# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Qun-Li Luo'
_publ_contact_author_email       qunli.luo@gmail.com
loop_
_publ_author_name
'Qun-Li Luo'
'Jian-Ping Tan'
'Zhi-Fu Li'
'Yue Qin'
'Lin Ma'
'Dong-Rong Xiao'

data_compound-1
_database_code_depnum_ccdc_archive 'CCDC 785152'
#TrackingRef '- compounds 1 and 2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H11 Br N2 O2 Pd'
_chemical_formula_weight         425.56

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'
Br Br -0.2901 2.4595 '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   Cmc2(1)

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

_cell_length_a                   6.7355(13)
_cell_length_b                   11.269(2)
_cell_length_c                   18.178(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1379.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5015
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      28.26

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    4.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3265
_exptl_absorpt_correction_T_max  0.7278
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_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 APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5015
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         28.26
_reflns_number_total             1760
_reflns_number_gt                1643
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.028(7)
_refine_ls_number_reflns         1760
_refine_ls_number_parameters     123
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0188
_refine_ls_wR_factor_ref         0.0395
_refine_ls_wR_factor_gt          0.0392
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_restrained_S_all      0.830
_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
Pd1 Pd 1.0000 0.32589(2) 0.931740(16) 0.03111(7) Uani 1 2 d S . .
Br1 Br 1.0000 0.36862(5) 1.06908(3) 0.05576(15) Uani 1 2 d S . .
O1 O 1.0000 0.6828(3) 0.8526(2) 0.0514(11) Uani 1 2 d S . .
O2 O 1.0000 -0.0513(3) 0.9476(2) 0.0504(9) Uani 1 2 d S . .
N1 N 1.0000 0.4965(3) 0.88967(17) 0.0332(7) Uani 1 2 d S . .
N2 N 1.0000 0.1414(2) 0.9348(3) 0.0367(6) Uani 1 2 d S . .
C1 C 1.0000 0.6595(4) 0.9855(3) 0.0431(13) Uani 1 2 d S . .
H1A H 0.9009 0.7206 0.9887 0.043 Uiso 0.50 1 calc PR . .
H1B H 1.1282 0.6928 0.9960 0.043 Uiso 0.50 1 calc PR . .
H1C H 0.9709 0.5982 1.0205 0.043 Uiso 0.50 1 calc PR . .
C2 C 1.0000 0.6087(4) 0.9104(3) 0.0384(10) Uani 1 2 d S . .
C3 C 1.0000 0.6132(4) 0.7907(3) 0.0470(10) Uani 1 2 d S . .
H3A H 1.0000 0.6406 0.7425 0.056 Uiso 1 2 calc SR . .
C4 C 1.0000 0.4998(4) 0.8114(2) 0.0396(8) Uani 1 2 d S . .
C5 C 1.0000 0.3833(4) 0.7764(2) 0.0391(10) Uani 1 2 d S . .
C6 C 1.0000 0.3569(4) 0.7014(3) 0.0588(13) Uani 1 2 d S . .
H6A H 1.0000 0.4178 0.6669 0.071 Uiso 1 2 calc SR . .
C7 C 1.0000 0.2407(5) 0.6786(3) 0.0691(14) Uani 1 2 d S . .
H7A H 1.0000 0.2240 0.6285 0.083 Uiso 1 2 calc SR . .
C8 C 1.0000 0.1472(4) 0.7290(3) 0.0556(13) Uani 1 2 d S . .
H8A H 1.0000 0.0689 0.7129 0.067 Uiso 1 2 calc SR . .
C9 C 1.0000 0.1732(3) 0.8033(3) 0.0388(8) Uani 1 2 d S . .
C10 C 1.0000 0.2912(3) 0.8274(2) 0.0346(8) Uani 1 2 d S . .
C11 C 1.0000 0.0890(4) 0.8645(2) 0.0383(10) Uani 1 2 d S . .
C12 C 1.0000 -0.0292(4) 0.8733(3) 0.0500(11) Uani 1 2 d S . .
H12A H 1.0000 -0.0857 0.8360 0.060 Uiso 1 2 calc SR . .
C13 C 1.0000 0.0536(4) 0.9811(3) 0.0409(11) Uani 1 2 d S . .
C14 C 1.0000 0.0535(4) 1.0624(3) 0.0528(11) Uani 1 2 d S . .
H14A H 0.9080 -0.0050 1.0800 0.053 Uiso 0.50 1 calc PR . .
H14B H 0.9612 0.1304 1.0800 0.053 Uiso 0.50 1 calc PR . .
H14C H 1.1308 0.0351 1.0800 0.053 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.04120(12) 0.02416(11) 0.02796(13) 0.00221(15) 0.000 0.000
Br1 0.0903(4) 0.0430(3) 0.0340(2) -0.0019(2) 0.000 0.000
O1 0.073(2) 0.0252(14) 0.057(3) 0.0102(16) 0.000 0.000
O2 0.0608(16) 0.0284(13) 0.062(3) 0.0104(15) 0.000 0.000
N1 0.0401(16) 0.0259(15) 0.0337(19) 0.0039(12) 0.000 0.000
N2 0.0422(14) 0.0302(13) 0.0376(18) 0.001(3) 0.000 0.000
C1 0.053(2) 0.029(3) 0.048(4) -0.007(2) 0.000 0.000
C2 0.0416(19) 0.0273(18) 0.046(3) 0.0042(16) 0.000 0.000
C3 0.065(3) 0.039(2) 0.037(3) 0.015(2) 0.000 0.000
C4 0.048(2) 0.0349(19) 0.036(2) 0.0073(15) 0.000 0.000
C5 0.050(2) 0.030(2) 0.038(3) 0.0042(18) 0.000 0.000
C6 0.086(4) 0.046(3) 0.045(3) 0.014(2) 0.000 0.000
C7 0.117(4) 0.061(3) 0.029(2) -0.003(2) 0.000 0.000
C8 0.082(3) 0.038(2) 0.047(3) -0.0109(19) 0.000 0.000
C9 0.050(2) 0.0296(18) 0.037(2) -0.0009(16) 0.000 0.000
C10 0.0389(19) 0.0300(18) 0.035(2) 0.0063(17) 0.000 0.000
C11 0.047(2) 0.0312(19) 0.037(3) 0.0037(19) 0.000 0.000
C12 0.064(3) 0.031(2) 0.055(3) 0.000(2) 0.000 0.000
C13 0.046(2) 0.035(3) 0.042(3) 0.005(2) 0.000 0.000
C14 0.074(3) 0.047(3) 0.037(3) 0.015(2) 0.000 0.000

