# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © The Royal Society of Chemistry 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_import

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H26 Au Cl3 N2 O5 P'
_chemical_formula_weight         828.81

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, y, z+1/2'
'x, y+1/2, -z+1/2'

_cell_length_a                   7.894(5)
_cell_length_b                   15.290(5)
_cell_length_c                   25.892(5)
_cell_angle_alpha                90.028(5)
_cell_angle_beta                 90.039(5)
_cell_angle_gamma                90.581(5)
_cell_volume                     3125(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1620
_exptl_absorpt_coefficient_mu    5.057
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13901
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         27.60
_reflns_number_total             6371
_reflns_number_gt                5012
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_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)+(0.0976P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(11)
_refine_ls_number_reflns         6371
_refine_ls_number_parameters     379
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1509
_refine_ls_wR_factor_gt          0.1397
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
Au1 Au 0.64925(3) 0.75468(5) 0.886742(12) 0.04199(13) Uani 1 1 d . . .
P1 P 0.5561(3) 0.94637(16) 0.93693(9) 0.0383(5) Uani 1 1 d . . .
Cl1 Cl 0.6418(5) 0.6072(3) 0.8740(2) 0.0687(11) Uani 1 1 d . . .
N1 N 0.6539(12) 0.8881(9) 0.8923(4) 0.044(3) Uani 1 1 d . . .
C1 C 0.5941(15) 0.7316(10) 0.7728(5) 0.070(4) Uani 1 1 d . . .
H01A H 0.5590 0.6745 0.7796 0.084 Uiso 1 1 calc R . .
O1 O 0.7510(17) 0.2121(15) 0.1783(9) 0.209(11) Uani 1 1 d . . .
Cl2 Cl 0.7012(3) 0.73050(18) 0.97114(11) 0.0545(6) Uani 1 1 d . . .
N2 N 0.6308(11) 0.7851(7) 0.8119(3) 0.050(3) Uani 1 1 d . . .
C2 C 0.6773(12) 0.8724(8) 0.8017(4) 0.051(3) Uani 1 1 d . . .
O2 O 0.9869(18) 0.2937(19) 0.1569(7) 0.218(16) Uani 1 1 d . . .
C3 C 0.7076(18) 0.9044(12) 0.7501(5) 0.077(4) Uani 1 1 d . . .
O3 O 0.796(6) 0.329(2) 0.2037(17) 0.32(2) Uani 1 1 d . . .
Cl3 Cl 0.8903(3) 0.2559(4) 0.19310(11) 0.0647(6) Uani 1 1 d . . .
O4 O 0.985(2) 0.2248(15) 0.2332(7) 0.194(10) Uani 1 1 d . . .
O5 O 0.6279(14) 0.8970(9) 0.1325(5) 0.093(3) Uani 1 1 d . . .
C5 C 0.7102(12) 0.9304(10) 0.8410(5) 0.056(3) Uani 1 1 d . . .
C6 C 0.7588(17) 0.9989(13) 0.8358(6) 0.098(7) Uani 1 1 d . . .
C7 C 0.8029(18) 1.0387(10) 0.7872(7) 0.080(5) Uani 1 1 d . . .
H7A H 0.8519 1.0941 0.7850 0.096 Uiso 1 1 calc R . .
C8 C 0.7675(17) 0.9891(12) 0.7448(6) 0.076(5) Uani 1 1 d . . .
H8A H 0.7838 1.0125 0.7120 0.091 Uiso 1 1 calc R . .
C9 C 0.6615(19) 0.8436(16) 0.7117(5) 0.091(6) Uani 1 1 d . . .
H9A H 0.6676 0.8609 0.6774 0.110 Uiso 1 1 calc R . .
C10 C 0.6073(16) 0.759(2) 0.7225(5) 0.087(5) Uani 1 1 d . . .
H10A H 0.5798 0.7213 0.6957 0.105 Uiso 1 1 calc R . .
