#_______________________________________________________________________
#
# Requested by: Takeru Furuya and Tobias Ritter
# Harvard University
# Department of Chemistry and Chemical Biology
# 12 Oxford Street
# Cambridge, MA 02138
# Tel: (617) 496-0750
# Fax: (617) 496-4591
# Email: ritter@chemistry.harvard.edu
#
# Crystallography by: Douglas M. Ho, Takeru Furuya and Jessica Y. Wu
# Harvard University
# Department of Chemistry and Chemical Biology
# 12 Oxford Street, B05-B06
# Cambridge, MA 02138
# Tel: (617) 495-0787
# Fax: (617) 496-8783
# Email: ho@chemistry.harvard.edu
#
# Comments: compound11 = [PdF2(C17H12N3O4S)(C13H8N)] . C2H3N
# = (Benzo[h]quinolinato){(2-nitrophenyl-
# sulfonyl)[(2-(pyridin-2-yl)phenyl]amido}-
# difluoropalladium(IV) Acetonitrile Solvate
# at 193(2) K
#
# This compound crystallizes as orange prisms
# from acetonitrile in the monoclinic space
# group P2(1)/n (No. 14) with 4 molecules per
# unit cell.
#
# Version date: April 25, 2008
#_______________________________________________________________________
data_compound_3
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
(Benzo[h]quinolinato){(2-nitrophenyl-sulfonyl)[(2-(pyridine-2-yl)phenyl]
amido}-difluoropalladium(IV) Acetonitrile Solvate
;
_chemical_name_common 'TF04054'
_chemical_formula_iupac
;
[Pd F2 (C17 H12 N3 O4 S) (C13 H8 N)] . (C2 H3 N)
;
_chemical_formula_moiety 'C30 H20 F2 N4 O4 Pd S, C2 H3 N'
_chemical_formula_structural
;
(Pd F2 (C17 H12 N3 O4 S) (C13 H8 N)) (C2 H3 N)
;
_chemical_formula_analytical ?
_chemical_formula_sum 'C32 H23 F2 N5 O4 Pd S'
_chemical_formula_weight 718.01
_chemical_melting_point '143\%C dec.'
_chemical_compound_source 'chemical synthesis'
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'
'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_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.0089(3)
_cell_length_b 13.3937(4)
_cell_length_c 21.0503(7)
_cell_angle_alpha 90.00
_cell_angle_beta 99.197(3)
_cell_angle_gamma 90.00
_cell_volume 2785.65(15)
_cell_formula_units_Z 4
_cell_measurement_temperature 193(2)
_cell_measurement_reflns_used 1442
_cell_measurement_theta_min 2.42
_cell_measurement_theta_max 17.95
_exptl_crystal_description 'prism'
_exptl_crystal_colour 'orange'
_exptl_crystal_size_max 0.075
_exptl_crystal_size_mid 0.050
_exptl_crystal_size_min 0.025
_exptl_crystal_density_diffrn 1.712
_exptl_crystal_density_method 'not measured'
_exptl_crystal_density_meas ?
_exptl_crystal_F_000 1448
_exptl_absorpt_coefficient_mu 0.805
_exptl_absorpt_correction_type 'multi-scan'
_exptl_absorpt_correction_T_min 0.9421
_exptl_absorpt_correction_T_max 0.9802
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)'
_exptl_special_details
;
The compound was crystallized from an acetonitrile solution as orange
prisms. A crystal 0.025 mm x 0.050 mm x 0.075 mm in size was selected,
mounted on a nylon loop with Paratone-N oil, and transferred to a Bruker
SMART APEX II diffractometer equipped with an Oxford Cryosystems 700
Series Cryostream Cooler and Mo K\a radiation (\l = 0.71073 \%A). A total
of 2147 frames were collected at 193(2) K to \q~max~ = 22.49\% with an
oscillation range of 0.5\%/frame, and an exposure time of 15 s/frame
using the APEX2 suite of software. (Bruker AXS, 2006a) Data were
collected to \q~max~ = 22.49\% rather than the routine value of
\q~max~ = 27.50\% because the crystal examined did not exhibit usable
diffraction beyond 22.49\%. Unit cell refinement on all observed
reflections, and data reduction with corrections for Lp and decay were
performed using SAINT. (Bruker AXS, 2006b) Scaling and a multi-scan
absorption correction were done using SADABS. (Bruker AXS, 2004) The
minimum and maximum transmission factors were 0.9421 and 0.9802,
respectively. A total of 34170 reflections were collected, 3643
were unique (R~int~ = 0.147), and 2584 had I > 2\s(I).
Systematic absences were consistent with the compound having crystallized
in the monoclinic space group P2~1/n. The observed mean |E^2^-1|
value was 0.912 (versus the expectation values of 0.968 and 0.736 for
centric and noncentric data, respectively).
________________________________________________________________________
Bruker AXS (2004). SADABS. Bruker Analytical X-ray Systems Inc.,
Madison, Wisconsin, USA.