_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 C10 1.937(4) . ?
Pd1 N1 2.069(3) . ?
Pd1 N2 2.080(2) . ?
Pd1 Br1 2.5425(8) . ?
O1 C2 1.343(5) . ?
O1 C3 1.370(6) . ?
O2 C13 1.329(6) . ?
O2 C12 1.373(7) . ?
N1 C2 1.320(5) . ?
N1 C4 1.423(5) . ?
N2 C13 1.300(6) . ?
N2 C11 1.408(6) . ?
C1 C2 1.480(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 C4 1.332(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.459(6) . ?
C5 C10 1.392(5) . ?
C5 C6 1.396(8) . ?
C6 C7 1.373(7) . ?
C6 H6A 0.9300 . ?
C7 C8 1.397(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.381(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.400(5) . ?
C9 C11 1.462(6) . ?
C11 C12 1.341(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.477(8) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?

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
C10 Pd1 N1 79.96(14) . . ?
C10 Pd1 N2 79.89(18) . . ?
N1 Pd1 N2 159.85(16) . . ?
C10 Pd1 Br1 179.27(11) . . ?
N1 Pd1 Br1 100.77(9) . . ?
N2 Pd1 Br1 99.38(14) . . ?
C2 O1 C3 106.7(3) . . ?
C13 O2 C12 106.9(4) . . ?
C2 N1 C4 105.1(3) . . ?
C2 N1 Pd1 141.7(3) . . ?
C4 N1 Pd1 113.2(3) . . ?
C13 N2 C11 105.6(4) . . ?
C13 N2 Pd1 141.2(4) . . ?
C11 N2 Pd1 113.3(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 O1 111.8(4) . . ?
N1 C2 C1 129.4(4) . . ?
O1 C2 C1 118.8(4) . . ?
C4 C3 O1 108.5(4) . . ?
C4 C3 H3A 125.7 . . ?
O1 C3 H3A 125.7 . . ?
C3 C4 N1 107.9(4) . . ?
C3 C4 C5 137.8(5) . . ?
N1 C4 C5 114.4(4) . . ?
C10 C5 C6 119.5(4) . . ?
C10 C5 C4 112.4(4) . . ?
C6 C5 C4 128.2(4) . . ?
C7 C6 C5 119.9(5) . . ?
C7 C6 H6A 120.1 . . ?
C5 C6 H6A 120.1 . . ?
C6 C7 C8 121.4(5) . . ?
C6 C7 H7A 119.3 . . ?
C8 C7 H7A 119.3 . . ?
C9 C8 C7 118.8(4) . . ?
C9 C8 H8A 120.6 . . ?
C7 C8 H8A 120.6 . . ?
C8 C9 C10 120.4(4) . . ?
C8 C9 C11 127.3(4) . . ?
C10 C9 C11 112.2(4) . . ?
C5 C10 C9 120.0(4) . . ?
C5 C10 Pd1 120.1(3) . . ?
C9 C10 Pd1 119.9(3) . . ?
C12 C11 N2 107.9(4) . . ?
C12 C11 C9 137.3(5) . . ?
N2 C11 C9 114.7(4) . . ?
C11 C12 O2 107.3(4) . . ?
C11 C12 H12A 126.4 . . ?
O2 C12 H12A 126.4 . . ?
N2 C13 O2 112.3(4) . . ?
N2 C13 C14 130.4(5) . . ?
O2 C13 C14 117.3(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 Pd1 N1 C2 180.000(3) . . . . ?
N2 Pd1 N1 C2 180.000(3) . . . . ?
