 
data_04src0851
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C55 H44 Cl4 O6 P2 Pd'
_chemical_formula_weight          1111.04
_chemical_absolute_configuration  unk
 
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'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd'  'Pd'  -0.9988   1.0072
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P21
_symmetry_space_group_name_hall   'P 2yb'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    11.268(3)
_cell_length_b                    20.164(3)
_cell_length_c                    11.420(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  109.820(15)
_cell_angle_gamma                 90.00
_cell_volume                      2441.1(9)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4038
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        shard
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.512
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1132
_exptl_absorpt_coefficient_mu     0.717
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8818
_exptl_absorpt_correction_T_max   0.9858
_exptl_absorpt_process_details    'SORTAV (R.H.Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             25786
_diffrn_reflns_av_R_equivalents   0.0669
_diffrn_reflns_av_sigmaI/netI     0.0836
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -26
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          2.98
_diffrn_reflns_theta_max          27.50
_reflns_number_total              10212
_reflns_number_gt                 8801
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'PLATON (Watkin, Pearce 1995)'
_computing_publication_material   SHELXL-97
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.1517P)²+37.1511P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.030(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.18(7)
_refine_ls_number_reflns          10212
_refine_ls_number_parameters      621
_refine_ls_number_restraints      7
_refine_ls_R_factor_all           0.1246
_refine_ls_R_factor_gt            0.1121
_refine_ls_wR_factor_ref          0.3115
_refine_ls_wR_factor_gt           0.3015
_refine_ls_goodness_of_fit_ref    1.069
_refine_ls_restrained_S_all       1.068
_refine_ls_shift/su_max           0.026
_refine_ls_shift/su_mean          0.001
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.2499(11) 0.9344(9) 0.8399(10) 0.030(2) Uani 1 1 d . . .
C2 C 0.2678(13) 0.8932(6) 0.9403(12) 0.027(3) Uani 1 1 d . . .
C3 C 0.3845(13) 0.8869(6) 1.0379(13) 0.030(3) Uani 1 1 d . . .
C4 C 0.490(2) 0.9265(8) 1.036(2) 0.076(7) Uani 1 1 d . . .
H4 H 0.5681 0.9246 1.1027 0.091 Uiso 1 1 calc R . .
C5 C 0.4768(14) 0.9681(6) 0.9321(11) 0.030(3) Uani 1 1 d . . .
C6 C 0.3591(11) 0.9707(6) 0.8374(12) 0.025(2) Uani 1 1 d . . .
C7 C 0.3979(17) 0.8369(7) 1.1411(16) 0.043(4) Uani 1 1 d . . .
C8 C 0.372(2) 0.7663(9) 1.0911(19) 0.057(5) Uani 1 1 d . . .
H8A H 0.3275 0.7419 1.1376 0.085 Uiso 1 1 calc R . .
H8B H 0.4525 0.7441 1.1009 0.085 Uiso 1 1 calc R . .
H8C H 0.3205 0.7675 1.0028 0.085 Uiso 1 1 calc R . .
C9 C 0.5360(18) 0.8341(7) 1.2296(17) 0.046(4) Uani 1 1 d . . .
H9A H 0.5436 0.8015 1.2955 0.069 Uiso 1 1 calc R . .
H9B H 0.5615 0.8779 1.2669 0.069 Uiso 1 1 calc R . .
H9C H 0.5907 0.8210 1.1827 0.069 Uiso 1 1 calc R . .
C10 C 0.3155(15) 0.8543(8) 1.2162(15) 0.040(3) Uani 1 1 d . . .
H10A H 0.2267 0.8483 1.1650 0.060 Uiso 1 1 calc R . .
H10B H 0.3299 0.9006 1.2433 0.060 Uiso 1 1 calc R . .
H10C H 0.3360 0.8253 1.2893 0.060 Uiso 1 1 calc R . .
C11 C 0.5887(13) 1.0072(6) 0.9263(11) 0.029(3) Uani 1 1 d U . .
C12 C 0.7092(14) 0.9928(7) 1.0469(15) 0.041(3) Uani 1 1 d . . .
H12A H 0.7443 0.9492 1.0389 0.061 Uiso 1 1 calc R . .
