# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_7473a
_database_code_depnum_ccdc_archive 'CCDC 2119516'
loop_
_audit_author_name
_audit_author_address
'Geok Kheng Tan '
;Department of Chemistry, National University of Singapore
Singapore
;
_audit_update_record             
;
2021-11-01 deposited with the CCDC.	2021-11-25 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         ?
_chemical_formula_sum            'C32 H50 Br2 N4 O2 Pd2 S2'
_chemical_formula_weight         959.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 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, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.0247(9)
_cell_length_b                   20.8936(15)
_cell_length_c                   8.5817(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2156.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    8748
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.52

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    2.813
_shelx_estimated_absorpt_T_min   0.283
_shelx_estimated_absorpt_T_max   0.399
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.49870
_exptl_absorpt_correction_T_max  0.74567
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Microfocus Sealed Tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15399
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.949
_diffrn_reflns_theta_max         27.495
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4936
_reflns_number_gt                4704
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.996

_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. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL--2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT--(Sheldrick 2015)'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+0.1986P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Dual Space'
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.040(13)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4936
_refine_ls_number_parameters     228
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.094
_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 0.48542(3) 0.42952(2) 0.44395(4) 0.02512(11) Uani 1 1 d . . . . .
Br1 Br 0.33432(5) 0.37620(3) 0.30287(8) 0.04982(17) Uani 1 1 d . . . . .
S1 S 0.61859(10) 0.48920(5) 0.57189(13) 0.0291(2) Uani 1 1 d . . . . .
N1 N 0.6410(4) 0.3729(2) 0.2072(5) 0.0327(9) Uani 1 1 d . . . . .
N2 N 0.6108(4) 0.30752(19) 0.4018(5) 0.0324(9) Uani 1 1 d . . . . .
C1 C 0.5866(4) 0.3665(2) 0.3444(6) 0.0292(10) Uani 1 1 d . . . . .
C2 C 0.7016(5) 0.3172(2) 0.1758(7) 0.0370(11) Uani 1 1 d . . . . .
C3 C 0.7709(5) 0.2990(3) 0.0550(8) 0.0491(14) Uani 1 1 d . . . . .
H3 H 0.784879 0.326702 -0.029082 0.059 Uiso 1 1 calc R U . . .
C4 C 0.8192(6) 0.2389(3) 0.0616(9) 0.0589(16) Uani 1 1 d . . . . .
H4 H 0.864099 0.225216 -0.021579 0.071 Uiso 1 1 calc R U . . .
C5 C 0.8030(6) 0.1984(3) 0.1878(9) 0.0596(18) Uani 1 1 d . . . . .
H5 H 0.838674 0.158375 0.190628 0.071 Uiso 1 1 calc R U . . .
C6 C 0.7346(5) 0.2167(3) 0.3096(8) 0.0455(13) Uani 1 1 d . . . . .
H6 H 0.722976 0.189615 0.395425 0.055 Uiso 1 1 calc R U . . .
C7 C 0.6834(4) 0.2762(2) 0.3016(7) 0.0368(11) Uani 1 1 d . . . . .
C8 C 0.6219(5) 0.4280(3) 0.1033(6) 0.0411(12) Uani 1 1 d . . . . .
H8 H 0.582250 0.460945 0.164889 0.049 Uiso 1 1 calc R U . . .
C9 C 0.5454(7) 0.4084(3) -0.0293(7) 0.0569(17) Uani 1 1 d . . . . .
H9A H 0.580082 0.374452 -0.089174 0.085 Uiso 1 1 calc R U . . .
H9B H 0.531890 0.444947 -0.096406 0.085 Uiso 1 1 calc R U . . .
H9C H 0.475360 0.393274 0.012992 0.085 Uiso 1 1 calc R U . . .
C10 C 0.7312(7) 0.4587(3) 0.0448(9) 0.0605(17) Uani 1 1 d . . . . .
H10A H 0.783668 0.461639 0.130388 0.091 Uiso 1 1 calc R U . . .
H10B H 0.715880 0.501231 0.004865 0.091 Uiso 1 1 calc R U . . .
H10C H 0.762607 0.432512 -0.037450 0.091 Uiso 1 1 calc R U . . .
C11 C 0.5592(5) 0.2816(2) 0.5420(7) 0.0407(12) Uani 1 1 d . . . . .
H11 H 0.507225 0.314940 0.579687 0.049 Uiso 1 1 calc R U . . .
C12 C 0.6445(7) 0.2724(4) 0.6707(8) 0.0606(18) Uani 1 1 d . . . . .
H12A H 0.683996 0.232504 0.654235 0.091 Uiso 1 1 calc R U . . .
H12B H 0.607068 0.271203 0.770738 0.091 Uiso 1 1 calc R U . . .
H12C H 0.696981 0.307696 0.669233 0.091 Uiso 1 1 calc R U . . .
C13 C 0.4878(7) 0.2220(3) 0.5083(10) 0.067(2) Uani 1 1 d . . . . .
H13A H 0.441498 0.229842 0.417818 0.101 Uiso 1 1 calc R U . . .
H13B H 0.441060 0.212905 0.597731 0.101 Uiso 1 1 calc R U . . .
H13C H 0.536002 0.185669 0.488305 0.101 Uiso 1 1 calc R U . . .
C14 C 0.7621(4) 0.4854(2) 0.5037(7) 0.0369(11) Uani 1 1 d . . . . .
H14 H 0.764201 0.495090 0.390860 0.044 Uiso 1 1 calc R U . . .
C15 C 0.8149(5) 0.4204(3) 0.5323(10) 0.0578(18) Uani 1 1 d . . . . .
H15A H 0.891483 0.421088 0.496932 0.087 Uiso 1 1 calc R U . . .
H15B H 0.774063 0.387891 0.475305 0.087 Uiso 1 1 calc R U . . .
H15C H 0.812775 0.410702 0.642765 0.087 Uiso 1 1 calc R U . . .
C16 C 0.8260(5) 0.5367(3) 0.5919(10) 0.0583(18) Uani 1 1 d . . . . .
H16A H 0.822782 0.527854 0.702789 0.088 Uiso 1 1 calc R U . . .
H16B H 0.793161 0.578235 0.571255 0.088 Uiso 1 1 calc R U . . .
H16C H 0.902978 0.536723 0.557958 0.088 Uiso 1 1 calc R U . . .
O1W O 0.9246(19) 0.6200(10) 0.070(3) 0.130(7) Uani 0.446(4) 1 d . U P A 1
O2W O 0.959(2) 0.5778(10) 0.155(3) 0.119(7) Uani 0.387(4) 1 d . U P B 2
O3W O 0.970(3) 0.6074(15) -0.039(4) 0.071(8) Uani 0.167(4) 1 d . U P C 3


_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 1.986(5) . ?
Pd1 S1 2.3075(12) . ?
Pd1 S1 2.3778(12) 2_665 ?
Pd1 Br1 2.4511(7) . ?
Pd1 Pd1 2.9660(6) 2_665 ?
S1 C14 1.823(5) . ?
N1 C1 1.354(6) . ?
N1 C2 1.398(7) . ?
N1 C8 1.475(7) . ?
N2 C1 1.359(6) . ?
N2 C7 1.390(7) . ?
N2 C11 1.457(7) . ?
C2 C3 1.383(8) . ?
C2 C7 1.395(8) . ?
C3 C4 1.384(9) . ?
C3 H3 0.9400 . ?
C4 C5 1.389(10) . ?
C4 H4 0.9400 . ?
C5 C6 1.384(9) . ?
C5 H5 0.9400 . ?
C6 C7 1.388(7) . ?
C6 H6 0.9400 . ?
C8 C9 1.520(9) . ?
C8 C10 1.545(9) . ?
C8 H8 0.9900 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 C12 1.520(9) . ?
C11 C13 1.541(9) . ?
C11 H11 0.9900 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 C15 1.519(7) . ?
C14 C16 1.521(8) . ?
C14 H14 0.9900 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 S1 97.90(14) . . ?
C1 Pd1 S1 173.93(14) . 2_665 ?
S1 Pd1 S1 76.07(5) . 2_665 ?
C1 Pd1 Br1 86.59(14) . . ?
S1 Pd1 Br1 174.29(3) . . ?
S1 Pd1 Br1 99.37(4) 2_665 . ?
C1 Pd1 Pd1 125.85(14) . 2_665 ?
S1 Pd1 Pd1 51.78(3) . 2_665 ?
S1 Pd1 Pd1 49.68(3) 2_665 2_665 ?
Br1 Pd1 Pd1 122.61(2) . 2_665 ?
C14 S1 Pd1 118.72(18) . . ?
C14 S1 Pd1 112.37(18) . 2_665 ?
Pd1 S1 Pd1 78.53(4) . 2_665 ?
C1 N1 C2 109.7(4) . . ?
C1 N1 C8 121.8(4) . . ?
C2 N1 C8 127.9(5) . . ?
C1 N2 C7 109.7(4) . . ?
C1 N2 C11 123.0(4) . . ?
C7 N2 C11 127.1(4) . . ?
N1 C1 N2 107.5(4) . . ?
N1 C1 Pd1 127.2(4) . . ?
N2 C1 Pd1 125.2(4) . . ?
C3 C2 C7 120.3(5) . . ?
C3 C2 N1 133.4(5) . . ?
C7 C2 N1 106.3(5) . . ?
C2 C3 C4 118.1(6) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C3 C4 C5 121.8(6) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C6 C5 C4 120.2(6) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 118.3(6) . . ?
C5 C6 H6 120.8 . . ?
C7 C6 H6 120.8 . . ?
C6 C7 N2 132.0(6) . . ?
C6 C7 C2 121.3(5) . . ?
N2 C7 C2 106.7(4) . . ?
N1 C8 C9 109.6(5) . . ?
N1 C8 C10 112.8(5) . . ?
C9 C8 C10 112.6(5) . . ?
N1 C8 H8 107.2 . . ?
C9 C8 H8 107.2 . . ?
C10 C8 H8 107.2 . . ?
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 . . ?
N2 C11 C12 111.1(5) . . ?
N2 C11 C13 112.5(5) . . ?
C12 C11 C13 114.2(5) . . ?
N2 C11 H11 106.1 . . ?
C12 C11 H11 106.1 . . ?
C13 C11 H11 106.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C16 109.8(5) . . ?
C15 C14 S1 112.5(4) . . ?
C16 C14 S1 106.8(4) . . ?
C15 C14 H14 109.2 . . ?
C16 C14 H14 109.2 . . ?
S1 C14 H14 109.2 . . ?
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 . . ?

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 -0.2(6) . . . . ?
C8 N1 C1 N2 172.0(4) . . . . ?
C2 N1 C1 Pd1 -178.3(4) . . . . ?
C8 N1 C1 Pd1 -6.1(7) . . . . ?
C7 N2 C1 N1 1.3(6) . . . . ?
C11 N2 C1 N1 -174.6(4) . . . . ?
C7 N2 C1 Pd1 179.4(4) . . . . ?
C11 N2 C1 Pd1 3.6(7) . . . . ?
C1 N1 C2 C3 -179.2(6) . . . . ?
C8 N1 C2 C3 9.2(10) . . . . ?
C1 N1 C2 C7 -0.9(6) . . . . ?
C8 N1 C2 C7 -172.5(5) . . . . ?
C7 C2 C3 C4 1.4(9) . . . . ?
N1 C2 C3 C4 179.5(6) . . . . ?
C2 C3 C4 C5 -2.6(10) . . . . ?
C3 C4 C5 C6 2.0(11) . . . . ?
C4 C5 C6 C7 -0.1(10) . . . . ?
C5 C6 C7 N2 179.2(6) . . . . ?
C5 C6 C7 C2 -1.0(9) . . . . ?
C1 N2 C7 C6 178.0(6) . . . . ?
C11 N2 C7 C6 -6.4(10) . . . . ?
C1 N2 C7 C2 -1.8(6) . . . . ?
C11 N2 C7 C2 173.8(5) . . . . ?
C3 C2 C7 C6 0.4(9) . . . . ?
N1 C2 C7 C6 -178.2(5) . . . . ?
C3 C2 C7 N2 -179.8(5) . . . . ?
N1 C2 C7 N2 1.6(6) . . . . ?
C1 N1 C8 C9 -101.2(6) . . . . ?
C2 N1 C8 C9 69.5(7) . . . . ?
C1 N1 C8 C10 132.5(5) . . . . ?
C2 N1 C8 C10 -56.8(7) . . . . ?
C1 N2 C11 C12 -114.7(6) . . . . ?
C7 N2 C11 C12 70.2(7) . . . . ?
C1 N2 C11 C13 115.9(6) . . . . ?
C7 N2 C11 C13 -59.2(7) . . . . ?
Pd1 S1 C14 C15 -68.2(5) . . . . ?
Pd1 S1 C14 C15 -157.1(4) 2_665 . . . ?
Pd1 S1 C14 C16 171.3(3) . . . . ?
Pd1 S1 C14 C16 82.4(4) 2_665 . . . ?

