# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_cis-Pd2_2_4-BF4_4
_database_code_depnum_ccdc_archive 'CCDC 1946272'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2019-11-25 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H56 N8 Pd2, 4(B F4), 4(C4 H10 O)'
_chemical_formula_sum            'C104 H96 B4 F16 N8 O4 Pd2'
_chemical_formula_weight         2081.92

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'
B B 0.0090 0.0039 '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'
Pd Pd 0.1215 3.9337 '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        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   28.3600(4)
_cell_length_b                   12.35285(17)
_cell_length_c                   27.6660(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.6541(14)
_cell_angle_gamma                90
_cell_volume                     9660.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7401
_cell_measurement_theta_min      4.2760
_cell_measurement_theta_max      72.7860

_exptl_crystal_description       'platy needles'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_F_000             4256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.749
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            15734
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.905
_diffrn_reflns_theta_max         73.463
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             9259
_reflns_number_gt                7879
_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. 
  
 Structure factors included contributions from the .fab file. 
  
 _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, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0580P)²+8.4784P] 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         9259
_refine_ls_number_parameters     555
_refine_ls_number_restraints     198
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1190
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.38683(2) 0.35765(2) 0.84274(2) 0.04936(9) Uani 1 1 d . . . . .
N1 N 0.44962(9) 0.3660(2) 0.81262(10) 0.0523(6) Uani 1 1 d . . . . .
C2 C 0.45706(10) 0.3199(3) 0.77065(11) 0.0505(7) Uani 1 1 d . . . . .
H2A H 0.432165 0.279141 0.754422 0.061 Uiso 1 1 calc R U . . .
C3 C 0.49996(11) 0.3286(3) 0.74912(13) 0.0542(7) Uani 1 1 d . . . . .
C4 C 0.50719(11) 0.2842(3) 0.70267(13) 0.0593(8) Uani 1 1 d . . . . .
C5 C 0.55132(12) 0.2948(4) 0.68510(16) 0.0734(10) Uani 1 1 d . . . . .
H5A H 0.556896 0.263205 0.654787 0.088 Uiso 1 1 calc R U . . .
C6 C 0.58778(13) 0.3512(4) 0.71111(18) 0.0828(12) Uani 1 1 d . . . . .
H6A H 0.617377 0.359187 0.697702 0.099 Uiso 1 1 calc R U . . .
C7 C 0.58168(13) 0.3946(4) 0.75512(17) 0.0804(12) Uani 1 1 d . . . . .
H7A H 0.607257 0.430427 0.772756 0.096 Uiso 1 1 calc R U . . .
C8 C 0.53722(12) 0.3868(3) 0.77497(15) 0.0661(9) Uani 1 1 d . . . . .
C9 C 0.52794(13) 0.4362(4) 0.81824(16) 0.0786(11) Uani 1 1 d . . . . .
H9A H 0.552207 0.476369 0.835825 0.094 Uiso 1 1 calc R U . . .
C10 C 0.48493(13) 0.4281(3) 0.83581(15) 0.0731(10) Uani 1 1 d . . . . .
H10A H 0.478978 0.465855 0.864611 0.088 Uiso 1 1 calc R U . . .
C11 C 0.46953(11) 0.2349(3) 0.67317(13) 0.0592(8) Uani 1 1 d . . . . .
C12 C 0.43936(11) 0.1975(3) 0.64577(13) 0.0604(8) Uani 1 1 d . . . . .
C13 C 0.40300(12) 0.1512(3) 0.61298(12) 0.0570(7) Uani 1 1 d . . . . .
C14 C 0.35572(12) 0.1595(3) 0.62309(12) 0.0576(8) Uani 1 1 d . . . . .
H14A H 0.348017 0.195665 0.651715 0.069 Uiso 1 1 calc R U . . .
C15 C 0.31976(11) 0.1159(3) 0.59206(11) 0.0525(7) Uani 1 1 d D . . . .
C16 C 0.33217(13) 0.0610(3) 0.55064(12) 0.0650(9) Uani 1 1 d . . . . .
H16A H 0.308165 0.030151 0.528958 0.078 Uiso 1 1 calc R U . . .
C17 C 0.37889(14) 0.0516(4) 0.54111(14) 0.0744(10) Uani 1 1 d . . . . .
H17A H 0.386779 0.013141 0.513133 0.089 Uiso 1 1 calc R U . . .
C18 C 0.41429(13) 0.0969(3) 0.57145(13) 0.0667(9) Uani 1 1 d . . . . .
H18A H 0.446327 0.091057 0.564076 0.080 Uiso 1 1 calc R U . . .
