data_04sjc002
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C33 H33 N3 O6 Pd S3'
_chemical_formula_weight          770.20
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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                    8.5627(2)
_cell_length_b                    10.4508(6)
_cell_length_c                    35.5429(17)
_cell_angle_alpha                 90.00
_cell_angle_beta                  94.294(3)
_cell_angle_gamma                 90.00
_cell_volume                      3171.7(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     34239
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.613
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1576
_exptl_absorpt_coefficient_mu     0.834
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9213
_exptl_absorpt_correction_T_max   0.9917
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD'
_diffrn_measurement_method        'φ & ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_decay_%         'negligible'
_diffrn_reflns_number             17853
_diffrn_reflns_av_R_equivalents   0.0464
_diffrn_reflns_av_sigmaI/netI     0.0386
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -44
_diffrn_reflns_limit_l_max        45
_diffrn_reflns_theta_min          3.01
_diffrn_reflns_theta_max          27.39
_reflns_number_total              6374
_reflns_number_gt                 5781
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_cell_refinement        'DENZO & COLLECT'
_computing_data_reduction         'DENZO & COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0358P)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     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0160(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          6374
_refine_ls_number_parameters      419
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0461
_refine_ls_R_factor_gt            0.0388
_refine_ls_wR_factor_ref          0.1104
_refine_ls_wR_factor_gt           0.0982
_refine_ls_goodness_of_fit_ref    1.811
_refine_ls_restrained_S_all       1.811
_refine_ls_shift/su_max           0.064
_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 0.9307(3) 0.2297(3) 0.20622(7) 0.0227(6) Uani 1 1 d . . .
H1A H 1.0434 0.2094 0.2054 0.027 Uiso 1 1 calc R . .
H1B H 0.9204 0.3240 0.2066 0.027 Uiso 1 1 calc R . .
C2 C 0.8454(3) 0.1803(3) 0.17117(7) 0.0202(6) Uani 1 1 d . . .
C3 C 0.7851(3) 0.1778(3) 0.13852(7) 0.0194(6) Uani 1 1 d . . .
C4 C 0.7291(3) 0.2312(3) 0.10175(7) 0.0216(6) Uani 1 1 d . . .
H4A H 0.8097 0.2902 0.0932 0.026 Uiso 1 1 calc R . .
H4B H 0.6333 0.2820 0.1049 0.026 Uiso 1 1 calc R . .
C5 C 0.5588(3) 0.0495(3) 0.07949(8) 0.0192(6) Uani 1 1 d . . .
H5A H 0.4686 0.1039 0.0850 0.023 Uiso 1 1 calc R . .
H5B H 0.5281 -0.0008 0.0565 0.023 Uiso 1 1 calc R . .
C6 C 0.5934(3) -0.0391(3) 0.11127(7) 0.0177(5) Uani 1 1 d . . .
C7 C 0.5868(3) -0.1361(3) 0.13054(7) 0.0195(6) Uani 1 1 d . . .
C8 C 0.5484(3) -0.2689(3) 0.14247(8) 0.0235(6) Uani 1 1 d . . .
H8A H 0.4555 -0.2651 0.1574 0.028 Uiso 1 1 calc R . .
H8B H 0.5196 -0.3204 0.1196 0.028 Uiso 1 1 calc R . .
C9 C 0.7157(4) -0.2839(3) 0.20306(7) 0.0233(6) Uani 1 1 d . . .
H9A H 0.8015 -0.3364 0.2152 0.028 Uiso 1 1 calc R . .
H9B H 0.6235 -0.2948 0.2180 0.028 Uiso 1 1 calc R . .
C10 C 0.7643(3) -0.1474(3) 0.20546(7) 0.0221(6) Uani 1 1 d . . .
C11 C 0.8180(3) -0.0469(3) 0.21970(7) 0.0205(6) Uani 1 1 d . . .
C12 C 0.9013(4) 0.0399(3) 0.24752(8) 0.0242(6) Uani 1 1 d . . .
H12A H 0.8686 0.0182 0.2729 0.029 Uiso 1 1 calc R . .
H12B H 1.0149 0.0224 0.2476 0.029 Uiso 1 1 calc R . .
C13 C 0.5717(3) 0.2584(3) 0.22260(7) 0.0206(6) Uani 1 1 d . . .
C14 C 0.4774(3) 0.1524(3) 0.21453(7) 0.0211(6) Uani 1 1 d . . .
H14 H 0.4949 0.0748 0.2281 0.025 Uiso 1 1 calc R . .
C15 C 0.3569(3) 0.1620(3) 0.18622(8) 0.0229(6) Uani 1 1 d . . .
