# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_Pdacpd2
_database_code_depnum_ccdc_archive 'CCDC 1431131'
_audit_update_record             
;
2015-10-14 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H18 O6 Pd, C H2 Cl2'
_chemical_formula_sum            'C15 H20 Cl2 O6 Pd'
_chemical_formula_weight         473.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   11.6869(5)
_cell_length_b                   8.8935(4)
_cell_length_c                   8.5510(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.2230(10)
_cell_angle_gamma                90
_cell_volume                     888.76(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6469
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      32.63

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_F_000             476
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.372
_shelx_estimated_absorpt_T_min   0.684
_shelx_estimated_absorpt_T_max   0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6959
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.382
_diffrn_reflns_theta_max         32.639
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1717
_reflns_number_gt                1712
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+2.0123P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1717
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0217
_refine_ls_wR_factor_ref         0.0555
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.5000 0.0000 0.01225(6) Uani 1 4 d S T P . .
O1 O 0.40620(8) 0.33721(11) 0.09003(12) 0.01676(18) Uani 1 1 d . . . . .
O2 O 0.16994(15) 0.5000 0.4521(2) 0.0325(4) Uani 1 2 d S T P . .
C1 C 0.31601(11) 0.35934(15) 0.17149(15) 0.0149(2) Uani 1 1 d . . . . .
C2 C 0.26872(15) 0.5000 0.2102(2) 0.0147(3) Uani 1 2 d S T P . .
C3 C 0.26097(12) 0.21724(16) 0.22888(18) 0.0205(2) Uani 1 1 d . . . . .
H3A H 0.2849 0.1328 0.1630 0.031 Uiso 1 1 calc R U . . .
H3B H 0.1776 0.2277 0.2239 0.031 Uiso 1 1 calc R U . . .
H3C H 0.2845 0.1985 0.3373 0.031 Uiso 1 1 calc R U . . .
C4 C 0.16192(16) 0.5000 0.3109(2) 0.0178(3) Uani 1 2 d S T P . .
C5 C 0.04800(18) 0.5000 0.2293(3) 0.0252(4) Uani 1 2 d S T P . .
H5A H -0.0120 0.5000 0.3056 0.038 Uiso 1 2 d R U P . .
H5B H 0.0416 0.5881 0.1651 0.038 Uiso 1 1 d R U . . .
Cl1 Cl 0.5000 0.66659(8) 0.5000 0.03440(13) Uani 1 2 d S T P . .
C6 C 0.5543(3) 0.5000 0.4329(5) 0.0198(7) Uani 0.5 2 d S T P . .
H6A H 0.6349 0.5000 0.4549 0.024 Uiso 0.5 2 d R U P . .
H6B H 0.5459 0.5000 0.3212 0.024 Uiso 0.5 2 d R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01321(9) 0.01147(9) 0.01207(9) 0.000 0.00179(6) 0.000
O1 0.0175(4) 0.0139(4) 0.0189(4) 0.0007(3) 0.0047(3) -0.0005(3)
O2 0.0237(8) 0.0548(12) 0.0189(7) 0.000 0.0049(6) 0.000
C1 0.0153(5) 0.0153(5) 0.0143(5) 0.0007(4) 0.0002(4) -0.0012(4)
C2 0.0133(7) 0.0159(7) 0.0150(7) 0.000 0.0020(5) 0.000
C3 0.0203(6) 0.0166(6) 0.0245(6) 0.0031(5) 0.0039(5) -0.0028(5)
C4 0.0149(7) 0.0185(8) 0.0199(8) 0.000 0.0031(6) 0.000
C5 0.0147(8) 0.0303(11) 0.0306(10) 0.000 -0.0008(7) 0.000
Cl1 0.0369(3) 0.0301(3) 0.0361(3) 0.000 -0.0058(2) 0.000
C6 0.0177(16) 0.0249(18) 0.0167(15) 0.000 0.0025(12) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O1 1.9741(10) . ?
O1 C1 1.2808(15) . ?
O2 C4 1.211(3) . ?
C1 C2 1.4076(15) . ?
C1 C3 1.5014(19) . ?
C2 C4 1.519(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.501(3) . ?
C5 H5A 0.9599 . ?
C5 H5B 0.9601 . ?
Cl1 C6 1.712(2) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pd1 O1 94.34(6) . 6_565 ?
O1 Pd1 O1 85.66(6) . 2_655 ?
C1 O1 Pd1 123.97(9) . . ?
O1 C1 C2 126.09(13) . . ?
O1 C1 C3 113.77(12) . . ?
C2 C1 C3 120.14(12) . . ?
C1 C2 C1 125.44(16) . 6_565 ?
C1 C2 C4 117.22(8) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O2 C4 C5 121.91(19) . . ?
O2 C4 C2 120.33(18) . . ?
C5 C4 C2 117.76(18) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Cl1 C6 Cl1 119.9(2) 5_666 . ?
Cl1 C6 H6A 107.4 . . ?
Cl1 C6 H6B 107.3 . . ?
H6A C6 H6B 106.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C1 C2 0.1(2) . . . . ?
Pd1 O1 C1 C3 -179.04(9) . . . . ?
O1 C1 C2 C1 -3.1(3) . . . 6_565 ?
C3 C1 C2 C1 175.99(13) . . . 6_565 ?
O1 C1 C2 C4 -178.96(14) . . . . ?
C3 C1 C2 C4 0.2(2) . . . . ?
C1 C2 C4 O2 88.09(14) . . . . ?
C1 C2 C4 C5 -91.91(14) . . . . ?

