#====================
data_global 
 
_publ_contact_author 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
_publ_contact_author_email      hmalinakova@ku.edu 
_publ_contact_author_fax        1(785)8645396 
_publ_contact_author_phone      1(785)8644743 
 
_publ_requested_journal         'Organometallics Chemistry'  
 
loop_ 
    _publ_author_name 
    _publ_author_address 
  'Guo, Ruiyun' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Portscheller, Jannelle L.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Day, Victor W.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Malinakova, Helena C.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
 
_publ_section_title 
; 
 Allylpalladium(IV) Intermediate inthe Synthesis of Highly Substituted 
 Benzoxepines and Benzopyrans via Reactions of Stable Palla(II)cycles 
 with Allyl Bromides                            
; 
_publ_section_references 
;
  Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
 
  Flack, H. D. (1983) Acta Cryst. A39, 876-881. 
 
  Flack, H. D. and Schwarzenbach, D. (1988) Acta Cryst. A44, 
  499-506. 
 
  Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
;
_publ_section_acknowledgements 
; 
 The authors wish to thank the National Science Foundation 
 (CHE-0079282) and the University of Kansas for funds to 
 acquire the diffractometer and computers used in this work.  
; 
  
data_k99a(3a) 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C25 H35 Cl3 N2 O3 Pd' 
_chemical_formula_weight          624.30 
  
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' 
 '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            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    16.4476(11) 
_cell_length_b                    9.9513(6) 
_cell_length_c                    17.7253(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  113.0110(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2670.3(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     7484 
_cell_measurement_theta_min       2.33 
_cell_measurement_theta_max       30.02 
  
_exptl_crystal_description        'Near cube' 
_exptl_crystal_colour             Gold/yellow 
_exptl_crystal_size_max           0.24 
_exptl_crystal_size_mid           0.24 
_exptl_crystal_size_min           0.22 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.553 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1280 
_exptl_absorpt_coefficient_mu     1.025 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.6508 
_exptl_absorpt_correction_T_max   0.7125 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       100(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 SMART 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_%         0.00 
_diffrn_reflns_number             30984 
_diffrn_reflns_av_R_equivalents   0.0344 
_diffrn_reflns_av_sigmaI/netI     0.0300 
_diffrn_reflns_limit_h_min        -23 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          2.33 
_diffrn_reflns_theta_max          30.03 
_reflns_number_total              7774 
_reflns_number_gt                 6769 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_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)+(0.0365P)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_number_reflns          7774 
_refine_ls_number_parameters      317 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0292 
_refine_ls_R_factor_gt            0.0248 
_refine_ls_wR_factor_ref          0.0637 
_refine_ls_wR_factor_gt           0.0624 
_refine_ls_goodness_of_fit_ref    1.014 
_refine_ls_restrained_S_all       1.014 
_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 
Pd Pd 0.107858(7) 0.357352(11) -0.012179(6) 0.01171(4) Uani 1 1 d . . . 
O1 O 0.17318(7) 0.53813(11) -0.10542(6) 0.0169(2) Uani 1 1 d . . . 
O2 O 0.29939(7) 0.24822(11) -0.01802(6) 0.0192(2) Uani 1 1 d . . . 
O3 O 0.22436(8) 0.30299(13) -0.14999(7) 0.0267(3) Uani 1 1 d . . . 
N1 N 0.01642(8) 0.26212(12) 0.03160(7) 0.0137(2) Uani 1 1 d . . . 
N2 N 0.18872(8) 0.30238(12) 0.11004(7) 0.0136(2) Uani 1 1 d . . . 
C1 C 0.03555(9) 0.43907(14) -0.12198(8) 0.0138(3) Uani 1 1 d . . . 
C2 C 0.08466(9) 0.52431(15) -0.15159(9) 0.0148(3) Uani 1 1 d . . . 
C3 C 0.04861(10) 0.60017(16) -0.22266(9) 0.0177(3) Uani 1 1 d . . . 
H3 H 0.0849 0.6572 -0.2392 0.021 Uiso 1 1 calc R . . 
C4 C -0.04155(10) 0.59124(16) -0.26915(9) 0.0189(3) Uani 1 1 d . . . 
H4 H -0.0678 0.6428 -0.3178 0.023 Uiso 1 1 calc R . . 
C5 C -0.09275(10) 0.50641(16) -0.24379(9) 0.0193(3) Uani 1 1 d . . . 
H5 H -0.1542 0.4986 -0.2759 0.023 Uiso 1 1 calc R . . 
C6 C -0.05489(10) 0.43222(15) -0.17145(9) 0.0164(3) Uani 1 1 d . . . 
H6 H -0.0916 0.3753 -0.1553 0.020 Uiso 1 1 calc R . . 
C7 C 0.20363(9) 0.43435(15) -0.04455(8) 0.0141(3) Uani 1 1 d . . . 
H7 H 0.2516 0.4718 0.0055 0.017 Uiso 1 1 calc R . . 
C8 C 0.24136(10) 0.32370(16) -0.07822(9) 0.0162(3) Uani 1 1 d . . . 
C9 C 0.33956(12) 0.13828(17) -0.04416(10) 0.0250(4) Uani 1 1 d . . . 
H9A H 0.3672 0.1713 -0.0813 0.030 Uiso 1 1 calc R . . 
H9B H 0.2946 0.0700 -0.0737 0.030 Uiso 1 1 calc R . . 
C10 C 0.40837(11) 0.07847(18) 0.03194(10) 0.0242(3) Uani 1 1 d . . . 
H10A H 0.4315 -0.0043 0.0177 0.036 Uiso 1 1 calc R . . 
H10B H 0.3818 0.0579 0.0714 0.036 Uiso 1 1 calc R . . 
H10C H 0.4567 0.1428 0.0563 0.036 Uiso 1 1 calc R . . 
C11 C 0.05236(10) 0.22630(14) 0.10664(9) 0.0155(3) Uani 1 1 d . . . 
H11 H 0.0187 0.1844 0.1330 0.019 Uiso 1 1 calc R . . 
C12 C 0.14731(10) 0.25176(15) 0.15104(9) 0.0161(3) Uani 1 1 d . . . 
H12 H 0.1766 0.2315 0.2077 0.019 Uiso 1 1 calc R . . 
C21 C -0.07790(9) 0.23209(14) -0.01620(8) 0.0138(3) Uani 1 1 d . . . 
H21 H -0.1071 0.3178 -0.0424 0.017 Uiso 1 1 calc R . . 
C22 C -0.08375(10) 0.13469(15) -0.08528(9) 0.0155(3) Uani 1 1 d . . . 
H22A H -0.0491 0.1706 -0.1155 0.019 Uiso 1 1 calc R . . 
H22B H -0.0582 0.0469 -0.0615 0.019 Uiso 1 1 calc R . . 
C23 C -0.17982(10) 0.11535(16) -0.14437(9) 0.0192(3) Uani 1 1 d . . . 
H23A H -0.1826 0.0473 -0.1860 0.023 Uiso 1 1 calc R . . 
H23B H -0.2030 0.2010 -0.1731 0.023 Uiso 1 1 calc R . . 
C24 C -0.23772(10) 0.06988(16) -0.09927(9) 0.0206(3) Uani 1 1 d . . . 
H24A H -0.3004 0.0691 -0.1380 0.025 Uiso 1 1 calc R . . 
H24B H -0.2213 -0.0229 -0.0788 0.025 Uiso 1 1 calc R . . 
C25 C -0.22734(10) 0.16214(16) -0.02757(10) 0.0202(3) Uani 1 1 d . . . 
H25A H -0.2620 0.1259 0.0026 0.024 Uiso 1 1 calc R . . 
H25B H -0.2511 0.2521 -0.0487 0.024 Uiso 1 1 calc R . . 
C26 C -0.13031(10) 0.17538(16) 0.03111(9) 0.0171(3) Uani 1 1 d . . . 
H26A H -0.1252 0.2361 0.0770 0.021 Uiso 1 1 calc R . . 
H26B H -0.1066 0.0863 0.0541 0.021 Uiso 1 1 calc R . . 
C31 C 0.28321(9) 0.33803(15) 0.15145(9) 0.0146(3) Uani 1 1 d . . . 
H31 H 0.3106 0.3261 0.1105 0.018 Uiso 1 1 calc R . . 
C32 C 0.29089(10) 0.48650(15) 0.17441(9) 0.0176(3) Uani 1 1 d . . . 
H32A H 0.2685 0.5014 0.2181 0.021 Uiso 1 1 calc R . . 
H32B H 0.2545 0.5406 0.1261 0.021 Uiso 1 1 calc R . . 
C33 C 0.38718(10) 0.53097(17) 0.20434(10) 0.0223(3) Uani 1 1 d . . . 
H33A H 0.3921 0.6262 0.2217 0.027 Uiso 1 1 calc R . . 
H33B H 0.4076 0.5239 0.1589 0.027 Uiso 1 1 calc R . . 
C34 C 0.44594(10) 0.44412(18) 0.27625(10) 0.0249(3) Uani 1 1 d . . . 
H34A H 0.5085 0.4688 0.2906 0.030 Uiso 1 1 calc R . . 
H34B H 0.4316 0.4627 0.3245 0.030 Uiso 1 1 calc R . . 
C35 C 0.43404(10) 0.29429(18) 0.25646(10) 0.0244(3) Uani 1 1 d . . . 
H35A H 0.4688 0.2420 0.3062 0.029 Uiso 1 1 calc R . . 
H35B H 0.4568 0.2731 0.2137 0.029 Uiso 1 1 calc R . . 
C36 C 0.33649(10) 0.25294(16) 0.22618(9) 0.0194(3) Uani 1 1 d . . . 
H36A H 0.3301 0.1565 0.2113 0.023 Uiso 1 1 calc R . . 
H36B H 0.3144 0.2671 0.2701 0.023 Uiso 1 1 calc R . . 
Cl1 Cl 0.41352(4) 0.63828(6) -0.00453(3) 0.04341(13) Uani 1 1 d . . . 
Cl2 Cl 0.31614(4) 0.80188(5) -0.14558(3) 0.04087(13) Uani 1 1 d . . . 
Cl3 Cl 0.4101(2) 0.5743(3) -0.1663(2) 0.0364(4) Uani 0.70 1 d P A 1 
C1S C 0.34913(11) 0.63841(17) -0.11021(11) 0.0257(4) Uani 0.70 1 d P A 1 
H1S H 0.2956 0.5814 -0.1215 0.031 Uiso 0.70 1 calc PR A 1 
Cl3' Cl 0.4005(5) 0.5469(8) -0.1570(5) 0.0479(14) Uani 0.30 1 d P A 2 
C1S' C 0.34913(11) 0.63841(17) -0.11021(11) 0.0257(4) Uani 0.30 1 d P A 2 
H1S' H 0.2938 0.5884 -0.1175 0.031 Uiso 0.30 1 calc PR A 2 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Pd C1 2.0134(14) . ? 
Pd C7 2.0259(14) . ? 
Pd N2 2.1234(12) . ? 
Pd N1 2.1620(12) . ? 
O1 C2 1.3699(17) . ? 
O1 C7 1.4350(17) . ? 
O2 C8 1.3482(18) . ? 
O2 C9 1.4447(18) . ? 
O3 C8 1.2088(17) . ? 
N1 C11 1.2770(18) . ? 
N1 C21 1.4786(18) . ? 
N2 C12 1.2778(19) . ? 
N2 C31 1.4793(18) . ? 
C1 C6 1.402(2) . ? 
C1 C2 1.4069(19) . ? 
C2 C3 1.387(2) . ? 
C3 C4 1.389(2) . ? 
C4 C5 1.386(2) . ? 
C5 C6 1.397(2) . ? 
C7 C8 1.498(2) . ? 
C9 C10 1.504(2) . ? 
C11 C12 1.470(2) . ? 
C21 C26 1.527(2) . ? 
C21 C22 1.5348(19) . ? 
C22 C23 1.529(2) . ? 
C23 C24 1.532(2) . ? 
C24 C25 1.522(2) . ? 
C25 C26 1.532(2) . ? 
C31 C32 1.525(2) . ? 
C31 C36 1.527(2) . ? 
C32 C33 1.526(2) . ? 
C33 C34 1.531(2) . ? 
C34 C35 1.527(3) . ? 
C35 C36 1.536(2) . ? 
Cl1 C1S 1.7549(19) . ? 
Cl2 C1S 1.7515(17) . ? 
Cl3 C1S 1.783(4) . ? 
  
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 
C1 Pd C7 78.72(6) . . ? 
C1 Pd N2 171.11(5) . . ? 
C7 Pd N2 98.06(5) . . ? 
C1 Pd N1 107.04(5) . . ? 
C7 Pd N1 173.93(5) . . ? 
N2 Pd N1 76.53(5) . . ? 
C2 O1 C7 110.73(11) . . ? 
C8 O2 C9 116.05(12) . . ? 
C11 N1 C21 119.69(12) . . ? 
C11 N1 Pd 113.11(10) . . ? 
C21 N1 Pd 127.16(9) . . ? 
C12 N2 C31 120.17(12) . . ? 
C12 N2 Pd 114.92(10) . . ? 
C31 N2 Pd 124.19(9) . . ? 
C6 C1 C2 114.79(13) . . ? 
C6 C1 Pd 131.78(11) . . ? 
C2 C1 Pd 113.32(10) . . ? 
O1 C2 C3 117.72(13) . . ? 
O1 C2 C1 117.95(12) . . ? 
C3 C2 C1 124.26(13) . . ? 
C2 C3 C4 118.82(14) . . ? 
C5 C4 C3 119.32(14) . . ? 
C4 C5 C6 120.67(14) . . ? 
C5 C6 C1 122.11(13) . . ? 
O1 C7 C8 107.86(11) . . ? 
O1 C7 Pd 113.81(9) . . ? 
C8 C7 Pd 108.90(10) . . ? 
O3 C8 O2 122.61(14) . . ? 
O3 C8 C7 125.68(14) . . ? 
O2 C8 C7 111.70(12) . . ? 
O2 C9 C10 106.87(13) . . ? 
N1 C11 C12 118.15(13) . . ? 
N2 C12 C11 117.02(13) . . ? 
N1 C21 C26 116.82(12) . . ? 
N1 C21 C22 108.02(11) . . ? 
C26 C21 C22 109.39(12) . . ? 
C23 C22 C21 110.60(12) . . ? 
C22 C23 C24 111.51(12) . . ? 
C25 C24 C23 111.58(13) . . ? 
C24 C25 C26 111.45(13) . . ? 
C21 C26 C25 108.71(12) . . ? 
N2 C31 C32 109.04(12) . . ? 
N2 C31 C36 115.65(12) . . ? 
C32 C31 C36 110.26(12) . . ? 
C31 C32 C33 109.89(13) . . ? 
C32 C33 C34 110.94(13) . . ? 
C35 C34 C33 112.18(13) . . ? 
C34 C35 C36 111.39(14) . . ? 
C31 C36 C35 108.76(13) . . ? 
Cl2 C1S Cl1 110.86(10) . . ? 
Cl2 C1S Cl3 107.20(14) . . ? 
Cl1 C1S Cl3 111.01(15) . . ? 
  
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 
C1 Pd N1 C11 -168.75(10) . . . . ? 
C7 Pd N1 C11 29.9(5) . . . . ? 
N2 Pd N1 C11 2.80(10) . . . . ? 
C1 Pd N1 C21 13.67(12) . . . . ? 
C7 Pd N1 C21 -147.7(4) . . . . ? 
N2 Pd N1 C21 -174.78(12) . . . . ? 
C1 Pd N2 C12 110.0(3) . . . . ? 
C7 Pd N2 C12 178.08(11) . . . . ? 
N1 Pd N2 C12 -4.71(10) . . . . ? 
C1 Pd N2 C31 -60.3(4) . . . . ? 
C7 Pd N2 C31 7.81(12) . . . . ? 
N1 Pd N2 C31 -174.98(11) . . . . ? 
C7 Pd C1 C6 171.73(15) . . . . ? 
N2 Pd C1 C6 -118.8(3) . . . . ? 
N1 Pd C1 C6 -6.29(15) . . . . ? 
C7 Pd C1 C2 -12.35(10) . . . . ? 
N2 Pd C1 C2 57.1(4) . . . . ? 
N1 Pd C1 C2 169.62(10) . . . . ? 
C7 O1 C2 C3 -167.88(13) . . . . ? 
C7 O1 C2 C1 15.02(17) . . . . ? 
C6 C1 C2 O1 178.61(12) . . . . ? 
Pd C1 C2 O1 1.96(17) . . . . ? 
C6 C1 C2 C3 1.7(2) . . . . ? 
Pd C1 C2 C3 -174.94(12) . . . . ? 
O1 C2 C3 C4 -177.93(14) . . . . ? 
C1 C2 C3 C4 -1.0(2) . . . . ? 
C2 C3 C4 C5 -0.5(2) . . . . ? 
C3 C4 C5 C6 1.2(2) . . . . ? 
C4 C5 C6 C1 -0.5(2) . . . . ? 
C2 C1 C6 C5 -0.9(2) . . . . ? 
Pd C1 C6 C5 174.94(11) . . . . ? 
C2 O1 C7 C8 95.72(13) . . . . ? 
C2 O1 C7 Pd -25.22(14) . . . . ? 
C1 Pd C7 O1 20.72(10) . . . . ? 
N2 Pd C7 O1 -150.87(9) . . . . ? 
N1 Pd C7 O1 -177.5(4) . . . . ? 
C1 Pd C7 C8 -99.64(10) . . . . ? 
N2 Pd C7 C8 88.77(10) . . . . ? 
N1 Pd C7 C8 62.2(5) . . . . ? 
C9 O2 C8 O3 -1.1(2) . . . . ? 
C9 O2 C8 C7 179.90(13) . . . . ? 
O1 C7 C8 O3 -22.0(2) . . . . ? 
Pd C7 C8 O3 101.95(16) . . . . ? 
O1 C7 C8 O2 156.94(11) . . . . ? 
Pd C7 C8 O2 -79.09(13) . . . . ? 
C8 O2 C9 C10 173.86(13) . . . . ? 
C21 N1 C11 C12 176.97(12) . . . . ? 
Pd N1 C11 C12 -0.81(16) . . . . ? 
C31 N2 C12 C11 176.52(12) . . . . ? 
Pd N2 C12 C11 5.83(17) . . . . ? 
N1 C11 C12 N2 -3.4(2) . . . . ? 
C11 N1 C21 C26 7.88(19) . . . . ? 
Pd N1 C21 C26 -174.68(10) . . . . ? 
C11 N1 C21 C22 -115.87(14) . . . . ? 
Pd N1 C21 C22 61.57(14) . . . . ? 
N1 C21 C22 C23 -171.86(11) . . . . ? 
C26 C21 C22 C23 60.01(16) . . . . ? 
C21 C22 C23 C24 -54.90(17) . . . . ? 
C22 C23 C24 C25 52.11(18) . . . . ? 
C23 C24 C25 C26 -54.65(18) . . . . ? 
N1 C21 C26 C25 175.44(12) . . . . ? 
C22 C21 C26 C25 -61.51(15) . . . . ? 
C24 C25 C26 C21 59.31(16) . . . . ? 
C12 N2 C31 C32 -95.15(15) . . . . ? 
Pd N2 C31 C32 74.63(13) . . . . ? 
C12 N2 C31 C36 29.75(19) . . . . ? 
Pd N2 C31 C36 -160.47(10) . . . . ? 
N2 C31 C32 C33 -170.77(12) . . . . ? 
C36 C31 C32 C33 61.25(16) . . . . ? 
C31 C32 C33 C34 -56.31(17) . . . . ? 
C32 C33 C34 C35 52.99(18) . . . . ? 
C33 C34 C35 C36 -53.67(17) . . . . ? 
N2 C31 C36 C35 174.73(12) . . . . ? 
C32 C31 C36 C35 -61.00(16) . . . . ? 
C34 C35 C36 C31 56.94(17) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              30.03 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.752 
_refine_diff_density_min   -0.528 
_refine_diff_density_rms    0.079 
  
data_02035f(3b) 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry 
   University of Kansas 
   Rm 2010 Malott Hall 
   1251 Wescoe Hall Dr. 
   Lawrence, KS  66045-7582  USA 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C20 H18 N2 O3 Pd' 
_chemical_formula_sum 
 'C20 H18 N2 O3 Pd' 
_chemical_formula_weight          440.76 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pd'  'Pd'  -0.9988   1.0072 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    Pc 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x, -y, z+1/2' 
  
_cell_length_a                    7.9471(7) 
_cell_length_b                    19.6757(17) 
_cell_length_c                    11.1282(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.475(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      1716.3(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     4967 
_cell_measurement_theta_min       2.53 
_cell_measurement_theta_max       30.0 
  
_exptl_crystal_description        plate 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.21 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.706 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              888 
_exptl_absorpt_coefficient_mu     1.104 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.822 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    'SADABS, 2000' 
  
_exptl_special_details 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry 
   University of Kansas 
   Rm 2010 Malott Hall 
   1251 Wescoe Hall Dr. 
   Lawrence, KS  66045-7582  USA 
; 
  
