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

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

data_291215_0m-sr
_database_code_depnum_ccdc_archive 'CCDC 1977286'
loop_
_audit_author_name
_audit_author_address
jy
;Nanjing university
China
;
_audit_update_record             
;
2020-01-13 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H23 Cl3 N4 O9 Pd2'
_chemical_formula_weight         698.50

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5139(10)
_cell_length_b                   10.7443(12)
_cell_length_c                   14.4956(16)
_cell_angle_alpha                70.4900(10)
_cell_angle_beta                 73.6940(10)
_cell_angle_gamma                71.3320(10)
_cell_volume                     1161.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_T_max  0.7335
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5854
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4041
_reflns_number_gt                3270
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.146 0.000 0.681 7 8 ' '
2 0.854 0.000 0.319 7 8 ' '
_platon_squeeze_details          
;
;

_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)+(0.0687P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4041
_refine_ls_number_parameters     324
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1106
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.061
_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 0.23723(5) 0.23839(4) 0.25829(3) 0.04385(15) Uani 1 1 d . . .
Pd2 Pd 0.36835(5) -0.05284(4) 0.37589(3) 0.04350(15) Uani 1 1 d . . .
O5 O 0.6878(16) 0.2564(10) 0.2273(11) 0.127(5) Uani 0.600(17) 1 d PDU A 1
O7 O 0.5980(14) 0.4766(12) 0.1499(11) 0.105(4) Uani 0.600(17) 1 d PDU A 1
O8 O 0.7446(14) 0.4157(14) 0.2796(8) 0.089(4) Uani 0.600(17) 1 d PDU A 1
O9 O 0.8845(13) 0.3713(16) 0.1232(8) 0.116(5) Uani 0.600(17) 1 d PDU A 1
Cl1 Cl 0.7321(2) 0.38784(19) 0.19342(12) 0.0703(5) Uani 0.600(17) 1 d PD A 1
O4 O 0.2747(12) 0.5754(10) 0.3686(8) 0.111(3) Uani 0.80 1 d PU B 1
O10 O -0.0135(14) 0.6492(13) 0.4014(10) 0.121(4) Uani 0.80 1 d P B 1
Cl3 Cl 0.1173(2) 0.10900(15) 0.40960(12) 0.0642(4) Uani 1 1 d . . .
O1 O 0.3693(5) 0.0552(4) 0.2312(3) 0.0507(9) Uani 1 1 d . . .
N4 N 0.5879(6) -0.1861(4) 0.3438(3) 0.0486(11) Uani 1 1 d . . .
H4A H 0.6738 -0.1499 0.3394 0.058 Uiso 1 1 calc R . .
N2 N 0.3402(7) 0.3456(5) 0.1269(3) 0.0536(12) Uani 1 1 d . . .
H2A H 0.4393 0.3547 0.1328 0.064 Uiso 1 1 calc R . .
N3 N 0.3648(7) -0.1682(5) 0.5179(3) 0.0569(12) Uani 1 1 d . . .
H3A H 0.3415 -0.1149 0.5590 0.068 Uiso 1 1 calc R . .
H3B H 0.2844 -0.2143 0.5368 0.068 Uiso 1 1 calc R . .
C3 C 0.5138(8) 0.1435(6) 0.0653(4) 0.0546(15) Uani 1 1 d . . .
C7 C 0.6033(8) -0.2103(6) 0.2470(5) 0.0590(15) Uani 1 1 d . . .
H7A H 0.5046 -0.2380 0.2485 0.071 Uiso 1 1 calc R . .
H7B H 0.7017 -0.2847 0.2373 0.071 Uiso 1 1 calc R . .
N1 N 0.0991(7) 0.4207(5) 0.2798(4) 0.0554(12) Uani 1 1 d . . .
H1A H -0.0104 0.4307 0.2807 0.067 Uiso 1 1 calc R . .
H1B H 0.1072 0.4267 0.3387 0.067 Uiso 1 1 calc R . .
