# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_cc218c
_database_code_depnum_ccdc_archive 'CCDC 1002269'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H154 I4 O P8 Pd4'
_chemical_formula_weight         2601.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_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                   16.2343(6)
_cell_length_b                   15.9423(6)
_cell_length_c                   20.8753(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.7040(14)
_cell_angle_gamma                90.00
_cell_volume                     5384.6(4)
_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          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2604
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6774
_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  ?
_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            131164
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9479
_reflns_number_gt                8389
_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)+(0.0368P)²+0.1221P] 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         9479
_refine_ls_number_parameters     477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_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
C1 C 0.33153(19) 0.1629(2) 0.26023(15) 0.0176(7) Uani 1 1 d . . .
I1 I 0.124228(14) 0.164057(15) 0.083611(11) 0.02900(7) Uani 1 1 d . . .
Pd1 Pd 0.228688(15) 0.161018(15) 0.190196(11) 0.01728(7) Uani 1 1 d . . .
C2 C 0.65139(19) 0.1826(2) 0.16751(15) 0.0186(7) Uani 1 1 d . . .
I2 I 0.667193(14) 0.277488(14) -0.045750(10) 0.02406(7) Uani 1 1 d . . .
Pd2 Pd 0.661429(14) 0.222172(15) 0.075380(11) 0.01620(7) Uani 1 1 d . . .
P11 P 0.23227(5) 0.01697(5) 0.21072(4) 0.01856(17) Uani 1 1 d . . .
O9 O 1.0000 0.5000 0.0000 0.0658(14) Uani 1 2 d S . .
C11 C 0.31086(19) 0.1016(2) 0.31291(15) 0.0190(7) Uani 1 1 d . . .
P12 P 0.21527(5) 0.29868(6) 0.21480(4) 0.02249(19) Uani 1 1 d . . .
C12 C 0.27613(19) 0.0236(2) 0.29410(15) 0.0206(7) Uani 1 1 d . . .
C13 C 0.2660(2) -0.0388(2) 0.33990(16) 0.0248(7) Uani 1 1 d . . .
H13 H 0.2459 -0.0925 0.3265 0.030 Uiso 1 1 calc R . .
C14 C 0.2852(2) -0.0230(2) 0.40492(17) 0.0268(8) Uani 1 1 d . . .
H14 H 0.2786 -0.0655 0.4360 0.032 Uiso 1 1 calc R . .
C15 C 0.3137(2) 0.0553(2) 0.42348(17) 0.0284(8) Uani 1 1 d . . .
H15 H 0.3244 0.0676 0.4679 0.034 Uiso 1 1 calc R . .
C16 C 0.3272(2) 0.1167(2) 0.37838(16) 0.0238(7) Uani 1 1 d . . .
H16 H 0.3479 0.1699 0.3924 0.029 Uiso 1 1 calc R . .
P21 P 0.52317(5) 0.24298(5) 0.07745(4) 0.01620(7) Uani 1 1 d . . .
C21 C 0.3566(2) 0.2511(2) 0.28317(15) 0.0195(7) Uani 1 1 d . . .
P22 P 0.79370(5) 0.16841(6) 0.09114(4) 0.01907(18) Uani 1 1 d . . .
C22 C 0.3109(2) 0.3221(2) 0.26250(16) 0.0232(7) Uani 1 1 d . . .
C26 C 0.4284(2) 0.2652(2) 0.32375(15) 0.0222(7) Uani 1 1 d . . .
H26 H 0.4605 0.2184 0.3392 0.027 Uiso 1 1 calc R . .
C25 C 0.4539(2) 0.3450(2) 0.34195(16) 0.0278(8) Uani 1 1 d . . .
H25 H 0.5030 0.3526 0.3693 0.033 Uiso 1 1 calc R . .
C24 C 0.4079(3) 0.4141(2) 0.32028(18) 0.0333(9) Uani 1 1 d . . .
H24 H 0.4254 0.4691 0.3324 0.040 Uiso 1 1 calc R . .
C23 C 0.3364(2) 0.4023(2) 0.28094(17) 0.0305(8) Uani 1 1 d . . .
H23 H 0.3044 0.4495 0.2663 0.037 Uiso 1 1 calc R . .
C31 C 0.1304(2) -0.0329(3) 0.2190(2) 0.0368(5) Uani 1 1 d . . .
H31 H 0.1403 -0.0857 0.2443 0.044 Uiso 1 1 calc R . .
C32 C 0.2875(2) -0.0652(2) 0.16639(18) 0.0312(5) Uani 1 1 d . . .
H32 H 0.2449 -0.1080 0.1523 0.037 Uiso 1 1 calc R . .
C33 C 0.0769(2) 0.0241(3) 0.2566(2) 0.0368(5) Uani 1 1 d . . .
H33A H 0.0654 0.0761 0.2325 0.055 Uiso 1 1 calc R . .
H33B H 0.1060 0.0373 0.2984 0.055 Uiso 1 1 calc R . .
H33C H 0.0247 -0.0043 0.2632 0.055 Uiso 1 1 calc R . .
C94 C 0.9289(18) 0.5887(19) 0.0616(15) 0.108(10) Uani 0.540(14) 1 d P A 2
H94A H 0.9791 0.6229 0.0679 0.162 Uiso 0.540(14) 1 calc PR A 2
H94B H 0.9260 0.5506 0.0981 0.162 Uiso 0.540(14) 1 calc PR A 2
H94C H 0.8803 0.6253 0.0583 0.162 Uiso 0.540(14) 1 calc PR A 2
C95 C 1.0890(15) 0.3932(19) -0.0434(16) 0.065(6) Uani 0.460(14) 1 d P A 1
H95A H 1.0917 0.3604 -0.0829 0.078 Uiso 0.460(14) 1 calc PR A 1
H95B H 1.0887 0.3551 -0.0065 0.078 Uiso 0.460(14) 1 calc PR A 1
H95C H 1.1371 0.4303 -0.0377 0.078 Uiso 0.460(14) 1 calc PR A 1
C93 C 0.9310(7) 0.5430(7) 0.0062(6) 0.069(4) Uani 0.540(14) 1 d P A 2
H93A H 0.8841 0.5031 0.0037 0.083 Uiso 0.540(14) 1 calc PR A 2
H93B H 0.9222 0.5817 -0.0308 0.083 Uiso 0.540(14) 1 calc PR A 2
C92 C 1.0090(7) 0.4463(7) -0.0482(5) 0.049(4) Uani 0.460(14) 1 d P A 1
H92A H 1.0068 0.4787 -0.0888 0.058 Uiso 0.460(14) 1 calc PR A 1
H92B H 0.9612 0.4076 -0.0512 0.058 Uiso 0.460(14) 1 calc PR A 1
C34 C 0.0857(2) -0.0566(3) 0.1540(2) 0.0368(5) Uani 1 1 d . . .
H34A H 0.0785 -0.0064 0.1270 0.055 Uiso 1 1 calc R . .
H34B H 0.0314 -0.0804 0.1608 0.055 Uiso 1 1 calc R . .
H34C H 0.1185 -0.0981 0.1326 0.055 Uiso 1 1 calc R . .
C35 C 0.3185(2) -0.0296(2) 0.10504(17) 0.0312(5) Uani 1 1 d . . .
H35A H 0.3343 -0.0758 0.0776 0.047 Uiso 1 1 calc R . .
H35B H 0.3666 0.0063 0.1160 0.047 Uiso 1 1 calc R . .
H35C H 0.2746 0.0035 0.0821 0.047 Uiso 1 1 calc R . .
C36 C 0.3536(2) -0.1114(2) 0.20680(18) 0.0312(5) Uani 1 1 d . . .
H36A H 0.3748 -0.1575 0.1817 0.047 Uiso 1 1 calc R . .
H36B H 0.3304 -0.1342 0.2450 0.047 Uiso 1 1 calc R . .
H36C H 0.3989 -0.0728 0.2200 0.047 Uiso 1 1 calc R . .
C43 C 0.1484(3) 0.2641(3) 0.3310(2) 0.0420(6) Uani 1 1 d . . .
H43A H 0.1490 0.2046 0.3192 0.063 Uiso 1 1 calc R . .
H43B H 0.1041 0.2743 0.3592 0.063 Uiso 1 1 calc R . .
H43C H 0.2017 0.2792 0.3535 0.063 Uiso 1 1 calc R . .
C42 C 0.1923(3) 0.3773(3) 0.1509(2) 0.0377(5) Uani 1 1 d . . .
H42 H 0.1434 0.3549 0.1239 0.045 Uiso 1 1 calc R . .
C41 C 0.1338(3) 0.3170(3) 0.2707(2) 0.0420(6) Uani 1 1 d . . .
H41 H 0.1366 0.3773 0.2839 0.050 Uiso 1 1 calc R . .
C44 C 0.0489(3) 0.3012(3) 0.2365(2) 0.0420(6) Uani 1 1 d . . .
H44A H 0.0387 0.3417 0.2014 0.063 Uiso 1 1 calc R . .
H44B H 0.0066 0.3076 0.2670 0.063 Uiso 1 1 calc R . .
H44C H 0.0467 0.2441 0.2189 0.063 Uiso 1 1 calc R . .
C46 C 0.2626(2) 0.3799(3) 0.1068(2) 0.0377(5) Uani 1 1 d . . .
H46A H 0.2739 0.3230 0.0921 0.057 Uiso 1 1 calc R . .
H46B H 0.3122 0.4028 0.1303 0.057 Uiso 1 1 calc R . .
H46C H 0.2467 0.4156 0.0696 0.057 Uiso 1 1 calc R . .
C45 C 0.1684(3) 0.4648(2) 0.1697(2) 0.0377(5) Uani 1 1 d . . .
H45A H 0.1502 0.4968 0.1310 0.057 Uiso 1 1 calc R . .
H45B H 0.2162 0.4927 0.1921 0.057 Uiso 1 1 calc R . .
H45C H 0.1233 0.4619 0.1981 0.057 Uiso 1 1 calc R . .
C54 C 0.40429(19) 0.1232(2) 0.22377(15) 0.0174(6) Uani 1 1 d . . .
H54 H 0.3823 0.0682 0.2069 0.021 Uiso 1 1 calc R . .
C55 C 0.48277(19) 0.1020(2) 0.26418(15) 0.0178(7) Uani 1 1 d . . .
H55 H 0.4777 0.0750 0.3042 0.021 Uiso 1 1 calc R . .
C56 C 0.5591(2) 0.1184(2) 0.24773(15) 0.0198(7) Uani 1 1 d . . .
H56 H 0.6049 0.1007 0.2758 0.024 Uiso 1 1 calc R . .
C61 C 0.7302(2) 0.1756(2) 0.20820(15) 0.0208(7) Uani 1 1 d . . .
C62 C 0.8043(2) 0.1615(2) 0.17839(16) 0.0230(7) Uani 1 1 d . . .
C63 C 0.8796(2) 0.1527(2) 0.21527(17) 0.0282(8) Uani 1 1 d . . .
H63 H 0.9283 0.1403 0.1949 0.034 Uiso 1 1 calc R . .
C64 C 0.8836(2) 0.1621(3) 0.28144(18) 0.0326(9) Uani 1 1 d . . .
H64 H 0.9348 0.1553 0.3064 0.039 Uiso 1 1 calc R . .
C65 C 0.8124(2) 0.1815(3) 0.31108(17) 0.0300(8) Uani 1 1 d . . .
H65 H 0.8154 0.1907 0.3562 0.036 Uiso 1 1 calc R . .
C66 C 0.7373(2) 0.1873(2) 0.27527(16) 0.0244(7) Uani 1 1 d . . .
H66 H 0.6891 0.1997 0.2964 0.029 Uiso 1 1 calc R . .
C71 C 0.4632(2) 0.1953(2) 0.00745(16) 0.0224(4) Uani 1 1 d . . .
H71 H 0.4834 0.2221 -0.0317 0.027 Uiso 1 1 calc R . .
C72 C 0.47774(19) 0.3463(2) 0.08870(14) 0.01620(7) Uani 1 1 d . . .
H72 H 0.4166 0.3386 0.0889 0.019 Uiso 1 1 calc R . .
C73 C 0.3694(2) 0.2063(2) 0.00217(16) 0.0224(4) Uani 1 1 d . . .
H73A H 0.3559 0.2658 0.0068 0.034 Uiso 1 1 calc R . .
H73B H 0.3459 0.1740 0.0362 0.034 Uiso 1 1 calc R . .
H73C H 0.3463 0.1861 -0.0399 0.034 Uiso 1 1 calc R . .
C74 C 0.4863(2) 0.1024(2) 0.00464(16) 0.0224(4) Uani 1 1 d . . .
H74A H 0.4559 0.0762 -0.0327 0.034 Uiso 1 1 calc R . .
H74B H 0.4719 0.0743 0.0440 0.034 Uiso 1 1 calc R . .
H74C H 0.5458 0.0970 0.0008 0.034 Uiso 1 1 calc R . .
C75 C 0.49276(18) 0.4059(2) 0.03365(14) 0.01620(7) Uani 1 1 d . . .
H75A H 0.4735 0.3797 -0.0073 0.024 Uiso 1 1 calc R . .
H75B H 0.5520 0.4179 0.0340 0.024 Uiso 1 1 calc R . .
H75C H 0.4625 0.4583 0.0389 0.024 Uiso 1 1 calc R . .
C76 C 0.50863(18) 0.3843(2) 0.15335(14) 0.01620(7) Uani 1 1 d . . .
H76A H 0.5684 0.3938 0.1544 0.024 Uiso 1 1 calc R . .
H76B H 0.4968 0.3458 0.1880 0.024 Uiso 1 1 calc R . .
H76C H 0.4805 0.4379 0.1592 0.024 Uiso 1 1 calc R . .
C81 C 0.8056(2) 0.0622(2) 0.0581(2) 0.0332(5) Uani 1 1 d . . .
H81 H 0.8035 0.0678 0.0103 0.040 Uiso 1 1 calc R . .
C82 C 0.8875(2) 0.2260(2) 0.07079(19) 0.0321(5) Uani 1 1 d . . .
H82 H 0.9360 0.1996 0.0957 0.039 Uiso 1 1 calc R . .
C83 C 0.7333(2) 0.0070(2) 0.07329(19) 0.0332(5) Uani 1 1 d . . .
H83A H 0.6814 0.0331 0.0562 0.050 Uiso 1 1 calc R . .
H83B H 0.7331 0.0006 0.1200 0.050 Uiso 1 1 calc R . .
H83C H 0.7388 -0.0482 0.0535 0.050 Uiso 1 1 calc R . .
C84 C 0.8881(2) 0.0195(2) 0.08015(19) 0.0332(5) Uani 1 1 d . . .
H84A H 0.8918 -0.0345 0.0582 0.050 Uiso 1 1 calc R . .
H84B H 0.8911 0.0104 0.1267 0.050 Uiso 1 1 calc R . .
H84C H 0.9340 0.0555 0.0696 0.050 Uiso 1 1 calc R . .
C85 C 0.9016(2) 0.2189(2) -0.00022(19) 0.0321(5) Uani 1 1 d . . .
H85A H 0.8529 0.2398 -0.0262 0.048 Uiso 1 1 calc R . .
H85B H 0.9110 0.1600 -0.0110 0.048 Uiso 1 1 calc R . .
H85C H 0.9500 0.2523 -0.0092 0.048 Uiso 1 1 calc R . .
C86 C 0.8834(2) 0.3164(2) 0.09231(19) 0.0321(5) Uani 1 1 d . . .
H86A H 0.9344 0.3454 0.0834 0.048 Uiso 1 1 calc R . .
H86B H 0.8769 0.3184 0.1386 0.048 Uiso 1 1 calc R . .
H86C H 0.8361 0.3441 0.0689 0.048 Uiso 1 1 calc R . .
C53 C 0.42313(19) 0.17205(19) 0.16555(15) 0.0172(6) Uani 1 1 d . . .
H53 H 0.3782 0.1946 0.1390 0.021 Uiso 1 1 calc R . .
C52 C 0.50027(19) 0.18573(19) 0.14881(14) 0.0160(6) Uani 1 1 d . . .
C51 C 0.5754(2) 0.16236(19) 0.18845(15) 0.0174(7) 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
C1 C11 1.529(4) . ?
C1 C21 1.530(4) . ?
C1 C54 1.588(4) . ?
C1 Pd1 2.127(3) . ?
I1 Pd1 2.6851(3) . ?
Pd1 P12 2.2686(9) . ?
Pd1 P11 2.3359(9) . ?
C2 C51 1.380(4) . ?
C2 C61 1.481(4) . ?
C2 Pd2 2.043(3) . ?
I2 Pd2 2.6868(3) . ?
Pd2 P21 2.2728(8) . ?
Pd2 P22 2.3104(9) . ?
P11 C12 1.829(3) . ?
P11 C31 1.855(4) . ?
P11 C32 1.874(4) . ?
O9 C93 1.329(11) 3_765 ?
O9 C93 1.329(11) . ?
O9 C92 1.338(11) 3_765 ?
O9 C92 1.338(11) . ?
C11 C16 1.392(5) . ?
C11 C12 1.409(5) . ?
P12 C22 1.813(4) . ?
P12 C42 1.846(4) . ?
P12 C41 1.857(4) . ?
C12 C13 1.398(5) . ?
C13 C14 1.390(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
P21 C52 1.811(3) . ?
P21 C72 1.828(3) . ?
P21 C71 1.851(3) . ?
C21 C22 1.402(5) . ?
C21 C26 1.402(5) . ?
P22 C62 1.819(3) . ?
P22 C81 1.844(4) . ?
P22 C82 1.856(4) . ?
C22 C23 1.389(5) . ?
C26 C25 1.383(5) . ?
C26 H26 0.9500 . ?
C25 C24 1.386(5) . ?
C25 H25 0.9500 . ?
C24 C23 1.378(6) . ?
C24 H24 0.9500 . ?
C23 H23 0.9500 . ?
C31 C33 1.520(6) . ?
C31 C34 1.534(6) . ?
C31 H31 1.0000 . ?
C32 C36 1.503(5) . ?
C32 C35 1.523(5) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C94 C93 1.37(4) . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
C95 C92 1.55(3) . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
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 . ?
C43 C41 1.517(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C42 C45 1.509(6) . ?
C42 C46 1.524(5) . ?
C42 H42 1.0000 . ?
C41 C44 1.522(6) . ?
C41 H41 1.0000 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C54 C53 1.496(4) . ?
C54 C55 1.508(4) . ?
C54 H54 1.0000 . ?
C55 C56 1.339(4) . ?
C55 H55 0.9500 . ?
C56 C51 1.465(4) . ?
C56 H56 0.9500 . ?
C61 C66 1.408(5) . ?
C61 C62 1.418(5) . ?
C62 C63 1.396(5) . ?
C63 C64 1.385(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.390(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.380(5) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C73 1.528(5) . ?
C71 C74 1.531(5) . ?
C71 H71 1.0000 . ?
C72 C75 1.526(4) . ?
C72 C76 1.526(4) . ?
C72 H72 1.0000 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C81 C83 1.522(5) . ?
C81 C84 1.539(5) . ?
C81 H81 1.0000 . ?
C82 C86 1.513(6) . ?
