# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2021

####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 2074482'
loop_
_audit_author_name
_audit_author_address
'Victor Khrustalev'
;Peoples Friendship University of Russia (RUDN University, Moscow)
Russia
;
_audit_update_record             
;
2021-03-31 deposited with the CCDC.	2021-05-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H21 Cl2 N5 Pd'
_chemical_formula_sum            'C25 H21 Cl2 N5 Pd'
_chemical_formula_weight         568.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0070 0.0030 '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'
N N 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.2290 0.2910 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.4000 1.7510 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.187(2)
_cell_length_b                   15.370(3)
_cell_length_c                   15.567(3)
_cell_angle_alpha                81.04(3)
_cell_angle_beta                 84.72(3)
_cell_angle_gamma                82.80(3)
_cell_volume                     2382.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    600
_cell_measurement_theta_min      3.6
_cell_measurement_theta_max      36.0

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.340
_shelx_estimated_absorpt_T_min   0.663
_shelx_estimated_absorpt_T_max   0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   'Scala (Evans, 2006)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.96600
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58909
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.379
_diffrn_reflns_theta_max         36.372
_diffrn_reflns_theta_full        35.422
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measured_fraction_theta_full 0.869
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_Laue_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_point_group_measured_fraction_full 0.869
_reflns_number_total             7824
_reflns_number_gt                6585
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_reduction        iMosflm
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.07P)²+2.4P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0047(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7824
_refine_ls_number_parameters     602
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1260
_refine_ls_wR_factor_gt          0.1098
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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 0.69742(3) 0.62450(2) 0.62369(2) 0.02977(13) Uani 1 1 d . . . . .
Cl1 Cl 0.49728(11) 0.63152(6) 0.56397(6) 0.0386(3) Uani 1 1 d . . . . .
Cl2 Cl 0.90485(11) 0.59721(7) 0.67948(6) 0.0410(3) Uani 1 1 d . . . . .
N1 N 0.7036(3) 0.42833(18) 0.65362(19) 0.0320(7) Uani 1 1 d . . . . .
C2 C 0.7247(4) 0.5022(2) 0.6006(2) 0.0311(9) Uani 1 1 d . . . . .
N3 N 0.7721(3) 0.47486(18) 0.52350(18) 0.0297(7) Uani 1 1 d . . . . .
C4 C 0.7799(4) 0.3829(2) 0.5356(2) 0.0314(9) Uani 1 1 d . . . . .
N5 N 0.7381(4) 0.35196(19) 0.61482(19) 0.0343(8) Uani 1 1 d . . . . .
C6 C 0.6512(4) 0.4180(2) 0.7425(2) 0.0333(9) Uani 1 1 d . . . . .
C7 C 0.5455(4) 0.4753(3) 0.7688(2) 0.0386(10) Uani 1 1 d . . . . .
H7 H 0.5084 0.5230 0.7285 0.046 Uiso 1 1 calc R U . . .
C8 C 0.4938(5) 0.4624(3) 0.8552(3) 0.0480(11) Uani 1 1 d . . . . .
H8 H 0.4214 0.5019 0.8742 0.058 Uiso 1 1 calc R U . . .
C9 C 0.5465(6) 0.3930(3) 0.9131(3) 0.0554(13) Uani 1 1 d . . . . .
H9 H 0.5106 0.3842 0.9719 0.066 Uiso 1 1 calc R U . . .
C10 C 0.6521(6) 0.3360(3) 0.8855(3) 0.0590(14) Uani 1 1 d . . . . .
H10 H 0.6877 0.2875 0.9254 0.071 Uiso 1 1 calc R U . . .
C11 C 0.7068(5) 0.3485(3) 0.8000(3) 0.0480(11) Uani 1 1 d . . . . .
H11 H 0.7809 0.3101 0.7815 0.058 Uiso 1 1 calc R U . . .
C12 C 0.8048(4) 0.5326(2) 0.4446(2) 0.0306(9) Uani 1 1 d . . . . .
C13 C 0.7403(4) 0.5295(3) 0.3707(2) 0.0384(10) Uani 1 1 d . . . . .
H13 H 0.6757 0.4898 0.3717 0.046 Uiso 1 1 calc R U . . .
C14 C 0.7727(5) 0.5860(3) 0.2953(3) 0.0479(12) Uani 1 1 d . . . . .
H14 H 0.7312 0.5839 0.2436 0.057 Uiso 1 1 calc R U . . .
C15 C 0.8635(5) 0.6446(3) 0.2944(3) 0.0473(11) Uani 1 1 d . . . . .
H15 H 0.8839 0.6833 0.2424 0.057 Uiso 1 1 calc R U . . .
C16 C 0.9259(5) 0.6477(3) 0.3691(3) 0.0416(10) Uani 1 1 d . . . . .
H16 H 0.9888 0.6885 0.3684 0.050 Uiso 1 1 calc R U . . .
C17 C 0.8965(4) 0.5912(2) 0.4448(2) 0.0348(9) Uani 1 1 d . . . . .
H17 H 0.9390 0.5928 0.4962 0.042 Uiso 1 1 calc R U . . .
N6 N 0.8316(4) 0.3356(2) 0.4713(2) 0.0356(8) Uani 1 1 d . . . . .
H4 H 0.875(5) 0.363(3) 0.429(3) 0.043 Uiso 1 1 d . U . . .
C18 C 0.8322(5) 0.2437(2) 0.4736(2) 0.0379(10) Uani 1 1 d . . . . .
C19 C 0.7470(5) 0.1936(3) 0.5291(3) 0.0459(11) Uani 1 1 d . . . . .
H19 H 0.6856 0.2206 0.5695 0.055 Uiso 1 1 calc R U . . .
C20 C 0.7518(5) 0.1040(3) 0.5252(3) 0.0556(13) Uani 1 1 d . . . . .
H20 H 0.6933 0.0696 0.5633 0.067 Uiso 1 1 calc R U . . .
C21 C 0.8399(7) 0.0638(3) 0.4670(3) 0.0698(16) Uani 1 1 d . . . . .
H21 H 0.8416 0.0024 0.4639 0.084 Uiso 1 1 calc R U . . .
C22 C 0.9256(8) 0.1143(3) 0.4131(4) 0.093(2) Uani 1 1 d . . . . .
H22 H 0.9881 0.0867 0.3738 0.111 Uiso 1 1 calc R U . . .
C23 C 0.9227(6) 0.2033(3) 0.4150(3) 0.0690(16) Uani 1 1 d . . . . .
H23 H 0.9817 0.2372 0.3768 0.083 Uiso 1 1 calc R U . . .
N7 N 0.6610(4) 0.7584(2) 0.6510(2) 0.0373(8) Uani 1 1 d . . . . .
C24 C 0.5581(5) 0.8131(3) 0.6211(3) 0.0558(13) Uani 1 1 d . . . . .
H24 H 0.5057 0.7939 0.5817 0.067 Uiso 1 1 calc R U . . .
C25 C 0.5241(6) 0.8964(3) 0.6446(4) 0.0688(16) Uani 1 1 d . . . . .
H25 H 0.4501 0.9338 0.6216 0.083 Uiso 1 1 calc R U . . .
C26 C 0.5992(6) 0.9244(3) 0.7017(3) 0.0585(14) Uani 1 1 d . . . . .
H26 H 0.5784 0.9815 0.7187 0.070 Uiso 1 1 calc R U . . .
C27 C 0.7032(6) 0.8689(3) 0.7330(3) 0.0613(14) Uani 1 1 d . . . . .
H27 H 0.7558 0.8864 0.7733 0.074 Uiso 1 1 calc R U . . .
C28 C 0.7325(5) 0.7866(3) 0.7062(3) 0.0526(12) Uani 1 1 d . . . . .
H28 H 0.8067 0.7487 0.7281 0.063 Uiso 1 1 calc R U . . .
Pd2 Pd 0.75874(3) 0.82162(2) 0.03198(2) 0.03201(14) Uani 1 1 d . . . . .
Cl3 Cl 0.56018(12) 0.86027(8) -0.03011(8) 0.0525(3) Uani 1 1 d . . . . .
Cl4 Cl 0.96063(11) 0.79573(6) 0.09534(6) 0.0378(2) Uani 1 1 d . . . . .
N29 N 0.7055(3) 0.95908(19) 0.14785(18) 0.0326(7) Uani 1 1 d . . . . .
C30 C 0.7391(4) 0.9385(2) 0.0685(2) 0.0322(9) Uani 1 1 d . . . . .
N31 N 0.7675(3) 1.01635(18) 0.01998(18) 0.0302(7) Uani 1 1 d . . . . .
C32 C 0.7534(4) 1.0798(2) 0.0757(2) 0.0302(8) Uani 1 1 d . . . . .
N33 N 0.7151(3) 1.04721(18) 0.15466(19) 0.0336(8) Uani 1 1 d . . . . .
C34 C 0.6696(4) 0.9010(2) 0.2251(2) 0.0344(9) Uani 1 1 d . . . . .
C35 C 0.5906(5) 0.8359(3) 0.2215(3) 0.0414(10) Uani 1 1 d . . . . .
H35 H 0.5582 0.8292 0.1679 0.050 Uiso 1 1 calc R U . . .
C36 C 0.5584(5) 0.7799(3) 0.2977(3) 0.0511(12) Uani 1 1 d . . . . .
H36 H 0.5037 0.7345 0.2963 0.061 Uiso 1 1 calc R U . . .
C37 C 0.6054(5) 0.7900(3) 0.3747(3) 0.0533(12) Uani 1 1 d . . . . .
H37 H 0.5843 0.7509 0.4264 0.064 Uiso 1 1 calc R U . . .
C38 C 0.6825(6) 0.8559(3) 0.3777(3) 0.0578(13) Uani 1 1 d . . . . .
H38 H 0.7129 0.8632 0.4318 0.069 Uiso 1 1 calc R U . . .
C39 C 0.7165(5) 0.9120(3) 0.3032(3) 0.0466(11) Uani 1 1 d . . . . .
H39 H 0.7711 0.9573 0.3052 0.056 Uiso 1 1 calc R U . . .
C40 C 0.8083(4) 1.0296(2) -0.0717(2) 0.0303(9) Uani 1 1 d . . . . .
C41 C 0.7366(5) 1.0933(2) -0.1267(2) 0.0390(10) Uani 1 1 d . . . . .
H41 H 0.6598 1.1271 -0.1047 0.047 Uiso 1 1 calc R U . . .
C42 C 0.7787(5) 1.1072(3) -0.2147(3) 0.0469(12) Uani 1 1 d . . . . .
H42 H 0.7311 1.1516 -0.2532 0.056 Uiso 1 1 calc R U . . .
C43 C 0.8885(5) 1.0574(3) -0.2464(3) 0.0448(11) Uani 1 1 d . . . . .
H43 H 0.9165 1.0673 -0.3067 0.054 Uiso 1 1 calc R U . . .
C44 C 0.9590(5) 0.9922(3) -0.1905(2) 0.0417(10) Uani 1 1 d . . . . .
H44 H 1.0343 0.9572 -0.2126 0.050 Uiso 1 1 calc R U . . .
C45 C 0.9184(4) 0.9788(2) -0.1025(2) 0.0367(9) Uani 1 1 d . . . . .
H45 H 0.9662 0.9348 -0.0637 0.044 Uiso 1 1 calc R U . . .
N34 N 0.7840(4) 1.16381(19) 0.04797(19) 0.0328(8) Uani 1 1 d . . . . .
H32 H 0.845(5) 1.170(3) 0.007(3) 0.039 Uiso 1 1 d . U . . .
C46 C 0.7802(4) 1.2247(2) 0.1090(2) 0.0329(9) Uani 1 1 d . . . . .
C47 C 0.6664(5) 1.2434(3) 0.1609(3) 0.0502(12) Uani 1 1 d . . . . .
H47 H 0.5896 1.2156 0.1566 0.060 Uiso 1 1 calc R U . . .
C48 C 0.6645(6) 1.3024(3) 0.2192(3) 0.0598(14) Uani 1 1 d . . . . .
H48 H 0.5863 1.3153 0.2553 0.072 Uiso 1 1 calc R U . . .
C49 C 0.7772(6) 1.3432(3) 0.2252(3) 0.0568(14) Uani 1 1 d . . . . .
H49 H 0.7763 1.3833 0.2661 0.068 Uiso 1 1 calc R U . . .
C50 C 0.8893(5) 1.3257(3) 0.1722(3) 0.0533(13) Uani 1 1 d . . . . .
H50 H 0.9655 1.3546 0.1753 0.064 Uiso 1 1 calc R U . . .
C51 C 0.8911(5) 1.2658(3) 0.1142(3) 0.0417(10) Uani 1 1 d . . . . .
H51 H 0.9691 1.2530 0.0779 0.050 Uiso 1 1 calc R U . . .
N35 N 0.7777(4) 0.6938(2) -0.0037(2) 0.0425(9) Uani 1 1 d . . . . .
C52 C 0.7317(5) 0.6795(3) -0.0771(3) 0.0578(13) Uani 1 1 d . . . . .
H52 H 0.6898 0.7283 -0.1139 0.069 Uiso 1 1 calc R U . . .
C53 C 0.7429(7) 0.5961(4) -0.1013(4) 0.082(2) Uani 1 1 d . . . . .
H53 H 0.7129 0.5880 -0.1552 0.098 Uiso 1 1 calc R U . . .
C54 C 0.7975(7) 0.5256(4) -0.0469(6) 0.094(3) Uani 1 1 d . . . . .
H54 H 0.8047 0.4675 -0.0619 0.113 Uiso 1 1 calc R U . . .
C55 C 0.8419(6) 0.5396(3) 0.0295(4) 0.0747(18) Uani 1 1 d . . . . .
H55 H 0.8785 0.4909 0.0689 0.090 Uiso 1 1 calc R U . . .
C56 C 0.8334(5) 0.6245(3) 0.0491(3) 0.0538(13) Uani 1 1 d . . . . .
H56 H 0.8677 0.6342 0.1011 0.065 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 C2 1.950(4) . ?
Pd1 N7 2.146(3) . ?
Pd1 Cl1 2.3011(12) . ?
Pd1 Cl2 2.3231(12) . ?
N1 C2 1.324(5) . ?
N1 N5 1.394(4) . ?
N1 C6 1.429(5) . ?
C2 N3 1.359(5) . ?
N3 C4 1.390(4) . ?
N3 C12 1.437(4) . ?
C4 N5 1.304(5) . ?
C4 N6 1.356(5) . ?
C6 C7 1.377(6) . ?
C6 C11 1.381(5) . ?
C7 C8 1.393(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.373(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(6) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C17 1.377(5) . ?
C12 C13 1.387(5) . ?
C13 C14 1.387(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.367(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
N6 C18 1.408(5) . ?
N6 H4 0.84(4) . ?
C18 C19 1.383(6) . ?
C18 C23 1.394(6) . ?
C19 C20 1.382(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.376(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.377(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.370(7) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
N7 C28 1.330(5) . ?
N7 C24 1.330(6) . ?
