4) . ?
C13 C14 1.394(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

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
C21 C C11 114.5(2) . . ?
C21 C Pd 116.05(19) . . ?
C11 C Pd 109.77(18) . . ?
C21 C H 105.1 . . ?
C11 C H 105.1 . . ?
Pd C H 105.1 . . ?
C Pd P2 83.19(8) . . ?
C Pd P1 80.46(7) . . ?
P2 Pd P1 158.68(3) . . ?
C Pd Si 165.27(8) . . ?
P2 Pd Si 100.08(3) . . ?
P1 Pd Si 99.20(3) . . ?
C51 Si C61 108.17(12) . . ?
C51 Si C71 101.76(12) . . ?
C61 Si C71 98.65(12) . . ?
C51 Si Pd 106.01(9) . . ?
C61 Si Pd 121.34(9) . . ?
C71 Si Pd 119.01(9) . . ?
C22 C21 C26 118.3(3) . . ?
C22 C21 C 120.4(2) . . ?
C26 C21 C 121.3(3) . . ?
C21 C22 C23 119.6(3) . . ?
C21 C22 P2 114.4(2) . . ?
C23 C22 P2 125.7(2) . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 120.0(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 120.1(3) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 121.2(3) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
C33 C31 C34 112.2(2) . . ?
C33 C31 P1 113.29(19) . . ?
C34 C31 P1 109.37(19) . . ?
C33 C31 H31 107.2 . . ?
C34 C31 H31 107.2 . . ?
P1 C31 H31 107.2 . . ?
C35 C32 C36 110.0(2) . . ?
C35 C32 P1 109.4(2) . . ?
C36 C32 P1 114.3(2) . . ?
C35 C32 H32 107.6 . . ?
C36 C32 H32 107.6 . . ?
P1 C32 H32 107.6 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C82 C81 H81A 109.5 . . ?
C82 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C82 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C82 C83 C84 110.3(9) . . ?
C82 C83 H83A 109.6 . . ?
C84 C83 H83A 109.6 . . ?
C82 C83 H83B 109.6 . . ?
C84 C83 H83B 109.6 . . ?
H83A C83 H83B 108.1 . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C85 C84 C83 122.1(10) . . ?
C85 C84 H84A 106.8 . . ?
C83 C84 H84A 106.8 . . ?
C85 C84 H84B 106.8 . . ?
C83 C84 H84B 106.8 . . ?
H84A C84 H84B 106.7 . . ?
C83 C82 C81 102.6(9) . . ?
C83 C82 H82A 111.2 . . ?
C81 C82 H82A 111.2 . . ?
C83 C82 H82B 111.2 . . ?
C81 C82 H82B 111.2 . . ?
H82A C82 H82B 109.2 . . ?
C93 C92 C91 122.0(14) . . ?
C93 C92 H92A 106.8 . . ?
C91 C92 H92A 106.8 . . ?
C93 C92 H92B 106.8 . . ?
C91 C92 H92B 106.8 . . ?
H92A C92 H92B 106.7 . . ?
C92 C93 C94 137.9(13) . . ?
C92 C93 H93A 102.6 . . ?
C94 C93 H93A 102.6 . . ?
C92 C93 H93B 102.6 . . ?
C94 C93 H93B 102.6 . . ?
H93A C93 H93B 105.0 . . ?
C93 C94 C95 114.1(12) . . ?
C93 C94 H94A 108.7 . . ?
C95 C94 H94A 108.7 . . ?
C93 C94 H94B 108.7 . . ?
C95 C94 H94B 108.7 . . ?
H94A C94 H94B 107.6 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C43 C41 C44 111.0(2) . . ?
C43 C41 P2 108.40(19) . . ?
C44 C41 P2 116.7(2) . . ?
C43 C41 H41 106.7 . . ?
C44 C41 H41 106.7 . . ?
P2 C41 H41 106.7 . . ?
C45 C42 C46 111.1(3) . . ?
C45 C42 P2 113.2(2) . . ?
C46 C42 P2 108.5(2) . . ?
C45 C42 H42 108.0 . . ?
C46 C42 H42 108.0 . . ?
P2 C42 H42 108.0 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C56 C51 C52 116.1(3) . . ?
C56 C51 Si 125.6(2) . . ?
C52 C51 Si 118.2(2) . . ?
C53 C52 C51 121.9(3) . . ?
C53 C52 H52 119.0 . . ?
C51 C52 H52 119.0 . . ?
C54 C53 C52 120.5(3) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C55 C54 C53 119.0(3) . . ?
C55 C54 H54 120.5 . . ?
C53 C54 H54 120.5 . . ?
C54 C55 C56 120.3(3) . . ?
C54 C55 H55 119.8 . . ?
C56 C55 H55 119.8 . . ?
C55 C56 C51 122.1(3) . . ?
C55 C56 H56 118.9 . . ?
C51 C56 H56 118.9 . . ?
C66 C61 C62 116.5(3) . . ?
C66 C61 Si 122.1(2) . . ?
C62 C61 Si 121.2(2) . . ?
C63 C62 C61 122.0(3) . . ?
C63 C62 H62 119.0 . . ?
C61 C62 H62 119.0 . . ?
C64 C63 C62 120.0(3) . . ?
C64 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
C65 C64 C63 119.7(3) . . ?
C65 C64 H64 120.1 . . ?
C63 C64 H64 120.1 . . ?
C64 C65 C66 119.8(3) . . ?
C64 C65 H65 120.1 . . ?
C66 C65 H65 120.1 . . ?
C65 C66 C61 122.0(3) . . ?
C65 C66 H66 119.0 . . ?
C61 C66 H66 119.0 . . ?
C72 C71 C76 116.1(3) . . ?
C72 C71 Si 123.9(2) . . ?
C76 C71 Si 119.9(2) . . ?
C73 C72 C71 121.8(3) . . ?
C73 C72 H72 119.1 . . ?
C71 C72 H72 119.1 . . ?
C74 C73 C72 120.3(3) . . ?
C74 C73 H73 119.8 . . ?
C72 C73 H73 119.8 . . ?
C73 C74 C75 119.5(3) . . ?
C73 C74 H74 120.2 . . ?
C75 C74 H74 120.2 . . ?
C74 C75 C76 119.9(3) . . ?
C74 C75 H75 120.0 . . ?
C76 C75 H75 120.0 . . ?
C75 C76 C71 122.3(3) . . ?
C75 C76 H76 118.9 . . ?
C71 C76 H76 118.9 . . ?
C12 P1 C32 107.04(13) . . ?
C12 P1 C31 100.82(12) . . ?
C32 P1 C31 105.13(13) . . ?
C12 P1 Pd 100.69(9) . . ?
C32 P1 Pd 119.91(9) . . ?
C31 P1 Pd 120.58(9) . . ?
C22 P2 C42 102.90(13) . . ?
C22 P2 C41 104.70(12) . . ?
C42 P2 C41 107.33(13) . . ?
C22 P2 Pd 104.80(9) . . ?
C42 P2 Pd 116.26(10) . . ?
C41 P2 Pd 118.93(9) . . ?
C16 C11 C12 117.3(3) . . ?
C16 C11 C 125.5(3) . . ?
C12 C11 C 117.0(2) . . ?
C13 C12 C11 120.6(3) . . ?
C13 C12 P1 124.8(2) . . ?
C11 C12 P1 114.12(19) . . ?
C12 C13 C14 120.3(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 119.2(3) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C11 121.3(3) . . ?
C15 C16 H16 119.3 . . ?
C11 C16 H16 119.3 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.455
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.101
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc181a
_database_code_depnum_ccdc_archive 'CCDC 1436838'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H49 B O2 P2 Pd'
_chemical_formula_weight         632.85

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'
B B 0.0013 0.0007 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   17.3966(10)
_cell_length_b                   10.0819(6)
_cell_length_c                   19.8141(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.8960(18)
_cell_angle_gamma                90.00
_cell_volume                     3126.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6655
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            71734
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0119
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5509
_reflns_number_gt                4985
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0246P)²+2.2939P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5509
_refine_ls_number_parameters     350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_ref         0.0528
_refine_ls_wR_factor_gt          0.0513
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.675705(8) 0.508606(12) 0.274167(7) 0.01323(5) Uani 1 1 d . . .
B B 0.82663(12) 0.65902(19) 0.35972(11) 0.0162(4) Uani 1 1 d . . .
C C 0.80525(10) 0.51143(16) 0.36439(9) 0.0140(3) Uani 1 1 d . . .
P1 P 0.63274(3) 0.46931(4) 0.36433(2) 0.01333(9) Uani 1 1 d . . .
P2 P 0.73929(3) 0.48864(4) 0.19578(2) 0.01458(10) Uani 1 1 d . . .
C21 C 0.84049(10) 0.41650(16) 0.26252(9) 0.0152(3) Uani 1 1 d . . .
C16 C 0.73781(11) 0.41854(17) 0.51905(10) 0.0189(4) Uani 1 1 d . . .
H16 H 0.6874 0.3934 0.5232 0.023 Uiso 1 1 calc R . .
C15 C 0.81471(11) 0.42228(17) 0.58264(9) 0.0197(4) Uani 1 1 d . . .
H15 H 0.8176 0.3979 0.6300 0.024 Uiso 1 1 calc R . .
C14 C 0.88772(11) 0.46203(17) 0.57652(10) 0.0199(4) Uani 1 1 d . . .
H14 H 0.9405 0.4693 0.6201 0.024 Uiso 1 1 calc R . .
C13 C 0.88350(11) 0.49106(16) 0.50663(10) 0.0179(4) Uani 1 1 d . . .
H13 H 0.9341 0.5183 0.5034 0.021 Uiso 1 1 calc R . .
C12 C 0.80730(11) 0.48171(15) 0.44053(9) 0.0137(3) Uani 1 1 d . . .
C11 C 0.73283(10) 0.45121(16) 0.44856(9) 0.0142(3) Uani 1 1 d . . .
C22 C 0.85567(10) 0.41832(16) 0.33891(9) 0.0137(3) Uani 1 1 d . . .
C23 C 0.92059(10) 0.33429(16) 0.38734(10) 0.0169(4) Uani 1 1 d . . .
H23 H 0.9295 0.3266 0.4380 0.020 Uiso 1 1 calc R . .
C24 C 0.97223(11) 0.26208(17) 0.36381(10) 0.0205(4) Uani 1 1 d . . .
H24 H 1.0159 0.2070 0.3985 0.025 Uiso 1 1 calc R . .
C25 C 0.96078(11) 0.26947(17) 0.29016(10) 0.0217(4) Uani 1 1 d . . .
H25 H 0.9979 0.2233 0.2746 0.026 Uiso 1 1 calc R . .
C26 C 0.89418(11) 0.34549(17) 0.23982(10) 0.0193(4) Uani 1 1 d . . .
H26 H 0.8848 0.3495 0.1889 0.023 Uiso 1 1 calc R . .
O31 O 0.86186(8) 0.70894(11) 0.31424(7) 0.0188(3) Uani 1 1 d . . .
C31 C 0.88600(11) 0.84627(17) 0.33615(10) 0.0195(4) Uani 1 1 d . . .
O32 O 0.81480(8) 0.75777(12) 0.40274(7) 0.0196(3) Uani 1 1 d . . .
C33 C 0.87166(12) 0.92697(18) 0.26680(10) 0.0241(4) Uani 1 1 d . . .
H33A H 0.9110 0.8966 0.2466 0.036 Uiso 1 1 calc R . .
H33B H 0.8822 1.0210 0.2803 0.036 Uiso 1 1 calc R . .
H33C H 0.8126 0.9154 0.2288 0.036 Uiso 1 1 calc R . .
H H 0.5830(18) 0.489(2) 0.2091(16) 0.062(8) Uiso 1 1 d . . .
C34 C 0.98066(12) 0.8445(2) 0.39001(11) 0.0275(4) Uani 1 1 d . . .
H34A H 1.0125 0.7999 0.3662 0.041 Uiso 1 1 calc R . .