C82 C85 1.523(5) . ?
C82 H82 1.0000 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C53 C52 1.345(4) . ?
C53 H53 0.9500 . ?
C52 C51 1.465(4) . ?

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
C11 C1 C21 115.5(3) . . ?
C11 C1 C54 107.8(2) . . ?
C21 C1 C54 109.1(3) . . ?
C11 C1 Pd1 106.2(2) . . ?
C21 C1 Pd1 113.7(2) . . ?
C54 C1 Pd1 103.74(19) . . ?
C1 Pd1 P12 85.13(9) . . ?
C1 Pd1 P11 83.20(9) . . ?
P12 Pd1 P11 155.64(3) . . ?
C1 Pd1 I1 167.42(8) . . ?
P12 Pd1 I1 95.99(2) . . ?
P11 Pd1 I1 100.04(2) . . ?
C51 C2 C61 123.6(3) . . ?
C51 C2 Pd2 120.8(2) . . ?
C61 C2 Pd2 115.6(2) . . ?
C2 Pd2 P21 82.65(9) . . ?
C2 Pd2 P22 84.06(9) . . ?
P21 Pd2 P22 163.58(3) . . ?
C2 Pd2 I2 177.19(9) . . ?
P21 Pd2 I2 94.63(2) . . ?
P22 Pd2 I2 98.75(2) . . ?
C12 P11 C31 102.49(17) . . ?
C12 P11 C32 110.21(16) . . ?
C31 P11 C32 102.30(18) . . ?
C12 P11 Pd1 96.89(11) . . ?
C31 P11 Pd1 115.43(14) . . ?
C32 P11 Pd1 127.02(12) . . ?
C93 O9 C93 180.0(11) 3_765 . ?
C93 O9 C92 123.2(6) 3_765 3_765 ?
C93 O9 C92 56.8(6) . 3_765 ?
C93 O9 C92 56.8(6) 3_765 . ?
C93 O9 C92 123.2(6) . . ?
C92 O9 C92 180.0(9) 3_765 . ?
C16 C11 C12 117.8(3) . . ?
C16 C11 C1 124.1(3) . . ?
C12 C11 C1 118.1(3) . . ?
C22 P12 C42 111.73(18) . . ?
C22 P12 C41 104.10(18) . . ?
C42 P12 C41 103.62(19) . . ?
C22 P12 Pd1 103.29(12) . . ?
C42 P12 Pd1 120.70(14) . . ?
C41 P12 Pd1 112.40(15) . . ?
C13 C12 C11 120.3(3) . . ?
C13 C12 P11 123.5(3) . . ?
C11 C12 P11 115.6(2) . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 118.9(3) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 121.1(3) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C11 121.1(3) . . ?
C15 C16 H16 119.4 . . ?
C11 C16 H16 119.4 . . ?
C52 P21 C72 103.66(14) . . ?
C52 P21 C71 108.20(15) . . ?
C72 P21 C71 106.24(15) . . ?
C52 P21 Pd2 102.22(10) . . ?
C72 P21 Pd2 122.92(10) . . ?
C71 P21 Pd2 112.41(11) . . ?
C22 C21 C26 116.8(3) . . ?
C22 C21 C1 121.7(3) . . ?
C26 C21 C1 121.5(3) . . ?
C62 P22 C81 108.33(17) . . ?
C62 P22 C82 104.29(17) . . ?
C81 P22 C82 104.79(17) . . ?
C62 P22 Pd2 100.14(11) . . ?
C81 P22 Pd2 114.33(12) . . ?
C82 P22 Pd2 123.64(13) . . ?
C23 C22 C21 121.3(3) . . ?
C23 C22 P12 124.4(3) . . ?
C21 C22 P12 114.2(3) . . ?
C25 C26 C21 121.9(3) . . ?
C25 C26 H26 119.1 . . ?
C21 C26 H26 119.1 . . ?
C26 C25 C24 120.1(3) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C23 C24 C25 119.4(3) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C24 C23 C22 120.6(3) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C33 C31 C34 110.8(3) . . ?
C33 C31 P11 110.1(3) . . ?
C34 C31 P11 112.6(3) . . ?
C33 C31 H31 107.7 . . ?
C34 C31 H31 107.7 . . ?
P11 C31 H31 107.7 . . ?
C36 C32 C35 112.6(3) . . ?
C36 C32 P11 114.5(3) . . ?
C35 C32 P11 111.1(3) . . ?
C36 C32 H32 106.0 . . ?
C35 C32 H32 106.0 . . ?
P11 C32 H32 106.0 . . ?
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 . . ?
C93 C94 H94A 109.5 . . ?
C93 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C93 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
O9 C93 C94 115.8(14) . . ?
O9 C93 H93A 108.3 . . ?
C94 C93 H93A 108.3 . . ?
O9 C93 H93B 108.3 . . ?
C94 C93 H93B 108.3 . . ?
H93A C93 H93B 107.4 . . ?
O9 C92 C95 116.4(15) . . ?
O9 C92 H92A 108.2 . . ?
C95 C92 H92A 108.2 . . ?
O9 C92 H92B 108.2 . . ?
C95 C92 H92B 108.2 . . ?
H92A C92 H92B 107.3 . . ?
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 . . ?
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 . . ?
C45 C42 C46 110.6(3) . . ?
C45 C42 P12 118.8(3) . . ?
C46 C42 P12 109.8(3) . . ?
C45 C42 H42 105.5 . . ?
C46 C42 H42 105.5 . . ?
P12 C42 H42 105.5 . . ?
C43 C41 C44 111.8(4) . . ?
C43 C41 P12 111.3(3) . . ?
C44 C41 P12 110.0(3) . . ?
C43 C41 H41 107.8 . . ?
C44 C41 H41 107.8 . . ?
P12 C41 H41 107.8 . . ?
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 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 . . ?
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 . . ?
C53 C54 C55 110.6(3) . . ?
C53 C54 C1 113.1(3) . . ?
C55 C54 C1 116.7(3) . . ?
C53 C54 H54 105.1 . . ?
C55 C54 H54 105.1 . . ?
C1 C54 H54 105.1 . . ?
C56 C55 C54 124.8(3) . . ?
C56 C55 H55 117.6 . . ?
C54 C55 H55 117.6 . . ?
C55 C56 C51 123.0(3) . . ?
C55 C56 H56 118.5 . . ?
C51 C56 H56 118.5 . . ?
C66 C61 C62 117.0(3) . . ?
C66 C61 C2 123.8(3) . . ?
C62 C61 C2 119.0(3) . . ?
C63 C62 C61 120.6(3) . . ?
C63 C62 P22 124.4(3) . . ?
C61 C62 P22 114.5(2) . . ?
C64 C63 C62 120.5(3) . . ?
C64 C63 H63 119.8 . . ?
C62 C63 H63 119.8 . . ?
C63 C64 C65 119.6(3) . . ?
C63 C64 H64 120.2 . . ?
C65 C64 H64 120.2 . . ?
C66 C65 C64 120.3(3) . . ?
C66 C65 H65 119.9 . . ?
C64 C65 H65 119.9 . . ?
C65 C66 C61 121.7(3) . . ?
C65 C66 H66 119.1 . . ?
C61 C66 H66 119.1 . . ?
C73 C71 C74 110.7(3) . . ?
C73 C71 P21 117.8(2) . . ?
C74 C71 P21 108.2(2) . . ?
C73 C71 H71 106.5 . . ?
C74 C71 H71 106.5 . . ?
P21 C71 H71 106.5 . . ?
C75 C72 C76 111.0(3) . . ?
C75 C72 P21 111.9(2) . . ?
C76 C72 P21 111.4(2) . . ?
C75 C72 H72 107.4 . . ?
C76 C72 H72 107.4 . . ?
P21 C72 H72 107.4 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C72 C75 H75A 109.5 . . ?
C72 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C72 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C72 C76 H76A 109.5 . . ?
C72 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C72 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C83 C81 C84 110.5(3) . . ?
C83 C81 P22 110.3(3) . . ?
C84 C81 P22 114.2(3) . . ?
C83 C81 H81 107.2 . . ?
C84 C81 H81 107.2 . . ?
P22 C81 H81 107.2 . . ?
C86 C82 C85 111.9(3) . . ?
C86 C82 P22 110.3(2) . . ?
C85 C82 P22 112.2(3) . . ?
C86 C82 H82 107.4 . . ?
C85 C82 H82 107.4 . . ?
P22 C82 H82 107.4 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C81 C84 H84A 109.5 . . ?
C81 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C81 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C82 C85 H85A 109.5 . . ?
C82 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C82 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C82 C86 H86A 109.5 . . ?
C82 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C82 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C52 C53 C54 123.5(3) . . ?
C52 C53 H53 118.2 . . ?
C54 C53 H53 118.2 . . ?
C53 C52 C51 124.2(3) . . ?
C53 C52 P21 123.6(2) . . ?
C51 C52 P21 112.0(2) . . ?
C2 C51 C52 119.1(3) . . ?
C2 C51 C56 127.4(3) . . ?
C52 C51 C56 113.5(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.964
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.096
####################################################################### 
# 
# 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_cc277
_database_code_depnum_ccdc_archive 'CCDC 1058170'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H36 Br P2 Pd'
_chemical_formula_weight         584.79

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'
Br Br -0.2901 2.4595 '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)/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                   12.5686(12)
_cell_length_b                   13.9781(13)
_cell_length_c                   14.9939(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.3300(18)
_cell_angle_gamma                90.00
_cell_volume                     2612.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7682
_cell_measurement_theta_min      2.190
_cell_measurement_theta_max      26.905

_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    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1188
_exptl_absorpt_coefficient_mu    2.372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6456
_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       '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            33653
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4601
_reflns_number_gt                3834
_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)+(0.0285P)²+0.4709P] 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         4601
_refine_ls_number_parameters     270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0258
_refine_ls_wR_factor_ref         0.0569
_refine_ls_wR_factor_gt          0.0542
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 0.466094(16) 0.675362(14) 0.282253(14) 0.02214(7) Uani 1 1 d . . .
C C 0.5626(3) 0.7301(3) 0.3880(3) 0.0246(17) Uani 1 1 d . . .
Br Br 0.33607(2) 0.602752(19) 0.159750(19) 0.02232(8) Uani 1 1 d . . .
P2 P 0.35448(5) 0.79619(5) 0.31262(5) 0.01807(16) Uani 1 1 d . . .
P1 P 0.60486(6) 0.57043(5) 0.27643(5) 0.01938(16) Uani 1 1 d . . .
C11 C 0.6776(2) 0.7085(2) 0.39585(19) 0.0261(7) Uani 1 1 d . . .
C12 C 0.7106(2) 0.62699(19) 0.35196(18) 0.0216(6) Uani 1 1 d . . .
C13 C 0.8179(2) 0.6013(2) 0.3607(2) 0.0397(9) Uani 1 1 d . . .
H13 H 0.8391 0.5454 0.3316 0.048 Uiso 1 1 calc R . .
C14 C 0.8942(3) 0.6566(3) 0.4114(2) 0.0408(10) Uani 1 1 d . . .
H14 H 0.9673 0.6375 0.4194 0.061 Uiso 1 1 calc R . .
C15 C 0.8636(3) 0.7393(2) 0.4501(2) 0.0388(8) Uani 1 1 d . . .
H15 H 0.9166 0.7788 0.4825 0.047 Uiso 1 1 calc R . .
C16 C 0.7581(2) 0.7659(2) 0.44299(19) 0.0291(7) Uani 1 1 d . . .
H16 H 0.7389 0.8237 0.4701 0.035 Uiso 1 1 calc R . .
C21 C 0.5161(2) 0.7942(2) 0.4498(2) 0.0286(7) Uani 1 1 d . . .
C22 C 0.4175(2) 0.83952(18) 0.41989(19) 0.0201(6) Uani 1 1 d . . .
C23 C 0.3745(2) 0.90667(19) 0.47272(19) 0.0232(6) Uani 1 1 d . . .
H23 H 0.3107 0.9397 0.4500 0.028 Uiso 1 1 calc R . .
C24 C 0.4240(2) 0.9260(2) 0.5588(2) 0.0304(7) Uani 1 1 d . . .
H24 H 0.3950 0.9728 0.5947 0.036 Uiso 1 1 calc R . .
C25 C 0.5164(2) 0.8765(2) 0.5920(2) 0.0298(7) Uani 1 1 d . . .
H25 H 0.5482 0.8869 0.6521 0.036 Uiso 1 1 calc R . .
C26 C 0.5620(2) 0.81261(19) 0.5386(2) 0.0310(8) Uani 1 1 d . . .
H26 H 0.6259 0.7802 0.5621 0.037 Uiso 1 1 calc R . .
C31 C 0.5865(3) 0.4469(2) 0.3139(2) 0.0345(8) Uani 1 1 d . . .
H31 H 0.5273 0.4185 0.2712 0.041 Uiso 1 1 calc R . .
C32 C 0.6617(2) 0.5635(2) 0.1692(2) 0.0305(7) Uani 1 1 d . . .
H32 H 0.7364 0.5378 0.1811 0.037 Uiso 1 1 calc R . .
C33 C 0.5474(3) 0.4495(3) 0.4060(2) 0.0481(9) Uani 1 1 d . . .
H33A H 0.4828 0.4893 0.4031 0.072 Uiso 1 1 calc R . .
H33B H 0.6036 0.4765 0.4502 0.072 Uiso 1 1 calc R . .
H33C H 0.5306 0.3844 0.4240 0.072 Uiso 1 1 calc R . .
C34 C 0.6825(3) 0.3812(3) 0.3145(3) 0.0666(13) Uani 1 1 d . . .
H34A H 0.7090 0.3838 0.2558 0.100 Uiso 1 1 calc R . .
H34B H 0.6613 0.3155 0.3266 0.100 Uiso 1 1 calc R . .
H34C H 0.7394 0.4018 0.3613 0.100 Uiso 1 1 calc R . .
C35 C 0.5962(3) 0.4993(2) 0.1011(2) 0.0411(9) Uani 1 1 d . . .
H35A H 0.5227 0.5238 0.0890 0.062 Uiso 1 1 calc R . .
H35B H 0.5949 0.4342 0.1252 0.062 Uiso 1 1 calc R . .
H35C H 0.6288 0.4984 0.0451 0.062 Uiso 1 1 calc R . .
C36 C 0.6660(3) 0.6650(3) 0.1335(2) 0.0561(11) Uani 1 1 d . . .
H36A H 0.7038 0.6652 0.0802 0.084 Uiso 1 1 calc R . .
H36B H 0.7042 0.7061 0.1799 0.084 Uiso 1 1 calc R . .
H36C H 0.5929 0.6890 0.1173 0.084 Uiso 1 1 calc R . .
C41 C 0.2199(2) 0.75156(19) 0.32807(19) 0.0228(6) Uani 1 1 d . . .
H41 H 0.1885 0.7239 0.2690 0.027 Uiso 1 1 calc R . .
C42 C 0.3372(2) 0.90126(19) 0.23770(19) 0.0213(6) Uani 1 1 d . . .
H42 H 0.3051 0.9544 0.2702 0.026 Uiso 1 1 calc R . .
C43 C 0.2325(3) 0.6685(2) 0.3953(2) 0.0365(8) Uani 1 1 d . . .
H43A H 0.1620 0.6406 0.4003 0.055 Uiso 1 1 calc R . .
H43B H 0.2643 0.6922 0.4542 0.055 Uiso 1 1 calc R . .
H43C H 0.2793 0.6195 0.3742 0.055 Uiso 1 1 calc R . .
C44 C 0.1401(2) 0.8257(2) 0.3534(2) 0.0285(7) Uani 1 1 d . . .
H44A H 0.1409 0.8815 0.3140 0.043 Uiso 1 1 calc R . .
H44B H 0.1600 0.8453 0.4160 0.043 Uiso 1 1 calc R . .
H44C H 0.0679 0.7978 0.3465 0.043 Uiso 1 1 calc R . .
C45 C 0.2627(2) 0.8796(2) 0.15154(19) 0.0288(7) Uani 1 1 d . . .
H45A H 0.2612 0.9346 0.1108 0.043 Uiso 1 1 calc R . .
H45B H 0.1902 0.8672 0.1662 0.043 Uiso 1 1 calc R . .
H45C H 0.2890 0.8232 0.1223 0.043 Uiso 1 1 calc R . .
C46 C 0.4476(2) 0.9329(2) 0.2169(2) 0.0344(8) Uani 1 1 d . . .
H46A H 0.4785 0.8828 0.1823 0.052 Uiso 1 1 calc R . .
H46B H 0.4946 0.9438 0.2733 0.052 Uiso 1 1 calc R . .
H46C H 0.4407 0.9922 0.1818 0.052 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 2.020(3) . ?
Pd P2 2.2783(7) . ?
Pd P1 2.2891(7) . ?
Pd Br 2.5117(4) . ?
C C21 1.463(4) . ?
C C11 1.467(4) . ?
P2 C22 1.805(3) . ?
P2 C41 1.845(3) . ?
P2 C42 1.845(3) . ?
P1 C12 1.814(3) . ?
P1 C31 1.839(3) . ?
P1 C32 1.844(3) . ?
C11 C12 1.404(4) . ?
C11 C16 1.409(4) . ?
C12 C13 1.385(4) . ?
C13 C14 1.382(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.369(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.369(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.404(4) . ?
C21 C22 1.413(4) . ?
C22 C23 1.382(4) . ?
C23 C24 1.386(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.373(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C34 1.516(5) . ?
C31 C33 1.525(5) . ?
C31 H31 1.0000 . ?
C32 C36 1.519(5) . ?
C32 C35 1.520(4) . ?
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 1.524(4) . ?
C41 C43 1.532(4) . ?
C41 H41 1.0000 . ?
C42 C45 1.526(4) . ?
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 . ?

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 83.43(10) . . ?
C Pd P1 83.61(10) . . ?
P2 Pd P1 166.96(3) . . ?
C Pd Br 175.31(15) . . ?
P2 Pd Br 94.93(2) . . ?
P1 Pd Br 98.10(2) . . ?
C21 C C11 123.0(3) . . ?
C21 C Pd 118.7(2) . . ?
C11 C Pd 118.1(2) . . ?
C22 P2 C41 107.88(13) . . ?
C22 P2 C42 106.24(12) . . ?
C41 P2 C42 107.87(12) . . ?
C22 P2 Pd 102.43(9) . . ?
C41 P2 Pd 111.84(9) . . ?
C42 P2 Pd 119.76(9) . . ?
C12 P1 C31 109.20(14) . . ?
C12 P1 C32 103.48(13) . . ?
C31 P1 C32 107.14(15) . . ?
C12 P1 Pd 101.42(9) . . ?
C31 P1 Pd 117.65(11) . . ?
C32 P1 Pd 116.67(10) . . ?
C12 C11 C16 117.5(3) . . ?
C12 C11 C 118.5(3) . . ?
C16 C11 C 124.0(3) . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 P1 125.0(2) . . ?
C11 C12 P1 114.2(2) . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 119.5(3) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C15 C14 121.2(3) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C11 120.7(3) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
C26 C21 C22 117.1(3) . . ?
C26 C21 C 124.3(3) . . ?
