# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006
data_global
_journal_name_full 'Private Communication'
_journal_coden_cambridge 1078
_journal_year 2004
_journal_volume ?
_journal_page_first ?
loop_
_publ_author_name
B.Dassonneville
E.Rafii
M.Giorgi
A.Heumann
_publ_contact_author_name 'Andreas Heumann'
_publ_contact_author_email andreas.heumann@univ.u-3mrs.fr
_ccdc_publ_extra_info
;
author says structure will be published - Jan 2006 - Also requested for
Chem.Comm. B613961B. Deposited with 629162 for Chem.Comm. B613961B
;
data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 243522'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C20 H28 Cl2 N2 O Pd'
_chemical_formula_weight 489.78
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'
Pd Pd -0.9988 1.0072 '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'
O O 0.0106 0.0060 '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'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'P 21 21 21'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_cell_length_a 10.3870(1)
_cell_length_b 11.1000(1)
_cell_length_c 19.2250(3)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2216.56(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 4548
_cell_measurement_theta_min 2.12
_cell_measurement_theta_max 26.59
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_exptl_crystal_size_max .3
_exptl_crystal_size_mid .25
_exptl_crystal_size_min .15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.474
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1008
_exptl_absorpt_coefficient_mu 1.089
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method 'Phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 4548
_diffrn_reflns_av_R_equivalents 0.03
_diffrn_reflns_av_sigmaI/netI 0.0174
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 4.06
_diffrn_reflns_theta_max 26.59
_reflns_number_total 2417
_reflns_number_gt 2388
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'KappaCCD (Bruker-Nonius, 1998)'
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_publ_section_references
;
Altamore, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. and Camalli, M. J. Appl. Cryst. (1994) 27, 435-436
Bruker-Nonius (1998). Kappa CCD Reference Manual. Nonius B.V., P.O. Box 811,
2600 Av, Delft, The Netherlands.
Otwinowski, Z. and Minor, W. " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds.,
Academic Press.
Sheldrick, G.M. (1990). Acta Cryst. A46, 467-473.
Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal
structures. Univ. of G\"ottingen, Germany.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+1.3703P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack none
_refine_ls_number_reflns 2417
_refine_ls_number_parameters 234
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0253
_refine_ls_R_factor_gt 0.0249
_refine_ls_wR_factor_ref 0.0715
_refine_ls_wR_factor_gt 0.0712
_refine_ls_goodness_of_fit_ref 1.151
_refine_ls_restrained_S_all 1.151
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.001
_diffrn_measured_fraction_theta_max 0.922
_diffrn_reflns_theta_full 26.59
_diffrn_measured_fraction_theta_full 0.922
_refine_diff_density_max 0.747
_refine_diff_density_min -0.523
_refine_diff_density_rms 0.063
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 0.76708(3) 0.18535(2) 0.056154(13) 0.02754(10) Uani 1 1 d . . .
Cl1 Cl 0.91251(12) 0.09909(10) -0.01939(6) 0.0429(3) Uani 1 1 d . . .
Cl2 Cl 0.59978(11) 0.07523(10) 0.00819(6) 0.0419(3) Uani 1 1 d . . .
O22 O 0.1511(9) 0.3124(8) 0.4890(5) 0.085(2) Uiso 0.60 1 d P . .
O23 O 0.4160(17) 0.2916(13) 0.4525(8) 0.105(4) Uiso 0.40 1 d P . .
N21 N 0.9054(3) 0.2903(3) 0.10070(16) 0.0302(7) Uani 1 1 d . . .
H21 H 0.9744 0.3040 0.0684 0.036 Uiso 1 1 d R . .
N22 N 0.6419(3) 0.2849(3) 0.11697(17) 0.0302(7) Uani 1 1 d . . .
H22 H 0.5846 0.3211 0.0838 0.036 Uiso 1 1 d R . .
C1 C 0.8382(4) 0.4081(4) 0.11529(19) 0.0306(8) Uani 1 1 d . . .
H1 H 0.8140 0.4389 0.0705 0.037 Uiso 1 1 d R . .
C2 C 0.9179(5) 0.5033(4) 0.1526(3) 0.0417(10) Uani 1 1 d . . .
H2A H 0.9418 0.4724 0.1975 0.050 Uiso 1 1 d R . .
H2B H 0.9940 0.5195 0.1259 0.050 Uiso 1 1 d R . .
C3 C 0.8397(5) 0.6181(4) 0.1623(3) 0.0534(12) Uani 1 1 d . . .
H3A H 0.8898 0.6741 0.1890 0.064 Uiso 1 1 d R . .
H3B H 0.8209 0.6522 0.1176 0.064 Uiso 1 1 d R . .
C4 C 0.7131(6) 0.5926(4) 0.2006(3) 0.0529(13) Uani 1 1 d . . .
H4A H 0.7310 0.5655 0.2470 0.063 Uiso 1 1 d R . .
H4B H 0.6635 0.6655 0.2024 0.063 Uiso 1 1 d R . .
C5 C 0.6345(5) 0.4953(4) 0.1635(3) 0.0438(10) Uani 1 1 d . . .
H5A H 0.5586 0.4767 0.1898 0.053 Uiso 1 1 d R . .
H5B H 0.6102 0.5246 0.1184 0.053 Uiso 1 1 d R . .
C6 C 0.7147(4) 0.3819(3) 0.15459(19) 0.0298(8) Uani 1 1 d . . .
H6 H 0.7362 0.3533 0.2003 0.036 Uiso 1 1 d R . .
C7 C 0.9696(4) 0.2333(4) 0.1621(2) 0.0398(10) Uani 1 1 d . . .
H7A H 1.0194 0.2924 0.1867 0.048 Uiso 1 1 d R . .
H7B H 0.9035 0.2025 0.1922 0.048 Uiso 1 1 d R . .
C8 C 1.0556(4) 0.1309(4) 0.1406(2) 0.0351(9) Uani 1 1 d . . .
