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

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1503417'
_audit_update_record             
;
2016-09-08 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H18 O4 Pd'
_chemical_formula_sum            'C14 H18 O4 Pd'
_chemical_formula_weight         356.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   7.2285(6)
_cell_length_b                   7.6427(9)
_cell_length_c                   7.6586(7)
_cell_angle_alpha                62.479(10)
_cell_angle_beta                 67.121(8)
_cell_angle_gamma                63.114(9)
_cell_volume                     325.90(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    111
_cell_measurement_reflns_used    2048
_cell_measurement_theta_min      3.9300
_cell_measurement_theta_max      28.2110


_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_F_000             180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    1.431
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.75795
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      111
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2563
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.934
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             1131
_reflns_number_gt                1122
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;

_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0323P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1131
_refine_ls_number_parameters     127
_refine_ls_number_restraints     125
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0552
_refine_ls_wR_factor_gt          0.0552
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.046
_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 1.0000 0.0000 1.0000 0.02206(13) Uani 1 2 d S U P . .
O2 O 1.2117(3) -0.0365(3) 1.1292(3) 0.0259(4) Uani 1 1 d . U . . .
O1 O 0.7841(3) 0.2499(3) 1.0675(3) 0.0253(4) Uani 1 1 d . U . . .
C2 C 0.8121(4) 0.3301(4) 1.1662(4) 0.0237(6) Uani 1 1 d D U . . .
C3 C 0.9898(4) 0.2570(4) 1.2438(4) 0.0243(6) Uani 1 1 d D U . . .
C4 C 1.1710(4) 0.0852(4) 1.2207(4) 0.0242(6) Uani 1 1 d D U . . .
C1 C 0.6275(12) 0.5223(14) 1.1949(17) 0.0272(15) Uani 0.75 1 d . U P A 1
H5B1 H 0.5329 0.5664 1.1114 0.041 Uiso 0.75 1 calc R U P A 1
H5B2 H 0.6803 0.6327 1.1573 0.041 Uiso 0.75 1 calc R U P A 1
H5B3 H 0.5521 0.4898 1.3341 0.041 Uiso 0.75 1 calc R U P A 1
C5 C 1.3283(15) 0.053(2) 1.325(2) 0.031(2) Uani 0.75 1 d . U P B 1
H5A H 1.3505 -0.0808 1.4346 0.037 Uiso 0.75 1 calc R U P B 1
H5B H 1.4641 0.0563 1.2301 0.037 Uiso 0.75 1 calc R U P B 1
C6 C 1.2333(7) 0.2279(9) 1.4031(8) 0.0465(12) Uani 0.75 1 d . U P B 1
H6A H 1.3212 0.3166 1.3360 0.056 Uiso 0.75 1 calc R U P B 1
H6B H 1.2258 0.1728 1.5470 0.056 Uiso 0.75 1 calc R U P B 1
C7 C 1.0100(14) 0.3552(13) 1.3635(17) 0.0258(15) Uani 0.75 1 d . U P B 1
H7A H 0.9027 0.3450 1.4894 0.031 Uiso 0.75 1 calc R U P B 1
H7B H 0.9959 0.5014 1.2866 0.031 Uiso 0.75 1 calc R U P B 1
C1A C 1.359(4) 0.035(6) 1.297(6) 0.018(4) Uani 0.25 1 d D U P B 2
H1A1 H 1.4264 -0.1139 1.3473 0.026 Uiso 0.25 1 calc R U P B 2
H1A2 H 1.3111 0.0893 1.4033 0.026 Uiso 0.25 1 calc R U P B 2
H1A3 H 1.4587 0.0978 1.1880 0.026 Uiso 0.25 1 calc R U P B 2
C6A C 0.776(2) 0.573(2) 1.299(2) 0.047(3) Uani 0.25 1 d D U P A 2
H6A1 H 0.6867 0.6208 1.4118 0.057 Uiso 0.25 1 calc R U P A 2
H6A2 H 0.8221 0.6873 1.1895 0.057 Uiso 0.25 1 calc R U P A 2
C7A C 0.971(5) 0.385(4) 1.363(6) 0.037(5) Uani 0.25 1 d D U P A 2
H7A1 H 0.9437 0.3107 1.5075 0.044 Uiso 0.25 1 calc R U P A 2
H7A2 H 1.0957 0.4246 1.3193 0.044 Uiso 0.25 1 calc R U P A 2
C5A C 0.651(4) 0.513(4) 1.230(5) 0.030(4) Uani 0.25 1 d D U P A 2
H1A H 0.5360 0.4723 1.3397 0.035 Uiso 0.25 1 calc R U P A 2
H1B H 0.5920 0.6273 1.1178 0.035 Uiso 0.25 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O2 1.9832(18) . ?
Pd1 O2 1.9832(18) 2_757 ?
Pd1 O1 1.9848(19) 2_757 ?
Pd1 O1 1.9848(19) . ?
O2 C4 1.280(4) . ?
O1 C2 1.284(4) . ?
C2 C3 1.398(4) . ?
C2 C5A 1.503(18) . ?
C2 C1 1.511(7) . ?
C3 C4 1.396(4) . ?
C3 C7 1.505(7) . ?
C3 C7A 1.551(19) . ?
C4 C5 1.502(8) . ?
C4 C1A 1.505(18) . ?
C1 H5B1 0.9600 . ?
C1 H5B2 0.9600 . ?
C1 H5B3 0.9600 . ?
C5 C6 1.488(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.527(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C1A H1A1 0.9600 . ?
C1A H1A2 0.9600 . ?
C1A H1A3 0.9600 . ?
C6A C5A 1.513(18) . ?
C6A C7A 1.529(18) . ?
C6A H6A1 0.9700 . ?
C6A H6A2 0.9700 . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C5A H1A 0.9700 . ?
C5A H1B 0.9700 . ?