H12B H 0.6841 0.9932 1.1211 0.061 Uiso 1 1 calc R . .
H12C H 0.7731 1.0270 1.0548 0.061 Uiso 1 1 calc R . .
C13 C 0.5643(14) 1.0809(7) 0.9237(14) 0.037(3) Uani 1 1 d . . .
H13A H 0.6429 1.1049 0.9346 0.055 Uiso 1 1 calc R . .
H13B H 0.5328 1.0926 0.9911 0.055 Uiso 1 1 calc R . .
H13C H 0.5013 1.0930 0.8435 0.055 Uiso 1 1 calc R . .
C14 C 0.6289(14) 0.9872(7) 0.8200(13) 0.035(3) Uani 1 1 d . . .
H14A H 0.5657 1.0019 0.7418 0.053 Uiso 1 1 calc R . .
H14B H 0.6372 0.9388 0.8191 0.053 Uiso 1 1 calc R . .
H14C H 0.7104 1.0077 0.8289 0.053 Uiso 1 1 calc R . .
C15 C -0.1495(12) 0.7877(7) 0.7526(12) 0.033(3) Uani 1 1 d . . .
C16 C -0.1965(16) 0.7681(7) 0.6241(14) 0.038(3) Uani 1 1 d . . .
H16 H -0.1425 0.7602 0.5773 0.046 Uiso 1 1 calc R . .
C17 C -0.3272(14) 0.7616(6) 0.5733(13) 0.036(3) Uani 1 1 d . . .
H17 H -0.3630 0.7485 0.4887 0.043 Uiso 1 1 calc R . .
C18 C -0.4064(14) 0.7731(6) 0.6392(13) 0.033(3) Uani 1 1 d . . .
C19 C -0.5444(13) 0.7720(7) 0.5808(14) 0.037(3) Uani 1 1 d . . .
H19 H -0.5810 0.7602 0.4955 0.044 Uiso 1 1 calc R . .
C20 C -0.6175(14) 0.7869(7) 0.6448(13) 0.037(3) Uani 1 1 d . . .
H20 H -0.7064 0.7858 0.6044 0.044 Uiso 1 1 calc R . .
C21 C -0.5705(15) 0.8040(7) 0.7674(17) 0.044(4) Uani 1 1 d . . .
H21 H -0.6254 0.8152 0.8117 0.052 Uiso 1 1 calc R . .
C22 C -0.4410(14) 0.8045(6) 0.8259(13) 0.033(3) Uani 1 1 d . . .
H22 H -0.4067 0.8150 0.9120 0.039 Uiso 1 1 calc R . .
C23 C -0.3620(12) 0.7903(6) 0.7615(12) 0.029(3) Uani 1 1 d . . .
C24 C -0.2249(14) 0.7964(6) 0.8245(12) 0.032(3) Uani 1 1 d . . .
C25 C -0.1638(13) 0.8188(7) 0.9555(14) 0.035(3) Uani 1 1 d . . .
C26 C -0.1807(14) 0.7800(6) 1.0561(13) 0.033(3) Uani 1 1 d . . .
C27 C -0.2466(14) 0.7185(6) 1.0388(15) 0.035(3) Uani 1 1 d . . .
H27 H -0.2840 0.7005 0.9578 0.043 Uiso 1 1 calc R . .
C28 C -0.2552(13) 0.6860(7) 1.1399(15) 0.039(3) Uani 1 1 d . . .
H28 H -0.2927 0.6432 1.1299 0.047 Uiso 1 1 calc R . .
C29 C -0.2084(14) 0.7152(7) 1.2615(14) 0.035(3) Uani 1 1 d . . .
H29 H -0.2226 0.6939 1.3299 0.042 Uiso 1 1 calc R . .
C30 C -0.1450(16) 0.7720(8) 1.2785(16) 0.044(4) Uani 1 1 d . . .
H30 H -0.1108 0.7894 1.3604 0.052 Uiso 1 1 calc R . .
C31 C -0.1271(14) 0.8069(6) 1.1816(12) 0.032(3) Uani 1 1 d . . .
C32 C -0.0575(14) 0.8658(7) 1.1965(14) 0.035(3) Uani 1 1 d . . .
H32 H -0.0287 0.8857 1.2766 0.042 Uiso 1 1 calc R . .
