# Supplementary Material (ESI) for Chemical Science
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_coden_Cambridge 1475
loop_
_publ_author_name
'Dong, Vy'
'Borduas, Nadine'
'Zhao, Xiaodan'
'Yeung, Charles'
_publ_contact_author_name 'Dong, Vy'
_publ_contact_author_email vdong@chem.utoronto.ca
_publ_section_title
;
Pd-Catalyzed ortho-Arylation of Phenylacetamides,
Benzamides, and Anilides with Simple Arenes
;
# Attachment '- k1031a.txt'
data_k1031a
_database_code_depnum_ccdc_archive 'CCDC 770196'
#TrackingRef '- k1031a.txt'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C28 H32 F6 N2 O6 Pd2, C H2 Cl2'
_chemical_formula_sum 'C29 H34 Cl2 F6 N2 O6 Pd2'
_chemical_formula_weight 904.28
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'
F F 0.0171 0.0103 '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'
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'
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 c a 21'
_symmetry_space_group_name_Hall 'P 2c -2ac'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'
_cell_length_a 33.6360(3)
_cell_length_b 11.4193(5)
_cell_length_c 18.0125(9)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 6918.6(5)
_cell_formula_units_Z 8
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 38514
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description needle
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.736
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3600
_exptl_absorpt_coefficient_mu 1.269
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.719
_exptl_absorpt_correction_T_max 0.894
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_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 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 38514
_diffrn_reflns_av_R_equivalents 0.0622
_diffrn_reflns_av_sigmaI/netI 0.0796
_diffrn_reflns_limit_h_min -43
_diffrn_reflns_limit_h_max 39
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 27.53
_reflns_number_total 14407
_reflns_number_gt 10501
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_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^)+(0.0568P)^2^+11.8909P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.01(3)
_refine_ls_number_reflns 14407
_refine_ls_number_parameters 863
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0898
_refine_ls_R_factor_gt 0.0546
_refine_ls_wR_factor_ref 0.1359
_refine_ls_wR_factor_gt 0.1166
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_restrained_S_all 1.031
_refine_ls_shift/su_max 0.002
_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
Pd1A Pd 0.434881(16) 0.04521(5) 0.23918(3) 0.03376(14) Uani 1 1 d . . .
Pd2A Pd 0.483322(17) 0.01746(6) 0.37468(4) 0.03480(15) Uani 1 1 d . . .
F1A F 0.39283(17) -0.3215(5) 0.3748(3) 0.0605(14) Uani 1 1 d . . .
F2A F 0.34561(14) -0.1945(5) 0.3826(3) 0.0621(15) Uani 1 1 d . . .
F3A F 0.38608(15) -0.2179(5) 0.4743(3) 0.0582(15) Uani 1 1 d . . .
F4A F 0.3661(2) 0.3343(7) 0.3703(5) 0.126(4) Uani 1 1 d . . .
F5A F 0.3932(2) 0.3010(7) 0.4711(4) 0.103(3) Uani 1 1 d . . .
F6A F 0.4218(3) 0.3990(6) 0.3908(6) 0.122(3) Uani 1 1 d . . .
O1A O 0.45086(16) -0.0984(5) 0.1833(3) 0.0387(13) Uani 1 1 d . . .
O2A O 0.51700(16) 0.1591(5) 0.3606(3) 0.0400(14) Uani 1 1 d . . .
O3A O 0.39916(16) -0.0725(5) 0.3093(3) 0.0384(13) Uani 1 1 d . . .
O4A O 0.44485(15) -0.1181(5) 0.3971(3) 0.0400(14) Uani 1 1 d . . .
O5A O 0.41447(17) 0.1885(5) 0.2995(3) 0.0433(14) Uani 1 1 d . . .
O6A O 0.43786(16) 0.1367(6) 0.4123(3) 0.0410(14) Uani 1 1 d . . .
N1A N 0.4971(2) -0.0201(6) 0.1078(4) 0.0377(16) Uani 1 1 d . . .
H1AA H 0.5175 -0.0369 0.0790 0.045 Uiso 1 1 calc R . .
N2A N 0.5621(2) 0.0791(6) 0.2812(4) 0.0396(17) Uani 1 1 d . . .
H2AA H 0.5785 0.0953 0.2445 0.048 Uiso 1 1 calc R . .
C1A C 0.4794(2) -0.1108(7) 0.1377(4) 0.0347(18) Uani 1 1 d . . .
C2A C 0.4886(2) 0.0999(7) 0.1148(5) 0.0365(18) Uani 1 1 d . . .
C3A C 0.5069(3) 0.1750(8) 0.0630(5) 0.043(2) Uani 1 1 d . . .
H3AA H 0.5244 0.1424 0.0271 0.052 Uiso 1 1 calc R . .
C4A C 0.5004(2) 0.2940(8) 0.0626(5) 0.039(2) Uani 1 1 d . . .
C5A C 0.4746(2) 0.3388(8) 0.1150(5) 0.045(2) Uani 1 1 d . . .
H5AA H 0.4698 0.4208 0.1164 0.054 Uiso 1 1 calc R . .
C6A C 0.4553(2) 0.2657(8) 0.1660(5) 0.040(2) Uani 1 1 d . . .
H6AA H 0.4369 0.2991 0.2000 0.048 Uiso 1 1 calc R . .
C7A C 0.4622(2) 0.1458(7) 0.1684(4) 0.0354(19) Uani 1 1 d . . .
C8A C 0.5218(3) 0.3771(9) 0.0103(5) 0.057(3) Uani 1 1 d . . .
H8AA H 0.5379 0.3320 -0.0248 0.085 Uiso 1 1 calc R . .
H8AB H 0.5391 0.4293 0.0391 0.085 Uiso 1 1 calc R . .
H8AC H 0.5022 0.4238 -0.0170 0.085 Uiso 1 1 calc R . .
C9A C 0.4898(2) -0.2356(7) 0.1148(5) 0.0378(19) Uani 1 1 d . . .
C10A C 0.4866(3) -0.3132(9) 0.1829(6) 0.057(3) Uani 1 1 d . . .
H10A H 0.4595 -0.3093 0.2027 0.086 Uiso 1 1 calc R . .
H10B H 0.5054 -0.2861 0.2208 0.086 Uiso 1 1 calc R . .
H10C H 0.4929 -0.3942 0.1693 0.086 Uiso 1 1 calc R . .
C11A C 0.5331(3) -0.2421(11) 0.0855(8) 0.085(4) Uani 1 1 d . . .
H11A H 0.5358 -0.1919 0.0417 0.127 Uiso 1 1 calc R . .
H11B H 0.5395 -0.3232 0.0721 0.127 Uiso 1 1 calc R . .
H11C H 0.5514 -0.2154 0.1243 0.127 Uiso 1 1 calc R . .
C12A C 0.4613(4) -0.2715(10) 0.0543(7) 0.086(4) Uani 1 1 d . . .
H12A H 0.4343 -0.2754 0.0746 0.129 Uiso 1 1 calc R . .
H12B H 0.4689 -0.3485 0.0350 0.129 Uiso 1 1 calc R . .
H12C H 0.4621 -0.2138 0.0141 0.129 Uiso 1 1 calc R . .
C13A C 0.5443(3) 0.1701(7) 0.3136(5) 0.038(2) Uani 1 1 d . . .
C14A C 0.5575(2) -0.0406(7) 0.2994(5) 0.0360(19) Uani 1 1 d . . .
C15A C 0.5875(2) -0.1151(8) 0.2734(5) 0.046(2) Uani 1 1 d . . .
H15A H 0.6079 -0.0840 0.2427 0.055 Uiso 1 1 calc R . .
C16A C 0.5881(3) -0.2325(9) 0.2912(5) 0.046(2) Uani 1 1 d . . .
C17A C 0.5574(3) -0.2757(8) 0.3362(5) 0.046(2) Uani 1 1 d . . .
H17A H 0.5571 -0.3559 0.3503 0.055 Uiso 1 1 calc R . .
C18A C 0.5274(3) -0.2006(8) 0.3601(5) 0.043(2) Uani 1 1 d . . .
H18A H 0.5067 -0.2314 0.3903 0.051 Uiso 1 1 calc R . .
C19A C 0.5264(2) -0.0829(8) 0.3416(4) 0.0352(19) Uani 1 1 d . . .