_refine_diff_density_max         1.134
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.132



####################################################################### 
# 
# 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_8084r
_database_code_depnum_ccdc_archive 'CCDC 2119517'
loop_
_audit_author_name
_audit_author_address
'Geok Kheng Tan '
;Department of Chemistry, National University of Singapore
Singapore
;
_audit_update_record             
;
2021-11-01 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H56 N6 Pd S2'
_chemical_formula_weight         743.39

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.7132(4)
_cell_length_b                   16.3123(6)
_cell_length_c                   11.7957(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.4020(10)
_cell_angle_gamma                90.00
_cell_volume                     1862.09(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7498
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7146
_exptl_absorpt_correction_T_max  0.8505
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13116
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4267
_reflns_number_gt                3967
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0332P)²+0.9322P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4267
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0657
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.0000 0.0000 0.01114(6) Uani 1 2 d S . .
S1 S 0.01050(4) 0.14177(2) -0.02403(4) 0.01649(9) Uani 1 1 d . . .
N1 N 0.12619(13) 0.01950(8) 0.28150(12) 0.0134(3) Uani 1 1 d . . .
N2 N -0.08490(13) 0.06506(8) 0.20261(12) 0.0134(3) Uani 1 1 d . . .
C1 C 0.01043(15) 0.02748(9) 0.17229(14) 0.0133(3) Uani 1 1 d . . .
C2 C 0.10744(16) 0.05453(9) 0.38131(14) 0.0137(3) Uani 1 1 d . . .
C3 C 0.19698(17) 0.06722(9) 0.50734(14) 0.0168(3) Uani 1 1 d . . .
H3 H 0.2899 0.0484 0.5415 0.020 Uiso 1 1 calc R . .
C4 C 0.14471(17) 0.10843(10) 0.58061(14) 0.0185(3) Uani 1 1 d . . .
H4 H 0.2031 0.1183 0.6667 0.022 Uiso 1 1 calc R . .
C5 C 0.00792(17) 0.13567(10) 0.53016(16) 0.0193(3) Uani 1 1 d . . .
H5 H -0.0250 0.1632 0.5830 0.023 Uiso 1 1 calc R . .
C6 C -0.08082(17) 0.12353(10) 0.40505(15) 0.0170(3) Uani 1 1 d . . .
H6 H -0.1738 0.1421 0.3711 0.020 Uiso 1 1 calc R . .
C7 C -0.02830(16) 0.08301(9) 0.33085(14) 0.0138(3) Uani 1 1 d . . .
C8 C 0.25497(16) -0.01793(10) 0.28941(15) 0.0162(3) Uani 1 1 d . . .
H8 H 0.2345 -0.0416 0.2050 0.019 Uiso 1 1 calc R . .
C9 C 0.36656(17) 0.04692(11) 0.31685(17) 0.0244(4) Uani 1 1 d . . .
H9A H 0.3310 0.0910 0.2547 0.037 Uiso 1 1 calc R . .
H9B H 0.4476 0.0220 0.3125 0.037 Uiso 1 1 calc R . .
H9C H 0.3928 0.0694 0.4010 0.037 Uiso 1 1 calc R . .
C10 C 0.29754(18) -0.08902(11) 0.38309(15) 0.0216(3) Uani 1 1 d . . .
H10A H 0.3092 -0.0689 0.4653 0.032 Uiso 1 1 calc R . .
H10B H 0.3850 -0.1123 0.3902 0.032 Uiso 1 1 calc R . .
H10C H 0.2257 -0.1314 0.3537 0.032 Uiso 1 1 calc R . .
C11 C -0.22498(15) 0.08906(10) 0.11043(14) 0.0162(3) Uani 1 1 d . . .
H11 H -0.2366 0.0692 0.0262 0.019 Uiso 1 1 calc R . .
C12 C -0.33652(17) 0.04816(11) 0.13858(16) 0.0225(3) Uani 1 1 d . . .
H12A H -0.3220 -0.0113 0.1446 0.034 Uiso 1 1 calc R . .
H12B H -0.4276 0.0605 0.0710 0.034 Uiso 1 1 calc R . .
H12C H -0.3317 0.0690 0.2183 0.034 Uiso 1 1 calc R . .
C13 C -0.23828(17) 0.18219(10) 0.10336(16) 0.0201(3) Uani 1 1 d . . .
H13A H -0.2167 0.2042 0.1870 0.030 Uiso 1 1 calc R . .
H13B H -0.3330 0.1973 0.0457 0.030 Uiso 1 1 calc R . .
H13C H -0.1737 0.2049 0.0728 0.030 Uiso 1 1 calc R . .
C14 C 0.10734(17) 0.16470(10) -0.11588(15) 0.0182(3) Uani 1 1 d . . .
H14 H 0.0825 0.1234 -0.1848 0.022 Uiso 1 1 calc R . .
C15 C 0.26276(19) 0.16084(12) -0.03446(18) 0.0292(4) Uani 1 1 d . . .
H15A H 0.3119 0.1721 -0.0862 0.044 Uiso 1 1 calc R . .
H15B H 0.2877 0.1061 0.0026 0.044 Uiso 1 1 calc R . .
H15C H 0.2885 0.2018 0.0325 0.044 Uiso 1 1 calc R . .
C16 C 0.0643(2) 0.24961(11) -0.17393(17) 0.0257(4) Uani 1 1 d . . .
H16A H 0.0868 0.2904 -0.1071 0.039 Uiso 1 1 calc R . .
H16B H -0.0354 0.2502 -0.2272 0.039 Uiso 1 1 calc R . .
H16C H 0.1139 0.2627 -0.2248 0.039 Uiso 1 1 calc R . .
N1S N 0.51357(17) -0.12924(11) 0.21574(17) 0.0351(4) Uani 1 1 d . . .
C1S C 0.44089(18) -0.18159(11) 0.21131(16) 0.0238(4) Uani 1 1 d . . .
C2S C 0.34583(19) -0.24708(11) 0.20503(17) 0.0250(4) Uani 1 1 d . . .
H2SA H 0.2526 -0.2246 0.1776 0.038 Uiso 1 1 calc R . .
H2SB H 0.3755 -0.2720 0.2882 0.038 Uiso 1 1 calc R . .
H2SC H 0.3454 -0.2888 0.1451 0.038 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.0369(15) 3 ?
Pd1 C1 2.0369(15) . ?
Pd1 S1 2.3384(4) 3 ?
Pd1 S1 2.3385(4) . ?
S1 C14 1.8316(16) . ?
N1 C1 1.3578(19) . ?
N1 C2 1.3985(19) . ?
N1 C8 1.4746(19) . ?
N2 C1 1.3639(19) . ?
N2 C7 1.3981(19) . ?
N2 C11 1.4791(19) . ?
C2 C7 1.394(2) . ?
C2 C3 1.396(2) . ?
C3 C4 1.388(2) . ?
C4 C5 1.397(2) . ?
C5 C6 1.385(2) . ?
C6 C7 1.394(2) . ?
C8 C9 1.524(2) . ?
C8 C10 1.530(2) . ?
C11 C12 1.524(2) . ?
C11 C13 1.525(2) . ?
C14 C15 1.525(2) . ?
C14 C16 1.526(2) . ?
N1S C1S 1.142(2) . ?
C1S C2S 1.456(3) . ?

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 C1 180.0 3 . ?
C1 Pd1 S1 85.32(4) 3 3 ?
C1 Pd1 S1 94.68(4) . 3 ?
C1 Pd1 S1 94.68(4) 3 . ?
C1 Pd1 S1 85.32(4) . . ?
S1 Pd1 S1 180.0 3 . ?
C14 S1 Pd1 110.03(5) . . ?
C1 N1 C2 110.91(13) . . ?
C1 N1 C8 123.28(13) . . ?
C2 N1 C8 125.75(13) . . ?
C1 N2 C7 110.60(12) . . ?
C1 N2 C11 124.33(12) . . ?
C7 N2 C11 124.91(13) . . ?
N1 C1 N2 106.03(13) . . ?
N1 C1 Pd1 124.22(11) . . ?
N2 C1 Pd1 129.33(11) . . ?
C7 C2 C3 121.31(14) . . ?
C7 C2 N1 106.08(13) . . ?
C3 C2 N1 132.51(14) . . ?
C4 C3 C2 117.27(15) . . ?
C3 C4 C5 121.22(15) . . ?
C6 C5 C4 121.59(15) . . ?
C5 C6 C7 117.36(14) . . ?
C6 C7 C2 121.22(14) . . ?
C6 C7 N2 132.40(14) . . ?
C2 C7 N2 106.32(13) . . ?
N1 C8 C9 110.71(13) . . ?
N1 C8 C10 109.90(13) . . ?
C9 C8 C10 114.16(14) . . ?
N2 C11 C12 111.53(13) . . ?
N2 C11 C13 110.21(13) . . ?
C12 C11 C13 112.60(13) . . ?
C15 C14 C16 110.98(14) . . ?
C15 C14 S1 111.18(12) . . ?
C16 C14 S1 108.18(11) . . ?
N1S C1S C2S 178.78(19) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_K291
_database_code_depnum_ccdc_archive 'CCDC 2119521'
loop_
_audit_author_name
_audit_author_address
'Geok Kheng Tan '
;Department of Chemistry, National University of Singapore
Singapore
;
_audit_update_record             
;
2021-11-01 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H42 Cl2 N12 O6 Pd2 S2'
_chemical_formula_weight         918.49

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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 '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                   9.1475(3)
_cell_length_b                   10.4335(4)
_cell_length_c                   11.9175(4)
_cell_angle_alpha                83.3350(10)
_cell_angle_beta                 80.5710(10)
_cell_angle_gamma                64.6560(10)
_cell_volume                     1012.71(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9950
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      29.61

