# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_coden_Cambridge 222
loop_
_publ_author_name
'Ingmar Grenthe'
'Andreas Fischer'
'Zoltan Szabo'
'Valerie Vallet'
_publ_contact_author_name 'Ingmar Grenthe'
_publ_contact_author_email INGMARG@KTH.SE
_publ_section_title
;
Structure and Dynamics of Binary and Ternary Lanthanide(III)
and Actinide(III) - Tris[4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione]
(TTA) - Tributylphosphate (TBP) Complexes. Part 1, The Structure and
Bonding of Y, Eu, Am and Cm Complexes as Studied by Quantum Chemical
Methods and X-Ray crystallography
;
# Submission details
_publ_requested_journal ?????
# Attachment 'Eu.CIF'
data_Eu
_database_code_depnum_ccdc_archive 'CCDC 758487'
#TrackingRef 'Eu.CIF'
_audit_update_record
;
2008-12-11 # Formatted by publCIF
;
_chemical_compound_source 'Local laboratory'
_exptl_crystal_description Block
_exptl_crystal_colour Colourless
_exptl_crystal_F_000 832
_cell_measurement_temperature 173
_refine_ls_hydrogen_treatment noref
_diffrn_measurement_device 'Bruker-Nonius KappaCCD'
_computing_data_collection Collect
_computing_data_reduction EvalCCD
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
loop_
_diffrn_radiation_wavelength
0.71073
_diffrn_radiation_wavelength_id all
_cell_formula_units_Z 2
_exptl_crystal_density_diffrn 1.908
_exptl_crystal_density_method 'not measured'
_exptl_special_details
;
?
;
_chemical_formula_weight 851.518
_diffrn_radiation_type ' MoK\a'
loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
-X,-Y,-Z
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_cell_setting triclinic
_chemical_formula_moiety 'C24 H16 Eu F9 O8 S3'
_chemical_formula_sum 'C24 H16 Eu F9 O8 S3'
_chemical_name_systematic
;
?
;
_cell_length_a 10.311(2)
_cell_length_b 11.835(2)
_cell_length_c 14.257(2)
_cell_angle_alpha 110.729(12)
_cell_angle_beta 103.190(13)
_cell_angle_gamma 103.929(10)
_cell_volume 1482.2(5)
_diffrn_reflns_number 26078
_diffrn_reflns_av_R_equivalents 0.0700
_diffrn_reflns_av_sigmaI/netI 0.0628
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 4.57
_diffrn_reflns_theta_full 27.50
_cell_measurement_reflns_used 53
_cell_measurement_theta_min 3.8
_cell_measurement_theta_max 17.1
_diffrn_measurement_method '\f & \w'
_computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_crystal_size_min 0.30
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_max 0.30
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'
Eu Eu -0.1578 3.6682 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_exptl_absorpt_coefficient_mu 2.430
_reflns_number_total 6748
_reflns_number_gt 5506
_reflns_threshold_expression I>2\s(I)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0537P)^2^+6.7142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6748
_refine_ls_number_parameters 407
_refine_ls_number_restraints 34
_refine_ls_R_factor_all 0.0707
_refine_ls_R_factor_gt 0.0501
_refine_ls_wR_factor_ref 0.1182
_refine_ls_wR_factor_gt 0.1085
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_restrained_S_all 1.077
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean <0.001
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.20890(3) 0.42081(3) 0.89800(2) 0.01956(10) Uani 1 1 d . A .
S1 S 0.0311(2) 0.21417(17) 0.49075(13) 0.0387(4) Uani 1 1 d . . .
S2 S 0.2314(3) 0.34395(19) 1.30876(15) 0.0503(5) Uani 1 1 d . . .
C22a C 0.442(5) 0.279(3) 0.528(4) 0.0366(6) Uani 0.30 1 d PU A 1
S3a S 0.5201(14) 0.2290(14) 0.6914(8) 0.0366(6) Uani 0.30 1 d P A 1
C22b C 0.520(2) 0.227(2) 0.7066(14) 0.0366(6) Uani 0.70 1 d PU A 2
S3b S 0.4602(4) 0.3123(3) 0.5425(4) 0.0366(6) Uani 0.70 1 d P A 2
C1 C -0.1896(8) 0.0958(7) 0.8512(5) 0.0372(15) Uani 1 1 d . . .
C2 C -0.0967(6) 0.1753(6) 0.8107(5) 0.0270(13) Uani 1 1 d . . .
C3 C -0.1071(6) 0.1191(6) 0.7070(5) 0.0270(13) Uani 1 1 d . . .
C4 C -0.0297(6) 0.1873(5) 0.6597(5) 0.0233(12) Uani 1 1 d . . .
C5 C -0.0683(6) 0.1332(6) 0.5447(5) 0.0247(12) Uani 1 1 d . . .
C6 C -0.1803(6) 0.0165(6) 0.4641(4) 0.0237(12) Uani 1 1 d . . .
C7 C -0.1724(8) 0.0050(7) 0.3616(5) 0.0372(16) Uani 1 1 d . . .
C8 C -0.0678(8) 0.1018(7) 0.3658(6) 0.0409(16) Uani 1 1 d . . .
C9 C 0.3202(8) 0.0890(7) 0.9578(6) 0.0376(16) Uani 1 1 d . . .
C10 C 0.2851(6) 0.2112(6) 0.9895(5) 0.0265(13) Uani 1 1 d . . .
C11 C 0.2717(7) 0.2631(6) 1.0871(5) 0.0301(13) Uani 1 1 d . . .
C12 C 0.2378(6) 0.3767(6) 1.1248(4) 0.0245(12) Uani 1 1 d . . .
C13 C 0.2124(6) 0.4192(6) 1.2262(5) 0.0282(13) Uani 1 1 d . . .
C14 C 0.1663(5) 0.5289(5) 1.2689(4) 0.0171(10) Uani 1 1 d . . .
C15 C 0.1522(8) 0.5363(7) 1.3690(5) 0.0398(16) Uani 1 1 d . . .
C16 C 0.1839(9) 0.4470(7) 1.3976(6) 0.049(2) Uani 1 1 d . . .
C17 C 0.2838(9) 0.6858(7) 0.7199(6) 0.0397(17) Uani 1 1 d . . .
C18 C 0.2990(7) 0.5775(6) 0.7514(5) 0.0266(13) Uani 1 1 d . . .
C19 C 0.3629(7) 0.4993(6) 0.6988(5) 0.0285(13) Uani 1 1 d . . .
C20 C 0.3945(6) 0.4033(6) 0.7253(4) 0.0235(12) Uani 1 1 d . A .
C21 C 0.4550(6) 0.3184(6) 0.6606(5) 0.0269(13) Uani 1 1 d . . .