H34B H 0.9891 0.7968 0.4358 0.041 Uiso 1 1 calc R . .
H34C H 1.0014 0.9358 0.4027 0.041 Uiso 1 1 calc R . .
C35 C 0.74001(12) 0.9329(2) 0.31776(12) 0.0300(4) Uani 1 1 d . . .
H35A H 0.7459 1.0189 0.2974 0.045 Uiso 1 1 calc R . .
H35B H 0.7028 0.9426 0.3430 0.045 Uiso 1 1 calc R . .
H35C H 0.7149 0.8685 0.2768 0.045 Uiso 1 1 calc R . .
C36 C 0.86618(15) 0.98158(19) 0.43829(12) 0.0321(5) Uani 1 1 d . . .
H36A H 0.8810 1.0640 0.4205 0.048 Uiso 1 1 calc R . .
H36B H 0.9178 0.9427 0.4779 0.048 Uiso 1 1 calc R . .
H36C H 0.8248 1.0007 0.4583 0.048 Uiso 1 1 calc R . .
C41 C 0.57146(11) 0.60208(17) 0.38368(9) 0.0173(4) Uani 1 1 d . . .
H41 H 0.5196 0.6189 0.3356 0.021 Uiso 1 1 calc R . .
C42 C 0.57194(11) 0.31656(17) 0.35790(10) 0.0193(4) Uani 1 1 d . . .
H42 H 0.5667 0.3059 0.4059 0.023 Uiso 1 1 calc R . .
C43 C 0.53990(12) 0.57012(19) 0.44247(11) 0.0249(4) Uani 1 1 d . . .
H43A H 0.5056 0.6442 0.4463 0.037 Uiso 1 1 calc R . .
H43B H 0.5890 0.5560 0.4911 0.037 Uiso 1 1 calc R . .
H43C H 0.5048 0.4896 0.4278 0.037 Uiso 1 1 calc R . .
C44 C 0.62376(12) 0.72993(18) 0.40306(11) 0.0242(4) Uani 1 1 d . . .
H44A H 0.6440 0.7474 0.3649 0.036 Uiso 1 1 calc R . .
H44B H 0.6728 0.7206 0.4522 0.036 Uiso 1 1 calc R . .
H44C H 0.5880 0.8039 0.4045 0.036 Uiso 1 1 calc R . .
C45 C 0.48215(12) 0.3272(2) 0.29398(11) 0.0292(4) Uani 1 1 d . . .
H45A H 0.4859 0.3447 0.2469 0.044 Uiso 1 1 calc R . .
H45B H 0.4515 0.4000 0.3043 0.044 Uiso 1 1 calc R . .
H45C H 0.4514 0.2439 0.2897 0.044 Uiso 1 1 calc R . .
C46 C 0.61953(13) 0.19601(19) 0.34826(12) 0.0299(4) Uani 1 1 d . . .
H46A H 0.5881 0.1150 0.3478 0.045 Uiso 1 1 calc R . .
H46B H 0.6769 0.1922 0.3900 0.045 Uiso 1 1 calc R . .
H46C H 0.6241 0.2035 0.3008 0.045 Uiso 1 1 calc R . .
C51 C 0.69203(11) 0.35461(18) 0.12545(9) 0.0198(4) Uani 1 1 d . . .
H51 H 0.7330 0.3323 0.1041 0.024 Uiso 1 1 calc R . .
C52 C 0.76273(12) 0.62836(18) 0.14690(10) 0.0211(4) Uani 1 1 d . . .
H52 H 0.8109 0.6783 0.1867 0.025 Uiso 1 1 calc R . .
C53 C 0.60712(12) 0.3972(2) 0.06107(10) 0.0281(4) Uani 1 1 d . . .
H53A H 0.6170 0.4719 0.0342 0.042 Uiso 1 1 calc R . .
H53B H 0.5673 0.4241 0.0814 0.042 Uiso 1 1 calc R . .
H53C H 0.5828 0.3227 0.0264 0.042 Uiso 1 1 calc R . .
C54 C 0.67952(12) 0.23130(18) 0.16460(10) 0.0239(4) Uani 1 1 d . . .
H54A H 0.6596 0.1576 0.1288 0.036 Uiso 1 1 calc R . .
H54B H 0.6370 0.2500 0.1833 0.036 Uiso 1 1 calc R . .
H54C H 0.7339 0.2073 0.2067 0.036 Uiso 1 1 calc R . .
C55 C 0.68801(13) 0.7259(2) 0.11497(11) 0.0294(4) Uani 1 1 d . . .
H55A H 0.7060 0.8063 0.0979 0.044 Uiso 1 1 calc R . .
H55B H 0.6700 0.7491 0.1540 0.044 Uiso 1 1 calc R . .
H55C H 0.6401 0.6848 0.0725 0.044 Uiso 1 1 calc R . .
C56 C 0.79422(14) 0.5892(2) 0.08850(11) 0.0309(5) Uani 1 1 d . . .
H56A H 0.7487 0.5418 0.0471 0.046 Uiso 1 1 calc R . .
H56B H 0.8444 0.5317 0.1119 0.046 Uiso 1 1 calc R . .
H56C H 0.8096 0.6693 0.0691 0.046 Uiso 1 1 calc R . .
C32 C 0.82732(12) 0.88456(17) 0.37363(10) 0.0207(4) 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
Pd C 2.1809(17) . ?
Pd P1 2.2524(4) . ?
Pd P2 2.2754(4) . ?
Pd H 1.58(3) . ?
B O32 1.383(2) . ?
B O31 1.387(2) . ?
B C 1.546(2) . ?
C C22 1.514(2) . ?
C C12 1.523(2) . ?
P1 C11 1.8200(17) . ?
P1 C42 1.8408(17) . ?
P1 C41 1.8526(17) . ?
P2 C21 1.8285(17) . ?
P2 C52 1.8529(18) . ?
P2 C51 1.8555(18) . ?
C21 C26 1.398(2) . ?
C21 C22 1.418(2) . ?
C16 C15 1.381(2) . ?
C16 C11 1.400(2) . ?
C16 H16 0.9500 . ?
C15 C14 1.387(3) . ?
C15 H15 0.9500 . ?
C14 C13 1.386(2) . ?
C14 H14 0.9500 . ?
C13 C12 1.402(2) . ?
C13 H13 0.9500 . ?
C12 C11 1.407(2) . ?
C22 C23 1.403(2) . ?
C23 C24 1.386(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.386(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
O31 C31 1.457(2) . ?
C31 C33 1.521(2) . ?
C31 C34 1.522(3) . ?
C31 C32 1.551(2) . ?
O32 C32 1.457(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C32 1.517(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C32 1.516(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 C43 1.523(2) . ?
C41 C44 1.527(2) . ?
C41 H41 1.0000 . ?
C42 C45 1.526(2) . ?
C42 C46 1.529(3) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C54 1.530(2) . ?
C51 C53 1.532(3) . ?
C51 H51 1.0000 . ?
C52 C55 1.529(3) . ?
C52 C56 1.532(3) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C Pd P1 86.23(4) . . ?
C Pd P2 85.66(4) . . ?
P1 Pd P2 162.648(17) . . ?
C Pd H 173.4(9) . . ?
P1 Pd H 92.9(10) . . ?
P2 Pd H 93.4(10) . . ?
O32 B O31 111.48(15) . . ?
O32 B C 123.46(16) . . ?
O31 B C 125.04(16) . . ?
C22 C C12 116.23(13) . . ?
C22 C B 112.77(14) . . ?
C12 C B 110.26(14) . . ?
C22 C Pd 105.09(10) . . ?
C12 C Pd 112.22(11) . . ?
B C Pd 98.80(11) . . ?
C11 P1 C42 105.68(8) . . ?
C11 P1 C41 106.81(8) . . ?
C42 P1 C41 104.70(8) . . ?
C11 P1 Pd 103.23(5) . . ?
C42 P1 Pd 118.16(6) . . ?
C41 P1 Pd 117.21(6) . . ?
C21 P2 C52 108.56(8) . . ?
C21 P2 C51 102.96(8) . . ?
C52 P2 C51 106.72(8) . . ?
C21 P2 Pd 98.23(5) . . ?
C52 P2 Pd 124.97(6) . . ?
C51 P2 Pd 112.89(6) . . ?
C26 C21 C22 120.71(15) . . ?
C26 C21 P2 122.59(13) . . ?
C22 C21 P2 116.00(12) . . ?
C15 C16 C11 121.13(16) . . ?
C15 C16 H16 119.4 . . ?
C11 C16 H16 119.4 . . ?
C16 C15 C14 119.17(16) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C13 C14 C15 119.85(16) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C14 C13 C12 122.36(16) . . ?
C14 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C13 C12 C11 116.81(15) . . ?
C13 C12 C 121.05(15) . . ?
C11 C12 C 122.05(15) . . ?
C16 C11 C12 120.36(15) . . ?
C16 C11 P1 123.77(13) . . ?
C12 C11 P1 115.72(12) . . ?
C23 C22 C21 116.19(15) . . ?
C23 C22 C 123.84(15) . . ?
C21 C22 C 119.93(14) . . ?
C24 C23 C22 122.25(16) . . ?
C24 C23 H23 118.9 . . ?
C22 C23 H23 118.9 . . ?
C23 C24 C25 120.65(16) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C26 C25 C24 118.60(16) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C25 C26 C21 121.23(16) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
B O31 C31 107.63(13) . . ?
O31 C31 C33 109.08(14) . . ?
O31 C31 C34 106.31(14) . . ?
C33 C31 C34 109.88(15) . . ?
O31 C31 C32 102.41(13) . . ?
C33 C31 C32 114.65(15) . . ?
C34 C31 C32 113.83(15) . . ?
B O32 C32 107.41(13) . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C43 C41 C44 111.13(15) . . ?
C43 C41 P1 115.95(12) . . ?
C44 C41 P1 109.18(12) . . ?
C43 C41 H41 106.7 . . ?
C44 C41 H41 106.7 . . ?
P1 C41 H41 106.7 . . ?
C45 C42 C46 111.50(16) . . ?
C45 C42 P1 110.33(12) . . ?
C46 C42 P1 110.34(12) . . ?
C45 C42 H42 108.2 . . ?
C46 C42 H42 108.2 . . ?
P1 C42 H42 108.2 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C54 C51 C53 110.53(15) . . ?
C54 C51 P2 108.99(12) . . ?
C53 C51 P2 111.79(13) . . ?
C54 C51 H51 108.5 . . ?
C53 C51 H51 108.5 . . ?
P2 C51 H51 108.5 . . ?
C55 C52 C56 111.88(15) . . ?
C55 C52 P2 111.34(13) . . ?
C56 C52 P2 115.58(13) . . ?
C55 C52 H52 105.7 . . ?
C56 C52 H52 105.7 . . ?
P2 C52 H52 105.7 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 C56 H56A 109.5 . . ?
C52 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C52 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O32 C32 C36 108.66(14) . . ?
O32 C32 C35 107.20(14) . . ?
C36 C32 C35 110.13(16) . . ?
O32 C32 C31 102.39(13) . . ?
C36 C32 C31 114.92(15) . . ?
C35 C32 C31 112.90(15) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.052
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc293
_database_code_depnum_ccdc_archive 'CCDC 1436839'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H44 Ge P2 Pd'
_chemical_formula_weight         657.59

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3636(3)
_cell_length_b                   10.0092(4)
_cell_length_c                   18.4078(7)
_cell_angle_alpha                94.2185(11)
_cell_angle_beta                 93.3363(11)
_cell_angle_gamma                100.7761(11)
_cell_volume                     1505.62(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9732
_cell_measurement_theta_min      2.272
_cell_measurement_theta_max      26.868

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6773
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'combination of ω- and φ-scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            32263
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5270
_reflns_number_gt                4607
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0181P)²+4.0326P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5270
_refine_ls_number_parameters     332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0725
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.17687(3) 0.89245(3) 0.241572(14) 0.01732(8) Uani 1 1 d . . .