C20A C 0.6206(3) -0.3141(9) 0.2612(7) 0.067(3) Uani 1 1 d . . .
H20A H 0.6193 -0.3893 0.2873 0.100 Uiso 1 1 calc R . .
H20B H 0.6467 -0.2782 0.2692 0.100 Uiso 1 1 calc R . .
H20C H 0.6164 -0.3268 0.2080 0.100 Uiso 1 1 calc R . .
C21A C 0.5592(2) 0.2926(8) 0.2968(5) 0.043(2) Uani 1 1 d . . .
C22A C 0.5696(3) 0.3058(9) 0.2142(5) 0.055(3) Uani 1 1 d . . .
H22A H 0.5465 0.2846 0.1840 0.082 Uiso 1 1 calc R . .
H22B H 0.5919 0.2540 0.2020 0.082 Uiso 1 1 calc R . .
H22C H 0.5771 0.3871 0.2040 0.082 Uiso 1 1 calc R . .
C23A C 0.5962(3) 0.3150(9) 0.3443(6) 0.056(3) Uani 1 1 d . . .
H23A H 0.5890 0.3121 0.3970 0.085 Uiso 1 1 calc R . .
H23B H 0.6071 0.3923 0.3324 0.085 Uiso 1 1 calc R . .
H23C H 0.6162 0.2548 0.3338 0.085 Uiso 1 1 calc R . .
C24A C 0.5271(3) 0.3801(9) 0.3176(6) 0.058(3) Uani 1 1 d . . .
H24A H 0.5023 0.3596 0.2922 0.087 Uiso 1 1 calc R . .
H24B H 0.5354 0.4589 0.3025 0.087 Uiso 1 1 calc R . .
H24C H 0.5229 0.3785 0.3714 0.087 Uiso 1 1 calc R . .
C25A C 0.4118(2) -0.1246(7) 0.3656(5) 0.0356(18) Uani 1 1 d . . .
C26A C 0.3834(3) -0.2162(8) 0.3988(5) 0.043(2) Uani 1 1 d . . .
C27A C 0.4194(2) 0.1985(8) 0.3680(5) 0.041(2) Uani 1 1 d . . .
C28A C 0.3991(3) 0.3082(9) 0.4009(5) 0.048(2) Uani 1 1 d . . .
Pd1B Pd 0.682252(17) 0.20008(6) 0.22945(4) 0.03873(16) Uani 1 1 d . . .
Pd2B Pd 0.738584(17) 0.19437(6) 0.10591(3) 0.03645(15) Uani 1 1 d . . .
F1B F 0.6811(3) 0.5686(6) 0.0664(7) 0.150(5) Uani 1 1 d . . .
F2B F 0.6256(3) 0.5128(8) 0.0980(5) 0.134(4) Uani 1 1 d . . .
F3B F 0.6482(2) 0.4653(6) -0.0040(4) 0.096(2) Uani 1 1 d . . .
F4B F 0.59470(16) -0.0008(6) 0.0776(3) 0.0718(18) Uani 1 1 d . . .
F5B F 0.63839(17) -0.0398(6) -0.0067(3) 0.0684(17) Uani 1 1 d . . .
F6B F 0.63645(19) -0.1391(5) 0.0943(3) 0.0716(17) Uani 1 1 d . . .
O1B O 0.70459(17) 0.3388(5) 0.2800(3) 0.0462(15) Uani 1 1 d . . .
O2B O 0.76494(15) 0.0440(5) 0.1328(3) 0.0397(14) Uani 1 1 d . . .
O3B O 0.65817(16) 0.3272(6) 0.1517(3) 0.0465(15) Uani 1 1 d . . .
O4B O 0.70841(17) 0.3397(5) 0.0694(3) 0.0445(15) Uani 1 1 d . . .
O5B O 0.65290(16) 0.0695(6) 0.1712(3) 0.0455(15) Uani 1 1 d . . .
O6B O 0.68891(16) 0.0896(6) 0.0659(3) 0.0431(15) Uani 1 1 d . . .
N1B N 0.7416(2) 0.2479(6) 0.3676(4) 0.0449(18) Uani 1 1 d . . .
H1BA H 0.7597 0.2603 0.4018 0.054 Uiso 1 1 calc R . .
N2B N 0.8172(2) 0.1140(6) 0.1967(4) 0.0393(17) Uani 1 1 d . . .
H2BA H 0.8359 0.0944 0.2285 0.047 Uiso 1 1 calc R . .
C1B C 0.7293(3) 0.3435(8) 0.3323(5) 0.040(2) Uani 1 1 d . . .
C2B C 0.7304(3) 0.1317(8) 0.3591(5) 0.043(2) Uani 1 1 d . . .
C3B C 0.7459(3) 0.0523(9) 0.4109(5) 0.048(2) Uani 1 1 d . . .
H3BA H 0.7634 0.0810 0.4481 0.057 Uiso 1 1 calc R . .
C4B C 0.7372(3) -0.0638(8) 0.4101(5) 0.044(2) Uani 1 1 d . . .
C5B C 0.7116(3) -0.1038(8) 0.3556(5) 0.045(2) Uani 1 1 d . . .
H5BA H 0.7051 -0.1846 0.3532 0.054 Uiso 1 1 calc R . .
C6B C 0.6952(2) -0.0254(8) 0.3036(5) 0.041(2) Uani 1 1 d . . .
H6BA H 0.6770 -0.0546 0.2676 0.049 Uiso 1 1 calc R . .
C7B C 0.7046(2) 0.0932(8) 0.3030(5) 0.040(2) Uani 1 1 d . . .
C8B C 0.7560(3) -0.1486(8) 0.4656(5) 0.055(3) Uani 1 1 d . . .
H8BA H 0.7611 -0.1077 0.5124 0.083 Uiso 1 1 calc R . .
H8BB H 0.7811 -0.1784 0.4454 0.083 Uiso 1 1 calc R . .
H8BC H 0.7378 -0.2142 0.4745 0.083 Uiso 1 1 calc R . .
C9B C 0.7443(3) 0.4620(8) 0.3558(5) 0.047(2) Uani 1 1 d . . .
C10B C 0.7321(4) 0.5556(9) 0.3001(7) 0.071(3) Uani 1 1 d . . .
H10D H 0.7030 0.5594 0.2973 0.106 Uiso 1 1 calc R . .
H10E H 0.7429 0.5359 0.2511 0.106 Uiso 1 1 calc R . .
H10F H 0.7426 0.6317 0.3160 0.106 Uiso 1 1 calc R . .
C11B C 0.7902(3) 0.4597(11) 0.3620(9) 0.092(4) Uani 1 1 d . . .
H11D H 0.8017 0.4417 0.3133 0.138 Uiso 1 1 calc R . .
H11E H 0.7982 0.3996 0.3978 0.138 Uiso 1 1 calc R . .
H11F H 0.7997 0.5364 0.3787 0.138 Uiso 1 1 calc R . .
C12B C 0.7259(5) 0.4901(11) 0.4305(8) 0.104(5) Uani 1 1 d . . .
H12D H 0.6975 0.5061 0.4241 0.156 Uiso 1 1 calc R . .
H12E H 0.7389 0.5591 0.4518 0.156 Uiso 1 1 calc R . .
H12F H 0.7293 0.4232 0.4640 0.156 Uiso 1 1 calc R . .
C13B C 0.7950(2) 0.0271(7) 0.1738(5) 0.0359(19) Uani 1 1 d . . .
C14B C 0.8158(2) 0.2356(7) 0.1781(5) 0.0352(18) Uani 1 1 d . . .
C15B C 0.8495(2) 0.3004(8) 0.1997(5) 0.040(2) Uani 1 1 d . . .
H15B H 0.8707 0.2630 0.2251 0.048 Uiso 1 1 calc R . .
C16B C 0.8516(3) 0.4192(8) 0.1837(5) 0.044(2) Uani 1 1 d . . .
C17B C 0.8202(3) 0.4706(9) 0.1450(6) 0.050(2) Uani 1 1 d . . .
H17B H 0.8212 0.5513 0.1325 0.060 Uiso 1 1 calc R . .
C18B C 0.7875(3) 0.4033(8) 0.1247(5) 0.045(2) Uani 1 1 d . . .