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
O2 Pd1 O2 180.0 . 2_757 ?
O2 Pd1 O1 84.48(8) . 2_757 ?
O2 Pd1 O1 95.52(8) 2_757 2_757 ?
O2 Pd1 O1 95.52(8) . . ?
O2 Pd1 O1 84.48(8) 2_757 . ?
O1 Pd1 O1 180.0 2_757 . ?
C4 O2 Pd1 120.89(17) . . ?
C2 O1 Pd1 122.86(17) . . ?
O1 C2 C3 126.6(3) . . ?
O1 C2 C5A 125.3(7) . . ?
C3 C2 C5A 107.9(8) . . ?
O1 C2 C1 113.1(3) . . ?
C3 C2 C1 120.3(3) . . ?
C4 C3 C2 124.9(3) . . ?
C4 C3 C7 111.2(3) . . ?
C2 C3 C7 123.9(3) . . ?
C4 C3 C7A 121.3(8) . . ?
C2 C3 C7A 113.8(8) . . ?
O2 C4 C3 129.2(3) . . ?
O2 C4 C5 120.9(5) . . ?
C3 C4 C5 110.0(5) . . ?
O2 C4 C1A 111.4(12) . . ?
C3 C4 C1A 119.2(12) . . ?
C2 C1 H5B1 109.5 . . ?
C2 C1 H5B2 109.5 . . ?
H5B1 C1 H5B2 109.5 . . ?
C2 C1 H5B3 109.5 . . ?
H5B1 C1 H5B3 109.5 . . ?
H5B2 C1 H5B3 109.5 . . ?
C6 C5 C4 105.8(6) . . ?
C6 C5 H5A 110.6 . . ?
C4 C5 H5A 110.6 . . ?
C6 C5 H5B 110.6 . . ?
C4 C5 H5B 110.6 . . ?
H5A C5 H5B 108.7 . . ?
C5 C6 C7 108.9(5) . . ?
C5 C6 H6A 109.9 . . ?
C7 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
C7 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
C3 C7 C6 103.9(5) . . ?
C3 C7 H7A 111.0 . . ?
C6 C7 H7A 111.0 . . ?
C3 C7 H7B 111.0 . . ?
C6 C7 H7B 111.0 . . ?
H7A C7 H7B 109.0 . . ?
C4 C1A H1A1 109.5 . . ?
C4 C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 109.5 . . ?
C4 C1A H1A3 109.5 . . ?
H1A1 C1A H1A3 109.5 . . ?
H1A2 C1A H1A3 109.5 . . ?
C5A C6A C7A 109.7(15) . . ?
C5A C6A H6A1 109.7 . . ?
C7A C6A H6A1 109.7 . . ?
C5A C6A H6A2 109.7 . . ?
C7A C6A H6A2 109.7 . . ?
H6A1 C6A H6A2 108.2 . . ?
C6A C7A C3 98.8(13) . . ?
C6A C7A H7A1 112.0 . . ?
C3 C7A H7A1 112.0 . . ?
C6A C7A H7A2 112.0 . . ?
C3 C7A H7A2 112.0 . . ?
H7A1 C7A H7A2 109.7 . . ?
C2 C5A C6A 104.2(13) . . ?
C2 C5A H1A 110.9 . . ?
C6A C5A H1A 110.9 . . ?
C2 C5A H1B 110.9 . . ?
C6A C5A H1B 110.9 . . ?
H1A C5A H1B 108.9 . . ?