C11 C 0.3385(14) 1.0066(9) 0.8604(6) 0.063(3) Uani 1 1 d . . .
H11A H 0.3356 0.9494 0.8484 0.076 Uiso 1 1 calc R . .
C12 C 0.4400(12) 1.0307(7) 0.9041(4) 0.041(2) Uani 1 1 d . . .
C13 C 0.4408(14) 1.1171(7) 0.9206(4) 0.052(2) Uani 1 1 d . . .
H13A H 0.5037 1.1336 0.9495 0.062 Uiso 1 1 calc R . .
C14 C 0.3463(17) 1.1792(10) 0.8936(5) 0.066(4) Uani 1 1 d . . .
H14A H 0.3530 1.2376 0.9034 0.079 Uiso 1 1 calc R . .
C15 C 0.2459(19) 1.1559(8) 0.8537(5) 0.069(4) Uani 1 1 d . . .
H15A H 0.1776 1.1970 0.8376 0.082 Uiso 1 1 calc R . .
C16 C 0.1524(13) 0.7925(9) 0.9695(6) 0.057(3) Uani 1 1 d . . .
H16A H 0.0639 0.7657 0.9516 0.068 Uiso 1 1 calc R . .
C21 C 0.4049(12) 0.8808(6) 0.9729(4) 0.041(2) Uani 1 1 d . . .
C22 C 0.4189(16) 0.8686(7) 1.0245(4) 0.053(3) Uani 1 1 d . . .
H22A H 0.5089 0.8931 1.0429 0.064 Uiso 1 1 calc R . .
C23 C 0.2952(19) 0.8183(9) 1.0496(5) 0.069(3) Uani 1 1 d . . .
H23A H 0.3029 0.8096 1.0850 0.083 Uiso 1 1 calc R . .
C24 C 0.1665(16) 0.7828(9) 1.0235(6) 0.071(4) Uani 1 1 d . . .
H24A H 0.0842 0.7509 1.0412 0.085 Uiso 1 1 calc R . .
C25 C 0.2721(13) 0.8426(7) 0.9434(5) 0.049(2) Uani 1 1 d . . .
H25A H 0.2655 0.8508 0.9079 0.058 Uiso 1 1 calc R . .
C26 C 0.2459(19) 1.0704(10) 0.8370(5) 0.066(4) Uani 1 1 d . . .
H26A H 0.1799 1.0554 0.8085 0.079 Uiso 1 1 calc R . .
C31 C 0.7048(12) 0.9959(7) 0.9811(4) 0.040(2) Uani 1 1 d . . .
C32 C 0.8763(11) 0.9816(7) 0.9713(5) 0.046(2) Uani 1 1 d . . .
H32A H 0.9121 0.9494 0.9428 0.055 Uiso 1 1 calc R . .
C33 C 0.9926(19) 1.0186(8) 1.0068(7) 0.066(4) Uani 1 1 d . . .
H33A H 1.1074 1.0074 1.0028 0.079 Uiso 1 1 calc R . .
C34 C 0.9444(17) 1.0676(8) 1.0449(6) 0.069(4) Uani 1 1 d . . .
H34A H 1.0257 1.0941 1.0659 0.082 Uiso 1 1 calc R . .
C35 C 0.7704(17) 1.0816(8) 1.0552(5) 0.060(3) Uani 1 1 d . . .
H35A H 0.7366 1.1154 1.0831 0.072 Uiso 1 1 calc R . .
C36 C 0.6545(13) 1.0444(7) 1.0230(5) 0.046(2) Uani 1 1 d . . .
H36A H 0.5396 1.0518 1.0294 0.055 Uiso 1 1 calc R . .
C40 C 0.925(3) 0.8925(12) 0.1409(10) 0.111(6) Uani 1 1 d . . .
H40A H 0.9162 0.8529 0.1122 0.166 Uiso 1 1 calc R . .
H40B H 0.9771 0.8634 0.1695 0.166 Uiso 1 1 calc R . .
H40C H 0.9922 0.9424 0.1312 0.166 Uiso 1 1 calc R . .