_exptl_crystal_description       Thin_Plate
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_F_000             464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.056
_exptl_absorpt_coefficient_mu    1.170
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6789
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Microfocus Sealed Tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21939
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.206
_diffrn_reflns_theta_max         29.613
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5674
_reflns_number_gt                5306
_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_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL--2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT--(Sheldrick 2015)'
_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)+(0.0652P)²+2.0292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Dual Space'
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5674
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.1054
_refine_ls_goodness_of_fit_ref   1.050
_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 0.96425(2) 0.48644(2) 0.64724(2) 0.01522(8) Uani 1 1 d . . . . .
Cl1 Cl 1.1622(2) 0.91182(18) 0.95173(14) 0.0364(4) Uani 0.568(3) 1 d . . P . .
Cl2 Cl 0.8288(3) 0.0255(2) 0.49986(17) 0.0355(6) Uani 0.432(3) 1 d . . P . .
S1 S 0.84979(8) 0.46351(7) 0.49198(5) 0.01777(13) Uani 1 1 d . . . . .
N1 N 1.0744(3) 0.6292(3) 0.8026(2) 0.0239(5) Uani 1 1 d . . . . .
N2 N 1.1369(3) 0.4138(3) 0.8591(2) 0.0216(5) Uani 1 1 d . . . . .
N3 N 1.1935(3) 0.4676(3) 0.9339(2) 0.0311(6) Uani 1 1 d . . . . .
N4 N 0.7688(3) 0.3292(3) 0.7707(2) 0.0228(5) Uani 1 1 d . . . . .
N5 N 0.6595(3) 0.5435(3) 0.8154(2) 0.0255(5) Uani 1 1 d . . . . .
C1 C 1.0644(3) 0.5102(3) 0.7779(2) 0.0182(5) Uani 1 1 d . . . . .
C2 C 1.1538(4) 0.6005(4) 0.8969(3) 0.0293(6) Uani 1 1 d . . . . .
H2 H 1.176628 0.667065 0.930494 0.035 Uiso 1 1 calc R U . . .
C4 C 1.0145(5) 0.7676(4) 0.7395(3) 0.0348(7) Uani 1 1 d . . . . .
H4A H 0.932069 0.773622 0.693503 0.052 Uiso 1 1 calc R U . . .
H4B H 1.105602 0.778010 0.689497 0.052 Uiso 1 1 calc R U . . .
H4C H 0.966020 0.843521 0.793362 0.052 Uiso 1 1 calc R U . . .
C5 C 1.1658(4) 0.2656(3) 0.8714(3) 0.0281(6) Uani 1 1 d . . . . .
H5A H 1.188961 0.227638 0.795810 0.042 Uiso 1 1 calc R U . . .
H5B H 1.068798 0.256339 0.913012 0.042 Uiso 1 1 calc R U . . .
H5C H 1.259154 0.212287 0.913529 0.042 Uiso 1 1 calc R U . . .
C6 C 0.7896(3) 0.4506(3) 0.7537(2) 0.0184(5) Uani 1 1 d . . . . .
N6 N 0.5570(4) 0.4835(4) 0.8689(2) 0.0376(7) Uani 1 1 d . . . . .
C9 C 0.8760(4) 0.1931(3) 0.7230(3) 0.0300(6) Uani 1 1 d . . . . .
H9A H 0.811921 0.156658 0.688768 0.045 Uiso 1 1 calc R U . . .
H9B H 0.929958 0.125660 0.783512 0.045 Uiso 1 1 calc R U . . .
H9C H 0.958508 0.205318 0.664511 0.045 Uiso 1 1 calc R U . . .
C7 C 0.6273(4) 0.3508(4) 0.8412(3) 0.0307(7) Uani 1 1 d . . . . .
H7 H 0.586602 0.280927 0.865925 0.037 Uiso 1 1 calc R U . . .
C10 C 0.6208(5) 0.6926(4) 0.8286(3) 0.0368(8) Uani 1 1 d . . . . .
H10A H 0.502211 0.747590 0.836596 0.055 Uiso 1 1 calc R U . . .
H10B H 0.671164 0.729388 0.761469 0.055 Uiso 1 1 calc R U . . .
H10C H 0.662876 0.700710 0.896728 0.055 Uiso 1 1 calc R U . . .
C11 C 0.6532(3) 0.6211(3) 0.4961(2) 0.0213(5) Uani 1 1 d . . . . .
H11 H 0.585643 0.613314 0.569319 0.026 Uiso 1 1 calc R U . . .
C12 C 0.6731(4) 0.7593(3) 0.4949(3) 0.0261(6) Uani 1 1 d . . . . .
H12A H 0.565416 0.839476 0.500926 0.039 Uiso 1 1 calc R U . . .
H12B H 0.737845 0.770787 0.423541 0.039 Uiso 1 1 calc R U . . .
H12C H 0.728722 0.756337 0.559401 0.039 Uiso 1 1 calc R U . . .
C13 C 0.5631(4) 0.6210(4) 0.3994(3) 0.0282(6) Uani 1 1 d . . . . .
H13A H 0.448299 0.687677 0.414197 0.042 Uiso 1 1 calc R U . . .
H13B H 0.570403 0.525267 0.394337 0.042 Uiso 1 1 calc R U . . .
H13C H 0.612607 0.649811 0.327457 0.042 Uiso 1 1 calc R U . . .
O1 O 0.6041(5) 1.0483(6) 0.9297(3) 0.0777(13) Uani 1 1 d . . . . .
O2 O 0.6035(4) 1.0084(3) 0.7055(3) 0.0454(7) Uani 1 1 d . . . . .
O3 O 0.3052(4) 0.9675(4) 0.7046(3) 0.0541(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 2.010(3) . ?
Pd1 C1 2.019(3) . ?
Pd1 S1 2.3514(7) . ?
Pd1 S1 2.3566(7) 2_766 ?
S1 C11 1.843(3) . ?
N1 C1 1.352(4) . ?
N1 C2 1.372(4) . ?
N1 C4 1.469(4) . ?
N2 C1 1.342(4) . ?
N2 N3 1.376(3) . ?
N2 C5 1.447(4) . ?
N3 C2 1.316(5) . ?
N4 C6 1.347(4) . ?
N4 C7 1.367(4) . ?
N4 C9 1.454(4) . ?
N5 C6 1.337(4) . ?
N5 N6 1.376(4) . ?
N5 C10 1.461(5) . ?
C2 H2 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
N6 C7 1.310(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C7 H7 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.524(4) . ?
C11 C12 1.526(4) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 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
C6 Pd1 C1 92.04(11) . . ?
C6 Pd1 S1 89.31(8) . . ?
C1 Pd1 S1 178.39(8) . . ?
C6 Pd1 S1 174.04(7) . 2_766 ?
C1 Pd1 S1 93.36(8) . 2_766 ?
S1 Pd1 S1 85.25(2) . 2_766 ?
C11 S1 Pd1 103.70(9) . . ?
C11 S1 Pd1 107.37(9) . 2_766 ?
Pd1 S1 Pd1 94.75(2) . 2_766 ?
C1 N1 C2 109.0(3) . . ?
C1 N1 C4 126.8(3) . . ?
C2 N1 C4 124.1(3) . . ?
C1 N2 N3 112.8(3) . . ?
C1 N2 C5 127.6(2) . . ?
N3 N2 C5 119.5(2) . . ?
C2 N3 N2 104.1(3) . . ?
C6 N4 C7 109.9(3) . . ?
C6 N4 C9 127.0(3) . . ?
C7 N4 C9 123.0(3) . . ?
C6 N5 N6 112.0(3) . . ?
C6 N5 C10 127.3(3) . . ?
N6 N5 C10 120.7(3) . . ?
N2 C1 N1 104.0(2) . . ?
N2 C1 Pd1 128.9(2) . . ?
N1 C1 Pd1 127.1(2) . . ?
N3 C2 N1 110.1(3) . . ?
N3 C2 H2 124.9 . . ?
N1 C2 H2 124.9 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N5 C6 N4 103.9(2) . . ?
N5 C6 Pd1 128.4(2) . . ?
N4 C6 Pd1 127.4(2) . . ?
C7 N6 N5 105.3(3) . . ?
N4 C9 H9A 109.5 . . ?
N4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N6 C7 N4 108.8(3) . . ?
N6 C7 H7 125.6 . . ?
N4 C7 H7 125.6 . . ?
N5 C10 H10A 109.5 . . ?
N5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C12 112.0(3) . . ?
C13 C11 S1 109.9(2) . . ?
C12 C11 S1 112.43(19) . . ?
C13 C11 H11 107.4 . . ?
C12 C11 H11 107.4 . . ?
S1 C11 H11 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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
C1 N2 N3 C2 0.1(3) . . . . ?
C5 N2 N3 C2 177.5(3) . . . . ?
N3 N2 C1 N1 -0.5(3) . . . . ?
C5 N2 C1 N1 -177.5(3) . . . . ?
N3 N2 C1 Pd1 179.1(2) . . . . ?
C5 N2 C1 Pd1 2.0(4) . . . . ?
C2 N1 C1 N2 0.6(3) . . . . ?
C4 N1 C1 N2 179.5(3) . . . . ?
C2 N1 C1 Pd1 -178.9(2) . . . . ?
C4 N1 C1 Pd1 -0.1(4) . . . . ?
N2 N3 C2 N1 0.3(3) . . . . ?
C1 N1 C2 N3 -0.6(4) . . . . ?
C4 N1 C2 N3 -179.5(3) . . . . ?
N6 N5 C6 N4 -1.0(3) . . . . ?
C10 N5 C6 N4 179.4(3) . . . . ?
N6 N5 C6 Pd1 173.3(2) . . . . ?
C10 N5 C6 Pd1 -6.3(4) . . . . ?
C7 N4 C6 N5 0.4(3) . . . . ?
C9 N4 C6 N5 -180.0(3) . . . . ?
C7 N4 C6 Pd1 -174.0(2) . . . . ?
C9 N4 C6 Pd1 5.6(4) . . . . ?
C6 N5 N6 C7 1.2(4) . . . . ?
C10 N5 N6 C7 -179.2(3) . . . . ?
N5 N6 C7 N4 -0.9(4) . . . . ?
C6 N4 C7 N6 0.3(4) . . . . ?
C9 N4 C7 N6 -179.3(3) . . . . ?
Pd1 S1 C11 C13 -179.78(18) . . . . ?
Pd1 S1 C11 C13 80.7(2) 2_766 . . . ?
Pd1 S1 C11 C12 54.8(2) . . . . ?
Pd1 S1 C11 C12 -44.7(2) 2_766 . . . ?

_refine_diff_density_max         1.889
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.132

# start Validation Reply Form
_vrf_PLAT306_K291                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 Check
RESPONSE: H atoms could not be located.
;
_vrf_PLAT430_K291                
;
PROBLEM: Short Inter D...A Contact O1 ..O2 . 2.75 Ang.
RESPONSE: H-bond distance.
;
# end Validation Reply Form



####################################################################### 
# 
# 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_K225
_database_code_depnum_ccdc_archive 'CCDC 2119519'
loop_
_audit_author_name
_audit_author_address
'Geok Kheng Tan '
;Department of Chemistry, National University of Singapore
Singapore
;
_audit_update_record             
;
2021-11-01 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H46 Cl1.50 I0.50 N8 O1.75 Pd2 S2'
_chemical_formula_weight         892.25

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'
Cl Cl 0.1484 0.1585 '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'
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'
S S 0.1246 0.1234 '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'

_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                   23.4302(5)
_cell_length_b                   17.5754(5)
_cell_length_c                   9.5225(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.8600(10)
_cell_angle_gamma                90
_cell_volume                     3884.48(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9793
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      29.62

