# Supplementary Information (SI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_kv-sam-35-cl-pd
_database_code_depnum_ccdc_archive 'CCDC 2373260'
loop_
_audit_author_name
_audit_author_address
'Krishnan Venkatasubbaiah'
;National Institute of Science Education and Research (NISER)
India
;
_audit_update_record             
;
2024-07-24 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_kv-sam-35-cl-pd     
;
PROBLEM: Check Calcd Resid. Dens. 1.35Ang From Pd1 2.94 eA-3
RESPONSE: The largest peak is located close to the palladium atom, which is usual. 
The atom type was assigned carefully, as palladium based reagents used, in the reaction. 
The data was carefully analyzed and no twin reflections were detected.
;
# end Validation Reply Form
_audit_creation_date             2018-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H26 Cl2 F12 N4 Pd2'
_chemical_formula_sum            'C46 H26 Cl2 F12 N4 Pd2'
_chemical_formula_weight         1146.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H26 N4 Pd2 Cl2 F12'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   27.7832(6)
_cell_length_b                   27.7832(6)
_cell_length_c                   15.2098(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10167.6(5)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    9380
_cell_measurement_temperature    107(10)
_cell_measurement_theta_max      75.0460
_cell_measurement_theta_min      3.4070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5076
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14690
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.581
_diffrn_reflns_theta_max         66.581
_diffrn_reflns_theta_min         3.438
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      107(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00  14.00   0.50    0.50    --  -38.50 106.00-149.00  184
  2  ω      8.00  89.00   0.50    0.50    --   49.06-106.00 110.00  162
  3  ω    101.00 171.00   0.50    2.00    --  102.63 106.00-149.00  140
  4  ω     34.00 112.00   0.50    2.00    --  102.63-106.00 110.00  156
  5  ω    -42.00  28.00   0.50    0.50    --  -38.50  37.00   0.00  140
  6  ω    -17.00  52.00   0.50    0.50    --   49.06 -37.00-120.00  138
  7  ω     40.00 116.00   0.50    2.00    --  102.63 -61.00-180.00  152
  8  ω     94.00 159.00   0.50    2.00    --  102.63 125.00 -60.00  130
  9  ω    139.00 165.00   0.50    2.00    --  102.63  45.00-150.00   52
 10  ω     37.00 106.00   0.50    2.00    --  102.63 -30.00-180.00  138
 11  ω     35.00  94.00   0.50    2.00    --  102.63 -15.00 150.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0584999000
_diffrn_orient_matrix_UB_12      0.0449692000
_diffrn_orient_matrix_UB_13      -0.0294927000
_diffrn_orient_matrix_UB_21      -0.0207833000
_diffrn_orient_matrix_UB_22      0.0417548000
_diffrn_orient_matrix_UB_23      -0.0104639000
_diffrn_orient_matrix_UB_31      0.0156503000
_diffrn_orient_matrix_UB_32      0.0181723000
_diffrn_orient_matrix_UB_33      0.0963823000
_diffrn_oxdiff_ac3_digest_frames 
;
01b5def9435e792714acf64aa2459d979d0162605e5
;
_diffrn_oxdiff_ac3_digest_hkl    
;
0150118dd45b20cee74762263a719fb5f609ac
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3602
_reflns_number_total             3906
_reflns_odcompleteness_completeness 97.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.958
_refine_diff_density_min         -2.706
_refine_diff_density_rms         0.274
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3906
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.1006
_refine_ls_restrained_S_all      1.349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2893
_refine_ls_wR_factor_ref         0.2945
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-F6
 1.34 with sigma of 0.002
 C22-F5A
 1.34 with sigma of 0.002
 C22-F5
 1.34 with sigma of 0.002
 C22-F4
 1.34 with sigma of 0.002
 C22-F4A
 1.34 with sigma of 0.002
 C22-F6A
 1.34 with sigma of 0.002
3. Rigid body (RIGU) restrains
 F4, F5, F5A, F6, F6A, F4A, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4A, F4, F5, F5A, F6, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: F6(0.5) F6A(0.5) F4(0.5) F4A(0.5) F5(0.5) F5A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C5(H5), C17(H17), C13(H13), C1AA(H1AA), C19(H19), C6(H6),
 C7(H7), C9(H9), C14(H14), C8(H8), C15(H15)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.51781(2) 0.55611(2) 0.57240(3) 0.0210(4) Uani 1 1 d . . . . .
Cl1 Cl 0.45942(6) 0.51773(7) 0.45202(11) 0.0244(5) Uani 1 1 d . . . . .
N2 N 0.5643(3) 0.5941(3) 0.6813(4) 0.0265(13) Uani 1 1 d . . . . .
N1 N 0.6054(2) 0.5933(2) 0.7294(4) 0.0249(13) Uani 1 1 d . . . . .
C2 C 0.6012(3) 0.6667(3) 0.7761(5) 0.0260(15) Uani 1 1 d . . . . .
H2 H 0.607610 0.698509 0.806179 0.031 Uiso 1 1 calc R . . . .
C11 C 0.4987(3) 0.6156(3) 0.5871(5) 0.0235(15) Uani 1 1 d . . . . .
F1 F 0.7787(3) 0.6245(3) 0.5847(6) 0.083(2) Uani 1 1 d . . . . .
C1 C 0.5612(3) 0.6382(3) 0.7098(5) 0.0237(14) Uani 1 1 d . . . . .
C12 C 0.4657(3) 0.6271(3) 0.5326(5) 0.0279(16) Uani 1 1 d . . . . .
H12 H 0.449260 0.605304 0.483073 0.033 Uiso 1 1 calc R . . . .
C5 C 0.7261(3) 0.6968(3) 0.8280(5) 0.0290(16) Uani 1 1 d . . . . .
H5 H 0.727658 0.722443 0.787200 0.035 Uiso 1 1 calc R . . . .
C17 C 0.6778(3) 0.5797(3) 0.6675(5) 0.0330(17) Uani 1 1 d . . . . .
H17 H 0.695451 0.616469 0.648575 0.040 Uiso 1 1 calc R . . . .
C3 C 0.6285(3) 0.6376(3) 0.7868(5) 0.0290(16) Uani 1 1 d . . . . .
C13 C 0.4571(3) 0.6715(3) 0.5519(5) 0.0313(17) Uani 1 1 d . . . . .
H13 H 0.435914 0.679604 0.513820 0.038 Uiso 1 1 calc R . . . .
C1AA C 0.5990(3) 0.5023(3) 0.7368(5) 0.0294(16) Uani 1 1 d . . . . .
H1AA H 0.564701 0.487267 0.764635 0.035 Uiso 1 1 calc R . . . .
C20 C 0.6235(4) 0.4701(3) 0.7200(6) 0.0369(19) Uani 1 1 d . . . . .
C16 C 0.6273(3) 0.5575(3) 0.7107(4) 0.0238(15) Uani 1 1 d . . . . .
C10 C 0.5229(3) 0.6494(3) 0.6621(5) 0.0263(15) Uani 1 1 d . . . . .
C4 C 0.6765(3) 0.6473(3) 0.8426(5) 0.0285(16) Uani 1 1 d . . . . .
C19 C 0.6741(4) 0.4925(4) 0.6779(6) 0.044(2) Uani 1 1 d . . . . .
H19 H 0.689668 0.470322 0.666727 0.053 Uiso 1 1 calc R . . . .
C6 C 0.7735(4) 0.7073(4) 0.8753(6) 0.0392(19) Uani 1 1 d . . . . .
H6 H 0.806826 0.740165 0.865743 0.047 Uiso 1 1 calc R . . . .
C7 C 0.7714(4) 0.6690(4) 0.9367(6) 0.043(2) Uani 1 1 d . . . . .
H7 H 0.802879 0.676309 0.968609 0.052 Uiso 1 1 calc R . . . .
C9 C 0.6744(4) 0.6085(3) 0.9025(5) 0.0358(18) Uani 1 1 d . . . . .
H9 H 0.641439 0.575102 0.910935 0.043 Uiso 1 1 calc R . . . .
C14 C 0.4791(3) 0.7032(3) 0.6256(5) 0.0295(16) Uani 1 1 d . . . . .
H14 H 0.471601 0.731487 0.638515 0.035 Uiso 1 1 calc R . . . .
C8 C 0.7216(4) 0.6199(4) 0.9496(6) 0.041(2) Uani 1 1 d . . . . .
H8 H 0.719866 0.594165 0.990435 0.050 Uiso 1 1 calc R . . . .
F2 F 0.7552(4) 0.5472(4) 0.5331(7) 0.109(3) Uani 1 1 d . . . . .
C15 C 0.5128(3) 0.6929(3) 0.6815(5) 0.0280(15) Uani 1 1 d . . . . .
H15 H 0.528502 0.714797 0.731119 0.034 Uiso 1 1 calc R . . . .