Ge Ge 0.15572(5) 0.72582(4) 0.33352(2) 0.01885(10) Uani 1 1 d . . .
P1 P 0.18342(12) 1.08788(9) 0.31773(5) 0.0190(2) Uani 1 1 d . . .
H1 H 0.187(5) 0.594(4) 0.315(2) 0.043(12) Uiso 1 1 d . . .
P2 P 0.21556(11) 0.74690(9) 0.14668(5) 0.01585(19) Uani 1 1 d . . .
H2 H 0.260(5) 0.760(4) 0.402(2) 0.038(12) Uiso 1 1 d . . .
C C 0.1922(4) 1.0386(3) 0.16188(18) 0.0199(8) Uani 1 1 d . . .
H H 0.0856 1.0703 0.1606 0.024 Uiso 1 1 calc R . .
C11 C 0.3194(5) 1.1615(3) 0.19230(19) 0.0213(8) Uani 1 1 d . . .
C12 C 0.3069(4) 1.2119(4) 0.26524(19) 0.0212(8) Uani 1 1 d . . .
C13 C 0.4068(5) 1.3332(4) 0.2948(2) 0.0253(8) Uani 1 1 d . . .
H13 H 0.3910 1.3704 0.3423 0.030 Uiso 1 1 calc R . .
C14 C 0.5288(5) 1.4000(4) 0.2555(2) 0.0305(9) Uani 1 1 d . . .
H14 H 0.5966 1.4829 0.2756 0.037 Uiso 1 1 calc R . .
C15 C 0.5510(5) 1.3448(4) 0.1867(2) 0.0297(9) Uani 1 1 d . . .
H15 H 0.6394 1.3869 0.1609 0.036 Uiso 1 1 calc R . .
C16 C 0.4459(5) 1.2288(4) 0.1546(2) 0.0247(8) Uani 1 1 d . . .
H16 H 0.4605 1.1947 0.1064 0.030 Uiso 1 1 calc R . .
C21 C 0.2102(4) 0.9855(4) 0.08431(19) 0.0193(8) Uani 1 1 d . . .
C22 C 0.2208(4) 0.8487(3) 0.06831(18) 0.0174(7) Uani 1 1 d . . .
C25 C 0.2070(4) 1.0175(4) -0.0442(2) 0.0233(8) Uani 1 1 d . . .
H25 H 0.2010 1.0753 -0.0826 0.028 Uiso 1 1 calc R . .
C24 C 0.2185(4) 0.8827(4) -0.06031(19) 0.0234(8) Uani 1 1 d . . .
H24 H 0.2227 0.8484 -0.1095 0.028 Uiso 1 1 calc R . .
C23 C 0.2239(4) 0.7979(4) -0.00475(18) 0.0204(8) Uani 1 1 d . . .
H23 H 0.2296 0.7048 -0.0159 0.025 Uiso 1 1 calc R . .
C26 C 0.2043(4) 1.0683(4) 0.0269(2) 0.0235(8) Uani 1 1 d . . .
H26 H 0.1982 1.1615 0.0373 0.028 Uiso 1 1 calc R . .
C31 C 0.2966(5) 1.1184(4) 0.40875(19) 0.0232(8) Uani 1 1 d . . .
H31 H 0.3151 1.2187 0.4231 0.028 Uiso 1 1 calc R . .
C32 C -0.0150(5) 1.1388(4) 0.3338(2) 0.0257(8) Uani 1 1 d . . .
H32 H -0.0724 1.0734 0.3667 0.031 Uiso 1 1 calc R . .
C34 C 0.1969(5) 1.0463(4) 0.4666(2) 0.0282(9) Uani 1 1 d . . .
H34A H 0.1001 1.0866 0.4733 0.042 Uiso 1 1 calc R . .
H34B H 0.2638 1.0571 0.5130 0.042 Uiso 1 1 calc R . .
H34C H 0.1630 0.9490 0.4507 0.042 Uiso 1 1 calc R . .
C35 C -0.1238(5) 1.1253(4) 0.2630(2) 0.0305(9) Uani 1 1 d . . .
H35A H -0.0769 1.1943 0.2312 0.046 Uiso 1 1 calc R . .
H35B H -0.2331 1.1387 0.2743 0.046 Uiso 1 1 calc R . .
H35C H -0.1313 1.0341 0.2382 0.046 Uiso 1 1 calc R . .
C36 C 0.0016(5) 1.2807(4) 0.3718(2) 0.0334(10) Uani 1 1 d . . .
H36A H 0.0629 1.3476 0.3425 0.050 Uiso 1 1 calc R . .
H36B H 0.0598 1.2848 0.4200 0.050 Uiso 1 1 calc R . .
H36C H -0.1071 1.3015 0.3777 0.050 Uiso 1 1 calc R . .
C41 C 0.4172(4) 0.7003(4) 0.1568(2) 0.0239(8) Uani 1 1 d . . .
H41 H 0.4134 0.6359 0.1960 0.029 Uiso 1 1 calc R . .
C42 C 0.0729(4) 0.5879(3) 0.1122(2) 0.0203(8) Uani 1 1 d . . .
H42 H 0.1059 0.5588 0.0630 0.024 Uiso 1 1 calc R . .
C43 C 0.5425(4) 0.8292(4) 0.1841(2) 0.0304(9) Uani 1 1 d . . .
H43A H 0.6507 0.8058 0.1912 0.046 Uiso 1 1 calc R . .
H43B H 0.5116 0.8675 0.2305 0.046 Uiso 1 1 calc R . .
H43C H 0.5453 0.8966 0.1479 0.046 Uiso 1 1 calc R . .
C44 C 0.4670(5) 0.6284(5) 0.0884(2) 0.0358(10) Uani 1 1 d . . .
H44A H 0.3826 0.5483 0.0720 0.054 Uiso 1 1 calc R . .
H44B H 0.5707 0.5995 0.0994 0.054 Uiso 1 1 calc R . .
H44C H 0.4796 0.6912 0.0498 0.054 Uiso 1 1 calc R . .
C45 C -0.0984(4) 0.6186(4) 0.1016(2) 0.0304(9) Uani 1 1 d . . .
H45A H -0.0966 0.6937 0.0702 0.046 Uiso 1 1 calc R . .
H45B H -0.1357 0.6446 0.1491 0.046 Uiso 1 1 calc R . .
H45C H -0.1729 0.5371 0.0786 0.046 Uiso 1 1 calc R . .
C46 C 0.0749(5) 0.4698(4) 0.1599(2) 0.0342(10) Uani 1 1 d . . .
H46A H 0.0032 0.3874 0.1363 0.051 Uiso 1 1 calc R . .
H46B H 0.0364 0.4929 0.2077 0.051 Uiso 1 1 calc R . .
H46C H 0.1865 0.4532 0.1665 0.051 Uiso 1 1 calc R . .
C51 C -0.0655(4) 0.6861(3) 0.37003(18) 0.0191(8) Uani 1 1 d . . .
C52 C -0.1896(4) 0.7479(4) 0.3436(2) 0.0229(8) Uani 1 1 d . . .
H52 H -0.1681 0.8094 0.3069 0.028 Uiso 1 1 calc R . .
C53 C -0.3448(5) 0.7226(4) 0.3693(2) 0.0311(9) Uani 1 1 d . . .
H53 H -0.4273 0.7669 0.3505 0.037 Uiso 1 1 calc R . .
C54 C -0.3780(5) 0.6327(4) 0.4221(2) 0.0328(10) Uani 1 1 d . . .
H54 H -0.4839 0.6142 0.4396 0.039 Uiso 1 1 calc R . .
C55 C -0.2571(5) 0.5696(4) 0.4495(2) 0.0339(10) Uani 1 1 d . . .
H55 H -0.2797 0.5079 0.4860 0.041 Uiso 1 1 calc R . .
C56 C -0.1028(5) 0.5959(4) 0.4240(2) 0.0256(8) Uani 1 1 d . . .
H56 H -0.0206 0.5519 0.4435 0.031 Uiso 1 1 calc R . .
C33 C 0.4638(5) 1.0795(4) 0.4049(2) 0.0311(9) Uani 1 1 d . . .
H33A H 0.4504 0.9805 0.3942 0.047 Uiso 1 1 calc R . .
H33B H 0.5272 1.1071 0.4518 0.047 Uiso 1 1 calc R . .
H33C H 0.5214 1.1260 0.3662 0.047 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
Pd C 2.139(3) . ?
Pd P2 2.2685(9) . ?
Pd P1 2.3113(9) . ?
Pd Ge 2.4531(4) . ?
Ge C51 1.986(4) . ?
Ge H1 1.41(4) . ?
Ge H2 1.47(4) . ?
P1 C12 1.831(4) . ?
P1 C31 1.852(4) . ?
P1 C32 1.858(4) . ?
P2 C22 1.824(3) . ?
P2 C41 1.835(4) . ?
P2 C42 1.847(3) . ?
C C21 1.513(5) . ?
C C11 1.516(5) . ?
C H 1.0000 . ?
C11 C16 1.393(5) . ?
C11 C12 1.416(5) . ?
C12 C13 1.393(5) . ?
C13 C14 1.384(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.394(5) . ?
C21 C22 1.400(5) . ?
C22 C23 1.406(5) . ?
C25 C26 1.373(5) . ?
C25 C24 1.383(5) . ?
C25 H25 0.9500 . ?
C24 C23 1.380(5) . ?
C24 H24 0.9500 . ?
C23 H23 0.9500 . ?
C26 H26 0.9500 . ?
C31 C33 1.524(5) . ?
C31 C34 1.531(5) . ?
C31 H31 1.0000 . ?
C32 C36 1.515(5) . ?
C32 C35 1.528(5) . ?
C32 H32 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 C44 1.522(5) . ?
C41 C43 1.534(5) . ?
C41 H41 1.0000 . ?
C42 C45 1.525(5) . ?
C42 C46 1.526(5) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C52 1.387(5) . ?
C51 C56 1.400(5) . ?
C52 C53 1.392(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.378(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.379(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.384(5) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C Pd P2 84.20(10) . . ?
C Pd P1 80.63(10) . . ?
P2 Pd P1 162.61(3) . . ?
C Pd Ge 179.17(10) . . ?
P2 Pd Ge 96.34(3) . . ?
P1 Pd Ge 98.93(3) . . ?
C51 Ge Pd 112.45(10) . . ?
C51 Ge H1 102.8(17) . . ?
Pd Ge H1 119.2(17) . . ?
C51 Ge H2 101.9(16) . . ?
Pd Ge H2 118.7(16) . . ?
H1 Ge H2 99(2) . . ?
C12 P1 C31 102.26(17) . . ?
C12 P1 C32 110.32(17) . . ?
C31 P1 C32 104.11(17) . . ?
C12 P1 Pd 99.10(12) . . ?
C31 P1 Pd 122.39(13) . . ?
C32 P1 Pd 117.20(12) . . ?
C22 P2 C41 105.78(16) . . ?
C22 P2 C42 102.62(16) . . ?
C41 P2 C42 105.64(17) . . ?
C22 P2 Pd 104.10(11) . . ?
C41 P2 Pd 111.36(12) . . ?
C42 P2 Pd 125.47(12) . . ?
C21 C C11 115.5(3) . . ?
C21 C Pd 116.2(2) . . ?
C11 C Pd 107.1(2) . . ?
C21 C H 105.7 . . ?
C11 C H 105.7 . . ?
Pd C H 105.7 . . ?
C16 C11 C12 117.7(3) . . ?
C16 C11 C 125.7(3) . . ?
C12 C11 C 116.6(3) . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 P1 125.1(3) . . ?
C11 C12 P1 113.3(3) . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 119.4(4) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.9(4) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C11 120.8(3) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
C26 C21 C22 118.8(3) . . ?
C26 C21 C 120.9(3) . . ?
C22 C21 C 120.2(3) . . ?