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.207
_exptl_absorpt_coefficient_mu    1.566
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6594
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Microfocus Sealed Tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43348
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.501
_diffrn_reflns_theta_max         29.627
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10825
_reflns_number_gt                9356
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0420P)²+9.8290P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10825
_refine_ls_number_parameters     443
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0992
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_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 -0.32138(2) 0.45813(2) -0.54162(2) 0.01310(5) Uani 1 1 d . . . . .
Pd2 Pd -0.17574(2) 0.46045(2) -0.45023(2) 0.01229(5) Uani 1 1 d . . . . .
S1 S -0.24120(2) 0.42017(4) -0.64766(6) 0.01645(12) Uani 1 1 d . . . . .
S2 S -0.25654(3) 0.45126(4) -0.32936(6) 0.01591(12) Uani 1 1 d . . . . .
N1 N -0.39122(9) 0.42052(13) -0.8263(2) 0.0168(4) Uani 1 1 d . . . . .
N2 N -0.39170(10) 0.54069(12) -0.7853(2) 0.0189(4) Uani 1 1 d . . . . .
N3 N -0.43289(9) 0.43578(14) -0.4219(2) 0.0202(4) Uani 1 1 d . . . . .
N4 N -0.39582(10) 0.54407(14) -0.3571(2) 0.0221(5) Uani 1 1 d . . . . .
N5 N -0.08191(10) 0.54240(14) -0.5820(3) 0.0226(5) Uani 1 1 d . . . . .
N6 N -0.07750(9) 0.42220(13) -0.6176(2) 0.0189(4) Uani 1 1 d . . . . .
N7 N -0.09152(9) 0.42650(12) -0.1906(2) 0.0163(4) Uani 1 1 d . . . . .
N8 N -0.12329(9) 0.54060(12) -0.1789(2) 0.0168(4) Uani 1 1 d . . . . .
C1 C -0.37217(10) 0.47365(14) -0.7279(3) 0.0155(4) Uani 1 1 d . . . . .
C2 C -0.42210(12) 0.45421(16) -0.9449(3) 0.0235(5) Uani 1 1 d . . . . .
H2 H -0.439735 0.429059 -1.028000 0.028 Uiso 1 1 calc R U . . .
C3 C -0.42215(12) 0.52974(17) -0.9190(3) 0.0244(6) Uani 1 1 d . . . . .
H3 H -0.439727 0.568059 -0.980769 0.029 Uiso 1 1 calc R U . . .
C4 C -0.38072(12) 0.33884(15) -0.8140(3) 0.0217(5) Uani 1 1 d . . . . .
H4A H -0.414993 0.313454 -0.787952 0.033 Uiso 1 1 calc R U . . .
H4B H -0.347839 0.329281 -0.740874 0.033 Uiso 1 1 calc R U . . .
H4C H -0.372262 0.318909 -0.905083 0.033 Uiso 1 1 calc R U . . .
C5 C -0.38171(13) 0.61532(16) -0.7188(3) 0.0271(6) Uani 1 1 d . . . . .
H5A H -0.343141 0.616638 -0.664053 0.041 Uiso 1 1 calc R U . . .
H5B H -0.410620 0.624643 -0.655549 0.041 Uiso 1 1 calc R U . . .
H5C H -0.384673 0.654716 -0.792294 0.041 Uiso 1 1 calc R U . . .
C6 C -0.38769(11) 0.48201(15) -0.4352(3) 0.0168(4) Uani 1 1 d . . . . .
C7 C -0.44593(13) 0.53688(19) -0.2958(3) 0.0283(6) Uani 1 1 d . . . . .
H7 H -0.460994 0.573057 -0.236433 0.034 Uiso 1 1 calc R U . . .
C8 C -0.46905(13) 0.46942(19) -0.3359(3) 0.0274(6) Uani 1 1 d . . . . .
H8A H -0.503591 0.448518 -0.310446 0.033 Uiso 1 1 calc R U . . .
C9 C -0.35644(15) 0.60830(19) -0.3319(4) 0.0334(7) Uani 1 1 d . . . . .
H9A H -0.339545 0.609056 -0.231864 0.050 Uiso 1 1 calc R U . . .
H9B H -0.377574 0.655768 -0.355199 0.050 Uiso 1 1 calc R U . . .
H9C H -0.325726 0.603288 -0.391518 0.050 Uiso 1 1 calc R U . . .
C10 C -0.44316(12) 0.36138(17) -0.4882(3) 0.0257(6) Uani 1 1 d . . . . .
H10A H -0.462919 0.328581 -0.426977 0.039 Uiso 1 1 calc R U . . .
H10B H -0.406267 0.338277 -0.502020 0.039 Uiso 1 1 calc R U . . .
H10C H -0.467198 0.367253 -0.580207 0.039 Uiso 1 1 calc R U . . .
C11 C -0.10733(10) 0.47597(15) -0.5553(3) 0.0158(4) Uani 1 1 d . . . . .
C12 C -0.03744(13) 0.5307(2) -0.6612(3) 0.0288(6) Uani 1 1 d . . . . .
H12 H -0.013603 0.568773 -0.693743 0.035 Uiso 1 1 calc R U . . .
C13 C -0.03429(12) 0.45563(18) -0.6833(3) 0.0251(6) Uani 1 1 d . . . . .
H13 H -0.007721 0.430191 -0.733968 0.030 Uiso 1 1 calc R U . . .
C14 C -0.09814(16) 0.61703(18) -0.5328(4) 0.0357(7) Uani 1 1 d . . . . .
H14A H -0.072857 0.630417 -0.445696 0.054 Uiso 1 1 calc R U . . .
H14B H -0.138191 0.615566 -0.513868 0.054 Uiso 1 1 calc R U . . .
H14C H -0.094254 0.655196 -0.605971 0.054 Uiso 1 1 calc R U . . .
C15 C -0.08992(14) 0.34088(17) -0.6229(3) 0.0273(6) Uani 1 1 d . . . . .
H15A H -0.128142 0.331934 -0.595228 0.041 Uiso 1 1 calc R U . . .
H15B H -0.060836 0.313948 -0.557466 0.041 Uiso 1 1 calc R U . . .
H15C H -0.089140 0.322092 -0.719496 0.041 Uiso 1 1 calc R U . . .
C16 C -0.12664(10) 0.47869(14) -0.2636(2) 0.0142(4) Uani 1 1 d . . . . .
C17 C -0.06608(11) 0.45589(15) -0.0620(3) 0.0203(5) Uani 1 1 d . . . . .
H17 H -0.039884 0.430501 0.007427 0.024 Uiso 1 1 calc R U . . .
C18 C -0.08595(12) 0.52801(16) -0.0551(3) 0.0206(5) Uani 1 1 d . . . . .
H18 H -0.076183 0.563165 0.020175 0.025 Uiso 1 1 calc R U . . .
C19 C -0.08396(12) 0.34819(15) -0.2345(3) 0.0231(5) Uani 1 1 d . . . . .
H19A H -0.121131 0.321773 -0.244165 0.035 Uiso 1 1 calc R U . . .
H19B H -0.056624 0.322291 -0.163117 0.035 Uiso 1 1 calc R U . . .
H19C H -0.069054 0.347806 -0.325754 0.035 Uiso 1 1 calc R U . . .
C20 C -0.15648(12) 0.61029(15) -0.2068(3) 0.0233(5) Uani 1 1 d . . . . .
H20A H -0.130189 0.653184 -0.212735 0.035 Uiso 1 1 calc R U . . .
H20B H -0.179476 0.619256 -0.129868 0.035 Uiso 1 1 calc R U . . .
H20C H -0.182124 0.605346 -0.296719 0.035 Uiso 1 1 calc R U . . .
C21 C -0.23958(12) 0.47016(18) -0.8174(3) 0.0250(6) Uani 1 1 d . . . . .
H21 H -0.278293 0.462911 -0.874509 0.030 Uiso 1 1 calc R U . . .
C22 C -0.23013(15) 0.5553(2) -0.8009(4) 0.0349(7) Uani 1 1 d . . . . .
H22A H -0.191378 0.564975 -0.751119 0.052 Uiso 1 1 calc R U . . .
H22B H -0.258803 0.576756 -0.746189 0.052 Uiso 1 1 calc R U . . .
H22C H -0.234121 0.579167 -0.894743 0.052 Uiso 1 1 calc R U . . .
C23 C -0.19584(13) 0.4329(2) -0.8995(3) 0.0320(7) Uani 1 1 d . . . . .
H23A H -0.203104 0.378040 -0.906107 0.048 Uiso 1 1 calc R U . . .
H23B H -0.156896 0.442017 -0.850369 0.048 Uiso 1 1 calc R U . . .
H23C H -0.199317 0.454701 -0.995046 0.048 Uiso 1 1 calc R U . . .
C24 C -0.25697(11) 0.35469(16) -0.2545(3) 0.0205(5) Uani 1 1 d . . . . .
H24 H -0.221736 0.349443 -0.182970 0.025 Uiso 1 1 calc R U . . .
C25 C -0.25514(14) 0.29191(17) -0.3638(3) 0.0275(6) Uani 1 1 d . . . . .
H25A H -0.252245 0.242395 -0.315989 0.041 Uiso 1 1 calc R U . . .
H25B H -0.221612 0.299341 -0.413489 0.041 Uiso 1 1 calc R U . . .
H25C H -0.290398 0.293556 -0.432168 0.041 Uiso 1 1 calc R U . . .
C26 C -0.30937(13) 0.34754(19) -0.1755(3) 0.0283(6) Uani 1 1 d . . . . .
H26A H -0.309625 0.389900 -0.108674 0.042 Uiso 1 1 calc R U . . .
H26B H -0.307378 0.299286 -0.123523 0.042 Uiso 1 1 calc R U . . .
H26C H -0.344679 0.348869 -0.243792 0.042 Uiso 1 1 calc R U . . .
I1 I -0.45786(5) 0.70800(6) -0.10900(11) 0.0500(3) Uani 0.25 1 d . . P . .
I2 I 0.00851(3) 0.29294(4) 0.12408(8) 0.02427(14) Uani 0.25 1 d . . P . .
Cl1 Cl -0.07647(13) 0.69658(16) 0.1330(3) 0.0705(7) Uani 0.5 1 d . . P . .
Cl2 Cl -0.52197(9) 0.80143(12) -0.3483(2) 0.0479(4) Uani 0.5 1 d . . P . .
Cl3 Cl -0.2787(4) 0.7546(5) -0.7274(9) 0.0705(7) Uani 0.25 1 d . . P A 1
Cl4 Cl -0.2590(2) 0.7563(3) -0.2173(8) 0.0575(15) Uani 0.25 1 d . . P . .
O1 O -0.3200(4) 0.7240(5) -0.0179(9) 0.067(2) Uani 0.5 1 d . U P B 1
O2 O -0.3416(6) 0.7089(8) -0.0085(14) 0.045(3) Uani 0.25 1 d . U P C 2
O3 O -0.2152(6) 0.7318(8) -0.5169(14) 0.0359(14) Uani 0.187(5) 1 d . U P D 1
O4 O -0.1908(3) 0.7525(5) -0.4362(8) 0.0359(14) Uani 0.313(5) 1 d . U P D 3
O5 O -0.2743(4) 0.7530(6) -0.6014(11) 0.099(3) Uani 0.5 1 d . U P E 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 2.012(2) . ?
Pd1 C1 2.015(2) . ?
Pd1 S1 2.3480(6) . ?
Pd1 S2 2.3597(6) . ?
Pd2 C16 2.007(2) . ?
Pd2 C11 2.021(2) . ?
Pd2 S2 2.3518(6) . ?
Pd2 S1 2.3663(6) . ?
S1 C21 1.844(3) . ?
S2 C24 1.841(3) . ?
N1 C1 1.355(3) . ?
N1 C2 1.388(3) . ?
N1 C4 1.458(3) . ?
N2 C1 1.352(3) . ?
N2 C3 1.385(3) . ?
N2 C5 1.461(4) . ?
N3 C6 1.354(3) . ?
N3 C8 1.388(4) . ?
N3 C10 1.458(4) . ?
N4 C6 1.348(3) . ?
N4 C7 1.387(4) . ?
N4 C9 1.457(4) . ?
N5 C11 1.351(3) . ?
N5 C12 1.382(4) . ?
N5 C14 1.460(4) . ?
N6 C11 1.359(3) . ?
N6 C13 1.391(4) . ?
N6 C15 1.458(4) . ?
N7 C16 1.358(3) . ?
N7 C17 1.386(3) . ?
N7 C19 1.456(3) . ?
N8 C16 1.350(3) . ?
N8 C18 1.387(3) . ?
N8 C20 1.456(3) . ?
C2 C3 1.350(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 C8 1.337(5) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 C13 1.340(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 C18 1.355(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.518(5) . ?
C21 C23 1.520(4) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.521(4) . ?
C24 C26 1.530(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
Cl3 Cl4 0.497(9) 4_575 ?
Cl4 O5 1.217(12) 4_576 ?
Cl4 O3 2.050(15) 4_576 ?

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
C6 Pd1 C1 90.66(10) . . ?
C6 Pd1 S1 173.89(7) . . ?
C1 Pd1 S1 94.06(7) . . ?
C6 Pd1 S2 91.73(7) . . ?
C1 Pd1 S2 174.03(7) . . ?
S1 Pd1 S2 83.95(2) . . ?
C16 Pd2 C11 91.13(9) . . ?
C16 Pd2 S2 88.84(7) . . ?
C11 Pd2 S2 176.14(8) . . ?
C16 Pd2 S1 169.23(7) . . ?
C11 Pd2 S1 96.82(7) . . ?
S2 Pd2 S1 83.72(2) . . ?
C21 S1 Pd1 110.79(10) . . ?
C21 S1 Pd2 117.70(9) . . ?
Pd1 S1 Pd2 92.47(2) . . ?
C24 S2 Pd2 107.47(9) . . ?
C24 S2 Pd1 109.99(8) . . ?
Pd2 S2 Pd1 92.54(2) . . ?
C1 N1 C2 110.8(2) . . ?
C1 N1 C4 125.9(2) . . ?
C2 N1 C4 123.3(2) . . ?
C1 N2 C3 110.7(2) . . ?
C1 N2 C5 125.5(2) . . ?
C3 N2 C5 123.7(2) . . ?
C6 N3 C8 110.3(2) . . ?
C6 N3 C10 125.6(2) . . ?
C8 N3 C10 124.0(2) . . ?
C6 N4 C7 110.5(2) . . ?
C6 N4 C9 125.7(2) . . ?
C7 N4 C9 123.7(3) . . ?
C11 N5 C12 111.0(2) . . ?
C11 N5 C14 125.1(2) . . ?
C12 N5 C14 123.8(2) . . ?
C11 N6 C13 110.6(2) . . ?
C11 N6 C15 125.8(2) . . ?
C13 N6 C15 123.5(2) . . ?
C16 N7 C17 110.9(2) . . ?
C16 N7 C19 125.5(2) . . ?
C17 N7 C19 123.5(2) . . ?
C16 N8 C18 110.9(2) . . ?
C16 N8 C20 125.7(2) . . ?
C18 N8 C20 123.3(2) . . ?
N2 C1 N1 105.0(2) . . ?
N2 C1 Pd1 126.92(19) . . ?
N1 C1 Pd1 127.95(18) . . ?
C3 C2 N1 106.5(2) . . ?
C3 C2 H2 126.7 . . ?
N1 C2 H2 126.7 . . ?
C2 C3 N2 106.9(2) . . ?
C2 C3 H3 126.5 . . ?
N2 C3 H3 126.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 N3 105.2(2) . . ?
N4 C6 Pd1 128.6(2) . . ?
N3 C6 Pd1 126.11(19) . . ?
C8 C7 N4 107.1(3) . . ?
C8 C7 H7 126.5 . . ?
N4 C7 H7 126.5 . . ?
C7 C8 N3 106.9(3) . . ?
C7 C8 H8A 126.6 . . ?
N3 C8 H8A 126.6 . . ?
N4 C9 H9A 109.5 . . ?
N4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 N6 104.6(2) . . ?
N5 C11 Pd2 127.58(19) . . ?
N6 C11 Pd2 127.76(19) . . ?
C13 C12 N5 107.1(3) . . ?
C13 C12 H12 126.5 . . ?
N5 C12 H12 126.5 . . ?
C12 C13 N6 106.6(2) . . ?
C12 C13 H13 126.7 . . ?
N6 C13 H13 126.7 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N8 C16 N7 104.9(2) . . ?
N8 C16 Pd2 129.57(18) . . ?
N7 C16 Pd2 125.40(18) . . ?
C18 C17 N7 106.4(2) . . ?
C18 C17 H17 126.8 . . ?
N7 C17 H17 126.8 . . ?
C17 C18 N8 106.8(2) . . ?
C17 C18 H18 126.6 . . ?
N8 C18 H18 126.6 . . ?
N7 C19 H19A 109.5 . . ?
N7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N8 C20 H20A 109.5 . . ?
N8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C23 112.2(3) . . ?
C22 C21 S1 113.5(2) . . ?
C23 C21 S1 110.0(2) . . ?
C22 C21 H21 106.9 . . ?
C23 C21 H21 106.9 . . ?
S1 C21 H21 106.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C26 112.1(2) . . ?
C25 C24 S2 113.67(18) . . ?
C26 C24 S2 108.3(2) . . ?
C25 C24 H24 107.5 . . ?
C26 C24 H24 107.5 . . ?
S2 C24 H24 107.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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
C3 N2 C1 N1 -0.6(3) . . . . ?
C5 N2 C1 N1 -179.5(2) . . . . ?
C3 N2 C1 Pd1 175.76(19) . . . . ?
C5 N2 C1 Pd1 -3.2(4) . . . . ?
C2 N1 C1 N2 0.4(3) . . . . ?
C4 N1 C1 N2 179.4(2) . . . . ?
C2 N1 C1 Pd1 -175.91(19) . . . . ?
C4 N1 C1 Pd1 3.1(4) . . . . ?
C1 N1 C2 C3 -0.1(3) . . . . ?
C4 N1 C2 C3 -179.1(3) . . . . ?
N1 C2 C3 N2 -0.3(3) . . . . ?
C1 N2 C3 C2 0.6(3) . . . . ?
C5 N2 C3 C2 179.5(3) . . . . ?
C7 N4 C6 N3 -0.2(3) . . . . ?
C9 N4 C6 N3 176.3(3) . . . . ?
C7 N4 C6 Pd1 -177.26(19) . . . . ?
C9 N4 C6 Pd1 -0.8(4) . . . . ?
C8 N3 C6 N4 0.2(3) . . . . ?
C10 N3 C6 N4 179.8(2) . . . . ?
C8 N3 C6 Pd1 177.29(19) . . . . ?
C10 N3 C6 Pd1 -3.1(4) . . . . ?
C6 N4 C7 C8 0.2(3) . . . . ?
C9 N4 C7 C8 -176.4(3) . . . . ?
N4 C7 C8 N3 -0.1(3) . . . . ?
C6 N3 C8 C7 -0.1(3) . . . . ?
C10 N3 C8 C7 -179.7(3) . . . . ?
C12 N5 C11 N6 0.8(3) . . . . ?
C14 N5 C11 N6 -178.4(3) . . . . ?
C12 N5 C11 Pd2 -177.9(2) . . . . ?
C14 N5 C11 Pd2 2.9(4) . . . . ?
C13 N6 C11 N5 -0.5(3) . . . . ?
C15 N6 C11 N5 -177.6(2) . . . . ?
C13 N6 C11 Pd2 178.14(18) . . . . ?
C15 N6 C11 Pd2 1.1(4) . . . . ?
C11 N5 C12 C13 -0.8(3) . . . . ?
C14 N5 C12 C13 178.4(3) . . . . ?
N5 C12 C13 N6 0.4(3) . . . . ?
C11 N6 C13 C12 0.1(3) . . . . ?
C15 N6 C13 C12 177.2(3) . . . . ?
C18 N8 C16 N7 0.8(3) . . . . ?
C20 N8 C16 N7 -175.6(2) . . . . ?
C18 N8 C16 Pd2 176.74(19) . . . . ?
C20 N8 C16 Pd2 0.3(4) . . . . ?
C17 N7 C16 N8 -0.6(3) . . . . ?
C19 N7 C16 N8 175.5(2) . . . . ?
C17 N7 C16 Pd2 -176.70(18) . . . . ?
C19 N7 C16 Pd2 -0.7(4) . . . . ?
C16 N7 C17 C18 0.1(3) . . . . ?
C19 N7 C17 C18 -176.0(2) . . . . ?
N7 C17 C18 N8 0.4(3) . . . . ?
C16 N8 C18 C17 -0.8(3) . . . . ?
C20 N8 C18 C17 175.8(2) . . . . ?
Pd1 S1 C21 C22 65.7(2) . . . . ?
Pd2 S1 C21 C22 -38.8(2) . . . . ?
Pd1 S1 C21 C23 -167.55(18) . . . . ?
Pd2 S1 C21 C23 87.9(2) . . . . ?
Pd2 S2 C24 C25 -54.7(2) . . . . ?
Pd1 S2 C24 C25 44.8(2) . . . . ?
Pd2 S2 C24 C26 -179.90(16) . . . . ?
Pd1 S2 C24 C26 -80.46(18) . . . . ?

