# Electronic Supplementary Material (ESI) for RSC Advances
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_coden_Cambridge 222
loop_
_publ_author_name
'Schulz, A.'
_publ_contact_author_name 'Schulz, Axel'
_publ_contact_author_email axel.schulz@uni-rostock.de
_publ_section_title
;
Sulfate and Nitrate Adduct Anions
;
# Attachment '- boran-sauerstoff.cif'
#=============================================================================
data_kv12
_database_code_depnum_ccdc_archive 'CCDC 817745'
#TrackingRef '- boran-sauerstoff.cif'
_audit_author_name 'Villinger, A.'
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C18 B F15 H2O, O2 H4'
_chemical_formula_sum 'C18 H6 B F15 O3'
_chemical_formula_weight 566.04
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'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_Int_Tables_number 15
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 19.367(4)
_cell_length_b 10.729(2)
_cell_length_c 19.820(4)
_cell_angle_alpha 90.00
_cell_angle_beta 96.45(3)
_cell_angle_gamma 90.00
_cell_volume 4092.2(14)
_cell_formula_units_Z 8
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 8416
_cell_measurement_theta_min 4.414
_cell_measurement_theta_max 57.923
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.17
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.837
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2224
_exptl_absorpt_coefficient_mu 0.213
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9293
_exptl_absorpt_correction_T_max 0.9648
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method 'phi and psi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 21007
_diffrn_reflns_av_R_equivalents 0.0212
_diffrn_reflns_av_sigmaI/netI 0.0207
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 2.36
_diffrn_reflns_theta_max 28.50
_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full 28.50
_diffrn_measured_fraction_theta_full 0.980
_reflns_number_total 5088
_reflns_number_gt 3946
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex v2.0-2'
_computing_cell_refinement 'Bruker Apex v2.0-2'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups) or 0.99 \%A (methylene groups) and with
U~iso~(H) = 1.5 times U~eq~(C) (methyl groups) or with
U~iso~(H) = 1.2 times U~eq~(C) (methylene groups). Torsion
angles of all methyl groups were allowed to refine.
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^)+(0.0546P)^2^+2.3740P] 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 5088
_refine_ls_number_parameters 358
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0539
_refine_ls_R_factor_gt 0.0387
_refine_ls_wR_factor_ref 0.1059
_refine_ls_wR_factor_gt 0.0998
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_restrained_S_all 1.046
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.443
_refine_diff_density_min -0.331
_refine_diff_density_rms 0.050
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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
O1 O 0.10695(5) 0.88523(10) 0.31002(6) 0.0275(2) Uani 1 1 d . . .
H1 H 0.0997(13) 0.820(2) 0.2752(13) 0.068(7) Uiso 1 1 d . . .
H2 H 0.0905(11) 0.859(2) 0.3443(12) 0.052(6) Uiso 1 1 d . . .
B B 0.15663(8) 1.00129(15) 0.30579(8) 0.0211(3) Uani 1 1 d . . .
C1 C 0.11127(7) 1.12617(14) 0.32424(7) 0.0236(3) Uani 1 1 d . . .
C2 C 0.10687(7) 1.23982(14) 0.28872(8) 0.0271(3) Uani 1 1 d . . .
C3 C 0.06918(8) 1.34359(15) 0.30749(9) 0.0303(3) Uani 1 1 d . . .
C4 C 0.03272(8) 1.33624(16) 0.36327(9) 0.0329(4) Uani 1 1 d . . .
C5 C 0.03509(8) 1.22556(17) 0.40037(8) 0.0324(4) Uani 1 1 d . . .
C6 C 0.07457(7) 1.12513(15) 0.38083(7) 0.0261(3) Uani 1 1 d . . .
C7 C 0.17254(7) 0.99812(13) 0.22661(7) 0.0212(3) Uani 1 1 d . . .
C8 C 0.23847(7) 1.00290(13) 0.20359(8) 0.0232(3) Uani 1 1 d . . .
C9 C 0.24886(7) 0.99150(14) 0.13583(8) 0.0257(3) Uani 1 1 d . . .
C10 C 0.19175(8) 0.97374(15) 0.08709(8) 0.0281(3) Uani 1 1 d . . .
C11 C 0.12498(8) 0.97105(15) 0.10655(8) 0.0271(3) Uani 1 1 d . . .
C12 C 0.11697(7) 0.98457(14) 0.17441(7) 0.0235(3) Uani 1 1 d . . .
C13 C 0.22680(7) 0.98427(14) 0.36199(7) 0.0225(3) Uani 1 1 d . . .
C14 C 0.26959(8) 1.08688(14) 0.38257(8) 0.0277(3) Uani 1 1 d . . .
C15 C 0.32945(8) 1.08008(15) 0.42957(8) 0.0306(3) Uani 1 1 d . . .
C16 C 0.34902(8) 0.96551(16) 0.45917(8) 0.0302(3) Uani 1 1 d . . .
C17 C 0.30915(9) 0.86038(16) 0.44058(9) 0.0351(4) Uani 1 1 d . . .
C18 C 0.24969(8) 0.87122(14) 0.39291(9) 0.0307(3) Uani 1 1 d . . .
F1 F 0.14119(5) 1.25599(9) 0.23348(5) 0.0395(2) Uani 1 1 d . . .
F2 F 0.06819(5) 1.45225(9) 0.27198(6) 0.0425(3) Uani 1 1 d . . .
F3 F -0.00459(5) 1.43638(11) 0.38129(6) 0.0471(3) Uani 1 1 d . . .
F4 F -0.00104(6) 1.21704(12) 0.45462(5) 0.0474(3) Uani 1 1 d . . .
F5 F 0.07629(5) 1.01907(9) 0.41939(4) 0.0332(2) Uani 1 1 d . . .
F6 F 0.29747(4) 1.02065(10) 0.24780(5) 0.0368(2) Uani 1 1 d . . .
F7 F 0.31421(5) 0.99644(10) 0.11704(5) 0.0376(2) Uani 1 1 d . . .
F8 F 0.20129(5) 0.95911(11) 0.02150(5) 0.0428(3) Uani 1 1 d . . .
F9 F 0.06849(5) 0.95377(11) 0.05981(5) 0.0413(3) Uani 1 1 d . . .
F10 F 0.04960(4) 0.98283(9) 0.18965(5) 0.0319(2) Uani 1 1 d . . .
F11 F 0.25495(5) 1.20115(9) 0.35390(6) 0.0483(3) Uani 1 1 d . . .
F12 F 0.36836(6) 1.18377(11) 0.44698(7) 0.0543(3) Uani 1 1 d . . .
F13 F 0.40664(5) 0.95723(11) 0.50561(5) 0.0417(3) Uani 1 1 d . . .
F14 F 0.32749(6) 0.74793(11) 0.46969(7) 0.0607(4) Uani 1 1 d . . .
F15 F 0.21397(6) 0.76206(10) 0.37768(7) 0.0584(4) Uani 1 1 d . . .
O2 O 0.08263(9) 0.71203(14) 0.21966(8) 0.0486(4) Uani 1 1 d . . .
H3 H 0.0497(15) 0.713(3) 0.1919(15) 0.069(9) Uiso 1 1 d . . .
H4 H 0.0977(15) 0.641(3) 0.2263(15) 0.081(9) Uiso 1 1 d . . .
O3 O 0.03155(8) 0.75387(15) 0.39420(7) 0.0454(3) Uani 1 1 d . . .
H5 H 0.0523(15) 0.699(3) 0.4162(15) 0.079(9) Uiso 1 1 d . . .
H6 H 0.0109(17) 0.798(3) 0.4214(17) 0.095(11) Uiso 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
O1 0.0301(5) 0.0319(6) 0.0214(5) 0.0005(5) 0.0063(4) -0.0096(4)
B 0.0194(7) 0.0243(8) 0.0197(7) 0.0007(6) 0.0018(6) -0.0028(6)
C1 0.0191(6) 0.0290(7) 0.0220(7) -0.0037(6) -0.0011(5) -0.0002(5)
C2 0.0212(6) 0.0311(8) 0.0292(8) 0.0003(6) 0.0043(6) -0.0017(6)
C3 0.0216(6) 0.0276(8) 0.0403(9) 0.0005(7) -0.0030(6) -0.0006(6)
C4 0.0243(7) 0.0349(9) 0.0383(9) -0.0118(7) -0.0027(6) 0.0063(6)
C5 0.0275(7) 0.0459(10) 0.0235(7) -0.0101(7) 0.0019(6) 0.0030(7)
C6 0.0236(6) 0.0335(8) 0.0201(7) -0.0024(6) -0.0023(5) -0.0014(6)
C7 0.0208(6) 0.0220(7) 0.0206(7) 0.0011(5) 0.0016(5) -0.0013(5)
C8 0.0208(6) 0.0250(7) 0.0238(7) 0.0004(5) 0.0020(5) 0.0000(5)
C9 0.0225(6) 0.0284(7) 0.0275(8) 0.0043(6) 0.0086(6) 0.0028(5)
C10 0.0337(8) 0.0323(8) 0.0192(7) 0.0019(6) 0.0076(6) 0.0023(6)
C11 0.0260(7) 0.0342(8) 0.0200(7) 0.0010(6) -0.0013(6) -0.0018(6)
C12 0.0206(6) 0.0280(7) 0.0223(7) 0.0023(6) 0.0044(5) -0.0010(5)
C13 0.0214(6) 0.0290(7) 0.0173(6) -0.0010(5) 0.0034(5) 0.0012(5)
C14 0.0261(7) 0.0279(8) 0.0284(8) 0.0053(6) -0.0008(6) -0.0004(6)
C15 0.0266(7) 0.0328(8) 0.0313(8) -0.0005(6) -0.0019(6) -0.0050(6)
C16 0.0237(7) 0.0425(9) 0.0235(7) -0.0005(7) -0.0016(6) 0.0068(6)
C17 0.0356(8) 0.0295(8) 0.0386(9) 0.0044(7) -0.0029(7) 0.0103(7)
C18 0.0322(7) 0.0237(7) 0.0349(9) -0.0034(6) -0.0015(7) 0.0026(6)
F1 0.0425(5) 0.0348(5) 0.0447(6) 0.0110(4) 0.0204(5) 0.0037(4)
F2 0.0297(5) 0.0300(5) 0.0674(7) 0.0099(5) 0.0041(5) 0.0030(4)
F3 0.0411(6) 0.0454(6) 0.0545(7) -0.0168(5) 0.0037(5) 0.0149(5)
F4 0.0496(6) 0.0657(7) 0.0294(5) -0.0076(5) 0.0154(5) 0.0141(5)
F5 0.0377(5) 0.0429(5) 0.0197(4) 0.0033(4) 0.0057(4) 0.0032(4)
F6 0.0198(4) 0.0623(7) 0.0282(5) -0.0015(4) 0.0020(4) -0.0055(4)
F7 0.0251(4) 0.0565(6) 0.0334(5) 0.0059(4) 0.0133(4) 0.0044(4)
F8 0.0430(6) 0.0679(7) 0.0191(5) -0.0008(5) 0.0099(4) 0.0016(5)
F9 0.0315(5) 0.0703(7) 0.0206(5) 0.0002(5) -0.0030(4) -0.0046(5)
F10 0.0182(4) 0.0520(6) 0.0255(5) 0.0029(4) 0.0026(3) -0.0011(4)
F11 0.0385(5) 0.0314(5) 0.0696(8) 0.0198(5) -0.0176(5) -0.0099(4)
F12 0.0418(6) 0.0445(6) 0.0699(8) 0.0026(6) -0.0238(5) -0.0146(5)
F13 0.0316(5) 0.0570(7) 0.0335(5) 0.0028(5) -0.0097(4) 0.0073(4)
F14 0.0602(7) 0.0382(6) 0.0771(9) 0.0162(6) -0.0209(6) 0.0118(5)
F15 0.0563(7) 0.0230(5) 0.0883(10) -0.0012(5) -0.0255(6) -0.0002(5)
O2 0.0656(10) 0.0291(7) 0.0486(9) -0.0049(6) -0.0050(7) 0.0029(6)
O3 0.0536(8) 0.0454(8) 0.0390(8) 0.0170(6) 0.0136(6) 0.0076(7)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
O1 B 1.5816(18) . ?
O1 H1 0.98(3) . ?
O1 H2 0.83(2) . ?
B C7 1.633(2) . ?
B C1 1.665(2) . ?
B C13 1.668(2) . ?
C1 C6 1.394(2) . ?
C1 C2 1.406(2) . ?
C2 F1 1.3543(18) . ?
C2 C3 1.404(2) . ?
C3 F2 1.3608(19) . ?
C3 C4 1.379(2) . ?
C4 F3 1.3646(18) . ?
C4 C5 1.395(3) . ?
C5 F4 1.3502(19) . ?
C5 C6 1.401(2) . ?
C6 F5 1.3690(18) . ?
C7 C8 1.404(2) . ?
C7 C12 1.414(2) . ?
C8 F6 1.3728(17) . ?
C8 C9 1.386(2) . ?
C9 F7 1.3599(17) . ?
C9 C10 1.397(2) . ?
C10 F8 1.3428(18) . ?
C10 C11 1.391(2) . ?
C11 F9 1.3644(17) . ?
C11 C12 1.379(2) . ?
C12 F10 1.3720(16) . ?
C13 C18 1.408(2) . ?
C13 C14 1.410(2) . ?
C14 F11 1.3676(18) . ?
C14 C15 1.405(2) . ?
C15 F12 1.3661(19) . ?
C15 C16 1.396(2) . ?
C16 F13 1.3674(17) . ?
C16 C17 1.393(2) . ?
C17 F14 1.3670(19) . ?
C17 C18 1.410(2) . ?
C18 F15 1.3764(19) . ?
O2 H3 0.79(3) . ?
O2 H4 0.82(3) . ?
O3 H5 0.82(3) . ?
O3 H6 0.85(3) . ?
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
B O1 H1 124.2(15) . . ?
B O1 H2 126.9(16) . . ?
H1 O1 H2 107(2) . . ?
O1 B C7 102.48(11) . . ?
O1 B C1 106.42(11) . . ?
C7 B C1 112.88(12) . . ?
O1 B C13 109.47(11) . . ?
C7 B C13 114.34(11) . . ?
C1 B C13 110.60(11) . . ?
C6 C1 C2 113.72(13) . . ?
C6 C1 B 119.98(13) . . ?
C2 C1 B 126.28(13) . . ?
F1 C2 C3 115.43(14) . . ?
F1 C2 C1 120.55(13) . . ?
C3 C2 C1 124.00(14) . . ?
F2 C3 C4 119.00(14) . . ?
F2 C3 C2 121.33(15) . . ?
C4 C3 C2 119.67(15) . . ?
F3 C4 C3 119.90(16) . . ?
F3 C4 C5 121.30(15) . . ?
C3 C4 C5 118.80(14) . . ?
F4 C5 C4 119.22(14) . . ?
F4 C5 C6 121.05(15) . . ?
C4 C5 C6 119.73(15) . . ?
F5 C6 C1 118.24(13) . . ?
F5 C6 C5 117.70(14) . . ?
C1 C6 C5 124.05(15) . . ?
C8 C7 C12 114.28(13) . . ?
C8 C7 B 126.01(13) . . ?
C12 C7 B 119.67(12) . . ?
F6 C8 C9 115.46(13) . . ?
F6 C8 C7 121.32(13) . . ?
C9 C8 C7 123.22(14) . . ?
F7 C9 C8 120.19(14) . . ?
F7 C9 C10 120.31(14) . . ?