C23 C 0.5584(8) 0.1635(7) 0.6004(6) 0.0432(17) Uani 1 1 d . . .
C24 C 0.5311(8) 0.1995(7) 0.5207(6) 0.0457(19) Uani 1 1 d . A .
F1 F -0.1144(7) 0.1016(8) 0.9412(5) 0.107(3) Uani 1 1 d . . .
F2 F -0.2852(6) 0.1445(5) 0.8759(6) 0.086(2) Uani 1 1 d . . .
F3 F -0.2579(7) -0.0246(4) 0.7836(5) 0.088(2) Uani 1 1 d . . .
F4 F 0.4210(7) 0.0984(6) 0.9141(5) 0.083(2) Uani 1 1 d . . .
F5 F 0.2076(7) -0.0118(4) 0.8845(4) 0.0716(16) Uani 1 1 d . . .
F6 F 0.3630(5) 0.0574(4) 1.0364(3) 0.0471(10) Uani 1 1 d . . .
F7 F 0.2945(16) 0.7814(7) 0.7903(6) 0.194(5) Uani 1 1 d U . .
F8 F 0.3693(12) 0.7183(9) 0.6736(9) 0.148(4) Uani 1 1 d U . .
F9 F 0.1712(10) 0.6491(9) 0.6449(10) 0.184(5) Uani 1 1 d U . .
O1 O -0.0183(4) 0.2895(4) 0.8820(3) 0.0299(9) Uani 1 1 d . . .
O2 O 0.0703(4) 0.2946(4) 0.7146(3) 0.0251(9) Uani 1 1 d . . .
O3 O 0.2264(4) 0.4438(4) 1.0736(3) 0.0263(9) Uani 1 1 d . . .
O4 O 0.2693(5) 0.2506(4) 0.9168(3) 0.0307(10) Uani 1 1 d . . .
O5 O 0.2502(5) 0.5740(4) 0.8237(3) 0.0273(9) Uani 1 1 d . . .
O6 O 0.3764(4) 0.3861(4) 0.8063(3) 0.0254(9) Uani 1 1 d . . .
O7 O 0.0995(5) 0.5797(4) 0.9523(3) 0.0303(9) Uani 1 1 d D . .
O8 O 0.4200(4) 0.6043(4) 1.0252(3) 0.0313(10) Uani 1 1 d D . .
H22 H 0.3920 0.3020 0.4771 0.044 Uiso 0.30 1 calc PR A 1
H22A H 0.5306 0.2150 0.7702 0.044 Uiso 0.70 1 calc PR A 2
H3 H -0.1677 0.0316 0.6640 0.032 Uiso 1 1 calc R . .
H6 H -0.2474 -0.0425 0.4762 0.028 Uiso 1 1 calc R . .
H7 H -0.2361 -0.0655 0.2963 0.045 Uiso 1 1 calc R . .
H8 H -0.0513 0.1062 0.3041 0.049 Uiso 1 1 calc R . .
H11 H 0.2858 0.2211 1.1324 0.036 Uiso 1 1 calc R . .
H14 H 0.1492 0.5843 1.2368 0.021 Uiso 1 1 calc R . .
H15 H 0.1225 0.5999 1.4117 0.048 Uiso 1 1 calc R . .
H16 H 0.1798 0.4426 1.4621 0.058 Uiso 1 1 calc R . .
H19 H 0.3870 0.5108 0.6415 0.034 Uiso 1 1 calc R . .
H23 H 0.5999 0.0994 0.5973 0.052 Uiso 1 1 calc R A 1
H24 H 0.5671 0.1752 0.4639 0.055 Uiso 1 1 calc R B 1
H7A H 0.0721 0.6134 1.0024 0.045 Uiso 1 1 d RD A .
H7B H 0.0976 0.6200 0.9173 0.045 Uiso 1 1 d RD . .
H8A H 0.4523 0.6682 1.0144 0.047 Uiso 1 1 d RD A .
H8B H 0.4745 0.6088 1.0799 0.047 Uiso 1 1 d RD . .
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
Eu1 0.02090(15) 0.02293(16) 0.01687(15) 0.00924(11) 0.00749(11) 0.00921(11)
S1 0.0448(10) 0.0396(9) 0.0288(9) 0.0157(7) 0.0106(7) 0.0104(8)
S2 0.0813(15) 0.0460(11) 0.0347(10) 0.0237(8) 0.0255(10) 0.0263(10)
C22a 0.0411(14) 0.0357(14) 0.0319(17) 0.0089(15) 0.0177(12) 0.0158(12)
S3a 0.0411(14) 0.0357(14) 0.0319(17) 0.0089(15) 0.0177(12) 0.0158(12)
C22b 0.0411(14) 0.0357(14) 0.0319(17) 0.0089(15) 0.0177(12) 0.0158(12)
S3b 0.0411(14) 0.0357(14) 0.0319(17) 0.0089(15) 0.0177(12) 0.0158(12)
C1 0.042(4) 0.036(4) 0.033(4) 0.014(3) 0.019(3) 0.010(3)
C2 0.022(3) 0.029(3) 0.035(3) 0.016(3) 0.012(3) 0.011(2)
C3 0.027(3) 0.024(3) 0.026(3) 0.008(2) 0.009(3) 0.008(2)
C4 0.022(3) 0.026(3) 0.023(3) 0.010(2) 0.007(2) 0.011(2)
C5 0.027(3) 0.030(3) 0.020(3) 0.011(2) 0.009(2) 0.014(2)
C6 0.027(3) 0.027(3) 0.013(3) 0.002(2) 0.005(2) 0.015(2)
C7 0.039(4) 0.039(4) 0.020(3) 0.001(3) 0.003(3) 0.014(3)
C8 0.048(4) 0.050(4) 0.032(4) 0.021(3) 0.017(3) 0.022(4)
C9 0.051(4) 0.039(4) 0.041(4) 0.025(3) 0.023(3) 0.026(3)
C10 0.027(3) 0.025(3) 0.030(3) 0.014(3) 0.010(3) 0.008(2)
C11 0.034(3) 0.028(3) 0.026(3) 0.013(3) 0.006(3) 0.009(3)
C12 0.025(3) 0.027(3) 0.018(3) 0.011(2) 0.004(2) 0.005(2)
C13 0.027(3) 0.029(3) 0.026(3) 0.013(3) 0.007(3) 0.006(2)
C14 0.018(3) 0.020(3) 0.006(2) 0.0019(19) 0.003(2) 0.000(2)
C15 0.046(4) 0.043(4) 0.027(3) 0.010(3) 0.018(3) 0.013(3)
C16 0.071(6) 0.044(4) 0.026(4) 0.016(3) 0.021(4) 0.006(4)
C17 0.066(5) 0.043(4) 0.030(4) 0.024(3) 0.025(4) 0.032(4)