C18 C 0.7020(3) 0.5476(4) 0.6522(5) 0.0355(18) Uani 1 1 d . . . . .
F3 F 0.7938(3) 0.5688(6) 0.6579(7) 0.138(5) Uani 1 1 d . . . . .
C22 C 0.5941(3) 0.4109(3) 0.7482(5) 0.0495(19) Uani 1 1 d D U . . .
C21 C 0.7590(5) 0.5724(5) 0.6101(9) 0.063(3) Uani 1 1 d . . . . .
F6 F 0.6026(10) 0.3782(7) 0.6933(11) 0.102(5) Uani 0.5 1 d D U P . .
F6A F 0.5587(6) 0.3759(4) 0.6880(8) 0.075(3) Uani 0.5 1 d D U P . .
F4 F 0.5616(7) 0.4001(7) 0.8190(9) 0.086(4) Uani 0.5 1 d D U P . .
F4A F 0.5408(4) 0.3900(6) 0.7717(13) 0.081(4) Uani 0.5 1 d D U P . .
F5 F 0.6124(7) 0.4049(6) 0.8266(8) 0.083(4) Uani 0.5 1 d D U P . .
F5A F 0.6277(5) 0.3897(5) 0.7578(14) 0.083(4) Uani 0.5 1 d D U P . .


_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 Cl1 2.4585(16) 10_666 ?
Pd1 Cl1 2.3219(16) . ?
Pd1 N2 2.039(6) . ?
Pd1 C11 1.985(7) . ?
Cl1 Pd1 2.4584(16) 10_666 ?
N2 N1 1.366(9) . ?
N2 C1 1.343(9) . ?
N1 C3 1.376(10) . ?
N1 C16 1.431(9) . ?
C2 H2 0.9300 . ?
C2 C1 1.414(10) . ?
C2 C3 1.367(10) . ?
C11 C12 1.387(10) . ?
C11 C10 1.416(10) . ?
F1 C21 1.325(14) . ?
C1 C10 1.444(10) . ?
C12 H12 0.9300 . ?
C12 C13 1.401(10) . ?
C5 H5 0.9300 . ?
C5 C4 1.395(11) . ?
C5 C6 1.397(11) . ?
C17 H17 0.9300 . ?
C17 C16 1.384(11) . ?
C17 C18 1.379(11) . ?
C3 C4 1.488(10) . ?
C13 H13 0.9300 . ?
C13 C14 1.366(11) . ?
C1AA H1AA 0.9300 . ?
C1AA C20 1.392(11) . ?
C1AA C16 1.386(11) . ?
C20 C19 1.377(14) . ?
C20 C22 1.488(11) . ?
C10 C15 1.404(10) . ?
C4 C9 1.389(12) . ?
C19 H19 0.9300 . ?
C19 C18 1.382(13) . ?
C6 H6 0.9300 . ?
C6 C7 1.394(13) . ?
C7 H7 0.9300 . ?
C7 C8 1.389(14) . ?
C9 H9 0.9300 . ?
C9 C8 1.384(12) . ?
C14 H14 0.9300 . ?
C14 C15 1.396(11) . ?
C8 H8 0.9300 . ?
F2 C21 1.340(14) . ?
C15 H15 0.9300 . ?
C18 C21 1.519(13) . ?
F3 C21 1.251(15) . ?
C22 F6 1.340(2) . ?
C22 F6A 1.339(2) . ?
C22 F4 1.340(2) . ?
C22 F4A 1.339(2) . ?
C22 F5 1.340(2) . ?
C22 F5A 1.340(2) . ?
F6 F6A 1.19(2) . ?
F6 F5A 1.15(2) . ?
F6A F4A 1.49(2) . ?
F4 F4A 0.88(2) . ?
F4 F5 1.36(2) . ?
F5 F5A 1.28(2) . ?

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
Cl1 Pd1 Cl1 84.82(6) . 10_666 ?
N2 Pd1 Cl1 101.18(17) . 10_666 ?
N2 Pd1 Cl1 173.71(17) . . ?
C11 Pd1 Cl1 177.7(2) . 10_666 ?
C11 Pd1 Cl1 93.1(2) . . ?
C11 Pd1 N2 80.9(3) . . ?
Pd1 Cl1 Pd1 95.18(6) . 10_666 ?
N1 N2 Pd1 138.2(5) . . ?
C1 N2 Pd1 115.0(5) . . ?
C1 N2 N1 106.0(6) . . ?
N2 N1 C3 110.3(6) . . ?
N2 N1 C16 123.6(5) . . ?
C3 N1 C16 125.1(6) . . ?
C1 C2 H2 127.3 . . ?
C3 C2 H2 127.3 . . ?
C3 C2 C1 105.5(6) . . ?
C12 C11 Pd1 127.4(5) . . ?
C12 C11 C10 118.6(6) . . ?
C10 C11 Pd1 113.9(5) . . ?
N2 C1 C2 110.6(6) . . ?
N2 C1 C10 115.0(6) . . ?
C2 C1 C10 134.1(7) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.1(7) . . ?
C13 C12 H12 120.0 . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.2(8) . . ?
C6 C5 H5 120.4 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C18 C17 C16 120.3(8) . . ?
N1 C3 C4 120.0(7) . . ?
C2 C3 N1 107.7(6) . . ?
C2 C3 C4 132.3(7) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 C12 121.4(7) . . ?
C14 C13 H13 119.3 . . ?
C20 C1AA H1AA 121.0 . . ?
C16 C1AA H1AA 121.0 . . ?
C16 C1AA C20 118.0(8) . . ?
C1AA C20 C22 118.9(8) . . ?
C19 C20 C1AA 120.7(8) . . ?
C19 C20 C22 120.4(8) . . ?
C17 C16 N1 118.3(7) . . ?
C17 C16 C1AA 121.1(7) . . ?
C1AA C16 N1 120.6(7) . . ?
C11 C10 C1 114.9(6) . . ?
C15 C10 C11 120.5(7) . . ?
C15 C10 C1 124.5(7) . . ?
C5 C4 C3 116.2(7) . . ?
C9 C4 C5 120.5(7) . . ?
C9 C4 C3 123.1(7) . . ?
C20 C19 H19 119.6 . . ?
C20 C19 C18 120.8(8) . . ?
C18 C19 H19 119.6 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(8) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 120.5 . . ?
C8 C7 C6 119.1(8) . . ?
C8 C7 H7 120.5 . . ?
C4 C9 H9 120.2 . . ?
C8 C9 C4 119.5(8) . . ?
C8 C9 H9 120.2 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.9(7) . . ?
C15 C14 H14 120.1 . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.1(8) . . ?
C9 C8 H8 119.5 . . ?
C10 C15 H15 120.3 . . ?
C14 C15 C10 119.5(7) . . ?
C14 C15 H15 120.3 . . ?
C17 C18 C19 118.9(8) . . ?
C17 C18 C21 121.0(8) . . ?
C19 C18 C21 120.1(8) . . ?
F6 C22 C20 112.7(10) . . ?
F6 C22 F4 132.5(14) . . ?
F6A C22 C20 113.9(7) . . ?
F6A C22 F6 52.8(11) . . ?
F6A C22 F4 102.6(13) . . ?
F6A C22 F4A 67.5(12) . . ?
F6A C22 F5 134.7(10) . . ?
F6A C22 F5A 100.0(11) . . ?
F4 C22 C20 114.6(10) . . ?
F4A C22 C20 115.7(9) . . ?
F4A C22 F6 113.8(14) . . ?
F4A C22 F4 38.1(9) . . ?
F4A C22 F5 96.5(11) . . ?
F4A C22 F5A 129.9(11) . . ?
F5 C22 C20 111.2(8) . . ?
F5 C22 F6 105.2(13) . . ?
F5 C22 F4 60.7(12) . . ?
F5A C22 C20 113.6(8) . . ?
F5A C22 F6 51.0(11) . . ?
F5A C22 F4 110.7(13) . . ?
F5A C22 F5 57.0(11) . . ?
F1 C21 F2 101.4(10) . . ?
F1 C21 C18 112.6(8) . . ?
F2 C21 C18 109.8(10) . . ?
F3 C21 F1 110.1(11) . . ?
F3 C21 F2 109.3(11) . . ?
F3 C21 C18 113.1(11) . . ?
F6A F6 C22 63.6(6) . . ?
F5A F6 C22 64.5(6) . . ?
F5A F6 F6A 122.3(11) . . ?
C22 F6A F4A 56.2(6) . . ?
F6 F6A C22 63.6(6) . . ?
F6 F6A F4A 113.3(9) . . ?
C22 F4 F5 59.6(6) . . ?
F4A F4 C22 70.9(5) . . ?
F4A F4 F5 125.9(12) . . ?
C22 F4A F6A 56.2(6) . . ?