C33 C -0.0295(13) 0.8955(7) 1.1059(14) 0.037(3) Uani 1 1 d . . .
H33 H 0.0264 0.9323 1.1225 0.044 Uiso 1 1 calc R . .
C34 C -0.0849(13) 0.8710(6) 0.9844(14) 0.033(3) Uani 1 1 d . . .
C35 C 0.3513(15) 0.9769(6) 0.4720(13) 0.034(3) Uani 1 1 d . . .
C36 C 0.4662(13) 0.9437(5) 0.5112(13) 0.033(3) Uani 1 1 d . . .
H36 H 0.4804 0.9085 0.5697 0.040 Uiso 1 1 calc R . .
C37 C 0.5551(16) 0.9613(8) 0.4670(15) 0.044(4) Uani 1 1 d . . .
H37 H 0.6325 0.9375 0.4917 0.053 Uiso 1 1 calc R . .
C38 C 0.5379(12) 1.0136(7) 0.3854(13) 0.031(3) Uani 1 1 d . . .
C39 C 0.6406(15) 1.0375(7) 0.3430(15) 0.039(3) Uani 1 1 d . . .
H39 H 0.7184 1.0141 0.3670 0.046 Uiso 1 1 calc R . .
C40 C 0.6252(15) 1.0929(6) 0.2694(14) 0.038(3) Uani 1 1 d . . .
H40 H 0.6894 1.1064 0.2380 0.045 Uiso 1 1 calc R . .
C41 C 0.5097(17) 1.1302(6) 0.2408(15) 0.040(4) Uani 1 1 d . . .
H41 H 0.4992 1.1699 0.1935 0.048 Uiso 1 1 calc R . .
C42 C 0.4158(16) 1.1089(8) 0.2809(16) 0.041(3) Uani 1 1 d . . .
H42 H 0.3406 1.1344 0.2599 0.049 Uiso 1 1 calc R . .
C43 C 0.4245(15) 1.0504(7) 0.3528(14) 0.036(3) Uani 1 1 d . . .
C44 C 0.3195(14) 1.0283(6) 0.3893(12) 0.032(3) Uani 1 1 d . . .
C45 C 0.1994(13) 1.0626(6) 0.3583(14) 0.032(3) Uani 1 1 d . . .
C46 C 0.1276(15) 1.0750(6) 0.2226(14) 0.036(3) Uani 1 1 d . . .
C47 C 0.1613(16) 1.0499(6) 0.1230(14) 0.038(3) Uani 1 1 d . . .
H47 H 0.2315 1.0208 0.1406 0.046 Uiso 1 1 calc R . .
C48 C 0.0984(15) 1.0655(7) 0.0059(14) 0.038(3) Uani 1 1 d . . .
H48 H 0.1257 1.0479 -0.0579 0.046 Uiso 1 1 calc R . .
C49 C -0.010(2) 1.1082(9) -0.0278(16) 0.055(5) Uani 1 1 d . . .
H49 H -0.0524 1.1196 -0.1124 0.066 Uiso 1 1 calc R . .
C50 C -0.0519(19) 1.1327(10) 0.0663(18) 0.056(5) Uani 1 1 d . . .
H50 H -0.1244 1.1602 0.0461 0.067 Uiso 1 1 calc R . .
C51 C 0.0152(13) 1.1158(8) 0.1916(13) 0.036(3) Uani 1 1 d . . .
C52 C -0.0304(16) 1.1349(8) 0.2815(15) 0.048(4) Uani 1 1 d . . .
H52 H -0.1037 1.1619 0.2592 0.057 Uiso 1 1 calc R . .
C53 C 0.0257(14) 1.1164(6) 0.4051(14) 0.034(3) Uani 1 1 d . . .
H53 H -0.0100 1.1274 0.4669 0.041 Uiso 1 1 calc R . .
C54 C 0.1410(13) 1.0796(6) 0.4336(12) 0.029(3) Uani 1 1 d . . .
C55 C 0.253(2) 0.6416(8) 0.4062(15) 0.054(5) Uani 1 1 d . . .
H55 H 0.2893 0.6458 0.4988 0.064 Uiso 1 1 calc R . .
