# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1516139'
_audit_update_record             
;
2016-11-10 deposited with the CCDC.
2016-11-14 downloaded from the CCDC.
;
_audit_creation_date             2016-10-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C24 H22 Cl4 Co N4 O12 Pd2'
_chemical_formula_sum            'C24 H22 Cl4 Co N4 O12 Pd2'
_chemical_formula_weight         971.99
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   5.3010(11)
_cell_length_b                   12.470(3)
_cell_length_c                   12.610(3)
_cell_angle_alpha                76.80(3)
_cell_angle_beta                 79.55(3)
_cell_angle_gamma                81.30(3)
_cell_volume                     792.8(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1569
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_exptl_absorpt_coefficient_mu    2.043
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             477
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7993
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         3.36
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1865
	          2theta: 30.0223
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1865
	          2theta: 30.0223
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1865
	          2theta: 30.0223
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.050155
_diffrn_orient_matrix_UB_12      -0.175852
_diffrn_orient_matrix_UB_13      -0.062073
_diffrn_orient_matrix_UB_21      0.005697
_diffrn_orient_matrix_UB_22      -0.019550
_diffrn_orient_matrix_UB_23      0.080358
_diffrn_orient_matrix_UB_31      -0.073960
_diffrn_orient_matrix_UB_32      0.036155
_diffrn_orient_matrix_UB_33      -0.003535
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2321
_reflns_number_total             3591
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3591
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0753
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1045P)²+0.6485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2171
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5A,H5B} of O5
 At 1.5 times of:
  All O(H) groups, {H6A,H6B} of O6
2.a Riding coordinates:
 O4(H4), O5(H5A,H5B), O6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4A), C8(H8), C10(H10), C11(H11)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd -0.15807(13) 0.70740(5) 0.74450(6) 0.0397(3) Uani 1 d . . 1 . . .
Co1 Co 0.5000 0.0000 1.0000 0.0384(4) Uani 1 d . . 2 S T P
Cl1 Cl -0.5128(5) 0.6828(2) 0.8789(2) 0.0519(6) Uani 1 d . . 1 . . .
Cl2 Cl -0.3275(5) 0.8871(2) 0.6810(2) 0.0560(7) Uani 1 d . . 1 . . .
O1 O 0.3332(11) 0.1583(5) 0.9329(5) 0.0382(13) Uani 1 d . . 1 . . .
O2 O 0.6540(13) 0.2108(5) 0.8001(6) 0.062(2) Uani 1 d . . 1 . . .
O3 O 1.0247(13) 0.6143(5) 0.4161(6) 0.0556(18) Uani 1 d . . 1 . . .
O4 O 0.9028(13) 0.7876(5) 0.3294(6) 0.0582(19) Uani 1 d . . 1 . . .
H4 H 1.0463 0.7814 0.2923 0.087 Uiso 1 d . . 1 R . .
O5 O 0.2708(12) -0.0769(5) 0.9321(6) 0.0546(17) Uani 1 d . . 1 . . .
H5A H 0.3259 -0.0942 0.8699 0.066 Uiso 1 d . . 1 R . .
H5B H 0.1219 -0.0913 0.9658 0.066 Uiso 1 d . . 1 R . .
O6 O 0.8032(11) -0.0023(5) 0.8622(5) 0.0475(16) Uani 1 d . . 1 . . .
H6A H 0.8111 0.0527 0.8082 0.071 Uiso 1 d . . 1 R . .
H6B H 0.9153 -0.0588 0.8617 0.071 Uiso 1 d . . 1 R . .
N1 N 0.0147(13) 0.5501(6) 0.7908(6) 0.0365(16) Uani 1 d . . 1 . . .
N2 N 0.1665(12) 0.7163(5) 0.6271(6) 0.0337(15) Uani 1 d . . 1 . . .
C1 C -0.0744(17) 0.4720(7) 0.8732(8) 0.043(2) Uani 1 d . . 1 . . .
H1 H -0.2325 0.4885 0.9155 0.052 Uiso 1 calc . . 1 R . .
C2 C 0.0555(17) 0.3673(7) 0.8996(8) 0.045(2) Uani 1 d . . 1 . . .
H2 H -0.0130 0.3139 0.9577 0.054 Uiso 1 calc . . 1 R . .
C3 C 0.2946(15) 0.3442(6) 0.8357(7) 0.0343(18) Uani 1 d . . 1 . . .
C4 C 0.3878(15) 0.4246(7) 0.7498(7) 0.0370(19) Uani 1 d . . 1 . . .
H4A H 0.5458 0.4097 0.7067 0.044 Uiso 1 calc . . 1 R . .
C5 C 0.2473(15) 0.5275(7) 0.7273(7) 0.0347(18) Uani 1 d . . 1 . . .
C6 C 0.4408(17) 0.2290(7) 0.8578(7) 0.041(2) Uani 1 d . . 1 . . .