C41 C 0.756(2) 0.9210(9) 0.1557(6) 0.065(4) Uani 1 1 d . . .
C42 C 0.739(3) 0.9814(14) 0.1990(7) 0.107(6) Uani 1 1 d . . .
H42A H 0.6211 0.9943 0.2043 0.161 Uiso 1 1 calc R . .
H42B H 0.7998 1.0345 0.1917 0.161 Uiso 1 1 calc R . .
H42C H 0.7839 0.9551 0.2297 0.161 Uiso 1 1 calc R . .


_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
Au1 N2 1.998(8) . ?
Au1 N1 2.045(13) . ?
Au1 Cl2 2.254(3) . ?
Au1 Cl1 2.278(5) . ?
P1 N1 1.656(11) . ?
P1 C31 1.799(9) . ?
P1 C12 1.802(10) . ?
P1 C21 1.809(10) . ?
N1 C5 1.540(18) . ?
C1 N2 1.332(15) . ?
C1 C10 1.37(2) . ?
O1 Cl3 1.338(14) . ?
N2 C2 1.407(16) . ?
C2 C5 1.373(18) . ?
C2 C3 1.441(16) . ?
O2 Cl3 1.337(15) . ?
C3 C8 1.38(2) . ?
C3 C9 1.41(3) . ?
O3 Cl3 1.38(3) . ?
Cl3 O4 1.368(15) . ?
O5 C41 1.226(18) . ?
C5 C6 1.12(2) . ?
C6 C7 1.438(18) . ?
C7 C8 1.36(2) . ?
C9 C10 1.38(3) . ?
C11 C26 1.367(19) . ?
C11 C12 1.432(17) . ?
C12 C13 1.388(14) . ?
C13 C14 1.401(17) . ?
C14 C15 1.347(19) . ?
C15 C26 1.376(19) . ?
C16 C25 1.386(16) . ?
C16 C24 1.41(2) . ?
C21 C22 1.356(15) . ?
C21 C25 1.416(15) . ?
C22 C23 1.396(18) . ?
C23 C24 1.331(19) . ?
C31 C36 1.374(15) . ?
C31 C32 1.398(14) . ?
C32 C33 1.414(18) . ?
C33 C34 1.30(2) . ?
C34 C35 1.42(2) . ?
C35 C36 1.358(16) . ?
C40 C41 1.46(3) . ?
C41 C42 1.46(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
N2 Au1 N1 80.5(4) . . ?
N2 Au1 Cl2 172.7(3) . . ?
N1 Au1 Cl2 95.4(3) . . ?
N2 Au1 Cl1 95.1(3) . . ?
N1 Au1 Cl1 175.7(3) . . ?
Cl2 Au1 Cl1 88.88(15) . . ?
N1 P1 C31 111.4(5) . . ?
N1 P1 C12 107.4(5) . . ?
C31 P1 C12 109.4(5) . . ?
N1 P1 C21 111.7(5) . . ?
C31 P1 C21 109.3(5) . . ?
C12 P1 C21 107.5(5) . . ?
C5 N1 P1 120.7(9) . . ?
C5 N1 Au1 111.2(8) . . ?
P1 N1 Au1 125.5(6) . . ?
N2 C1 C10 121.1(17) . . ?
C1 N2 C2 119.5(10) . . ?
C1 N2 Au1 127.6(10) . . ?
C2 N2 Au1 112.7(7) . . ?
C5 C2 N2 121.2(10) . . ?
C5 C2 C3 116.0(14) . . ?
N2 C2 C3 122.5(13) . . ?
C8 C3 C9 129.3(15) . . ?
C8 C3 C2 117.6(15) . . ?
C9 C3 C2 112.9(16) . . ?
O2 Cl3 O1 118.5(14) . . ?
O2 Cl3 O4 111.7(10) . . ?
O1 Cl3 O4 119.6(14) . . ?
O2 Cl3 O3 96(2) . . ?