_refine_diff_density_max         1.404
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.116



####################################################################### 
# 
# 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_J187
_database_code_depnum_ccdc_archive 'CCDC 2119522'
loop_
_audit_author_name
_audit_author_address
'Geok Kheng Tan '
;Department of Chemistry, National University of Singapore
Singapore
;
_audit_update_record             
;
2021-11-01 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H26 Br2 N4 Pd'
_chemical_formula_weight         564.65

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'
Br Br -0.2901 2.4595 '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'

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

_cell_length_a                   9.0107(6)
_cell_length_b                   16.9043(11)
_cell_length_c                   29.042(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4423.7(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9881
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.29

_exptl_crystal_description       Plate
_exptl_crystal_colour            Pale_Yellow
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_F_000             2224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.102
_exptl_absorpt_coefficient_mu    4.460
_shelx_estimated_absorpt_T_min   0.375
_shelx_estimated_absorpt_T_max   0.659
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5106
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Microfocus Sealed Tube'
_diffrn_measurement_device_type  'Bruker D8 venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            90883
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.656
_diffrn_reflns_theta_max         28.290
_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             5487
_reflns_number_gt                4356
_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_bruker_data_scaling   'SADABS V2018/1 (Bruker AXS Inc.)'
_computing_cell_refinement       'APEX3 v2018.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL--2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT--(Sheldrick 2015)'
_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)+(0.0928P)²+57.1669P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Intrisinic Phasing'
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5487
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0775
_refine_ls_wR_factor_ref         0.2204
_refine_ls_wR_factor_gt          0.2051
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.56003(6) 0.31892(3) 0.39645(2) 0.0336(2) Uani 1 1 d . . . . .
Br1 Br 0.34887(13) 0.26003(7) 0.35811(5) 0.0676(4) Uani 1 1 d . . . . .
Br2 Br 0.76003(10) 0.38560(5) 0.43793(4) 0.0470(3) Uani 1 1 d . . . . .
N1 N 0.4524(6) 0.4792(4) 0.3633(2) 0.0285(13) Uani 1 1 d . . . . .
N2 N 0.6279(7) 0.4323(4) 0.3195(3) 0.0361(15) Uani 1 1 d . . . . .
N3 N 0.5520(10) 0.2130(4) 0.4814(3) 0.054(2) Uani 1 1 d . . . . .
N4 N 0.6421(8) 0.1501(4) 0.4243(3) 0.0388(16) Uani 1 1 d . . . . .
C1 C 0.5423(7) 0.4154(5) 0.3567(3) 0.0325(16) Uani 1 1 d . . . . .
C2 C 0.4769(8) 0.5368(5) 0.3305(3) 0.0329(16) Uani 1 1 d . . . . .
C3 C 0.4176(9) 0.6105(5) 0.3231(4) 0.045(2) Uani 1 1 d . . . . .
H3 H 0.342017 0.631071 0.342480 0.054 Uiso 1 1 calc R U . . .
C4 C 0.4723(11) 0.6537(6) 0.2862(4) 0.055(3) Uani 1 1 d . . . . .
H4 H 0.432579 0.704712 0.280121 0.066 Uiso 1 1 calc R U . . .
C5 C 0.5861(12) 0.6236(7) 0.2573(4) 0.057(3) Uani 1 1 d . . . . .
H5 H 0.621546 0.654661 0.232317 0.068 Uiso 1 1 calc R U . . .
C6 C 0.6451(11) 0.5504(6) 0.2650(3) 0.048(2) Uani 1 1 d . . . . .
H6 H 0.721408 0.529812 0.245821 0.057 Uiso 1 1 calc R U . . .
C7 C 0.5896(9) 0.5070(5) 0.3018(3) 0.0353(17) Uani 1 1 d . . . . .
C8 C 0.3471(9) 0.4834(6) 0.4027(3) 0.042(2) Uani 1 1 d . . . . .
H8 H 0.355003 0.432640 0.420233 0.051 Uiso 1 1 calc R U . . .
C9 C 0.3903(15) 0.5490(8) 0.4344(4) 0.067(3) Uani 1 1 d . . . . .
H9A H 0.493511 0.541748 0.444212 0.101 Uiso 1 1 calc R U . . .
H9B H 0.325366 0.548525 0.461511 0.101 Uiso 1 1 calc R U . . .
H9C H 0.380380 0.599741 0.418425 0.101 Uiso 1 1 calc R U . . .
C10 C 0.1868(10) 0.4903(7) 0.3847(5) 0.063(3) Uani 1 1 d . . . . .
H10A H 0.173588 0.541566 0.369530 0.095 Uiso 1 1 calc R U . . .
H10B H 0.117309 0.485858 0.410519 0.095 Uiso 1 1 calc R U . . .
H10C H 0.167581 0.447711 0.362559 0.095 Uiso 1 1 calc R U . . .
C11 C 0.7497(11) 0.3799(6) 0.3051(4) 0.054(2) Uani 1 1 d . . . . .
H11 H 0.745101 0.332653 0.325780 0.065 Uiso 1 1 calc R U . . .
C12 C 0.7327(14) 0.3498(8) 0.2575(5) 0.070(3) Uani 1 1 d . . . . .
H12A H 0.714185 0.394162 0.236566 0.106 Uiso 1 1 calc R U . . .
H12B H 0.648935 0.312864 0.256249 0.106 Uiso 1 1 calc R U . . .
H12C H 0.823726 0.322373 0.248199 0.106 Uiso 1 1 calc R U . . .
C13 C 0.9008(11) 0.4181(7) 0.3135(5) 0.061(3) Uani 1 1 d . . . . .
H13A H 0.978470 0.377644 0.311694 0.092 Uiso 1 1 calc R U . . .
H13B H 0.902189 0.442566 0.344071 0.092 Uiso 1 1 calc R U . . .
H13C H 0.918839 0.458670 0.290017 0.092 Uiso 1 1 calc R U . . .
C14 C 0.5847(9) 0.2208(4) 0.4371(3) 0.0388(19) Uani 1 1 d . . . . .
C15 C 0.487(2) 0.2743(6) 0.5107(5) 0.092(6) Uani 1 1 d . . . . .
H15A H 0.528949 0.325833 0.502274 0.138 Uiso 1 1 calc R U . . .
H15B H 0.509955 0.262825 0.542976 0.138 Uiso 1 1 calc R U . . .
H15C H 0.379400 0.275242 0.506324 0.138 Uiso 1 1 calc R U . . .
C16 C 0.5876(14) 0.1374(6) 0.4969(4) 0.061(3) Uani 1 1 d . . . . .
H16 H 0.574177 0.116990 0.527105 0.073 Uiso 1 1 calc R U . . .
C17 C 0.6442(10) 0.0996(5) 0.4608(4) 0.051(3) Uani 1 1 d . . . . .
H17 H 0.679798 0.046685 0.460568 0.061 Uiso 1 1 calc R U . . .
C18 C 0.6927(14) 0.1313(6) 0.3785(4) 0.060(3) Uani 1 1 d . . . . .
H18A H 0.621098 0.151147 0.355927 0.089 Uiso 1 1 calc R U . . .
H18B H 0.702043 0.073764 0.375342 0.089 Uiso 1 1 calc R U . . .
H18C H 0.789501 0.156078 0.373196 0.089 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 2.005(9) . ?
Pd1 C14 2.047(8) . ?
Pd1 Br1 2.4189(12) . ?
Pd1 Br2 2.4432(11) . ?
N1 C1 1.362(9) . ?
N1 C2 1.382(10) . ?
N1 C8 1.488(10) . ?
N2 C1 1.356(11) . ?
N2 C7 1.405(11) . ?
N2 C11 1.470(11) . ?
N3 C14 1.328(12) . ?
N3 C16 1.392(13) . ?
N3 C15 1.460(13) . ?
N4 C14 1.355(10) . ?
N4 C17 1.363(12) . ?
N4 C18 1.440(13) . ?
C2 C3 1.372(12) . ?
C2 C7 1.406(11) . ?
C3 C4 1.387(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.420(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.365(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(13) . ?
C6 H6 0.9500 . ?
C8 C9 1.493(15) . ?
C8 C10 1.540(13) . ?
C8 H8 1.0000 . ?
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 C12 1.483(16) . ?
C11 C13 1.526(14) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.329(15) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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 C14 178.3(3) . . ?
C1 Pd1 Br1 90.4(2) . . ?
C14 Pd1 Br1 91.0(3) . . ?
C1 Pd1 Br2 88.1(2) . . ?
C14 Pd1 Br2 90.5(3) . . ?
Br1 Pd1 Br2 175.58(5) . . ?
C1 N1 C2 111.4(6) . . ?
C1 N1 C8 121.8(7) . . ?
C2 N1 C8 126.8(7) . . ?
C1 N2 C7 109.9(7) . . ?
C1 N2 C11 121.6(8) . . ?
C7 N2 C11 128.3(8) . . ?
C14 N3 C16 110.7(8) . . ?
C14 N3 C15 125.6(8) . . ?
C16 N3 C15 123.7(9) . . ?
C14 N4 C17 110.1(8) . . ?
C14 N4 C18 124.7(8) . . ?
C17 N4 C18 125.2(7) . . ?
N2 C1 N1 106.5(7) . . ?
N2 C1 Pd1 125.8(6) . . ?
N1 C1 Pd1 127.5(6) . . ?
C3 C2 N1 133.3(8) . . ?
C3 C2 C7 121.0(8) . . ?
N1 C2 C7 105.7(7) . . ?
C2 C3 C4 117.4(9) . . ?
C2 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
C3 C4 C5 121.6(9) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C6 C5 C4 120.6(10) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 117.7(10) . . ?
C5 C6 H6 121.2 . . ?
C7 C6 H6 121.2 . . ?
C6 C7 N2 131.8(8) . . ?
C6 C7 C2 121.7(8) . . ?
N2 C7 C2 106.5(7) . . ?
C9 C8 N1 110.1(8) . . ?
C9 C8 C10 113.5(9) . . ?
N1 C8 C10 109.9(8) . . ?
C9 C8 H8 107.7 . . ?
N1 C8 H8 107.7 . . ?
C10 C8 H8 107.7 . . ?
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 . . ?
N2 C11 C12 113.3(9) . . ?
N2 C11 C13 111.5(8) . . ?
C12 C11 C13 112.7(10) . . ?
N2 C11 H11 106.3 . . ?
C12 C11 H11 106.3 . . ?
C13 C11 H11 106.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 N4 105.3(7) . . ?
N3 C14 Pd1 128.0(6) . . ?
N4 C14 Pd1 126.7(7) . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N3 106.0(9) . . ?
C17 C16 H16 127.0 . . ?
N3 C16 H16 127.0 . . ?
C16 C17 N4 107.9(8) . . ?
C16 C17 H17 126.0 . . ?
N4 C17 H17 126.0 . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
C7 N2 C1 N1 -1.3(8) . . . . ?
C11 N2 C1 N1 173.5(7) . . . . ?
C7 N2 C1 Pd1 -176.5(5) . . . . ?
C11 N2 C1 Pd1 -1.7(11) . . . . ?
C2 N1 C1 N2 1.0(8) . . . . ?
C8 N1 C1 N2 -177.2(7) . . . . ?
C2 N1 C1 Pd1 176.1(5) . . . . ?
C8 N1 C1 Pd1 -2.1(10) . . . . ?
C1 N1 C2 C3 -178.8(8) . . . . ?
C8 N1 C2 C3 -0.7(14) . . . . ?
C1 N1 C2 C7 -0.3(8) . . . . ?
C8 N1 C2 C7 177.8(7) . . . . ?
N1 C2 C3 C4 178.7(8) . . . . ?
C7 C2 C3 C4 0.5(12) . . . . ?
C2 C3 C4 C5 -0.5(14) . . . . ?
C3 C4 C5 C6 0.2(16) . . . . ?
C4 C5 C6 C7 0.1(14) . . . . ?
C5 C6 C7 N2 -178.0(9) . . . . ?
C5 C6 C7 C2 -0.1(13) . . . . ?
C1 N2 C7 C6 179.3(9) . . . . ?
C11 N2 C7 C6 4.9(15) . . . . ?
C1 N2 C7 C2 1.1(9) . . . . ?
C11 N2 C7 C2 -173.2(8) . . . . ?
C3 C2 C7 C6 -0.2(12) . . . . ?
N1 C2 C7 C6 -178.8(7) . . . . ?
C3 C2 C7 N2 178.2(7) . . . . ?
N1 C2 C7 N2 -0.5(8) . . . . ?
C1 N1 C8 C9 115.2(9) . . . . ?
C2 N1 C8 C9 -62.7(11) . . . . ?
C1 N1 C8 C10 -119.1(9) . . . . ?
C2 N1 C8 C10 62.9(11) . . . . ?
C1 N2 C11 C12 121.1(11) . . . . ?
C7 N2 C11 C12 -65.2(13) . . . . ?
C1 N2 C11 C13 -110.6(10) . . . . ?
C7 N2 C11 C13 63.2(13) . . . . ?
C16 N3 C14 N4 -0.2(11) . . . . ?
C15 N3 C14 N4 179.8(12) . . . . ?
C16 N3 C14 Pd1 -178.8(8) . . . . ?
C15 N3 C14 Pd1 1.2(16) . . . . ?
C17 N4 C14 N3 -0.1(10) . . . . ?
C18 N4 C14 N3 179.7(9) . . . . ?
C17 N4 C14 Pd1 178.5(7) . . . . ?
C18 N4 C14 Pd1 -1.7(13) . . . . ?
C14 N3 C16 C17 0.5(13) . . . . ?
C15 N3 C16 C17 -179.6(12) . . . . ?
N3 C16 C17 N4 -0.6(13) . . . . ?
C14 N4 C17 C16 0.4(12) . . . . ?
C18 N4 C17 C16 -179.4(10) . . . . ?

