# 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_[Pd{OC(CH3)2(1-H)}](SbF6)
_database_code_depnum_ccdc_archive 'CCDC 987857'
_audit_update_record             
;
2015-08-14 deposited with the CCDC.
2016-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 N5 O Pd, F6 Sb'
_chemical_formula_sum            'C18 H18 F6 N5 O Pd Sb'
_chemical_formula_weight         662.52

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'
F F 0.0171 0.0103 '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'
Sb Sb -0.5866 1.5461 '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                   12.8162(3)
_cell_length_b                   8.13176(16)
_cell_length_c                   20.6429(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.132(2)
_cell_angle_gamma                90.00
_cell_volume                     2117.82(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    7918
_cell_measurement_theta_min      2.9743
_cell_measurement_theta_max      32.5068

_exptl_crystal_description       'platy needles'
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 15.9825
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22209
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         32.58
_reflns_number_total             7140
_reflns_number_gt                5857
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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)+(0.0274P)²+1.4017P] 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         7140
_refine_ls_number_parameters     335
_refine_ls_number_restraints     387
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0693
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.095
_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
Pd Pd 0.600520(13) 0.36328(2) 0.520862(8) 0.02423(5) Uani 1 1 d . . .
N1 N 0.56814(15) 0.2776(2) 0.43253(9) 0.0263(4) Uani 1 1 d . . .
C2 C 0.6367(2) 0.3132(3) 0.39178(12) 0.0311(5) Uani 1 1 d . . .
C3 C 0.6186(2) 0.2500(4) 0.32856(13) 0.0392(6) Uani 1 1 d . . .
H3A H 0.6656 0.2730 0.2989 0.047 Uiso 1 1 calc R . .
C4 C 0.5305(2) 0.1528(4) 0.30981(13) 0.0433(7) Uani 1 1 d . . .
H4A H 0.5171 0.1083 0.2666 0.052 Uiso 1 1 calc R . .
C5 C 0.4606(2) 0.1178(4) 0.35249(13) 0.0381(6) Uani 1 1 d . . .
H5A H 0.4001 0.0505 0.3389 0.046 Uiso 1 1 calc R . .
C6 C 0.48167(19) 0.1840(3) 0.41564(12) 0.0294(5) Uani 1 1 d . . .
C7 C 0.7258(2) 0.4186(3) 0.42292(13) 0.0315(5) Uani 1 1 d . . .
N8 N 0.72701(16) 0.4506(3) 0.48848(10) 0.0281(4) Uani 1 1 d . . .
C9 C 0.80369(19) 0.5434(3) 0.52400(13) 0.0294(5) Uani 1 1 d . . .
C10 C 0.8834(2) 0.6120(3) 0.49225(15) 0.0378(6) Uani 1 1 d . . .
H10A H 0.9375 0.6791 0.5162 0.045 Uiso 1 1 calc R . .
C11 C 0.8816(2) 0.5811(4) 0.42735(15) 0.0399(6) Uani 1 1 d . . .
H11A H 0.9351 0.6265 0.4062 0.048 Uiso 1 1 calc R . .
C12 C 0.8018(2) 0.4830(4) 0.39116(14) 0.0387(6) Uani 1 1 d . . .
H12A H 0.8006 0.4618 0.3458 0.046 Uiso 1 1 calc R . .
N13 N 0.80180(17) 0.5733(3) 0.58781(11) 0.0332(5) Uani 1 1 d D . .
H13A H 0.8595(16) 0.628(4) 0.6078(15) 0.056(10) Uiso 1 1 d D . .
C14 C 0.7462(2) 0.4759(3) 0.63300(12) 0.0311(5) Uani 1 1 d . . .
O15 O 0.63842(13) 0.4636(2) 0.60950(8) 0.0316(4) Uani 1 1 d . . .
C16 C 0.7610(2) 0.5706(4) 0.69764(14) 0.0413(6) Uani 1 1 d . . .
H16A H 0.7271 0.6786 0.6903 0.062 Uiso 1 1 calc R . .
H16B H 0.8369 0.5850 0.7144 0.062 Uiso 1 1 calc R . .
H16C H 0.7287 0.5091 0.7298 0.062 Uiso 1 1 calc R . .
C17 C 0.7984(2) 0.3068(3) 0.64296(14) 0.0411(6) Uani 1 1 d . . .
H17A H 0.7881 0.2479 0.6009 0.062 Uiso 1 1 calc R . .
H17B H 0.7662 0.2440 0.6749 0.062 Uiso 1 1 calc R . .
H17C H 0.8744 0.3200 0.6595 0.062 Uiso 1 1 calc R . .