C18 0.033(3) 0.023(3) 0.020(3) 0.009(2) 0.006(3) 0.007(2)
C19 0.037(4) 0.029(3) 0.024(3) 0.013(2) 0.016(3) 0.012(3)
C20 0.019(3) 0.027(3) 0.020(3) 0.008(2) 0.006(2) 0.005(2)
C21 0.022(3) 0.030(3) 0.024(3) 0.006(2) 0.008(2) 0.008(2)
C23 0.036(4) 0.036(4) 0.049(5) 0.010(3) 0.008(3) 0.018(3)
C24 0.044(4) 0.051(4) 0.033(4) 0.004(3) 0.024(3) 0.014(3)
F1 0.072(4) 0.159(7) 0.096(5) 0.104(5) 0.010(3) -0.007(4)
F2 0.078(4) 0.069(4) 0.151(6) 0.057(4) 0.089(4) 0.031(3)
F3 0.136(5) 0.033(3) 0.079(4) 0.011(2) 0.071(4) -0.011(3)
F4 0.129(5) 0.092(4) 0.133(5) 0.088(4) 0.109(5) 0.091(4)
F5 0.110(5) 0.033(2) 0.053(3) 0.007(2) 0.007(3) 0.032(3)
F6 0.067(3) 0.048(2) 0.050(3) 0.034(2) 0.025(2) 0.036(2)
F7 0.494(16) 0.085(5) 0.103(5) 0.071(4) 0.148(8) 0.178(8)
F8 0.223(9) 0.138(6) 0.242(9) 0.164(7) 0.168(8) 0.118(6)
F9 0.120(6) 0.147(7) 0.281(11) 0.170(8) -0.041(7) 0.025(5)
O1 0.029(2) 0.031(2) 0.024(2) 0.0064(18) 0.0117(18) 0.0061(18)
O2 0.024(2) 0.026(2) 0.022(2) 0.0088(17) 0.0067(17) 0.0058(17)
O3 0.034(2) 0.028(2) 0.020(2) 0.0124(17) 0.0092(18) 0.0141(18)
O4 0.043(3) 0.034(2) 0.031(2) 0.0199(19) 0.021(2) 0.022(2)
O5 0.036(2) 0.030(2) 0.027(2) 0.0168(18) 0.0169(19) 0.0175(19)
O6 0.026(2) 0.032(2) 0.022(2) 0.0138(17) 0.0107(17) 0.0134(17)
O7 0.038(3) 0.036(2) 0.031(2) 0.0182(19) 0.020(2) 0.022(2)
O8 0.027(2) 0.036(2) 0.026(2) 0.0165(19) 0.0029(18) 0.0063(19)
_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
Eu1 O4 2.329(4) . ?
Eu1 O2 2.369(4) . ?
Eu1 O3 2.380(4) . ?
Eu1 O1 2.390(4) . ?
Eu1 O5 2.405(4) . ?
Eu1 O7 2.408(4) . ?
Eu1 O6 2.420(4) . ?
Eu1 O8 2.425(4) . ?
S1 C8 1.680(8) . ?
S1 C5 1.723(6) . ?
S2 C16 1.676(8) . ?
S2 C13 1.714(6) . ?
C22a C24 1.46(4) . ?
C22a C21 1.74(6) . ?
S3a C23 1.452(13) . ?
S3a C21 1.517(14) . ?
C22b C23 1.620(18) . ?
C22b C21 1.65(2) . ?
S3b C24 1.641(9) . ?
S3b C21 1.673(8) . ?
C1 F3 1.301(8) . ?
C1 F1 1.307(9) . ?
C1 F2 1.310(9) . ?
C1 C2 1.529(9) . ?
C2 O1 1.281(7) . ?
C2 C3 1.356(9) . ?
C3 C4 1.437(8) . ?
C4 O2 1.259(7) . ?
C4 C5 1.446(8) . ?
C5 C6 1.437(8) . ?
C6 C7 1.442(9) . ?
C7 C8 1.344(10) . ?
C9 F6 1.319(7) . ?
C9 F5 1.327(9) . ?
C9 F4 1.331(8) . ?
C9 C10 1.513(9) . ?
C10 O4 1.274(7) . ?
C10 C11 1.362(9) . ?
C11 C12 1.422(9) . ?
C12 O3 1.261(7) . ?
C12 C13 1.460(8) . ?
C13 C14 1.466(8) . ?
C14 C15 1.442(8) . ?
C15 C16 1.342(11) . ?
C17 F7 1.177(9) . ?
C17 F9 1.241(11) . ?
C17 F8 1.282(10) . ?
C17 C18 1.531(9) . ?
C18 O5 1.255(7) . ?
C18 C19 1.371(9) . ?
C19 C20 1.402(8) . ?
C20 O6 1.286(7) . ?
C20 C21 1.469(8) . ?
C23 C24 1.343(11) . ?
Eu1 H7B 2.8170 . ?
C22a H22 0.9500 . ?
C22b H22A 0.9500 . ?
C3 H3 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C11 H11 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C19 H19 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
O7 H7A 0.8330 . ?
O7 H7B 0.8026 . ?
O8 H8A 0.8308 . ?
O8 H8B 0.8271 . ?
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
O4 Eu1 O2 93.26(15) . . ?
O4 Eu1 O3 72.41(14) . . ?
O2 Eu1 O3 143.86(14) . . ?
O4 Eu1 O1 81.03(16) . . ?
O2 Eu1 O1 70.85(14) . . ?
O3 Eu1 O1 74.16(14) . . ?
O4 Eu1 O5 144.10(14) . . ?
O2 Eu1 O5 77.26(14) . . ?
O3 Eu1 O5 132.87(14) . . ?
O1 Eu1 O5 125.94(15) . . ?
O4 Eu1 O7 148.43(14) . . ?
O2 Eu1 O7 102.67(15) . . ?
O3 Eu1 O7 78.84(14) . . ?
O1 Eu1 O7 78.82(15) . . ?
O5 Eu1 O7 66.94(14) . . ?
O4 Eu1 O6 73.11(14) . . ?
O2 Eu1 O6 74.03(14) . . ?
O3 Eu1 O6 128.85(14) . . ?
O1 Eu1 O6 134.59(14) . . ?
O5 Eu1 O6 70.99(13) . . ?
O7 Eu1 O6 137.35(14) . . ?
O4 Eu1 O8 101.32(16) . . ?
O2 Eu1 O8 145.05(14) . . ?
O3 Eu1 O8 71.09(14) . . ?
O1 Eu1 O8 142.46(14) . . ?
O5 Eu1 O8 72.31(15) . . ?
O7 Eu1 O8 80.96(15) . . ?
O6 Eu1 O8 80.07(15) . . ?
C8 S1 C5 91.9(3) . . ?