C21 C22 C23 119.5(3) . . ?
C21 C22 P2 115.2(3) . . ?
C23 C22 P2 125.1(3) . . ?
C26 C25 C24 120.3(3) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C23 C24 C25 119.9(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C23 C22 120.3(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C26 C21 121.2(3) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
C33 C31 C34 112.6(3) . . ?
C33 C31 P1 110.6(3) . . ?
C34 C31 P1 111.5(3) . . ?
C33 C31 H31 107.3 . . ?
C34 C31 H31 107.3 . . ?
P1 C31 H31 107.3 . . ?
C36 C32 C35 110.1(3) . . ?
C36 C32 P1 113.8(3) . . ?
C35 C32 P1 111.5(3) . . ?
C36 C32 H32 107.0 . . ?
C35 C32 H32 107.0 . . ?
P1 C32 H32 107.0 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C44 C41 C43 112.0(3) . . ?
C44 C41 P2 114.4(3) . . ?
C43 C41 P2 108.3(3) . . ?
C44 C41 H41 107.3 . . ?
C43 C41 H41 107.3 . . ?
P2 C41 H41 107.3 . . ?
C45 C42 C46 111.1(3) . . ?
C45 C42 P2 108.9(2) . . ?
C46 C42 P2 114.1(3) . . ?
C45 C42 H42 107.5 . . ?
C46 C42 H42 107.5 . . ?
P2 C42 H42 107.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C52 C51 C56 117.1(3) . . ?
C52 C51 Ge 121.2(3) . . ?
C56 C51 Ge 121.7(3) . . ?
C51 C52 C53 122.0(4) . . ?
C51 C52 H52 119.0 . . ?
C53 C52 H52 119.0 . . ?
C54 C53 C52 119.6(4) . . ?
C54 C53 H53 120.2 . . ?
C52 C53 H53 120.2 . . ?
C53 C54 C55 119.8(4) . . ?
C53 C54 H54 120.1 . . ?
C55 C54 H54 120.1 . . ?
C54 C55 C56 120.4(4) . . ?
C54 C55 H55 119.8 . . ?
C56 C55 H55 119.8 . . ?
C55 C56 C51 121.2(4) . . ?
C55 C56 H56 119.4 . . ?
C51 C56 H56 119.4 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.090
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc307
_database_code_depnum_ccdc_archive 'CCDC 1436840'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H48 Ge P2 Pd'
_chemical_formula_weight         733.68

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   I2/a

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

_cell_length_a                   22.9918(15)
_cell_length_b                   12.0605(7)
_cell_length_c                   25.6249(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.728(4)
_cell_angle_gamma                90.00
_cell_volume                     6839.6(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3024
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7094
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48072
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6020
_reflns_number_gt                4867
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0362P)²+11.1820P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6020
_refine_ls_number_parameters     392
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.094963(12) 0.33779(2) 0.147920(10) 0.02388(9) Uani 1 1 d . . .
Ge Ge 0.024192(15) 0.18328(3) 0.135185(14) 0.02132(10) Uani 1 1 d . A .
P1 P 0.06050(4) 0.41908(7) 0.21412(4) 0.0269(2) Uani 1 1 d . A .
P2 P 0.15294(4) 0.27901(7) 0.09461(4) 0.0249(2) Uani 1 1 d . A .
H2 H 0.0007(14) 0.169(3) 0.1797(13) 0.032(9) Uiso 1 1 d . . .
C11 C 0.16439(18) 0.5286(3) 0.21554(17) 0.0416(10) Uani 1 1 d . . .
C12 C 0.11754(15) 0.5246(3) 0.24027(14) 0.0276(8) Uani 1 1 d . A .
C13 C 0.11887(16) 0.5904(3) 0.28504(14) 0.0289(8) Uani 1 1 d . . .
H13 H 0.0850 0.5923 0.2995 0.035 Uiso 1 1 calc R A .
C14 C 0.16924(16) 0.6531(3) 0.30852(15) 0.0335(9) Uani 1 1 d . A .
H14 H 0.1698 0.6998 0.3385 0.040 Uiso 1 1 calc R . .
C15 C 0.21830(16) 0.6473(3) 0.28832(15) 0.0305(8) Uani 1 1 d . . .
H15 H 0.2544 0.6851 0.3063 0.037 Uiso 1 1 calc R A .
C16 C 0.21587(16) 0.5871(3) 0.24206(16) 0.0375(10) Uani 1 1 d . A .
H16 H 0.2501 0.5856 0.2281 0.045 Uiso 1 1 calc R . .
C21 C 0.19990(16) 0.4802(3) 0.13058(15) 0.0344(9) Uani 1 1 d . . .
C22 C 0.20819(15) 0.3898(3) 0.10030(14) 0.0279(8) Uani 1 1 d . A .
C23 C 0.2504(2) 0.3944(4) 0.07139(19) 0.0574(13) Uani 1 1 d . . .
H23 H 0.2565 0.3312 0.0514 0.069 Uiso 1 1 calc R A .
C24 C 0.2838(2) 0.4882(4) 0.07075(19) 0.0646(15) Uani 1 1 d . A .
H24 H 0.3144 0.4885 0.0522 0.078 Uiso 1 1 calc R . .
C25 C 0.27287(17) 0.5813(3) 0.09714(15) 0.0375(9) Uani 1 1 d . . .
H25 H 0.2939 0.6482 0.0950 0.045 Uiso 1 1 calc R A .
C26 C 0.23173(16) 0.5771(3) 0.12628(16) 0.0364(9) Uani 1 1 d . A .
H26 H 0.2243 0.6421 0.1444 0.044 Uiso 1 1 calc R . .
C32 C -0.01196(15) 0.4914(3) 0.20001(14) 0.0315(8) Uani 1 1 d . . .
H32 H -0.0125 0.5370 0.2325 0.038 Uiso 1 1 calc R A .
C31 C 0.06260(16) 0.3244(3) 0.27146(14) 0.0285(8) Uani 1 1 d . . .
H31 H 0.0281 0.2716 0.2588 0.034 Uiso 1 1 calc R A .
C33 C 0.12021(17) 0.2555(3) 0.28330(15) 0.0396(9) Uani 1 1 d . A .
H33A H 0.1215 0.2141 0.2507 0.059 Uiso 1 1 calc R . .
H33B H 0.1208 0.2035 0.3128 0.059 Uiso 1 1 calc R . .
H33C H 0.1554 0.3047 0.2940 0.059 Uiso 1 1 calc R . .
C34 C 0.05533(19) 0.3772(3) 0.32287(15) 0.0403(10) Uani 1 1 d . A .
H34A H 0.0224 0.4315 0.3137 0.061 Uiso 1 1 calc R . .
H34B H 0.0930 0.4146 0.3418 0.061 Uiso 1 1 calc R . .
H34C H 0.0459 0.3198 0.3464 0.061 Uiso 1 1 calc R . .
C35 C -0.06542(15) 0.4122(3) 0.18853(15) 0.0331(8) Uani 1 1 d . A .
H35A H -0.1030 0.4547 0.1819 0.050 Uiso 1 1 calc R . .
H35B H -0.0617 0.3633 0.2198 0.050 Uiso 1 1 calc R . .
H35C H -0.0659 0.3675 0.1565 0.050 Uiso 1 1 calc R . .
C36 C -0.01628(19) 0.5696(3) 0.15230(16) 0.0467(10) Uani 1 1 d . A .
H36A H -0.0113 0.5272 0.1212 0.070 Uiso 1 1 calc R . .
H36B H 0.0156 0.6258 0.1624 0.070 Uiso 1 1 calc R . .
H36C H -0.0559 0.6060 0.1426 0.070 Uiso 1 1 calc R . .
C C 0.1463(2) 0.4875(4) 0.15454(19) 0.0194(15) Uani 0.676(9) 1 d P A 1
H1 H 0.1186 0.5449 0.1331 0.023 Uiso 0.676(9) 1 calc PR A 1
C3 C 0.1787(5) 0.4285(8) 0.1832(4) 0.021(3) Uani 0.324(9) 1 d P A 2
H3 H 0.2106 0.3796 0.2063 0.026 Uiso 0.324(9) 1 calc PR A 2
C41 C 0.19345(18) 0.1491(3) 0.11822(19) 0.0480(11) Uani 1 1 d . . .
H41 H 0.1625 0.0886 0.1113 0.058 Uiso 1 1 calc R A .
C42 C 0.1220(2) 0.2699(4) 0.02101(16) 0.0518(12) Uani 1 1 d . . .
H42 H 0.1568 0.2667 0.0045 0.062 Uiso 1 1 calc R A .
C43 C 0.2194(2) 0.1570(4) 0.1794(2) 0.0673(15) Uani 1 1 d . A .
H43A H 0.2425 0.0897 0.1929 0.101 Uiso 1 1 calc R . .
H43B H 0.1863 0.1645 0.1966 0.101 Uiso 1 1 calc R . .
H43C H 0.2460 0.2217 0.1883 0.101 Uiso 1 1 calc R . .
C44 C 0.24107(19) 0.1155(4) 0.0902(2) 0.0678(15) Uani 1 1 d . A .
H44A H 0.2241 0.1207 0.0508 0.102 Uiso 1 1 calc R . .
H44B H 0.2539 0.0391 0.1000 0.102 Uiso 1 1 calc R . .
H44C H 0.2760 0.1652 0.1015 0.102 Uiso 1 1 calc R . .
C45 C 0.0849(2) 0.1692(4) 0.00401(19) 0.0649(14) Uani 1 1 d . A .
H45A H 0.0700 0.1675 -0.0356 0.097 Uiso 1 1 calc R . .
H45B H 0.0506 0.1702 0.0198 0.097 Uiso 1 1 calc R . .
H45C H 0.1096 0.1032 0.0166 0.097 Uiso 1 1 calc R . .
C46 C 0.0867(2) 0.3755(4) 0.00124(18) 0.0766(17) Uani 1 1 d . A .
H46A H 0.0719 0.3740 -0.0384 0.115 Uiso 1 1 calc R . .
H46B H 0.1131 0.4399 0.0125 0.115 Uiso 1 1 calc R . .
H46C H 0.0523 0.3806 0.0169 0.115 Uiso 1 1 calc R . .
C51 C 0.05544(14) 0.0316(3) 0.13095(14) 0.0247(7) Uani 1 1 d . . .
C52 C 0.04290(15) -0.0311(3) 0.08399(15) 0.0312(8) Uani 1 1 d . A .
H52 H 0.0183 -0.0005 0.0513 0.037 Uiso 1 1 calc R . .
C53 C 0.06546(18) -0.1374(3) 0.08373(19) 0.0467(11) Uani 1 1 d . . .
H53 H 0.0563 -0.1788 0.0510 0.056 Uiso 1 1 calc R A .
C54 C 0.10079(19) -0.1829(3) 0.1302(2) 0.0485(11) Uani 1 1 d . A .
H54 H 0.1164 -0.2557 0.1298 0.058 Uiso 1 1 calc R . .
C55 C 0.11379(16) -0.1239(3) 0.17756(18) 0.0405(10) Uani 1 1 d . . .
H55 H 0.1380 -0.1558 0.2101 0.049 Uiso 1 1 calc R A .
C56 C 0.09148(15) -0.0179(3) 0.17774(15) 0.0310(8) Uani 1 1 d . A .
H56 H 0.1010 0.0227 0.2107 0.037 Uiso 1 1 calc R . .
C61 C -0.05226(14) 0.1947(3) 0.07705(13) 0.0224(7) Uani 1 1 d . . .
C62 C -0.06819(16) 0.2912(3) 0.04672(14) 0.0288(8) Uani 1 1 d . A .
H62 H -0.0402 0.3508 0.0519 0.035 Uiso 1 1 calc R . .
C63 C -0.12386(17) 0.3023(3) 0.00912(15) 0.0370(9) Uani 1 1 d . . .
H63 H -0.1336 0.3691 -0.0110 0.044 Uiso 1 1 calc R A .
