# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex_1(p2r)

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H33 N3 Pd S4'
_chemical_formula_weight         730.28

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'

_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                   20.803(3)
_cell_length_b                   6.3637(8)
_cell_length_c                   25.240(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.136(2)
_cell_angle_gamma                90
_cell_volume                     3299.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3931
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      26.34

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_F_000             1496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.845
_shelx_estimated_absorpt_T_min   0.729
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6508
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS v2009/1, Sheldrick, G.M., (2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16346
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.634
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4121
_reflns_number_gt                3417
_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 APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_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)+(0.0252P)²+2.2860P] 
 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         4121
_refine_ls_number_parameters     197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0640
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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 0.7500 1.2500 0.5000 0.01913(6) Uani 1 2 d S . P . .
S1 S 0.68918(2) 0.95070(8) 0.51177(2) 0.02225(11) Uani 1 1 d . . . . .
S2 S 0.72068(2) 1.11437(8) 0.41437(2) 0.02273(11) Uani 1 1 d . . . . .
C1 C 0.68112(9) 0.9187(3) 0.44329(7) 0.0197(4) Uani 1 1 d . . . . .
N1 N 0.64856(7) 0.7645(2) 0.41588(6) 0.0205(3) Uani 1 1 d . . . . .
C2 C 0.63986(9) 0.7573(3) 0.35667(7) 0.0231(4) Uani 1 1 d . . . . .
H2A H 0.6501 0.8974 0.3431 0.028 Uiso 1 1 calc R U . . .
H2B H 0.5937 0.7264 0.3426 0.028 Uiso 1 1 calc R U . . .
C3 C 0.68207(10) 0.5951(3) 0.33548(7) 0.0227(4) Uani 1 1 d . . . . .
C4 C 0.74940(10) 0.5964(3) 0.35054(8) 0.0263(4) Uani 1 1 d . . . . .
H4 H 0.7695 0.6994 0.3750 0.032 Uiso 1 1 calc R U . . .
C5 C 0.78714(11) 0.4471(4) 0.32986(9) 0.0331(5) Uani 1 1 d . . . . .
H5 H 0.8330 0.4473 0.3406 0.040 Uiso 1 1 calc R U . . .
C6 C 0.75848(13) 0.2976(4) 0.29365(9) 0.0382(6) Uani 1 1 d . . . . .
H6 H 0.7846 0.1968 0.2792 0.046 Uiso 1 1 calc R U . . .
C7 C 0.69202(13) 0.2962(4) 0.27874(9) 0.0369(6) Uani 1 1 d . . . . .
H7 H 0.6722 0.1939 0.2540 0.044 Uiso 1 1 calc R U . . .
C8 C 0.65372(11) 0.4428(3) 0.29959(8) 0.0297(5) Uani 1 1 d . . . . .
H8 H 0.6078 0.4394 0.2894 0.036 Uiso 1 1 calc R U . . .
C9 C 0.61989(9) 0.5888(3) 0.44189(8) 0.0232(4) Uani 1 1 d . . . . .
H9A H 0.6355 0.5946 0.4810 0.028 Uiso 1 1 calc R U . . .
H9B H 0.6352 0.4548 0.4283 0.028 Uiso 1 1 calc R U . . .
C10 C 0.54626(9) 0.5915(3) 0.43208(8) 0.0242(4) Uani 1 1 d . . . . .
C11 C 0.51221(11) 0.7679(4) 0.44323(10) 0.0384(5) Uani 1 1 d . . . . .
H11 H 0.5351 0.8921 0.4557 0.046 Uiso 1 1 calc R U . . .
C12 C 0.44456(12) 0.7644(5) 0.43631(11) 0.0501(7) Uani 1 1 d . . . . .
H12 H 0.4215 0.8867 0.4440 0.060 Uiso 1 1 calc R U . . .
C13 C 0.41089(12) 0.5875(5) 0.41858(11) 0.0518(7) Uani 1 1 d . . . . .
H13 H 0.3647 0.5860 0.4142 0.062 Uiso 1 1 calc R U . . .
C14 C 0.44432(13) 0.4116(5) 0.40720(12) 0.0567(8) Uani 1 1 d . . . . .
H14 H 0.4210 0.2879 0.3949 0.068 Uiso 1 1 calc R U . . .
C15 C 0.51217(11) 0.4125(4) 0.41346(11) 0.0419(6) Uani 1 1 d . . . . .
H15 H 0.5349 0.2907 0.4050 0.050 Uiso 1 1 calc R U . . .
N20 N 0.5000 0.6822(5) 0.2500 0.0400(7) Uani 1 2 d S T P . .
C21 C 0.47047(12) 0.7898(5) 0.28403(11) 0.0471(7) Uani 1 1 d . . . . .
H21 H 0.4489 0.7142 0.3085 0.057 Uiso 1 1 calc R U . . .
C22 C 0.46959(14) 1.0040(5) 0.28565(15) 0.0693(10) Uani 1 1 d . . . . .
H22 H 0.4483 1.0755 0.3110 0.083 Uiso 1 1 calc R U . . .
C23 C 0.5000 1.1144(7) 0.2500 0.086(2) Uani 1 2 d S T P . .
H23 H 0.5000 1.2637 0.2500 0.103 Uiso 1 2 calc R 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 S2 2.3171(5) 7_676 ?
Pd1 S2 2.3172(5) . ?
Pd1 S1 2.3315(5) . ?
Pd1 S1 2.3316(5) 7_676 ?
S1 C1 1.7220(19) . ?
S2 C1 1.718(2) . ?
C1 N1 1.323(2) . ?
N1 C9 1.470(2) . ?
N1 C2 1.477(2) . ?
C2 C3 1.507(3) . ?
C3 C4 1.392(3) . ?
C3 C8 1.393(3) . ?
C4 C5 1.386(3) . ?
C5 C6 1.387(3) . ?
C6 C7 1.374(4) . ?
C7 C8 1.384(3) . ?
C9 C10 1.512(3) . ?
C10 C11 1.380(3) . ?
C10 C15 1.384(3) . ?
C11 C12 1.390(3) . ?
C12 C13 1.364(4) . ?
C13 C14 1.372(4) . ?
C14 C15 1.395(3) . ?
N20 C21 1.323(3) . ?
N20 C21 1.323(3) 2_655 ?
C21 C22 1.364(4) . ?
C22 C23 1.373(4) . ?
C23 C22 1.373(4) 2_655 ?