C24 C25 1.381(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.373(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.352(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.382(6) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
Pd2 C30 1.949(4) . ?
Pd2 N35 2.104(3) . ?
Pd2 Cl3 2.2931(13) . ?
Pd2 Cl4 2.3251(12) . ?
N29 C30 1.326(5) . ?
N29 N33 1.391(4) . ?
N29 C34 1.429(5) . ?
C30 N31 1.360(5) . ?
N31 C32 1.390(4) . ?
N31 C40 1.440(4) . ?
C32 N33 1.297(5) . ?
C32 N34 1.361(5) . ?
C34 C35 1.370(6) . ?
C34 C39 1.388(5) . ?
C35 C36 1.392(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.368(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.366(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.378(6) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C45 1.376(6) . ?
C40 C41 1.378(5) . ?
C41 C42 1.389(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.373(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.392(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.386(5) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
N34 C46 1.429(4) . ?
N34 H32 0.85(4) . ?
C46 C51 1.376(6) . ?
C46 C47 1.376(6) . ?
C47 C48 1.377(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.392(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.370(7) . ?
C49 H49 0.9500 . ?
C50 C51 1.384(6) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
N35 C52 1.333(6) . ?
N35 C56 1.339(6) . ?
C52 C53 1.380(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.360(10) . ?
C53 H53 0.9500 . ?
C54 C55 1.368(10) . ?
C54 H54 0.9500 . ?
C55 C56 1.376(6) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pd1 N7 178.11(15) . . ?
C2 Pd1 Cl1 85.41(12) . . ?
N7 Pd1 Cl1 93.33(10) . . ?
C2 Pd1 Cl2 86.56(12) . . ?
N7 Pd1 Cl2 94.71(10) . . ?
Cl1 Pd1 Cl2 171.96(3) . . ?
C2 N1 N5 113.4(3) . . ?
C2 N1 C6 128.8(3) . . ?
N5 N1 C6 117.8(3) . . ?
N1 C2 N3 104.7(3) . . ?
N1 C2 Pd1 129.4(3) . . ?
N3 C2 Pd1 125.9(3) . . ?
C2 N3 C4 107.5(3) . . ?
C2 N3 C12 125.0(3) . . ?
C4 N3 C12 127.5(3) . . ?
N5 C4 N6 127.3(3) . . ?
N5 C4 N3 111.2(3) . . ?
N6 C4 N3 121.4(3) . . ?
C4 N5 N1 103.1(3) . . ?
C7 C6 C11 121.4(4) . . ?
C7 C6 N1 120.1(3) . . ?
C11 C6 N1 118.5(4) . . ?
C6 C7 C8 119.0(4) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C9 C8 C7 120.5(5) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 119.7(4) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C10 C11 120.9(4) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C6 C11 C10 118.6(4) . . ?
C6 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C17 C12 C13 121.6(3) . . ?
C17 C12 N3 119.4(3) . . ?
C13 C12 N3 119.0(3) . . ?
C12 C13 C14 118.2(4) . . ?
C12 C13 H13 120.9 . . ?
C14 C13 H13 120.9 . . ?
C15 C14 C13 121.0(4) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 120.2(4) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 119.9(4) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C12 C17 C16 119.2(3) . . ?
C12 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C4 N6 C18 125.8(3) . . ?
C4 N6 H4 116(3) . . ?
C18 N6 H4 118(3) . . ?
C19 C18 C23 119.9(4) . . ?
C19 C18 N6 123.3(4) . . ?
C23 C18 N6 116.8(4) . . ?
C18 C19 C20 119.5(4) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C21 C20 C19 121.1(5) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 118.8(4) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C23 C22 C21 121.6(5) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C22 C23 C18 119.2(5) . . ?
C22 C23 H23 120.4 . . ?
C18 C23 H23 120.4 . . ?
C28 N7 C24 117.3(4) . . ?
C28 N7 Pd1 120.8(3) . . ?
C24 N7 Pd1 121.5(3) . . ?
N7 C24 C25 123.0(5) . . ?
N7 C24 H24 118.5 . . ?
C25 C24 H24 118.5 . . ?
C26 C25 C24 118.8(5) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
C27 C26 C25 118.6(4) . . ?
C27 C26 H26 120.7 . . ?
C25 C26 H26 120.7 . . ?
C26 C27 C28 119.6(5) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
N7 C28 C27 122.7(5) . . ?
N7 C28 H28 118.7 . . ?
C27 C28 H28 118.7 . . ?
C30 Pd2 N35 178.28(14) . . ?
C30 Pd2 Cl3 88.14(12) . . ?
N35 Pd2 Cl3 92.10(12) . . ?
C30 Pd2 Cl4 86.98(12) . . ?
N35 Pd2 Cl4 92.82(11) . . ?
Cl3 Pd2 Cl4 174.91(4) . . ?
C30 N29 N33 113.8(3) . . ?
C30 N29 C34 127.7(3) . . ?
N33 N29 C34 118.4(3) . . ?
N29 C30 N31 104.3(3) . . ?
N29 C30 Pd2 127.9(3) . . ?
N31 C30 Pd2 127.7(3) . . ?
C30 N31 C32 107.3(3) . . ?
C30 N31 C40 126.2(3) . . ?
C32 N31 C40 126.5(3) . . ?
N33 C32 N34 126.5(3) . . ?
N33 C32 N31 111.7(3) . . ?
N34 C32 N31 121.7(3) . . ?
C32 N33 N29 102.8(3) . . ?
C35 C34 C39 121.1(4) . . ?
C35 C34 N29 120.4(3) . . ?
C39 C34 N29 118.6(4) . . ?
C34 C35 C36 119.0(4) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C37 C36 C35 120.2(4) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C38 C37 C36 120.3(4) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 120.7(4) . . ?
C37 C38 H38 119.7 . . ?
C39 C38 H38 119.7 . . ?
C38 C39 C34 118.8(4) . . ?
C38 C39 H39 120.6 . . ?
C34 C39 H39 120.6 . . ?
C45 C40 C41 121.5(4) . . ?
C45 C40 N31 119.3(3) . . ?
C41 C40 N31 119.2(4) . . ?
C40 C41 C42 118.8(4) . . ?
C40 C41 H41 120.6 . . ?
C42 C41 H41 120.6 . . ?
C43 C42 C41 120.5(4) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C42 C43 C44 120.2(4) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C45 C44 C43 119.5(4) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C40 C45 C44 119.5(4) . . ?
C40 C45 H45 120.3 . . ?
C44 C45 H45 120.3 . . ?
C32 N34 C46 120.0(3) . . ?
C32 N34 H32 117(3) . . ?
C46 N34 H32 114(3) . . ?
C51 C46 C47 120.3(4) . . ?
C51 C46 N34 119.1(4) . . ?
C47 C46 N34 120.5(4) . . ?
C48 C47 C46 119.7(5) . . ?
C48 C47 H47 120.1 . . ?
C46 C47 H47 120.1 . . ?
C47 C48 C49 120.0(5) . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C50 C49 C48 120.0(4) . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C49 C50 C51 119.8(4) . . ?
C49 C50 H50 120.1 . . ?
C51 C50 H50 120.1 . . ?
C46 C51 C50 120.1(4) . . ?
C46 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C52 N35 C56 118.7(4) . . ?
C52 N35 Pd2 121.3(3) . . ?
C56 N35 Pd2 119.9(3) . . ?
N35 C52 C53 122.0(5) . . ?
N35 C52 H52 119.0 . . ?
C53 C52 H52 119.0 . . ?
C54 C53 C52 119.1(6) . . ?
C54 C53 H53 120.4 . . ?
C52 C53 H53 120.4 . . ?
C53 C54 C55 119.1(5) . . ?
C53 C54 H54 120.5 . . ?
C55 C54 H54 120.5 . . ?
C54 C55 C56 119.6(6) . . ?
C54 C55 H55 120.2 . . ?
C56 C55 H55 120.2 . . ?
N35 C56 C55 121.4(5) . . ?
N35 C56 H56 119.3 . . ?
C55 C56 H56 119.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N5 N1 C2 N3 1.3(4) . . . . ?
C6 N1 C2 N3 -178.5(4) . . . . ?
N5 N1 C2 Pd1 -178.3(3) . . . . ?
C6 N1 C2 Pd1 1.9(6) . . . . ?
N1 C2 N3 C4 -1.4(4) . . . . ?
Pd1 C2 N3 C4 178.2(3) . . . . ?
N1 C2 N3 C12 177.6(3) . . . . ?
Pd1 C2 N3 C12 -2.8(6) . . . . ?
C2 N3 C4 N5 1.1(5) . . . . ?
C12 N3 C4 N5 -177.8(4) . . . . ?
C2 N3 C4 N6 -176.0(4) . . . . ?
C12 N3 C4 N6 5.1(6) . . . . ?
N6 C4 N5 N1 176.5(4) . . . . ?
N3 C4 N5 N1 -0.4(4) . . . . ?
C2 N1 N5 C4 -0.6(4) . . . . ?
C6 N1 N5 C4 179.2(4) . . . . ?
C2 N1 C6 C7 41.4(6) . . . . ?
N5 N1 C6 C7 -138.3(4) . . . . ?
C2 N1 C6 C11 -140.1(4) . . . . ?
N5 N1 C6 C11 40.2(5) . . . . ?
C11 C6 C7 C8 -0.2(6) . . . . ?
N1 C6 C7 C8 178.2(4) . . . . ?
C6 C7 C8 C9 -0.7(6) . . . . ?
C7 C8 C9 C10 0.4(7) . . . . ?
C8 C9 C10 C11 0.8(8) . . . . ?
C7 C6 C11 C10 1.4(7) . . . . ?
N1 C6 C11 C10 -177.1(4) . . . . ?
C9 C10 C11 C6 -1.7(7) . . . . ?
C2 N3 C12 C17 57.2(6) . . . . ?
C4 N3 C12 C17 -124.0(4) . . . . ?
C2 N3 C12 C13 -121.1(4) . . . . ?
C4 N3 C12 C13 57.7(6) . . . . ?
C17 C12 C13 C14 1.5(6) . . . . ?
N3 C12 C13 C14 179.7(4) . . . . ?
C12 C13 C14 C15 -1.5(7) . . . . ?
C13 C14 C15 C16 0.7(8) . . . . ?
C14 C15 C16 C17 0.1(7) . . . . ?
C13 C12 C17 C16 -0.7(6) . . . . ?
N3 C12 C17 C16 -178.9(4) . . . . ?
C15 C16 C17 C12 -0.2(6) . . . . ?
N5 C4 N6 C18 10.1(7) . . . . ?
N3 C4 N6 C18 -173.3(4) . . . . ?
C4 N6 C18 C19 20.1(6) . . . . ?
C4 N6 C18 C23 -161.1(5) . . . . ?
C23 C18 C19 C20 -0.6(7) . . . . ?
N6 C18 C19 C20 178.1(4) . . . . ?
C18 C19 C20 C21 -0.1(7) . . . . ?
C19 C20 C21 C22 1.1(8) . . . . ?
C20 C21 C22 C23 -1.5(10) . . . . ?
C21 C22 C23 C18 0.9(10) . . . . ?
C19 C18 C23 C22 0.1(8) . . . . ?
N6 C18 C23 C22 -178.6(5) . . . . ?
C28 N7 C24 C25 0.2(7) . . . . ?
Pd1 N7 C24 C25 173.3(4) . . . . ?
N7 C24 C25 C26 -0.2(9) . . . . ?
C24 C25 C26 C27 -0.3(9) . . . . ?
C25 C26 C27 C28 0.9(8) . . . . ?
C24 N7 C28 C27 0.4(7) . . . . ?
Pd1 N7 C28 C27 -172.7(4) . . . . ?
C26 C27 C28 N7 -0.9(8) . . . . ?
N33 N29 C30 N31 -2.2(5) . . . . ?
C34 N29 C30 N31 -178.3(4) . . . . ?
N33 N29 C30 Pd2 172.9(3) . . . . ?
C34 N29 C30 Pd2 -3.2(6) . . . . ?
N29 C30 N31 C32 2.3(4) . . . . ?
Pd2 C30 N31 C32 -172.9(3) . . . . ?
N29 C30 N31 C40 -179.4(4) . . . . ?
Pd2 C30 N31 C40 5.4(6) . . . . ?
C30 N31 C32 N33 -1.7(5) . . . . ?
C40 N31 C32 N33 -180.0(4) . . . . ?
C30 N31 C32 N34 175.4(4) . . . . ?
C40 N31 C32 N34 -2.9(6) . . . . ?
N34 C32 N33 N29 -176.6(4) . . . . ?
N31 C32 N33 N29 0.3(4) . . . . ?
C30 N29 N33 C32 1.2(5) . . . . ?
C34 N29 N33 C32 177.7(4) . . . . ?
C30 N29 C34 C35 -40.4(6) . . . . ?
N33 N29 C34 C35 143.7(4) . . . . ?
C30 N29 C34 C39 139.5(4) . . . . ?
N33 N29 C34 C39 -36.4(5) . . . . ?
C39 C34 C35 C36 -0.6(7) . . . . ?
N29 C34 C35 C36 179.4(4) . . . . ?
C34 C35 C36 C37 0.0(7) . . . . ?
C35 C36 C37 C38 1.0(8) . . . . ?
C36 C37 C38 C39 -1.4(8) . . . . ?
C37 C38 C39 C34 0.8(8) . . . . ?
C35 C34 C39 C38 0.2(7) . . . . ?
N29 C34 C39 C38 -179.8(4) . . . . ?
C30 N31 C40 C45 -55.9(5) . . . . ?
C32 N31 C40 C45 122.0(4) . . . . ?
C30 N31 C40 C41 124.4(4) . . . . ?
C32 N31 C40 C41 -57.6(5) . . . . ?
C45 C40 C41 C42 -1.3(6) . . . . ?
N31 C40 C41 C42 178.3(4) . . . . ?
C40 C41 C42 C43 1.0(7) . . . . ?
C41 C42 C43 C44 0.0(7) . . . . ?
C42 C43 C44 C45 -0.8(6) . . . . ?
C41 C40 C45 C44 0.5(6) . . . . ?
N31 C40 C45 C44 -179.1(3) . . . . ?
C43 C44 C45 C40 0.5(6) . . . . ?
N33 C32 N34 C46 2.5(6) . . . . ?
N31 C32 N34 C46 -174.1(4) . . . . ?
C32 N34 C46 C51 125.1(4) . . . . ?
C32 N34 C46 C47 -56.1(5) . . . . ?
C51 C46 C47 C48 -1.0(7) . . . . ?
N34 C46 C47 C48 -179.8(4) . . . . ?
C46 C47 C48 C49 0.2(7) . . . . ?
C47 C48 C49 C50 1.0(8) . . . . ?
C48 C49 C50 C51 -1.5(7) . . . . ?
C47 C46 C51 C50 0.5(6) . . . . ?
N34 C46 C51 C50 179.3(4) . . . . ?
C49 C50 C51 C46 0.8(7) . . . . ?
C56 N35 C52 C53 -1.8(7) . . . . ?
Pd2 N35 C52 C53 -179.8(4) . . . . ?
N35 C52 C53 C54 2.9(9) . . . . ?
C52 C53 C54 C55 -1.2(9) . . . . ?
C53 C54 C55 C56 -1.5(9) . . . . ?
C52 N35 C56 C55 -0.9(7) . . . . ?
Pd2 N35 C56 C55 177.1(4) . . . . ?
C54 C55 C56 N35 2.6(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N6 H4 Cl2 0.84(4) 2.75(5) 3.544(4) 157(4) 2_766
N34 H32 Cl4 0.85(4) 2.48(5) 3.322(4) 170(4) 2_775