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 C2 C3 -1.3(4) . . . . ?
Pd1 O1 C2 C5A -177.0(18) . . . . ?
Pd1 O1 C2 C1 178.7(5) . . . . ?
O1 C2 C3 C4 2.0(4) . . . . ?
C5A C2 C3 C4 178.3(15) . . . . ?
C1 C2 C3 C4 -178.0(6) . . . . ?
O1 C2 C3 C7 -178.2(6) . . . . ?
C5A C2 C3 C7 -1.9(16) . . . . ?
C1 C2 C3 C7 1.8(9) . . . . ?
O1 C2 C3 C7A -177.9(19) . . . . ?
C5A C2 C3 C7A -2(3) . . . . ?
C1 C2 C3 C7A 2.1(19) . . . . ?
Pd1 O2 C4 C3 -1.7(4) . . . . ?
Pd1 O2 C4 C5 177.9(7) . . . . ?
Pd1 O2 C4 C1A -176.9(17) . . . . ?
C2 C3 C4 O2 -0.3(5) . . . . ?
C7 C3 C4 O2 179.9(6) . . . . ?
C7A C3 C4 O2 180(2) . . . . ?
C2 C3 C4 C5 -179.9(7) . . . . ?
C7 C3 C4 C5 0.4(9) . . . . ?
C7A C3 C4 C5 0(2) . . . . ?
C2 C3 C4 C1A 174.7(18) . . . . ?
C7 C3 C4 C1A -5.1(19) . . . . ?
C7A C3 C4 C1A -5(3) . . . . ?
O2 C4 C5 C6 177.0(5) . . . . ?
C3 C4 C5 C6 -3.4(11) . . . . ?
C1A C4 C5 C6 150(12) . . . . ?
C4 C5 C6 C7 5.0(12) . . . . ?
C4 C3 C7 C6 2.7(9) . . . . ?
C2 C3 C7 C6 -177.1(4) . . . . ?
C7A C3 C7 C6 -179(13) . . . . ?
C5 C6 C7 C3 -4.7(11) . . . . ?
C5A C6A C7A C3 22(3) . . . . ?
C4 C3 C7A C6A 167.5(12) . . . . ?
C2 C3 C7A C6A -13(3) . . . . ?
C7 C3 C7A C6A 166(14) . . . . ?
O1 C2 C5A C6A -168.2(11) . . . . ?
C3 C2 C5A C6A 15(2) . . . . ?
C1 C2 C5A C6A -150(10) . . . . ?
C7A C6A C5A C2 -24(3) . . . . ?

_refine_diff_density_max         0.399
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_colin007
_database_code_depnum_ccdc_archive 'CCDC 1503418'
_audit_update_record             
;
2016-10-12 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 O4 Pd'
_chemical_formula_sum            'C16 H22 O4 Pd'
_chemical_formula_weight         384.74

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'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

_cell_length_a                   14.4316(5)
_cell_length_b                   6.5451(2)
_cell_length_c                   15.6537(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1478.59(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    115
_cell_measurement_reflns_used    1816
_cell_measurement_theta_min      2.9532
_cell_measurement_theta_max      24.9946