C8 C9 C10 119.49(13) . . ?
F8 C10 C11 119.96(14) . . ?
F8 C10 C9 120.07(14) . . ?
C11 C10 C9 119.98(14) . . ?
F9 C11 C12 120.48(13) . . ?
F9 C11 C10 120.95(13) . . ?
C12 C11 C10 118.57(14) . . ?
F10 C12 C11 115.29(13) . . ?
F10 C12 C7 120.32(12) . . ?
C11 C12 C7 124.39(13) . . ?
C18 C13 C14 113.61(13) . . ?
C18 C13 B 125.33(13) . . ?
C14 C13 B 121.06(13) . . ?
F11 C14 C15 116.05(13) . . ?
F11 C14 C13 119.47(13) . . ?
C15 C14 C13 124.43(14) . . ?
F12 C15 C16 119.66(14) . . ?
F12 C15 C14 121.05(14) . . ?
C16 C15 C14 119.28(14) . . ?
F13 C16 C17 120.78(14) . . ?
F13 C16 C15 120.17(15) . . ?
C17 C16 C15 119.05(14) . . ?
F14 C17 C16 119.54(14) . . ?
F14 C17 C18 120.64(15) . . ?
C16 C17 C18 119.82(14) . . ?
F15 C18 C13 120.78(14) . . ?
F15 C18 C17 115.42(14) . . ?
C13 C18 C17 123.80(14) . . ?
H3 O2 H4 112(3) . . ?
H5 O3 H6 108(3) . . ?
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
O1 B C1 C6 47.77(16) . . . . ?
C7 B C1 C6 159.42(12) . . . . ?
C13 B C1 C6 -71.05(16) . . . . ?
O1 B C1 C2 -134.19(14) . . . . ?
C7 B C1 C2 -22.55(19) . . . . ?
C13 B C1 C2 106.99(15) . . . . ?
C6 C1 C2 F1 178.43(12) . . . . ?
B C1 C2 F1 0.3(2) . . . . ?
C6 C1 C2 C3 -0.2(2) . . . . ?
B C1 C2 C3 -178.30(14) . . . . ?
F1 C2 C3 F2 -0.2(2) . . . . ?
C1 C2 C3 F2 178.42(13) . . . . ?
F1 C2 C3 C4 -179.77(13) . . . . ?
C1 C2 C3 C4 -1.1(2) . . . . ?
F2 C3 C4 F3 1.2(2) . . . . ?
C2 C3 C4 F3 -179.29(14) . . . . ?
F2 C3 C4 C5 -178.65(14) . . . . ?
C2 C3 C4 C5 0.9(2) . . . . ?
F3 C4 C5 F4 0.9(2) . . . . ?
C3 C4 C5 F4 -179.30(13) . . . . ?
F3 C4 C5 C6 -179.28(14) . . . . ?
C3 C4 C5 C6 0.5(2) . . . . ?
C2 C1 C6 F5 -179.21(12) . . . . ?
B C1 C6 F5 -0.94(19) . . . . ?
C2 C1 C6 C5 1.7(2) . . . . ?
B C1 C6 C5 179.95(13) . . . . ?
F4 C5 C6 F5 -1.2(2) . . . . ?
C4 C5 C6 F5 178.96(13) . . . . ?
F4 C5 C6 C1 177.89(13) . . . . ?
C4 C5 C6 C1 -1.9(2) . . . . ?
O1 B C7 C8 -129.25(14) . . . . ?
C1 B C7 C8 116.69(15) . . . . ?
C13 B C7 C8 -10.9(2) . . . . ?
O1 B C7 C12 48.09(16) . . . . ?
C1 B C7 C12 -65.97(16) . . . . ?
C13 B C7 C12 166.44(13) . . . . ?
C12 C7 C8 F6 177.47(13) . . . . ?
B C7 C8 F6 -5.1(2) . . . . ?
C12 C7 C8 C9 -1.9(2) . . . . ?
B C7 C8 C9 175.55(14) . . . . ?
F6 C8 C9 F7 0.9(2) . . . . ?
C7 C8 C9 F7 -179.71(13) . . . . ?
F6 C8 C9 C10 -179.71(13) . . . . ?
C7 C8 C9 C10 -0.3(2) . . . . ?
F7 C9 C10 F8 1.3(2) . . . . ?
C8 C9 C10 F8 -178.16(14) . . . . ?
F7 C9 C10 C11 -178.83(14) . . . . ?
C8 C9 C10 C11 1.8(2) . . . . ?
F8 C10 C11 F9 -0.1(2) . . . . ?
C9 C10 C11 F9 -179.96(14) . . . . ?
F8 C10 C11 C12 179.08(14) . . . . ?
C9 C10 C11 C12 -0.8(2) . . . . ?
F9 C11 C12 F10 -1.8(2) . . . . ?
C10 C11 C12 F10 179.07(13) . . . . ?
F9 C11 C12 C7 177.51(14) . . . . ?
C10 C11 C12 C7 -1.6(2) . . . . ?
C8 C7 C12 F10 -177.81(12) . . . . ?
B C7 C12 F10 4.5(2) . . . . ?
C8 C7 C12 C11 2.9(2) . . . . ?
B C7 C12 C11 -174.72(14) . . . . ?
O1 B C13 C18 18.29(19) . . . . ?
C7 B C13 C18 -96.01(17) . . . . ?
C1 B C13 C18 135.24(15) . . . . ?
O1 B C13 C14 -162.07(13) . . . . ?
C7 B C13 C14 83.63(17) . . . . ?
C1 B C13 C14 -45.12(18) . . . . ?
C18 C13 C14 F11 176.94(14) . . . . ?
B C13 C14 F11 -2.7(2) . . . . ?
C18 C13 C14 C15 -0.3(2) . . . . ?
B C13 C14 C15 -179.99(14) . . . . ?
F11 C14 C15 F12 2.6(2) . . . . ?
C13 C14 C15 F12 179.95(15) . . . . ?
F11 C14 C15 C16 -177.81(15) . . . . ?
C13 C14 C15 C16 -0.5(3) . . . . ?
F12 C15 C16 F13 0.3(2) . . . . ?
C14 C15 C16 F13 -179.24(14) . . . . ?
F12 C15 C16 C17 -179.53(15) . . . . ?
C14 C15 C16 C17 0.9(2) . . . . ?
F13 C16 C17 F14 0.7(2) . . . . ?
C15 C16 C17 F14 -179.44(16) . . . . ?
F13 C16 C17 C18 179.61(15) . . . . ?
C15 C16 C17 C18 -0.5(3) . . . . ?
C14 C13 C18 F15 -179.35(14) . . . . ?
B C13 C18 F15 0.3(2) . . . . ?
C14 C13 C18 C17 0.7(2) . . . . ?
B C13 C18 C17 -179.63(15) . . . . ?
F14 C17 C18 F15 -1.4(2) . . . . ?
C16 C17 C18 F15 179.74(15) . . . . ?
F14 C17 C18 C13 178.58(16) . . . . ?
C16 C17 C18 C13 -0.3(3) . . . . ?
#=============================================================================
data_KV56
_database_code_depnum_ccdc_archive 'CCDC 817746'
#TrackingRef '- boran-sauerstoff.cif'
_audit_author_name 'Voss, K.'
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C30 H30 Ag B F15 N O6'
_chemical_formula_sum 'C30 H30 Ag B F15 N O6'
_chemical_formula_weight 904.23
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'
B B 0.0013 0.0007 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CHEMICAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
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 9.384(7)
_cell_length_b 16.395(11)
_cell_length_c 22.826(14)
_cell_angle_alpha 90.00
_cell_angle_beta 92.49(5)
_cell_angle_gamma 90.00
_cell_volume 3509(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9870
_cell_measurement_theta_min 6.116
_cell_measurement_theta_max 51.538
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.67
_exptl_crystal_size_mid 0.39
_exptl_crystal_size_min 0.30
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.712
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1808
_exptl_absorpt_coefficient_mu 0.697
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6523
_exptl_absorpt_correction_T_max 0.8181
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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 Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and psi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 52126
_diffrn_reflns_av_R_equivalents 0.0395
_diffrn_reflns_av_sigmaI/netI 0.0234
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 1.53
_diffrn_reflns_theta_max 25.50
_reflns_number_total 6505
_reflns_number_gt 5351
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex v2.0-2'
_computing_cell_refinement 'Bruker Apex v2.0-2'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a
riding model , with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_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^)+(0.0467P)^2^+7.5811P] 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 6505
_refine_ls_number_parameters 493
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0595
_refine_ls_R_factor_gt 0.0453
_refine_ls_wR_factor_ref 0.1160
_refine_ls_wR_factor_gt 0.1089
_refine_ls_goodness_of_fit_ref 1.074
_refine_ls_restrained_S_all 1.074
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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
N1 N 0.0031(3) 0.34431(17) 0.86124(11) 0.0279(6) Uani 1 1 d . . .
O1 O -0.1000(2) 0.31172(13) 0.89204(9) 0.0265(5) Uani 1 1 d . . .
O2 O 0.1278(2) 0.32737(15) 0.87442(10) 0.0332(5) Uani 1 1 d . . .
O3 O -0.0359(3) 0.38863(16) 0.82140(11) 0.0392(6) Uani 1 1 d . . .
B1 B -0.0559(4) 0.2555(2) 0.94424(15) 0.0242(7) Uani 1 1 d . . .
C1 C -0.2106(3) 0.2242(2) 0.96702(14) 0.0266(7) Uani 1 1 d . . .
C2 C -0.3085(4) 0.1878(2) 0.92813(16) 0.0318(8) Uani 1 1 d . . .
C3 C -0.4335(4) 0.1512(2) 0.94401(19) 0.0412(9) Uani 1 1 d . . .
C4 C -0.4657(4) 0.1493(3) 1.0018(2) 0.0429(10) Uani 1 1 d . . .
C5 C -0.3745(4) 0.1853(2) 1.04226(17) 0.0386(9) Uani 1 1 d . . .
C6 C -0.2502(4) 0.2213(2) 1.02463(15) 0.0318(8) Uani 1 1 d . . .
C7 C 0.0335(3) 0.3129(2) 0.99117(14) 0.0266(7) Uani 1 1 d . . .
C8 C 0.1760(4) 0.3038(2) 1.00982(15) 0.0323(8) Uani 1 1 d . . .
C9 C 0.2442(4) 0.3527(3) 1.05128(18) 0.0422(9) Uani 1 1 d . . .
C10 C 0.1727(5) 0.4167(3) 1.07489(17) 0.0450(10) Uani 1 1 d . . .
C11 C 0.0345(4) 0.4310(2) 1.05655(16) 0.0384(9) Uani 1 1 d . . .
C12 C -0.0305(4) 0.3800(2) 1.01563(15) 0.0307(7) Uani 1 1 d . . .
C13 C 0.0240(3) 0.17237(19) 0.92361(14) 0.0246(7) Uani 1 1 d . . .
C14 C 0.0420(4) 0.1472(2) 0.86651(15) 0.0308(7) Uani 1 1 d . . .
C15 C 0.1075(4) 0.0747(2) 0.85218(16) 0.0378(8) Uani 1 1 d . . .
C16 C 0.1578(4) 0.0237(2) 0.89554(18) 0.0373(8) Uani 1 1 d . . .
C17 C 0.1383(4) 0.0440(2) 0.95289(17) 0.0335(8) Uani 1 1 d . . .
C18 C 0.0715(3) 0.1162(2) 0.96541(14) 0.0277(7) Uani 1 1 d . . .
F1 F -0.2812(2) 0.18470(14) 0.87063(9) 0.0431(5) Uani 1 1 d . . .
F2 F -0.5231(3) 0.11704(17) 0.90379(13) 0.0628(7) Uani 1 1 d . . .
F3 F -0.5834(2) 0.11122(16) 1.01852(14) 0.0636(8) Uani 1 1 d . . .
F4 F -0.4057(3) 0.18525(16) 1.09910(10) 0.0554(7) Uani 1 1 d . . .
F5 F -0.1658(2) 0.25244(14) 1.06830(9) 0.0431(5) Uani 1 1 d . . .
F6 F 0.2561(2) 0.24435(13) 0.98771(10) 0.0423(5) Uani 1 1 d . . .
F7 F 0.3813(3) 0.33777(18) 1.06814(12) 0.0646(7) Uani 1 1 d . . .
F8 F 0.2377(3) 0.46519(18) 1.11495(12) 0.0688(8) Uani 1 1 d . . .
F9 F -0.0369(3) 0.49466(14) 1.07850(10) 0.0525(6) Uani 1 1 d . . .
F10 F -0.1673(2) 0.39805(13) 0.99944(9) 0.0388(5) Uani 1 1 d . . .
F11 F -0.0051(2) 0.19286(13) 0.82053(8) 0.0387(5) Uani 1 1 d . . .
F12 F 0.1201(3) 0.05463(15) 0.79546(10) 0.0543(6) Uani 1 1 d . . .
F13 F 0.2243(3) -0.04604(14) 0.88237(12) 0.0554(6) Uani 1 1 d . . .
F14 F 0.1848(2) -0.00661(13) 0.99605(10) 0.0459(6) Uani 1 1 d . . .
F15 F 0.0539(2) 0.13245(12) 1.02266(8) 0.0351(5) Uani 1 1 d . . .
Ag1 Ag 0.27854(3) 0.38332(2) 0.795989(12) 0.04287(12) Uani 1 1 d . . .
O4 O 0.3513(3) 0.48423(18) 0.86423(12) 0.0492(7) Uani 1 1 d . . .
C19 C 0.4172(5) 0.4666(3) 0.9205(2) 0.0593(12) Uani 1 1 d . . .
H19A H 0.3455 0.4712 0.9508 0.071 Uiso 1 1 calc R . .
H19B H 0.4933 0.5071 0.9296 0.071 Uiso 1 1 calc R . .
C20 C 0.4785(5) 0.3843(3) 0.9218(2) 0.0618(13) Uani 1 1 d . . .
H20A H 0.4033 0.3443 0.9124 0.093 Uiso 1 1 calc R . .
H20B H 0.5208 0.3732 0.9610 0.093 Uiso 1 1 calc R . .
H20C H 0.5523 0.3805 0.8928 0.093 Uiso 1 1 calc R . .
C21 C 0.6267(5) 0.3524(4) 0.7588(2) 0.0669(14) Uani 1 1 d . . .
H21A H 0.6612 0.3374 0.7199 0.080 Uiso 1 1 calc R . .
H21B H 0.6963 0.3317 0.7891 0.080 Uiso 1 1 calc R . .
C22 C 0.4927(6) 0.2304(3) 0.7540(3) 0.0748(15) Uani 1 1 d . . .
H22A H 0.5720 0.2039 0.7768 0.090 Uiso 1 1 calc R . .
H22B H 0.5078 0.2218 0.7118 0.090 Uiso 1 1 calc R . .
C23 C 0.0035(8) 0.2824(5) 0.6867(3) 0.112(3) Uani 1 1 d . . .
H23A H 0.0735 0.2480 0.6678 0.168 Uiso 1 1 calc R . .
H23B H -0.0905 0.2751 0.6670 0.168 Uiso 1 1 calc R . .
H23C H -0.0010 0.2669 0.7281 0.168 Uiso 1 1 calc R . .
O5 O 0.1900(3) 0.3758(2) 0.70000(12) 0.0606(9) Uani 1 1 d . . .
C24 C 0.0447(6) 0.3648(5) 0.6828(2) 0.0787(18) Uani 1 1 d . . .
H24A H -0.0150 0.3983 0.7083 0.094 Uiso 1 1 calc R . .