_diffrn_ambient_temperature       100(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        'ω scan frames' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          132 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0.0 
_diffrn_reflns_number             12411 
_diffrn_reflns_av_R_equivalents   0.0213 
_diffrn_reflns_av_sigmaI/netI     0.0421 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          1.86 
_diffrn_reflns_theta_max          30.03 
_reflns_number_total              7662 
_reflns_number_gt                 6162 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections except 2 which were flagged 
 by the user for being in the beamstop.  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)+(0.0384P)²+15.3066P] 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(6) 
_refine_ls_number_reflns          7662 
_refine_ls_number_parameters      398 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0961 
_refine_ls_R_factor_gt            0.0762 
_refine_ls_wR_factor_ref          0.1760 
_refine_ls_wR_factor_gt           0.1619 
_refine_ls_goodness_of_fit_ref    1.076 
_refine_ls_restrained_S_all       1.076 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pd1 Pd 0.00567(8) -0.42081(7) -0.35821(6) 0.0445(3) Uani 1 1 d . . . 
O1 O -0.0973(16) -0.2835(6) -0.4207(12) 0.057(3) Uani 1 1 d . . . 
O2 O 0.3408(15) -0.3272(7) -0.3094(10) 0.061(4) Uani 1 1 d . . . 
O3 O 0.2378(19) -0.2943(7) -0.4994(11) 0.061(4) Uani 1 1 d . . . 
C1 C -0.1793(13) -0.3233(4) -0.5163(8) 0.051(4) Uani 1 1 d G . . 
C2 C -0.1487(12) -0.3929(4) -0.5130(7) 0.042(3) Uani 1 1 d G . . 
C3 C -0.2241(13) -0.4339(3) -0.6086(9) 0.080(6) Uani 1 1 d G . . 
H3 H -0.2032 -0.4815 -0.6063 0.096 Uiso 1 1 calc R . . 
C4 C -0.3302(16) -0.4053(4) -0.7075(9) 0.129(11) Uani 1 1 d G . . 
H4 H -0.3817 -0.4334 -0.7728 0.155 Uiso 1 1 calc R . . 
C5 C -0.3608(16) -0.3358(4) -0.7108(10) 0.148(13) Uani 1 1 d G . . 
H5 H -0.4332 -0.3162 -0.7784 0.177 Uiso 1 1 calc R . . 
C6 C -0.2853(15) -0.2947(4) -0.6152(11) 0.095(8) Uani 1 1 d G . . 
H6 H -0.3062 -0.2472 -0.6175 0.114 Uiso 1 1 calc R . . 
C7 C 0.045(2) -0.3158(7) -0.3482(13) 0.051(5) Uani 1 1 d . . . 
H7 H 0.0593 -0.2998 -0.2619 0.061 Uiso 1 1 calc R . . 
C8 C 0.209(2) -0.3099(9) -0.3962(12) 0.050(4) Uani 1 1 d . . . 
C9 C 0.509(2) -0.3330(11) -0.3362(16) 0.076(7) Uani 1 1 d . . . 
H9A H 0.5553 -0.2873 -0.3489 0.092 Uiso 1 1 calc R . . 
H9B H 0.5078 -0.3599 -0.4115 0.092 Uiso 1 1 calc R . . 
C10 C 0.619(3) -0.3681(17) -0.2291(19) 0.120(12) Uani 1 1 d . . . 
H10A H 0.7362 -0.3723 -0.2456 0.180 Uiso 1 1 calc R . . 
H10B H 0.5731 -0.4135 -0.2179 0.180 Uiso 1 1 calc R . . 
H10C H 0.6193 -0.3412 -0.1550 0.180 Uiso 1 1 calc R . . 
N1 N -0.0415(9) -0.5303(3) -0.3467(7) 0.043(2) Uani 1 1 d G . . 
C11 C -0.1648(8) -0.5681(4) -0.4212(6) 0.048(3) Uani 1 1 d G . . 
H11 H -0.2497 -0.5457 -0.4775 0.058 Uiso 1 1 calc R . . 
C12 C -0.1640(10) -0.6386(4) -0.4132(6) 0.056(4) Uani 1 1 d G . . 
H12 H -0.2483 -0.6644 -0.4641 0.067 Uiso 1 1 calc R . . 
C13 C -0.0399(12) -0.6713(3) -0.3308(7) 0.051(3) Uani 1 1 d G . . 
H13 H -0.0393 -0.7195 -0.3253 0.061 Uiso 1 1 calc R . . 
C14 C 0.0834(11) -0.6336(4) -0.2563(6) 0.053(5) Uani 1 1 d G . . 
H14 H 0.1683 -0.6559 -0.2000 0.064 Uiso 1 1 calc R . . 
C15 C 0.0826(9) -0.5631(4) -0.2643(6) 0.052(5) Uani 1 1 d G . . 
N2 N 0.1648(13) -0.4479(4) -0.1909(7) 0.055(5) Uani 1 1 d G . . 
C16 C 0.1767(12) -0.5175(4) -0.1700(8) 0.050(4) Uani 1 1 d G . . 
C17 C 0.2900(15) -0.5426(3) -0.0715(9) 0.067(6) Uani 1 1 d G . . 
H17 H 0.2981 -0.5902 -0.0572 0.080 Uiso 1 1 calc R . . 
C18 C 0.3914(16) -0.4982(4) 0.0061(9) 0.108(9) Uani 1 1 d G . . 
H18 H 0.4689 -0.5154 0.0734 0.130 Uiso 1 1 calc R . . 
C19 C 0.3796(16) -0.4285(4) -0.0148(8) 0.084(6) Uani 1 1 d G . . 
H19 H 0.4489 -0.3982 0.0383 0.101 Uiso 1 1 calc R . . 
C20 C 0.2663(16) -0.4034(3) -0.1133(7) 0.058(4) Uani 1 1 d G . . 
H20 H 0.2582 -0.3558 -0.1276 0.069 Uiso 1 1 calc R . . 
Pd2 Pd -0.00470(8) 0.08025(7) 0.35800(5) 0.0446(3) Uani 1 1 d . . . 
O21 O 0.0763(16) 0.2236(6) 0.4342(10) 0.071(4) Uani 1 1 d . . . 
O22 O -0.3449(15) 0.1771(5) 0.3134(10) 0.045(3) Uani 1 1 d . . . 
O23 O -0.228(2) 0.2146(7) 0.4988(9) 0.062(4) Uani 1 1 d . . . 
C21 C 0.1726(13) 0.1872(5) 0.5096(9) 0.062(5) Uani 1 1 d G . . 
C22 C 0.1581(12) 0.1168(5) 0.5071(8) 0.054(4) Uani 1 1 d G . . 
C23 C 0.2680(13) 0.0775(4) 0.5892(8) 0.047(3) Uani 1 1 d G . . 
H23 H 0.2581 0.0294 0.5875 0.056 Uiso 1 1 calc R . . 
C25 C 0.3924(10) 0.1087(5) 0.6738(7) 0.053(3) Uani 1 1 d G . . 
H25 H 0.4675 0.0818 0.7299 0.063 Uiso 1 1 calc R . . 
C26 C 0.4069(11) 0.1791(5) 0.6763(7) 0.055(3) Uani 1 1 d G . . 
H26 H 0.4919 0.2003 0.7341 0.066 Uiso 1 1 calc R . . 
C24 C 0.2970(15) 0.2184(4) 0.5942(10) 0.083(6) Uani 1 1 d G . . 
H24 H 0.3069 0.2665 0.5959 0.099 Uiso 1 1 calc R . . 
C27 C -0.044(2) 0.1786(8) 0.3602(14) 0.044(4) Uani 1 1 d . . . 
H27 H -0.0552 0.1948 0.2741 0.053 Uiso 1 1 calc R . . 
C28 C -0.213(2) 0.1939(7) 0.4026(14) 0.044(4) Uani 1 1 d . . . 
C29 C -0.514(3) 0.1805(11) 0.3441(16) 0.067(5) Uani 1 1 d . . . 
H29A H -0.5496 0.2282 0.3521 0.080 Uiso 1 1 calc R . . 
H29B H -0.5190 0.1562 0.4213 0.080 Uiso 1 1 calc R . . 
C30 C -0.625(3) 0.1458(16) 0.2378(19) 0.112(11) Uani 1 1 d . . . 
H30A H -0.7442 0.1472 0.2498 0.168 Uiso 1 1 calc R . . 
H30B H -0.5887 0.0984 0.2328 0.168 Uiso 1 1 calc R . . 
H30C H -0.6134 0.1694 0.1620 0.168 Uiso 1 1 calc R . . 
N21 N -0.1551(14) 0.0550(5) 0.1925(7) 0.064(5) Uani 1 1 d G . . 
C31 C -0.2177(15) 0.1004(5) 0.1002(8) 0.076(6) Uani 1 1 d G . . 
H31 H -0.1964 0.1477 0.1111 0.091 Uiso 1 1 calc R . . 
C32 C -0.3114(13) 0.0766(6) -0.0082(6) 0.066(5) Uani 1 1 d G . . 
H32 H -0.3542 0.1076 -0.0713 0.079 Uiso 1 1 calc R . . 
C33 C -0.3425(14) 0.0074(6) -0.0242(6) 0.069(5) Uani 1 1 d G . . 
H33 H -0.4066 -0.0089 -0.0982 0.083 Uiso 1 1 calc R . . 
C34 C -0.2799(17) -0.0380(5) 0.0681(9) 0.072(6) Uani 1 1 d G . . 
H34 H -0.3012 -0.0853 0.0572 0.087 Uiso 1 1 calc R . . 
C35 C -0.1862(15) -0.0142(5) 0.1765(8) 0.050(4) Uani 1 1 d G . . 
N22 N -0.0033(15) -0.0237(3) 0.3628(7) 0.085(5) Uani 1 1 d G . . 
C36 C -0.0848(15) -0.0558(4) 0.2579(6) 0.057(5) Uani 1 1 d G . . 
C37 C -0.0915(17) -0.1264(4) 0.2524(6) 0.065(6) Uani 1 1 d G . . 
H37 H -0.1472 -0.1483 0.1807 0.078 Uiso 1 1 calc R . . 
C38 C -0.0166(18) -0.1648(3) 0.3518(9) 0.118(9) Uani 1 1 d G . . 
H38 H -0.0212 -0.2130 0.3480 0.141 Uiso 1 1 calc R . . 
C39 C 0.0649(18) -0.1327(4) 0.4567(8) 0.137(12) Uani 1 1 d G . . 
H39 H 0.1161 -0.1590 0.5246 0.164 Uiso 1 1 calc R . . 
C40 C 0.0716(16) -0.0621(4) 0.4622(7) 0.103(8) Uani 1 1 d G . . 
H40 H 0.1273 -0.0402 0.5339 0.123 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 C2 2.019(5) . ? 
Pd1 C7 2.091(15) . ? 
Pd1 N2 2.139(6) . ? 
Pd1 N1 2.194(6) . ? 
O1 C1 1.393(14) . ? 
O1 C7 1.427(17) . ? 
O2 C8 1.347(18) . ? 
O2 C9 1.42(2) . ? 
O3 C8 1.25(2) . ? 
C1 C2 1.3900 . ? 
C1 C6 1.3900 . ? 
C2 C3 1.3900 . ? 
C3 C4 1.3900 . ? 
C4 C5 1.3900 . ? 
C5 C6 1.3900 . ? 
C7 C8 1.49(3) . ? 
C9 C10 1.52(3) . ? 
N1 C11 1.3900 . ? 
N1 C15 1.3900 . ? 
C11 C12 1.3900 . ? 
C12 C13 1.3900 . ? 
C13 C14 1.3900 . ? 
C14 C15 1.3900 . ? 
C15 C16 1.485(8) . ? 
N2 C16 1.3900 . ? 
N2 C20 1.3900 . ? 
C16 C17 1.3900 . ? 
C17 C18 1.3900 . ? 
C18 C19 1.3900 . ? 
C19 C20 1.3900 . ? 
Pd2 C27 1.961(16) . ? 
Pd2 N22 2.046(6) . ? 
Pd2 C22 2.059(7) . ? 
Pd2 N21 2.084(6) . ? 
O21 C21 1.262(14) . ? 
O21 C27 1.457(18) . ? 
O22 C28 1.360(19) . ? 
O22 C29 1.44(2) . ? 
O23 C28 1.17(2) . ? 
C21 C22 1.3900 . ? 
C21 C24 1.3900 . ? 
C22 C23 1.3900 . ? 
C23 C25 1.3900 . ? 
C25 C26 1.3900 . ? 
C26 C24 1.3900 . ? 
C27 C28 1.52(2) . ? 
C29 C30 1.52(3) . ? 
N21 C31 1.3900 . ? 
N21 C35 1.3900 . ? 
C31 C32 1.3900 . ? 
C32 C33 1.3900 . ? 
C33 C34 1.3900 . ? 
C34 C35 1.3900 . ? 
C35 C36 1.379(10) . ? 
N22 C36 1.3900 . ? 
N22 C40 1.3900 . ? 
C36 C37 1.3900 . ? 
C37 C38 1.3900 . ? 
C38 C39 1.3900 . ? 
C39 C40 1.3900 . ? 
  
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 
C2 Pd1 C7 80.9(4) . . ? 
C2 Pd1 N2 178.0(4) . . ? 
C7 Pd1 N2 97.9(4) . . ? 
C2 Pd1 N1 103.4(3) . . ? 
C7 Pd1 N1 173.3(5) . . ? 
N2 Pd1 N1 77.7(3) . . ? 
C1 O1 C7 114.2(11) . . ? 
C8 O2 C9 121.2(14) . . ? 
C2 C1 C6 120.0 . . ? 
C2 C1 O1 118.4(8) . . ? 
C6 C1 O1 121.6(8) . . ? 
C3 C2 C1 120.0 . . ? 
C3 C2 Pd1 128.3(5) . . ? 
C1 C2 Pd1 111.7(5) . . ? 
C2 C3 C4 120.0 . . ? 
C5 C4 C3 120.0 . . ? 
C4 C5 C6 120.0 . . ? 
C5 C6 C1 120.0 . . ? 
O1 C7 C8 115.0(15) . . ? 
O1 C7 Pd1 108.1(10) . . ? 
C8 C7 Pd1 101.0(9) . . ? 
O3 C8 O2 118.9(16) . . ? 
O3 C8 C7 130.8(14) . . ? 
O2 C8 C7 110.2(13) . . ? 
O2 C9 C10 108.2(19) . . ? 
C11 N1 C15 120.0 . . ? 
C11 N1 Pd1 126.9(4) . . ? 
C15 N1 Pd1 112.6(4) . . ? 
C12 C11 N1 120.0 . . ? 
C11 C12 C13 120.0 . . ? 
C14 C13 C12 120.0 . . ? 
C15 C14 C13 120.0 . . ? 
C14 C15 N1 120.0 . . ? 
C14 C15 C16 124.1(6) . . ? 
N1 C15 C16 114.0(6) . . ? 
C16 N2 C20 120.0 . . ? 
C16 N2 Pd1 113.9(4) . . ? 
C20 N2 Pd1 125.7(5) . . ? 
C17 C16 N2 120.0 . . ? 
C17 C16 C15 121.8(6) . . ? 
N2 C16 C15 117.7(6) . . ? 
C16 C17 C18 120.0 . . ? 
C17 C18 C19 120.0 . . ? 
C18 C19 C20 120.0 . . ? 
C19 C20 N2 120.0 . . ? 
C27 Pd2 N22 170.5(6) . . ? 
C27 Pd2 C22 74.1(5) . . ? 
N22 Pd2 C22 109.2(4) . . ? 
C27 Pd2 N21 100.2(5) . . ? 
N22 Pd2 N21 77.6(4) . . ? 
C22 Pd2 N21 171.3(4) . . ? 
C21 O21 C27 107.6(11) . . ? 
C28 O22 C29 116.8(15) . . ? 
O21 C21 C22 120.9(9) . . ? 
O21 C21 C24 119.1(9) . . ? 
C22 C21 C24 120.0 . . ? 
C23 C22 C21 120.0 . . ? 
C23 C22 Pd2 125.4(5) . . ? 
C21 C22 Pd2 113.8(5) . . ? 
C22 C23 C25 120.0 . . ? 
C26 C25 C23 120.0 . . ? 
C25 C26 C24 120.0 . . ? 
C26 C24 C21 120.0 . . ? 
O21 C27 C28 103.6(13) . . ? 
O21 C27 Pd2 121.0(11) . . ? 
C28 C27 Pd2 110.5(9) . . ? 
O23 C28 O22 125.0(18) . . ? 
O23 C28 C27 125.3(16) . . ? 
O22 C28 C27 109.7(14) . . ? 
O22 C29 C30 103.9(16) . . ? 
C31 N21 C35 120.0 . . ? 
C31 N21 Pd2 125.7(5) . . ? 
C35 N21 Pd2 114.3(5) . . ? 
N21 C31 C32 120.0 . . ? 
C31 C32 C33 120.0 . . ? 
C34 C33 C32 120.0 . . ? 
C35 C34 C33 120.0 . . ? 
C36 C35 C34 122.8(8) . . ? 
C36 C35 N21 115.1(8) . . ? 
C34 C35 N21 120.0 . . ? 
C36 N22 C40 120.0 . . ? 
C36 N22 Pd2 115.6(4) . . ? 
C40 N22 Pd2 124.4(4) . . ? 
C35 C36 N22 115.0(7) . . ? 
C35 C36 C37 123.4(7) . . ? 
N22 C36 C37 120.0 . . ? 
C36 C37 C38 120.0 . . ? 
C39 C38 C37 120.0 . . ? 
C38 C39 C40 120.0 . . ? 
C39 C40 N22 120.0 . . ? 
  
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 
C7 O1 C1 C2 17.2(17) . . . . ? 
C7 O1 C1 C6 -160.9(12) . . . . ? 
C6 C1 C2 C3 0.0 . . . . ? 
O1 C1 C2 C3 -178.1(12) . . . . ? 
C6 C1 C2 Pd1 -178.9(7) . . . . ? 
O1 C1 C2 Pd1 3.0(10) . . . . ? 
C7 Pd1 C2 C3 167.0(9) . . . . ? 
N2 Pd1 C2 C3 -141(12) . . . . ? 
N1 Pd1 C2 C3 -18.3(7) . . . . ? 
C7 Pd1 C2 C1 -14.2(7) . . . . ? 
N2 Pd1 C2 C1 38(13) . . . . ? 
N1 Pd1 C2 C1 160.5(5) . . . . ? 
C1 C2 C3 C4 0.0 . . . . ? 
Pd1 C2 C3 C4 178.7(9) . . . . ? 
C2 C3 C4 C5 0.0 . . . . ? 
C3 C4 C5 C6 0.0 . . . . ? 
C4 C5 C6 C1 0.0 . . . . ? 
C2 C1 C6 C5 0.0 . . . . ? 
O1 C1 C6 C5 178.0(12) . . . . ? 
C1 O1 C7 C8 84.7(16) . . . . ? 
C1 O1 C7 Pd1 -27.3(17) . . . . ? 
C2 Pd1 C7 O1 22.4(12) . . . . ? 
N2 Pd1 C7 O1 -156.1(11) . . . . ? 
N1 Pd1 C7 O1 -108(4) . . . . ? 
C2 Pd1 C7 C8 -98.7(9) . . . . ? 
N2 Pd1 C7 C8 82.9(8) . . . . ? 
N1 Pd1 C7 C8 131(4) . . . . ? 
C9 O2 C8 O3 -5(3) . . . . ? 
C9 O2 C8 C7 173.0(15) . . . . ? 
O1 C7 C8 O3 -17(3) . . . . ? 
Pd1 C7 C8 O3 99.2(19) . . . . ? 
O1 C7 C8 O2 165.5(13) . . . . ? 
Pd1 C7 C8 O2 -78.4(13) . . . . ? 
C8 O2 C9 C10 -167.5(18) . . . . ? 
C2 Pd1 N1 C11 -7.2(6) . . . . ? 
C7 Pd1 N1 C11 122(4) . . . . ? 
N2 Pd1 N1 C11 171.1(6) . . . . ? 
C2 Pd1 N1 C15 164.5(5) . . . . ? 
C7 Pd1 N1 C15 -66(4) . . . . ? 
N2 Pd1 N1 C15 -17.2(4) . . . . ? 
C15 N1 C11 C12 0.0 . . . . ? 
Pd1 N1 C11 C12 171.2(6) . . . . ? 
N1 C11 C12 C13 0.0 . . . . ? 
C11 C12 C13 C14 0.0 . . . . ? 
C12 C13 C14 C15 0.0 . . . . ? 
C13 C14 C15 N1 0.0 . . . . ? 
C13 C14 C15 C16 163.4(9) . . . . ? 
C11 N1 C15 C14 0.0 . . . . ? 
Pd1 N1 C15 C14 -172.4(5) . . . . ? 
C11 N1 C15 C16 -165.0(8) . . . . ? 
Pd1 N1 C15 C16 22.6(7) . . . . ? 
C2 Pd1 N2 C16 132(12) . . . . ? 
C7 Pd1 N2 C16 -176.6(7) . . . . ? 
N1 Pd1 N2 C16 8.5(5) . . . . ? 
C2 Pd1 N2 C20 -56(13) . . . . ? 
C7 Pd1 N2 C20 -4.0(8) . . . . ? 
N1 Pd1 N2 C20 -178.9(7) . . . . ? 
C20 N2 C16 C17 0.0 . . . . ? 
Pd1 N2 C16 C17 173.1(7) . . . . ? 
C20 N2 C16 C15 -172.2(10) . . . . ? 
Pd1 N2 C16 C15 0.9(9) . . . . ? 
C14 C15 C16 C17 7.5(10) . . . . ? 
N1 C15 C16 C17 171.8(6) . . . . ? 
C14 C15 C16 N2 179.6(6) . . . . ? 
N1 C15 C16 N2 -16.2(9) . . . . ? 
N2 C16 C17 C18 0.0 . . . . ? 
C15 C16 C17 C18 171.8(10) . . . . ? 
C16 C17 C18 C19 0.0 . . . . ? 
C17 C18 C19 C20 0.0 . . . . ? 
C18 C19 C20 N2 0.0 . . . . ? 
C16 N2 C20 C19 0.0 . . . . ? 
Pd1 N2 C20 C19 -172.2(8) . . . . ? 
C27 O21 C21 C22 3.4(16) . . . . ? 
C27 O21 C21 C24 -178.1(9) . . . . ? 
O21 C21 C22 C23 178.5(13) . . . . ? 
C24 C21 C22 C23 0.0 . . . . ? 
O21 C21 C22 Pd2 8.4(12) . . . . ? 
C24 C21 C22 Pd2 -170.1(7) . . . . ? 
C27 Pd2 C22 C23 178.3(8) . . . . ? 
N22 Pd2 C22 C23 7.7(8) . . . . ? 
N21 Pd2 C22 C23 -132(3) . . . . ? 
C27 Pd2 C22 C21 -12.2(6) . . . . ? 
N22 Pd2 C22 C21 177.2(6) . . . . ? 
N21 Pd2 C22 C21 37(3) . . . . ? 
C21 C22 C23 C25 0.0 . . . . ? 
Pd2 C22 C23 C25 168.9(8) . . . . ? 
C22 C23 C25 C26 0.0 . . . . ? 
C23 C25 C26 C24 0.0 . . . . ? 
C25 C26 C24 C21 0.0 . . . . ? 
O21 C21 C24 C26 -178.5(13) . . . . ? 
C22 C21 C24 C26 0.0 . . . . ? 
C21 O21 C27 C28 109.1(14) . . . . ? 
C21 O21 C27 Pd2 -15.4(17) . . . . ? 
N22 Pd2 C27 O21 127(3) . . . . ? 
C22 Pd2 C27 O21 15.4(11) . . . . ? 
N21 Pd2 C27 O21 -158.0(11) . . . . ? 
N22 Pd2 C27 C28 6(4) . . . . ? 
C22 Pd2 C27 C28 -105.8(11) . . . . ? 
N21 Pd2 C27 C28 80.8(11) . . . . ? 
C29 O22 C28 O23 -5(2) . . . . ? 
C29 O22 C28 C27 172.5(13) . . . . ? 
O21 C27 C28 O23 -26.4(19) . . . . ? 
Pd2 C27 C28 O23 104.6(16) . . . . ? 
O21 C27 C28 O22 156.2(10) . . . . ? 
Pd2 C27 C28 O22 -72.8(12) . . . . ? 
C28 O22 C29 C30 -168.9(13) . . . . ? 
C27 Pd2 N21 C31 16.6(8) . . . . ? 
N22 Pd2 N21 C31 -172.9(8) . . . . ? 
C22 Pd2 N21 C31 -31(4) . . . . ? 
C27 Pd2 N21 C35 -165.8(7) . . . . ? 
N22 Pd2 N21 C35 4.8(6) . . . . ? 
C22 Pd2 N21 C35 146(3) . . . . ? 
C35 N21 C31 C32 0.0 . . . . ? 
Pd2 N21 C31 C32 177.5(9) . . . . ? 
N21 C31 C32 C33 0.0 . . . . ? 
C31 C32 C33 C34 0.0 . . . . ? 
C32 C33 C34 C35 0.0 . . . . ? 
C33 C34 C35 C36 -162.9(12) . . . . ? 
C33 C34 C35 N21 0.0 . . . . ? 
C31 N21 C35 C36 164.2(11) . . . . ? 
Pd2 N21 C35 C36 -13.6(10) . . . . ? 
C31 N21 C35 C34 0.0 . . . . ? 
Pd2 N21 C35 C34 -177.8(8) . . . . ? 
C27 Pd2 N22 C36 82(3) . . . . ? 
C22 Pd2 N22 C36 -169.7(6) . . . . ? 
N21 Pd2 N22 C36 4.7(7) . . . . ? 
C27 Pd2 N22 C40 -98(3) . . . . ? 
C22 Pd2 N22 C40 10.6(8) . . . . ? 
N21 Pd2 N22 C40 -175.0(8) . . . . ? 
C34 C35 C36 N22 -178.6(6) . . . . ? 
N21 C35 C36 N22 17.7(11) . . . . ? 
C34 C35 C36 C37 -13.0(14) . . . . ? 
N21 C35 C36 C37 -176.7(7) . . . . ? 
C40 N22 C36 C35 166.1(12) . . . . ? 
Pd2 N22 C36 C35 -13.6(10) . . . . ? 
C40 N22 C36 C37 0.0 . . . . ? 
Pd2 N22 C36 C37 -179.7(8) . . . . ? 
C35 C36 C37 C38 -164.9(13) . . . . ? 
N22 C36 C37 C38 0.0 . . . . ? 
C36 C37 C38 C39 0.0 . . . . ? 
C37 C38 C39 C40 0.0 . . . . ? 
C38 C39 C40 N22 0.0 . . . . ? 
C36 N22 C40 C39 0.0 . . . . ? 
Pd2 N22 C40 C39 179.7(8) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.963 
_diffrn_reflns_theta_full              30.03 
_diffrn_measured_fraction_theta_full   0.963 
_refine_diff_density_max    2.228 
_refine_diff_density_min   -3.087 
_refine_diff_density_rms    0.168 
 