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_min  0.79381
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      115
_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  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3634
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         24.98
_reflns_number_total             1296
_reflns_number_gt                1037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET)
(compiled Mar 22 2010,13:57:49)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_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)+(0.0283P)²+0.9027P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1296
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0671
_refine_ls_wR_factor_gt          0.0626
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6793(2) 0.4580(4) 0.40271(19) 0.0270(7) Uani 1 1 d . . .
H1A H 0.6763 0.3889 0.3487 0.040 Uiso 1 1 calc R . .
H1B H 0.7425 0.4630 0.4218 0.040 Uiso 1 1 calc R . .
H1C H 0.6559 0.5945 0.3965 0.040 Uiso 1 1 calc R . .
Pd1 Pd 0.5000 0.0000 0.5000 0.02016(14) Uani 1 2 d S . .
O2 O 0.51566(13) 0.1543(3) 0.60666(12) 0.0258(5) Uani 1 1 d . . .
O1 O 0.58390(13) 0.1827(3) 0.43666(12) 0.0244(5) Uani 1 1 d . . .
C2 C 0.62163(18) 0.3442(4) 0.46730(18) 0.0210(6) Uani 1 1 d . . .
C4 C 0.56526(18) 0.3161(4) 0.61550(17) 0.0203(6) Uani 1 1 d . . .
C3 C 0.61537(19) 0.4165(4) 0.55171(16) 0.0197(6) Uani 1 1 d . . .
C6 C 0.6370(2) 0.5500(4) 0.72784(18) 0.0287(7) Uani 1 1 d . . .
H6A H 0.6223 0.6143 0.7820 0.034 Uiso 1 1 calc R . .
H6B H 0.6974 0.4861 0.7328 0.034 Uiso 1 1 calc R . .
C5 C 0.5647(2) 0.3908(4) 0.70662(17) 0.0247(7) Uani 1 1 d . . .
H5A H 0.5738 0.2744 0.7441 0.030 Uiso 1 1 calc R . .
H5B H 0.5041 0.4473 0.7189 0.030 Uiso 1 1 calc R . .
C8 C 0.6670(2) 0.6130(4) 0.57314(18) 0.0254(7) Uani 1 1 d . . .
H8A H 0.7330 0.5843 0.5747 0.030 Uiso 1 1 calc R . .
H8B H 0.6563 0.7115 0.5279 0.030 Uiso 1 1 calc R . .
C7 C 0.6386(2) 0.7082(4) 0.65789(18) 0.0304(7) Uani 1 1 d . . .
H7A H 0.6819 0.8157 0.6728 0.037 Uiso 1 1 calc R . .
H7B H 0.5776 0.7688 0.6523 0.037 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.507(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
Pd1 O2 1.9644(19) . ?
Pd1 O2 1.9644(19) 5_656 ?
Pd1 O1 1.9695(17) 5_656 ?
Pd1 O1 1.9695(17) . ?
O2 C4 1.285(3) . ?
O1 C2 1.282(3) . ?
C2 C3 1.407(4) . ?
C4 C3 1.397(4) . ?
C4 C5 1.508(4) . ?
C3 C8 1.524(4) . ?
C6 C7 1.507(4) . ?
C6 C5 1.512(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C8 C7 1.522(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Pd1 O2 180.0 . 5_656 ?
O2 Pd1 O1 87.42(7) . 5_656 ?
O2 Pd1 O1 92.58(7) 5_656 5_656 ?
O2 Pd1 O1 92.58(7) . . ?
O2 Pd1 O1 87.42(7) 5_656 . ?
O1 Pd1 O1 180.0 5_656 . ?
C4 O2 Pd1 125.38(18) . . ?
C2 O1 Pd1 124.98(18) . . ?
O1 C2 C3 127.0(3) . . ?
O1 C2 C1 113.0(2) . . ?
C3 C2 C1 120.0(2) . . ?
O2 C4 C3 126.8(2) . . ?
O2 C4 C5 111.5(2) . . ?
C3 C4 C5 121.7(2) . . ?
C4 C3 C2 123.1(2) . . ?
C4 C3 C8 119.5(2) . . ?
C2 C3 C8 117.4(2) . . ?
C7 C6 C5 108.9(2) . . ?
C7 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
C7 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
C4 C5 C6 115.3(2) . . ?
C4 C5 H5A 108.4 . . ?
C6 C5 H5A 108.4 . . ?
C4 C5 H5B 108.4 . . ?
C6 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
C7 C8 C3 113.9(2) . . ?
C7 C8 H8A 108.8 . . ?
C3 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
C3 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C6 C7 C8 110.9(2) . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?