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
S2 Pd1 S2 180.00(2) 7_676 . ?
S2 Pd1 S1 104.671(17) 7_676 . ?
S2 Pd1 S1 75.329(17) . . ?
S2 Pd1 S1 75.331(17) 7_676 7_676 ?
S2 Pd1 S1 104.669(17) . 7_676 ?
S1 Pd1 S1 180.0 . 7_676 ?
C1 S1 Pd1 86.40(7) . . ?
C1 S2 Pd1 86.95(6) . . ?
N1 C1 S2 123.74(14) . . ?
N1 C1 S1 124.94(15) . . ?
S2 C1 S1 111.32(11) . . ?
C1 N1 C9 122.73(16) . . ?
C1 N1 C2 121.46(16) . . ?
C9 N1 C2 115.80(15) . . ?
N1 C2 C3 113.29(15) . . ?
C4 C3 C8 119.05(19) . . ?
C4 C3 C2 121.12(18) . . ?
C8 C3 C2 119.82(18) . . ?
C5 C4 C3 119.9(2) . . ?
C4 C5 C6 120.6(2) . . ?
C7 C6 C5 119.6(2) . . ?
C6 C7 C8 120.4(2) . . ?
C7 C8 C3 120.5(2) . . ?
N1 C9 C10 112.98(16) . . ?
C11 C10 C15 119.1(2) . . ?
C11 C10 C9 121.02(19) . . ?
C15 C10 C9 119.82(19) . . ?
C10 C11 C12 120.2(2) . . ?
C13 C12 C11 120.8(2) . . ?
C12 C13 C14 119.4(2) . . ?
C13 C14 C15 120.7(3) . . ?
C10 C15 C14 119.8(2) . . ?
C21 N20 C21 117.7(3) . 2_655 ?
N20 C21 C22 123.1(3) . . ?
C21 C22 C23 118.8(3) . . ?
C22 C23 C22 118.4(4) 2_655 . ?

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.070

_shelxl_version_number           2012-9

_database_code_depnum_ccdc_archive 'CCDC 995675'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Complex_2(p1)

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H49 N3 Pd S4'
_chemical_formula_weight         698.37

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   9.9610(13)
_cell_length_b                   14.0277(19)
_cell_length_c                   12.1552(16)
_cell_angle_alpha                90
_cell_angle_beta                 104.023(2)
_cell_angle_gamma                90
_cell_volume                     1647.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3121
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      23.77

