# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_coden_Cambridge 182
loop_
_publ_author_name
'Luo, Jia'
'Khusnutdinova, Julia'
'Rath, Nigam'
'Mirica, Liviu'
_publ_contact_author_name 'Mirica, Liviu'
_publ_contact_author_email mirica@wustl.edu
_publ_section_title
;
Unsupported d8-d8 interactions in
cationic PdII and PtII complexes:
Evidence for a significant metal-metal bonding character
;
# Attachment '- CombinedCIFs.cif'
data_l23710
_database_code_depnum_ccdc_archive 'CCDC 842462'
#TrackingRef '- CombinedCIFs.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C18 H17 F6 N3 O6 Pd S4'
_chemical_formula_weight 719.99
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_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 12.3492(5)
_cell_length_b 17.5047(6)
_cell_length_c 12.2940(5)
_cell_angle_alpha 90.00
_cell_angle_beta 112.870(2)
_cell_angle_gamma 90.00
_cell_volume 2448.67(16)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9811
_cell_measurement_theta_min 2.30
_cell_measurement_theta_max 34.17
_exptl_crystal_description rectangular
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.17
_exptl_crystal_density_meas no
_exptl_crystal_density_diffrn 1.953
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1432
_exptl_absorpt_coefficient_mu 1.187
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7238
_exptl_absorpt_correction_T_max 0.8282
_exptl_absorpt_process_details 'sadabs v2008/1'
_exptl_special_details
;
All H atoms were added in their calculated positions
and were treated using appropriate riding models.
;
_diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 52737
_diffrn_reflns_av_R_equivalents 0.0302
_diffrn_reflns_av_sigmaI/netI 0.0251
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.13
_diffrn_reflns_theta_max 34.30
_reflns_number_total 10171
_reflns_number_gt 8530
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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^)+(0.0429P)^2^+2.6650P] 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 10171
_refine_ls_number_parameters 348
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0419
_refine_ls_R_factor_gt 0.0323
_refine_ls_wR_factor_ref 0.0877
_refine_ls_wR_factor_gt 0.0816
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_restrained_S_all 1.026
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
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 0.628757(11) 0.511408(7) 1.017375(11) 0.01538(4) Uani 1 1 d . . .
S1 S 0.65441(4) 0.63360(3) 1.09817(4) 0.02150(9) Uani 1 1 d . . .
S2 S 0.64554(4) 0.40202(2) 0.91808(4) 0.02134(9) Uani 1 1 d . . .
S3 S 0.26642(4) 0.37674(3) 0.52697(4) 0.02109(9) Uani 1 1 d . . .
S4 S 0.26779(5) 0.79373(4) 0.85420(6) 0.01895(13) Uani 0.946(3) 1 d P A 1
S4' S 0.2580(9) 0.7715(8) 0.8204(12) 0.01895(13) Uani 0.054(3) 1 d P A 2
F1 F 0.11971(15) 0.44538(10) 0.60033(16) 0.0445(4) Uani 1 1 d . . .
F2 F 0.04934(15) 0.34675(11) 0.49258(19) 0.0541(5) Uani 1 1 d . . .
F3 F 0.07337(16) 0.45166(12) 0.41323(17) 0.0577(5) Uani 1 1 d . . .
F4 F 0.11727(14) 0.68045(8) 0.78322(15) 0.0381(3) Uani 1 1 d . A .
F5 F 0.05863(17) 0.77499(11) 0.8574(2) 0.0542(5) Uani 1 1 d . A .
F6 F 0.06024(14) 0.78403(11) 0.68328(16) 0.0489(4) Uani 1 1 d . A .
O1 O 0.24789(14) 0.33497(9) 0.42068(14) 0.0277(3) Uani 1 1 d . . .
O2 O 0.3018(2) 0.33029(11) 0.63057(16) 0.0443(5) Uani 1 1 d . . .
O3 O 0.32977(15) 0.44700(10) 0.54057(19) 0.0383(4) Uani 1 1 d . . .
O4 O 0.31648(17) 0.75756(10) 0.96764(15) 0.0359(4) Uani 1 1 d . . .
O5 O 0.31653(14) 0.76948(9) 0.77121(15) 0.0299(3) Uani 1 1 d . . .
O6 O 0.25038(17) 0.87499(9) 0.85612(16) 0.0335(4) Uani 1 1 d . . .
N1 N 0.58087(12) 0.56441(8) 0.86151(13) 0.0137(2) Uani 1 1 d . . .
N2 N 0.83436(13) 0.53320(10) 1.03163(14) 0.0200(3) Uani 1 1 d . . .
N3 N 0.67953(14) 0.45814(10) 1.17464(14) 0.0197(3) Uani 1 1 d . . .
C1 C 0.57139(15) 0.52458(9) 0.76395(15) 0.0161(3) Uani 1 1 d . . .
C2 C 0.55222(16) 0.56093(11) 0.65865(16) 0.0205(3) Uani 1 1 d . . .
H2A H 0.5482 0.5323 0.5915 0.025 Uiso 1 1 calc R . .
C3 C 0.53887(17) 0.63953(11) 0.65171(17) 0.0223(3) Uani 1 1 d . . .
H3A H 0.5250 0.6653 0.5795 0.027 Uiso 1 1 calc R . .
C4 C 0.54586(16) 0.67998(10) 0.75019(17) 0.0205(3) Uani 1 1 d . . .
H4A H 0.5355 0.7338 0.7462 0.025 Uiso 1 1 calc R . .
C5 C 0.56811(15) 0.64170(9) 0.85481(15) 0.0156(3) Uani 1 1 d . . .
C6 C 0.57356(17) 0.68322(10) 0.96198(17) 0.0197(3) Uani 1 1 d . . .
H6A H 0.4924 0.6923 0.9564 0.024 Uiso 1 1 calc R . .
H6B H 0.6106 0.7337 0.9641 0.024 Uiso 1 1 calc R . .
C7 C 0.80853(18) 0.65032(12) 1.11842(19) 0.0256(4) Uani 1 1 d . . .
H7A H 0.8210 0.7058 1.1129 0.031 Uiso 1 1 calc R . .
H7B H 0.8608 0.6333 1.1985 0.031 Uiso 1 1 calc R . .
C8 C 0.84214(16) 0.60902(12) 1.02847(17) 0.0219(3) Uani 1 1 d . . .
C9 C 0.86681(19) 0.64570(14) 0.9410(2) 0.0297(4) Uani 1 1 d . . .
H9A H 0.8744 0.6997 0.9410 0.036 Uiso 1 1 calc R . .
C10 C 0.88010(19) 0.60145(15) 0.8532(2) 0.0320(5) Uani 1 1 d . . .
H10A H 0.8998 0.6249 0.7937 0.038 Uiso 1 1 calc R . .
C11 C 0.86450(18) 0.52269(14) 0.85257(19) 0.0284(4) Uani 1 1 d . . .
H11A H 0.8707 0.4917 0.7918 0.034 Uiso 1 1 calc R . .
C12 C 0.83962(16) 0.49093(12) 0.94319(17) 0.0216(3) Uani 1 1 d . . .
C13 C 0.80196(18) 0.40923(12) 0.94384(19) 0.0256(4) Uani 1 1 d . . .
H13A H 0.8496 0.3857 1.0210 0.031 Uiso 1 1 calc R . .
H13B H 0.8168 0.3804 0.8817 0.031 Uiso 1 1 calc R . .
C14 C 0.57583(17) 0.43956(10) 0.77118(17) 0.0209(3) Uani 1 1 d . . .
H14A H 0.6183 0.4204 0.7230 0.025 Uiso 1 1 calc R . .
H14B H 0.4945 0.4196 0.7359 0.025 Uiso 1 1 calc R . .
C15 C 0.71265(16) 0.42937(11) 1.26399(17) 0.0198(3) Uani 1 1 d . . .
C16 C 0.75459(18) 0.39194(11) 1.37789(16) 0.0215(3) Uani 1 1 d . . .
H16A H 0.7221 0.3402 1.3690 0.032 Uiso 1 1 calc R . .
H16B H 0.7294 0.4211 1.4321 0.032 Uiso 1 1 calc R . .
H16C H 0.8406 0.3893 1.4098 0.032 Uiso 1 1 calc R . .
C17 C 0.11962(19) 0.40696(14) 0.5067(2) 0.0304(4) Uani 1 1 d . . .
C18 C 0.1181(2) 0.75690(13) 0.7918(2) 0.0301(4) Uani 1 1 d . . .