C22 C21 C 118.6(3) . . ?
C23 C22 C21 120.9(3) . . ?
C23 C22 P2 125.4(2) . . ?
C21 C22 P2 113.6(2) . . ?
C22 C23 C24 120.2(3) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C25 119.5(3) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C26 C25 C24 120.5(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 121.3(3) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
C34 C31 C33 111.0(3) . . ?
C34 C31 P1 116.1(3) . . ?
C33 C31 P1 108.8(2) . . ?
C34 C31 H31 106.8 . . ?
C33 C31 H31 106.8 . . ?
P1 C31 H31 106.8 . . ?
C36 C32 C35 110.8(3) . . ?
C36 C32 P1 107.1(2) . . ?
C35 C32 P1 112.3(2) . . ?
C36 C32 H32 108.8 . . ?
C35 C32 H32 108.8 . . ?
P1 C32 H32 108.8 . . ?
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 111.6(2) . . ?
C44 C41 P2 116.42(19) . . ?
C43 C41 P2 108.63(19) . . ?
C44 C41 H41 106.6 . . ?
C43 C41 H41 106.6 . . ?
P2 C41 H41 106.6 . . ?
C45 C42 C46 111.1(2) . . ?
C45 C42 P2 111.70(18) . . ?
C46 C42 P2 108.4(2) . . ?
C45 C42 H42 108.5 . . ?
C46 C42 H42 108.5 . . ?
P2 C42 H42 108.5 . . ?
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 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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_cc271
_database_code_depnum_ccdc_archive 'CCDC 1058171'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H37 Br P2 Pd'
_chemical_formula_weight         585.80

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'
Br Br -0.2901 2.4595 '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)/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                   11.2438(8)
_cell_length_b                   13.7677(10)
_cell_length_c                   17.4246(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.9775(12)
_cell_angle_gamma                90.00
_cell_volume                     2579.8(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          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6879
_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  ?
_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            33493
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4546
_reflns_number_gt                3801
_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)+(0.0317P)²+1.2910P] 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         4546
_refine_ls_number_parameters     270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0742
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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 0.02187(3) 0.65787(2) 0.182175(18) 0.01876(9) Uani 1 1 d . . .
P1 P -0.16836(10) 0.57786(7) 0.15980(6) 0.0220(2) Uani 1 1 d . . .
Br Br 0.14254(4) 0.58796(3) 0.31483(2) 0.02476(11) Uani 1 1 d . . .
C C -0.0624(4) 0.7074(3) 0.0669(2) 0.0221(9) Uani 1 1 d . . .
H H -0.0666 0.6491 0.0320 0.027 Uiso 1 1 calc R . .
P2 P 0.16165(9) 0.77727(7) 0.18634(6) 0.0174(2) Uani 1 1 d . . .
C11 C -0.1977(4) 0.7319(3) 0.0586(2) 0.0241(9) Uani 1 1 d . . .
C12 C -0.2653(4) 0.6656(3) 0.0910(2) 0.0235(9) Uani 1 1 d . . .
C13 C -0.3923(4) 0.6779(3) 0.0787(3) 0.0292(10) Uani 1 1 d . . .
H13 H -0.4380 0.6309 0.0982 0.035 Uiso 1 1 calc R . .
C14 C -0.4522(4) 0.7591(3) 0.0378(3) 0.0344(11) Uani 1 1 d . . .
H14 H -0.5389 0.7676 0.0294 0.041 Uiso 1 1 calc R . .
C15 C -0.3865(4) 0.8268(3) 0.0096(3) 0.0300(10) Uani 1 1 d . . .
H15 H -0.4271 0.8835 -0.0165 0.036 Uiso 1 1 calc R . .
C16 C -0.2606(4) 0.8131(3) 0.0189(2) 0.0288(10) Uani 1 1 d . . .
H16 H -0.2165 0.8600 -0.0021 0.035 Uiso 1 1 calc R . .
C21 C 0.0106(4) 0.7824(3) 0.0343(2) 0.0227(9) Uani 1 1 d . . .
C22 C 0.1203(4) 0.8214(3) 0.0840(2) 0.0209(9) Uani 1 1 d . . .
C23 C 0.1880(4) 0.8894(3) 0.0539(3) 0.0265(9) Uani 1 1 d . . .
H23 H 0.2619 0.9169 0.0883 0.032 Uiso 1 1 calc R . .
C24 C 0.1467(4) 0.9163(3) -0.0261(3) 0.0334(11) Uani 1 1 d . . .
H24 H 0.1918 0.9627 -0.0468 0.040 Uiso 1 1 calc R . .
C26 C -0.0289(4) 0.8098(3) -0.0465(3) 0.0325(10) Uani 1 1 d . . .
H26 H -0.1031 0.7832 -0.0813 0.039 Uiso 1 1 calc R . .
C31 C -0.2339(4) 0.5750(3) 0.2457(3) 0.0266(10) Uani 1 1 d . . .
H31 H -0.3258 0.5653 0.2241 0.032 Uiso 1 1 calc R . .
C32 C -0.1970(4) 0.4556(3) 0.1143(3) 0.0325(10) Uani 1 1 d . . .
H32 H -0.1536 0.4084 0.1570 0.039 Uiso 1 1 calc R . .
C33 C -0.2110(4) 0.6723(3) 0.2893(3) 0.0347(11) Uani 1 1 d . . .
H33A H -0.2400 0.7250 0.2505 0.052 Uiso 1 1 calc R . .
H33B H -0.1218 0.6802 0.3159 0.052 Uiso 1 1 calc R . .
H33C H -0.2564 0.6744 0.3294 0.052 Uiso 1 1 calc R . .
C34 C -0.1804(4) 0.4908(3) 0.3027(3) 0.0322(10) Uani 1 1 d . . .
H34A H -0.2018 0.4291 0.2740 0.048 Uiso 1 1 calc R . .
H34B H -0.2155 0.4922 0.3480 0.048 Uiso 1 1 calc R . .
H34C H -0.0898 0.4971 0.3227 0.048 Uiso 1 1 calc R . .
C35 C -0.1365(5) 0.4462(3) 0.0470(3) 0.0445(13) Uani 1 1 d . . .
H35A H -0.1436 0.3789 0.0278 0.067 Uiso 1 1 calc R . .
H35B H -0.0484 0.4640 0.0672 0.067 Uiso 1 1 calc R . .
H35C H -0.1784 0.4895 0.0027 0.067 Uiso 1 1 calc R . .
C36 C -0.3332(5) 0.4262(4) 0.0873(3) 0.0507(14) Uani 1 1 d . . .
H36A H -0.3791 0.4692 0.0439 0.076 Uiso 1 1 calc R . .
H36B H -0.3679 0.4315 0.1326 0.076 Uiso 1 1 calc R . .
H36C H -0.3406 0.3590 0.0680 0.076 Uiso 1 1 calc R . .
C41 C 0.3250(3) 0.7389(3) 0.2201(3) 0.0232(9) Uani 1 1 d . . .
H41 H 0.3393 0.7128 0.2757 0.028 Uiso 1 1 calc R . .
C42 C 0.1446(4) 0.8840(3) 0.2458(2) 0.0211(9) Uani 1 1 d . . .
H42 H 0.1907 0.9397 0.2310 0.025 Uiso 1 1 calc R . .
C43 C 0.3431(4) 0.6533(3) 0.1689(3) 0.0323(10) Uani 1 1 d . . .
H43A H 0.3269 0.6744 0.1130 0.048 Uiso 1 1 calc R . .
H43B H 0.2852 0.6011 0.1716 0.048 Uiso 1 1 calc R . .
H43C H 0.4287 0.6294 0.1890 0.048 Uiso 1 1 calc R . .
C44 C 0.4241(4) 0.8165(3) 0.2261(3) 0.0355(11) Uani 1 1 d . . .
H44A H 0.4241 0.8362 0.1720 0.053 Uiso 1 1 calc R . .
H44B H 0.5059 0.7902 0.2550 0.053 Uiso 1 1 calc R . .
H44C H 0.4061 0.8730 0.2551 0.053 Uiso 1 1 calc R . .
C45 C 0.1960(5) 0.8659(3) 0.3357(3) 0.0340(11) Uani 1 1 d . . .
H45A H 0.1612 0.8053 0.3495 0.051 Uiso 1 1 calc R . .
H45B H 0.1731 0.9200 0.3651 0.051 Uiso 1 1 calc R . .
H45C H 0.2868 0.8606 0.3504 0.051 Uiso 1 1 calc R . .
C46 C 0.0057(4) 0.9097(3) 0.2230(3) 0.0270(9) Uani 1 1 d . . .
H46A H -0.0263 0.9182 0.1647 0.041 Uiso 1 1 calc R . .
H46B H -0.0054 0.9701 0.2498 0.041 Uiso 1 1 calc R . .
H46C H -0.0398 0.8571 0.2398 0.041 Uiso 1 1 calc R . .
C25 C 0.0395(5) 0.8752(3) -0.0756(3) 0.0370(11) Uani 1 1 d . . .
H25 H 0.0126 0.8925 -0.1308 0.044 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 2.071(4) . ?
Pd P2 2.2608(10) . ?
Pd P1 2.3352(11) . ?
Pd Br 2.5057(5) . ?
P1 C12 1.822(4) . ?
P1 C32 1.849(4) . ?
P1 C31 1.852(4) . ?
C C11 1.523(6) . ?
C C21 1.527(5) . ?
C H 1.0000 . ?
P2 C22 1.812(4) . ?
P2 C41 1.835(4) . ?
P2 C42 1.840(4) . ?
C11 C16 1.394(6) . ?
C11 C12 1.407(5) . ?
C12 C13 1.392(6) . ?
C13 C14 1.389(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.366(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.391(5) . ?
C21 C26 1.398(6) . ?
C22 C23 1.402(5) . ?
C23 C24 1.384(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.382(6) . ?
C24 H24 0.9500 . ?
C26 C25 1.374(6) . ?
C26 H26 0.9500 . ?
C31 C33 1.524(6) . ?
C31 C34 1.531(6) . ?
C31 H31 1.0000 . ?
C32 C36 1.520(7) . ?
C32 C35 1.524(6) . ?
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 1.526(5) . ?
C41 C43 1.528(5) . ?
C41 H41 1.0000 . ?
C42 C45 1.525(6) . ?
C42 C46 1.536(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 . ?
C25 H25 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 84.74(11) . . ?
C Pd P1 81.73(11) . . ?
P2 Pd P1 160.49(4) . . ?
C Pd Br 173.06(11) . . ?
P2 Pd Br 93.76(3) . . ?
P1 Pd Br 101.28(3) . . ?
C12 P1 C32 109.0(2) . . ?
C12 P1 C31 104.12(19) . . ?
C32 P1 C31 105.46(19) . . ?
C12 P1 Pd 98.03(13) . . ?
C32 P1 Pd 122.51(15) . . ?
C31 P1 Pd 115.87(14) . . ?
C11 C C21 116.4(3) . . ?
C11 C Pd 109.0(3) . . ?
C21 C Pd 116.1(3) . . ?
C11 C H 104.6 . . ?
C21 C H 104.6 . . ?
Pd C H 104.6 . . ?
C22 P2 C41 110.95(19) . . ?
C22 P2 C42 104.33(17) . . ?
C41 P2 C42 107.96(18) . . ?
C22 P2 Pd 103.63(13) . . ?
C41 P2 Pd 114.97(13) . . ?
C42 P2 Pd 114.42(13) . . ?
C16 C11 C12 117.7(4) . . ?
C16 C11 C 124.9(4) . . ?
C12 C11 C 117.4(4) . . ?
C13 C12 C11 120.6(4) . . ?
C13 C12 P1 124.9(3) . . ?
C11 C12 P1 113.9(3) . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.1(4) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.3(4) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 121.2(4) . . ?
C15 C16 H16 119.4 . . ?
C11 C16 H16 119.4 . . ?
C22 C21 C26 119.0(4) . . ?
C22 C21 C 120.3(3) . . ?
C26 C21 C 120.6(4) . . ?
C21 C22 C23 120.3(4) . . ?
C21 C22 P2 114.2(3) . . ?
C23 C22 P2 125.5(3) . . ?
C24 C23 C22 119.8(4) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C25 C24 C23 119.5(4) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C25 C26 C21 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C33 C31 C34 111.4(4) . . ?
C33 C31 P1 109.5(3) . . ?
C34 C31 P1 111.6(3) . . ?
C33 C31 H31 108.1 . . ?
C34 C31 H31 108.1 . . ?
P1 C31 H31 108.1 . . ?
C36 C32 C35 112.1(4) . . ?
C36 C32 P1 114.1(3) . . ?
C35 C32 P1 110.3(3) . . ?
C36 C32 H32 106.6 . . ?
C35 C32 H32 106.6 . . ?
P1 C32 H32 106.6 . . ?
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 . . ?
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 111.2(3) . . ?
C44 C41 P2 117.6(3) . . ?
C43 C41 P2 109.0(3) . . ?
C44 C41 H41 106.1 . . ?
C43 C41 H41 106.1 . . ?
P2 C41 H41 106.1 . . ?
C45 C42 C46 110.8(3) . . ?
C45 C42 P2 112.1(3) . . ?
C46 C42 P2 107.7(3) . . ?
C45 C42 H42 108.7 . . ?
C46 C42 H42 108.7 . . ?
P2 C42 H42 108.7 . . ?
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 . . ?
C26 C25 C24 121.2(4) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.970
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.094
####################################################################### 
# 
# 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_cc250
_database_code_depnum_ccdc_archive 'CCDC 1058172'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H36 Cl P2 Pd'
_chemical_formula_weight         540.33

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   11.6639(11)
_cell_length_b                   13.5934(13)
_cell_length_c                   16.5680(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1159(14)
_cell_angle_gamma                90.00
_cell_volume                     2536.0(4)
_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          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1116
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6929
_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  ?
_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            36052
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4436
_reflns_number_gt                3928
_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)+(0.0225P)²+1.9419P] 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         4436
_refine_ls_number_parameters     270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0541
_refine_ls_wR_factor_gt          0.0523
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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 0.015799(15) 0.827903(12) 0.194506(11) 0.01566(6) Uani 1 1 d . . .
P1 P 0.15024(5) 0.70808(4) 0.19016(4) 0.01508(13) Uani 1 1 d . . .
Cl Cl 0.14068(5) 0.90818(4) 0.31356(3) 0.02092(13) Uani 1 1 d . . .
P2 P -0.15260(5) 0.92214(4) 0.17604(4) 0.01656(13) Uani 1 1 d . . .
C C -0.0783(2) 0.7603(2) 0.09076(16) 0.0306(6) Uani 1 1 d . . .
C11 C -0.0156(2) 0.69972(16) 0.04320(15) 0.0198(5) Uani 1 1 d . . .
C12 C 0.09701(19) 0.66181(16) 0.08448(14) 0.0166(5) Uani 1 1 d . . .
C13 C 0.1558(2) 0.59550(16) 0.04562(14) 0.0183(5) Uani 1 1 d . . .
H13 H 0.2286 0.5669 0.0760 0.022 Uiso 1 1 calc R . .
C14 C 0.1078(2) 0.57109(17) -0.03797(15) 0.0220(5) Uani 1 1 d . . .
H14 H 0.1477 0.5259 -0.0650 0.026 Uiso 1 1 calc R . .
C15 C 0.0016(2) 0.61327(17) -0.08147(15) 0.0231(5) Uani 1 1 d . . .
H15 H -0.0294 0.5990 -0.1392 0.028 Uiso 1 1 calc R . .
C16 C -0.0600(2) 0.67567(17) -0.04212(15) 0.0236(5) Uani 1 1 d . . .
H16 H -0.1334 0.7029 -0.0730 0.028 Uiso 1 1 calc R . .
C21 C -0.2064(2) 0.76799(16) 0.06865(14) 0.0181(5) Uani 1 1 d . . .
C22 C -0.2590(2) 0.84699(16) 0.10216(14) 0.0177(5) Uani 1 1 d . . .
C23 C -0.3814(2) 0.85604(18) 0.08361(16) 0.0248(6) Uani 1 1 d . . .
H23 H -0.4153 0.9101 0.1055 0.030 Uiso 1 1 calc R . .
C24 C -0.4551(2) 0.7876(2) 0.03375(16) 0.0296(6) Uani 1 1 d . . .
H24 H -0.5389 0.7950 0.0208 0.035 Uiso 1 1 calc R . .
C25 C -0.4050(2) 0.70819(18) 0.00288(15) 0.0248(5) Uani 1 1 d . . .
H25 H -0.4550 0.6601 -0.0303 0.030 Uiso 1 1 calc R . .
C31 C 0.30244(19) 0.75402(16) 0.20566(15) 0.0194(5) Uani 1 1 d . . .
H31 H 0.3258 0.7834 0.2630 0.023 Uiso 1 1 calc R . .
C32 C 0.1532(2) 0.60218(16) 0.25986(14) 0.0186(5) Uani 1 1 d . . .
H32 H 0.1939 0.5460 0.2400 0.022 Uiso 1 1 calc R . .
C33 C 0.2996(2) 0.83900(18) 0.14424(17) 0.0284(6) Uani 1 1 d . . .
H33A H 0.2744 0.8141 0.0868 0.043 Uiso 1 1 calc R . .
H33B H 0.3791 0.8678 0.1542 0.043 Uiso 1 1 calc R . .
H33C H 0.2436 0.8893 0.1525 0.043 Uiso 1 1 calc R . .
C34 C 0.3980(2) 0.67946(18) 0.20206(18) 0.0304(6) Uani 1 1 d . . .
H34A H 0.3881 0.6584 0.1441 0.046 Uiso 1 1 calc R . .
H34B H 0.3912 0.6223 0.2366 0.046 Uiso 1 1 calc R . .
H34C H 0.4765 0.7096 0.2232 0.046 Uiso 1 1 calc R . .
C35 C 0.2189(2) 0.62597(18) 0.34978(15) 0.0269(6) Uani 1 1 d . . .
H35A H 0.3033 0.6362 0.3535 0.040 Uiso 1 1 calc R . .
H35B H 0.2101 0.5712 0.3861 0.040 Uiso 1 1 calc R . .
H35C H 0.1856 0.6859 0.3676 0.040 Uiso 1 1 calc R . .
C36 C 0.0242(2) 0.57315(19) 0.25372(16) 0.0272(6) Uani 1 1 d . . .
H36A H -0.0181 0.5630 0.1949 0.041 Uiso 1 1 calc R . .
H36B H -0.0146 0.6257 0.2773 0.041 Uiso 1 1 calc R . .
H36C H 0.0229 0.5122 0.2850 0.041 Uiso 1 1 calc R . .
C41 C -0.1519(2) 1.04615(17) 0.13154(15) 0.0231(5) Uani 1 1 d . . .
H41 H -0.1048 1.0891 0.1772 0.028 Uiso 1 1 calc R . .
C42 C -0.2167(2) 0.93535(17) 0.26625(15) 0.0217(5) Uani 1 1 d . . .
H42 H -0.3011 0.9573 0.2454 0.026 Uiso 1 1 calc R . .
C43 C -0.0862(2) 1.0439(2) 0.06309(17) 0.0360(7) Uani 1 1 d . . .