H15 H 0.2912 0.0901 0.1808 0.027 Uiso 1 1 calc R . .
C16 C 0.3300(3) 0.2740(3) 0.16571(8) 0.0245(6) Uani 1 1 d . . .
C17 C 0.1989(4) 0.2863(3) 0.13522(8) 0.0338(8) Uani 1 1 d . . .
H17A H 0.2426 0.3047 0.1111 0.051 Uiso 1 1 calc R . .
H17B H 0.1291 0.3562 0.1415 0.051 Uiso 1 1 calc R . .
H17C H 0.1397 0.2061 0.1332 0.051 Uiso 1 1 calc R . .
C18 C 0.4286(4) 0.3789(3) 0.17416(9) 0.0294(7) Uani 1 1 d . . .
H18 H 0.4130 0.4561 0.1603 0.035 Uiso 1 1 calc R . .
C19 C 0.5485(4) 0.3715(3) 0.20256(9) 0.0265(6) Uani 1 1 d . . .
H19 H 0.6142 0.4433 0.2082 0.032 Uiso 1 1 calc R . .
C20 C 0.5163(3) 0.2978(3) 0.02803(7) 0.0178(6) Uani 1 1 d . . .
C21 C 0.3674(3) 0.2492(3) 0.01794(7) 0.0187(6) Uani 1 1 d . . .
H21 H 0.3554 0.1655 0.0076 0.022 Uiso 1 1 calc R . .
C22 C 0.2368(3) 0.3244(3) 0.02314(7) 0.0222(6) Uani 1 1 d . . .
H22 H 0.1351 0.2923 0.0160 0.027 Uiso 1 1 calc R . .
C23 C 0.2536(3) 0.4471(3) 0.03877(7) 0.0218(6) Uani 1 1 d . . .
C24 C 0.1108(4) 0.5253(3) 0.04683(9) 0.0320(7) Uani 1 1 d . . .
H24A H 0.1036 0.6004 0.0303 0.048 Uiso 1 1 calc R . .
H24B H 0.1199 0.5531 0.0732 0.048 Uiso 1 1 calc R . .
H24C H 0.0164 0.4728 0.0422 0.048 Uiso 1 1 calc R . .
C25 C 0.4029(4) 0.4940(3) 0.04744(8) 0.0238(7) Uani 1 1 d . . .
H25 H 0.4155 0.5784 0.0572 0.029 Uiso 1 1 calc R . .
C26 C 0.5353(3) 0.4208(3) 0.04226(7) 0.0215(6) Uani 1 1 d . . .
H26 H 0.6371 0.4545 0.0484 0.026 Uiso 1 1 calc R . .
C27 C 0.9117(3) -0.2861(3) 0.11814(8) 0.0217(6) Uani 1 1 d . . .
C28 C 1.0383(3) -0.2217(3) 0.13607(8) 0.0263(6) Uani 1 1 d . . .
H28 H 1.0779 -0.2459 0.1607 0.032 Uiso 1 1 calc R . .
C29 C 1.1060(4) -0.1217(3) 0.11741(9) 0.0292(7) Uani 1 1 d . . .
H29 H 1.1934 -0.0780 0.1294 0.035 Uiso 1 1 calc R . .
C30 C 1.0482(3) -0.0844(3) 0.08155(8) 0.0242(6) Uani 1 1 d . . .
C31 C 1.1162(4) 0.0268(3) 0.06152(10) 0.0341(8) Uani 1 1 d . . .
H31A H 1.2039 0.0630 0.0774 0.051 Uiso 1 1 calc R . .
H31B H 1.0355 0.0924 0.0566 0.051 Uiso 1 1 calc R . .
H31C H 1.1536 -0.0024 0.0376 0.051 Uiso 1 1 calc R . .
C32 C 0.9233(3) -0.1515(3) 0.06393(8) 0.0239(6) Uani 1 1 d . . .
H32 H 0.8844 -0.1278 0.0392 0.029 Uiso 1 1 calc R . .
C33 C 0.8545(4) -0.2517(3) 0.08173(8) 0.0216(6) Uani 1 1 d . . .
H33 H 0.7692 -0.2969 0.0694 0.026 Uiso 1 1 calc R . .
N1 N 0.8764(3) 0.1782(2) 0.24133(6) 0.0206(5) Uani 1 1 d . . .
N2 N 0.6934(3) 0.1330(2) 0.07200(6) 0.0167(5) Uani 1 1 d . . .
N3 N 0.6762(3) -0.3353(2) 0.16503(6) 0.0224(5) Uani 1 1 d . . .
O1 O 0.6803(2) 0.1717(2) 0.28864(5) 0.0283(5) Uani 1 1 d . . .