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 0.01553(6) 0.01731(6) 0.01368(6) 0.00279(4) 0.00609(4) -0.00016(4)
S1 0.0250(2) 0.0247(2) 0.01555(18) -0.00370(15) 0.00862(16) -0.00119(16)
S2 0.0263(2) 0.01455(17) 0.0231(2) 0.00332(15) 0.00954(17) 0.00129(15)
S3 0.02045(19) 0.02072(19) 0.0192(2) -0.00198(15) 0.00449(16) 0.00303(15)
S4 0.0233(2) 0.0161(3) 0.0173(3) 0.0015(2) 0.00773(18) 0.00314(17)
S4' 0.0233(2) 0.0161(3) 0.0173(3) 0.0015(2) 0.00773(18) 0.00314(17)
F1 0.0468(9) 0.0425(8) 0.0577(10) -0.0178(7) 0.0353(8) -0.0007(7)
F2 0.0341(8) 0.0510(10) 0.0849(14) -0.0244(10) 0.0317(9) -0.0174(7)
F3 0.0468(10) 0.0651(12) 0.0497(10) 0.0137(9) 0.0063(8) 0.0342(9)
F4 0.0401(8) 0.0313(7) 0.0443(9) -0.0002(6) 0.0178(7) -0.0084(6)
F5 0.0505(10) 0.0521(10) 0.0828(14) 0.0028(9) 0.0510(10) 0.0055(8)
F6 0.0287(7) 0.0594(11) 0.0458(9) 0.0204(8) 0.0003(7) 0.0017(7)
O1 0.0333(8) 0.0285(7) 0.0230(7) -0.0052(6) 0.0127(6) 0.0029(6)
O2 0.0629(13) 0.0410(10) 0.0229(8) 0.0084(7) 0.0099(8) 0.0219(9)
O3 0.0299(8) 0.0313(8) 0.0581(12) -0.0144(8) 0.0218(8) -0.0076(6)
O4 0.0473(10) 0.0296(8) 0.0235(8) 0.0069(6) 0.0058(7) 0.0040(7)
O5 0.0301(8) 0.0292(7) 0.0364(9) -0.0074(6) 0.0197(7) -0.0014(6)
O6 0.0525(10) 0.0185(6) 0.0355(9) 0.0017(6) 0.0237(8) 0.0040(6)
N1 0.0131(6) 0.0141(5) 0.0136(6) 0.0005(4) 0.0047(5) 0.0003(4)
N2 0.0144(6) 0.0256(7) 0.0181(7) 0.0028(6) 0.0043(5) 0.0015(5)
N3 0.0166(6) 0.0251(7) 0.0180(7) 0.0046(6) 0.0072(5) -0.0006(5)
C1 0.0159(7) 0.0161(7) 0.0159(7) -0.0012(5) 0.0055(6) -0.0008(5)
C2 0.0211(8) 0.0255(8) 0.0137(7) -0.0001(6) 0.0055(6) -0.0020(6)
C3 0.0213(8) 0.0261(8) 0.0172(8) 0.0067(6) 0.0049(6) -0.0011(6)
C4 0.0197(8) 0.0178(7) 0.0229(8) 0.0048(6) 0.0072(7) 0.0000(6)
C5 0.0143(6) 0.0153(6) 0.0171(7) 0.0009(5) 0.0060(6) 0.0003(5)
C6 0.0218(8) 0.0170(7) 0.0210(8) -0.0026(6) 0.0092(7) 0.0010(6)
C7 0.0215(8) 0.0249(8) 0.0239(9) -0.0037(7) 0.0016(7) -0.0045(7)
C8 0.0141(7) 0.0268(8) 0.0209(8) 0.0013(7) 0.0024(6) -0.0032(6)
C9 0.0228(9) 0.0333(10) 0.0277(10) 0.0074(8) 0.0040(8) -0.0093(8)
C10 0.0218(9) 0.0495(13) 0.0233(9) 0.0092(9) 0.0074(8) -0.0081(9)
C11 0.0188(8) 0.0461(12) 0.0198(8) 0.0015(8) 0.0070(7) 0.0008(8)
C12 0.0140(7) 0.0298(9) 0.0193(8) 0.0024(7) 0.0046(6) 0.0042(6)
C13 0.0238(9) 0.0265(9) 0.0242(9) 0.0021(7) 0.0067(7) 0.0093(7)
C14 0.0240(8) 0.0165(7) 0.0191(8) -0.0023(6) 0.0051(7) 0.0006(6)
C15 0.0182(7) 0.0222(8) 0.0192(8) 0.0009(6) 0.0075(6) -0.0006(6)
C16 0.0248(8) 0.0227(8) 0.0155(7) 0.0028(6) 0.0062(6) 0.0025(6)
C17 0.0230(9) 0.0327(10) 0.0355(11) -0.0068(9) 0.0114(8) 0.0012(8)
C18 0.0279(10) 0.0326(10) 0.0327(11) 0.0082(8) 0.0151(9) 0.0036(8)
_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 2.0004(14) . ?
Pd1 N3 2.0146(16) . ?
Pd1 S2 2.3230(5) . ?
Pd1 S1 2.3275(5) . ?
Pd1 N2 2.5054(16) . ?
Pd1 Pd1 3.0657(3) 3_667 ?
S1 C6 1.8043(19) . ?
S1 C7 1.844(2) . ?
S2 C14 1.796(2) . ?
S2 C13 1.836(2) . ?
S3 O2 1.4288(18) . ?
S3 O3 1.4321(18) . ?
S3 O1 1.4360(15) . ?
S3 C17 1.810(2) . ?
S4 O4 1.4337(17) . ?
S4 O5 1.4355(17) . ?
S4 O6 1.4402(17) . ?
S4 C18 1.822(2) . ?
S4' O5 1.108(11) . ?
S4' C18 1.644(10) . ?
S4' O4 1.686(13) . ?
S4' O6 1.875(15) . ?
F1 C17 1.333(3) . ?
F2 C17 1.333(3) . ?
F3 C17 1.322(3) . ?
F4 C18 1.342(3) . ?
F5 C18 1.323(3) . ?
F6 C18 1.332(3) . ?
N1 C1 1.352(2) . ?
N1 C5 1.361(2) . ?
N2 C8 1.332(3) . ?
N2 C12 1.338(3) . ?
N3 C15 1.131(2) . ?
C1 C2 1.378(2) . ?
C1 C14 1.491(2) . ?
C2 C3 1.384(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.376(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.380(2) . ?
C4 H4A 0.9500 . ?
C5 C6 1.483(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.508(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.384(3) . ?
C9 C10 1.389(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.392(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.382(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.505(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.447(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
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 N3 179.14(6) . . ?
N1 Pd1 S2 86.13(4) . . ?
N3 Pd1 S2 93.71(5) . . ?
N1 Pd1 S1 85.59(4) . . ?
N3 Pd1 S1 94.35(5) . . ?
S2 Pd1 S1 163.060(18) . . ?
N1 Pd1 N2 84.87(5) . . ?
N3 Pd1 N2 94.27(6) . . ?
S2 Pd1 N2 82.38(4) . . ?
S1 Pd1 N2 82.19(4) . . ?
N1 Pd1 Pd1 91.29(4) . 3_667 ?
N3 Pd1 Pd1 89.57(4) . 3_667 ?
S2 Pd1 Pd1 96.831(14) . 3_667 ?
S1 Pd1 Pd1 98.103(14) . 3_667 ?
N2 Pd1 Pd1 176.12(4) . 3_667 ?
C6 S1 C7 102.64(9) . . ?
C6 S1 Pd1 96.43(6) . . ?
C7 S1 Pd1 99.53(7) . . ?
C14 S2 C13 102.08(10) . . ?
C14 S2 Pd1 96.95(6) . . ?
C13 S2 Pd1 98.94(7) . . ?
O2 S3 O3 114.87(13) . . ?
O2 S3 O1 114.00(11) . . ?
O3 S3 O1 115.48(11) . . ?
O2 S3 C17 103.43(13) . . ?
O3 S3 C17 103.74(11) . . ?
O1 S3 C17 103.09(10) . . ?
O4 S4 O5 115.31(11) . . ?
O4 S4 O6 115.41(12) . . ?
O5 S4 O6 114.22(10) . . ?
O4 S4 C18 103.09(11) . . ?
O5 S4 C18 103.49(11) . . ?
O6 S4 C18 102.87(11) . . ?
O5 S4' C18 137.1(12) . . ?
O5 S4' O4 118.9(8) . . ?
C18 S4' O4 100.5(6) . . ?
O5 S4' O6 105.2(8) . . ?
C18 S4' O6 93.2(6) . . ?
O4 S4' O6 85.9(7) . . ?
S4 O4 S4' 18.0(5) . . ?
S4' O5 S4 20.0(8) . . ?
S4 O6 S4' 11.6(4) . . ?
C1 N1 C5 119.39(15) . . ?
C1 N1 Pd1 120.12(11) . . ?
C5 N1 Pd1 120.21(11) . . ?
C8 N2 C12 120.04(17) . . ?
C8 N2 Pd1 103.43(12) . . ?
C12 N2 Pd1 103.12(12) . . ?
C15 N3 Pd1 177.12(16) . . ?
N1 C1 C2 121.28(16) . . ?
N1 C1 C14 118.25(15) . . ?
C2 C1 C14 120.39(16) . . ?
C1 C2 C3 119.32(17) . . ?
C1 C2 H2A 120.3 . . ?
C3 C2 H2A 120.3 . . ?
C4 C3 C2 119.47(17) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 119.47(17) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
N1 C5 C4 121.03(16) . . ?
N1 C5 C6 117.99(15) . . ?
C4 C5 C6 120.93(16) . . ?
C5 C6 S1 113.96(12) . . ?
C5 C6 H6A 108.8 . . ?
S1 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
S1 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C8 C7 S1 112.86(13) . . ?
C8 C7 H7A 109.0 . . ?
S1 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
S1 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
N2 C8 C9 121.7(2) . . ?
N2 C8 C7 114.37(17) . . ?
C9 C8 C7 123.6(2) . . ?
C8 C9 C10 118.2(2) . . ?
C8 C9 H9A 120.9 . . ?
C10 C9 H9A 120.9 . . ?
C9 C10 C11 119.9(2) . . ?
C9 C10 H10A 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C12 C11 C10 117.9(2) . . ?
C12 C11 H11A 121.1 . . ?
C10 C11 H11A 121.1 . . ?
N2 C12 C11 121.9(2) . . ?
N2 C12 C13 114.12(17) . . ?
C11 C12 C13 123.54(19) . . ?
C12 C13 S2 111.77(13) . . ?
C12 C13 H13A 109.3 . . ?
S2 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
S2 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C1 C14 S2 114.67(13) . . ?
C1 C14 H14A 108.6 . . ?
S2 C14 H14A 108.6 . . ?
C1 C14 H14B 108.6 . . ?
S2 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
N3 C15 C16 179.5(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
F3 C17 F1 107.9(2) . . ?
F3 C17 F2 108.4(2) . . ?
F1 C17 F2 107.1(2) . . ?
F3 C17 S3 111.34(17) . . ?
F1 C17 S3 111.33(16) . . ?