Br1 Pd1 N1 C2 0.000(3) . . . . ?
C10 Pd1 N1 C4 0.000(1) . . . . ?
N2 Pd1 N1 C4 0.000(2) . . . . ?
Br1 Pd1 N1 C4 180.000(1) . . . . ?
C10 Pd1 N2 C13 180.000(3) . . . . ?
N1 Pd1 N2 C13 180.000(2) . . . . ?
Br1 Pd1 N2 C13 0.000(3) . . . . ?
C10 Pd1 N2 C11 0.000(1) . . . . ?
N1 Pd1 N2 C11 0.000(2) . . . . ?
Br1 Pd1 N2 C11 180.000(1) . . . . ?
C4 N1 C2 O1 0.000(2) . . . . ?
Pd1 N1 C2 O1 180.000(2) . . . . ?
C4 N1 C2 C1 180.000(3) . . . . ?
Pd1 N1 C2 C1 0.000(4) . . . . ?
C3 O1 C2 N1 0.000(2) . . . . ?
C3 O1 C2 C1 180.000(2) . . . . ?
C2 O1 C3 C4 0.000(2) . . . . ?
O1 C3 C4 N1 0.000(2) . . . . ?
O1 C3 C4 C5 180.000(3) . . . . ?
C2 N1 C4 C3 0.000(2) . . . . ?
Pd1 N1 C4 C3 180.000(2) . . . . ?
C2 N1 C4 C5 180.000(2) . . . . ?
Pd1 N1 C4 C5 0.000(2) . . . . ?
C3 C4 C5 C10 180.000(2) . . . . ?
N1 C4 C5 C10 0.000(2) . . . . ?
C3 C4 C5 C6 0.000(4) . . . . ?
N1 C4 C5 C6 180.000(2) . . . . ?
C10 C5 C6 C7 0.000(3) . . . . ?
C4 C5 C6 C7 180.000(2) . . . . ?
C5 C6 C7 C8 0.000(2) . . . . ?
C6 C7 C8 C9 0.000(2) . . . . ?
C7 C8 C9 C10 0.000(2) . . . . ?
C7 C8 C9 C11 180.000(2) . . . . ?
C6 C5 C10 C9 0.000(2) . . . . ?
C4 C5 C10 C9 180.000(2) . . . . ?
C6 C5 C10 Pd1 180.000(1) . . . . ?
C4 C5 C10 Pd1 0.000(2) . . . . ?
C8 C9 C10 C5 0.000(2) . . . . ?
C11 C9 C10 C5 180.000(2) . . . . ?
C8 C9 C10 Pd1 180.000(1) . . . . ?
C11 C9 C10 Pd1 0.000(1) . . . . ?
N1 Pd1 C10 C5 0.000(1) . . . . ?
N2 Pd1 C10 C5 180.000(1) . . . . ?
Br1 Pd1 C10 C5 180.00(6) . . . . ?
N1 Pd1 C10 C9 180.000(1) . . . . ?
N2 Pd1 C10 C9 0.000(1) . . . . ?
Br1 Pd1 C10 C9 0.00(6) . . . . ?
C13 N2 C11 C12 0.000(2) . . . . ?
Pd1 N2 C11 C12 180.000(2) . . . . ?
C13 N2 C11 C9 180.000(2) . . . . ?
Pd1 N2 C11 C9 0.000(2) . . . . ?
C8 C9 C11 C12 0.000(3) . . . . ?
C10 C9 C11 C12 180.000(2) . . . . ?
C8 C9 C11 N2 180.000(1) . . . . ?
C10 C9 C11 N2 0.000(2) . . . . ?
N2 C11 C12 O2 0.000(2) . . . . ?
C9 C11 C12 O2 180.000(2) . . . . ?
C13 O2 C12 C11 0.000(2) . . . . ?
C11 N2 C13 O2 0.000(2) . . . . ?
Pd1 N2 C13 O2 180.000(2) . . . . ?
C11 N2 C13 C14 180.000(2) . . . . ?
Pd1 N2 C13 C14 0.000(4) . . . . ?
C12 O2 C13 N2 0.000(2) . . . . ?
C12 O2 C13 C14 180.000(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.26
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.164