C16 S2 C13 92.2(3) . . ?
C24 C22a C21 97(3) . . ?
C23 S3a C21 104.0(6) . . ?
C23 C22b C21 91.5(8) . . ?
C24 S3b C21 93.5(4) . . ?
F3 C1 F1 109.1(7) . . ?
F3 C1 F2 106.8(7) . . ?
F1 C1 F2 103.8(7) . . ?
F3 C1 C2 114.4(6) . . ?
F1 C1 C2 111.0(6) . . ?
F2 C1 C2 111.1(6) . . ?
O1 C2 C3 128.5(6) . . ?
O1 C2 C1 113.7(5) . . ?
C3 C2 C1 117.9(6) . . ?
C2 C3 C4 122.2(5) . . ?
O2 C4 C3 122.5(5) . . ?
O2 C4 C5 118.0(5) . . ?
C3 C4 C5 119.5(5) . . ?
C6 C5 C4 129.4(5) . . ?
C6 C5 S1 112.2(4) . . ?
C4 C5 S1 118.4(4) . . ?
C5 C6 C7 107.7(5) . . ?
C8 C7 C6 114.7(6) . . ?
C7 C8 S1 113.5(5) . . ?
F6 C9 F5 105.9(6) . . ?
F6 C9 F4 107.6(6) . . ?
F5 C9 F4 106.4(6) . . ?
F6 C9 C10 115.1(6) . . ?
F5 C9 C10 110.9(6) . . ?
F4 C9 C10 110.5(5) . . ?
O4 C10 C11 128.5(6) . . ?
O4 C10 C9 112.9(5) . . ?
C11 C10 C9 118.6(5) . . ?
C10 C11 C12 123.4(6) . . ?
O3 C12 C11 122.9(5) . . ?
O3 C12 C13 117.2(5) . . ?
C11 C12 C13 119.9(5) . . ?
C12 C13 C14 124.6(5) . . ?
C12 C13 S2 123.3(5) . . ?
C14 C13 S2 112.1(4) . . ?
C15 C14 C13 106.7(5) . . ?
C16 C15 C14 115.2(6) . . ?
C15 C16 S2 113.8(5) . . ?
F7 C17 F9 109.6(10) . . ?
F7 C17 F8 106.9(9) . . ?
F9 C17 F8 97.3(9) . . ?
F7 C17 C18 115.0(6) . . ?
F9 C17 C18 111.8(7) . . ?
F8 C17 C18 114.7(6) . . ?
O5 C18 C19 129.1(6) . . ?
O5 C18 C17 113.7(5) . . ?
C19 C18 C17 117.2(5) . . ?
C18 C19 C20 123.4(5) . . ?
O6 C20 C19 123.4(5) . . ?
O6 C20 C21 116.8(5) . . ?
C19 C20 C21 119.8(5) . . ?
C20 C21 S3a 125.3(6) . . ?
C20 C21 C22b 118.5(7) . . ?
C20 C21 S3 122.2(5) . . ?
C20 C21 C22a 128.1(16) . . ?
C24 C23 S3a 115.6(7) . . ?
C24 C23 C22b 121.4(9) . . ?
C23 C24 C22 115(2) . . ?
C23 C24 S3b 114.3(6) . . ?
C2 O1 Eu1 128.6(4) . . ?
C4 O2 Eu1 136.1(4) . . ?
C12 O3 Eu1 137.0(4) . . ?
C10 O4 Eu1 134.9(4) . . ?
C18 O5 Eu1 132.9(4) . . ?
C20 O6 Eu1 132.9(4) . . ?
O4 Eu1 H7B 163.6 . . ?
O2 Eu1 H7B 94.1 . . ?
O3 Eu1 H7B 93.2 . . ?
O1 Eu1 H7B 87.5 . . ?
O5 Eu1 H7B 52.2 . . ?
O7 Eu1 H7B 15.2 . . ?
O6 Eu1 H7B 123.1 . . ?
O8 Eu1 H7B 80.7 . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C6 H6 126.2 . . ?
C7 C6 H6 126.2 . . ?
C8 C7 H7 122.6 . . ?
C6 C7 H7 122.6 . . ?
C7 C8 H8 123.2 . . ?
S1 C8 H8 123.2 . . ?
C10 C11 H11 118.3 . . ?
C12 C11 H11 118.3 . . ?
C15 C14 H14 126.6 . . ?
C13 C14 H14 126.6 . . ?
C16 C15 H15 122.4 . . ?
C14 C15 H15 122.4 . . ?
C15 C16 H16 123.1 . . ?
S2 C16 H16 123.1 . . ?
C18 C19 H19 118.3 . . ?
C20 C19 H19 118.3 . . ?
C24 C23 H23 122.2 . . ?
S3a C23 H23 122.2 . . ?
C22b C23 H23 116.4 . . ?
C23 C24 H24 122.5 . . ?
C22a C24 H24 122.5 . . ?
S3b C24 H24 122.0 . . ?
Eu1 O7 H7A 138.7 . . ?
Eu1 O7 H7B 112.7 . . ?
H7A O7 H7B 107.9 . . ?
Eu1 O8 H8A 122.7 . . ?
Eu1 O8 H8B 125.9 . . ?
H8A O8 H8B 110.9 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O1 0.83 1.93 2.759(6) 173 2_567
O8 H8A F4 0.83 2.46 3.199(7) 149 2_667
O8 H8A O4 0.83 2.62 3.006(6) 110 2_667
O8 H8B O6 0.83 1.94 2.754(6) 170 2_667
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max 2.243
_refine_diff_density_min -1.283
_refine_diff_density_rms 0.164
_publ_section_references
;
Mackay, S., Gilmore, C. J., Edwards, C., Stewart, N. & Shankland, K. (1999).
maXus Computer Program for the Solution and Refinement of Crystal
Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University
of Glasgow.
Johnson, C. K. (1976). ORTEPII. A Fortran Thermal-Ellipsoid Plot
Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge,
Tennessee, USA.
Otwinowski, Z. & Minor, W. (1997). In Methods in Enzymology, 276, edited
by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press.
Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C.,
Guagliardi, A., Moliterni, A. G. G. & Spagna, R. (1999). J. Appl.
Cryst. 32, 115--119.
Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal
Structures. University of G\"ottingen, Germany.
;
# Attachment 'yttrium.CIF'
data_Y
_database_code_depnum_ccdc_archive 'CCDC 758488'
#TrackingRef 'yttrium.CIF'
_audit_update_record
;
2008-12-03 # Formatted by publCIF
;
_chemical_compound_source 'Local laboratory'
_exptl_crystal_description plate
_exptl_crystal_colour Colourless
_exptl_crystal_F_000 780
_cell_measurement_temperature 200
_refine_ls_hydrogen_treatment constr
_diffrn_measurement_device 'Bruker-Nonius KappaCCD'
_computing_data_collection Collect
_computing_data_reduction EvalCCD
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
loop_
_diffrn_radiation_wavelength
0.71073
_diffrn_radiation_wavelength_id all
_cell_formula_units_Z 2
_exptl_crystal_density_diffrn 1.768
_exptl_crystal_density_method 'not measured'
_exptl_special_details
;
?