H18B H 0.7662 0.4408 0.0993 0.054 Uiso 1 1 calc R . .
C19B C 0.7843(2) 0.2836(7) 0.1395(4) 0.0364(19) Uani 1 1 d . . .
C20B C 0.8868(3) 0.4908(9) 0.2058(6) 0.057(3) Uani 1 1 d . . .
H20D H 0.8788 0.5728 0.2117 0.086 Uiso 1 1 calc R . .
H20E H 0.9073 0.4852 0.1673 0.086 Uiso 1 1 calc R . .
H20F H 0.8974 0.4614 0.2529 0.086 Uiso 1 1 calc R . .
C21B C 0.8060(2) -0.0983(8) 0.1952(5) 0.039(2) Uani 1 1 d . . .
C22B C 0.8159(3) -0.1038(9) 0.2779(5) 0.049(2) Uani 1 1 d . . .
H22D H 0.7937 -0.0714 0.3066 0.074 Uiso 1 1 calc R . .
H22E H 0.8400 -0.0581 0.2876 0.074 Uiso 1 1 calc R . .
H22F H 0.8203 -0.1855 0.2924 0.074 Uiso 1 1 calc R . .
C23B C 0.8424(3) -0.1343(9) 0.1494(5) 0.053(2) Uani 1 1 d . . .
H23D H 0.8641 -0.0788 0.1585 0.079 Uiso 1 1 calc R . .
H23E H 0.8355 -0.1338 0.0966 0.079 Uiso 1 1 calc R . .
H23F H 0.8508 -0.2131 0.1640 0.079 Uiso 1 1 calc R . .
C24B C 0.7713(2) -0.1807(8) 0.1790(6) 0.049(2) Uani 1 1 d . . .
H24D H 0.7471 -0.1499 0.2023 0.073 Uiso 1 1 calc R . .
H24E H 0.7771 -0.2585 0.1992 0.073 Uiso 1 1 calc R . .
H24F H 0.7673 -0.1864 0.1252 0.073 Uiso 1 1 calc R . .
C25B C 0.6770(2) 0.3700(8) 0.0980(5) 0.044(2) Uani 1 1 d . . .
C26B C 0.6575(3) 0.4785(9) 0.0654(6) 0.051(2) Uani 1 1 d . . .
C27B C 0.6617(2) 0.0519(8) 0.1044(5) 0.043(2) Uani 1 1 d . . .
C28B C 0.6323(3) -0.0327(10) 0.0667(6) 0.054(3) Uani 1 1 d . . .
C1S C 0.3676(4) -0.0458(13) -0.0415(6) 0.091(4) Uani 1 1 d . . .
H1SA H 0.3736 -0.0674 -0.0936 0.109 Uiso 1 1 calc R . .
H1SB H 0.3472 0.0168 -0.0425 0.109 Uiso 1 1 calc R . .
Cl1 Cl 0.34767(9) -0.1693(4) 0.0046(2) 0.0961(12) Uani 1 1 d . . .
Cl2 Cl 0.40959(9) 0.0076(3) -0.0013(2) 0.0866(10) Uani 1 1 d . . .
C2S C 0.3939(3) 0.3188(11) 0.0050(7) 0.074(3) Uani 1 1 d . . .
H2SA H 0.4162 0.2739 -0.0166 0.089 Uiso 1 1 calc R . .
H2SB H 0.3929 0.3017 0.0588 0.089 Uiso 1 1 calc R . .
Cl3 Cl 0.34947(10) 0.2739(3) -0.0363(2) 0.0911(10) Uani 1 1 d . . .
Cl4 Cl 0.40220(11) 0.4688(3) -0.00833(19) 0.0880(10) 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
Pd1A 0.0342(3) 0.0369(3) 0.0302(3) -0.0016(3) 0.0003(3) 0.0007(3)
Pd2A 0.0322(3) 0.0391(3) 0.0331(3) 0.0001(3) -0.0011(3) -0.0010(3)
F1A 0.078(4) 0.043(3) 0.060(4) -0.005(3) 0.010(3) -0.007(3)
F2A 0.042(3) 0.079(4) 0.066(4) 0.010(3) 0.000(3) -0.011(3)
F3A 0.063(3) 0.067(4) 0.044(3) 0.005(3) 0.007(3) -0.011(3)
F4A 0.114(6) 0.139(7) 0.126(7) -0.083(6) -0.052(5) 0.084(5)
F5A 0.160(7) 0.095(6) 0.053(4) 0.007(4) 0.041(4) 0.069(5)
F6A 0.127(6) 0.056(5) 0.184(9) -0.038(5) 0.054(6) -0.018(4)
O1A 0.040(3) 0.037(4) 0.039(3) 0.003(3) 0.006(3) 0.000(3)
O2A 0.037(3) 0.038(3) 0.046(4) -0.006(3) 0.003(3) -0.002(3)
O3A 0.038(3) 0.036(4) 0.041(3) 0.004(3) 0.001(3) -0.003(3)
O4A 0.037(3) 0.041(4) 0.042(4) 0.004(3) 0.002(2) -0.002(3)
O5A 0.050(3) 0.047(4) 0.033(3) -0.001(3) 0.001(3) 0.002(3)
O6A 0.039(3) 0.053(4) 0.032(3) -0.004(3) 0.004(3) 0.004(3)
N1A 0.045(4) 0.028(4) 0.040(4) -0.008(3) 0.008(4) -0.001(3)
N2A 0.044(4) 0.040(4) 0.035(4) 0.004(3) 0.003(3) -0.008(3)
C1A 0.032(4) 0.038(5) 0.034(5) 0.004(4) -0.002(3) 0.002(4)
C2A 0.038(4) 0.035(5) 0.036(5) 0.005(4) -0.004(4) 0.002(4)
C3A 0.047(5) 0.048(6) 0.035(5) -0.007(4) 0.007(4) -0.001(4)
C4A 0.044(5) 0.042(6) 0.032(5) 0.002(4) 0.009(4) -0.002(4)
C5A 0.049(5) 0.035(5) 0.049(5) 0.005(4) -0.002(4) -0.005(4)
C6A 0.039(4) 0.043(6) 0.037(5) -0.001(4) 0.006(4) 0.002(4)
C7A 0.040(4) 0.031(5) 0.035(5) -0.006(4) -0.009(4) 0.004(4)
C8A 0.081(7) 0.048(6) 0.041(5) 0.001(5) 0.007(5) -0.004(5)
C9A 0.052(5) 0.030(5) 0.032(4) -0.001(4) 0.006(4) 0.002(4)
C10A 0.080(7) 0.042(6) 0.051(6) -0.007(5) 0.009(5) 0.008(5)
C11A 0.080(8) 0.053(7) 0.121(12) 0.006(7) 0.050(8) 0.012(6)
C12A 0.124(10) 0.041(7) 0.092(9) -0.027(6) -0.056(8) 0.021(7)
C13A 0.044(5) 0.031(5) 0.039(5) -0.004(4) -0.007(4) 0.002(4)
C14A 0.045(4) 0.028(5) 0.035(5) -0.003(4) -0.010(4) 0.008(4)
C15A 0.036(4) 0.048(6) 0.052(5) -0.003(5) 0.000(4) 0.000(4)
C16A 0.042(5) 0.047(6) 0.049(6) -0.012(5) -0.007(4) 0.004(4)
C17A 0.059(6) 0.034(5) 0.044(5) 0.001(4) -0.002(4) 0.000(4)
C18A 0.045(5) 0.046(5) 0.037(5) -0.003(4) -0.001(4) 0.004(4)
C19A 0.036(4) 0.035(5) 0.035(5) -0.001(4) -0.006(3) -0.001(4)
C20A 0.056(6) 0.058(7) 0.086(8) -0.006(6) 0.002(6) 0.017(5)
C21A 0.041(5) 0.036(5) 0.053(6) -0.003(4) -0.006(4) -0.009(4)
C22A 0.059(5) 0.049(6) 0.057(7) 0.018(5) -0.006(5) -0.009(5)
C23A 0.052(5) 0.041(6) 0.077(7) 0.007(5) -0.018(5) -0.009(5)
C24A 0.064(6) 0.042(6) 0.068(7) -0.006(5) -0.006(5) -0.006(5)