H43A H -0.1298 1.0024 0.0168 0.054 Uiso 1 1 calc R . .
H43B H -0.0063 1.0169 0.0858 0.054 Uiso 1 1 calc R . .
H43C H -0.0801 1.1108 0.0426 0.054 Uiso 1 1 calc R . .
C44 C -0.2738(2) 1.09319(19) 0.10055(18) 0.0338(6) Uani 1 1 d . . .
H44A H -0.2648 1.1609 0.0828 0.051 Uiso 1 1 calc R . .
H44B H -0.3137 1.0936 0.1458 0.051 Uiso 1 1 calc R . .
H44C H -0.3212 1.0554 0.0531 0.051 Uiso 1 1 calc R . .
C45 C -0.1491(2) 1.0115(2) 0.32843(16) 0.0304(6) Uani 1 1 d . . .
H45A H -0.0640 0.9965 0.3426 0.046 Uiso 1 1 calc R . .
H45B H -0.1771 1.0096 0.3793 0.046 Uiso 1 1 calc R . .
H45C H -0.1627 1.0771 0.3034 0.046 Uiso 1 1 calc R . .
C46 C -0.2148(3) 0.83412(19) 0.30722(17) 0.0329(6) Uani 1 1 d . . .
H46A H -0.2575 0.7867 0.2656 0.049 Uiso 1 1 calc R . .
H46B H -0.2534 0.8385 0.3531 0.049 Uiso 1 1 calc R . .
H46C H -0.1324 0.8125 0.3292 0.049 Uiso 1 1 calc R . .
C26 C -0.2837(2) 0.69837(17) 0.01975(14) 0.0210(5) Uani 1 1 d . . .
H26 H -0.2513 0.6434 -0.0021 0.025 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 2.005(2) . ?
Pd P1 2.2751(6) . ?
Pd P2 2.2977(6) . ?
Pd Cl 2.3884(6) . ?
P1 C12 1.811(2) . ?
P1 C31 1.836(2) . ?
P1 C32 1.840(2) . ?
P2 C22 1.814(2) . ?
P2 C41 1.841(2) . ?
P2 C42 1.846(2) . ?
C C21 1.446(3) . ?
C C11 1.461(3) . ?
C11 C12 1.411(3) . ?
C11 C16 1.411(3) . ?
C12 C13 1.389(3) . ?
C13 C14 1.392(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.380(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.409(3) . ?
C21 C22 1.420(3) . ?
C22 C23 1.385(3) . ?
C23 C24 1.384(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.375(3) . ?
C25 H25 0.9500 . ?
C31 C34 1.519(3) . ?
C31 C33 1.534(3) . ?
C31 H31 1.0000 . ?
C32 C35 1.522(3) . ?
C32 C36 1.533(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 C44 1.520(3) . ?
C41 C43 1.526(3) . ?
C41 H41 1.0000 . ?
C42 C45 1.526(3) . ?
C42 C46 1.532(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 . ?
C26 H26 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 82.69(7) . . ?
C Pd P2 83.30(7) . . ?
P1 Pd P2 165.30(2) . . ?
C Pd Cl 175.61(8) . . ?
P1 Pd Cl 94.38(2) . . ?
P2 Pd Cl 99.86(2) . . ?
C12 P1 C31 109.19(11) . . ?
C12 P1 C32 106.30(10) . . ?
C31 P1 C32 108.61(10) . . ?
C12 P1 Pd 102.35(7) . . ?
C31 P1 Pd 113.67(7) . . ?
C32 P1 Pd 116.13(8) . . ?
C22 P2 C41 108.61(11) . . ?
C22 P2 C42 104.53(11) . . ?
C41 P2 C42 106.27(11) . . ?
C22 P2 Pd 100.76(7) . . ?
C41 P2 Pd 118.10(8) . . ?
C42 P2 Pd 117.32(8) . . ?
C21 C C11 122.2(2) . . ?
C21 C Pd 118.87(17) . . ?
C11 C Pd 118.78(17) . . ?
C12 C11 C16 116.9(2) . . ?
C12 C11 C 118.6(2) . . ?
C16 C11 C 124.5(2) . . ?
C13 C12 C11 121.5(2) . . ?
C13 C12 P1 125.98(18) . . ?
C11 C12 P1 112.51(16) . . ?
C12 C13 C14 119.8(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C15 C14 C13 119.5(2) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 C14 120.9(2) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C11 121.0(2) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C26 C21 C22 117.1(2) . . ?
C26 C21 C 124.1(2) . . ?
C22 C21 C 118.6(2) . . ?
C23 C22 C21 120.4(2) . . ?
C23 C22 P2 125.73(18) . . ?
C21 C22 P2 113.60(16) . . ?
C24 C23 C22 121.1(2) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 119.2(2) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C26 C25 C24 120.7(2) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C34 C31 C33 111.4(2) . . ?
C34 C31 P1 117.41(16) . . ?
C33 C31 P1 108.10(16) . . ?
C34 C31 H31 106.4 . . ?
C33 C31 H31 106.4 . . ?
P1 C31 H31 106.4 . . ?
C35 C32 C36 110.8(2) . . ?
C35 C32 P1 111.74(16) . . ?
C36 C32 P1 107.60(16) . . ?
C35 C32 H32 108.9 . . ?
C36 C32 H32 108.9 . . ?
P1 C32 H32 108.9 . . ?
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 111.4(2) . . ?
C44 C41 P2 114.78(17) . . ?
C43 C41 P2 109.55(17) . . ?
C44 C41 H41 106.9 . . ?
C43 C41 H41 106.9 . . ?
P2 C41 H41 106.9 . . ?
C45 C42 C46 111.4(2) . . ?
C45 C42 P2 111.44(16) . . ?
C46 C42 P2 108.04(16) . . ?
C45 C42 H42 108.6 . . ?
C46 C42 H42 108.6 . . ?
P2 C42 H42 108.6 . . ?
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 . . ?
C25 C26 C21 121.5(2) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.062
####################################################################### 
# 
# 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_cc252
_database_code_depnum_ccdc_archive 'CCDC 1058173'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H47 P3 Pd'
_chemical_formula_weight         594.98

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   10.3086(7)
_cell_length_b                   24.0617(16)
_cell_length_c                   12.5709(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.5771(18)
_cell_angle_gamma                90.00
_cell_volume                     2972.5(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          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_T_max  0.7459
_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  ?
_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            71407
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5233
_reflns_number_gt                4714
_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)+(0.0188P)²+2.3586P] 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         5233
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0512
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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 0.329627(15) 0.902466(6) 0.773050(12) 0.01095(5) Uani 1 1 d . . .
C1 C 0.36707(19) 0.83153(8) 0.89193(15) 0.0117(4) Uani 1 1 d . . .
P1 P 0.31818(5) 0.83411(2) 0.63170(4) 0.01151(11) Uani 1 1 d . . .
C2 C 0.4938(2) 0.85538(8) 0.90181(16) 0.0148(4) Uani 1 1 d . . .
H2A H 0.5573 0.8331 0.8736 0.018 Uiso 1 1 calc R . .
H2B H 0.5387 0.8751 0.9724 0.018 Uiso 1 1 calc R . .
P2 P 0.13457(5) 0.91283(2) 0.82673(4) 0.01355(11) Uani 1 1 d . . .
P3 P 0.43807(5) 0.98108(2) 0.73622(5) 0.01715(12) Uani 1 1 d . . .
C12 C 0.31246(19) 0.77155(8) 0.71434(16) 0.0130(4) Uani 1 1 d . . .
C11 C 0.32562(19) 0.77739(8) 0.82891(16) 0.0123(4) Uani 1 1 d . . .
C13 C 0.2883(2) 0.71872(8) 0.66585(17) 0.0177(4) Uani 1 1 d . . .
H13 H 0.2860 0.7142 0.5902 0.021 Uiso 1 1 calc R . .
C14 C 0.2678(2) 0.67300(8) 0.72535(18) 0.0215(5) Uani 1 1 d . . .
H14 H 0.2509 0.6376 0.6906 0.026 Uiso 1 1 calc R . .
C15 C 0.2720(2) 0.67916(8) 0.83545(18) 0.0195(5) Uani 1 1 d . . .
H15 H 0.2542 0.6482 0.8760 0.023 Uiso 1 1 calc R . .
C16 C 0.3021(2) 0.73050(8) 0.88673(17) 0.0165(4) Uani 1 1 d . . .
H16 H 0.3070 0.7341 0.9631 0.020 Uiso 1 1 calc R . .
C22 C 0.1882(2) 0.87742(8) 0.96274(16) 0.0162(4) Uani 1 1 d . . .
C21 C 0.3031(2) 0.84337(8) 0.98238(16) 0.0139(4) Uani 1 1 d . . .
C23 C 0.1256(2) 0.88392(9) 1.04636(18) 0.0233(5) Uani 1 1 d . . .
H23 H 0.0454 0.9057 1.0322 0.028 Uiso 1 1 calc R . .
C24 C 0.1791(2) 0.85897(9) 1.14957(18) 0.0257(5) Uani 1 1 d . . .
H24 H 0.1355 0.8635 1.2057 0.031 Uiso 1 1 calc R . .
C25 C 0.2963(2) 0.82744(8) 1.17066(17) 0.0216(5) Uani 1 1 d . . .
H25 H 0.3347 0.8111 1.2421 0.026 Uiso 1 1 calc R . .
C26 C 0.3582(2) 0.81956(8) 1.08791(16) 0.0171(4) Uani 1 1 d . . .
H26 H 0.4386 0.7978 1.1031 0.020 Uiso 1 1 calc R . .
C31 C 0.6124(2) 0.97107(9) 0.7320(2) 0.0278(5) Uani 1 1 d . . .
H31A H 0.6124 0.9447 0.6726 0.042 Uiso 1 1 calc R . .
H31B H 0.6687 0.9564 0.8038 0.042 Uiso 1 1 calc R . .
H31C H 0.6495 1.0067 0.7171 0.042 Uiso 1 1 calc R . .
C32 C 0.3622(3) 1.01382(10) 0.6000(2) 0.0356(6) Uani 1 1 d . . .
H32A H 0.3604 0.9871 0.5407 0.053 Uiso 1 1 calc R . .
H32B H 0.4164 1.0463 0.5929 0.053 Uiso 1 1 calc R . .
H32C H 0.2691 1.0256 0.5935 0.053 Uiso 1 1 calc R . .
C33 C 0.4656(2) 1.04266(9) 0.8262(2) 0.0297(5) Uani 1 1 d . . .
H33A H 0.5180 1.0703 0.7992 0.045 Uiso 1 1 calc R . .
H33B H 0.5161 1.0321 0.9028 0.045 Uiso 1 1 calc R . .
H33C H 0.3776 1.0585 0.8248 0.045 Uiso 1 1 calc R . .
C41 C 0.1569(2) 0.83120(8) 0.51212(16) 0.0151(4) Uani 1 1 d . . .
H41 H 0.0833 0.8204 0.5449 0.018 Uiso 1 1 calc R . .
C42 C 0.4498(2) 0.81260(8) 0.56574(16) 0.0162(4) Uani 1 1 d . . .
H42 H 0.4183 0.7776 0.5228 0.019 Uiso 1 1 calc R . .
C43 C 0.1218(2) 0.89011(9) 0.46509(17) 0.0208(5) Uani 1 1 d . . .
H43A H 0.1855 0.9012 0.4248 0.031 Uiso 1 1 calc R . .
H43B H 0.1287 0.9161 0.5265 0.031 Uiso 1 1 calc R . .
H43C H 0.0288 0.8906 0.4139 0.031 Uiso 1 1 calc R . .
C44 C 0.1475(2) 0.79022(9) 0.41706(17) 0.0193(4) Uani 1 1 d . . .
H44A H 0.0606 0.7953 0.3586 0.029 Uiso 1 1 calc R . .
H44B H 0.1535 0.7521 0.4457 0.029 Uiso 1 1 calc R . .
H44C H 0.2226 0.7970 0.3860 0.029 Uiso 1 1 calc R . .
C45 C 0.4695(2) 0.85690(9) 0.48451(17) 0.0203(5) Uani 1 1 d . . .
H45A H 0.5402 0.8447 0.4522 0.030 Uiso 1 1 calc R . .
H45B H 0.4971 0.8920 0.5246 0.030 Uiso 1 1 calc R . .
H45C H 0.3838 0.8623 0.4248 0.030 Uiso 1 1 calc R . .
C46 C 0.5858(2) 0.80074(9) 0.65435(18) 0.0224(5) Uani 1 1 d . . .
H46A H 0.6524 0.7883 0.6179 0.034 Uiso 1 1 calc R . .
H46B H 0.5732 0.7716 0.7049 0.034 Uiso 1 1 calc R . .
H46C H 0.6188 0.8347 0.6970 0.034 Uiso 1 1 calc R . .
C51 C -0.0360(2) 0.87909(8) 0.76584(17) 0.0184(4) Uani 1 1 d . . .
H51 H -0.0942 0.8891 0.8138 0.022 Uiso 1 1 calc R . .
C52 C 0.0845(2) 0.98315(8) 0.86488(17) 0.0192(4) Uani 1 1 d . . .
H52 H 0.0006 0.9794 0.8885 0.023 Uiso 1 1 calc R . .
C53 C -0.1084(2) 0.89886(9) 0.64709(18) 0.0247(5) Uani 1 1 d . . .
H53A H -0.0485 0.8936 0.6005 0.037 Uiso 1 1 calc R . .
H53B H -0.1311 0.9384 0.6484 0.037 Uiso 1 1 calc R . .
H53C H -0.1921 0.8773 0.6163 0.037 Uiso 1 1 calc R . .
C54 C -0.0206(2) 0.81582(9) 0.7674(2) 0.0263(5) Uani 1 1 d . . .
H54A H -0.1100 0.7987 0.7347 0.039 Uiso 1 1 calc R . .
H54B H 0.0180 0.8031 0.8446 0.039 Uiso 1 1 calc R . .
H54C H 0.0400 0.8052 0.7240 0.039 Uiso 1 1 calc R . .
C55 C 0.1983(2) 1.00752(9) 0.96142(18) 0.0248(5) Uani 1 1 d . . .
H55A H 0.2848 1.0049 0.9445 0.037 Uiso 1 1 calc R . .
H55B H 0.2046 0.9867 1.0298 0.037 Uiso 1 1 calc R . .
H55C H 0.1784 1.0466 0.9719 0.037 Uiso 1 1 calc R . .
C56 C 0.0548(2) 1.02229(9) 0.76451(19) 0.0266(5) Uani 1 1 d . . .
H56A H 0.1338 1.0235 0.7366 0.040 Uiso 1 1 calc R . .
H56B H 0.0362 1.0597 0.7872 0.040 Uiso 1 1 calc R . .
H56C H -0.0246 1.0087 0.7055 0.040 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 C1 2.2242(18) . ?
Pd C2 2.2613(19) . ?
Pd P3 2.3140(5) . ?
Pd P2 2.3196(5) . ?
Pd P1 2.3978(5) . ?
C1 C2 1.398(3) . ?
C1 C21 1.504(3) . ?
C1 C11 1.517(3) . ?
P1 C12 1.8402(19) . ?
P1 C42 1.864(2) . ?
P1 C41 1.876(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
P2 C22 1.839(2) . ?
P2 C52 1.873(2) . ?
P2 C51 1.877(2) . ?
P3 C31 1.830(2) . ?
P3 C32 1.832(2) . ?
P3 C33 1.834(2) . ?
C12 C13 1.399(3) . ?
C12 C11 1.412(3) . ?
C11 C16 1.402(3) . ?
C13 C14 1.382(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C22 C23 1.398(3) . ?
C22 C21 1.399(3) . ?
C21 C26 1.398(3) . ?
C23 C24 1.384(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C41 C44 1.530(3) . ?
C41 C43 1.536(3) . ?
C41 H41 1.0000 . ?
C42 C46 1.531(3) . ?
C42 C45 1.532(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 C53 1.529(3) . ?
C51 C54 1.530(3) . ?
C51 H51 1.0000 . ?
C52 C55 1.527(3) . ?
C52 C56 1.529(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
C1 Pd C2 36.30(7) . . ?
C1 Pd P3 139.94(5) . . ?
C2 Pd P3 104.50(5) . . ?
C1 Pd P2 82.92(5) . . ?
C2 Pd P2 111.89(5) . . ?
P3 Pd P2 118.946(19) . . ?
C1 Pd P1 86.06(5) . . ?
C2 Pd P1 92.61(5) . . ?
P3 Pd P1 109.332(19) . . ?
P2 Pd P1 115.868(19) . . ?
C2 C1 C21 117.82(17) . . ?
C2 C1 C11 120.48(17) . . ?
C21 C1 C11 116.01(16) . . ?
C2 C1 Pd 73.29(11) . . ?
C21 C1 Pd 109.62(12) . . ?
C11 C1 Pd 110.10(12) . . ?
C12 P1 C42 100.11(9) . . ?
C12 P1 C41 104.48(9) . . ?
C42 P1 C41 102.78(9) . . ?
C12 P1 Pd 98.37(6) . . ?
C42 P1 Pd 129.83(7) . . ?
C41 P1 Pd 116.92(6) . . ?
C1 C2 Pd 70.40(11) . . ?
C1 C2 H2A 116.6 . . ?
Pd C2 H2A 116.6 . . ?
C1 C2 H2B 116.6 . . ?
Pd C2 H2B 116.6 . . ?
H2A C2 H2B 113.6 . . ?
C22 P2 C52 102.07(9) . . ?
C22 P2 C51 99.22(9) . . ?
C52 P2 C51 101.46(9) . . ?
C22 P2 Pd 100.20(7) . . ?
C52 P2 Pd 120.10(7) . . ?
C51 P2 Pd 128.50(7) . . ?
C31 P3 C32 100.09(12) . . ?
C31 P3 C33 98.85(11) . . ?
C32 P3 C33 99.91(12) . . ?
C31 P3 Pd 115.87(8) . . ?
C32 P3 Pd 116.29(8) . . ?
C33 P3 Pd 122.09(8) . . ?
C13 C12 C11 118.97(18) . . ?
C13 C12 P1 121.94(15) . . ?
C11 C12 P1 119.00(14) . . ?
C16 C11 C12 118.04(18) . . ?
C16 C11 C1 119.06(17) . . ?
C12 C11 C1 122.89(17) . . ?
C14 C13 C12 121.57(19) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C15 C14 C13 119.60(19) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 119.83(19) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C11 121.75(19) . . ?
C15 C16 H16 119.1 . . ?
C11 C16 H16 119.1 . . ?
C23 C22 C21 119.39(18) . . ?
C23 C22 P2 124.73(16) . . ?
C21 C22 P2 115.84(15) . . ?
C26 C21 C22 119.14(18) . . ?
C26 C21 C1 119.62(17) . . ?
C22 C21 C1 121.24(17) . . ?
C24 C23 C22 120.8(2) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C25 C24 C23 119.7(2) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.26(19) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 120.55(19) . . ?
C25 C26 H26 119.7 . . ?
C21 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 . . ?
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 . . ?
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 . . ?
C44 C41 C43 110.01(16) . . ?
C44 C41 P1 118.77(14) . . ?