_refine_diff_density_max         3.738
_refine_diff_density_min         -2.182
_refine_diff_density_rms         0.200



####################################################################### 
# 
# 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_9104
_database_code_depnum_ccdc_archive 'CCDC 2119518'
loop_
_audit_author_name
_audit_author_address
'Geok Kheng Tan '
;Department of Chemistry, National University of Singapore
Singapore
;
_audit_update_record             
;
2021-11-01 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H58 Cl12 I2 N8 Pd2 S2'
_chemical_formula_weight         1679.12

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'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.1677(11)
_cell_length_b                   14.0905(14)
_cell_length_c                   20.730(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.045(2)
_cell_angle_gamma                90.00
_cell_volume                     3260.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    3701
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      22.99

_exptl_crystal_description       Rod
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    2.092
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5726
_exptl_absorpt_correction_T_max  0.8505
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21819
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7468
_reflns_number_gt                6062
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0407P)²+25.6997P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7468
_refine_ls_number_parameters     331
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0753
_refine_ls_wR_factor_ref         0.1683
_refine_ls_wR_factor_gt          0.1611
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.144
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.55292(5) 0.38311(4) 0.50014(3) 0.02511(14) Uani 1 1 d . . .
I1 I 0.10142(6) 0.41098(5) 0.77122(3) 0.0561(2) Uani 1 1 d . . .
S1 S 0.63002(15) 0.53688(12) 0.52072(9) 0.0295(4) Uani 1 1 d . . .
N1 N 0.7805(5) 0.2784(4) 0.4714(3) 0.0296(13) Uani 1 1 d . . .
N2 N 0.7835(6) 0.3242(4) 0.5707(3) 0.0338(14) Uani 1 1 d . . .
N3 N 0.4572(5) 0.1873(4) 0.5319(3) 0.0302(13) Uani 1 1 d . . .
N4 N 0.4223(5) 0.2228(4) 0.4308(3) 0.0290(13) Uani 1 1 d . . .
C1 C 0.7138(6) 0.3234(5) 0.5156(3) 0.0280(14) Uani 1 1 d . . .
C2 C 0.8911(6) 0.2523(5) 0.4979(4) 0.0302(15) Uani 1 1 d . . .
C3 C 0.9878(7) 0.2059(6) 0.4706(4) 0.0409(19) Uani 1 1 d . . .
H3 H 0.9871 0.1873 0.4270 0.049 Uiso 1 1 calc R . .
C4 C 1.0847(7) 0.1893(7) 0.5128(5) 0.053(2) Uani 1 1 d . . .
H4 H 1.1509 0.1560 0.4976 0.063 Uiso 1 1 calc R . .
C5 C 1.0882(7) 0.2200(7) 0.5771(5) 0.053(3) Uani 1 1 d . . .
H5 H 1.1576 0.2093 0.6030 0.064 Uiso 1 1 calc R . .
C6 C 0.9922(7) 0.2657(6) 0.6032(4) 0.0425(19) Uani 1 1 d . . .
H6 H 0.9938 0.2858 0.6464 0.051 Uiso 1 1 calc R . .
C7 C 0.8931(7) 0.2805(5) 0.5623(4) 0.0349(17) Uani 1 1 d . . .
C8 C 0.7451(7) 0.2630(7) 0.4041(4) 0.0423(19) Uani 1 1 d . . .
H8A H 0.6583 0.2610 0.3997 0.064 Uiso 1 1 calc R . .
H8B H 0.7780 0.2033 0.3897 0.064 Uiso 1 1 calc R . .
H8C H 0.7751 0.3144 0.3781 0.064 Uiso 1 1 calc R . .
C9 C 0.7496(8) 0.3658(6) 0.6319(4) 0.044(2) Uani 1 1 d . . .
H9A H 0.6913 0.4159 0.6238 0.066 Uiso 1 1 calc R . .
H9B H 0.8200 0.3920 0.6541 0.066 Uiso 1 1 calc R . .
H9C H 0.7148 0.3172 0.6586 0.066 Uiso 1 1 calc R . .
C10 C 0.4734(6) 0.2553(5) 0.4871(3) 0.0259(14) Uani 1 1 d . . .
C11 C 0.3940(6) 0.1117(5) 0.5050(4) 0.0329(16) Uani 1 1 d . . .
C12 C 0.3529(7) 0.0267(6) 0.5318(5) 0.044(2) Uani 1 1 d . . .
H12 H 0.3682 0.0113 0.5754 0.053 Uiso 1 1 calc R . .
C13 C 0.2885(8) -0.0332(6) 0.4905(6) 0.052(2) Uani 1 1 d . . .
H13 H 0.2580 -0.0902 0.5069 0.062 Uiso 1 1 calc R . .
C14 C 0.2675(8) -0.0115(7) 0.4252(6) 0.058(3) Uani 1 1 d . . .
H14 H 0.2242 -0.0545 0.3987 0.070 Uiso 1 1 calc R . .
C15 C 0.3094(7) 0.0727(6) 0.3984(5) 0.045(2) Uani 1 1 d . . .
H15 H 0.2952 0.0879 0.3547 0.054 Uiso 1 1 calc R . .
C16 C 0.3736(7) 0.1328(5) 0.4403(4) 0.0331(16) Uani 1 1 d . . .
C17 C 0.4928(8) 0.1931(6) 0.5999(4) 0.043(2) Uani 1 1 d . . .
H17A H 0.5683 0.1601 0.6074 0.065 Uiso 1 1 calc R . .
H17B H 0.4318 0.1640 0.6255 0.065 Uiso 1 1 calc R . .
H17C H 0.5022 0.2592 0.6123 0.065 Uiso 1 1 calc R . .
C18 C 0.4139(8) 0.2725(6) 0.3701(4) 0.0409(18) Uani 1 1 d . . .
H18A H 0.4667 0.3271 0.3718 0.061 Uiso 1 1 calc R . .
H18B H 0.3320 0.2934 0.3619 0.061 Uiso 1 1 calc R . .
H18C H 0.4372 0.2304 0.3357 0.061 Uiso 1 1 calc R . .
C19 C 0.7279(7) 0.5739(6) 0.4559(5) 0.047(2) Uani 1 1 d . . .
H19 H 0.7387 0.6434 0.4603 0.056 Uiso 1 1 calc R . .
C20 C 0.8520(8) 0.5292(7) 0.4661(6) 0.061(3) Uani 1 1 d . . .
H20A H 0.8477 0.4622 0.4557 0.092 Uiso 1 1 calc R . .
H20B H 0.8788 0.5370 0.5108 0.092 Uiso 1 1 calc R . .
H20C H 0.9081 0.5602 0.4383 0.092 Uiso 1 1 calc R . .
C21 C 0.6753(10) 0.5570(9) 0.3898(5) 0.066(3) Uani 1 1 d . . .
H21A H 0.7264 0.5853 0.3582 0.098 Uiso 1 1 calc R . .
H21B H 0.5962 0.5855 0.3861 0.098 Uiso 1 1 calc R . .
H21C H 0.6690 0.4893 0.3820 0.098 Uiso 1 1 calc R . .
C1S C 0.5518(10) 0.1302(8) 0.7812(5) 0.062(3) Uani 1 1 d . . .
H1S H 0.4969 0.0807 0.7636 0.075 Uiso 1 1 calc R . .
Cl1 Cl 0.6882(3) 0.1228(4) 0.74275(17) 0.1106(14) Uani 1 1 d . . .
Cl2 Cl 0.5751(4) 0.1122(3) 0.86465(15) 0.0936(11) Uani 1 1 d . . .
Cl3 Cl 0.4866(6) 0.2414(3) 0.76876(18) 0.138(2) Uani 1 1 d . . .
C2S C 0.0896(9) 0.0153(7) 0.7250(5) 0.055(2) Uani 1 1 d . . .
H2S H 0.1538 -0.0263 0.7432 0.066 Uiso 1 1 calc R . .
Cl4 Cl 0.1266(4) 0.1339(2) 0.74153(14) 0.0822(10) Uani 1 1 d . . .
Cl5 Cl -0.0450(3) -0.0117(3) 0.7617(2) 0.1011(12) Uani 1 1 d . . .
Cl6 Cl 0.0734(3) -0.0046(2) 0.64096(14) 0.0800(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.999(7) . ?
Pd1 C10 2.022(7) . ?
Pd1 S1 2.3599(18) 3_666 ?
Pd1 S1 2.3647(18) . ?
S1 C19 1.838(9) . ?
S1 Pd1 2.3599(18) 3_666 ?
N1 C1 1.359(9) . ?
N1 C2 1.384(9) . ?
N1 C8 1.451(10) . ?
N2 C1 1.359(9) . ?
N2 C7 1.387(9) . ?
N2 C9 1.460(10) . ?
N3 C10 1.351(9) . ?
N3 C11 1.385(9) . ?
N3 C17 1.453(9) . ?
N4 C10 1.359(9) . ?
N4 C16 1.397(9) . ?
N4 C18 1.440(10) . ?
C2 C7 1.391(11) . ?
C2 C3 1.400(10) . ?
C3 C4 1.387(12) . ?
C4 C5 1.401(14) . ?
C5 C6 1.378(13) . ?
C6 C7 1.385(11) . ?
C11 C16 1.384(11) . ?
C11 C12 1.404(11) . ?
C12 C13 1.385(13) . ?
C13 C14 1.401(15) . ?
C14 C15 1.397(13) . ?
C15 C16 1.393(11) . ?
C19 C21 1.490(14) . ?
C19 C20 1.530(12) . ?
C1S Cl3 1.744(11) . ?
C1S Cl1 1.747(12) . ?
C1S Cl2 1.759(11) . ?
C2S Cl5 1.750(10) . ?
C2S Cl4 1.752(11) . ?
C2S Cl6 1.768(10) . ?