C5 C 0.6194(7) -0.0877(6) 0.1608(4) 0.0510(14) Uani 1 1 d . . .
C4 C 0.5022(7) 0.0373(6) 0.1542(4) 0.0485(13) Uani 1 1 d . . .
C12 C 0.1635(9) 0.5279(6) 0.1979(5) 0.0669(17) Uani 1 1 d . . .
H12A H 0.2564 0.5450 0.2141 0.080 Uiso 1 1 calc R . .
H12B H 0.0748 0.6118 0.1891 0.080 Uiso 1 1 calc R . .
C11 C 0.2224(9) 0.4847(6) 0.1040(5) 0.0634(17) Uani 1 1 d . . .
H11A H 0.2805 0.5482 0.0522 0.076 Uiso 1 1 calc R . .
H11B H 0.1271 0.4817 0.0813 0.076 Uiso 1 1 calc R . .
C6 C 0.7512(8) -0.1045(7) 0.0763(5) 0.0601(16) Uani 1 1 d . . .
H6 H 0.8302 -0.1881 0.0797 0.072 Uiso 1 1 calc R . .
C1 C 0.7649(8) -0.0014(8) -0.0095(5) 0.0626(17) Uani 1 1 d . . .
C8 C 0.3772(9) 0.2744(6) 0.0493(4) 0.0621(16) Uani 1 1 d . . .
H8A H 0.4116 0.3345 -0.0152 0.075 Uiso 1 1 calc R . .
H8B H 0.2748 0.2543 0.0480 0.075 Uiso 1 1 calc R . .
C2 C 0.6459(9) 0.1193(7) -0.0138(4) 0.0617(16) Uani 1 1 d . . .
H2 H 0.6534 0.1891 -0.0726 0.074 Uiso 1 1 calc R . .
C10 C 0.5330(8) -0.2648(6) 0.5236(5) 0.0630(16) Uani 1 1 d . . .
H10A H 0.5249 -0.3422 0.5816 0.076 Uiso 1 1 calc R . .
H10B H 0.6115 -0.2202 0.5290 0.076 Uiso 1 1 calc R . .
C9 C 0.5929(8) -0.3110(6) 0.4298(5) 0.0584(15) Uani 1 1 d . . .
H9A H 0.7072 -0.3686 0.4275 0.070 Uiso 1 1 calc R . .
H9B H 0.5200 -0.3627 0.4274 0.070 Uiso 1 1 calc R . .
Cl2 Cl 0.1343(2) 0.66509(16) 0.41290(14) 0.0679(4) Uani 1 1 d . . .
C13 C 0.9060(9) -0.0198(9) -0.0994(5) 0.081(2) Uani 1 1 d . . .
H13A H 0.9326 0.0660 -0.1357 0.121 Uiso 1 1 calc R . .
H13B H 0.8697 -0.0524 -0.1421 0.121 Uiso 1 1 calc R . .
H13C H 1.0045 -0.0848 -0.0772 0.121 Uiso 1 1 calc R . .
O2 O 0.1468(7) 0.7976(6) 0.3556(4) 0.090 Uani 1 1 d U B .
O3 O 0.1598(7) 0.6459(5) 0.5118(4) 0.090 Uani 1 1 d U B .
O5' O 0.8363(19) 0.479(2) 0.1297(11) 0.103(6) Uani 0.400(17) 1 d PDU A 2
O9' O 0.757(3) 0.285(2) 0.1518(19) 0.174(11) Uani 0.400(17) 1 d PDU A 2
O7' O 0.564(2) 0.471(2) 0.1946(16) 0.123(8) Uani 0.400(17) 1 d PDU A 2
O8' O 0.770(2) 0.346(2) 0.2873(11) 0.105(6) Uani 0.400(17) 1 d PDU A 2
Cl1' Cl 0.7321(2) 0.38784(19) 0.19342(12) 0.0703(5) Uani 0.400(17) 1 d PD A 2
O10' O -0.046(4) 0.669(5) 0.458(3) 0.092(12) Uani 0.20 1 d P B 2
O4' O 0.199(3) 0.534(3) 0.3981(19) 0.057(6) Uani 0.20 1 d PU 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 N2 1.992(5) . ?