C43 C41 P1 108.81(13) . . ?
C44 C41 H41 106.2 . . ?
C43 C41 H41 106.2 . . ?
P1 C41 H41 106.2 . . ?
C46 C42 C45 109.76(17) . . ?
C46 C42 P1 110.95(14) . . ?
C45 C42 P1 111.35(14) . . ?
C46 C42 H42 108.2 . . ?
C45 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 . . ?
C53 C51 C54 109.90(18) . . ?
C53 C51 P2 112.61(14) . . ?
C54 C51 P2 110.14(14) . . ?
C53 C51 H51 108.0 . . ?
C54 C51 H51 108.0 . . ?
P2 C51 H51 108.0 . . ?
C55 C52 C56 109.49(18) . . ?
C55 C52 P2 110.22(14) . . ?
C56 C52 P2 110.30(14) . . ?
C55 C52 H52 108.9 . . ?
C56 C52 H52 108.9 . . ?
P2 C52 H52 108.9 . . ?
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         0.407
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.057
####################################################################### 
# 
# 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_cc251
_database_code_depnum_ccdc_archive 'CCDC 1058174'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H40 Cl2 P2 Pd'
_chemical_formula_weight         591.82

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   13.0569(14)
_cell_length_b                   16.8080(14)
_cell_length_c                   31.261(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.209(2)
_cell_angle_gamma                90.00
_cell_volume                     6849.8(11)
_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          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2448
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_T_max  0.7455
_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  ?
_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            38696
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6002
_reflns_number_gt                5140
_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)+(0.0209P)²+2.8935P] 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         6002
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0779
_refine_ls_wR_factor_gt          0.0751
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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 0.403208(18) 0.334601(15) 0.890946(8) 0.01602(8) Uani 1 1 d . . .
C1 C 0.4436(2) 0.20985(19) 0.97301(10) 0.0186(7) Uani 1 1 d . . .
H1 H 0.4376 0.2661 0.9627 0.022 Uiso 1 1 calc R . .
Cl1 Cl 0.22633(6) 0.36860(5) 0.88942(3) 0.02446(19) Uani 1 1 d . . .
P1 P 0.34981(6) 0.20549(5) 0.87347(3) 0.01857(19) Uani 1 1 d . . .
C2 C 0.4730(3) 0.2126(2) 1.02138(11) 0.0277(8) Uani 1 1 d . . .
H2A H 0.4773 0.1582 1.0327 0.042 Uiso 1 1 calc R . .
H2B H 0.4208 0.2423 1.0361 0.042 Uiso 1 1 calc R . .
H2C H 0.5396 0.2389 1.0262 0.042 Uiso 1 1 calc R . .
Cl2 Cl 0.43656(7) 0.47011(5) 0.90297(3) 0.0328(2) Uani 1 1 d . . .
P2 P 0.57394(6) 0.31313(5) 0.90471(3) 0.01832(19) Uani 1 1 d . . .
C12 C 0.2913(2) 0.1660(2) 0.92139(10) 0.0213(7) Uani 1 1 d . . .
C11 C 0.3403(2) 0.16972(19) 0.96279(10) 0.0183(7) Uani 1 1 d . . .
C13 C 0.1941(3) 0.1325(2) 0.91653(12) 0.0253(8) Uani 1 1 d . . .
H13 H 0.1596 0.1323 0.8890 0.030 Uiso 1 1 calc R . .
C14 C 0.1457(3) 0.0990(2) 0.95070(13) 0.0296(9) Uani 1 1 d . . .
H14 H 0.0799 0.0752 0.9463 0.036 Uiso 1 1 calc R . .
C15 C 0.1935(3) 0.1008(2) 0.99046(12) 0.0287(9) Uani 1 1 d . . .
H15 H 0.1619 0.0776 1.0141 0.034 Uiso 1 1 calc R . .
C16 C 0.2885(3) 0.1367(2) 0.99630(12) 0.0248(8) Uani 1 1 d . . .
H16 H 0.3199 0.1390 1.0244 0.030 Uiso 1 1 calc R . .
C21 C 0.5330(2) 0.1720(2) 0.95103(10) 0.0202(7) Uani 1 1 d . . .
C22 C 0.6007(2) 0.2127(2) 0.92514(10) 0.0198(7) Uani 1 1 d . . .
C23 C 0.6866(3) 0.1721(2) 0.91099(11) 0.0279(8) Uani 1 1 d . . .
H23 H 0.7344 0.2000 0.8948 0.033 Uiso 1 1 calc R . .
C24 C 0.7032(3) 0.0922(2) 0.92015(12) 0.0351(10) Uani 1 1 d . . .
H24 H 0.7617 0.0657 0.9103 0.042 Uiso 1 1 calc R . .
C25 C 0.6343(3) 0.0518(2) 0.94356(12) 0.0377(10) Uani 1 1 d . . .
H25 H 0.6434 -0.0035 0.9489 0.045 Uiso 1 1 calc R . .
C26 C 0.5517(3) 0.0911(2) 0.95948(12) 0.0309(9) Uani 1 1 d . . .
H26 H 0.5063 0.0626 0.9766 0.037 Uiso 1 1 calc R . .
C31 C 0.4364(3) 0.1245(2) 0.85593(11) 0.0272(8) Uani 1 1 d . . .
H31 H 0.5055 0.1356 0.8701 0.033 Uiso 1 1 calc R . .
C32 C 0.2437(3) 0.2123(2) 0.83131(11) 0.0310(9) Uani 1 1 d . . .
H32 H 0.1853 0.2376 0.8456 0.037 Uiso 1 1 calc R . .
C33 C 0.4059(3) 0.0416(2) 0.87072(15) 0.0421(10) Uani 1 1 d . . .
H33A H 0.3414 0.0257 0.8555 0.063 Uiso 1 1 calc R . .
H33B H 0.3969 0.0424 0.9016 0.063 Uiso 1 1 calc R . .
H33C H 0.4598 0.0035 0.8645 0.063 Uiso 1 1 calc R . .
C34 C 0.4513(3) 0.1229(3) 0.80729(12) 0.0410(11) Uani 1 1 d . . .
H34A H 0.3907 0.0994 0.7923 0.061 Uiso 1 1 calc R . .
H34B H 0.5119 0.0910 0.8017 0.061 Uiso 1 1 calc R . .
H34C H 0.4609 0.1773 0.7970 0.061 Uiso 1 1 calc R . .
C35 C 0.2710(3) 0.2704(3) 0.79609(13) 0.0476(12) Uani 1 1 d . . .
H35A H 0.3250 0.2473 0.7794 0.071 Uiso 1 1 calc R . .
H35B H 0.2954 0.3205 0.8091 0.071 Uiso 1 1 calc R . .
H35C H 0.2101 0.2807 0.7772 0.071 Uiso 1 1 calc R . .
C36 C 0.1992(3) 0.1350(3) 0.81069(14) 0.0469(12) Uani 1 1 d . . .
H36A H 0.1284 0.1444 0.7999 0.070 Uiso 1 1 calc R . .
H36B H 0.2004 0.0926 0.8322 0.070 Uiso 1 1 calc R . .
H36C H 0.2407 0.1191 0.7869 0.070 Uiso 1 1 calc R . .
C41 C 0.6389(3) 0.3820(2) 0.94404(12) 0.0280(8) Uani 1 1 d . . .
H41 H 0.6333 0.4365 0.9312 0.034 Uiso 1 1 calc R . .
C42 C 0.6503(3) 0.3286(2) 0.85717(12) 0.0296(8) Uani 1 1 d . . .
H42 H 0.7229 0.3135 0.8652 0.036 Uiso 1 1 calc R . .
C43 C 0.5898(3) 0.3863(2) 0.98697(13) 0.0358(10) Uani 1 1 d . . .
H43A H 0.5156 0.3939 0.9822 0.054 Uiso 1 1 calc R . .
H43B H 0.6190 0.4310 1.0036 0.054 Uiso 1 1 calc R . .
H43C H 0.6031 0.3366 1.0028 0.054 Uiso 1 1 calc R . .
C44 C 0.7534(3) 0.3639(3) 0.95072(16) 0.0526(13) Uani 1 1 d . . .
H44A H 0.7854 0.3663 0.9231 0.079 Uiso 1 1 calc R . .
H44B H 0.7626 0.3105 0.9630 0.079 Uiso 1 1 calc R . .
H44C H 0.7856 0.4032 0.9703 0.079 Uiso 1 1 calc R . .
C45 C 0.6133(3) 0.2771(3) 0.81971(13) 0.0385(10) Uani 1 1 d . . .
H45A H 0.5437 0.2933 0.8099 0.058 Uiso 1 1 calc R . .
H45B H 0.6127 0.2212 0.8287 0.058 Uiso 1 1 calc R . .
H45C H 0.6594 0.2835 0.7963 0.058 Uiso 1 1 calc R . .
C46 C 0.6492(3) 0.4162(3) 0.84395(15) 0.0447(11) Uani 1 1 d . . .
H46A H 0.6847 0.4224 0.8174 0.067 Uiso 1 1 calc R . .
H46B H 0.6840 0.4481 0.8666 0.067 Uiso 1 1 calc R . .
H46C H 0.5781 0.4344 0.8394 0.067 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 P2 2.2754(9) . ?
Pd P1 2.3348(9) . ?
Pd Cl2 2.3452(9) . ?
Pd Cl1 2.3771(8) . ?
C1 C11 1.526(5) . ?
C1 C21 1.527(4) . ?
C1 C2 1.540(5) . ?
C1 H1 1.0000 . ?
P1 C12 1.843(3) . ?
P1 C32 1.862(4) . ?
P1 C31 1.871(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
P2 C22 1.831(3) . ?
P2 C42 1.854(3) . ?
P2 C41 1.858(4) . ?
C12 C13 1.390(5) . ?
C12 C11 1.412(5) . ?
C11 C16 1.393(5) . ?
C13 C14 1.390(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.360(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.403(5) . ?
C21 C22 1.409(5) . ?
C22 C23 1.404(5) . ?
C23 C24 1.389(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.371(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.381(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C33 1.528(5) . ?
C31 C34 1.544(5) . ?
C31 H31 1.0000 . ?
C32 C35 1.529(6) . ?
C32 C36 1.549(6) . ?
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 1.521(5) . ?
C41 C44 1.529(5) . ?
C41 H41 1.0000 . ?
C42 C45 1.513(5) . ?
C42 C46 1.530(6) . ?
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 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 Pd P1 99.98(3) . . ?
P2 Pd Cl2 87.28(3) . . ?
P1 Pd Cl2 172.10(3) . . ?
P2 Pd Cl1 169.23(3) . . ?
P1 Pd Cl1 86.66(3) . . ?
Cl2 Pd Cl1 86.63(3) . . ?
C11 C1 C21 114.3(3) . . ?
C11 C1 C2 112.8(3) . . ?
C21 C1 C2 107.4(3) . . ?
C11 C1 H1 107.3 . . ?
C21 C1 H1 107.3 . . ?
C2 C1 H1 107.3 . . ?
C12 P1 C32 105.75(16) . . ?
C12 P1 C31 105.16(16) . . ?
C32 P1 C31 105.98(17) . . ?
C12 P1 Pd 106.04(11) . . ?
C32 P1 Pd 108.01(13) . . ?
C31 P1 Pd 124.55(12) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C22 P2 C42 107.93(16) . . ?
C22 P2 C41 105.80(17) . . ?
C42 P2 C41 101.38(17) . . ?
C22 P2 Pd 112.22(11) . . ?
C42 P2 Pd 113.04(12) . . ?
C41 P2 Pd 115.60(11) . . ?
C13 C12 C11 118.8(3) . . ?
C13 C12 P1 118.4(3) . . ?
C11 C12 P1 122.8(2) . . ?
C16 C11 C12 117.2(3) . . ?
C16 C11 C1 118.6(3) . . ?
C12 C11 C1 124.1(3) . . ?
C14 C13 C12 122.1(4) . . ?
C14 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C15 C14 C13 119.2(3) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 119.6(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C11 123.0(3) . . ?
C15 C16 H16 118.5 . . ?
C11 C16 H16 118.5 . . ?
C26 C21 C22 118.1(3) . . ?
C26 C21 C1 116.6(3) . . ?
C22 C21 C1 125.2(3) . . ?
C23 C22 C21 118.8(3) . . ?
C23 C22 P2 118.6(3) . . ?
C21 C22 P2 122.3(2) . . ?
C24 C23 C22 121.6(4) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C25 C24 C23 119.3(3) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C24 C25 C26 120.3(4) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 121.8(4) . . ?
C25 C26 H26 119.1 . . ?
C21 C26 H26 119.1 . . ?
C33 C31 C34 109.4(3) . . ?
C33 C31 P1 113.7(3) . . ?
C34 C31 P1 114.4(3) . . ?
C33 C31 H31 106.2 . . ?
C34 C31 H31 106.2 . . ?
P1 C31 H31 106.2 . . ?
C35 C32 C36 109.5(3) . . ?
C35 C32 P1 110.8(3) . . ?
C36 C32 P1 119.3(3) . . ?
C35 C32 H32 105.4 . . ?
C36 C32 H32 105.4 . . ?
P1 C32 H32 105.4 . . ?
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 . . ?
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 110.2(3) . . ?
C43 C41 P2 114.5(2) . . ?
C44 C41 P2 111.9(3) . . ?
C43 C41 H41 106.6 . . ?
C44 C41 H41 106.6 . . ?
P2 C41 H41 106.6 . . ?
C45 C42 C46 110.1(3) . . ?
C45 C42 P2 112.2(3) . . ?
C46 C42 P2 110.7(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 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.077
# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.038 0.690 0.250 1006 354 ' '
2 0.076 0.233 0.750 1006 354 ' '
_platon_squeeze_details          
'A disordered molecule of chloroform and one of dichloromethane was sqeezed using PLATON'
####################################################################### 
# 
# 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_cc254
_database_code_depnum_ccdc_archive 'CCDC 1058175'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H39 Cl P2 Pd'
_chemical_formula_weight         555.36

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   11.2685(8)
_cell_length_b                   20.7303(14)
_cell_length_c                   23.1605(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.2340(13)
_cell_angle_gamma                90.00
_cell_volume                     5340.2(6)
_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          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2304
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7137
_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  ?
_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            62725
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9411
_reflns_number_gt                7826
_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)+(0.0230P)²+12.8625P] 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         9411
_refine_ls_number_parameters     569
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.0867
_refine_ls_wR_factor_gt          0.0827
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.004
_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
C12 C 0.5034(4) 0.2251(2) 0.47734(19) 0.0298(10) Uani 1 1 d . A 1
C22 C 0.6189(4) 0.1951(2) 0.4586(2) 0.0333(11) Uani 1 1 d . A 1
H22A H 0.6031 0.1501 0.4468 0.050 Uiso 1 1 calc R A 1
H22B H 0.6852 0.1968 0.4915 0.050 Uiso 1 1 calc R A 1
H22C H 0.6406 0.2196 0.4256 0.050 Uiso 1 1 calc R A 1
Pd3 Pd 0.439(2) 0.1817(7) 0.5558(4) 0.030(2) Uani 0.131(12) 1 d P A 2
Cl2 Cl 0.45948(9) 0.09518(5) 0.62723(5) 0.0274(2) Uani 1 1 d . . .
Pd2 Pd 0.4786(2) 0.16822(9) 0.54898(5) 0.0155(4) Uani 0.869(12) 1 d P A .
P22 P 0.30408(10) 0.13795(5) 0.49142(5) 0.0252(2) Uani 1 1 d . . .
P21 P 0.62632(10) 0.23339(5) 0.60021(5) 0.0223(2) Uani 1 1 d . . .
Pd1 Pd 0.08191(3) 0.511401(14) 0.308263(14) 0.01813(9) Uani 1 1 d . . .
Cl1 Cl 0.09327(10) 0.62588(5) 0.29280(5) 0.0330(3) Uani 1 1 d . . .
C11 C 0.0853(3) 0.41436(18) 0.33183(17) 0.0182(8) Uani 1 1 d . . .
P11 P 0.22457(9) 0.47953(5) 0.25065(5) 0.0191(2) Uani 1 1 d . . .
P12 P -0.09210(9) 0.51448(5) 0.34486(5) 0.0206(2) Uani 1 1 d . . .
C21 C 0.2024(3) 0.4071(2) 0.37683(18) 0.0225(9) Uani 1 1 d . . .
H21A H 0.2710 0.4222 0.3593 0.034 Uiso 1 1 calc R . .
H21B H 0.2141 0.3617 0.3879 0.034 Uiso 1 1 calc R . .
H21C H 0.1960 0.4330 0.4116 0.034 Uiso 1 1 calc R . .
C31 C 0.0956(3) 0.37538(18) 0.27703(17) 0.0179(8) Uani 1 1 d . . .
C32 C 0.1788(3) 0.39557(18) 0.24116(17) 0.0186(8) Uani 1 1 d . . .
C33 C 0.2088(3) 0.35674(19) 0.19694(17) 0.0215(9) Uani 1 1 d . . .
H33 H 0.2700 0.3698 0.1756 0.026 Uiso 1 1 calc R . .
C34 C 0.1491(4) 0.2988(2) 0.18408(19) 0.0264(10) Uani 1 1 d . . .
H34 H 0.1711 0.2711 0.1549 0.032 Uiso 1 1 calc R . .
C35 C 0.0571(4) 0.2815(2) 0.21410(19) 0.0267(10) Uani 1 1 d . . .
H35 H 0.0112 0.2438 0.2031 0.032 Uiso 1 1 calc R . .
C36 C 0.0314(3) 0.31892(19) 0.26011(18) 0.0232(9) Uani 1 1 d . . .
H36 H -0.0312 0.3059 0.2806 0.028 Uiso 1 1 calc R . .
C41 C -0.0164(3) 0.39225(19) 0.36368(17) 0.0206(9) Uani 1 1 d . . .
C43 C -0.2004(4) 0.4140(2) 0.40293(19) 0.0287(10) Uani 1 1 d . . .
H43 H -0.2622 0.4433 0.4088 0.034 Uiso 1 1 calc R . .
C42 C -0.1071(3) 0.43467(19) 0.37406(18) 0.0206(9) Uani 1 1 d . . .
C44 C -0.2029(4) 0.3516(2) 0.4228(2) 0.0326(11) Uani 1 1 d . . .
H44 H -0.2668 0.3375 0.4420 0.039 Uiso 1 1 calc R . .
C45 C -0.1115(4) 0.3094(2) 0.4147(2) 0.0305(10) Uani 1 1 d . . .
H45 H -0.1121 0.2664 0.4289 0.037 Uiso 1 1 calc R . .
C46 C -0.0195(4) 0.3295(2) 0.38596(19) 0.0274(10) Uani 1 1 d . . .
H46 H 0.0430 0.3001 0.3812 0.033 Uiso 1 1 calc R . .
C51 C 0.5321(4) 0.2951(2) 0.49934(19) 0.0289(10) Uani 1 1 d . . .
C52 C 0.6091(4) 0.3044(2) 0.55354(19) 0.0246(9) Uani 1 1 d . A .
C54 C 0.6182(4) 0.4188(2) 0.5359(2) 0.0358(11) Uani 1 1 d . A .