F2 C17 S3 110.70(16) . . ?
F5 C18 F6 108.5(2) . . ?
F5 C18 F4 107.32(19) . . ?
F6 C18 F4 107.0(2) . . ?
F5 C18 S4' 128.2(6) . . ?
F6 C18 S4' 105.6(4) . . ?
F4 C18 S4' 98.5(5) . . ?
F5 C18 S4 111.80(19) . . ?
F6 C18 S4 110.90(15) . . ?
F4 C18 S4 111.18(15) . . ?
S4' C18 S4 17.2(5) . . ?
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
N1 Pd1 S1 C6 15.54(7) . . . . ?
N3 Pd1 S1 C6 -165.32(8) . . . . ?
S2 Pd1 S1 C6 76.48(9) . . . . ?
N2 Pd1 S1 C6 100.96(7) . . . . ?
Pd1 Pd1 S1 C6 -75.14(6) 3_667 . . . ?
N1 Pd1 S1 C7 -88.48(8) . . . . ?
N3 Pd1 S1 C7 90.66(8) . . . . ?
S2 Pd1 S1 C7 -27.53(10) . . . . ?
N2 Pd1 S1 C7 -3.06(8) . . . . ?
Pd1 Pd1 S1 C7 -179.15(7) 3_667 . . . ?
N1 Pd1 S2 C14 -10.92(8) . . . . ?
N3 Pd1 S2 C14 169.93(8) . . . . ?
S1 Pd1 S2 C14 -71.79(9) . . . . ?
N2 Pd1 S2 C14 -96.26(8) . . . . ?
Pd1 Pd1 S2 C14 79.91(7) 3_667 . . . ?
N1 Pd1 S2 C13 92.52(8) . . . . ?
N3 Pd1 S2 C13 -86.63(8) . . . . ?
S1 Pd1 S2 C13 31.65(10) . . . . ?
N2 Pd1 S2 C13 7.19(8) . . . . ?
Pd1 Pd1 S2 C13 -176.64(7) 3_667 . . . ?
O5 S4 O4 S4' -46.9(11) . . . . ?
O6 S4 O4 S4' 176.5(11) . . . . ?
C18 S4 O4 S4' 65.2(11) . . . . ?
O5 S4' O4 S4 102.6(16) . . . . ?
C18 S4' O4 S4 -94.9(12) . . . . ?
O6 S4' O4 S4 -2.4(8) . . . . ?
C18 S4' O5 S4 144(2) . . . . ?
O4 S4' O5 S4 -61.4(14) . . . . ?
O6 S4' O5 S4 32.3(10) . . . . ?
O4 S4 O5 S4' 90.2(14) . . . . ?
O6 S4 O5 S4' -132.6(14) . . . . ?
C18 S4 O5 S4' -21.5(14) . . . . ?
O4 S4 O6 S4' -175.2(15) . . . . ?
O5 S4 O6 S4' 47.7(15) . . . . ?
C18 S4 O6 S4' -63.7(15) . . . . ?
O5 S4' O6 S4 -115.1(19) . . . . ?
C18 S4' O6 S4 104.0(16) . . . . ?
O4 S4' O6 S4 3.7(12) . . . . ?
N3 Pd1 N1 C1 81(4) . . . . ?
S2 Pd1 N1 C1 2.09(12) . . . . ?
S1 Pd1 N1 C1 167.30(13) . . . . ?
N2 Pd1 N1 C1 84.77(13) . . . . ?
Pd1 Pd1 N1 C1 -94.67(12) 3_667 . . . ?
N3 Pd1 N1 C5 -93(4) . . . . ?
S2 Pd1 N1 C5 -171.89(12) . . . . ?
S1 Pd1 N1 C5 -6.68(12) . . . . ?
N2 Pd1 N1 C5 -89.21(13) . . . . ?
Pd1 Pd1 N1 C5 91.35(12) 3_667 . . . ?
N1 Pd1 N2 C8 60.88(13) . . . . ?
N3 Pd1 N2 C8 -119.17(13) . . . . ?
S2 Pd1 N2 C8 147.65(12) . . . . ?
S1 Pd1 N2 C8 -25.36(12) . . . . ?
Pd1 Pd1 N2 C8 69.2(6) 3_667 . . . ?
N1 Pd1 N2 C12 -64.86(12) . . . . ?
N3 Pd1 N2 C12 115.09(13) . . . . ?
S2 Pd1 N2 C12 21.91(12) . . . . ?
S1 Pd1 N2 C12 -151.09(12) . . . . ?
Pd1 Pd1 N2 C12 -56.6(6) 3_667 . . . ?
N1 Pd1 N3 C15 18(7) . . . . ?
S2 Pd1 N3 C15 97(3) . . . . ?
S1 Pd1 N3 C15 -68(3) . . . . ?
N2 Pd1 N3 C15 14(3) . . . . ?
Pd1 Pd1 N3 C15 -166(3) 3_667 . . . ?
C5 N1 C1 C2 1.8(2) . . . . ?
Pd1 N1 C1 C2 -172.25(13) . . . . ?
C5 N1 C1 C14 -175.02(15) . . . . ?
Pd1 N1 C1 C14 10.9(2) . . . . ?
N1 C1 C2 C3 -2.0(3) . . . . ?
C14 C1 C2 C3 174.75(17) . . . . ?
C1 C2 C3 C4 0.5(3) . . . . ?
C2 C3 C4 C5 1.1(3) . . . . ?
C1 N1 C5 C4 -0.1(2) . . . . ?
Pd1 N1 C5 C4 173.92(13) . . . . ?
C1 N1 C5 C6 177.23(15) . . . . ?
Pd1 N1 C5 C6 -8.7(2) . . . . ?
C3 C4 C5 N1 -1.3(3) . . . . ?
C3 C4 C5 C6 -178.60(17) . . . . ?
N1 C5 C6 S1 24.4(2) . . . . ?
C4 C5 C6 S1 -158.22(14) . . . . ?
C7 S1 C6 C5 76.85(15) . . . . ?
Pd1 S1 C6 C5 -24.46(13) . . . . ?
C6 S1 C7 C8 -68.89(16) . . . . ?
Pd1 S1 C7 C8 29.97(15) . . . . ?
C12 N2 C8 C9 -6.2(3) . . . . ?
Pd1 N2 C8 C9 -120.27(17) . . . . ?
C12 N2 C8 C7 167.18(16) . . . . ?
Pd1 N2 C8 C7 53.12(17) . . . . ?
S1 C7 C8 N2 -61.8(2) . . . . ?
S1 C7 C8 C9 111.46(19) . . . . ?
N2 C8 C9 C10 1.9(3) . . . . ?
C7 C8 C9 C10 -170.89(19) . . . . ?
C8 C9 C10 C11 2.2(3) . . . . ?
C9 C10 C11 C12 -2.1(3) . . . . ?
C8 N2 C12 C11 6.4(3) . . . . ?
Pd1 N2 C12 C11 120.65(17) . . . . ?
C8 N2 C12 C13 -166.48(16) . . . . ?
Pd1 N2 C12 C13 -52.26(17) . . . . ?
C10 C11 C12 N2 -2.3(3) . . . . ?
C10 C11 C12 C13 169.96(19) . . . . ?
N2 C12 C13 S2 65.3(2) . . . . ?
C11 C12 C13 S2 -107.4(2) . . . . ?
C14 S2 C13 C12 63.70(16) . . . . ?
Pd1 S2 C13 C12 -35.45(15) . . . . ?
N1 C1 C14 S2 -21.8(2) . . . . ?
C2 C1 C14 S2 161.35(15) . . . . ?
C13 S2 C14 C1 -81.35(15) . . . . ?
Pd1 S2 C14 C1 19.38(14) . . . . ?
Pd1 N3 C15 C16 -130(27) . . . . ?
O2 S3 C17 F3 179.58(18) . . . . ?
O3 S3 C17 F3 59.3(2) . . . . ?
O1 S3 C17 F3 -61.42(19) . . . . ?
O2 S3 C17 F1 59.2(2) . . . . ?
O3 S3 C17 F1 -61.1(2) . . . . ?
O1 S3 C17 F1 178.16(17) . . . . ?
O2 S3 C17 F2 -59.8(2) . . . . ?
O3 S3 C17 F2 179.97(18) . . . . ?
O1 S3 C17 F2 59.2(2) . . . . ?
O5 S4' C18 F5 -166.9(11) . . . . ?
O4 S4' C18 F5 35.9(8) . . . . ?
O6 S4' C18 F5 -50.5(6) . . . . ?
O5 S4' C18 F6 -37.3(14) . . . . ?
O4 S4' C18 F6 165.5(5) . . . . ?
O6 S4' C18 F6 79.2(5) . . . . ?
O5 S4' C18 F4 73.0(13) . . . . ?
O4 S4' C18 F4 -84.1(6) . . . . ?
O6 S4' C18 F4 -170.5(3) . . . . ?
O5 S4' C18 S4 -148(2) . . . . ?
O4 S4' C18 S4 54.9(10) . . . . ?
O6 S4' C18 S4 -31.5(8) . . . . ?
O4 S4 C18 F5 60.21(19) . . . . ?
O5 S4 C18 F5 -179.31(16) . . . . ?
O6 S4 C18 F5 -60.12(18) . . . . ?
O4 S4 C18 F6 -178.59(17) . . . . ?
O5 S4 C18 F6 -58.11(19) . . . . ?
O6 S4 C18 F6 61.08(19) . . . . ?
O4 S4 C18 F4 -59.71(19) . . . . ?
O5 S4 C18 F4 60.77(18) . . . . ?
O6 S4 C18 F4 179.96(16) . . . . ?
O4 S4 C18 S4' -103.8(11) . . . . ?
O5 S4 C18 S4' 16.7(11) . . . . ?