#===END

data_compound-2
_database_code_depnum_ccdc_archive 'CCDC 785153'
#TrackingRef '- compounds 1 and 2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H11 Br N2 O Pd S'
_chemical_formula_weight         441.62

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'
Br Br -0.2901 2.4595 '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   P2(1)/n

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

_cell_length_a                   10.610(2)
_cell_length_b                   11.703(2)
_cell_length_c                   12.051(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.59(3)
_cell_angle_gamma                90.00
_cell_volume                     1434.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10463
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.34

_exptl_crystal_description       prism
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3453
_exptl_absorpt_correction_T_max  0.6539
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_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 APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10463
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         28.34
_reflns_number_total             3437
_reflns_number_gt                2365
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         3437
_refine_ls_number_parameters     183
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1185
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.005
_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
Pd1 Pd 0.55218(3) 0.91136(3) 0.19248(3) 0.05231(16) Uani 1 1 d . . .
Br1 Br 0.43573(8) 0.84305(8) 0.33757(7) 0.1087(3) Uani 1 1 d U . .
S1 S 0.6587(2) 0.56443(17) 0.0847(2) 0.0717(5) Uani 0.50 1 d PU A 1
O1A O 0.6587(2) 0.56443(17) 0.0847(2) 0.0717(5) Uani 0.50 1 d PU A 2
O1 O 0.4911(3) 1.2848(2) 0.2323(2) 0.0931(8) Uani 0.50 1 d PU B 1
S1A S 0.4911(3) 1.2848(2) 0.2323(2) 0.0931(8) Uani 0.50 1 d PU B 2
N1 N 0.5315(4) 1.0868(4) 0.2058(4) 0.0611(11) Uani 1 1 d . B .
N2 N 0.6060(3) 0.7541(4) 0.1377(3) 0.0558(9) Uani 1 1 d . A .
C1 C 0.3773(8) 1.1337(9) 0.3248(7) 0.108(2) Uani 1 1 d U B .
H1A H 0.3261 1.0669 0.2957 0.108 Uiso 1 1 calc R . .
H1B H 0.3197 1.1979 0.3206 0.108 Uiso 1 1 calc R . .
H1C H 0.4272 1.1213 0.4039 0.108 Uiso 1 1 calc R . .
C2 C 0.4683(6) 1.1572(5) 0.2540(5) 0.0748(16) Uani 1 1 d U . .
C3 C 0.5888(6) 1.2622(6) 0.1594(6) 0.0851(18) Uani 1 1 d U . .
H3A H 0.6301 1.3192 0.1288 0.102 Uiso 1 1 calc R B 1