_refine_diff_density_max         1.607
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.089

_shelx_res_file                  
; 
  
TITL Pd(acpd)2 in C2/m 
CELL  0.71073  11.6869   8.8935   8.5510   90.000   90.223   90.000 
ZERR    2.000   0.0005   0.0004   0.0004    0.000    0.001    0.000 
LATT  7 
SYMM -X, Y, -Z 
SFAC C H O CL PD 
UNIT 30 40 12 4 2 
TEMP -153.0 
SIZE 0.20 0.25 0.30 
  
L.S. 12 
BOND $H 
ACTA 
CONF 
  
WGHT    0.023400    2.012300 
FVAR       0.38885 
PD1   5    0.500000    0.500000    0.000000    10.25000    0.01321    0.01147 = 
         0.01207    0.00000    0.00179    0.00000 
O1    3    0.406203    0.337213    0.090033    11.00000    0.01750    0.01393 = 
         0.01888    0.00073    0.00475   -0.00049 
O2    3    0.169938    0.500000    0.452120    10.50000    0.02368    0.05483 = 
         0.01891    0.00000    0.00493    0.00000 
C1    1    0.316014    0.359337    0.171486    11.00000    0.01527    0.01527 = 
         0.01431    0.00071    0.00018   -0.00120 
C2    1    0.268721    0.500000    0.210160    10.50000    0.01327    0.01589 = 
         0.01498    0.00000    0.00197    0.00000 
C3    1    0.260968    0.217240    0.228881    11.00000    0.02033    0.01662 = 
         0.02451    0.00312    0.00394   -0.00280 
AFIX 137 
H3A   2    0.284894    0.132824    0.163001    11.00000   -1.50000 
H3B   2    0.177557    0.227677    0.223853    11.00000   -1.50000 
H3C   2    0.284524    0.198470    0.337252    11.00000   -1.50000 
AFIX   0 
C4    1    0.161921    0.500000    0.310903    10.50000    0.01493    0.01845 = 
         0.01993    0.00000    0.00308    0.00000 
C5    1    0.047996    0.500000    0.229328    10.50000    0.01469    0.03033 = 
         0.03058    0.00000   -0.00085    0.00000 
AFIX   3 
H5A   2   -0.012044    0.500000    0.305618    10.50000   -1.50000 
H5B   2    0.041566    0.588140    0.165068    11.00000   -1.50000 
AFIX   0 
CL1   4    0.500000    0.666594    0.500000    10.50000    0.03692    0.03008 = 
         0.03615    0.00000   -0.00582    0.00000 
C6    1    0.554290    0.500000    0.432903    10.25000    0.01772    0.02486 = 
         0.01673    0.00000    0.00245    0.00000 
AFIX   3 
H6A   2    0.634910    0.500000    0.454853    10.25000   -1.20000 
H6B   2    0.545880    0.500000    0.321183    10.25000   -1.20000 
  
AFIX   0 
HKLF 4 
  
REM Pd(acpd)2 in C2/m 
REM R1 =  0.0217 for    1712 Fo > 4sig(Fo)  and  0.0217 for all    1717 data 
REM     68 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0234      2.0124 
  