O6 S4 C18 S4' 135.8(11) . . . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 1.437
_refine_diff_density_min -0.949
_refine_diff_density_rms 0.107
#===END
data_l25810
_database_code_depnum_ccdc_archive 'CCDC 842463'
#TrackingRef '- CombinedCIFs.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C18 H17 F6 N3 O6 Pt S4'
_chemical_formula_weight 808.68
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'
Pt Pt -1.7033 8.3905 '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 12.3114(7)
_cell_length_b 17.5704(10)
_cell_length_c 12.2608(7)
_cell_angle_alpha 90.00
_cell_angle_beta 112.402(3)
_cell_angle_gamma 90.00
_cell_volume 2452.1(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9988
_cell_measurement_theta_min 2.31
_cell_measurement_theta_max 25.83
_exptl_crystal_description irregular
_exptl_crystal_colour red
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas no
_exptl_crystal_density_diffrn 2.191
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1560
_exptl_absorpt_coefficient_mu 6.151
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.4754
_exptl_absorpt_correction_T_max 0.7168
_exptl_absorpt_process_details 'sadabs v2008/1'
_exptl_special_details
;
All H atoms were added in their calculated positions
and were treated using appropriate riding models.
;
_diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 72537
_diffrn_reflns_av_R_equivalents 0.0696
_diffrn_reflns_av_sigmaI/netI 0.0318
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 1.79
_diffrn_reflns_theta_max 26.54
_reflns_number_total 5083
_reflns_number_gt 4202
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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.
Shelx restraints used:
same s4' > f6'
same s4 > f6
;
_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^)+(0.0236P)^2^+1.2566P] 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 5083
_refine_ls_number_parameters 411
_refine_ls_number_restraints 19
_refine_ls_R_factor_all 0.0375
_refine_ls_R_factor_gt 0.0241
_refine_ls_wR_factor_ref 0.0497
_refine_ls_wR_factor_gt 0.0464
_refine_ls_goodness_of_fit_ref 1.047
_refine_ls_restrained_S_all 1.046
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
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
Pt1 Pt 0.869764(12) 0.511832(8) 0.479116(12) 0.01724(5) Uani 1 1 d . . .
S1 S 0.84488(9) 0.40399(5) 0.57569(9) 0.0256(2) Uani 1 1 d . . .
S2 S 0.84637(9) 0.63336(6) 0.39972(8) 0.0245(2) Uani 1 1 d . . .
S3 S 0.76821(8) 0.62293(6) 0.03062(8) 0.0236(2) Uani 1 1 d . . .
F1 F 0.5815(3) 0.54453(18) -0.0884(2) 0.0610(9) Uani 1 1 d . . .
F2 F 0.5481(2) 0.64923(17) -0.0163(3) 0.0628(9) Uani 1 1 d . . .
F3 F 0.6159(2) 0.55293(15) 0.0955(2) 0.0455(7) Uani 1 1 d . . .
O1 O 0.7540(2) 0.66390(15) -0.0752(2) 0.0299(7) Uani 1 1 d . . .
O2 O 0.8347(3) 0.55415(17) 0.0490(3) 0.0435(8) Uani 1 1 d . . .
O3 O 0.7956(3) 0.67029(18) 0.1321(3) 0.0481(9) Uani 1 1 d . . .
N1 N 0.9168(2) 0.56446(16) 0.6355(2) 0.0152(6) Uani 1 1 d . . .
N2 N 0.6573(3) 0.53700(19) 0.4629(3) 0.0229(7) Uani 1 1 d . . .
N3 N 0.8195(3) 0.45993(19) 0.3229(3) 0.0226(7) Uani 1 1 d . . .
C1 C 0.9178(3) 0.4394(2) 0.7236(3) 0.0230(9) Uani 1 1 d . . .
H1A H 0.8755 0.4205 0.7726 0.028 Uiso 1 1 calc R . .
H1B H 0.9984 0.4182 0.7567 0.028 Uiso 1 1 calc R . .
C2 C 0.9253(3) 0.5243(2) 0.7326(3) 0.0175(8) Uani 1 1 d . . .
C3 C 0.9467(3) 0.5602(2) 0.8383(3) 0.0231(9) Uani 1 1 d . . .
H3 H 0.9510 0.5315 0.9055 0.028 Uiso 1 1 calc R . .
C4 C 0.9620(3) 0.6381(2) 0.8464(3) 0.0231(9) Uani 1 1 d . . .
H4 H 0.9771 0.6634 0.9192 0.028 Uiso 1 1 calc R . .
C5 C 0.9551(3) 0.6786(2) 0.7481(3) 0.0212(8) Uani 1 1 d . . .
H5 H 0.9670 0.7321 0.7531 0.025 Uiso 1 1 calc R . .
C6 C 0.9312(3) 0.6417(2) 0.6430(3) 0.0177(8) Uani 1 1 d . . .
C7 C 0.9254(3) 0.6828(2) 0.5360(3) 0.0213(8) Uani 1 1 d . . .
H7A H 1.0065 0.6926 0.5414 0.026 Uiso 1 1 calc R . .
H7B H 0.8874 0.7328 0.5338 0.026 Uiso 1 1 calc R . .
C8 C 0.6909(3) 0.6517(2) 0.3770(4) 0.0294(10) Uani 1 1 d . . .
H8A H 0.6788 0.7072 0.3805 0.035 Uiso 1 1 calc R . .
H8B H 0.6395 0.6336 0.2975 0.035 Uiso 1 1 calc R . .
C9 C 0.6564(3) 0.6127(2) 0.4677(3) 0.0245(9) Uani 1 1 d . . .
C10 C 0.6381(3) 0.6515(3) 0.5581(4) 0.0320(10) Uani 1 1 d . . .
H10 H 0.6344 0.7055 0.5590 0.038 Uiso 1 1 calc R . .
C11 C 0.6254(3) 0.6082(3) 0.6465(4) 0.0356(11) Uani 1 1 d . . .
H11 H 0.6085 0.6326 0.7073 0.043 Uiso 1 1 calc R . .
C12 C 0.6370(3) 0.5299(3) 0.6479(4) 0.0316(10) Uani 1 1 d . . .
H12 H 0.6328 0.5002 0.7109 0.038 Uiso 1 1 calc R . .
C13 C 0.6550(3) 0.4964(2) 0.5543(4) 0.0257(9) Uani 1 1 d . . .
C14 C 0.6895(3) 0.4143(2) 0.5524(4) 0.0316(10) Uani 1 1 d . . .
H14A H 0.6406 0.3915 0.4755 0.038 Uiso 1 1 calc R . .
H14B H 0.6739 0.3861 0.6149 0.038 Uiso 1 1 calc R . .
C15 C 0.6212(4) 0.5906(2) 0.0032(4) 0.0329(10) Uani 1 1 d . . .
C17 C 0.7872(3) 0.4305(2) 0.2350(3) 0.0200(8) Uani 1 1 d . . .
C18 C 0.7463(3) 0.3921(2) 0.1208(3) 0.0237(9) Uani 1 1 d . . .
H18A H 0.7727 0.4204 0.0666 0.035 Uiso 1 1 calc R . .
H18B H 0.6602 0.3898 0.0883 0.035 Uiso 1 1 calc R . .
H18C H 0.7783 0.3404 0.1308 0.035 Uiso 1 1 calc R . .