C25A 0.035(4) 0.039(5) 0.033(5) -0.005(4) -0.001(4) -0.001(3)
C26A 0.043(5) 0.046(6) 0.040(5) 0.004(4) -0.005(4) -0.005(4)
C27A 0.038(4) 0.044(5) 0.040(5) -0.004(5) 0.007(4) -0.003(4)
C28A 0.045(5) 0.061(7) 0.039(6) 0.003(5) -0.004(4) -0.001(5)
Pd1B 0.0352(3) 0.0491(4) 0.0320(3) 0.0025(3) -0.0008(3) -0.0021(3)
Pd2B 0.0339(3) 0.0412(4) 0.0343(3) 0.0019(3) -0.0011(3) -0.0007(3)
F1B 0.129(7) 0.044(5) 0.276(13) 0.037(6) -0.091(8) -0.011(5)
F2B 0.144(7) 0.146(8) 0.112(7) 0.068(6) 0.056(6) 0.101(6)
F3B 0.152(7) 0.075(5) 0.059(4) 0.003(4) -0.026(4) 0.045(5)
F4B 0.051(3) 0.091(5) 0.074(4) 0.001(4) -0.019(3) -0.011(3)
F5B 0.069(4) 0.080(5) 0.057(4) -0.003(3) -0.012(3) -0.024(3)
F6B 0.099(4) 0.050(4) 0.066(4) -0.001(3) -0.007(4) -0.015(3)
O1B 0.050(3) 0.049(4) 0.039(4) 0.004(3) -0.004(3) 0.004(3)
O2B 0.032(3) 0.044(4) 0.042(3) 0.001(3) -0.006(2) -0.006(2)
O3B 0.040(3) 0.056(4) 0.044(4) 0.007(3) -0.001(3) 0.012(3)
O4B 0.043(3) 0.044(4) 0.047(4) 0.008(3) 0.004(3) -0.001(3)
O5B 0.042(3) 0.060(4) 0.034(3) -0.001(3) -0.006(3) -0.012(3)
O6B 0.038(3) 0.053(4) 0.038(3) -0.002(3) -0.004(3) -0.004(3)
N1B 0.049(4) 0.039(4) 0.047(5) 0.011(4) -0.019(4) 0.000(3)
N2B 0.042(4) 0.033(4) 0.043(4) -0.007(3) -0.004(3) 0.003(3)
C1B 0.046(5) 0.045(6) 0.029(5) -0.002(4) 0.004(4) -0.003(4)
C2B 0.048(5) 0.040(5) 0.041(6) 0.012(4) 0.008(4) 0.003(4)
C3B 0.056(5) 0.058(7) 0.029(5) -0.001(4) -0.005(4) 0.001(5)
C4B 0.051(5) 0.044(6) 0.038(5) 0.005(4) 0.002(4) -0.003(4)
C5B 0.051(5) 0.033(5) 0.051(6) 0.005(4) 0.009(4) -0.007(4)
C6B 0.040(4) 0.052(6) 0.030(5) 0.002(4) 0.006(4) -0.003(4)
C7B 0.037(4) 0.043(6) 0.039(5) -0.001(4) 0.007(4) -0.006(4)
C8B 0.078(7) 0.042(6) 0.047(6) 0.009(4) -0.009(5) 0.009(5)
C9B 0.054(5) 0.040(5) 0.047(6) 0.000(4) 0.004(4) 0.005(4)
C10B 0.097(9) 0.037(6) 0.079(8) 0.000(6) -0.020(6) -0.006(6)
C11B 0.066(7) 0.064(8) 0.146(14) -0.013(9) -0.020(8) -0.002(6)
C12B 0.181(15) 0.051(8) 0.080(10) -0.020(7) 0.040(10) -0.005(9)
C13B 0.032(4) 0.040(5) 0.036(5) 0.003(4) 0.009(4) -0.001(4)
C14B 0.035(4) 0.029(5) 0.042(5) 0.004(4) 0.000(4) 0.000(3)
C15B 0.036(4) 0.049(6) 0.036(5) -0.002(4) -0.002(4) -0.008(4)
C16B 0.048(5) 0.038(5) 0.047(5) -0.001(4) -0.001(4) -0.012(4)
C17B 0.049(5) 0.039(6) 0.061(7) 0.006(5) -0.001(5) -0.009(4)
C18B 0.045(5) 0.047(6) 0.042(5) 0.010(4) -0.004(4) 0.001(4)
C19B 0.040(4) 0.035(5) 0.034(4) -0.006(4) 0.004(4) 0.000(4)
C20B 0.053(5) 0.049(6) 0.070(7) 0.004(5) -0.004(5) -0.013(5)
C21B 0.031(4) 0.033(5) 0.054(6) 0.005(4) 0.001(4) 0.001(4)
C22B 0.045(5) 0.058(7) 0.045(6) 0.014(5) -0.002(4) -0.004(5)
C23B 0.060(6) 0.047(6) 0.052(6) -0.004(5) 0.007(5) 0.004(5)
C24B 0.045(5) 0.042(6) 0.060(6) 0.000(5) -0.003(4) 0.000(4)
C25B 0.039(4) 0.061(6) 0.032(5) 0.005(4) -0.011(4) -0.003(4)
C26B 0.055(6) 0.039(6) 0.058(7) 0.004(5) -0.004(5) 0.010(5)
C27B 0.036(4) 0.047(6) 0.047(6) -0.003(5) -0.013(4) -0.004(4)
C28B 0.047(5) 0.062(7) 0.054(7) 0.003(5) -0.007(5) -0.012(5)
C1S 0.113(10) 0.118(12) 0.041(6) 0.010(7) -0.008(7) 0.029(9)
Cl1 0.0709(18) 0.147(4) 0.071(2) 0.022(2) 0.0130(16) 0.001(2)
Cl2 0.0629(17) 0.099(3) 0.098(3) 0.026(2) 0.0079(17) 0.0159(16)
C2S 0.071(7) 0.088(10) 0.062(7) 0.015(7) -0.011(6) -0.019(7)
Cl3 0.083(2) 0.104(3) 0.086(2) 0.012(2) -0.0220(18) -0.0161(19)
Cl4 0.107(2) 0.073(2) 0.084(2) 0.0098(18) -0.0053(19) -0.0095(18)
_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
Pd1A C7A 1.947(9) . ?
Pd1A O1A 1.997(6) . ?
Pd1A O5A 2.081(6) . ?
Pd1A O3A 2.201(5) . ?
Pd1A Pd2A 2.9515(9) . ?
Pd2A C19A 1.942(8) . ?
Pd2A O2A 1.991(5) . ?
Pd2A O4A 2.058(6) . ?
Pd2A O6A 2.157(6) . ?
F1A C26A 1.317(10) . ?
F2A C26A 1.329(9) . ?
F3A C26A 1.362(10) . ?
F4A C28A 1.274(11) . ?
F5A C28A 1.284(11) . ?
F6A C28A 1.301(11) . ?
O1A C1A 1.271(9) . ?
O2A C13A 1.256(10) . ?
O3A C25A 1.250(10) . ?
O4A C25A 1.249(9) . ?
O5A C27A 1.250(10) . ?
O6A C27A 1.233(10) . ?
N1A C1A 1.312(10) . ?
N1A C2A 1.405(10) . ?
N2A C13A 1.333(10) . ?
N2A C14A 1.414(10) . ?
C1A C9A 1.525(11) . ?
C2A C3A 1.410(12) . ?
C2A C7A 1.412(11) . ?
C3A C4A 1.376(12) . ?
C4A C5A 1.381(12) . ?
C4A C8A 1.518(12) . ?
C5A C6A 1.402(12) . ?
C6A C7A 1.390(12) . ?
C9A C12A 1.509(13) . ?
C9A C10A 1.516(13) . ?
C9A C11A 1.551(13) . ?
C13A C21A 1.516(12) . ?
C14A C19A 1.379(11) . ?
C14A C15A 1.401(11) . ?
C15A C16A 1.379(13) . ?
C16A C17A 1.402(13) . ?
C16A C20A 1.534(12) . ?
C17A C18A 1.394(12) . ?
C18A C19A 1.385(11) . ?
C21A C24A 1.517(12) . ?
C21A C23A 1.533(12) . ?
C21A C22A 1.536(13) . ?