C19 C 0.26894(12) 0.1237(4) 0.60523(19) 0.0470(18) Uani 0.670(15) 1 d DG U P A
1
C20 C 0.25867(11) 0.1894(6) 0.6438(3) 0.065(2) Uani 0.670(15) 1 d G U P A 1
H20A H 0.283234 0.228921 0.661281 0.078 Uiso 0.670(15) 1 calc R U P A 1
C21 C 0.21247(12) 0.1973(6) 0.6568(3) 0.069(2) Uani 0.670(15) 1 d G U P A 1
H21A H 0.205460 0.242126 0.683181 0.083 Uiso 0.670(15) 1 calc R U P A 1
N22 N 0.17654(10) 0.1394(4) 0.63125(19) 0.0434(12) Uani 0.670(15) 1 d G U P A 1
C23 C 0.18680(15) 0.0738(5) 0.59267(18) 0.058(2) Uani 0.670(15) 1 d G U P A 1
H23A H 0.162242 0.034260 0.575195 0.070 Uiso 0.670(15) 1 calc R U P A 1
C24 C 0.23300(18) 0.0659(5) 0.57966(16) 0.0516(17) Uani 0.670(15) 1 d G U P A 1
H24A H 0.240016 0.021053 0.553294 0.062 Uiso 0.670(15) 1 calc R U P A 1
C19' C 0.2696(3) 0.1355(8) 0.6001(4) 0.055(4) Uiso 0.330(15) 1 d DG U P A 2
C20' C 0.2566(2) 0.2270(8) 0.6250(4) 0.055(3) Uiso 0.330(15) 1 d G U P A 2
H20B H 0.279260 0.281778 0.633552 0.066 Uiso 0.330(15) 1 calc R U P A 2
C21' C 0.2103(3) 0.2385(9) 0.6374(4) 0.057(3) Uiso 0.330(15) 1 d G U P A 2
H21B H 0.201371 0.301055 0.654400 0.068 Uiso 0.330(15) 1 calc R U P A 2
N22' N 0.1771(2) 0.1584(8) 0.6249(4) 0.057(4) Uiso 0.330(15) 1 d G U P A 2
C23' C 0.1902(3) 0.0669(7) 0.6000(5) 0.030(2) Uiso 0.330(15) 1 d G U P A 2
H23B H 0.167488 0.012134 0.591405 0.036 Uiso 0.330(15) 1 calc R U P A 2
C24' C 0.2364(4) 0.0554(7) 0.5876(5) 0.042(3) Uiso 0.330(15) 1 d G U P A 2
H24B H 0.245378 -0.007144 0.570556 0.051 Uiso 0.330(15) 1 calc R U P A 2
N31 N 0.08664(8) 0.2361(2) 0.60073(9) 0.0511(6) Uani 1 1 d . . . . .
C32 C 0.09991(10) 0.3376(3) 0.59482(11) 0.0513(7) Uani 1 1 d . . . . .
H32A H 0.120133 0.370762 0.619591 0.062 Uiso 1 1 calc R U . . .
C33 C 0.08524(11) 0.3984(3) 0.55331(11) 0.0533(7) Uani 1 1 d . . . . .
C34 C 0.10032(12) 0.5075(3) 0.54612(12) 0.0588(8) Uani 1 1 d . . . . .
C35 C 0.08394(14) 0.5622(3) 0.50479(13) 0.0699(9) Uani 1 1 d . . . . .
H35A H 0.092976 0.635401 0.500442 0.084 Uiso 1 1 calc R U . . .
C36 C 0.05359(15) 0.5101(4) 0.46854(14) 0.0796(11) Uani 1 1 d . . . . .
H36A H 0.043076 0.548587 0.439950 0.096 Uiso 1 1 calc R U . . .
C37 C 0.03943(14) 0.4065(4) 0.47406(13) 0.0755(11) Uani 1 1 d . . . . .
H37A H 0.019547 0.372741 0.449197 0.091 Uiso 1 1 calc R U . . .
C38 C 0.05409(12) 0.3485(3) 0.51667(12) 0.0605(8) Uani 1 1 d . . . . .
C39 C 0.04027(13) 0.2409(3) 0.52508(13) 0.0670(9) Uani 1 1 d . . . . .
H39A H 0.019049 0.205436 0.501898 0.080 Uiso 1 1 calc R U . . .
C40 C 0.05665(12) 0.1876(3) 0.56539(13) 0.0624(8) Uani 1 1 d . . . . .
H40A H 0.047303 0.114585 0.569649 0.075 Uiso 1 1 calc R U . . .
C41 C 0.13439(12) 0.5597(3) 0.57974(12) 0.0578(8) Uani 1 1 d . . . . .
C42 C 0.16483(12) 0.6068(3) 0.60343(12) 0.0583(8) Uani 1 1 d . . . . .
C43 C 0.20303(13) 0.6608(3) 0.63096(12) 0.0575(8) Uani 1 1 d . . . . .
C44 C 0.23283(11) 0.6016(3) 0.66348(12) 0.0547(7) Uani 1 1 d . . . . .
H44A H 0.227150 0.526500 0.667531 0.066 Uiso 1 1 calc R U . . .
C45 C 0.27092(12) 0.6503(3) 0.69030(12) 0.0556(7) Uani 1 1 d D . . . .
C46 C 0.27776(14) 0.7604(3) 0.68509(15) 0.0729(11) Uani 1 1 d . . . . .
H46A H 0.302793 0.795602 0.703860 0.087 Uiso 1 1 calc R U . . .
C47 C 0.24834(17) 0.8196(3) 0.65270(19) 0.0899(15) Uani 1 1 d . . . . .
H47A H 0.253825 0.894938 0.649026 0.108 Uiso 1 1 calc R U . . .
C48 C 0.21116(15) 0.7712(3) 0.62563(16) 0.0758(11) Uani 1 1 d . . . . .
H48A H 0.191232 0.812795 0.603495 0.091 Uiso 1 1 calc R U . . .