H54 H 0.6512 0.4601 0.5462 0.043 Uiso 1 1 calc R . .
C55 C 0.5330(4) 0.4109(2) 0.4863(2) 0.0391(12) Uani 1 1 d . . .
H55 H 0.5023 0.4478 0.4646 0.047 Uiso 1 1 calc R A .
C56 C 0.4915(4) 0.3503(2) 0.4676(2) 0.0347(11) Uani 1 1 d . A .
H56 H 0.4346 0.3462 0.4328 0.042 Uiso 1 1 calc R . .
C61 C 0.4043(4) 0.2213(2) 0.42489(19) 0.0331(11) Uani 1 1 d . . .
C62 C 0.3043(4) 0.1834(2) 0.42524(18) 0.0273(10) Uani 1 1 d . A .
C63 C 0.2183(5) 0.1761(2) 0.3751(2) 0.0413(13) Uani 1 1 d . . .
H63 H 0.1513 0.1485 0.3760 0.050 Uiso 1 1 calc R A .
C64 C 0.2295(6) 0.2080(2) 0.3247(2) 0.0526(16) Uani 1 1 d . A .
H64 H 0.1683 0.2052 0.2914 0.063 Uiso 1 1 calc R . .
C65 C 0.3308(6) 0.2443(3) 0.3228(2) 0.0476(15) Uani 1 1 d . . .
H65 H 0.3405 0.2653 0.2874 0.057 Uiso 1 1 calc R A .
C66 C 0.4180(5) 0.2510(2) 0.3708(2) 0.0415(12) Uani 1 1 d . A .
H66 H 0.4882 0.2755 0.3681 0.050 Uiso 1 1 calc R . .
C71 C -0.2309(4) 0.5222(2) 0.2908(2) 0.0315(11) Uani 1 1 d . . .
H71 H -0.3008 0.5143 0.3116 0.038 Uiso 1 1 calc R . .
C72 C -0.0998(4) 0.5764(2) 0.4014(2) 0.0357(11) Uani 1 1 d . . .
H72 H -0.0998 0.6190 0.3812 0.043 Uiso 1 1 calc R . .
C73 C -0.2332(4) 0.4705(3) 0.2438(2) 0.0446(13) Uani 1 1 d . . .
H73A H -0.3102 0.4723 0.2173 0.067 Uiso 1 1 calc R . .
H73B H -0.2234 0.4279 0.2623 0.067 Uiso 1 1 calc R . .
H73C H -0.1674 0.4782 0.2216 0.067 Uiso 1 1 calc R . .
C74 C -0.2441(5) 0.5891(3) 0.2650(3) 0.0531(15) Uani 1 1 d . . .
H74A H -0.1748 0.5987 0.2458 0.080 Uiso 1 1 calc R . .
H74B H -0.2483 0.6206 0.2961 0.080 Uiso 1 1 calc R . .
H74C H -0.3180 0.5914 0.2362 0.080 Uiso 1 1 calc R . .
C75 C 0.0132(5) 0.5743(3) 0.4457(2) 0.0459(13) Uani 1 1 d . . .
H75A H 0.0827 0.5829 0.4264 0.069 Uiso 1 1 calc R . .
H75B H 0.0216 0.5316 0.4640 0.069 Uiso 1 1 calc R . .
H75C H 0.0089 0.6071 0.4758 0.069 Uiso 1 1 calc R . .
C76 C -0.2127(5) 0.5755(3) 0.4309(2) 0.0514(15) Uani 1 1 d . . .
H76A H -0.2845 0.5723 0.4009 0.077 Uiso 1 1 calc R . .
H76B H -0.2162 0.6152 0.4534 0.077 Uiso 1 1 calc R . .
H76C H -0.2093 0.5382 0.4572 0.077 Uiso 1 1 calc R . .
C77 C 0.3923(3) 0.48509(19) 0.2656(2) 0.0255(10) Uani 1 1 d . . .
H77 H 0.4191 0.4920 0.2269 0.031 Uiso 1 1 calc R . .
C78 C 0.1884(4) 0.5105(2) 0.17456(19) 0.0290(10) Uani 1 1 d . . .
H78 H 0.2272 0.4811 0.1489 0.035 Uiso 1 1 calc R . .
C79 C 0.4261(4) 0.5456(2) 0.3015(3) 0.0512(16) Uani 1 1 d . . .
H79A H 0.5113 0.5554 0.3018 0.077 Uiso 1 1 calc R . .
H79B H 0.4118 0.5387 0.3417 0.077 Uiso 1 1 calc R . .
H79C H 0.3770 0.5819 0.2842 0.077 Uiso 1 1 calc R . .
C80 C 0.4574(4) 0.4258(2) 0.2922(2) 0.0330(11) Uani 1 1 d . . .
H80A H 0.4296 0.3879 0.2685 0.049 Uiso 1 1 calc R . .
H80B H 0.4406 0.4198 0.3321 0.049 Uiso 1 1 calc R . .
H80C H 0.5441 0.4312 0.2932 0.049 Uiso 1 1 calc R . .
C81 C 0.0529(4) 0.5082(2) 0.1536(2) 0.0409(12) Uani 1 1 d . . .
H81A H 0.0357 0.5202 0.1122 0.061 Uiso 1 1 calc R . .
H81B H 0.0127 0.5385 0.1766 0.061 Uiso 1 1 calc R . .
H81C H 0.0233 0.4644 0.1586 0.061 Uiso 1 1 calc R . .
C82 C 0.2363(5) 0.5785(2) 0.1673(2) 0.0431(13) Uani 1 1 d . . .
H82A H 0.2108 0.5930 0.1270 0.065 Uiso 1 1 calc R . .
H82B H 0.3243 0.5781 0.1761 0.065 Uiso 1 1 calc R . .
H82C H 0.2045 0.6079 0.1942 0.065 Uiso 1 1 calc R . .
C83 C 0.7894(4) 0.2129(2) 0.6167(2) 0.0306(10) Uani 1 1 d . A .
H83 H 0.8167 0.2252 0.6584 0.037 Uiso 1 1 calc R . .
C84 C 0.5950(4) 0.2647(2) 0.67091(19) 0.0286(10) Uani 1 1 d . A .
H84 H 0.6467 0.3037 0.6809 0.034 Uiso 1 1 calc R . .
C85 C 0.8701(4) 0.2496(2) 0.5808(2) 0.0391(12) Uani 1 1 d . . .
H85A H 0.8393 0.2443 0.5390 0.059 Uiso 1 1 calc R A .
H85B H 0.9521 0.2324 0.5894 0.059 Uiso 1 1 calc R . .
H85C H 0.8707 0.2955 0.5910 0.059 Uiso 1 1 calc R . .
C86 C 0.8054(4) 0.1399(2) 0.6135(2) 0.0448(13) Uani 1 1 d . . .
H86A H 0.7859 0.1258 0.5727 0.067 Uiso 1 1 calc R A .
H86B H 0.7517 0.1185 0.6369 0.067 Uiso 1 1 calc R . .
H86C H 0.8890 0.1287 0.6289 0.067 Uiso 1 1 calc R . .
C87 C 0.6253(5) 0.2170(2) 0.7204(2) 0.0404(12) Uani 1 1 d . . .
H87A H 0.5830 0.1763 0.7099 0.061 Uiso 1 1 calc R A .
H87B H 0.6003 0.2344 0.7559 0.061 Uiso 1 1 calc R . .
H87C H 0.7122 0.2092 0.7275 0.061 Uiso 1 1 calc R . .
C88 C 0.4637(4) 0.2865(2) 0.6648(2) 0.0412(12) Uani 1 1 d . . .
H88A H 0.4472 0.3184 0.6333 0.062 Uiso 1 1 calc R A .
H88B H 0.4494 0.3059 0.7017 0.062 Uiso 1 1 calc R . .
H88C H 0.4107 0.2492 0.6556 0.062 Uiso 1 1 calc R . .
C89 C 0.2750(4) 0.0542(2) 0.4674(2) 0.0399(12) Uani 1 1 d . A .
H89 H 0.1991 0.0537 0.4384 0.048 Uiso 1 1 calc R . .
C90 C 0.1713(4) 0.1658(2) 0.5228(2) 0.0376(12) Uani 1 1 d . A .
H90 H 0.1778 0.1477 0.5632 0.045 Uiso 1 1 calc R . .
C91 C 0.3755(5) 0.0323(2) 0.4365(2) 0.0464(13) Uani 1 1 d . . .
H91A H 0.3640 -0.0132 0.4257 0.070 Uiso 1 1 calc R A .
H91B H 0.4525 0.0377 0.4625 0.070 Uiso 1 1 calc R . .
H91C H 0.3754 0.0583 0.4011 0.070 Uiso 1 1 calc R . .
C92 C 0.2568(5) 0.0096(2) 0.5187(2) 0.0501(14) Uani 1 1 d . . .
H92A H 0.2416 -0.0346 0.5042 0.075 Uiso 1 1 calc R A .
H92B H 0.1879 0.0247 0.5360 0.075 Uiso 1 1 calc R . .
H92C H 0.3292 0.0102 0.5484 0.075 Uiso 1 1 calc R . .
C93 C 0.1794(4) 0.2400(2) 0.5280(2) 0.0415(12) Uani 1 1 d . . .
H93A H 0.1683 0.2591 0.4887 0.062 Uiso 1 1 calc R A .
H93B H 0.2585 0.2522 0.5492 0.062 Uiso 1 1 calc R . .
H93C H 0.1166 0.2558 0.5491 0.062 Uiso 1 1 calc R . .
C94 C 0.0513(4) 0.1451(3) 0.4886(3) 0.0595(17) Uani 1 1 d . . .
H94A H 0.0412 0.1638 0.4493 0.089 Uiso 1 1 calc R A .
H94B H -0.0136 0.1601 0.5088 0.089 Uiso 1 1 calc R . .
H94C H 0.0486 0.0980 0.4857 0.089 Uiso 1 1 calc R . .
C53 C 0.6552(4) 0.3650(2) 0.5706(2) 0.0282(10) Uani 1 1 d . . .
H53 H 0.7115 0.3697 0.6055 0.034 Uiso 1 1 calc R A .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C12 C61 1.514(6) . ?
C12 C51 1.555(6) . ?
C12 C22 1.566(6) . ?
C12 Pd2 2.091(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Pd3 Pd2 0.57(2) . ?
Pd3 P22 2.154(7) . ?
Pd3 Cl2 2.425(7) . ?
Pd3 P21 2.440(11) . ?
Cl2 Pd2 2.3978(12) . ?
Pd2 P22 2.2795(16) . ?
Pd2 P21 2.3176(13) . ?
P22 C62 1.799(5) . ?
P22 C89 1.836(5) . ?
P22 C90 1.856(5) . ?
P21 C52 1.818(4) . ?
P21 C84 1.847(4) . ?
P21 C83 1.865(4) . ?
Pd1 C11 2.083(4) . ?
Pd1 P12 2.2585(10) . ?
Pd1 P11 2.3430(10) . ?
Pd1 Cl1 2.4065(10) . ?
C11 C31 1.525(5) . ?
C11 C41 1.530(5) . ?
C11 C21 1.551(5) . ?
P11 C32 1.819(4) . ?
P11 C78 1.859(4) . ?
P11 C77 1.869(4) . ?
P12 C42 1.806(4) . ?
P12 C72 1.845(5) . ?
P12 C71 1.847(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C31 C36 1.399(5) . ?
C31 C32 1.412(5) . ?
C32 C33 1.387(5) . ?
C33 C34 1.386(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.385(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.398(5) . ?
C41 C46 1.403(6) . ?
C43 C44 1.376(6) . ?
C43 C42 1.400(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.387(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.383(6) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C56 1.396(6) . ?
C51 C52 1.420(6) . ?
C52 C53 1.392(6) . ?
C54 C55 1.383(7) . ?
C54 C53 1.398(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.386(7) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C62 1.375(6) . ?
C61 C66 1.425(6) . ?
C62 C63 1.397(6) . ?
C63 C64 1.366(7) . ?
C63 H63 0.9500 . ?
C64 C65 1.373(8) . ?
C64 H64 0.9500 . ?
C65 C66 1.367(7) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C74 1.508(6) . ?
C71 C73 1.524(7) . ?
C71 H71 1.0000 . ?
C72 C75 1.503(7) . ?
C72 C76 1.538(6) . ?
C72 H72 1.0000 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 C80 1.511(6) . ?
C77 C79 1.521(6) . ?
C77 H77 1.0000 . ?
C78 C82 1.527(6) . ?
C78 C81 1.527(6) . ?
C78 H78 1.0000 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 C86 1.526(6) . ?
C83 C85 1.530(6) . ?
C83 H83 1.0000 . ?
C84 C87 1.512(6) . ?
C84 C88 1.531(6) . ?
C84 H84 1.0000 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 C91 1.503(7) . ?
C89 C92 1.545(7) . ?
C89 H89 1.0000 . ?
C90 C94 1.516(6) . ?
C90 C93 1.545(7) . ?
C90 H90 1.0000 . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
C53 H53 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
C61 C12 C51 113.5(4) . . ?
C61 C12 C22 107.2(4) . . ?
C51 C12 C22 108.9(4) . . ?
C61 C12 Pd2 115.6(3) . . ?
C51 C12 Pd2 108.3(3) . . ?
C22 C12 Pd2 102.7(3) . . ?
Pd2 Pd3 P22 95.5(9) . . ?
Pd2 Pd3 Cl2 80.5(8) . . ?
P22 Pd3 Cl2 98.0(2) . . ?
Pd2 Pd3 P21 71.0(9) . . ?
P22 Pd3 P21 160.7(10) . . ?
Cl2 Pd3 P21 93.3(4) . . ?
Pd3 Pd2 C12 98.9(6) . . ?
Pd3 Pd2 P22 70.2(6) . . ?
C12 Pd2 P22 84.48(13) . . ?
Pd3 Pd2 P21 95.6(6) . . ?
C12 Pd2 P21 84.32(13) . . ?
P22 Pd2 P21 160.27(13) . . ?
Pd3 Pd2 Cl2 86.0(6) . . ?
C12 Pd2 Cl2 174.7(2) . . ?
P22 Pd2 Cl2 95.43(6) . . ?
P21 Pd2 Cl2 97.20(4) . . ?
C62 P22 C89 105.2(2) . . ?
C62 P22 C90 106.4(2) . . ?
C89 P22 C90 107.3(2) . . ?
C62 P22 Pd3 105.8(2) . . ?
C89 P22 Pd3 132.8(5) . . ?
C90 P22 Pd3 97.0(7) . . ?
C62 P22 Pd2 103.59(15) . . ?
C89 P22 Pd2 122.17(18) . . ?
C90 P22 Pd2 111.05(17) . . ?
C52 P21 C84 103.0(2) . . ?
C52 P21 C83 108.33(19) . . ?
C84 P21 C83 102.8(2) . . ?
C52 P21 Pd2 99.67(14) . . ?
C84 P21 Pd2 115.79(16) . . ?
C83 P21 Pd2 125.09(17) . . ?
C52 P21 Pd3 95.9(3) . . ?
C84 P21 Pd3 104.6(6) . . ?
C83 P21 Pd3 137.9(6) . . ?
C11 Pd1 P12 84.81(10) . . ?
C11 Pd1 P11 83.77(11) . . ?
P12 Pd1 P11 159.73(4) . . ?
C11 Pd1 Cl1 172.80(11) . . ?
P12 Pd1 Cl1 95.63(4) . . ?
P11 Pd1 Cl1 97.79(4) . . ?
C31 C11 C41 113.9(3) . . ?
C31 C11 C21 109.8(3) . . ?
C41 C11 C21 105.6(3) . . ?
C31 C11 Pd1 107.1(2) . . ?
C41 C11 Pd1 115.6(3) . . ?
C21 C11 Pd1 104.3(2) . . ?
C32 P11 C78 101.63(19) . . ?
C32 P11 C77 109.87(17) . . ?
C78 P11 C77 102.4(2) . . ?
C32 P11 Pd1 97.57(13) . . ?
C78 P11 Pd1 112.13(14) . . ?
C77 P11 Pd1 130.02(14) . . ?
C42 P12 C72 110.7(2) . . ?
C42 P12 C71 102.29(19) . . ?
C72 P12 C71 106.8(2) . . ?
C42 P12 Pd1 104.71(13) . . ?
C72 P12 Pd1 115.38(15) . . ?
C71 P12 Pd1 116.12(15) . . ?
C11 C21 H21A 109.5 . . ?
C11 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C11 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C36 C31 C32 116.5(4) . . ?
C36 C31 C11 124.9(3) . . ?
C32 C31 C11 118.6(3) . . ?
C33 C32 C31 121.8(4) . . ?
C33 C32 P11 123.2(3) . . ?
C31 C32 P11 114.5(3) . . ?
C34 C33 C32 119.6(4) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C35 C34 C33 119.6(4) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C34 C35 C36 120.5(4) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 121.4(4) . . ?
C35 C36 H36 119.3 . . ?
C31 C36 H36 119.3 . . ?
C42 C41 C46 117.3(4) . . ?
C42 C41 C11 121.3(3) . . ?
C46 C41 C11 121.3(3) . . ?
C44 C43 C42 120.3(4) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C41 C42 C43 121.0(4) . . ?
C41 C42 P12 113.4(3) . . ?
C43 C42 P12 125.6(3) . . ?
C43 C44 C45 119.5(4) . . ?
C43 C44 H44 120.3 . . ?
C45 C44 H44 120.3 . . ?
C46 C45 C44 120.4(4) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C41 121.4(4) . . ?
C45 C46 H46 119.3 . . ?
C41 C46 H46 119.3 . . ?
C56 C51 C52 117.1(4) . . ?
C56 C51 C12 124.0(4) . . ?
C52 C51 C12 118.8(4) . . ?
C53 C52 C51 121.4(4) . . ?
C53 C52 P21 124.2(3) . . ?
C51 C52 P21 114.1(3) . . ?
C55 C54 C53 119.1(4) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C54 C55 C56 121.4(4) . . ?
C54 C55 H55 119.3 . . ?
C56 C55 H55 119.3 . . ?
C55 C56 C51 120.8(4) . . ?
C55 C56 H56 119.6 . . ?
C51 C56 H56 119.6 . . ?
C62 C61 C66 117.1(4) . . ?
C62 C61 C12 121.6(4) . . ?
C66 C61 C12 120.8(4) . . ?
C61 C62 C63 121.1(4) . . ?
C61 C62 P22 114.7(3) . . ?
C63 C62 P22 123.8(4) . . ?
C64 C63 C62 120.8(5) . . ?
C64 C63 H63 119.6 . . ?
C62 C63 H63 119.6 . . ?
C63 C64 C65 118.9(5) . . ?
C63 C64 H64 120.6 . . ?
C65 C64 H64 120.6 . . ?
C66 C65 C64 121.5(5) . . ?
C66 C65 H65 119.2 . . ?
C64 C65 H65 119.2 . . ?
C65 C66 C61 120.3(5) . . ?
C65 C66 H66 119.8 . . ?
C61 C66 H66 119.8 . . ?
C74 C71 C73 111.9(4) . . ?
