# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2014

data_publication_text
_publ_contact_author_name        'Mark J. Muldoon'
_publ_contact_author_address     
;Centre for the Theory and Application of Catalysis (CenTACat)' 
'and Queen's University Ionic Liquid Laboratories (QUILL),' 
'School of Chemistry and Chemical Engineering,' 
'Queen's University Belfast, UK
;
_publ_contact_author_email       m.j.muldoon@qub.ac.uk
_publ_contact_author_phone       '+44 (0)28 9097 4420 '
_publ_contact_author_fax         '+44 (0)28 9097 6524'
loop_
_publ_author_name
_publ_author_address
'Dornan, Laura M.'
;Centre for the Theory and Application of Catalysis (CenTACat)' 
'and Queen's University Ionic Liquid Laboratories (QUILL),' 
'School of Chemistry and Chemical Engineering,' 
'Queen's University Belfast, UK
;
"Clendenning, Gráinne M.A."
;Centre for the Theory and Application of Catalysis (CenTACat)' 
'and Queen's University Ionic Liquid Laboratories (QUILL),' 
'School of Chemistry and Chemical Engineering,' 
'Queen's University Belfast, UK
;
'Pitak, Mateusz B.'
;National Crystallography Service, School of Chemistry,
University of Southampton, Highfield Campus, Southampton SO17 1BJ UK
;
'Coles, Simon J.'
;National Crystallography Service, School of Chemistry,
University of Southampton, Highfield Campus, Southampton SO17 1BJ UK
;
'Muldoon, Mark J.'
;Centre for the Theory and Application of Catalysis (CenTACat)' 
'and Queen's University Ionic Liquid Laboratories (QUILL),' 
'School of Chemistry and Chemical Engineering,' 
'Queen's University Belfast, UK
;

 
data_PdHCADMF
 
_audit_creation_method            SHELXL-2014
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C13 H12 N2 O4 Pd'
_chemical_formula_sum
 'C13 H12 N2 O4 Pd' 
_chemical_formula_weight          366.65

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'
 '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       orthorhombic
_space_group_IT_number            33
_space_group_name_H-M_alt         'P n a 21'
_space_group_name_Hall            'P 2c -2n'
 
_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+1/2'
 'x+1/2, -y+1/2, z'
 
_cell_length_a                    10.9190(7)
_cell_length_b                    23.8725(14)
_cell_length_c                    4.8372(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1260.88(13)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       2.91 
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             yellow 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.931          
_exptl_crystal_F_000              728
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.160
_exptl_crystal_size_mid           0.060
_exptl_crystal_size_min           0.020
_exptl_absorpt_coefficient_mu     1.487
_shelx_estimated_absorpt_T_min    0.797
_shelx_estimated_absorpt_T_max    0.971
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.797 
_exptl_absorpt_correction_T_max   0.971 
_exptl_absorpt_process_details    'SADABS 2007/2 (Sheldrick, G.M., 2007)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   '10cm confocal mirrors'
_diffrn_measurement_device_type   
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method        'φ & ω scans'
_diffrn_detector_area_resol_mean  '4096x4096pixels / 62x62mm'
_diffrn_reflns_number             8455
_diffrn_reflns_av_unetI/netI      0.0559
_diffrn_reflns_av_R_equivalents   0.0509
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -27
_diffrn_reflns_limit_k_max        30
_diffrn_reflns_limit_l_min        -6
_diffrn_reflns_limit_l_max        6
_diffrn_reflns_theta_min          3.168
_diffrn_reflns_theta_max          27.561
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.992
_diffrn_measured_fraction_theta_full  0.996
_diffrn_reflns_Laue_measured_fraction_max    0.992
_diffrn_reflns_Laue_measured_fraction_full   0.996
_diffrn_reflns_point_group_measured_fraction_max   0.993
_diffrn_reflns_point_group_measured_fraction_full  0.997
_reflns_number_total              2621
_reflns_number_gt                 2242
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.789
_reflns_Friedel_fraction_max      0.995
_reflns_Friedel_fraction_full     0.999
 
_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        'COLLECT (Hooft, R.W.W., 1998)' 
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'  
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL2014 (Sheldrick, 2008)'
_computing_molecular_graphics     'MERCURY 3.1(J.Appl.Cryst.41,466-470, 2008'
_computing_publication_material   'WinGX, ver.2013.3 (L.J. Farrugia, J.App.Cryst.(2012),45,849-854)'
 