O1 Cl3 O3 90.9(19) . . ?
O4 Cl3 O3 115.7(19) . . ?
C6 C5 C2 125.1(17) . . ?
C6 C5 N1 126.2(14) . . ?
C2 C5 N1 108.4(12) . . ?
C5 C6 C7 125(2) . . ?
C8 C7 C6 115.0(17) . . ?
C7 C8 C3 120.5(14) . . ?
C10 C9 C3 123.3(14) . . ?
C1 C10 C9 120.1(17) . . ?
C26 C11 C12 118.0(12) . . ?
C13 C12 C11 118.9(10) . . ?
C13 C12 P1 122.6(8) . . ?
C11 C12 P1 118.4(8) . . ?
C12 C13 C14 119.6(11) . . ?
C15 C14 C13 121.3(14) . . ?
C14 C15 C26 119.0(12) . . ?
C25 C16 C24 119.2(11) . . ?
C22 C21 C25 122.3(10) . . ?
C22 C21 P1 122.0(8) . . ?
C25 C21 P1 115.7(8) . . ?
C21 C22 C23 118.5(12) . . ?
C24 C23 C22 121.1(13) . . ?
C23 C24 C16 121.3(12) . . ?
C16 C25 C21 117.6(11) . . ?
C11 C26 C15 122.9(13) . . ?
C36 C31 C32 121.0(9) . . ?
C36 C31 P1 122.5(8) . . ?
C32 C31 P1 116.5(8) . . ?
C31 C32 C33 116.4(11) . . ?
C34 C33 C32 122.2(13) . . ?
C33 C34 C35 121.3(11) . . ?
C36 C35 C34 118.1(12) . . ?
C35 C36 C31 120.8(11) . . ?
O5 C41 C42 119.1(17) . . ?
O5 C41 C40 122.2(17) . . ?
C42 C41 C40 118.8(16) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.774
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.304
_database_code_depnum_ccdc_archive 'CCDC 977990'
#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H24 Cl11 N2 P Pd'
_chemical_formula_weight         939.83

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   19.497(4)
_cell_length_b                   10.517(2)
_cell_length_c                   18.232(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3738.5(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1864
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7986
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         27.49
_reflns_number_total             7986
_reflns_number_gt                6804
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0718P)²+4.0043P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(4)
_refine_ls_number_reflns         7986
_refine_ls_number_parameters     406
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1343
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          2.281
_refine_ls_shift/su_mean         0.138

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.406414(17) 0.61455(3) 1.07223(3) 0.04052(10) Uani 1 1 d . . .
P1 P 0.46751(7) 0.86812(12) 0.98838(8) 0.0421(3) Uani 1 1 d . . .
Cl1 Cl 0.35531(8) 0.48244(14) 1.15581(8) 0.0572(3) Uani 1 1 d . . .
N2 N 0.3949(3) 0.4896(4) 0.9879(3) 0.0510(10) Uani 1 1 d . . .
C1 C 0.3589(4) 0.3835(6) 0.9875(5) 0.0677(17) Uani 1 1 d . . .
H1A H 0.3272 0.3691 1.0247 0.081 Uiso 1 1 calc R . .
Cl2 Cl 0.43790(9) 0.74766(14) 1.16456(8) 0.0568(3) Uani 1 1 d . . .
N1 N 0.4544(2) 0.7159(4) 0.9903(3) 0.0458(10) Uani 1 1 d . . .
C2 C 0.3673(5) 0.2916(7) 0.9321(5) 0.082(2) Uani 1 1 d . . .
H2A H 0.3401 0.2189 0.9319 0.098 Uiso 1 1 calc R . .
C3 C 0.4150(5) 0.3093(7) 0.8792(5) 0.087(3) Uani 1 1 d . . .
H3A H 0.4212 0.2477 0.8431 0.104 Uiso 1 1 calc R . .
Cl3 Cl 0.56910(19) 0.4180(3) 0.05096(18) 0.1309(10) Uani 1 1 d . . .