F4 F4A C22 71.0(5) . . ?
F4 F4A F6A 122.4(11) . . ?
C22 F5 F4 59.7(6) . . ?
F5A F5 C22 61.5(6) . . ?
F5A F5 F4 113.7(9) . . ?
F6 F5A C22 64.5(6) . . ?
F6 F5A F5 122.2(10) . . ?
F5 F5A C22 61.5(6) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 211.9 9.5 ?
2 0.333 0.667 0.667 211.9 9.5 ?
3 0.667 0.333 0.333 211.9 9.5 ?

_shelx_SHELXL_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.108
_oxdiff_exptl_absorpt_empirical_full_min 0.114
####################################################################### 
# 
# 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_kv-sam-35cf-bnl-dme
_database_code_depnum_ccdc_archive 'CCDC 2373261'
loop_
_audit_author_name
_audit_author_address
'Krishnan Venkatasubbaiah'
;National Institute of Science Education and Research (NISER)
India
;
_audit_update_record             
;
2024-07-24 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_kv-sam-35cf-bnl-dme 
;
PROBLEM: Check Calcd Resid. Dens.  0.98Ang From Pd1             5.04 eA-3
RESPONSE: The largest peak is located close to the palladium atom, which is usual. 
The atom type was assigned carefully, as palladium based reagents used, in the reaction. 
The data was carefully analyzed.
;
# end Validation Reply Form
_audit_creation_date             2020-11-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C86 H50 F12 N4 O8 P2 Pd2, C4 H10 O2'
_chemical_formula_sum            'C90 H60 F12 N4 O10 P2 Pd2'
_chemical_formula_weight         1860.16
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C148 H136 F26 N42 O14 P4 Pd4 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.2159(5)
_cell_length_b                   19.6780(4)
_cell_length_c                   15.4208(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.902(4)
_cell_angle_gamma                90
_cell_volume                     3880.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    27749
_cell_measurement_temperature    112.2(4)
_cell_measurement_theta_max      75.0170
_cell_measurement_theta_min      3.8200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52529
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.759
_diffrn_reflns_theta_min         3.456
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112.2(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -102.00 -31.00   0.50    1.50    --  -38.50 -51.00 -38.00  142
  2  ω    -45.00  25.00   0.50    1.50    --  -38.50  51.00 106.00  140
  3  ω    -15.00  56.00   0.50    1.50    --   48.56 -51.00 -38.00  142
  4  ω     42.00 112.00   0.50    1.50    --   48.56  51.00 106.00  140
  5  ω     96.00 166.00   0.50    6.00    --  102.63  51.00 106.00  140
  6  ω     39.00 110.00   0.50    6.00    --  102.63 -51.00 -38.00  142
  7  ω    -42.00  28.00   0.50    1.50    --  -38.50  37.00-120.00  140
  8  ω   -105.00 -35.00   0.50    1.50    --  -38.50 -37.00  60.00  140
  9  ω    -50.00  24.00   0.50    1.50    --  -38.50  57.00 -30.00  148
 10  ω     25.00 113.00   0.50    1.50    --   48.56  77.00 -90.00  176
 11  ω     45.00 115.00   0.50    1.50    --   48.56  37.00-180.00  140
 12  ω     25.00 113.00   0.50    1.50    --   48.56  77.00-150.00  176
 13  ω     45.00 115.00   0.50    1.50    --   48.56  37.00 -30.00  140
 14  ω     43.00 117.00   0.50    1.50    --   48.56  19.00  90.00  148
 15  ω     25.00 113.00   0.50    1.50    --   48.56  77.00-180.00  176
 16  ω     38.00 126.00   0.50    6.00    --  102.63 -77.00 -30.00  176
 17  ω     80.00 167.00   0.50    6.00    --  102.63  77.00 150.00  174
 18  ω     90.00 165.00   0.50    6.00    --  102.63  61.00-180.00  150
 19  ω     80.00 108.00   0.50    6.00    --  102.63  77.00-180.00   56
 20  ω     39.00 103.00   0.50    6.00    --  102.63 -45.00-120.00  128
 21  ω     43.00 112.00   0.50    6.00    --  102.63 -61.00  60.00  138
 22  ω     80.00 108.00   0.50    6.00    --  102.63  77.00-150.00   56
 23  ω     88.00 117.00   0.50    6.00    --  102.63  64.00-176.28   58
 24  ω     78.00 105.00   0.50    6.00    --  102.63 -94.00  90.00   54
 25  ω     90.00 118.00   0.50    6.00    --  102.63  61.00-150.00   56
 26  ω     98.00 161.00   0.50    6.00    --  102.63  45.00-120.00  126
 27  ω     80.00 165.00   0.50    6.00    --  102.63  77.00-120.00  170
 28  ω    129.00 158.00   0.50    6.00    --  102.63  77.00-150.00   58
 29  ω    117.00 157.00   0.50    6.00    --  102.63  30.00 -30.00   80
 30  ω     38.00  87.00   0.50    6.00    --  102.63 -45.00 150.00   98
 31  ω    107.00 139.00   0.50    6.00    --  102.63  45.00  30.00   64
 32  ω     76.00 107.00   0.50    6.00    --  102.63 -94.00 -60.00   62
 33  ω     89.00 117.00   0.50    6.00    --  102.63  62.00-125.49   56
 34  ω    115.00 167.00   0.50    6.00    --  102.63  45.00 120.00  104
 35  ω    103.00 165.00   0.50    6.00    --  102.63  45.00 -90.00  124
 36  ω     99.00 138.00   0.50    6.00    --  102.63  45.00-150.00   78
 37  ω     90.00 117.00   0.50    6.00    --  102.63  61.00 150.00   54
 38  ω     35.00  70.00   0.50    6.00    --  102.63 -94.00 -60.00   70
 39  ω     90.00 128.00   0.50    6.00    --  102.63  61.00-120.00   76
 40  ω     38.00 109.00   0.50    6.00    --  102.63 -77.00  60.00  142
 41  ω    104.00 154.00   0.50    6.00    --  102.63  45.00-180.00  100
 42  ω     93.00 120.00   0.50    6.00    --  102.63  55.00 144.70   54
 43  ω    131.00 164.00   0.50    6.00    --  102.63  55.00 144.70   66
 44  ω    134.00 166.00   0.50    6.00    --  102.63  77.00-180.00   64
 45  ω     54.00  84.00   0.50    6.00    --  102.63 -45.00-180.00   60
 46  ω    106.00 155.00   0.50    6.00    --  102.63 125.00   0.00   98
 47  ω    100.00 162.00   0.50    6.00    --  102.63  15.00-150.00  124
 48  ω     36.00 106.00   0.50    6.00    --  102.63 -30.00 120.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0945357000
_diffrn_orient_matrix_UB_12      0.0407365000
_diffrn_orient_matrix_UB_13      -0.0045056000
_diffrn_orient_matrix_UB_21      -0.0196972000
_diffrn_orient_matrix_UB_22      0.0274094000
_diffrn_orient_matrix_UB_23      -0.1000723000
_diffrn_orient_matrix_UB_31      -0.0721854000
_diffrn_orient_matrix_UB_32      -0.0609352000
_diffrn_orient_matrix_UB_33      -0.0480501000
_diffrn_oxdiff_ac3_digest_frames 
;
016c97a3a7a1ae2ef26d8e1f95fa7927ac053443706
;
_diffrn_oxdiff_ac3_digest_hkl    
;
01a3a54d8643ac3278718d3d490ce612512a9b
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                14099
_reflns_number_total             15378
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         5.306
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.025(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         15378
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0922
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1063P)²+53.6460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2250
_refine_ls_wR_factor_ref         0.2359
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.025(15) -0.025(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C88(H88A,H88B), C87(H87A,H87B)
3.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C54(H54), C6(H6), C31(H31), C8(H8), C42(H42), C79(H79), C44(H44),
 C21(H21), C85(H85), C2(H2), C61(H61), C69(H69), C59(H59), C15(H15), C64(H64),
 C30(H30), C60(H60), C73(H73), C7(H7), C80(H80), C84(H84), C74(H74), C35(H35),
 C25(H25), C19(H19), C37(H37), C36(H36), C72(H72), C17(H17), C53(H53), C48(H48),
  C28(H28), C11(H11), C5(H5), C29(H29), C14(H14), C71(H71), C49(H49), C65(H65),
 C62(H62), C51(H51), C81(H81), C68(H68), C52(H52), C34(H34), C38(H38), C12(H12),
  C82(H82), C13(H13)
3.c Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C90(H90A,H90B,H90C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd2 Pd 0.54348(8) 0.42357(5) 0.74663(8) 0.0276(3) Uani 1 1 d . . . . .
Pd1 Pd 0.43387(8) 0.53580(5) 0.82489(8) 0.0282(3) Uani 1 1 d . . . . .