_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)+9.6050P] 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_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.14(10)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          2621
_refine_ls_number_parameters      184
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0620
_refine_ls_R_factor_gt            0.0486
_refine_ls_wR_factor_ref          0.1057
_refine_ls_wR_factor_gt           0.0985
_refine_ls_goodness_of_fit_ref    1.087
_refine_ls_restrained_S_all       1.087
_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
C9 C 0.1205(9) 0.2144(4) 0.808(2) 0.023(3) Uani 1 1 d . . . . .
C8 C 0.0065(10) 0.2357(4) 0.913(2) 0.024(2) Uani 1 1 d . . . . .
H8 H -0.0282 0.2690 0.8392 0.029 Uiso 1 1 calc R U . . .
C7 C -0.0513(10) 0.2069(4) 1.121(2) 0.024(2) Uani 1 1 d . . . . .
H7 H -0.1248 0.2216 1.1969 0.029 Uiso 1 1 calc R U . . .
C6 C -0.0044(8) 0.1558(4) 1.227(3) 0.0227(19) Uani 1 1 d . . . . .
C5 C -0.0554(11) 0.1214(5) 1.436(2) 0.031(3) Uani 1 1 d . . . . .
H5 H -0.1300 0.1316 1.5239 0.037 Uiso 1 1 calc R U . . .
C4 C 0.0041(11) 0.0734(5) 1.510(2) 0.034(3) Uani 1 1 d . . . . .
H4 H -0.0294 0.0518 1.6562 0.041 Uiso 1 1 calc R U . . .
C3 C 0.1132(11) 0.0537(4) 1.382(2) 0.030(3) Uani 1 1 d . . . . .
H3 H 0.1486 0.0192 1.4378 0.036 Uiso 1 1 calc R U . . .
C2 C 0.1672(9) 0.0852(4) 1.1755(19) 0.023(3) Uani 1 1 d . . . . .
C1 C 0.1035(9) 0.1364(4) 1.106(2) 0.020(2) Uani 1 1 d . . . . .
C13 C 0.1972(9) 0.2375(4) 0.580(2) 0.021(2) Uani 1 1 d . . . . .
C10 C 0.5011(10) 0.1159(4) 0.366(2) 0.027(2) Uani 1 1 d . . . . .
H10 H 0.4738 0.1512 0.2990 0.032 Uiso 1 1 calc R U . . .
C11 C 0.6338(10) 0.0352(4) 0.316(3) 0.040(4) Uani 1 1 d . . . . .
H11A H 0.5807 0.0205 0.4625 0.060 Uiso 1 1 calc R U . . .
H11B H 0.7186 0.0365 0.3823 0.060 Uiso 1 1 calc R U . . .
H11C H 0.6287 0.0108 0.1536 0.060 Uiso 1 1 calc R U . . .
C12 C 0.6599(10) 0.1187(5) 0.016(2) 0.031(3) Uani 1 1 d . . . . .
H12A H 0.6481 0.0974 -0.1549 0.047 Uiso 1 1 calc R U . . .
H12B H 0.7474 0.1204 0.0604 0.047 Uiso 1 1 calc R U . . .
H12C H 0.6279 0.1567 -0.0077 0.047 Uiso 1 1 calc R U . . .
N1 N 0.1604(7) 0.1671(3) 0.9037(16) 0.0174(17) Uani 1 1 d . . . . .
N2 N 0.5944(6) 0.0910(3) 0.242(3) 0.0253(15) Uani 1 1 d . . . . .
O1 O 0.2694(7) 0.0730(3) 1.0351(16) 0.0242(16) Uani 1 1 d . . . . .
O2 O 0.2903(6) 0.2049(3) 0.5100(16) 0.0260(16) Uani 1 1 d . . . . .
O4 O 0.1764(7) 0.2832(3) 0.4784(18) 0.0315(18) Uani 1 1 d . . . . .
O3 O 0.4481(6) 0.0946(3) 0.5673(16) 0.0268(16) Uani 1 1 d . . . . .
Pd1 Pd 0.30045(5) 0.13353(3) 0.7436(3) 0.02131(18) 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
C9 N1 1.294(12) . ?
C9 C8 1.436(14) . ?
C9 C13 1.493(13) . ?
C8 C7 1.375(14) . ?
C8 H8 0.9500 . ?
C7 C6 1.417(14) . ?
C7 H7 0.9500 . ?
C6 C1 1.394(13) . ?
C6 C5 1.419(17) . ?
C5 C4 1.364(16) . ?
C5 H5 0.9500 . ?
C4 C3 1.422(17) . ?
C4 H4 0.9500 . ?
C3 C2 1.382(14) . ?
C3 H3 0.9500 . ?
C2 O1 1.338(12) . ?
C2 C1 1.446(13) . ?
C1 N1 1.371(12) . ?
C13 O4 1.217(12) . ?
C13 O2 1.324(11) . ?
C10 O3 1.242(13) . ?
C10 N2 1.323(14) . ?
C10 H10 0.9500 . ?
C11 N2 1.444(13) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.463(16) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N1 Pd1 1.893(8) . ?
O1 Pd1 2.047(7) . ?
O2 Pd1 2.047(7) . ?
O3 Pd1 2.048(7) . ?
 