C9 C 1.1740(4) 0.1533(4) 0.1095(2) 0.0397(10) Uani 1 1 d . . .
H9 H 1.2020 0.2348 0.1022 0.048 Uiso 1 1 d R . .
C10 C 1.2505(5) 0.0581(5) 0.0884(2) 0.0507(11) Uani 1 1 d . . .
H10 H 1.3312 0.0742 0.0659 0.061 Uiso 1 1 d R . .
C11 C 1.2106(6) -0.0594(5) 0.0978(3) 0.0619(15) Uani 1 1 d . . .
H11 H 1.2688 -0.1230 0.0852 0.074 Uiso 1 1 d R . .
C12 C 1.0961(8) -0.0811(5) 0.1297(4) 0.0706(17) Uani 1 1 d . . .
H12 H 1.0661 -0.1624 0.1349 0.085 Uiso 1 1 d R . .
C13 C 1.0180(5) 0.0128(5) 0.1507(3) 0.0524(12) Uani 1 1 d . . .
H13 H 0.9364 -0.0027 0.1724 0.063 Uiso 1 1 d R . .
C14 C 0.5505(4) 0.2180(4) 0.1632(2) 0.0368(9) Uani 1 1 d . . .
H14A H 0.4982 0.2748 0.1881 0.044 Uiso 1 1 d R . .
H14B H 0.4964 0.1671 0.1354 0.044 Uiso 1 1 d R . .
C15 C 0.6154(4) 0.1397(4) 0.2164(2) 0.0358(9) Uani 1 1 d . . .
C16 C 0.6504(5) 0.0231(4) 0.2001(3) 0.0476(11) Uani 1 1 d . . .
H16 H 0.6337 -0.0051 0.1537 0.057 Uiso 1 1 d R . .
C17 C 0.7102(6) -0.0507(5) 0.2506(3) 0.0608(15) Uani 1 1 d . . .
H17 H 0.7310 -0.1329 0.2398 0.073 Uiso 1 1 d R . .
C18 C 0.7317(6) -0.0059(5) 0.3162(3) 0.0604(14) Uani 1 1 d . . .
H18 H 0.7734 -0.0561 0.3501 0.073 Uiso 1 1 d R . .
C19 C 0.6964(6) 0.1067(6) 0.3322(3) 0.0615(15) Uani 1 1 d . . .
H19 H 0.7158 0.1382 0.3775 0.074 Uiso 1 1 d R . .
C20 C 0.6386(5) 0.1793(5) 0.2831(2) 0.0471(10) Uani 1 1 d . . .
H20 H 0.6108 0.2584 0.2966 0.056 Uiso 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.02671(16) 0.03214(15) 0.02378(14) -0.00158(10) -0.00130(9) -0.00041(10)
Cl1 0.0413(6) 0.0489(6) 0.0384(5) -0.0121(4) 0.0118(4) -0.0042(5)
Cl2 0.0377(6) 0.0449(5) 0.0430(5) -0.0060(4) -0.0107(4) -0.0061(4)
N21 0.0257(17) 0.0378(17) 0.0270(14) -0.0051(13) 0.0001(12) 0.0005(13)
N22 0.0236(17) 0.0360(17) 0.0310(15) -0.0022(13) -0.0015(12) 0.0001(12)
C1 0.026(2) 0.038(2) 0.0277(17) -0.0007(15) 0.0020(14) -0.0014(15)
C2 0.033(2) 0.045(2) 0.046(2) -0.010(2) 0.0040(19) -0.0056(18)
C3 0.054(3) 0.040(2) 0.066(3) -0.011(2) 0.001(3) -0.008(2)
C4 0.045(3) 0.045(2) 0.069(3) -0.024(2) 0.007(2) -0.001(2)
C5 0.036(2) 0.041(2) 0.055(3) -0.011(2) 0.002(2) 0.0051(18)
C6 0.0225(19) 0.0369(18) 0.0299(17) -0.0054(14) 0.0013(14) -0.0005(15)
C7 0.032(2) 0.055(2) 0.0325(19) -0.0052(19) -0.0064(17) 0.0103(18)
C8 0.026(2) 0.046(2) 0.0334(19) 0.0006(17) -0.0029(16) 0.0032(17)
C9 0.032(2) 0.047(2) 0.040(2) 0.0017(18) -0.0012(17) -0.0009(18)
C10 0.033(3) 0.074(3) 0.045(2) -0.004(2) 0.0023(19) 0.011(2)
C11 0.060(4) 0.053(3) 0.073(4) -0.009(3) -0.003(3) 0.019(3)
C12 0.078(5) 0.046(3) 0.088(4) 0.008(3) 0.000(4) -0.001(3)
C13 0.044(3) 0.056(3) 0.057(3) 0.010(2) 0.003(2) -0.007(2)
C14 0.025(2) 0.045(2) 0.040(2) -0.0006(18) 0.0045(16) -0.0041(16)
C15 0.029(2) 0.0384(19) 0.040(2) 0.0015(17) 0.0077(17) -0.0068(16)
C16 0.048(3) 0.043(2) 0.051(3) 0.001(2) 0.013(2) -0.004(2)
C17 0.047(3) 0.046(3) 0.090(4) 0.018(3) 0.024(3) 0.006(2)
C18 0.043(3) 0.071(3) 0.066(3) 0.027(3) 0.002(3) -0.009(3)
C19 0.068(4) 0.074(4) 0.042(2) 0.015(3) -0.007(3) -0.026(3)
C20 0.055(3) 0.046(2) 0.040(2) -0.001(2) 0.0056(19) -0.013(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
Pd1 N21 2.039(3) . ?
Pd1 N22 2.069(3) . ?
Pd1 Cl1 2.3039(11) . ?
Pd1 Cl2 2.3160(11) . ?
N21 C7 1.497(5) . ?
N21 C1 1.509(5) . ?
N21 H21 0.9598 . ?
N22 C14 1.498(5) . ?
N22 C6 1.501(5) . ?
N22 H22 0.9600 . ?