#====================

 
_publ_contact_author 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
_publ_contact_author_email      hmalinakova@ku.edu 
_publ_contact_author_fax        1(785)8645396 
_publ_contact_author_phone      1(785)8644743 
 
_publ_requested_journal         'Organometallics'  
 
loop_ 
    _publ_author_name 
    _publ_author_address 
  'Guo, Ruiyun' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Portscheller, Jannelle L.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Day, Victor W.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Malinakova, Helena C.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
 
_publ_section_title 
; 
 article title here 
 Allylpalladium(IV) Intermediate inthe Synthesis of Highly Substituted 
 Benzoxepines and Benzopyrans via Reactions of Stable Palla(II)cycles 
 with Allyl Bromides  
; 
_publ_section_references 
;
  Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
 
  Flack, H. D. (1983) Acta Cryst. A39, 876-881. 
 
  Flack, H. D. and Schwarzenbach, D. (1988) Acta Cryst. A44, 
  499-506. 
 
  Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
;
_publ_section_acknowledgements 
; 
 The authors wish to thank the National Science Foundation 
 (CHE-0079282) and the University of Kansas for funds to 
 acquire the diffractometer and computers used in this work.  
;  
data_k37b(8) 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C14 H24 Br2 N2 Pd' 
_chemical_formula_weight          486.57 
  
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' 
 '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    Pbca 
  
loop_ 
 _symmetry_equiv_pos_as_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                    7.3144(13) 
_cell_length_b                    10.3190(18) 
_cell_length_c                    43.365(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3273.0(10) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     491 
_cell_measurement_theta_min       2.94 
_cell_measurement_theta_max       19.09 
  
_exptl_crystal_description        Needle 
_exptl_crystal_colour             Yellow 
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.03 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.975 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1904 
_exptl_absorpt_coefficient_mu     6.007 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.654 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       100(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 SMART 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_%         0.00 
_diffrn_reflns_number             26920 
_diffrn_reflns_av_R_equivalents   0.2138 
_diffrn_reflns_av_sigmaI/netI     0.1140 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -53 
_diffrn_reflns_limit_l_max        53 
_diffrn_reflns_theta_min          2.82 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              3204 
_reflns_number_gt                 1972 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections except 1 which was flagged 
 by the user for being in the beamstop.  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)+(0.0443P)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     noref 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3204 
_refine_ls_number_parameters      172 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1164 
_refine_ls_R_factor_gt            0.0586 
_refine_ls_wR_factor_ref          0.1157 
_refine_ls_wR_factor_gt           0.1021 
_refine_ls_goodness_of_fit_ref    0.949 
_refine_ls_restrained_S_all       0.949 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pd Pd 0.12043(9) 0.34497(7) 0.127199(15) 0.01638(19) Uani 1 1 d . . . 
Br1 Br -0.04545(13) 0.21612(9) 0.16403(2) 0.0215(2) Uani 1 1 d . . . 
Br2 Br -0.14062(13) 0.32941(9) 0.09276(2) 0.0224(2) Uani 1 1 d . . . 
N1 N 0.3521(10) 0.3555(7) 0.15264(17) 0.0213(18) Uani 1 1 d . . . 
N2 N 0.2790(9) 0.4585(7) 0.09907(16) 0.0150(17) Uani 1 1 d . . . 
C1 C 0.4818(12) 0.4204(8) 0.1395(2) 0.017(2) Uani 1 1 d . . . 
H1 H 0.5989 0.4295 0.1487 0.021 Uiso 1 1 calc R . . 
C2 C 0.4385(12) 0.4795(8) 0.1095(2) 0.017(2) Uani 1 1 d . . . 
H2 H 0.5250 0.5304 0.0985 0.021 Uiso 1 1 calc R . . 
C11 C 0.3855(13) 0.2869(9) 0.1822(2) 0.020(2) Uani 1 1 d . . . 
H11 H 0.2663 0.2834 0.1934 0.024 Uiso 1 1 calc R . . 
C12 C 0.5229(12) 0.3522(9) 0.2035(2) 0.022(2) Uani 1 1 d . . . 
H12A H 0.6443 0.3550 0.1935 0.026 Uiso 1 1 calc R . . 
H12B H 0.4838 0.4423 0.2077 0.026 Uiso 1 1 calc R . . 
C13 C 0.5358(14) 0.2780(10) 0.2334(2) 0.025(2) Uani 1 1 d . . . 
H13A H 0.4165 0.2816 0.2441 0.030 Uiso 1 1 calc R . . 
H13B H 0.6281 0.3196 0.2468 0.030 Uiso 1 1 calc R . . 
C14 C 0.5892(13) 0.1354(10) 0.2281(2) 0.031(3) Uani 1 1 d . . . 
H14A H 0.7151 0.1312 0.2197 0.037 Uiso 1 1 calc R . . 
H14B H 0.5872 0.0885 0.2480 0.037 Uiso 1 1 calc R . . 
C15 C 0.4577(14) 0.0698(9) 0.2055(2) 0.024(2) Uani 1 1 d . . . 
H15A H 0.3357 0.0620 0.2152 0.029 Uiso 1 1 calc R . . 
H15B H 0.5023 -0.0186 0.2008 0.029 Uiso 1 1 calc R . . 
C16 C 0.4406(13) 0.1474(9) 0.1751(2) 0.022(2) Uani 1 1 d . . . 
H16A H 0.5589 0.1465 0.1640 0.026 Uiso 1 1 calc R . . 
H16B H 0.3474 0.1067 0.1617 0.026 Uiso 1 1 calc R . . 
C21 C 0.2193(13) 0.5100(9) 0.0691(2) 0.019(2) Uani 1 1 d . . . 
H21 H 0.1465 0.4400 0.0589 0.023 Uiso 1 1 calc R . . 
C22 C 0.3761(12) 0.5443(8) 0.04682(19) 0.017(2) Uani 1 1 d . . . 
H22A H 0.4474 0.6185 0.0549 0.020 Uiso 1 1 calc R . . 
H22B H 0.4594 0.4694 0.0444 0.020 Uiso 1 1 calc R . . 
C23 C 0.2891(14) 0.5798(9) 0.0157(2) 0.023(2) Uani 1 1 d . . . 
H23A H 0.3866 0.6048 0.0011 0.028 Uiso 1 1 calc R . . 
H23B H 0.2260 0.5028 0.0073 0.028 Uiso 1 1 calc R . . 
C24 C 0.1527(13) 0.6908(9) 0.0186(2) 0.025(2) Uani 1 1 d . . . 
H24A H 0.0929 0.7051 -0.0016 0.030 Uiso 1 1 calc R . . 
H24B H 0.2190 0.7712 0.0242 0.030 Uiso 1 1 calc R . . 
C25 C 0.0062(13) 0.6637(10) 0.0430(2) 0.024(2) Uani 1 1 d . . . 
H25A H -0.0690 0.7425 0.0460 0.029 Uiso 1 1 calc R . . 
H25B H -0.0752 0.5937 0.0355 0.029 Uiso 1 1 calc R . . 
C26 C 0.0899(12) 0.6238(8) 0.0738(2) 0.019(2) Uani 1 1 d . . . 
H26A H 0.1575 0.6978 0.0828 0.023 Uiso 1 1 calc R . . 
H26B H -0.0084 0.5989 0.0883 0.023 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 
Pd N1 2.025(7) . ? 
Pd N2 2.051(7) . ? 
Pd Br1 2.4065(12) . ? 
Pd Br2 2.4295(12) . ? 
N1 C1 1.294(11) . ? 
N1 C11 1.484(11) . ? 
N2 C2 1.269(11) . ? 
N2 C21 1.470(10) . ? 
C1 C2 1.472(12) . ? 
C11 C12 1.523(12) . ? 
C11 C16 1.525(12) . ? 
C12 C13 1.507(12) . ? 
C13 C14 1.540(13) . ? 
C14 C15 1.530(13) . ? 
C15 C16 1.547(12) . ? 
C21 C26 1.521(12) . ? 
C21 C22 1.541(12) . ? 
C22 C23 1.535(12) . ? 
C23 C24 1.525(12) . ? 
C24 C25 1.531(12) . ? 
C25 C26 1.527(12) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Pd N2 79.7(3) . . ? 
N1 Pd Br1 95.2(2) . . ? 
N2 Pd Br1 174.6(2) . . ? 
N1 Pd Br2 175.0(2) . . ? 
N2 Pd Br2 96.7(2) . . ? 
Br1 Pd Br2 88.59(4) . . ? 
C1 N1 C11 120.5(8) . . ? 
C1 N1 Pd 113.6(6) . . ? 
C11 N1 Pd 125.6(6) . . ? 
C2 N2 C21 121.7(8) . . ? 
C2 N2 Pd 114.0(6) . . ? 
C21 N2 Pd 124.4(5) . . ? 
N1 C1 C2 116.6(8) . . ? 
N2 C2 C1 116.2(8) . . ? 
N1 C11 C12 115.0(7) . . ? 
N1 C11 C16 108.6(7) . . ? 
C12 C11 C16 111.5(7) . . ? 
C13 C12 C11 109.8(8) . . ? 
C12 C13 C14 111.9(8) . . ? 
C15 C14 C13 111.1(8) . . ? 
C14 C15 C16 111.5(8) . . ? 
C11 C16 C15 109.8(7) . . ? 
N2 C21 C26 110.2(7) . . ? 
N2 C21 C22 114.6(7) . . ? 
C26 C21 C22 111.7(7) . . ? 
C23 C22 C21 107.3(8) . . ? 
C24 C23 C22 112.2(7) . . ? 
C23 C24 C25 112.2(7) . . ? 
C26 C25 C24 111.9(8) . . ? 
C21 C26 C25 109.9(7) . . ? 
  
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 
N2 Pd N1 C1 -2.0(6) . . . . ? 
Br1 Pd N1 C1 179.5(6) . . . . ? 
Br2 Pd N1 C1 41(3) . . . . ? 
N2 Pd N1 C11 -176.1(7) . . . . ? 
Br1 Pd N1 C11 5.4(7) . . . . ? 
Br2 Pd N1 C11 -133(2) . . . . ? 
N1 Pd N2 C2 1.2(6) . . . . ? 
Br1 Pd N2 C2 17(3) . . . . ? 
Br2 Pd N2 C2 -175.3(6) . . . . ? 
N1 Pd N2 C21 179.8(7) . . . . ? 
Br1 Pd N2 C21 -164.5(17) . . . . ? 
Br2 Pd N2 C21 3.3(6) . . . . ? 
C11 N1 C1 C2 176.9(7) . . . . ? 
Pd N1 C1 C2 2.5(10) . . . . ? 
C21 N2 C2 C1 -179.0(7) . . . . ? 
Pd N2 C2 C1 -0.3(10) . . . . ? 
N1 C1 C2 N2 -1.5(12) . . . . ? 
C1 N1 C11 C12 32.5(11) . . . . ? 
Pd N1 C11 C12 -153.7(6) . . . . ? 
C1 N1 C11 C16 -93.1(9) . . . . ? 
Pd N1 C11 C16 80.6(8) . . . . ? 
N1 C11 C12 C13 176.5(7) . . . . ? 
C16 C11 C12 C13 -59.3(10) . . . . ? 
C11 C12 C13 C14 57.2(10) . . . . ? 
C12 C13 C14 C15 -54.9(11) . . . . ? 
C13 C14 C15 C16 53.2(11) . . . . ? 
N1 C11 C16 C15 -174.5(7) . . . . ? 
C12 C11 C16 C15 57.9(10) . . . . ? 
C14 C15 C16 C11 -54.8(11) . . . . ? 
C2 N2 C21 C26 -105.3(9) . . . . ? 
Pd N2 C21 C26 76.1(9) . . . . ? 
C2 N2 C21 C22 21.7(11) . . . . ? 
Pd N2 C21 C22 -156.9(6) . . . . ? 
N2 C21 C22 C23 173.0(7) . . . . ? 
C26 C21 C22 C23 -60.7(9) . . . . ? 
C21 C22 C23 C24 57.2(9) . . . . ? 
C22 C23 C24 C25 -54.1(10) . . . . ? 
C23 C24 C25 C26 51.6(11) . . . . ? 
N2 C21 C26 C25 -171.5(7) . . . . ? 
C22 C21 C26 C25 59.9(10) . . . . ? 
C24 C25 C26 C21 -53.9(10) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              26.00 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.841 
_refine_diff_density_min   -0.983 
_refine_diff_density_rms    0.201 
#====================
_publ_contact_author 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
_publ_contact_author_email      hmalinakova@ku.edu 
_publ_contact_author_fax        1(785)8645396 
_publ_contact_author_phone      1(785)8644743 
 
_publ_requested_journal         'Organometallics'  
 
loop_ 
    _publ_author_name 
    _publ_author_address 
   'Guo, Ruiyun' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Portscheller, Jannelle L.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Day, Victor W.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Malinakova, Helena C.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
;  
 
_publ_section_title 
; 
 article title here
 Allylpalladium(IV) Intermediate inthe Synthesis of Highly Substituted 
 Benzoxepines and Benzopyrans via Reactions of Stable Palla(II)cycles 
 with Allyl Bromides  
; 
_publ_section_references 
;
  Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
 
  Flack, H. D. (1983) Acta Cryst. A39, 876-881. 
 
  Flack, H. D. and Schwarzenbach, D. (1988) Acta Cryst. A44, 
  499-506. 
 
  Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
;
_publ_section_acknowledgements 
; 
 The authors wish to thank the National Science Foundation 
 (CHE-0079282) and the University of Kansas for funds to 
 acquire the diffractometer and computers used in this work.  
; 
   
data_k46b(9) 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C10 H14 Br2 O4 Pd2' 
_chemical_formula_weight          570.83 
  
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' 
 '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            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    5.0296(5) 
_cell_length_b                    5.9963(6) 
_cell_length_c                    12.2441(11) 
_cell_angle_alpha                 85.413(2) 
_cell_angle_beta                  80.885(2) 
_cell_angle_gamma                 86.155(2) 
_cell_volume                      362.88(6) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     2479 
_cell_measurement_theta_min       3.38 
_cell_measurement_theta_max       30.48 
  
_exptl_crystal_description        'Rectangular parallelepiped' 
_exptl_crystal_colour             Gold 
_exptl_crystal_size_max           0.06 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     2.612 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              268 
_exptl_absorpt_coefficient_mu     7.984 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.580 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       100(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 SMART 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_%         0.00 
_diffrn_reflns_number             4425 
_diffrn_reflns_av_R_equivalents   0.0529 
_diffrn_reflns_av_sigmaI/netI     0.0532 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -8 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.38 
_diffrn_reflns_theta_max          30.50 
_reflns_number_total              2174 
_reflns_number_gt                 1948 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections except 1 which was flagged 
 by the user for being in the beamstop.  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)+(0.0389P)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_number_reflns          2174 
_refine_ls_number_parameters      110 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0342 
_refine_ls_R_factor_gt            0.0310 
_refine_ls_wR_factor_ref          0.0779 
_refine_ls_wR_factor_gt           0.0767 
_refine_ls_goodness_of_fit_ref    1.010 
_refine_ls_restrained_S_all       1.010 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pd Pd 0.14796(5) 0.10607(4) 0.10575(2) 0.01415(9) Uani 1 1 d . . . 
Br Br 0.13349(8) 0.21855(6) -0.09471(3) 0.02079(10) Uani 1 1 d . . . 
O1 O -0.0159(6) -0.2392(4) 0.3729(2) 0.0233(5) Uani 1 1 d . . . 
O2 O -0.2056(6) 0.1088(5) 0.3923(3) 0.0317(7) Uani 1 1 d . . . 
C1 C 0.4156(8) 0.3448(7) 0.1431(3) 0.0211(7) Uani 1 1 d . . . 
H1A H 0.423(8) 0.472(6) 0.105(3) 0.003(8) Uiso 1 1 d . . . 
H1B H 0.586(9) 0.255(7) 0.138(3) 0.017(10) Uiso 1 1 d . . . 
C2 C 0.2315(8) 0.2840(6) 0.2373(3) 0.0213(7) Uani 1 1 d . . . 
H2 H 0.103(10) 0.376(8) 0.260(4) 0.034(13) Uiso 1 1 d . . . 
C3 C 0.2128(8) 0.0564(6) 0.2723(3) 0.0202(7) Uani 1 1 d . . . 
H3 H 0.375(12) -0.057(9) 0.267(4) 0.046(15) Uiso 1 1 d . . . 
C4 C -0.0240(8) -0.0177(6) 0.3529(3) 0.0206(7) Uani 1 1 d . . . 
C5 C -0.2538(9) -0.3232(7) 0.4430(4) 0.0248(8) Uani 1 1 d . . . 
H5A H -0.222(10) -0.485(8) 0.450(4) 0.027(12) Uiso 1 1 d . . . 
H5B H -0.263(10) -0.279(8) 0.507(4) 0.031(13) Uiso 1 1 d . . . 
H5C H -0.395(10) -0.295(8) 0.404(4) 0.025(12) Uiso 1 1 d . . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Pd C3 2.111(4) . ? 
Pd C2 2.111(4) . ? 
Pd C1 2.151(4) . ? 
Pd Br 2.5040(5) . ? 
Pd Br 2.5066(5) 2 ? 
Br Pd 2.5066(5) 2 ? 
O1 C4 1.331(4) . ? 
O1 C5 1.452(5) . ? 
O2 C4 1.212(5) . ? 
C1 C2 1.400(5) . ? 
C1 H1A 0.86(4) . ? 
C1 H1B 0.98(4) . ? 
C2 C3 1.402(5) . ? 
C2 H2 0.85(5) . ? 
C3 C4 1.489(5) . ? 
C3 H3 1.02(6) . ? 
C5 H5A 0.97(5) . ? 
C5 H5B 0.84(5) . ? 
C5 H5C 0.92(5) . ? 
  