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.842
_shelx_estimated_absorpt_T_min   0.824
_shelx_estimated_absorpt_T_max   0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6288
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS v2009/1, Sheldrick, G.M., (2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16333
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.256
_diffrn_reflns_theta_max         28.347
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4109
_reflns_number_gt                3135
_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 APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_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)+(0.0438P)²] 
 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         4109
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0773
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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 0.5000 0.5000 0.5000 0.02289(8) Uani 1 2 d S . P . .
S1 S 0.29497(6) 0.43575(5) 0.39469(5) 0.02969(15) Uani 1 1 d . . . . .
S2 S 0.56729(6) 0.37897(4) 0.39431(5) 0.02556(14) Uani 1 1 d . . . . .
C1 C 0.3927(2) 0.35557(16) 0.33886(19) 0.0227(5) Uani 1 1 d . . . . .
N1 N 0.34478(19) 0.28685(14) 0.26479(16) 0.0233(4) Uani 1 1 d . . . . .
C2 C 0.1947(2) 0.26188(18) 0.2254(2) 0.0273(5) Uani 1 1 d . . . . .
H2 H 0.1908 0.2050 0.1752 0.033 Uiso 1 1 calc R U . . .
C3 C 0.1345(3) 0.22920(19) 0.3227(2) 0.0330(6) Uani 1 1 d . . . . .
H3A H 0.1436 0.2809 0.3795 0.040 Uiso 1 1 calc R U . . .
H3B H 0.1867 0.1732 0.3602 0.040 Uiso 1 1 calc R U . . .
C4 C -0.0193(3) 0.2026(2) 0.2784(3) 0.0407(7) Uani 1 1 d . . . . .
H4A H -0.0273 0.1457 0.2291 0.049 Uiso 1 1 calc R U . . .
H4B H -0.0592 0.1866 0.3432 0.049 Uiso 1 1 calc R U . . .
C5 C -0.1000(3) 0.2844(2) 0.2119(3) 0.0427(7) Uani 1 1 d . . . . .
H5A H -0.1983 0.2657 0.1843 0.051 Uiso 1 1 calc R U . . .
H5B H -0.0958 0.3404 0.2622 0.051 Uiso 1 1 calc R U . . .
C6 C -0.0415(3) 0.3108(2) 0.1120(2) 0.0397(7) Uani 1 1 d . . . . .
H6A H -0.0952 0.3645 0.0703 0.048 Uiso 1 1 calc R U . . .
H6B H -0.0508 0.2558 0.0596 0.048 Uiso 1 1 calc R U . . .
C7 C 0.1119(2) 0.33939(19) 0.1507(2) 0.0321(6) Uani 1 1 d . . . . .
H7A H 0.1498 0.3496 0.0835 0.038 Uiso 1 1 calc R U . . .
H7B H 0.1202 0.4000 0.1936 0.038 Uiso 1 1 calc R U . . .
C8 C 0.4459(2) 0.22556(16) 0.22565(19) 0.0228(5) Uani 1 1 d . . . . .
H8 H 0.5354 0.2613 0.2422 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4070(3) 0.20643(18) 0.0979(2) 0.0302(6) Uani 1 1 d . . . . .
H9A H 0.3209 0.1682 0.0775 0.036 Uiso 1 1 calc R U . . .
H9B H 0.3904 0.2675 0.0560 0.036 Uiso 1 1 calc R U . . .
C10 C 0.5247(3) 0.15243(19) 0.0655(2) 0.0334(6) Uani 1 1 d . . . . .
H10A H 0.4975 0.1369 -0.0164 0.040 Uiso 1 1 calc R U . . .
H10B H 0.6075 0.1939 0.0787 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5613(3) 0.06065(19) 0.1330(2) 0.0378(6) Uani 1 1 d . . . . .
H11A H 0.6434 0.0314 0.1143 0.045 Uiso 1 1 calc R U . . .
H11B H 0.4834 0.0152 0.1110 0.045 Uiso 1 1 calc R U . . .
C12 C 0.5917(3) 0.0784(2) 0.2605(2) 0.0363(6) Uani 1 1 d . . . . .
H12A H 0.6783 0.1156 0.2846 0.044 Uiso 1 1 calc R U . . .
H12B H 0.6055 0.0166 0.3010 0.044 Uiso 1 1 calc R U . . .
C13 C 0.4729(3) 0.13291(18) 0.2929(2) 0.0300(5) Uani 1 1 d . . . . .
H13A H 0.3882 0.0932 0.2762 0.036 Uiso 1 1 calc R U . . .
H13B H 0.4979 0.1471 0.3751 0.036 Uiso 1 1 calc R U . . .
N20 N 0.3590(3) 0.5171(2) -0.0063(3) 0.0484(7) Uani 0.5 1 d . . P A 1
C20 C 0.3590(3) 0.5171(2) -0.0063(3) 0.0484(7) Uani 0.5 1 d . . P A 2
H20 H 0.2639 0.5286 -0.0104 0.058 Uiso 0.5 1 calc R U P A 2
C21 C 0.4461(4) 0.4815(2) 0.0886(3) 0.0480(8) Uani 1 1 d . . . . .
H21 H 0.4105 0.4678 0.1526 0.058 Uiso 1 1 calc R U . A 1
C22 C 0.5836(3) 0.4647(2) 0.0955(3) 0.0481(8) Uani 1 1 d . . . . .
H22 H 0.6402 0.4398 0.1638 0.058 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 S1 2.3140(6) 3_666 ?
Pd1 S1 2.3141(6) . ?
Pd1 S2 2.3237(6) . ?
Pd1 S2 2.3237(6) 3_666 ?
S1 C1 1.730(2) . ?
S2 C1 1.738(2) . ?
C1 N1 1.326(3) . ?
N1 C8 1.487(3) . ?
N1 C2 1.496(3) . ?
C2 C3 1.521(3) . ?
C2 C7 1.525(3) . ?
C3 C4 1.542(3) . ?
C4 C5 1.517(4) . ?
C5 C6 1.515(4) . ?
C6 C7 1.538(3) . ?
C8 C13 1.524(3) . ?
C8 C9 1.530(3) . ?
C9 C10 1.526(3) . ?
C10 C11 1.523(4) . ?
C11 C12 1.525(4) . ?
C12 C13 1.538(3) . ?
N20 C21 1.359(4) . ?
N20 C22 1.367(4) 3_665 ?
C21 C22 1.372(4) . ?
C22 C20 1.367(4) 3_665 ?
C22 N20 1.367(4) 3_665 ?