C74 C71 P12 111.6(3) . . ?
C73 C71 P12 109.8(3) . . ?
C74 C71 H71 107.8 . . ?
C73 C71 H71 107.8 . . ?
P12 C71 H71 107.8 . . ?
C75 C72 C76 111.5(4) . . ?
C75 C72 P12 109.5(3) . . ?
C76 C72 P12 116.3(3) . . ?
C75 C72 H72 106.3 . . ?
C76 C72 H72 106.3 . . ?
P12 C72 H72 106.3 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C72 C75 H75A 109.5 . . ?
C72 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C72 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C72 C76 H76A 109.5 . . ?
C72 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C72 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C80 C77 C79 112.7(4) . . ?
C80 C77 P11 115.8(3) . . ?
C79 C77 P11 108.0(3) . . ?
C80 C77 H77 106.6 . . ?
C79 C77 H77 106.6 . . ?
P11 C77 H77 106.6 . . ?
C82 C78 C81 110.3(4) . . ?
C82 C78 P11 113.3(3) . . ?
C81 C78 P11 110.2(3) . . ?
C82 C78 H78 107.6 . . ?
C81 C78 H78 107.6 . . ?
P11 C78 H78 107.6 . . ?
C77 C79 H79A 109.5 . . ?
C77 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C77 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C77 C80 H80A 109.5 . . ?
C77 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C77 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C78 C81 H81A 109.5 . . ?
C78 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C78 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C78 C82 H82A 109.5 . . ?
C78 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C78 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C86 C83 C85 112.4(4) . . ?
C86 C83 P21 109.7(3) . . ?
C85 C83 P21 115.3(3) . . ?
C86 C83 H83 106.3 . . ?
C85 C83 H83 106.3 . . ?
P21 C83 H83 106.3 . . ?
C87 C84 C88 111.1(4) . . ?
C87 C84 P21 112.9(3) . . ?
C88 C84 P21 110.0(3) . . ?
C87 C84 H84 107.5 . . ?
C88 C84 H84 107.5 . . ?
P21 C84 H84 107.5 . . ?
C83 C85 H85A 109.5 . . ?
C83 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C83 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C83 C86 H86A 109.5 . . ?
C83 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C83 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C84 C87 H87A 109.5 . . ?
C84 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C84 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C84 C88 H88A 109.5 . . ?
C84 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C84 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C91 C89 C92 112.9(4) . . ?
C91 C89 P22 108.6(4) . . ?
C92 C89 P22 111.9(3) . . ?
C91 C89 H89 107.8 . . ?
C92 C89 H89 107.8 . . ?
P22 C89 H89 107.8 . . ?
C94 C90 C93 111.0(4) . . ?
C94 C90 P22 114.6(3) . . ?
C93 C90 P22 107.4(3) . . ?
C94 C90 H90 107.9 . . ?
C93 C90 H90 107.9 . . ?
P22 C90 H90 107.9 . . ?
C89 C91 H91A 109.5 . . ?
C89 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C89 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C89 C92 H92A 109.5 . . ?
C89 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C89 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C90 C93 H93A 109.5 . . ?
C90 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C90 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C90 C94 H94A 109.5 . . ?
C90 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C90 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
C52 C53 C54 119.5(4) . . ?
C52 C53 H53 120.2 . . ?
C54 C53 H53 120.2 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.089
####################################################################### 
# 
# 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_cc56
_database_code_depnum_ccdc_archive 'CCDC 1058176'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H37 I P2 Pd'
_chemical_formula_weight         632.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   29.176(6)
_cell_length_b                   12.515(2)
_cell_length_c                   22.247(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.315(4)
_cell_angle_gamma                90.00
_cell_volume                     7835(2)
_cell_formula_units_Z            12
_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          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3792
_exptl_absorpt_coefficient_mu    2.025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6649
_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  ?
_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            55501
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0103
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_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         1.78
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6893
_reflns_number_gt                6564
_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)+(0.0123P)²+3.9621P] 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         6893
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0519
_refine_ls_wR_factor_gt          0.0511
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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
C67 C -0.0326(2) 0.2608(5) 0.2713(3) 0.0274(3) Uani 0.50 1 d P . 2
C69 C -0.0431(2) 0.1606(5) 0.2441(3) 0.0274(3) Uani 0.50 1 d P A 2
H69 H -0.0215 0.1262 0.2250 0.033 Uiso 0.50 1 calc PR A 2
C66 C -0.0527(2) 0.2590(5) 0.2412(3) 0.0274(3) Uani 0.50 1 d P . 1
C70 C -0.0660(2) 0.1541(5) 0.2216(3) 0.0274(3) Uani 0.50 1 d P . 1
H70 H -0.0547 0.1225 0.1894 0.033 Uiso 0.50 1 calc PR . 1
C64 C -0.09194(11) 0.1039(3) 0.24571(14) 0.0274(3) Uani 1 1 d . . .
H64 H -0.0951 0.0292 0.2382 0.033 Uiso 1 1 calc R A 1
I1 I 0.271888(7) 0.646317(15) 0.365308(9) 0.02369(5) Uani 1 1 d . . .
C1 C 0.39437(10) 0.4058(2) 0.46606(13) 0.0194(6) Uani 1 1 d . . .
H1 H 0.4121 0.3998 0.4334 0.023 Uiso 1 1 calc R . .
Pd1 Pd 0.337605(7) 0.506345(16) 0.426751(9) 0.01617(5) Uani 1 1 d . . .
P1 P 0.31054(2) 0.35751(6) 0.36599(3) 0.01717(14) Uani 1 1 d . . .
I2 I 0.0000 0.69270(2) 0.2500 0.02498(7) Uani 1 2 d S . .
Pd2 Pd -0.00594(4) 0.47853(3) 0.23895(3) 0.01438(17) Uani 0.50 1 d P . .
P2 P 0.36354(3) 0.59939(6) 0.51720(3) 0.01831(15) Uani 1 1 d . . .
P3 P -0.06005(3) 0.45376(6) 0.29734(4) 0.02435(17) Uani 1 1 d . . .
C3 C -0.01539(19) 0.3167(4) 0.2178(2) 0.0159(11) Uani 0.50 1 d P . .
H3 H -0.0267 0.3173 0.1739 0.019 Uiso 0.50 1 d P . .
C11 C 0.37607(10) 0.2939(2) 0.47133(13) 0.0196(6) Uani 1 1 d . . .
C12 C 0.34020(10) 0.2541(2) 0.42041(13) 0.0189(6) Uani 1 1 d . . .
C13 C 0.32637(10) 0.1472(2) 0.41872(14) 0.0217(6) Uani 1 1 d . . .
H13 H 0.3041 0.1199 0.3829 0.026 Uiso 1 1 calc R . .
C14 C 0.34504(11) 0.0804(2) 0.46918(15) 0.0266(7) Uani 1 1 d . . .
H14 H 0.3355 0.0077 0.4680 0.032 Uiso 1 1 calc R . .
C15 C 0.37763(11) 0.1208(2) 0.52116(15) 0.0262(7) Uani 1 1 d . . .
H15 H 0.3893 0.0763 0.5565 0.031 Uiso 1 1 calc R . .
C16 C 0.39344(10) 0.2258(2) 0.52215(14) 0.0235(6) Uani 1 1 d . . .
H16 H 0.4164 0.2516 0.5579 0.028 Uiso 1 1 calc R . .
C21 C 0.43089(10) 0.4491(2) 0.52306(13) 0.0223(6) Uani 1 1 d . . .
C22 C 0.42107(10) 0.5405(2) 0.55357(13) 0.0214(6) Uani 1 1 d . . .
C23 C 0.45474(11) 0.5803(3) 0.60619(14) 0.0272(7) Uani 1 1 d . . .
H23 H 0.4476 0.6415 0.6273 0.033 Uiso 1 1 calc R . .
C24 C 0.49820(11) 0.5299(3) 0.62705(15) 0.0319(7) Uani 1 1 d . . .
H24 H 0.5210 0.5566 0.6627 0.038 Uiso 1 1 calc R . .
C25 C 0.50869(11) 0.4411(3) 0.59638(16) 0.0332(8) Uani 1 1 d . . .
H25 H 0.5387 0.4072 0.6108 0.040 Uiso 1 1 calc R . .
C26 C 0.47551(11) 0.4011(3) 0.54443(15) 0.0284(7) Uani 1 1 d . . .
H26 H 0.4832 0.3405 0.5233 0.034 Uiso 1 1 calc R . .
C31 C 0.32089(11) 0.3272(2) 0.28938(14) 0.0242(6) Uani 1 1 d . . .
H31 H 0.3103 0.2523 0.2777 0.029 Uiso 1 1 calc R . .
C32 C 0.24592(10) 0.3413(2) 0.35603(13) 0.0213(6) Uani 1 1 d . . .
H32 H 0.2305 0.4067 0.3337 0.026 Uiso 1 1 calc R . .
C36 C 0.22246(11) 0.2461(3) 0.31670(14) 0.0284(7) Uani 1 1 d . . .
H36A H 0.1881 0.2484 0.3116 0.043 Uiso 1 1 calc R . .
H36B H 0.2354 0.1795 0.3376 0.043 Uiso 1 1 calc R . .
H36C H 0.2289 0.2494 0.2757 0.043 Uiso 1 1 calc R . .
C35 C 0.23516(11) 0.3420(3) 0.41967(14) 0.0293(7) Uani 1 1 d . . .
H35A H 0.2007 0.3391 0.4139 0.044 Uiso 1 1 calc R . .
H35B H 0.2478 0.4076 0.4420 0.044 Uiso 1 1 calc R . .
H35C H 0.2501 0.2798 0.4438 0.044 Uiso 1 1 calc R . .
C34 C 0.29222(11) 0.4026(3) 0.23943(14) 0.0282(7) Uani 1 1 d . . .
H34A H 0.3003 0.3896 0.2000 0.042 Uiso 1 1 calc R . .
H34B H 0.2998 0.4768 0.2524 0.042 Uiso 1 1 calc R . .
H34C H 0.2582 0.3899 0.2338 0.042 Uiso 1 1 calc R . .
C33 C 0.37407(12) 0.3354(3) 0.29457(16) 0.0328(7) Uani 1 1 d . . .
H33A H 0.3800 0.3161 0.2546 0.049 Uiso 1 1 calc R . .
H33B H 0.3915 0.2865 0.3270 0.049 Uiso 1 1 calc R . .
H33C H 0.3848 0.4088 0.3055 0.049 Uiso 1 1 calc R . .
C43 C 0.40940(14) 0.7730(3) 0.48481(17) 0.0411(9) Uani 1 1 d . . .
H43A H 0.4053 0.7328 0.4459 0.062 Uiso 1 1 calc R . .
H43B H 0.4399 0.7541 0.5137 0.062 Uiso 1 1 calc R . .
H43C H 0.4088 0.8497 0.4759 0.062 Uiso 1 1 calc R . .
C42 C 0.32747(11) 0.5722(2) 0.57239(13) 0.0250(6) Uani 1 1 d . . .
H42 H 0.3428 0.6090 0.6126 0.030 Uiso 1 1 calc R . .
C41 C 0.36929(12) 0.7455(2) 0.51405(14) 0.0273(7) Uani 1 1 d . . .
H41 H 0.3394 0.7717 0.4844 0.033 Uiso 1 1 calc R . .
C44 C 0.37399(14) 0.8065(3) 0.57491(15) 0.0379(8) Uani 1 1 d . . .
H44A H 0.3739 0.8835 0.5668 0.057 Uiso 1 1 calc R . .
H44B H 0.4038 0.7866 0.6050 0.057 Uiso 1 1 calc R . .
H44C H 0.3472 0.7886 0.5919 0.057 Uiso 1 1 calc R . .
C45 C 0.32662(12) 0.4521(3) 0.58528(15) 0.0311(7) Uani 1 1 d . . .
H45A H 0.3111 0.4145 0.5466 0.047 Uiso 1 1 calc R . .
H45B H 0.3089 0.4391 0.6164 0.047 Uiso 1 1 calc R . .
H45C H 0.3592 0.4259 0.6011 0.047 Uiso 1 1 calc R . .
C46 C 0.27719(12) 0.6163(3) 0.54834(16) 0.0349(8) Uani 1 1 d . . .
H46A H 0.2787 0.6935 0.5416 0.052 Uiso 1 1 calc R . .
H46B H 0.2592 0.6026 0.5791 0.052 Uiso 1 1 calc R . .
H46C H 0.2614 0.5813 0.5089 0.052 Uiso 1 1 calc R . .
C51 C -0.11538(11) 0.5207(2) 0.25533(13) 0.0237(6) Uani 1 1 d . . .
H51 H -0.1090 0.5993 0.2584 0.028 Uiso 1 1 calc R . .
C52 C -0.05156(12) 0.4810(3) 0.38051(15) 0.0330(8) Uani 1 1 d . . .
H52 H -0.0791 0.4500 0.3934 0.040 Uiso 1 1 calc R . .
C53 C -0.15841(11) 0.5008(3) 0.28087(15) 0.0311(7) Uani 1 1 d . . .
H53A H -0.1846 0.5474 0.2594 0.047 Uiso 1 1 calc R . .
H53B H -0.1499 0.5163 0.3256 0.047 Uiso 1 1 calc R . .
H53C H -0.1683 0.4260 0.2740 0.047 Uiso 1 1 calc R . .
C54 C -0.12646(15) 0.4913(3) 0.18617(15) 0.0427(9) Uani 1 1 d . . .
H54A H -0.1547 0.5304 0.1630 0.064 Uiso 1 1 calc R . .
H54B H -0.1324 0.4143 0.1812 0.064 Uiso 1 1 calc R . .
H54C H -0.0994 0.5104 0.1700 0.064 Uiso 1 1 calc R . .
C55 C -0.04938(15) 0.6002(3) 0.39489(19) 0.0514(8) Uani 1 1 d . . .
H55A H -0.0231 0.6325 0.3815 0.077 Uiso 1 1 calc R . .
H55B H -0.0442 0.6107 0.4398 0.077 Uiso 1 1 calc R . .
H55C H -0.0794 0.6339 0.3726 0.077 Uiso 1 1 calc R . .
C56 C -0.00661(14) 0.4238(3) 0.41657(19) 0.0514(8) Uani 1 1 d . . .
H56A H -0.0084 0.3483 0.4046 0.077 Uiso 1 1 calc R . .
H56B H -0.0036 0.4297 0.4614 0.077 Uiso 1 1 calc R . .
H56C H 0.0211 0.4568 0.4070 0.077 Uiso 1 1 calc R . .
C61 C -0.07152(11) 0.3109(2) 0.28764(15) 0.0274(3) Uani 1 1 d . . .
C62 C -0.10734(11) 0.2546(2) 0.30357(15) 0.0274(3) Uani 1 1 d . . .
H62 H -0.1254 0.2876 0.3283 0.033 Uiso 1 1 calc R . .
C63 C -0.11705(11) 0.1501(2) 0.28348(14) 0.0274(3) Uani 1 1 d . . .
H63 H -0.1409 0.1106 0.2957 0.033 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
C67 C69 1.391(9) . ?
C67 C61 1.427(7) . ?
C67 C3 1.525(8) 2 ?
C67 C3 1.572(8) . ?
C69 C64 1.602(7) . ?
C69 H69 0.9500 . ?
C66 C70 1.406(9) . ?
C66 C61 1.446(7) . ?
C66 C3 1.508(8) . ?
C70 C64 1.211(7) . ?
C70 H70 0.9500 . ?
C64 C63 1.379(4) . ?
C64 H64 0.9500 . ?
I1 Pd1 2.6887(4) . ?
C1 C11 1.515(4) . ?
C1 C21 1.524(4) . ?
C1 Pd1 2.080(3) . ?
C1 H1 1.0000 . ?
Pd1 P2 2.2744(8) . ?
Pd1 P1 2.3144(8) . ?
P1 C12 1.827(3) . ?
P1 C31 1.847(3) . ?
P1 C32 1.851(3) . ?
I2 Pd2 2.6930(6) . ?
I2 Pd2 2.6930(6) 2 ?
Pd2 Pd2 0.5212(9) 2 ?
Pd2 C3 2.082(5) . ?
Pd2 C3 2.259(5) 2 ?
Pd2 P3 2.2968(15) 2 ?
Pd2 P3 2.3151(15) . ?
P2 C22 1.816(3) . ?
P2 C41 1.839(3) . ?
P2 C42 1.848(3) . ?
P3 C61 1.821(3) . ?
P3 C52 1.833(4) . ?
P3 C51 1.840(3) . ?
P3 Pd2 2.2968(15) 2 ?
C3 C3 1.478(10) 2 ?
C3 C67 1.525(8) 2 ?
C3 Pd2 2.259(5) 2 ?
C3 H3 0.9440 . ?
C11 C16 1.400(4) . ?
C11 C12 1.414(4) . ?
C12 C13 1.395(4) . ?
C13 C14 1.390(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.391(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.398(4) . ?
C21 C26 1.398(4) . ?
C22 C23 1.406(4) . ?
C23 C24 1.382(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C34 1.528(4) . ?
C31 C33 1.529(4) . ?
C31 H31 1.0000 . ?
C32 C35 1.529(4) . ?
C32 C36 1.529(4) . ?
C32 H32 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C43 C41 1.521(5) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C42 C46 1.526(4) . ?
C42 C45 1.532(4) . ?
C42 H42 1.0000 . ?
C41 C44 1.529(4) . ?
C41 H41 1.0000 . ?
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(4) . ?
C51 C54 1.531(4) . ?
C51 H51 1.0000 . ?
C52 C55 1.523(5) . ?
C52 C56 1.523(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 1.382(4) . ?
C62 C63 1.387(4) . ?
C62 H62 0.9500 . ?
C63 H63 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
C69 C67 C61 114.1(6) . . ?
C69 C67 C3 124.8(6) . 2 ?
C61 C67 C3 121.1(5) . 2 ?
C69 C67 C3 98.6(5) . . ?
C61 C67 C3 115.6(5) . . ?
C3 C67 C3 57.0(4) 2 . ?
C67 C69 C64 119.0(5) . . ?
C67 C69 H69 120.5 . . ?
C64 C69 H69 120.5 . . ?
C70 C66 C61 120.9(5) . . ?
C70 C66 C3 120.4(6) . . ?
C61 C66 C3 118.5(5) . . ?
C64 C70 C66 120.1(6) . . ?
C64 C70 H70 120.0 . . ?
C66 C70 H70 120.0 . . ?
C70 C64 C63 123.1(4) . . ?
C63 C64 C69 116.5(3) . . ?
C70 C64 H64 118.4 . . ?
C63 C64 H64 118.4 . . ?
C69 C64 H64 118.6 . . ?
C11 C1 C21 116.6(2) . . ?
C11 C1 Pd1 109.52(18) . . ?
C21 C1 Pd1 116.03(19) . . ?
C11 C1 H1 104.4 . . ?
C21 C1 H1 104.4 . . ?
Pd1 C1 H1 104.4 . . ?
C1 Pd1 P2 84.02(8) . . ?
C1 Pd1 P1 82.51(8) . . ?
P2 Pd1 P1 155.68(3) . . ?
C1 Pd1 I1 171.75(8) . . ?