C4 C 0.6053(5) 1.1501(5) 0.1467(5) 0.0663(13) Uani 1 1 d U B .
C5 C 0.6786(5) 1.0792(5) 0.0860(5) 0.0632(13) Uani 1 1 d . . .
C6 C 0.7592(6) 1.1179(6) 0.0202(6) 0.0792(17) Uani 1 1 d . B .
H6A H 0.7709 1.1958 0.0111 0.095 Uiso 1 1 calc R . .
C7 C 0.8219(6) 1.0377(6) -0.0316(5) 0.0790(16) Uani 1 1 d . . .
H7A H 0.8743 1.0625 -0.0770 0.095 Uiso 1 1 calc R B .
C8 C 0.8070(5) 0.9211(5) -0.0161(5) 0.0706(15) Uani 1 1 d . B .
H8A H 0.8514 0.8685 -0.0491 0.085 Uiso 1 1 calc R . .
C9 C 0.7255(5) 0.8830(5) 0.0489(4) 0.0576(11) Uani 1 1 d . . .
C10 C 0.6616(4) 0.9636(4) 0.0976(4) 0.0533(10) Uani 1 1 d . B .
C11 C 0.6936(4) 0.7660(5) 0.0701(4) 0.0586(12) Uani 1 1 d . A .
C12 C 0.7279(5) 0.6624(5) 0.0398(5) 0.0709(14) Uani 1 1 d U . .
H12A H 0.7868 0.6512 -0.0034 0.085 Uiso 1 1 calc R A 1
C13 C 0.5802(5) 0.6474(5) 0.1474(4) 0.0636(13) Uani 1 1 d . . .
C14 C 0.4903(8) 0.5933(6) 0.2040(7) 0.092(2) Uani 1 1 d U A .
H14A H 0.5376 0.5380 0.2591 0.092 Uiso 1 1 calc R . .
H14B H 0.4206 0.5560 0.1468 0.092 Uiso 1 1 calc R . .
H14C H 0.4540 0.6504 0.2431 0.092 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0509(2) 0.0619(3) 0.0492(2) -0.00562(15) 0.02241(17) -0.00161(15)
Br1 0.1385(7) 0.1194(7) 0.1024(5) -0.0001(4) 0.0894(5) -0.0063(5)
S1 0.0781(13) 0.0585(11) 0.0804(13) -0.0098(9) 0.0257(11) -0.0051(9)
O1A 0.0781(13) 0.0585(11) 0.0804(13) -0.0098(9) 0.0257(11) -0.0051(9)
O1 0.1050(18) 0.0646(13) 0.0964(16) -0.0063(12) 0.0074(14) 0.0095(12)
S1A 0.1050(18) 0.0646(13) 0.0964(16) -0.0063(12) 0.0074(14) 0.0095(12)
N1 0.054(2) 0.066(3) 0.061(2) -0.0058(19) 0.012(2) 0.0003(19)
N2 0.0488(19) 0.071(3) 0.052(2) -0.0071(18) 0.0201(17) -0.0057(19)
C1 0.100(5) 0.132(5) 0.099(5) -0.024(4) 0.039(4) 0.030(4)
C2 0.069(3) 0.080(4) 0.069(3) -0.021(3) 0.008(3) 0.022(3)
C3 0.078(4) 0.082(4) 0.085(4) 0.018(3) 0.006(3) -0.003(3)
C4 0.063(3) 0.061(3) 0.067(3) 0.000(3) 0.004(3) 0.002(3)
C5 0.054(3) 0.074(3) 0.060(3) 0.006(2) 0.015(2) -0.003(2)
C6 0.070(3) 0.085(4) 0.083(4) 0.023(3) 0.023(3) -0.002(3)
C7 0.067(3) 0.102(5) 0.077(4) 0.024(3) 0.035(3) -0.002(3)
C8 0.056(3) 0.097(4) 0.065(3) 0.005(3) 0.026(3) -0.001(3)
C9 0.054(3) 0.072(3) 0.048(2) 0.003(2) 0.017(2) -0.003(2)
C10 0.044(2) 0.067(3) 0.051(2) 0.005(2) 0.017(2) -0.003(2)
C11 0.051(2) 0.082(4) 0.045(2) -0.006(2) 0.017(2) -0.001(3)
C12 0.076(3) 0.076(4) 0.066(3) -0.015(3) 0.029(3) 0.013(3)
C13 0.058(3) 0.073(4) 0.059(3) -0.010(3) 0.015(2) -0.013(3)
C14 0.098(4) 0.094(4) 0.091(4) -0.001(3) 0.037(4) -0.035(4)