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 
C3 Pd C2 38.79(14) . . ? 
C3 Pd C1 68.95(15) . . ? 
C2 Pd C1 38.32(14) . . ? 
C3 Pd Br 169.47(10) . . ? 
C2 Pd Br 132.24(11) . . ? 
C1 Pd Br 100.55(11) . . ? 
C3 Pd Br 100.35(10) . 2 ? 
C2 Pd Br 134.03(11) . 2 ? 
C1 Pd Br 168.44(11) . 2 ? 
Br Pd Br 90.052(14) . 2 ? 
Pd Br Pd 89.948(14) . 2 ? 
C4 O1 C5 114.2(3) . . ? 
C2 C1 Pd 69.3(2) . . ? 
C2 C1 H1A 128(3) . . ? 
Pd C1 H1A 118(2) . . ? 
C2 C1 H1B 113(2) . . ? 
Pd C1 H1B 101(2) . . ? 
H1A C1 H1B 115(3) . . ? 
C1 C2 C3 118.9(4) . . ? 
C1 C2 Pd 72.4(2) . . ? 
C3 C2 Pd 70.6(2) . . ? 
C1 C2 H2 119(3) . . ? 
C3 C2 H2 119(4) . . ? 
Pd C2 H2 112(3) . . ? 
C2 C3 C4 119.7(3) . . ? 
C2 C3 Pd 70.6(2) . . ? 
C4 C3 Pd 115.2(2) . . ? 
C2 C3 H3 123(3) . . ? 
C4 C3 H3 114(3) . . ? 
Pd C3 H3 102(3) . . ? 
O2 C4 O1 124.4(4) . . ? 
O2 C4 C3 123.8(3) . . ? 
O1 C4 C3 111.8(3) . . ? 
O1 C5 H5A 105(3) . . ? 
O1 C5 H5B 109(4) . . ? 
H5A C5 H5B 107(4) . . ? 
O1 C5 H5C 107(3) . . ? 
H5A C5 H5C 106(4) . . ? 
H5B C5 H5C 121(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 
C3 Pd Br Pd 171.1(6) . . . 2 ? 
C2 Pd Br Pd -159.99(15) . . . 2 ? 
C1 Pd Br Pd 175.36(11) . . . 2 ? 
Br Pd Br Pd 0.0 2 . . 2 ? 
C3 Pd C1 C2 -30.7(2) . . . . ? 
Br Pd C1 C2 150.1(2) . . . . ? 
Br Pd C1 C2 -53.7(6) 2 . . . ? 
Pd C1 C2 C3 55.0(3) . . . . ? 
C3 Pd C2 C1 130.5(3) . . . . ? 
Br Pd C2 C1 -41.4(3) . . . . ? 
Br Pd C2 C1 167.03(18) 2 . . . ? 
C1 Pd C2 C3 -130.5(3) . . . . ? 
Br Pd C2 C3 -171.89(17) . . . . ? 
Br Pd C2 C3 36.5(3) 2 . . . ? 
C1 C2 C3 C4 -164.5(3) . . . . ? 
Pd C2 C3 C4 -108.6(3) . . . . ? 
C1 C2 C3 Pd -55.9(3) . . . . ? 
C1 Pd C3 C2 30.3(2) . . . . ? 
Br Pd C3 C2 34.9(7) . . . . ? 
Br Pd C3 C2 -154.2(2) 2 . . . ? 
C2 Pd C3 C4 114.5(4) . . . . ? 
C1 Pd C3 C4 144.9(3) . . . . ? 
Br Pd C3 C4 149.4(4) . . . . ? 
Br Pd C3 C4 -39.7(3) 2 . . . ? 
C5 O1 C4 O2 3.1(5) . . . . ? 
C5 O1 C4 C3 -174.7(3) . . . . ? 
C2 C3 C4 O2 -0.9(6) . . . . ? 
Pd C3 C4 O2 -82.0(4) . . . . ? 
C2 C3 C4 O1 177.0(3) . . . . ? 
Pd C3 C4 O1 95.8(3) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.982 
_diffrn_reflns_theta_full              30.50 
_diffrn_measured_fraction_theta_full   0.982 
_refine_diff_density_max    1.140 
_refine_diff_density_min   -1.764 
_refine_diff_density_rms    0.188 
#====================
_publ_contact_author 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
_publ_contact_author_email      hmalinakova@ku.edu 
_publ_contact_author_fax        1(785)8645396 
_publ_contact_author_phone      1(785)8644743 
 
_publ_requested_journal         'Organometallics'  
 
loop_ 
    _publ_author_name 
    _publ_author_address 
   'Guo, Ruiyun' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Portscheller, Jannelle L.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Day, Victor W.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Malinakova, Helena C.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
 
_publ_section_title 
; 
 article title here
 Allylpalladium(IV) Intermediate inthe Synthesis of Highly Substituted 
 Benzoxepines and Benzopyrans via Reactions of Stable Palla(II)cycles 
 with Allyl Bromides  
; 
_publ_section_references 
;
  Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
 
  Flack, H. D. (1983) Acta Cryst. A39, 876-881. 
 
  Flack, H. D. and Schwarzenbach, D. (1988) Acta Cryst. A44, 
  499-506. 
 
  Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
;
_publ_section_acknowledgements 
; 
 The authors wish to thank the National Science Foundation 
 (CHE-0079282) and the University of Kansas for funds to 
 acquire the diffractometer and computers used in this work.  
; 
    
data_k48c(10) 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C33 H49 Br N2 O7 Pd' 
_chemical_formula_weight          772.05 
  
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            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    8.2999(8) 
_cell_length_b                    10.7468(10) 
_cell_length_c                    20.757(2) 
_cell_angle_alpha                 102.346(2) 
_cell_angle_beta                  91.945(2) 
_cell_angle_gamma                 102.168(2) 
_cell_volume                      1761.9(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     5262 
_cell_measurement_theta_min       2.52 
_cell_measurement_theta_max       30.50 
  
_exptl_crystal_description        Parallelepiped 
_exptl_crystal_colour             Yellow/gold 
_exptl_crystal_size_max           0.36 
_exptl_crystal_size_mid           0.28 
_exptl_crystal_size_min           0.14 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.455 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              796 
_exptl_absorpt_coefficient_mu     1.707 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.834 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       100(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 SMART 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_%         0.00 
_diffrn_reflns_number             21632 
_diffrn_reflns_av_R_equivalents   0.0295 
_diffrn_reflns_av_sigmaI/netI     0.0428 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -29 
_diffrn_reflns_limit_l_max        29 
_diffrn_reflns_theta_min          2.43 
_diffrn_reflns_theta_max          30.59 
_reflns_number_total              10621 
_reflns_number_gt                 8784 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_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)+(0.0545P)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_number_reflns          10621 
_refine_ls_number_parameters      418 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0461 
_refine_ls_R_factor_gt            0.0371 
_refine_ls_wR_factor_ref          0.0946 
_refine_ls_wR_factor_gt           0.0922 
_refine_ls_goodness_of_fit_ref    1.028 
_refine_ls_restrained_S_all       1.028 
_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 
Pd Pd 0.31246(2) -0.084646(15) 0.238612(8) 0.01738(5) Uani 1 1 d . . . 
Br Br 0.54464(3) -0.17009(2) 0.270420(12) 0.02388(6) Uani 1 1 d . . . 
O1 O 0.5074(2) -0.12372(15) 0.10157(8) 0.0234(3) Uani 1 1 d . . . 
O2 O 0.4513(2) 0.16576(15) 0.20416(8) 0.0222(3) Uani 1 1 d . . . 
O3 O 0.9276(2) 0.65007(17) 0.12534(9) 0.0334(4) Uani 1 1 d . . . 
O4 O 0.3552(2) 0.01682(17) 0.08166(8) 0.0264(4) Uani 1 1 d . . . 
O5 O 0.8060(2) 0.45751(17) 0.05796(9) 0.0330(4) Uani 1 1 d . . . 
N1 N 0.0962(2) -0.03180(18) 0.21391(9) 0.0192(4) Uani 1 1 d . . . 
N2 N 0.1362(2) -0.20802(18) 0.28356(9) 0.0213(4) Uani 1 1 d . . . 
C1 C 0.4703(3) 0.0348(2) 0.19264(11) 0.0195(4) Uani 1 1 d . . . 
H1 H 0.5869 0.0345 0.2064 0.023 Uiso 1 1 calc R . . 
C2 C 0.4361(3) -0.0215(2) 0.11969(11) 0.0213(4) Uani 1 1 d . . . 
C3 C 0.4847(3) -0.1881(2) 0.03179(11) 0.0256(5) Uani 1 1 d . . . 
H3A H 0.5286 -0.1251 0.0047 0.031 Uiso 1 1 calc R . . 
H3B H 0.3657 -0.2243 0.0180 0.031 Uiso 1 1 calc R . . 
C4 C 0.5768(4) -0.2960(3) 0.02263(13) 0.0365(6) Uani 1 1 d . . . 
H4A H 0.5643 -0.3415 -0.0241 0.055 Uiso 1 1 calc R . . 
H4B H 0.5318 -0.3579 0.0495 0.055 Uiso 1 1 calc R . . 
H4C H 0.6942 -0.2590 0.0365 0.055 Uiso 1 1 calc R . . 
C5 C 0.5156(3) 0.2483(2) 0.26366(11) 0.0231(4) Uani 1 1 d . . . 
C6 C 0.5827(3) 0.2095(2) 0.31597(12) 0.0286(5) Uani 1 1 d . . . 
H6 H 0.5871 0.1207 0.3122 0.034 Uiso 1 1 calc R . . 
C7 C 0.6440(4) 0.3025(3) 0.37444(13) 0.0373(6) Uani 1 1 d . . . 
H7 H 0.6902 0.2765 0.4106 0.045 Uiso 1 1 calc R . . 
C8 C 0.6378(4) 0.4322(3) 0.38008(13) 0.0375(6) Uani 1 1 d . . . 
H8 H 0.6785 0.4949 0.4201 0.045 Uiso 1 1 calc R . . 
C9 C 0.5724(3) 0.4697(3) 0.32729(13) 0.0333(6) Uani 1 1 d . . . 
H9 H 0.5701 0.5591 0.3312 0.040 Uiso 1 1 calc R . . 
C10 C 0.5094(3) 0.3800(2) 0.26827(12) 0.0257(5) Uani 1 1 d . . . 
C11 C 0.4495(3) 0.4245(2) 0.20947(13) 0.0285(5) Uani 1 1 d . . . 
H11A H 0.3466 0.3626 0.1879 0.034 Uiso 1 1 calc R . . 
H11B H 0.4239 0.5115 0.2246 0.034 Uiso 1 1 calc R . . 
C12 C 0.5785(3) 0.4323(2) 0.16020(12) 0.0265(5) Uani 1 1 d . . . 
H12 H 0.5908 0.3529 0.1324 0.032 Uiso 1 1 calc R . . 
C13 C 0.6752(3) 0.5418(2) 0.15311(12) 0.0255(5) Uani 1 1 d . . . 
H13 H 0.6609 0.6226 0.1788 0.031 Uiso 1 1 calc R . . 
C14 C 0.8045(3) 0.5422(2) 0.10658(12) 0.0262(5) Uani 1 1 d . . . 
C15 C 1.0662(4) 0.6557(3) 0.08480(15) 0.0428(7) Uani 1 1 d . . . 
H15A H 1.1509 0.7351 0.1034 0.064 Uiso 1 1 calc R . . 
H15B H 1.0286 0.6567 0.0397 0.064 Uiso 1 1 calc R . . 
H15C H 1.1130 0.5789 0.0838 0.064 Uiso 1 1 calc R . . 
C21 C 0.0658(3) 0.0637(2) 0.17508(11) 0.0214(4) Uani 1 1 d . . . 
H21 H 0.1752 0.1080 0.1629 0.026 Uiso 1 1 calc R . . 
C22 C -0.0408(3) -0.0070(2) 0.11087(12) 0.0248(5) Uani 1 1 d . . . 
H22A H 0.0151 -0.0711 0.0845 0.030 Uiso 1 1 calc R . . 
H22B H -0.1485 -0.0551 0.1213 0.030 Uiso 1 1 calc R . . 
C23 C -0.0692(3) 0.0909(3) 0.07087(13) 0.0296(5) Uani 1 1 d . . . 
H23A H -0.1415 0.0444 0.0302 0.036 Uiso 1 1 calc R . . 
H23B H 0.0378 0.1339 0.0574 0.036 Uiso 1 1 calc R . . 
C24 C -0.1495(3) 0.1942(2) 0.11128(13) 0.0293(5) Uani 1 1 d . . . 
H24A H -0.1630 0.2584 0.0849 0.035 Uiso 1 1 calc R . . 
H24B H -0.2607 0.1519 0.1214 0.035 Uiso 1 1 calc R . . 
C25 C -0.0462(3) 0.2643(2) 0.17518(14) 0.0324(6) Uani 1 1 d . . . 
H25A H -0.1053 0.3259 0.2016 0.039 Uiso 1 1 calc R . . 
H25B H 0.0597 0.3157 0.1650 0.039 Uiso 1 1 calc R . . 
C26 C -0.0101(3) 0.1683(2) 0.21621(12) 0.0284(5) Uani 1 1 d . . . 
H26A H 0.0668 0.2167 0.2553 0.034 Uiso 1 1 calc R . . 
H26B H -0.1142 0.1263 0.2322 0.034 Uiso 1 1 calc R . . 
C27 C -0.0312(3) -0.0990(2) 0.23371(12) 0.0270(5) Uani 1 1 d . . . 
H27 H -0.1384 -0.0864 0.2239 0.032 Uiso 1 1 calc R . . 
C28 C -0.0096(3) -0.1956(2) 0.27175(12) 0.0273(5) Uani 1 1 d . . . 
H28 H -0.1017 -0.2470 0.2870 0.033 Uiso 1 1 calc R . . 
C29 C 0.1689(3) -0.3014(2) 0.32207(12) 0.0242(5) Uani 1 1 d . . . 
H29 H 0.2591 -0.3406 0.3013 0.029 Uiso 1 1 calc R . . 
C30 C 0.2377(4) -0.2244(3) 0.39176(12) 0.0314(5) Uani 1 1 d . . . 
H30A H 0.1516 -0.1847 0.4145 0.038 Uiso 1 1 calc R . . 
H30B H 0.3330 -0.1532 0.3891 0.038 Uiso 1 1 calc R . . 
C31 C 0.2927(4) -0.3157(3) 0.43120(14) 0.0445(7) Uani 1 1 d . . . 
H31A H 0.3883 -0.3462 0.4114 0.053 Uiso 1 1 calc R . . 
H31B H 0.3292 -0.2665 0.4772 0.053 Uiso 1 1 calc R . . 
C32 C 0.1550(5) -0.4334(3) 0.43217(17) 0.0521(9) Uani 1 1 d . . . 
H32A H 0.1983 -0.4936 0.4546 0.063 Uiso 1 1 calc R . . 
H32B H 0.0654 -0.4043 0.4574 0.063 Uiso 1 1 calc R . . 
C33 C 0.0862(4) -0.5049(3) 0.36245(17) 0.0473(8) Uani 1 1 d . . . 
H33A H -0.0068 -0.5785 0.3643 0.057 Uiso 1 1 calc R . . 
H33B H 0.1731 -0.5415 0.3387 0.057 Uiso 1 1 calc R . . 
C34 C 0.0252(4) -0.4138(3) 0.32415(16) 0.0375(6) Uani 1 1 d . . . 
H34A H -0.0173 -0.4625 0.2786 0.045 Uiso 1 1 calc R . . 
H34B H -0.0656 -0.3799 0.3463 0.045 Uiso 1 1 calc R . . 
O1S O 0.1868(6) 0.2687(4) 0.5175(2) 0.0755(18) Uani 0.621(7) 1 d P A 1 
O2S O 0.2772(5) 0.0967(3) 0.48375(13) 0.0854(10) Uani 1 1 d . A 1 
C1S C 0.2028(6) 0.1873(4) 0.3963(2) 0.0682(11) Uani 1 1 d . A 1 
H1SA H 0.1680 0.2648 0.3884 0.102 Uiso 1 1 calc R A 1 
H1SB H 0.1168 0.1091 0.3769 0.102 Uiso 1 1 calc R A 1 
H1SC H 0.3061 0.1804 0.3757 0.102 Uiso 1 1 calc R A 1 
C2S C 0.2292(6) 0.1988(4) 0.4686(2) 0.0760(13) Uani 0.621(7) 1 d P A 1 
C3S C 0.3195(10) 0.0760(8) 0.5476(3) 0.069(2) Uani 0.621(7) 1 d P A 1 
H3SA H 0.4236 0.0448 0.5460 0.083 Uiso 0.621(7) 1 calc PR A 1 
H3SB H 0.3402 0.1607 0.5803 0.083 Uiso 0.621(7) 1 calc PR A 1 
C4S C 0.2039(9) -0.0096(5) 0.5683(2) 0.130(3) Uani 1 1 d . A 1 
H4SA H 0.2423 -0.0202 0.6115 0.195 Uiso 1 1 calc R A 1 
H4SB H 0.1827 -0.0941 0.5364 0.195 Uiso 1 1 calc R A 1 
H4SC H 0.1017 0.0224 0.5721 0.195 Uiso 1 1 calc R A 1 
O1S' O 0.2032(14) 0.2056(12) 0.5832(5) 0.114(4) Uani 0.379(7) 1 d P A 2 
C2S' C 0.2263(11) 0.1060(9) 0.5517(4) 0.039(2) Uani 0.379(7) 1 d P A 2 
C3S' C 0.2292(6) 0.1988(4) 0.4686(2) 0.0760(13) Uani 0.379(7) 1 d P A 2 
H3SA H 0.3129 0.2808 0.4861 0.091 Uiso 0.379(7) 1 d PR A 2 
H3SB H 0.1254 0.2114 0.4883 0.091 Uiso 0.379(7) 1 d PR A 2 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Pd C1 2.043(2) . ? 
Pd N1 2.0736(18) . ? 
Pd N2 2.1386(19) . ? 
Pd Br 2.4314(3) . ? 
O1 C2 1.345(3) . ? 
O1 C3 1.453(3) . ? 
O2 C5 1.373(3) . ? 
O2 C1 1.420(3) . ? 
O3 C14 1.349(3) . ? 
O3 C15 1.447(3) . ? 
O4 C2 1.210(3) . ? 
O5 C14 1.208(3) . ? 
N1 C27 1.282(3) . ? 
N1 C21 1.488(3) . ? 
N2 C28 1.266(3) . ? 
N2 C29 1.470(3) . ? 
C1 C2 1.499(3) . ? 
C3 C4 1.501(3) . ? 
C5 C6 1.383(3) . ? 
C5 C10 1.410(3) . ? 
C6 C7 1.398(4) . ? 
C7 C8 1.386(4) . ? 
C8 C9 1.378(4) . ? 
C9 C10 1.394(3) . ? 
C10 C11 1.508(3) . ? 
C11 C12 1.507(3) . ? 
C12 C13 1.317(3) . ? 
C13 C14 1.468(3) . ? 
C21 C26 1.521(3) . ? 
C21 C22 1.530(3) . ? 
C22 C23 1.522(3) . ? 
C23 C24 1.527(4) . ? 
C24 C25 1.512(4) . ? 
C25 C26 1.539(3) . ? 
C27 C28 1.467(3) . ? 
C29 C34 1.518(3) . ? 
C29 C30 1.528(3) . ? 
C30 C31 1.532(4) . ? 
C31 C32 1.520(5) . ? 
C32 C33 1.515(5) . ? 
C33 C34 1.536(4) . ? 
O1S C2S 1.237(5) . ? 
O2S C2S 1.336(5) . ? 
O2S C3S 1.434(7) . ? 
C1S C2S 1.484(6) . ? 
C3S C4S 1.333(8) . ? 
O1S' C2S' 1.185(13) . ? 
  