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
O2 Pd1 O2 C4 -13(49) 5_656 . . . ?
O1 Pd1 O2 C4 -178.6(2) 5_656 . . . ?
O1 Pd1 O2 C4 1.4(2) . . . . ?
O2 Pd1 O1 C2 -4.0(2) . . . . ?
O2 Pd1 O1 C2 176.0(2) 5_656 . . . ?
O1 Pd1 O1 C2 177(100) 5_656 . . . ?
Pd1 O1 C2 C3 3.8(4) . . . . ?
Pd1 O1 C2 C1 -177.61(17) . . . . ?
Pd1 O2 C4 C3 1.8(4) . . . . ?
Pd1 O2 C4 C5 -177.84(17) . . . . ?
O2 C4 C3 C2 -3.4(4) . . . . ?
C5 C4 C3 C2 176.2(2) . . . . ?
O2 C4 C3 C8 177.2(2) . . . . ?
C5 C4 C3 C8 -3.2(4) . . . . ?
O1 C2 C3 C4 0.3(4) . . . . ?
C1 C2 C3 C4 -178.2(3) . . . . ?
O1 C2 C3 C8 179.7(2) . . . . ?
C1 C2 C3 C8 1.2(4) . . . . ?
O2 C4 C5 C6 166.9(2) . . . . ?
C3 C4 C5 C6 -12.7(4) . . . . ?
C7 C6 C5 C4 45.1(3) . . . . ?
C4 C3 C8 C7 -14.6(4) . . . . ?
C2 C3 C8 C7 166.0(2) . . . . ?
C5 C6 C7 C8 -62.8(3) . . . . ?
C3 C8 C7 C6 48.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.069
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1503419'
_audit_update_record             
;
2016-09-08 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C15 H24 O2 Pd), H2 O'
_chemical_formula_sum            'C30 H50 O5 Pd2'
_chemical_formula_weight         703.50

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'
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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+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                   24.443(7)
_cell_length_b                   5.4443(9)
_cell_length_c                   23.838(8)
_cell_angle_alpha                90
_cell_angle_beta                 111.49(3)
_cell_angle_gamma                90
_cell_volume                     2951.7(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    120
_cell_measurement_reflns_used    1151
_cell_measurement_theta_min      3.6840
_cell_measurement_theta_max      25.5570