C1 C6 1.517(5) . ?
C1 C2 1.522(6) . ?
C1 H1 0.9602 . ?
C2 C3 1.522(7) . ?
C2 H2A 0.9601 . ?
C2 H2B 0.9599 . ?
C3 C4 1.533(8) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9601 . ?
C4 C5 1.530(6) . ?
C4 H4A 0.9598 . ?
C4 H4B 0.9600 . ?
C5 C6 1.520(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9601 . ?
C6 H6 0.9600 . ?
C7 C8 1.504(6) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9599 . ?
C8 C13 1.381(7) . ?
C8 C9 1.389(6) . ?
C9 C10 1.384(7) . ?
C9 H9 0.9601 . ?
C10 C11 1.380(8) . ?
C10 H10 0.9599 . ?
C11 C12 1.359(9) . ?
C11 H11 0.9600 . ?
C12 C13 1.382(8) . ?
C12 H12 0.9600 . ?
C13 H13 0.9600 . ?
C14 C15 1.501(6) . ?
C14 H14A 0.9599 . ?
C14 H14B 0.9602 . ?
C15 C20 1.377(6) . ?
C15 C16 1.381(7) . ?
C16 C17 1.414(8) . ?
C16 H16 0.9601 . ?
C17 C18 1.374(9) . ?
C17 H17 0.9600 . ?
C18 C19 1.339(9) . ?
C18 H18 0.9600 . ?
C19 C20 1.380(8) . ?
C19 H19 0.9600 . ?
C20 H20 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N21 Pd1 N22 84.28(13) . . ?
N21 Pd1 Cl1 92.31(9) . . ?
N22 Pd1 Cl1 172.08(10) . . ?
N21 Pd1 Cl2 176.16(10) . . ?
N22 Pd1 Cl2 92.02(9) . . ?
Cl1 Pd1 Cl2 91.24(4) . . ?
C7 N21 C1 115.2(3) . . ?
C7 N21 Pd1 113.8(3) . . ?
C1 N21 Pd1 104.3(2) . . ?
C7 N21 H21 104.2 . . ?
C1 N21 H21 109.2 . . ?
Pd1 N21 H21 110.2 . . ?
C14 N22 C6 112.9(3) . . ?
C14 N22 Pd1 118.0(2) . . ?
C6 N22 Pd1 109.8(2) . . ?
C14 N22 H22 102.0 . . ?
C6 N22 H22 109.4 . . ?
Pd1 N22 H22 103.8 . . ?
N21 C1 C6 108.5(3) . . ?
N21 C1 C2 115.9(3) . . ?
C6 C1 C2 111.0(3) . . ?
N21 C1 H1 105.2 . . ?
C6 C1 H1 107.1 . . ?
C2 C1 H1 108.6 . . ?
C1 C2 C3 110.4(4) . . ?
C1 C2 H2A 108.5 . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2B 109.0 . . ?
C3 C2 H2B 110.4 . . ?
H2A C2 H2B 109.5 . . ?
C2 C3 C4 111.2(4) . . ?
C2 C3 H3A 108.6 . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 109.5 . . ?
C5 C4 C3 111.4(4) . . ?
C5 C4 H4A 108.3 . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4B 109.0 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 109.5 . . ?
C6 C5 C4 110.2(4) . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5A 110.2 . . ?
C6 C5 H5B 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 109.5 . . ?
N22 C6 C1 108.9(3) . . ?
N22 C6 C5 111.9(3) . . ?
C1 C6 C5 111.1(3) . . ?
N22 C6 H6 108.7 . . ?
C1 C6 H6 108.8 . . ?
C5 C6 H6 107.3 . . ?
N21 C7 C8 111.5(3) . . ?
N21 C7 H7A 109.8 . . ?
C8 C7 H7A 109.4 . . ?
N21 C7 H7B 107.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 109.5 . . ?
C13 C8 C9 118.7(4) . . ?
C13 C8 C7 120.7(4) . . ?
C9 C8 C7 120.6(4) . . ?
C10 C9 C8 119.8(4) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 120.7(5) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.4 . . ?
C12 C11 C10 119.3(5) . . ?
C12 C11 H11 122.2 . . ?
C10 C11 H11 118.2 . . ?
C11 C12 C13 120.8(5) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.2 . . ?
C8 C13 C12 120.6(5) . . ?
C8 C13 H13 118.7 . . ?
C12 C13 H13 120.7 . . ?
N22 C14 C15 114.0(3) . . ?
N22 C14 H14A 109.2 . . ?
C15 C14 H14A 107.2 . . ?
N22 C14 H14B 109.4 . . ?
C15 C14 H14B 107.5 . . ?
H14A C14 H14B 109.5 . . ?
C20 C15 C16 117.7(5) . . ?
C20 C15 C14 121.8(4) . . ?
C16 C15 C14 120.4(4) . . ?
C15 C16 C17 120.2(5) . . ?
C15 C16 H16 117.9 . . ?
C17 C16 H16 121.9 . . ?
C18 C17 C16 119.5(5) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.0 . . ?
C19 C18 C17 120.3(5) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 120.5(5) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 120.0 . . ?
C15 C20 C19 121.8(5) . . ?
C15 C20 H20 119.5 . . ?
C19 C20 H20 118.6 . . ?