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 
C1 Pd N1 97.93(8) . . ? 
C1 Pd N2 176.85(8) . . ? 
N1 Pd N2 79.06(7) . . ? 
C1 Pd Br 88.69(6) . . ? 
N1 Pd Br 173.05(5) . . ? 
N2 Pd Br 94.29(5) . . ? 
C2 O1 C3 116.33(17) . . ? 
C5 O2 C1 118.04(17) . . ? 
C14 O3 C15 115.5(2) . . ? 
C27 N1 C21 116.67(19) . . ? 
C27 N1 Pd 112.27(15) . . ? 
C21 N1 Pd 130.97(14) . . ? 
C28 N2 C29 121.1(2) . . ? 
C28 N2 Pd 111.62(16) . . ? 
C29 N2 Pd 127.22(15) . . ? 
O2 C1 C2 107.04(17) . . ? 
O2 C1 Pd 115.11(14) . . ? 
C2 C1 Pd 106.90(14) . . ? 
O4 C2 O1 123.8(2) . . ? 
O4 C2 C1 126.0(2) . . ? 
O1 C2 C1 110.25(18) . . ? 
O1 C3 C4 107.30(19) . . ? 
O2 C5 C6 124.4(2) . . ? 
O2 C5 C10 114.6(2) . . ? 
C6 C5 C10 121.0(2) . . ? 
C5 C6 C7 119.3(2) . . ? 
C8 C7 C6 120.5(3) . . ? 
C9 C8 C7 119.6(2) . . ? 
C8 C9 C10 121.7(2) . . ? 
C9 C10 C5 117.9(2) . . ? 
C9 C10 C11 120.8(2) . . ? 
C5 C10 C11 121.1(2) . . ? 
C12 C11 C10 110.9(2) . . ? 
C13 C12 C11 124.4(2) . . ? 
C12 C13 C14 121.8(2) . . ? 
O5 C14 O3 122.8(2) . . ? 
O5 C14 C13 125.9(2) . . ? 
O3 C14 C13 111.4(2) . . ? 
N1 C21 C26 111.14(18) . . ? 
N1 C21 C22 110.42(18) . . ? 
C26 C21 C22 111.94(19) . . ? 
C23 C22 C21 110.2(2) . . ? 
C22 C23 C24 110.9(2) . . ? 
C25 C24 C23 111.3(2) . . ? 
C24 C25 C26 111.8(2) . . ? 
C21 C26 C25 110.9(2) . . ? 
N1 C27 C28 119.3(2) . . ? 
N2 C28 C27 117.6(2) . . ? 
N2 C29 C34 116.3(2) . . ? 
N2 C29 C30 108.04(19) . . ? 
C34 C29 C30 111.2(2) . . ? 
C29 C30 C31 109.8(2) . . ? 
C32 C31 C30 112.1(3) . . ? 
C33 C32 C31 110.7(2) . . ? 
C32 C33 C34 111.6(3) . . ? 
C29 C34 C33 108.6(2) . . ? 
C2S O2S C3S 129.0(5) . . ? 
O1S C2S O2S 111.7(5) . . ? 
O1S C2S C1S 133.2(5) . . ? 
O2S C2S C1S 113.4(3) . . ? 
C4S C3S O2S 114.1(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 
C1 Pd N1 C27 176.19(17) . . . . ? 
N2 Pd N1 C27 -2.89(16) . . . . ? 
Br Pd N1 C27 14.2(5) . . . . ? 
C1 Pd N1 C21 -0.24(19) . . . . ? 
N2 Pd N1 C21 -179.31(19) . . . . ? 
Br Pd N1 C21 -162.2(3) . . . . ? 
C1 Pd N2 C28 -13.9(15) . . . . ? 
N1 Pd N2 C28 3.00(17) . . . . ? 
Br Pd N2 C28 -174.96(17) . . . . ? 
C1 Pd N2 C29 164.1(14) . . . . ? 
N1 Pd N2 C29 -179.00(19) . . . . ? 
Br Pd N2 C29 3.05(18) . . . . ? 
C5 O2 C1 C2 -163.84(18) . . . . ? 
C5 O2 C1 Pd 77.5(2) . . . . ? 
N1 Pd C1 O2 46.39(16) . . . . ? 
N2 Pd C1 O2 63.1(15) . . . . ? 
Br Pd C1 O2 -135.76(15) . . . . ? 
N1 Pd C1 C2 -72.35(15) . . . . ? 
N2 Pd C1 C2 -55.6(15) . . . . ? 
Br Pd C1 C2 105.51(14) . . . . ? 
C3 O1 C2 O4 0.7(3) . . . . ? 
C3 O1 C2 C1 -179.86(18) . . . . ? 
O2 C1 C2 O4 -22.9(3) . . . . ? 
Pd C1 C2 O4 100.9(2) . . . . ? 
O2 C1 C2 O1 157.68(17) . . . . ? 
Pd C1 C2 O1 -78.47(19) . . . . ? 
C2 O1 C3 C4 178.7(2) . . . . ? 
C1 O2 C5 C6 -7.0(3) . . . . ? 
C1 O2 C5 C10 172.74(19) . . . . ? 
O2 C5 C6 C7 -179.7(2) . . . . ? 
C10 C5 C6 C7 0.5(4) . . . . ? 
C5 C6 C7 C8 0.0(4) . . . . ? 
C6 C7 C8 C9 -0.7(4) . . . . ? 
C7 C8 C9 C10 1.0(4) . . . . ? 
C8 C9 C10 C5 -0.5(4) . . . . ? 
C8 C9 C10 C11 -175.6(2) . . . . ? 
O2 C5 C10 C9 180.0(2) . . . . ? 
C6 C5 C10 C9 -0.2(4) . . . . ? 
O2 C5 C10 C11 -5.0(3) . . . . ? 
C6 C5 C10 C11 174.8(2) . . . . ? 
C9 C10 C11 C12 100.0(3) . . . . ? 
C5 C10 C11 C12 -74.9(3) . . . . ? 
C10 C11 C12 C13 -102.8(3) . . . . ? 
C11 C12 C13 C14 176.7(2) . . . . ? 
C15 O3 C14 O5 -2.5(4) . . . . ? 
C15 O3 C14 C13 176.3(2) . . . . ? 
C12 C13 C14 O5 24.3(4) . . . . ? 
C12 C13 C14 O3 -154.5(2) . . . . ? 
C27 N1 C21 C26 62.6(3) . . . . ? 
Pd N1 C21 C26 -121.10(19) . . . . ? 
C27 N1 C21 C22 -62.2(3) . . . . ? 
Pd N1 C21 C22 114.06(19) . . . . ? 
N1 C21 C22 C23 -179.13(19) . . . . ? 
C26 C21 C22 C23 56.5(3) . . . . ? 
C21 C22 C23 C24 -57.2(3) . . . . ? 
C22 C23 C24 C25 57.0(3) . . . . ? 
C23 C24 C25 C26 -54.9(3) . . . . ? 
N1 C21 C26 C25 -178.26(19) . . . . ? 
C22 C21 C26 C25 -54.3(3) . . . . ? 
C24 C25 C26 C21 53.4(3) . . . . ? 
C21 N1 C27 C28 179.5(2) . . . . ? 
Pd N1 C27 C28 2.5(3) . . . . ? 
C29 N2 C28 C27 179.2(2) . . . . ? 
Pd N2 C28 C27 -2.6(3) . . . . ? 
N1 C27 C28 N2 0.2(4) . . . . ? 
C28 N2 C29 C34 22.5(3) . . . . ? 
Pd N2 C29 C34 -155.35(18) . . . . ? 
C28 N2 C29 C30 -103.4(3) . . . . ? 
Pd N2 C29 C30 78.8(2) . . . . ? 
N2 C29 C30 C31 -173.4(2) . . . . ? 
C34 C29 C30 C31 57.9(3) . . . . ? 
C29 C30 C31 C32 -54.7(3) . . . . ? 
C30 C31 C32 C33 54.2(3) . . . . ? 
C31 C32 C33 C34 -56.2(3) . . . . ? 
N2 C29 C34 C33 176.3(2) . . . . ? 
C30 C29 C34 C33 -59.5(3) . . . . ? 
C32 C33 C34 C29 58.7(3) . . . . ? 
C3S O2S C2S O1S -15.3(8) . . . . ? 
C3S O2S C2S C1S 177.6(5) . . . . ? 
C2S O2S C3S C4S 105.1(8) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.979 
_diffrn_reflns_theta_full              30.59 
_diffrn_measured_fraction_theta_full   0.979 
_refine_diff_density_max    1.609 
_refine_diff_density_min   -0.886 
_refine_diff_density_rms    0.099 
 
#====================
_publ_contact_author 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
_publ_contact_author_email      hmalinakova@ku.edu 
_publ_contact_author_fax        1(785)8645396 
_publ_contact_author_phone      1(785)8644743 
 
_publ_requested_journal         'Organometallics'  
 
loop_ 
    _publ_author_name 
    _publ_author_address 
    'Guo, Ruiyun' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Portscheller, Jannelle L.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Day, Victor W.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Malinakova, Helena C.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
 
_publ_section_title 
; 
 article title here
 Allylpalladium(IV) Intermediate inthe Synthesis of Highly Substituted 
 Benzoxepines and Benzopyrans via Reactions of Stable Palla(II)cycles 
 with Allyl Bromides  
; 
_publ_section_references 
;
  Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
 
  Flack, H. D. (1983) Acta Cryst. A39, 876-881. 
 
  Flack, H. D. and Schwarzenbach, D. (1988) Acta Cryst. A44, 
  499-506. 
 
  Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
;
_publ_section_acknowledgements 
; 
 The authors wish to thank the National Science Foundation 
 (CHE-0079282) and the University of Kansas for funds to 
 acquire the diffractometer and computers used in this work.  
;    
data_k43b(11) 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C25 H25 Br N2 O5 Pd' 
_chemical_formula_weight          619.78 
  
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            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    8.2576(9) 
_cell_length_b                    12.5536(14) 
_cell_length_c                    13.0012(14) 
_cell_angle_alpha                 112.321(3) 
_cell_angle_beta                  93.136(3) 
_cell_angle_gamma                 101.218(3) 
_cell_volume                      1210.6(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     4604 
_cell_measurement_theta_min       2.54 
_cell_measurement_theta_max       29.52 
  
_exptl_crystal_description        'Near cube' 
_exptl_crystal_colour             Yellow 
_exptl_crystal_size_max           0.16 
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.700 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              620 
_exptl_absorpt_coefficient_mu     2.456 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.705 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       100(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 SMART 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_%         0.00 
_diffrn_reflns_number             11341 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0689 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.54 
_diffrn_reflns_theta_max          30.60 
_reflns_number_total              11342 
_reflns_number_gt                 8834 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections except 4 which were flagged 
 by the user for possible systematic errors.  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)+(0.0583P)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     noref 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          11342 
_refine_ls_number_parameters      310 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0656 
_refine_ls_R_factor_gt            0.0507 
_refine_ls_wR_factor_ref          0.1191 
_refine_ls_wR_factor_gt           0.1141 
_refine_ls_goodness_of_fit_ref    1.039 
_refine_ls_restrained_S_all       1.039 
_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 
Pd Pd 0.15157(4) 0.69264(3) 0.38838(3) 0.01717(7) Uani 1 1 d . . . 
Br Br 0.06723(5) 0.84655(4) 0.34266(3) 0.02392(10) Uani 1 1 d . . . 
O1 O 0.4525(3) 0.7739(3) 0.2613(3) 0.0279(7) Uani 1 1 d . . . 
O2 O 0.1679(3) 0.5026(2) 0.1673(2) 0.0226(6) Uani 1 1 d . . . 
O3 O 0.4190(4) 0.1428(3) 0.2223(3) 0.0344(8) Uani 1 1 d . . . 
O4 O 0.4866(4) 0.5995(3) 0.2604(2) 0.0279(7) Uani 1 1 d . . . 
O5 O 0.2093(4) 0.0108(3) 0.0927(3) 0.0328(7) Uani 1 1 d . . . 
N1 N 0.2146(4) 0.5684(3) 0.4419(3) 0.0191(7) Uani 1 1 d . . . 
N2 N 0.1160(4) 0.7649(3) 0.5596(3) 0.0195(7) Uani 1 1 d . . . 
C1 C 0.2112(5) 0.6270(3) 0.2289(3) 0.0202(8) Uani 1 1 d . . . 
H1 H 0.1679 0.6674 0.1838 0.024 Uiso 1 1 calc R . . 
C2 C 0.3973(5) 0.6616(4) 0.2502(3) 0.0210(8) Uani 1 1 d . . . 
C3 C 0.6270(5) 0.8260(4) 0.3072(4) 0.0354(11) Uani 1 1 d . . . 
H3A H 0.6718 0.8874 0.2793 0.043 Uiso 1 1 calc R . . 
H3B H 0.6919 0.7643 0.2832 0.043 Uiso 1 1 calc R . . 
C4 C 0.6420(6) 0.8798(5) 0.4321(5) 0.0492(15) Uani 1 1 d . . . 
H4A H 0.7596 0.9152 0.4641 0.074 Uiso 1 1 calc R . . 
H4B H 0.5981 0.8184 0.4592 0.074 Uiso 1 1 calc R . . 
H4C H 0.5783 0.9412 0.4553 0.074 Uiso 1 1 calc R . . 
C5 C 0.0062(5) 0.4489(3) 0.1157(3) 0.0197(8) Uani 1 1 d . . . 
C6 C -0.1283(5) 0.4989(3) 0.1454(3) 0.0208(8) Uani 1 1 d . . . 
H6 H -0.1110 0.5770 0.2012 0.025 Uiso 1 1 calc R . . 
C7 C -0.2894(5) 0.4346(4) 0.0936(3) 0.0241(9) Uani 1 1 d . . . 
H7 H -0.3821 0.4686 0.1140 0.029 Uiso 1 1 calc R . . 
C8 C -0.3133(5) 0.3209(4) 0.0123(4) 0.0256(9) Uani 1 1 d . . . 
H8 H -0.4229 0.2751 -0.0209 0.031 Uiso 1 1 calc R . . 
C9 C -0.1764(5) 0.2740(4) -0.0206(3) 0.0244(9) Uani 1 1 d . . . 
H9 H -0.1938 0.1972 -0.0788 0.029 Uiso 1 1 calc R . . 
C10 C -0.0152(5) 0.3362(3) 0.0292(3) 0.0224(8) Uani 1 1 d . . . 
C11 C 0.1352(5) 0.2890(4) -0.0130(4) 0.0251(9) Uani 1 1 d . . . 
H11A H 0.1188 0.2556 -0.0961 0.030 Uiso 1 1 calc R . . 
H11B H 0.2358 0.3551 0.0140 0.030 Uiso 1 1 calc R . . 
C12 C 0.1617(5) 0.1956(4) 0.0266(4) 0.0253(9) Uani 1 1 d . . . 
H12 H 0.0829 0.1215 -0.0046 0.030 Uiso 1 1 calc R . . 
C13 C 0.2873(5) 0.2082(4) 0.1023(4) 0.0252(9) Uani 1 1 d . . . 
H13 H 0.3693 0.2806 0.1348 0.030 Uiso 1 1 calc R . . 
C14 C 0.2988(5) 0.1101(4) 0.1354(4) 0.0254(9) Uani 1 1 d . . . 
C15 C 0.4399(6) 0.0499(4) 0.2595(4) 0.0385(12) Uani 1 1 d . . . 
H15A H 0.5292 0.0823 0.3234 0.058 Uiso 1 1 calc R . . 
H15B H 0.4689 -0.0146 0.1978 0.058 Uiso 1 1 calc R . . 
H15C H 0.3355 0.0196 0.2822 0.058 Uiso 1 1 calc R . . 
C21 C 0.2543(5) 0.4678(3) 0.3791(3) 0.0229(8) Uani 1 1 d . . . 
H21 H 0.2558 0.4490 0.3012 0.028 Uiso 1 1 calc R . . 
C22 C 0.2932(5) 0.3900(4) 0.4225(4) 0.0257(9) Uani 1 1 d . . . 
H22 H 0.3193 0.3185 0.3749 0.031 Uiso 1 1 calc R . . 
C23 C 0.2940(5) 0.4165(4) 0.5348(4) 0.0300(10) Uani 1 1 d . . . 
H23 H 0.3217 0.3643 0.5663 0.036 Uiso 1 1 calc R . . 
C24 C 0.2540(5) 0.5196(4) 0.6012(4) 0.0250(8) Uani 1 1 d . . . 
H24 H 0.2545 0.5399 0.6795 0.030 Uiso 1 1 calc R . . 
C25 C 0.2129(5) 0.5942(4) 0.5531(4) 0.0221(8) Uani 1 1 d . . . 
C26 C 0.1644(5) 0.7061(4) 0.6201(4) 0.0220(8) Uani 1 1 d . . . 
C27 C 0.1663(5) 0.7490(4) 0.7361(4) 0.0264(9) Uani 1 1 d . . . 
H27 H 0.2003 0.7066 0.7770 0.032 Uiso 1 1 calc R . . 
C28 C 0.1188(6) 0.8531(4) 0.7909(4) 0.0308(10) Uani 1 1 d . . . 
H28 H 0.1221 0.8846 0.8702 0.037 Uiso 1 1 calc R . . 
C29 C 0.0657(6) 0.9112(4) 0.7280(4) 0.0300(10) Uani 1 1 d . . . 
H29 H 0.0299 0.9823 0.7636 0.036 Uiso 1 1 calc R . . 
C30 C 0.0657(5) 0.8646(4) 0.6134(4) 0.0255(8) Uani 1 1 d . . . 
H30 H 0.0286 0.9046 0.5710 0.031 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 
Pd C1 2.048(4) . ? 
Pd N1 2.071(3) . ? 
Pd N2 2.123(3) . ? 
Pd Br 2.4335(5) . ? 
O1 C2 1.343(5) . ? 
O1 C3 1.450(5) . ? 
O2 C5 1.377(5) . ? 
O2 C1 1.418(4) . ? 
O3 C14 1.340(5) . ? 
O3 C15 1.456(5) . ? 
O4 C2 1.209(5) . ? 
O5 C14 1.216(5) . ? 
N1 C21 1.332(5) . ? 
N1 C25 1.359(5) . ? 
N2 C30 1.341(5) . ? 
N2 C26 1.357(5) . ? 
C1 C2 1.494(5) . ? 
C3 C4 1.491(7) . ? 
C5 C6 1.382(5) . ? 
C5 C10 1.404(6) . ? 
C6 C7 1.395(6) . ? 
C7 C8 1.384(6) . ? 
C8 C9 1.388(6) . ? 
C9 C10 1.385(6) . ? 
C10 C11 1.519(6) . ? 
C11 C12 1.495(5) . ? 
C12 C13 1.331(6) . ? 
C13 C14 1.468(6) . ? 
C21 C22 1.377(5) . ? 
C22 C23 1.368(6) . ? 
C23 C24 1.371(6) . ? 
C24 C25 1.387(5) . ? 
C25 C26 1.491(6) . ? 
C26 C27 1.393(6) . ? 
C27 C28 1.375(6) . ? 
C28 C29 1.390(6) . ? 
C29 C30 1.378(6) . ? 
  
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 
C1 Pd N1 98.67(14) . . ? 
C1 Pd N2 174.20(14) . . ? 
N1 Pd N2 79.17(13) . . ? 
C1 Pd Br 86.83(10) . . ? 
N1 Pd Br 174.47(10) . . ? 
N2 Pd Br 95.40(9) . . ? 
C2 O1 C3 115.2(3) . . ? 
C5 O2 C1 118.8(3) . . ? 
C14 O3 C15 115.4(3) . . ? 
C21 N1 C25 118.0(3) . . ? 
C21 N1 Pd 127.0(3) . . ? 
C25 N1 Pd 114.9(3) . . ? 
C30 N2 C26 118.6(4) . . ? 
C30 N2 Pd 127.2(3) . . ? 
C26 N2 Pd 113.9(3) . . ? 
O2 C1 C2 106.0(3) . . ? 
O2 C1 Pd 118.0(2) . . ? 
C2 C1 Pd 101.8(2) . . ? 
O4 C2 O1 124.3(4) . . ? 
O4 C2 C1 125.2(4) . . ? 
O1 C2 C1 110.4(3) . . ? 
O1 C3 C4 108.8(4) . . ? 
O2 C5 C6 124.0(4) . . ? 
O2 C5 C10 115.0(3) . . ? 
C6 C5 C10 121.0(4) . . ? 
C5 C6 C7 120.0(4) . . ? 
C8 C7 C6 119.6(4) . . ? 
C7 C8 C9 119.7(4) . . ? 
C10 C9 C8 121.8(4) . . ? 
C9 C10 C5 117.7(4) . . ? 
C9 C10 C11 121.7(4) . . ? 
C5 C10 C11 120.4(4) . . ? 
C12 C11 C10 111.6(3) . . ? 
C13 C12 C11 125.1(4) . . ? 
C12 C13 C14 120.0(4) . . ? 
O5 C14 O3 122.5(4) . . ? 
O5 C14 C13 125.5(4) . . ? 
O3 C14 C13 112.0(4) . . ? 
N1 C21 C22 122.7(4) . . ? 
C23 C22 C21 119.4(4) . . ? 
C22 C23 C24 119.0(4) . . ? 
C23 C24 C25 119.4(4) . . ? 
N1 C25 C24 121.4(4) . . ? 
N1 C25 C26 116.5(3) . . ? 
C24 C25 C26 122.1(4) . . ? 
N2 C26 C27 121.3(4) . . ? 
N2 C26 C25 115.1(4) . . ? 
C27 C26 C25 123.6(4) . . ? 
C28 C27 C26 119.6(4) . . ? 
C27 C28 C29 118.6(4) . . ? 
C30 C29 C28 119.3(4) . . ? 
N2 C30 C29 122.4(4) . . ? 
  