;
_chemical_formula_weight 786.47
_diffrn_radiation_type ' MoK\a'
loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
-X,-Y,-Z
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_cell_setting triclinic
_chemical_formula_moiety 'C24 H14 F9 O8 S3 Y'
_chemical_formula_sum 'C24 H14 F9 O8 S3 Y'
_chemical_name_systematic
;
?
;
_cell_length_a 10.299(3)
_cell_length_b 11.817(3)
_cell_length_c 14.192(3)
_cell_angle_alpha 110.51(2)
_cell_angle_beta 103.10(2)
_cell_angle_gamma 103.75(2)
_cell_volume 1477.3(8)
_diffrn_reflns_number 33483
_diffrn_reflns_av_R_equivalents 0.1237
_diffrn_reflns_av_sigmaI/netI 0.1292
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 4.56
_diffrn_reflns_theta_full 27.50
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 3.9
_cell_measurement_theta_max 18.7
_diffrn_measurement_method '\f & \w'
_computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.650
_exptl_absorpt_correction_T_max 0.913
_exptl_crystal_size_min 0.06
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_max 0.41
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_exptl_absorpt_coefficient_mu 2.289
_reflns_number_total 6763
_reflns_number_gt 3974
_reflns_threshold_expression >2sigma(I)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0511P)^2^+4.1087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6763
_refine_ls_number_parameters 452
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.1450
_refine_ls_R_factor_gt 0.0681
_refine_ls_wR_factor_ref 0.1548
_refine_ls_wR_factor_gt 0.1260
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_restrained_S_all 1.036
_refine_ls_shift/su_max 0.013
_refine_ls_shift/su_mean <0.001
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0616(7) 0.1069(6) -0.1291(5) 0.0428(16) Uani 1 1 d . . .
C2 C -0.1688(8) 0.0093(7) -0.1338(5) 0.0459(17) Uani 1 1 d . . .
C3 C -0.1783(6) 0.0203(5) -0.0313(4) 0.0260(12) Uani 1 1 d . . .
C4 C -0.0632(6) 0.1383(5) 0.0485(4) 0.0286(13) Uani 1 1 d . . .
C5 C -0.0253(6) 0.1918(5) 0.1653(4) 0.0270(12) Uani 1 1 d . . .
C6 C -0.1039(6) 0.1232(5) 0.2114(4) 0.0311(13) Uani 1 1 d . . .
C7 C -0.0907(6) 0.1793(6) 0.3155(4) 0.0304(13) Uani 1 1 d . . .
C8 C -0.1836(7) 0.1004(7) 0.3573(5) 0.0450(16) Uani 1 1 d . . .
C9 C 0.1862(8) 0.4481(7) 0.8972(5) 0.0513(18) Uani 1 1 d . . .
C10 C 0.1553(7) 0.5367(6) 0.8677(5) 0.0463(17) Uani 1 1 d . . .
C11 C 0.1692(5) 0.5280(5) 0.7685(4) 0.0221(11) Uani 1 1 d . . .
C12 C 0.2143(6) 0.4214(5) 0.7256(4) 0.0319(13) Uani 1 1 d . . .
C13 C 0.2383(6) 0.3779(5) 0.6226(4) 0.0278(12) Uani 1 1 d . . .
C14 C 0.2705(6) 0.2647(5) 0.5851(4) 0.0341(14) Uani 1 1 d . . .
C15 C 0.2836(6) 0.2132(6) 0.4867(5) 0.0311(13) Uani 1 1 d . . .
C16 C 0.3185(8) 0.0907(7) 0.4537(5) 0.0453(17) Uani 1 1 d . . .
C18 C 0.5570(7) 0.1627(6) 0.1029(6) 0.0481(18) Uani 1 1 d . . .
C19 C 0.5311(8) 0.2008(7) 0.0244(6) 0.0559(19) Uani 1 1 d . C .
C21 C 0.4534(6) 0.3202(6) 0.1631(4) 0.0323(13) Uani 1 1 d . . .
C22 C 0.3929(6) 0.4035(5) 0.2286(4) 0.0284(12) Uani 1 1 d . C .
C23 C 0.3589(6) 0.4983(5) 0.2001(4) 0.0315(13) Uani 1 1 d . . .
C24 C 0.2940(6) 0.5764(5) 0.2527(4) 0.0301(13) Uani 1 1 d . C .
C25 C 0.2780(9) 0.6854(7) 0.2217(6) 0.0495(18) Uani 1 1 d . . .
F1 F -0.2811(6) 0.1477(5) 0.3799(5) 0.104(2) Uani 1 1 d . . .
F2 F -0.2505(7) -0.0182(4) 0.2914(4) 0.112(2) Uani 1 1 d . . .
F3 F -0.1125(6) 0.1098(7) 0.4478(5) 0.135(3) Uani 1 1 d . . .
F4 F 0.2064(6) -0.0083(4) 0.3808(4) 0.0869(16) Uani 1 1 d . . .
F5 F 0.3597(5) 0.0570(4) 0.5320(3) 0.0574(11) Uani 1 1 d . . .
F6 F 0.4210(6) 0.1000(5) 0.4115(5) 0.099(2) Uani 1 1 d . . .
F7 F 0.1606(17) 0.708(3) 0.230(3) 0.107(8) Uani 0.50 1 d P C .
F8 F 0.265(5) 0.773(2) 0.2885(16) 0.110(8) Uani 0.50 1 d P C .
F9 F 0.374(2) 0.7963(16) 0.295(2) 0.123(10) Uani 0.50 1 d P C .
F10 F 0.3838(19) 0.731(2) 0.193(2) 0.091(6) Uani 0.50 1 d P C .
F11 F 0.290(6) 0.678(3) 0.1342(18) 0.175(16) Uani 0.50 1 d P C .
F12 F 0.1643(15) 0.6321(13) 0.1315(15) 0.077(4) Uani 0.50 1 d P C .
O1 O 0.0741(4) 0.2983(4) 0.2198(3) 0.0309(9) Uani 1 1 d . . .
O2 O -0.0118(4) 0.2934(4) 0.3860(3) 0.0344(9) Uani 1 1 d . . .
O3 O 0.2268(4) 0.4460(4) 0.5722(3) 0.0304(9) Uani 1 1 d . . .
O4 O 0.2701(4) 0.2547(4) 0.4151(3) 0.0347(10) Uani 1 1 d . . .