# Attachment 'ds8c.cif'
data_2
_database_code_depnum_ccdc_archive 'CCDC 629162'
_audit_update_record
;
2006-11-24 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C20 H24 Cl2 F2 N2 Pd1'
_chemical_formula_weight 507.73
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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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 'P 21'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 14.214(5)
_cell_length_b 9.039(1)
_cell_length_c 16.311(3)
_cell_angle_alpha 90.00
_cell_angle_beta 100.552(8)
_cell_angle_gamma 90.00
_cell_volume 2060.2(9)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 14479
_cell_measurement_theta_min 0.00
_cell_measurement_theta_max 25.97
_exptl_crystal_description prism
_exptl_crystal_colour orange
_exptl_crystal_size_max .3
_exptl_crystal_size_mid .2
_exptl_crystal_size_min .05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.643
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1024
_exptl_absorpt_coefficient_mu 1.189
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.860
_exptl_absorpt_correction_T_max 0.944
_exptl_absorpt_process_details
;
Sortav (Blessing, 1997)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method 'Phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number none
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 14477
_diffrn_reflns_av_R_equivalents 0.07
_diffrn_reflns_av_sigmaI/netI 0.105
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 1.27
_diffrn_reflns_theta_max 25.97
_reflns_number_total 7681
_reflns_number_gt 6291
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'KappaCCD (Bruker-Nonius, 1998)'
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. and Camalli, M. J. Appl. Cryst. (1994). 27, 435-436
Blessing, R. H. (1997). J. Appl. Cryst. 30, 421--426.
Bruker-Nonius (1998). Kappa CCD Reference Manual. Nonius B.V., P.O. Box
811, 2600 Av, Delft, The Netherlands.
Flack, H. D. (1983). Acta Cryst. A39, 876--881.
Otwinowski, Z. and Minor, W. " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds.,
Academic Press.
Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of crystal
structures. Univ. of G\"ottingen, Germany.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+2.3231P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_chemical_absolute_configuration rmad
_refine_ls_abs_structure_details 'Flack (1983); 3506 Friedel pairs'
_refine_ls_abs_structure_Flack 0.00(4)
_refine_ls_number_reflns 7681
_refine_ls_number_parameters 487
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0668
_refine_ls_R_factor_gt 0.0482
_refine_ls_wR_factor_ref 0.1094
_refine_ls_wR_factor_gt 0.0965
_refine_ls_goodness_of_fit_ref 1.048
_refine_ls_restrained_S_all 1.048
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full 25.97
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max 0.785
_refine_diff_density_min -0.757
_refine_diff_density_rms 0.093
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 0.39385(4) 0.38715(5) 0.73909(3) 0.03294(16) Uani 1 1 d . . .
Pd2 Pd 0.40412(4) 0.10715(5) 0.23267(3) 0.03109(15) Uani 1 1 d . . .
Cl1 Cl 0.49884(16) 0.2089(2) 0.80496(13) 0.0469(5) Uani 1 1 d . . .
Cl2 Cl 0.37061(15) 0.4894(3) 0.86458(12) 0.0477(5) Uani 1 1 d . . .
Cl3 Cl 0.50806(16) 0.2962(2) 0.28418(14) 0.0467(5) Uani 1 1 d . . .
Cl4 Cl 0.39463(14) 0.0245(2) 0.36569(12) 0.0413(5) Uani 1 1 d . . .
F1 F 0.0434(4) -0.0930(7) 0.5897(4) 0.0786(17) Uani 1 1 d . . .
F2 F -0.0579(5) 0.1272(8) 0.6860(5) 0.103(2) Uani 1 1 d . . .
F3 F -0.0618(5) 0.3158(9) 0.2137(4) 0.107(3) Uani 1 1 d . . .
F4 F 0.0211(5) 0.5173(11) 0.0860(5) 0.125(3) Uani 1 1 d . . .
N1 N 0.4098(4) 0.3170(7) 0.6223(4) 0.0309(14) Uani 1 1 d . . .
H1N H 0.4693 0.3478 0.6169 0.037 Uiso 1 1 calc R . .
N2 N 0.3144(5) 0.5579(7) 0.6758(4) 0.0368(17) Uani 1 1 d . . .
H2N H 0.3451 0.6399 0.6994 0.044 Uiso 1 1 calc R . .
N3 N 0.4220(4) 0.1573(7) 0.1142(4) 0.0358(16) Uani 1 1 d . . .
H3N H 0.4866 0.1548 0.1174 0.043 Uiso 1 1 calc R . .
N4 N 0.3162(5) -0.0589(8) 0.1757(4) 0.0350(17) Uani 1 1 d . . .
H4N H 0.3544 -0.1404 0.1809 0.042 Uiso 1 1 calc R . .
C1 C 0.3423(5) 0.4015(8) 0.5568(4) 0.0349(15) Uani 1 1 d . . .
H1 H 0.2785 0.3570 0.5498 0.042 Uiso 1 1 calc R . .
C2 C 0.3381(5) 0.5587(8) 0.5890(4) 0.0347(17) Uani 1 1 d . . .
H2 H 0.4027 0.5998 0.5942 0.042 Uiso 1 1 calc R . .
C3 C 0.2728(7) 0.6558(10) 0.5275(5) 0.054(3) Uani 1 1 d . . .
H3A H 0.2723 0.7553 0.5497 0.065 Uiso 1 1 calc R . .
H3B H 0.2080 0.6174 0.5193 0.065 Uiso 1 1 calc R . .
C4 C 0.3072(8) 0.6600(10) 0.4436(5) 0.063(3) Uani 1 1 d . . .
H4A H 0.3697 0.7065 0.4508 0.076 Uiso 1 1 calc R . .
H4B H 0.2631 0.7182 0.4039 0.076 Uiso 1 1 calc R . .
C5 C 0.3133(7) 0.5018(10) 0.4097(5) 0.059(2) Uani 1 1 d . . .
H5A H 0.2494 0.4602 0.3961 0.070 Uiso 1 1 calc R . .
H5B H 0.3396 0.5054 0.3590 0.070 Uiso 1 1 calc R . .
C6 C 0.3755(6) 0.4029(11) 0.4729(5) 0.050(2) Uani 1 1 d . . .
H6A H 0.4412 0.4374 0.4810 0.060 Uiso 1 1 calc R . .
H6B H 0.3739 0.3028 0.4512 0.060 Uiso 1 1 calc R . .
C7 C 0.4086(6) 0.1528(8) 0.6039(5) 0.0379(19) Uani 1 1 d . . .
H7A H 0.4285 0.1367 0.5508 0.045 Uiso 1 1 calc R . .
H7B H 0.4541 0.1031 0.6467 0.045 Uiso 1 1 calc R . .