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 
C1 Pd N1 C21 -9.6(3) . . . . ? 
N2 Pd N1 C21 175.9(3) . . . . ? 
Br Pd N1 C21 164.9(8) . . . . ? 
C1 Pd N1 C25 171.0(3) . . . . ? 
N2 Pd N1 C25 -3.5(3) . . . . ? 
Br Pd N1 C25 -14.6(11) . . . . ? 
C1 Pd N2 C30 111.5(13) . . . . ? 
N1 Pd N2 C30 -179.9(3) . . . . ? 
Br Pd N2 C30 -0.9(3) . . . . ? 
C1 Pd N2 C26 -62.7(14) . . . . ? 
N1 Pd N2 C26 6.0(3) . . . . ? 
Br Pd N2 C26 -175.1(3) . . . . ? 
C5 O2 C1 C2 -166.7(3) . . . . ? 
C5 O2 C1 Pd 80.2(4) . . . . ? 
N1 Pd C1 O2 41.2(3) . . . . ? 
N2 Pd C1 O2 109.0(13) . . . . ? 
Br Pd C1 O2 -138.2(3) . . . . ? 
N1 Pd C1 C2 -74.2(3) . . . . ? 
N2 Pd C1 C2 -6.4(15) . . . . ? 
Br Pd C1 C2 106.4(2) . . . . ? 
C3 O1 C2 O4 -10.9(6) . . . . ? 
C3 O1 C2 C1 166.6(3) . . . . ? 
O2 C1 C2 O4 -29.9(5) . . . . ? 
Pd C1 C2 O4 94.1(4) . . . . ? 
O2 C1 C2 O1 152.7(3) . . . . ? 
Pd C1 C2 O1 -83.4(3) . . . . ? 
C2 O1 C3 C4 -87.6(5) . . . . ? 
C1 O2 C5 C6 -20.3(5) . . . . ? 
C1 O2 C5 C10 160.4(3) . . . . ? 
O2 C5 C6 C7 -175.6(3) . . . . ? 
C10 C5 C6 C7 3.6(6) . . . . ? 
C5 C6 C7 C8 -0.2(6) . . . . ? 
C6 C7 C8 C9 -3.0(6) . . . . ? 
C7 C8 C9 C10 2.7(6) . . . . ? 
C8 C9 C10 C5 0.6(6) . . . . ? 
C8 C9 C10 C11 -175.1(4) . . . . ? 
O2 C5 C10 C9 175.5(3) . . . . ? 
C6 C5 C10 C9 -3.8(5) . . . . ? 
O2 C5 C10 C11 -8.7(5) . . . . ? 
C6 C5 C10 C11 172.0(3) . . . . ? 
C9 C10 C11 C12 -78.4(5) . . . . ? 
C5 C10 C11 C12 106.0(4) . . . . ? 
C10 C11 C12 C13 -110.0(5) . . . . ? 
C11 C12 C13 C14 179.3(4) . . . . ? 
C15 O3 C14 O5 2.5(6) . . . . ? 
C15 O3 C14 C13 -179.3(4) . . . . ? 
C12 C13 C14 O5 6.4(7) . . . . ? 
C12 C13 C14 O3 -171.7(4) . . . . ? 
C25 N1 C21 C22 0.0(6) . . . . ? 
Pd N1 C21 C22 -179.4(3) . . . . ? 
N1 C21 C22 C23 -0.9(6) . . . . ? 
C21 C22 C23 C24 0.7(6) . . . . ? 
C22 C23 C24 C25 0.4(6) . . . . ? 
C21 N1 C25 C24 1.2(6) . . . . ? 
Pd N1 C25 C24 -179.4(3) . . . . ? 
C21 N1 C25 C26 -178.7(3) . . . . ? 
Pd N1 C25 C26 0.8(4) . . . . ? 
C23 C24 C25 N1 -1.4(6) . . . . ? 
C23 C24 C25 C26 178.5(4) . . . . ? 
C30 N2 C26 C27 -1.6(6) . . . . ? 
Pd N2 C26 C27 173.1(3) . . . . ? 
C30 N2 C26 C25 178.0(3) . . . . ? 
Pd N2 C26 C25 -7.3(4) . . . . ? 
N1 C25 C26 N2 4.5(5) . . . . ? 
C24 C25 C26 N2 -175.4(3) . . . . ? 
N1 C25 C26 C27 -175.9(4) . . . . ? 
C24 C25 C26 C27 4.2(6) . . . . ? 
N2 C26 C27 C28 -0.1(6) . . . . ? 
C25 C26 C27 C28 -179.7(4) . . . . ? 
C26 C27 C28 C29 1.6(7) . . . . ? 
C27 C28 C29 C30 -1.4(7) . . . . ? 
C26 N2 C30 C29 1.9(6) . . . . ? 
Pd N2 C30 C29 -172.0(3) . . . . ? 
C28 C29 C30 N2 -0.4(7) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.966 
_diffrn_reflns_theta_full              30.60 
_diffrn_measured_fraction_theta_full   0.966 
_refine_diff_density_max    1.404 
_refine_diff_density_min   -1.058 
_refine_diff_density_rms    0.154 
 
#====================
_publ_contact_author 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
_publ_contact_author_email      hmalinakova@ku.edu 
_publ_contact_author_fax        1(785)8645396 
_publ_contact_author_phone      1(785)8644743 
 
_publ_requested_journal         'Organometallics'  
 
loop_ 
    _publ_author_name 
    _publ_author_address 
   'Guo, Ruiyun' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Portscheller, Jannelle L.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Day, Victor W.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Malinakova, Helena C.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
;  
_publ_section_title 
; 
 article title here 
 Allylpalladium(IV) Intermediate inthe Synthesis of Highly Substituted 
 Benzoxepines and Benzopyrans via Reactions of Stable Palla(II)cycles 
 with Allyl Bromides  
; 
_publ_section_references 
;
  Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
 
  Flack, H. D. (1983) Acta Cryst. A39, 876-881. 
 
  Flack, H. D. and Schwarzenbach, D. (1988) Acta Cryst. A44, 
  499-506. 
 
  Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
;
_publ_section_acknowledgements 
; 
 The authors wish to thank the National Science Foundation 
 (CHE-0079282) and the University of Kansas for funds to 
 acquire the diffractometer and computers used in this work.  
;    
data_k63c(12-polymorph1) 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C27 H29 Br N2 O6 Pd' 
_chemical_formula_weight          663.83 
  
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' 
 '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            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    22.264(6) 
_cell_length_b                    15.392(4) 
_cell_length_c                    15.987(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  100.678(7) 
_cell_angle_gamma                 90.00 
_cell_volume                      5384(3) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     530 
_cell_measurement_theta_min       2.45 
_cell_measurement_theta_max       15.75 
  
_exptl_crystal_description        Rectangular 
_exptl_crystal_colour             'Pale yellow' 
_exptl_crystal_size_max           0.12 
_exptl_crystal_size_mid           0.08 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.638 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2672 
_exptl_absorpt_coefficient_mu     2.217 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.903 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       100(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 SMART 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_%         0.00 
_diffrn_reflns_number             34479 
_diffrn_reflns_av_R_equivalents   0.2432 
_diffrn_reflns_av_sigmaI/netI     0.1954 
_diffrn_reflns_limit_h_min        -23 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          2.28 
_diffrn_reflns_theta_max          22.50 
_reflns_number_total              7034 
_reflns_number_gt                 3417 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections except 5 which were flagged
 by the user for possible systematic errors.  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)+(0.0541P)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_number_reflns          7034 
_refine_ls_number_parameters      667 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.1692 
_refine_ls_R_factor_gt            0.0734 
_refine_ls_wR_factor_ref          0.1536 
_refine_ls_wR_factor_gt           0.1298 
_refine_ls_goodness_of_fit_ref    0.903 
_refine_ls_restrained_S_all       0.903 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pd1 Pd 0.09913(5) 0.26458(7) 0.50837(6) 0.0293(3) Uani 1 1 d . . . 
Br1 Br -0.01066(6) 0.26319(9) 0.41683(9) 0.0353(4) Uani 1 1 d . . . 
O1 O 0.2020(4) 0.1624(6) 0.5936(5) 0.034(2) Uani 1 1 d . . . 
O2 O 0.2039(4) 0.3851(6) 0.6509(5) 0.031(2) Uani 1 1 d . . . 
O3 O 0.1850(4) 0.2658(6) 0.7276(6) 0.037(2) Uani 1 1 d . . . 
O4 O 0.0960(5) -0.0668(6) 0.3584(6) 0.049(3) Uani 1 1 d . . . 
O5 O 0.1896(5) -0.1054(7) 0.4212(7) 0.070(4) Uani 1 1 d . . . 
N1 N 0.0656(4) 0.3479(7) 0.5999(7) 0.025(3) Uani 1 1 d . . . 
N2 N 0.1100(5) 0.3935(7) 0.4635(6) 0.031(3) Uani 1 1 d . . . 
C1 C 0.1501(6) 0.1155(9) 0.6014(8) 0.026(3) Uani 1 1 d . . . 
C2 C 0.0943(7) 0.1496(8) 0.5653(8) 0.030(4) Uani 1 1 d . . . 
C3 C 0.0433(6) 0.0998(10) 0.5677(8) 0.031(4) Uani 1 1 d . . . 
H3 H 0.0037 0.1207 0.5439 0.037 Uiso 1 1 calc R . . 
C4 C 0.0511(8) 0.0172(9) 0.6062(8) 0.038(4) Uani 1 1 d . . . 
H4 H 0.0161 -0.0181 0.6063 0.045 Uiso 1 1 calc R . . 
C5 C 0.1062(7) -0.0135(10) 0.6427(9) 0.038(4) Uani 1 1 d . . . 
H5 H 0.1099 -0.0685 0.6701 0.045 Uiso 1 1 calc R . . 
C6 C 0.1564(7) 0.0351(10) 0.6399(9) 0.037(4) Uani 1 1 d . . . 
H6 H 0.1958 0.0138 0.6643 0.045 Uiso 1 1 calc R . . 
C7 C 0.1853(6) 0.2526(9) 0.5761(8) 0.031(4) Uani 1 1 d . . . 
H7 H 0.2145 0.2791 0.5429 0.038 Uiso 1 1 calc R . . 
C8 C 0.1915(6) 0.2993(10) 0.6614(9) 0.030(4) Uani 1 1 d . . . 
C9 C 0.2069(7) 0.4374(9) 0.7276(8) 0.042(4) Uani 1 1 d . . . 
H9A H 0.2384 0.4138 0.7740 0.050 Uiso 1 1 calc R . . 
H9B H 0.1670 0.4363 0.7465 0.050 Uiso 1 1 calc R . . 
C10 C 0.2228(7) 0.5285(9) 0.7074(9) 0.049(5) Uani 1 1 d . . . 
H10A H 0.2249 0.5649 0.7582 0.074 Uiso 1 1 calc R . . 
H10B H 0.1914 0.5513 0.6615 0.074 Uiso 1 1 calc R . . 
H10C H 0.2625 0.5290 0.6892 0.074 Uiso 1 1 calc R . . 
C11 C 0.1309(6) 0.2000(9) 0.4110(8) 0.032(4) Uani 1 1 d . . . 
H11A H 0.1130 0.2286 0.3566 0.038 Uiso 1 1 calc R . . 
H11B H 0.1757 0.2085 0.4196 0.038 Uiso 1 1 calc R . . 
C12 C 0.1188(7) 0.1069(10) 0.4012(8) 0.038(4) Uani 1 1 d . . . 
H12 H 0.0777 0.0887 0.3833 0.045 Uiso 1 1 calc R . . 
C13 C 0.1626(7) 0.0452(10) 0.4160(8) 0.040(4) Uani 1 1 d . . . 
H13 H 0.2031 0.0641 0.4376 0.049 Uiso 1 1 calc R . . 
C14 C 0.1532(8) -0.0480(12) 0.4020(11) 0.052(5) Uani 1 1 d . . . 
C15 C 0.0818(8) -0.1576(9) 0.3368(10) 0.067(5) Uani 1 1 d . . . 
H15A H 0.0396 -0.1622 0.3059 0.100 Uiso 1 1 calc R . . 
H15B H 0.0865 -0.1922 0.3891 0.100 Uiso 1 1 calc R . . 
H15C H 0.1097 -0.1795 0.3010 0.100 Uiso 1 1 calc R . . 
C16 C 0.0401(6) 0.3165(10) 0.6625(8) 0.033(4) Uani 1 1 d . . . 
H16 H 0.0389 0.2556 0.6715 0.040 Uiso 1 1 calc R . . 
C17 C 0.0156(6) 0.3724(10) 0.7142(8) 0.034(4) Uani 1 1 d . . . 
H17 H -0.0004 0.3506 0.7611 0.041 Uiso 1 1 calc R . . 
C18 C 0.0144(6) 0.4616(9) 0.6975(9) 0.033(4) Uani 1 1 d . . . 
H18 H -0.0039 0.5007 0.7315 0.040 Uiso 1 1 calc R . . 
C19 C 0.0403(6) 0.4922(10) 0.6310(9) 0.036(4) Uani 1 1 d . . . 
H19 H 0.0405 0.5526 0.6188 0.043 Uiso 1 1 calc R . . 
C20 C 0.0655(6) 0.4333(10) 0.5829(9) 0.032(4) Uani 1 1 d . . . 
C21 C 0.0935(6) 0.4608(9) 0.5092(8) 0.026(3) Uani 1 1 d . . . 
C22 C 0.0996(6) 0.5479(9) 0.4901(8) 0.032(4) Uani 1 1 d . . . 
H22 H 0.0843 0.5926 0.5213 0.039 Uiso 1 1 calc R . . 
C23 C 0.1292(6) 0.5666(10) 0.4231(9) 0.040(4) Uani 1 1 d . . . 
H23 H 0.1381 0.6250 0.4106 0.049 Uiso 1 1 calc R . . 
C24 C 0.1459(6) 0.4976(11) 0.3735(8) 0.031(4) Uani 1 1 d . . . 
H24 H 0.1641 0.5098 0.3255 0.037 Uiso 1 1 calc R . . 
C25 C 0.1361(6) 0.4151(11) 0.3943(9) 0.041(4) Uani 1 1 d . . . 
H25 H 0.1476 0.3698 0.3601 0.049 Uiso 1 1 calc R . . 
Pd2 Pd 0.37692(5) 0.32269(7) 0.36270(7) 0.0315(3) Uani 1 1 d . . . 
Br2 Br 0.47417(7) 0.37657(11) 0.31376(10) 0.0463(5) Uani 1 1 d . . . 
O21 O 0.2689(4) 0.3527(6) 0.4343(6) 0.037(3) Uani 1 1 d . . . 
O22 O 0.3184(4) 0.1362(6) 0.4347(5) 0.028(2) Uani 1 1 d . . . 
O23 O 0.3253(4) 0.2296(6) 0.5466(5) 0.040(3) Uani 1 1 d . . . 
O24 O 0.3603(5) 0.6764(8) 0.2109(7) 0.060(3) Uani 1 1 d . . . 
O25 O 0.3971(5) 0.5767(6) 0.1301(6) 0.048(3) Uani 1 1 d . . . 
N21 N 0.4409(5) 0.2536(8) 0.4599(7) 0.037(3) Uani 1 1 d . . . 
N22 N 0.3934(5) 0.2030(7) 0.3014(7) 0.032(3) Uani 1 1 d . . . 
C31 C 0.3058(6) 0.4241(10) 0.4578(8) 0.031(4) Uani 1 1 d . . . 
C32 C 0.3618(6) 0.4241(9) 0.4296(8) 0.030(4) Uani 1 1 d . . . 
C33 C 0.3990(7) 0.4944(10) 0.4538(9) 0.038(4) Uani 1 1 d . . . 
H33 H 0.4373 0.4976 0.4359 0.045 Uiso 1 1 calc R . . 
C34 C 0.3822(7) 0.5619(10) 0.5044(10) 0.044(4) Uani 1 1 d . . . 
H34 H 0.4091 0.6092 0.5216 0.052 Uiso 1 1 calc R . . 
C35 C 0.3263(7) 0.5580(9) 0.5283(8) 0.040(4) Uani 1 1 d . . . 
H35 H 0.3139 0.6045 0.5602 0.048 Uiso 1 1 calc R . . 
C36 C 0.2881(7) 0.4893(9) 0.5077(8) 0.034(4) Uani 1 1 d . . . 
H36 H 0.2503 0.4861 0.5270 0.041 Uiso 1 1 calc R . . 
C37 C 0.2977(6) 0.2834(8) 0.4010(8) 0.027(3) Uani 1 1 d . . . 
H37 H 0.2692 0.2577 0.3515 0.033 Uiso 1 1 calc R . . 
C38 C 0.3156(5) 0.2140(10) 0.4693(10) 0.033(4) Uani 1 1 d . . . 
C39 C 0.3368(6) 0.0641(9) 0.4924(8) 0.038(4) Uani 1 1 d . . . 
H39A H 0.3074 0.0563 0.5312 0.046 Uiso 1 1 calc R . . 
H39B H 0.3779 0.0748 0.5269 0.046 Uiso 1 1 calc R . . 
C40 C 0.3376(6) -0.0137(9) 0.4381(9) 0.042(4) Uani 1 1 d . . . 
H40A H 0.3496 -0.0646 0.4742 0.063 Uiso 1 1 calc R . . 
H40B H 0.3670 -0.0050 0.4003 0.063 Uiso 1 1 calc R . . 
H40C H 0.2968 -0.0230 0.4040 0.063 Uiso 1 1 calc R . . 
C41 C 0.3146(6) 0.3806(9) 0.2669(8) 0.040(4) Uani 1 1 d . . . 
H41A H 0.2967 0.3357 0.2253 0.048 Uiso 1 1 calc R . . 
H41B H 0.2811 0.4064 0.2916 0.048 Uiso 1 1 calc R . . 
C42 C 0.3431(6) 0.4487(10) 0.2226(8) 0.031(4) Uani 1 1 d . . . 
H42 H 0.3687 0.4299 0.1846 0.037 Uiso 1 1 calc R . . 
C43 C 0.3367(6) 0.5305(10) 0.2302(9) 0.037(4) Uani 1 1 d . . . 
H43 H 0.3104 0.5502 0.2667 0.044 Uiso 1 1 calc R . . 
C44 C 0.3671(7) 0.5956(12) 0.1870(10) 0.044(4) Uani 1 1 d . . . 
C45 C 0.3894(8) 0.7410(10) 0.1667(11) 0.066(5) Uani 1 1 d . . . 
H45A H 0.3818 0.7988 0.1881 0.099 Uiso 1 1 calc R . . 
H45B H 0.3727 0.7379 0.1056 0.099 Uiso 1 1 calc R . . 
H45C H 0.4335 0.7300 0.1764 0.099 Uiso 1 1 calc R . . 
C46 C 0.4608(7) 0.2809(9) 0.5389(10) 0.042(4) Uani 1 1 d . . . 
H46 H 0.4450 0.3338 0.5566 0.050 Uiso 1 1 calc R . . 
C47 C 0.5036(7) 0.2356(11) 0.5968(10) 0.051(4) Uani 1 1 d . . . 
H47 H 0.5162 0.2571 0.6530 0.061 Uiso 1 1 calc R . . 
C48 C 0.5268(7) 0.1619(12) 0.5731(11) 0.060(5) Uani 1 1 d . . . 
H48 H 0.5561 0.1303 0.6122 0.072 Uiso 1 1 calc R . . 
C49 C 0.5079(6) 0.1320(10) 0.4920(8) 0.041(4) Uani 1 1 d . . . 
H49 H 0.5254 0.0808 0.4735 0.049 Uiso 1 1 calc R . . 
C50 C 0.4622(6) 0.1776(10) 0.4356(8) 0.035(4) Uani 1 1 d . . . 
C51 C 0.4375(6) 0.1520(9) 0.3482(9) 0.031(4) Uani 1 1 d . . . 
C52 C 0.4556(6) 0.0763(10) 0.3117(10) 0.042(4) Uani 1 1 d . . . 
H52 H 0.4858 0.0399 0.3439 0.051 Uiso 1 1 calc R . . 
C53 C 0.4302(7) 0.0541(10) 0.2298(10) 0.047(4) Uani 1 1 d . . . 
H53 H 0.4442 0.0039 0.2045 0.057 Uiso 1 1 calc R . . 
C54 C 0.3846(7) 0.1042(11) 0.1840(9) 0.046(4) Uani 1 1 d . . . 
H54 H 0.3652 0.0874 0.1283 0.055 Uiso 1 1 calc R . . 
C55 C 0.3669(7) 0.1812(11) 0.2210(8) 0.045(4) Uani 1 1 d . . . 
H55 H 0.3365 0.2177 0.1895 0.054 Uiso 1 1 calc R . . 
O1S O 0.2354(5) 0.7393(8) 0.7137(9) 0.081(4) Uani 1 1 d . . . 
O2S O 0.2881(9) 0.7479(12) 0.8586(11) 0.162(7) Uani 1 1 d . . . 
C1S C 0.2017(7) 0.8409(9) 0.7862(9) 0.044(4) Uani 1 1 d U . . 
H1SA H 0.1776 0.8490 0.7289 0.066 Uiso 1 1 calc R . . 
H1SB H 0.2226 0.8952 0.8056 0.066 Uiso 1 1 calc R . . 
H1SC H 0.1746 0.8243 0.8253 0.066 Uiso 1 1 calc R . . 
C2S C 0.2393(8) 0.7839(14) 0.7846(14) 0.069(6) Uani 1 1 d . . . 
C3S C 0.1924(8) 0.7738(13) 0.6342(13) 0.077(6) Uani 1 1 d . . . 
H3SA H 0.1495 0.7584 0.6365 0.093 Uiso 1 1 calc R . . 
H3SB H 0.1955 0.8379 0.6313 0.093 Uiso 1 1 calc R . . 
C4S C 0.2092(12) 0.7372(16) 0.5653(15) 0.141(10) Uani 1 1 d . . . 
H4SA H 0.1824 0.7581 0.5136 0.211 Uiso 1 1 calc R . . 
H4SB H 0.2058 0.6738 0.5687 0.211 Uiso 1 1 calc R . . 
H4SC H 0.2516 0.7529 0.5636 0.211 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 C2 2.002(13) . ? 
Pd1 C7 2.029(12) . ? 
Pd1 C11 2.079(12) . ? 
Pd1 N2 2.139(11) . ? 
Pd1 N1 2.179(10) . ? 
Pd1 Br1 2.6060(18) . ? 
O1 C1 1.387(14) . ? 
O1 C7 1.451(15) . ? 
O2 C8 1.367(15) . ? 
O2 C9 1.458(14) . ? 
O3 C8 1.209(14) . ? 
O4 C14 1.365(18) . ? 
O4 C15 1.460(15) . ? 
O5 C14 1.200(17) . ? 
N1 C16 1.330(15) . ? 
N1 C20 1.342(16) . ? 
N2 C21 1.358(15) . ? 
N2 C25 1.383(16) . ? 
C1 C2 1.374(17) . ? 
C1 C6 1.378(17) . ? 
C2 C3 1.376(17) . ? 
C3 C4 1.410(17) . ? 
C4 C5 1.343(18) . ? 
C5 C6 1.351(18) . ? 
C7 C8 1.525(17) . ? 
C9 C10 1.496(18) . ? 
C11 C12 1.460(17) . ? 
C12 C13 1.350(18) . ? 
C13 C14 1.46(2) . ? 
C16 C17 1.374(17) . ? 
C17 C18 1.398(17) . ? 
C18 C19 1.382(17) . ? 
C19 C20 1.375(18) . ? 
C20 C21 1.492(18) . ? 
C21 C22 1.387(17) . ? 
C22 C23 1.387(18) . ? 
C23 C24 1.414(18) . ? 
C24 C25 1.341(17) . ? 
Pd2 C32 1.957(14) . ? 
Pd2 C37 2.061(12) . ? 
Pd2 C41 2.067(12) . ? 
Pd2 N22 2.150(11) . ? 
Pd2 N21 2.180(11) . ? 
Pd2 Br2 2.5721(19) . ? 
O21 C31 1.380(15) . ? 
O21 C37 1.400(14) . ? 
O22 C38 1.325(15) . ? 
O22 C39 1.453(14) . ? 
O23 C38 1.239(15) . ? 
O24 C44 1.317(17) . ? 
O24 C45 1.441(16) . ? 
O25 C44 1.258(17) . ? 
N21 C46 1.328(16) . ? 
N21 C50 1.347(16) . ? 
N22 C55 1.353(15) . ? 
N22 C51 1.367(16) . ? 
C31 C36 1.384(18) . ? 
C31 C32 1.401(17) . ? 
C32 C33 1.375(18) . ? 
C33 C34 1.410(19) . ? 
C34 C35 1.368(18) . ? 
C35 C36 1.359(17) . ? 
C37 C38 1.525(18) . ? 
C39 C40 1.480(17) . ? 
C41 C42 1.473(18) . ? 
C42 C43 1.275(17) . ? 
C43 C44 1.454(19) . ? 
C46 C47 1.387(19) . ? 
C47 C48 1.331(19) . ? 
C48 C49 1.367(19) . ? 
C49 C50 1.415(17) . ? 
C50 C51 1.457(18) . ? 
C51 C52 1.396(18) . ? 
C52 C53 1.371(18) . ? 
C53 C54 1.374(19) . ? 
C54 C55 1.413(19) . ? 
O1S C2S 1.32(2) . ? 
O1S C3S 1.54(2) . ? 
O2S C2S 1.55(2) . ? 
C1S C2S 1.22(2) . ? 
C3S C4S 1.35(3) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 Pd1 C7 78.6(6) . . ? 
C2 Pd1 C11 88.4(5) . . ? 
C7 Pd1 C11 86.4(5) . . ? 
C2 Pd1 N2 172.5(5) . . ? 
C7 Pd1 N2 96.2(5) . . ? 
C11 Pd1 N2 96.7(5) . . ? 
C2 Pd1 N1 99.3(5) . . ? 
C7 Pd1 N1 95.9(4) . . ? 
C11 Pd1 N1 172.3(5) . . ? 
N2 Pd1 N1 75.7(4) . . ? 
C2 Pd1 Br1 97.1(4) . . ? 
C7 Pd1 Br1 174.1(4) . . ? 
C11 Pd1 Br1 89.4(4) . . ? 
N2 Pd1 Br1 88.4(3) . . ? 
N1 Pd1 Br1 88.8(3) . . ? 
C1 O1 C7 109.1(10) . . ? 
C8 O2 C9 114.1(10) . . ? 
C14 O4 C15 117.7(13) . . ? 
C16 N1 C20 121.5(12) . . ? 
C16 N1 Pd1 122.6(10) . . ? 
C20 N1 Pd1 115.4(10) . . ? 
C21 N2 C25 116.3(12) . . ? 
C21 N2 Pd1 117.9(9) . . ? 
C25 N2 Pd1 125.6(10) . . ? 
C2 C1 C6 122.7(13) . . ? 
C2 C1 O1 117.8(12) . . ? 
C6 C1 O1 119.4(13) . . ? 
C1 C2 C3 117.5(13) . . ? 
C1 C2 Pd1 114.1(11) . . ? 
C3 C2 Pd1 128.3(11) . . ? 
C2 C3 C4 118.7(13) . . ? 
C5 C4 C3 122.3(15) . . ? 
C4 C5 C6 119.1(15) . . ? 
C5 C6 C1 119.7(14) . . ? 
O1 C7 C8 107.5(10) . . ? 
O1 C7 Pd1 111.9(8) . . ? 
C8 C7 Pd1 110.8(9) . . ? 
O3 C8 O2 125.4(13) . . ? 
O3 C8 C7 125.2(14) . . ? 
O2 C8 C7 109.4(12) . . ? 
O2 C9 C10 108.1(11) . . ? 
C12 C11 Pd1 117.9(9) . . ? 
C13 C12 C11 123.9(15) . . ? 
C12 C13 C14 125.8(15) . . ? 
O5 C14 O4 119.8(17) . . ? 
O5 C14 C13 127.8(18) . . ? 
O4 C14 C13 112.3(15) . . ? 
N1 C16 C17 119.8(14) . . ? 
C16 C17 C18 119.8(14) . . ? 
C19 C18 C17 119.0(13) . . ? 
C20 C19 C18 118.6(14) . . ? 
N1 C20 C19 121.2(13) . . ? 
N1 C20 C21 116.9(13) . . ? 
C19 C20 C21 121.9(14) . . ? 
N2 C21 C22 124.8(13) . . ? 
N2 C21 C20 113.8(13) . . ? 
C22 C21 C20 121.4(13) . . ? 
C21 C22 C23 116.8(14) . . ? 
C22 C23 C24 119.3(14) . . ? 
C25 C24 C23 120.0(14) . . ? 
C24 C25 N2 122.5(15) . . ? 
C32 Pd2 C37 80.1(5) . . ? 
C32 Pd2 C41 84.3(5) . . ? 
C37 Pd2 C41 81.6(5) . . ? 
C32 Pd2 N22 173.8(5) . . ? 
C37 Pd2 N22 96.4(5) . . ? 
C41 Pd2 N22 100.3(5) . . ? 
C32 Pd2 N21 98.9(5) . . ? 
C37 Pd2 N21 97.3(5) . . ? 
C41 Pd2 N21 176.3(5) . . ? 
N22 Pd2 N21 76.3(4) . . ? 
C32 Pd2 Br2 98.6(4) . . ? 
C37 Pd2 Br2 178.2(4) . . ? 
C41 Pd2 Br2 97.0(4) . . ? 
N22 Pd2 Br2 85.0(3) . . ? 
N21 Pd2 Br2 84.2(3) . . ? 
C31 O21 C37 114.8(10) . . ? 
C38 O22 C39 117.0(10) . . ? 
C44 O24 C45 114.9(13) . . ? 
C46 N21 C50 118.5(12) . . ? 
C46 N21 Pd2 125.6(11) . . ? 
C50 N21 Pd2 115.9(8) . . ? 
C55 N22 C51 121.3(13) . . ? 
C55 N22 Pd2 124.4(10) . . ? 
C51 N22 Pd2 114.1(9) . . ? 
O21 C31 C36 121.0(13) . . ? 
O21 C31 C32 115.6(14) . . ? 
C36 C31 C32 123.4(13) . . ? 
C33 C32 C31 115.9(14) . . ? 
C33 C32 Pd2 128.7(12) . . ? 
C31 C32 Pd2 115.4(10) . . ? 
C32 C33 C34 122.0(14) . . ? 
C35 C34 C33 118.7(14) . . ? 
C36 C35 C34 121.9(14) . . ? 
C35 C36 C31 118.1(14) . . ? 
O21 C37 C38 109.8(11) . . ? 
O21 C37 Pd2 111.5(8) . . ? 
C38 C37 Pd2 107.1(8) . . ? 
O23 C38 O22 125.4(13) . . ? 
O23 C38 C37 123.5(14) . . ? 
O22 C38 C37 111.1(12) . . ? 
O22 C39 C40 106.2(11) . . ? 
C42 C41 Pd2 112.0(9) . . ? 
C43 C42 C41 126.2(14) . . ? 
C42 C43 C44 124.4(15) . . ? 
O25 C44 O24 122.3(15) . . ? 
O25 C44 C43 122.7(16) . . ? 
O24 C44 C43 115.1(15) . . ? 
N21 C46 C47 122.8(14) . . ? 
C48 C47 C46 119.6(15) . . ? 
C47 C48 C49 119.3(15) . . ? 
C48 C49 C50 119.8(14) . . ? 
N21 C50 C49 119.8(12) . . ? 
N21 C50 C51 114.9(12) . . ? 
C49 C50 C51 125.2(14) . . ? 
N22 C51 C52 119.0(13) . . ? 
N22 C51 C50 118.4(13) . . ? 
C52 C51 C50 122.6(13) . . ? 
C53 C52 C51 120.5(14) . . ? 
C52 C53 C54 120.1(15) . . ? 
C53 C54 C55 118.9(14) . . ? 
N22 C55 C54 120.0(15) . . ? 
C2S O1S C3S 117.6(15) . . ? 
C1S C2S O1S 117(2) . . ? 
C1S C2S O2S 129(2) . . ? 
O1S C2S O2S 113.3(19) . . ? 
C4S C3S O1S 107.7(16) . . ? 
  