P2 Pd1 I1 98.17(2) . . ?
P1 Pd1 I1 98.05(2) . . ?
C12 P1 C31 107.58(13) . . ?
C12 P1 C32 106.93(13) . . ?
C31 P1 C32 106.07(13) . . ?
C12 P1 Pd1 98.88(9) . . ?
C31 P1 Pd1 126.19(10) . . ?
C32 P1 Pd1 109.73(10) . . ?
Pd2 Pd2 C3 103.23(14) 2 . ?
Pd2 Pd2 C3 63.79(13) 2 2 ?
C3 Pd2 C3 39.5(3) . 2 ?
Pd2 Pd2 P3 85.5(3) 2 2 ?
C3 Pd2 P3 82.08(15) . 2 ?
C3 Pd2 P3 82.34(14) 2 2 ?
Pd2 Pd2 P3 81.5(3) 2 . ?
C3 Pd2 P3 85.84(15) . . ?
C3 Pd2 P3 78.03(14) 2 . ?
P3 Pd2 P3 159.77(4) 2 . ?
Pd2 Pd2 I2 84.447(10) 2 . ?
C3 Pd2 I2 172.19(14) . . ?
C3 Pd2 I2 148.20(13) 2 . ?
P3 Pd2 I2 97.28(4) 2 . ?
P3 Pd2 I2 96.84(4) . . ?
C22 P2 C41 109.72(14) . . ?
C22 P2 C42 104.53(14) . . ?
C41 P2 C42 106.38(14) . . ?
C22 P2 Pd1 103.82(10) . . ?
C41 P2 Pd1 119.19(10) . . ?
C42 P2 Pd1 112.27(10) . . ?
C61 P3 C52 105.90(15) . . ?
C61 P3 C51 106.11(14) . . ?
C52 P3 C51 107.14(14) . . ?
C61 P3 Pd2 103.64(11) . 2 ?
C52 P3 Pd2 115.31(11) . 2 ?
C51 P3 Pd2 117.68(10) . 2 ?
C61 P3 Pd2 101.32(11) . . ?
C52 P3 Pd2 127.68(11) . . ?
C51 P3 Pd2 106.91(10) . . ?
C3 C3 C66 88.5(5) 2 . ?
C3 C3 C67 63.1(4) 2 2 ?
C66 C3 C67 116.1(5) . 2 ?
C3 C3 C67 59.9(4) 2 . ?
C67 C3 C67 97.9(5) 2 . ?
C3 C3 Pd2 76.70(14) 2 . ?
C66 C3 Pd2 116.9(4) . . ?
C67 C3 Pd2 110.4(4) 2 . ?
C67 C3 Pd2 108.1(4) . . ?
C3 C3 Pd2 63.76(13) 2 2 ?
C66 C3 Pd2 115.1(4) . 2 ?
C67 C3 Pd2 101.8(4) 2 2 ?
C67 C3 Pd2 100.5(3) . 2 ?
C3 C3 H3 163.8 2 . ?
C66 C3 H3 105.9 . . ?
C67 C3 H3 103.0 2 . ?
C67 C3 H3 133.8 . . ?
Pd2 C3 H3 102.4 . . ?
Pd2 C3 H3 114.5 2 . ?
C16 C11 C12 117.8(3) . . ?
C16 C11 C1 124.5(3) . . ?
C12 C11 C1 117.7(2) . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 P1 125.4(2) . . ?
C11 C12 P1 113.7(2) . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C11 121.0(3) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C22 C21 C26 118.6(3) . . ?
C22 C21 C1 120.5(3) . . ?
C26 C21 C1 120.9(3) . . ?
C21 C22 C23 120.4(3) . . ?
C21 C22 P2 113.6(2) . . ?
C23 C22 P2 126.0(2) . . ?
C24 C23 C22 119.7(3) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C25 C24 C23 120.3(3) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 120.6(3) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C34 C31 C33 111.3(2) . . ?
C34 C31 P1 110.7(2) . . ?
C33 C31 P1 109.1(2) . . ?
C34 C31 H31 108.6 . . ?
C33 C31 H31 108.6 . . ?
P1 C31 H31 108.6 . . ?
C35 C32 C36 111.3(3) . . ?
C35 C32 P1 109.90(19) . . ?
C36 C32 P1 116.2(2) . . ?
C35 C32 H32 106.2 . . ?
C36 C32 H32 106.2 . . ?
P1 C32 H32 106.2 . . ?
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 . . ?
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 . . ?
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 . . ?
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 . . ?
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 . . ?
C46 C42 C45 111.0(3) . . ?
C46 C42 P2 111.3(2) . . ?
C45 C42 P2 110.2(2) . . ?
C46 C42 H42 108.0 . . ?
C45 C42 H42 108.0 . . ?
P2 C42 H42 108.0 . . ?
C43 C41 C44 111.5(3) . . ?
C43 C41 P2 109.2(2) . . ?
C44 C41 P2 116.8(2) . . ?
C43 C41 H41 106.2 . . ?
C44 C41 H41 106.2 . . ?
P2 C41 H41 106.2 . . ?
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 111.0(3) . . ?
C53 C51 P3 115.7(2) . . ?
C54 C51 P3 109.0(2) . . ?
C53 C51 H51 106.9 . . ?
C54 C51 H51 106.9 . . ?
P3 C51 H51 106.9 . . ?
C55 C52 C56 111.5(3) . . ?
C55 C52 P3 112.4(2) . . ?
C56 C52 P3 108.2(3) . . ?
C55 C52 H52 108.2 . . ?
C56 C52 H52 108.2 . . ?
P3 C52 H52 108.2 . . ?
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 C67 123.3(4) . . ?
C62 C61 C66 114.2(4) . . ?
C62 C61 P3 126.7(2) . . ?
C67 C61 P3 109.1(3) . . ?
C66 C61 P3 115.6(3) . . ?
C61 C62 C63 120.1(3) . . ?
C61 C62 H62 119.9 . . ?
C63 C62 H62 119.9 . . ?
C64 C63 C62 119.7(3) . . ?
C64 C63 H63 120.1 . . ?
C62 C63 H63 120.1 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.412
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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_cc298
_database_code_depnum_ccdc_archive 'CCDC 1058177'
_audit_update_record             
;
2015-04-06 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51 H78 Br4 Cl2 P4 Pd2'
_chemical_formula_weight         1418.35

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'
Br Br -0.2901 2.4595 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   10.3876(9)
_cell_length_b                   16.2993(14)
_cell_length_c                   17.0895(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.4770(14)
_cell_angle_gamma                90.00
_cell_volume                     2813.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9847
_cell_measurement_theta_min      2.237
_cell_measurement_theta_max      23.629

_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    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1420
_exptl_absorpt_coefficient_mu    3.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5977
_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            50587
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4956
_reflns_number_gt                4411
_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)+(0.0211P)²+1.6590P] 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         4956
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0435
_refine_ls_wR_factor_gt          0.0423
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 0.395156(15) 0.403540(9) 0.721214(9) 0.01237(5) Uani 1 1 d . . .
Br1 Br 0.49003(2) 0.545123(13) 0.739042(15) 0.02224(6) Uani 1 1 d . . .
P1 P 0.61024(5) 0.35928(3) 0.72070(3) 0.01487(12) Uani 1 1 d . . .
P2 P 0.27881(5) 0.28512(3) 0.68228(3) 0.01305(12) Uani 1 1 d . . .
Br2 Br 0.18270(2) 0.466668(13) 0.732010(15) 0.02282(6) Uani 1 1 d . . .
C C 0.4226(2) 0.34341(13) 0.54284(13) 0.0148(4) Uani 1 1 d . . .
H1 H 0.3720 0.3511 0.4866 0.018 Uiso 1 1 calc R . .
H2 H 0.3751 0.3733 0.5780 0.018 Uiso 1 1 calc R . .
C11 C 0.5573(2) 0.38260(13) 0.55160(13) 0.0159(5) Uani 1 1 d . . .
C12 C 0.6446(2) 0.39761(13) 0.62652(13) 0.0161(5) Uani 1 1 d . . .
C13 C 0.7599(2) 0.44243(14) 0.62756(15) 0.0224(5) Uani 1 1 d . . .
H13 H 0.8172 0.4560 0.6778 0.027 Uiso 1 1 calc R . .
C14 C 0.7928(2) 0.46752(14) 0.55758(16) 0.0265(6) Uani 1 1 d . . .
H14 H 0.8724 0.4972 0.5601 0.032 Uiso 1 1 calc R . .
C15 C 0.7099(2) 0.44941(14) 0.48379(15) 0.0244(5) Uani 1 1 d . . .
H15 H 0.7332 0.4648 0.4353 0.029 Uiso 1 1 calc R . .
C16 C 0.5924(2) 0.40860(13) 0.48176(14) 0.0204(5) Uani 1 1 d . . .
H16 H 0.5338 0.3980 0.4312 0.024 Uiso 1 1 calc R . .
C21 C 0.4219(2) 0.25286(13) 0.56285(12) 0.0143(4) Uani 1 1 d . . .
C22 C 0.3565(2) 0.21949(13) 0.61934(12) 0.0141(4) Uani 1 1 d . . .
C23 C 0.3576(2) 0.13442(13) 0.63028(13) 0.0185(5) Uani 1 1 d . . .
H23 H 0.3104 0.1113 0.6663 0.022 Uiso 1 1 calc R . .
C24 C 0.4260(2) 0.08330(14) 0.58972(14) 0.0231(5) Uani 1 1 d . . .
H24 H 0.4255 0.0257 0.5979 0.028 Uiso 1 1 calc R . .
C25 C 0.4951(2) 0.11613(14) 0.53724(14) 0.0241(5) Uani 1 1 d . . .
H25 H 0.5456 0.0815 0.5111 0.029 Uiso 1 1 calc R . .
C26 C 0.4905(2) 0.19980(14) 0.52280(13) 0.0198(5) Uani 1 1 d . . .
H26 H 0.5351 0.2216 0.4848 0.024 Uiso 1 1 calc R . .
C31 C 0.7298(2) 0.41123(16) 0.80335(14) 0.0261(6) Uani 1 1 d . . .
H31 H 0.7263 0.4707 0.7885 0.031 Uiso 1 1 calc R . .
C32 C 0.6620(2) 0.24818(14) 0.72453(13) 0.0186(5) Uani 1 1 d . . .
H32 H 0.5815 0.2165 0.6974 0.022 Uiso 1 1 calc R . .
C33 C 0.6844(3) 0.4066(2) 0.88244(16) 0.0424(8) Uani 1 1 d . . .
H33A H 0.5899 0.4198 0.8722 0.064 Uiso 1 1 calc R . .
H33B H 0.7349 0.4460 0.9210 0.064 Uiso 1 1 calc R . .
H33C H 0.6994 0.3511 0.9047 0.064 Uiso 1 1 calc R . .
C5 C 0.4278(15) 0.5135(6) 0.9606(9) 0.043(3) Uani 0.50 1 d P A -1
H5A H 0.4447 0.5201 0.9063 0.052 Uiso 0.50 1 calc PR A -1
H5B H 0.3698 0.5591 0.9693 0.052 Uiso 0.50 1 calc PR A -1
Cl52 Cl 0.34493(16) 0.41964(9) 0.96465(9) 0.0448(4) Uani 0.50 1 d P A -1
Cl51 Cl 0.5775(3) 0.51970(16) 1.0320(2) 0.0446(7) Uani 0.50 1 d P A -1
C34 C 0.8769(2) 0.38661(17) 0.81821(16) 0.0310(6) Uani 1 1 d . . .
H34A H 0.9029 0.3840 0.7667 0.046 Uiso 1 1 calc R . .
H34B H 0.8898 0.3327 0.8443 0.046 Uiso 1 1 calc R . .
H34C H 0.9314 0.4274 0.8530 0.046 Uiso 1 1 calc R . .
C35 C 0.7672(2) 0.23084(14) 0.67644(14) 0.0227(5) Uani 1 1 d . . .
H35A H 0.7329 0.2471 0.6202 0.034 Uiso 1 1 calc R . .
H35B H 0.7881 0.1721 0.6790 0.034 Uiso 1 1 calc R . .
H35C H 0.8475 0.2623 0.6995 0.034 Uiso 1 1 calc R . .
C36 C 0.7074(2) 0.21172(17) 0.80940(15) 0.0325(6) Uani 1 1 d . . .
H36A H 0.7010 0.1518 0.8063 0.049 Uiso 1 1 calc R . .
H36B H 0.6507 0.2325 0.8435 0.049 Uiso 1 1 calc R . .
H36C H 0.7994 0.2276 0.8325 0.049 Uiso 1 1 calc R . .
C41 C 0.2548(2) 0.22043(13) 0.76663(13) 0.0179(5) Uani 1 1 d . . .
H41 H 0.2120 0.1682 0.7433 0.021 Uiso 1 1 calc R . .
C42 C 0.1085(2) 0.29878(13) 0.61879(13) 0.0174(5) Uani 1 1 d . . .
H42 H 0.0548 0.3260 0.6529 0.021 Uiso 1 1 calc R . .
C43 C 0.1622(2) 0.26151(15) 0.81267(15) 0.0273(6) Uani 1 1 d . . .
H43A H 0.0750 0.2697 0.7764 0.041 Uiso 1 1 calc R . .
H43B H 0.1991 0.3147 0.8334 0.041 Uiso 1 1 calc R . .
H43C H 0.1533 0.2264 0.8577 0.041 Uiso 1 1 calc R . .
C44 C 0.3858(2) 0.19839(15) 0.82388(14) 0.0256(5) Uani 1 1 d . . .
H44A H 0.4423 0.1697 0.7942 0.038 Uiso 1 1 calc R . .
H44B H 0.3692 0.1627 0.8666 0.038 Uiso 1 1 calc R . .
H44C H 0.4302 0.2486 0.8477 0.038 Uiso 1 1 calc R . .
C45 C 0.0426(2) 0.21639(14) 0.59144(15) 0.0237(5) Uani 1 1 d . . .
H45A H -0.0495 0.2256 0.5627 0.036 Uiso 1 1 calc R . .
H45B H 0.0449 0.1816 0.6385 0.036 Uiso 1 1 calc R . .
H45C H 0.0903 0.1892 0.5555 0.036 Uiso 1 1 calc R . .
C46 C 0.1027(2) 0.35380(15) 0.54563(14) 0.0231(5) Uani 1 1 d . . .
H46A H 0.1493 0.3271 0.5088 0.035 Uiso 1 1 calc R . .
H46B H 0.1450 0.4065 0.5633 0.035 Uiso 1 1 calc R . .
H46C H 0.0101 0.3631 0.5179 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 P2 2.2922(6) . ?
Pd P1 2.3497(6) . ?
Pd Br2 2.4806(3) . ?
Pd Br1 2.4999(3) . ?
P1 C12 1.837(2) . ?
P1 C31 1.854(2) . ?
P1 C32 1.886(2) . ?
P2 C22 1.832(2) . ?
P2 C41 1.849(2) . ?
P2 C42 1.861(2) . ?
C C11 1.513(3) . ?
C C21 1.515(3) . ?
C H1 0.9900 . ?
C H2 0.9900 . ?
C11 C16 1.392(3) . ?
C11 C12 1.407(3) . ?
C12 C13 1.400(3) . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.397(3) . ?
C21 C22 1.412(3) . ?
C22 C23 1.399(3) . ?
C23 C24 1.382(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C33 1.534(3) . ?
C31 C34 1.542(3) . ?
C31 H31 1.0000 . ?
C32 C36 1.536(3) . ?
C32 C35 1.539(3) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C5 Cl51 1.741(12) . ?
C5 Cl52 1.764(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
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(3) . ?
C41 C43 1.532(3) . ?
C41 H41 1.0000 . ?
C42 C46 1.528(3) . ?
C42 C45 1.530(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 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 Pd P1 100.25(2) . . ?
P2 Pd Br2 87.297(16) . . ?
P1 Pd Br2 172.235(16) . . ?
P2 Pd Br1 168.212(17) . . ?
P1 Pd Br1 86.311(16) . . ?
Br2 Pd Br1 86.579(10) . . ?
C12 P1 C31 106.23(11) . . ?
C12 P1 C32 104.17(10) . . ?
C31 P1 C32 106.08(11) . . ?
C12 P1 Pd 106.13(7) . . ?
C31 P1 Pd 109.02(8) . . ?
C32 P1 Pd 123.94(7) . . ?
C22 P2 C41 106.41(10) . . ?
C22 P2 C42 102.51(10) . . ?
C41 P2 C42 103.89(10) . . ?
C22 P2 Pd 112.80(7) . . ?
C41 P2 Pd 114.31(8) . . ?
C42 P2 Pd 115.71(7) . . ?
C11 C C21 116.24(17) . . ?
C11 C H1 108.2 . . ?
C21 C H1 108.2 . . ?
C11 C H2 108.2 . . ?
C21 C H2 108.2 . . ?
H1 C H2 107.4 . . ?
C16 C11 C12 119.0(2) . . ?
C16 C11 C 117.6(2) . . ?
C12 C11 C 123.24(19) . . ?
C13 C12 C11 118.1(2) . . ?
C13 C12 P1 120.45(17) . . ?
C11 C12 P1 121.49(16) . . ?
C14 C13 C12 121.8(2) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C15 120.0(2) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 118.9(2) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C11 122.0(2) . . ?
C15 C16 H16 119.0 . . ?
C11 C16 H16 119.0 . . ?
C26 C21 C22 118.56(19) . . ?
C26 C21 C 117.52(19) . . ?
C22 C21 C 123.92(18) . . ?
C23 C22 C21 118.86(19) . . ?
C23 C22 P2 119.44(16) . . ?
C21 C22 P2 121.61(16) . . ?
C24 C23 C22 121.3(2) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C25 C24 C23 119.9(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 119.8(2) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C21 121.5(2) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
C33 C31 C34 109.8(2) . . ?
C33 C31 P1 111.08(17) . . ?
C34 C31 P1 117.95(17) . . ?
C33 C31 H31 105.7 . . ?
C34 C31 H31 105.7 . . ?
P1 C31 H31 105.7 . . ?
C36 C32 C35 109.48(19) . . ?
C36 C32 P1 115.25(17) . . ?
C35 C32 P1 112.96(15) . . ?
C36 C32 H32 106.2 . . ?
C35 C32 H32 106.2 . . ?
P1 C32 H32 106.2 . . ?
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 . . ?
Cl51 C5 Cl52 112.8(6) . . ?
Cl51 C5 H5A 109.0 . . ?
Cl52 C5 H5A 109.0 . . ?
Cl51 C5 H5B 109.0 . . ?
Cl52 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
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 110.33(19) . . ?
C44 C41 P2 111.89(15) . . ?
C43 C41 P2 111.48(15) . . ?
C44 C41 H41 107.6 . . ?
C43 C41 H41 107.6 . . ?
P2 C41 H41 107.6 . . ?
C46 C42 C45 109.61(19) . . ?
C46 C42 P2 113.44(15) . . ?
C45 C42 P2 111.70(15) . . ?
C46 C42 H42 107.3 . . ?
C45 C42 H42 107.3 . . ?
P2 C42 H42 107.3 . . ?
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 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.061