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 C9 C8 118.4(9) . . ?
N1 C9 C13 113.4(9) . . ?
C8 C9 C13 127.9(9) . . ?
C7 C8 C9 118.5(9) . . ?
C7 C8 H8 120.8 . . ?
C9 C8 H8 120.8 . . ?
C8 C7 C6 122.0(10) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C1 C6 C7 116.1(11) . . ?
C1 C6 C5 116.0(10) . . ?
C7 C6 C5 127.8(10) . . ?
C4 C5 C6 119.1(11) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C4 C3 124.2(11) . . ?
C5 C4 H4 117.9 . . ?
C3 C4 H4 117.9 . . ?
C2 C3 C4 119.5(10) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
O1 C2 C3 127.1(10) . . ?
O1 C2 C1 117.9(8) . . ?
C3 C2 C1 115.0(9) . . ?
N1 C1 C6 120.3(9) . . ?
N1 C1 C2 113.6(8) . . ?
C6 C1 C2 126.1(10) . . ?
O4 C13 O2 124.5(9) . . ?
O4 C13 C9 121.7(9) . . ?
O2 C13 C9 113.7(8) . . ?
O3 C10 N2 122.0(11) . . ?
O3 C10 H10 119.0 . . ?
N2 C10 H10 119.0 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 N1 C1 124.6(8) . . ?
C9 N1 Pd1 119.7(7) . . ?
C1 N1 Pd1 115.5(6) . . ?
C10 N2 C11 122.1(11) . . ?
C10 N2 C12 120.8(9) . . ?
C11 N2 C12 117.1(9) . . ?
C2 O1 Pd1 109.5(6) . . ?
C13 O2 Pd1 113.0(6) . . ?
C10 O3 Pd1 120.5(7) . . ?
N1 Pd1 O1 83.3(3) . . ?
N1 Pd1 O2 80.2(3) . . ?
O1 Pd1 O2 163.4(3) . . ?
N1 Pd1 O3 177.8(3) . . ?
O1 Pd1 O3 95.6(3) . . ?
O2 Pd1 O3 101.0(3) . . ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C8 H8 O2  0.95 2.62 3.373(13) 136.8 4_455
C10 H10 O2  0.95 2.59 3.209(13) 123.2 .
C12 H12A O3  0.98 2.57 3.224(14) 124.6 1_554
 
_refine_diff_density_max    1.031
_refine_diff_density_min   -0.885
_refine_diff_density_rms    0.157

_shelxl_version_number 2014-1



#===END
##############################################################

 
data_PdHSADMF
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C12 H12 N2 O5 Pd S'
_chemical_formula_sum
 'C12 H12 N2 O5 Pd S'
_chemical_formula_weight          402.70
 
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'
 '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    P21/c
_symmetry_space_group_name_Hall   '-P 2ybc'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    19.681(3)
_cell_length_b                    7.1866(8)
_cell_length_c                    20.443(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  107.332(2)
_cell_angle_gamma                 90.00
_cell_volume                      2760.2(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     14148
_cell_measurement_theta_min       2.5
_cell_measurement_theta_max       34.8
 