_refine_diff_density_max         0.676
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.108

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT029_3a                  
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.869 Why?  
RESPONSE: 
1. Because of triclinic crystal system of the crystal and use of phi-scanning 
mode only, at least two runs with different orientations of the single-crystal 
being measured are needed to achieve sufficient completeness of a diffraction 
dataset. Unfortunately, the single-crystal of 3a had been destroying under 
X-ray radiation that did not allow to carry out data collection for other
orientation of the crystal. 

2. In the applied setup of the synchrotron diffractometer, the low-temperature 
device eclipsed a small region of the 2D detector near the high-angle limit. 
This small shadowed region has not been masked during integration of the 
diffraction frames, which erroneously resulted in zero intensity of some 
reflections.
;
_vrf_PLAT911_3a                  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        889 Report
RESPONSE: 
In order to achieve bettter I/sigma statistics for high-angle reflections 
we selected exposure time so as to admit a minor fraction of intensity 
overloads in the low-angle part of the detector. These low-angle reflections 
with unprecisely measured intensities were excluded from final steps of the 
refinement.
;
####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 2074483'
loop_
_audit_author_name
_audit_author_address
'Victor Khrustalev'
;Peoples Friendship University of Russia (RUDN University, Moscow)
Russia
;
_audit_update_record             
;
2021-03-31 deposited with the CCDC.	2021-05-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H25 Cl2 N5 O Pd'
_chemical_formula_sum            'C20 H25 Cl2 N5 O Pd'
_chemical_formula_weight         528.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0050 0.0020 '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'
N N 0.0090 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0150 0.0080 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1780 0.2030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.7210 1.2579 '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                   15.332(3)
_cell_length_b                   9.4559(19)
_cell_length_c                   31.070(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.70(3)
_cell_angle_gamma                90
_cell_volume                     4502.5(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    600
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      30.3

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_F_000             2144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    1.486
_shelx_estimated_absorpt_T_min   0.660
_shelx_estimated_absorpt_T_max   0.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_process_details   'Scala (Evans, 2006)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.80246
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30928
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         3.387
_diffrn_reflns_theta_max         30.870
_diffrn_reflns_theta_full        28.782
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             4851
_reflns_number_gt                4779
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_reduction        iMosflm
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+150.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0031(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4851
_refine_ls_number_parameters     267
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.1662
_refine_ls_wR_factor_gt          0.1659
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.050
_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 0.66224(3) 0.38183(5) 0.64142(2) 0.0171(2) Uani 1 1 d . . . . .
Cl1 Cl 0.66726(9) 0.62473(15) 0.63045(5) 0.0195(3) Uani 1 1 d . . . . .
Cl2 Cl 0.66780(10) 0.13758(15) 0.64841(5) 0.0222(3) Uani 1 1 d . . . . .
O1 O 0.9777(3) 0.5236(5) 0.55791(14) 0.0226(9) Uani 1 1 d . . . . .
N1 N 0.8464(3) 0.3817(6) 0.67754(16) 0.0182(10) Uani 1 1 d . . . . .
N2 N 0.9320(3) 0.3669(6) 0.66578(16) 0.0200(10) Uani 1 1 d . . . . .
N3 N 0.8421(3) 0.3592(6) 0.60885(16) 0.0178(10) Uani 1 1 d . . . . .
N4 N 0.9997(3) 0.3287(5) 0.59924(16) 0.0172(10) Uani 1 1 d . . . . .
H4 H 1.0311 0.2521 0.6039 0.021 Uiso 1 1 calc R U . . .
N5 N 0.5252(3) 0.3815(5) 0.64223(16) 0.0181(10) Uani 1 1 d . . . . .
C1 C 0.7906(4) 0.3781(6) 0.64352(19) 0.0187(11) Uani 1 1 d . . . . .
C2 C 0.9268(4) 0.3535(6) 0.62418(19) 0.0177(11) Uani 1 1 d . . . . .
C3 C 0.8327(3) 0.4142(6) 0.72366(18) 0.0217(13) Uani 1 1 d D . . . .
C4 C 0.8617(11) 0.2802(11) 0.7483(5) 0.030(2) Uani 0.5 1 d D . P A 1
H4A H 0.8222 0.2021 0.7407 0.045 Uiso 0.5 1 calc R U P A 1
H4B H 0.8602 0.2980 0.7793 0.045 Uiso 0.5 1 calc R U P A 1
H4C H 0.9213 0.2552 0.7405 0.045 Uiso 0.5 1 calc R U P A 1
C5 C 0.7386(5) 0.4570(19) 0.7335(5) 0.030(2) Uani 0.5 1 d D . P A 1
H5A H 0.6989 0.3793 0.7256 0.045 Uiso 0.5 1 calc R U P A 1
H5B H 0.7224 0.5415 0.7168 0.045 Uiso 0.5 1 calc R U P A 1
H5C H 0.7345 0.4773 0.7643 0.045 Uiso 0.5 1 calc R U P A 1
C6 C 0.8962(9) 0.5345(13) 0.7364(4) 0.030(2) Uani 0.5 1 d D . P A 1
H6A H 0.9536 0.5150 0.7246 0.045 Uiso 0.5 1 calc R U P A 1
H6B H 0.9015 0.5408 0.7678 0.045 Uiso 0.5 1 calc R U P A 1
H6C H 0.8739 0.6242 0.7247 0.045 Uiso 0.5 1 calc R U P A 1
C4' C 0.8852(10) 0.3134(15) 0.7534(4) 0.0260(18) Uani 0.5 1 d D . P A 2
H4'A H 0.8586 0.2192 0.7523 0.039 Uiso 0.5 1 calc R U P A 2
H4'B H 0.8850 0.3492 0.7830 0.039 Uiso 0.5 1 calc R U P A 2
H4'C H 0.9454 0.3077 0.7438 0.039 Uiso 0.5 1 calc R U P A 2
C5' C 0.7361(4) 0.3946(17) 0.7345(5) 0.0260(18) Uani 0.5 1 d D . P A 2
H5'A H 0.7144 0.3057 0.7220 0.039 Uiso 0.5 1 calc R U P A 2
H5'B H 0.7018 0.4737 0.7227 0.039 Uiso 0.5 1 calc R U P A 2
H5'C H 0.7306 0.3919 0.7659 0.039 Uiso 0.5 1 calc R U P A 2
C6' C 0.8547(9) 0.5721(7) 0.7289(4) 0.0260(18) Uani 0.5 1 d D . P A 2
H6'A H 0.8041 0.6290 0.7196 0.039 Uiso 0.5 1 calc R U P A 2
H6'B H 0.9045 0.5957 0.7112 0.039 Uiso 0.5 1 calc R U P A 2
H6'C H 0.8695 0.5923 0.7592 0.039 Uiso 0.5 1 calc R U P A 2
C7 C 1.0230(4) 0.4215(7) 0.56776(19) 0.0183(12) Uani 1 1 d . . . . .
C8 C 1.1072(4) 0.3885(8) 0.5463(2) 0.0267(14) Uani 1 1 d . . . . .
H8A H 1.0957 0.3731 0.5154 0.040 Uiso 1 1 calc R U . . .
H8B H 1.1331 0.3030 0.5591 0.040 Uiso 1 1 calc R U . . .
H8C H 1.1477 0.4679 0.5503 0.040 Uiso 1 1 calc R U . . .
C9 C 0.8105(4) 0.3548(7) 0.5636(2) 0.0223(13) Uani 1 1 d . . . . .
H9A H 0.8309 0.4408 0.5488 0.027 Uiso 1 1 calc R U . . .
H9B H 0.7460 0.3568 0.5629 0.027 Uiso 1 1 calc R U . . .
C10 C 0.8404(4) 0.2265(7) 0.53919(18) 0.0192(12) Uani 1 1 d . . . . .
C11 C 0.8898(4) 0.2452(7) 0.50261(19) 0.0213(12) Uani 1 1 d . . . . .
H11 H 0.9073 0.3375 0.4944 0.026 Uiso 1 1 calc R U . . .
C12 C 0.9135(5) 0.1289(8) 0.4781(2) 0.0284(14) Uani 1 1 d . . . . .
H12 H 0.9470 0.1419 0.4531 0.034 Uiso 1 1 calc R U . . .
C13 C 0.8884(5) -0.0056(8) 0.4901(2) 0.0271(14) Uani 1 1 d . . . . .
H13 H 0.9038 -0.0849 0.4731 0.032 Uiso 1 1 calc R U . . .
C14 C 0.8405(5) -0.0249(8) 0.5270(2) 0.0290(15) Uani 1 1 d . . . . .
H14 H 0.8237 -0.1174 0.5353 0.035 Uiso 1 1 calc R U . . .
C15 C 0.8171(4) 0.0911(7) 0.5517(2) 0.0239(13) Uani 1 1 d . . . . .
H15 H 0.7853 0.0776 0.5772 0.029 Uiso 1 1 calc R U . . .
C16 C 0.4786(4) 0.2736(7) 0.6255(2) 0.0210(12) Uani 1 1 d . . . . .
H16 H 0.5086 0.1978 0.6124 0.025 Uiso 1 1 calc R U . . .
C17 C 0.3884(4) 0.2680(7) 0.6266(2) 0.0238(13) Uani 1 1 d . . . . .
H17 H 0.3573 0.1904 0.6142 0.029 Uiso 1 1 calc R U . . .
C18 C 0.3445(4) 0.3771(7) 0.6459(2) 0.0240(13) Uani 1 1 d . . . . .
H18 H 0.2827 0.3747 0.6475 0.029 Uiso 1 1 calc R U . . .
C19 C 0.3912(4) 0.4900(7) 0.6629(2) 0.0245(14) Uani 1 1 d . . . . .
H19 H 0.3622 0.5672 0.6758 0.029 Uiso 1 1 calc R U . . .
C20 C 0.4811(4) 0.4884(7) 0.6607(2) 0.0205(12) Uani 1 1 d . . . . .
H20 H 0.5133 0.5654 0.6728 0.025 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 C1 1.968(6) . ?
Pd1 N5 2.103(5) . ?
Pd1 Cl2 2.3211(16) . ?
Pd1 Cl1 2.3236(15) . ?
O1 C7 1.223(7) . ?
N1 C1 1.340(8) . ?
N1 N2 1.380(7) . ?
N1 C3 1.487(7) . ?
N2 C2 1.299(8) . ?
N3 C1 1.366(7) . ?
N3 C2 1.371(8) . ?
N3 C9 1.472(8) . ?
N4 C7 1.369(8) . ?
N4 C2 1.398(7) . ?
N4 H4 0.8800 . ?
N5 C16 1.342(8) . ?
N5 C20 1.353(8) . ?
C3 C4' 1.538(3) . ?
C3 C5 1.538(3) . ?
C3 C6' 1.538(3) . ?
C3 C4 1.540(3) . ?
C3 C5' 1.541(3) . ?
C3 C6 1.541(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C4' H4'A 0.9800 . ?
C4' H4'B 0.9800 . ?
C4' H4'C 0.9800 . ?
C5' H5'A 0.9800 . ?
C5' H5'B 0.9800 . ?
C5' H5'C 0.9800 . ?
C6' H6'A 0.9800 . ?
C6' H6'B 0.9800 . ?
C6' H6'C 0.9800 . ?
C7 C8 1.503(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.510(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C15 1.387(9) . ?
C10 C11 1.396(8) . ?
C11 C12 1.392(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.392(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.385(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.379(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.382(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.382(9) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 N5 177.2(2) . . ?
C1 Pd1 Cl2 86.86(18) . . ?
N5 Pd1 Cl2 91.80(15) . . ?
C1 Pd1 Cl1 89.15(18) . . ?
N5 Pd1 Cl1 92.32(15) . . ?
Cl2 Pd1 Cl1 174.89(5) . . ?
C1 N1 N2 112.2(5) . . ?
C1 N1 C3 131.4(5) . . ?
N2 N1 C3 116.0(4) . . ?
C2 N2 N1 104.1(5) . . ?
C1 N3 C2 107.1(5) . . ?
C1 N3 C9 125.1(5) . . ?
C2 N3 C9 127.7(5) . . ?
C7 N4 C2 121.3(5) . . ?
C7 N4 H4 119.4 . . ?
C2 N4 H4 119.4 . . ?
C16 N5 C20 117.8(5) . . ?
C16 N5 Pd1 121.1(4) . . ?
C20 N5 Pd1 121.0(4) . . ?
N1 C1 N3 104.8(5) . . ?
N1 C1 Pd1 129.8(4) . . ?
N3 C1 Pd1 125.2(4) . . ?
N2 C2 N3 111.8(5) . . ?
N2 C2 N4 122.8(5) . . ?
N3 C2 N4 125.3(5) . . ?
N1 C3 C4' 111.4(7) . . ?
N1 C3 C5 114.0(7) . . ?
N1 C3 C6' 105.4(6) . . ?
C4' C3 C6' 115.4(9) . . ?
N1 C3 C4 105.2(7) . . ?
C5 C3 C4 112.1(10) . . ?
N1 C3 C5' 110.5(7) . . ?
C4' C3 C5' 106.4(9) . . ?
C6' C3 C5' 107.6(9) . . ?
N1 C3 C6 107.1(6) . . ?
C5 C3 C6 110.2(9) . . ?
C4 C3 C6 108.0(9) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C4' H4'A 109.5 . . ?
C3 C4' H4'B 109.5 . . ?
H4'A C4' H4'B 109.5 . . ?
C3 C4' H4'C 109.5 . . ?
H4'A C4' H4'C 109.5 . . ?
H4'B C4' H4'C 109.5 . . ?
C3 C5' H5'A 109.5 . . ?
C3 C5' H5'B 109.5 . . ?
H5'A C5' H5'B 109.5 . . ?
C3 C5' H5'C 109.5 . . ?
H5'A C5' H5'C 109.5 . . ?
H5'B C5' H5'C 109.5 . . ?
C3 C6' H6'A 109.5 . . ?
C3 C6' H6'B 109.5 . . ?
H6'A C6' H6'B 109.5 . . ?
C3 C6' H6'C 109.5 . . ?
H6'A C6' H6'C 109.5 . . ?
H6'B C6' H6'C 109.5 . . ?
O1 C7 N4 121.7(6) . . ?
O1 C7 C8 122.8(6) . . ?
N4 C7 C8 115.5(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 114.0(5) . . ?
N3 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N3 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.6 . . ?
C15 C10 C11 119.7(6) . . ?
C15 C10 C9 121.1(5) . . ?
C11 C10 C9 119.2(6) . . ?
C12 C11 C10 120.2(6) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 119.9(6) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.1(6) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 120.1(7) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C10 C15 C14 120.0(6) . . ?
C10 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
N5 C16 C17 122.7(6) . . ?
N5 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C18 C17 C16 118.9(6) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 119.3(6) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 118.7(6) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
N5 C20 C19 122.7(6) . . ?
N5 C20 H20 118.7 . . ?
C19 C20 H20 118.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 C2 -0.4(7) . . . . ?
C3 N1 N2 C2 -173.9(5) . . . . ?
N2 N1 C1 N3 0.5(7) . . . . ?
C3 N1 C1 N3 172.7(6) . . . . ?
N2 N1 C1 Pd1 175.6(4) . . . . ?
C3 N1 C1 Pd1 -12.2(10) . . . . ?
C2 N3 C1 N1 -0.5(7) . . . . ?
C9 N3 C1 N1 -177.2(6) . . . . ?
C2 N3 C1 Pd1 -175.9(4) . . . . ?
C9 N3 C1 Pd1 7.4(9) . . . . ?
N1 N2 C2 N3 0.1(7) . . . . ?
N1 N2 C2 N4 -176.8(5) . . . . ?
C1 N3 C2 N2 0.3(7) . . . . ?
C9 N3 C2 N2 176.8(6) . . . . ?
C1 N3 C2 N4 177.0(6) . . . . ?
C9 N3 C2 N4 -6.5(10) . . . . ?
C7 N4 C2 N2 -119.9(7) . . . . ?
C7 N4 C2 N3 63.8(8) . . . . ?
C1 N1 C3 C4' 139.0(9) . . . . ?
N2 N1 C3 C4' -49.0(9) . . . . ?
C1 N1 C3 C5 -2.8(11) . . . . ?
N2 N1 C3 C5 169.2(9) . . . . ?
C1 N1 C3 C6' -95.1(9) . . . . ?
N2 N1 C3 C6' 76.8(8) . . . . ?
C1 N1 C3 C4 120.4(9) . . . . ?
N2 N1 C3 C4 -67.6(9) . . . . ?
C1 N1 C3 C5' 20.9(10) . . . . ?
N2 N1 C3 C5' -167.1(7) . . . . ?
C1 N1 C3 C6 -124.9(9) . . . . ?
N2 N1 C3 C6 47.1(9) . . . . ?
C2 N4 C7 O1 -5.7(9) . . . . ?
C2 N4 C7 C8 174.6(6) . . . . ?
C1 N3 C9 C10 -127.9(6) . . . . ?
C2 N3 C9 C10 56.1(8) . . . . ?
N3 C9 C10 C15 61.6(8) . . . . ?
N3 C9 C10 C11 -120.4(6) . . . . ?
C15 C10 C11 C12 1.9(9) . . . . ?
C9 C10 C11 C12 -176.1(6) . . . . ?
C10 C11 C12 C13 -0.3(10) . . . . ?
C11 C12 C13 C14 -0.9(10) . . . . ?
C12 C13 C14 C15 0.5(11) . . . . ?
C11 C10 C15 C14 -2.3(10) . . . . ?
C9 C10 C15 C14 175.7(6) . . . . ?
C13 C14 C15 C10 1.1(11) . . . . ?
C20 N5 C16 C17 0.0(9) . . . . ?
Pd1 N5 C16 C17 178.1(5) . . . . ?
N5 C16 C17 C18 -0.5(10) . . . . ?
C16 C17 C18 C19 1.2(10) . . . . ?
C17 C18 C19 C20 -1.3(10) . . . . ?
C16 N5 C20 C19 -0.1(9) . . . . ?
Pd1 N5 C20 C19 -178.3(5) . . . . ?
C18 C19 C20 N5 0.8(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4 Cl1 0.88 2.53 3.334(5) 152.7 3_545