H24B H 0.0282 0.3839 0.6420 0.094 Uiso 1 1 calc R . .
C25 C 0.2819(5) 0.3885(3) 0.65203(19) 0.0578(12) Uani 1 1 d . . .
H25A H 0.2458 0.3568 0.6176 0.069 Uiso 1 1 calc R . .
H25B H 0.3790 0.3687 0.6631 0.069 Uiso 1 1 calc R . .
C26 C 0.2883(7) 0.4754(4) 0.6364(3) 0.0806(17) Uani 1 1 d . . .
H26A H 0.1945 0.4934 0.6209 0.121 Uiso 1 1 calc R . .
H26B H 0.3590 0.4834 0.6066 0.121 Uiso 1 1 calc R . .
H26C H 0.3156 0.5074 0.6714 0.121 Uiso 1 1 calc R . .
C27 C 0.3577(8) 0.1942(4) 0.7692(4) 0.113(3) Uani 1 1 d . . .
H27A H 0.3436 0.2024 0.8111 0.170 Uiso 1 1 calc R . .
H27B H 0.3590 0.1356 0.7607 0.170 Uiso 1 1 calc R . .
H27C H 0.2796 0.2201 0.7462 0.170 Uiso 1 1 calc R . .
O6 O 0.4913(3) 0.31572(19) 0.76653(13) 0.0538(8) Uani 1 1 d . . .
C28 C 0.6165(5) 0.4396(4) 0.7632(2) 0.0723(15) Uani 1 1 d . . .
H28A H 0.5506 0.4601 0.7322 0.108 Uiso 1 1 calc R . .
H28B H 0.7110 0.4638 0.7588 0.108 Uiso 1 1 calc R . .
H28C H 0.5812 0.4543 0.8015 0.108 Uiso 1 1 calc R . .
C29 C 0.3136(5) 0.5677(3) 0.8553(2) 0.0580(12) Uani 1 1 d . . .
H29A H 0.4010 0.6010 0.8521 0.070 Uiso 1 1 calc R . .
H29B H 0.2611 0.5879 0.8890 0.070 Uiso 1 1 calc R . .
C30 C 0.2232(7) 0.5753(3) 0.8007(3) 0.0749(15) Uani 1 1 d . . .
H30A H 0.2739 0.5528 0.7678 0.112 Uiso 1 1 calc R . .
H30B H 0.2017 0.6330 0.7932 0.112 Uiso 1 1 calc R . .
H30C H 0.1340 0.5452 0.8050 0.112 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0335(16) 0.0274(15) 0.0231(14) -0.0030(12) 0.0050(12) -0.0039(12)
O1 0.0265(11) 0.0285(12) 0.0245(11) 0.0026(9) 0.0020(9) -0.0022(9)
O2 0.0281(13) 0.0401(14) 0.0318(13) -0.0010(11) 0.0061(10) -0.0044(11)
O3 0.0508(16) 0.0394(14) 0.0272(13) 0.0105(11) -0.0005(11) -0.0051(12)
B1 0.0250(17) 0.0268(19) 0.0207(17) 0.0009(14) 0.0005(14) -0.0001(15)
C1 0.0218(15) 0.0268(17) 0.0314(17) 0.0061(14) 0.0024(13) 0.0025(13)
C2 0.0269(17) 0.0313(18) 0.0371(19) 0.0050(15) -0.0012(14) -0.0014(14)
C3 0.0235(17) 0.038(2) 0.061(3) 0.0090(19) -0.0062(17) -0.0019(16)
C4 0.0192(17) 0.042(2) 0.068(3) 0.021(2) 0.0087(17) 0.0005(16)
C5 0.0346(19) 0.038(2) 0.044(2) 0.0186(17) 0.0145(17) 0.0112(16)
C6 0.0267(17) 0.0356(19) 0.0332(18) 0.0070(15) 0.0028(14) 0.0060(14)
C7 0.0296(17) 0.0270(17) 0.0232(16) 0.0005(13) 0.0017(13) -0.0036(14)
C8 0.0288(17) 0.0337(19) 0.0342(18) -0.0020(15) -0.0008(14) -0.0008(15)
C9 0.0321(19) 0.049(2) 0.045(2) -0.0010(19) -0.0082(17) -0.0090(17)
C10 0.052(2) 0.047(2) 0.035(2) -0.0131(18) -0.0026(18) -0.0148(19)
C11 0.053(2) 0.0317(19) 0.0315(18) -0.0096(15) 0.0100(17) -0.0061(17)
C12 0.0318(18) 0.0328(18) 0.0277(17) 0.0014(14) 0.0044(14) -0.0023(15)
C13 0.0216(15) 0.0241(16) 0.0280(16) -0.0007(13) 0.0007(12) -0.0046(13)
C14 0.0331(18) 0.0282(17) 0.0311(18) -0.0006(14) 0.0035(14) -0.0004(14)
C15 0.039(2) 0.039(2) 0.0361(19) -0.0096(17) 0.0062(16) -0.0018(17)
C16 0.0315(18) 0.0257(18) 0.055(2) -0.0059(17) 0.0033(17) 0.0037(15)
C17 0.0250(17) 0.0295(18) 0.045(2) 0.0047(16) -0.0056(15) -0.0032(14)
C18 0.0238(16) 0.0301(17) 0.0287(17) 0.0000(14) -0.0029(13) -0.0063(14)
F1 0.0394(12) 0.0559(14) 0.0334(11) -0.0037(10) -0.0068(9) -0.0126(10)
F2 0.0362(13) 0.0683(18) 0.0824(19) 0.0055(14) -0.0161(12) -0.0200(12)
F3 0.0271(11) 0.0669(17) 0.098(2) 0.0351(15) 0.0133(12) -0.0064(11)
F4 0.0492(14) 0.0699(17) 0.0489(14) 0.0240(12) 0.0243(11) 0.0096(12)
F5 0.0463(12) 0.0577(14) 0.0257(10) 0.0037(10) 0.0060(9) -0.0044(11)
F6 0.0252(10) 0.0408(12) 0.0602(14) -0.0109(10) -0.0056(9) 0.0019(9)
F7 0.0404(13) 0.0751(19) 0.0760(18) -0.0175(15) -0.0239(12) -0.0106(13)
F8 0.0728(18) 0.0741(19) 0.0584(16) -0.0330(14) -0.0104(14) -0.0239(15)
F9 0.0710(16) 0.0389(13) 0.0488(13) -0.0194(11) 0.0161(12) -0.0041(12)
F10 0.0363(11) 0.0373(12) 0.0431(12) -0.0076(9) 0.0044(9) 0.0072(9)
F11 0.0565(13) 0.0361(11) 0.0233(10) -0.0021(8) 0.0007(9) 0.0050(10)
F12 0.0731(17) 0.0492(14) 0.0417(13) -0.0177(11) 0.0134(12) 0.0082(12)
F13 0.0571(15) 0.0366(13) 0.0723(17) -0.0120(12) 0.0022(13) 0.0176(11)
F14 0.0455(13) 0.0332(12) 0.0579(14) 0.0121(10) -0.0100(11) 0.0032(10)
F15 0.0397(11) 0.0386(11) 0.0266(10) 0.0032(8) -0.0019(8) -0.0001(9)
Ag1 0.04144(18) 0.0545(2) 0.03331(17) -0.00395(13) 0.00922(12) -0.00741(14)
O4 0.0598(18) 0.0457(16) 0.0424(16) -0.0085(13) 0.0063(13) -0.0082(14)
C19 0.054(3) 0.079(4) 0.044(2) -0.014(2) -0.002(2) -0.013(2)
C20 0.051(3) 0.081(4) 0.053(3) 0.007(2) -0.006(2) -0.004(3)
C21 0.035(2) 0.100(4) 0.065(3) -0.009(3) 0.002(2) -0.005(3)
C22 0.076(4) 0.068(3) 0.079(4) -0.004(3) -0.012(3) 0.024(3)
C23 0.112(6) 0.153(7) 0.068(4) 0.038(4) -0.031(4) -0.044(5)
O5 0.0505(18) 0.098(3) 0.0330(15) 0.0081(15) 0.0007(13) -0.0008(17)
C24 0.054(3) 0.142(6) 0.040(3) 0.003(3) 0.000(2) 0.012(3)
C25 0.066(3) 0.075(3) 0.034(2) 0.003(2) 0.012(2) 0.006(3)
C26 0.110(5) 0.070(4) 0.064(3) -0.001(3) 0.021(3) 0.001(3)
C27 0.090(5) 0.049(3) 0.202(9) 0.017(4) 0.021(5) 0.002(3)
O6 0.0449(16) 0.0594(19) 0.0569(18) -0.0074(15) 0.0002(14) 0.0023(14)
C28 0.049(3) 0.097(4) 0.072(3) 0.003(3) 0.011(2) -0.026(3)
C29 0.067(3) 0.044(3) 0.065(3) -0.009(2) 0.023(2) -0.011(2)
C30 0.094(4) 0.052(3) 0.078(4) 0.010(3) 0.009(3) 0.013(3)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
N1 O3 1.208(4) . ?
N1 O2 1.228(4) . ?
N1 O1 1.332(3) . ?
O1 B1 1.548(4) . ?
O2 Ag1 2.504(3) . ?
B1 C7 1.630(5) . ?
B1 C13 1.635(5) . ?
B1 C1 1.645(5) . ?
C1 C6 1.383(5) . ?
C1 C2 1.385(5) . ?
C2 F1 1.349(4) . ?
C2 C3 1.380(5) . ?
C3 F2 1.340(5) . ?
C3 C4 1.367(6) . ?
C4 F3 1.339(4) . ?
C4 C5 1.365(6) . ?
C5 F4 1.342(4) . ?
C5 C6 1.383(5) . ?
C6 F5 1.346(4) . ?
C7 C12 1.384(5) . ?
C7 C8 1.393(5) . ?
C8 F6 1.343(4) . ?
C8 C9 1.377(5) . ?
C9 F7 1.349(5) . ?
C9 C10 1.370(6) . ?
C10 F8 1.338(4) . ?
C10 C11 1.365(6) . ?
C11 F9 1.348(4) . ?
C11 C12 1.377(5) . ?
C12 F10 1.353(4) . ?
C13 C14 1.384(5) . ?
C13 C18 1.386(5) . ?
C14 F11 1.348(4) . ?
C14 C15 1.384(5) . ?
C15 F12 1.346(4) . ?
C15 C16 1.365(6) . ?
C16 F13 1.343(4) . ?
C16 C17 1.371(5) . ?
C17 F14 1.346(4) . ?
C17 C18 1.376(5) . ?
C18 F15 1.351(4) . ?
Ag1 O5 2.313(3) . ?
Ag1 O4 2.353(3) . ?
Ag1 O6 2.405(3) . ?
O4 C29 1.426(6) . ?
O4 C19 1.430(5) . ?
C19 C20 1.467(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 O6 1.424(6) . ?
C21 C28 1.436(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 O6 1.428(6) . ?
C22 C27 1.455(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.409(10) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O5 C24 1.414(6) . ?
O5 C25 1.438(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.470(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.482(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
O3 N1 O2 125.1(3) . . ?
O3 N1 O1 115.8(3) . . ?
O2 N1 O1 119.1(3) . . ?
N1 O1 B1 118.0(2) . . ?
N1 O2 Ag1 107.71(19) . . ?
O1 B1 C7 106.0(3) . . ?
O1 B1 C13 112.7(3) . . ?
C7 B1 C13 116.2(3) . . ?
O1 B1 C1 102.7(2) . . ?
C7 B1 C1 114.1(3) . . ?
C13 B1 C1 104.6(3) . . ?
C6 C1 C2 113.4(3) . . ?
C6 C1 B1 126.0(3) . . ?
C2 C1 B1 120.1(3) . . ?
F1 C2 C3 116.0(3) . . ?
F1 C2 C1 119.4(3) . . ?
C3 C2 C1 124.5(3) . . ?
F2 C3 C4 119.6(3) . . ?
F2 C3 C2 121.1(4) . . ?
C4 C3 C2 119.3(4) . . ?
F3 C4 C5 120.7(4) . . ?
F3 C4 C3 120.3(4) . . ?
C5 C4 C3 119.0(3) . . ?
F4 C5 C4 119.8(3) . . ?
F4 C5 C6 120.2(4) . . ?
C4 C5 C6 120.0(3) . . ?
F5 C6 C1 121.2(3) . . ?
F5 C6 C5 115.0(3) . . ?
C1 C6 C5 123.8(4) . . ?
C12 C7 C8 112.9(3) . . ?
C12 C7 B1 120.3(3) . . ?
C8 C7 B1 126.8(3) . . ?
F6 C8 C9 115.4(3) . . ?
F6 C8 C7 120.5(3) . . ?
C9 C8 C7 124.1(3) . . ?
F7 C9 C10 120.3(4) . . ?
F7 C9 C8 120.0(4) . . ?
C10 C9 C8 119.7(4) . . ?
F8 C10 C11 120.4(4) . . ?
F8 C10 C9 120.5(4) . . ?
C11 C10 C9 119.1(3) . . ?
F9 C11 C10 120.0(3) . . ?
F9 C11 C12 120.6(4) . . ?
C10 C11 C12 119.4(3) . . ?
F10 C12 C11 116.1(3) . . ?
F10 C12 C7 119.2(3) . . ?
C11 C12 C7 124.7(3) . . ?
C14 C13 C18 113.7(3) . . ?
C14 C13 B1 126.6(3) . . ?
C18 C13 B1 119.6(3) . . ?
F11 C14 C15 115.3(3) . . ?
F11 C14 C13 121.2(3) . . ?
C15 C14 C13 123.5(3) . . ?
F12 C15 C16 120.4(3) . . ?
F12 C15 C14 119.7(3) . . ?
C16 C15 C14 119.9(3) . . ?
F13 C16 C15 120.6(4) . . ?
F13 C16 C17 120.2(3) . . ?
C15 C16 C17 119.2(3) . . ?
F14 C17 C16 119.8(3) . . ?
F14 C17 C18 121.0(3) . . ?
C16 C17 C18 119.2(3) . . ?
F15 C18 C17 116.5(3) . . ?
F15 C18 C13 119.0(3) . . ?
C17 C18 C13 124.4(3) . . ?
O5 Ag1 O4 138.32(12) . . ?
O5 Ag1 O6 88.78(12) . . ?
O4 Ag1 O6 106.78(11) . . ?
O5 Ag1 O2 117.84(11) . . ?
O4 Ag1 O2 86.62(10) . . ?
O6 Ag1 O2 122.19(10) . . ?
C29 O4 C19 114.7(4) . . ?
C29 O4 Ag1 121.1(3) . . ?
C19 O4 Ag1 123.6(3) . . ?
O4 C19 C20 111.0(4) . . ?
O4 C19 H19A 109.4 . . ?
C20 C19 H19A 109.4 . . ?
O4 C19 H19B 109.4 . . ?
C20 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C21 C28 110.4(4) . . ?
O6 C21 H21A 109.6 . . ?
C28 C21 H21A 109.6 . . ?
O6 C21 H21B 109.6 . . ?
C28 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
O6 C22 C27 109.6(5) . . ?
O6 C22 H22A 109.7 . . ?
C27 C22 H22A 109.7 . . ?
O6 C22 H22B 109.7 . . ?
C27 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C24 O5 C25 114.2(4) . . ?
C24 O5 Ag1 124.9(3) . . ?
C25 O5 Ag1 120.7(3) . . ?
C23 C24 O5 111.6(6) . . ?