C4 C 0.4560(4) 0.4225(6) 0.8784(4) 0.0636(16) Uani 1 1 d . . .
Cl4 Cl 0.61544(16) 0.5314(3) 0.1832(2) 0.1208(10) Uani 1 1 d . . .
C5 C 0.4418(3) 0.5129(5) 0.9331(3) 0.0507(12) Uani 1 1 d . . .
Cl5 Cl 0.5476(2) 0.2876(2) 0.1872(2) 0.1218(10) Uani 1 1 d . . .
C6 C 0.4780(3) 0.6314(5) 0.9356(3) 0.0493(12) Uani 1 1 d . . .
Cl6 Cl 0.6557(2) 0.2088(4) 0.8720(2) 0.1498(14) Uani 1 1 d . . .
C7 C 0.5295(4) 0.6497(7) 0.8868(4) 0.0640(16) Uani 1 1 d . . .
H7A H 0.5556 0.7237 0.8887 0.077 Uiso 1 1 calc R . .
Cl7 Cl 0.7259(2) 0.4351(4) 0.8502(4) 0.184(2) Uani 1 1 d . . .
C8 C 0.5435(4) 0.5565(8) 0.8332(4) 0.0744(19) Uani 1 1 d . . .
H8A H 0.5789 0.5714 0.8002 0.089 Uiso 1 1 calc R . .
Cl8 Cl 0.7525(2) 0.2286(6) 0.7580(3) 0.192(2) Uani 1 1 d . . .
C9 C 0.5084(4) 0.4487(8) 0.8275(4) 0.077(2) Uani 1 1 d . . .
H9A H 0.5184 0.3911 0.7903 0.092 Uiso 1 1 calc R . .
Cl9 Cl 0.7193(4) 0.8515(7) 0.9200(3) 0.211(3) Uani 1 1 d . . .
C10 C 0.5518(4) 0.4369(9) 0.1449(6) 0.092(3) Uani 1 1 d . . .
H10A H 0.5075 0.4797 0.1506 0.110 Uiso 1 1 calc R . .
Cl10 Cl 0.7229(5) 0.7411(6) 0.7745(4) 0.275(5) Uani 1 1 d . . .
C11 C 0.4661(3) 0.9265(5) 0.8946(3) 0.0475(11) Uani 1 1 d . . .
Cl11 Cl 0.8163(4) 0.8617(11) 0.8321(8) 0.346(6) Uani 1 1 d . . .
C12 C 0.4044(3) 0.9326(7) 0.8569(4) 0.0564(14) Uani 1 1 d . . .
H12A H 0.3642 0.9086 0.8806 0.068 Uiso 1 1 calc R . .
C13 C 0.4013(4) 0.9726(7) 0.7867(4) 0.0682(17) Uani 1 1 d . . .
H13A H 0.3594 0.9735 0.7623 0.082 Uiso 1 1 calc R . .
C14 C 0.4607(4) 1.0129(7) 0.7503(4) 0.0679(17) Uani 1 1 d . . .
H14A H 0.4584 1.0416 0.7021 0.081 Uiso 1 1 calc R . .
C15 C 0.5227(4) 1.0095(7) 0.7870(4) 0.076(2) Uani 1 1 d . . .
H15A H 0.5626 1.0357 0.7635 0.091 Uiso 1 1 calc R . .
C16 C 0.5253(4) 0.9667(6) 0.8593(4) 0.0639(16) Uani 1 1 d . . .
H16A H 0.5670 0.9652 0.8840 0.077 Uiso 1 1 calc R . .
C20 C 0.6903(5) 0.3049(11) 0.8070(6) 0.104(3) Uani 1 1 d . . .
H20A H 0.6541 0.3335 0.7736 0.124 Uiso 1 1 calc R . .
C21 C 0.5478(3) 0.9135(5) 1.0278(3) 0.0492(12) Uani 1 1 d . . .
C22 C 0.5875(3) 0.8190(6) 1.0613(4) 0.0573(16) Uani 1 1 d . . .