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 C10 92.0(3) . . ?
C1 Pd1 S1 176.0(2) . 3_666 ?
C10 Pd1 S1 91.58(19) . 3_666 ?
C1 Pd1 S1 92.2(2) . . ?
C10 Pd1 S1 174.64(19) . . ?
S1 Pd1 S1 84.41(6) 3_666 . ?
C19 S1 Pd1 105.3(3) . 3_666 ?
C19 S1 Pd1 110.5(3) . . ?
Pd1 S1 Pd1 95.59(6) 3_666 . ?
C1 N1 C2 111.0(6) . . ?
C1 N1 C8 125.4(6) . . ?
C2 N1 C8 123.5(6) . . ?
C1 N2 C7 111.9(6) . . ?
C1 N2 C9 125.1(6) . . ?
C7 N2 C9 123.0(7) . . ?
C10 N3 C11 110.3(6) . . ?
C10 N3 C17 126.1(6) . . ?
C11 N3 C17 123.5(6) . . ?
C10 N4 C16 109.8(6) . . ?
C10 N4 C18 126.7(6) . . ?
C16 N4 C18 123.5(6) . . ?
N1 C1 N2 105.0(6) . . ?
N1 C1 Pd1 126.9(5) . . ?
N2 C1 Pd1 128.0(5) . . ?
N1 C2 C7 106.9(6) . . ?
N1 C2 C3 130.8(7) . . ?
C7 C2 C3 122.4(7) . . ?
C4 C3 C2 114.8(8) . . ?
C3 C4 C5 122.9(8) . . ?
C6 C5 C4 121.5(8) . . ?
C5 C6 C7 116.5(8) . . ?
C6 C7 N2 132.8(8) . . ?
C6 C7 C2 121.9(7) . . ?
N2 C7 C2 105.2(6) . . ?
N3 C10 N4 106.8(6) . . ?
N3 C10 Pd1 127.4(5) . . ?
N4 C10 Pd1 125.7(5) . . ?
C16 C11 N3 106.8(6) . . ?
C16 C11 C12 121.4(8) . . ?
N3 C11 C12 131.8(8) . . ?
C13 C12 C11 116.5(9) . . ?
C12 C13 C14 122.0(8) . . ?
C15 C14 C13 121.5(9) . . ?
C16 C15 C14 116.2(9) . . ?
C11 C16 C15 122.4(7) . . ?
C11 C16 N4 106.3(6) . . ?
C15 C16 N4 131.2(8) . . ?
C21 C19 C20 112.7(8) . . ?
C21 C19 S1 113.7(6) . . ?
C20 C19 S1 109.9(7) . . ?
Cl3 C1S Cl1 110.7(6) . . ?
Cl3 C1S Cl2 108.7(6) . . ?
Cl1 C1S Cl2 109.9(6) . . ?
Cl5 C2S Cl4 108.8(5) . . ?
Cl5 C2S Cl6 109.6(6) . . ?
Cl4 C2S Cl6 111.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.377
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.155
####################################################################### 
# 
# 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_J308
_database_code_depnum_ccdc_archive 'CCDC 2119523'
loop_
_audit_author_name
_audit_author_address
'Geok Kheng Tan '
;Department of Chemistry, National University of Singapore
Singapore
;
_audit_update_record             
;
2021-11-01 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H29 Br2 Cl3 N4 Pd'
_chemical_formula_weight         734.07

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'
Br Br -0.2901 2.4595 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   10.6178(3)
_cell_length_b                   11.6652(2)
_cell_length_c                   11.9931(3)
_cell_angle_alpha                90
_cell_angle_beta                 112.9470(10)
_cell_angle_gamma                90
_cell_volume                     1367.90(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9932
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      29.58

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_F_000             724
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.072
_exptl_absorpt_coefficient_mu    3.912
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14299
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.458
_diffrn_reflns_theta_max         29.585
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7341
_reflns_number_gt                7111
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.997

_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_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL--2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT--(Sheldrick 2015)'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+0.2973P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.050(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7341
_refine_ls_number_parameters     361
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0661
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.192
_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
Pd1 Pd 0.62360(3) 0.40974(3) 0.75879(2) 0.01506(7) Uani 1 1 d . . . . .
Br1 Br 0.61499(6) 0.57601(5) 0.87993(6) 0.02038(14) Uani 0.8421(19) 1 d D U P A
1
Br2 Br 0.65076(6) 0.23121(4) 0.66496(6) 0.02470(16) Uani 0.8421(19) 1 d D U P A
1
Br1A Br 0.6431(5) 0.5312(5) 0.9224(5) 0.0432(10) Uani 0.1579(19) 1 d D U P A 2
Br2A Br 0.6171(3) 0.2783(3) 0.5935(3) 0.0303(9) Uani 0.1579(19) 1 d D U P A 2
N1 N 0.8584(3) 0.5235(3) 0.7197(3) 0.0156(6) Uani 1 1 d . . . . .
N2 N 0.9318(3) 0.4130(3) 0.8790(3) 0.0166(6) Uani 1 1 d . . . . .
N3 N 0.3851(4) 0.2861(3) 0.7831(3) 0.0190(7) Uani 1 1 d . . . . .
N4 N 0.3141(3) 0.3998(3) 0.6281(3) 0.0181(6) Uani 1 1 d . . . . .
C1 C 0.8179(4) 0.4516(3) 0.7887(4) 0.0155(7) Uani 1 1 d . . . . .
C2 C 0.9997(4) 0.5322(3) 0.7676(4) 0.0157(7) Uani 1 1 d . . . . .
C3 C 1.0907(5) 0.5972(3) 0.7342(4) 0.0199(8) Uani 1 1 d . . . . .
H3 H 1.059016 0.647222 0.666330 0.024 Uiso 1 1 calc R U . . .
C4 C 1.2284(5) 0.5851(4) 0.8045(4) 0.0231(8) Uani 1 1 d . . . . .
H4 H 1.292474 0.626895 0.783063 0.028 Uiso 1 1 calc R U . . .
C5 C 1.2765(5) 0.5141(4) 0.9054(4) 0.0243(9) Uani 1 1 d . . . . .
H5 H 1.372108 0.508556 0.951317 0.029 Uiso 1 1 calc R U . . .
C6 C 1.1866(5) 0.4510(4) 0.9401(4) 0.0215(8) Uani 1 1 d . . . . .
H6 H 1.218879 0.402737 1.009349 0.026 Uiso 1 1 calc R U . . .
C7 C 1.0471(4) 0.4613(3) 0.8691(4) 0.0162(7) Uani 1 1 d . . . . .
C8 C 0.7583(4) 0.5882(4) 0.6166(4) 0.0200(8) Uani 1 1 d . . . . .
H8 H 0.665448 0.559456 0.605451 0.024 Uiso 1 1 calc R U . . .
C9 C 0.7771(5) 0.5630(4) 0.4987(4) 0.0259(9) Uani 1 1 d . . . . .
H9A H 0.702237 0.598164 0.430608 0.039 Uiso 1 1 calc R U . . .
H9B H 0.776645 0.479945 0.486355 0.039 Uiso 1 1 calc R U . . .
H9C H 0.864542 0.594881 0.503555 0.039 Uiso 1 1 calc R U . . .
C10 C 0.7618(5) 0.7148(4) 0.6464(4) 0.0280(10) Uani 1 1 d . . . . .
H10A H 0.684137 0.753500 0.584198 0.042 Uiso 1 1 calc R U . . .
H10B H 0.847387 0.748412 0.648778 0.042 Uiso 1 1 calc R U . . .
H10C H 0.756057 0.724304 0.725475 0.042 Uiso 1 1 calc R U . . .
C11 C 0.9264(5) 0.3404(4) 0.9770(4) 0.0216(8) Uani 1 1 d . . . . .
H11 H 0.827686 0.322494 0.956170 0.026 Uiso 1 1 calc R U . . .
C12 C 0.9987(5) 0.2253(4) 0.9829(5) 0.0298(10) Uani 1 1 d . . . . .
H12A H 0.994665 0.179516 1.049917 0.045 Uiso 1 1 calc R U . . .
H12B H 1.094487 0.239067 0.995899 0.045 Uiso 1 1 calc R U . . .
H12C H 0.953188 0.183780 0.906584 0.045 Uiso 1 1 calc R U . . .
C13 C 0.9767(5) 0.4040(5) 1.0971(4) 0.0305(9) Uani 1 1 d . . . . .
H13A H 0.975170 0.352275 1.160960 0.046 Uiso 1 1 calc R U . . .
H13B H 0.916985 0.469813 1.091025 0.046 Uiso 1 1 calc R U . . .
H13C H 1.070368 0.430920 1.116810 0.046 Uiso 1 1 calc R U . . .
C14 C 0.4271(4) 0.3655(4) 0.7225(4) 0.0189(8) Uani 1 1 d . . . . .
C15 C 0.2450(4) 0.2699(3) 0.7274(4) 0.0195(8) Uani 1 1 d . . . . .
C16 C 0.1562(5) 0.1972(4) 0.7543(5) 0.0268(10) Uani 1 1 d . . . . .
H16 H 0.187725 0.146889 0.821965 0.032 Uiso 1 1 calc R U . . .
C17 C 0.0197(6) 0.2023(4) 0.6770(5) 0.0337(12) Uani 1 1 d . . . . .
H17 H -0.044106 0.154375 0.692465 0.040 Uiso 1 1 calc R U . . .
C18 C -0.0277(5) 0.2762(4) 0.5763(5) 0.0337(12) Uani 1 1 d . . . . .
H18 H -0.122257 0.276895 0.525570 0.040 Uiso 1 1 calc R U . . .
C19 C 0.0616(5) 0.3487(4) 0.5493(5) 0.0290(10) Uani 1 1 d . . . . .
H19 H 0.030516 0.398807 0.481523 0.035 Uiso 1 1 calc R U . . .
C20 C 0.1982(5) 0.3430(3) 0.6275(4) 0.0215(9) Uani 1 1 d . . . . .
C21 C 0.4743(5) 0.2291(4) 0.8926(4) 0.0285(9) Uani 1 1 d . . . . .
H21A H 0.460655 0.145987 0.882980 0.043 Uiso 1 1 calc R U . . .
H21B H 0.452862 0.255108 0.960913 0.043 Uiso 1 1 calc R U . . .
H21C H 0.569680 0.247493 0.908066 0.043 Uiso 1 1 calc R U . . .
C22 C 0.3118(5) 0.4879(4) 0.5411(4) 0.0250(9) Uani 1 1 d . . . . .
H22A H 0.244871 0.547028 0.537845 0.038 Uiso 1 1 calc R U . . .
H22B H 0.286305 0.453259 0.460789 0.038 Uiso 1 1 calc R U . . .
H22C H 0.402700 0.522714 0.566059 0.038 Uiso 1 1 calc R U . . .
Cl1S Cl 0.59129(16) 0.28769(12) 0.37870(14) 0.0382(4) Uani 0.858(3) 1 d D U P B
1
Cl2S Cl 0.6584(3) 0.3971(3) 0.1936(2) 0.0520(6) Uani 0.858(3) 1 d D U P B 1
Cl3S Cl 0.4278(3) 0.47572(18) 0.2457(2) 0.0388(5) Uani 0.858(3) 1 d D U P B 1
C1S C 0.5231(7) 0.3540(6) 0.2369(6) 0.0402(9) Uani 0.858(3) 1 d D U P B 1
H1S H 0.461881 0.299035 0.175706 0.048 Uiso 0.858(3) 1 calc R U P B 1
Cl1A Cl 0.4707(11) 0.2620(8) 0.2206(9) 0.0407(14) Uani 0.142(3) 1 d D U P B 2
Cl2A Cl 0.6199(17) 0.3992(18) 0.1609(14) 0.0450(15) Uani 0.142(3) 1 d D U P B 2
Cl3A Cl 0.439(2) 0.4984(14) 0.2747(16) 0.0437(17) Uani 0.142(3) 1 d D U P B 2
C1A C 0.557(3) 0.388(2) 0.281(3) 0.0425(11) Uani 0.142(3) 1 d D U P B 2
H1A H 0.631211 0.377966 0.362738 0.051 Uiso 0.142(3) 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.012(4) . ?
Pd1 C14 2.025(4) . ?
Pd1 Br1A 2.363(4) . ?
Pd1 Br2 2.4372(6) . ?
Pd1 Br1 2.4462(6) . ?
Pd1 Br2A 2.486(3) . ?
N1 C1 1.359(5) . ?
N1 C2 1.385(5) . ?
N1 C8 1.485(5) . ?
N2 C1 1.348(5) . ?
N2 C7 1.395(5) . ?
N2 C11 1.468(5) . ?
N3 C14 1.356(5) . ?
N3 C15 1.385(6) . ?
N3 C21 1.447(6) . ?
N4 C14 1.349(5) . ?
N4 C20 1.394(5) . ?
N4 C22 1.459(6) . ?
C2 C7 1.393(6) . ?
C2 C3 1.404(6) . ?
C3 C4 1.381(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.396(6) . ?
C6 H6 0.9500 . ?
C8 C10 1.517(6) . ?
C8 C9 1.532(6) . ?
C8 H8 1.0000 . ?
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 C13 1.520(7) . ?
C11 C12 1.535(6) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 C20 1.395(6) . ?
C15 C16 1.397(6) . ?
C16 C17 1.384(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.408(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.399(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(7) . ?
C19 H19 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Cl1S C1S 1.748(7) . ?
Cl2S C1S 1.780(7) . ?
Cl3S C1S 1.770(7) . ?
C1S H1S 1.0000 . ?
Cl1A C1A 1.73(2) . ?
Cl2A C1A 1.81(2) . ?
Cl3A C1A 1.77(2) . ?
C1A H1A 1.0000 . ?