_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 C10 1.946(5) . ?
Pd1 N1 2.076(4) . ?
Pd1 N2 2.089(4) . ?
Pd1 Br1 2.5411(9) . ?
S1 C12 1.541(6) . ?
S1 C13 1.602(6) . ?
O1 C3 1.561(9) . ?
O1 C2 1.547(7) . ?
N1 C2 1.299(7) . ?
N1 C4 1.411(8) . ?
N2 C13 1.291(7) . ?
N2 C11 1.406(6) . ?
C1 C2 1.486(11) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 C4 1.339(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.467(8) . ?
C5 C10 1.378(7) . ?
C5 C6 1.397(9) . ?
C6 C7 1.397(10) . ?
C6 H6A 0.9300 . ?
C7 C8 1.393(9) . ?
C7 H7A 0.9300 . ?
C8 C9 1.395(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.387(8) . ?
C9 C11 1.450(8) . ?
C11 C12 1.347(7) . ?
C12 H12A 0.9300 . ?
C13 C14 1.465(9) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?

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
C10 Pd1 N1 80.2(2) . . ?
C10 Pd1 N2 80.09(19) . . ?
N1 Pd1 N2 160.09(18) . . ?
C10 Pd1 Br1 172.77(13) . . ?
N1 Pd1 Br1 100.07(14) . . ?
N2 Pd1 Br1 99.84(11) . . ?
C12 S1 C13 94.5(3) . . ?
C3 O1 C2 95.3(4) . . ?
C2 N1 C4 108.9(5) . . ?
C2 N1 Pd1 137.9(5) . . ?
C4 N1 Pd1 113.2(4) . . ?
C13 N2 C11 109.9(4) . . ?
C13 N2 Pd1 137.7(4) . . ?
C11 N2 Pd1 112.4(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 129.9(6) . . ?
N1 C2 O1 114.3(5) . . ?
C1 C2 O1 115.7(5) . . ?
C4 C3 O1 111.1(6) . . ?
C4 C3 H3A 124.5 . . ?
O1 C3 H3A 124.5 . . ?
C3 C4 N1 110.3(6) . . ?
C3 C4 C5 135.8(6) . . ?
N1 C4 C5 113.9(5) . . ?
C10 C5 C6 119.7(6) . . ?
C10 C5 C4 113.7(5) . . ?
C6 C5 C4 126.7(5) . . ?
C7 C6 C5 118.9(6) . . ?
C7 C6 H6A 120.6 . . ?
C5 C6 H6A 120.6 . . ?
C8 C7 C6 120.8(5) . . ?
C8 C7 H7A 119.6 . . ?
C6 C7 H7A 119.6 . . ?
C7 C8 C9 120.1(6) . . ?
C7 C8 H8A 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C10 C9 C8 118.5(5) . . ?
C10 C9 C11 113.6(4) . . ?
C8 C9 C11 127.9(5) . . ?
C5 C10 C9 122.1(5) . . ?
C5 C10 Pd1 119.0(4) . . ?
C9 C10 Pd1 118.8(4) . . ?
C12 C11 N2 110.0(5) . . ?
C12 C11 C9 135.0(5) . . ?
N2 C11 C9 115.0(4) . . ?
C11 C12 S1 112.5(4) . . ?
C11 C12 H12A 123.8 . . ?
S1 C12 H12A 123.8 . . ?
N2 C13 C14 130.1(6) . . ?
N2 C13 S1 113.0(4) . . ?
C14 C13 S1 116.9(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 Pd1 N1 C2 178.1(6) . . . . ?