_refine_diff_density_max         1.170
_refine_diff_density_min         -2.170
_refine_diff_density_rms         0.155

_shelxl_version_number           2013-4

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

data_4a
_database_code_depnum_ccdc_archive 'CCDC 2074562'
loop_
_audit_author_name
_audit_author_address
'Mikhail Minyaev'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2021-03-31 deposited with the CCDC.	2021-05-28 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         'C22 H44 I4 N8 Pd2, C H2 Cl2'
_chemical_formula_sum            'C23 H46 Cl2 I4 N8 Pd2'
_chemical_formula_weight         1225.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   15.1329(14)
_cell_length_b                   22.941(2)
_cell_length_c                   24.370(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8460.4(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9619
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      30.95

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_F_000             4624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    3.919
_shelx_estimated_absorpt_T_min   0.240
_shelx_estimated_absorpt_T_max   0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0086
_exptl_absorpt_correction_T_max  0.0333
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-Ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS D8 QUEST, Photon III detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            118510
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.322
_diffrn_reflns_theta_max         29.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11772
_reflns_number_gt                8524
_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       'APEX3 (Bruker, 2018)'
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_solution    
;
SHELXT, SHELXS-2013 (Sheldrick, Acta Cryst., 2015, A71, 3-8)
;
_computing_structure_refinement  
;
SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)
;
_computing_molecular_graphics    
;
SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_computing_publication_material  
;
SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 The SQUEEZE method (Spek, Acta Cryst., 2015, C71, 9-18) implemented
 in the PLATON program (Spek, Acta Cryst., 2009, D65, 148-155) was used
 to remove a disodered non-coordinating hexene molecule and an
 unidentified molecule (DMSO or dichloroethane) located at the same place.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0275P)²+40.4720P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11772
_refine_ls_number_parameters     387
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0777
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.019
_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 0.68340(2) 0.40901(2) 0.28778(2) 0.02688(8) Uani 1 1 d . . . . .
Pd2 Pd 0.64479(2) 0.26542(2) 0.21575(2) 0.02839(8) Uani 1 1 d . . . . .
I1 I 0.77319(2) 0.31212(2) 0.27652(2) 0.03530(8) Uani 1 1 d . . . . .
I2 I 0.55245(2) 0.36063(2) 0.23086(2) 0.03288(8) Uani 1 1 d . . . . .
I3 I 0.60500(2) 0.50909(2) 0.29452(2) 0.03356(8) Uani 1 1 d . . . . .
I4 I 0.72299(2) 0.16589(2) 0.20393(2) 0.03979(9) Uani 1 1 d . . . . .
N1 N 0.8764(3) 0.46491(18) 0.40030(17) 0.0311(9) Uani 1 1 d . . . . .
N2 N 0.7967(3) 0.43820(17) 0.38577(16) 0.0273(8) Uani 1 1 d . . . . .
C1 C 0.7794(3) 0.4419(2) 0.3325(2) 0.0290(10) Uani 1 1 d . . . . .
N3 N 0.8487(3) 0.47271(17) 0.31143(17) 0.0282(8) Uani 1 1 d . . . . .
C2 C 0.9057(3) 0.4858(2) 0.3540(2) 0.0292(10) Uani 1 1 d . . . . .
C3 C 0.7493(3) 0.4087(2) 0.4318(2) 0.0305(10) Uani 1 1 d . . . . .
C4 C 0.7379(4) 0.4534(2) 0.4779(2) 0.0399(13) Uani 1 1 d . . . . .
H4A H 0.708929 0.434786 0.509303 0.060 Uiso 1 1 calc R U . . .
H4B H 0.701366 0.485786 0.464746 0.060 Uiso 1 1 calc R U . . .
H4C H 0.795900 0.468121 0.489031 0.060 Uiso 1 1 calc R U . . .
C5 C 0.8079(4) 0.3586(2) 0.4505(2) 0.0381(12) Uani 1 1 d . . . . .
H5A H 0.779618 0.338330 0.481217 0.057 Uiso 1 1 calc R U . . .
H5B H 0.865301 0.373897 0.462233 0.057 Uiso 1 1 calc R U . . .
H5C H 0.816384 0.331324 0.420001 0.057 Uiso 1 1 calc R U . . .
C6 C 0.6602(3) 0.3865(3) 0.4134(2) 0.0409(13) Uani 1 1 d . . . . .
H6A H 0.630489 0.367400 0.444296 0.061 Uiso 1 1 calc R U . . .
H6B H 0.668197 0.358430 0.383530 0.061 Uiso 1 1 calc R U . . .
H6C H 0.624213 0.419244 0.400532 0.061 Uiso 1 1 calc R U . . .
C7 C 0.8581(4) 0.4915(2) 0.2545(2) 0.0345(11) Uani 1 1 d . . . . .
H7A H 0.868319 0.533621 0.253335 0.052 Uiso 1 1 calc R U . . .
H7B H 0.804011 0.482102 0.234214 0.052 Uiso 1 1 calc R U . . .
H7C H 0.908319 0.471220 0.237687 0.052 Uiso 1 1 calc R U . . .
N4 N 0.9797(3) 0.51808(19) 0.34627(18) 0.0303(9) Uani 1 1 d . . . . .
H4 H 1.001(4) 0.524(3) 0.313(3) 0.050(19) Uiso 1 1 d . . . . .
C8 C 1.0466(3) 0.5271(2) 0.3904(2) 0.0325(11) Uani 1 1 d . . . . .
C9 C 1.1180(4) 0.5647(3) 0.3649(2) 0.0428(13) Uani 1 1 d . . . . .
H9A H 1.162030 0.574634 0.392848 0.064 Uiso 1 1 calc R U . . .
H9B H 1.091504 0.600477 0.350391 0.064 Uiso 1 1 calc R U . . .
H9C H 1.146521 0.543178 0.335032 0.064 Uiso 1 1 calc R U . . .
C11 C 1.0849(4) 0.4687(2) 0.4091(2) 0.0409(13) Uani 1 1 d . . . . .
H11A H 1.129588 0.475458 0.437490 0.061 Uiso 1 1 calc R U . . .
H11B H 1.112110 0.448886 0.377752 0.061 Uiso 1 1 calc R U . . .
H11C H 1.037458 0.444321 0.424064 0.061 Uiso 1 1 calc R U . . .
C10 C 1.0054(4) 0.5600(2) 0.4382(2) 0.0374(12) Uani 1 1 d . . . . .
H10A H 1.049243 0.564561 0.467496 0.056 Uiso 1 1 calc R U . . .
H10B H 0.954566 0.538073 0.452195 0.056 Uiso 1 1 calc R U . . .
H10C H 0.985841 0.598512 0.425773 0.056 Uiso 1 1 calc R U . . .
N5 N 0.4544(3) 0.21486(18) 0.09949(17) 0.0311(9) Uani 1 1 d . . . . .
N6 N 0.5342(3) 0.24058(18) 0.11571(17) 0.0301(9) Uani 1 1 d . . . . .
C12 C 0.5497(3) 0.2349(2) 0.1688(2) 0.0284(10) Uani 1 1 d . . . . .
N7 N 0.4792(3) 0.20431(17) 0.18841(17) 0.0286(8) Uani 1 1 d . . . . .
C13 C 0.4234(3) 0.1933(2) 0.1452(2) 0.0278(10) Uani 1 1 d . . . . .
C14 C 0.5886(3) 0.2649(2) 0.0697(2) 0.0313(10) Uani 1 1 d . . . . .
C15 C 0.5312(4) 0.3069(3) 0.0380(3) 0.0443(14) Uani 1 1 d . . . . .
H15A H 0.564846 0.323002 0.007158 0.066 Uiso 1 1 calc R U . . .
H15B H 0.512261 0.338650 0.062194 0.066 Uiso 1 1 calc R U . . .
H15C H 0.479101 0.286296 0.023991 0.066 Uiso 1 1 calc R U . . .
C16 C 0.6155(4) 0.2126(2) 0.0350(3) 0.0456(14) Uani 1 1 d . . . . .
H16A H 0.651280 0.225850 0.003857 0.068 Uiso 1 1 calc R U . . .
H16B H 0.562465 0.192859 0.021356 0.068 Uiso 1 1 calc R U . . .
H16C H 0.650141 0.185485 0.057410 0.068 Uiso 1 1 calc R U . . .
C17 C 0.6684(4) 0.2966(3) 0.0917(2) 0.0492(15) Uani 1 1 d . . . . .
H17A H 0.703622 0.311588 0.061043 0.074 Uiso 1 1 calc R U . . .
H17B H 0.704328 0.269678 0.113536 0.074 Uiso 1 1 calc R U . . .
H17C H 0.649138 0.329169 0.114835 0.074 Uiso 1 1 calc R U . . .
C18 C 0.4675(4) 0.1840(2) 0.2444(2) 0.0349(11) Uani 1 1 d . . . . .
H18A H 0.459148 0.141652 0.244339 0.052 Uiso 1 1 calc R U . . .
H18B H 0.415534 0.202841 0.260499 0.052 Uiso 1 1 calc R U . . .
H18C H 0.520024 0.193838 0.266021 0.052 Uiso 1 1 calc R U . . .
N8 N 0.3472(3) 0.16340(19) 0.15122(19) 0.0313(9) Uani 1 1 d . . . . .
H8 H 0.333(3) 0.157(2) 0.180(2) 0.018(13) Uiso 1 1 d . . . . .
C19 C 0.2878(4) 0.1476(2) 0.1055(2) 0.0367(12) Uani 1 1 d . . . . .
C22 C 0.3363(5) 0.1084(3) 0.0653(2) 0.0480(15) Uani 1 1 d . . . . .
H22A H 0.296620 0.098027 0.035087 0.072 Uiso 1 1 calc R U . . .
H22B H 0.355567 0.072906 0.084211 0.072 Uiso 1 1 calc R U . . .
H22C H 0.387920 0.129031 0.050784 0.072 Uiso 1 1 calc R U . . .