C64 C -0.16496(16) 0.2176(3) 0.00077(16) 0.0374(9) Uani 1 1 d . A .
H64 H -0.2032 0.2254 -0.0250 0.045 Uiso 1 1 calc R . .
C65 C -0.15038(16) 0.1213(3) 0.02994(15) 0.0365(9) Uani 1 1 d . . .
H65 H -0.1787 0.0621 0.0243 0.044 Uiso 1 1 calc R A .
C66 C -0.09477(15) 0.1100(3) 0.06745(14) 0.0295(8) Uani 1 1 d . A .
H66 H -0.0854 0.0426 0.0871 0.035 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
Pd C 2.139(4) . ?
Pd C3 2.186(9) . ?
Pd P2 2.2655(9) . ?
Pd P1 2.2793(9) . ?
Pd Ge 2.4369(4) . ?
Ge C61 1.977(3) . ?
Ge C51 1.980(3) . ?
Ge H2 1.40(3) . ?
P1 C12 1.820(3) . ?
P1 C32 1.828(4) . ?
P1 C31 1.851(3) . ?
P2 C22 1.822(3) . ?
P2 C42 1.830(4) . ?
P2 C41 1.839(4) . ?
C11 C16 1.387(5) . ?
C11 C12 1.391(5) . ?
C11 C3 1.548(10) . ?
C11 C 1.584(6) . ?
C12 C13 1.388(5) . ?
C13 C14 1.377(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.364(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.380(5) . ?
C21 C26 1.399(5) . ?
C21 C 1.520(6) . ?
C21 C3 1.673(10) . ?
C22 C23 1.372(5) . ?
C23 C24 1.371(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.369(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.356(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C32 C35 1.521(5) . ?
C32 C36 1.526(5) . ?
C32 H32 1.0000 . ?
C31 C34 1.513(5) . ?
C31 C33 1.523(5) . ?
C31 H31 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C H1 1.0000 . ?
C3 H3 1.0000 . ?
C41 C44 1.519(6) . ?
C41 C43 1.523(6) . ?
C41 H41 1.0000 . ?
C42 C45 1.480(6) . ?
C42 C46 1.522(7) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C52 1.383(5) . ?
C51 C56 1.393(5) . ?
C52 C53 1.383(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.363(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.367(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.378(5) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C66 1.389(4) . ?
C61 C62 1.392(5) . ?
C62 C63 1.384(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.368(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.373(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.382(5) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?

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
C Pd C3 30.6(3) . . ?
C Pd P2 84.81(12) . . ?
C3 Pd P2 79.0(3) . . ?
C Pd P1 82.74(12) . . ?
C3 Pd P1 85.5(3) . . ?
P2 Pd P1 164.45(3) . . ?
C Pd Ge 172.05(14) . . ?
C3 Pd Ge 156.8(3) . . ?
P2 Pd Ge 99.24(2) . . ?
P1 Pd Ge 94.27(2) . . ?
C61 Ge C51 106.54(13) . . ?
C61 Ge Pd 118.22(9) . . ?
C51 Ge Pd 118.37(9) . . ?
C61 Ge H2 99.3(13) . . ?
C51 Ge H2 98.9(13) . . ?
Pd Ge H2 112.2(13) . . ?
C12 P1 C32 105.43(16) . . ?
C12 P1 C31 106.14(16) . . ?
C32 P1 C31 106.12(16) . . ?
C12 P1 Pd 102.35(11) . . ?
C32 P1 Pd 122.70(12) . . ?
C31 P1 Pd 112.71(11) . . ?
C22 P2 C42 101.20(17) . . ?
C22 P2 C41 108.58(17) . . ?
C42 P2 C41 108.0(2) . . ?
C22 P2 Pd 103.50(11) . . ?
C42 P2 Pd 120.85(16) . . ?
C41 P2 Pd 113.36(14) . . ?
C16 C11 C12 117.2(3) . . ?
C16 C11 C3 112.4(5) . . ?
C12 C11 C3 121.4(4) . . ?
C16 C11 C 127.1(3) . . ?
C12 C11 C 114.3(3) . . ?
C13 C12 C11 120.7(3) . . ?
C13 C12 P1 123.8(3) . . ?
C11 C12 P1 115.2(2) . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C11 121.3(3) . . ?
C15 C16 H16 119.3 . . ?
C11 C16 H16 119.3 . . ?
C22 C21 C26 117.4(3) . . ?
C22 C21 C 121.6(3) . . ?
C26 C21 C 118.8(3) . . ?
C22 C21 C3 105.9(4) . . ?
C26 C21 C3 130.3(4) . . ?
C23 C22 C21 119.8(3) . . ?
C23 C22 P2 124.4(3) . . ?
C21 C22 P2 115.1(3) . . ?
C24 C23 C22 121.4(4) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C25 C24 C23 119.5(4) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C26 C25 C24 119.4(3) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C21 122.2(3) . . ?
C25 C26 H26 118.9 . . ?
C21 C26 H26 118.9 . . ?
C35 C32 C36 111.1(3) . . ?
C35 C32 P1 112.6(2) . . ?
C36 C32 P1 108.1(3) . . ?
C35 C32 H32 108.3 . . ?
C36 C32 H32 108.3 . . ?
P1 C32 H32 108.3 . . ?
C34 C31 C33 110.6(3) . . ?
C34 C31 P1 116.5(2) . . ?
C33 C31 P1 109.2(2) . . ?
C34 C31 H31 106.7 . . ?
C33 C31 H31 106.7 . . ?
P1 C31 H31 106.7 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C21 C C11 113.1(4) . . ?
C21 C Pd 114.1(3) . . ?
C11 C Pd 109.5(3) . . ?
C21 C H1 106.5 . . ?
C11 C H1 106.5 . . ?
Pd C H1 106.5 . . ?
C11 C3 C21 107.0(6) . . ?
C11 C3 Pd 108.7(6) . . ?
C21 C3 Pd 105.6(5) . . ?
C11 C3 H3 111.8 . . ?
C21 C3 H3 111.8 . . ?
Pd C3 H3 111.8 . . ?
C44 C41 C43 111.9(4) . . ?
C44 C41 P2 115.9(3) . . ?
C43 C41 P2 107.9(3) . . ?
C44 C41 H41 106.9 . . ?
C43 C41 H41 106.9 . . ?
P2 C41 H41 106.9 . . ?
C45 C42 C46 112.0(4) . . ?
C45 C42 P2 112.6(3) . . ?
C46 C42 P2 108.4(3) . . ?
C45 C42 H42 107.9 . . ?
C46 C42 H42 107.9 . . ?
P2 C42 H42 107.9 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C52 C51 C56 116.7(3) . . ?
C52 C51 Ge 124.0(3) . . ?
C56 C51 Ge 119.2(2) . . ?
C53 C52 C51 121.4(4) . . ?
C53 C52 H52 119.3 . . ?
C51 C52 H52 119.3 . . ?
C54 C53 C52 120.3(4) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
C53 C54 C55 120.1(4) . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C54 C55 C56 119.6(4) . . ?
C54 C55 H55 120.2 . . ?
C56 C55 H55 120.2 . . ?
C55 C56 C51 121.9(4) . . ?
C55 C56 H56 119.0 . . ?
C51 C56 H56 119.0 . . ?
C66 C61 C62 116.7(3) . . ?
C66 C61 Ge 121.5(2) . . ?
C62 C61 Ge 121.6(2) . . ?
C63 C62 C61 121.6(3) . . ?
C63 C62 H62 119.2 . . ?
C61 C62 H62 119.2 . . ?
C64 C63 C62 120.4(3) . . ?
C64 C63 H63 119.8 . . ?
C62 C63 H63 119.8 . . ?
C63 C64 C65 119.3(3) . . ?
C63 C64 H64 120.3 . . ?
C65 C64 H64 120.3 . . ?
C64 C65 C66 120.3(3) . . ?
C64 C65 H65 119.8 . . ?
C66 C65 H65 119.8 . . ?
C65 C66 C61 121.7(3) . . ?
C65 C66 H66 119.2 . . ?
C61 C66 H66 119.2 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.080
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc294
_database_code_depnum_ccdc_archive 'CCDC 1436841'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Ge P2 Pd'
_chemical_formula_weight         809.78

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.6399(15)
_cell_length_b                   19.396(3)
_cell_length_c                   17.6306(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.713(2)
_cell_angle_gamma                90.00
_cell_volume                     3831.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3336
_cell_measurement_theta_min      2.422
_cell_measurement_theta_max      22.303

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'combination of ω- and φ-scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            28856
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6706
_reflns_number_gt                4441
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0476P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6706
_refine_ls_number_parameters     426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1041
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.34093(3) 0.53317(2) 0.27519(2) 0.01905(12) Uani 1 1 d . . .
P1 P 0.29412(11) 0.43823(8) 0.19210(8) 0.0213(3) Uani 1 1 d . . .
Ge Ge 0.13522(4) 0.56408(3) 0.28232(3) 0.01763(15) Uani 1 1 d . . .
P2 P 0.44506(11) 0.62511(7) 0.33964(8) 0.0207(3) Uani 1 1 d . . .
C C 0.5161(4) 0.4907(3) 0.2914(3) 0.0204(12) Uani 1 1 d . . .
H H 0.5166 0.4483 0.3238 0.024 Uiso 1 1 calc R . .
C21 C 0.6198(4) 0.5327(3) 0.3385(3) 0.0217(12) Uani 1 1 d . . .
C22 C 0.6020(4) 0.5999(3) 0.3620(3) 0.0213(13) Uani 1 1 d . . .
C23 C 0.6993(4) 0.6402(3) 0.4009(3) 0.0265(14) Uani 1 1 d . . .
H23 H 0.6871 0.6862 0.4156 0.032 Uiso 1 1 calc R . .
C24 C 0.8137(4) 0.6133(3) 0.4182(3) 0.0251(13) Uani 1 1 d . . .
H24 H 0.8802 0.6414 0.4429 0.030 Uiso 1 1 calc R . .
C25 C 0.8309(4) 0.5459(3) 0.3994(3) 0.0292(15) Uani 1 1 d . . .
H25 H 0.9090 0.5269 0.4139 0.035 Uiso 1 1 calc R . .
C26 C 0.7358(4) 0.5058(3) 0.3599(3) 0.0263(13) Uani 1 1 d . . .
H26 H 0.7490 0.4595 0.3469 0.032 Uiso 1 1 calc R . .
C31 C 0.1942(4) 0.4471(3) 0.0924(3) 0.0292(14) Uani 1 1 d . . .
H31 H 0.2079 0.4060 0.0617 0.035 Uiso 1 1 calc R . .
C32 C 0.2507(4) 0.3565(3) 0.2302(3) 0.0258(14) Uani 1 1 d . . .
H32 H 0.1726 0.3650 0.2420 0.031 Uiso 1 1 calc R . .
C33 C 0.2283(5) 0.5111(3) 0.0520(3) 0.0432(18) Uani 1 1 d . . .
H33A H 0.3130 0.5086 0.0535 0.065 Uiso 1 1 calc R . .
H33B H 0.2140 0.5526 0.0797 0.065 Uiso 1 1 calc R . .
H33C H 0.1798 0.5128 -0.0029 0.065 Uiso 1 1 calc R . .
C34 C 0.0630(4) 0.4467(3) 0.0907(3) 0.0308(15) Uani 1 1 d . . .
H34A H 0.0141 0.4439 0.0359 0.046 Uiso 1 1 calc R . .
H34B H 0.0438 0.4892 0.1147 0.046 Uiso 1 1 calc R . .
H34C H 0.0464 0.4069 0.1202 0.046 Uiso 1 1 calc R . .
C35 C 0.3394(5) 0.3383(3) 0.3074(3) 0.0353(15) Uani 1 1 d . . .
H35A H 0.3138 0.2960 0.3285 0.053 Uiso 1 1 calc R . .