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
S1 Pd1 S1 180.0 3_666 . ?
S1 Pd1 S2 104.85(2) 3_666 . ?
S1 Pd1 S2 75.15(2) . . ?
S1 Pd1 S2 75.15(2) 3_666 3_666 ?
S1 Pd1 S2 104.85(2) . 3_666 ?
S2 Pd1 S2 180.0 . 3_666 ?
C1 S1 Pd1 88.01(8) . . ?
C1 S2 Pd1 87.52(8) . . ?
N1 C1 S1 126.50(17) . . ?
N1 C1 S2 124.21(17) . . ?
S1 C1 S2 109.29(13) . . ?
C1 N1 C8 118.51(18) . . ?
C1 N1 C2 123.67(19) . . ?
C8 N1 C2 117.61(18) . . ?
N1 C2 C3 111.92(19) . . ?
N1 C2 C7 112.22(19) . . ?
C3 C2 C7 114.8(2) . . ?
C2 C3 C4 110.3(2) . . ?
C5 C4 C3 110.9(2) . . ?
C6 C5 C4 110.8(2) . . ?
C5 C6 C7 111.4(2) . . ?
C2 C7 C6 110.5(2) . . ?
N1 C8 C13 111.54(19) . . ?
N1 C8 C9 113.67(19) . . ?
C13 C8 C9 111.28(19) . . ?
C10 C9 C8 109.1(2) . . ?
C11 C10 C9 112.2(2) . . ?
C10 C11 C12 111.9(2) . . ?
C11 C12 C13 111.4(2) . . ?
C8 C13 C12 109.5(2) . . ?
C21 N20 C22 115.9(3) . 3_665 ?
N20 C21 C22 122.6(3) . . ?
C20 C22 C21 121.5(3) 3_665 . ?
N20 C22 C21 121.5(3) 3_665 . ?

_refine_diff_density_max         0.479
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.082

_shelxl_version_number           2012-9

_database_code_depnum_ccdc_archive 'CCDC 995676'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex_3(p4)

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H52 N2 Pd S4'
_chemical_formula_weight         627.33

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'

_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                   12.3351(11)
_cell_length_b                   20.5728(19)
_cell_length_c                   25.918(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6577.2(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6444
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      23.79