C21 C 0.2113(4) 0.1146(3) 0.1321(3) 0.0518(17) Uani 1 1 d . . . . .
H21A H 0.169965 0.101686 0.103607 0.078 Uiso 1 1 calc R U . . .
H21B H 0.180498 0.140357 0.157867 0.078 Uiso 1 1 calc R U . . .
H21C H 0.234248 0.080623 0.151832 0.078 Uiso 1 1 calc R U . . .
C20 C 0.2534(4) 0.2024(2) 0.0774(3) 0.0451(14) Uani 1 1 d . . . . .
H20A H 0.207546 0.191708 0.050816 0.068 Uiso 1 1 calc R U . . .
H20B H 0.302158 0.221852 0.058263 0.068 Uiso 1 1 calc R U . . .
H20C H 0.228451 0.228796 0.104897 0.068 Uiso 1 1 calc R U . . .
Cl1 Cl 0.52706(15) 0.23903(10) 0.37829(8) 0.0758(6) Uani 1 1 d D . . . .
Cl2A Cl 0.4074(4) 0.3080(3) 0.44044(17) 0.0691(19) Uani 0.429(3) 1 d D . P A 1
Cl2B Cl 0.4117(6) 0.3340(4) 0.4249(4) 0.0691(19) Uani 0.296(3) 1 d D . P A 2
Cl2C Cl 0.4023(17) 0.3499(6) 0.4002(12) 0.0691(19) Uani 0.088(3) 1 d D . P A 3
Cl2D Cl 0.3938(11) 0.2844(6) 0.4429(3) 0.0691(19) Uani 0.187(3) 1 d D . P A 4
C23 C 0.4299(5) 0.2807(3) 0.3745(3) 0.089(3) Uani 1 1 d D . . . .
H23A H 0.380151 0.256217 0.361628 0.106 Uiso 0.429(3) 1 calc R U P A 1
H23B H 0.437776 0.313280 0.348246 0.106 Uiso 0.429(3) 1 calc R U P A 1
H23C H 0.429125 0.300364 0.338286 0.106 Uiso 0.296(3) 1 calc R U P A 2
H23D H 0.379141 0.253495 0.375193 0.106 Uiso 0.296(3) 1 calc R U P A 2
H23E H 0.383538 0.254688 0.389335 0.106 Uiso 0.088(3) 1 calc R U P A 3
H23F H 0.417682 0.283642 0.334638 0.106 Uiso 0.088(3) 1 calc R U P A 3
H23G H 0.385251 0.261450 0.350936 0.106 Uiso 0.187(3) 1 calc R U P A 4
H23H H 0.442181 0.320110 0.359721 0.106 Uiso 0.187(3) 1 calc R U P A 4


_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 C1 1.967(5) . ?
Pd1 I3 2.5895(5) . ?
Pd1 I1 2.6197(5) . ?
Pd1 I2 2.6614(5) . ?
Pd2 C12 1.967(5) . ?
Pd2 I4 2.5879(5) . ?
Pd2 I2 2.6188(5) . ?
Pd2 I1 2.6676(5) . ?
N1 C2 1.303(6) . ?
N1 N2 1.398(5) . ?
N2 C1 1.327(6) . ?
N2 C3 1.494(6) . ?
C1 N3 1.365(6) . ?
N3 C2 1.382(6) . ?
N3 C7 1.460(6) . ?
C2 N4 1.356(6) . ?
C3 C6 1.510(7) . ?
C3 C5 1.521(7) . ?
C3 C4 1.528(7) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N4 C8 1.491(6) . ?
N4 H4 0.88(7) . ?
C8 C9 1.515(7) . ?
C8 C10 1.521(7) . ?
C8 C11 1.530(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N5 C13 1.307(6) . ?
N5 N6 1.400(6) . ?
N6 C12 1.321(6) . ?
N6 C14 1.499(6) . ?
C12 N7 1.364(6) . ?
N7 C13 1.373(6) . ?
N7 C18 1.452(6) . ?
C13 N8 1.350(6) . ?
C14 C17 1.508(8) . ?
C14 C15 1.510(7) . ?
C14 C16 1.524(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N8 C19 1.477(7) . ?
N8 H8 0.76(5) . ?
C19 C22 1.518(8) . ?
C19 C20 1.523(7) . ?
C19 C21 1.527(8) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Cl1 C23 1.757(5) . ?
Cl2A C23 1.759(5) . ?
Cl2B C23 1.756(5) . ?
Cl2C C23 1.757(5) . ?
Cl2D C23 1.758(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 H23C 0.9900 . ?
C23 H23D 0.9900 . ?
C23 H23E 0.9900 . ?
C23 H23F 0.9900 . ?
C23 H23G 0.9900 . ?
C23 H23H 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 I3 87.88(14) . . ?
C1 Pd1 I1 90.03(14) . . ?
I3 Pd1 I1 175.27(2) . . ?
C1 Pd1 I2 177.29(14) . . ?
I3 Pd1 I2 93.540(16) . . ?
I1 Pd1 I2 88.722(16) . . ?
C12 Pd2 I4 87.47(14) . . ?
C12 Pd2 I2 89.32(14) . . ?
I4 Pd2 I2 174.56(2) . . ?
C12 Pd2 I1 176.95(14) . . ?
I4 Pd2 I1 94.762(17) . . ?
I2 Pd2 I1 88.609(16) . . ?
Pd1 I1 Pd2 91.208(16) . . ?
Pd2 I2 Pd1 91.365(16) . . ?
C2 N1 N2 103.6(4) . . ?
C1 N2 N1 112.9(4) . . ?
C1 N2 C3 132.1(4) . . ?
N1 N2 C3 114.9(4) . . ?
N2 C1 N3 104.5(4) . . ?
N2 C1 Pd1 131.5(4) . . ?
N3 C1 Pd1 123.9(4) . . ?
C1 N3 C2 108.0(4) . . ?
C1 N3 C7 125.8(4) . . ?
C2 N3 C7 126.1(4) . . ?
N1 C2 N4 127.1(5) . . ?
N1 C2 N3 111.0(4) . . ?
N4 C2 N3 121.9(4) . . ?
N2 C3 C6 111.0(4) . . ?
N2 C3 C5 106.7(4) . . ?
C6 C3 C5 110.7(4) . . ?
N2 C3 C4 107.6(4) . . ?
C6 C3 C4 110.0(5) . . ?
C5 C3 C4 110.7(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 N4 C8 122.4(4) . . ?
C2 N4 H4 121(4) . . ?
C8 N4 H4 113(4) . . ?
N4 C8 C9 105.5(4) . . ?
N4 C8 C10 110.1(4) . . ?
C9 C8 C10 108.9(4) . . ?
N4 C8 C11 110.5(4) . . ?
C9 C8 C11 110.5(5) . . ?
C10 C8 C11 111.2(5) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 N5 N6 103.2(4) . . ?
C12 N6 N5 112.9(4) . . ?
C12 N6 C14 132.1(4) . . ?
N5 N6 C14 114.8(4) . . ?
N6 C12 N7 104.8(4) . . ?
N6 C12 Pd2 131.7(4) . . ?
N7 C12 Pd2 123.4(4) . . ?
C12 N7 C13 107.9(4) . . ?
C12 N7 C18 126.2(4) . . ?
C13 N7 C18 125.9(4) . . ?
N5 C13 N8 126.3(5) . . ?
N5 C13 N7 111.3(4) . . ?
N8 C13 N7 122.4(4) . . ?
N6 C14 C17 110.7(4) . . ?
N6 C14 C15 107.7(4) . . ?
C17 C14 C15 109.6(5) . . ?
N6 C14 C16 105.6(4) . . ?
C17 C14 C16 111.3(5) . . ?
C15 C14 C16 111.8(5) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N7 C18 H18A 109.5 . . ?
N7 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N7 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 N8 C19 124.3(5) . . ?
C13 N8 H8 117(4) . . ?
C19 N8 H8 118(4) . . ?
N8 C19 C22 109.7(5) . . ?
N8 C19 C20 110.2(4) . . ?
C22 C19 C20 111.3(5) . . ?
N8 C19 C21 105.3(5) . . ?
C22 C19 C21 110.3(5) . . ?
C20 C19 C21 109.9(5) . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Cl2B C23 Cl1 118.2(6) . . ?
Cl1 C23 Cl2C 132.2(10) . . ?
Cl1 C23 Cl2D 103.6(7) . . ?
Cl1 C23 Cl2A 107.9(5) . . ?
Cl1 C23 H23A 110.1 . . ?
Cl2A C23 H23A 110.1 . . ?
Cl1 C23 H23B 110.1 . . ?
Cl2A C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
Cl2B C23 H23C 107.8 . . ?
Cl1 C23 H23C 107.8 . . ?
Cl2B C23 H23D 107.8 . . ?
Cl1 C23 H23D 107.8 . . ?
H23C C23 H23D 107.1 . . ?
Cl1 C23 H23E 104.2 . . ?
Cl2C C23 H23E 104.2 . . ?
Cl1 C23 H23F 104.2 . . ?
Cl2C C23 H23F 104.2 . . ?
H23E C23 H23F 105.5 . . ?
Cl1 C23 H23G 111.0 . . ?
Cl2D C23 H23G 111.0 . . ?
Cl1 C23 H23H 111.0 . . ?
Cl2D C23 H23H 111.0 . . ?
H23G C23 H23H 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 N2 C1 1.1(5) . . . . ?
C2 N1 N2 C3 178.4(4) . . . . ?
N1 N2 C1 N3 -1.0(5) . . . . ?
C3 N2 C1 N3 -177.7(5) . . . . ?
N1 N2 C1 Pd1 175.5(3) . . . . ?
C3 N2 C1 Pd1 -1.2(8) . . . . ?
N2 C1 N3 C2 0.5(5) . . . . ?
Pd1 C1 N3 C2 -176.3(3) . . . . ?
N2 C1 N3 C7 -176.2(4) . . . . ?
Pd1 C1 N3 C7 7.0(7) . . . . ?
N2 N1 C2 N4 176.9(5) . . . . ?
N2 N1 C2 N3 -0.7(5) . . . . ?
C1 N3 C2 N1 0.2(6) . . . . ?
C7 N3 C2 N1 176.9(4) . . . . ?
C1 N3 C2 N4 -177.6(4) . . . . ?
C7 N3 C2 N4 -0.9(8) . . . . ?
C1 N2 C3 C6 -9.0(7) . . . . ?
N1 N2 C3 C6 174.4(4) . . . . ?
C1 N2 C3 C5 111.7(6) . . . . ?
N1 N2 C3 C5 -64.9(5) . . . . ?
C1 N2 C3 C4 -129.4(6) . . . . ?
N1 N2 C3 C4 53.9(5) . . . . ?
N1 C2 N4 C8 9.3(8) . . . . ?
N3 C2 N4 C8 -173.3(4) . . . . ?
C2 N4 C8 C9 179.5(5) . . . . ?
C2 N4 C8 C10 -63.2(6) . . . . ?
C2 N4 C8 C11 60.0(6) . . . . ?
C13 N5 N6 C12 -0.4(5) . . . . ?
C13 N5 N6 C14 175.1(4) . . . . ?
N5 N6 C12 N7 0.5(5) . . . . ?
C14 N6 C12 N7 -174.0(5) . . . . ?
N5 N6 C12 Pd2 -175.6(4) . . . . ?
C14 N6 C12 Pd2 9.9(8) . . . . ?
N6 C12 N7 C13 -0.5(5) . . . . ?
Pd2 C12 N7 C13 176.0(3) . . . . ?
N6 C12 N7 C18 176.3(4) . . . . ?
Pd2 C12 N7 C18 -7.2(7) . . . . ?
N6 N5 C13 N8 -179.4(5) . . . . ?
N6 N5 C13 N7 0.0(5) . . . . ?
C12 N7 C13 N5 0.3(6) . . . . ?
C18 N7 C13 N5 -176.5(4) . . . . ?
C12 N7 C13 N8 179.7(4) . . . . ?
C18 N7 C13 N8 2.9(7) . . . . ?
C12 N6 C14 C17 -11.0(8) . . . . ?
N5 N6 C14 C17 174.6(5) . . . . ?
C12 N6 C14 C15 -130.9(6) . . . . ?
N5 N6 C14 C15 54.7(5) . . . . ?
C12 N6 C14 C16 109.5(6) . . . . ?
N5 N6 C14 C16 -64.9(5) . . . . ?
N5 C13 N8 C19 3.1(8) . . . . ?
N7 C13 N8 C19 -176.3(5) . . . . ?
C13 N8 C19 C22 61.4(6) . . . . ?
C13 N8 C19 C20 -61.4(7) . . . . ?
C13 N8 C19 C21 -179.9(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N4 H4 I3 0.88(7) 3.08(7) 3.926(4) 162(5) 8_656 yes
N8 H8 I4 0.76(5) 3.28(5) 4.000(5) 160(5) 8_556 yes