O2 O 0.7745(2) 0.37978(19) 0.26635(6) 0.0279(5) Uani 1 1 d . . .
O3 O 0.8188(2) 0.27032(19) 0.02588(5) 0.0249(5) Uani 1 1 d . . .
O4 O 0.6468(2) 0.09113(18) 0.00330(5) 0.0226(4) Uani 1 1 d . . .
O5 O 0.7297(3) -0.48203(19) 0.11385(6) 0.0319(5) Uani 1 1 d . . .
O6 O 0.9191(3) -0.4620(2) 0.17002(6) 0.0315(5) Uani 1 1 d . . .
S1 S 0.72741(8) 0.25064(7) 0.258387(19) 0.02096(17) Uani 1 1 d . . .
S2 S 0.68022(8) 0.19489(6) 0.028874(18) 0.01805(17) Uani 1 1 d . . .
S3 S 0.81241(9) -0.40430(7) 0.142026(19) 0.02367(18) Uani 1 1 d . . .
Pd1 Pd 0.73311(2) -0.002534(18) 0.162712(5) 0.01671(10) 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
C1 N1 1.466(3) . ?
C1 C2 1.488(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.235(4) . ?
C2 Pd1 2.150(3) . ?
C3 C4 1.468(4) . ?
C3 Pd1 2.133(3) . ?
C4 N2 1.489(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.473(4) . ?
C5 N2 1.485(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.227(4) . ?
C6 Pd1 2.143(3) . ?
C7 C8 1.495(4) . ?
C7 Pd1 2.148(3) . ?
C8 N3 1.480(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N3 1.470(3) . ?
C9 C10 1.486(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.240(4) . ?
C10 Pd1 2.147(3) . ?
C11 C12 1.484(4) . ?
C11 Pd1 2.151(3) . ?
C12 N1 1.475(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C19 1.387(4) . ?
C13 C14 1.388(4) . ?
C13 S1 1.774(3) . ?
C14 C15 1.390(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(4) . ?
C15 H15 0.9500 . ?
C16 C18 1.402(4) . ?
C16 C17 1.506(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.387(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C26 1.386(4) . ?
C20 C21 1.394(4) . ?
C20 S2 1.767(3) . ?
C21 C22 1.391(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.401(4) . ?
C22 H22 0.9500 . ?
C23 C25 1.382(4) . ?
C23 C24 1.516(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.391(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.389(4) . ?
C27 C33 1.396(4) . ?
C27 S3 1.754(3) . ?
C28 C29 1.388(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(4) . ?
C29 H29 0.9500 . ?
C30 C32 1.388(4) . ?
C30 C31 1.503(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.378(4) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
N1 S1 1.639(2) . ?
N2 S2 1.660(2) . ?
N3 S3 1.641(2) . ?
O1 S1 1.437(2) . ?
O2 S1 1.431(2) . ?
O3 S2 1.435(2) . ?
O4 S2 1.4299(19) . ?
O5 S3 1.435(2) . ?
O6 S3 1.433(2) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N1 C1 C2 114.7(2) . . ?
N1 C1 H1A 108.6 . . ?
C2 C1 H1A 108.6 . . ?
N1 C1 H1B 108.6 . . ?
C2 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C1 159.8(3) . . ?
C3 C2 Pd1 72.46(17) . . ?
C1 C2 Pd1 127.7(2) . . ?
C2 C3 C4 156.1(3) . . ?
C2 C3 Pd1 74.03(17) . . ?
C4 C3 Pd1 129.1(2) . . ?
C3 C4 N2 114.0(2) . . ?
C3 C4 H4A 108.8 . . ?
N2 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
N2 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C6 C5 N2 113.1(2) . . ?
C6 C5 H5A 109.0 . . ?
N2 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
N2 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
C7 C6 C5 158.7(3) . . ?
C7 C6 Pd1 73.59(18) . . ?
C5 C6 Pd1 127.6(2) . . ?
C6 C7 C8 161.0(3) . . ?
C6 C7 Pd1 73.16(18) . . ?
C8 C7 Pd1 125.77(19) . . ?
N3 C8 C7 114.8(2) . . ?
N3 C8 H8A 108.6 . . ?
C7 C8 H8A 108.6 . . ?
N3 C8 H8B 108.6 . . ?
C7 C8 H8B 108.6 . . ?
H8A C8 H8B 107.5 . . ?
N3 C9 C10 116.6(2) . . ?
N3 C9 H9A 108.1 . . ?
C10 C9 H9A 108.1 . . ?
N3 C9 H9B 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C11 C10 C9 158.5(3) . . ?