O5 O 0.3753(4) 0.3870(4) 0.3091(3) 0.0288(9) Uani 1 1 d . . .
O6 O 0.2452(4) 0.5711(4) 0.3247(3) 0.0321(9) Uani 1 1 d . . .
O7 O 0.0970(4) 0.5723(4) 0.4503(3) 0.0345(9) Uani 1 1 d . . .
O8 O 0.4168(4) 0.5990(4) 0.5211(3) 0.0349(9) Uani 1 1 d . . .
S1A S 0.5179(10) 0.2259(9) 0.2024(9) 0.040(2) Uani 0.37 1 d P C 1
C20 C 0.473(5) 0.302(5) 0.064(3) 0.030(9) Uani 0.37 1 d PU C 1
S1B S 0.4574(9) 0.3108(8) 0.0418(5) 0.0394(14) Uani 0.63 1 d P C 2
C17 C 0.511(4) 0.230(3) 0.190(3) 0.085(11) Uani 0.63 1 d P C 2
S2 S 0.0353(2) 0.21809(17) -0.00515(13) 0.0470(4) Uani 1 1 d . . .
S3 S 0.2338(2) 0.34518(18) 0.80780(14) 0.0567(5) Uani 1 1 d . . .
Y1 Y 0.20927(6) 0.42110(5) 0.39858(4) 0.02436(17) Uani 1 1 d . C .
H1 H -0.0442 0.1110 -0.1895 0.051 Uiso 1 1 calc R . .
H2 H -0.2309 -0.0589 -0.1981 0.055 Uiso 1 1 calc R . .
H3 H -0.2443 -0.0362 -0.0186 0.031 Uiso 1 1 calc R . .
H6 H -0.1650 0.0387 0.1690 0.037 Uiso 1 1 calc R . .
H9 H 0.1819 0.4439 0.9606 0.062 Uiso 1 1 calc R . .
H10 H 0.1266 0.5997 0.9092 0.056 Uiso 1 1 calc R . .
H11 H 0.1520 0.5823 0.7368 0.026 Uiso 1 1 calc R . .
H14 H 0.2836 0.2229 0.6293 0.041 Uiso 1 1 calc R . .
H18 H 0.5978 0.0994 0.0976 0.058 Uiso 1 1 calc R A 1
H19 H 0.5466 0.1698 -0.0405 0.067 Uiso 1 1 calc R B 1
H23 H 0.3814 0.5086 0.1430 0.038 Uiso 1 1 calc R C .
H7A H 0.0625 0.5992 0.4015 0.052 Uiso 1 1 d R C .
H7B H 0.0840 0.6151 0.5017 0.052 Uiso 1 1 d R . .
H20 H 0.4503 0.3507 0.0271 0.036 Uiso 0.37 1 calc PR C 1
H17 H 0.5169 0.2165 0.2512 0.102 Uiso 0.63 1 calc PR C 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
C1 0.053(4) 0.053(4) 0.028(3) 0.020(3) 0.014(3) 0.023(4)
C2 0.054(4) 0.043(4) 0.028(3) 0.005(3) 0.004(3) 0.022(4)
C3 0.032(3) 0.031(3) 0.007(2) -0.001(2) 0.001(2) 0.016(3)
C4 0.033(3) 0.034(3) 0.026(3) 0.017(3) 0.010(2) 0.019(3)
C5 0.029(3) 0.031(3) 0.026(3) 0.012(3) 0.010(2) 0.017(3)
C6 0.031(3) 0.028(3) 0.031(3) 0.008(3) 0.011(3) 0.009(3)
C7 0.028(3) 0.037(3) 0.031(3) 0.015(3) 0.012(3) 0.016(3)
C8 0.051(4) 0.045(4) 0.037(4) 0.016(3) 0.021(3) 0.009(4)
C9 0.076(5) 0.055(4) 0.024(3) 0.022(3) 0.023(3) 0.013(4)
C10 0.054(4) 0.047(4) 0.036(4) 0.013(3) 0.020(3) 0.017(4)
C11 0.021(3) 0.028(3) 0.009(2) 0.003(2) 0.004(2) 0.003(2)
C12 0.036(3) 0.034(3) 0.025(3) 0.017(3) 0.008(3) 0.008(3)
C13 0.029(3) 0.030(3) 0.023(3) 0.011(3) 0.010(2) 0.008(3)
C14 0.045(4) 0.033(3) 0.026(3) 0.016(3) 0.010(3) 0.013(3)
C15 0.031(3) 0.036(3) 0.035(3) 0.021(3) 0.014(3) 0.015(3)
C16 0.065(5) 0.051(4) 0.044(4) 0.032(4) 0.031(4) 0.032(4)
C18 0.043(4) 0.034(4) 0.054(4) 0.004(3) 0.012(3) 0.018(3)
C19 0.062(5) 0.061(5) 0.041(4) 0.010(4) 0.030(4) 0.020(4)
C21 0.035(3) 0.041(4) 0.027(3) 0.017(3) 0.013(3) 0.020(3)
C22 0.024(3) 0.035(3) 0.023(3) 0.007(3) 0.010(2) 0.010(3)
C23 0.040(3) 0.040(3) 0.019(3) 0.015(3) 0.014(3) 0.015(3)
C24 0.037(3) 0.035(3) 0.020(3) 0.013(3) 0.011(3) 0.011(3)
C25 0.077(6) 0.053(5) 0.040(4) 0.029(4) 0.031(4) 0.035(5)
F1 0.101(4) 0.089(4) 0.176(6) 0.070(4) 0.109(4) 0.042(3)
F2 0.178(6) 0.042(3) 0.098(4) 0.012(3) 0.096(4) -0.012(3)
F3 0.085(4) 0.213(7) 0.115(5) 0.137(5) 0.008(3) -0.014(4)
F4 0.130(5) 0.044(3) 0.057(3) 0.002(2) 0.004(3) 0.036(3)
F5 0.087(3) 0.057(2) 0.054(2) 0.035(2) 0.029(2) 0.046(2)
F6 0.154(5) 0.108(4) 0.164(5) 0.108(4) 0.135(5) 0.110(4)
F7 0.076(9) 0.119(15) 0.21(2) 0.132(16) 0.061(10) 0.065(9)
F8 0.28(3) 0.061(12) 0.063(10) 0.046(9) 0.101(15) 0.112(17)
F9 0.106(12) 0.051(8) 0.18(2) 0.055(11) -0.010(13) 0.014(9)
F10 0.095(10) 0.100(14) 0.144(17) 0.098(15) 0.074(11) 0.045(8)
F11 0.47(5) 0.125(18) 0.072(12) 0.086(13) 0.16(2) 0.21(3)
F12 0.090(9) 0.095(9) 0.076(10) 0.062(8) 0.019(7) 0.055(8)
O1 0.031(2) 0.036(2) 0.024(2) 0.0124(19) 0.0080(17) 0.011(2)
O2 0.034(2) 0.037(2) 0.026(2) 0.0065(19) 0.0144(18) 0.010(2)
O3 0.040(2) 0.036(2) 0.021(2) 0.0148(18) 0.0117(17) 0.0170(19)
O4 0.054(3) 0.041(2) 0.030(2) 0.0242(19) 0.025(2) 0.028(2)
O5 0.033(2) 0.042(2) 0.023(2) 0.0182(18) 0.0152(17) 0.0206(19)
O6 0.043(2) 0.035(2) 0.028(2) 0.0162(18) 0.0169(18) 0.021(2)
O7 0.047(3) 0.042(2) 0.028(2) 0.0180(19) 0.0202(19) 0.027(2)
O8 0.032(2) 0.044(2) 0.027(2) 0.0139(19) 0.0066(17) 0.014(2)
S1A 0.036(4) 0.033(4) 0.041(4) 0.003(3) 0.010(3) 0.018(4)
C20 0.019(10) 0.050(14) 0.020(14) 0.023(10) -0.004(9) 0.009(9)
S1B 0.054(3) 0.052(2) 0.026(2) 0.019(2) 0.023(2) 0.029(2)
C17 0.11(2) 0.10(2) 0.070(17) 0.046(15) 0.064(17) 0.032(18)
S2 0.0572(11) 0.0501(10) 0.0325(9) 0.0189(8) 0.0145(8) 0.0158(9)
S3 0.0948(15) 0.0556(11) 0.0378(10) 0.0289(9) 0.0314(10) 0.0347(11)
Y1 0.0282(3) 0.0312(3) 0.0190(3) 0.0122(2) 0.0107(2) 0.0144(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.364(9) . ?