H22A H 0.5715 0.7358 1.0630 0.069 Uiso 1 1 calc R . .
C23 C 0.6505(4) 0.8491(9) 1.0917(4) 0.076(2) Uani 1 1 d . . .
H23A H 0.6770 0.7859 1.1132 0.091 Uiso 1 1 calc R . .
C24 C 0.6737(4) 0.9717(9) 1.0901(4) 0.080(2) Uani 1 1 d . . .
H24A H 0.7155 0.9915 1.1118 0.096 Uiso 1 1 calc R . .
C25 C 0.6365(4) 1.0652(8) 1.0574(5) 0.078(2) Uani 1 1 d . . .
H25A H 0.6529 1.1483 1.0568 0.093 Uiso 1 1 calc R . .
C26 C 0.5734(3) 1.0362(6) 1.0247(4) 0.0622(15) Uani 1 1 d . . .
H26A H 0.5486 1.0994 1.0008 0.075 Uiso 1 1 calc R . .
C31 C 0.3978(3) 0.9459(5) 1.0351(3) 0.0479(11) Uani 1 1 d . . .
C32 C 0.3318(3) 0.9025(6) 1.0245(4) 0.0626(15) Uani 1 1 d . . .
H32A H 0.3242 0.8296 0.9968 0.075 Uiso 1 1 calc R . .
C33 C 0.2774(4) 0.9667(8) 1.0549(5) 0.079(2) Uani 1 1 d . . .
H33A H 0.2327 0.9389 1.0466 0.095 Uiso 1 1 calc R . .
C34 C 0.2893(4) 1.0723(8) 1.0974(5) 0.086(2) Uani 1 1 d . . .
H34A H 0.2525 1.1141 1.1192 0.103 Uiso 1 1 calc R . .
C35 C 0.3548(4) 1.1171(6) 1.1081(5) 0.073(2) Uani 1 1 d . . .
H35A H 0.3621 1.1902 1.1357 0.087 Uiso 1 1 calc R . .
C36 C 0.4091(3) 1.0535(5) 1.0780(6) 0.0644(15) Uani 1 1 d . . .
H36A H 0.4536 1.0821 1.0861 0.077 Uiso 1 1 calc R . .
C30 C 0.7364(7) 0.8651(13) 0.8347(10) 0.139(5) Uani 1 1 d . . .
H30 H 0.7186 0.9452 0.8149 0.166 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N2 2.034(5) . ?
Pd1 N1 2.060(5) . ?
Pd1 Cl2 2.2738(15) . ?
Pd1 Cl1 2.2903(15) . ?
P1 N1 1.622(5) . ?
P1 C21 1.788(6) . ?
P1 C31 1.801(5) . ?
P1 C11 1.817(6) . ?
N2 C1 1.319(8) . ?
N2 C5 1.376(8) . ?
C1 C2 1.407(10) . ?
N1 C6 1.412(7) . ?
C2 C3 1.353(13) . ?
C3 C4 1.435(12) . ?
Cl3 C10 1.756(11) . ?
C4 C9 1.406(11) . ?
C4 C5 1.406(8) . ?
Cl4 C10 1.737(11) . ?
C5 C6 1.432(8) . ?
Cl5 C10 1.752(9) . ?
C6 C7 1.355(9) . ?
Cl6 C20 1.698(10) . ?
C7 C8 1.411(10) . ?
Cl7 C20 1.725(13) . ?
C8 C9 1.329(12) . ?
Cl8 C20 1.707(13) . ?
Cl9 C30 1.597(18) . ?
Cl10 C30 1.724(17) . ?
C11 C12 1.387(8) . ?
C11 C16 1.387(9) . ?
Cl11 C30 1.559(16) . ?
C12 C13 1.349(9) . ?
C13 C14 1.400(11) . ?
C14 C15 1.382(11) . ?
C15 C16 1.394(10) . ?
C21 C26 1.384(8) . ?