C49 C 0.30305(13) 0.5865(2) 0.72330(11) 0.0477(17) Uani 0.678(8) 1 d DG U P B 1
C50 C 0.30906(16) 0.4772(3) 0.71360(12) 0.0621(17) Uani 0.678(8) 1 d G U P B 1
H50A H 0.294302 0.446237 0.684789 0.075 Uiso 0.678(8) 1 calc R U P B 1
C51 C 0.33668(16) 0.4131(2) 0.74606(14) 0.0615(17) Uani 0.678(8) 1 d G U P B 1
H51A H 0.340793 0.338378 0.739433 0.074 Uiso 0.678(8) 1 calc R U P B 1
N52 N 0.35828(12) 0.4583(2) 0.78822(11) 0.0484(14) Uani 0.678(8) 1 d G U P B 1
C53 C 0.35226(15) 0.5677(2) 0.79792(11) 0.0533(12) Uani 0.678(8) 1 d G U P B 1
H53A H 0.367024 0.598579 0.826735 0.064 Uiso 0.678(8) 1 calc R U P B 1
C54 C 0.32465(15) 0.63173(19) 0.76546(13) 0.0546(12) Uani 0.678(8) 1 d G U P B
1
H54A H 0.320534 0.706440 0.772092 0.066 Uiso 0.678(8) 1 calc R U P B 1
C49' C 0.3008(3) 0.5740(6) 0.7267(3) 0.062(5) Uiso 0.322(8) 1 d DG U P B 2
C50' C 0.2883(3) 0.4664(6) 0.7330(3) 0.056(3) Uiso 0.322(8) 1 d G U P B 2
H50B H 0.261553 0.436986 0.714653 0.068 Uiso 0.322(8) 1 calc R U P B 2
C51' C 0.3150(3) 0.4019(5) 0.7660(3) 0.061(3) Uiso 0.322(8) 1 d G U P B 2
H51B H 0.306466 0.328373 0.770314 0.073 Uiso 0.322(8) 1 calc R U P B 2
N52' N 0.3542(3) 0.4450(6) 0.7928(3) 0.056(3) Uiso 0.322(8) 1 d G U P B 2
C53' C 0.3666(2) 0.5526(7) 0.7865(3) 0.043(2) Uiso 0.322(8) 1 d G U P B 2
H53B H 0.393391 0.582044 0.804843 0.052 Uiso 0.322(8) 1 calc R U P B 2
C54' C 0.3400(3) 0.6171(5) 0.7535(3) 0.049(3) Uiso 0.322(8) 1 d G U P B 2
H54B H 0.348479 0.690659 0.749182 0.058 Uiso 0.322(8) 1 calc R U P B 2
B60 B 0.3274(2) 0.0988(6) 0.7577(3) 0.056(2) Uani 0.687(14) 1 d D U P C 1
F61 F 0.3609(3) 0.1641(6) 0.73905(18) 0.0866(17) Uani 0.687(14) 1 d D U P C 1
F62 F 0.3430(2) 0.0733(6) 0.80481(14) 0.0784(13) Uani 0.687(14) 1 d D U P C 1
F63 F 0.28476(18) 0.1529(5) 0.7577(3) 0.102(3) Uani 0.687(14) 1 d D U P C 1
F64 F 0.3204(2) 0.0059(4) 0.7304(3) 0.080(2) Uani 0.687(14) 1 d D U P C 1
B60' B 0.3318(5) 0.1059(12) 0.7510(6) 0.071(6) Uiso 0.313(14) 1 d D U P C 2
F61' F 0.3757(4) 0.1373(10) 0.7391(5) 0.079(3) Uiso 0.313(14) 1 d D U P C 2
F62' F 0.3313(5) 0.0996(11) 0.8008(4) 0.078(4) Uiso 0.313(14) 1 d D U P C 2
F63' F 0.2989(3) 0.1819(6) 0.7340(4) 0.068(2) Uiso 0.313(14) 1 d D U P C 2
F64' F 0.3203(6) 0.0070(10) 0.7305(6) 0.096(6) Uiso 0.313(14) 1 d D U P C 2
B70 B 0.57234(14) 0.1324(3) 0.56164(14) 0.0565(8) Uani 1 1 d . . . . .
F71 F 0.55053(10) 0.2280(2) 0.56911(10) 0.0912(7) Uani 1 1 d . . . . .
F72 F 0.54221(9) 0.0655(2) 0.53399(11) 0.0977(8) Uani 1 1 d . . . . .
F73 F 0.61320(12) 0.1497(3) 0.53944(13) 0.1123(10) Uani 1 1 d . . . . .
F74 F 0.58520(11) 0.0809(2) 0.60471(10) 0.1049(9) 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
Pd1 N52' 1.930(5) . ?
Pd1 N22 1.990(17) 7_556 ?
Pd1 N1 2.029(3) . ?
Pd1 N31 2.040(3) 7_556 ?
Pd1 N52 2.069(2) . ?
Pd1 N22' 2.10(5) 7_556 ?
N1 C2 1.325(4) . ?
N1 C10 1.378(4) . ?
C2 C3 1.401(5) . ?
C3 C8 1.422(5) . ?
C3 C4 1.427(5) . ?
C4 C5 1.385(5) . ?
C4 C11 1.427(5) . ?
C5 C6 1.397(6) . ?
C6 C7 1.354(7) . ?
C7 C8 1.419(6) . ?
C8 C9 1.388(6) . ?
C9 C10 1.353(6) . ?
C11 C12 1.190(5) . ?
C12 C13 1.436(5) . ?
C13 C18 1.390(5) . ?
C13 C14 1.396(5) . ?
C14 C15 1.388(4) . ?
C15 C16 1.400(4) . ?
C15 C19' 1.476(7) . ?
C15 C19 1.518(4) . ?
C16 C17 1.377(5) . ?