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_F_000             2656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.834
_shelx_estimated_absorpt_T_min   0.765
_shelx_estimated_absorpt_T_max   0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6641
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS 2012/1, Sheldrick, G.M., (2012)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            64543
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.571
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8186
_reflns_number_gt                5263
_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 APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_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)+(0.0351P)²+4.0416P] 
 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         8186
_refine_ls_number_parameters     311
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0817
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.017
_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 0.75066(2) 0.20252(2) 0.37186(2) 0.03209(7) Uani 1 1 d . . . . .
S1 S 0.60730(6) 0.14575(4) 0.40896(3) 0.03734(17) Uani 1 1 d . . . . .
S2 S 0.69591(6) 0.26743(4) 0.43998(3) 0.03706(17) Uani 1 1 d . . . . .
C1 C 0.6035(2) 0.20718(14) 0.45425(11) 0.0338(6) Uani 1 1 d . . . . .
N1 N 0.53900(19) 0.20860(11) 0.49463(9) 0.0387(6) Uani 1 1 d . . . . .
C2 C 0.4552(2) 0.15901(15) 0.50369(13) 0.0466(8) Uani 1 1 d . . . . .
H2A H 0.4457 0.1331 0.4718 0.056 Uiso 1 1 calc R U . . .
H2B H 0.3856 0.1810 0.5111 0.056 Uiso 1 1 calc R U . . .
C3 C 0.4815(3) 0.11318(16) 0.54805(13) 0.0514(9) Uani 1 1 d . . . . .
H3A H 0.4906 0.1392 0.5799 0.062 Uiso 1 1 calc R U . . .
H3B H 0.4189 0.0839 0.5534 0.062 Uiso 1 1 calc R U . . .
C4 C 0.5819(3) 0.07223(16) 0.54043(12) 0.0488(8) Uani 1 1 d . . . . .
H4A H 0.6452 0.1013 0.5361 0.059 Uiso 1 1 calc R U . . .
H4B H 0.5738 0.0466 0.5083 0.059 Uiso 1 1 calc R U . . .
C5 C 0.6037(3) 0.02607(17) 0.58509(13) 0.0533(9) Uani 1 1 d . . . . .
H5A H 0.6128 0.0519 0.6170 0.064 Uiso 1 1 calc R U . . .
H5B H 0.5396 -0.0023 0.5898 0.064 Uiso 1 1 calc R U . . .
C6 C 0.7030(3) -0.01637(17) 0.57782(13) 0.0575(9) Uani 1 1 d . . . . .
H6A H 0.6943 -0.0422 0.5459 0.069 Uiso 1 1 calc R U . . .
H6B H 0.7674 0.0118 0.5734 0.069 Uiso 1 1 calc R U . . .
C7 C 0.7226(4) -0.0620(2) 0.62250(16) 0.0835(14) Uani 1 1 d . . . . .
H7A H 0.7873 -0.0882 0.6156 0.125 Uiso 1 1 calc R U . . .
H7B H 0.6598 -0.0906 0.6267 0.125 Uiso 1 1 calc R U . . .
H7C H 0.7335 -0.0367 0.6541 0.125 Uiso 1 1 calc R U . . .
C8 C 0.5434(3) 0.26356(15) 0.53137(11) 0.0413(7) Uani 1 1 d . . . . .
H8A H 0.6191 0.2792 0.5340 0.050 Uiso 1 1 calc R U . . .
H8B H 0.5209 0.2481 0.5659 0.050 Uiso 1 1 calc R U . . .
C9 C 0.4711(2) 0.31967(15) 0.51528(12) 0.0405(7) Uani 1 1 d . . . . .
H9A H 0.3949 0.3046 0.5140 0.049 Uiso 1 1 calc R U . . .
H9B H 0.4918 0.3342 0.4802 0.049 Uiso 1 1 calc R U . . .
C10 C 0.4799(2) 0.37677(14) 0.55250(11) 0.0406(7) Uani 1 1 d . . . . .
H10A H 0.4651 0.3611 0.5879 0.049 Uiso 1 1 calc R U . . .
H10B H 0.5551 0.3935 0.5517 0.049 Uiso 1 1 calc R U . . .
C11 C 0.4029(3) 0.43199(14) 0.54034(12) 0.0428(7) Uani 1 1 d . . . . .
H11A H 0.3276 0.4154 0.5415 0.051 Uiso 1 1 calc R U . . .
H11B H 0.4171 0.4474 0.5048 0.051 Uiso 1 1 calc R U . . .
C12 C 0.4128(3) 0.48903(15) 0.57706(13) 0.0512(8) Uani 1 1 d . . . . .
H12A H 0.3977 0.4739 0.6126 0.061 Uiso 1 1 calc R U . . .
H12B H 0.4882 0.5055 0.5762 0.061 Uiso 1 1 calc R U . . .
C13 C 0.3363(4) 0.54376(17) 0.56389(17) 0.0750(12) Uani 1 1 d . . . . .
H13A H 0.3461 0.5794 0.5885 0.112 Uiso 1 1 calc R U . . .
H13B H 0.2614 0.5280 0.5657 0.112 Uiso 1 1 calc R U . . .
H13C H 0.3515 0.5594 0.5289 0.112 Uiso 1 1 calc R U . . .
S3 S 0.89840(6) 0.25742(4) 0.33725(3) 0.03849(18) Uani 1 1 d . . . . .
S4 S 0.81300(6) 0.13466(4) 0.30663(3) 0.03913(18) Uani 1 1 d . . . . .
C14 C 0.9157(2) 0.19052(15) 0.29833(10) 0.0364(7) Uani 1 1 d . . . . .
N2 N 0.99744(19) 0.18216(13) 0.26631(9) 0.0375(6) Uani 1 1 d . . . . .
C15 C 1.0872(2) 0.22925(16) 0.26544(11) 0.0421(7) Uani 1 1 d . . . . .