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 C14 177.87(17) . . ?
C1 Pd1 Br1A 87.41(16) . . ?
C14 Pd1 Br1A 94.62(16) . . ?
C1 Pd1 Br2 89.55(11) . . ?
C14 Pd1 Br2 88.89(12) . . ?
C1 Pd1 Br1 88.56(11) . . ?
C14 Pd1 Br1 93.19(12) . . ?
Br2 Pd1 Br1 172.00(2) . . ?
C1 Pd1 Br2A 89.96(14) . . ?
C14 Pd1 Br2A 88.04(14) . . ?
Br1A Pd1 Br2A 176.65(16) . . ?
C1 N1 C2 110.0(3) . . ?
C1 N1 C8 121.8(3) . . ?
C2 N1 C8 128.0(3) . . ?
C1 N2 C7 109.8(3) . . ?
C1 N2 C11 122.2(3) . . ?
C7 N2 C11 127.7(3) . . ?
C14 N3 C15 110.5(4) . . ?
C14 N3 C21 124.4(4) . . ?
C15 N3 C21 125.1(4) . . ?
C14 N4 C20 111.0(4) . . ?
C14 N4 C22 124.7(4) . . ?
C20 N4 C22 124.2(4) . . ?
N2 C1 N1 107.3(3) . . ?
N2 C1 Pd1 126.7(3) . . ?
N1 C1 Pd1 126.0(3) . . ?
N1 C2 C7 106.4(3) . . ?
N1 C2 C3 132.6(4) . . ?
C7 C2 C3 121.0(4) . . ?
C4 C3 C2 117.0(4) . . ?
C4 C3 H3 121.5 . . ?
C2 C3 H3 121.5 . . ?
C3 C4 C5 122.3(4) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C4 C5 C6 120.9(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C7 117.4(4) . . ?
C5 C6 H6 121.3 . . ?
C7 C6 H6 121.3 . . ?
C2 C7 N2 106.5(3) . . ?
C2 C7 C6 121.4(4) . . ?
N2 C7 C6 132.2(4) . . ?
N1 C8 C10 110.8(4) . . ?
N1 C8 C9 111.3(4) . . ?
C10 C8 C9 113.8(4) . . ?
N1 C8 H8 106.8 . . ?
C10 C8 H8 106.8 . . ?
C9 C8 H8 106.8 . . ?
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 . . ?
N2 C11 C13 111.6(4) . . ?
N2 C11 C12 111.5(3) . . ?
C13 C11 C12 113.5(4) . . ?
N2 C11 H11 106.6 . . ?
C13 C11 H11 106.6 . . ?
C12 C11 H11 106.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C14 N3 106.3(4) . . ?
N4 C14 Pd1 127.6(3) . . ?
N3 C14 Pd1 125.8(3) . . ?
N3 C15 C20 106.7(4) . . ?
N3 C15 C16 131.8(4) . . ?
C20 C15 C16 121.5(4) . . ?
C17 C16 C15 116.4(5) . . ?
C17 C16 H16 121.8 . . ?
C15 C16 H16 121.8 . . ?
C16 C17 C18 122.1(4) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C19 C18 C17 121.4(5) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C20 C19 C18 116.0(5) . . ?
C20 C19 H19 122.0 . . ?
C18 C19 H19 122.0 . . ?
C19 C20 N4 132.0(4) . . ?
C19 C20 C15 122.5(4) . . ?
N4 C20 C15 105.5(4) . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Cl1S C1S Cl3S 109.1(4) . . ?
Cl1S C1S Cl2S 109.5(4) . . ?
Cl3S C1S Cl2S 109.6(4) . . ?
Cl1S C1S H1S 109.6 . . ?
Cl3S C1S H1S 109.6 . . ?
Cl2S C1S H1S 109.6 . . ?
Cl1A C1A Cl3A 110.5(17) . . ?
Cl1A C1A Cl2A 91.7(14) . . ?
Cl3A C1A Cl2A 112.8(18) . . ?
Cl1A C1A H1A 113.4 . . ?
Cl3A C1A H1A 113.4 . . ?
Cl2A C1A H1A 113.4 . . ?

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
C7 N2 C1 N1 0.6(5) . . . . ?
C11 N2 C1 N1 174.9(4) . . . . ?
C7 N2 C1 Pd1 179.8(3) . . . . ?
C11 N2 C1 Pd1 -5.9(6) . . . . ?
C2 N1 C1 N2 -0.9(4) . . . . ?
C8 N1 C1 N2 -175.7(4) . . . . ?
C2 N1 C1 Pd1 179.9(3) . . . . ?
C8 N1 C1 Pd1 5.2(5) . . . . ?
C1 N1 C2 C7 0.8(4) . . . . ?
C8 N1 C2 C7 175.2(4) . . . . ?
C1 N1 C2 C3 -177.2(4) . . . . ?
C8 N1 C2 C3 -2.9(7) . . . . ?
N1 C2 C3 C4 179.5(4) . . . . ?
C7 C2 C3 C4 1.7(6) . . . . ?
C2 C3 C4 C5 -1.3(6) . . . . ?
C3 C4 C5 C6 0.2(7) . . . . ?
C4 C5 C6 C7 0.5(6) . . . . ?
N1 C2 C7 N2 -0.4(4) . . . . ?
C3 C2 C7 N2 177.9(4) . . . . ?
N1 C2 C7 C6 -179.3(4) . . . . ?
C3 C2 C7 C6 -1.0(6) . . . . ?
C1 N2 C7 C2 -0.1(5) . . . . ?
C11 N2 C7 C2 -174.0(4) . . . . ?
C1 N2 C7 C6 178.6(4) . . . . ?
C11 N2 C7 C6 4.7(7) . . . . ?
C5 C6 C7 C2 -0.1(6) . . . . ?
C5 C6 C7 N2 -178.7(4) . . . . ?
C1 N1 C8 C10 108.7(4) . . . . ?
C2 N1 C8 C10 -65.1(5) . . . . ?
C1 N1 C8 C9 -123.6(4) . . . . ?
C2 N1 C8 C9 62.7(5) . . . . ?
C1 N2 C11 C13 -110.5(5) . . . . ?
C7 N2 C11 C13 62.7(6) . . . . ?
C1 N2 C11 C12 121.4(5) . . . . ?
C7 N2 C11 C12 -65.4(6) . . . . ?
C20 N4 C14 N3 0.3(5) . . . . ?
C22 N4 C14 N3 177.8(4) . . . . ?
C20 N4 C14 Pd1 174.5(3) . . . . ?
C22 N4 C14 Pd1 -8.0(6) . . . . ?
C15 N3 C14 N4 -0.2(4) . . . . ?
C21 N3 C14 N4 -178.5(4) . . . . ?
C15 N3 C14 Pd1 -174.5(3) . . . . ?
C21 N3 C14 Pd1 7.2(6) . . . . ?
C14 N3 C15 C20 0.0(4) . . . . ?
C21 N3 C15 C20 178.3(4) . . . . ?
C14 N3 C15 C16 178.9(4) . . . . ?
C21 N3 C15 C16 -2.8(7) . . . . ?
N3 C15 C16 C17 -179.1(4) . . . . ?
C20 C15 C16 C17 -0.4(6) . . . . ?
C15 C16 C17 C18 0.3(7) . . . . ?
C16 C17 C18 C19 -0.1(7) . . . . ?
C17 C18 C19 C20 0.0(7) . . . . ?
C18 C19 C20 N4 178.8(4) . . . . ?
C18 C19 C20 C15 -0.1(6) . . . . ?
C14 N4 C20 C19 -179.3(4) . . . . ?
C22 N4 C20 C19 3.1(7) . . . . ?
C14 N4 C20 C15 -0.3(5) . . . . ?
C22 N4 C20 C15 -177.9(4) . . . . ?
N3 C15 C20 C19 179.3(4) . . . . ?
C16 C15 C20 C19 0.3(6) . . . . ?
N3 C15 C20 N4 0.2(4) . . . . ?
C16 C15 C20 N4 -178.8(4) . . . . ?

_refine_diff_density_max         0.661
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.083



####################################################################### 
# 
# 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_K292
_database_code_depnum_ccdc_archive 'CCDC 2119520'
loop_
_audit_author_name
_audit_author_address
'Geok Kheng Tan '
;Department of Chemistry, National University of Singapore
Singapore
;
_audit_update_record             
;
2021-11-01 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H30 N6 O Pd S2'
_chemical_formula_weight         468.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 '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                   19.2127(5)
_cell_length_b                   8.3951(3)
_cell_length_c                   14.5503(5)
_cell_angle_alpha                90
_cell_angle_beta                 120.6380(10)
_cell_angle_gamma                90
_cell_volume                     2019.24(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      29.69

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_F_000             968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.124
_exptl_absorpt_coefficient_mu    1.140
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.616681
_exptl_absorpt_correction_T_max  0.745909
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2566
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.721
_diffrn_reflns_theta_max         28.276
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2566
_reflns_number_gt                2351
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _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_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL--2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT--(Sheldrick 2015)'
_refine_special_details          
; 
 Refined as a 2-component twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²+9.9655P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2566
_refine_ls_number_parameters     122
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0919
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.750000 0.250000 0.500000 0.01188(11) Uani 1 2 d S . P . .
S1 S 0.62560(5) 0.13597(10) 0.45817(8) 0.01966(19) Uani 1 1 d . . . . .
N1 N 0.66956(17) 0.5782(3) 0.4468(2) 0.0176(6) Uani 1 1 d . . . . .
N2 N 0.74170(17) 0.5464(3) 0.6140(2) 0.0169(6) Uani 1 1 d . . . . .
N3 N 0.70972(19) 0.6958(4) 0.6021(3) 0.0241(7) Uani 1 1 d . . . . .
C1 C 0.71873(19) 0.4705(4) 0.5216(3) 0.0142(6) Uani 1 1 d . . . . .
C2 C 0.6659(2) 0.7117(4) 0.4988(4) 0.0242(8) Uani 1 1 d . . . . .
H2 H 0.635149 0.804036 0.463787 0.029 Uiso 1 1 calc R U . . .
C3 C 0.7963(2) 0.4865(5) 0.7210(3) 0.0251(8) Uani 1 1 d . . . . .
H3A H 0.794606 0.369819 0.720439 0.038 Uiso 1 1 calc R U . . .
H3B H 0.779600 0.527215 0.770002 0.038 Uiso 1 1 calc R U . . .
H3C H 0.851535 0.522113 0.744860 0.038 Uiso 1 1 calc R U . . .
C4 C 0.6304(2) 0.5568(5) 0.3316(3) 0.0239(8) Uani 1 1 d . . . . .
H4A H 0.588531 0.638269 0.295384 0.036 Uiso 1 1 calc R U . . .
H4B H 0.605648 0.450869 0.312189 0.036 Uiso 1 1 calc R U . . .
H4C H 0.670739 0.566954 0.309705 0.036 Uiso 1 1 calc R U . . .
C5 C 0.5556(2) 0.2786(4) 0.4608(3) 0.0184(7) Uani 1 1 d . . . . .
H5 H 0.562124 0.382488 0.432386 0.022 Uiso 1 1 calc R U . . .
C6 C 0.5720(2) 0.3056(5) 0.5732(3) 0.0251(8) Uani 1 1 d . . . . .
H6A H 0.535112 0.387404 0.571957 0.038 Uiso 1 1 calc R U . . .
H6B H 0.628021 0.340811 0.619223 0.038 Uiso 1 1 calc R U . . .
H6C H 0.563370 0.205931 0.601131 0.038 Uiso 1 1 calc R U . . .
C7 C 0.4697(2) 0.2186(5) 0.3870(3) 0.0245(8) Uani 1 1 d . . . . .
H7A H 0.459942 0.208294 0.314279 0.037 Uiso 1 1 calc R U . . .
H7B H 0.431040 0.294419 0.387293 0.037 Uiso 1 1 calc R U . . .
H7C H 0.462995 0.114565 0.412043 0.037 Uiso 1 1 calc R U . . .
O1S O 0.500000 -0.1054(5) 0.250000 0.0315(9) Uani 1 2 d DS T P . .
H1A H 0.479(6) -0.041(11) 0.188(5) 0.038 Uiso 0.5 1 d D U P . .
H1B H 0.549(3) -0.056(12) 0.301(7) 0.038 Uiso 0.5 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.020(3) . ?
Pd1 C1 2.020(3) 7_656 ?
Pd1 S1 2.3486(8) . ?
Pd1 S1 2.3487(8) 7_656 ?
S1 C5 1.816(3) . ?
N1 C1 1.358(4) . ?
N1 C2 1.374(5) . ?
N1 C4 1.458(5) . ?
N2 C1 1.342(4) . ?
N2 N3 1.369(4) . ?
N2 C3 1.454(5) . ?
N3 C2 1.302(5) . ?
C2 H2 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.517(5) . ?
C5 C7 1.524(5) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
O1S H1A 0.949(10) . ?
O1S H1B 0.949(10) . ?

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 C1 180.0 . 7_656 ?
C1 Pd1 S1 94.00(9) . . ?
C1 Pd1 S1 85.99(9) 7_656 . ?
C1 Pd1 S1 86.00(9) . 7_656 ?
C1 Pd1 S1 94.00(9) 7_656 7_656 ?
S1 Pd1 S1 180.0 . 7_656 ?
C5 S1 Pd1 113.11(11) . . ?
C1 N1 C2 108.2(3) . . ?
C1 N1 C4 125.4(3) . . ?
C2 N1 C4 126.4(3) . . ?
C1 N2 N3 114.3(3) . . ?
C1 N2 C3 126.7(3) . . ?
N3 N2 C3 119.0(3) . . ?
C2 N3 N2 103.0(3) . . ?
N2 C1 N1 103.0(3) . . ?
N2 C1 Pd1 128.2(2) . . ?
N1 C1 Pd1 128.8(3) . . ?
N3 C2 N1 111.6(3) . . ?
N3 C2 H2 124.2 . . ?
N1 C2 H2 124.2 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C7 111.4(3) . . ?
C6 C5 S1 111.9(3) . . ?
C7 C5 S1 108.3(2) . . ?
C6 C5 H5 108.4 . . ?
C7 C5 H5 108.4 . . ?
S1 C5 H5 108.4 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
H1A O1S H1B 106(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 N2 N3 C2 -0.1(4) . . . . ?
C3 N2 N3 C2 179.0(3) . . . . ?
N3 N2 C1 N1 0.2(4) . . . . ?
C3 N2 C1 N1 -178.9(3) . . . . ?
N3 N2 C1 Pd1 -179.8(2) . . . . ?
C3 N2 C1 Pd1 1.1(5) . . . . ?
C2 N1 C1 N2 -0.1(4) . . . . ?
C4 N1 C1 N2 177.6(3) . . . . ?
C2 N1 C1 Pd1 179.8(2) . . . . ?
C4 N1 C1 Pd1 -2.4(5) . . . . ?
N2 N3 C2 N1 0.0(4) . . . . ?
C1 N1 C2 N3 0.1(4) . . . . ?
C4 N1 C2 N3 -177.7(3) . . . . ?
Pd1 S1 C5 C6 -82.5(3) . . . . ?
Pd1 S1 C5 C7 154.3(2) . . . . ?

_refine_diff_density_max         1.875
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.118