H35B H 0.3437 0.3761 0.3451 0.053 Uiso 1 1 calc R . .
H35C H 0.4182 0.3311 0.2988 0.053 Uiso 1 1 calc R . .
C36 C 0.2318(5) 0.2964(3) 0.1734(4) 0.0387(16) Uani 1 1 d . . .
H36A H 0.1665 0.3071 0.1267 0.058 Uiso 1 1 calc R . .
H36B H 0.2117 0.2551 0.1991 0.058 Uiso 1 1 calc R . .
H36C H 0.3051 0.2881 0.1576 0.058 Uiso 1 1 calc R . .
C41 C 0.4371(4) 0.7028(3) 0.2787(3) 0.0245(13) Uani 1 1 d . . .
H41 H 0.5052 0.7335 0.3051 0.029 Uiso 1 1 calc R . .
C42 C 0.4221(4) 0.6517(3) 0.4349(3) 0.0242(13) Uani 1 1 d . . .
H42 H 0.3360 0.6643 0.4244 0.029 Uiso 1 1 calc R . .
C43 C 0.4530(5) 0.6817(3) 0.1985(3) 0.0371(16) Uani 1 1 d . . .
H43A H 0.3876 0.6511 0.1717 0.056 Uiso 1 1 calc R . .
H43B H 0.5293 0.6576 0.2060 0.056 Uiso 1 1 calc R . .
H43C H 0.4523 0.7230 0.1663 0.056 Uiso 1 1 calc R . .
C44 C 0.3226(4) 0.7433(3) 0.2679(3) 0.0290(14) Uani 1 1 d . . .
H44A H 0.3255 0.7847 0.2366 0.044 Uiso 1 1 calc R . .
H44B H 0.3136 0.7569 0.3195 0.044 Uiso 1 1 calc R . .
H44C H 0.2546 0.7147 0.2406 0.044 Uiso 1 1 calc R . .
C45 C 0.4421(4) 0.5887(3) 0.4894(3) 0.0303(14) Uani 1 1 d . . .
H45A H 0.3924 0.5504 0.4627 0.045 Uiso 1 1 calc R . .
H45B H 0.4204 0.6002 0.5378 0.045 Uiso 1 1 calc R . .
H45C H 0.5263 0.5751 0.5025 0.045 Uiso 1 1 calc R . .
C46 C 0.4942(5) 0.7138(3) 0.4770(3) 0.0360(15) Uani 1 1 d . . .
H46A H 0.4902 0.7513 0.4391 0.054 Uiso 1 1 calc R . .
H46B H 0.5776 0.7002 0.4994 0.054 Uiso 1 1 calc R . .
H46C H 0.4606 0.7296 0.5193 0.054 Uiso 1 1 calc R . .
C51 C 0.0629(4) 0.4756(3) 0.3029(3) 0.0197(8) Uani 1 1 d . . .
C52 C 0.1229(4) 0.4326(3) 0.3646(3) 0.0197(8) Uani 1 1 d . . .
H52 H 0.1937 0.4489 0.4009 0.024 Uiso 1 1 calc R . .
C53 C 0.0821(5) 0.3666(3) 0.3745(3) 0.0274(14) Uani 1 1 d . . .
H53 H 0.1244 0.3390 0.4175 0.033 Uiso 1 1 calc R . .
C54 C -0.0189(5) 0.3412(3) 0.3224(3) 0.0268(14) Uani 1 1 d . . .
H54 H -0.0452 0.2957 0.3281 0.032 Uiso 1 1 calc R . .
C55 C -0.0817(4) 0.3825(3) 0.2617(3) 0.0265(14) Uani 1 1 d . . .
H55 H -0.1525 0.3656 0.2260 0.032 Uiso 1 1 calc R . .
C56 C -0.0423(4) 0.4483(3) 0.2526(3) 0.0201(13) Uani 1 1 d . . .
H56 H -0.0879 0.4762 0.2110 0.024 Uiso 1 1 calc R . .
C61 C 0.0084(4) 0.6095(3) 0.1977(3) 0.0192(12) Uani 1 1 d . . .
C62 C -0.1066(4) 0.6158(3) 0.2079(3) 0.0231(13) Uani 1 1 d . . .
H62 H -0.1223 0.5973 0.2540 0.028 Uiso 1 1 calc R . .
C63 C -0.1972(4) 0.6481(3) 0.1527(3) 0.0291(14) Uani 1 1 d . . .
H63 H -0.2747 0.6509 0.1604 0.035 Uiso 1 1 calc R . .
C64 C -0.1754(5) 0.6765(3) 0.0860(3) 0.0288(14) Uani 1 1 d . . .
H64 H -0.2378 0.6988 0.0478 0.035 Uiso 1 1 calc R . .
C65 C -0.0628(5) 0.6723(3) 0.0752(3) 0.0272(14) Uani 1 1 d . . .
H65 H -0.0470 0.6925 0.0300 0.033 Uiso 1 1 calc R . .
C66 C 0.0273(4) 0.6388(3) 0.1300(3) 0.0197(12) Uani 1 1 d . . .
H66 H 0.1041 0.6356 0.1212 0.024 Uiso 1 1 calc R . .
C71 C 0.1222(4) 0.6246(3) 0.3713(3) 0.0183(12) Uani 1 1 d . . .
C72 C 0.1009(4) 0.6945(3) 0.3603(3) 0.0239(13) Uani 1 1 d . . .
H72 H 0.0813 0.7120 0.3081 0.029 Uiso 1 1 calc R . .
C73 C 0.1068(4) 0.7400(3) 0.4215(3) 0.0312(14) Uani 1 1 d . . .
H73 H 0.0925 0.7878 0.4112 0.037 Uiso 1 1 calc R . .
C74 C 0.1336(5) 0.7153(3) 0.4980(4) 0.0356(16) Uani 1 1 d . . .
H74 H 0.1410 0.7462 0.5408 0.043 Uiso 1 1 calc R . .
C75 C 0.1497(4) 0.6453(3) 0.5116(3) 0.0313(15) Uani 1 1 d . . .
H75 H 0.1644 0.6277 0.5637 0.038 Uiso 1 1 calc R . .
C76 C 0.1444(4) 0.6004(3) 0.4489(3) 0.0262(13) Uani 1 1 d . . .
H76 H 0.1560 0.5524 0.4590 0.031 Uiso 1 1 calc R . .
C11 C 0.5295(4) 0.4640(3) 0.2136(3) 0.0238(13) Uani 1 1 d . . .
C12 C 0.4360(4) 0.4241(3) 0.1674(3) 0.0231(13) Uani 1 1 d . . .
C13 C 0.4483(5) 0.3909(3) 0.1001(3) 0.0331(15) Uani 1 1 d . . .
H13 H 0.3863 0.3617 0.0713 0.040 Uiso 1 1 calc R . .
C14 C 0.5496(5) 0.3999(3) 0.0746(3) 0.0392(17) Uani 1 1 d . . .
H14 H 0.5586 0.3763 0.0293 0.047 Uiso 1 1 calc R . .
C15 C 0.6366(5) 0.4434(3) 0.1159(3) 0.0365(16) Uani 1 1 d . . .
H15 H 0.7041 0.4526 0.0969 0.044 Uiso 1 1 calc R . .
C16 C 0.6277(4) 0.4744(3) 0.1850(3) 0.0311(14) Uani 1 1 d . . .
H16 H 0.6906 0.5034 0.2134 0.037 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
Pd C 2.145(5) . ?
Pd P2 2.2791(15) . ?
Pd P1 2.3242(15) . ?
Pd Ge 2.5043(7) . ?
P1 C31 1.834(6) . ?
P1 C12 1.839(5) . ?
P1 C32 1.845(6) . ?
Ge C51 1.989(5) . ?
Ge C71 1.997(5) . ?
Ge C61 1.997(5) . ?
P2 C22 1.828(5) . ?
P2 C41 1.838(5) . ?
P2 C42 1.843(5) . ?
C C21 1.507(7) . ?
C C11 1.513(7) . ?
C H 1.0000 . ?
C21 C22 1.399(7) . ?
C21 C26 1.400(6) . ?
C22 C23 1.393(7) . ?
C23 C24 1.386(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.376(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.378(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C34 1.519(7) . ?
C31 C33 1.536(8) . ?
C31 H31 1.0000 . ?
C32 C35 1.511(7) . ?
C32 C36 1.513(7) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 C44 1.514(7) . ?
C41 C43 1.532(7) . ?
C41 H41 1.0000 . ?
C42 C45 1.534(7) . ?
C42 C46 1.539(7) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C52 1.398(7) . ?
C51 C56 1.405(7) . ?
C52 C53 1.393(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.372(7) . ?
C53 H53 0.9500 . ?
C54 C55 1.377(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.381(7) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C66 1.393(7) . ?
C61 C62 1.403(6) . ?
C62 C63 1.378(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.383(7) . ?
C63 H63 0.9500 . ?
C64 C65 1.377(7) . ?
C64 H64 0.9500 . ?
C65 C66 1.380(7) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C72 1.382(7) . ?
C71 C76 1.403(7) . ?
C72 C73 1.381(7) . ?
C72 H72 0.9500 . ?
C73 C74 1.386(8) . ?
C73 H73 0.9500 . ?
C74 C75 1.383(8) . ?
C74 H74 0.9500 . ?
C75 C76 1.395(7) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C11 C16 1.384(7) . ?
C11 C12 1.403(7) . ?
C12 C13 1.390(7) . ?
C13 C14 1.382(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.367(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

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
C Pd P2 82.89(14) . . ?
C Pd P1 80.31(14) . . ?
P2 Pd P1 159.47(5) . . ?
C Pd Ge 166.50(14) . . ?
P2 Pd Ge 100.04(4) . . ?
P1 Pd Ge 99.04(4) . . ?
C31 P1 C12 99.5(2) . . ?
C31 P1 C32 105.3(2) . . ?
C12 P1 C32 108.0(2) . . ?
C31 P1 Pd 120.6(2) . . ?
C12 P1 Pd 101.26(18) . . ?
C32 P1 Pd 119.48(18) . . ?
C51 Ge C71 103.8(2) . . ?
C51 Ge C61 104.7(2) . . ?
C71 Ge C61 97.4(2) . . ?
C51 Ge Pd 105.09(13) . . ?
C71 Ge Pd 117.19(13) . . ?
C61 Ge Pd 126.27(14) . . ?
C22 P2 C41 103.6(2) . . ?
C22 P2 C42 105.2(2) . . ?
C41 P2 C42 107.8(3) . . ?
C22 P2 Pd 105.29(18) . . ?
C41 P2 Pd 114.47(18) . . ?
C42 P2 Pd 118.97(17) . . ?
C21 C C11 114.9(4) . . ?
C21 C Pd 117.2(3) . . ?
C11 C Pd 109.8(3) . . ?
C21 C H 104.5 . . ?
C11 C H 104.5 . . ?
Pd C H 104.5 . . ?
C22 C21 C26 118.5(5) . . ?
C22 C21 C 120.4(4) . . ?
C26 C21 C 121.1(5) . . ?
C23 C22 C21 120.2(5) . . ?
C23 C22 P2 126.0(4) . . ?
C21 C22 P2 113.8(4) . . ?
C24 C23 C22 120.1(5) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 119.9(5) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.6(5) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 120.6(5) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C34 C31 C33 112.2(5) . . ?
C34 C31 P1 113.1(4) . . ?
C33 C31 P1 110.1(4) . . ?
C34 C31 H31 107.0 . . ?
C33 C31 H31 107.0 . . ?
P1 C31 H31 107.0 . . ?
C35 C32 C36 111.0(5) . . ?
C35 C32 P1 109.9(4) . . ?
C36 C32 P1 115.2(4) . . ?
C35 C32 H32 106.7 . . ?
C36 C32 H32 106.7 . . ?
P1 C32 H32 106.7 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C44 C41 C43 110.2(4) . . ?
C44 C41 P2 113.8(4) . . ?
C43 C41 P2 108.8(4) . . ?