C11 C10 Pd1 73.38(18) . . ?
C9 C10 Pd1 128.06(19) . . ?
C10 C11 C12 159.2(3) . . ?
C10 C11 Pd1 73.09(18) . . ?
C12 C11 Pd1 127.4(2) . . ?
N1 C12 C11 116.3(2) . . ?
N1 C12 H12A 108.2 . . ?
C11 C12 H12A 108.2 . . ?
N1 C12 H12B 108.2 . . ?
C11 C12 H12B 108.2 . . ?
H12A C12 H12B 107.4 . . ?
C19 C13 C14 121.0(3) . . ?
C19 C13 S1 118.6(2) . . ?
C14 C13 S1 120.4(2) . . ?
C13 C14 C15 118.8(3) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 121.7(3) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C18 118.2(3) . . ?
C15 C16 C17 122.3(3) . . ?
C18 C16 C17 119.5(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C16 120.9(3) . . ?
C19 C18 H18 119.6 . . ?
C16 C18 H18 119.6 . . ?
C13 C19 C18 119.4(3) . . ?
C13 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C26 C20 C21 120.8(3) . . ?
C26 C20 S2 119.1(2) . . ?
C21 C20 S2 119.5(2) . . ?
C22 C21 C20 119.2(3) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C22 C23 120.7(3) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C25 C23 C22 118.6(3) . . ?
C25 C23 C24 120.9(3) . . ?
C22 C23 C24 120.5(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 C26 121.6(3) . . ?
C23 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C20 C26 C25 118.9(3) . . ?
C20 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C28 C27 C33 120.5(3) . . ?
C28 C27 S3 120.6(2) . . ?
C33 C27 S3 118.8(2) . . ?
C29 C28 C27 119.0(3) . . ?
C29 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
C30 C29 C28 121.1(3) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C32 118.8(3) . . ?
C29 C30 C31 121.9(3) . . ?
C32 C30 C31 119.3(3) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C30 121.2(3) . . ?
C33 C32 H32 119.4 . . ?
C30 C32 H32 119.4 . . ?
C32 C33 C27 119.3(3) . . ?
C32 C33 H33 120.3 . . ?
C27 C33 H33 120.3 . . ?
C1 N1 C12 115.8(2) . . ?
C1 N1 S1 116.77(19) . . ?
C12 N1 S1 120.35(19) . . ?
C5 N2 C4 113.5(2) . . ?
C5 N2 S2 113.23(17) . . ?
C4 N2 S2 112.53(17) . . ?
C9 N3 C8 115.9(2) . . ?
C9 N3 S3 119.7(2) . . ?
C8 N3 S3 117.41(18) . . ?
O2 S1 O1 118.97(13) . . ?
O2 S1 N1 107.06(12) . . ?
O1 S1 N1 106.36(12) . . ?
O2 S1 C13 106.53(13) . . ?
O1 S1 C13 108.94(13) . . ?
N1 S1 C13 108.65(12) . . ?
O4 S2 O3 119.77(11) . . ?
O4 S2 N2 106.73(11) . . ?
O3 S2 N2 106.46(12) . . ?
O4 S2 C20 109.28(13) . . ?
O3 S2 C20 108.92(12) . . ?
N2 S2 C20 104.60(11) . . ?
O6 S3 O5 120.15(14) . . ?
O6 S3 N3 106.21(12) . . ?
O5 S3 N3 105.33(14) . . ?
O6 S3 C27 108.99(14) . . ?
O5 S3 C27 107.03(13) . . ?
N3 S3 C27 108.67(12) . . ?
C3 Pd1 C6 86.19(11) . . ?
C3 Pd1 C10 152.85(11) . . ?
C6 Pd1 C10 120.66(11) . . ?
C3 Pd1 C7 119.41(10) . . ?
C6 Pd1 C7 33.25(10) . . ?
C10 Pd1 C7 87.42(11) . . ?
C3 Pd1 C2 33.51(10) . . ?
C6 Pd1 C2 119.53(11) . . ?
C10 Pd1 C2 119.80(11) . . ?
C7 Pd1 C2 152.77(11) . . ?
C3 Pd1 C11 120.27(11) . . ?
C6 Pd1 C11 153.24(12) . . ?
C10 Pd1 C11 33.53(11) . . ?
C7 Pd1 C11 120.27(11) . . ?
C2 Pd1 C11 86.77(11) . . ?
 
_diffrn_measured_fraction_theta_max    0.884
_diffrn_reflns_theta_full              27.39
_diffrn_measured_fraction_theta_full   0.884
_refine_diff_density_max    0.721
_refine_diff_density_min   -0.730
_refine_diff_density_rms    0.188