C25A C26A 1.538(11) . ?
C27A C28A 1.545(13) . ?
Pd1B C7B 1.952(9) . ?
Pd1B O1B 1.976(6) . ?
Pd1B O5B 2.074(6) . ?
Pd1B O3B 2.174(6) . ?
Pd1B Pd2B 2.9233(9) . ?
Pd2B C19B 1.941(8) . ?
Pd2B O2B 1.992(6) . ?
Pd2B O4B 2.053(6) . ?
Pd2B O6B 2.178(6) . ?
F1B C26B 1.300(12) . ?
F2B C26B 1.283(11) . ?
F3B C26B 1.297(12) . ?
F4B C28B 1.332(11) . ?
F5B C28B 1.341(12) . ?
F6B C28B 1.321(11) . ?
O1B C1B 1.259(10) . ?
O2B C13B 1.266(9) . ?
O3B C25B 1.254(10) . ?
O4B C25B 1.226(10) . ?
O5B C27B 1.254(11) . ?
O6B C27B 1.227(10) . ?
N1B C1B 1.329(11) . ?
N1B C2B 1.388(11) . ?
N2B C13B 1.309(10) . ?
N2B C14B 1.430(10) . ?
C1B C9B 1.504(12) . ?
C2B C3B 1.401(12) . ?
C2B C7B 1.403(12) . ?
C3B C4B 1.357(12) . ?
C4B C5B 1.383(12) . ?
C4B C8B 1.528(12) . ?
C5B C6B 1.409(12) . ?
C6B C7B 1.391(12) . ?
C9B C12B 1.515(15) . ?
C9B C10B 1.522(14) . ?
C9B C11B 1.548(14) . ?
C13B C21B 1.529(11) . ?
C14B C19B 1.381(11) . ?
C14B C15B 1.407(11) . ?
C15B C16B 1.389(12) . ?
C16B C17B 1.394(13) . ?
C16B C20B 1.492(12) . ?
C17B C18B 1.390(12) . ?
C18B C19B 1.397(12) . ?
C21B C24B 1.527(12) . ?
C21B C22B 1.527(12) . ?
C21B C23B 1.531(12) . ?
C25B C26B 1.519(13) . ?
C27B C28B 1.538(12) . ?
C1S Cl2 1.701(14) . ?
C1S Cl1 1.768(14) . ?
C2S Cl3 1.745(11) . ?
C2S Cl4 1.752(12) . ?
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
C7A Pd1A O1A 91.6(3) . . ?
C7A Pd1A O5A 91.9(3) . . ?
O1A Pd1A O5A 175.9(2) . . ?
C7A Pd1A O3A 173.6(3) . . ?
O1A Pd1A O3A 86.3(2) . . ?
O5A Pd1A O3A 90.0(2) . . ?
C7A Pd1A Pd2A 110.1(2) . . ?
O1A Pd1A Pd2A 100.37(16) . . ?
O5A Pd1A Pd2A 80.49(16) . . ?
O3A Pd1A Pd2A 76.19(15) . . ?
C19A Pd2A O2A 90.9(3) . . ?
C19A Pd2A O4A 94.9(3) . . ?
O2A Pd2A O4A 173.7(2) . . ?
C19A Pd2A O6A 176.8(3) . . ?
O2A Pd2A O6A 86.0(2) . . ?
O4A Pd2A O6A 88.1(2) . . ?
C19A Pd2A Pd1A 102.8(2) . . ?
O2A Pd2A Pd1A 96.98(16) . . ?
O4A Pd2A Pd1A 84.04(15) . . ?
O6A Pd2A Pd1A 78.50(15) . . ?
C1A O1A Pd1A 128.4(5) . . ?
C13A O2A Pd2A 125.7(5) . . ?
C25A O3A Pd1A 124.7(5) . . ?
C25A O4A Pd2A 120.9(5) . . ?
C27A O5A Pd1A 122.9(6) . . ?
C27A O6A Pd2A 121.0(5) . . ?
C1A N1A C2A 129.7(7) . . ?
C13A N2A C14A 127.0(7) . . ?
O1A C1A N1A 121.4(8) . . ?
O1A C1A C9A 117.0(7) . . ?
N1A C1A C9A 121.5(7) . . ?
N1A C2A C3A 116.4(8) . . ?
N1A C2A C7A 123.5(7) . . ?
C3A C2A C7A 120.1(8) . . ?
C4A C3A C2A 122.3(8) . . ?
C3A C4A C5A 117.6(8) . . ?
C3A C4A C8A 123.0(8) . . ?
C5A C4A C8A 119.3(8) . . ?
C4A C5A C6A 121.2(8) . . ?
C7A C6A C5A 122.0(8) . . ?
C6A C7A C2A 116.8(8) . . ?
C6A C7A Pd1A 121.5(6) . . ?
C2A C7A Pd1A 121.7(6) . . ?
C12A C9A C10A 112.4(9) . . ?
C12A C9A C1A 107.6(7) . . ?
C10A C9A C1A 108.1(7) . . ?
C12A C9A C11A 109.8(10) . . ?
C10A C9A C11A 108.3(8) . . ?
C1A C9A C11A 110.7(8) . . ?
O2A C13A N2A 123.1(8) . . ?
O2A C13A C21A 117.8(8) . . ?
N2A C13A C21A 119.0(8) . . ?
C19A C14A C15A 121.2(8) . . ?
C19A C14A N2A 123.3(7) . . ?
C15A C14A N2A 115.5(8) . . ?
C16A C15A C14A 121.6(8) . . ?
C15A C16A C17A 117.8(8) . . ?
C15A C16A C20A 121.3(9) . . ?
C17A C16A C20A 120.9(9) . . ?
C18A C17A C16A 119.7(9) . . ?
C19A C18A C17A 122.6(8) . . ?
C14A C19A C18A 117.1(8) . . ?
C14A C19A Pd2A 121.9(6) . . ?
C18A C19A Pd2A 121.0(6) . . ?
C13A C21A C24A 109.0(7) . . ?
C13A C21A C23A 108.1(7) . . ?
C24A C21A C23A 109.3(8) . . ?
C13A C21A C22A 111.0(8) . . ?
C24A C21A C22A 109.7(8) . . ?
C23A C21A C22A 109.7(8) . . ?
O4A C25A O3A 130.1(8) . . ?
O4A C25A C26A 114.5(7) . . ?
O3A C25A C26A 115.3(7) . . ?
F1A C26A F2A 109.1(7) . . ?
F1A C26A F3A 107.4(7) . . ?
F2A C26A F3A 106.5(7) . . ?
F1A C26A C25A 110.2(7) . . ?
F2A C26A C25A 112.5(7) . . ?
F3A C26A C25A 111.0(7) . . ?
O6A C27A O5A 130.8(8) . . ?
O6A C27A C28A 116.0(8) . . ?
O5A C27A C28A 113.2(8) . . ?
F4A C28A F5A 108.0(9) . . ?
F4A C28A F6A 105.4(10) . . ?
F5A C28A F6A 106.1(9) . . ?
F4A C28A C27A 114.2(8) . . ?
F5A C28A C27A 113.1(8) . . ?
F6A C28A C27A 109.5(8) . . ?
C7B Pd1B O1B 92.4(3) . . ?
C7B Pd1B O5B 94.4(3) . . ?
O1B Pd1B O5B 172.3(2) . . ?
C7B Pd1B O3B 176.8(3) . . ?
O1B Pd1B O3B 84.4(2) . . ?
O5B Pd1B O3B 88.7(2) . . ?
C7B Pd1B Pd2B 104.7(2) . . ?
O1B Pd1B Pd2B 97.01(17) . . ?
O5B Pd1B Pd2B 84.67(16) . . ?
O3B Pd1B Pd2B 76.47(15) . . ?
C19B Pd2B O2B 91.4(3) . . ?
C19B Pd2B O4B 93.8(3) . . ?
O2B Pd2B O4B 173.9(2) . . ?
C19B Pd2B O6B 177.7(3) . . ?
O2B Pd2B O6B 87.0(2) . . ?
O4B Pd2B O6B 87.6(2) . . ?
C19B Pd2B Pd1B 105.3(2) . . ?
O2B Pd2B Pd1B 97.05(16) . . ?
O4B Pd2B Pd1B 84.55(17) . . ?