REM Highest difference peak  1.607,  deepest hole -1.416,  1-sigma level  0.089 
Q1    1   0.5316  0.6226  0.4542  11.00000  0.05    1.61 
Q2    1   0.2923  0.4317  0.1837  11.00000  0.05    0.44 
Q3    1   0.1002  0.5000  0.2775  10.50000  0.05    0.43 
Q4    1   0.2879  0.2880  0.1983  11.00000  0.05    0.43 
Q5    1   0.5111  0.5000  0.0903  10.50000  0.05    0.43 
Q6    1   0.5000  0.7038  0.5000  10.50000  0.05    0.35 
Q7    1   0.5594  0.5000 -0.0057  10.50000  0.05    0.30 
Q8    1   0.2198  0.5000  0.2484  10.50000  0.05    0.27 
Q9    1   0.1560  0.4495  0.3921  11.00000  0.05    0.25 
Q10   1   0.2173  0.5000  0.4759  10.50000  0.05    0.23 
Q11   1   0.1864  0.1854  0.1561  11.00000  0.05    0.19 
Q12   1   0.0410  0.5463  0.1570  11.00000  0.05    0.19 
Q13   1   0.5632  0.7313  0.4331  11.00000  0.05    0.19 
Q14   1   0.5000  0.5452  0.5000  10.50000  0.05    0.18 
Q15   1   0.6009  0.6266  0.6416  11.00000  0.05    0.18 
Q16   1   0.1065  0.5000  0.4687  10.50000  0.05    0.18 
Q17   1   0.5962  0.5000  0.1420  10.50000  0.05    0.17 
Q18   1   0.1908  0.5000  0.0313  10.50000  0.05    0.17 
Q19   1   0.1835  0.5000  0.5650  10.50000  0.05    0.17 
Q20   1   0.1410  0.5000  0.0443  10.50000  0.05    0.17 
;
_shelx_res_checksum              16634
####################################################################### 
# 
# 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_Pdtfpd2
_database_code_depnum_ccdc_archive 'CCDC 1431132'
_audit_update_record             
;
2015-10-14 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H8 F6 O4 Pd'
_chemical_formula_sum            'C10 H8 F6 O4 Pd'
_chemical_formula_weight         412.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.7881(8)
_cell_length_b                   7.9629(13)
_cell_length_c                   8.7923(15)
_cell_angle_alpha                80.994(3)
_cell_angle_beta                 77.330(3)
_cell_angle_gamma                72.621(3)
_cell_volume                     310.64(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2165
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      32.17