Bruker AXS (2006a). APEX2 v2.1-0. Bruker Analytical
X-ray Systems Inc., Madison, Wisconsin, USA.
Bruker AXS (2006b). SAINT V7.34A. Bruker Analytical
X-ray Systems Inc., Madison, Wisconsin, USA.
________________________________________________________________________
;
_diffrn_ambient_temperature 193(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device_type 'Bruker APEX II CCD'
_diffrn_measurement_method '\w scans, 2147 0.5\% rotations'
_diffrn_detector_area_resol_mean 836.6
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% 0
_diffrn_reflns_number 34170
_diffrn_reflns_av_R_equivalents 0.1469
_diffrn_reflns_av_sigmaI/netI 0.0690
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 1.81
_diffrn_reflns_theta_max 22.49
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 22.49
_diffrn_measured_fraction_theta_full 1.000
_reflns_number_total 3643
_reflns_number_gt 2584
_reflns_threshold_expression 'I>2\s(I)'
_computing_data_collection 'APEX2 v2.1-0 (Bruker AXS, 2006a)'
_computing_cell_refinement 'SAINT V7.34A (Bruker AXS, 2006b)'
_computing_data_reduction
;
SAINT V7.34A (Bruker AXS, 2006b), SADABS (Bruker AXS, 2004)
;
_computing_structure_solution 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_refinement 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'SHELXTL v6.12 (Bruker AXS, 2001)'
_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^ > 2\s(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.
The structure was solved by direct methods and refined by full-matrix
least-squares on F^2^ using SHELXTL. (Bruker AXS, 2001) The
asymmetric unit was found to contain one molecule of (Benzo[h]quinolinato)
{(2-nitrophenyl-sulfonyl)[(2-(pyridine-2-yl)phenyl]amido}-
difluoropalladium(IV) and one molecule of acetonitrile. All of the
nonhydrogen atoms were refined with anisotropic displacement
coefficients. The hydrogen atoms were assigned isotropic displacement
coefficients U(H) = 1.2U(C) or 1.5U(C~methyl~),
and their coordinates were allowed to ride on their respective carbons.
The acetonitrile was treated with a two-site disorder model consisting
of partial atoms with fixed site occupancy factors of a half. The atoms
associated with one of the two sites were specified with an asterisk,
e.g. N1S and N1S*, and included in the least-squares refinement with
1,2-distance, rigid-bond and similar U~ij~ restraints. The refinement
converged to R(F) = 0.0383, wR(F^2^) =
0.0703, and S = 1.042 for 2584 reflections with
I > 2\s(I), and R(F) = 0.0728,
wR(F^2^) = 0.0829, and S = 1.042 for 3643 unique
reflections, 424 parameters, and 58 restraints. The maximum |\D/\s| in
the final cycle of least-squares was 0.001, and the residual peaks on
the final difference-Fourier map ranged from -0.505 to 0.392 e\%A^-3^.
Scattering factors were taken from the International Tables for
Crystallography, Volume C. (Maslen et al., 1992, and Creagh & McAuley,
1992)
________________________________________________________________________
R(F ) = R1 =
\S ||F~o~|-|F~c~|| / \S|F~o~|,
wR(F ^2^) = wR2 =
[ \S w (F~o~^2^-F~c~^2^)^2^ /
\S w (F~o~^2^)^2^ ]^1/2^, and
S = Goodness-of-fit on F ^2^ =
[ \S w (F~o~^2^-F~c~^2^)^2^ /
(n-p) ]^1/2^, where n is the number of reflections
and p is the number of parameters refined.
________________________________________________________________________
Bruker AXS (2001). SHELXTL v6.12. Bruker Analytical
X-ray Systems Inc., Madison, Wisconsin, USA.
Creagh, D. C. & McAuley, W. J. (1992). International Tables for
Crystallography: Mathematical, Physical and Chemical Tables, Vol C,
edited by A. J. C. Wilson, pp. 206-222. Dordrecht, The Netherlands:
Kluwer.
Maslen, E. N., Fox, A. G. & O'Keefe, M. A. (1992). International
Tables for Crystallography: Mathematical, Physical and Chemical
Tables, Vol C, edited by A. J. C. Wilson, pp. 476-516. Dordrecht,
The Netherlands: Kluwer.
________________________________________________________________________
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+3.0772P] 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 ?
_refine_ls_number_reflns 3643
_refine_ls_number_parameters 424
_refine_ls_number_restraints 58
_refine_ls_R_factor_all 0.0728
_refine_ls_R_factor_gt 0.0383
_refine_ls_wR_factor_ref 0.0829
_refine_ls_wR_factor_gt 0.0703
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_restrained_S_all 1.034
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.392
_refine_diff_density_min -0.505
_refine_diff_density_rms 0.095
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.38382(4) 0.14240(3) 0.11830(2) 0.02164(14) Uani 1 1 d . . .