C1 S2 1.667(6) . ?
C2 C3 1.443(8) . ?
C3 C4 1.459(8) . ?
C4 C5 1.469(7) . ?
C4 S2 1.701(6) . ?
C5 O1 1.256(6) . ?
C5 C6 1.427(8) . ?
C6 C7 1.350(7) . ?
C7 O2 1.282(7) . ?
C7 C8 1.536(8) . ?
C8 F3 1.278(8) . ?
C8 F2 1.282(8) . ?
C8 F1 1.308(8) . ?
C9 C10 1.333(9) . ?
C9 S3 1.677(7) . ?
C10 C11 1.418(8) . ?
C11 C12 1.429(7) . ?
C12 C13 1.469(7) . ?
C12 S3 1.712(6) . ?
C13 O3 1.258(6) . ?
C13 C14 1.406(8) . ?
C14 C15 1.366(8) . ?
C15 O4 1.269(6) . ?
C15 C16 1.514(8) . ?
C16 F4 1.319(8) . ?
C16 F5 1.322(7) . ?
C16 F6 1.328(8) . ?
C18 C19 1.338(10) . ?
C18 C17 1.46(3) . ?
C18 S1A 1.542(14) . ?
C19 C20 1.46(5) . ?
C19 S1B 1.630(11) . ?
C21 C20 1.42(4) . ?
C21 C17 1.46(3) . ?
C21 C22 1.460(7) . ?
C21 S1A 1.617(12) . ?
C21 S1B 1.697(8) . ?
C22 O5 1.269(6) . ?
C22 C23 1.407(8) . ?
C23 C24 1.377(8) . ?
C24 O6 1.250(6) . ?
C24 C25 1.531(8) . ?
C25 F8 1.196(12) . ?
C25 F11 1.253(15) . ?
C25 F10 1.310(14) . ?
C25 F9 1.320(17) . ?
C25 F7 1.320(15) . ?
C25 F12 1.346(14) . ?
F7 F8 1.09(2) . ?
F7 F12 1.38(2) . ?
F8 F9 1.07(3) . ?
F9 F10 1.42(3) . ?
F10 F11 1.00(4) . ?
F11 F12 1.27(4) . ?
O1 Y1 2.311(4) . ?
O2 Y1 2.343(4) . ?
O3 Y1 2.336(4) . ?
O4 Y1 2.271(4) . ?
O5 Y1 2.378(3) . ?
O6 Y1 2.355(4) . ?
O7 Y1 2.349(4) . ?
O8 Y1 2.373(4) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C23 H23 0.9300 . ?
O7 H7A 0.8966 . ?
O7 H7B 0.7900 . ?
C20 H20 0.9300 . ?
C17 H17 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 S2 113.9(5) . . ?
C1 C2 C3 114.6(6) . . ?
C2 C3 C4 106.0(5) . . ?
C3 C4 C5 127.6(5) . . ?
C3 C4 S2 113.7(4) . . ?
C5 C4 S2 118.8(4) . . ?
O1 C5 C6 123.2(5) . . ?
O1 C5 C4 117.5(5) . . ?
C6 C5 C4 119.2(5) . . ?
C7 C6 C5 121.0(5) . . ?
O2 C7 C6 128.5(5) . . ?
O2 C7 C8 114.0(5) . . ?
C6 C7 C8 117.5(5) . . ?
F3 C8 F2 110.7(7) . . ?
F3 C8 F1 102.3(6) . . ?
F2 C8 F1 105.8(6) . . ?
F3 C8 C7 111.6(6) . . ?
F2 C8 C7 114.4(5) . . ?
F1 C8 C7 111.2(6) . . ?
C10 C9 S3 112.9(5) . . ?
C9 C10 C11 115.2(6) . . ?
C10 C11 C12 108.2(5) . . ?
C11 C12 C13 125.4(5) . . ?
C11 C12 S3 111.7(4) . . ?
C13 C12 S3 122.9(4) . . ?
O3 C13 C14 123.7(5) . . ?
O3 C13 C12 116.5(5) . . ?
C14 C13 C12 119.8(5) . . ?
C15 C14 C13 123.0(5) . . ?
O4 C15 C14 128.4(5) . . ?
O4 C15 C16 112.7(5) . . ?
C14 C15 C16 118.9(5) . . ?
F4 C16 F5 105.5(6) . . ?
F4 C16 F6 107.2(6) . . ?
F5 C16 F6 106.8(6) . . ?
F4 C16 C15 110.8(5) . . ?
F5 C16 C15 114.8(5) . . ?
F6 C16 C15 111.3(5) . . ?
C19 C18 C17 111.6(15) . . ?
C19 C18 S1A 118.6(7) . . ?
C17 C18 S1A 7.1(17) . . ?
C18 C19 C20 104.3(15) . . ?
C18 C19 S1B 116.4(6) . . ?
C20 C19 S1B 12.4(15) . . ?
C20 C21 C17 102(2) . . ?