P2 P 0.3878(3) 0.54980(18) 0.6098(3) 0.0284(8) Uani 1 1 d . . . . .
P1 P 0.6565(3) 0.56701(18) 0.8220(3) 0.0281(8) Uani 1 1 d . . . . .
O3 O 0.7731(8) 0.5780(5) 0.9077(8) 0.031(2) Uani 1 1 d . . . . .
O2 O 0.6489(9) 0.5009(5) 0.7714(9) 0.033(2) Uani 1 1 d . . . . .
O8 O 0.2752(8) 0.5419(5) 0.5197(7) 0.030(2) Uani 1 1 d . . . . .
F11 F 0.1912(9) 0.4809(5) 0.3155(8) 0.050(3) Uani 1 1 d . . . . .
O7 O 0.4415(8) 0.6043(5) 0.5692(8) 0.032(2) Uani 1 1 d . . . . .
F6 F 0.7323(10) 0.7338(6) 1.1603(9) 0.058(3) Uani 1 1 d . . . . .
F4 F 0.5794(10) 0.7144(5) 1.0500(10) 0.061(3) Uani 1 1 d . . . . .
F12 F 0.3398(9) 0.4302(6) 0.3662(9) 0.055(3) Uani 1 1 d . . . . .
N1 N 0.4685(10) 0.4796(6) 0.9466(8) 0.027(3) Uani 1 1 d . . . . .
F7 F -0.0075(9) 0.3461(7) 0.5704(9) 0.054(3) Uani 1 1 d . . . . .
F10 F 0.1984(13) 0.3774(6) 0.2763(9) 0.072(4) Uani 1 1 d . . . . .
F9 F -0.0459(8) 0.4301(7) 0.4714(9) 0.061(3) Uani 1 1 d . . . . .
O6 O 0.4346(9) 0.4811(6) 0.6236(8) 0.035(2) Uani 1 1 d . . . . .
O1 O 0.5847(8) 0.5816(5) 0.8651(9) 0.034(2) Uani 1 1 d . . . . .
O4 O 0.6498(8) 0.6240(5) 0.7455(8) 0.031(2) Uani 1 1 d . . . . .
O5 O 0.3817(10) 0.5846(6) 0.6940(8) 0.038(3) Uani 1 1 d . . . . .
N3 N 0.4622(10) 0.3354(6) 0.7273(10) 0.028(3) Uani 1 1 d . . . . .
F8 F -0.0584(9) 0.3288(7) 0.4183(9) 0.064(4) Uani 1 1 d . . . . .
F5 F 0.7075(13) 0.7271(6) 1.0140(11) 0.073(4) Uani 1 1 d . . . . .
N2 N 0.5552(10) 0.4636(6) 1.0282(10) 0.031(3) Uani 1 1 d . . . . .
C32 C 0.6457(10) 0.3706(8) 0.8551(9) 0.026(3) Uani 1 1 d . . . . .
C16 C 0.6398(12) 0.5101(8) 1.0654(11) 0.030(3) Uani 1 1 d . . . . .
C39 C 0.2906(12) 0.3431(7) 0.5876(11) 0.027(3) Uani 1 1 d . . . . .
N4 N 0.3719(10) 0.3058(6) 0.6616(10) 0.031(3) Uani 1 1 d . . . . .
O9 O 0.7381(13) 0.4382(9) 0.5711(13) 0.069(4) Uani 1 1 d . . . . .
C41 C 0.2277(12) 0.3983(7) 0.4346(12) 0.031(3) Uani 1 1 d . . . . .
C40 C 0.3098(13) 0.3704(7) 0.5129(11) 0.030(3) Uani 1 1 d . . . . .
H40 H 0.3767 0.3697 0.5163 0.036 Uiso 1 1 calc R . . . .
C20 C 0.8234(12) 0.5332(10) 1.1388(11) 0.037(3) Uani 1 1 d . . . . .
C54 C 0.9476(13) 0.7337(9) 0.7777(12) 0.033(3) Uani 1 1 d . . . . .
H54 H 0.8983 0.7676 0.7676 0.040 Uiso 1 1 calc R . . . .
C24 C 0.3706(12) 0.2375(7) 0.6771(11) 0.029(3) Uani 1 1 d . . . . .
F1 F 0.9438(11) 0.4435(8) 1.2009(16) 0.104(6) Uani 1 1 d . . . . .
C27 C 0.6188(12) 0.3028(8) 0.8611(11) 0.032(3) Uani 1 1 d . . . . .
C26 C 0.5160(12) 0.2843(6) 0.7860(12) 0.029(3) Uani 1 1 d . . . . .
C6 C 0.1111(11) 0.4256(9) 0.7576(12) 0.034(3) Uani 1 1 d . . . . .
H6 H 0.0486 0.4041 0.7464 0.041 Uiso 1 1 calc R . . . .
C31 C 0.7433(12) 0.3928(7) 0.9203(13) 0.032(3) Uani 1 1 d . . . . .
H31 H 0.7649 0.4367 0.9158 0.039 Uiso 1 1 calc R . . . .
C8 C 0.2035(11) 0.5103(8) 0.7120(12) 0.030(3) Uani 1 1 d . . . . .
H8 H 0.2019 0.5446 0.6699 0.036 Uiso 1 1 calc R . . . .
C47 C 0.8541(12) 0.5940(7) 0.8836(11) 0.027(3) Uani 1 1 d . . . . .
O10 O 0.5419(12) 0.3164(8) 0.5515(13) 0.061(4) Uani 1 1 d . . . . .
C1 C 0.5381(13) 0.4037(8) 1.0674(12) 0.033(3) Uani 1 1 d . . . . .
C42 C 0.1277(14) 0.3991(9) 0.4305(13) 0.038(4) Uani 1 1 d . . . . .
H42 H 0.0724 0.4185 0.3779 0.046 Uiso 1 1 calc R . . . .
C78 C 0.1968(14) 0.6842(8) 0.3458(12) 0.036(3) Uani 1 1 d . . . . .
C79 C 0.2334(15) 0.7259(8) 0.2904(14) 0.040(4) Uani 1 1 d . . . . .
H79 H 0.3006 0.7197 0.2957 0.048 Uiso 1 1 calc R . . . .
C3 C 0.3982(11) 0.4309(8) 0.9338(11) 0.031(3) Uani 1 1 d . . . . .
C58 C 0.7954(12) 0.7761(7) 0.8757(12) 0.029(3) Uani 1 1 d . . . . .
C63 C 0.7113(12) 0.8216(8) 0.8495(12) 0.031(3) Uani 1 1 d . . . . .
C44 C 0.1919(13) 0.3450(8) 0.5842(12) 0.031(3) Uani 1 1 d . . . . .
H44 H 0.1811 0.3288 0.6358 0.037 Uiso 1 1 calc R . . . .
C21 C 0.7428(13) 0.4871(8) 1.1062(12) 0.033(3) Uani 1 1 d . . . . .
H21 H 0.7570 0.4407 1.1113 0.040 Uiso 1 1 calc R . . . .
C85 C 0.1269(14) 0.6158(9) 0.4650(13) 0.039(4) Uani 1 1 d . . . . .
H85 H 0.1058 0.5939 0.5069 0.047 Uiso 1 1 calc R . . . .
C43 C 0.1108(12) 0.3708(8) 0.5052(11) 0.031(3) Uani 1 1 d . . . . .
C2 C 0.4379(13) 0.3827(8) 1.0069(13) 0.034(3) Uani 1 1 d . . . . .
H2 H 0.4039 0.3442 1.0137 0.041 Uiso 1 1 calc R . . . .
C61 C 0.8302(15) 0.9097(8) 0.9460(14) 0.043(4) Uani 1 1 d . . . . .
H61 H 0.8425 0.9544 0.9679 0.051 Uiso 1 1 calc R . . . .
C69 C 0.5412(13) 0.5565(8) 0.3985(14) 0.039(4) Uani 1 1 d . . . . .
H69 H 0.6036 0.5415 0.3992 0.047 Uiso 1 1 calc R . . . .
C76 C 0.3530(12) 0.6025(7) 0.3969(11) 0.029(3) Uani 1 1 d . . . . .
C86 C 0.2205(12) 0.5974(7) 0.4636(11) 0.029(3) Uani 1 1 d . . . . .
C67 C 0.4421(12) 0.5916(8) 0.4811(12) 0.031(3) Uani 1 1 d . . . . .
C33 C 0.2871(12) 0.1901(7) 0.6171(12) 0.031(3) Uani 1 1 d . . . . .
C59 C 0.8973(13) 0.7982(8) 0.9404(12) 0.034(3) Uani 1 1 d . . . . .
H59 H 0.9534 0.7683 0.9588 0.041 Uiso 1 1 calc R . . . .