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_F_000             200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.584
_shelx_estimated_absorpt_T_min   0.742
_shelx_estimated_absorpt_T_max   0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4832
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.386
_diffrn_reflns_theta_max         32.596
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2252
_reflns_number_gt                2196
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²+0.3673P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_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         2252
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0593
_refine_ls_wR_factor_gt          0.0585
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.5000 0.5000 0.01010(6) Uani 1 2 d S . P . .
F1 F 0.2639(3) 0.8336(2) 0.04636(16) 0.0239(3) Uani 1 1 d . . . . .
F2 F 0.5104(3) 0.88890(19) 0.19946(17) 0.0247(3) Uani 1 1 d . . . . .
F3 F 0.7337(3) 0.7088(2) 0.02389(18) 0.0293(4) Uani 1 1 d . . . . .
O1 O 0.1616(3) 0.66507(19) 0.33685(18) 0.0143(3) Uani 1 1 d . . . . .
O2 O 0.3449(3) 0.29213(19) 0.45149(18) 0.0139(3) Uani 1 1 d . . . . .
C1 C 0.4114(5) 0.6109(3) 0.2456(2) 0.0121(4) Uani 1 1 d . . . . .
C2 C 0.6099(5) 0.4456(3) 0.2424(2) 0.0142(4) Uani 1 1 d . . . . .
H2 H 0.7864 0.4309 0.1653 0.017 Uiso 1 1 calc R U . . .
C3 C 0.5711(4) 0.2955(3) 0.3456(2) 0.0123(4) Uani 1 1 d . . . . .
C4 C 0.4821(5) 0.7614(3) 0.1276(3) 0.0155(4) Uani 1 1 d . . . . .
C5 C 0.8147(5) 0.1266(3) 0.3336(3) 0.0156(4) Uani 1 1 d . . . . .
H5A H 0.7365 0.0281 0.3873 0.023 Uiso 1 1 calc R U . . .
H5B H 0.9754 0.1337 0.3827 0.023 Uiso 1 1 calc R U . . .
H5C H 0.8920 0.1073 0.2231 0.023 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.00929(10) 0.00906(10) 0.01046(10) 0.00074(7) 0.00022(7) -0.00265(7)
F1 0.0254(7) 0.0276(7) 0.0183(7) 0.0086(6) -0.0080(6) -0.0094(6)
F2 0.0347(8) 0.0197(7) 0.0248(7) 0.0000(6) -0.0052(6) -0.0163(6)
F3 0.0246(8) 0.0235(7) 0.0282(8) 0.0022(6) 0.0145(6) -0.0052(6)
O1 0.0134(7) 0.0124(7) 0.0145(7) 0.0006(5) 0.0018(6) -0.0036(5)
O2 0.0129(7) 0.0126(7) 0.0142(7) -0.0009(5) 0.0001(5) -0.0024(5)
C1 0.0139(9) 0.0138(9) 0.0097(8) -0.0013(7) -0.0013(7) -0.0060(7)
C2 0.0132(9) 0.0147(9) 0.0132(9) -0.0012(7) 0.0006(7) -0.0037(7)
C3 0.0119(9) 0.0140(9) 0.0119(9) -0.0036(7) -0.0026(7) -0.0034(7)
C4 0.0144(9) 0.0161(9) 0.0138(9) -0.0005(7) 0.0011(7) -0.0043(8)
C5 0.0143(9) 0.0135(9) 0.0160(10) -0.0020(7) -0.0015(8) 0.0001(7)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O1 1.9785(15) . ?
Pd1 O2 1.9819(15) . ?
F1 C4 1.331(3) . ?
F2 C4 1.330(3) . ?
F3 C4 1.339(2) . ?
O1 C1 1.281(2) . ?
O2 C3 1.268(2) . ?
C1 C2 1.374(3) . ?
C1 C4 1.525(3) . ?
C2 C3 1.416(3) . ?
C2 H2 0.9500 . ?
C3 C5 1.495(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 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
O1 Pd1 O1 180.0 2_566 . ?
O1 Pd1 O2 94.81(6) . . ?
C1 O1 Pd1 120.84(13) . . ?
C3 O2 Pd1 124.40(14) . . ?
O1 C1 C2 129.80(19) . . ?
O1 C1 C4 110.77(17) . . ?
C2 C1 C4 119.42(18) . . ?
C1 C2 C3 124.92(19) . . ?
C1 C2 H2 117.5 . . ?
C3 C2 H2 117.5 . . ?
O2 C3 C2 125.18(19) . . ?
O2 C3 C5 116.03(18) . . ?
C2 C3 C5 118.78(18) . . ?
F2 C4 F1 107.28(18) . . ?
F2 C4 F3 107.54(18) . . ?
F1 C4 F3 107.14(18) . . ?
F2 C4 C1 111.04(18) . . ?
F1 C4 C1 110.68(17) . . ?
F3 C4 C1 112.90(18) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C1 C2 -2.2(3) . . . . ?
Pd1 O1 C1 C4 178.32(13) . . . . ?
O1 C1 C2 C3 0.3(4) . . . . ?
C4 C1 C2 C3 179.8(2) . . . . ?
Pd1 O2 C3 C2 -2.0(3) . . . . ?
Pd1 O2 C3 C5 176.72(13) . . . . ?
C1 C2 C3 O2 2.1(4) . . . . ?
C1 C2 C3 C5 -176.6(2) . . . . ?
O1 C1 C4 F2 62.7(2) . . . . ?
C2 C1 C4 F2 -116.9(2) . . . . ?
O1 C1 C4 F1 -56.4(2) . . . . ?
C2 C1 C4 F1 124.1(2) . . . . ?
O1 C1 C4 F3 -176.48(18) . . . . ?
C2 C1 C4 F3 4.0(3) . . . . ?