C20 C21 C22 132.7(19) . . ?
C17 C21 C22 125.0(15) . . ?
C20 C21 S1A 106.7(19) . . ?
C17 C21 S1A 4.6(17) . . ?
C22 C21 S1A 120.6(6) . . ?
C20 C21 S1B 9(2) . . ?
C17 C21 S1B 111.0(14) . . ?
C22 C21 S1B 123.9(5) . . ?
S1A C21 S1B 115.4(6) . . ?
O5 C22 C23 123.6(5) . . ?
O5 C22 C21 117.9(5) . . ?
C23 C22 C21 118.6(5) . . ?
C24 C23 C22 123.1(5) . . ?
O6 C24 C23 128.3(5) . . ?
O6 C24 C25 114.0(5) . . ?
C23 C24 C25 117.7(5) . . ?
F8 C25 F11 127.1(10) . . ?
F8 C25 F10 108.8(15) . . ?
F11 C25 F10 45.8(18) . . ?
F8 C25 F9 49.8(13) . . ?
F11 C25 F9 105.9(19) . . ?
F10 C25 F9 65.6(13) . . ?
F8 C25 F7 51.1(13) . . ?
F11 C25 F7 110.5(18) . . ?
F10 C25 F7 136.7(10) . . ?
F9 C25 F7 99.9(12) . . ?
F8 C25 F12 110.1(17) . . ?
F11 C25 F12 58(2) . . ?
F10 C25 F12 103.9(11) . . ?
F9 C25 F12 143.3(10) . . ?
F7 C25 F12 62.5(11) . . ?
F8 C25 C24 115.2(7) . . ?
F11 C25 C24 117.4(8) . . ?
F10 C25 C24 111.5(9) . . ?
F9 C25 C24 109.8(9) . . ?
F7 C25 C24 111.7(8) . . ?
F12 C25 C24 106.7(8) . . ?
F8 F7 C25 58.6(11) . . ?
F8 F7 F12 114.2(19) . . ?
C25 F7 F12 59.6(11) . . ?
F9 F8 F7 139(2) . . ?
F9 F8 C25 71.2(14) . . ?
F7 F8 C25 70.3(12) . . ?
F8 F9 C25 59.0(11) . . ?
F8 F9 F10 109.1(19) . . ?
C25 F9 F10 56.9(11) . . ?
F11 F10 C25 64.1(17) . . ?
F11 F10 F9 115(2) . . ?
C25 F10 F9 57.5(9) . . ?
F10 F11 C25 70.1(12) . . ?
F10 F11 F12 134(2) . . ?
C25 F11 F12 64.4(15) . . ?
F11 F12 C25 57.1(11) . . ?
F11 F12 F7 105.5(15) . . ?
C25 F12 F7 57.8(8) . . ?
C5 O1 Y1 136.3(3) . . ?
C7 O2 Y1 128.7(3) . . ?
C13 O3 Y1 135.6(3) . . ?
C15 O4 Y1 134.4(3) . . ?
C22 O5 Y1 132.6(3) . . ?
C24 O6 Y1 133.2(3) . . ?
C18 S1A C21 96.7(8) . . ?
C21 C20 C19 114(3) . . ?
C19 S1B C21 92.9(4) . . ?
C21 C17 C18 108(2) . . ?
C1 S2 C4 91.8(3) . . ?
C9 S3 C12 92.0(3) . . ?
O4 Y1 O1 92.65(14) . . ?
O4 Y1 O3 73.93(13) . . ?
O1 Y1 O3 144.15(14) . . ?
O4 Y1 O2 81.28(14) . . ?
O1 Y1 O2 71.37(13) . . ?
O3 Y1 O2 73.77(13) . . ?
O4 Y1 O7 148.67(13) . . ?
O1 Y1 O7 101.98(13) . . ?
O3 Y1 O7 78.14(13) . . ?
O2 Y1 O7 77.50(14) . . ?
O4 Y1 O6 144.05(13) . . ?
O1 Y1 O6 77.14(13) . . ?
O3 Y1 O6 132.05(13) . . ?
O2 Y1 O6 125.57(14) . . ?
O7 Y1 O6 66.99(13) . . ?
O4 Y1 O8 101.09(14) . . ?
O1 Y1 O8 144.70(14) . . ?
O3 Y1 O8 71.15(14) . . ?
O2 Y1 O8 142.51(13) . . ?
O7 Y1 O8 82.76(14) . . ?
O6 Y1 O8 72.68(14) . . ?
O4 Y1 O5 71.94(13) . . ?
O1 Y1 O5 74.56(13) . . ?
O3 Y1 O5 128.60(12) . . ?
O2 Y1 O5 135.12(13) . . ?
O7 Y1 O5 138.56(13) . . ?
O6 Y1 O5 72.12(12) . . ?
O8 Y1 O5 79.05(13) . . ?
C2 C1 H1 123.0 . . ?
S2 C1 H1 123.0 . . ?
C1 C2 H2 122.7 . . ?
C3 C2 H2 122.7 . . ?
C2 C3 H3 127.0 . . ?
C4 C3 H3 127.0 . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C10 C9 H9 123.5 . . ?
S3 C9 H9 123.5 . . ?
C9 C10 H10 122.4 . . ?
C11 C10 H10 122.4 . . ?
C10 C11 H11 125.9 . . ?
C12 C11 H11 125.9 . . ?
C15 C14 H14 118.5 . . ?
C13 C14 H14 118.5 . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 127.6 . . ?
S1A C18 H18 120.7 . . ?
C18 C19 H19 127.9 . . ?
C20 C19 H19 127.9 . . ?
S1B C19 H19 115.7 . . ?
C24 C23 H23 118.5 . . ?
C22 C23 H23 118.5 . . ?
Y1 O7 H7A 116.5 . . ?
Y1 O7 H7B 139.8 . . ?
H7A O7 H7B 103.4 . . ?
C21 C20 H20 123.2 . . ?
C19 C20 H20 123.2 . . ?
C21 C17 H17 125.9 . . ?
C18 C17 H17 125.9 . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.834
_refine_diff_density_min -0.780
_refine_diff_density_rms 0.115
_publ_section_references
;
Mackay, S., Gilmore, C. J., Edwards, C., Stewart, N. & Shankland, K. (1999).
maXus Computer Program for the Solution and Refinement of Crystal
Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University
of Glasgow.
Johnson, C. K. (1976). ORTEPII. A Fortran Thermal-Ellipsoid Plot
Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge,
Tennessee, USA.
Otwinowski, Z. & Minor, W. (1997). In Methods in Enzymology, 276, edited
by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press.
Sheldrick, G. M. (1997). SHELXS97. Program for Crystal Structure
Solution. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal
Structures. University of G\"ottingen, Germany.
;