O1 O 0.1589(10) 0.8564(4) 0.9376(9) 0.035(2) Uani 1 1 d . . .
O2 O 0.3425(9) 1.0088(5) 0.7302(9) 0.032(2) Uani 1 1 d . . .
O3 O -0.0194(9) 0.7986(5) 0.7996(9) 0.032(2) Uani 1 1 d . . .
O4 O -0.0625(9) 0.9045(4) 0.8855(8) 0.0281(19) Uani 1 1 d . . .
O5 O 0.2568(10) 0.9486(4) 0.5133(8) 0.038(3) Uani 1 1 d . . .
O6 O 0.2040(9) 1.0695(5) 0.5652(9) 0.031(2) Uani 1 1 d . . .
P1 P 0.0330(3) 0.87223(16) 0.8273(3) 0.0302(7) Uani 1 1 d . . .
P2 P 0.2160(3) 0.99445(15) 0.6156(3) 0.0280(7) Uani 1 1 d . . .
Cl1 Cl -0.0886(3) 0.92179(17) 0.5139(3) 0.0397(8) Uani 1 1 d . . .
Cl2 Cl 0.1544(5) 0.7119(2) 0.3466(5) 0.0646(14) Uani 1 1 d . . .
Cl3 Cl 0.3745(5) 0.6359(2) 0.3493(5) 0.0575(12) Uani 1 1 d . . .
Cl4 Cl 0.1557(5) 0.5691(2) 0.3700(4) 0.0526(10) Uani 1 1 d . . .
Pd1 Pd 0.09055(9) 0.93438(4) 0.69278(8) 0.0293(3) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C2 1.374(19) . ?
C1 C6 1.440(19) . ?
C1 Pd1 2.001(11) . ?
C2 C3 1.412(19) . ?
C2 O1 1.425(16) . ?
C3 C4 1.44(2) . ?
C3 C7 1.52(2) . ?
C4 C5 1.42(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(18) . ?
C5 C11 1.51(2) . ?
C6 O2 1.403(16) . ?
C7 C10 1.50(2) . ?
C7 C8 1.52(2) . ?
C7 C9 1.54(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.49(2) . ?
C11 C13 1.510(18) . ?
C11 C12 1.599(18) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C24 1.38(2) . ?
C15 O3 1.398(16) . ?
C15 C16 1.435(19) . ?
C16 C17 1.39(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.37(2) . ?
C17 H17 0.9500 . ?
C18 C23 1.360(19) . ?
C18 C19 1.47(2) . ?
C19 C20 1.31(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.36(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.38(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.36(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.471(19) . ?
C24 C25 1.490(19) . ?
C25 C34 1.344(19) . ?
C25 C26 1.46(2) . ?
C26 C27 1.424(17) . ?
C26 C31 1.459(18) . ?
C27 C28 1.36(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.43(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.33(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.38(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.403(19) . ?
C32 C33 1.32(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.40(2) . ?
C33 H33 0.9500 . ?
C34 O4 1.410(17) . ?
C35 C44 1.366(18) . ?
C35 C36 1.39(2) . ?
C35 O5 1.422(18) . ?
C36 C37 1.31(2) . ?
C36 H36 0.9500 . ?
C37 C38 1.38(2) . ?
C37 H37 0.9500 . ?
C38 C43 1.41(2) . ?
C38 C39 1.48(2) . ?
C39 C40 1.37(2) . ?
C39 H39 0.9500 . ?
C40 C41 1.44(2) . ?
C40 H40 0.9500 . ?
C41 C42 1.36(2) . ?
C41 H41 0.9500 . ?
C42 C43 1.42(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.45(2) . ?
C44 C45 1.452(18) . ?
C45 C54 1.29(2) . ?
C45 C46 1.51(2) . ?
C46 C47 1.41(2) . ?
C46 C51 1.45(2) . ?
C47 C48 1.32(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.43(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.40(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.42(2) . ?
C50 H50 0.9500 . ?
C51 C52 1.35(2) . ?
C52 C53 1.39(2) . ?
C52 H52 0.9500 . ?
C53 C54 1.43(2) . ?
C53 H53 0.9500 . ?
C54 O6 1.443(15) . ?
C55 Cl3 1.71(2) . ?
C55 Cl2 1.79(2) . ?