S4 S 0.76937(16) 0.20515(13) 0.35377(19) 0.0174(4) Uani 0.832(4) 1 d PD A 1
O4 O 0.8161(3) 0.2288(2) 0.2685(4) 0.0270(9) Uani 0.832(4) 1 d PD A 1
O5 O 0.8217(3) 0.23999(19) 0.4673(3) 0.0319(9) Uani 0.832(4) 1 d PD A 1
O6 O 0.7487(3) 0.12435(18) 0.3547(3) 0.0290(9) Uani 0.832(4) 1 d PD A 1
C16 C 0.6216(4) 0.2442(3) 0.2964(5) 0.0288(12) Uani 0.832(4) 1 d PD A 1
F4 F 0.6226(2) 0.31986(16) 0.2901(3) 0.0344(8) Uani 0.832(4) 1 d PD A 1
F5 F 0.5599(3) 0.2177(2) 0.1886(3) 0.0475(10) Uani 0.832(4) 1 d PD A 1
F6 F 0.5635(4) 0.2263(2) 0.3642(4) 0.0484(11) Uani 0.832(4) 1 d PD A 1
S4' S 0.7590(11) 0.2274(7) 0.3219(11) 0.035(3) Uani 0.168(4) 1 d PD A 2
O4' O 0.752(2) 0.2116(11) 0.2077(16) 0.051(6) Uani 0.168(4) 1 d PD A 2
O5' O 0.8260(17) 0.1710(14) 0.4068(18) 0.070(9) Uani 0.168(4) 1 d PD A 2
O6' O 0.7816(18) 0.3053(9) 0.3597(18) 0.056(7) Uani 0.168(4) 1 d PD A 2
C16' C 0.6139(14) 0.2121(12) 0.3248(17) 0.0288(12) Uani 0.168(4) 1 d PD A 2
F4' F 0.612(2) 0.2289(15) 0.4299(17) 0.066(8) Uani 0.168(4) 1 d PD A 2
F5' F 0.5351(16) 0.2547(12) 0.244(2) 0.072(7) Uani 0.168(4) 1 d PD A 2
F6' F 0.5824(15) 0.1409(8) 0.298(2) 0.079(7) Uani 0.168(4) 1 d PD 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
Pt1 0.01600(7) 0.01973(9) 0.01598(7) -0.00394(6) 0.00608(5) 0.00031(6)
S1 0.0324(6) 0.0166(5) 0.0280(5) -0.0053(4) 0.0117(4) -0.0031(4)
S2 0.0270(5) 0.0284(6) 0.0184(5) 0.0040(4) 0.0088(4) 0.0015(4)
S3 0.0210(5) 0.0225(6) 0.0235(5) 0.0022(4) 0.0043(4) -0.0038(4)
F1 0.0539(19) 0.075(2) 0.0458(18) -0.0184(16) 0.0096(14) -0.0425(16)
F2 0.0338(16) 0.059(2) 0.103(3) 0.0324(18) 0.0340(17) 0.0188(14)
F3 0.0467(16) 0.0434(17) 0.0575(18) 0.0160(13) 0.0324(14) -0.0008(13)
O1 0.0329(16) 0.0307(17) 0.0268(16) 0.0057(12) 0.0123(13) -0.0059(12)
O2 0.0298(17) 0.0325(19) 0.072(2) 0.0188(16) 0.0237(16) 0.0089(14)
O3 0.072(2) 0.041(2) 0.0243(17) -0.0077(14) 0.0108(16) -0.0195(17)
N1 0.0116(14) 0.0166(17) 0.0162(15) -0.0018(12) 0.0039(12) -0.0016(11)
N2 0.0124(15) 0.032(2) 0.0217(17) -0.0060(14) 0.0039(13) -0.0022(13)
N3 0.0170(16) 0.032(2) 0.0187(17) -0.0076(14) 0.0070(13) 0.0000(13)
C1 0.024(2) 0.021(2) 0.023(2) 0.0028(16) 0.0068(16) 0.0001(16)
C2 0.0114(16) 0.021(2) 0.0194(18) -0.0006(15) 0.0051(14) 0.0019(14)
C3 0.0141(18) 0.035(3) 0.0183(19) 0.0010(16) 0.0041(15) 0.0039(16)
C4 0.0199(19) 0.027(2) 0.020(2) -0.0062(16) 0.0048(16) 0.0036(16)
C5 0.0145(18) 0.016(2) 0.030(2) -0.0047(16) 0.0051(16) 0.0012(14)
C6 0.0086(16) 0.018(2) 0.025(2) 0.0008(15) 0.0040(14) 0.0008(14)
C7 0.0208(19) 0.016(2) 0.025(2) 0.0021(15) 0.0067(16) 0.0000(15)
C8 0.021(2) 0.033(3) 0.025(2) 0.0031(18) -0.0015(17) 0.0083(17)
C9 0.0128(18) 0.032(3) 0.021(2) -0.0029(17) -0.0022(15) 0.0018(16)
C10 0.017(2) 0.039(3) 0.033(2) -0.0080(19) 0.0025(18) 0.0111(17)
C11 0.018(2) 0.062(3) 0.023(2) -0.012(2) 0.0033(17) 0.010(2)
C12 0.0154(19) 0.056(3) 0.023(2) -0.0011(19) 0.0063(16) -0.0038(18)
C13 0.0104(16) 0.034(3) 0.030(2) -0.0062(17) 0.0045(15) -0.0073(15)
C14 0.026(2) 0.037(3) 0.030(2) -0.0057(19) 0.0081(18) -0.0149(18)
C15 0.031(2) 0.033(3) 0.038(3) 0.008(2) 0.017(2) 0.0013(19)
C17 0.0149(18) 0.022(2) 0.026(2) 0.0000(17) 0.0101(16) 0.0006(15)
C18 0.025(2) 0.022(2) 0.021(2) -0.0025(16) 0.0048(16) -0.0027(16)
S4 0.0185(8) 0.0157(12) 0.0166(11) 0.0003(7) 0.0053(8) -0.0009(7)
O4 0.027(2) 0.029(2) 0.032(2) 0.0096(17) 0.0194(19) 0.0042(16)
O5 0.040(2) 0.027(2) 0.0227(19) -0.0039(15) 0.0046(16) -0.0035(16)
O6 0.042(2) 0.0158(19) 0.033(2) -0.0020(15) 0.0192(18) -0.0015(15)
C16 0.028(3) 0.026(4) 0.037(3) -0.004(2) 0.018(3) -0.004(2)
F4 0.0352(17) 0.0244(18) 0.0454(19) 0.0008(13) 0.0175(14) 0.0088(13)
F5 0.0256(18) 0.054(2) 0.047(2) -0.0175(18) -0.0039(15) -0.0001(15)
F6 0.043(3) 0.047(2) 0.073(3) 0.000(3) 0.043(2) -0.0028(19)
S4' 0.051(6) 0.027(7) 0.014(5) 0.004(4) -0.003(4) 0.002(5)
O4' 0.082(19) 0.028(13) 0.045(15) 0.004(10) 0.027(14) 0.011(12)
O5' 0.030(13) 0.14(3) 0.040(14) 0.044(18) 0.017(11) 0.016(16)
O6' 0.075(16) 0.040(13) 0.065(15) -0.033(11) 0.039(13) -0.032(11)
C16' 0.028(3) 0.026(4) 0.037(3) -0.004(2) 0.018(3) -0.004(2)
F4' 0.065(17) 0.101(18) 0.049(14) 0.025(15) 0.042(12) 0.012(14)
F5' 0.038(13) 0.079(18) 0.076(17) 0.031(13) -0.005(11) 0.015(11)
F6' 0.046(11) 0.039(11) 0.16(2) 0.006(12) 0.047(13) -0.009(8)
_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
Pt1 N3 1.995(3) . ?
Pt1 N1 2.005(3) . ?
Pt1 S1 2.3157(10) . ?
Pt1 S2 2.3187(10) . ?
Pt1 Pt1 3.0768(3) 3_766 ?
S1 C1 1.800(4) . ?
S1 C14 1.832(4) . ?
S2 C7 1.804(4) . ?
S2 C8 1.854(4) . ?
S3 O3 1.426(3) . ?
S3 O2 1.429(3) . ?
S3 O1 1.435(3) . ?
S3 C15 1.802(4) . ?
F1 C15 1.318(5) . ?
F2 C15 1.328(5) . ?
F3 C15 1.334(5) . ?
N1 C2 1.353(4) . ?
N1 C6 1.367(5) . ?
N2 C9 1.332(5) . ?
N2 C13 1.338(5) . ?
N3 C17 1.122(5) . ?
C1 C2 1.496(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.374(5) . ?
C3 C4 1.380(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.372(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.476(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.498(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.391(6) . ?
C10 C11 1.380(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.506(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C17 C18 1.460(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
S4 O5 1.430(4) . ?
S4 O4 1.434(4) . ?
S4 O6 1.443(4) . ?
S4 C16 1.816(5) . ?
C16 F6 1.326(7) . ?
C16 F4 1.332(6) . ?
C16 F5 1.332(6) . ?
S4' O4' 1.398(15) . ?
S4' O6' 1.438(15) . ?
S4' O5' 1.446(15) . ?
S4' C16' 1.820(15) . ?
C16' F6' 1.313(18) . ?
C16' F5' 1.322(17) . ?
C16' F4' 1.329(17) . ?
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
N3 Pt1 N1 178.80(12) . . ?
N3 Pt1 S1 93.65(10) . . ?
N1 Pt1 S1 86.25(9) . . ?
N3 Pt1 S2 94.27(10) . . ?
N1 Pt1 S2 85.48(9) . . ?
S1 Pt1 S2 161.57(4) . . ?
N3 Pt1 Pt1 91.17(9) . 3_766 ?
N1 Pt1 Pt1 90.03(8) . 3_766 ?
S1 Pt1 Pt1 97.87(3) . 3_766 ?
S2 Pt1 Pt1 98.58(3) . 3_766 ?
C1 S1 C14 102.31(19) . . ?
C1 S1 Pt1 96.90(12) . . ?
C14 S1 Pt1 100.00(14) . . ?
C7 S2 C8 102.55(18) . . ?
C7 S2 Pt1 96.78(12) . . ?
C8 S2 Pt1 100.30(14) . . ?
O3 S3 O2 115.2(2) . . ?
O3 S3 O1 113.75(18) . . ?
O2 S3 O1 115.59(19) . . ?
O3 S3 C15 103.5(2) . . ?
O2 S3 C15 103.73(19) . . ?
O1 S3 C15 102.83(18) . . ?
C2 N1 C6 119.6(3) . . ?
C2 N1 Pt1 119.9(2) . . ?
C6 N1 Pt1 120.3(2) . . ?
C9 N2 C13 119.5(3) . . ?
C17 N3 Pt1 177.5(3) . . ?
C2 C1 S1 114.3(3) . . ?
C2 C1 H1A 108.7 . . ?
S1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
S1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
N1 C2 C3 120.9(3) . . ?
N1 C2 C1 118.3(3) . . ?
C3 C2 C1 120.8(3) . . ?
C2 C3 C4 119.7(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 119.3(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C6 C5 C4 119.9(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
N1 C6 C5 120.6(3) . . ?
N1 C6 C7 117.8(3) . . ?
C5 C6 C7 121.6(3) . . ?
C6 C7 S2 114.4(3) . . ?
C6 C7 H7A 108.7 . . ?
S2 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
S2 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C9 C8 S2 112.2(3) . . ?
C9 C8 H8A 109.2 . . ?
S2 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
S2 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N2 C9 C10 122.1(4) . . ?
N2 C9 C8 114.4(3) . . ?
C10 C9 C8 123.1(4) . . ?
C11 C10 C9 117.2(4) . . ?
C11 C10 H10 121.4 . . ?
C9 C10 H10 121.4 . . ?
C10 C11 C12 121.1(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 117.6(4) . . ?
C13 C12 H12 121.2 . . ?
C11 C12 H12 121.2 . . ?
N2 C13 C12 122.0(4) . . ?
N2 C13 C14 113.7(4) . . ?
C12 C13 C14 123.8(4) . . ?
C13 C14 S1 112.1(3) . . ?
C13 C14 H14A 109.2 . . ?
S1 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
S1 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
F1 C15 F2 108.5(4) . . ?
F1 C15 F3 107.2(4) . . ?
F2 C15 F3 106.8(4) . . ?
F1 C15 S3 111.8(3) . . ?