C23 C24 H24A 109.3 . . ?
O5 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
O5 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
O5 C25 C26 111.0(4) . . ?
O5 C25 H25A 109.4 . . ?
C26 C25 H25A 109.4 . . ?
O5 C25 H25B 109.4 . . ?
C26 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C21 O6 C22 111.9(4) . . ?
C21 O6 Ag1 126.6(3) . . ?
C22 O6 Ag1 121.5(3) . . ?
C21 C28 H28A 109.5 . . ?
C21 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C21 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O4 C29 C30 109.3(4) . . ?
O4 C29 H29A 109.8 . . ?
C30 C29 H29A 109.8 . . ?
O4 C29 H29B 109.8 . . ?
C30 C29 H29B 109.8 . . ?
H29A C29 H29B 108.3 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
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
O3 N1 O1 B1 -179.1(3) . . . . ?
O2 N1 O1 B1 1.6(4) . . . . ?
O3 N1 O2 Ag1 -8.3(4) . . . . ?
O1 N1 O2 Ag1 171.1(2) . . . . ?
N1 O1 B1 C7 63.5(3) . . . . ?
N1 O1 B1 C13 -64.5(3) . . . . ?
N1 O1 B1 C1 -176.5(2) . . . . ?
O1 B1 C1 C6 -134.1(3) . . . . ?
C7 B1 C1 C6 -20.0(5) . . . . ?
C13 B1 C1 C6 108.1(4) . . . . ?
O1 B1 C1 C2 54.1(4) . . . . ?
C7 B1 C1 C2 168.3(3) . . . . ?
C13 B1 C1 C2 -63.7(4) . . . . ?
C6 C1 C2 F1 -178.5(3) . . . . ?
B1 C1 C2 F1 -5.8(5) . . . . ?
C6 C1 C2 C3 -0.5(5) . . . . ?
B1 C1 C2 C3 172.2(3) . . . . ?
F1 C2 C3 F2 -1.9(5) . . . . ?
C1 C2 C3 F2 -179.9(3) . . . . ?
F1 C2 C3 C4 177.7(3) . . . . ?
C1 C2 C3 C4 -0.4(6) . . . . ?
F2 C3 C4 F3 2.3(6) . . . . ?
C2 C3 C4 F3 -177.3(3) . . . . ?
F2 C3 C4 C5 -179.0(3) . . . . ?
C2 C3 C4 C5 1.4(6) . . . . ?
F3 C4 C5 F4 -2.5(5) . . . . ?
C3 C4 C5 F4 178.9(3) . . . . ?
F3 C4 C5 C6 177.2(3) . . . . ?
C3 C4 C5 C6 -1.5(6) . . . . ?
C2 C1 C6 F5 178.7(3) . . . . ?
B1 C1 C6 F5 6.4(5) . . . . ?
C2 C1 C6 C5 0.4(5) . . . . ?
B1 C1 C6 C5 -171.8(3) . . . . ?
F4 C5 C6 F5 1.8(5) . . . . ?
C4 C5 C6 F5 -177.8(3) . . . . ?
F4 C5 C6 C1 -179.8(3) . . . . ?
C4 C5 C6 C1 0.6(6) . . . . ?
O1 B1 C7 C12 60.6(4) . . . . ?
C13 B1 C7 C12 -173.5(3) . . . . ?
C1 B1 C7 C12 -51.6(4) . . . . ?
O1 B1 C7 C8 -117.4(3) . . . . ?
C13 B1 C7 C8 8.5(5) . . . . ?
C1 B1 C7 C8 130.4(3) . . . . ?
C12 C7 C8 F6 -176.2(3) . . . . ?
B1 C7 C8 F6 1.9(5) . . . . ?
C12 C7 C8 C9 4.3(5) . . . . ?
B1 C7 C8 C9 -177.5(3) . . . . ?
F6 C8 C9 F7 -1.7(5) . . . . ?
C7 C8 C9 F7 177.8(3) . . . . ?
F6 C8 C9 C10 177.8(4) . . . . ?
C7 C8 C9 C10 -2.8(6) . . . . ?
F7 C9 C10 F8 -0.1(6) . . . . ?
C8 C9 C10 F8 -179.5(4) . . . . ?
F7 C9 C10 C11 179.2(4) . . . . ?
C8 C9 C10 C11 -0.2(6) . . . . ?
F8 C10 C11 F9 0.5(6) . . . . ?
C9 C10 C11 F9 -178.8(4) . . . . ?
F8 C10 C11 C12 -179.5(4) . . . . ?
C9 C10 C11 C12 1.2(6) . . . . ?
F9 C11 C12 F10 0.2(5) . . . . ?
C10 C11 C12 F10 -179.9(3) . . . . ?
F9 C11 C12 C7 -179.3(3) . . . . ?
C10 C11 C12 C7 0.7(6) . . . . ?
C8 C7 C12 F10 177.3(3) . . . . ?
B1 C7 C12 F10 -1.0(5) . . . . ?
C8 C7 C12 C11 -3.3(5) . . . . ?
B1 C7 C12 C11 178.4(3) . . . . ?
O1 B1 C13 C14 -5.9(5) . . . . ?
C7 B1 C13 C14 -128.3(3) . . . . ?
C1 B1 C13 C14 104.9(4) . . . . ?
O1 B1 C13 C18 179.3(3) . . . . ?
C7 B1 C13 C18 56.8(4) . . . . ?
C1 B1 C13 C18 -70.0(3) . . . . ?
C18 C13 C14 F11 176.6(3) . . . . ?
B1 C13 C14 F11 1.5(5) . . . . ?
C18 C13 C14 C15 -3.0(5) . . . . ?
B1 C13 C14 C15 -178.1(3) . . . . ?
F11 C14 C15 F12 0.0(5) . . . . ?
C13 C14 C15 F12 179.6(3) . . . . ?
F11 C14 C15 C16 -179.4(3) . . . . ?
C13 C14 C15 C16 0.3(6) . . . . ?
F12 C15 C16 F13 2.1(6) . . . . ?
C14 C15 C16 F13 -178.5(3) . . . . ?
F12 C15 C16 C17 -177.3(3) . . . . ?
C14 C15 C16 C17 2.1(6) . . . . ?
F13 C16 C17 F14 -0.7(5) . . . . ?
C15 C16 C17 F14 178.7(3) . . . . ?
F13 C16 C17 C18 179.2(3) . . . . ?
C15 C16 C17 C18 -1.4(5) . . . . ?
F14 C17 C18 F15 -0.9(5) . . . . ?
C16 C17 C18 F15 179.3(3) . . . . ?
F14 C17 C18 C13 178.2(3) . . . . ?
C16 C17 C18 C13 -1.6(5) . . . . ?
C14 C13 C18 F15 -177.2(3) . . . . ?
B1 C13 C18 F15 -1.7(4) . . . . ?
C14 C13 C18 C17 3.7(5) . . . . ?
B1 C13 C18 C17 179.2(3) . . . . ?
N1 O2 Ag1 O5 -38.3(2) . . . . ?
N1 O2 Ag1 O4 106.3(2) . . . . ?
N1 O2 Ag1 O6 -145.95(19) . . . . ?
O5 Ag1 O4 C29 16.1(4) . . . . ?
O6 Ag1 O4 C29 123.9(3) . . . . ?
O2 Ag1 O4 C29 -113.5(3) . . . . ?
O5 Ag1 O4 C19 -173.0(3) . . . . ?
O6 Ag1 O4 C19 -65.3(3) . . . . ?
O2 Ag1 O4 C19 57.4(3) . . . . ?
C29 O4 C19 C20 -168.4(4) . . . . ?
Ag1 O4 C19 C20 20.2(5) . . . . ?
O4 Ag1 O5 C24 -99.9(5) . . . . ?
O6 Ag1 O5 C24 145.9(5) . . . . ?
O2 Ag1 O5 C24 19.6(5) . . . . ?
O4 Ag1 O5 C25 75.2(4) . . . . ?
O6 Ag1 O5 C25 -39.1(3) . . . . ?
O2 Ag1 O5 C25 -165.3(3) . . . . ?
C25 O5 C24 C23 104.5(6) . . . . ?
Ag1 O5 C24 C23 -80.2(6) . . . . ?
C24 O5 C25 C26 87.2(6) . . . . ?
Ag1 O5 C25 C26 -88.4(5) . . . . ?
C28 C21 O6 C22 171.4(5) . . . . ?
C28 C21 O6 Ag1 -8.0(6) . . . . ?
C27 C22 O6 C21 173.2(5) . . . . ?
C27 C22 O6 Ag1 -7.3(7) . . . . ?
O5 Ag1 O6 C21 104.7(4) . . . . ?
O4 Ag1 O6 C21 -36.0(4) . . . . ?
O2 Ag1 O6 C21 -132.7(3) . . . . ?
O5 Ag1 O6 C22 -74.7(4) . . . . ?
O4 Ag1 O6 C22 144.6(3) . . . . ?
O2 Ag1 O6 C22 47.9(4) . . . . ?
C19 O4 C29 C30 -169.5(4) . . . . ?
Ag1 O4 C29 C30 2.2(5) . . . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 25.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 1.465
_refine_diff_density_min -1.322
_refine_diff_density_rms 0.085
#=============================================================================
data_kv57
_database_code_depnum_ccdc_archive 'CCDC 817747'
#TrackingRef '- boran-sauerstoff.cif'
_audit_author_name 'Voss, K.'
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H10 B F15 O'
_chemical_formula_sum 'C22 H10 B F15 O'
_chemical_formula_weight 586.11
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'
B B 0.0013 0.0007 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.381(3)
_cell_length_b 10.673(3)
_cell_length_c 10.849(3)
_cell_angle_alpha 65.507(17)
_cell_angle_beta 85.51(2)
_cell_angle_gamma 75.68(2)
_cell_volume 1059.5(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9892
_cell_measurement_theta_min 6.692
_cell_measurement_theta_max 65.130
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.66
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.27
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.837
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 580
_exptl_absorpt_coefficient_mu 0.202
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8781
_exptl_absorpt_correction_T_max 0.9474
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method 'phi and psi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 20497
_diffrn_reflns_av_R_equivalents 0.0366
_diffrn_reflns_av_sigmaI/netI 0.0281
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 3.79
_diffrn_reflns_theta_max 29.00
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full 29.00
_diffrn_measured_fraction_theta_full 0.992
_reflns_number_total 5582
_reflns_number_gt 4828
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex v2.0-2'
_computing_cell_refinement 'Bruker Apex v2.0-2'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups) or 0.99 \%A (methylene groups) and with
U~iso~(H) = 1.5 times U~eq~(C) (methyl groups) or with
U~iso~(H) = 1.2 times U~eq~(C) (methylene groups). Torsion
angles of all methyl groups were allowed to refine.
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^)+(0.0686P)^2^+0.1700P] 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 5582
_refine_ls_number_parameters 354
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0445
_refine_ls_R_factor_gt 0.0382
_refine_ls_wR_factor_ref 0.1143
_refine_ls_wR_factor_gt 0.1096
_refine_ls_goodness_of_fit_ref 1.089
_refine_ls_restrained_S_all 1.089
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.488
_refine_diff_density_min -0.356
_refine_diff_density_rms 0.083
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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
O O 0.80311(8) 0.24322(8) 0.10083(8) 0.02123(17) Uani 1 1 d . . .
B B 0.70204(12) 0.15322(12) 0.09401(13) 0.0185(2) Uani 1 1 d . . .
C1 C 0.76201(11) -0.01539(11) 0.19025(11) 0.0192(2) Uani 1 1 d . . .
C2 C 0.87284(11) -0.07748(12) 0.27689(12) 0.0230(2) Uani 1 1 d . . .
C3 C 0.90757(11) -0.21994(12) 0.36349(12) 0.0248(2) Uani 1 1 d . . .
C4 C 0.82779(12) -0.30770(11) 0.36945(12) 0.0243(2) Uani 1 1 d . . .
C5 C 0.71457(12) -0.25144(11) 0.28732(12) 0.0221(2) Uani 1 1 d . . .
C6 C 0.68439(11) -0.10907(11) 0.20113(11) 0.0199(2) Uani 1 1 d . . .
C7 C 0.56264(11) 0.19765(10) 0.16369(11) 0.0190(2) Uani 1 1 d . . .
C8 C 0.56184(11) 0.16775(11) 0.30164(12) 0.0217(2) Uani 1 1 d . . .
C9 C 0.44825(13) 0.18427(12) 0.37411(12) 0.0261(2) Uani 1 1 d . . .
C10 C 0.32608(12) 0.23076(13) 0.30890(13) 0.0279(3) Uani 1 1 d . . .
C11 C 0.32064(11) 0.26028(11) 0.17304(13) 0.0236(2) Uani 1 1 d . . .
C12 C 0.43641(11) 0.24450(11) 0.10337(11) 0.0206(2) Uani 1 1 d . . .
C13 C 0.69140(10) 0.19283(11) -0.06830(11) 0.0193(2) Uani 1 1 d . . .
C14 C 0.64723(11) 0.33420(11) -0.15843(12) 0.0216(2) Uani 1 1 d . . .
C15 C 0.63979(12) 0.38178(12) -0.29721(12) 0.0255(2) Uani 1 1 d . . .
C16 C 0.67672(12) 0.28497(13) -0.35486(12) 0.0263(2) Uani 1 1 d . . .
C17 C 0.72112(11) 0.14347(12) -0.27142(12) 0.0241(2) Uani 1 1 d . . .
C18 C 0.72881(11) 0.10091(11) -0.13226(12) 0.0213(2) Uani 1 1 d . . .
F1 F 0.95432(8) -0.00078(8) 0.28586(9) 0.03513(19) Uani 1 1 d . . .
F2 F 1.01599(8) -0.27122(8) 0.44500(9) 0.0374(2) Uani 1 1 d . . .
F3 F 0.85707(9) -0.44451(8) 0.45512(9) 0.0375(2) Uani 1 1 d . . .
F4 F 0.63463(8) -0.33521(8) 0.29515(8) 0.03188(18) Uani 1 1 d . . .
F5 F 0.57146(7) -0.05949(7) 0.12582(7) 0.02555(16) Uani 1 1 d . . .
F6 F 0.67794(7) 0.11969(8) 0.37218(7) 0.02810(17) Uani 1 1 d . . .
F7 F 0.45642(9) 0.15383(9) 0.50679(8) 0.0374(2) Uani 1 1 d . . .
F8 F 0.21371(8) 0.24759(11) 0.37541(9) 0.0445(2) Uani 1 1 d . . .
F9 F 0.20160(7) 0.30568(8) 0.10819(8) 0.03252(18) Uani 1 1 d . . .
F10 F 0.41826(7) 0.27548(8) -0.02823(7) 0.02787(16) Uani 1 1 d . . .
F11 F 0.60840(8) 0.43469(7) -0.10868(8) 0.02943(17) Uani 1 1 d . . .
F12 F 0.59539(9) 0.51979(8) -0.37651(8) 0.0374(2) Uani 1 1 d . . .
F13 F 0.66933(9) 0.32792(9) -0.48892(8) 0.03725(19) Uani 1 1 d . . .
F14 F 0.75710(8) 0.04776(8) -0.32491(8) 0.03396(18) Uani 1 1 d . . .
F15 F 0.77730(8) -0.03940(7) -0.06006(7) 0.02917(17) Uani 1 1 d . . .
C19 C 0.93388(12) 0.22370(13) 0.03876(14) 0.0271(2) Uani 1 1 d . . .
H19A H 0.9466 0.1414 0.0151 0.033 Uiso 1 1 calc R . .