C17 C18 1.374(5) . ?
C19 C20 1.3900 . ?
C19 C24 1.3900 . ?
C20 C21 1.3900 . ?
C21 N22 1.3900 . ?
N22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C19' C20' 1.3900 . ?
C19' C24' 1.3900 . ?
C20' C21' 1.3900 . ?
C21' N22' 1.3900 . ?
N22' C23' 1.3900 . ?
C23' C24' 1.3900 . ?
N31 C32 1.324(4) . ?
N31 C40 1.380(4) . ?
C32 C33 1.406(5) . ?
C33 C38 1.430(4) . ?
C33 C34 1.433(5) . ?
C34 C35 1.376(5) . ?
C34 C41 1.438(4) . ?
C35 C36 1.422(5) . ?
C36 C37 1.353(7) . ?
C37 C38 1.413(5) . ?
C38 C39 1.411(6) . ?
C39 C40 1.345(5) . ?
C41 C42 1.192(5) . ?
C42 C43 1.437(5) . ?
C43 C44 1.391(4) . ?
C43 C48 1.393(5) . ?
C44 C45 1.396(4) . ?
C45 C46 1.384(5) . ?
C45 C49 1.466(4) . ?
C45 C49' 1.575(6) . ?
C46 C47 1.383(6) . ?
C47 C48 1.380(6) . ?
C49 C50 1.3900 . ?
C49 C54 1.3900 . ?
C50 C51 1.3900 . ?
C51 N52 1.3900 . ?
N52 C53 1.3900 . ?
C53 C54 1.3900 . ?
C49' C50' 1.3900 . ?
C49' C54' 1.3900 . ?
C50' C51' 1.3900 . ?
C51' N52' 1.3900 . ?
N52' C53' 1.3900 . ?
C53' C54' 1.3900 . ?
B60 F62 1.379(8) . ?
B60 F61 1.379(8) . ?
B60 F64 1.380(6) . ?
B60 F63 1.381(7) . ?
B60' F61' 1.369(13) . ?
B60' F64' 1.375(13) . ?
B60' F63' 1.379(13) . ?
B60' F62' 1.381(13) . ?
B70 F71 1.357(4) . ?
B70 F73 1.372(5) . ?
B70 F74 1.373(5) . ?
B70 F72 1.376(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N52' Pd1 N1 93.7(3) . . ?
N22 Pd1 N1 175.0(13) 7_556 . ?
N52' Pd1 N31 172.7(3) . 7_556 ?
N22 Pd1 N31 91.2(11) 7_556 7_556 ?
N1 Pd1 N31 93.58(10) . 7_556 ?
N22 Pd1 N52 86.6(12) 7_556 . ?
N1 Pd1 N52 88.54(14) . . ?
N31 Pd1 N52 176.76(12) 7_556 . ?
N22 Pd1 N22' 7.7(15) 7_556 7_556 ?
N1 Pd1 N22' 177.2(19) . 7_556 ?
N31 Pd1 N22' 84.1(15) 7_556 7_556 ?
N52 Pd1 N22' 93.9(15) . 7_556 ?
C2 N1 C10 119.1(3) . . ?
C2 N1 Pd1 123.03(19) . . ?
C10 N1 Pd1 117.8(2) . . ?
N1 C2 C3 123.0(3) . . ?
C2 C3 C8 117.4(3) . . ?
C2 C3 C4 123.1(3) . . ?
C8 C3 C4 119.5(3) . . ?
C5 C4 C11 119.7(3) . . ?
C5 C4 C3 118.6(3) . . ?
C11 C4 C3 121.6(3) . . ?
C4 C5 C6 121.2(4) . . ?
C7 C6 C5 121.2(4) . . ?
C6 C7 C8 120.2(4) . . ?
C9 C8 C7 122.7(3) . . ?
C9 C8 C3 118.1(3) . . ?
C7 C8 C3 119.2(4) . . ?
C10 C9 C8 121.2(3) . . ?
C9 C10 N1 121.1(4) . . ?
C12 C11 C4 175.3(4) . . ?
C11 C12 C13 179.3(4) . . ?
C18 C13 C14 119.4(3) . . ?
C18 C13 C12 120.9(3) . . ?
C14 C13 C12 119.8(3) . . ?
C15 C14 C13 121.1(3) . . ?
C14 C15 C16 118.2(3) . . ?
C14 C15 C19' 120.7(5) . . ?
C16 C15 C19' 120.8(5) . . ?
C14 C15 C19 119.4(3) . . ?
C16 C15 C19 122.3(3) . . ?
C17 C16 C15 120.5(3) . . ?
C18 C17 C16 121.0(3) . . ?
C17 C18 C13 119.7(3) . . ?
C20 C19 C24 120.0 . . ?
C20 C19 C15 118.9(3) . . ?
C24 C19 C15 121.1(3) . . ?
C19 C20 C21 120.0 . . ?
N22 C21 C20 120.0 . . ?
C21 N22 C23 120.0 . . ?
C21 N22 Pd1 116.9(2) . 7_556 ?
C23 N22 Pd1 122.7(2) . 7_556 ?
N22 C23 C24 120.0 . . ?
C23 C24 C19 120.0 . . ?
C20' C19' C24' 120.0 . . ?
C20' C19' C15 120.5(6) . . ?
C24' C19' C15 119.1(6) . . ?
C21' C20' C19' 120.0 . . ?
C20' C21' N22' 120.0 . . ?
C23' N22' C21' 120.0 . . ?