H15A H 1.0576 0.2736 0.2702 0.051 Uiso 1 1 calc R U . . .
H15B H 1.1230 0.2277 0.2313 0.051 Uiso 1 1 calc R U . . .
C16 C 1.1712(3) 0.21582(16) 0.30735(12) 0.0466(8) Uani 1 1 d . . . . .
H16A H 1.1341 0.2112 0.3410 0.056 Uiso 1 1 calc R U . . .
H16B H 1.2085 0.1743 0.2997 0.056 Uiso 1 1 calc R U . . .
C17 C 1.2536(3) 0.26956(17) 0.31077(12) 0.0473(7) Uani 1 1 d . . . . .
H17A H 1.2160 0.3107 0.3193 0.057 Uiso 1 1 calc R U . . .
H17B H 1.2884 0.2751 0.2766 0.057 Uiso 1 1 calc R U . . .
C18 C 1.3421(3) 0.25678(17) 0.35151(15) 0.0579(9) Uani 1 1 d . . . . .
H18A H 1.3075 0.2521 0.3858 0.069 Uiso 1 1 calc R U . . .
H18B H 1.3788 0.2152 0.3434 0.069 Uiso 1 1 calc R U . . .
C19 C 1.4248(3) 0.3094(2) 0.35415(18) 0.0732(12) Uani 1 1 d . . . . .
H19A H 1.4545 0.3168 0.3192 0.088 Uiso 1 1 calc R U . . .
H19B H 1.4852 0.2948 0.3765 0.088 Uiso 1 1 calc R U . . .
C20 C 1.3807(4) 0.3732(2) 0.37492(18) 0.0882(15) Uani 1 1 d . . . . .
H20A H 1.4385 0.4059 0.3750 0.132 Uiso 1 1 calc R U . . .
H20B H 1.3542 0.3668 0.4102 0.132 Uiso 1 1 calc R U . . .
H20C H 1.3210 0.3881 0.3530 0.132 Uiso 1 1 calc R U . . .
C21 C 1.0031(3) 0.12491(15) 0.23198(11) 0.0443(8) Uani 1 1 d . . . . .
H21A H 1.0383 0.1380 0.1993 0.053 Uiso 1 1 calc R U . . .
H21B H 0.9284 0.1109 0.2237 0.053 Uiso 1 1 calc R U . . .
C22 C 1.0639(3) 0.06790(16) 0.25402(13) 0.0510(8) Uani 1 1 d . . . . .
H22A H 1.0295 0.0541 0.2868 0.061 Uiso 1 1 calc R U . A 1
H22B H 1.1396 0.0808 0.2616 0.061 Uiso 1 1 calc R U . A 1
C23 C 1.0636(4) 0.0115(2) 0.21601(16) 0.0800(13) Uani 0.741(9) 1 d D U P B 1
H23A H 1.0829 0.0276 0.1812 0.096 Uiso 0.741(9) 1 calc R U P B 1
H23B H 0.9901 -0.0076 0.2142 0.096 Uiso 0.741(9) 1 calc R U P B 1
C24 C 1.1451(8) -0.0406(5) 0.2329(4) 0.132(4) Uani 0.741(9) 1 d D U P B 1
H24A H 1.1461 -0.0411 0.2711 0.158 Uiso 0.741(9) 1 calc R U P B 1
H24B H 1.1165 -0.0832 0.2216 0.158 Uiso 0.741(9) 1 calc R U P B 1
C25 C 1.2462(6) -0.0366(4) 0.2171(4) 0.113(3) Uani 0.741(9) 1 d D U P B 1
H25A H 1.2805 -0.0019 0.2379 0.136 Uiso 0.741(9) 1 calc R U P B 1
H25B H 1.2434 -0.0204 0.1812 0.136 Uiso 0.741(9) 1 calc R U P B 1
C26 C 1.3218(7) -0.0911(4) 0.2170(4) 0.110(3) Uani 0.741(9) 1 d D U P B 1
H26A H 1.3914 -0.0770 0.2026 0.165 Uiso 0.741(9) 1 calc R U P B 1
H26B H 1.2923 -0.1265 0.1960 0.165 Uiso 0.741(9) 1 calc R U P B 1
H26C H 1.3326 -0.1064 0.2525 0.165 Uiso 0.741(9) 1 calc R U P B 1
C23' C 1.0636(4) 0.0115(2) 0.21601(16) 0.0800(13) Uani 0.259(9) 1 d D . P B 2
H23C H 0.9867 -0.0018 0.2132 0.096 Uiso 0.259(9) 1 calc R U P B 2
H23D H 1.0826 0.0311 0.1823 0.096 Uiso 0.259(9) 1 calc R U P B 2
C24' C 1.1273(12) -0.0516(7) 0.2184(7) 0.051(4) Uiso 0.259(9) 1 d D . P B 2
H24C H 1.1619 -0.0516 0.2529 0.061 Uiso 0.259(9) 1 calc R U P B 2
H24D H 1.0717 -0.0863 0.2195 0.061 Uiso 0.259(9) 1 calc R U P B 2
C25' C 1.2032(10) -0.0736(7) 0.1864(5) 0.048(4) Uiso 0.259(9) 1 d D . P B 2
H25C H 1.2285 -0.0346 0.1677 0.058 Uiso 0.259(9) 1 calc R U P B 2
H25D H 1.1630 -0.0998 0.1607 0.058 Uiso 0.259(9) 1 calc R U P B 2
C26' C 1.3019(15) -0.1109(10) 0.1966(9) 0.072(6) Uiso 0.259(9) 1 d D . P B 2
H26D H 1.3405 -0.1185 0.1641 0.107 Uiso 0.259(9) 1 calc R U P B 2
H26E H 1.2826 -0.1528 0.2122 0.107 Uiso 0.259(9) 1 calc R U P B 2
H26F H 1.3486 -0.0866 0.2202 0.107 Uiso 0.259(9) 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 S2 2.3143(7) . ?
Pd1 S4 2.3236(8) . ?
Pd1 S3 2.3241(8) . ?
Pd1 S1 2.3272(8) . ?
S1 C1 1.725(3) . ?
S2 C1 1.724(3) . ?
C1 N1 1.315(3) . ?
N1 C2 1.471(4) . ?
N1 C8 1.479(4) . ?
C2 C3 1.522(4) . ?
C3 C4 1.510(4) . ?
C4 C5 1.521(4) . ?
C5 C6 1.516(5) . ?
C6 C7 1.510(5) . ?
C8 C9 1.517(4) . ?
C9 C10 1.524(4) . ?
C10 C11 1.514(4) . ?
C11 C12 1.516(4) . ?
C12 C13 1.509(5) . ?
S3 C14 1.720(3) . ?
S4 C14 1.724(3) . ?
C14 N2 1.317(3) . ?
N2 C15 1.471(4) . ?
N2 C21 1.478(4) . ?
C15 C16 1.526(4) . ?
C16 C17 1.505(4) . ?
C17 C18 1.541(4) . ?
C18 C19 1.488(5) . ?
C19 C20 1.520(5) . ?
C21 C22 1.505(4) . ?
C22 C23 1.521(5) . ?
C23 C24 1.534(8) . ?
C24 C25 1.315(10) . ?
C25 C26 1.459(8) . ?
C24' C25' 1.330(13) . ?
C25' C26' 1.463(14) . ?