H19B H 1.0039 0.2009 0.1067 0.033 Uiso 1 1 calc R . .
C20 C 0.77132(12) 0.36196(12) 0.14274(13) 0.0268(2) Uani 1 1 d . . .
H20A H 0.6791 0.3730 0.1752 0.032 Uiso 1 1 calc R . .
H20B H 0.7762 0.4506 0.0634 0.032 Uiso 1 1 calc R . .
C21 C 0.86481(15) 0.33950(17) 0.25315(16) 0.0385(3) Uani 1 1 d . . .
H21A H 0.8665 0.2476 0.3286 0.058 Uiso 1 1 calc R . .
H21B H 0.8344 0.4151 0.2851 0.058 Uiso 1 1 calc R . .
H21C H 0.9544 0.3411 0.2177 0.058 Uiso 1 1 calc R . .
C22 C 0.95214(15) 0.35006(16) -0.08627(15) 0.0378(3) Uani 1 1 d . . .
H22A H 0.8842 0.3728 -0.1550 0.057 Uiso 1 1 calc R . .
H22B H 1.0406 0.3283 -0.1219 0.057 Uiso 1 1 calc R . .
H22C H 0.9435 0.4314 -0.0633 0.057 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O 0.0189(4) 0.0219(4) 0.0272(4) -0.0139(3) 0.0037(3) -0.0064(3)
B 0.0172(5) 0.0184(5) 0.0202(6) -0.0083(4) 0.0001(4) -0.0039(4)
C1 0.0182(5) 0.0195(4) 0.0194(5) -0.0084(4) 0.0001(4) -0.0028(4)
C2 0.0195(5) 0.0231(5) 0.0267(6) -0.0104(4) -0.0022(4) -0.0043(4)
C3 0.0201(5) 0.0250(5) 0.0253(6) -0.0083(4) -0.0051(4) 0.0000(4)
C4 0.0260(6) 0.0184(5) 0.0229(6) -0.0054(4) -0.0010(4) -0.0010(4)
C5 0.0234(5) 0.0209(5) 0.0228(5) -0.0090(4) 0.0017(4) -0.0068(4)
C6 0.0179(5) 0.0216(5) 0.0194(5) -0.0084(4) -0.0012(4) -0.0025(4)
C7 0.0190(5) 0.0176(4) 0.0207(5) -0.0086(4) 0.0011(4) -0.0037(4)
C8 0.0219(5) 0.0213(5) 0.0220(5) -0.0091(4) 0.0007(4) -0.0047(4)
C9 0.0313(6) 0.0259(5) 0.0212(6) -0.0102(4) 0.0067(5) -0.0074(4)
C10 0.0235(6) 0.0291(5) 0.0321(7) -0.0149(5) 0.0118(5) -0.0071(4)
C11 0.0176(5) 0.0214(5) 0.0311(6) -0.0111(4) 0.0006(4) -0.0031(4)
C12 0.0215(5) 0.0196(4) 0.0210(5) -0.0094(4) 0.0006(4) -0.0037(4)
C13 0.0175(5) 0.0199(5) 0.0205(5) -0.0085(4) 0.0013(4) -0.0041(4)
C14 0.0217(5) 0.0206(5) 0.0231(5) -0.0102(4) 0.0010(4) -0.0040(4)
C15 0.0258(6) 0.0234(5) 0.0228(6) -0.0047(4) -0.0017(4) -0.0056(4)
C16 0.0254(6) 0.0343(6) 0.0191(5) -0.0096(5) 0.0008(4) -0.0095(5)
C17 0.0221(5) 0.0300(6) 0.0255(6) -0.0166(5) 0.0037(4) -0.0067(4)
C18 0.0190(5) 0.0213(5) 0.0232(5) -0.0096(4) 0.0019(4) -0.0035(4)
F1 0.0284(4) 0.0295(4) 0.0451(5) -0.0086(3) -0.0141(3) -0.0098(3)
F2 0.0285(4) 0.0315(4) 0.0419(5) -0.0057(3) -0.0178(3) 0.0001(3)
F3 0.0396(5) 0.0192(3) 0.0408(5) -0.0005(3) -0.0108(4) -0.0020(3)
F4 0.0352(4) 0.0252(3) 0.0348(4) -0.0073(3) -0.0039(3) -0.0138(3)
F5 0.0221(3) 0.0246(3) 0.0285(4) -0.0085(3) -0.0076(3) -0.0048(3)
F6 0.0256(4) 0.0354(4) 0.0224(4) -0.0120(3) -0.0032(3) -0.0043(3)
F7 0.0426(5) 0.0471(5) 0.0218(4) -0.0153(4) 0.0091(3) -0.0097(4)
F8 0.0277(4) 0.0633(6) 0.0419(5) -0.0254(4) 0.0171(4) -0.0082(4)
F9 0.0171(3) 0.0367(4) 0.0425(5) -0.0170(3) -0.0008(3) -0.0022(3)
F10 0.0223(4) 0.0383(4) 0.0232(4) -0.0147(3) -0.0027(3) -0.0027(3)
F11 0.0390(4) 0.0197(3) 0.0288(4) -0.0117(3) -0.0003(3) -0.0021(3)
F12 0.0509(5) 0.0241(3) 0.0261(4) -0.0013(3) -0.0059(4) -0.0032(3)
F13 0.0470(5) 0.0448(4) 0.0182(4) -0.0109(3) -0.0004(3) -0.0110(4)
F14 0.0412(5) 0.0382(4) 0.0307(4) -0.0242(3) 0.0048(3) -0.0069(3)
F15 0.0369(4) 0.0203(3) 0.0272(4) -0.0113(3) 0.0021(3) 0.0011(3)
C19 0.0195(5) 0.0312(6) 0.0359(7) -0.0186(5) 0.0067(5) -0.0082(4)
C20 0.0293(6) 0.0238(5) 0.0344(7) -0.0181(5) 0.0069(5) -0.0093(4)
C21 0.0396(8) 0.0505(8) 0.0426(8) -0.0311(7) 0.0073(6) -0.0208(6)
C22 0.0297(7) 0.0477(8) 0.0358(7) -0.0145(6) 0.0104(6) -0.0165(6)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
O C20 1.4728(13) . ?
O C19 1.4740(15) . ?
O B 1.6121(14) . ?
B C7 1.6361(17) . ?
B C13 1.6377(18) . ?
B C1 1.6450(16) . ?
C1 C2 1.3863(16) . ?
C1 C6 1.3961(15) . ?
C2 F1 1.3479(13) . ?
C2 C3 1.3863(16) . ?
C3 F2 1.3409(14) . ?
C3 C4 1.3758(17) . ?
C4 F3 1.3371(13) . ?
C4 C5 1.3809(17) . ?
C5 F4 1.3373(13) . ?
C5 C6 1.3834(15) . ?
C6 F5 1.3440(13) . ?
C7 C12 1.3907(16) . ?
C7 C8 1.3948(16) . ?
C8 F6 1.3470(14) . ?
C8 C9 1.3807(17) . ?
C9 F7 1.3426(15) . ?
C9 C10 1.3759(19) . ?
C10 F8 1.3362(14) . ?
C10 C11 1.3764(19) . ?
C11 F9 1.3468(14) . ?
C11 C12 1.3809(16) . ?
C12 F10 1.3428(14) . ?
C13 C18 1.3887(15) . ?
C13 C14 1.3956(15) . ?
C14 F11 1.3551(13) . ?
C14 C15 1.3767(17) . ?
C15 F12 1.3408(14) . ?
C15 C16 1.3814(17) . ?
C16 F13 1.3336(14) . ?
C16 C17 1.3785(18) . ?
C17 F14 1.3375(13) . ?
C17 C18 1.3872(17) . ?
C18 F15 1.3512(13) . ?
C19 C22 1.5047(19) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.504(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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
C20 O C19 114.58(8) . . ?
C20 O B 126.45(8) . . ?
C19 O B 118.14(8) . . ?
O B C7 108.99(8) . . ?
O B C13 102.92(8) . . ?
C7 B C13 115.55(9) . . ?
O B C1 109.09(9) . . ?
C7 B C1 104.81(9) . . ?
C13 B C1 115.32(9) . . ?
C2 C1 C6 113.66(10) . . ?
C2 C1 B 128.77(9) . . ?
C6 C1 B 117.06(9) . . ?
F1 C2 C1 121.62(10) . . ?
F1 C2 C3 114.37(10) . . ?
C1 C2 C3 123.99(10) . . ?
F2 C3 C4 119.94(10) . . ?
F2 C3 C2 120.16(10) . . ?
C4 C3 C2 119.86(11) . . ?
F3 C4 C3 120.95(11) . . ?
F3 C4 C5 120.19(10) . . ?
C3 C4 C5 118.84(10) . . ?
F4 C5 C4 119.20(10) . . ?
F4 C5 C6 121.32(10) . . ?
C4 C5 C6 119.46(10) . . ?
F5 C6 C5 116.86(10) . . ?
F5 C6 C1 118.97(9) . . ?
C5 C6 C1 124.16(10) . . ?
C12 C7 C8 113.78(10) . . ?
C12 C7 B 125.79(10) . . ?
C8 C7 B 119.67(10) . . ?
F6 C8 C9 116.00(10) . . ?
F6 C8 C7 119.54(10) . . ?
C9 C8 C7 124.46(11) . . ?
F7 C9 C10 120.26(11) . . ?
F7 C9 C8 120.63(12) . . ?
C10 C9 C8 119.10(11) . . ?
F8 C10 C9 121.01(12) . . ?
F8 C10 C11 119.96(12) . . ?
C9 C10 C11 119.03(11) . . ?
F9 C11 C10 119.55(11) . . ?
F9 C11 C12 120.18(11) . . ?
C10 C11 C12 120.26(11) . . ?
F10 C12 C11 114.74(10) . . ?
F10 C12 C7 121.89(10) . . ?
C11 C12 C7 123.36(11) . . ?
C18 C13 C14 113.24(10) . . ?
C18 C13 B 127.32(10) . . ?
C14 C13 B 119.34(9) . . ?
F11 C14 C15 116.06(10) . . ?
F11 C14 C13 119.03(10) . . ?
C15 C14 C13 124.92(10) . . ?
F12 C15 C14 121.05(11) . . ?
F12 C15 C16 119.77(11) . . ?
C14 C15 C16 119.18(11) . . ?
F13 C16 C17 120.70(11) . . ?
F13 C16 C15 120.47(11) . . ?
C17 C16 C15 118.83(11) . . ?
F14 C17 C16 119.90(11) . . ?
F14 C17 C18 120.23(11) . . ?
C16 C17 C18 119.87(10) . . ?
F15 C18 C17 115.15(10) . . ?
F15 C18 C13 120.90(10) . . ?
C17 C18 C13 123.95(10) . . ?
O C19 C22 114.49(11) . . ?
O C19 H19A 108.6 . . ?
C22 C19 H19A 108.6 . . ?
O C19 H19B 108.6 . . ?
C22 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
O C20 C21 112.06(11) . . ?
O C20 H20A 109.2 . . ?
C21 C20 H20A 109.2 . . ?
O C20 H20B 109.2 . . ?
C21 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
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
C20 O B C7 -8.77(14) . . . . ?
C19 O B C7 -177.73(9) . . . . ?
C20 O B C13 114.39(11) . . . . ?
C19 O B C13 -54.56(11) . . . . ?
C20 O B C1 -122.67(11) . . . . ?
C19 O B C1 68.37(12) . . . . ?
O B C1 C2 6.24(15) . . . . ?
C7 B C1 C2 -110.36(12) . . . . ?
C13 B C1 C2 121.43(12) . . . . ?
O B C1 C6 177.41(9) . . . . ?
C7 B C1 C6 60.82(12) . . . . ?
C13 B C1 C6 -67.40(13) . . . . ?
C6 C1 C2 F1 -175.87(11) . . . . ?
B C1 C2 F1 -4.45(19) . . . . ?
C6 C1 C2 C3 2.14(17) . . . . ?
B C1 C2 C3 173.56(11) . . . . ?
F1 C2 C3 F2 -1.26(17) . . . . ?
C1 C2 C3 F2 -179.40(11) . . . . ?
F1 C2 C3 C4 176.26(11) . . . . ?
C1 C2 C3 C4 -1.88(19) . . . . ?
F2 C3 C4 F3 -0.43(18) . . . . ?
C2 C3 C4 F3 -177.96(11) . . . . ?
F2 C3 C4 C5 178.11(11) . . . . ?
C2 C3 C4 C5 0.58(18) . . . . ?
F3 C4 C5 F4 0.33(17) . . . . ?
C3 C4 C5 F4 -178.22(11) . . . . ?
F3 C4 C5 C6 178.77(11) . . . . ?
C3 C4 C5 C6 0.21(17) . . . . ?
F4 C5 C6 F5 -0.15(16) . . . . ?
C4 C5 C6 F5 -178.55(10) . . . . ?
F4 C5 C6 C1 178.59(10) . . . . ?
C4 C5 C6 C1 0.19(18) . . . . ?
C2 C1 C6 F5 177.42(10) . . . . ?
B C1 C6 F5 4.92(15) . . . . ?
C2 C1 C6 C5 -1.29(17) . . . . ?
B C1 C6 C5 -173.79(10) . . . . ?
O B C7 C12 125.74(10) . . . . ?
C13 B C7 C12 10.48(14) . . . . ?
C1 B C7 C12 -117.60(11) . . . . ?
O B C7 C8 -64.95(12) . . . . ?
C13 B C7 C8 179.79(9) . . . . ?
C1 B C7 C8 51.72(12) . . . . ?
C12 C7 C8 F6 179.14(9) . . . . ?
B C7 C8 F6 8.61(14) . . . . ?
C12 C7 C8 C9 -1.06(15) . . . . ?
B C7 C8 C9 -171.60(10) . . . . ?
F6 C8 C9 F7 0.24(15) . . . . ?
C7 C8 C9 F7 -179.56(10) . . . . ?
F6 C8 C9 C10 -178.94(10) . . . . ?
C7 C8 C9 C10 1.26(17) . . . . ?
F7 C9 C10 F8 0.53(17) . . . . ?
C8 C9 C10 F8 179.71(11) . . . . ?
F7 C9 C10 C11 -179.56(10) . . . . ?
C8 C9 C10 C11 -0.38(17) . . . . ?
F8 C10 C11 F9 -0.17(16) . . . . ?
C9 C10 C11 F9 179.92(10) . . . . ?
F8 C10 C11 C12 179.34(10) . . . . ?
C9 C10 C11 C12 -0.57(17) . . . . ?
F9 C11 C12 F10 -0.96(14) . . . . ?
C10 C11 C12 F10 179.53(10) . . . . ?
F9 C11 C12 C7 -179.74(9) . . . . ?
C10 C11 C12 C7 0.75(16) . . . . ?
C8 C7 C12 F10 -178.65(9) . . . . ?
B C7 C12 F10 -8.79(16) . . . . ?
C8 C7 C12 C11 0.04(14) . . . . ?
B C7 C12 C11 169.90(10) . . . . ?
O B C13 C18 117.69(11) . . . . ?
C7 B C13 C18 -123.64(12) . . . . ?
C1 B C13 C18 -0.98(15) . . . . ?
O B C13 C14 -58.49(12) . . . . ?
C7 B C13 C14 60.18(13) . . . . ?
C1 B C13 C14 -177.16(9) . . . . ?
C18 C13 C14 F11 -179.68(10) . . . . ?
B C13 C14 F11 -2.99(15) . . . . ?