C8 C 0.2156(6) 0.5788(10) 0.6912(5) 0.046(2) Uani 1 1 d . . .
H8A H 0.1846 0.6524 0.6521 0.056 Uiso 1 1 calc R . .
H8B H 0.2201 0.6201 0.7467 0.056 Uiso 1 1 calc R . .
C9 C 0.3105(5) 0.0868(8) 0.6010(4) 0.0327(16) Uani 1 1 d . . .
C10 C 0.2812(6) 0.0404(10) 0.6738(5) 0.046(2) Uani 1 1 d . . .
H10 H 0.3223 0.0496 0.7249 0.055 Uiso 1 1 calc R . .
C11 C 0.1914(6) -0.0189(10) 0.6699(6) 0.050(2) Uani 1 1 d . . .
H11 H 0.1709 -0.0501 0.7180 0.060 Uiso 1 1 calc R . .
C12 C 0.1325(6) -0.0312(9) 0.5931(5) 0.046(2) Uani 1 1 d . . .
C13 C 0.1589(6) 0.0135(9) 0.5205(5) 0.046(2) Uani 1 1 d . . .
H13 H 0.1172 0.0046 0.4696 0.056 Uiso 1 1 calc R . .
C14 C 0.2482(6) 0.0716(8) 0.5249(5) 0.0389(19) Uani 1 1 d . . .
H14 H 0.2679 0.1016 0.4762 0.047 Uiso 1 1 calc R . .
C15 C 0.1503(6) 0.4438(9) 0.6849(5) 0.043(2) Uani 1 1 d . . .
C16 C 0.1383(6) 0.3777(14) 0.7585(5) 0.060(2) Uani 1 1 d . . .
H16 H 0.1764 0.4064 0.8086 0.072 Uiso 1 1 calc R . .
C17 C 0.0687(9) 0.2672(14) 0.7580(7) 0.075(3) Uani 1 1 d . . .
H17 H 0.0612 0.2213 0.8075 0.090 Uiso 1 1 calc R . .
C18 C 0.0119(7) 0.2276(11) 0.6840(8) 0.066(3) Uani 1 1 d . . .
C19 C 0.0224(7) 0.2889(12) 0.6101(7) 0.066(3) Uani 1 1 d . . .
H19 H -0.0155 0.2587 0.5603 0.079 Uiso 1 1 calc R . .
C20 C 0.0903(6) 0.3969(10) 0.6114(6) 0.055(2) Uani 1 1 d . . .
H20 H 0.0970 0.4410 0.5612 0.066 Uiso 1 1 calc R . .
C21 C 0.3868(5) 0.0255(9) 0.0610(4) 0.0375(16) Uani 1 1 d . . .
H21 H 0.4339 -0.0533 0.0772 0.045 Uiso 1 1 calc R . .
C22 C 0.3817(6) 0.0501(11) -0.0333(5) 0.051(2) Uani 1 1 d . . .
H22A H 0.3369 0.1290 -0.0528 0.061 Uiso 1 1 calc R . .
H22B H 0.4441 0.0785 -0.0440 0.061 Uiso 1 1 calc R . .
C23 C 0.3491(7) -0.0929(13) -0.0794(5) 0.066(3) Uani 1 1 d . . .
H23A H 0.3442 -0.0776 -0.1389 0.079 Uiso 1 1 calc R . .
H23B H 0.3965 -0.1695 -0.0622 0.079 Uiso 1 1 calc R . .
C24 C 0.2539(6) -0.1429(13) -0.0618(5) 0.067(3) Uani 1 1 d . . .
H24A H 0.2348 -0.2337 -0.0920 0.080 Uiso 1 1 calc R . .
H24B H 0.2059 -0.0682 -0.0808 0.080 Uiso 1 1 calc R . .
C25 C 0.2601(7) -0.1695(11) 0.0333(5) 0.050(2) Uani 1 1 d . . .
H25A H 0.1976 -0.1973 0.0441 0.060 Uiso 1 1 calc R . .
H25B H 0.3041 -0.2501 0.0514 0.060 Uiso 1 1 calc R . .
C26 C 0.2948(5) -0.0288(9) 0.0827(4) 0.0354(17) Uani 1 1 d . . .
H26 H 0.2458 0.0485 0.0705 0.042 Uiso 1 1 calc R . .
C27 C 0.3944(6) 0.3106(10) 0.0819(5) 0.045(2) Uani 1 1 d . . .
H27A H 0.4041 0.3167 0.0246 0.054 Uiso 1 1 calc R . .
H27B H 0.4374 0.3811 0.1142 0.054 Uiso 1 1 calc R . .
C28 C 0.2921(6) 0.3568(9) 0.0844(5) 0.044(2) Uani 1 1 d . . .
C29 C 0.2219(7) 0.3550(12) 0.0128(6) 0.065(3) Uani 1 1 d . . .
H29 H 0.2371 0.3186 -0.0365 0.078 Uiso 1 1 calc R . .
C30 C 0.1326(7) 0.4046(13) 0.0128(7) 0.076(3) Uani 1 1 d . . .
H30 H 0.0864 0.4010 -0.0355 0.091 Uiso 1 1 calc R . .
C31 C 0.1112(8) 0.4592(13) 0.0835(8) 0.079(3) Uani 1 1 d . . .
C32 C 0.1784(8) 0.4695(12) 0.1586(7) 0.071(3) Uani 1 1 d . . .
H32 H 0.1622 0.5098 0.2066 0.085 Uiso 1 1 calc R . .
C33 C 0.2704(7) 0.4164(10) 0.1575(6) 0.055(2) Uani 1 1 d . . .
H33 H 0.3171 0.4208 0.2054 0.066 Uiso 1 1 calc R . .
C34 C 0.2298(5) -0.1066(12) 0.2118(5) 0.0455(19) Uani 1 1 d . . .
H34A H 0.2007 -0.1916 0.1807 0.055 Uiso 1 1 calc R . .