C7 C 0.3284(16) 0.6207(7) 0.6372(6) 0.0362(19) Uani 1 d . . 1 . . .
C8 C 0.5610(16) 0.6138(7) 0.5648(7) 0.0389(19) Uani 1 d . . 1 . . .
H8 H 0.6757 0.5492 0.5726 0.047 Uiso 1 calc . . 1 R . .
C9 C 0.6184(17) 0.7046(7) 0.4810(7) 0.041(2) Uani 1 d . . 1 . . .
C10 C 0.4467(17) 0.8004(8) 0.4745(8) 0.044(2) Uani 1 d . . 1 . . .
H10 H 0.4819 0.8627 0.4199 0.053 Uiso 1 calc . . 1 R . .
C11 C 0.2248(18) 0.8027(7) 0.5493(7) 0.045(2) Uani 1 d . . 1 . . .
H11 H 0.1112 0.8676 0.5448 0.054 Uiso 1 calc . . 1 R . .
C12 C 0.8730(17) 0.6968(8) 0.4048(7) 0.041(2) Uani 1 d . . 1 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl1 2.299(3) . ?
Pd1 Cl2 2.302(3) . ?
Pd1 N1 2.039(7) . ?
Pd1 N2 2.055(7) . ?
Co1 O1 2.092(5) 2_657 ?
Co1 O1 2.092(5) . ?
Co1 O5 2.057(6) . ?
Co1 O5 2.057(6) 2_657 ?
Co1 O6 2.144(6) . ?
Co1 O6 2.144(6) 2_657 ?
O1 C6 1.254(10) . ?
O2 C6 1.248(10) . ?
O3 C12 1.205(11) . ?
O4 H4 0.8200 . ?
O4 C12 1.311(10) . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8500 . ?
O6 H6A 0.8499 . ?
O6 H6B 0.8500 . ?
N1 C1 1.323(11) . ?
N1 C5 1.372(10) . ?
N2 C7 1.354(10) . ?
N2 C11 1.315(11) . ?
C1 H1 0.9300 . ?
C1 C2 1.379(11) . ?
C2 H2 0.9300 . ?
C2 C3 1.401(12) . ?
C3 C4 1.372(11) . ?
C3 C6 1.517(11) . ?
C4 H4A 0.9300 . ?
C4 C5 1.380(11) . ?
C5 C7 1.483(11) . ?
C7 C8 1.399(11) . ?
C8 H8 0.9300 . ?
C8 C9 1.390(12) . ?
C9 C10 1.384(12) . ?
C9 C12 1.512(12) . ?
C10 H10 0.9300 . ?
C10 C11 1.369(12) . ?
C11 H11 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 Cl2 90.35(10) . . ?
N1 Pd1 Cl1 94.1(2) . . ?
N1 Pd1 Cl2 175.6(2) . . ?
N1 Pd1 N2 81.6(3) . . ?
N2 Pd1 Cl1 175.53(18) . . ?
N2 Pd1 Cl2 94.00(19) . . ?
O1 Co1 O1 180.000(2) 2_657 . ?
O1 Co1 O6 86.5(2) . 2_657 ?
O1 Co1 O6 86.5(2) 2_657 . ?
O1 Co1 O6 93.5(2) 2_657 2_657 ?
O1 Co1 O6 93.5(2) . . ?
O5 Co1 O1 92.8(3) . . ?
O5 Co1 O1 87.2(3) . 2_657 ?
O5 Co1 O1 92.8(3) 2_657 2_657 ?
O5 Co1 O1 87.2(3) 2_657 . ?
O5 Co1 O5 180.000(1) 2_657 . ?
O5 Co1 O6 91.9(3) . . ?
O5 Co1 O6 88.1(3) 2_657 . ?
O5 Co1 O6 91.9(3) 2_657 2_657 ?
O5 Co1 O6 88.1(3) . 2_657 ?
O6 Co1 O6 180.000(1) . 2_657 ?
C6 O1 Co1 126.4(5) . . ?
C12 O4 H4 109.4 . . ?
Co1 O5 H5A 119.5 . . ?
Co1 O5 H5B 120.5 . . ?
H5A O5 H5B 120.0 . . ?
Co1 O6 H6A 120.3 . . ?
Co1 O6 H6B 119.7 . . ?
H6A O6 H6B 120.0 . . ?
C1 N1 Pd1 126.8(6) . . ?
C1 N1 C5 119.4(7) . . ?
C5 N1 Pd1 113.8(5) . . ?
C7 N2 Pd1 112.8(5) . . ?
C11 N2 Pd1 126.6(5) . . ?
C11 N2 C7 120.6(7) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.3(8) . . ?
C2 C1 H1 118.4 . . ?
C1 C2 H2 121.2 . . ?
C1 C2 C3 117.6(8) . . ?
C3 C2 H2 121.2 . . ?