C21 C22 1.399(8) . ?
C22 C23 1.383(10) . ?
C23 C24 1.366(12) . ?
C24 C25 1.359(12) . ?
C25 C26 1.401(10) . ?
C31 C32 1.379(9) . ?
C31 C36 1.393(10) . ?
C32 C33 1.375(10) . ?
C33 C34 1.374(12) . ?
C34 C35 1.375(12) . ?
C35 C36 1.368(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 N1 80.5(2) . . ?
N2 Pd1 Cl2 170.63(15) . . ?
N1 Pd1 Cl2 95.51(13) . . ?
N2 Pd1 Cl1 93.62(15) . . ?
N1 Pd1 Cl1 173.73(14) . . ?
Cl2 Pd1 Cl1 89.91(6) . . ?
N1 P1 C21 113.2(3) . . ?
N1 P1 C31 108.6(2) . . ?
C21 P1 C31 110.5(3) . . ?
N1 P1 C11 110.6(3) . . ?
C21 P1 C11 107.5(3) . . ?
C31 P1 C11 106.3(3) . . ?
C1 N2 C5 120.0(5) . . ?
C1 N2 Pd1 127.5(5) . . ?
C5 N2 Pd1 111.1(4) . . ?
N2 C1 C2 121.6(8) . . ?
C6 N1 P1 123.7(4) . . ?
C6 N1 Pd1 109.5(4) . . ?
P1 N1 Pd1 126.7(3) . . ?
C3 C2 C1 119.8(7) . . ?
C2 C3 C4 120.3(6) . . ?
C9 C4 C5 118.6(7) . . ?
C9 C4 C3 125.0(7) . . ?
C5 C4 C3 116.4(7) . . ?
N2 C5 C4 121.7(6) . . ?
N2 C5 C6 117.3(5) . . ?
C4 C5 C6 120.9(6) . . ?
C7 C6 N1 128.0(6) . . ?
C7 C6 C5 117.9(6) . . ?
N1 C6 C5 114.1(5) . . ?
C6 C7 C8 119.9(7) . . ?
C9 C8 C7 123.2(7) . . ?
C8 C9 C4 119.3(6) . . ?
Cl4 C10 Cl5 111.7(5) . . ?
Cl4 C10 Cl3 108.6(5) . . ?
Cl5 C10 Cl3 109.7(6) . . ?
C12 C11 C16 118.5(6) . . ?
C12 C11 P1 119.7(4) . . ?
C16 C11 P1 121.9(5) . . ?
C13 C12 C11 121.6(6) . . ?
C12 C13 C14 120.5(6) . . ?
C15 C14 C13 119.1(6) . . ?
C14 C15 C16 119.9(7) . . ?
C11 C16 C15 120.5(7) . . ?
Cl6 C20 Cl8 111.6(7) . . ?
Cl6 C20 Cl7 108.3(7) . . ?
Cl8 C20 Cl7 109.1(6) . . ?
C26 C21 C22 118.7(6) . . ?
C26 C21 P1 123.2(5) . . ?
C22 C21 P1 118.1(4) . . ?
C23 C22 C21 120.2(6) . . ?
C24 C23 C22 120.1(7) . . ?
C25 C24 C23 121.1(7) . . ?
C24 C25 C26 119.8(7) . . ?
C21 C26 C25 120.1(7) . . ?
C32 C31 C36 119.7(5) . . ?
C32 C31 P1 119.1(5) . . ?
C36 C31 P1 121.0(4) . . ?
C33 C32 C31 120.1(7) . . ?
C34 C33 C32 119.6(7) . . ?
C35 C34 C33 120.9(6) . . ?
C36 C35 C34 119.7(7) . . ?
C35 C36 C31 120.0(6) . . ?
Cl11 C30 Cl9 103.6(12) . . ?
Cl11 C30 Cl10 96.7(10) . . ?
Cl9 C30 Cl10 121.4(9) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.081
_database_code_depnum_ccdc_archive 'CCDC 977991'