Pd1 N1 2.011(5) . ?
Pd1 O1 2.036(4) . ?
Pd1 Cl3 2.3240(15) . ?
Pd1 Pd2 3.0353(6) . ?
Pd2 N4 2.001(4) . ?
Pd2 N3 2.015(5) . ?
Pd2 O1 2.029(4) . ?
Pd2 Cl3 2.3310(15) . ?
O5 Cl1 1.467(10) . ?
O7 Cl1 1.384(9) . ?
O8 Cl1 1.416(9) . ?
O9 Cl1 1.408(10) . ?
O4 Cl2 1.420(8) . ?
O10 Cl2 1.384(11) . ?
O1 C4 1.363(7) . ?
N4 C7 1.474(7) . ?
N4 C9 1.494(7) . ?
N4 H4A 0.9100 . ?
N2 C8 1.473(7) . ?
N2 C11 1.499(7) . ?
N2 H2A 0.9100 . ?
N3 C10 1.481(8) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
C3 C2 1.391(8) . ?
C3 C4 1.411(8) . ?
C3 C8 1.506(9) . ?
C7 C5 1.495(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
N1 C12 1.470(8) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
C5 C4 1.386(8) . ?
C5 C6 1.428(8) . ?
C12 C11 1.487(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C6 C1 1.367(9) . ?
C6 H6 0.9300 . ?
C1 C2 1.361(9) . ?
C1 C13 1.524(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2 H2 0.9300 . ?
C10 C9 1.501(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
Cl2 O4' 1.41(2) . ?
Cl2 O2 1.409(6) . ?
Cl2 O3 1.447(6) . ?
Cl2 O10' 1.48(3) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?

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
N2 Pd1 N1 85.3(2) . . ?
N2 Pd1 O1 93.80(17) . . ?
N1 Pd1 O1 176.92(18) . . ?
N2 Pd1 Cl3 178.47(14) . . ?
N1 Pd1 Cl3 95.88(15) . . ?
O1 Pd1 Cl3 84.95(11) . . ?
N2 Pd1 Pd2 129.80(14) . . ?
N1 Pd1 Pd2 140.48(14) . . ?
O1 Pd1 Pd2 41.60(10) . . ?
Cl3 Pd1 Pd2 49.40(4) . . ?
N4 Pd2 N3 85.38(19) . . ?
N4 Pd2 O1 93.68(17) . . ?
N3 Pd2 O1 176.95(18) . . ?
N4 Pd2 Cl3 177.86(14) . . ?
N3 Pd2 Cl3 96.10(14) . . ?
O1 Pd2 Cl3 84.93(11) . . ?
N4 Pd2 Pd1 128.85(13) . . ?
N3 Pd2 Pd1 140.43(14) . . ?
O1 Pd2 Pd1 41.77(10) . . ?
Cl3 Pd2 Pd1 49.20(4) . . ?
O7 Cl1 O9 112.3(7) . . ?
O7 Cl1 O8 113.6(7) . . ?
O9 Cl1 O8 114.2(6) . . ?
O7 Cl1 O5 103.1(6) . . ?
O9 Cl1 O5 105.9(6) . . ?
O8 Cl1 O5 106.5(6) . . ?
Pd1 Cl3 Pd2 81.39(5) . . ?
C4 O1 Pd2 124.9(3) . . ?
C4 O1 Pd1 124.9(3) . . ?
Pd2 O1 Pd1 96.63(16) . . ?
C7 N4 C9 114.3(5) . . ?
C7 N4 Pd2 110.1(3) . . ?
C9 N4 Pd2 106.7(3) . . ?
C7 N4 H4A 108.6 . . ?