_exptl_crystal_description        needle
_exptl_crystal_colour             Yellow
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.02
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.938
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1600
_exptl_absorpt_coefficient_mu     1.518
_exptl_absorpt_correction_type    Multi-scan
_exptl_absorpt_correction_T_min   0.7510
_exptl_absorpt_correction_T_max   0.9703
_exptl_absorpt_process_details    'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_source_power                    1.2
_diffrn_source_voltage                  50.0
_diffrn_source_current                  24.0
_diffrn_radiation_wavelength            0.71075
_diffrn_radiation_type                  'Mo K\a'
_diffrn_source                          'Rotating Anode'
_diffrn_radiation_monochromator         'Confocal'
_diffrn_measurement_specimen_support    'Mitegen'
_diffrn_detector                        'CCD'
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean        28.5714
_diffrn_measurement_method              'profile data from ω-scans'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             34176
_diffrn_reflns_av_R_equivalents   0.0453
_diffrn_reflns_av_sigmaI/netI     0.0324
_diffrn_reflns_limit_h_min        -25
_diffrn_reflns_limit_h_max        25
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          3.02
_diffrn_reflns_theta_max          27.48
_reflns_number_total              6318
_reflns_number_gt                 5831
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_cell_refinement        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction         'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_solution     'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     'MERCURY 3.1(J.Appl.Cryst.41,466-470, 2008'
_computing_publication_material   'WinGX, ver.2013.3 (L.J. Farrugia, J.App.Cryst.(2012),45,849-854)'
 