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 
C2 Pd1 N1 C16 -10.8(11) . . . . ? 
C7 Pd1 N1 C16 -90.1(10) . . . . ? 
C11 Pd1 N1 C16 163(3) . . . . ? 
N2 Pd1 N1 C16 174.9(10) . . . . ? 
Br1 Pd1 N1 C16 86.3(9) . . . . ? 
C2 Pd1 N1 C20 176.9(9) . . . . ? 
C7 Pd1 N1 C20 97.5(9) . . . . ? 
C11 Pd1 N1 C20 -9(4) . . . . ? 
N2 Pd1 N1 C20 2.6(8) . . . . ? 
Br1 Pd1 N1 C20 -86.1(8) . . . . ? 
C2 Pd1 N2 C21 -48(4) . . . . ? 
C7 Pd1 N2 C21 -93.6(10) . . . . ? 
C11 Pd1 N2 C21 179.3(9) . . . . ? 
N1 Pd1 N2 C21 0.9(9) . . . . ? 
Br1 Pd1 N2 C21 90.1(9) . . . . ? 
C2 Pd1 N2 C25 128(4) . . . . ? 
C7 Pd1 N2 C25 82.2(11) . . . . ? 
C11 Pd1 N2 C25 -4.9(11) . . . . ? 
N1 Pd1 N2 C25 176.7(11) . . . . ? 
Br1 Pd1 N2 C25 -94.1(10) . . . . ? 
C7 O1 C1 C2 21.2(15) . . . . ? 
C7 O1 C1 C6 -162.7(11) . . . . ? 
C6 C1 C2 C3 -1(2) . . . . ? 
O1 C1 C2 C3 175.2(11) . . . . ? 
C6 C1 C2 Pd1 -176.8(10) . . . . ? 
O1 C1 C2 Pd1 -0.8(15) . . . . ? 
C7 Pd1 C2 C1 -13.5(9) . . . . ? 
C11 Pd1 C2 C1 73.2(10) . . . . ? 
N2 Pd1 C2 C1 -60(4) . . . . ? 
N1 Pd1 C2 C1 -107.7(9) . . . . ? 
Br1 Pd1 C2 C1 162.4(9) . . . . ? 
C7 Pd1 C2 C3 171.0(13) . . . . ? 
C11 Pd1 C2 C3 -102.4(12) . . . . ? 
N2 Pd1 C2 C3 124(4) . . . . ? 
N1 Pd1 C2 C3 76.8(12) . . . . ? 
Br1 Pd1 C2 C3 -13.2(12) . . . . ? 
C1 C2 C3 C4 -0.4(18) . . . . ? 
Pd1 C2 C3 C4 175.1(9) . . . . ? 
C2 C3 C4 C5 2.0(19) . . . . ? 
C3 C4 C5 C6 -2(2) . . . . ? 
C4 C5 C6 C1 1(2) . . . . ? 
C2 C1 C6 C5 0(2) . . . . ? 
O1 C1 C6 C5 -175.7(12) . . . . ? 
C1 O1 C7 C8 90.4(11) . . . . ? 
C1 O1 C7 Pd1 -31.5(11) . . . . ? 
C2 Pd1 C7 O1 24.7(8) . . . . ? 
C11 Pd1 C7 O1 -64.4(9) . . . . ? 
N2 Pd1 C7 O1 -160.8(8) . . . . ? 
N1 Pd1 C7 O1 123.0(8) . . . . ? 
Br1 Pd1 C7 O1 -19(4) . . . . ? 
C2 Pd1 C7 C8 -95.2(10) . . . . ? 
C11 Pd1 C7 C8 175.7(11) . . . . ? 
N2 Pd1 C7 C8 79.3(10) . . . . ? 
N1 Pd1 C7 C8 3.1(10) . . . . ? 
Br1 Pd1 C7 C8 -139(3) . . . . ? 
C9 O2 C8 O3 -2.0(18) . . . . ? 
C9 O2 C8 C7 176.2(10) . . . . ? 
O1 C7 C8 O3 -29.2(17) . . . . ? 
Pd1 C7 C8 O3 93.4(14) . . . . ? 
O1 C7 C8 O2 152.6(10) . . . . ? 
Pd1 C7 C8 O2 -84.8(11) . . . . ? 
C8 O2 C9 C10 178.1(11) . . . . ? 
C2 Pd1 C11 C12 20.2(11) . . . . ? 
C7 Pd1 C11 C12 98.8(11) . . . . ? 
N2 Pd1 C11 C12 -165.3(10) . . . . ? 
N1 Pd1 C11 C12 -154(3) . . . . ? 
Br1 Pd1 C11 C12 -77.0(10) . . . . ? 
Pd1 C11 C12 C13 -112.3(13) . . . . ? 
C11 C12 C13 C14 -175.9(13) . . . . ? 
C15 O4 C14 O5 0(2) . . . . ? 
C15 O4 C14 C13 177.3(12) . . . . ? 
C12 C13 C14 O5 -172.9(16) . . . . ? 
C12 C13 C14 O4 10(2) . . . . ? 
C20 N1 C16 C17 -3.2(18) . . . . ? 
Pd1 N1 C16 C17 -175.0(9) . . . . ? 
N1 C16 C17 C18 3.7(19) . . . . ? 
C16 C17 C18 C19 -2.5(19) . . . . ? 
C17 C18 C19 C20 0.8(19) . . . . ? 
C16 N1 C20 C19 1.4(19) . . . . ? 
Pd1 N1 C20 C19 173.8(10) . . . . ? 
C16 N1 C20 C21 -177.9(11) . . . . ? 
Pd1 N1 C20 C21 -5.5(14) . . . . ? 
C18 C19 C20 N1 0(2) . . . . ? 
C18 C19 C20 C21 179.1(12) . . . . ? 
C25 N2 C21 C22 1.6(18) . . . . ? 
Pd1 N2 C21 C22 177.8(10) . . . . ? 
C25 N2 C21 C20 179.9(11) . . . . ? 
Pd1 N2 C21 C20 -3.9(14) . . . . ? 
N1 C20 C21 N2 6.2(16) . . . . ? 
C19 C20 C21 N2 -173.1(12) . . . . ? 
N1 C20 C21 C22 -175.4(11) . . . . ? 
C19 C20 C21 C22 5.3(19) . . . . ? 
N2 C21 C22 C23 -5.2(19) . . . . ? 
C20 C21 C22 C23 176.6(11) . . . . ? 
C21 C22 C23 C24 6.0(18) . . . . ? 
C22 C23 C24 C25 -3.6(19) . . . . ? 
C23 C24 C25 N2 0(2) . . . . ? 
C21 N2 C25 C24 1.2(19) . . . . ? 
Pd1 N2 C25 C24 -174.6(10) . . . . ? 
C32 Pd2 N21 C46 -1.0(12) . . . . ? 
C37 Pd2 N21 C46 -82.1(12) . . . . ? 
C41 Pd2 N21 C46 -154(8) . . . . ? 
N22 Pd2 N21 C46 -176.9(12) . . . . ? 
Br2 Pd2 N21 C46 96.8(11) . . . . ? 
C32 Pd2 N21 C50 -179.8(10) . . . . ? 
C37 Pd2 N21 C50 99.1(10) . . . . ? 
C41 Pd2 N21 C50 27(8) . . . . ? 
N22 Pd2 N21 C50 4.3(10) . . . . ? 
Br2 Pd2 N21 C50 -82.0(10) . . . . ? 
C32 Pd2 N22 C55 138(4) . . . . ? 
C37 Pd2 N22 C55 83.1(11) . . . . ? 
C41 Pd2 N22 C55 0.5(11) . . . . ? 
N21 Pd2 N22 C55 179.0(11) . . . . ? 
Br2 Pd2 N22 C55 -95.8(10) . . . . ? 
C32 Pd2 N22 C51 -47(5) . . . . ? 
C37 Pd2 N22 C51 -102.1(9) . . . . ? 
C41 Pd2 N22 C51 175.3(9) . . . . ? 
N21 Pd2 N22 C51 -6.1(9) . . . . ? 
Br2 Pd2 N22 C51 79.1(8) . . . . ? 
C37 O21 C31 C36 -166.1(11) . . . . ? 
C37 O21 C31 C32 12.4(15) . . . . ? 
O21 C31 C32 C33 -179.1(11) . . . . ? 
C36 C31 C32 C33 -0.7(19) . . . . ? 
O21 C31 C32 Pd2 -0.2(14) . . . . ? 
C36 C31 C32 Pd2 178.2(10) . . . . ? 
C37 Pd2 C32 C33 171.3(13) . . . . ? 
C41 Pd2 C32 C33 -106.3(12) . . . . ? 
N22 Pd2 C32 C33 115(4) . . . . ? 
N21 Pd2 C32 C33 75.4(12) . . . . ? 
Br2 Pd2 C32 C33 -10.0(12) . . . . ? 
C37 Pd2 C32 C31 -7.5(9) . . . . ? 
C41 Pd2 C32 C31 74.9(10) . . . . ? 
N22 Pd2 C32 C31 -64(5) . . . . ? 
N21 Pd2 C32 C31 -103.4(10) . . . . ? 
Br2 Pd2 C32 C31 171.2(9) . . . . ? 
C31 C32 C33 C34 0.5(19) . . . . ? 
Pd2 C32 C33 C34 -178.2(10) . . . . ? 
C32 C33 C34 C35 -2(2) . . . . ? 
C33 C34 C35 C36 3(2) . . . . ? 
C34 C35 C36 C31 -3(2) . . . . ? 
O21 C31 C36 C35 -179.7(11) . . . . ? 
C32 C31 C36 C35 2(2) . . . . ? 
C31 O21 C37 C38 100.6(12) . . . . ? 
C31 O21 C37 Pd2 -18.0(12) . . . . ? 
C32 Pd2 C37 O21 13.7(8) . . . . ? 
C41 Pd2 C37 O21 -71.9(9) . . . . ? 
N22 Pd2 C37 O21 -171.5(8) . . . . ? 
N21 Pd2 C37 O21 111.6(9) . . . . ? 
Br2 Pd2 C37 O21 -31(12) . . . . ? 
C32 Pd2 C37 C38 -106.4(10) . . . . ? 
C41 Pd2 C37 C38 167.9(10) . . . . ? 
N22 Pd2 C37 C38 68.4(10) . . . . ? 
N21 Pd2 C37 C38 -8.6(10) . . . . ? 
Br2 Pd2 C37 C38 -151(11) . . . . ? 
C39 O22 C38 O23 -2.5(18) . . . . ? 
C39 O22 C38 C37 178.1(10) . . . . ? 
O21 C37 C38 O23 -25.8(17) . . . . ? 
Pd2 C37 C38 O23 95.4(13) . . . . ? 
O21 C37 C38 O22 153.6(10) . . . . ? 
Pd2 C37 C38 O22 -85.2(10) . . . . ? 
C38 O22 C39 C40 -178.7(11) . . . . ? 
C32 Pd2 C41 C42 81.6(11) . . . . ? 
C37 Pd2 C41 C42 162.4(11) . . . . ? 
N22 Pd2 C41 C42 -102.6(10) . . . . ? 
N21 Pd2 C41 C42 -125(8) . . . . ? 
Br2 Pd2 C41 C42 -16.4(10) . . . . ? 
Pd2 C41 C42 C43 -105.9(14) . . . . ? 
C41 C42 C43 C44 178.2(13) . . . . ? 
C45 O24 C44 O25 0(2) . . . . ? 
C45 O24 C44 C43 -178.9(12) . . . . ? 
C42 C43 C44 O25 9(2) . . . . ? 
C42 C43 C44 O24 -172.3(13) . . . . ? 
C50 N21 C46 C47 2(2) . . . . ? 
Pd2 N21 C46 C47 -177.2(11) . . . . ? 
N21 C46 C47 C48 1(2) . . . . ? 
C46 C47 C48 C49 0(2) . . . . ? 
C47 C48 C49 C50 -3(2) . . . . ? 
C46 N21 C50 C49 -4(2) . . . . ? 
Pd2 N21 C50 C49 174.5(10) . . . . ? 
C46 N21 C50 C51 179.3(12) . . . . ? 
Pd2 N21 C50 C51 -1.8(16) . . . . ? 
C48 C49 C50 N21 5(2) . . . . ? 
C48 C49 C50 C51 -179.0(14) . . . . ? 
C55 N22 C51 C52 0.5(19) . . . . ? 
Pd2 N22 C51 C52 -174.6(10) . . . . ? 
C55 N22 C51 C50 -177.5(12) . . . . ? 
Pd2 N22 C51 C50 7.4(15) . . . . ? 
N21 C50 C51 N22 -3.8(19) . . . . ? 
C49 C50 C51 N22 -179.8(13) . . . . ? 
N21 C50 C51 C52 178.3(12) . . . . ? 
C49 C50 C51 C52 2(2) . . . . ? 
N22 C51 C52 C53 1(2) . . . . ? 
C50 C51 C52 C53 178.8(13) . . . . ? 
C51 C52 C53 C54 -3(2) . . . . ? 
C52 C53 C54 C55 4(2) . . . . ? 
C51 N22 C55 C54 0.2(19) . . . . ? 
Pd2 N22 C55 C54 174.7(9) . . . . ? 
C53 C54 C55 N22 -2(2) . . . . ? 
C3S O1S C2S C1S 12(2) . . . . ? 
C3S O1S C2S O2S -174.9(14) . . . . ? 
C2S O1S C3S C4S 160.6(18) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              22.50 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.822 
_refine_diff_density_min   -0.701 
_refine_diff_density_rms    0.142 
 
#====================
_publ_contact_author 
; 
   Prof. Helena C. Malinakova 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
_publ_contact_author_email      hmalinakova@ku.edu 
_publ_contact_author_fax        1(785)8645396 
_publ_contact_author_phone      1(785)8644743 
 
_publ_requested_journal         'Organometallics'  
 
loop_ 
    _publ_author_name 
    _publ_author_address 
   'Guo, Ruiyun' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Portscheller, Jannelle L.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Day, Victor W.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
  'Malinakova, Helena C.' 
;  Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
; 
 
_publ_section_title 
; 
 article title here
 
; 
_publ_section_references 
;
  Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
 
  Flack, H. D. (1983) Acta Cryst. A39, 876-881. 
 