_refine_diff_density_max         0.928
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.140

_shelx_res_file                  
; 
  
    vpa4.res created by SHELXL-2014/7 
  
  
TITL Pd(tfpd)2 in P-1 
CELL  0.71073   4.7881   7.9629   8.7923   80.994   77.330   72.621 
ZERR    1.000   0.0008   0.0013   0.0015    0.003    0.003    0.003 
LATT  1 
SFAC C H O F PD 
UNIT 10 8 4 6 1 
TEMP -173.0 
SIZE 0.15 0.15 0.20 
  
L.S. 12 
BOND $H 
ACTA 
CONF 
  
WGHT    0.016900    0.367300 
FVAR       0.89390 
PD1   5    0.000000    0.500000    0.500000    10.50000    0.00929    0.00906 = 
         0.01046    0.00074    0.00022   -0.00265 
F1    4    0.263860    0.833607    0.046358    11.00000    0.02536    0.02760 = 
         0.01833    0.00862   -0.00803   -0.00935 
F2    4    0.510425    0.888903    0.199457    11.00000    0.03474    0.01967 = 
         0.02483    0.00005   -0.00524   -0.01628 
F3    4    0.733671    0.708783    0.023891    11.00000    0.02458    0.02348 = 
         0.02817    0.00222    0.01446   -0.00524 
O1    3    0.161597    0.665072    0.336851    11.00000    0.01338    0.01243 = 
         0.01454    0.00056    0.00176   -0.00364 
O2    3    0.344872    0.292126    0.451494    11.00000    0.01294    0.01258 = 
         0.01420   -0.00093    0.00010   -0.00241 
C1    1    0.411407    0.610894    0.245585    11.00000    0.01390    0.01377 = 
         0.00970   -0.00128   -0.00133   -0.00601 
C2    1    0.609862    0.445595    0.242436    11.00000    0.01321    0.01466 = 
         0.01321   -0.00115    0.00057   -0.00368 
AFIX  43 
H2    2    0.786356    0.430949    0.165263    11.00000   -1.20000 
AFIX   0 
C3    1    0.571052    0.295498    0.345554    11.00000    0.01191    0.01396 = 
         0.01192   -0.00364   -0.00265   -0.00344 
C4    1    0.482135    0.761439    0.127591    11.00000    0.01444    0.01615 = 
         0.01377   -0.00054    0.00112   -0.00432 
C5    1    0.814719    0.126597    0.333631    11.00000    0.01426    0.01346 = 
         0.01604   -0.00199   -0.00149    0.00013 
AFIX 137 
H5A   2    0.736459    0.028104    0.387318    11.00000   -1.50000 
H5B   2    0.975438    0.133674    0.382677    11.00000   -1.50000 
H5C   2    0.892020    0.107273    0.223082    11.00000   -1.50000 
  
AFIX   0 
HKLF 4 
  
REM Pd(tfpd)2 in P-1 
REM R1 =  0.0307 for    2196 Fo > 4sig(Fo)  and  0.0321 for all    2252 data 
REM     98 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0169      0.3672 
  
REM Highest difference peak  0.928,  deepest hole -1.474,  1-sigma level  0.140 
Q1    1   0.0635  0.4756  0.5833  11.00000  0.05    0.93 
Q2    1  -0.0060  0.4186  0.5033  11.00000  0.05    0.91 
Q3    1   0.1473  0.4788  0.4673  11.00000  0.05    0.82 
Q4    1   0.1524  0.5606  0.5275  11.00000  0.05    0.76 
Q5    1   0.4378  0.6896  0.1744  11.00000  0.05    0.64 
Q6    1   0.6987  0.2044  0.3302  11.00000  0.05    0.56 
Q7    1   0.1466  0.5749  0.3923  11.00000  0.05    0.55 
Q8    1   0.2302  0.1978  0.4193  11.00000  0.05    0.51 
Q9    1   0.5247  0.5323  0.2538  11.00000  0.05    0.49 
Q10   1   0.0521  0.9054  0.1471  11.00000  0.05    0.49 
Q11   1   0.8037  0.0969  0.2178  11.00000  0.05    0.48 
Q12   1   0.2076  0.3403  0.2582  11.00000  0.05    0.48 
Q13   1   0.1088  0.7262  0.2751  11.00000  0.05    0.47 
Q14   1   0.5471  0.3878  0.2926  11.00000  0.05    0.46 
Q15   1   0.0824  0.6246  0.3028  11.00000  0.05    0.46 
Q16   1   0.6319  0.7744  0.0336  11.00000  0.05    0.46 
Q17   1   0.8347  0.1091  0.4024  11.00000  0.05    0.45 
Q18   1   0.4962  0.5211  0.2078  11.00000  0.05    0.44 
Q19   1   0.2008  0.3079  0.6223  11.00000  0.05    0.44 
Q20   1   0.3839  0.1753  0.4519  11.00000  0.05    0.44 
;
_shelx_res_checksum              33964