C44 C41 H41 108.0 . . ?
C43 C41 H41 108.0 . . ?
P2 C41 H41 108.0 . . ?
C45 C42 C46 110.6(5) . . ?
C45 C42 P2 108.3(4) . . ?
C46 C42 P2 117.7(4) . . ?
C45 C42 H42 106.6 . . ?
C46 C42 H42 106.6 . . ?
P2 C42 H42 106.6 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C52 C51 C56 115.6(5) . . ?
C52 C51 Ge 120.6(4) . . ?
C56 C51 Ge 123.3(4) . . ?
C53 C52 C51 122.0(5) . . ?
C53 C52 H52 119.0 . . ?
C51 C52 H52 119.0 . . ?
C54 C53 C52 120.3(5) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C53 C54 C55 119.4(5) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
C54 C55 C56 120.3(5) . . ?
C54 C55 H55 119.9 . . ?
C56 C55 H55 119.9 . . ?
C55 C56 C51 122.3(5) . . ?
C55 C56 H56 118.8 . . ?
C51 C56 H56 118.8 . . ?
C66 C61 C62 116.9(5) . . ?
C66 C61 Ge 124.3(3) . . ?
C62 C61 Ge 118.7(4) . . ?
C63 C62 C61 121.6(5) . . ?
C63 C62 H62 119.2 . . ?
C61 C62 H62 119.2 . . ?
C62 C63 C64 120.0(5) . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C65 C64 C63 119.6(5) . . ?
C65 C64 H64 120.2 . . ?
C63 C64 H64 120.2 . . ?
C64 C65 C66 120.2(5) . . ?
C64 C65 H65 119.9 . . ?
C66 C65 H65 119.9 . . ?
C65 C66 C61 121.7(5) . . ?
C65 C66 H66 119.2 . . ?
C61 C66 H66 119.2 . . ?
C72 C71 C76 116.3(5) . . ?
C72 C71 Ge 121.0(4) . . ?
C76 C71 Ge 122.5(4) . . ?
C73 C72 C71 123.4(5) . . ?
C73 C72 H72 118.3 . . ?
C71 C72 H72 118.3 . . ?
C72 C73 C74 119.3(6) . . ?
C72 C73 H73 120.4 . . ?
C74 C73 H73 120.4 . . ?
C75 C74 C73 119.5(5) . . ?
C75 C74 H74 120.2 . . ?
C73 C74 H74 120.2 . . ?
C74 C75 C76 120.0(5) . . ?
C74 C75 H75 120.0 . . ?
C76 C75 H75 120.0 . . ?
C75 C76 C71 121.4(5) . . ?
C75 C76 H76 119.3 . . ?
C71 C76 H76 119.3 . . ?
C16 C11 C12 117.2(5) . . ?
C16 C11 C 125.4(5) . . ?
C12 C11 C 117.4(4) . . ?
C13 C12 C11 120.5(5) . . ?
C13 C12 P1 125.3(4) . . ?
C11 C12 P1 112.6(4) . . ?
C14 C13 C12 120.9(5) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C15 C14 C13 118.6(5) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C16 120.9(5) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 121.5(5) . . ?
C11 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.113
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cc275
_database_code_depnum_ccdc_archive 'CCDC 1436842'
_audit_update_record             
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C85 H114 Ge2 P6 Pd2'
_chemical_formula_weight         1679.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.5430(4)
_cell_length_b                   20.3870(10)
_cell_length_c                   21.3674(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.3602(14)
_cell_angle_gamma                90.00
_cell_volume                     4101.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9712
_cell_measurement_theta_min      2.163
_cell_measurement_theta_max      28.542

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1740
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'combination of ω- and φ-scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            98578
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7227
_reflns_number_gt                6323
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0267P)²+1.4463P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7227
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.39060(2) 0.859712(10) 0.196899(9) 0.01511(6) Uani 1 1 d . . .
Ge Ge 0.39830(3) 0.792381(15) 0.293172(14) 0.02187(8) Uani 1 1 d . . .
P1 P 0.42680(7) 0.97796(3) 0.20088(3) 0.01756(15) Uani 1 1 d . . .
P3 P 0.61304(8) 0.81877(4) 0.18838(4) 0.02506(17) Uani 1 1 d . . .
P2 P 0.24669(8) 0.81122(4) 0.10323(3) 0.02283(16) Uani 1 1 d . . .
H2 H 0.466(3) 0.7282(16) 0.2897(15) 0.038(9) Uiso 1 1 d . . .
C11 C 0.1931(3) 0.95042(13) 0.25466(12) 0.0194(6) Uani 1 1 d . . .
C12 C 0.2960(3) 0.99844(13) 0.25200(13) 0.0210(6) Uani 1 1 d . . .
C13 C 0.2955(3) 1.05516(15) 0.28847(15) 0.0315(7) Uani 1 1 d . . .
H13 H 0.3642 1.0884 0.2861 0.038 Uiso 1 1 calc R . .
C14 C 0.1955(4) 1.06328(16) 0.32810(16) 0.0401(8) Uani 1 1 d . . .
H14 H 0.1959 1.1021 0.3527 0.048 Uiso 1 1 calc R . .
C15 C 0.0955(4) 1.01549(17) 0.33215(16) 0.0388(8) Uani 1 1 d . . .
H15 H 0.0285 1.0208 0.3601 0.047 Uiso 1 1 calc R . .
C16 C 0.0936(3) 0.95982(15) 0.29524(14) 0.0280(7) Uani 1 1 d . . .
H16 H 0.0233 0.9273 0.2974 0.034 Uiso 1 1 calc R . .
C21 C 0.0931(3) 0.90973(14) 0.14624(13) 0.0199(6) Uani 1 1 d . . .
C22 C 0.1043(3) 0.87207(14) 0.09243(13) 0.0242(6) Uani 1 1 d . . .
C23 C 0.0147(3) 0.88494(18) 0.03508(14) 0.0336(8) Uani 1 1 d . . .
H23 H 0.0192 0.8578 -0.0007 0.040 Uiso 1 1 calc R . .
C24 C -0.0796(3) 0.93640(19) 0.02990(16) 0.0397(9) Uani 1 1 d . . .
H24 H -0.1391 0.9450 -0.0093 0.048 Uiso 1 1 calc R . .
C25 C -0.0872(3) 0.97504(17) 0.08147(16) 0.0367(8) Uani 1 1 d . . .
H25 H -0.1507 1.0112 0.0776 0.044 Uiso 1 1 calc R . .
C26 C -0.0026(3) 0.96193(15) 0.13977(15) 0.0267(7) Uani 1 1 d . . .
H26 H -0.0104 0.9888 0.1754 0.032 Uiso 1 1 calc R . .
C31 C 0.7607(3) 0.83655(18) 0.25135(16) 0.0378(8) Uani 1 1 d . . .
H31A H 0.8459 0.8138 0.2427 0.057 Uiso 1 1 calc R . .
H31B H 0.7374 0.8216 0.2920 0.057 Uiso 1 1 calc R . .
H31C H 0.7783 0.8839 0.2532 0.057 Uiso 1 1 calc R . .
C81 C 0.0000 1.0000 0.5000 0.081(3) Uani 1 2 d S . .
C82 C 0.1247(10) 0.9855(8) 0.5180(6) 0.102(4) Uani 0.50 1 d P . .
C84 C -0.2110(12) 1.0573(4) 0.4993(5) 0.162(4) Uani 1 1 d . . .
C83 C -0.049(3) 1.0496(13) 0.5191(7) 0.180(12) Uani 0.50 1 d P . .
C32 C 0.6339(4) 0.73049(16) 0.18152(19) 0.0421(9) Uani 1 1 d . . .
H32A H 0.5662 0.7141 0.1454 0.063 Uiso 1 1 calc R . .
H32B H 0.6157 0.7092 0.2205 0.063 Uiso 1 1 calc R . .
H32C H 0.7309 0.7206 0.1749 0.063 Uiso 1 1 calc R . .
C C 0.1833(3) 0.89286(13) 0.21004(12) 0.0169(5) Uani 1 1 d . . .
H1 H 0.1356 0.8561 0.2293 0.020 Uiso 1 1 calc R . .
C41 C 0.5851(3) 1.02448(14) 0.24120(14) 0.0268(7) Uani 1 1 d . . .
H41 H 0.5563 1.0714 0.2442 0.032 Uiso 1 1 calc R . .
C33 C 0.6841(3) 0.84623(17) 0.11840(16) 0.0352(8) Uani 1 1 d . . .
H33A H 0.6273 0.8276 0.0802 0.053 Uiso 1 1 calc R . .
H33B H 0.7828 0.8316 0.1215 0.053 Uiso 1 1 calc R . .
H33C H 0.6803 0.8942 0.1160 0.053 Uiso 1 1 calc R . .
C43 C 0.6305(3) 0.99882(16) 0.30876(15) 0.0358(8) Uani 1 1 d . . .
H43A H 0.6462 0.9514 0.3075 0.054 Uiso 1 1 calc R . .
H43B H 0.5558 1.0081 0.3340 0.054 Uiso 1 1 calc R . .
H43C H 0.7187 1.0206 0.3280 0.054 Uiso 1 1 calc R . .
C44 C 0.7078(3) 1.02243(16) 0.20422(16) 0.0358(8) Uani 1 1 d . . .
H44A H 0.7248 0.9770 0.1925 0.054 Uiso 1 1 calc R . .
H44B H 0.7933 1.0400 0.2305 0.054 Uiso 1 1 calc R . .
H44C H 0.6845 1.0490 0.1657 0.054 Uiso 1 1 calc R . .
C45 C 0.3567(4) 1.10018(15) 0.13565(16) 0.0363(8) Uani 1 1 d . . .
H45A H 0.3097 1.1201 0.0960 0.054 Uiso 1 1 calc R . .
H45B H 0.4535 1.1174 0.1463 0.054 Uiso 1 1 calc R . .
H45C H 0.3032 1.1107 0.1698 0.054 Uiso 1 1 calc R . .
C46 C 0.4417(3) 1.00812(16) 0.07363(14) 0.0328(7) Uani 1 1 d . . .
H46A H 0.3895 1.0248 0.0335 0.049 Uiso 1 1 calc R . .
H46B H 0.4500 0.9603 0.0712 0.049 Uiso 1 1 calc R . .
H46C H 0.5368 1.0277 0.0815 0.049 Uiso 1 1 calc R . .
C51 C 0.1484(3) 0.73868(15) 0.12805(15) 0.0325(7) Uani 1 1 d . . .
H51 H 0.1080 0.7537 0.1660 0.039 Uiso 1 1 calc R . .
C52 C 0.2702(4) 0.79272(17) 0.02012(14) 0.0366(8) Uani 1 1 d . . .
H52 H 0.1750 0.7813 -0.0044 0.044 Uiso 1 1 calc R . .
C53 C 0.0207(4) 0.71724(19) 0.07968(18) 0.0485(10) Uani 1 1 d . . .
H53A H -0.0386 0.7555 0.0659 0.073 Uiso 1 1 calc R . .
H53B H -0.0351 0.6850 0.0992 0.073 Uiso 1 1 calc R . .
H53C H 0.0539 0.6975 0.0429 0.073 Uiso 1 1 calc R . .
C54 C 0.2454(4) 0.68061(16) 0.15130(17) 0.0418(8) Uani 1 1 d . . .
H54A H 0.2817 0.6609 0.1153 0.063 Uiso 1 1 calc R . .
H54B H 0.1912 0.6477 0.1708 0.063 Uiso 1 1 calc R . .
H54C H 0.3251 0.6961 0.1826 0.063 Uiso 1 1 calc R . .
C55 C 0.3685(5) 0.73486(19) 0.01586(18) 0.0532(10) Uani 1 1 d . . .
H55A H 0.3848 0.7299 -0.0280 0.080 Uiso 1 1 calc R . .
H55B H 0.3247 0.6948 0.0292 0.080 Uiso 1 1 calc R . .
