data_02src222
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Robin Bedford
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C15 H20 F3 N2 O3 Pd'
_chemical_formula_weight          439.73
 
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'
 'F'  'F'   0.0171   0.0103
 '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                    9.3727(9)
_cell_length_b                    19.1440(15)
_cell_length_c                    20.2492(19)
_cell_angle_alpha                 90.00
_cell_angle_beta                  101.41
_cell_angle_gamma                 90.00
_cell_volume                      3561.5(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     37006
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       22.99
 
_exptl_crystal_description        needle
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.32
_exptl_crystal_size_mid           0.01
_exptl_crystal_size_min           0.005
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.640
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1768
_exptl_absorpt_coefficient_mu     1.086
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7225
_exptl_absorpt_correction_T_max   1.0000
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD'
_diffrn_measurement_method        'Φ & ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             9643
_diffrn_reflns_av_R_equivalents   0.0537
_diffrn_reflns_av_sigmaI/netI     0.0509
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.96
_diffrn_reflns_theta_max          23.03
_reflns_number_total              2323
_reflns_number_gt                 1940
_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, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0000P)²+44.8438P] 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      SHELXL
_refine_ls_extinction_coef        0.00023(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2323
_refine_ls_number_parameters      438
_refine_ls_number_restraints      240
_refine_ls_R_factor_all           0.0682
_refine_ls_R_factor_gt            0.0535
_refine_ls_wR_factor_ref          0.1147
_refine_ls_wR_factor_gt           0.1097
_refine_ls_goodness_of_fit_ref    1.283
_refine_ls_restrained_S_all       1.210
_refine_ls_shift/su_max           0.007
_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 0.1819(13) 0.2589(6) 0.3314(6) 0.013(3) Uani 1 1 d U . .
H1A H 0.2748 0.2333 0.3350 0.016 Uiso 1 1 calc R . .
H1B H 0.1042 0.2242 0.3328 0.016 Uiso 1 1 calc R . .
C2 C 0.1928(13) 0.3076(7) 0.3905(6) 0.017(4) Uani 1 1 d U . .
H2A H 0.2187 0.2808 0.4330 0.020 Uiso 1 1 calc R . .
H2B H 0.2708 0.3423 0.3895 0.020 Uiso 1 1 calc R . .
C3 C 0.0246(13) 0.3841(7) 0.3265(6) 0.019(4) Uani 1 1 d U . .
H3A H 0.1030 0.4187 0.3266 0.023 Uiso 1 1 calc R . .
H3B H -0.0679 0.4098 0.3241 0.023 Uiso 1 1 calc R . .
C4 C 0.0127(13) 0.3370(7) 0.2651(6) 0.017(3) Uani 1 1 d U . .
H4A H -0.0693 0.3041 0.2638 0.021 Uiso 1 1 calc R . .
H4B H -0.0086 0.3659 0.2238 0.021 Uiso 1 1 calc R . .
C5 C 0.0173(15) 0.1189(7) 0.2578(6) 0.023(4) Uani 1 1 d U . .
C6 C 0.0256(17) 0.0481(9) 0.2916(8) 0.033(4) Uani 1 1 d U . .
C7 C 0.2337(13) 0.1586(7) 0.0738(7) 0.028(4) Uani 1 1 d U . .
H7A H 0.2173 0.1349 0.0301 0.042 Uiso 1 1 calc R . .
H7B H 0.2900 0.1280 0.1082 0.042 Uiso 1 1 calc R . .
H7C H 0.2877 0.2020 0.0712 0.042 Uiso 1 1 calc R . .
C8 C 0.0133(15) 0.1063(7) 0.0944(7) 0.035(4) Uani 1 1 d U . .
H8A H -0.0745 0.1137 0.1130 0.053 Uiso 1 1 calc R . .
H8B H 0.0780 0.0735 0.1231 0.053 Uiso 1 1 calc R . .
H8C H -0.0140 0.0872 0.0488 0.053 Uiso 1 1 calc R . .
C9 C 0.0052(14) 0.2215(6) 0.0403(7) 0.023(4) Uani 1 1 d U . .
H9A H 0.0134 0.2051 -0.0051 0.028 Uiso 1 1 calc R . .
H9B H -0.0987 0.2199 0.0436 0.028 Uiso 1 1 calc R . .
C10 C 0.0577(13) 0.2923(7) 0.0498(6) 0.016(3) Uani 1 1 d U . .
C11 C 0.0510(13) 0.3421(7) -0.0007(7) 0.022(4) Uani 1 1 d U . .
H11 H 0.0151 0.3293 -0.0463 0.026 Uiso 1 1 calc R . .