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    1.255
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.30102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8771
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.848
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2594
_reflns_number_gt                1759
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0843P)²+9.4617P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2594
_refine_ls_number_parameters     173
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0786
_refine_ls_wR_factor_ref         0.1969
_refine_ls_wR_factor_gt          0.1772
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
C9 C 0.1005(5) 0.6159(16) 0.3861(4) 0.054(3) Uani 1 1 d . . . . .
H10A H 0.1117 0.7806 0.3790 0.065 Uiso 1 1 calc R U . . .
H10B H 0.0584 0.5884 0.3699 0.065 Uiso 1 1 calc R U . . .
C10 C 0.1320(4) 0.5125(16) 0.4430(4) 0.049(2) Uani 1 1 d . . . . .
C11 C 0.1937(4) 0.5214(17) 0.4576(4) 0.053(3) Uani 1 1 d . . . . .
H11A H 0.2177 0.4264 0.4923 0.063 Uiso 1 1 calc R U . . .
H11B H 0.2103 0.6804 0.4546 0.063 Uiso 1 1 calc R U . . .
C12 C 0.1024(4) 0.3715(17) 0.4787(4) 0.052(3) Uani 1 1 d . . . . .
C13 C 0.0478(4) 0.2265(18) 0.4384(5) 0.060(3) Uani 1 1 d . . . . .
H21A H 0.0305 0.1429 0.4633 0.090 Uiso 1 1 calc R U . . .
H21B H 0.0593 0.1085 0.4149 0.090 Uiso 1 1 calc R U . . .
H21C H 0.0196 0.3380 0.4120 0.090 Uiso 1 1 calc R U . . .
C14 C 0.0802(4) 0.5592(17) 0.5147(4) 0.052(2) Uani 1 1 d . . . . .
H40A H 0.0620 0.4728 0.5384 0.078 Uiso 1 1 calc R U . . .
H40B H 0.0521 0.6676 0.4872 0.078 Uiso 1 1 calc R U . . .
H40C H 0.1129 0.6531 0.5409 0.078 Uiso 1 1 calc R U . . .
C15 C 0.1454(4) 0.1943(16) 0.5231(4) 0.052(2) Uani 1 1 d . . . . .
H22A H 0.1260 0.1113 0.5461 0.077 Uiso 1 1 calc R U . . .
H22B H 0.1784 0.2845 0.5498 0.077 Uiso 1 1 calc R U . . .
H22C H 0.1588 0.0757 0.5012 0.077 Uiso 1 1 calc R U . . .
O3 O 0.0000 0.4986(18) 0.2500 0.061(3) Uani 1 2 d DS T P . .
H3O H 0.032(4) 0.40(2) 0.252(8) 0.14(6) Uiso 1 1 d D . . . .
C1 C 0.1135(4) 0.0285(18) 0.2609(4) 0.053(2) Uani 1 1 d . . . . .
C2 C 0.0636(4) -0.0127(17) 0.2020(4) 0.049(2) Uani 1 1 d . . . . .
H2A H 0.0471 0.1452 0.1854 0.059 Uiso 1 1 calc R U . . .
H2B H 0.0331 -0.1058 0.2094 0.059 Uiso 1 1 calc R U . . .
C3 C 0.0813(6) -0.148(2) 0.1558(5) 0.076(4) Uani 1 1 d . . . . .
H3A H 0.0463 -0.1928 0.1217 0.092 Uiso 1 1 calc R U . . .
H3B H 0.1049 -0.0406 0.1412 0.092 Uiso 1 1 calc R U . . .
C4 C 0.1149(5) -0.369(2) 0.1821(5) 0.077(4) Uani 1 1 d . . . . .
H4A H 0.1246 -0.4557 0.1514 0.093 Uiso 1 1 calc R U . . .
H4B H 0.0909 -0.4769 0.1961 0.093 Uiso 1 1 calc R U . . .
C5 C 0.1716(4) -0.3054(17) 0.2350(5) 0.054(3) Uani 1 1 d . . . . .
H5A H 0.1870 -0.4539 0.2578 0.065 Uiso 1 1 calc R U . . .
H5B H 0.2006 -0.2476 0.2191 0.065 Uiso 1 1 calc R U . . .
C6 C 0.1642(4) -0.1115(17) 0.2776(4) 0.051(3) Uani 1 1 d . . . . .
C7 C 0.2118(4) -0.0822(17) 0.3332(4) 0.050(2) Uani 1 1 d . . . . .
C8 C 0.2646(4) -0.2508(18) 0.3473(5) 0.063(3) Uani 1 1 d . . . . .
H8A H 0.2927 -0.2133 0.3866 0.094 Uiso 1 1 calc R U . . .
H8B H 0.2823 -0.2272 0.3178 0.094 Uiso 1 1 calc R U . . .
H8C H 0.2522 -0.4185 0.3463 0.094 Uiso 1 1 calc R U . . .
O1 O 0.1014(3) 0.1962(11) 0.2927(3) 0.0558(19) Uani 1 1 d . . . . .
O2 O 0.2158(3) 0.0689(12) 0.3744(3) 0.0519(17) Uani 1 1 d . . . . .
Pd1 Pd 0.15355(3) 0.32659(13) 0.37646(3) 0.0509(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.408(12) . ?
C9 Pd1 2.106(10) . ?
C9 H10A 0.9700 . ?
C9 H10B 0.9700 . ?
C10 C11 1.418(13) . ?
C10 C12 1.514(14) . ?
C10 Pd1 2.104(10) . ?
C11 Pd1 2.107(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C15 1.529(12) . ?
C12 C13 1.546(13) . ?
C12 C14 1.554(14) . ?
C13 H21A 0.9600 . ?
C13 H21B 0.9600 . ?
C13 H21C 0.9600 . ?
C14 H40A 0.9600 . ?
C14 H40B 0.9600 . ?
C14 H40C 0.9600 . ?
C15 H22A 0.9600 . ?
C15 H22B 0.9600 . ?
C15 H22C 0.9600 . ?
O3 H3O 0.95(2) . ?
C1 O1 1.288(12) . ?
C1 C6 1.383(14) . ?
C1 C2 1.502(12) . ?
C2 C3 1.512(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.464(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.534(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.522(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.417(12) . ?
C7 O2 1.256(11) . ?
C7 C8 1.518(13) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
O1 Pd1 2.062(6) . ?
O2 Pd1 2.083(6) . ?