O6B Pd2B Pd1B 76.51(16) . . ?
C1B O1B Pd1B 129.1(6) . . ?
C13B O2B Pd2B 128.9(6) . . ?
C25B O3B Pd1B 124.7(5) . . ?
C25B O4B Pd2B 121.4(6) . . ?
C27B O5B Pd1B 119.3(5) . . ?
C27B O6B Pd2B 125.4(6) . . ?
C1B N1B C2B 130.5(8) . . ?
C13B N2B C14B 130.1(7) . . ?
O1B C1B N1B 121.9(8) . . ?
O1B C1B C9B 118.0(8) . . ?
N1B C1B C9B 120.1(8) . . ?
N1B C2B C3B 116.4(8) . . ?
N1B C2B C7B 123.1(8) . . ?
C3B C2B C7B 120.5(9) . . ?
C4B C3B C2B 123.0(9) . . ?
C3B C4B C5B 117.6(8) . . ?
C3B C4B C8B 121.6(8) . . ?
C5B C4B C8B 120.8(9) . . ?
C4B C5B C6B 120.5(8) . . ?
C7B C6B C5B 122.2(8) . . ?
C6B C7B C2B 116.1(8) . . ?
C6B C7B Pd1B 121.7(6) . . ?
C2B C7B Pd1B 122.1(7) . . ?
C1B C9B C12B 107.7(8) . . ?
C1B C9B C10B 110.9(8) . . ?
C12B C9B C10B 109.1(9) . . ?
C1B C9B C11B 109.7(8) . . ?
C12B C9B C11B 110.3(11) . . ?
C10B C9B C11B 109.1(9) . . ?
O2B C13B N2B 121.6(8) . . ?
O2B C13B C21B 118.9(7) . . ?
N2B C13B C21B 119.4(7) . . ?
C19B C14B C15B 123.2(8) . . ?
C19B C14B N2B 121.9(7) . . ?
C15B C14B N2B 114.9(7) . . ?
C16B C15B C14B 119.9(8) . . ?
C15B C16B C17B 118.4(8) . . ?
C15B C16B C20B 121.4(8) . . ?
C17B C16B C20B 120.2(9) . . ?
C18B C17B C16B 119.9(9) . . ?
C17B C18B C19B 123.4(8) . . ?
C14B C19B C18B 115.2(8) . . ?
C14B C19B Pd2B 123.8(6) . . ?
C18B C19B Pd2B 121.0(6) . . ?
C24B C21B C22B 109.1(8) . . ?
C24B C21B C13B 110.0(7) . . ?
C22B C21B C13B 109.7(8) . . ?
C24B C21B C23B 110.1(8) . . ?
C22B C21B C23B 109.8(7) . . ?
C13B C21B C23B 108.0(7) . . ?
O4B C25B O3B 130.4(9) . . ?
O4B C25B C26B 116.1(8) . . ?
O3B C25B C26B 113.4(8) . . ?
F2B C26B F3B 105.9(9) . . ?
F2B C26B F1B 105.2(10) . . ?
F3B C26B F1B 104.6(10) . . ?
F2B C26B C25B 115.7(9) . . ?
F3B C26B C25B 112.5(8) . . ?
F1B C26B C25B 112.1(8) . . ?
O6B C27B O5B 131.4(8) . . ?
O6B C27B C28B 116.8(9) . . ?
O5B C27B C28B 111.9(8) . . ?
F6B C28B F4B 107.2(8) . . ?
F6B C28B F5B 107.4(9) . . ?
F4B C28B F5B 107.8(8) . . ?
F6B C28B C27B 110.2(8) . . ?
F4B C28B C27B 111.9(9) . . ?
F5B C28B C27B 112.1(8) . . ?
Cl2 C1S Cl1 113.6(6) . . ?
Cl3 C2S Cl4 111.4(7) . . ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 27.53
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 1.039
_refine_diff_density_min -0.963
_refine_diff_density_rms 0.121
_vrf_PLAT242_k1031a
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C26B
RESPONSE: C atom of a -CF3 group. As expected the anisotropic
displacement parameters of the F atoms are larger than those of
the other atoms in the molecule. This effect was not considered
severe enough to model the group as disordered.
;
# Attachment '- k1035.txt'
data_k1035
_database_code_depnum_ccdc_archive 'CCDC 770197'
#TrackingRef '- k1035.txt'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C24 H20 F6 N2 O6 Pd2'
_chemical_formula_sum 'C24 H20 F6 N2 O6 Pd2'
_chemical_formula_weight 759.22
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'
F F 0.0171 0.0103 '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'
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 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 27.0838(8)
_cell_length_b 16.8253(6)
_cell_length_c 14.3465(4)
_cell_angle_alpha 90.00
_cell_angle_beta 121.2360(15)
_cell_angle_gamma 90.00
_cell_volume 5589.9(3)
_cell_formula_units_Z 8
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 18556
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description needle
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.804
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2976
_exptl_absorpt_coefficient_mu 1.367
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.791
_exptl_absorpt_correction_T_max 0.899
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_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 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 19237
_diffrn_reflns_av_R_equivalents 0.066
_diffrn_reflns_av_sigmaI/netI 0.075
_diffrn_reflns_limit_h_min -35
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.55
_diffrn_reflns_theta_max 27.49
_reflns_number_total 6374
_reflns_number_gt 4082
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_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^)+(0.0750P)^2^] 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 6374
_refine_ls_number_parameters 374
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0928
_refine_ls_R_factor_gt 0.0501
_refine_ls_wR_factor_ref 0.1374
_refine_ls_wR_factor_gt 0.1200
_refine_ls_goodness_of_fit_ref 0.983
_refine_ls_restrained_S_all 0.985
_refine_ls_shift/su_max 0.000
_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 0.112824(16) 0.37121(2) 0.16774(3) 0.03066(14) Uani 1 1 d . . .
Pd2 Pd 0.138324(17) 0.24042(2) 0.07014(3) 0.03360(14) Uani 1 1 d . . .
F1 F -0.0395(2) 0.1722(4) 0.0668(5) 0.144(3) Uani 1 1 d . . .
F2 F -0.07672(18) 0.2699(4) -0.0388(4) 0.1022(17) Uani 1 1 d . . .
F3 F -0.05404(19) 0.1683(3) -0.0947(4) 0.1014(16) Uani 1 1 d . . .
F4 F 0.1610(3) 0.2117(3) 0.4646(4) 0.065(2) Uani 0.831(12) 1 d PD A 1
F5 F 0.1481(5) 0.1065(4) 0.3743(5) 0.146(5) Uani 0.831(12) 1 d PD A 1
F6 F 0.2270(3) 0.1640(6) 0.4493(4) 0.108(4) Uani 0.831(12) 1 d PD A 1
F4A F 0.1945(17) 0.221(2) 0.483(2) 0.110(14) Uiso 0.169(12) 1 d PD A 2
F5A F 0.1216(7) 0.159(2) 0.389(2) 0.076(10) Uiso 0.169(12) 1 d PD A 2
F6A F 0.2001(10) 0.1142(10) 0.4178(19) 0.041(6) Uiso 0.169(12) 1 d PD A 2
O1 O 0.06448(15) 0.4402(2) 0.0390(3) 0.0388(9) Uani 1 1 d . . .
O2 O 0.22425(15) 0.2475(2) 0.1518(3) 0.0397(9) Uani 1 1 d . . .
O3 O 0.03656(15) 0.2990(2) 0.1097(3) 0.0385(9) Uani 1 1 d . . .
O4 O 0.05024(15) 0.2223(2) -0.0054(3) 0.0399(9) Uani 1 1 d . . .
O5 O 0.15144(15) 0.2979(2) 0.3029(3) 0.0356(8) Uani 1 1 d . . .
O6 O 0.14595(16) 0.1845(2) 0.2139(3) 0.0398(9) Uani 1 1 d . . .
N1 N 0.13558(17) 0.5215(2) 0.0499(3) 0.0321(10) Uani 1 1 d . . .
N2 N 0.23348(17) 0.3461(3) 0.0489(3) 0.0352(10) Uani 1 1 d . . .
C1 C 0.0823(2) 0.4935(3) 0.0025(4) 0.0339(12) Uani 1 1 d . . .