F1 F 0.5817(3) 0.1199(2) 0.10968(14) 0.0319(9) Uani 1 1 d . . .
F2 F 0.3569(3) 0.2017(2) 0.03236(14) 0.0336(9) Uani 1 1 d . . .
N1 N 0.4481(4) 0.2737(3) 0.1604(2) 0.0259(12) Uani 1 1 d . . .
C2 C 0.5333(6) 0.3254(4) 0.1286(3) 0.0325(16) Uani 1 1 d . . .
H2 H 0.5444 0.3054 0.0865 0.039 Uiso 1 1 calc R . .
C3 C 0.6042(6) 0.4070(5) 0.1567(4) 0.0414(18) Uani 1 1 d . . .
H3 H 0.6627 0.4439 0.1341 0.050 Uiso 1 1 calc R . .
C4 C 0.5884(6) 0.4335(5) 0.2178(3) 0.0406(17) Uani 1 1 d . . .
H4 H 0.6383 0.4881 0.2382 0.049 Uiso 1 1 calc R . .
C5 C 0.5021(6) 0.3826(4) 0.2496(3) 0.0334(16) Uani 1 1 d . . .
H5 H 0.4911 0.4021 0.2918 0.040 Uiso 1 1 calc R . .
C6 C 0.4298(5) 0.3020(4) 0.2202(3) 0.0271(15) Uani 1 1 d . . .
C7 C 0.3327(5) 0.2461(4) 0.2521(2) 0.0197(13) Uani 1 1 d . . .
C8 C 0.2497(5) 0.3008(4) 0.2879(3) 0.0273(15) Uani 1 1 d . . .
H8 H 0.2622 0.3708 0.2930 0.033 Uiso 1 1 calc R . .
C9 C 0.1528(6) 0.2546(5) 0.3150(3) 0.0325(16) Uani 1 1 d . . .
H9 H 0.0957 0.2928 0.3376 0.039 Uiso 1 1 calc R . .
C10 C 0.1354(6) 0.1517(5) 0.3100(3) 0.0345(16) Uani 1 1 d . . .
H10 H 0.0684 0.1198 0.3301 0.041 Uiso 1 1 calc R . .
C11 C 0.2160(5) 0.0960(5) 0.2757(3) 0.0263(15) Uani 1 1 d . . .
H11 H 0.2040 0.0258 0.2723 0.032 Uiso 1 1 calc R . .
C12 C 0.3140(5) 0.1421(5) 0.2464(2) 0.0205(13) Uani 1 1 d . . .
N13 N 0.3895(4) 0.0854(3) 0.2075(2) 0.0209(11) Uani 1 1 d . . .
S14 S 0.51034(14) 0.01861(11) 0.24661(7) 0.0254(4) Uani 1 1 d . . .
O15 O 0.5754(4) -0.0350(3) 0.20167(18) 0.0313(10) Uani 1 1 d . . .
O16 O 0.4573(4) -0.0359(3) 0.29572(17) 0.0285(10) Uani 1 1 d . . .
C17 C 0.6294(5) 0.1061(4) 0.2875(3) 0.0234(14) Uani 1 1 d . . .
C18 C 0.7074(5) 0.1609(4) 0.2510(3) 0.0263(15) Uani 1 1 d . . .
H18 H 0.6995 0.1486 0.2061 0.032 Uiso 1 1 calc R . .
C19 C 0.7959(6) 0.2328(5) 0.2790(3) 0.0338(16) Uani 1 1 d . . .
H19 H 0.8505 0.2684 0.2537 0.041 Uiso 1 1 calc R . .
C20 C 0.8057(6) 0.2534(5) 0.3443(3) 0.0358(17) Uani 1 1 d . . .
H20 H 0.8643 0.3050 0.3630 0.043 Uiso 1 1 calc R . .
C21 C 0.7315(6) 0.1998(5) 0.3822(3) 0.0340(16) Uani 1 1 d . . .
H21 H 0.7400 0.2122 0.4271 0.041 Uiso 1 1 calc R . .
C22 C 0.6435(5) 0.1268(4) 0.3528(3) 0.0271(15) Uani 1 1 d . . .
N23 N 0.5678(6) 0.0732(5) 0.3970(2) 0.0391(14) Uani 1 1 d . . .
O24 O 0.6112(5) -0.0078(4) 0.4178(2) 0.0541(14) Uani 1 1 d . . .
O25 O 0.4687(5) 0.1156(4) 0.4113(2) 0.0633(16) Uani 1 1 d . . .
N26 N 0.3319(4) 0.0074(3) 0.0802(2) 0.0240(12) Uani 1 1 d . . .
C27 C 0.4128(6) -0.0563(5) 0.0580(3) 0.0297(15) Uani 1 1 d . . .
H27 H 0.5051 -0.0392 0.0585 0.036 Uiso 1 1 calc R . .
C28 C 0.3656(6) -0.1483(5) 0.0337(3) 0.0337(15) Uani 1 1 d . . .