  Flack, H. D. and Schwarzenbach, D. (1988) Acta Cryst. A44, 
  499-506. 
 
  Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, 
     Wisconsin, USA.
;
_publ_section_acknowledgements 
; 
 The authors wish to thank the National Science Foundation 
 (CHE-0079282) and the University of Kansas for funds to 
 acquire the diffractometer and computers used in this work.  
;   
data_k71c(12-polymorph2) 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C28 H25 Br N2 O5 Pd' 
_chemical_formula_weight          655.81 
  
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' 
 '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)/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    16.951(5) 
_cell_length_b                    12.186(4) 
_cell_length_c                    14.239(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  114.146(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      2683.8(14) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     863 
_cell_measurement_theta_min       2.29 
_cell_measurement_theta_max       21.10 
  
_exptl_crystal_description        Triangular 
_exptl_crystal_colour             Yellow 
_exptl_crystal_size_max           0.19 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.623 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1312 
_exptl_absorpt_coefficient_mu     2.221 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.714 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       100(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 SMART 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_%         0.00 
_diffrn_reflns_number             15891 
_diffrn_reflns_av_R_equivalents   0.1934 
_diffrn_reflns_av_sigmaI/netI     0.1664 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.63 
_diffrn_reflns_theta_max          22.49 
_reflns_number_total              3507 
_reflns_number_gt                 1875 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections except 3 which were flagged 
 by the user for being in the beamstop.  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)+(0.0977P)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     noref 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3507 
_refine_ls_number_parameters      336 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1509 
_refine_ls_R_factor_gt            0.0699 
_refine_ls_wR_factor_ref          0.1871 
_refine_ls_wR_factor_gt           0.1630 
_refine_ls_goodness_of_fit_ref    0.895 
_refine_ls_restrained_S_all       0.895 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pd Pd 0.25840(7) 0.05646(8) -0.00076(8) 0.0335(4) Uani 1 1 d . . . 
Br Br 0.36486(9) 0.22149(12) 0.05266(11) 0.0406(5) Uani 1 1 d . . . 
O1 O 0.1071(6) -0.0415(7) 0.0068(7) 0.040(2) Uani 1 1 d . . . 
O2 O 0.1790(8) -0.1641(9) -0.1682(10) 0.078(4) Uani 1 1 d . . . 
O3 O 0.0559(8) -0.0623(10) -0.2011(9) 0.068(3) Uani 1 1 d . . . 
O4 O -0.0317(7) 0.3174(8) 0.0530(8) 0.061(3) Uani 1 1 d . . . 
O5 O 0.0938(7) 0.4042(10) 0.0949(9) 0.074(4) Uani 1 1 d . . . 
N1 N 0.3637(7) -0.0521(9) 0.0729(9) 0.043(3) Uani 1 1 d . . . 
N2 N 0.3042(7) 0.0201(8) -0.1189(9) 0.037(3) Uani 1 1 d . . . 
C1 C 0.1448(9) 0.0167(11) 0.0977(11) 0.038(4) Uani 1 1 d . . . 
C2 C 0.2220(8) 0.0675(10) 0.1114(10) 0.028(3) Uani 1 1 d . . . 
C3 C 0.2654(9) 0.1254(11) 0.2070(11) 0.040(4) Uani 1 1 d . . . 
H3 H 0.3182 0.1628 0.2212 0.048 Uiso 1 1 calc R . . 
C4 C 0.2285(10) 0.1255(12) 0.2785(12) 0.050(4) Uani 1 1 d . . . 
H4 H 0.2581 0.1598 0.3435 0.060 Uiso 1 1 calc R . . 
C5 C 0.1512(9) 0.0774(12) 0.2566(12) 0.044(4) Uani 1 1 d . . . 
H5 H 0.1251 0.0829 0.3041 0.053 Uiso 1 1 calc R . . 
C6 C 0.1105(10) 0.0216(11) 0.1679(13) 0.048(4) Uani 1 1 d . . . 
H6 H 0.0574 -0.0145 0.1548 0.057 Uiso 1 1 calc R . . 
C7 C 0.1691(9) -0.0649(12) -0.0278(11) 0.044(4) Uani 1 1 d . . . 
H7 H 0.2008 -0.1311 0.0108 0.053 Uiso 1 1 calc R . . 
C8 C 0.1238(13) -0.0984(14) -0.1429(15) 0.059(5) Uani 1 1 d . . . 
C9 C 0.1416(14) -0.1812(16) -0.2846(15) 0.092(7) Uani 1 1 d . . . 
H9A H 0.0867 -0.2228 -0.3083 0.110 Uiso 1 1 calc R . . 
H9B H 0.1306 -0.1099 -0.3210 0.110 Uiso 1 1 calc R . . 
C10 C 0.2100(15) -0.2456(15) -0.303(2) 0.122(9) Uani 1 1 d . . . 
H10A H 0.1886 -0.2644 -0.3766 0.184 Uiso 1 1 calc R . . 
H10B H 0.2232 -0.3130 -0.2623 0.184 Uiso 1 1 calc R . . 
H10C H 0.2625 -0.2010 -0.2836 0.184 Uiso 1 1 calc R . . 
C11 C 0.1579(9) 0.1583(10) -0.0852(10) 0.037(4) Uani 1 1 d . . . 
H11A H 0.1724 0.1956 -0.1378 0.045 Uiso 1 1 calc R . . 
H11B H 0.1059 0.1128 -0.1219 0.045 Uiso 1 1 calc R . . 
C12 C 0.1352(10) 0.2479(12) -0.0208(12) 0.055(5) Uani 1 1 d . . . 
H12 H 0.1754 0.3048 0.0117 0.065 Uiso 1 1 calc R . . 
C13 C 0.0609(9) 0.2450(11) -0.0114(10) 0.040(4) Uani 1 1 d . . . 
H13 H 0.0196 0.1891 -0.0438 0.048 Uiso 1 1 calc R . . 
C14 C 0.0436(12) 0.3308(13) 0.0506(12) 0.050(4) Uani 1 1 d . . . 
C15 C -0.0544(11) 0.3982(12) 0.1126(13) 0.066(5) Uani 1 1 d . . . 
H15A H -0.0898 0.3635 0.1441 0.098 Uiso 1 1 calc R . . 
H15B H -0.0871 0.4579 0.0673 0.098 Uiso 1 1 calc R . . 
H15C H -0.0015 0.4278 0.1666 0.098 Uiso 1 1 calc R . . 
C16 C 0.3879(9) -0.0927(12) 0.1691(11) 0.046(4) Uani 1 1 d . . . 
H16 H 0.3594 -0.0686 0.2105 0.055 Uiso 1 1 calc R . . 
C17 C 0.4548(9) -0.1701(11) 0.2083(12) 0.045(4) Uani 1 1 d . . . 
H17 H 0.4708 -0.1991 0.2755 0.054 Uiso 1 1 calc R . . 
C18 C 0.4967(10) -0.2033(11) 0.1497(13) 0.048(4) Uani 1 1 d . . . 
H18 H 0.5428 -0.2546 0.1763 0.058 Uiso 1 1 calc R . . 
C19 C 0.4726(8) -0.1632(10) 0.0536(11) 0.035(3) Uani 1 1 d . . . 
H19 H 0.5020 -0.1859 0.0127 0.041 Uiso 1 1 calc R . . 
C20 C 0.4058(8) -0.0898(10) 0.0151(11) 0.035(4) Uani 1 1 d . . . 
C21 C 0.3734(8) -0.0437(10) -0.0920(10) 0.033(3) Uani 1 1 d . . . 
C22 C 0.4146(10) -0.0642(11) -0.1534(11) 0.047(4) Uani 1 1 d . . . 
H22 H 0.4659 -0.1070 -0.1293 0.057 Uiso 1 1 calc R . . 
C23 C 0.3799(11) -0.0205(11) -0.2554(12) 0.050(4) Uani 1 1 d . . . 
H23 H 0.4052 -0.0365 -0.3023 0.060 Uiso 1 1 calc R . . 
C24 C 0.3080(10) 0.0459(12) -0.2831(11) 0.046(4) Uani 1 1 d . . . 
H24 H 0.2836 0.0788 -0.3493 0.055 Uiso 1 1 calc R . . 
C25 C 0.2725(10) 0.0637(11) -0.2151(12) 0.050(4) Uani 1 1 d . . . 
H25 H 0.2227 0.1091 -0.2356 0.060 Uiso 1 1 calc R . . 
C1S C 0.308(4) -0.373(4) -0.024(3) 0.35(4) Uani 1 1 d . . . 
C2S C 0.392(3) -0.400(4) -0.065(5) 0.33(4) Uani 1 1 d . . . 
C3S C 0.482(3) -0.466(2) 0.032(3) 0.190(18) Uani 1 1 d . . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Pd C2 1.938(12) . ? 
Pd C7 2.037(13) . ? 
Pd C11 2.052(12) . ? 
Pd N1 2.123(12) . ? 
Pd N2 2.167(11) . ? 
Pd Br 2.5993(18) . ? 
O1 C7 1.361(16) . ? 
O1 C1 1.382(16) . ? 
O2 C8 1.387(19) . ? 
O2 C9 1.53(2) . ? 
O3 C8 1.193(19) . ? 
O4 C14 1.301(19) . ? 
O4 C15 1.450(16) . ? 
O5 C14 1.218(18) . ? 
N1 C16 1.352(17) . ? 
N1 C20 1.372(16) . ? 
N2 C21 1.326(15) . ? 
N2 C25 1.358(17) . ? 
C1 C6 1.348(19) . ? 
C1 C2 1.387(18) . ? 
C2 C3 1.440(18) . ? 
C3 C4 1.396(19) . ? 
C4 C5 1.350(19) . ? 
C5 C6 1.349(19) . ? 
C7 C8 1.55(2) . ? 
C9 C10 1.51(2) . ? 
C11 C12 1.571(18) . ? 
C12 C13 1.320(18) . ? 
C13 C14 1.473(19) . ? 
C16 C17 1.402(18) . ? 
C17 C18 1.360(19) . ? 
C18 C19 1.349(19) . ? 
C19 C20 1.368(17) . ? 
C20 C21 1.502(18) . ? 
C21 C22 1.348(18) . ? 
C22 C23 1.43(2) . ? 
C23 C24 1.38(2) . ? 
C24 C25 1.350(19) . ? 
C1S C2S 1.78(8) . ? 
C2S C3S 1.78(7) . ? 
C3S C3S 1.51(6) 3_645 ? 
  
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 
C2 Pd C7 75.2(6) . . ? 
C2 Pd C11 88.5(5) . . ? 
C7 Pd C11 87.3(6) . . ? 
C2 Pd N1 97.0(5) . . ? 
C7 Pd N1 92.9(5) . . ? 
C11 Pd N1 174.4(5) . . ? 
C2 Pd N2 171.8(5) . . ? 
C7 Pd N2 100.3(5) . . ? 
C11 Pd N2 98.3(5) . . ? 
N1 Pd N2 76.1(4) . . ? 
C2 Pd Br 97.0(4) . . ? 
C7 Pd Br 172.0(4) . . ? 
C11 Pd Br 90.8(4) . . ? 
N1 Pd Br 89.7(3) . . ? 
N2 Pd Br 87.7(3) . . ? 
C7 O1 C1 108.5(10) . . ? 
C8 O2 C9 109.5(15) . . ? 
C14 O4 C15 115.3(12) . . ? 
C16 N1 C20 118.0(12) . . ? 
C16 N1 Pd 125.1(10) . . ? 
C20 N1 Pd 116.8(9) . . ? 
C21 N2 C25 117.3(12) . . ? 
C21 N2 Pd 116.8(9) . . ? 
C25 N2 Pd 125.7(10) . . ? 
C6 C1 O1 122.8(13) . . ? 
C6 C1 C2 123.0(14) . . ? 
O1 C1 C2 114.2(12) . . ? 
C1 C2 C3 116.1(12) . . ? 
C1 C2 Pd 116.9(10) . . ? 
C3 C2 Pd 127.0(10) . . ? 
C4 C3 C2 118.8(13) . . ? 
C5 C4 C3 120.8(15) . . ? 
C6 C5 C4 120.8(14) . . ? 
C1 C6 C5 120.4(14) . . ? 
O1 C7 C8 108.4(12) . . ? 
O1 C7 Pd 113.8(9) . . ? 
C8 C7 Pd 113.5(10) . . ? 
O3 C8 O2 126.5(17) . . ? 
O3 C8 C7 123.8(16) . . ? 
O2 C8 C7 109.3(16) . . ? 
C10 C9 O2 104.7(18) . . ? 
C12 C11 Pd 114.9(9) . . ? 
C13 C12 C11 120.9(14) . . ? 
C12 C13 C14 118.3(15) . . ? 
O5 C14 O4 124.3(14) . . ? 
O5 C14 C13 124.3(17) . . ? 
O4 C14 C13 111.4(16) . . ? 
N1 C16 C17 120.7(14) . . ? 
C18 C17 C16 119.7(15) . . ? 
C19 C18 C17 119.8(14) . . ? 
C18 C19 C20 120.1(14) . . ? 
C19 C20 N1 121.7(13) . . ? 
C19 C20 C21 123.4(13) . . ? 
N1 C20 C21 114.8(12) . . ? 
N2 C21 C22 123.6(13) . . ? 
N2 C21 C20 115.2(12) . . ? 
C22 C21 C20 121.2(13) . . ? 
C21 C22 C23 118.9(14) . . ? 
C24 C23 C22 117.2(14) . . ? 
C25 C24 C23 119.4(15) . . ? 
C24 C25 N2 123.5(15) . . ? 
C1S C2S C3S 112(4) . . ? 
C3S C3S C2S 102(4) 3_645 . ? 
  
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 
C2 Pd N1 C16 0.2(12) . . . . ? 
C7 Pd N1 C16 -75.2(12) . . . . ? 
C11 Pd N1 C16 -167(5) . . . . ? 
N2 Pd N1 C16 -175.1(12) . . . . ? 
Br Pd N1 C16 97.2(11) . . . . ? 
C2 Pd N1 C20 175.1(9) . . . . ? 
C7 Pd N1 C20 99.7(10) . . . . ? 
C11 Pd N1 C20 7(5) . . . . ? 
N2 Pd N1 C20 -0.2(9) . . . . ? 
Br Pd N1 C20 -87.9(9) . . . . ? 
C2 Pd N2 C21 -37(4) . . . . ? 
C7 Pd N2 C21 -93.2(10) . . . . ? 
C11 Pd N2 C21 178.0(9) . . . . ? 
N1 Pd N2 C21 -2.8(9) . . . . ? 
Br Pd N2 C21 87.5(9) . . . . ? 
C2 Pd N2 C25 148(3) . . . . ? 
C7 Pd N2 C25 92.3(11) . . . . ? 
C11 Pd N2 C25 3.5(12) . . . . ? 
N1 Pd N2 C25 -177.2(12) . . . . ? 
Br Pd N2 C25 -87.0(11) . . . . ? 
C7 O1 C1 C6 -157.7(13) . . . . ? 
C7 O1 C1 C2 20.8(15) . . . . ? 
C6 C1 C2 C3 1(2) . . . . ? 
O1 C1 C2 C3 -177.5(10) . . . . ? 
C6 C1 C2 Pd -177.4(11) . . . . ? 
O1 C1 C2 Pd 4.0(15) . . . . ? 
C7 Pd C2 C1 -18.0(10) . . . . ? 
C11 Pd C2 C1 69.6(10) . . . . ? 
N1 Pd C2 C1 -109.2(10) . . . . ? 
N2 Pd C2 C1 -75(4) . . . . ? 
Br Pd C2 C1 160.3(9) . . . . ? 
C7 Pd C2 C3 163.8(12) . . . . ? 
C11 Pd C2 C3 -108.6(11) . . . . ? 
N1 Pd C2 C3 72.6(11) . . . . ? 
N2 Pd C2 C3 106(3) . . . . ? 
Br Pd C2 C3 -17.9(11) . . . . ? 
C1 C2 C3 C4 0.8(19) . . . . ? 
Pd C2 C3 C4 179.0(10) . . . . ? 
C2 C3 C4 C5 -4(2) . . . . ? 
C3 C4 C5 C6 5(2) . . . . ? 
O1 C1 C6 C5 178.3(13) . . . . ? 
C2 C1 C6 C5 0(2) . . . . ? 
C4 C5 C6 C1 -3(2) . . . . ? 
C1 O1 C7 C8 -163.4(11) . . . . ? 
C1 O1 C7 Pd -36.1(13) . . . . ? 
C2 Pd C7 O1 30.4(9) . . . . ? 
C11 Pd C7 O1 -58.7(10) . . . . ? 
N1 Pd C7 O1 126.9(10) . . . . ? 
N2 Pd C7 O1 -156.7(9) . . . . ? 
Br Pd C7 O1 18(4) . . . . ? 
C2 Pd C7 C8 155.0(13) . . . . ? 
C11 Pd C7 C8 65.9(12) . . . . ? 
N1 Pd C7 C8 -108.5(12) . . . . ? 
N2 Pd C7 C8 -32.1(12) . . . . ? 
Br Pd C7 C8 143(2) . . . . ? 
C9 O2 C8 O3 2(2) . . . . ? 
C9 O2 C8 C7 -170.4(12) . . . . ? 
O1 C7 C8 O3 32(2) . . . . ? 
Pd C7 C8 O3 -95.6(18) . . . . ? 
O1 C7 C8 O2 -155.3(12) . . . . ? 
Pd C7 C8 O2 77.3(14) . . . . ? 
C8 O2 C9 C10 175.6(13) . . . . ? 
C2 Pd C11 C12 33.7(11) . . . . ? 
C7 Pd C11 C12 108.9(11) . . . . ? 
N1 Pd C11 C12 -159(4) . . . . ? 
N2 Pd C11 C12 -151.1(10) . . . . ? 
Br Pd C11 C12 -63.3(10) . . . . ? 
Pd C11 C12 C13 -113.2(14) . . . . ? 
C11 C12 C13 C14 179.5(12) . . . . ? 
C15 O4 C14 O5 1(2) . . . . ? 
C15 O4 C14 C13 179.9(12) . . . . ? 
C12 C13 C14 O5 -1(2) . . . . ? 
C12 C13 C14 O4 -180.0(13) . . . . ? 
C20 N1 C16 C17 0.7(19) . . . . ? 
Pd N1 C16 C17 175.5(9) . . . . ? 
N1 C16 C17 C18 1(2) . . . . ? 
C16 C17 C18 C19 -1(2) . . . . ? 
C17 C18 C19 C20 0(2) . . . . ? 
C18 C19 C20 N1 2.3(19) . . . . ? 
C18 C19 C20 C21 -178.2(12) . . . . ? 
C16 N1 C20 C19 -2.4(19) . . . . ? 
Pd N1 C20 C19 -177.6(9) . . . . ? 
C16 N1 C20 C21 178.1(11) . . . . ? 
Pd N1 C20 C21 2.8(14) . . . . ? 
C25 N2 C21 C22 2(2) . . . . ? 
Pd N2 C21 C22 -172.8(10) . . . . ? 
C25 N2 C21 C20 180.0(11) . . . . ? 
Pd N2 C21 C20 5.1(14) . . . . ? 
C19 C20 C21 N2 175.3(12) . . . . ? 
N1 C20 C21 N2 -5.2(16) . . . . ? 
C19 C20 C21 C22 -7(2) . . . . ? 
N1 C20 C21 C22 172.8(12) . . . . ? 
N2 C21 C22 C23 -4(2) . . . . ? 
C20 C21 C22 C23 178.5(12) . . . . ? 
C21 C22 C23 C24 4(2) . . . . ? 
C22 C23 C24 C25 -2(2) . . . . ? 
C23 C24 C25 N2 1(2) . . . . ? 
C21 N2 C25 C24 0(2) . . . . ? 
Pd N2 C25 C24 174.0(10) . . . . ? 
C1S C2S C3S C3S 150(3) . . . 3_645 ? 
  
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              22.49 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.898 
_refine_diff_density_min   -0.741 
_refine_diff_density_rms    0.162 