C18 C13 C14 C15 0.14(16) . . . . ?
B C13 C14 C15 176.83(11) . . . . ?
F11 C14 C15 F12 -0.53(17) . . . . ?
C13 C14 C15 F12 179.64(11) . . . . ?
F11 C14 C15 C16 -179.45(10) . . . . ?
C13 C14 C15 C16 0.73(18) . . . . ?
F12 C15 C16 F13 0.43(18) . . . . ?
C14 C15 C16 F13 179.36(11) . . . . ?
F12 C15 C16 C17 -179.50(11) . . . . ?
C14 C15 C16 C17 -0.57(18) . . . . ?
F13 C16 C17 F14 -0.10(17) . . . . ?
C15 C16 C17 F14 179.83(11) . . . . ?
F13 C16 C17 C18 179.65(10) . . . . ?
C15 C16 C17 C18 -0.42(17) . . . . ?
F14 C17 C18 F15 1.65(16) . . . . ?
C16 C17 C18 F15 -178.10(10) . . . . ?
F14 C17 C18 C13 -178.86(10) . . . . ?
C16 C17 C18 C13 1.39(18) . . . . ?
C14 C13 C18 F15 178.26(10) . . . . ?
B C13 C18 F15 1.88(17) . . . . ?
C14 C13 C18 C17 -1.20(16) . . . . ?
B C13 C18 C17 -177.58(10) . . . . ?
C20 O C19 C22 -58.99(14) . . . . ?
B O C19 C22 111.26(12) . . . . ?
C19 O C20 C21 -64.11(13) . . . . ?
B O C20 C21 126.59(11) . . . . ?
#=============================================================================
data_KV60
_database_code_depnum_ccdc_archive 'CCDC 817748'
#TrackingRef '- boran-sauerstoff.cif'
_audit_author_name 'Voss, K.'
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C26 H18 B F15 O3'
_chemical_formula_sum 'C26 H18 B F15 O3'
_chemical_formula_weight 674.21
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'
B B 0.0013 0.0007 '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'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
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 9.285(4)
_cell_length_b 30.031(9)
_cell_length_c 10.049(4)
_cell_angle_alpha 90.00
_cell_angle_beta 105.14(3)
_cell_angle_gamma 90.00
_cell_volume 2704.9(17)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 30910
_cell_measurement_theta_min 2.72
_cell_measurement_theta_max 61.00
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.53
_exptl_crystal_size_mid 0.31
_exptl_crystal_size_min 0.24
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.656
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1352
_exptl_absorpt_coefficient_mu 0.176
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9127
_exptl_absorpt_correction_T_max 0.9591
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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 Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and psi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 30910
_diffrn_reflns_av_R_equivalents 0.0346
_diffrn_reflns_av_sigmaI/netI 0.0341
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -42
_diffrn_reflns_limit_k_max 42
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 1.36
_diffrn_reflns_theta_max 30.50
_reflns_number_total 8102
_reflns_number_gt 5479
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex v2.0-2'
_computing_cell_refinement 'Bruker Apex v2.0-2'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a
riding model , with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_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^)+(0.1126P)^2^+0.2039P] 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 8102
_refine_ls_number_parameters 466
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0900
_refine_ls_R_factor_gt 0.0597
_refine_ls_wR_factor_ref 0.1884
_refine_ls_wR_factor_gt 0.1708
_refine_ls_goodness_of_fit_ref 1.079
_refine_ls_restrained_S_all 1.079
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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
O1 O 0.45598(14) 0.13615(4) 0.60728(13) 0.0284(3) Uani 1 1 d . . .
H1 H 0.436(4) 0.1182(13) 0.563(4) 0.093(13) Uiso 1 1 d . . .
H2 H 0.548(3) 0.1497(9) 0.621(3) 0.062(8) Uiso 1 1 d . . .
B1 B 0.4217(2) 0.13148(6) 0.74946(19) 0.0256(3) Uani 1 1 d . . .
C1 C 0.58080(18) 0.12099(5) 0.86055(17) 0.0275(3) Uani 1 1 d . . .
C2 C 0.6444(2) 0.14518(6) 0.97974(18) 0.0327(4) Uani 1 1 d . . .
C3 C 0.7875(2) 0.13729(7) 1.06212(19) 0.0401(4) Uani 1 1 d . . .
C4 C 0.8723(2) 0.10376(8) 1.0296(2) 0.0432(5) Uani 1 1 d . . .
C5 C 0.8135(2) 0.07826(7) 0.9139(2) 0.0407(4) Uani 1 1 d . . .
C6 C 0.6724(2) 0.08731(6) 0.83412(18) 0.0325(4) Uani 1 1 d . . .
C7 C 0.34829(18) 0.17855(5) 0.78200(18) 0.0290(3) Uani 1 1 d . . .
C8 C 0.2476(2) 0.18071(6) 0.86260(19) 0.0330(4) Uani 1 1 d . . .
C9 C 0.1842(2) 0.21988(7) 0.8924(2) 0.0422(5) Uani 1 1 d . . .
C10 C 0.2219(2) 0.25940(6) 0.8399(2) 0.0479(5) Uani 1 1 d . . .
C11 C 0.3227(2) 0.25945(6) 0.7623(2) 0.0444(5) Uani 1 1 d . . .
C12 C 0.3831(2) 0.21950(6) 0.7343(2) 0.0368(4) Uani 1 1 d . . .
C13 C 0.29566(18) 0.09201(5) 0.72608(17) 0.0274(3) Uani 1 1 d . . .
C14 C 0.3026(2) 0.05339(6) 0.8020(2) 0.0341(4) Uani 1 1 d . . .
C15 C 0.1880(3) 0.02201(6) 0.7771(2) 0.0445(5) Uani 1 1 d . . .
C16 C 0.0615(2) 0.02862(7) 0.6726(3) 0.0469(5) Uani 1 1 d . . .
C17 C 0.0485(2) 0.06646(7) 0.5939(2) 0.0417(5) Uani 1 1 d . . .
C18 C 0.16437(19) 0.09696(6) 0.6224(2) 0.0326(4) Uani 1 1 d . . .
F1 F 0.56918(14) 0.17812(4) 1.02299(13) 0.0487(3) Uani 1 1 d . . .
F2 F 0.84184(17) 0.16237(5) 1.17554(14) 0.0618(4) Uani 1 1 d . . .
F3 F 1.00947(14) 0.09584(6) 1.10882(16) 0.0645(4) Uani 1 1 d . . .
F4 F 0.89467(15) 0.04470(5) 0.88318(15) 0.0612(4) Uani 1 1 d . . .
F5 F 0.62121(14) 0.06070(4) 0.72320(11) 0.0437(3) Uani 1 1 d . . .
F6 F 0.20880(15) 0.14363(4) 0.92037(13) 0.0475(3) Uani 1 1 d . . .
F7 F 0.08552(16) 0.21914(5) 0.96993(16) 0.0620(4) Uani 1 1 d . . .
F8 F 0.15873(19) 0.29776(5) 0.86614(19) 0.0738(5) Uani 1 1 d . . .
F9 F 0.36137(19) 0.29785(4) 0.71181(18) 0.0665(4) Uani 1 1 d . . .
F10 F 0.48564(16) 0.22239(4) 0.66058(16) 0.0537(3) Uani 1 1 d . . .
F11 F 0.42227(14) 0.04448(4) 0.90763(12) 0.0453(3) Uani 1 1 d . . .
F12 F 0.2015(2) -0.01451(4) 0.85696(18) 0.0678(5) Uani 1 1 d . . .
F13 F -0.04874(17) -0.00148(5) 0.64781(19) 0.0700(5) Uani 1 1 d . . .
F14 F -0.07474(14) 0.07338(5) 0.49144(16) 0.0606(4) Uani 1 1 d . . .
F15 F 0.14260(12) 0.13347(4) 0.54200(13) 0.0423(3) Uani 1 1 d . . .
C23A C 0.2880(18) 0.0841(4) 0.3116(17) 0.044(4) Uani 0.314(13) 1 d P A 1
H23A H 0.2450 0.1134 0.3254 0.053 Uiso 0.314(13) 1 calc PR A 1
H23B H 0.2074 0.0618 0.2844 0.053 Uiso 0.314(13) 1 calc PR A 1
C24A C 0.3818(12) 0.0867(4) 0.2098(8) 0.046(3) Uani 0.314(13) 1 d P A 1
H24A H 0.3203 0.0757 0.1200 0.055 Uiso 0.314(13) 1 calc PR A 1
H24B H 0.4030 0.1185 0.1974 0.055 Uiso 0.314(13) 1 calc PR A 1
C25A C 0.528(2) 0.0621(7) 0.242(2) 0.045(3) Uani 0.314(13) 1 d P A 1
H25A H 0.6113 0.0809 0.2303 0.054 Uiso 0.314(13) 1 calc PR A 1
H25B H 0.5225 0.0343 0.1875 0.054 Uiso 0.314(13) 1 calc PR A 1
C26A C 0.5341(19) 0.0529(5) 0.4007(10) 0.030(3) Uani 0.314(13) 1 d P A 1
H26A H 0.5410 0.0204 0.4185 0.036 Uiso 0.314(13) 1 calc PR A 1
H26B H 0.6244 0.0671 0.4602 0.036 Uiso 0.314(13) 1 calc PR A 1
O3A O 0.4058(19) 0.0700(3) 0.4342(15) 0.0209(17) Uani 0.314(13) 1 d P A 1
C23B C 0.2985(7) 0.0782(3) 0.3198(8) 0.050(2) Uani 0.686(13) 1 d P A 2
H23C H 0.2698 0.1100 0.3093 0.060 Uiso 0.686(13) 1 calc PR A 2
H23D H 0.2115 0.0610 0.3311 0.060 Uiso 0.686(13) 1 calc PR A 2
C24B C 0.3394(5) 0.0630(2) 0.1962(4) 0.0531(14) Uani 0.686(13) 1 d P A 2
H24C H 0.3033 0.0324 0.1696 0.064 Uiso 0.686(13) 1 calc PR A 2
H24D H 0.3026 0.0834 0.1172 0.064 Uiso 0.686(13) 1 calc PR A 2
C25B C 0.5013(12) 0.0647(5) 0.2487(14) 0.081(4) Uani 0.686(13) 1 d P A 2
H25C H 0.5462 0.0420 0.2004 0.097 Uiso 0.686(13) 1 calc PR A 2
H25D H 0.5369 0.0943 0.2275 0.097 Uiso 0.686(13) 1 calc PR A 2
C26B C 0.5510(12) 0.0571(4) 0.3935(9) 0.062(3) Uani 0.686(13) 1 d P A 2
H26C H 0.6419 0.0746 0.4355 0.075 Uiso 0.686(13) 1 calc PR A 2
H26D H 0.5714 0.0251 0.4143 0.075 Uiso 0.686(13) 1 calc PR A 2
O3B O 0.4233(11) 0.0726(2) 0.4422(9) 0.049(2) Uani 0.686(13) 1 d P A 2
C19 C 0.8290(2) 0.18180(8) 0.6811(2) 0.0478(5) Uani 1 1 d . . .
C20 C 0.8754(4) 0.22014(10) 0.6085(3) 0.0755(9) Uani 1 1 d . . .
H20A H 0.8668 0.2483 0.6569 0.091 Uiso 1 1 calc R . .
H20B H 0.9801 0.2165 0.6043 0.091 Uiso 1 1 calc R . .
C21 C 0.7735(4) 0.22040(10) 0.4681(3) 0.0748(9) Uani 1 1 d . . .
H21A H 0.8283 0.2276 0.3985 0.090 Uiso 1 1 calc R . .
H21B H 0.6926 0.2425 0.4610 0.090 Uiso 1 1 calc R . .
C22 C 0.7123(3) 0.17444(10) 0.4481(2) 0.0620(7) Uani 1 1 d . . .
H22A H 0.6089 0.1747 0.3883 0.074 Uiso 1 1 calc R . .
H22B H 0.7743 0.1554 0.4047 0.074 Uiso 1 1 calc R . .
O2 O 0.71504(16) 0.15821(5) 0.58289(15) 0.0437(3) Uani 1 1 d . . .
H19A H 0.909(3) 0.1597(9) 0.716(3) 0.052 Uiso 1 1 d . . .
H19B H 0.792(3) 0.1858(9) 0.771(3) 0.052 Uiso 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
O1 0.0281(6) 0.0328(6) 0.0249(6) 0.0000(5) 0.0081(5) -0.0043(5)
B1 0.0279(8) 0.0257(7) 0.0247(8) -0.0014(6) 0.0097(7) 0.0001(6)
C1 0.0301(8) 0.0297(7) 0.0241(7) 0.0010(6) 0.0095(6) 0.0004(6)
C2 0.0344(9) 0.0358(8) 0.0273(8) -0.0019(7) 0.0072(7) 0.0004(7)
C3 0.0372(10) 0.0509(11) 0.0280(9) 0.0002(8) 0.0008(7) -0.0051(8)
C4 0.0287(9) 0.0649(13) 0.0332(10) 0.0131(9) 0.0033(7) 0.0036(8)
C5 0.0355(9) 0.0536(11) 0.0363(10) 0.0099(8) 0.0154(8) 0.0152(8)
C6 0.0338(9) 0.0397(9) 0.0255(8) 0.0014(7) 0.0105(7) 0.0064(7)
C7 0.0279(8) 0.0253(7) 0.0318(8) -0.0029(6) 0.0044(6) 0.0016(6)
C8 0.0346(9) 0.0299(8) 0.0340(9) -0.0057(7) 0.0083(7) 0.0050(6)
C9 0.0375(10) 0.0433(10) 0.0440(11) -0.0159(8) 0.0073(8) 0.0097(8)
C10 0.0493(11) 0.0301(9) 0.0550(13) -0.0167(8) -0.0030(9) 0.0129(8)
C11 0.0488(11) 0.0239(8) 0.0528(12) -0.0046(8) -0.0002(9) 0.0004(7)
C12 0.0376(9) 0.0278(8) 0.0432(10) -0.0034(7) 0.0074(8) -0.0022(7)
C13 0.0300(8) 0.0258(7) 0.0313(8) -0.0042(6) 0.0165(6) -0.0011(6)
C14 0.0429(10) 0.0294(7) 0.0371(10) -0.0017(7) 0.0233(8) 0.0004(7)
C15 0.0614(13) 0.0262(8) 0.0607(13) -0.0041(8) 0.0421(11) -0.0064(8)
C16 0.0474(11) 0.0388(10) 0.0659(14) -0.0234(9) 0.0353(11) -0.0192(8)
C17 0.0296(9) 0.0459(10) 0.0531(12) -0.0203(9) 0.0172(8) -0.0088(7)
C18 0.0280(8) 0.0334(8) 0.0394(10) -0.0061(7) 0.0137(7) -0.0026(6)
F1 0.0525(7) 0.0471(7) 0.0406(7) -0.0178(5) 0.0017(5) 0.0100(5)
F2 0.0586(8) 0.0725(9) 0.0406(7) -0.0126(6) -0.0113(6) -0.0059(7)
F3 0.0324(6) 0.0967(11) 0.0549(8) 0.0123(8) -0.0055(6) 0.0108(7)
F4 0.0506(8) 0.0823(10) 0.0530(8) 0.0038(7) 0.0179(6) 0.0377(7)
F5 0.0502(7) 0.0460(6) 0.0337(6) -0.0085(5) 0.0089(5) 0.0157(5)
F6 0.0626(8) 0.0409(6) 0.0508(7) -0.0011(5) 0.0362(6) 0.0041(5)
F7 0.0575(8) 0.0662(9) 0.0701(10) -0.0237(7) 0.0304(7) 0.0129(7)
F8 0.0791(10) 0.0397(7) 0.0971(12) -0.0248(7) 0.0133(9) 0.0229(7)
F9 0.0833(11) 0.0238(5) 0.0870(11) 0.0005(6) 0.0128(8) -0.0047(6)
F10 0.0597(8) 0.0344(6) 0.0758(10) 0.0023(6) 0.0331(7) -0.0111(5)
F11 0.0597(8) 0.0388(6) 0.0413(7) 0.0129(5) 0.0199(6) 0.0059(5)
F12 0.0984(12) 0.0325(6) 0.0916(12) 0.0096(6) 0.0591(10) -0.0085(7)
F13 0.0673(9) 0.0546(8) 0.1045(12) -0.0360(8) 0.0515(9) -0.0379(7)
F14 0.0307(6) 0.0716(9) 0.0752(10) -0.0231(8) 0.0058(6) -0.0105(6)
F15 0.0326(6) 0.0441(6) 0.0461(7) 0.0056(5) 0.0030(5) 0.0008(4)
C23A 0.067(8) 0.023(3) 0.027(5) -0.003(3) -0.015(4) 0.010(3)
C24A 0.061(5) 0.047(5) 0.028(3) 0.000(3) 0.007(3) 0.013(4)
C25A 0.029(5) 0.080(7) 0.033(5) -0.017(4) 0.023(4) 0.004(5)
C26A 0.038(6) 0.043(5) 0.006(3) 0.003(3) 0.000(3) 0.014(4)
O3A 0.022(4) 0.023(3) 0.018(3) -0.005(2) 0.006(3) -0.003(2)
C23B 0.0230(19) 0.092(5) 0.036(3) -0.009(3) 0.0087(19) -0.010(2)
C24B 0.055(2) 0.068(3) 0.0325(17) -0.0141(18) 0.0032(14) 0.011(2)
C25B 0.053(5) 0.154(7) 0.044(3) -0.011(3) 0.029(3) 0.030(4)
C26B 0.042(3) 0.073(5) 0.077(5) -0.019(3) 0.024(3) 0.006(3)
O3B 0.034(3) 0.076(4) 0.035(2) -0.0186(19) 0.0050(16) -0.0131(18)
C19 0.0356(10) 0.0562(12) 0.0491(13) 0.0060(10) 0.0067(9) -0.0141(9)
C20 0.093(2) 0.0671(16) 0.0566(16) 0.0091(13) 0.0020(15) -0.0455(16)
C21 0.089(2) 0.0686(17) 0.0590(17) 0.0234(14) 0.0046(15) -0.0185(15)
C22 0.0693(16) 0.0812(18) 0.0374(12) -0.0002(11) 0.0172(11) -0.0248(14)
O2 0.0431(8) 0.0526(8) 0.0400(8) -0.0061(6) 0.0189(6) -0.0175(6)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
O1 B1 1.549(2) . ?