_refine_diff_density_max         0.999
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.148


####################################################################### 
# 
# 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_3i
_database_code_depnum_ccdc_archive 'CCDC 2074560'
loop_
_audit_author_name
_audit_author_address
'Mikhail Minyaev'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2021-03-31 deposited with the CCDC.	2021-05-28 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         'C14 H21 I2 N5 O Pd'
_chemical_formula_sum            'C14 H21 I2 N5 O Pd'
_chemical_formula_weight         635.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   15.1906(5)
_cell_length_b                   15.3783(5)
_cell_length_c                   8.6698(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.3454(6)
_cell_angle_gamma                90
_cell_volume                     2023.62(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9676
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      31.51
_exptl_crystal_description       plate
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.978
_shelx_estimated_absorpt_T_min   0.210
_shelx_estimated_absorpt_T_max   0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0077
_exptl_absorpt_correction_T_max  0.0341
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-Ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS D8 QUEST, Photon III detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            94365
_diffrn_reflns_av_unetI/netI     0.0080
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.684
_diffrn_reflns_theta_max         31.535
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6741
_reflns_number_gt                6716
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_solution    
;
SHELXT, SHELXS-2013 (Sheldrick, Acta Cryst., 2015, A71, 3-8)
;
_computing_structure_refinement  
;
SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)
;
_computing_molecular_graphics    
;
SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_computing_publication_material  
;
SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0277P)²+5.1372P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6741
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_restrained_S_all      1.229
_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
I1 I 0.10736(2) 0.52764(2) 0.26333(3) 0.03427(6) Uani 1 1 d . . . . .
I2 I 0.35406(2) 0.39425(2) 0.62429(3) 0.04112(7) Uani 1 1 d . . . . .
Pd1 Pd 0.22154(2) 0.45673(2) 0.45969(3) 0.02815(6) Uani 1 1 d . . . . .
O1 O 0.48429(17) 0.80834(17) 0.5869(3) 0.0352(5) Uani 1 1 d . . . . .
N1 N 0.27187(16) 0.63135(16) 0.5964(3) 0.0253(4) Uani 1 1 d . . . . .
N2 N 0.33174(16) 0.69904(17) 0.5810(3) 0.0258(4) Uani 1 1 d . . . . .
N3 N 0.34392(17) 0.59969(16) 0.3983(3) 0.0261(4) Uani 1 1 d . . . . .
N4 N 0.43629(17) 0.72485(17) 0.3849(3) 0.0261(4) Uani 1 1 d . . . . .
H4 H 0.440(3) 0.717(3) 0.287(5) 0.040(12) Uiso 1 1 d . . . . .
N5 N 0.16099(19) 0.33503(19) 0.4444(4) 0.0354(6) Uani 1 1 d . . . . .
C1 C 0.27910(19) 0.56990(19) 0.4886(3) 0.0256(5) Uani 1 1 d . . . . .
C2 C 0.37363(18) 0.67745(19) 0.4580(3) 0.0244(5) Uani 1 1 d . . . . .
C3 C 0.2168(2) 0.6338(2) 0.7359(3) 0.0287(5) Uani 1 1 d . . . . .
C4 C 0.1364(2) 0.5748(2) 0.7126(4) 0.0356(7) Uani 1 1 d . . . . .
H4A H 0.099472 0.579297 0.802366 0.053 Uiso 1 1 calc R U . . .
H4B H 0.155725 0.514497 0.700745 0.053 Uiso 1 1 calc R U . . .
H4C H 0.102265 0.592900 0.619628 0.053 Uiso 1 1 calc R U . . .
C5 C 0.2737(2) 0.6027(2) 0.8745(4) 0.0351(7) Uani 1 1 d . . . . .
H5A H 0.238809 0.603295 0.967053 0.053 Uiso 1 1 calc R U . . .
H5B H 0.324526 0.641504 0.889771 0.053 Uiso 1 1 calc R U . . .
H5C H 0.294362 0.543444 0.855522 0.053 Uiso 1 1 calc R U . . .
C6 C 0.1865(2) 0.7274(2) 0.7568(4) 0.0328(6) Uani 1 1 d . . . . .
H6A H 0.155311 0.732396 0.853129 0.049 Uiso 1 1 calc R U . . .
H6B H 0.146868 0.744042 0.669692 0.049 Uiso 1 1 calc R U . . .
H6C H 0.237845 0.766081 0.760936 0.049 Uiso 1 1 calc R U . . .
C7 C 0.4861(2) 0.7896(2) 0.4512(3) 0.0276(5) Uani 1 1 d . . . . .
C8 C 0.5421(2) 0.8388(2) 0.3423(4) 0.0353(7) Uani 1 1 d . . . . .
H8A H 0.561312 0.799513 0.261243 0.053 Uiso 1 1 calc R U . . .
H8B H 0.593870 0.862373 0.399192 0.053 Uiso 1 1 calc R U . . .
H8C H 0.507831 0.886607 0.295366 0.053 Uiso 1 1 calc R U . . .
C9 C 0.3776(2) 0.5537(2) 0.2655(4) 0.0347(6) Uani 1 1 d . . . . .
H9A H 0.441885 0.548978 0.277293 0.052 Uiso 1 1 calc R U . . .
H9B H 0.361831 0.585901 0.170846 0.052 Uiso 1 1 calc R U . . .
H9C H 0.351762 0.495352 0.259370 0.052 Uiso 1 1 calc R U . . .
C10 C 0.0815(2) 0.3255(3) 0.5039(5) 0.0390(7) Uani 1 1 d . . . . .
H10 H 0.051337 0.375565 0.538151 0.047 Uiso 1 1 calc R U . . .
C11 C 0.0423(3) 0.2449(3) 0.5169(5) 0.0492(9) Uani 1 1 d . . . . .
H11 H -0.012700 0.239687 0.564502 0.059 Uiso 1 1 calc R U . . .
C12 C 0.0828(3) 0.1724(3) 0.4610(6) 0.0525(11) Uani 1 1 d . . . . .
H12 H 0.055709 0.116837 0.466774 0.063 Uiso 1 1 calc R U . . .
C13 C 0.1638(3) 0.1819(3) 0.3960(6) 0.0495(10) Uani 1 1 d . . . . .
H13 H 0.193989 0.132769 0.357968 0.059 Uiso 1 1 calc R U . . .
C14 C 0.2004(3) 0.2645(2) 0.3873(5) 0.0426(8) Uani 1 1 d . . . . .
H14 H 0.255144 0.271325 0.339407 0.051 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
I1 Pd1 2.6180(3) . ?
I2 Pd1 2.6032(3) . ?
Pd1 C1 1.959(3) . ?
Pd1 N5 2.087(3) . ?
O1 C7 1.213(4) . ?
N1 C1 1.337(4) . ?
N1 N2 1.392(3) . ?
N1 C3 1.499(4) . ?
N2 C2 1.307(4) . ?
N3 C1 1.362(4) . ?
N3 C2 1.372(4) . ?
N3 C9 1.462(4) . ?
N4 C7 1.364(4) . ?
N4 C2 1.374(4) . ?
N4 H4 0.87(5) . ?
N5 C10 1.340(4) . ?
N5 C14 1.343(5) . ?
C3 C6 1.525(5) . ?
C3 C5 1.528(5) . ?
C3 C4 1.528(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.501(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.383(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.371(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 N5 176.28(13) . . ?
C1 Pd1 I2 85.80(8) . . ?
N5 Pd1 I2 91.88(9) . . ?
C1 Pd1 I1 89.63(8) . . ?
N5 Pd1 I1 93.08(9) . . ?
I2 Pd1 I1 170.775(13) . . ?
C1 N1 N2 112.9(2) . . ?
C1 N1 C3 130.3(3) . . ?
N2 N1 C3 116.6(2) . . ?
C2 N2 N1 103.3(2) . . ?
C1 N3 C2 108.1(2) . . ?
C1 N3 C9 125.1(3) . . ?
C2 N3 C9 126.8(3) . . ?
C7 N4 C2 125.2(3) . . ?
C7 N4 H4 117(3) . . ?
C2 N4 H4 117(3) . . ?
C10 N5 C14 118.4(3) . . ?
C10 N5 Pd1 118.4(2) . . ?
C14 N5 Pd1 123.0(2) . . ?
N1 C1 N3 104.3(2) . . ?
N1 C1 Pd1 131.9(2) . . ?
N3 C1 Pd1 123.7(2) . . ?
N2 C2 N3 111.4(3) . . ?
N2 C2 N4 127.7(3) . . ?
N3 C2 N4 120.8(3) . . ?
N1 C3 C6 107.5(2) . . ?
N1 C3 C5 108.1(3) . . ?
C6 C3 C5 111.4(3) . . ?
N1 C3 C4 110.4(2) . . ?
C6 C3 C4 109.4(3) . . ?
C5 C3 C4 110.0(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C7 N4 123.2(3) . . ?
O1 C7 C8 121.8(3) . . ?
N4 C7 C8 115.0(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N5 C10 C11 121.9(4) . . ?
N5 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C12 C11 C10 120.0(4) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 118.5(4) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C12 C13 C14 119.0(4) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
N5 C14 C13 122.2(4) . . ?
N5 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 C2 1.6(3) . . . . ?
C3 N1 N2 C2 176.0(2) . . . . ?
N2 N1 C1 N3 -1.6(3) . . . . ?
C3 N1 C1 N3 -175.0(3) . . . . ?
N2 N1 C1 Pd1 174.3(2) . . . . ?
C3 N1 C1 Pd1 0.9(5) . . . . ?
C2 N3 C1 N1 0.9(3) . . . . ?
C9 N3 C1 N1 178.4(3) . . . . ?
C2 N3 C1 Pd1 -175.4(2) . . . . ?
C9 N3 C1 Pd1 2.1(4) . . . . ?
N1 N2 C2 N3 -1.0(3) . . . . ?
N1 N2 C2 N4 175.3(3) . . . . ?
C1 N3 C2 N2 0.1(3) . . . . ?
C9 N3 C2 N2 -177.4(3) . . . . ?
C1 N3 C2 N4 -176.5(3) . . . . ?
C9 N3 C2 N4 6.0(5) . . . . ?
C7 N4 C2 N2 21.7(5) . . . . ?
C7 N4 C2 N3 -162.3(3) . . . . ?
C1 N1 C3 C6 -144.2(3) . . . . ?
N2 N1 C3 C6 42.6(3) . . . . ?
C1 N1 C3 C5 95.4(4) . . . . ?
N2 N1 C3 C5 -77.8(3) . . . . ?
C1 N1 C3 C4 -24.9(4) . . . . ?
N2 N1 C3 C4 161.9(3) . . . . ?
C2 N4 C7 O1 5.3(5) . . . . ?
C2 N4 C7 C8 -172.9(3) . . . . ?
C14 N5 C10 C11 4.2(6) . . . . ?
Pd1 N5 C10 C11 -171.3(3) . . . . ?
N5 C10 C11 C12 -3.3(7) . . . . ?
C10 C11 C12 C13 1.7(7) . . . . ?
C11 C12 C13 C14 -1.1(7) . . . . ?
C10 N5 C14 C13 -3.7(6) . . . . ?
Pd1 N5 C14 C13 171.6(3) . . . . ?
C12 C13 C14 N5 2.2(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N4 H4 O1 0.87(5) 1.92(5) 2.761(3) 163(4) 4_575 yes