C12 C 0.0949(13) 0.4082(7) 0.0142(7) 0.023(4) Uani 1 1 d U . .
H12 H 0.0869 0.4417 -0.0210 0.028 Uiso 1 1 calc R . .
C13 C 0.1524(13) 0.4288(7) 0.0809(6) 0.021(4) Uani 1 1 d U . .
H13 H 0.1816 0.4758 0.0908 0.026 Uiso 1 1 calc R . .
C14 C 0.1658(13) 0.3795(7) 0.1318(7) 0.020(4) Uani 1 1 d U . .
H14 H 0.2083 0.3921 0.1768 0.024 Uiso 1 1 calc R . .
C15 C 0.1172(12) 0.3113(6) 0.1172(6) 0.009(3) Uani 1 1 d U . .
C16 C -0.3107(13) 0.2565(6) -0.1680(6) 0.015(3) Uani 1 1 d U . .
H16A H -0.2132 0.2347 -0.1618 0.018 Uiso 1 1 calc R . .
H16B H -0.3789 0.2217 -0.1555 0.018 Uiso 1 1 calc R . .
C17 C -0.3040(13) 0.3194(7) -0.1229(7) 0.023(4) Uani 1 1 d U . .
H17A H -0.2693 0.3049 -0.0755 0.028 Uiso 1 1 calc R . .
H17B H -0.2332 0.3533 -0.1346 0.028 Uiso 1 1 calc R . .
C18 C -0.4911(15) 0.3743(7) -0.1985(6) 0.031(4) Uani 1 1 d U . .
H18A H -0.4211 0.4089 -0.2098 0.037 Uiso 1 1 calc R . .
H18B H -0.5873 0.3974 -0.2039 0.037 Uiso 1 1 calc R . .
C19 C -0.5020(13) 0.3138(6) -0.2464(6) 0.019(4) Uani 1 1 d U . .
H19A H -0.5767 0.2807 -0.2371 0.023 Uiso 1 1 calc R . .
H19B H -0.5330 0.3309 -0.2932 0.023 Uiso 1 1 calc R . .
C20 C -0.4528(14) 0.0987(6) -0.2069(6) 0.015(3) Uani 1 1 d U . .
C21 C -0.4208(17) 0.0331(9) -0.1613(8) 0.032(4) Uani 1 1 d U . .
C22 C -0.2485(13) 0.1095(7) -0.4039(6) 0.022(4) Uani 1 1 d U . .
H22A H -0.2566 0.0765 -0.4415 0.033 Uiso 1 1 calc R . .
H22B H -0.1809 0.0909 -0.3647 0.033 Uiso 1 1 calc R . .
H22C H -0.2120 0.1544 -0.4169 0.033 Uiso 1 1 calc R . .
C23 C -0.4499(14) 0.0514(6) -0.3709(7) 0.026(4) Uani 1 1 d U . .
H23A H -0.5447 0.0572 -0.3582 0.039 Uiso 1 1 calc R . .
H23B H -0.3813 0.0301 -0.3335 0.039 Uiso 1 1 calc R . .
H23C H -0.4605 0.0212 -0.4107 0.039 Uiso 1 1 calc R . .
C24 C -0.4919(13) 0.1517(6) -0.4452(6) 0.017(3) Uani 1 1 d U . .
H24A H -0.4798 0.1277 -0.4870 0.021 Uiso 1 1 calc R . .
H24B H -0.5946 0.1465 -0.4405 0.021 Uiso 1 1 calc R . .
C25 C -0.4563(13) 0.2264(7) -0.4491(7) 0.018(4) Uani 1 1 d U . .
C26 C -0.4762(13) 0.2640(7) -0.5086(7) 0.022(4) Uani 1 1 d U . .
H26 H -0.5124 0.2414 -0.5503 0.026 Uiso 1 1 calc R . .
C27 C -0.4440(13) 0.3335(7) -0.5073(7) 0.020(4) Uani 1 1 d U . .
H27 H -0.4597 0.3587 -0.5485 0.023 Uiso 1 1 calc R . .
C28 C -0.3889(13) 0.3686(7) -0.4478(6) 0.022(4) Uani 1 1 d U . .
H28 H -0.3686 0.4172 -0.4475 0.027 Uiso 1 1 calc R . .
C29 C -0.3646(12) 0.3294(6) -0.3883(6) 0.015(3) Uani 1 1 d U . .
H29 H -0.3243 0.3519 -0.3470 0.018 Uiso 1 1 calc R . .
C30 C -0.3972(13) 0.2595(6) -0.3877(6) 0.013(3) Uani 1 1 d U . .
N1 N 0.1493(10) 0.2966(5) 0.2662(5) 0.010(3) Uani 1 1 d U . .