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
C10 C9 Pd1 70.4(6) . . ?
C10 C9 H10A 116.6 . . ?
Pd1 C9 H10A 116.6 . . ?
C10 C9 H10B 116.6 . . ?
Pd1 C9 H10B 116.6 . . ?
H10A C9 H10B 113.6 . . ?
C9 C10 C11 112.3(9) . . ?
C9 C10 C12 122.7(9) . . ?
C11 C10 C12 124.2(8) . . ?
C9 C10 Pd1 70.5(6) . . ?
C11 C10 Pd1 70.4(6) . . ?
C12 C10 Pd1 118.9(6) . . ?
C10 C11 Pd1 70.2(5) . . ?
C10 C11 H11A 116.6 . . ?
Pd1 C11 H11A 116.6 . . ?
C10 C11 H11B 116.6 . . ?
Pd1 C11 H11B 116.6 . . ?
H11A C11 H11B 113.6 . . ?
C10 C12 C15 111.1(8) . . ?
C10 C12 C13 113.0(8) . . ?
C15 C12 C13 109.0(8) . . ?
C10 C12 C14 108.2(8) . . ?
C15 C12 C14 108.9(8) . . ?
C13 C12 C14 106.4(8) . . ?
C12 C13 H21A 109.5 . . ?
C12 C13 H21B 109.5 . . ?
H21A C13 H21B 109.5 . . ?
C12 C13 H21C 109.5 . . ?
H21A C13 H21C 109.5 . . ?
H21B C13 H21C 109.5 . . ?
C12 C14 H40A 109.5 . . ?
C12 C14 H40B 109.5 . . ?
H40A C14 H40B 109.5 . . ?
C12 C14 H40C 109.5 . . ?
H40A C14 H40C 109.5 . . ?
H40B C14 H40C 109.5 . . ?
C12 C15 H22A 109.5 . . ?
C12 C15 H22B 109.5 . . ?
H22A C15 H22B 109.5 . . ?
C12 C15 H22C 109.5 . . ?
H22A C15 H22C 109.5 . . ?
H22B C15 H22C 109.5 . . ?
O1 C1 C6 126.5(9) . . ?
O1 C1 C2 112.0(8) . . ?
C6 C1 C2 121.4(9) . . ?
C1 C2 C3 113.8(9) . . ?
C1 C2 H2A 108.8 . . ?
C3 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 C2 110.6(10) . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C3 C4 C5 111.3(9) . . ?
C3 C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C6 C5 C4 114.3(8) . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C1 C6 C7 123.4(9) . . ?
C1 C6 C5 120.2(8) . . ?
C7 C6 C5 116.4(9) . . ?
O2 C7 C6 127.3(9) . . ?
O2 C7 C8 114.0(8) . . ?
C6 C7 C8 118.6(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C1 O1 Pd1 128.3(6) . . ?
C7 O2 Pd1 127.6(6) . . ?
O1 Pd1 O2 86.7(2) . . ?
O1 Pd1 C10 131.2(3) . . ?
O2 Pd1 C10 136.8(3) . . ?
O1 Pd1 C9 100.1(3) . . ?
O2 Pd1 C9 172.1(3) . . ?
C10 Pd1 C9 39.1(3) . . ?
O1 Pd1 C11 167.7(3) . . ?
O2 Pd1 C11 105.2(3) . . ?
C10 Pd1 C11 39.4(4) . . ?
C9 Pd1 C11 67.8(4) . . ?

_refine_diff_density_max         1.279
_refine_diff_density_min         -1.859
_refine_diff_density_rms         0.136

_shelxl_version_number           2013-4