C15 C 0.6129(14) 0.3019(9) 1.1631(15) 0.041(4) Uani 1 1 d . . . . .
H15 H 0.5828 0.2773 1.1060 0.049 Uiso 1 1 calc R . . . .
C64 C 0.6078(13) 0.7996(8) 0.7882(14) 0.037(4) Uani 1 1 d . . . . .
H64 H 0.5529 0.8305 0.7694 0.044 Uiso 1 1 calc R . . . .
C30 C 0.8109(14) 0.3484(9) 0.9946(13) 0.036(4) Uani 1 1 d . . . . .
H30 H 0.8741 0.3643 1.0417 0.044 Uiso 1 1 calc R . . . .
C60 C 0.9135(15) 0.8622(8) 0.9753(13) 0.039(4) Uani 1 1 d . . . . .
H60 H 0.9803 0.8754 1.0193 0.047 Uiso 1 1 calc R . . . .
C9 C 0.2983(14) 0.4929(9) 0.7906(12) 0.037(4) Uani 1 1 d . . . . .
C73 C 0.2738(15) 0.5775(8) 0.1323(13) 0.040(4) Uani 1 1 d . . . . .
H73 H 0.2142 0.5812 0.0741 0.048 Uiso 1 1 calc R . . . .
C23 C 0.9338(15) 0.5098(10) 1.1815(14) 0.045(4) Uani 1 1 d . . . . .
C7 C 0.1136(14) 0.4767(9) 0.6975(13) 0.038(4) Uani 1 1 d . . . . .
H7 H 0.0516 0.4889 0.6450 0.045 Uiso 1 1 calc R . . . .
C56 C 0.8595(11) 0.6575(8) 0.8503(11) 0.029(3) Uani 1 1 d . . . . .
C80 C 0.1698(16) 0.7749(9) 0.2295(14) 0.045(4) Uani 1 1 d . . . . .
H80 H 0.1930 0.8000 0.1915 0.054 Uiso 1 1 calc R . . . .
C46 C 0.2391(13) 0.4220(9) 0.3482(12) 0.038(3) Uani 1 1 d . . . . .
C84 C 0.0653(15) 0.6658(9) 0.4054(13) 0.042(4) Uani 1 1 d . . . . .
H84 H 0.0014 0.6764 0.4051 0.050 Uiso 1 1 calc R . . . .
C55 C 0.9409(12) 0.6719(8) 0.8222(11) 0.030(3) Uani 1 1 d . . . . .
C77 C 0.2576(12) 0.6283(8) 0.4030(12) 0.032(3) Uani 1 1 d . . . . .
C66 C 0.6724(11) 0.6905(7) 0.7815(11) 0.025(3) Uani 1 1 d . . . . .
C74 C 0.2692(15) 0.5904(8) 0.2168(12) 0.036(4) Uani 1 1 d . . . . .
H74 H 0.2050 0.6027 0.2145 0.043 Uiso 1 1 calc R . . . .
C35 C 0.1627(16) 0.1445(10) 0.4681(15) 0.048(4) Uani 1 1 d . . . . .
H35 H 0.1296 0.1469 0.4012 0.057 Uiso 1 1 calc R . . . .
C70 C 0.4533(14) 0.5650(8) 0.3096(13) 0.036(4) Uani 1 1 d . . . . .
C25 C 0.4617(13) 0.2226(7) 0.7573(12) 0.032(3) Uani 1 1 d . . . . .
H25 H 0.4829 0.1804 0.7865 0.039 Uiso 1 1 calc R . . . .
C19 C 0.8008(13) 0.6023(9) 1.1290(11) 0.036(4) Uani 1 1 d . . . . .
H19 H 0.8554 0.6336 1.1502 0.043 Uiso 1 1 calc R . . . .
C37 C 0.1893(14) 0.0884(8) 0.6113(14) 0.039(4) Uani 1 1 d . . . . .
H37 H 0.1749 0.0524 0.6427 0.047 Uiso 1 1 calc R . . . .
C36 C 0.1381(16) 0.0932(9) 0.5142(16) 0.047(4) Uani 1 1 d . . . . .
H36 H 0.0865 0.0618 0.4792 0.057 Uiso 1 1 calc R . . . .
C57 C 0.7748(12) 0.7079(8) 0.8347(12) 0.029(3) Uani 1 1 d . . . . .
C72 C 0.3723(17) 0.5578(8) 0.1339(14) 0.044(4) Uani 1 1 d . . . . .
H72 H 0.3783 0.5501 0.0771 0.053 Uiso 1 1 calc R . . . .
C17 C 0.6197(14) 0.5793(8) 1.0606(13) 0.035(4) Uani 1 1 d . . . . .
H17 H 0.5512 0.5946 1.0381 0.042 Uiso 1 1 calc R . . . .
C53 C 1.0252(14) 0.7445(10) 0.7493(14) 0.043(4) Uani 1 1 d . . . . .
H53 H 1.0268 0.7848 0.7184 0.051 Uiso 1 1 calc R . . . .
F3 F 0.9896(14) 0.5350(12) 1.2624(17) 0.157(12) Uani 1 1 d . . . . .
C22 C 0.6804(15) 0.7006(10) 1.0783(14) 0.043(4) Uani 1 1 d . . . . .
C48 C 0.9306(12) 0.5438(8) 0.8995(12) 0.036(3) Uani 1 1 d . . . . .
H48 H 0.9262 0.5017 0.9248 0.044 Uiso 1 1 calc R . . . .
C28 C 0.6843(13) 0.2597(9) 0.9303(12) 0.036(3) Uani 1 1 d . . . . .
H28 H 0.6635 0.2154 0.9334 0.043 Uiso 1 1 calc R . . . .
C18 C 0.7002(13) 0.6252(9) 1.0889(11) 0.033(3) Uani 1 1 d . . . . .
C11 C 0.6551(12) 0.4086(10) 1.2473(13) 0.041(4) Uani 1 1 d . . . . .
H11 H 0.6531 0.4558 1.2468 0.049 Uiso 1 1 calc R . . . .
C5 C 0.2048(13) 0.4066(7) 0.8359(12) 0.034(3) Uani 1 1 d . . . . .
H5 H 0.2064 0.3711 0.8762 0.041 Uiso 1 1 calc R . . . .
C83 C 0.0988(14) 0.7007(8) 0.3453(13) 0.039(4) Uani 1 1 d . . . . .
C29 C 0.7817(15) 0.2821(8) 0.9959(13) 0.039(4) Uani 1 1 d . . . . .
H29 H 0.8278 0.2520 1.0411 0.047 Uiso 1 1 calc R . . . .
F2 F 0.9762(15) 0.5132(19) 1.1266(19) 0.193(17) Uani 1 1 d . . . . .
C14 C 0.6620(15) 0.2696(10) 1.2492(16) 0.049(5) Uani 1 1 d . . . . .
H14 H 0.6657 0.2224 1.2499 0.058 Uiso 1 1 calc R . . . .
C71 C 0.4541(17) 0.5512(8) 0.2193(15) 0.045(4) Uani 1 1 d . . . . .
H71 H 0.5166 0.5364 0.2201 0.054 Uiso 1 1 calc R . . . .
C89 C 0.495(2) 0.2624(12) 0.495(2) 0.077(8) Uani 1 1 d . . . . .
H89A H 0.4394 0.2780 0.4357 0.115 Uiso 1 1 calc GR . . . .
H89B H 0.4659 0.2336 0.5278 0.115 Uiso 1 1 calc GR . . . .
H89C H 0.5447 0.2374 0.4818 0.115 Uiso 1 1 calc GR . . . .
C49 C 1.0113(12) 0.5581(8) 0.8770(14) 0.039(4) Uani 1 1 d . . . . .
H49 H 1.0621 0.5252 0.8874 0.047 Uiso 1 1 calc R . . . .
C65 C 0.5878(13) 0.7344(9) 0.7570(13) 0.037(4) Uani 1 1 d . . . . .
H65 H 0.5197 0.7195 0.7204 0.045 Uiso 1 1 calc R . . . .
C75 C 0.3558(13) 0.5865(7) 0.3077(12) 0.033(3) Uani 1 1 d . . . . .
C62 C 0.7313(15) 0.8886(8) 0.8849(14) 0.040(4) Uani 1 1 d . . . . .
H62 H 0.6762 0.9192 0.8664 0.048 Uiso 1 1 calc R . . . .
C51 C 1.1007(13) 0.6338(10) 0.8118(13) 0.041(4) Uani 1 1 d . . . . .
H51 H 1.1528 0.6016 0.8241 0.049 Uiso 1 1 calc R . . . .
C4 C 0.2967(13) 0.4429(7) 0.8520(12) 0.032(3) Uani 1 1 d . . . . .
C10 C 0.6084(13) 0.3736(9) 1.1618(12) 0.035(4) Uani 1 1 d . . . . .