C9 N4 H4A 108.6 . . ?
Pd2 N4 H4A 108.6 . . ?
C8 N2 C11 113.5(5) . . ?
C8 N2 Pd1 110.9(4) . . ?
C11 N2 Pd1 107.5(4) . . ?
C8 N2 H2A 108.3 . . ?
C11 N2 H2A 108.3 . . ?
Pd1 N2 H2A 108.3 . . ?
C10 N3 Pd2 108.2(4) . . ?
C10 N3 H3A 110.1 . . ?
Pd2 N3 H3A 110.1 . . ?
C10 N3 H3B 110.1 . . ?
Pd2 N3 H3B 110.1 . . ?
H3A N3 H3B 108.4 . . ?
C2 C3 C4 118.3(6) . . ?
C2 C3 C8 119.2(5) . . ?
C4 C3 C8 122.1(5) . . ?
N4 C7 C5 113.1(5) . . ?
N4 C7 H7A 109.0 . . ?
C5 C7 H7A 109.0 . . ?
N4 C7 H7B 109.0 . . ?
C5 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C12 N1 Pd1 108.4(4) . . ?
C12 N1 H1A 110.0 . . ?
Pd1 N1 H1A 110.0 . . ?
C12 N1 H1B 110.0 . . ?
Pd1 N1 H1B 110.0 . . ?
H1A N1 H1B 108.4 . . ?
C4 C5 C6 118.2(6) . . ?
C4 C5 C7 123.2(5) . . ?
C6 C5 C7 118.2(5) . . ?
O1 C4 C5 120.0(5) . . ?
O1 C4 C3 119.8(5) . . ?
C5 C4 C3 120.1(5) . . ?
N1 C12 C11 109.9(5) . . ?
N1 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
N1 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C12 C11 N2 106.9(5) . . ?
C12 C11 H11A 110.3 . . ?
N2 C11 H11A 110.3 . . ?
C12 C11 H11B 110.3 . . ?
N2 C11 H11B 110.3 . . ?
H11A C11 H11B 108.6 . . ?
C1 C6 C5 122.1(6) . . ?
C1 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C2 C1 C6 118.1(6) . . ?
C2 C1 C13 120.1(7) . . ?
C6 C1 C13 121.8(7) . . ?
N2 C8 C3 113.3(5) . . ?
N2 C8 H8A 108.9 . . ?
C3 C8 H8A 108.9 . . ?
N2 C8 H8B 108.9 . . ?
C3 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C1 C2 C3 123.2(6) . . ?
C1 C2 H2 118.4 . . ?
C3 C2 H2 118.4 . . ?
N3 C10 C9 107.3(5) . . ?
N3 C10 H10A 110.3 . . ?
C9 C10 H10A 110.3 . . ?
N3 C10 H10B 110.3 . . ?
C9 C10 H10B 110.3 . . ?
H10A C10 H10B 108.5 . . ?
N4 C9 C10 107.3(5) . . ?
N4 C9 H9A 110.3 . . ?
C10 C9 H9A 110.2 . . ?
N4 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
O10 Cl2 O4' 82.4(12) . . ?
O10 Cl2 O2 106.7(6) . . ?
O4' Cl2 O2 135.5(11) . . ?
O10 Cl2 O4 109.3(6) . . ?
O4' Cl2 O4 34.3(10) . . ?
O2 Cl2 O4 105.6(5) . . ?
O10 Cl2 O3 119.7(6) . . ?
O4' Cl2 O3 103.7(11) . . ?
O2 Cl2 O3 108.3(3) . . ?
O4 Cl2 O3 106.5(5) . . ?
O10 Cl2 O10' 35.0(13) . . ?
O4' Cl2 O10' 103.1(19) . . ?
O2 Cl2 O10' 108(2) . . ?
O4 Cl2 O10' 136.8(16) . . ?
O3 Cl2 O10' 87.3(17) . . ?
C1 C13 H13A 109.5 . . ?
C1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.119