O1 H1 0.70(4) . ?
O1 H2 0.92(3) . ?
B1 C1 1.633(3) . ?
B1 C7 1.639(2) . ?
B1 C13 1.639(2) . ?
C1 C6 1.391(2) . ?
C1 C2 1.393(2) . ?
C2 F1 1.347(2) . ?
C2 C3 1.390(3) . ?
C3 F2 1.349(2) . ?
C3 C4 1.369(3) . ?
C4 F3 1.335(2) . ?
C4 C5 1.380(3) . ?
C5 F4 1.342(2) . ?
C5 C6 1.373(3) . ?
C6 F5 1.353(2) . ?
C7 C12 1.388(2) . ?
C7 C8 1.389(3) . ?
C8 F6 1.348(2) . ?
C8 C9 1.383(2) . ?
C9 F7 1.349(3) . ?
C9 C10 1.381(3) . ?
C10 F8 1.350(2) . ?
C10 C11 1.366(3) . ?
C11 F9 1.346(2) . ?
C11 C12 1.384(3) . ?
C12 F10 1.353(2) . ?
C13 C14 1.380(2) . ?
C13 C18 1.389(3) . ?
C14 F11 1.348(2) . ?
C14 C15 1.394(3) . ?
C15 F12 1.346(2) . ?
C15 C16 1.370(4) . ?
C16 F13 1.340(2) . ?
C16 C17 1.372(3) . ?
C17 F14 1.340(3) . ?
C17 C18 1.385(2) . ?
C18 F15 1.346(2) . ?
C23A O3A 1.48(2) . ?
C23A C24A 1.508(19) . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C24A C25A 1.50(2) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
C25A C26A 1.61(3) . ?
C25A H25A 0.9900 . ?
C25A H25B 0.9900 . ?
C26A O3A 1.42(2) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
C23B O3B 1.463(12) . ?
C23B C24B 1.464(8) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C24B C25B 1.458(12) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C25B C26B 1.426(16) . ?
C25B H25C 0.9900 . ?
C25B H25D 0.9900 . ?
C26B O3B 1.471(14) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
C19 O2 1.432(3) . ?
C19 C20 1.486(3) . ?
C19 H19A 0.99(3) . ?
C19 H19B 1.05(3) . ?
C20 C21 1.480(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.486(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 O2 1.434(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
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
B1 O1 H1 116(3) . . ?
B1 O1 H2 108.1(18) . . ?
H1 O1 H2 121(3) . . ?
O1 B1 C1 106.31(13) . . ?
O1 B1 C7 107.59(13) . . ?
C1 B1 C7 112.28(13) . . ?
O1 B1 C13 104.14(13) . . ?
C1 B1 C13 116.30(13) . . ?
C7 B1 C13 109.50(13) . . ?
C6 C1 C2 113.59(16) . . ?
C6 C1 B1 119.92(15) . . ?
C2 C1 B1 126.28(15) . . ?
F1 C2 C3 115.38(16) . . ?
F1 C2 C1 121.41(16) . . ?
C3 C2 C1 123.21(17) . . ?
F2 C3 C4 120.03(18) . . ?
F2 C3 C2 119.76(19) . . ?
C4 C3 C2 120.21(18) . . ?
F3 C4 C3 120.5(2) . . ?
F3 C4 C5 120.6(2) . . ?
C3 C4 C5 118.90(17) . . ?
F4 C5 C6 121.44(19) . . ?
F4 C5 C4 119.24(18) . . ?
C6 C5 C4 119.31(18) . . ?
F5 C6 C5 116.15(16) . . ?
F5 C6 C1 119.08(16) . . ?
C5 C6 C1 124.76(17) . . ?
C12 C7 C8 114.38(15) . . ?
C12 C7 B1 123.27(15) . . ?
C8 C7 B1 122.34(15) . . ?
F6 C8 C9 115.63(17) . . ?
F6 C8 C7 120.60(14) . . ?
C9 C8 C7 123.75(18) . . ?
F7 C9 C10 120.88(17) . . ?
F7 C9 C8 120.2(2) . . ?
C10 C9 C8 118.92(19) . . ?
F8 C10 C11 120.5(2) . . ?
F8 C10 C9 119.5(2) . . ?
C11 C10 C9 119.94(17) . . ?
F9 C11 C10 120.43(18) . . ?
F9 C11 C12 120.2(2) . . ?
C10 C11 C12 119.33(19) . . ?
F10 C12 C11 115.87(17) . . ?
F10 C12 C7 120.42(16) . . ?
C11 C12 C7 123.66(19) . . ?
C14 C13 C18 114.18(16) . . ?
C14 C13 B1 126.86(16) . . ?
C18 C13 B1 118.94(14) . . ?
F11 C14 C13 120.81(16) . . ?
F11 C14 C15 116.13(17) . . ?
C13 C14 C15 123.05(19) . . ?
F12 C15 C16 120.19(18) . . ?
F12 C15 C14 119.7(2) . . ?
C16 C15 C14 120.07(19) . . ?
F13 C16 C15 120.4(2) . . ?
F13 C16 C17 120.2(2) . . ?
C15 C16 C17 119.41(17) . . ?
F14 C17 C16 120.06(18) . . ?
F14 C17 C18 121.2(2) . . ?
C16 C17 C18 118.8(2) . . ?
F15 C18 C17 115.31(18) . . ?
F15 C18 C13 120.15(14) . . ?
C17 C18 C13 124.53(18) . . ?
O3A C23A C24A 98.5(11) . . ?
O3A C23A H23A 112.1 . . ?
C24A C23A H23A 112.1 . . ?
O3A C23A H23B 112.1 . . ?
C24A C23A H23B 112.1 . . ?
H23A C23A H23B 109.7 . . ?
C25A C24A C23A 118.6(11) . . ?
C25A C24A H24A 107.7 . . ?
C23A C24A H24A 107.7 . . ?
C25A C24A H24B 107.7 . . ?
C23A C24A H24B 107.7 . . ?
H24A C24A H24B 107.1 . . ?
C24A C25A C26A 95.4(12) . . ?
C24A C25A H25A 112.7 . . ?
C26A C25A H25A 112.7 . . ?
C24A C25A H25B 112.7 . . ?
C26A C25A H25B 112.7 . . ?
H25A C25A H25B 110.2 . . ?
O3A C26A C25A 111.0(12) . . ?
O3A C26A H26A 109.4 . . ?
C25A C26A H26A 109.4 . . ?
O3A C26A H26B 109.4 . . ?
C25A C26A H26B 109.4 . . ?
H26A C26A H26B 108.0 . . ?
C26A O3A C23A 113.0(12) . . ?
O3B C23B C24B 110.7(5) . . ?
O3B C23B H23C 109.5 . . ?
C24B C23B H23C 109.5 . . ?
O3B C23B H23D 109.5 . . ?
C24B C23B H23D 109.5 . . ?
H23C C23B H23D 108.1 . . ?
C25B C24B C23B 98.8(6) . . ?
C25B C24B H24C 112.0 . . ?
C23B C24B H24C 112.0 . . ?
C25B C24B H24D 112.0 . . ?
C23B C24B H24D 112.0 . . ?
H24C C24B H24D 109.7 . . ?
C26B C25B C24B 113.1(9) . . ?
C26B C25B H25C 109.0 . . ?
C24B C25B H25C 109.0 . . ?
C26B C25B H25D 109.0 . . ?
C24B C25B H25D 109.0 . . ?
H25C C25B H25D 107.8 . . ?
C25B C26B O3B 102.5(8) . . ?
C25B C26B H26C 111.3 . . ?
O3B C26B H26C 111.3 . . ?
C25B C26B H26D 111.3 . . ?
O3B C26B H26D 111.3 . . ?
H26C C26B H26D 109.2 . . ?
C23B O3B C26B 106.7(7) . . ?
O2 C19 C20 107.57(19) . . ?
O2 C19 H19A 105.3(16) . . ?
C20 C19 H19A 113.8(15) . . ?
O2 C19 H19B 107.4(14) . . ?
C20 C19 H19B 122.2(14) . . ?
H19A C19 H19B 99(2) . . ?
C21 C20 C19 106.1(2) . . ?
C21 C20 H20A 110.5 . . ?
C19 C20 H20A 110.5 . . ?
C21 C20 H20B 110.5 . . ?
C19 C20 H20B 110.5 . . ?
H20A C20 H20B 108.7 . . ?
C20 C21 C22 104.5(2) . . ?
C20 C21 H21A 110.8 . . ?
C22 C21 H21A 110.8 . . ?
C20 C21 H21B 110.8 . . ?
C22 C21 H21B 110.8 . . ?
H21A C21 H21B 108.9 . . ?
O2 C22 C21 106.0(2) . . ?
O2 C22 H22A 110.5 . . ?
C21 C22 H22A 110.5 . . ?
O2 C22 H22B 110.5 . . ?
C21 C22 H22B 110.5 . . ?
H22A C22 H22B 108.7 . . ?
C19 O2 C22 108.11(16) . . ?
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
O1 B1 C1 C6 -50.10(19) . . . . ?
C7 B1 C1 C6 -167.51(15) . . . . ?
C13 B1 C1 C6 65.3(2) . . . . ?
O1 B1 C1 C2 124.33(17) . . . . ?
C7 B1 C1 C2 6.9(2) . . . . ?
C13 B1 C1 C2 -120.29(18) . . . . ?
C6 C1 C2 F1 -177.92(16) . . . . ?
B1 C1 C2 F1 7.3(3) . . . . ?
C6 C1 C2 C3 1.8(3) . . . . ?
B1 C1 C2 C3 -172.90(17) . . . . ?
F1 C2 C3 F2 -0.7(3) . . . . ?
C1 C2 C3 F2 179.49(17) . . . . ?
F1 C2 C3 C4 178.27(18) . . . . ?
C1 C2 C3 C4 -1.5(3) . . . . ?
F2 C3 C4 F3 -0.6(3) . . . . ?
C2 C3 C4 F3 -179.60(18) . . . . ?
F2 C3 C4 C5 179.29(19) . . . . ?
C2 C3 C4 C5 0.3(3) . . . . ?
F3 C4 C5 F4 1.4(3) . . . . ?
C3 C4 C5 F4 -178.49(18) . . . . ?
F3 C4 C5 C6 -179.71(18) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
F4 C5 C6 F5 -0.4(3) . . . . ?
C4 C5 C6 F5 -179.27(17) . . . . ?
F4 C5 C6 C1 178.93(17) . . . . ?
C4 C5 C6 C1 0.0(3) . . . . ?
C2 C1 C6 F5 178.17(15) . . . . ?
B1 C1 C6 F5 -6.7(2) . . . . ?
C2 C1 C6 C5 -1.1(3) . . . . ?
B1 C1 C6 C5 173.98(17) . . . . ?
O1 B1 C7 C12 -30.5(2) . . . . ?
C1 B1 C7 C12 86.2(2) . . . . ?
C13 B1 C7 C12 -143.07(17) . . . . ?
O1 B1 C7 C8 150.87(16) . . . . ?
C1 B1 C7 C8 -92.49(19) . . . . ?
C13 B1 C7 C8 38.3(2) . . . . ?
C12 C7 C8 F6 -177.22(16) . . . . ?
B1 C7 C8 F6 1.5(3) . . . . ?
C12 C7 C8 C9 1.0(3) . . . . ?
B1 C7 C8 C9 179.71(17) . . . . ?
F6 C8 C9 F7 -2.7(3) . . . . ?
C7 C8 C9 F7 179.01(17) . . . . ?
F6 C8 C9 C10 178.28(18) . . . . ?
C7 C8 C9 C10 0.0(3) . . . . ?
F7 C9 C10 F8 -0.2(3) . . . . ?
C8 C9 C10 F8 178.78(18) . . . . ?
F7 C9 C10 C11 179.67(18) . . . . ?
C8 C9 C10 C11 -1.4(3) . . . . ?
F8 C10 C11 F9 0.6(3) . . . . ?
C9 C10 C11 F9 -179.28(19) . . . . ?
F8 C10 C11 C12 -178.52(18) . . . . ?
C9 C10 C11 C12 1.6(3) . . . . ?
F9 C11 C12 F10 2.9(3) . . . . ?
C10 C11 C12 F10 -177.96(18) . . . . ?
F9 C11 C12 C7 -179.68(18) . . . . ?
C10 C11 C12 C7 -0.6(3) . . . . ?
C8 C7 C12 F10 176.58(16) . . . . ?
B1 C7 C12 F10 -2.2(3) . . . . ?
C8 C7 C12 C11 -0.7(3) . . . . ?
B1 C7 C12 C11 -179.42(17) . . . . ?