C2 C3 C6 119.9(7) . . ?
C4 C3 C2 119.5(7) . . ?
C4 C3 C6 120.5(7) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 C3 120.0(7) . . ?
C5 C4 H4A 120.0 . . ?
N1 C5 C4 120.2(8) . . ?
N1 C5 C7 114.9(7) . . ?
C4 C5 C7 124.9(7) . . ?
O1 C6 C3 116.4(7) . . ?
O2 C6 O1 125.0(8) . . ?
O2 C6 C3 118.6(7) . . ?
N2 C7 C5 117.0(7) . . ?
N2 C7 C8 119.9(8) . . ?
C8 C7 C5 123.1(7) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.1(8) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 C12 118.6(7) . . ?
C10 C9 C8 118.6(8) . . ?
C10 C9 C12 122.7(8) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.4(9) . . ?
C11 C10 H10 120.3 . . ?
N2 C11 C10 122.3(8) . . ?
N2 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
O3 C12 O4 126.3(9) . . ?
O3 C12 C9 121.2(8) . . ?
O4 C12 C9 112.5(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C1 C2 -179.7(7) . . . . ?
Pd1 N1 C5 C4 179.3(6) . . . . ?
Pd1 N1 C5 C7 -0.3(9) . . . . ?
Pd1 N2 C7 C5 0.7(10) . . . . ?
Pd1 N2 C7 C8 -178.8(6) . . . . ?
Pd1 N2 C11 C10 -180.0(7) . . . . ?
Co1 O1 C6 O2 10.5(14) . . . . ?
Co1 O1 C6 C3 -170.6(5) . . . . ?
Cl1 Pd1 N1 C1 -0.7(8) . . . . ?
Cl1 Pd1 N1 C5 179.5(6) . . . . ?
Cl1 Pd1 N2 C7 -13(3) . . . . ?
Cl1 Pd1 N2 C11 167(2) . . . . ?
Cl2 Pd1 N1 C1 -176(2) . . . . ?
Cl2 Pd1 N1 C5 4(3) . . . . ?
Cl2 Pd1 N2 C7 179.6(6) . . . . ?
Cl2 Pd1 N2 C11 0.3(8) . . . . ?
O1 Co1 O1 C6 51(100) 2_657 . . . ?
O5 Co1 O1 C6 -110.9(8) . . . . ?
O5 Co1 O1 C6 69.1(8) 2_657 . . . ?
O6 Co1 O1 C6 161.1(8) 2_657 . . . ?
O6 Co1 O1 C6 -18.9(8) . . . . ?
N1 Pd1 N2 C7 -0.7(6) . . . . ?
N1 Pd1 N2 C11 -179.9(8) . . . . ?
N1 C1 C2 C3 0.6(15) . . . . ?
N1 C5 C7 N2 -0.3(11) . . . . ?
N1 C5 C7 C8 179.2(8) . . . . ?
N2 Pd1 N1 C1 -179.7(8) . . . . ?
N2 Pd1 N1 C5 0.5(6) . . . . ?
N2 C7 C8 C9 -2.0(13) . . . . ?
C1 N1 C5 C4 -0.6(13) . . . . ?
C1 N1 C5 C7 179.9(8) . . . . ?
C1 C2 C3 C4 -0.8(14) . . . . ?
C1 C2 C3 C6 -177.4(8) . . . . ?
C2 C3 C4 C5 0.4(14) . . . . ?
C2 C3 C6 O1 1.4(13) . . . . ?
C2 C3 C6 O2 -179.6(9) . . . . ?
C3 C4 C5 N1 0.3(13) . . . . ?
C3 C4 C5 C7 179.8(8) . . . . ?
C4 C3 C6 O1 -175.1(8) . . . . ?
C4 C3 C6 O2 3.9(14) . . . . ?
C4 C5 C7 N2 -179.8(8) . . . . ?
C4 C5 C7 C8 -0.3(14) . . . . ?
C5 N1 C1 C2 0.1(14) . . . . ?
C5 C7 C8 C9 178.5(8) . . . . ?
C6 C3 C4 C5 177.0(8) . . . . ?
C7 N2 C11 C10 0.8(14) . . . . ?
C7 C8 C9 C10 2.2(14) . . . . ?
C7 C8 C9 C12 178.7(8) . . . . ?
C8 C9 C10 C11 -0.9(14) . . . . ?
C8 C9 C12 O3 -0.4(14) . . . . ?
C8 C9 C12 O4 179.7(8) . . . . ?
C9 C10 C11 N2 -0.6(15) . . . . ?
C10 C9 C12 O3 176.0(9) . . . . ?
C10 C9 C12 O4 -3.9(13) . . . . ?
C11 N2 C7 C5 -180.0(8) . . . . ?
C11 N2 C7 C8 0.5(13) . . . . ?
C12 C9 C10 C11 -177.3(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