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
S2 Pd1 S4 176.69(3) . . ?
S2 Pd1 S3 104.06(3) . . ?
S4 Pd1 S3 75.62(3) . . ?
S2 Pd1 S1 75.68(3) . . ?
S4 Pd1 S1 104.51(3) . . ?
S3 Pd1 S1 177.72(3) . . ?
C1 S1 Pd1 86.21(10) . . ?
C1 S2 Pd1 86.66(10) . . ?
N1 C1 S2 123.7(2) . . ?
N1 C1 S1 125.0(2) . . ?
S2 C1 S1 111.27(16) . . ?
C1 N1 C2 122.5(2) . . ?
C1 N1 C8 120.5(3) . . ?
C2 N1 C8 116.9(2) . . ?
N1 C2 C3 113.6(3) . . ?
C4 C3 C2 114.9(3) . . ?
C3 C4 C5 113.2(3) . . ?
C6 C5 C4 114.1(3) . . ?
C7 C6 C5 113.1(3) . . ?
N1 C8 C9 112.5(2) . . ?
C8 C9 C10 111.8(2) . . ?
C11 C10 C9 113.7(3) . . ?
C10 C11 C12 113.6(3) . . ?
C13 C12 C11 112.6(3) . . ?
C14 S3 Pd1 86.26(10) . . ?
C14 S4 Pd1 86.18(10) . . ?
N2 C14 S3 124.7(2) . . ?
N2 C14 S4 123.6(2) . . ?
S3 C14 S4 111.66(16) . . ?
C14 N2 C15 120.0(3) . . ?
C14 N2 C21 121.3(3) . . ?
C15 N2 C21 118.7(2) . . ?
N2 C15 C16 112.4(3) . . ?
C17 C16 C15 111.6(3) . . ?
C16 C17 C18 113.2(3) . . ?
C19 C18 C17 113.1(3) . . ?
C18 C19 C20 113.5(3) . . ?
N2 C21 C22 114.6(2) . . ?
C21 C22 C23 110.3(3) . . ?
C22 C23 C24 110.3(5) . . ?
C25 C24 C23 119.3(9) . . ?
C24 C25 C26 124.0(8) . . ?
C24' C25' C26' 130.7(15) . . ?