N2 N 0.0907(10) 0.1750(5) 0.0920(5) 0.016(3) Uani 1 1 d U . .
N3 N -0.3600(10) 0.2769(5) -0.2397(5) 0.018(3) Uani 1 1 d U . .
N4 N -0.3947(10) 0.1198(5) -0.3865(5) 0.013(3) Uani 1 1 d U . .
O1 O 0.0560(8) 0.3435(4) 0.3884(4) 0.022(2) Uani 1 1 d U . .
O2 O 0.1315(8) 0.1359(4) 0.2398(4) 0.017(2) Uani 1 1 d U . .
O3 O -0.0977(9) 0.1530(5) 0.2530(4) 0.032(2) Uani 1 1 d U . .
O4 O -0.4445(9) 0.3527(4) -0.1294(4) 0.025(2) Uani 1 1 d U . .
O5 O -0.3501(8) 0.1149(4) -0.2337(4) 0.019(2) Uani 1 1 d U . .
O6 O -0.5738(9) 0.1245(5) -0.2101(4) 0.030(3) Uani 1 1 d U . .
F1 F 0.0683(15) 0.0544(5) 0.3556(4) 0.106(5) Uani 1 1 d . . .
F2 F -0.1076(11) 0.0198(5) 0.2826(6) 0.089(4) Uani 1 1 d . . .
F3 F 0.1061(8) 0.0027(4) 0.2686(4) 0.043(2) Uani 1 1 d . . .
F4 F -0.5256(11) 0.0148(5) -0.1320(6) 0.093(4) Uani 1 1 d . . .
F5 F -0.3096(10) 0.0453(5) -0.1097(4) 0.065(3) Uani 1 1 d . . .
F6 F -0.3778(11) -0.0212(4) -0.1910(4) 0.062(3) Uani 1 1 d . . .
Pd1 Pd 0.12324(11) 0.23137(5) 0.18116(5) 0.0160(4) Uani 1 1 d . . .
Pd2 Pd -0.37605(11) 0.19441(5) -0.30966(5) 0.0172(4) 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 1.484(13) . ?
C1 C2 1.504(15) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O1 1.449(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O1 1.454(13) . ?
C3 C4 1.520(15) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N1 1.493(14) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O2 1.241(13) . ?
C5 O3 1.247(14) . ?
C5 C6 1.514(19) . ?
C6 F1 1.284(17) . ?
C6 F3 1.296(16) . ?
C6 F2 1.339(16) . ?
C7 N2 1.492(14) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N2 1.507(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.441(16) . ?
C9 N2 1.484(14) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.390(15) . ?
C10 C15 1.417(16) . ?
C11 C12 1.347(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.408(17) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(15) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(16) . ?
C14 H14 0.9500 . ?
C15 Pd1 1.998(12) . ?
C16 N3 1.487(14) . ?
C16 C17 1.504(16) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 O4 1.446(13) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 O4 1.441(14) . ?
C18 C19 1.502(16) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 N3 1.489(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 O6 1.226(13) . ?
C20 O5 1.234(13) . ?
C20 C21 1.553(18) . ?
C21 F4 1.292(15) . ?
C21 F6 1.304(16) . ?
C21 F5 1.343(16) . ?
C22 N4 1.493(14) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 N4 1.464(14) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.474(16) . ?
C24 N4 1.478(14) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.384(15) . ?
C25 C30 1.407(15) . ?
C26 C27 1.364(17) . ?
C26 H26 0.9500 . ?
C27 C28 1.386(16) . ?
C27 H27 0.9500 . ?
C28 C29 1.400(15) . ?
C28 H28 0.9500 . ?
C29 C30 1.373(16) . ?
C29 H29 0.9500 . ?
C30 Pd2 1.992(12) . ?
N1 Pd1 2.101(9) . ?
N2 Pd1 2.073(10) . ?
N3 Pd2 2.106(10) . ?
N4 Pd2 2.095(9) . ?
O2 Pd1 2.173(8) . ?
O5 Pd2 2.144(8) . ?
 
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 112.1(9) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
O1 C2 C1 110.5(9) . . ?
O1 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
O1 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O1 C3 C4 111.0(9) . . ?
O1 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
O1 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N1 C4 C3 111.8(9) . . ?
N1 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
O2 C5 O3 128.5(13) . . ?
O2 C5 C6 113.4(12) . . ?
O3 C5 C6 118.1(12) . . ?
F1 C6 F3 109.8(14) . . ?
F1 C6 F2 105.8(14) . . ?
F3 C6 F2 105.9(13) . . ?
F1 C6 C5 110.5(14) . . ?
F3 C6 C5 114.8(13) . . ?