C18 C 0.42091(19) 0.1614(3) 0.46932(12) 0.0291(5) Uani 1 1 d . . .
N19 N 0.46403(15) 0.2388(2) 0.52751(10) 0.0266(4) Uani 1 1 d . . .
C20 C 0.41647(18) 0.2247(3) 0.58056(12) 0.0297(5) Uani 1 1 d . . .
C21 C 0.3218(2) 0.1314(3) 0.57614(14) 0.0345(5) Uani 1 1 d . . .
H21A H 0.2883 0.1203 0.6135 0.041 Uiso 1 1 calc R . .
C22 C 0.2790(2) 0.0576(3) 0.51818(15) 0.0373(6) Uani 1 1 d . . .
H22A H 0.2152 -0.0037 0.5150 0.045 Uiso 1 1 calc R . .
C23 C 0.3289(2) 0.0722(3) 0.46356(14) 0.0356(6) Uani 1 1 d . . .
H23A H 0.2996 0.0211 0.4230 0.043 Uiso 1 1 calc R . .
N24 N 0.46131(18) 0.2996(3) 0.63605(11) 0.0352(5) Uani 1 1 d D . .
H24A H 0.5232(13) 0.354(3) 0.6393(16) 0.046(9) Uiso 1 1 d D . .
H24B H 0.426(2) 0.299(4) 0.6700(10) 0.053(10) Uiso 1 1 d D . .
Sb Sb 0.45960(5) 0.42507(11) 0.82890(4) 0.03120(13) Uani 0.913(6) 1 d PDU A 1
F1 F 0.5508(2) 0.4542(4) 0.76880(14) 0.0718(8) Uani 0.913(6) 1 d PDU A 1
F2 F 0.5710(2) 0.4601(5) 0.89829(13) 0.0789(10) Uani 0.913(6) 1 d PDU A 1
F3 F 0.49166(19) 0.1987(3) 0.83303(15) 0.0590(7) Uani 0.913(6) 1 d PDU A 1
F4 F 0.3503(2) 0.3812(4) 0.75787(12) 0.0599(7) Uani 0.913(6) 1 d PDU A 1
F5 F 0.4285(3) 0.6490(3) 0.82392(12) 0.0588(7) Uani 0.913(6) 1 d PDU A 1
F6 F 0.3660(3) 0.3933(4) 0.88682(15) 0.0637(7) Uani 0.913(6) 1 d PDU A 1
Sb' Sb 0.4603(7) 0.4456(15) 0.8386(6) 0.057(2) Uani 0.087(6) 1 d PDU A 2
F1' F 0.5525(18) 0.494(3) 0.7824(12) 0.087(6) Uiso 0.087(6) 1 d PDU A 2
F2' F 0.5418(17) 0.554(4) 0.9067(9) 0.077(5) Uiso 0.087(6) 1 d PDU A 2
F3' F 0.527(2) 0.247(3) 0.8620(14) 0.076(5) Uiso 0.087(6) 1 d PDU A 2
F4' F 0.371(2) 0.334(3) 0.7693(12) 0.066(5) Uiso 0.087(6) 1 d PDU A 2
F5' F 0.3813(17) 0.637(2) 0.8134(11) 0.050(5) Uiso 0.087(6) 1 d PDU A 2
F6' F 0.3605(18) 0.394(3) 0.8932(13) 0.066(5) Uiso 0.087(6) 1 d PDU A 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
Pd N1 1.928(2) . ?
Pd O15 1.9841(17) . ?
Pd N8 1.990(2) . ?
Pd N19 2.046(2) . ?
N1 C6 1.339(3) . ?
N1 C2 1.351(3) . ?
C2 C3 1.384(4) . ?
C2 C7 1.481(4) . ?
C3 C4 1.376(4) . ?
C4 C5 1.392(4) . ?
C5 C6 1.392(4) . ?
C6 C18 1.474(4) . ?
C7 C12 1.370(4) . ?
C7 N8 1.376(3) . ?
N8 C9 1.349(3) . ?
C9 N13 1.344(3) . ?
C9 C10 1.421(3) . ?
C10 C11 1.359(4) . ?
C11 C12 1.404(4) . ?
N13 C14 1.497(3) . ?
C14 O15 1.384(3) . ?
C14 C16 1.523(4) . ?
C14 C17 1.527(4) . ?
C18 C23 1.372(4) . ?
C18 N19 1.382(3) . ?
N19 C20 1.349(3) . ?
C20 N24 1.335(3) . ?
C20 C21 1.421(4) . ?
C21 C22 1.364(4) . ?
C22 C23 1.395(4) . ?
Sb F6 1.855(2) . ?
Sb F2 1.858(2) . ?