C24' C23' N22' 120.0 . . ?
C23' C24' C19' 120.0 . . ?
C32 N31 C40 119.3(3) . . ?
C32 N31 Pd1 122.80(19) . 7_556 ?
C40 N31 Pd1 117.7(2) . 7_556 ?
N31 C32 C33 122.6(3) . . ?
C32 C33 C38 118.2(3) . . ?
C32 C33 C34 123.0(3) . . ?
C38 C33 C34 118.8(3) . . ?
C35 C34 C33 119.5(3) . . ?
C35 C34 C41 118.8(3) . . ?
C33 C34 C41 121.6(3) . . ?
C34 C35 C36 120.5(4) . . ?
C37 C36 C35 121.1(4) . . ?
C36 C37 C38 120.3(3) . . ?
C39 C38 C37 123.3(3) . . ?
C39 C38 C33 117.0(3) . . ?
C37 C38 C33 119.7(3) . . ?
C40 C39 C38 121.1(3) . . ?
C39 C40 N31 121.8(3) . . ?
C42 C41 C34 173.1(4) . . ?
C41 C42 C43 177.4(4) . . ?
C44 C43 C48 119.1(3) . . ?
C44 C43 C42 119.5(3) . . ?
C48 C43 C42 121.5(3) . . ?
C43 C44 C45 121.4(3) . . ?
C46 C45 C44 118.5(3) . . ?
C46 C45 C49 120.5(3) . . ?
C44 C45 C49 121.0(3) . . ?
C46 C45 C49' 125.6(4) . . ?
C44 C45 C49' 115.8(4) . . ?
C47 C46 C45 120.3(3) . . ?
C48 C47 C46 121.1(4) . . ?
C47 C48 C43 119.5(3) . . ?
C50 C49 C54 120.0 . . ?
C50 C49 C45 118.8(2) . . ?
C54 C49 C45 121.0(2) . . ?
C49 C50 C51 120.0 . . ?
N52 C51 C50 120.0 . . ?
C51 N52 C53 120.0 . . ?
C51 N52 Pd1 119.33(16) . . ?
C53 N52 Pd1 119.36(16) . . ?
N52 C53 C54 120.0 . . ?
C53 C54 C49 120.0 . . ?
C50' C49' C54' 120.0 . . ?
C50' C49' C45 121.5(5) . . ?
C54' C49' C45 118.5(5) . . ?
C51' C50' C49' 120.0 . . ?
C50' C51' N52' 120.0 . . ?
C53' N52' C51' 120.0 . . ?
C53' N52' Pd1 120.8(4) . . ?
C51' N52' Pd1 119.0(4) . . ?
C54' C53' N52' 120.0 . . ?
C53' C54' C49' 120.0 . . ?
F62 B60 F61 107.9(5) . . ?
F62 B60 F64 110.5(6) . . ?
F61 B60 F64 110.8(6) . . ?
F62 B60 F63 109.0(6) . . ?
F61 B60 F63 110.3(6) . . ?
F64 B60 F63 108.4(5) . . ?
F61' B60' F64' 109.9(11) . . ?
F61' B60' F63' 109.1(11) . . ?
F64' B60' F63' 109.5(11) . . ?
F61' B60' F62' 109.8(11) . . ?
F64' B60' F62' 110.0(11) . . ?
F63' B60' F62' 108.6(11) . . ?
F71 B70 F73 110.2(3) . . ?
F71 B70 F74 111.3(3) . . ?
F73 B70 F74 106.6(3) . . ?
F71 B70 F72 109.7(3) . . ?
F73 B70 F72 110.7(3) . . ?
F74 B70 F72 108.3(3) . . ?

_refine_diff_density_max         0.620
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.054



#===END


####################################################################### 
# 
# 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_cis-Pd2_4_4-BF4_4
_database_code_depnum_ccdc_archive 'CCDC 1946273'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2019-08-09 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H56 N8 Pd2, 4(B F4), 9(C3 H7 N O)'
_chemical_formula_sum            'C123 H119 B4 F16 N17 O9 Pd2'
_chemical_formula_weight         2539.38

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'
B B 0.0090 0.0039 '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'
Pd Pd 0.1215 3.9337 '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                   23.2193(9)
_cell_length_b                   15.8896(5)
_cell_length_c                   38.7298(15)
_cell_angle_alpha                90
_cell_angle_beta                 112.281(5)
_cell_angle_gamma                90
_cell_volume                     13222.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5399
_cell_measurement_theta_min      3.3860
_cell_measurement_theta_max      71.5930

_exptl_crystal_description       tablets
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_F_000             5216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    2.884
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            14084
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         3.401
_diffrn_reflns_theta_max         73.447
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             14084
_reflns_number_gt                12479
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Structure factors included contributions from the .fab file. 
  
 _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. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          'Refined as a 2-component twin.,Twin,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1312P)²+148.9630P] 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         14084
_refine_ls_number_parameters     479
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0994
_refine_ls_wR_factor_ref         0.2743
_refine_ls_wR_factor_gt          0.2702
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.59402(3) 0.32755(4) 0.62490(2) 0.03815(18) Uani 1 1 d . . . . .
N1 N 0.5179(4) 0.2597(5) 0.5965(2) 0.0376(17) Uani 1 1 d . . . . .
C2 C 0.4751(4) 0.2879(7) 0.5626(3) 0.045(2) Uani 1 1 d . . . . .
H2A H 0.483992 0.338356 0.552403 0.054 Uiso 1 1 calc R U . . .