F2 C6 C5 109.6(12) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 110.4(10) . . ?
C10 C9 H9A 109.6 . . ?
N2 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
N2 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C15 119.0(11) . . ?
C11 C10 C9 125.6(12) . . ?
C15 C10 C9 115.4(12) . . ?
C12 C11 C10 120.8(13) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 121.4(14) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 119.0(12) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 120.1(12) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C10 119.6(12) . . ?
C14 C15 Pd1 127.8(9) . . ?
C10 C15 Pd1 112.5(9) . . ?
N3 C16 C17 110.4(10) . . ?
N3 C16 H16A 109.6 . . ?
C17 C16 H16A 109.6 . . ?
N3 C16 H16B 109.6 . . ?
C17 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
O4 C17 C16 111.7(10) . . ?
O4 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
O4 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
O4 C18 C19 112.0(11) . . ?
O4 C18 H18A 109.2 . . ?
C19 C18 H18A 109.2 . . ?
O4 C18 H18B 109.2 . . ?
C19 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
N3 C19 C18 111.3(10) . . ?
N3 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
N3 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
O6 C20 O5 132.0(12) . . ?
O6 C20 C21 115.1(11) . . ?
O5 C20 C21 112.9(11) . . ?
F4 C21 F6 109.2(13) . . ?
F4 C21 F5 103.5(13) . . ?
F6 C21 F5 103.6(13) . . ?
F4 C21 C20 114.7(13) . . ?
F6 C21 C20 114.3(12) . . ?
F5 C21 C20 110.5(12) . . ?
N4 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 H23A 109.5 . . ?
N4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 N4 109.5(10) . . ?
C25 C24 H24A 109.8 . . ?
N4 C24 H24A 109.8 . . ?
C25 C24 H24B 109.8 . . ?
N4 C24 H24B 109.8 . . ?
H24A C24 H24B 108.2 . . ?
C26 C25 C30 119.7(11) . . ?
C26 C25 C24 124.0(12) . . ?
C30 C25 C24 116.3(12) . . ?
C27 C26 C25 120.0(13) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 122.1(13) . . ?
C26 C27 H27 118.9 . . ?
C28 C27 H27 118.9 . . ?
C27 C28 C29 117.3(12) . . ?
C27 C28 H28 121.4 . . ?
C29 C28 H28 121.4 . . ?
C30 C29 C28 122.0(12) . . ?
C30 C29 H29 119.0 . . ?
C28 C29 H29 119.0 . . ?
C29 C30 C25 118.8(11) . . ?
C29 C30 Pd2 129.0(10) . . ?
C25 C30 Pd2 112.3(9) . . ?
C1 N1 C4 106.8(9) . . ?
C1 N1 Pd1 114.2(7) . . ?
C4 N1 Pd1 109.7(7) . . ?
C9 N2 C7 109.8(9) . . ?
C9 N2 C8 110.5(9) . . ?
C7 N2 C8 106.6(10) . . ?
C9 N2 Pd1 105.5(7) . . ?
C7 N2 Pd1 109.9(7) . . ?
C8 N2 Pd1 114.5(8) . . ?
C16 N3 C19 108.2(9) . . ?
C16 N3 Pd2 115.3(7) . . ?
C19 N3 Pd2 110.6(7) . . ?
C23 N4 C24 110.8(9) . . ?
C23 N4 C22 108.3(9) . . ?
C24 N4 C22 108.3(9) . . ?
C23 N4 Pd2 115.5(7) . . ?
C24 N4 Pd2 105.2(7) . . ?
C22 N4 Pd2 108.6(7) . . ?
C2 O1 C3 107.8(8) . . ?
C5 O2 Pd1 116.2(8) . . ?
C18 O4 C17 108.1(9) . . ?
C20 O5 Pd2 120.4(8) . . ?
C15 Pd1 N2 81.6(4) . . ?
C15 Pd1 N1 93.4(4) . . ?
N2 Pd1 N1 174.8(4) . . ?
C15 Pd1 O2 172.7(4) . . ?
N2 Pd1 O2 91.2(3) . . ?
N1 Pd1 O2 93.8(3) . . ?
C30 Pd2 N4 81.7(4) . . ?
C30 Pd2 N3 92.7(4) . . ?
N4 Pd2 N3 174.5(4) . . ?
C30 Pd2 O5 173.3(4) . . ?
N4 Pd2 O5 91.7(3) . . ?
N3 Pd2 O5 93.8(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.466
_diffrn_reflns_theta_full              23.03
_diffrn_measured_fraction_theta_full   0.466
_refine_diff_density_max    0.546
_refine_diff_density_min   -0.643
_refine_diff_density_rms    0.090