_refine_diff_density_max         2.395
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.122

####################################################################### 
# 
# 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_5a
_database_code_depnum_ccdc_archive 'CCDC 2074563'
loop_
_audit_author_name
_audit_author_address
'Mikhail Minyaev'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2021-03-31 deposited with the CCDC.	2021-05-28 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         'C15 H33 I2 N5 Pd'
_chemical_formula_sum            'C15 H33 I2 N5 Pd'
_chemical_formula_weight         643.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   20.0160(5)
_cell_length_b                   11.7895(3)
_cell_length_c                   9.9197(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.5118(10)
_cell_angle_gamma                90
_cell_volume                     2333.58(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9639
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      37.89

_exptl_crystal_description       block
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.31
_exptl_absorpt_coefficient_mu    3.447
_shelx_estimated_absorpt_T_min   0.240
_shelx_estimated_absorpt_T_max   0.415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0210
_exptl_absorpt_correction_T_max  0.0638
_exptl_absorpt_process_details   
'SADABS 2016/2 (Krause et al., J. Appl. Cryst. 2015, 48, 3-10)'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-Ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS D8 QUEST, Photon III detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            46494
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.006
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4581
_reflns_number_gt                4437
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker, 2019)'
_computing_cell_refinement       'SAINT (Bruker, 2019)'
_computing_data_reduction        'SAINT (Bruker, 2019)'
_computing_structure_solution    
'SHELXT, SHELXS-2013 (Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    
'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_computing_publication_material  
'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+8.6857P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     
'SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_refine_ls_extinction_coef       0.00112(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4581
_refine_ls_number_parameters     226
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0707
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.050
_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
I1 I 0.23899(2) 0.52922(3) 0.20500(3) 0.04637(10) Uani 1 1 d . . . . .
I2 I 0.11062(2) 0.43705(4) 0.62850(4) 0.06636(13) Uani 1 1 d . . . . .
Pd1 Pd 0.17366(2) 0.48699(3) 0.41612(3) 0.03413(10) Uani 1 1 d . . . . .
N1 N 0.26842(15) 0.3012(3) 0.4924(3) 0.0312(6) Uani 1 1 d . . . . .
C1 C 0.25492(18) 0.4139(3) 0.5045(4) 0.0323(8) Uani 1 1 d . . . . .
N2 N 0.30636(16) 0.4533(3) 0.5842(3) 0.0353(7) Uani 1 1 d . . . . .
N3 N 0.35269(15) 0.3695(3) 0.6251(3) 0.0352(7) Uani 1 1 d . . . . .
C2 C 0.32832(17) 0.2784(3) 0.5663(4) 0.0311(8) Uani 1 1 d . . . . .
C3 C 0.2293(2) 0.2203(4) 0.4079(4) 0.0409(9) Uani 1 1 d . . . . .
H3A H 0.191937 0.259760 0.358157 0.061 Uiso 1 1 calc R U . . .
H3B H 0.211661 0.161360 0.465095 0.061 Uiso 1 1 calc R U . . .
H3C H 0.257881 0.185398 0.343720 0.061 Uiso 1 1 calc R U . . .
C4 C 0.3241(2) 0.5697(4) 0.6331(5) 0.0437(10) Uani 1 1 d . . . . .
C5 C 0.2700(3) 0.6544(4) 0.5872(6) 0.0686(16) Uani 1 1 d . . . . .
H5A H 0.267122 0.660468 0.488338 0.103 Uiso 1 1 calc R U . . .
H5B H 0.281169 0.728766 0.627095 0.103 Uiso 1 1 calc R U . . .
H5C H 0.226867 0.628887 0.616340 0.103 Uiso 1 1 calc R U . . .
C6 C 0.3326(3) 0.5655(5) 0.7863(5) 0.0662(15) Uani 1 1 d . . . . .
H6A H 0.290379 0.541779 0.821441 0.099 Uiso 1 1 calc R U . . .
H6B H 0.344985 0.640938 0.821559 0.099 Uiso 1 1 calc R U . . .
H6C H 0.367952 0.511169 0.814918 0.099 Uiso 1 1 calc R U . . .
C7 C 0.3895(3) 0.6020(5) 0.5736(6) 0.0650(14) Uani 1 1 d . . . . .
H7A H 0.424336 0.546876 0.602659 0.097 Uiso 1 1 calc R U . . .
H7B H 0.403343 0.677793 0.605153 0.097 Uiso 1 1 calc R U . . .
H7C H 0.382769 0.601980 0.474626 0.097 Uiso 1 1 calc R U . . .
N4 N 0.35664(16) 0.1732(3) 0.5654(3) 0.0330(7) Uani 1 1 d D . . . .
H4 H 0.3301(18) 0.123(3) 0.566(4) 0.031(11) Uiso 1 1 d D . . . .
C8 C 0.41848(18) 0.1434(4) 0.6514(4) 0.0350(8) Uani 1 1 d . . . . .
C9 C 0.4315(2) 0.0185(4) 0.6238(4) 0.0436(10) Uani 1 1 d . . . . .
H9A H 0.392235 -0.026307 0.643595 0.065 Uiso 1 1 calc R U . . .
H9B H 0.470615 -0.007129 0.681521 0.065 Uiso 1 1 calc R U . . .
H9C H 0.440136 0.008593 0.528633 0.065 Uiso 1 1 calc R U . . .
C10 C 0.4772(2) 0.2144(4) 0.6096(5) 0.0474(11) Uani 1 1 d . . . . .
H10A H 0.484113 0.199524 0.514440 0.071 Uiso 1 1 calc R U . . .
H10B H 0.517845 0.194122 0.666018 0.071 Uiso 1 1 calc R U . . .
H10C H 0.467393 0.295038 0.621375 0.071 Uiso 1 1 calc R U . . .
C11 C 0.4084(2) 0.1594(4) 0.8007(4) 0.0425(10) Uani 1 1 d . . . . .
H11A H 0.397907 0.239035 0.817790 0.064 Uiso 1 1 calc R U . . .
H11B H 0.449452 0.137956 0.855038 0.064 Uiso 1 1 calc R U . . .
H11C H 0.371269 0.111388 0.825418 0.064 Uiso 1 1 calc R U . . .
N5 N 0.08454(19) 0.5612(3) 0.3210(4) 0.0484(9) Uani 1 1 d . . . . .
H5 H 0.055(3) 0.551(5) 0.385(5) 0.060(16) Uiso 1 1 d . . . . .
C12 C 0.0588(2) 0.5062(5) 0.1931(5) 0.0585(13) Uani 1 1 d . . . . .
H12A H 0.013630 0.536553 0.165468 0.070 Uiso 1 1 calc R U . . .
H12B H 0.088545 0.525328 0.121285 0.070 Uiso 1 1 calc R U . . .
C13 C 0.0547(4) 0.3824(6) 0.2057(8) 0.098(2) Uani 1 1 d . . . . .
H13A H 0.099768 0.351426 0.227080 0.147 Uiso 1 1 calc R U . . .
H13B H 0.035553 0.350067 0.120247 0.147 Uiso 1 1 calc R U . . .
H13C H 0.026222 0.363037 0.278256 0.147 Uiso 1 1 calc R U . . .
C14 C 0.0879(3) 0.6856(5) 0.3008(5) 0.0626(14) Uani 1 1 d . . . . .
H14A H 0.124268 0.702632 0.241690 0.075 Uiso 1 1 calc R U . . .
H14B H 0.045242 0.711710 0.253736 0.075 Uiso 1 1 calc R U . . .
C15 C 0.1002(3) 0.7496(6) 0.4287(7) 0.084(2) Uani 1 1 d . . . . .
H15A H 0.064695 0.732556 0.488243 0.126 Uiso 1 1 calc R U . . .
H15B H 0.100301 0.831084 0.409134 0.126 Uiso 1 1 calc R U . . .
H15C H 0.143667 0.727560 0.473279 0.126 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
I1 Pd1 2.6028(4) . ?
I2 Pd1 2.6068(4) . ?
Pd1 C1 1.983(4) . ?
Pd1 N5 2.139(4) . ?
N1 C1 1.362(5) . ?
N1 C2 1.382(4) . ?
N1 C3 1.457(5) . ?
C1 N2 1.331(5) . ?
N2 N3 1.393(4) . ?
N2 C4 1.490(5) . ?
N3 C2 1.299(5) . ?
C2 N4 1.364(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.516(6) . ?
C4 C6 1.517(7) . ?
C4 C7 1.526(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N4 C8 1.489(5) . ?
N4 H4 0.80(3) . ?
C8 C11 1.523(5) . ?
C8 C9 1.524(6) . ?
C8 C10 1.527(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
N5 C12 1.481(7) . ?
N5 C14 1.483(7) . ?
N5 H5 0.91(6) . ?
C12 C13 1.468(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.480(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 N5 178.32(16) . . ?
C1 Pd1 I1 89.56(11) . . ?
N5 Pd1 I1 91.21(12) . . ?
C1 Pd1 I2 88.67(11) . . ?
N5 Pd1 I2 90.53(12) . . ?
I1 Pd1 I2 177.752(17) . . ?
C1 N1 C2 108.2(3) . . ?
C1 N1 C3 126.0(3) . . ?
C2 N1 C3 125.6(3) . . ?
N2 C1 N1 104.1(3) . . ?
N2 C1 Pd1 132.8(3) . . ?
N1 C1 Pd1 123.1(3) . . ?
C1 N2 N3 113.1(3) . . ?
C1 N2 C4 131.9(3) . . ?
N3 N2 C4 115.0(3) . . ?
C2 N3 N2 103.7(3) . . ?
N3 C2 N4 127.8(3) . . ?
N3 C2 N1 110.9(3) . . ?
N4 C2 N1 121.2(3) . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 C5 111.3(3) . . ?
N2 C4 C6 107.6(4) . . ?
C5 C4 C6 110.1(4) . . ?
N2 C4 C7 107.0(4) . . ?
C5 C4 C7 109.5(5) . . ?
C6 C4 C7 111.3(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 N4 C8 122.6(3) . . ?
C2 N4 H4 114(3) . . ?
C8 N4 H4 110(3) . . ?
N4 C8 C11 111.1(3) . . ?
N4 C8 C9 105.8(3) . . ?
C11 C8 C9 109.4(3) . . ?
N4 C8 C10 109.8(3) . . ?
C11 C8 C10 111.1(4) . . ?
C9 C8 C10 109.5(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 N5 C14 109.5(4) . . ?
C12 N5 Pd1 114.9(3) . . ?
C14 N5 Pd1 114.8(3) . . ?
C12 N5 H5 109(3) . . ?
C14 N5 H5 105(3) . . ?
Pd1 N5 H5 102(3) . . ?
C13 C12 N5 112.3(5) . . ?
C13 C12 H12A 109.1 . . ?
N5 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
N5 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N5 113.3(5) . . ?
C15 C14 H14A 108.9 . . ?
N5 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
N5 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 N2 -0.1(4) . . . . ?
C3 N1 C1 N2 -175.9(4) . . . . ?
C2 N1 C1 Pd1 -179.8(2) . . . . ?
C3 N1 C1 Pd1 4.4(5) . . . . ?
N1 C1 N2 N3 -0.5(4) . . . . ?
Pd1 C1 N2 N3 179.2(3) . . . . ?
N1 C1 N2 C4 177.3(4) . . . . ?
Pd1 C1 N2 C4 -3.0(7) . . . . ?
C1 N2 N3 C2 0.9(4) . . . . ?
C4 N2 N3 C2 -177.3(3) . . . . ?
N2 N3 C2 N4 175.1(4) . . . . ?
N2 N3 C2 N1 -0.9(4) . . . . ?
C1 N1 C2 N3 0.7(4) . . . . ?
C3 N1 C2 N3 176.5(4) . . . . ?
C1 N1 C2 N4 -175.7(3) . . . . ?
C3 N1 C2 N4 0.1(6) . . . . ?
C1 N2 C4 C5 3.8(7) . . . . ?
N3 N2 C4 C5 -178.4(4) . . . . ?
C1 N2 C4 C6 124.6(5) . . . . ?
N3 N2 C4 C6 -57.6(5) . . . . ?
C1 N2 C4 C7 -115.7(5) . . . . ?
N3 N2 C4 C7 62.1(5) . . . . ?
N3 C2 N4 C8 8.8(6) . . . . ?
N1 C2 N4 C8 -175.5(3) . . . . ?
C2 N4 C8 C11 59.5(5) . . . . ?
C2 N4 C8 C9 178.1(3) . . . . ?
C2 N4 C8 C10 -63.8(5) . . . . ?
C14 N5 C12 C13 179.5(5) . . . . ?
Pd1 N5 C12 C13 48.6(6) . . . . ?
C12 N5 C14 C15 168.6(5) . . . . ?
Pd1 N5 C14 C15 -60.4(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N4 H4 I1 0.80(3) 2.97(3) 3.697(3) 152(4) 4_566 yes
N5 H5 I2 0.91(6) 2.91(5) 3.387(4) 114(4) . yes
N5 H5 I2 0.91(6) 3.30(6) 3.977(4) 133(4) 3_566 yes