Sb F5 1.863(2) . ?
Sb F1 1.863(2) . ?
Sb F4 1.876(2) . ?
Sb F3 1.885(2) . ?
Sb' F2' 1.824(11) . ?
Sb' F1' 1.838(12) . ?
Sb' F3' 1.851(12) . ?
Sb' F5' 1.877(11) . ?
Sb' F6' 1.895(12) . ?
Sb' F4' 1.900(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd O15 176.32(8) . . ?
N1 Pd N8 82.17(9) . . ?
O15 Pd N8 94.67(8) . . ?
N1 Pd N19 80.81(8) . . ?
O15 Pd N19 102.41(7) . . ?
N8 Pd N19 162.84(8) . . ?
C6 N1 C2 124.0(2) . . ?
C6 N1 Pd 118.84(16) . . ?
C2 N1 Pd 117.14(17) . . ?
N1 C2 C3 119.2(3) . . ?
N1 C2 C7 113.0(2) . . ?
C3 C2 C7 127.8(2) . . ?
C4 C3 C2 118.2(3) . . ?
C3 C4 C5 121.8(3) . . ?
C4 C5 C6 118.2(3) . . ?
N1 C6 C5 118.6(2) . . ?
N1 C6 C18 113.4(2) . . ?
C5 C6 C18 127.9(2) . . ?
C12 C7 N8 120.9(3) . . ?
C12 C7 C2 124.9(2) . . ?
N8 C7 C2 114.2(2) . . ?
C9 N8 C7 121.4(2) . . ?
C9 N8 Pd 125.15(17) . . ?
C7 N8 Pd 113.23(17) . . ?
N13 C9 N8 119.8(2) . . ?
N13 C9 C10 121.3(2) . . ?
N8 C9 C10 118.9(2) . . ?
C11 C10 C9 119.6(3) . . ?
C10 C11 C12 120.9(2) . . ?
C7 C12 C11 118.4(3) . . ?
C9 N13 C14 127.4(2) . . ?
O15 C14 N13 112.0(2) . . ?
O15 C14 C16 107.9(2) . . ?
N13 C14 C16 106.2(2) . . ?
O15 C14 C17 111.6(2) . . ?
N13 C14 C17 108.3(2) . . ?
C16 C14 C17 110.7(2) . . ?
C14 O15 Pd 114.85(15) . . ?
C23 C18 N19 121.5(2) . . ?
C23 C18 C6 124.1(2) . . ?
N19 C18 C6 114.4(2) . . ?
C20 N19 C18 119.9(2) . . ?
C20 N19 Pd 127.61(17) . . ?
C18 N19 Pd 112.51(16) . . ?
N24 C20 N19 118.0(2) . . ?
N24 C20 C21 122.2(2) . . ?
N19 C20 C21 119.8(2) . . ?
C22 C21 C20 119.9(3) . . ?
C21 C22 C23 120.1(2) . . ?
C18 C23 C22 118.9(3) . . ?
F6 Sb F2 91.19(14) . . ?
F6 Sb F5 90.90(12) . . ?
F2 Sb F5 91.17(13) . . ?
F6 Sb F1 178.34(12) . . ?
F2 Sb F1 90.40(13) . . ?
F5 Sb F1 89.53(12) . . ?
F6 Sb F4 89.91(12) . . ?
F2 Sb F4 177.44(14) . . ?
F5 Sb F4 91.13(12) . . ?
F1 Sb F4 88.48(12) . . ?
F6 Sb F3 89.73(12) . . ?
F2 Sb F3 89.04(12) . . ?
F5 Sb F3 179.34(11) . . ?
F1 Sb F3 89.83(11) . . ?
F4 Sb F3 88.65(11) . . ?
F2' Sb' F1' 92.2(7) . . ?
F2' Sb' F3' 92.6(6) . . ?
F1' Sb' F3' 91.9(7) . . ?
F2' Sb' F5' 91.2(6) . . ?
F1' Sb' F5' 91.3(7) . . ?
F3' Sb' F5' 175.0(8) . . ?
F2' Sb' F6' 90.2(7) . . ?
F1' Sb' F6' 177.4(8) . . ?
F3' Sb' F6' 88.9(7) . . ?
F5' Sb' F6' 87.8(6) . . ?
F2' Sb' F4' 177.7(8) . . ?
F1' Sb' F4' 89.9(7) . . ?
F3' Sb' F4' 88.3(6) . . ?
F5' Sb' F4' 87.8(6) . . ?
F6' Sb' F4' 87.7(6) . . ?

_diffrn_measured_fraction_theta_max 0.925
_diffrn_reflns_theta_full        31.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.165

#===END