H34B H 0.2514 -0.1377 0.2691 0.055 Uiso 1 1 calc R . .
C35 C 0.1551(5) 0.0112(9) 0.2103(5) 0.0404(19) Uani 1 1 d . . .
C36 C 0.0836(6) 0.0394(11) 0.1402(5) 0.056(2) Uani 1 1 d . . .
H36 H 0.0845 -0.0131 0.0913 0.068 Uiso 1 1 calc R . .
C37 C 0.0115(6) 0.1428(13) 0.1413(6) 0.068(3) Uani 1 1 d . . .
H37 H -0.0352 0.1594 0.0942 0.082 Uiso 1 1 calc R . .
C38 C 0.0110(7) 0.2178(13) 0.2118(6) 0.066(3) Uani 1 1 d . . .
C39 C 0.0792(8) 0.1961(16) 0.2838(7) 0.081(4) Uani 1 1 d . . .
H39 H 0.0764 0.2489 0.3322 0.097 Uiso 1 1 calc R . .
C40 C 0.1506(7) 0.0949(16) 0.2814(5) 0.069(3) Uani 1 1 d . . .
H40 H 0.1975 0.0816 0.3287 0.082 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0377(3) 0.0345(3) 0.0263(3) 0.0012(3) 0.0049(2) -0.0046(3)
Pd2 0.0356(3) 0.0325(3) 0.0247(3) 0.0020(3) 0.0042(2) 0.0026(3)
Cl1 0.0545(13) 0.0412(12) 0.0394(11) 0.0080(9) -0.0060(9) -0.0049(9)
Cl2 0.0481(12) 0.0658(15) 0.0308(10) -0.0080(9) 0.0117(9) -0.0083(10)
Cl3 0.0533(12) 0.0316(11) 0.0502(12) 0.0004(9) -0.0037(10) -0.0042(9)
Cl4 0.0479(11) 0.0504(12) 0.0272(9) 0.0018(8) 0.0107(8) 0.0055(9)
F1 0.062(3) 0.091(4) 0.085(4) 0.003(3) 0.019(3) -0.032(3)
F2 0.072(4) 0.095(5) 0.144(6) 0.015(5) 0.026(4) -0.037(4)
F3 0.070(4) 0.160(7) 0.089(5) -0.037(5) 0.006(3) 0.054(4)
F4 0.073(4) 0.175(8) 0.132(6) 0.015(6) 0.032(4) 0.063(5)
N1 0.033(3) 0.022(3) 0.036(3) 0.001(2) 0.004(3) 0.001(2)
N2 0.043(4) 0.030(4) 0.036(4) -0.001(3) 0.004(3) -0.001(3)
N3 0.033(3) 0.044(4) 0.029(3) 0.009(3) 0.005(3) 0.003(3)
N4 0.036(4) 0.042(4) 0.027(4) 0.004(3) 0.006(3) 0.008(3)
C1 0.043(4) 0.035(4) 0.026(3) 0.001(3) 0.003(3) -0.007(3)
C2 0.044(4) 0.029(4) 0.032(4) -0.001(3) 0.008(3) -0.005(3)
C3 0.076(7) 0.037(5) 0.051(6) 0.015(4) 0.012(5) 0.010(4)
C4 0.086(7) 0.055(6) 0.046(5) 0.017(4) 0.005(5) 0.001(5)
C5 0.088(7) 0.057(6) 0.028(4) 0.001(4) 0.003(4) 0.004(5)
C6 0.069(5) 0.049(5) 0.035(4) 0.006(4) 0.016(4) -0.001(5)
C7 0.046(5) 0.029(4) 0.039(4) -0.004(3) 0.010(4) 0.000(3)
C8 0.045(5) 0.046(6) 0.051(5) -0.001(4) 0.016(4) 0.018(4)
C9 0.042(4) 0.019(4) 0.037(4) -0.001(3) 0.005(3) 0.000(3)
C10 0.061(6) 0.046(5) 0.029(4) 0.006(4) 0.004(4) -0.009(4)
C11 0.052(5) 0.050(5) 0.048(5) 0.004(4) 0.012(4) -0.016(4)
C12 0.040(5) 0.046(5) 0.053(5) -0.004(4) 0.008(4) -0.016(4)
C13 0.048(5) 0.047(5) 0.041(5) -0.004(4) 0.002(4) -0.011(4)
C14 0.054(5) 0.030(4) 0.034(4) 0.000(3) 0.011(4) -0.008(3)
C15 0.038(4) 0.044(5) 0.048(5) 0.003(4) 0.008(4) 0.007(3)
C16 0.063(6) 0.076(7) 0.043(5) 0.008(5) 0.017(4) -0.010(6)
C17 0.079(8) 0.091(8) 0.061(7) 0.019(6) 0.028(6) -0.025(6)
C18 0.052(6) 0.059(6) 0.089(8) 0.002(6) 0.017(5) -0.007(5)
C19 0.040(5) 0.067(7) 0.085(8) 0.004(6) 0.000(5) 0.005(4)
C20 0.063(5) 0.043(5) 0.060(5) 0.012(4) 0.014(4) 0.006(5)
C21 0.042(4) 0.042(4) 0.030(4) 0.003(3) 0.012(3) 0.003(3)
C22 0.056(5) 0.072(7) 0.025(4) 0.007(4) 0.009(4) 0.006(4)
C23 0.080(7) 0.091(8) 0.028(4) -0.006(5) 0.012(4) 0.012(6)
C24 0.057(5) 0.104(9) 0.036(4) -0.020(5) -0.001(4) 0.016(6)
C25 0.045(5) 0.066(7) 0.038(5) -0.010(4) 0.004(4) 0.000(4)
C26 0.032(4) 0.050(5) 0.024(4) 0.003(3) 0.005(3) 0.003(3)
C27 0.045(5) 0.046(5) 0.044(5) 0.013(4) 0.011(4) 0.002(4)
C28 0.050(5) 0.042(6) 0.040(4) 0.009(4) 0.012(4) 0.010(4)
C29 0.069(6) 0.078(8) 0.043(5) 0.012(5) -0.003(4) 0.022(5)
C30 0.055(6) 0.092(8) 0.074(7) 0.015(7) -0.006(5) 0.022(6)
C31 0.060(7) 0.087(8) 0.088(8) 0.021(7) 0.013(6) 0.028(6)
C32 0.086(8) 0.068(7) 0.069(7) -0.004(5) 0.040(6) 0.013(6)
C33 0.062(6) 0.050(6) 0.049(5) 0.002(4) 0.005(4) 0.012(4)
C34 0.040(4) 0.050(5) 0.048(4) -0.003(5) 0.012(4) -0.009(4)
C35 0.030(4) 0.054(5) 0.038(4) -0.001(4) 0.009(3) -0.006(4)
C36 0.044(5) 0.078(7) 0.044(5) -0.018(4) 0.000(4) -0.008(5)
C37 0.037(5) 0.097(9) 0.061(6) -0.021(5) -0.013(4) 0.010(5)
C38 0.043(5) 0.096(8) 0.062(6) -0.016(6) 0.014(5) 0.020(5)
C39 0.062(7) 0.127(11) 0.054(6) -0.029(7) 0.016(5) 0.015(7)
C40 0.049(5) 0.115(9) 0.040(5) -0.017(6) 0.003(4) 0.008(6)
_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 N1 2.059(6) . ?