C3 C 0.4212(4) 0.2469(6) 0.5433(3) 0.039(2) Uani 1 1 d . . . . .
H3A H 0.392682 0.268989 0.520392 0.046 Uiso 1 1 calc R U . . .
C4 C 0.4077(4) 0.1686(6) 0.5581(2) 0.041(2) Uani 1 1 d . . . . .
C5 C 0.3530(4) 0.1225(6) 0.5405(3) 0.042(2) Uani 1 1 d . . . . .
C6 C 0.3422(5) 0.0516(7) 0.5588(3) 0.054(3) Uani 1 1 d . . . . .
H6A H 0.304280 0.021487 0.547654 0.065 Uiso 1 1 calc R U . . .
C7 C 0.3842(6) 0.0249(8) 0.5920(4) 0.067(3) Uani 1 1 d . . . . .
H7A H 0.375906 -0.024183 0.603318 0.080 Uiso 1 1 calc R U . . .
C8 C 0.4391(5) 0.0686(6) 0.6096(3) 0.049(2) Uani 1 1 d . . . . .
H8A H 0.468672 0.049129 0.632699 0.059 Uiso 1 1 calc R U . . .
C9 C 0.4512(5) 0.1425(6) 0.5929(3) 0.048(2) Uani 1 1 d . . . . .
C10 C 0.5062(4) 0.1921(4) 0.6110(2) 0.0321(18) Uani 1 1 d . U . . .
H10A H 0.535160 0.174219 0.634559 0.039 Uiso 1 1 calc R U . . .
C11 C 0.3077(5) 0.1518(6) 0.5043(3) 0.045(2) Uani 1 1 d . . . . .
C12 C 0.2725(5) 0.1784(6) 0.4759(3) 0.047(2) Uani 1 1 d . . . . .
C13 C 0.2293(5) 0.2035(6) 0.4404(3) 0.046(2) Uani 1 1 d . . . . .
C14 C 0.2433(4) 0.2717(6) 0.4227(3) 0.043(2) Uani 1 1 d . . . . .
H14A H 0.281402 0.300791 0.434872 0.051 Uiso 1 1 calc R U . . .
C15 C 0.2037(4) 0.2986(7) 0.3881(3) 0.046(2) Uani 1 1 d . . . . .
C16 C 0.1477(5) 0.2558(9) 0.3700(3) 0.060(3) Uani 1 1 d . . . . .
H16A H 0.120247 0.271326 0.345627 0.072 Uiso 1 1 calc R U . . .
C17 C 0.1339(5) 0.1908(5) 0.3886(3) 0.052(3) Uani 1 1 d . . . . .
H17A H 0.094272 0.164874 0.377268 0.062 Uiso 1 1 calc R U . . .
C18 C 0.1730(4) 0.1606(6) 0.4223(3) 0.041(2) Uani 1 1 d . . . . .
H18A H 0.162545 0.112240 0.433148 0.049 Uiso 1 1 calc R U . . .
C19 C 0.2201(5) 0.3677(7) 0.3703(3) 0.060(3) Uani 1 1 d . . . . .
C20 C 0.2378(6) 0.4296(8) 0.3561(3) 0.063(3) Uani 1 1 d . . . . .
C21 C 0.2555(5) 0.4972(7) 0.3383(3) 0.049(2) Uani 1 1 d . . . . .
C22 C 0.3073(4) 0.5406(6) 0.3595(3) 0.039(2) Uani 1 1 d . . . . .
H22A H 0.329719 0.524824 0.384713 0.047 Uiso 1 1 calc R U . . .
N23 N 0.3272(4) 0.6076(5) 0.3443(2) 0.0384(17) Uani 1 1 d . . . . .
C24 C 0.2963(5) 0.6306(7) 0.3092(3) 0.050(3) Uani 1 1 d . . . . .
H24A H 0.310274 0.677259 0.299125 0.060 Uiso 1 1 calc R U . . .
C25 C 0.2429(6) 0.5862(9) 0.2868(3) 0.064(3) Uani 1 1 d . . . . .
H25A H 0.219450 0.603356 0.261944 0.076 Uiso 1 1 calc R U . . .
C26 C 0.2248(5) 0.5151(8) 0.3024(3) 0.058(3) Uani 1 1 d . . . . .
H26A H 0.191226 0.480577 0.287394 0.070 Uiso 1 1 calc R U . . .
N31 N 0.6373(4) 0.2730(5) 0.5946(2) 0.0405(18) Uani 1 1 d . . . . .
C32 C 0.6308(5) 0.3036(5) 0.5607(3) 0.038(2) Uani 1 1 d . . . . .
H32A H 0.609842 0.355751 0.552883 0.046 Uiso 1 1 calc R U . . .
C33 C 0.6527(5) 0.2635(6) 0.5376(3) 0.044(2) Uani 1 1 d . . . . .
H33A H 0.646521 0.286713 0.513808 0.053 Uiso 1 1 calc R U . . .
C34 C 0.6864(4) 0.1829(6) 0.5495(3) 0.044(2) Uani 1 1 d . . . . .
C35 C 0.7099(5) 0.1336(6) 0.5261(3) 0.049(2) Uani 1 1 d . . . . .
C36 C 0.7435(6) 0.0600(8) 0.5412(4) 0.063(3) Uani 1 1 d . . . . .
H36A H 0.760442 0.026939 0.526856 0.076 Uiso 1 1 calc R U . . .