_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 > 2σ(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)+(0.0617P)²+2.4156P] 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          6318
_refine_ls_number_parameters      383
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0449
_refine_ls_R_factor_gt            0.0409
_refine_ls_wR_factor_ref          0.1060
_refine_ls_wR_factor_gt           0.1027
_refine_ls_goodness_of_fit_ref    1.072
_refine_ls_restrained_S_all       1.072
_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
C1 C 0.17702(16) 0.2246(4) 0.49334(17) 0.0186(6) Uani 1 1 d . . .
C2 C 0.15641(18) 0.1897(5) 0.42185(18) 0.0234(7) Uani 1 1 d . . .
C3 C 0.08556(19) 0.2223(5) 0.38633(19) 0.0272(8) Uani 1 1 d . . .
H3 H 0.0689 0.2054 0.3381 0.033 Uiso 1 1 calc R . .
C4 C 0.03853(18) 0.2806(5) 0.4223(2) 0.0288(8) Uani 1 1 d . . .
H4 H -0.0097 0.3022 0.3969 0.035 Uiso 1 1 calc R . .
C5 C 0.05813(19) 0.3081(5) 0.4919(2) 0.0281(8) Uani 1 1 d . . .
H5 H 0.0240 0.3451 0.5138 0.034 Uiso 1 1 calc R . .
C6 C 0.13069(17) 0.2802(5) 0.53066(18) 0.0223(7) Uani 1 1 d . . .
C7 C 0.16040(19) 0.2956(5) 0.60246(18) 0.0238(7) Uani 1 1 d . . .
H7 H 0.1307 0.3306 0.6295 0.029 Uiso 1 1 calc R . .
C8 C 0.23163(18) 0.2609(5) 0.63435(18) 0.0234(7) Uani 1 1 d . . .
H8 H 0.2510 0.2702 0.6827 0.028 Uiso 1 1 calc R . .
C9 C 0.27471(17) 0.2113(5) 0.59323(17) 0.0207(7) Uani 1 1 d . . .
C10 C 0.32503(19) -0.0368(5) 0.34574(19) 0.0237(7) Uani 1 1 d . . .
H10 H 0.2756 -0.0104 0.3285 0.028 Uiso 1 1 calc R . .
C11 C 0.3177(2) -0.1574(6) 0.23349(19) 0.0297(8) Uani 1 1 d . . .
H11A H 0.2669 -0.1329 0.2257 0.045 Uiso 1 1 calc R . .
H11B H 0.3245 -0.2892 0.2250 0.045 Uiso 1 1 calc R . .
H11C H 0.3352 -0.0807 0.2023 0.045 Uiso 1 1 calc R . .
C12 C 0.43296(19) -0.1608(5) 0.3271(2) 0.0298(8) Uani 1 1 d . . .
H12A H 0.4536 -0.1265 0.3753 0.045 Uiso 1 1 calc R . .
H12B H 0.4577 -0.0937 0.2992 0.045 Uiso 1 1 calc R . .
H12C H 0.4382 -0.2951 0.3218 0.045 Uiso 1 1 calc R . .
C101 C 0.18669(17) 0.6671(5) 0.43158(16) 0.0188(6) Uani 1 1 d . . .
C102 C 0.25482(17) 0.6354(5) 0.47918(17) 0.0189(6) Uani 1 1 d . . .
C103 C 0.26277(18) 0.6856(5) 0.54653(17) 0.0218(7) Uani 1 1 d . . .
H103 H 0.3074 0.6700 0.5804 0.026 Uiso 1 1 calc R . .
C104 C 0.20417(18) 0.7602(5) 0.56486(17) 0.0229(7) Uani 1 1 d . . .
H104 H 0.2105 0.7904 0.6115 0.028 Uiso 1 1 calc R . .
C105 C 0.13803(18) 0.7910(5) 0.51747(18) 0.0219(7) Uani 1 1 d . . .
H105 H 0.1002 0.8426 0.5316 0.026 Uiso 1 1 calc R . .
C106 C 0.12779(17) 0.7445(4) 0.44809(17) 0.0196(6) Uani 1 1 d . . .
C107 C 0.06481(18) 0.7714(5) 0.39230(17) 0.0229(7) Uani 1 1 d . . .
H107 H 0.0239 0.8236 0.4008 0.027 Uiso 1 1 calc R . .
C108 C 0.06204(18) 0.7234(5) 0.32652(18) 0.0247(7) Uani 1 1 d . . .
H108 H 0.0199 0.7422 0.2897 0.030 Uiso 1 1 calc R . .
C109 C 0.12314(17) 0.6455(5) 0.31488(17) 0.0229(7) Uani 1 1 d . . .
C110 C 0.41008(18) 0.3754(5) 0.39609(19) 0.0237(7) Uani 1 1 d . . .
H110 H 0.4021 0.3821 0.4396 0.028 Uiso 1 1 calc R . .
C111 C 0.5303(2) 0.2838(7) 0.4556(2) 0.0461(12) Uani 1 1 d . . .
H11D H 0.5118 0.2898 0.4951 0.069 Uiso 1 1 calc R . .
H11E H 0.5688 0.3747 0.4615 0.069 Uiso 1 1 calc R . .