Pd1 N2 2.073(7) . ?
Pd1 Cl1 2.322(2) . ?
Pd1 Cl2 2.324(2) . ?
Pd2 N3 2.045(6) . ?
Pd2 N4 2.062(7) . ?
Pd2 Cl3 2.314(2) . ?
Pd2 Cl4 2.322(2) . ?
F1 C12 1.376(9) . ?
F2 C18 1.350(11) . ?
F3 C38 1.368(11) . ?
F4 C31 1.392(11) . ?
N1 C1 1.507(8) . ?
N1 C7 1.513(9) . ?
N1 H1N 0.9100 . ?
N2 C8 1.482(10) . ?
N2 C2 1.514(9) . ?
N2 H2N 0.9100 . ?
N3 C21 1.505(9) . ?
N3 C27 1.508(10) . ?
N3 H3N 0.9100 . ?
N4 C26 1.516(9) . ?
N4 C34 1.519(9) . ?
N4 H4N 0.9100 . ?
C1 C2 1.520(10) . ?
C1 C6 1.527(9) . ?
C1 H1 0.9800 . ?
C2 C3 1.515(11) . ?
C2 H2 0.9800 . ?
C3 C4 1.536(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.541(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.520(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C9 1.510(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C15 1.526(12) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C14 1.393(10) . ?
C9 C10 1.393(10) . ?
C10 C11 1.376(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(12) . ?
C11 H11 0.9300 . ?
C12 C13 1.368(11) . ?
C13 C14 1.364(10) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.380(12) . ?
C15 C20 1.404(12) . ?
C16 C17 1.405(15) . ?
C16 H16 0.9300 . ?
C17 C18 1.371(15) . ?
C17 H17 0.9300 . ?
C18 C19 1.359(14) . ?
C19 C20 1.370(13) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C26 1.499(10) . ?
C21 C22 1.542(9) . ?
C21 H21 0.9800 . ?
C22 C23 1.524(14) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.503(13) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.555(11) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.538(11) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26 0.9800 . ?
C27 C28 1.521(10) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.390(11) . ?
C28 C33 1.394(11) . ?
C29 C30 1.347(12) . ?
C29 H29 0.9300 . ?
C30 C31 1.339(14) . ?
C30 H30 0.9300 . ?
C31 C32 1.411(15) . ?
C32 C33 1.395(13) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C35 1.500(12) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C40 1.397(12) . ?
C35 C36 1.408(11) . ?
C36 C37 1.389(13) . ?
C36 H36 0.9300 . ?
C37 C38 1.336(13) . ?
C37 H37 0.9300 . ?
C38 C39 1.393(14) . ?
C39 C40 1.372(16) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
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 Pd1 N2 84.9(2) . . ?
N1 Pd1 Cl1 92.52(17) . . ?
N2 Pd1 Cl1 173.07(18) . . ?
N1 Pd1 Cl2 174.13(18) . . ?
N2 Pd1 Cl2 89.44(18) . . ?
Cl1 Pd1 Cl2 92.94(8) . . ?
N3 Pd2 N4 84.6(3) . . ?
N3 Pd2 Cl3 89.9(2) . . ?
N4 Pd2 Cl3 174.29(18) . . ?
N3 Pd2 Cl4 173.04(19) . . ?
N4 Pd2 Cl4 93.03(18) . . ?
Cl3 Pd2 Cl4 92.34(8) . . ?
C1 N1 C7 112.0(6) . . ?
C1 N1 Pd1 109.7(4) . . ?
C7 N1 Pd1 119.1(5) . . ?
C1 N1 H1N 104.9 . . ?
C7 N1 H1N 104.9 . . ?
Pd1 N1 H1N 104.9 . . ?
C8 N2 C2 122.6(7) . . ?
C8 N2 Pd1 117.2(5) . . ?
C2 N2 Pd1 106.0(4) . . ?
C8 N2 H2N 102.7 . . ?
C2 N2 H2N 102.7 . . ?
Pd1 N2 H2N 102.7 . . ?
C21 N3 C27 119.2(6) . . ?
C21 N3 Pd2 106.5(4) . . ?
C27 N3 Pd2 117.7(5) . . ?
C21 N3 H3N 103.8 . . ?
C27 N3 H3N 103.8 . . ?
Pd2 N3 H3N 103.8 . . ?
C26 N4 C34 114.2(6) . . ?
C26 N4 Pd2 108.4(4) . . ?
C34 N4 Pd2 119.9(5) . . ?
C26 N4 H4N 104.2 . . ?
C34 N4 H4N 104.2 . . ?
Pd2 N4 H4N 104.2 . . ?