C81 C 0.0717(18) 0.7873(10) 0.2243(15) 0.051(5) Uani 1 1 d . . . . .
H81 H 0.0293 0.8203 0.1822 0.062 Uiso 1 1 calc R . . . .
C68 C 0.5378(14) 0.5693(9) 0.4824(15) 0.043(4) Uani 1 1 d . . . . .
H68 H 0.5970 0.5637 0.5405 0.052 Uiso 1 1 calc R . . . .
C52 C 1.1023(15) 0.6950(10) 0.7666(15) 0.047(5) Uani 1 1 d . . . . .
H52 H 1.1551 0.7031 0.7477 0.057 Uiso 1 1 calc R . . . .
C50 C 1.0191(14) 0.6212(9) 0.8385(13) 0.037(4) Uani 1 1 d . . . . .
C34 C 0.2365(14) 0.1930(8) 0.5203(13) 0.038(4) Uani 1 1 d . . . . .
H34 H 0.2513 0.2281 0.4878 0.046 Uiso 1 1 calc R . . . .
C38 C 0.2628(14) 0.1363(8) 0.6643(12) 0.035(3) Uani 1 1 d . . . . .
H38 H 0.2964 0.1332 0.7311 0.042 Uiso 1 1 calc R . . . .
C12 C 0.7044(15) 0.3750(12) 1.3331(15) 0.050(5) Uani 1 1 d . . . . .
H12 H 0.7368 0.3994 1.3903 0.059 Uiso 1 1 calc R . . . .
C82 C 0.0356(16) 0.7514(9) 0.2806(15) 0.047(4) Uani 1 1 d . . . . .
H82 H -0.0305 0.7605 0.2762 0.056 Uiso 1 1 calc R . . . .
C13 C 0.7062(15) 0.3040(11) 1.3350(16) 0.052(5) Uani 1 1 d . . . . .
H13 H 0.7367 0.2806 1.3931 0.062 Uiso 1 1 calc R . . . .
C45 C -0.0013(15) 0.3683(10) 0.4921(14) 0.045(4) Uani 1 1 d . . . . .
C88 C 0.6073(18) 0.3506(11) 0.5221(17) 0.055(5) Uani 1 1 d . . . . .
H88A H 0.5670 0.3709 0.4593 0.066 Uiso 1 1 calc R . . . .
H88B H 0.6573 0.3193 0.5170 0.066 Uiso 1 1 calc R . . . .
C90 C 0.8110(19) 0.4745(15) 0.6514(19) 0.070(7) Uani 1 1 d . . . . .
H90A H 0.8694 0.4876 0.6396 0.105 Uiso 1 1 calc GR . . . .
H90B H 0.8350 0.4461 0.7076 0.105 Uiso 1 1 calc GR . . . .
H90C H 0.7782 0.5143 0.6617 0.105 Uiso 1 1 calc GR . . . .
C87 C 0.6636(18) 0.4049(12) 0.5942(19) 0.064(6) Uani 1 1 d . . . . .
H87A H 0.6135 0.4378 0.5956 0.077 Uiso 1 1 calc R . . . .
H87B H 0.6988 0.3847 0.6579 0.077 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
Pd2 Pd1 3.2257(14) . ?
Pd2 O2 2.051(10) . ?
Pd2 O6 2.171(12) . ?
Pd2 N3 2.033(12) . ?
Pd2 C32 1.968(13) . ?
Pd1 N1 2.046(11) . ?
Pd1 O1 2.153(10) . ?
Pd1 O5 2.058(11) . ?
Pd1 C9 1.954(18) . ?
P2 O8 1.604(11) . ?
P2 O7 1.593(11) . ?
P2 O6 1.481(12) . ?
P2 O5 1.505(12) . ?
P1 O3 1.620(11) . ?
P1 O2 1.497(11) . ?
P1 O1 1.469(11) . ?
P1 O4 1.601(11) . ?
O3 C47 1.392(17) . ?
O8 C86 1.398(18) . ?
F11 C46 1.33(2) . ?
O7 C67 1.39(2) . ?
F6 C22 1.33(2) . ?
F4 C22 1.33(2) . ?
F12 C46 1.343(19) . ?
N1 N2 1.359(18) . ?
N1 C3 1.335(18) . ?
F7 C45 1.32(2) . ?
F10 C46 1.33(2) . ?
F9 C45 1.34(2) . ?
O4 C66 1.403(17) . ?
N3 N4 1.370(18) . ?
N3 C26 1.344(19) . ?
F8 C45 1.32(2) . ?
F5 C22 1.32(2) . ?
N2 C16 1.418(19) . ?
N2 C1 1.39(2) . ?
C32 C27 1.40(2) . ?
C32 C31 1.38(2) . ?
C16 C21 1.39(2) . ?
C16 C17 1.39(2) . ?
C39 N4 1.423(19) . ?
C39 C40 1.40(2) . ?
C39 C44 1.38(2) . ?
N4 C24 1.367(19) . ?
O9 C90 1.41(3) . ?
O9 C87 1.42(2) . ?
C41 C40 1.38(2) . ?
C41 C42 1.39(2) . ?
C41 C46 1.49(2) . ?
C40 H40 0.9300 . ?
C20 C21 1.37(2) . ?
C20 C23 1.49(2) . ?
C20 C19 1.39(3) . ?
C54 H54 0.9300 . ?
C54 C55 1.42(2) . ?
C54 C53 1.37(2) . ?
C24 C33 1.48(2) . ?
C24 C25 1.38(2) . ?
F1 C23 1.33(2) . ?
C27 C26 1.46(2) . ?
C27 C28 1.36(2) . ?
C26 C25 1.403(19) . ?
C6 H6 0.9300 . ?
C6 C7 1.38(2) . ?
C6 C5 1.40(2) . ?
C31 H31 0.9300 . ?
C31 C30 1.43(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.41(2) . ?
C8 C7 1.37(2) . ?
C47 C56 1.37(2) . ?
C47 C48 1.41(2) . ?
O10 C89 1.35(3) . ?
O10 C88 1.38(3) . ?
C1 C2 1.38(2) . ?
C1 C10 1.48(2) . ?
C42 H42 0.9300 . ?
C42 C43 1.39(2) . ?
C78 C79 1.44(2) . ?
C78 C77 1.44(2) . ?
C78 C83 1.43(2) . ?
C79 H79 0.9300 . ?
C79 C80 1.37(2) . ?
C3 C2 1.39(2) . ?
C3 C4 1.46(2) . ?
C58 C63 1.40(2) . ?
C58 C59 1.42(2) . ?
C58 C57 1.46(2) . ?
C63 C64 1.43(2) . ?
C63 C62 1.41(2) . ?
C44 H44 0.9300 . ?
C44 C43 1.36(2) . ?
C21 H21 0.9300 . ?
C85 H85 0.9300 . ?
C85 C86 1.39(2) . ?
C85 C84 1.37(2) . ?
C43 C45 1.52(2) . ?
C2 H2 0.9300 . ?
C61 H61 0.9300 . ?
C61 C60 1.42(3) . ?
C61 C62 1.37(3) . ?
C69 H69 0.9300 . ?
C69 C70 1.40(3) . ?
C69 C68 1.34(3) . ?
C76 C67 1.38(2) . ?
C76 C77 1.49(2) . ?
C76 C75 1.43(2) . ?
C86 C77 1.40(2) . ?
C67 C68 1.42(2) . ?
C33 C34 1.35(2) . ?
C33 C38 1.41(2) . ?
C59 H59 0.9300 . ?
C59 C60 1.35(2) . ?
C15 H15 0.9300 . ?
C15 C14 1.36(3) . ?
C15 C10 1.41(2) . ?
C64 H64 0.9300 . ?
C64 C65 1.35(2) . ?
C30 H30 0.9300 . ?
C30 C29 1.37(2) . ?
C60 H60 0.9300 . ?
C9 C4 1.37(2) . ?
C73 H73 0.9300 . ?
C73 C74 1.36(2) . ?
C73 C72 1.44(3) . ?
C23 F3 1.25(2) . ?
C23 F2 1.24(3) . ?
C7 H7 0.9300 . ?
C56 C55 1.43(2) . ?
C56 C57 1.50(2) . ?
C80 H80 0.9300 . ?
C80 C81 1.38(3) . ?
C84 H84 0.9300 . ?
C84 C83 1.40(2) . ?
C55 C50 1.43(2) . ?
C66 C57 1.37(2) . ?
C66 C65 1.39(2) . ?
C74 H74 0.9300 . ?
C74 C75 1.41(3) . ?
C35 H35 0.9300 . ?
C35 C36 1.37(3) . ?
C35 C34 1.39(3) . ?
C70 C71 1.42(3) . ?
C70 C75 1.44(2) . ?