C2 C 0.0420(2) 0.5356(3) -0.1014(4) 0.0411(13) Uani 1 1 d . . .
H2A H 0.0157 0.5712 -0.0922 0.049 Uiso 1 1 calc R . .
H2B H 0.0186 0.4971 -0.1605 0.049 Uiso 1 1 calc R . .
C3 C 0.0814(2) 0.5826(4) -0.1261(4) 0.0455(14) Uani 1 1 d . . .
H3A H 0.0661 0.6369 -0.1508 0.055 Uiso 1 1 calc R . .
H3B H 0.0853 0.5561 -0.1835 0.055 Uiso 1 1 calc R . .
C4 C 0.1401(2) 0.5855(3) -0.0179(4) 0.0392(13) Uani 1 1 d . . .
H4A H 0.1722 0.5746 -0.0301 0.047 Uiso 1 1 calc R . .
H4B H 0.1463 0.6381 0.0176 0.047 Uiso 1 1 calc R . .
C5 C 0.1835(2) 0.5013(3) 0.1546(4) 0.0319(11) Uani 1 1 d . . .
C6 C 0.2338(2) 0.5468(3) 0.1964(4) 0.0416(13) Uani 1 1 d . . .
H6A H 0.2346 0.5904 0.1551 0.050 Uiso 1 1 calc R . .
C7 C 0.2819(2) 0.5302(3) 0.2952(4) 0.0419(13) Uani 1 1 d . . .
H7A H 0.3158 0.5614 0.3215 0.050 Uiso 1 1 calc R . .
C8 C 0.2808(2) 0.4677(3) 0.3565(4) 0.0394(13) Uani 1 1 d . . .
H8A H 0.3139 0.4556 0.4254 0.047 Uiso 1 1 calc R . .
C9 C 0.2308(2) 0.4227(3) 0.3164(4) 0.0349(12) Uani 1 1 d . . .
H9A H 0.2305 0.3798 0.3591 0.042 Uiso 1 1 calc R . .
C10 C 0.1813(2) 0.4378(3) 0.2166(4) 0.0310(11) Uani 1 1 d . . .
C11 C 0.2531(2) 0.2983(3) 0.1356(4) 0.0354(12) Uani 1 1 d . . .
C12 C 0.3157(2) 0.3114(4) 0.2155(5) 0.0483(15) Uani 1 1 d . . .
H12A H 0.3386 0.2643 0.2196 0.058 Uiso 1 1 calc R . .
H12B H 0.3225 0.3226 0.2890 0.058 Uiso 1 1 calc R . .
C13 C 0.3315(2) 0.3833(4) 0.1710(5) 0.0489(15) Uani 1 1 d . . .
H13A H 0.3381 0.4307 0.2170 0.059 Uiso 1 1 calc R . .
H13B H 0.3669 0.3726 0.1691 0.059 Uiso 1 1 calc R . .
C14 C 0.2802(2) 0.3964(4) 0.0565(5) 0.0454(14) Uani 1 1 d . . .
H14A H 0.2686 0.4531 0.0450 0.055 Uiso 1 1 calc R . .
H14B H 0.2897 0.3804 0.0013 0.055 Uiso 1 1 calc R . .
C15 C 0.1766(2) 0.3448(3) -0.0466(4) 0.0349(12) Uani 1 1 d . . .
C16 C 0.1679(2) 0.3922(3) -0.1335(4) 0.0422(13) Uani 1 1 d . . .
H16A H 0.1983 0.4245 -0.1269 0.051 Uiso 1 1 calc R . .
C17 C 0.1144(2) 0.3919(3) -0.2300(4) 0.0426(13) Uani 1 1 d . . .
H17A H 0.1081 0.4252 -0.2888 0.051 Uiso 1 1 calc R . .
C18 C 0.0709(2) 0.3438(3) -0.2406(4) 0.0392(13) Uani 1 1 d . . .
H18A H 0.0347 0.3427 -0.3072 0.047 Uiso 1 1 calc R . .
C19 C 0.0800(2) 0.2967(3) -0.1535(4) 0.0360(12) Uani 1 1 d . . .
H19A H 0.0499 0.2630 -0.1616 0.043 Uiso 1 1 calc R . .
C20 C 0.1323(2) 0.2978(3) -0.0548(4) 0.0331(12) Uani 1 1 d . . .
C21 C 0.0229(2) 0.2483(3) 0.0367(5) 0.0400(13) Uani 1 1 d . . .
C22 C -0.0371(3) 0.2136(5) -0.0076(6) 0.0592(18) Uani 1 1 d . . .
C23 C 0.1539(2) 0.2244(3) 0.2923(4) 0.0350(12) Uani 1 1 d . A .
C24 C 0.1705(2) 0.1773(3) 0.3953(4) 0.0443(14) Uani 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 0.0327(2) 0.0270(2) 0.0353(2) 0.00413(16) 0.0198(2) 0.00235(17)
Pd2 0.0346(3) 0.0324(2) 0.0370(3) 0.00298(18) 0.0208(2) 0.00325(18)
F1 0.102(4) 0.192(6) 0.121(4) 0.036(4) 0.046(4) -0.075(4)
F2 0.046(3) 0.153(5) 0.095(3) -0.028(3) 0.028(3) -0.009(3)
F3 0.066(3) 0.107(4) 0.116(4) -0.043(3) 0.037(3) -0.031(3)
F4 0.098(5) 0.066(3) 0.064(3) 0.029(2) 0.065(3) 0.037(3)
F5 0.286(12) 0.061(5) 0.067(4) 0.004(3) 0.075(6) -0.073(6)
F6 0.098(5) 0.171(8) 0.058(4) 0.047(4) 0.042(4) 0.071(6)
O1 0.037(2) 0.036(2) 0.043(2) 0.0105(17) 0.0203(18) 0.0020(17)
O2 0.033(2) 0.046(2) 0.039(2) 0.0075(17) 0.0175(19) 0.0110(18)
O3 0.035(2) 0.036(2) 0.051(2) 0.0071(19) 0.027(2) 0.0046(17)
O4 0.036(2) 0.045(2) 0.039(2) -0.0051(18) 0.0196(19) -0.0097(18)
O5 0.040(2) 0.034(2) 0.0347(19) 0.0074(16) 0.0208(18) 0.0026(17)
O6 0.053(2) 0.033(2) 0.043(2) 0.0102(18) 0.032(2) 0.0102(18)
N1 0.035(2) 0.032(2) 0.037(2) 0.0008(19) 0.024(2) 0.002(2)
N2 0.029(2) 0.043(3) 0.036(2) -0.002(2) 0.018(2) 0.006(2)
C1 0.044(3) 0.029(3) 0.033(3) 0.001(2) 0.024(3) 0.005(2)
C2 0.040(3) 0.047(3) 0.036(3) 0.010(3) 0.019(3) 0.009(3)
C3 0.054(4) 0.046(4) 0.039(3) 0.011(3) 0.026(3) 0.005(3)
C4 0.042(3) 0.039(3) 0.043(3) 0.011(3) 0.026(3) 0.000(3)
C5 0.031(3) 0.032(3) 0.035(3) 0.005(2) 0.019(2) 0.004(2)
C6 0.044(3) 0.040(3) 0.045(3) 0.010(3) 0.026(3) 0.001(3)
C7 0.041(3) 0.041(3) 0.048(3) -0.002(3) 0.026(3) -0.008(3)
C8 0.035(3) 0.040(3) 0.039(3) -0.002(3) 0.017(3) -0.001(3)
C9 0.043(3) 0.032(3) 0.032(3) 0.002(2) 0.020(3) 0.001(2)
C10 0.040(3) 0.022(3) 0.035(3) 0.000(2) 0.022(3) 0.000(2)
C11 0.029(3) 0.042(3) 0.038(3) -0.007(3) 0.019(3) 0.006(3)
C12 0.037(3) 0.058(4) 0.050(4) -0.004(3) 0.023(3) 0.009(3)
C13 0.032(3) 0.058(4) 0.045(3) -0.005(3) 0.011(3) -0.003(3)
C14 0.036(3) 0.049(4) 0.050(3) -0.011(3) 0.022(3) -0.011(3)
C15 0.031(3) 0.042(3) 0.033(3) 0.002(2) 0.017(2) -0.001(2)
C16 0.041(3) 0.044(3) 0.047(3) -0.004(3) 0.026(3) -0.008(3)
C17 0.042(3) 0.046(3) 0.039(3) 0.006(3) 0.021(3) -0.003(3)
C18 0.035(3) 0.049(3) 0.033(3) -0.002(3) 0.017(3) 0.003(3)
C19 0.038(3) 0.039(3) 0.039(3) -0.001(2) 0.025(3) 0.000(3)
C20 0.032(3) 0.036(3) 0.038(3) -0.011(2) 0.023(3) -0.002(2)
C21 0.031(3) 0.045(4) 0.043(3) 0.011(3) 0.019(3) -0.002(3)
C22 0.042(4) 0.072(5) 0.062(4) 0.001(4) 0.026(4) -0.014(4)
C23 0.033(3) 0.033(3) 0.039(3) 0.007(3) 0.018(3) 0.003(2)
C24 0.046(4) 0.044(4) 0.039(3) 0.011(3) 0.020(3) 0.006(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 C10 1.960(5) . ?