N1 C1 C2 106.8(5) . . ?
N1 C1 C6 112.3(6) . . ?
C2 C1 C6 109.9(6) . . ?
N1 C1 H1 109.3 . . ?
C2 C1 H1 109.3 . . ?
C6 C1 H1 109.3 . . ?
N2 C2 C3 114.1(6) . . ?
N2 C2 C1 110.4(6) . . ?
C3 C2 C1 111.7(6) . . ?
N2 C2 H2 106.7 . . ?
C3 C2 H2 106.7 . . ?
C1 C2 H2 106.7 . . ?
C2 C3 C4 110.4(8) . . ?
C2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C3 C4 C5 110.1(7) . . ?
C3 C4 H4A 109.6 . . ?
C5 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 C4 111.5(7) . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 C1 112.1(7) . . ?
C5 C6 H6A 109.2 . . ?
C1 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C1 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C9 C7 N1 111.7(6) . . ?
C9 C7 H7A 109.3 . . ?
N1 C7 H7A 109.3 . . ?
C9 C7 H7B 109.3 . . ?
N1 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
N2 C8 C15 118.0(7) . . ?
N2 C8 H8A 107.8 . . ?
C15 C8 H8A 107.8 . . ?
N2 C8 H8B 107.8 . . ?
C15 C8 H8B 107.8 . . ?
H8A C8 H8B 107.1 . . ?
C14 C9 C10 119.3(7) . . ?
C14 C9 C7 120.0(6) . . ?
C10 C9 C7 120.7(7) . . ?
C11 C10 C9 119.8(8) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 118.6(8) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C13 C12 F1 118.7(8) . . ?
C13 C12 C11 123.1(7) . . ?
F1 C12 C11 118.2(7) . . ?
C14 C13 C12 117.9(7) . . ?
C14 C13 H13 121.0 . . ?
C12 C13 H13 121.0 . . ?
C13 C14 C9 121.3(7) . . ?
C13 C14 H14 119.4 . . ?
C9 C14 H14 119.4 . . ?
C16 C15 C20 117.4(8) . . ?
C16 C15 C8 117.2(8) . . ?
C20 C15 C8 124.5(8) . . ?
C15 C16 C17 120.1(9) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C18 C17 C16 119.4(9) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
F2 C18 C19 119.7(10) . . ?
F2 C18 C17 118.1(10) . . ?
C19 C18 C17 122.1(10) . . ?
C18 C19 C20 117.9(10) . . ?
C18 C19 H19 121.0 . . ?
C20 C19 H19 121.0 . . ?
C19 C20 C15 122.9(9) . . ?
C19 C20 H20 118.5 . . ?
C15 C20 H20 118.5 . . ?
C26 C21 N3 109.6(6) . . ?
C26 C21 C22 113.5(6) . . ?
N3 C21 C22 114.3(6) . . ?
C26 C21 H21 106.3 . . ?
N3 C21 H21 106.3 . . ?
C22 C21 H21 106.3 . . ?
C23 C22 C21 108.9(7) . . ?
C23 C22 H22A 109.9 . . ?
C21 C22 H22A 109.9 . . ?
C23 C22 H22B 109.9 . . ?
C21 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C24 C23 C22 111.3(8) . . ?
C24 C23 H23A 109.4 . . ?
C22 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C23 C24 C25 110.4(7) . . ?
C23 C24 H24A 109.6 . . ?
C25 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
C25 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C26 C25 C24 110.4(8) . . ?
C26 C25 H25A 109.6 . . ?
C24 C25 H25A 109.6 . . ?
C26 C25 H25B 109.6 . . ?
C24 C25 H25B 109.6 . . ?
H25A C25 H25B 108.1 . . ?
C21 C26 N4 105.7(5) . . ?
C21 C26 C25 110.9(6) . . ?
N4 C26 C25 111.3(6) . . ?
C21 C26 H26 109.6 . . ?
N4 C26 H26 109.6 . . ?
C25 C26 H26 109.6 . . ?
N3 C27 C28 115.6(6) . . ?
N3 C27 H27A 108.4 . . ?
C28 C27 H27A 108.4 . . ?
N3 C27 H27B 108.4 . . ?
C28 C27 H27B 108.4 . . ?
H27A C27 H27B 107.4 . . ?
C29 C28 C33 119.1(8) . . ?
C29 C28 C27 121.1(7) . . ?
C33 C28 C27 119.4(8) . . ?
C30 C29 C28 121.8(9) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C31 C30 C29 119.0(10) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C30 C31 F4 121.3(10) . . ?
C30 C31 C32 123.2(9) . . ?
F4 C31 C32 115.5(10) . . ?
C33 C32 C31 116.9(9) . . ?
C33 C32 H32 121.5 . . ?
C31 C32 H32 121.5 . . ?
C28 C33 C32 119.9(9) . . ?
C28 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 N4 114.3(8) . . ?
C35 C34 H34A 108.7 . . ?
N4 C34 H34A 108.7 . . ?
C35 C34 H34B 108.7 . . ?
N4 C34 H34B 108.7 . . ?
H34A C34 H34B 107.6 . . ?
C40 C35 C36 116.1(8) . . ?
C40 C35 C34 120.7(8) . . ?
C36 C35 C34 123.1(8) . . ?
C37 C36 C35 122.5(8) . . ?
C37 C36 H36 118.8 . . ?
C35 C36 H36 118.8 . . ?
C38 C37 C36 118.2(9) . . ?
C38 C37 H37 120.9 . . ?
C36 C37 H37 120.9 . . ?
C37 C38 F3 118.2(9) . . ?
C37 C38 C39 122.8(9) . . ?
F3 C38 C39 119.0(9) . . ?
C40 C39 C38 118.3(10) . . ?
C40 C39 H39 120.8 . . ?
C38 C39 H39 120.8 . . ?
C39 C40 C35 122.1(9) . . ?
C39 C40 H40 119.0 . . ?
C35 C40 H40 119.0 . . ?