C25 H25 0.9300 . ?
C19 H19 0.9300 . ?
C19 C18 1.36(2) . ?
C37 H37 0.9300 . ?
C37 C36 1.35(3) . ?
C37 C38 1.38(2) . ?
C36 H36 0.9300 . ?
C72 H72 0.9300 . ?
C72 C71 1.33(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.37(2) . ?
C53 H53 0.9300 . ?
C53 C52 1.40(3) . ?
C22 C18 1.51(3) . ?
C48 H48 0.9300 . ?
C48 C49 1.36(2) . ?
C28 H28 0.9300 . ?
C28 C29 1.38(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.37(3) . ?
C11 C12 1.37(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.41(2) . ?
C83 C82 1.42(2) . ?
C29 H29 0.9300 . ?
C14 H14 0.9300 . ?
C14 C13 1.37(3) . ?
C71 H71 0.9300 . ?
C89 H89A 0.9600 . ?
C89 H89B 0.9600 . ?
C89 H89C 0.9600 . ?
C49 H49 0.9300 . ?
C49 C50 1.40(3) . ?
C65 H65 0.9300 . ?
C62 H62 0.9300 . ?
C51 H51 0.9300 . ?
C51 C52 1.40(3) . ?
C51 C50 1.41(2) . ?
C81 H81 0.9300 . ?
C81 C82 1.38(3) . ?
C68 H68 0.9300 . ?
C52 H52 0.9300 . ?
C34 H34 0.9300 . ?
C38 H38 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.40(3) . ?
C82 H82 0.9300 . ?
C13 H13 0.9300 . ?
C88 H88A 0.9700 . ?
C88 H88B 0.9700 . ?
C88 C87 1.50(3) . ?
C90 H90A 0.9600 . ?
C90 H90B 0.9600 . ?
C90 H90C 0.9600 . ?
C87 H87A 0.9700 . ?
C87 H87B 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 Pd2 Pd1 81.7(3) . . ?
O2 Pd2 O6 87.7(4) . . ?
O6 Pd2 Pd1 72.2(3) . . ?
N3 Pd2 Pd1 107.6(4) . . ?
N3 Pd2 O2 169.3(5) . . ?
N3 Pd2 O6 100.1(5) . . ?
C32 Pd2 Pd1 110.0(4) . . ?
C32 Pd2 O2 91.5(6) . . ?
C32 Pd2 O6 177.5(5) . . ?
C32 Pd2 N3 80.4(6) . . ?
N1 Pd1 Pd2 90.6(4) . . ?
N1 Pd1 O1 98.8(5) . . ?
N1 Pd1 O5 172.5(5) . . ?
O1 Pd1 Pd2 79.1(3) . . ?
O5 Pd1 Pd2 88.8(3) . . ?
O5 Pd1 O1 88.5(5) . . ?
C9 Pd1 Pd2 100.6(5) . . ?
C9 Pd1 N1 80.1(6) . . ?
C9 Pd1 O1 178.8(6) . . ?
C9 Pd1 O5 92.6(6) . . ?
O7 P2 O8 101.1(6) . . ?
O6 P2 O8 104.6(6) . . ?
O6 P2 O7 114.1(6) . . ?
O6 P2 O5 118.9(6) . . ?
O5 P2 O8 112.3(7) . . ?
O5 P2 O7 104.5(6) . . ?
O2 P1 O3 110.9(6) . . ?
O2 P1 O4 104.9(6) . . ?
O1 P1 O3 105.7(7) . . ?
O1 P1 O2 120.0(6) . . ?
O1 P1 O4 111.5(6) . . ?
O4 P1 O3 102.6(6) . . ?
C47 O3 P1 118.9(10) . . ?
P1 O2 Pd2 128.5(7) . . ?
C86 O8 P2 122.4(10) . . ?
C67 O7 P2 118.3(9) . . ?
N2 N1 Pd1 137.1(9) . . ?
C3 N1 Pd1 112.8(10) . . ?
C3 N1 N2 106.8(12) . . ?
P2 O6 Pd2 134.9(7) . . ?
P1 O1 Pd1 126.1(7) . . ?
C66 O4 P1 115.6(9) . . ?
P2 O5 Pd1 120.1(7) . . ?
N4 N3 Pd2 139.4(10) . . ?
C26 N3 Pd2 114.8(10) . . ?
C26 N3 N4 104.7(11) . . ?
N1 N2 C16 119.5(12) . . ?
N1 N2 C1 109.8(13) . . ?
C1 N2 C16 130.4(14) . . ?
C27 C32 Pd2 116.0(11) . . ?
C31 C32 Pd2 125.8(12) . . ?
C31 C32 C27 118.0(13) . . ?
C21 C16 N2 120.9(14) . . ?
C17 C16 N2 119.5(15) . . ?
C17 C16 C21 119.6(15) . . ?
C40 C39 N4 118.3(13) . . ?
C44 C39 N4 120.0(13) . . ?
C44 C39 C40 121.2(14) . . ?
N3 N4 C39 123.0(12) . . ?
C24 N4 N3 111.6(12) . . ?
C24 N4 C39 125.4(13) . . ?
C90 O9 C87 110.8(19) . . ?
C40 C41 C42 120.1(15) . . ?
C40 C41 C46 121.9(14) . . ?
C42 C41 C46 117.7(15) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 C39 118.6(14) . . ?
C41 C40 H40 120.7 . . ?
C21 C20 C23 120.5(17) . . ?
C21 C20 C19 119.4(15) . . ?
C19 C20 C23 120.1(17) . . ?
C55 C54 H54 119.3 . . ?
C53 C54 H54 119.3 . . ?
C53 C54 C55 121.4(16) . . ?
N4 C24 C33 125.5(14) . . ?
N4 C24 C25 106.7(13) . . ?
C25 C24 C33 127.8(14) . . ?
C32 C27 C26 113.2(14) . . ?
C28 C27 C32 122.0(14) . . ?
C28 C27 C26 124.8(14) . . ?
N3 C26 C27 115.2(12) . . ?
N3 C26 C25 111.2(14) . . ?
C25 C26 C27 133.5(14) . . ?
C7 C6 H6 120.7 . . ?
C7 C6 C5 118.7(14) . . ?
C5 C6 H6 120.7 . . ?
C32 C31 H31 120.0 . . ?
C32 C31 C30 120.1(14) . . ?
C30 C31 H31 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 119.9(15) . . ?
O3 C47 C48 117.5(13) . . ?
C56 C47 O3 119.8(13) . . ?
C56 C47 C48 122.7(14) . . ?
C89 O10 C88 113.0(19) . . ?
N2 C1 C10 126.4(15) . . ?
C2 C1 N2 106.4(15) . . ?
C2 C1 C10 126.7(14) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 119.9(16) . . ?
C43 C42 H42 120.0 . . ?
C79 C78 C77 121.7(15) . . ?
C83 C78 C79 118.2(15) . . ?
C83 C78 C77 120.1(15) . . ?
C78 C79 H79 119.8 . . ?
C80 C79 C78 120.4(17) . . ?
C80 C79 H79 119.8 . . ?
N1 C3 C2 110.9(13) . . ?
N1 C3 C4 113.8(14) . . ?
C2 C3 C4 135.1(14) . . ?
C63 C58 C59 119.0(14) . . ?
C63 C58 C57 118.5(14) . . ?
C59 C58 C57 122.5(14) . . ?
C58 C63 C64 120.0(14) . . ?
C58 C63 C62 118.9(15) . . ?
C62 C63 C64 121.1(15) . . ?
C39 C44 H44 120.2 . . ?
C43 C44 C39 119.6(14) . . ?
C43 C44 H44 120.2 . . ?
C16 C21 H21 120.2 . . ?
C20 C21 C16 119.7(15) . . ?
C20 C21 H21 120.2 . . ?
C86 C85 H85 119.5 . . ?
C84 C85 H85 119.5 . . ?
C84 C85 C86 120.9(15) . . ?
C42 C43 C45 117.0(15) . . ?
C44 C43 C42 120.4(15) . . ?
C44 C43 C45 122.5(15) . . ?
C1 C2 C3 106.1(13) . . ?
C1 C2 H2 126.9 . . ?
C3 C2 H2 126.9 . . ?
C60 C61 H61 120.6 . . ?
C62 C61 H61 120.6 . . ?
C62 C61 C60 118.8(15) . . ?
C70 C69 H69 119.1 . . ?
C68 C69 H69 119.1 . . ?
C68 C69 C70 121.8(16) . . ?
C67 C76 C77 118.8(14) . . ?
C67 C76 C75 118.2(15) . . ?
C75 C76 C77 123.1(14) . . ?
C85 C86 O8 118.2(14) . . ?
C85 C86 C77 122.8(14) . . ?
C77 C86 O8 118.9(14) . . ?
O7 C67 C68 117.3(15) . . ?