H55C H 0.4592 0.7425 0.0437 0.080 Uiso 1 1 calc R . .
C56 C 0.3253(4) 0.85273(19) -0.01128(15) 0.0431(9) Uani 1 1 d . . .
H56A H 0.3225 0.8441 -0.0566 0.065 Uiso 1 1 calc R . .
H56B H 0.4233 0.8618 0.0086 0.065 Uiso 1 1 calc R . .
H56C H 0.2654 0.8907 -0.0060 0.065 Uiso 1 1 calc R . .
C61 C 0.2199(3) 0.76284(14) 0.32178(13) 0.0244(6) Uani 1 1 d . . .
C62 C 0.1658(4) 0.70062(17) 0.30742(17) 0.0406(8) Uani 1 1 d . . .
H62 H 0.2134 0.6722 0.2825 0.049 Uiso 1 1 calc R . .
C63 C 0.0435(4) 0.67861(19) 0.32856(19) 0.0496(10) Uani 1 1 d . . .
H63 H 0.0085 0.6357 0.3179 0.060 Uiso 1 1 calc R . .
C64 C -0.0261(3) 0.71854(19) 0.36455(17) 0.0422(9) Uani 1 1 d . . .
H64 H -0.1092 0.7034 0.3792 0.051 Uiso 1 1 calc R . .
C65 C 0.0244(3) 0.78078(18) 0.37959(16) 0.0372(8) Uani 1 1 d . . .
H65 H -0.0240 0.8088 0.4044 0.045 Uiso 1 1 calc R . .
C66 C 0.1466(3) 0.80241(15) 0.35833(14) 0.0286(7) Uani 1 1 d . . .
H66 H 0.1808 0.8454 0.3691 0.034 Uiso 1 1 calc R . .
C71 C 0.5084(3) 0.82604(18) 0.37222(14) 0.0343(8) Uani 1 1 d . . .
C72 C 0.6200(4) 0.7876(2) 0.40476(17) 0.0532(11) Uani 1 1 d . . .
H72 H 0.6408 0.7464 0.3875 0.064 Uiso 1 1 calc R . .
C73 C 0.6991(5) 0.8081(3) 0.4606(2) 0.0801(9) Uani 1 1 d . . .
H73 H 0.7740 0.7817 0.4820 0.096 Uiso 1 1 calc R . .
C74 C 0.6687(5) 0.8665(3) 0.4848(2) 0.0801(9) Uani 1 1 d . . .
H74 H 0.7237 0.8810 0.5234 0.096 Uiso 1 1 calc R . .
C75 C 0.5595(5) 0.9061(3) 0.4551(2) 0.0801(9) Uani 1 1 d . . .
H75 H 0.5395 0.9468 0.4733 0.096 Uiso 1 1 calc R . .
C76 C 0.4790(4) 0.8852(2) 0.39767(17) 0.0493(10) Uani 1 1 d . . .
H76 H 0.4044 0.9119 0.3766 0.059 Uiso 1 1 calc R . .
C42 C 0.3623(3) 1.02607(14) 0.12759(13) 0.0225(6) Uani 1 1 d . . .
H42 H 0.2619 1.0119 0.1134 0.027 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
Pd C 2.151(2) . ?
Pd P3 2.3155(7) . ?
Pd P1 2.4349(7) . ?
Pd P2 2.4444(7) . ?
Pd Ge 2.4642(4) . ?
Ge C71 1.962(3) . ?
Ge C61 1.994(3) . ?
Ge H2 1.47(3) . ?
P1 C12 1.835(3) . ?
P1 C42 1.865(3) . ?
P1 C41 1.871(3) . ?
P3 C32 1.819(3) . ?
P3 C31 1.819(3) . ?
P3 C33 1.827(3) . ?
P2 C22 1.827(3) . ?
P2 C52 1.864(3) . ?
P2 C51 1.873(3) . ?
C11 C12 1.394(4) . ?
C11 C16 1.400(4) . ?
C11 C 1.505(4) . ?
C12 C13 1.395(4) . ?
C13 C14 1.385(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.381(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.395(4) . ?
C21 C22 1.401(4) . ?
C21 C 1.529(4) . ?
C22 C23 1.400(4) . ?
C23 C24 1.375(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.366(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.395(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C81 C83 1.21(3) 3_576 ?
C81 C83 1.21(3) . ?
C81 C82 1.226(11) . ?
C81 C82 1.226(10) 3_576 ?
C82 C83 1.216(18) 3_576 ?
C82 C84 1.295(14) 3_576 ?
C84 C82 1.295(14) 3_576 ?
C84 C83 1.55(3) . ?
C83 C82 1.216(18) 3_576 ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C H1 1.0000 . ?
C41 C44 1.516(4) . ?
C41 C43 1.530(4) . ?
C41 H41 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C42 1.523(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C42 1.524(4) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C53 1.528(4) . ?
C51 C54 1.535(5) . ?
C51 H51 1.0000 . ?
C52 C55 1.518(5) . ?
C52 C56 1.529(5) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C61 C62 1.385(4) . ?
C61 C66 1.388(4) . ?
C62 C63 1.392(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.364(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.377(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.390(4) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C76 1.371(5) . ?
C71 C72 1.411(5) . ?
C72 C73 1.370(6) . ?
C72 H72 0.9500 . ?
C73 C74 1.348(7) . ?
C73 H73 0.9500 . ?
C74 C75 1.388(7) . ?
C74 H74 0.9500 . ?
C75 C76 1.404(5) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C42 H42 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C Pd P3 175.99(7) . . ?
C Pd P1 79.20(7) . . ?
P3 Pd P1 103.47(3) . . ?
C Pd P2 80.09(7) . . ?
P3 Pd P2 100.95(3) . . ?
P1 Pd P2 119.12(3) . . ?
C Pd Ge 88.24(7) . . ?
P3 Pd Ge 87.80(2) . . ?
P1 Pd Ge 122.52(2) . . ?
P2 Pd Ge 113.25(2) . . ?
C71 Ge C61 101.91(12) . . ?
C71 Ge Pd 117.57(10) . . ?
C61 Ge Pd 120.88(8) . . ?
C71 Ge H2 100.3(12) . . ?
C61 Ge H2 98.5(12) . . ?
Pd Ge H2 114.2(12) . . ?
C12 P1 C42 102.51(12) . . ?
C12 P1 C41 100.77(13) . . ?
C42 P1 C41 104.56(13) . . ?
C12 P1 Pd 98.03(9) . . ?
C42 P1 Pd 117.76(9) . . ?
C41 P1 Pd 128.12(10) . . ?
C32 P3 C31 100.08(17) . . ?
C32 P3 C33 100.20(16) . . ?
C31 P3 C33 101.43(16) . . ?
C32 P3 Pd 118.46(12) . . ?
C31 P3 Pd 118.66(11) . . ?
C33 P3 Pd 114.89(11) . . ?
C22 P2 C52 102.68(15) . . ?
C22 P2 C51 100.10(14) . . ?
C52 P2 C51 104.68(15) . . ?
C22 P2 Pd 97.82(9) . . ?
C52 P2 Pd 136.30(11) . . ?
C51 P2 Pd 109.14(10) . . ?
C12 C11 C16 118.8(3) . . ?
C12 C11 C 119.6(2) . . ?
C16 C11 C 121.4(3) . . ?
C11 C12 C13 119.5(3) . . ?
C11 C12 P1 114.6(2) . . ?
C13 C12 P1 125.8(2) . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 120.5(3) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.4(3) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C11 121.3(3) . . ?
C15 C16 H16 119.4 . . ?
C11 C16 H16 119.4 . . ?
C26 C21 C22 118.2(3) . . ?
C26 C21 C 121.7(3) . . ?
C22 C21 C 120.1(2) . . ?
C23 C22 C21 119.9(3) . . ?
C23 C22 P2 125.0(2) . . ?
C21 C22 P2 115.0(2) . . ?
C24 C23 C22 120.8(3) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.7(3) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 120.6(3) . . ?
C21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
P3 C31 H31A 109.5 . . ?
P3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
P3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C83 C81 C83 180.0(13) 3_576 . ?
C83 C81 C82 59.9(10) 3_576 . ?
C83 C81 C82 120.1(10) . . ?
C83 C81 C82 120.1(10) 3_576 3_576 ?
C83 C81 C82 59.9(10) . 3_576 ?
C82 C81 C82 180.000(4) . 3_576 ?
C83 C82 C81 59.4(16) 3_576 . ?
C83 C82 C84 75.9(17) 3_576 3_576 ?
C81 C82 C84 134.7(13) . 3_576 ?
C82 C84 C83 49.7(10) 3_576 . ?
C81 C83 C82 60.7(12) . 3_576 ?
C81 C83 C84 114.6(13) . . ?
C82 C83 C84 54.3(12) 3_576 . ?
P3 C32 H32A 109.5 . . ?
P3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
P3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C11 C C21 111.0(2) . . ?
C11 C Pd 111.33(17) . . ?
C21 C Pd 110.53(17) . . ?
C11 C H1 108.0 . . ?
C21 C H1 108.0 . . ?
Pd C H1 108.0 . . ?
C44 C41 C43 111.0(3) . . ?
C44 C41 P1 112.4(2) . . ?
C43 C41 P1 110.2(2) . . ?
C44 C41 H41 107.7 . . ?
C43 C41 H41 107.7 . . ?
P1 C41 H41 107.7 . . ?
P3 C33 H33A 109.5 . . ?
P3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
P3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C53 C51 C54 111.8(3) . . ?
C53 C51 P2 114.5(2) . . ?
C54 C51 P2 113.4(2) . . ?
C53 C51 H51 105.4 . . ?
C54 C51 H51 105.4 . . ?
P2 C51 H51 105.4 . . ?
C55 C52 C56 109.6(3) . . ?
C55 C52 P2 112.7(2) . . ?
C56 C52 P2 111.1(2) . . ?
C55 C52 H52 107.8 . . ?
C56 C52 H52 107.8 . . ?
P2 C52 H52 107.8 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 C56 H56A 109.5 . . ?
C52 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C52 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C62 C61 C66 117.0(3) . . ?
C62 C61 Ge 121.0(2) . . ?
C66 C61 Ge 122.0(2) . . ?
C61 C62 C63 121.7(3) . . ?
C61 C62 H62 119.2 . . ?
C63 C62 H62 119.2 . . ?
C64 C63 C62 120.1(3) . . ?
C64 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
C63 C64 C65 119.8(3) . . ?
C63 C64 H64 120.1 . . ?
C65 C64 H64 120.1 . . ?
C64 C65 C66 119.8(3) . . ?
C64 C65 H65 120.1 . . ?
C66 C65 H65 120.1 . . ?
C61 C66 C65 121.7(3) . . ?
C61 C66 H66 119.1 . . ?
C65 C66 H66 119.1 . . ?
C76 C71 C72 118.7(3) . . ?
C76 C71 Ge 122.2(3) . . ?
C72 C71 Ge 119.0(3) . . ?
C73 C72 C71 121.6(5) . . ?
C73 C72 H72 119.2 . . ?
C71 C72 H72 119.2 . . ?
C74 C73 C72 118.7(5) . . ?
C74 C73 H73 120.6 . . ?
C72 C73 H73 120.6 . . ?
C73 C74 C75 122.1(5) . . ?
C73 C74 H74 119.0 . . ?
C75 C74 H74 119.0 . . ?
C74 C75 C76 119.1(5) . . ?
C74 C75 H75 120.4 . . ?
C76 C75 H75 120.4 . . ?
C71 C76 C75 119.7(4) . . ?
C71 C76 H76 120.1 . . ?
C75 C76 H76 120.1 . . ?
C45 C42 C46 110.8(2) . . ?
C45 C42 P1 116.1(2) . . ?
C46 C42 P1 111.8(2) . . ?
C45 C42 H42 105.8 . . ?
C46 C42 H42 105.8 . . ?
P1 C42 H42 105.8 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.068