F2 C15 S3 110.7(3) . . ?
F3 C15 S3 111.6(3) . . ?
N3 C17 C18 179.5(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O5 S4 O4 115.3(3) . . ?
O5 S4 O6 115.4(3) . . ?
O4 S4 O6 114.3(2) . . ?
O5 S4 C16 103.2(2) . . ?
O4 S4 C16 103.3(3) . . ?
O6 S4 C16 102.8(2) . . ?
F6 C16 F4 107.0(4) . . ?
F6 C16 F5 107.4(4) . . ?
F4 C16 F5 107.8(5) . . ?
F6 C16 S4 111.6(4) . . ?
F4 C16 S4 111.7(3) . . ?
F5 C16 S4 111.2(4) . . ?
O4' S4' O6' 116.3(14) . . ?
O4' S4' O5' 112.7(15) . . ?
O6' S4' O5' 115.7(16) . . ?
O4' S4' C16' 107.6(13) . . ?
O6' S4' C16' 101.9(12) . . ?
O5' S4' C16' 100.4(11) . . ?
F6' C16' F5' 106.9(17) . . ?
F6' C16' F4' 110.0(19) . . ?
F5' C16' F4' 108.7(19) . . ?
F6' C16' S4' 109.5(14) . . ?
F5' C16' S4' 110.4(15) . . ?
F4' C16' S4' 111.2(14) . . ?
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
N3 Pt1 S1 C1 168.43(16) . . . . ?
N1 Pt1 S1 C1 -12.77(15) . . . . ?
S2 Pt1 S1 C1 -76.26(17) . . . . ?
Pt1 Pt1 S1 C1 76.74(13) 3_766 . . . ?
N3 Pt1 S1 C14 -87.72(16) . . . . ?
N1 Pt1 S1 C14 91.08(16) . . . . ?
S2 Pt1 S1 C14 27.59(18) . . . . ?
Pt1 Pt1 S1 C14 -179.42(14) 3_766 . . . ?
N3 Pt1 S2 C7 -166.06(15) . . . . ?
N1 Pt1 S2 C7 15.12(15) . . . . ?
S1 Pt1 S2 C7 78.71(17) . . . . ?
Pt1 Pt1 S2 C7 -74.23(13) 3_766 . . . ?
N3 Pt1 S2 C8 89.82(16) . . . . ?
N1 Pt1 S2 C8 -89.00(16) . . . . ?
S1 Pt1 S2 C8 -25.41(19) . . . . ?
Pt1 Pt1 S2 C8 -178.35(13) 3_766 . . . ?
S1 Pt1 N1 C2 4.2(2) . . . . ?
S2 Pt1 N1 C2 167.7(2) . . . . ?
Pt1 Pt1 N1 C2 -93.7(2) 3_766 . . . ?
S1 Pt1 N1 C6 -170.6(2) . . . . ?
S2 Pt1 N1 C6 -7.1(2) . . . . ?
Pt1 Pt1 N1 C6 91.5(2) 3_766 . . . ?
C14 S1 C1 C2 -80.7(3) . . . . ?
Pt1 S1 C1 C2 21.1(3) . . . . ?
C6 N1 C2 C3 0.9(5) . . . . ?
Pt1 N1 C2 C3 -174.0(3) . . . . ?
C6 N1 C2 C1 -175.6(3) . . . . ?
Pt1 N1 C2 C1 9.6(4) . . . . ?
S1 C1 C2 N1 -22.3(4) . . . . ?
S1 C1 C2 C3 161.2(3) . . . . ?
N1 C2 C3 C4 -1.2(5) . . . . ?
C1 C2 C3 C4 175.2(3) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C3 C4 C5 C6 1.2(5) . . . . ?
C2 N1 C6 C5 0.5(5) . . . . ?
Pt1 N1 C6 C5 175.3(3) . . . . ?
C2 N1 C6 C7 177.8(3) . . . . ?
Pt1 N1 C6 C7 -7.4(4) . . . . ?
C4 C5 C6 N1 -1.6(5) . . . . ?
C4 C5 C6 C7 -178.7(3) . . . . ?
N1 C6 C7 S2 22.7(4) . . . . ?
C5 C6 C7 S2 -160.0(3) . . . . ?
C8 S2 C7 C6 78.7(3) . . . . ?
Pt1 S2 C7 C6 -23.5(3) . . . . ?
C7 S2 C8 C9 -67.7(3) . . . . ?
Pt1 S2 C8 C9 31.7(3) . . . . ?
C13 N2 C9 C10 -8.3(5) . . . . ?
C13 N2 C9 C8 164.6(3) . . . . ?
S2 C8 C9 N2 -65.5(4) . . . . ?
S2 C8 C9 C10 107.3(4) . . . . ?
N2 C9 C10 C11 2.5(5) . . . . ?
C8 C9 C10 C11 -169.7(3) . . . . ?
C9 C10 C11 C12 3.5(6) . . . . ?
C10 C11 C12 C13 -3.6(6) . . . . ?
C9 N2 C13 C12 8.2(5) . . . . ?
C9 N2 C13 C14 -164.1(3) . . . . ?
C11 C12 C13 N2 -2.3(5) . . . . ?
C11 C12 C13 C14 169.2(3) . . . . ?
N2 C13 C14 S1 67.7(4) . . . . ?
C12 C13 C14 S1 -104.5(4) . . . . ?
C1 S1 C14 C13 64.4(3) . . . . ?
Pt1 S1 C14 C13 -35.0(3) . . . . ?
O3 S3 C15 F1 -179.2(3) . . . . ?
O2 S3 C15 F1 -58.6(4) . . . . ?
O1 S3 C15 F1 62.2(3) . . . . ?
O3 S3 C15 F2 59.7(4) . . . . ?
O2 S3 C15 F2 -179.7(3) . . . . ?
O1 S3 C15 F2 -58.9(3) . . . . ?
O3 S3 C15 F3 -59.1(3) . . . . ?
O2 S3 C15 F3 61.5(4) . . . . ?
O1 S3 C15 F3 -177.7(3) . . . . ?
O5 S4 C16 F6 -60.8(4) . . . . ?
O4 S4 C16 F6 178.8(4) . . . . ?
O6 S4 C16 F6 59.6(4) . . . . ?
O5 S4 C16 F4 59.0(4) . . . . ?
O4 S4 C16 F4 -61.5(4) . . . . ?
O6 S4 C16 F4 179.3(4) . . . . ?
O5 S4 C16 F5 179.4(4) . . . . ?
O4 S4 C16 F5 58.9(5) . . . . ?
O6 S4 C16 F5 -60.3(4) . . . . ?
O4' S4' C16' F6' 60.5(19) . . . . ?
O6' S4' C16' F6' -176.7(17) . . . . ?
O5' S4' C16' F6' -57(2) . . . . ?
O4' S4' C16' F5' -57(2) . . . . ?
O6' S4' C16' F5' 65.9(19) . . . . ?
O5' S4' C16' F5' -175(2) . . . . ?
O4' S4' C16' F4' -177.6(18) . . . . ?
O6' S4' C16' F4' -55(2) . . . . ?
O5' S4' C16' F4' 64(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 0.875
_refine_diff_density_min -0.603
_refine_diff_density_rms 0.112
#===END
data_l4611
_database_code_depnum_ccdc_archive 'CCDC 842464'
#TrackingRef '- CombinedCIFs.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C16 H19 F3 N2 O4 Pd S3'
_chemical_formula_weight 562.91
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 Triclinic
_symmetry_space_group_name_H-M P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.7020(6)
_cell_length_b 10.3167(7)
_cell_length_c 10.6734(7)
_cell_angle_alpha 79.150(2)
_cell_angle_beta 89.371(3)
_cell_angle_gamma 75.100(3)
_cell_volume 1013.16(11)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9698
_cell_measurement_theta_min 3.05
_cell_measurement_theta_max 43.80
_exptl_crystal_description rectangular
_exptl_crystal_colour red
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas no
_exptl_crystal_density_diffrn 1.845
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 564
_exptl_absorpt_coefficient_mu 1.278
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6697
_exptl_absorpt_correction_T_max 0.8464
_exptl_absorpt_process_details 'sadabs v2008/1'
_exptl_special_details
;
water H atoms were located and refined with geometrical
restraints.
All other H atoms were added in their calculated positions
and were treated using appropriate riding models.
;
_diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 74401
_diffrn_reflns_av_R_equivalents 0.0256
_diffrn_reflns_av_sigmaI/netI 0.0242
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 1.94
_diffrn_reflns_theta_max 44.13
_reflns_number_total 15753
_reflns_number_gt 13679
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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.
Shelx restraints and constraints used:
dfix 0.900 0.005 o1s h1s1 o1s h1s2
;
_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^)+(0.0281P)^2^+0.2145P] 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_number_reflns 15753
_refine_ls_number_parameters 271
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0314
_refine_ls_R_factor_gt 0.0241
_refine_ls_wR_factor_ref 0.0590
_refine_ls_wR_factor_gt 0.0561
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_restrained_S_all 1.020
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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 0.036808(6) 0.140656(5) 0.474837(5) 0.01354(1) Uani 1 1 d . . .
S1 S 0.28405(2) 0.04694(2) 0.474356(19) 0.01822(3) Uani 1 1 d . . .
S2 S -0.18529(2) 0.29643(2) 0.419933(19) 0.01683(3) Uani 1 1 d . . .
N1 N 0.04081(7) 0.12982(6) 0.27981(6) 0.01442(9) Uani 1 1 d . . .
N2 N 0.11886(7) 0.35869(7) 0.39272(6) 0.01578(10) Uani 1 1 d . . .
C1 C 0.04008(10) 0.16464(9) 0.65999(7) 0.01990(13) Uani 1 1 d . . .
H1A H 0.0818 0.2404 0.6659 0.030 Uiso 1 1 calc R . .