H28 H 0.4247 -0.1934 0.0170 0.040 Uiso 1 1 calc R . .
C29 C 0.2333(7) -0.1735(5) 0.0339(3) 0.0379(18) Uani 1 1 d . . .
H29 H 0.2017 -0.2376 0.0190 0.045 Uiso 1 1 calc R . .
C29A C 0.1433(6) -0.1060(5) 0.0560(3) 0.0339(16) Uani 1 1 d . . .
C30 C 0.0012(7) -0.1190(5) 0.0562(3) 0.0409(18) Uani 1 1 d . . .
H30 H -0.0402 -0.1805 0.0418 0.049 Uiso 1 1 calc R . .
C31 C -0.0753(7) -0.0461(5) 0.0763(3) 0.0381(17) Uani 1 1 d . . .
H31 H -0.1687 -0.0583 0.0764 0.046 Uiso 1 1 calc R . .
C31A C -0.0199(6) 0.0495(5) 0.0976(3) 0.0320(16) Uani 1 1 d . . .
C32 C -0.0953(6) 0.1317(6) 0.1133(3) 0.0389(17) Uani 1 1 d . . .
H32 H -0.1896 0.1248 0.1139 0.047 Uiso 1 1 calc R . .
C33 C -0.0330(6) 0.2224(6) 0.1277(3) 0.0403(18) Uani 1 1 d . . .
H33 H -0.0861 0.2779 0.1368 0.048 Uiso 1 1 calc R . .
C34 C 0.1070(6) 0.2354(5) 0.1295(3) 0.0277(15) Uani 1 1 d . . .
H34 H 0.1479 0.2987 0.1394 0.033 Uiso 1 1 calc R . .
C35 C 0.1834(5) 0.1549(5) 0.1167(2) 0.0249(14) Uani 1 1 d . . .
C35A C 0.1193(5) 0.0636(5) 0.0991(2) 0.0225(14) Uani 1 1 d . . .
C35B C 0.1984(6) -0.0138(4) 0.0791(3) 0.0232(14) Uani 1 1 d . . .
N1S N 0.416(2) 0.594(2) 0.023(2) 0.065(8) Uani 0.50 1 d PDU A 1
C2S C 0.343(5) 0.539(3) 0.040(3) 0.047(8) Uani 0.50 1 d PDU A 1
C3S C 0.2607(7) 0.4559(5) 0.0577(3) 0.0523(19) Uani 1 1 d DU . .
H3SA H 0.2038 0.4302 0.0189 0.078 Uiso 0.50 1 calc PR A 1
H3SB H 0.2030 0.4792 0.0882 0.078 Uiso 0.50 1 calc PR A 1
H3SC H 0.3201 0.4026 0.0776 0.078 Uiso 0.50 1 calc PR A 1
H3SD H 0.2798 0.4616 0.1047 0.078 Uiso 0.50 1 calc PR A 2
H3SE H 0.2951 0.3919 0.0445 0.078 Uiso 0.50 1 calc PR A 2
H3SF H 0.1627 0.4593 0.0433 0.078 Uiso 0.50 1 calc PR A 2
N1S* N 0.372(2) 0.608(2) 0.011(2) 0.055(7) Uani 0.50 1 d PDU A 2
C2S* C 0.327(6) 0.537(3) 0.029(3) 0.048(8) Uani 0.50 1 d PDU A 2
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
Pd 0.0194(2) 0.0236(3) 0.0223(3) 0.0001(2) 0.00444(17) 0.0001(2)
F1 0.0214(18) 0.042(2) 0.033(2) 0.0000(16) 0.0079(15) 0.0011(15)
F2 0.036(2) 0.040(2) 0.0259(19) 0.0061(17) 0.0080(16) -0.0007(17)
N1 0.023(3) 0.020(3) 0.034(3) -0.003(2) 0.005(2) -0.002(2)
C2 0.033(4) 0.031(4) 0.036(4) 0.007(3) 0.013(3) 0.000(3)
C3 0.027(4) 0.027(4) 0.072(6) 0.004(4) 0.013(4) -0.010(3)
C4 0.038(4) 0.023(4) 0.061(5) -0.013(4) 0.010(4) -0.002(3)
C5 0.028(4) 0.031(4) 0.041(4) -0.009(3) 0.005(3) -0.001(3)
C6 0.017(3) 0.025(4) 0.038(4) -0.002(3) 0.001(3) 0.005(3)
C7 0.018(3) 0.020(4) 0.019(3) -0.003(3) -0.001(3) 0.003(3)
C8 0.023(3) 0.024(4) 0.032(4) -0.006(3) -0.002(3) 0.003(3)
C9 0.019(3) 0.046(5) 0.032(4) -0.014(3) 0.001(3) 0.002(3)
C10 0.025(3) 0.052(5) 0.028(4) -0.003(4) 0.007(3) -0.008(4)
C11 0.019(3) 0.035(4) 0.025(4) 0.001(3) 0.004(3) -0.002(3)
C12 0.014(3) 0.027(3) 0.019(3) -0.001(3) -0.005(2) 0.006(3)
N13 0.015(2) 0.021(3) 0.026(3) 0.000(2) 0.002(2) 0.006(2)