Pd1 O1 1.991(3) . ?
Pd1 O5 2.067(3) . ?
Pd1 O3 2.157(4) . ?
Pd1 Pd2 2.8779(5) . ?
Pd2 C20 1.967(5) . ?
Pd2 O2 1.994(4) . ?
Pd2 O4 2.068(3) . ?
Pd2 O6 2.178(3) . ?
F1 C22 1.304(8) . ?
F2 C22 1.324(8) . ?
F3 C22 1.326(8) . ?
F4 C24 1.286(6) . ?
F5 C24 1.298(6) . ?
F6 C24 1.329(6) . ?
F4A C24 1.306(10) . ?
F5A C24 1.312(10) . ?
F6A C24 1.267(9) . ?
O1 C1 1.254(6) . ?
O2 C11 1.257(6) . ?
O3 C21 1.249(6) . ?
O4 C21 1.252(6) . ?
O5 C23 1.252(6) . ?
O6 C23 1.230(6) . ?
N1 C1 1.323(6) . ?
N1 C5 1.426(6) . ?
N1 C4 1.498(6) . ?
N2 C11 1.338(7) . ?
N2 C15 1.436(6) . ?
N2 C14 1.479(7) . ?
C1 C2 1.492(7) . ?
C2 C3 1.509(7) . ?
C3 C4 1.543(8) . ?
C5 C6 1.398(7) . ?
C5 C10 1.411(7) . ?
C6 C7 1.368(7) . ?
C7 C8 1.381(7) . ?
C8 C9 1.389(7) . ?
C9 C10 1.385(7) . ?
C11 C12 1.491(7) . ?
C12 C13 1.528(8) . ?
C13 C14 1.520(8) . ?
C15 C20 1.391(7) . ?
C15 C16 1.393(7) . ?
C16 C17 1.390(8) . ?
C17 C18 1.373(8) . ?
C18 C19 1.390(7) . ?
C19 C20 1.389(7) . ?
C21 C22 1.522(8) . ?
C23 C24 1.525(7) . ?
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
C10 Pd1 O1 92.49(18) . . ?
C10 Pd1 O5 94.66(17) . . ?
O1 Pd1 O5 170.93(13) . . ?
C10 Pd1 O3 178.51(17) . . ?
O1 Pd1 O3 86.15(14) . . ?
O5 Pd1 O3 86.75(13) . . ?
C10 Pd1 Pd2 100.96(14) . . ?
O1 Pd1 Pd2 101.72(10) . . ?
O5 Pd1 Pd2 82.40(10) . . ?
O3 Pd1 Pd2 78.75(9) . . ?
C20 Pd2 O2 91.51(18) . . ?
C20 Pd2 O4 93.80(18) . . ?
O2 Pd2 O4 174.01(14) . . ?
C20 Pd2 O6 176.19(17) . . ?
O2 Pd2 O6 87.76(14) . . ?
O4 Pd2 O6 87.11(14) . . ?
C20 Pd2 Pd1 98.07(14) . . ?
O2 Pd2 Pd1 99.77(10) . . ?
O4 Pd2 Pd1 82.23(10) . . ?
O6 Pd2 Pd1 78.38(9) . . ?
C1 O1 Pd1 126.4(3) . . ?
C11 O2 Pd2 125.4(3) . . ?
C21 O3 Pd1 121.1(3) . . ?
C21 O4 Pd2 120.4(4) . . ?
C23 O5 Pd1 120.6(3) . . ?
C23 O6 Pd2 121.1(3) . . ?
C1 N1 C5 127.7(4) . . ?
C1 N1 C4 110.9(4) . . ?
C5 N1 C4 121.2(4) . . ?
C11 N2 C15 126.2(4) . . ?
C11 N2 C14 111.4(4) . . ?
C15 N2 C14 122.1(4) . . ?
O1 C1 N1 126.4(5) . . ?
O1 C1 C2 121.1(5) . . ?
N1 C1 C2 112.5(4) . . ?
C1 C2 C3 104.1(4) . . ?
C2 C3 C4 105.4(4) . . ?
N1 C4 C3 104.0(4) . . ?
C6 C5 C10 119.6(5) . . ?
C6 C5 N1 118.3(4) . . ?
C10 C5 N1 122.1(4) . . ?
C7 C6 C5 121.7(5) . . ?
C6 C7 C8 119.4(5) . . ?
C7 C8 C9 119.3(5) . . ?
C10 C9 C8 122.8(5) . . ?
C9 C10 C5 117.1(5) . . ?
C9 C10 Pd1 119.6(4) . . ?
C5 C10 Pd1 123.3(4) . . ?
O2 C11 N2 126.5(5) . . ?
O2 C11 C12 121.8(5) . . ?
N2 C11 C12 111.7(5) . . ?
C11 C12 C13 104.5(5) . . ?
C14 C13 C12 105.6(5) . . ?
N2 C14 C13 105.3(4) . . ?
C20 C15 C16 120.7(5) . . ?
C20 C15 N2 122.8(4) . . ?
C16 C15 N2 116.5(4) . . ?
C17 C16 C15 119.7(5) . . ?
C18 C17 C16 120.2(5) . . ?
C17 C18 C19 119.7(5) . . ?
C20 C19 C18 121.3(5) . . ?
C19 C20 C15 118.2(5) . . ?
C19 C20 Pd2 118.8(4) . . ?
C15 C20 Pd2 122.8(4) . . ?
O3 C21 O4 130.6(5) . . ?
O3 C21 C22 113.6(5) . . ?
O4 C21 C22 115.8(6) . . ?
F1 C22 F2 106.4(6) . . ?
F1 C22 F3 109.0(6) . . ?
F2 C22 F3 105.7(6) . . ?
F1 C22 C21 111.0(6) . . ?
F2 C22 C21 111.7(6) . . ?
F3 C22 C21 112.8(5) . . ?
O6 C23 O5 131.0(5) . . ?
O6 C23 C24 115.2(5) . . ?
O5 C23 C24 113.8(5) . . ?
F6A C24 F4 122.3(11) . . ?
F4 C24 F5 109.7(6) . . ?
F6A C24 F4A 107(2) . . ?
F5 C24 F4A 133.1(18) . . ?
F6A C24 F5A 107.9(16) . . ?
F4A C24 F5A 100(2) . . ?
F4 C24 F6 104.9(5) . . ?
F5 C24 F6 103.8(7) . . ?
F5A C24 F6 144.9(13) . . ?
F6A C24 C23 120.7(10) . . ?
F4 C24 C23 116.0(5) . . ?
F5 C24 C23 112.6(5) . . ?
F4A C24 C23 112.9(18) . . ?
F5A C24 C23 105.8(12) . . ?
F6 C24 C23 108.8(5) . . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 27.49
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 1.555
_refine_diff_density_min -0.939
_refine_diff_density_rms 0.144
_vrf_PLAT601_k1035
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 362.00 A**3
RESPONSE: During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly dichloromethene/hexanes). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
solvent cavity of volume 362 \%A^3^ containing approximately 65
electrons. In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
_vrf_PLAT242_k1035
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C22
RESPONSE: C22 and C24 are the C atoms of the -CF3 groups. As
expected the F atoms have larger anisotropic displacement
parameters than these C atoms. The F atoms of one of the -CF3
groups was modelled as disordered.
;