_refine_diff_density_max         0.651
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.073

_shelxl_version_number           2012-9

_database_code_depnum_ccdc_archive 'CCDC 995677'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex_4(p3r)

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 N2 Pd S4'
_chemical_formula_weight         483.04

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   9.9199(7)
_cell_length_b                   11.0292(7)
_cell_length_c                   10.1444(7)
_cell_angle_alpha                90
_cell_angle_beta                 114.6960(10)
_cell_angle_gamma                90
_cell_volume                     1008.37(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3958
_cell_measurement_theta_min      2.88
_cell_measurement_theta_max      31.51

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_F_000             496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.335
_shelx_estimated_absorpt_T_min   0.706
_shelx_estimated_absorpt_T_max   0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6719
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_process_details   'SADABS v2009/1, Sheldrick, G.M., (2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11825
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.412
_diffrn_reflns_theta_max         31.804
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3217
_reflns_number_gt                2767
_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 APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_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)+(0.0335P)²+0.0751P] 
 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         3217
_refine_ls_number_parameters     107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0623
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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 1.0000 0.0000 1.0000 0.01690(6) Uani 1 2 d S . P . .
S1 S 0.87449(4) 0.06787(4) 0.76174(5) 0.02241(10) Uani 1 1 d . . . . .
S2 S 0.75458(5) 0.02191(4) 0.96658(5) 0.02183(9) Uani 1 1 d . . . . .
C1 C 0.71887(17) 0.07598(14) 0.79591(17) 0.0175(3) Uani 1 1 d . . . . .
N1 N 0.58869(14) 0.11999(13) 0.70459(14) 0.0184(3) Uani 1 1 d . . . . .
C2 C 0.57087(19) 0.17457(17) 0.56660(18) 0.0250(4) Uani 1 1 d . . . . .
H2A H 0.5154 0.1190 0.4869 0.038 Uiso 1 1 calc R U . . .
H2B H 0.6688 0.1900 0.5681 0.038 Uiso 1 1 calc R U . . .
H2C H 0.5166 0.2512 0.5525 0.038 Uiso 1 1 calc R U . . .
C3 C 0.46457(16) 0.13096(14) 0.74922(17) 0.0175(3) Uani 1 1 d . . . . .
H3 H 0.4815 0.0699 0.8274 0.021 Uiso 1 1 calc R U . . .
C5 C 0.34195(18) 0.26488(17) 0.86660(19) 0.0240(3) Uani 1 1 d . . . . .
H5A H 0.3402 0.3478 0.9031 0.029 Uiso 1 1 calc R U . . .
H5B H 0.3632 0.2076 0.9480 0.029 Uiso 1 1 calc R U . . .
C4 C 0.46427(17) 0.25616(15) 0.81312(18) 0.0205(3) Uani 1 1 d . . . . .
H4A H 0.5617 0.2713 0.8949 0.025 Uiso 1 1 calc R U . . .
H4B H 0.4485 0.3189 0.7383 0.025 Uiso 1 1 calc R U . . .
C6 C 0.19049(19) 0.23553(16) 0.7451(2) 0.0247(4) Uani 1 1 d . . . . .
H6A H 0.1639 0.2984 0.6687 0.030 Uiso 1 1 calc R U . . .
H6B H 0.1143 0.2362 0.7842 0.030 Uiso 1 1 calc R U . . .
C7 C 0.19253(17) 0.11114(16) 0.67910(18) 0.0227(3) Uani 1 1 d . . . . .
H7A H 0.2085 0.0476 0.7531 0.027 Uiso 1 1 calc R U . . .
H7B H 0.0951 0.0961 0.5973 0.027 Uiso 1 1 calc R U . . .
C8 C 0.31471(17) 0.10276(16) 0.62472(17) 0.0211(3) Uani 1 1 d . . . . .
H8A H 0.3164 0.0202 0.5871 0.025 Uiso 1 1 calc R U . . .
H8B H 0.2946 0.1612 0.5447 0.025 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 S2 2.3261(5) . ?
Pd1 S2 2.3261(5) 3_757 ?
Pd1 S1 2.3319(4) . ?
Pd1 S1 2.3319(4) 3_757 ?
Pd1 H2C 2.7872 4_666 ?
S1 C1 1.7201(16) . ?
S2 C1 1.7223(16) . ?
C1 N1 1.3273(19) . ?
N1 C2 1.465(2) . ?
N1 C3 1.4837(19) . ?
C3 C4 1.526(2) . ?
C3 C8 1.527(2) . ?
C5 C4 1.525(2) . ?
C5 C6 1.528(2) . ?
C6 C7 1.530(2) . ?
C7 C8 1.530(2) . ?

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
S2 Pd1 S2 180.0 . 3_757 ?
S2 Pd1 S1 75.080(14) . . ?
S2 Pd1 S1 104.919(14) 3_757 . ?
S2 Pd1 S1 104.919(14) . 3_757 ?
S2 Pd1 S1 75.081(14) 3_757 3_757 ?
S1 Pd1 S1 180.00(2) . 3_757 ?
S2 Pd1 H2C 84.3 . 4_666 ?
S2 Pd1 H2C 95.7 3_757 4_666 ?
S1 Pd1 H2C 81.1 . 4_666 ?
S1 Pd1 H2C 98.9 3_757 4_666 ?
C1 S1 Pd1 86.75(5) . . ?
C1 S2 Pd1 86.88(5) . . ?
N1 C1 S1 124.87(12) . . ?
N1 C1 S2 124.04(12) . . ?
S1 C1 S2 111.08(9) . . ?
C1 N1 C2 120.73(13) . . ?
C1 N1 C3 120.42(13) . . ?
C2 N1 C3 118.28(12) . . ?
N1 C3 C4 110.65(13) . . ?
N1 C3 C8 112.10(13) . . ?
C4 C3 C8 111.20(13) . . ?
C4 C5 C6 111.10(14) . . ?
C5 C4 C3 110.57(13) . . ?
C5 C6 C7 110.77(14) . . ?
C8 C7 C6 111.66(14) . . ?
C3 C8 C7 109.48(13) . . ?

_refine_diff_density_max         0.375
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.098

_shelxl_version_number           2012-9

_database_code_depnum_ccdc_archive 'CCDC 995678'