H11F H 0.5486 0.1585 0.4522 0.069 Uiso 1 1 calc R . .
C112 C 0.4889(2) 0.3137(6) 0.3275(2) 0.0326(9) Uani 1 1 d . . .
H11G H 0.4442 0.3024 0.2903 0.049 Uiso 1 1 calc R . .
H11H H 0.5186 0.2043 0.3277 0.049 Uiso 1 1 calc R . .
H11I H 0.5141 0.4261 0.3207 0.049 Uiso 1 1 calc R . .
N1 N 0.24727(14) 0.1942(4) 0.52648(14) 0.0186(5) Uani 1 1 d . . .
N2 N 0.35705(16) -0.1116(4) 0.30446(15) 0.0227(6) Uani 1 1 d . . .
N101 N 0.18167(14) 0.6215(4) 0.36589(14) 0.0196(6) Uani 1 1 d . . .
N102 N 0.47334(15) 0.3261(4) 0.39325(17) 0.0271(7) Uani 1 1 d . . .
O1 O 0.20622(13) 0.1262(3) 0.39434(12) 0.0238(5) Uani 1 1 d . . .
O2 O 0.38573(13) 0.1246(4) 0.55671(13) 0.0286(6) Uani 1 1 d . . .
O3 O 0.35701(13) 0.0018(3) 0.40744(13) 0.0245(5) Uani 1 1 d . . .
O4 O 0.37931(14) 0.0070(4) 0.66616(15) 0.0316(6) Uani 1 1 d . . .
O5 O 0.40210(13) 0.3351(4) 0.65304(15) 0.0354(7) Uani 1 1 d . . .
O101 O 0.30597(12) 0.5605(4) 0.45629(12) 0.0208(5) Uani 1 1 d . . .
O102 O 0.20643(13) 0.4957(4) 0.25319(13) 0.0284(6) Uani 1 1 d . . .
O103 O 0.35919(12) 0.4143(4) 0.34319(13) 0.0242(5) Uani 1 1 d . . .
O104 O 0.13129(16) 0.7537(5) 0.19648(14) 0.0499(9) Uani 1 1 d . . .
O105 O 0.07884(16) 0.4502(6) 0.20290(18) 0.0602(11) Uani 1 1 d . . .
S1 S 0.36865(4) 0.16607(12) 0.62187(4) 0.02159(18) Uani 1 1 d . . .
S101 S 0.13356(5) 0.58124(17) 0.23360(5) 0.0327(2) Uani 1 1 d . . .
Pd1 Pd 0.300145(13) 0.10607(4) 0.467451(13) 0.01925(9) Uani 1 1 d . . .
Pd2 Pd 0.267451(12) 0.51658(4) 0.355268(13) 0.01825(9) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 N1 1.364(4) . ?
C1 C6 1.410(5) . ?
C1 C2 1.418(5) . ?
C2 O1 1.347(4) . ?
C2 C3 1.387(5) . ?
C3 C4 1.407(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.426(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.413(5) . ?
C7 C8 1.381(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.406(5) . ?
C8 H8 0.9500 . ?
C9 N1 1.315(4) . ?
C9 S1 1.795(3) . ?
C10 O3 1.261(4) . ?
C10 N2 1.310(4) . ?
C10 H10 0.9500 . ?
C11 N2 1.464(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.470(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C101 N101 1.357(4) . ?
C101 C106 1.414(4) . ?
C101 C102 1.421(4) . ?
C102 O101 1.343(4) . ?
C102 C103 1.386(5) . ?
C103 C104 1.420(5) . ?
C103 H103 0.9500 . ?
C104 C105 1.389(5) . ?
C104 H104 0.9500 . ?
C105 C106 1.412(5) . ?
C105 H105 0.9500 . ?
C106 C107 1.426(5) . ?
C107 C108 1.374(5) . ?
C107 H107 0.9500 . ?
C108 C109 1.410(5) . ?
C108 H108 0.9500 . ?
C109 N101 1.315(4) . ?
C109 S101 1.794(4) . ?
C110 O103 1.267(4) . ?
C110 N102 1.312(4) . ?
C110 H110 0.9500 . ?
C111 N102 1.457(5) . ?
C111 H11D 0.9800 . ?
C111 H11E 0.9800 . ?
C111 H11F 0.9800 . ?
C112 N102 1.467(5) . ?
C112 H11G 0.9800 . ?
C112 H11H 0.9800 . ?
C112 H11I 0.9800 . ?
N1 Pd1 1.921(3) . ?
N101 Pd2 1.920(3) . ?
O1 Pd1 2.006(2) . ?
O2 S1 1.498(3) . ?
O2 Pd1 2.087(3) . ?
O3 Pd1 2.034(2) . ?
O4 S1 1.434(3) . ?
O5 S1 1.437(3) . ?
O101 Pd2 2.002(2) . ?
O102 S101 1.501(3) . ?
O102 Pd2 2.080(3) . ?
O103 Pd2 2.032(2) . ?
O104 S101 1.447(4) . ?
O105 S101 1.427(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
N1 C1 C6 120.0(3) . . ?
N1 C1 C2 114.8(3) . . ?
C6 C1 C2 125.1(3) . . ?
O1 C2 C3 125.6(3) . . ?
O1 C2 C1 118.0(3) . . ?