H1B H 0.0976 0.0804 0.7131 0.030 Uiso 1 1 calc R . .
H1C H -0.0576 0.1847 0.6900 0.030 Uiso 1 1 calc R . .
C2 C -0.07323(9) 0.19765(7) 0.20182(7) 0.01627(11) Uani 1 1 d . . .
C3 C -0.06750(11) 0.20346(9) 0.07071(8) 0.02260(15) Uani 1 1 d . . .
H3 H -0.1491 0.2499 0.0164 0.027 Uiso 1 1 calc R . .
C4 C 0.05864(13) 0.14069(10) 0.02038(8) 0.02589(17) Uani 1 1 d . . .
H4 H 0.0646 0.1447 -0.0691 0.031 Uiso 1 1 calc R . .
C5 C 0.17614(11) 0.07208(9) 0.10098(8) 0.02255(15) Uani 1 1 d . . .
H5 H 0.2636 0.0288 0.0679 0.027 Uiso 1 1 calc R . .
C6 C 0.16313(9) 0.06802(8) 0.23112(7) 0.01667(12) Uani 1 1 d . . .
C7 C 0.28450(10) -0.01083(9) 0.32383(8) 0.02103(14) Uani 1 1 d . . .
H7A H 0.3753 -0.0059 0.2824 0.025 Uiso 1 1 calc R . .
H7B H 0.2824 -0.1080 0.3421 0.025 Uiso 1 1 calc R . .
C8 C 0.34907(9) 0.20083(9) 0.42713(8) 0.01957(13) Uani 1 1 d . . .
H8A H 0.3684 0.2342 0.5046 0.023 Uiso 1 1 calc R . .
H8B H 0.4399 0.1771 0.3832 0.023 Uiso 1 1 calc R . .
C9 C 0.24303(8) 0.31280(8) 0.34016(7) 0.01591(11) Uani 1 1 d . . .
C10 C 0.26548(9) 0.35586(8) 0.21223(8) 0.01826(12) Uani 1 1 d . . .
H10 H 0.3543 0.3215 0.1763 0.022 Uiso 1 1 calc R . .
C11 C 0.15430(10) 0.45070(9) 0.13819(8) 0.02017(13) Uani 1 1 d . . .
H11 H 0.1681 0.4863 0.0516 0.024 Uiso 1 1 calc R . .
C12 C 0.02295(9) 0.49316(8) 0.19138(8) 0.01856(12) Uani 1 1 d . . .
H12A H -0.0550 0.5564 0.1418 0.022 Uiso 1 1 calc R . .
C13 C 0.00867(8) 0.44054(7) 0.31916(7) 0.01536(11) Uani 1 1 d . . .
C14 C -0.13275(9) 0.45789(8) 0.38177(8) 0.01810(12) Uani 1 1 d . . .
H14A H -0.2068 0.5264 0.3240 0.022 Uiso 1 1 calc R . .
H14B H -0.1269 0.4929 0.4613 0.022 Uiso 1 1 calc R . .
C15 C -0.20843(9) 0.26160(9) 0.26198(8) 0.01928(13) Uani 1 1 d . . .
H15A H -0.2726 0.2002 0.2676 0.023 Uiso 1 1 calc R . .
H15B H -0.2567 0.3486 0.2049 0.023 Uiso 1 1 calc R . .
S5 S 0.57008(2) 0.73108(2) 0.146595(19) 0.01726(3) Uani 1 1 d . . .
F1 F 0.32041(7) 0.70141(9) 0.22527(9) 0.03805(17) Uani 1 1 d . . .
F2 F 0.40844(8) 0.58683(8) 0.08220(8) 0.03387(14) Uani 1 1 d . . .
F3 F 0.49383(9) 0.52103(8) 0.27587(8) 0.03841(16) Uani 1 1 d . . .
O1 O 0.49458(10) 0.84433(8) 0.05139(8) 0.03352(17) Uani 1 1 d . . .
O2 O 0.59777(8) 0.76854(8) 0.26574(7) 0.02487(12) Uani 1 1 d . . .
O3 O 0.68690(8) 0.63564(9) 0.10317(8) 0.02927(15) Uani 1 1 d . . .
C16 C 0.44116(9) 0.63001(9) 0.18523(9) 0.02136(14) Uani 1 1 d . . .
O1S O 0.59856(10) 0.06283(8) 0.20707(7) 0.02882(14) Uani 1 1 d D . .
H1S1 H 0.618(2) -0.0284(5) 0.221(2) 0.057(6) Uiso 1 1 d D . .
H1S2 H 0.574(2) 0.088(2) 0.1240(6) 0.050(5) Uiso 1 1 d D . .
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 0.01499(2) 0.01407(2) 0.00968(2) -0.00196(1) 0.00029(1) -0.00065(2)
S1 0.01721(8) 0.01834(7) 0.01366(7) -0.00055(6) -0.00146(6) 0.00336(6)
S2 0.01397(7) 0.01876(7) 0.01619(7) -0.00364(6) 0.00092(6) -0.00125(6)
N1 0.0179(3) 0.0130(2) 0.0117(2) -0.00264(17) -0.00019(18) -0.00275(18)
N2 0.0152(2) 0.0164(2) 0.0153(2) -0.00583(19) -0.00203(19) -0.00118(19)
C1 0.0234(3) 0.0236(3) 0.0126(3) -0.0046(2) 0.0015(2) -0.0049(3)
C2 0.0217(3) 0.0136(2) 0.0139(3) -0.0030(2) -0.0032(2) -0.0050(2)
C3 0.0341(4) 0.0198(3) 0.0140(3) -0.0030(2) -0.0058(3) -0.0071(3)
C4 0.0435(5) 0.0240(4) 0.0122(3) -0.0057(2) 0.0013(3) -0.0108(4)
C5 0.0338(4) 0.0210(3) 0.0150(3) -0.0078(2) 0.0073(3) -0.0080(3)
C6 0.0217(3) 0.0147(2) 0.0138(3) -0.0046(2) 0.0030(2) -0.0038(2)
C7 0.0209(3) 0.0194(3) 0.0200(3) -0.0072(2) 0.0026(3) 0.0021(3)
C8 0.0143(3) 0.0230(3) 0.0194(3) -0.0046(2) -0.0032(2) -0.0007(2)
C9 0.0148(3) 0.0169(3) 0.0162(3) -0.0052(2) -0.0014(2) -0.0027(2)
C10 0.0182(3) 0.0187(3) 0.0188(3) -0.0045(2) 0.0020(2) -0.0058(2)
C11 0.0236(4) 0.0194(3) 0.0173(3) -0.0008(2) -0.0001(3) -0.0071(3)
C12 0.0207(3) 0.0149(3) 0.0187(3) -0.0014(2) -0.0038(2) -0.0033(2)
C13 0.0160(3) 0.0128(2) 0.0171(3) -0.0054(2) -0.0023(2) -0.0015(2)
C14 0.0168(3) 0.0155(3) 0.0209(3) -0.0074(2) -0.0012(2) 0.0006(2)
C15 0.0179(3) 0.0197(3) 0.0201(3) -0.0053(2) -0.0056(2) -0.0033(2)
S5 0.01584(7) 0.01711(7) 0.01694(7) -0.00106(6) -0.00199(6) -0.00238(6)
F1 0.0188(3) 0.0458(4) 0.0563(5) -0.0281(4) 0.0131(3) -0.0076(3)
F2 0.0331(3) 0.0387(4) 0.0392(4) -0.0221(3) 0.0021(3) -0.0156(3)
F3 0.0418(4) 0.0294(3) 0.0418(4) 0.0072(3) 0.0001(3) -0.0153(3)
O1 0.0425(4) 0.0230(3) 0.0286(3) 0.0065(3) -0.0137(3) -0.0046(3)
O2 0.0268(3) 0.0266(3) 0.0226(3) -0.0070(2) -0.0047(2) -0.0076(2)
O3 0.0176(3) 0.0390(4) 0.0294(3) -0.0106(3) 0.0055(2) -0.0014(3)
C16 0.0172(3) 0.0214(3) 0.0265(4) -0.0089(3) 0.0028(3) -0.0040(3)
O1S 0.0380(4) 0.0294(3) 0.0228(3) -0.0050(3) -0.0051(3) -0.0151(3)
_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 C1 2.0389(8) . ?
Pd1 N1 2.1049(6) . ?
Pd1 S2 2.3370(2) . ?
Pd1 S1 2.3447(3) . ?
Pd1 N2 2.5739(7) . ?
Pd1 Pd1 3.1132(2) 2_556 ?
S1 C7 1.8154(9) . ?
S1 C8 1.8383(10) . ?
S2 C15 1.8165(9) . ?
S2 C14 1.8376(9) . ?
N1 C6 1.3443(10) . ?
N1 C2 1.3452(10) . ?
N2 C13 1.3330(10) . ?
N2 C9 1.3349(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.3904(11) . ?
C2 C15 1.5048(12) . ?
C3 C4 1.3837(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.3849(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.3871(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.5025(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.5036(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.3871(11) . ?
C10 C11 1.3893(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.3889(13) . ?
C11 H11 0.9500 . ?
C12 C13 1.3892(11) . ?
C12 H12A 0.9500 . ?
C13 C14 1.5032(12) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
S5 O3 1.4336(8) . ?
S5 O1 1.4365(8) . ?
S5 O2 1.4438(7) . ?
S5 C16 1.8219(9) . ?
F1 C16 1.3272(11) . ?
F2 C16 1.3317(11) . ?
F3 C16 1.3294(12) . ?
O1S H1S1 0.895(5) . ?
O1S H1S2 0.892(5) . ?
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
C1 Pd1 N1 175.25(3) . . ?
C1 Pd1 S2 95.17(3) . . ?
N1 Pd1 S2 84.563(19) . . ?
C1 Pd1 S1 94.04(3) . . ?