C55 Cl4 1.789(17) . ?
C55 H55 1.0000 . ?
O1 P1 1.578(12) . ?
O2 P2 1.601(10) . ?
O3 P1 1.588(10) . ?
O4 P1 1.583(10) . ?
O5 P2 1.671(12) . ?
O6 P2 1.608(10) . ?
P1 Pd1 2.242(4) . ?
P2 Pd1 2.256(4) . ?
Cl1 Pd1 2.349(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 C1 C6 116.1(10) . . ?
C2 C1 Pd1 122.5(11) . . ?
C6 C1 Pd1 120.8(9) . . ?
C1 C2 C3 123.1(12) . . ?
C1 C2 O1 114.5(12) . . ?
C3 C2 O1 122.3(12) . . ?
C2 C3 C4 119.4(15) . . ?
C2 C3 C7 119.5(12) . . ?
C4 C3 C7 121.1(16) . . ?
C5 C4 C3 119(2) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 118.2(16) . . ?
C6 C5 C11 122.3(11) . . ?
C4 C5 C11 119.5(15) . . ?
C5 C6 O2 120.4(11) . . ?
C5 C6 C1 123.9(11) . . ?
O2 C6 C1 115.7(10) . . ?
C10 C7 C3 111.6(13) . . ?
C10 C7 C8 110.9(14) . . ?
C3 C7 C8 111.9(13) . . ?
C10 C7 C9 108.4(14) . . ?
C3 C7 C9 110.2(13) . . ?
C8 C7 C9 103.4(13) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C5 112.6(11) . . ?
C14 C11 C13 110.7(11) . . ?
C5 C11 C13 111.5(12) . . ?
C14 C11 C12 104.5(12) . . ?
C5 C11 C12 110.2(11) . . ?
C13 C11 C12 107.0(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C24 C15 O3 121.9(11) . . ?
C24 C15 C16 123.8(13) . . ?
O3 C15 C16 114.3(13) . . ?
C17 C16 C15 115.0(14) . . ?
C17 C16 H16 122.5 . . ?
C15 C16 H16 122.5 . . ?
C18 C17 C16 123.3(14) . . ?
C18 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
C23 C18 C17 121.8(14) . . ?
C23 C18 C19 115.7(14) . . ?
C17 C18 C19 122.4(14) . . ?
C20 C19 C18 120.9(14) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 122.2(15) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 H20 118.9 . . ?
C20 C21 C22 118.5(16) . . ?
C20 C21 H21 120.7 . . ?
C22 C21 H21 120.7 . . ?
C23 C22 C21 120.8(14) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C18 C23 C22 121.9(13) . . ?
C18 C23 C24 118.9(13) . . ?
C22 C23 C24 119.2(12) . . ?
C15 C24 C23 117.1(12) . . ?
C15 C24 C25 118.0(12) . . ?
C23 C24 C25 124.6(13) . . ?
C34 C25 C26 118.7(13) . . ?
C34 C25 C24 121.7(14) . . ?
C26 C25 C24 119.3(12) . . ?
C27 C26 C25 124.1(12) . . ?
C27 C26 C31 118.8(13) . . ?
C25 C26 C31 117.0(11) . . ?
C28 C27 C26 119.1(14) . . ?
C28 C27 H27 120.4 . . ?
C26 C27 H27 120.4 . . ?
C27 C28 C29 121.1(13) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C30 C29 C28 119.8(14) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 122.6(15) . . ?
C29 C30 H30 118.7 . . ?
C31 C30 H30 118.7 . . ?
C30 C31 C32 124.2(13) . . ?
C30 C31 C26 118.3(13) . . ?
C32 C31 C26 117.5(12) . . ?
C33 C32 C31 124.1(13) . . ?
C33 C32 H32 118.0 . . ?
C31 C32 H32 118.0 . . ?
C32 C33 C34 118.1(13) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
C25 C34 C33 123.6(14) . . ?
C25 C34 O4 117.5(13) . . ?
C33 C34 O4 118.9(12) . . ?
C44 C35 C36 125.8(14) . . ?
C44 C35 O5 118.9(13) . . ?
C36 C35 O5 114.9(11) . . ?
C37 C36 C35 119.7(13) . . ?