C76 C67 O7 119.9(13) . . ?
C76 C67 C68 122.8(16) . . ?
C34 C33 C24 124.2(14) . . ?
C34 C33 C38 118.2(15) . . ?
C38 C33 C24 117.5(15) . . ?
C58 C59 H59 119.6 . . ?
C60 C59 C58 120.7(16) . . ?
C60 C59 H59 119.6 . . ?
C14 C15 H15 120.6 . . ?
C14 C15 C10 118.8(19) . . ?
C10 C15 H15 120.6 . . ?
C63 C64 H64 119.4 . . ?
C65 C64 C63 121.2(15) . . ?
C65 C64 H64 119.4 . . ?
C31 C30 H30 120.3 . . ?
C29 C30 C31 119.5(16) . . ?
C29 C30 H30 120.3 . . ?
C61 C60 H60 119.5 . . ?
C59 C60 C61 121.0(17) . . ?
C59 C60 H60 119.5 . . ?
C8 C9 Pd1 126.1(13) . . ?
C4 C9 Pd1 115.7(13) . . ?
C4 C9 C8 118.1(16) . . ?
C74 C73 H73 120.4 . . ?
C74 C73 C72 119.1(17) . . ?
C72 C73 H73 120.4 . . ?
F1 C23 C20 113.1(17) . . ?
F3 C23 C20 113.9(17) . . ?
F3 C23 F1 102(2) . . ?
F2 C23 C20 114.5(17) . . ?
F2 C23 F1 100(2) . . ?
F2 C23 F3 112(3) . . ?
C6 C7 H7 118.7 . . ?
C8 C7 C6 122.6(16) . . ?
C8 C7 H7 118.7 . . ?
C47 C56 C55 118.8(14) . . ?
C47 C56 C57 119.5(13) . . ?
C55 C56 C57 121.4(13) . . ?
C79 C80 H80 119.7 . . ?
C79 C80 C81 120.6(17) . . ?
C81 C80 H80 119.7 . . ?
F11 C46 F12 107.2(14) . . ?
F11 C46 F10 107.2(15) . . ?
F11 C46 C41 112.0(14) . . ?
F12 C46 C41 112.1(14) . . ?
F10 C46 F12 106.8(14) . . ?
F10 C46 C41 111.2(14) . . ?
C85 C84 H84 120.2 . . ?
C85 C84 C83 119.7(15) . . ?
C83 C84 H84 120.2 . . ?
C54 C55 C56 123.3(14) . . ?
C54 C55 C50 118.1(14) . . ?
C50 C55 C56 118.5(14) . . ?
C78 C77 C76 122.7(14) . . ?
C86 C77 C78 116.2(14) . . ?
C86 C77 C76 121.0(14) . . ?
C57 C66 O4 118.2(13) . . ?
C57 C66 C65 125.0(14) . . ?
C65 C66 O4 116.8(13) . . ?
C73 C74 H74 118.0 . . ?
C73 C74 C75 123.9(17) . . ?
C75 C74 H74 118.0 . . ?
C36 C35 H35 119.7 . . ?
C36 C35 C34 120.5(19) . . ?
C34 C35 H35 119.7 . . ?
C69 C70 C71 123.3(17) . . ?
C69 C70 C75 119.6(15) . . ?
C71 C70 C75 117.1(17) . . ?
C24 C25 C26 105.7(13) . . ?
C24 C25 H25 127.1 . . ?
C26 C25 H25 127.1 . . ?
C20 C19 H19 119.4 . . ?
C18 C19 C20 121.2(16) . . ?
C18 C19 H19 119.4 . . ?
C36 C37 H37 119.6 . . ?
C36 C37 C38 120.7(16) . . ?
C38 C37 H37 119.6 . . ?
C35 C36 H36 120.3 . . ?
C37 C36 C35 119.4(17) . . ?
C37 C36 H36 120.3 . . ?
C58 C57 C56 123.0(13) . . ?
C66 C57 C58 116.8(14) . . ?
C66 C57 C56 120.1(13) . . ?
C73 C72 H72 121.1 . . ?
C71 C72 C73 117.9(16) . . ?
C71 C72 H72 121.1 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.4(16) . . ?
C18 C17 H17 119.8 . . ?
C54 C53 H53 119.9 . . ?
C54 C53 C52 120.2(18) . . ?
C52 C53 H53 119.9 . . ?
F6 C22 F4 106.4(15) . . ?
F6 C22 C18 112.5(16) . . ?
F4 C22 C18 111.0(15) . . ?
F5 C22 F6 107.4(16) . . ?
F5 C22 F4 107.4(17) . . ?
F5 C22 C18 111.8(15) . . ?
C47 C48 H48 120.6 . . ?
C49 C48 C47 118.9(15) . . ?
C49 C48 H48 120.6 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 119.9(15) . . ?
C29 C28 H28 120.0 . . ?
C19 C18 C17 119.5(16) . . ?
C19 C18 C22 118.9(16) . . ?
C17 C18 C22 121.7(16) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C12 C11 C10 121.0(18) . . ?
C6 C5 H5 120.9 . . ?
C6 C5 C4 118.3(14) . . ?
C4 C5 H5 120.9 . . ?
C84 C83 C78 120.0(16) . . ?
C84 C83 C82 121.2(16) . . ?
C82 C83 C78 118.8(17) . . ?
C30 C29 C28 120.3(16) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C15 C14 H14 118.8 . . ?
C15 C14 C13 122.4(19) . . ?
C13 C14 H14 118.8 . . ?
C70 C71 H71 117.5 . . ?
C72 C71 C70 124.9(18) . . ?
C72 C71 H71 117.5 . . ?
O10 C89 H89A 109.5 . . ?
O10 C89 H89B 109.5 . . ?
O10 C89 H89C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C48 C49 H49 119.3 . . ?
C48 C49 C50 121.3(14) . . ?
C50 C49 H49 119.3 . . ?
C64 C65 C66 118.0(16) . . ?
C64 C65 H65 121.0 . . ?
C66 C65 H65 121.0 . . ?
C76 C75 C70 118.5(16) . . ?
C74 C75 C76 124.5(15) . . ?
C74 C75 C70 116.9(15) . . ?
C63 C62 H62 119.2 . . ?
C61 C62 C63 121.6(15) . . ?
C61 C62 H62 119.2 . . ?
C52 C51 H51 120.3 . . ?
C52 C51 C50 119.4(16) . . ?
C50 C51 H51 120.3 . . ?
C9 C4 C3 113.9(14) . . ?
C9 C4 C5 122.3(16) . . ?
C5 C4 C3 123.8(14) . . ?
C15 C10 C1 114.9(16) . . ?
C11 C10 C1 125.3(16) . . ?
C11 C10 C15 119.1(16) . . ?
C80 C81 H81 119.5 . . ?
C82 C81 C80 121.0(17) . . ?
C82 C81 H81 119.5 . . ?
C69 C68 C67 118.9(17) . . ?
C69 C68 H68 120.5 . . ?
C67 C68 H68 120.5 . . ?
C53 C52 H52 119.6 . . ?
C51 C52 C53 120.8(15) . . ?
C51 C52 H52 119.6 . . ?
C49 C50 C55 119.6(14) . . ?
C49 C50 C51 120.3(16) . . ?
C51 C50 C55 120.0(16) . . ?
C33 C34 C35 121.1(16) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C33 C38 H38 120.0 . . ?
C37 C38 C33 120.0(16) . . ?
C37 C38 H38 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120(2) . . ?
C13 C12 H12 120.0 . . ?
C83 C82 H82 119.8 . . ?
C81 C82 C83 120.4(17) . . ?
C81 C82 H82 119.8 . . ?
C14 C13 C12 118.5(18) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
F7 C45 F9 107.6(14) . . ?
F7 C45 F8 109.3(17) . . ?
F7 C45 C43 112.0(15) . . ?
F9 C45 C43 111.1(16) . . ?
F8 C45 F9 106.2(16) . . ?
F8 C45 C43 110.4(14) . . ?
O10 C88 H88A 109.9 . . ?
O10 C88 H88B 109.9 . . ?
O10 C88 C87 108.9(17) . . ?
H88A C88 H88B 108.3 . . ?
C87 C88 H88A 109.9 . . ?
C87 C88 H88B 109.9 . . ?
O9 C90 H90A 109.5 . . ?
O9 C90 H90B 109.5 . . ?
O9 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
O9 C87 C88 111.0(18) . . ?
O9 C87 H87A 109.4 . . ?
O9 C87 H87B 109.4 . . ?
C88 C87 H87A 109.4 . . ?
C88 C87 H87B 109.4 . . ?
H87A C87 H87B 108.0 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.208
_oxdiff_exptl_absorpt_empirical_full_min 0.208
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.025(15)
2 -0.025(15)

#####