C37 C 0.7520(7) 0.0353(6) 0.5779(4) 0.061(3) Uani 1 1 d . . . . .
H37A H 0.775046 -0.014250 0.588125 0.073 Uiso 1 1 calc R U . . .
C38 C 0.7282(6) 0.0803(7) 0.5986(3) 0.062(3) Uani 1 1 d . . . . .
H38A H 0.735542 0.062430 0.623314 0.074 Uiso 1 1 calc R U . . .
C39 C 0.6930(5) 0.1525(6) 0.5848(3) 0.051(3) Uani 1 1 d . . . . .
C40 C 0.6685(5) 0.2016(6) 0.6059(3) 0.040(2) Uani 1 1 d . . . . .
H40A H 0.674616 0.182370 0.630275 0.048 Uiso 1 1 calc R U . . .
C41 C 0.6988(6) 0.1576(7) 0.4899(3) 0.059(3) Uani 1 1 d . . . . .
C42 C 0.6912(5) 0.1833(7) 0.4582(3) 0.054(3) Uani 1 1 d . . . . .
C43 C 0.6768(5) 0.2127(7) 0.4207(3) 0.050(2) Uani 1 1 d . . . . .
C44 C 0.6427(6) 0.2830(8) 0.4077(4) 0.061(3) Uani 1 1 d . . . . .
H44A H 0.628634 0.313732 0.424074 0.073 Uiso 1 1 calc R U . . .
C45 C 0.6273(5) 0.3120(6) 0.3716(3) 0.050(2) Uani 1 1 d . . . . .
C46 C 0.6511(7) 0.2686(8) 0.3488(4) 0.070(4) Uani 1 1 d . . . . .
H46A H 0.644290 0.289702 0.324631 0.084 Uiso 1 1 calc R U . . .
C47 C 0.6840(7) 0.1961(13) 0.3606(4) 0.090(6) Uani 1 1 d . . . . .
H47A H 0.697541 0.166273 0.343835 0.108 Uiso 1 1 calc R U . . .
C48 C 0.6983(5) 0.1647(8) 0.3959(3) 0.057(3) Uani 1 1 d . . . . .
H48A H 0.721093 0.113889 0.403800 0.068 Uiso 1 1 calc R U . . .
C49 C 0.5917(7) 0.3861(8) 0.3589(4) 0.068(4) Uani 1 1 d . . . . .
C50 C 0.5598(6) 0.4487(10) 0.3488(4) 0.074(4) Uani 1 1 d . . . . .
C51 C 0.5220(5) 0.5231(7) 0.3358(3) 0.048(2) Uani 1 1 d . . . . .
C52 C 0.4866(5) 0.5569(6) 0.3547(3) 0.043(2) Uani 1 1 d . . . . .
H52A H 0.488125 0.529702 0.376867 0.052 Uiso 1 1 calc R U . . .
N53 N 0.4523(4) 0.6226(5) 0.3439(2) 0.0413(18) Uani 1 1 d . . . . .
C54 C 0.4508(5) 0.6612(7) 0.3140(3) 0.053(3) Uani 1 1 d . . . . .
H54A H 0.425476 0.709949 0.306240 0.064 Uiso 1 1 calc R U . . .
C55 C 0.4836(7) 0.6353(10) 0.2932(4) 0.081(5) Uani 1 1 d . . . . .
H55A H 0.481314 0.665325 0.271479 0.097 Uiso 1 1 calc R U . . .
C56 C 0.5197(7) 0.5654(10) 0.3045(3) 0.073(4) Uani 1 1 d . . . . .
H56A H 0.543249 0.545953 0.290650 0.087 Uiso 1 1 calc R U . . .


_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 N1 2.006(9) . ?
Pd1 N31 2.007(8) . ?
Pd1 N23 2.044(8) 5_666 ?
Pd1 N53 2.056(8) 5_666 ?
N1 C10 1.288(11) . ?
N1 C2 1.386(13) . ?
C2 C3 1.357(14) . ?
C3 C4 1.453(12) . ?
C4 C5 1.401(12) . ?
C4 C9 1.405(14) . ?
C5 C6 1.404(15) . ?
C5 C11 1.472(14) . ?
C6 C7 1.353(17) . ?
C7 C8 1.383(16) . ?
C8 C9 1.420(13) . ?
C9 C10 1.436(13) . ?
C11 C12 1.172(14) . ?
C12 C13 1.417(14) . ?
C13 C14 1.386(14) . ?
C13 C18 1.404(14) . ?
C14 C15 1.376(14) . ?
C15 C16 1.397(15) . ?
C15 C19 1.424(15) . ?
C16 C17 1.364(16) . ?
C17 C18 1.365(15) . ?
C19 C20 1.266(17) . ?
C20 C21 1.419(16) . ?
C21 C26 1.330(15) . ?
C21 C22 1.360(13) . ?
C22 N23 1.379(12) . ?
N23 C24 1.325(13) . ?
C24 C25 1.404(14) . ?
C25 C26 1.417(17) . ?
N31 C40 1.327(11) . ?
N31 C32 1.355(11) . ?
C32 C33 1.346(13) . ?
C33 C34 1.481(14) . ?
C34 C39 1.404(15) . ?
C34 C35 1.452(14) . ?
C35 C41 1.377(16) . ?
C35 C36 1.405(17) . ?
C36 C37 1.416(17) . ?
C37 C38 1.338(15) . ?
C38 C39 1.394(13) . ?
C39 C40 1.397(14) . ?
C41 C42 1.243(16) . ?