C37 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C36 C37 C38 121.0(15) . . ?
C36 C37 H37 119.5 . . ?
C38 C37 H37 119.5 . . ?
C37 C38 C43 119.2(14) . . ?
C37 C38 C39 121.6(14) . . ?
C43 C38 C39 118.8(13) . . ?
C40 C39 C38 120.9(15) . . ?
C40 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
C39 C40 C41 118.7(14) . . ?
C39 C40 H40 120.6 . . ?
C41 C40 H40 120.6 . . ?
C42 C41 C40 120.4(14) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 123.2(15) . . ?
C41 C42 H42 118.4 . . ?
C43 C42 H42 118.4 . . ?
C38 C43 C42 117.8(13) . . ?
C38 C43 C44 121.1(13) . . ?
C42 C43 C44 121.1(13) . . ?
C35 C44 C43 112.5(13) . . ?
C35 C44 C45 122.3(14) . . ?
C43 C44 C45 124.5(12) . . ?
C54 C45 C44 127.3(13) . . ?
C54 C45 C46 115.0(12) . . ?
C44 C45 C46 117.4(12) . . ?
C47 C46 C51 117.3(14) . . ?
C47 C46 C45 125.0(14) . . ?
C51 C46 C45 117.7(13) . . ?
C48 C47 C46 122.2(15) . . ?
C48 C47 H47 118.9 . . ?
C46 C47 H47 118.9 . . ?
C47 C48 C49 122.0(15) . . ?
C47 C48 H48 119.0 . . ?
C49 C48 H48 119.0 . . ?
C50 C49 C48 118.9(16) . . ?
C50 C49 H49 120.6 . . ?
C48 C49 H49 120.6 . . ?
C49 C50 C51 119.1(19) . . ?
C49 C50 H50 120.4 . . ?
C51 C50 H50 120.4 . . ?
C52 C51 C50 119.3(15) . . ?
C52 C51 C46 120.2(13) . . ?
C50 C51 C46 120.4(16) . . ?
C51 C52 C53 122.5(15) . . ?
C51 C52 H52 118.8 . . ?
C53 C52 H52 118.8 . . ?
C52 C53 C54 115.7(15) . . ?
C52 C53 H53 122.1 . . ?
C54 C53 H53 122.1 . . ?
C45 C54 C53 127.7(13) . . ?
C45 C54 O6 118.3(12) . . ?
C53 C54 O6 113.4(12) . . ?
Cl3 C55 Cl2 112.5(9) . . ?
Cl3 C55 Cl4 111.4(10) . . ?
Cl2 C55 Cl4 107.9(11) . . ?
Cl3 C55 H55 108.3 . . ?
Cl2 C55 H55 108.3 . . ?
Cl4 C55 H55 108.3 . . ?
C2 O1 P1 116.5(8) . . ?
C6 O2 P2 115.6(8) . . ?
C15 O3 P1 119.7(9) . . ?
C34 O4 P1 118.1(8) . . ?
C35 O5 P2 115.1(8) . . ?
C54 O6 P2 117.2(8) . . ?
O1 P1 O4 107.6(5) . . ?
O1 P1 O3 98.2(5) . . ?
O4 P1 O3 102.0(5) . . ?
O1 P1 Pd1 105.6(4) . . ?
O4 P1 Pd1 117.0(3) . . ?
O3 P1 Pd1 124.0(4) . . ?
O2 P2 O6 93.8(5) . . ?
O2 P2 O5 106.9(5) . . ?
O6 P2 O5 106.3(5) . . ?
O2 P2 Pd1 106.2(4) . . ?
O6 P2 Pd1 131.1(4) . . ?
O5 P2 Pd1 109.5(3) . . ?
C1 Pd1 P1 79.1(4) . . ?
C1 Pd1 P2 79.9(4) . . ?
P1 Pd1 P2 158.95(13) . . ?
C1 Pd1 Cl1 173.0(5) . . ?
P1 Pd1 Cl1 99.93(13) . . ?
P2 Pd1 Cl1 100.70(13) . . ?
 
_diffrn_measured_fraction_theta_max    0.962
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.962
_refine_diff_density_max    2.479
_refine_diff_density_min   -1.795
_refine_diff_density_rms    0.240