C3 C2 C1 116.4(3) . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 124.0(3) . . ?
C5 C4 H4 118.0 . . ?
C3 C4 H4 118.0 . . ?
C4 C5 C6 118.8(3) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C1 C6 C7 116.7(3) . . ?
C1 C6 C5 116.2(3) . . ?
C7 C6 C5 127.0(3) . . ?
C8 C7 C6 121.6(3) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C7 C8 C9 118.1(3) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
N1 C9 C8 120.6(3) . . ?
N1 C9 S1 112.7(2) . . ?
C8 C9 S1 126.6(3) . . ?
O3 C10 N2 122.8(3) . . ?
O3 C10 H10 118.6 . . ?
N2 C10 H10 118.6 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N101 C101 C106 120.5(3) . . ?
N101 C101 C102 114.5(3) . . ?
C106 C101 C102 124.9(3) . . ?
O101 C102 C103 125.2(3) . . ?
O101 C102 C101 118.5(3) . . ?
C103 C102 C101 116.3(3) . . ?
C102 C103 C104 120.0(3) . . ?
C102 C103 H103 120.0 . . ?
C104 C103 H103 120.0 . . ?
C105 C104 C103 122.8(3) . . ?
C105 C104 H104 118.6 . . ?
C103 C104 H104 118.6 . . ?
C104 C105 C106 119.1(3) . . ?
C104 C105 H105 120.5 . . ?
C106 C105 H105 120.5 . . ?
C105 C106 C101 116.8(3) . . ?
C105 C106 C107 127.0(3) . . ?
C101 C106 C107 116.2(3) . . ?
C108 C107 C106 121.4(3) . . ?
C108 C107 H107 119.3 . . ?
C106 C107 H107 119.3 . . ?
C107 C108 C109 118.6(3) . . ?
C107 C108 H108 120.7 . . ?
C109 C108 H108 120.7 . . ?
N101 C109 C108 120.5(3) . . ?
N101 C109 S101 112.7(3) . . ?
C108 C109 S101 126.7(3) . . ?
O103 C110 N102 122.7(3) . . ?
O103 C110 H110 118.6 . . ?
N102 C110 H110 118.6 . . ?
N102 C111 H11D 109.5 . . ?
N102 C111 H11E 109.5 . . ?
H11D C111 H11E 109.5 . . ?
N102 C111 H11F 109.5 . . ?
H11D C111 H11F 109.5 . . ?
H11E C111 H11F 109.5 . . ?
N102 C112 H11G 109.5 . . ?
N102 C112 H11H 109.5 . . ?
H11G C112 H11H 109.5 . . ?
N102 C112 H11I 109.5 . . ?
H11G C112 H11I 109.5 . . ?
H11H C112 H11I 109.5 . . ?
C9 N1 C1 122.9(3) . . ?
C9 N1 Pd1 123.4(2) . . ?
C1 N1 Pd1 113.6(2) . . ?
C10 N2 C11 121.1(3) . . ?
C10 N2 C12 122.4(3) . . ?
C11 N2 C12 116.5(3) . . ?
C109 N101 C101 122.8(3) . . ?
C109 N101 Pd2 123.6(2) . . ?
C101 N101 Pd2 113.6(2) . . ?
C110 N102 C111 120.7(3) . . ?
C110 N102 C112 121.1(3) . . ?
C111 N102 C112 118.2(3) . . ?
C2 O1 Pd1 109.7(2) . . ?
S1 O2 Pd1 116.99(14) . . ?
C10 O3 Pd1 118.9(2) . . ?
C102 O101 Pd2 109.27(19) . . ?
S101 O102 Pd2 117.29(15) . . ?
C110 O103 Pd2 118.8(2) . . ?
O4 S1 O5 115.62(18) . . ?
O4 S1 O2 111.92(17) . . ?
O5 S1 O2 111.60(17) . . ?
O4 S1 C9 107.04(16) . . ?
O5 S1 C9 106.42(16) . . ?
O2 S1 C9 103.20(15) . . ?
O105 S101 O104 115.7(2) . . ?
O105 S101 O102 112.5(2) . . ?
O104 S101 O102 111.62(17) . . ?
O105 S101 C109 107.30(18) . . ?
O104 S101 C109 105.73(19) . . ?
O102 S101 C109 102.82(15) . . ?
N1 Pd1 O1 83.85(11) . . ?
N1 Pd1 O3 177.38(11) . . ?
O1 Pd1 O3 97.34(10) . . ?
N1 Pd1 O2 82.93(11) . . ?
O1 Pd1 O2 166.28(10) . . ?
O3 Pd1 O2 96.03(10) . . ?
N101 Pd2 O101 84.07(11) . . ?
N101 Pd2 O103 178.04(11) . . ?
O101 Pd2 O103 96.05(10) . . ?
N101 Pd2 O102 82.96(11) . . ?
O101 Pd2 O102 167.03(10) . . ?
O103 Pd2 O102 96.91(10) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    2.000
_refine_diff_density_min   -1.055
_refine_diff_density_rms    0.129

#===END
##############################################################