S14 0.0242(8) 0.0201(9) 0.0305(9) -0.0010(7) 0.0002(7) 0.0014(7)
O15 0.028(2) 0.026(2) 0.039(3) -0.006(2) 0.004(2) 0.0131(19)
O16 0.030(2) 0.023(2) 0.031(2) 0.0099(19) 0.0004(19) -0.0045(18)
C17 0.016(3) 0.023(4) 0.031(4) 0.000(3) 0.002(3) 0.006(3)
C18 0.018(3) 0.035(4) 0.027(3) 0.008(3) 0.005(3) 0.008(3)
C19 0.018(3) 0.039(4) 0.045(4) 0.002(3) 0.006(3) -0.003(3)
C20 0.024(4) 0.043(5) 0.039(4) -0.008(4) 0.001(3) -0.007(3)
C21 0.029(4) 0.038(4) 0.034(4) -0.011(3) 0.000(3) 0.001(3)
C22 0.024(3) 0.027(4) 0.031(4) 0.003(3) 0.007(3) 0.008(3)
N23 0.038(4) 0.053(4) 0.026(3) -0.007(3) 0.003(3) -0.011(3)
O24 0.059(3) 0.054(4) 0.044(3) 0.018(3) -0.006(2) -0.006(3)
O25 0.064(4) 0.062(4) 0.077(4) -0.013(3) 0.048(3) -0.010(3)
N26 0.025(3) 0.029(3) 0.019(3) -0.001(2) 0.005(2) 0.000(2)
C27 0.039(4) 0.030(4) 0.020(3) 0.003(3) 0.007(3) 0.006(3)
C28 0.044(4) 0.033(4) 0.022(3) -0.007(3) 0.000(3) 0.005(4)
C29 0.063(5) 0.025(4) 0.022(4) 0.001(3) -0.005(3) -0.003(4)
C29A 0.043(4) 0.034(4) 0.022(4) 0.005(3) -0.004(3) -0.010(3)
C30 0.043(4) 0.044(5) 0.029(4) 0.000(3) -0.011(3) -0.020(4)
C31 0.033(4) 0.055(5) 0.026(4) 0.005(4) 0.003(3) -0.019(4)
C31A 0.031(4) 0.044(5) 0.020(4) 0.004(3) 0.001(3) -0.001(3)
C32 0.021(3) 0.074(5) 0.021(3) 0.008(4) 0.001(3) 0.002(4)
C33 0.028(4) 0.062(5) 0.032(4) -0.001(4) 0.007(3) 0.017(4)
C34 0.023(3) 0.037(4) 0.023(3) 0.002(3) 0.001(3) 0.000(3)
C35 0.018(3) 0.039(4) 0.018(3) -0.001(3) 0.004(2) -0.002(3)
C35A 0.019(3) 0.040(4) 0.007(3) 0.004(3) -0.002(2) 0.001(3)
C35B 0.026(4) 0.027(4) 0.016(3) 0.002(3) 0.002(3) 0.002(3)
N1S 0.070(17) 0.051(11) 0.08(2) 0.013(10) 0.026(17) 0.023(12)
C2S 0.066(17) 0.051(13) 0.026(16) -0.003(11) 0.011(15) 0.015(10)
C3S 0.066(5) 0.048(5) 0.042(4) 0.004(4) 0.004(4) 0.009(4)
N1S* 0.055(14) 0.042(12) 0.069(16) -0.002(9) 0.010(14) 0.006(11)
C2S* 0.058(14) 0.044(12) 0.04(2) -0.014(11) -0.004(11) -0.003(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd F2 1.955(3) . ?
Pd C35 2.008(5) . ?
Pd N26 2.012(5) . ?
Pd N13 2.019(4) . ?
Pd N1 2.027(5) . ?
Pd F1 2.040(3) . ?
N1 C6 1.354(7) . ?
N1 C2 1.355(7) . ?
C2 C3 1.385(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.367(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.357(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.471(8) . ?
C7 C12 1.408(8) . ?
C7 C8 1.412(7) . ?
C8 C9 1.351(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(7) . ?
C11 H11 0.9500 . ?
C12 N13 1.421(7) . ?
N13 S14 1.619(4) . ?
S14 O15 1.426(4) . ?
S14 O16 1.435(4) . ?
S14 C17 1.791(6) . ?
C17 C22 1.386(8) . ?
C17 C18 1.389(7) . ?
C18 C19 1.376(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.376(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.393(8) . ?
C21 H21 0.9500 . ?
C22 N23 1.477(7) . ?
N23 O25 1.222(6) . ?
N23 O24 1.224(7) . ?
N26 C27 1.314(7) . ?
N26 C35B 1.363(7) . ?