C42 C43 1.439(16) . ?
C43 C44 1.351(17) . ?
C43 C48 1.453(15) . ?
C44 C45 1.386(17) . ?
C45 C46 1.389(15) . ?
C45 C49 1.415(15) . ?
C46 C47 1.36(2) . ?
C47 C48 1.373(19) . ?
C49 C50 1.213(18) . ?
C50 C51 1.445(18) . ?
C51 C56 1.372(16) . ?
C51 C52 1.397(14) . ?
C52 N53 1.282(13) . ?
N53 C54 1.298(13) . ?
C54 C55 1.367(15) . ?
C55 C56 1.360(19) . ?

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
N1 Pd1 N31 88.8(3) . . ?
N1 Pd1 N23 177.3(3) . 5_666 ?
N31 Pd1 N23 91.4(3) . 5_666 ?
N1 Pd1 N53 88.9(3) . 5_666 ?
N31 Pd1 N53 177.0(3) . 5_666 ?
N23 Pd1 N53 90.8(3) 5_666 5_666 ?
C10 N1 C2 119.2(9) . . ?
C10 N1 Pd1 119.8(7) . . ?
C2 N1 Pd1 120.8(6) . . ?
C3 C2 N1 123.1(9) . . ?
C2 C3 C4 119.0(9) . . ?
C5 C4 C9 120.2(9) . . ?
C5 C4 C3 123.1(9) . . ?
C9 C4 C3 116.6(9) . . ?
C4 C5 C6 118.4(9) . . ?
C4 C5 C11 119.1(9) . . ?
C6 C5 C11 122.4(9) . . ?
C7 C6 C5 122.0(10) . . ?
C6 C7 C8 120.6(11) . . ?
C7 C8 C9 119.7(11) . . ?
C4 C9 C8 119.1(10) . . ?
C4 C9 C10 119.3(9) . . ?
C8 C9 C10 121.7(10) . . ?
N1 C10 C9 122.7(9) . . ?
C12 C11 C5 177.4(10) . . ?
C11 C12 C13 175.2(11) . . ?
C14 C13 C18 118.7(9) . . ?
C14 C13 C12 119.2(10) . . ?
C18 C13 C12 122.0(9) . . ?
C15 C14 C13 122.1(9) . . ?
C14 C15 C16 119.2(10) . . ?
C14 C15 C19 120.6(9) . . ?
C16 C15 C19 120.2(10) . . ?
C17 C16 C15 117.7(10) . . ?
C16 C17 C18 124.5(10) . . ?
C17 C18 C13 117.6(9) . . ?
C20 C19 C15 176.5(13) . . ?
C19 C20 C21 176.8(12) . . ?
C26 C21 C22 121.5(9) . . ?
C26 C21 C20 122.1(10) . . ?
C22 C21 C20 116.3(10) . . ?
C21 C22 N23 119.8(9) . . ?
C24 N23 C22 120.8(8) . . ?
C24 N23 Pd1 118.5(6) . 5_666 ?
C22 N23 Pd1 120.7(6) . 5_666 ?
N23 C24 C25 120.1(9) . . ?
C24 C25 C26 118.3(10) . . ?
C21 C26 C25 119.2(9) . . ?
C40 N31 C32 118.2(8) . . ?
C40 N31 Pd1 120.5(6) . . ?
C32 N31 Pd1 121.0(6) . . ?
C33 C32 N31 123.0(9) . . ?
C32 C33 C34 119.4(9) . . ?
C39 C34 C35 119.7(9) . . ?
C39 C34 C33 116.7(9) . . ?
C35 C34 C33 123.5(9) . . ?
C41 C35 C36 121.0(10) . . ?
C41 C35 C34 121.0(10) . . ?
C36 C35 C34 118.1(10) . . ?
C35 C36 C37 119.5(10) . . ?
C38 C37 C36 121.5(10) . . ?
C37 C38 C39 121.7(11) . . ?
C38 C39 C40 123.1(10) . . ?
C38 C39 C34 119.2(10) . . ?
C40 C39 C34 117.4(9) . . ?
N31 C40 C39 125.2(9) . . ?
C42 C41 C35 176.2(13) . . ?
C41 C42 C43 175.2(12) . . ?
C44 C43 C42 121.5(10) . . ?
C44 C43 C48 119.2(11) . . ?
C42 C43 C48 119.3(11) . . ?
C43 C44 C45 122.7(10) . . ?
C44 C45 C46 117.6(10) . . ?
C44 C45 C49 121.3(11) . . ?
C46 C45 C49 120.9(11) . . ?
C47 C46 C45 120.9(12) . . ?
C46 C47 C48 122.4(12) . . ?
C47 C48 C43 116.9(12) . . ?
C50 C49 C45 177.5(15) . . ?
C49 C50 C51 178.4(14) . . ?
C56 C51 C52 116.2(11) . . ?
C56 C51 C50 121.6(11) . . ?
C52 C51 C50 122.2(11) . . ?
N53 C52 C51 123.9(10) . . ?
C52 N53 C54 118.6(9) . . ?
C52 N53 Pd1 121.4(7) . 5_666 ?
C54 N53 Pd1 119.9(7) . 5_666 ?
N53 C54 C55 123.5(11) . . ?
C56 C55 C54 118.0(11) . . ?
C55 C56 C51 119.8(11) . . ?

_refine_diff_density_max         1.074
_refine_diff_density_min         -1.790
_refine_diff_density_rms         0.126



#===END