N1 Pd1 S1 84.68(2) . . ?
S2 Pd1 S1 158.629(8) . . ?
C1 Pd1 N2 92.93(3) . . ?
N1 Pd1 N2 82.34(2) . . ?
S2 Pd1 N2 80.448(16) . . ?
S1 Pd1 N2 79.854(16) . . ?
C1 Pd1 Pd1 97.41(3) . 2_556 ?
N1 Pd1 Pd1 87.266(18) . 2_556 ?
S2 Pd1 Pd1 103.129(7) . 2_556 ?
S1 Pd1 Pd1 94.741(7) . 2_556 ?
N2 Pd1 Pd1 168.666(15) . 2_556 ?
C7 S1 C8 101.46(4) . . ?
C7 S1 Pd1 96.43(3) . . ?
C8 S1 Pd1 101.78(3) . . ?
C15 S2 C14 101.74(4) . . ?
C15 S2 Pd1 97.74(3) . . ?
C14 S2 Pd1 100.80(3) . . ?
C6 N1 C2 120.02(7) . . ?
C6 N1 Pd1 119.47(5) . . ?
C2 N1 Pd1 120.07(5) . . ?
C13 N2 C9 119.59(7) . . ?
C13 N2 Pd1 103.87(5) . . ?
C9 N2 Pd1 103.63(5) . . ?
Pd1 C1 H1A 109.5 . . ?
Pd1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Pd1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 120.92(8) . . ?
N1 C2 C15 117.68(7) . . ?
C3 C2 C15 121.35(8) . . ?
C4 C3 C2 119.11(8) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.73(8) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 118.47(9) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
N1 C6 C5 121.74(8) . . ?
N1 C6 C7 117.34(7) . . ?
C5 C6 C7 120.88(8) . . ?
C6 C7 S1 115.33(6) . . ?
C6 C7 H7A 108.4 . . ?
S1 C7 H7A 108.4 . . ?
C6 C7 H7B 108.4 . . ?
S1 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C9 C8 S1 111.93(6) . . ?
C9 C8 H8A 109.2 . . ?
S1 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
S1 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N2 C9 C10 122.12(7) . . ?
N2 C9 C8 114.35(7) . . ?
C10 C9 C8 123.21(7) . . ?
C9 C10 C11 118.08(8) . . ?
C9 C10 H10 121.0 . . ?
C11 C10 H10 121.0 . . ?
C12 C11 C10 119.70(8) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 118.14(7) . . ?
C11 C12 H12A 120.9 . . ?
C13 C12 H12A 120.9 . . ?
N2 C13 C12 121.94(7) . . ?
N2 C13 C14 114.47(7) . . ?
C12 C13 C14 123.27(7) . . ?
C13 C14 S2 111.94(5) . . ?
C13 C14 H14A 109.2 . . ?
S2 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
S2 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C2 C15 S2 115.39(6) . . ?
C2 C15 H15A 108.4 . . ?
S2 C15 H15A 108.4 . . ?
C2 C15 H15B 108.4 . . ?
S2 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
O3 S5 O1 116.11(5) . . ?
O3 S5 O2 115.03(5) . . ?
O1 S5 O2 113.81(5) . . ?
O3 S5 C16 102.00(5) . . ?
O1 S5 C16 103.25(5) . . ?
O2 S5 C16 104.23(4) . . ?
F1 C16 F3 107.97(9) . . ?
F1 C16 F2 107.38(8) . . ?
F3 C16 F2 108.10(8) . . ?
F1 C16 S5 112.18(7) . . ?
F3 C16 S5 111.02(7) . . ?
F2 C16 S5 110.04(7) . . ?
H1S1 O1S H1S2 103.4(18) . . ?
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
C1 Pd1 S1 C7 168.46(4) . . . . ?
N1 Pd1 S1 C7 -16.13(3) . . . . ?
S2 Pd1 S1 C7 -76.19(4) . . . . ?
N2 Pd1 S1 C7 -99.27(3) . . . . ?
Pd1 Pd1 S1 C7 70.67(3) 2_556 . . . ?
C1 Pd1 S1 C8 -88.37(4) . . . . ?
N1 Pd1 S1 C8 87.04(3) . . . . ?
S2 Pd1 S1 C8 26.98(4) . . . . ?
N2 Pd1 S1 C8 3.90(3) . . . . ?
Pd1 Pd1 S1 C8 173.85(3) 2_556 . . . ?
C1 Pd1 S2 C15 -171.80(4) . . . . ?
N1 Pd1 S2 C15 12.96(3) . . . . ?
S1 Pd1 S2 C15 73.05(4) . . . . ?
N2 Pd1 S2 C15 96.09(3) . . . . ?
Pd1 Pd1 S2 C15 -72.94(3) 2_556 . . . ?
C1 Pd1 S2 C14 84.61(4) . . . . ?
N1 Pd1 S2 C14 -90.62(3) . . . . ?
S1 Pd1 S2 C14 -30.54(4) . . . . ?
N2 Pd1 S2 C14 -7.50(3) . . . . ?
Pd1 Pd1 S2 C14 -176.53(3) 2_556 . . . ?
S2 Pd1 N1 C6 167.91(6) . . . . ?
S1 Pd1 N1 C6 6.40(5) . . . . ?
N2 Pd1 N1 C6 86.85(6) . . . . ?
Pd1 Pd1 N1 C6 -88.62(6) 2_556 . . . ?
S2 Pd1 N1 C2 -4.49(6) . . . . ?
S1 Pd1 N1 C2 -166.00(6) . . . . ?
N2 Pd1 N1 C2 -85.55(6) . . . . ?
Pd1 Pd1 N1 C2 98.98(6) 2_556 . . . ?
C1 Pd1 N2 C13 -115.88(5) . . . . ?
N1 Pd1 N2 C13 64.61(5) . . . . ?
S2 Pd1 N2 C13 -21.13(5) . . . . ?
S1 Pd1 N2 C13 150.54(5) . . . . ?
Pd1 Pd1 N2 C13 88.29(9) 2_556 . . . ?
C1 Pd1 N2 C9 118.45(5) . . . . ?
N1 Pd1 N2 C9 -61.07(5) . . . . ?
S2 Pd1 N2 C9 -146.80(5) . . . . ?
S1 Pd1 N2 C9 24.87(5) . . . . ?
Pd1 Pd1 N2 C9 -37.38(11) 2_556 . . . ?
C6 N1 C2 C3 0.91(11) . . . . ?
Pd1 N1 C2 C3 173.27(6) . . . . ?
C6 N1 C2 C15 178.39(7) . . . . ?
Pd1 N1 C2 C15 -9.26(9) . . . . ?
N1 C2 C3 C4 -1.35(12) . . . . ?
C15 C2 C3 C4 -178.73(8) . . . . ?
C2 C3 C4 C5 0.73(14) . . . . ?
C3 C4 C5 C6 0.27(14) . . . . ?
C2 N1 C6 C5 0.14(12) . . . . ?
Pd1 N1 C6 C5 -172.26(6) . . . . ?
C2 N1 C6 C7 -177.55(7) . . . . ?
Pd1 N1 C6 C7 10.05(9) . . . . ?
C4 C5 C6 N1 -0.73(13) . . . . ?
C4 C5 C6 C7 176.87(8) . . . . ?
N1 C6 C7 S1 -26.90(10) . . . . ?
C5 C6 C7 S1 155.39(7) . . . . ?
C8 S1 C7 C6 -76.77(7) . . . . ?
Pd1 S1 C7 C6 26.68(7) . . . . ?
C7 S1 C8 C9 67.92(7) . . . . ?
Pd1 S1 C8 C9 -31.24(6) . . . . ?
C13 N2 C9 C10 5.17(12) . . . . ?
Pd1 N2 C9 C10 120.09(7) . . . . ?
C13 N2 C9 C8 -168.62(7) . . . . ?
Pd1 N2 C9 C8 -53.70(7) . . . . ?
S1 C8 C9 N2 62.71(8) . . . . ?
S1 C8 C9 C10 -111.00(8) . . . . ?
N2 C9 C10 C11 0.55(12) . . . . ?
C8 C9 C10 C11 173.78(8) . . . . ?
C9 C10 C11 C12 -3.75(12) . . . . ?
C10 C11 C12 C13 1.38(12) . . . . ?
C9 N2 C13 C12 -7.74(11) . . . . ?
Pd1 N2 C13 C12 -122.54(7) . . . . ?
C9 N2 C13 C14 165.96(7) . . . . ?
Pd1 N2 C13 C14 51.16(7) . . . . ?
C11 C12 C13 N2 4.46(12) . . . . ?
C11 C12 C13 C14 -168.68(7) . . . . ?
N2 C13 C14 S2 -64.12(8) . . . . ?
C12 C13 C14 S2 109.48(8) . . . . ?
C15 S2 C14 C13 -64.90(6) . . . . ?
Pd1 S2 C14 C13 35.45(6) . . . . ?
N1 C2 C15 S2 22.53(9) . . . . ?
C3 C2 C15 S2 -160.00(7) . . . . ?
C14 S2 C15 C2 80.88(6) . . . . ?
Pd1 S2 C15 C2 -21.90(6) . . . . ?
O3 S5 C16 F1 -178.39(8) . . . . ?
O1 S5 C16 F1 -57.57(9) . . . . ?
O2 S5 C16 F1 61.60(8) . . . . ?
O3 S5 C16 F3 60.71(8) . . . . ?
O1 S5 C16 F3 -178.48(7) . . . . ?
O2 S5 C16 F3 -59.30(8) . . . . ?
O3 S5 C16 F2 -58.91(7) . . . . ?
O1 S5 C16 F2 61.90(8) . . . . ?
O2 S5 C16 F2 -178.92(7) . . . . ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full 44.13
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max 0.818
_refine_diff_density_min -0.711
_refine_diff_density_rms 0.090