C27 C28 1.388(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.367(8) . ?
C28 H28 0.9500 . ?
C29 C29A 1.408(8) . ?
C29 H29 0.9500 . ?
C29A C35B 1.407(8) . ?
C29A C30 1.433(8) . ?
C30 C31 1.350(9) . ?
C30 H30 0.9500 . ?
C31 C31A 1.438(8) . ?
C31 H31 0.9500 . ?
C31A C35A 1.401(8) . ?
C31A C32 1.403(8) . ?
C32 C33 1.378(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.406(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.374(8) . ?
C34 H34 0.9500 . ?
C35 C35A 1.403(8) . ?
C35A C35B 1.408(8) . ?
N1S C2S 1.139(10) . ?
C2S C3S 1.462(10) . ?
C3S C2S* 1.458(10) . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
C3S H3SD 0.9800 . ?
C3S H3SE 0.9800 . ?
C3S H3SF 0.9800 . ?
N1S* C2S* 1.136(10) . ?
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
F2 Pd C35 87.81(18) . . ?
F2 Pd N26 90.47(15) . . ?
C35 Pd N26 82.8(2) . . ?
F2 Pd N13 173.48(15) . . ?
C35 Pd N13 85.77(19) . . ?
N26 Pd N13 89.85(18) . . ?
F2 Pd N1 92.23(17) . . ?
C35 Pd N1 100.5(2) . . ?
N26 Pd N1 175.84(18) . . ?
N13 Pd N1 87.82(18) . . ?
F2 Pd F1 88.27(13) . . ?
C35 Pd F1 172.95(18) . . ?
N26 Pd F1 91.38(16) . . ?
N13 Pd F1 98.24(14) . . ?
N1 Pd F1 85.54(15) . . ?
C6 N1 C2 120.3(5) . . ?
C6 N1 Pd 124.6(4) . . ?
C2 N1 Pd 114.1(4) . . ?
N1 C2 C3 120.8(6) . . ?
N1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 C2 118.5(6) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 120.8(6) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 119.9(6) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
N1 C6 C5 119.5(5) . . ?
N1 C6 C7 118.7(5) . . ?
C5 C6 C7 121.8(5) . . ?
C12 C7 C8 118.5(5) . . ?
C12 C7 C6 123.5(5) . . ?
C8 C7 C6 117.9(5) . . ?
C9 C8 C7 120.7(6) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 120.8(6) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 119.8(6) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 120.4(6) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 119.8(5) . . ?
C11 C12 N13 119.9(5) . . ?
C7 C12 N13 120.2(5) . . ?
C12 N13 S14 115.2(3) . . ?
C12 N13 Pd 113.3(3) . . ?
S14 N13 Pd 126.1(2) . . ?
O15 S14 O16 118.9(2) . . ?
O15 S14 N13 108.9(2) . . ?
O16 S14 N13 108.4(2) . . ?
O15 S14 C17 108.0(2) . . ?
O16 S14 C17 106.3(3) . . ?
N13 S14 C17 105.6(2) . . ?
C22 C17 C18 117.7(5) . . ?
C22 C17 S14 124.2(4) . . ?
C18 C17 S14 118.0(4) . . ?
C19 C18 C17 120.8(5) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.1(6) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C21 C20 C19 120.7(6) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 118.0(6) . . ?
C20 C21 H21 121.0 . . ?
C22 C21 H21 121.0 . . ?
C17 C22 C21 122.5(6) . . ?
C17 C22 N23 123.1(5) . . ?
C21 C22 N23 114.3(5) . . ?
O25 N23 O24 125.4(6) . . ?
O25 N23 C22 116.6(6) . . ?
O24 N23 C22 117.9(6) . . ?
C27 N26 C35B 121.2(5) . . ?
C27 N26 Pd 126.2(4) . . ?
C35B N26 Pd 112.6(4) . . ?
N26 C27 C28 121.0(6) . . ?
N26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C29 C28 C27 119.4(6) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C29A 120.9(6) . . ?
C28 C29 H29 119.5 . . ?
C29A C29 H29 119.5 . . ?
C35B C29A C29 116.2(6) . . ?
C35B C29A C30 116.1(6) . . ?
C29 C29A C30 127.6(6) . . ?
C31 C30 C29A 121.7(6) . . ?
C31 C30 H30 119.2 . . ?
C29A C30 H30 119.2 . . ?
C30 C31 C31A 122.2(6) . . ?
C30 C31 H31 118.9 . . ?
C31A C31 H31 118.9 . . ?
C35A C31A C32 117.4(6) . . ?
C35A C31A C31 117.3(6) . . ?
C32 C31A C31 125.2(6) . . ?
C33 C32 C31A 120.1(6) . . ?
C33 C32 H32 119.9 . . ?
C31A C32 H32 119.9 . . ?
C32 C33 C34 121.9(6) . . ?
C32 C33 H33 119.0 . . ?
C34 C33 H33 119.0 . . ?