N2 Pd1 N1 C2 170.6(5) . . . . ?
Br1 Pd1 N1 C2 -9.3(6) . . . . ?
C10 Pd1 N1 C4 -1.8(3) . . . . ?
N2 Pd1 N1 C4 -9.3(7) . . . . ?
Br1 Pd1 N1 C4 170.8(3) . . . . ?
C10 Pd1 N2 C13 -176.0(5) . . . . ?
N1 Pd1 N2 C13 -168.5(5) . . . . ?
Br1 Pd1 N2 C13 11.4(5) . . . . ?
C10 Pd1 N2 C11 3.1(3) . . . . ?
N1 Pd1 N2 C11 10.6(6) . . . . ?
Br1 Pd1 N2 C11 -169.6(3) . . . . ?
C4 N1 C2 C1 179.6(6) . . . . ?
Pd1 N1 C2 C1 -0.3(10) . . . . ?
C4 N1 C2 O1 0.5(6) . . . . ?
Pd1 N1 C2 O1 -179.4(3) . . . . ?
C3 O1 C2 N1 -1.2(5) . . . . ?
C3 O1 C2 C1 179.6(5) . . . . ?
C2 O1 C3 C4 1.5(5) . . . . ?
O1 C3 C4 N1 -1.5(6) . . . . ?
O1 C3 C4 C5 177.5(5) . . . . ?
C2 N1 C4 C3 0.6(6) . . . . ?
Pd1 N1 C4 C3 -179.4(4) . . . . ?
C2 N1 C4 C5 -178.5(5) . . . . ?
Pd1 N1 C4 C5 1.4(5) . . . . ?
C3 C4 C5 C10 -178.7(6) . . . . ?
N1 C4 C5 C10 0.2(7) . . . . ?
C3 C4 C5 C6 0.8(11) . . . . ?
N1 C4 C5 C6 179.7(5) . . . . ?
C10 C5 C6 C7 -0.6(8) . . . . ?
C4 C5 C6 C7 179.9(5) . . . . ?
C5 C6 C7 C8 -1.4(9) . . . . ?
C6 C7 C8 C9 2.0(9) . . . . ?
C7 C8 C9 C10 -0.5(8) . . . . ?
C7 C8 C9 C11 177.1(5) . . . . ?
C6 C5 C10 C9 2.1(8) . . . . ?
C4 C5 C10 C9 -178.3(4) . . . . ?
C6 C5 C10 Pd1 178.6(4) . . . . ?
C4 C5 C10 Pd1 -1.9(6) . . . . ?
C8 C9 C10 C5 -1.6(8) . . . . ?
C11 C9 C10 C5 -179.5(4) . . . . ?
C8 C9 C10 Pd1 -178.0(4) . . . . ?
C11 C9 C10 Pd1 4.0(6) . . . . ?
N1 Pd1 C10 C5 2.1(4) . . . . ?
N2 Pd1 C10 C5 179.5(4) . . . . ?
Br1 Pd1 C10 C5 -90.4(13) . . . . ?
N1 Pd1 C10 C9 178.6(4) . . . . ?
N2 Pd1 C10 C9 -4.0(4) . . . . ?
Br1 Pd1 C10 C9 86.1(13) . . . . ?
C13 N2 C11 C12 -2.4(6) . . . . ?
Pd1 N2 C11 C12 178.3(3) . . . . ?
C13 N2 C11 C9 177.4(4) . . . . ?
Pd1 N2 C11 C9 -1.9(5) . . . . ?
C10 C9 C11 C12 178.6(6) . . . . ?
C8 C9 C11 C12 0.9(9) . . . . ?
C10 C9 C11 N2 -1.1(6) . . . . ?
C8 C9 C11 N2 -178.8(5) . . . . ?
N2 C11 C12 S1 1.6(6) . . . . ?
C9 C11 C12 S1 -178.1(5) . . . . ?
C13 S1 C12 C11 -0.4(5) . . . . ?
C11 N2 C13 C14 -176.7(6) . . . . ?
Pd1 N2 C13 C14 2.4(9) . . . . ?
C11 N2 C13 S1 2.1(5) . . . . ?
Pd1 N2 C13 S1 -178.8(3) . . . . ?
C12 S1 C13 N2 -1.1(5) . . . . ?
C12 S1 C13 C14 177.9(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.107

#===END