_refine_diff_density_max         2.487
_refine_diff_density_min         -2.185
_refine_diff_density_rms         0.089

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

data_3j
_database_code_depnum_ccdc_archive 'CCDC 2074561'
loop_
_audit_author_name
_audit_author_address
'Mikhail Minyaev'
;N D Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2021-03-31 deposited with the CCDC.	2021-05-28 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         'C16 H27 I2 N5 Pd'
_chemical_formula_sum            'C16 H27 I2 N5 Pd'
_chemical_formula_weight         649.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   20.4176(3)
_cell_length_b                   11.1135(2)
_cell_length_c                   10.0749(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.2749(5)
_cell_angle_gamma                90
_cell_volume                     2225.02(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9830
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      33.14
_exptl_crystal_description       plate
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    3.617
_shelx_estimated_absorpt_T_min   0.281
_shelx_estimated_absorpt_T_max   0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1583
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-Ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS D8 QUEST, Photon III detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            105746
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.100
_diffrn_reflns_theta_max         33.179
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8492
_reflns_number_gt                8254
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_solution    
;
SHELXT, SHELXS-2013 (Sheldrick, Acta Cryst., 2015, A71, 3-8)
;
_computing_structure_refinement  
;
SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)
;
_computing_molecular_graphics    
;
SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_computing_publication_material  
;
SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0133P)²+1.4224P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8492
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0173
_refine_ls_wR_factor_ref         0.0400
_refine_ls_wR_factor_gt          0.0395
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_restrained_S_all      1.210
_refine_ls_shift/su_max          0.005
_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
I1 I 0.28320(2) 0.47913(2) 0.88545(2) 0.01982(2) Uani 1 1 d . . . . .
I2 I 0.37407(2) 0.52252(2) 0.44441(2) 0.01869(2) Uani 1 1 d . . . . .
Pd1 Pd 0.33104(2) 0.49772(2) 0.66736(2) 0.01355(2) Uani 1 1 d . . . . .
N1 N 0.19146(5) 0.53314(9) 0.48433(11) 0.01478(17) Uani 1 1 d . . . . .
N2 N 0.14610(5) 0.62400(9) 0.42973(11) 0.01518(17) Uani 1 1 d . . . . .
N3 N 0.23533(5) 0.69518(9) 0.57679(10) 0.01352(17) Uani 1 1 d . . . . .
N4 N 0.14851(5) 0.83530(10) 0.48034(11) 0.01496(17) Uani 1 1 d . . . . .
N5 N 0.42293(5) 0.42570(10) 0.77240(11) 0.01784(19) Uani 1 1 d . . . . .
C1 C 0.24631(6) 0.57414(10) 0.57087(12) 0.01369(18) Uani 1 1 d . . . . .
C2 C 0.17440(6) 0.72145(11) 0.49009(11) 0.01344(18) Uani 1 1 d . . . . .
C3 C 0.17081(7) 0.40918(11) 0.43597(14) 0.0187(2) Uani 1 1 d . . . . .
C4 C 0.17017(9) 0.40372(15) 0.28433(16) 0.0300(3) Uani 1 1 d . . . . .
H4A H 0.154174 0.324467 0.248181 0.045 Uiso 1 1 calc R U . . .
H4B H 0.215815 0.417021 0.271793 0.045 Uiso 1 1 calc R U . . .
H4C H 0.140117 0.466151 0.235644 0.045 Uiso 1 1 calc R U . . .
C5 C 0.10037(7) 0.38835(14) 0.45971(18) 0.0274(3) Uani 1 1 d . . . . .
H5A H 0.084919 0.307515 0.428390 0.041 Uiso 1 1 calc R U . . .
H5B H 0.069335 0.448345 0.408741 0.041 Uiso 1 1 calc R U . . .
H5C H 0.101710 0.395831 0.557216 0.041 Uiso 1 1 calc R U . . .
C6 C 0.21874(8) 0.31625(12) 0.51536(17) 0.0269(3) Uani 1 1 d . . . . .
H6A H 0.202738 0.235346 0.485512 0.040 Uiso 1 1 calc R U . . .
H6B H 0.220668 0.325053 0.612971 0.040 Uiso 1 1 calc R U . . .
H6C H 0.263745 0.328352 0.498857 0.040 Uiso 1 1 calc R U . . .
C7 C 0.08699(6) 0.86834(11) 0.37578(12) 0.0157(2) Uani 1 1 d . . . . .
C8 C 0.07695(8) 1.00288(12) 0.39572(15) 0.0223(2) Uani 1 1 d . . . . .
H8A H 0.036206 1.030102 0.330905 0.033 Uiso 1 1 calc R U . . .
H8B H 0.115928 1.047327 0.380010 0.033 Uiso 1 1 calc R U . . .
H8C H 0.072265 1.017456 0.489029 0.033 Uiso 1 1 calc R U . . .
C9 C 0.09694(7) 0.84610(13) 0.23216(12) 0.0200(2) Uani 1 1 d . . . . .
H9A H 0.057246 0.874266 0.165044 0.030 Uiso 1 1 calc R U . . .
H9B H 0.103181 0.759807 0.219304 0.030 Uiso 1 1 calc R U . . .
H9C H 0.136782 0.889967 0.219959 0.030 Uiso 1 1 calc R U . . .
C10 C 0.02658(6) 0.79863(13) 0.40106(14) 0.0212(2) Uani 1 1 d . . . . .
H10A H -0.014349 0.825474 0.336525 0.032 Uiso 1 1 calc R U . . .
H10B H 0.022093 0.813252 0.494490 0.032 Uiso 1 1 calc R U . . .
H10C H 0.033201 0.712426 0.388388 0.032 Uiso 1 1 calc R U . . .
C11 C 0.27686(7) 0.77992(11) 0.67056(13) 0.0186(2) Uani 1 1 d . . . . .
H11A H 0.248991 0.821753 0.723243 0.028 Uiso 1 1 calc R U . . .
H11B H 0.296552 0.838766 0.618575 0.028 Uiso 1 1 calc R U . . .
H11C H 0.312925 0.736125 0.732820 0.028 Uiso 1 1 calc R U . . .
C12 C 0.47949(7) 0.49100(13) 0.78628(14) 0.0206(2) Uani 1 1 d . . . . .
H12 H 0.477167 0.566586 0.741389 0.025 Uiso 1 1 calc R U . . .
C13 C 0.54108(7) 0.45243(15) 0.86352(15) 0.0238(3) Uani 1 1 d . . . . .
H13 H 0.580037 0.501250 0.872246 0.029 Uiso 1 1 calc R U . . .
C14 C 0.54497(7) 0.34149(14) 0.92785(15) 0.0251(3) Uani 1 1 d . . . . .
H14 H 0.586588 0.312955 0.981310 0.030 Uiso 1 1 calc R U . . .
C15 C 0.48689(7) 0.27291(13) 0.91265(16) 0.0251(3) Uani 1 1 d . . . . .
H15 H 0.488195 0.196338 0.955084 0.030 Uiso 1 1 calc R U . . .
C16 C 0.42695(7) 0.31781(12) 0.83462(15) 0.0217(2) Uani 1 1 d . . . . .
H16 H 0.387273 0.270748 0.824698 0.026 Uiso 1 1 calc R U . . .
H4 H 0.1784(9) 0.8867(16) 0.4860(17) 0.014(4) Uiso 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
I1 Pd1 2.60963(13) . ?
I2 Pd1 2.60763(12) . ?
Pd1 C1 1.9716(11) . ?
Pd1 N5 2.0901(11) . ?
N1 C1 1.3318(15) . ?
N1 N2 1.3950(14) . ?
N1 C3 1.4895(16) . ?
N2 C2 1.3097(15) . ?
N3 C1 1.3672(15) . ?
N3 C2 1.3772(15) . ?
N3 C11 1.4597(16) . ?
N4 C2 1.3662(15) . ?
N4 C7 1.4881(15) . ?
N4 H4 0.829(18) . ?
N5 C12 1.3437(17) . ?
N5 C16 1.3468(17) . ?
C3 C6 1.5181(19) . ?
C3 C4 1.526(2) . ?
C3 C5 1.529(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C9 1.5267(17) . ?
C7 C10 1.5267(18) . ?
C7 C8 1.5287(18) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.3862(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.388(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.3868(19) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 N5 177.00(5) . . ?
C1 Pd1 I2 87.75(3) . . ?
N5 Pd1 I2 92.05(3) . . ?
C1 Pd1 I1 89.63(3) . . ?
N5 Pd1 I1 90.54(3) . . ?
I2 Pd1 I1 177.342(4) . . ?
C1 N1 N2 113.13(10) . . ?
C1 N1 C3 131.53(11) . . ?
N2 N1 C3 115.34(10) . . ?
C2 N2 N1 103.49(9) . . ?
C1 N3 C2 108.31(10) . . ?
C1 N3 C11 125.89(10) . . ?
C2 N3 C11 125.43(10) . . ?
C2 N4 C7 121.95(10) . . ?
C2 N4 H4 111.5(12) . . ?
C7 N4 H4 111.6(12) . . ?
C12 N5 C16 118.25(12) . . ?
C12 N5 Pd1 119.73(9) . . ?
C16 N5 Pd1 121.89(9) . . ?
N1 C1 N3 104.09(10) . . ?
N1 C1 Pd1 133.33(9) . . ?
N3 C1 Pd1 122.44(8) . . ?
N2 C2 N4 127.61(11) . . ?
N2 C2 N3 110.93(10) . . ?
N4 C2 N3 121.35(10) . . ?
N1 C3 C6 110.92(10) . . ?
N1 C3 C4 107.52(11) . . ?
C6 C3 C4 110.90(12) . . ?
N1 C3 C5 107.14(11) . . ?
C6 C3 C5 109.29(12) . . ?
C4 C3 C5 111.01(12) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 C9 110.89(10) . . ?
N4 C7 C10 109.86(10) . . ?
C9 C7 C10 111.37(11) . . ?
N4 C7 C8 105.38(10) . . ?
C9 C7 C8 109.51(11) . . ?
C10 C7 C8 109.66(11) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 C13 122.59(13) . . ?
N5 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
C12 C13 C14 118.98(13) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C13 C14 C15 118.74(13) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 119.04(13) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
N5 C16 C15 122.39(13) . . ?
N5 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 C2 -2.14(13) . . . . ?
C3 N1 N2 C2 178.25(10) . . . . ?
N2 N1 C1 N3 2.18(13) . . . . ?
C3 N1 C1 N3 -178.28(12) . . . . ?
N2 N1 C1 Pd1 -173.51(9) . . . . ?
C3 N1 C1 Pd1 6.0(2) . . . . ?
C2 N3 C1 N1 -1.36(13) . . . . ?
C11 N3 C1 N1 171.93(11) . . . . ?
C2 N3 C1 Pd1 174.92(8) . . . . ?
C11 N3 C1 Pd1 -11.78(17) . . . . ?
N1 N2 C2 N4 -174.97(12) . . . . ?
N1 N2 C2 N3 1.16(13) . . . . ?
C7 N4 C2 N2 -11.62(19) . . . . ?
C7 N4 C2 N3 172.61(11) . . . . ?
C1 N3 C2 N2 0.09(14) . . . . ?
C11 N3 C2 N2 -173.24(11) . . . . ?
C1 N3 C2 N4 176.50(11) . . . . ?
C11 N3 C2 N4 3.17(18) . . . . ?
C1 N1 C3 C6 8.13(19) . . . . ?
N2 N1 C3 C6 -172.34(11) . . . . ?
C1 N1 C3 C4 -113.27(15) . . . . ?
N2 N1 C3 C4 66.26(14) . . . . ?
C1 N1 C3 C5 127.33(14) . . . . ?
N2 N1 C3 C5 -53.14(14) . . . . ?
C2 N4 C7 C9 -59.36(15) . . . . ?
C2 N4 C7 C10 64.18(14) . . . . ?
C2 N4 C7 C8 -177.77(11) . . . . ?
C16 N5 C12 C13 -1.1(2) . . . . ?
Pd1 N5 C12 C13 174.89(11) . . . . ?
N5 C12 C13 C14 0.8(2) . . . . ?
C12 C13 C14 C15 0.0(2) . . . . ?
C13 C14 C15 C16 -0.4(2) . . . . ?
C12 N5 C16 C15 0.5(2) . . . . ?
Pd1 N5 C16 C15 -175.33(11) . . . . ?
C14 C15 C16 N5 0.2(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N4 H4 I1 0.829(18) 2.970(18) 3.7332(11) 154.1(15) 4_575 yes

_refine_diff_density_max         0.711
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.086