C35 C34 C33 118.8(6) . . ?
C35 C34 H34 120.6 . . ?
C33 C34 H34 120.6 . . ?
C34 C35 C35A 119.4(5) . . ?
C34 C35 Pd 130.4(5) . . ?
C35A C35 Pd 110.2(4) . . ?
C31A C35A C35 122.2(6) . . ?
C31A C35A C35B 119.9(6) . . ?
C35 C35A C35B 117.7(5) . . ?
N26 C35B C29A 121.2(5) . . ?
N26 C35B C35A 116.0(5) . . ?
C29A C35B C35A 122.7(5) . . ?
N1S C2S C3S 171(6) . . ?
C2S* C3S H3SA 99.0 . . ?
C2S C3S H3SA 109.5 . . ?
C2S* C3S H3SB 112.8 . . ?
C2S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C2S* C3S H3SC 116.1 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
C2S* C3S H3SD 109.5 . . ?
C2S C3S H3SD 99.5 . . ?
H3SA C3S H3SD 149.6 . . ?
H3SB C3S H3SD 49.8 . . ?
H3SC C3S H3SD 67.5 . . ?
C2S* C3S H3SE 109.5 . . ?
C2S C3S H3SE 110.9 . . ?
H3SA C3S H3SE 69.0 . . ?
H3SB C3S H3SE 137.3 . . ?
H3SD C3S H3SE 109.5 . . ?
C2S* C3S H3SF 109.5 . . ?
C2S C3S H3SF 117.5 . . ?
H3SA C3S H3SF 48.7 . . ?
H3SB C3S H3SF 61.5 . . ?
H3SC C3S H3SF 132.5 . . ?
H3SD C3S H3SF 109.5 . . ?
H3SE C3S H3SF 109.5 . . ?
N1S* C2S* C3S 172(6) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F2 Pd N1 C6 149.0(4) . . . . ?
C35 Pd N1 C6 60.8(5) . . . . ?
N13 Pd N1 C6 -24.5(4) . . . . ?
F1 Pd N1 C6 -122.9(4) . . . . ?
F2 Pd N1 C2 -42.1(4) . . . . ?
C35 Pd N1 C2 -130.3(4) . . . . ?
N13 Pd N1 C2 144.4(4) . . . . ?
F1 Pd N1 C2 46.0(4) . . . . ?
C6 N1 C2 C3 0.8(8) . . . . ?
Pd N1 C2 C3 -168.6(4) . . . . ?
N1 C2 C3 C4 1.1(9) . . . . ?
C2 C3 C4 C5 -1.8(10) . . . . ?
C3 C4 C5 C6 0.7(9) . . . . ?
C2 N1 C6 C5 -2.0(8) . . . . ?
Pd N1 C6 C5 166.2(4) . . . . ?
C2 N1 C6 C7 177.8(5) . . . . ?
Pd N1 C6 C7 -14.0(7) . . . . ?
C4 C5 C6 N1 1.2(9) . . . . ?
C4 C5 C6 C7 -178.5(5) . . . . ?
N1 C6 C7 C12 36.8(8) . . . . ?
C5 C6 C7 C12 -143.4(6) . . . . ?
N1 C6 C7 C8 -140.1(5) . . . . ?
C5 C6 C7 C8 39.6(8) . . . . ?
C12 C7 C8 C9 -1.3(8) . . . . ?
C6 C7 C8 C9 175.8(5) . . . . ?
C7 C8 C9 C10 2.2(9) . . . . ?
C8 C9 C10 C11 -1.6(9) . . . . ?
C9 C10 C11 C12 0.1(8) . . . . ?
C10 C11 C12 C7 0.7(8) . . . . ?
C10 C11 C12 N13 -175.5(5) . . . . ?
C8 C7 C12 C11 -0.1(7) . . . . ?
C6 C7 C12 C11 -177.0(5) . . . . ?
C8 C7 C12 N13 176.0(4) . . . . ?
C6 C7 C12 N13 -0.9(8) . . . . ?
C11 C12 N13 S14 -78.2(5) . . . . ?
C7 C12 N13 S14 105.6(5) . . . . ?
C11 C12 N13 Pd 126.1(4) . . . . ?
C7 C12 N13 Pd -50.0(5) . . . . ?
C35 Pd N13 C12 -46.7(4) . . . . ?
N26 Pd N13 C12 -129.5(4) . . . . ?
N1 Pd N13 C12 54.0(4) . . . . ?
F1 Pd N13 C12 139.1(3) . . . . ?
C35 Pd N13 S14 160.8(3) . . . . ?
N26 Pd N13 S14 78.0(3) . . . . ?
N1 Pd N13 S14 -98.5(3) . . . . ?
F1 Pd N13 S14 -13.4(3) . . . . ?
C12 N13 S14 O15 179.1(4) . . . . ?
Pd N13 S14 O15 -28.8(4) . . . . ?
C12 N13 S14 O16 48.5(5) . . . . ?
Pd N13 S14 O16 -159.5(3) . . . . ?
C12 N13 S14 C17 -65.1(4) . . . . ?
Pd N13 S14 C17 86.9(3) . . . . ?
O15 S14 C17 C22 -139.7(5) . . . . ?
O16 S14 C17 C22 -11.0(5) . . . . ?
N13 S14 C17 C22 103.9(5) . . . . ?
O15 S14 C17 C18 44.1(5) . . . . ?
O16 S14 C17 C18 172.7(4) . . . . ?
N13 S14 C17 C18 -72.3(5) . . . . ?
C22 C17 C18 C19 0.3(8) . . . . ?
S14 C17 C18 C19 176.8(4) . . . . ?
C17 C18 C19 C20 -1.7(9) . . . . ?
C18 C19 C20 C21 2.6(9) . . . . ?
C19 C20 C21 C22 -2.0(9) . . . . ?
C18 C17 C22 C21 0.2(8) . . . . ?
S14 C17 C22 C21 -176.0(4) . . . . ?
C18 C17 C22 N23 -179.3(5) . . . . ?
S14 C17 C22 N23 4.5(8) . . . . ?
C20 C21 C22 C17 0.6(9) . . . . ?
C20 C21 C22 N23 -179.9(5) . . . . ?
C17 C22 N23 O25 -100.3(7) . . . . ?
C21 C22 N23 O25 80.1(7) . . . . ?
C17 C22 N23 O24 81.9(7) . . . . ?
C21 C22 N23 O24 -97.7(6) . . . . ?
F2 Pd N26 C27 85.0(4) . . . . ?
C35 Pd N26 C27 172.8(5) . . . . ?
N13 Pd N26 C27 -101.5(5) . . . . ?
F1 Pd N26 C27 -3.2(5) . . . . ?
F2 Pd N26 C35B -94.7(4) . . . . ?
C35 Pd N26 C35B -7.0(4) . . . . ?
N13 Pd N26 C35B 78.7(4) . . . . ?
F1 Pd N26 C35B 177.0(4) . . . . ?
C35B N26 C27 C28 -1.3(8) . . . . ?
Pd N26 C27 C28 179.0(4) . . . . ?
N26 C27 C28 C29 -1.0(9) . . . . ?
C27 C28 C29 C29A 2.6(9) . . . . ?
C28 C29 C29A C35B -1.8(8) . . . . ?
C28 C29 C29A C30 176.4(6) . . . . ?
C35B C29A C30 C31 1.2(9) . . . . ?
C29 C29A C30 C31 -177.1(6) . . . . ?
C29A C30 C31 C31A 1.2(9) . . . . ?
C30 C31 C31A C35A -2.3(9) . . . . ?
C30 C31 C31A C32 173.5(6) . . . . ?
C35A C31A C32 C33 1.6(8) . . . . ?
C31 C31A C32 C33 -174.3(6) . . . . ?
C31A C32 C33 C34 -2.1(9) . . . . ?
C32 C33 C34 C35 -0.3(9) . . . . ?
C33 C34 C35 C35A 3.2(8) . . . . ?
C33 C34 C35 Pd -177.1(4) . . . . ?
F2 Pd C35 C34 -81.6(5) . . . . ?
N26 Pd C35 C34 -172.3(5) . . . . ?
N13 Pd C35 C34 97.3(5) . . . . ?
N1 Pd C35 C34 10.3(5) . . . . ?
F2 Pd C35 C35A 98.2(4) . . . . ?
N26 Pd C35 C35A 7.4(4) . . . . ?
N13 Pd C35 C35A -83.0(4) . . . . ?
N1 Pd C35 C35A -170.0(4) . . . . ?
C32 C31A C35A C35 1.4(8) . . . . ?
C31 C31A C35A C35 177.6(5) . . . . ?
C32 C31A C35A C35B -175.1(5) . . . . ?
C31 C31A C35A C35B 1.0(8) . . . . ?
C34 C35 C35A C31A -3.8(8) . . . . ?
Pd C35 C35A C31A 176.4(4) . . . . ?
C34 C35 C35A C35B 172.8(5) . . . . ?
Pd C35 C35A C35B -7.0(6) . . . . ?
C27 N26 C35B C29A 2.1(8) . . . . ?
Pd N26 C35B C29A -178.1(4) . . . . ?
C27 N26 C35B C35A -174.7(5) . . . . ?
Pd N26 C35B C35A 5.1(6) . . . . ?
C29 C29A C35B N26 -0.5(8) . . . . ?
C30 C29A C35B N26 -178.9(5) . . . . ?
C29 C29A C35B C35A 176.0(5) . . . . ?
C30 C29A C35B C35A -2.4(8) . . . . ?
C31A C35A C35B N26 178.0(5) . . . . ?
C35 C35A C35B N26 1.3(7) . . . . ?
C31A C35A C35B C29A 1.3(8) . . . . ?
C35 C35A C35B C29A -175.3(5) . . . . ?