O1 B1 C13 C14 125.25(17) . . . . ?
C1 B1 C13 C14 8.7(2) . . . . ?
C7 B1 C13 C14 -119.92(17) . . . . ?
O1 B1 C13 C18 -56.54(18) . . . . ?
C1 B1 C13 C18 -173.13(14) . . . . ?
C7 B1 C13 C18 58.29(19) . . . . ?
C18 C13 C14 F11 -178.78(14) . . . . ?
B1 C13 C14 F11 -0.5(2) . . . . ?
C18 C13 C14 C15 0.0(2) . . . . ?
B1 C13 C14 C15 178.26(16) . . . . ?
F11 C14 C15 F12 0.0(2) . . . . ?
C13 C14 C15 F12 -178.79(16) . . . . ?
F11 C14 C15 C16 179.29(17) . . . . ?
C13 C14 C15 C16 0.5(3) . . . . ?
F12 C15 C16 F13 -1.0(3) . . . . ?
C14 C15 C16 F13 179.75(16) . . . . ?
F12 C15 C16 C17 178.76(17) . . . . ?
C14 C15 C16 C17 -0.5(3) . . . . ?
F13 C16 C17 F14 -0.2(3) . . . . ?
C15 C16 C17 F14 -179.93(17) . . . . ?
F13 C16 C17 C18 179.84(16) . . . . ?
C15 C16 C17 C18 0.1(3) . . . . ?
F14 C17 C18 F15 0.8(3) . . . . ?
C16 C17 C18 F15 -179.20(16) . . . . ?
F14 C17 C18 C13 -179.58(16) . . . . ?
C16 C17 C18 C13 0.4(3) . . . . ?
C14 C13 C18 F15 179.15(15) . . . . ?
B1 C13 C18 F15 0.7(2) . . . . ?
C14 C13 C18 C17 -0.4(2) . . . . ?
B1 C13 C18 C17 -178.85(16) . . . . ?
O3A C23A C24A C25A 19.6(15) . . . . ?
C23A C24A C25A C26A -13.6(16) . . . . ?
C24A C25A C26A O3A 1.5(16) . . . . ?
C25A C26A O3A C23A 10.5(18) . . . . ?
C24A C23A O3A C26A -17.0(15) . . . . ?
O3B C23B C24B C25B -19.9(9) . . . . ?
C23B C24B C25B C26B 29.7(12) . . . . ?
C24B C25B C26B O3B -27.5(13) . . . . ?
C24B C23B O3B C26B 5.1(9) . . . . ?
C25B C26B O3B C23B 12.6(11) . . . . ?
O2 C19 C20 C21 5.5(4) . . . . ?
C19 C20 C21 C22 -20.3(4) . . . . ?
C20 C21 C22 O2 28.0(4) . . . . ?
C20 C19 O2 C22 12.3(3) . . . . ?
C21 C22 O2 C19 -25.3(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full 30.50
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max 0.674
_refine_diff_density_min -0.410
_refine_diff_density_rms 0.084
#=============================================================================
data_KV62
_database_code_depnum_ccdc_archive 'CCDC 817749'
#TrackingRef '- boran-sauerstoff.cif'
_audit_author_name 'Villinger, A.'
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
;
C36 B2 F30 O4 S 2-, C24 H48 K2 O12 2+, C1.28 H2.56 Cl2.56
;
_chemical_formula_sum 'C61.28 H50.56 B2 Cl2.56 F30 K2 O16 S'
_chemical_formula_weight 1835.45
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'
B B 0.0013 0.0007 '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'
K K 0.2009 0.2494 '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'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 14.309(5)
_cell_length_b 22.551(9)
_cell_length_c 24.200(8)
_cell_angle_alpha 102.53(3)
_cell_angle_beta 98.78(3)
_cell_angle_gamma 100.40(3)
_cell_volume 7347(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9992
_cell_measurement_theta_min 6.552
_cell_measurement_theta_max 48.640
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.41
_exptl_crystal_size_min 0.19
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.659
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3695
_exptl_absorpt_coefficient_mu 0.391
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8530
_exptl_absorpt_correction_T_max 0.9294
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and psi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 113434
_diffrn_reflns_av_R_equivalents 0.0414
_diffrn_reflns_av_sigmaI/netI 0.0428
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 0.88
_diffrn_reflns_theta_max 24.51
_reflns_number_total 24030
_reflns_number_gt 16214
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex v2.0-2'
_computing_cell_refinement 'Bruker Apex v2.0-2'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a
riding model , with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_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^)+(0.0810P)^2^+0.0000P] 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 24030
_refine_ls_number_parameters 2090
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0850
_refine_ls_R_factor_gt 0.0480
_refine_ls_wR_factor_ref 0.1384
_refine_ls_wR_factor_gt 0.1229
_refine_ls_goodness_of_fit_ref 1.092
_refine_ls_restrained_S_all 1.092
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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
S1 S 0.23393(5) 0.23616(3) 0.89368(3) 0.02759(17) Uani 1 1 d . . .
O1 O 0.30813(13) 0.19773(8) 0.90593(8) 0.0289(4) Uani 1 1 d . . .
O2 O 0.21054(13) 0.26122(8) 0.95289(8) 0.0270(4) Uani 1 1 d . . .
O3 O 0.28288(15) 0.28662(8) 0.87458(8) 0.0335(5) Uani 1 1 d . . .
O4 O 0.14695(14) 0.19825(9) 0.85676(8) 0.0348(5) Uani 1 1 d . . .
B1 B 0.3021(2) 0.13124(15) 0.91155(14) 0.0285(8) Uani 1 1 d . . .
C1 C 0.4085(2) 0.11626(13) 0.90318(12) 0.0305(7) Uani 1 1 d . . .
C2 C 0.4860(2) 0.15575(14) 0.89442(12) 0.0348(7) Uani 1 1 d . . .
C3 C 0.5670(2) 0.13720(17) 0.87927(13) 0.0448(8) Uani 1 1 d . . .
C4 C 0.5749(3) 0.07697(18) 0.87432(14) 0.0485(9) Uani 1 1 d . . .
C5 C 0.5026(3) 0.03651(16) 0.88595(14) 0.0464(9) Uani 1 1 d . . .
C6 C 0.4224(2) 0.05652(14) 0.89972(13) 0.0379(8) Uani 1 1 d . . .
C7 C 0.2778(2) 0.13088(12) 0.97593(12) 0.0297(7) Uani 1 1 d . . .
C8 C 0.3451(2) 0.13332(13) 1.02456(13) 0.0348(7) Uani 1 1 d . . .
C9 C 0.3234(3) 0.13897(14) 1.07911(13) 0.0415(8) Uani 1 1 d . . .
C10 C 0.2331(3) 0.14352(14) 1.08690(13) 0.0393(8) Uani 1 1 d . . .
C11 C 0.1633(2) 0.14044(13) 1.04050(14) 0.0357(7) Uani 1 1 d . . .
C12 C 0.1869(2) 0.13431(12) 0.98677(12) 0.0287(7) Uani 1 1 d . . .
C13 C 0.2222(2) 0.08113(13) 0.85756(12) 0.0294(7) Uani 1 1 d . . .
C14 C 0.1614(2) 0.02838(14) 0.86146(13) 0.0339(7) Uani 1 1 d . . .
C15 C 0.1001(2) -0.01462(14) 0.81528(15) 0.0441(8) Uani 1 1 d . . .
C16 C 0.0966(3) -0.00511(16) 0.76071(14) 0.0465(9) Uani 1 1 d . . .
C17 C 0.1552(3) 0.04627(16) 0.75428(13) 0.0437(8) Uani 1 1 d . . .
C18 C 0.2169(2) 0.08728(13) 0.80144(13) 0.0336(7) Uani 1 1 d . . .
F1 F 0.48781(12) 0.21655(8) 0.89987(8) 0.0473(5) Uani 1 1 d . . .
F2 F 0.63812(14) 0.17791(10) 0.86844(9) 0.0630(6) Uani 1 1 d . . .
F3 F 0.65247(15) 0.05809(11) 0.85745(9) 0.0706(6) Uani 1 1 d . . .
F4 F 0.50910(17) -0.02335(10) 0.88170(10) 0.0716(6) Uani 1 1 d . . .
F5 F 0.35346(14) 0.01358(8) 0.91060(8) 0.0504(5) Uani 1 1 d . . .
F6 F 0.43773(13) 0.13185(9) 1.02150(8) 0.0511(5) Uani 1 1 d . . .
F7 F 0.39281(16) 0.14204(10) 1.12500(8) 0.0624(6) Uani 1 1 d . . .
F8 F 0.21100(16) 0.14922(9) 1.13978(7) 0.0595(6) Uani 1 1 d . . .
F9 F 0.07185(13) 0.14096(8) 1.04657(8) 0.0474(5) Uani 1 1 d . . .
F10 F 0.11363(11) 0.13146(7) 0.94317(7) 0.0346(4) Uani 1 1 d . . .
F11 F 0.15933(13) 0.01418(7) 0.91346(7) 0.0445(5) Uani 1 1 d . . .
F12 F 0.04391(15) -0.06581(8) 0.82265(9) 0.0615(6) Uani 1 1 d . . .
F13 F 0.03598(16) -0.04632(10) 0.71560(9) 0.0736(7) Uani 1 1 d . . .
F14 F 0.15330(16) 0.05575(9) 0.70075(8) 0.0644(6) Uani 1 1 d . . .
F15 F 0.27620(13) 0.13473(8) 0.79089(7) 0.0433(4) Uani 1 1 d . . .
B2 B 0.2500(2) 0.32514(14) 0.99474(14) 0.0250(7) Uani 1 1 d . . .
C19 C 0.1917(2) 0.37754(12) 0.97709(12) 0.0275(7) Uani 1 1 d . . .
C20 C 0.1197(2) 0.36984(13) 0.92955(12) 0.0295(7) Uani 1 1 d . . .
C21 C 0.0721(2) 0.41569(14) 0.91997(13) 0.0344(7) Uani 1 1 d . . .
C22 C 0.0942(2) 0.47222(14) 0.95871(15) 0.0385(8) Uani 1 1 d . . .
C23 C 0.1656(2) 0.48256(14) 1.00744(14) 0.0395(8) Uani 1 1 d . . .
C24 C 0.2105(2) 0.43582(13) 1.01515(13) 0.0314(7) Uani 1 1 d . . .
C25 C 0.3664(2) 0.34465(12) 0.99861(12) 0.0255(6) Uani 1 1 d . . .
C26 C 0.4147(2) 0.39103(13) 0.97789(12) 0.0294(7) Uani 1 1 d . . .
C27 C 0.5132(2) 0.40544(13) 0.98218(13) 0.0332(7) Uani 1 1 d . . .
C28 C 0.5695(2) 0.37091(15) 1.00728(14) 0.0375(8) Uani 1 1 d . . .
C29 C 0.5252(2) 0.32379(15) 1.02776(14) 0.0391(8) Uani 1 1 d . . .
C30 C 0.4273(2) 0.31126(13) 1.02232(13) 0.0321(7) Uani 1 1 d . . .
C31 C 0.22015(19) 0.31429(12) 1.05600(12) 0.0247(6) Uani 1 1 d . . .
C32 C 0.1285(2) 0.28369(12) 1.05573(12) 0.0284(7) Uani 1 1 d . . .
C33 C 0.0951(2) 0.27102(13) 1.10330(14) 0.0342(7) Uani 1 1 d . . .
C34 C 0.1579(2) 0.29008(15) 1.15602(13) 0.0396(8) Uani 1 1 d . . .
C35 C 0.2492(2) 0.32180(14) 1.15990(13) 0.0378(8) Uani 1 1 d . . .
C36 C 0.2784(2) 0.33433(13) 1.11096(12) 0.0306(7) Uani 1 1 d . . .
F16 F 0.09218(12) 0.31612(8) 0.88839(7) 0.0425(4) Uani 1 1 d . . .
F17 F 0.00237(13) 0.40536(8) 0.87242(8) 0.0484(5) Uani 1 1 d . . .
F18 F 0.04782(15) 0.51731(9) 0.95026(9) 0.0560(5) Uani 1 1 d . . .
F19 F 0.18863(16) 0.53813(8) 1.04637(9) 0.0589(6) Uani 1 1 d . . .
F20 F 0.28075(13) 0.44891(7) 1.06379(7) 0.0435(4) Uani 1 1 d . . .
F21 F 0.36541(12) 0.42572(8) 0.95053(7) 0.0400(4) Uani 1 1 d . . .
F22 F 0.55578(13) 0.45234(8) 0.96263(8) 0.0462(5) Uani 1 1 d . . .
F23 F 0.66596(13) 0.38484(10) 1.01246(9) 0.0604(6) Uani 1 1 d . . .
F24 F 0.57897(13) 0.28981(10) 1.05352(10) 0.0638(6) Uani 1 1 d . . .
F25 F 0.38945(12) 0.26399(7) 1.04400(7) 0.0390(4) Uani 1 1 d . . .
F26 F 0.06229(11) 0.26387(7) 1.00527(7) 0.0374(4) Uani 1 1 d . . .
F27 F 0.00496(13) 0.23992(9) 1.09904(8) 0.0504(5) Uani 1 1 d . . .
F28 F 0.12812(15) 0.27763(10) 1.20352(8) 0.0589(5) Uani 1 1 d . . .
F29 F 0.31150(15) 0.34108(10) 1.21157(8) 0.0595(6) Uani 1 1 d . . .
F30 F 0.36988(12) 0.36805(8) 1.12048(7) 0.0394(4) Uani 1 1 d . . .
K1 K 0.30452(5) 0.34983(3) 0.79673(3) 0.03320(16) Uani 1 1 d . . .
O9 O 0.49224(15) 0.41926(9) 0.83302(9) 0.0416(5) Uani 1 1 d . . .
O10 O 0.34649(15) 0.48481(9) 0.82483(9) 0.0397(5) Uani 1 1 d . . .
O11 O 0.15774(15) 0.41509(10) 0.79225(9) 0.0413(5) Uani 1 1 d . . .
O12 O 0.13284(15) 0.29977(10) 0.71341(10) 0.0463(6) Uani 1 1 d . . .
O13 O 0.27934(15) 0.23394(9) 0.72129(9) 0.0403(5) Uani 1 1 d . . .
O14 O 0.46984(15) 0.29711(10) 0.77202(9) 0.0397(5) Uani 1 1 d . . .
C37 C 0.5139(2) 0.48364(15) 0.83532(15) 0.0463(8) Uani 1 1 d . . .
H37A H 0.5132 0.4897 0.7959 0.056 Uiso 1 1 calc R . .
H37B H 0.5792 0.5035 0.8592 0.056 Uiso 1 1 calc R . .
C38 C 0.4395(2) 0.51249(15) 0.86104(14) 0.0429(8) Uani 1 1 d . . .
H38A H 0.4395 0.5058 0.9001 0.052 Uiso 1 1 calc R . .
H38B H 0.4547 0.5579 0.8645 0.052 Uiso 1 1 calc R . .
C39 C 0.2710(2) 0.50343(15) 0.85166(15) 0.0443(8) Uani 1 1 d . . .
H39A H 0.2852 0.5494 0.8658 0.053 Uiso 1 1 calc R . .
H39B H 0.2656 0.4851 0.8850 0.053 Uiso 1 1 calc R . .
C40 C 0.1791(3) 0.48146(16) 0.80837(16) 0.0506(9) Uani 1 1 d . . .
H40A H 0.1260 0.4964 0.8250 0.061 Uiso 1 1 calc R . .
H40B H 0.1857 0.4978 0.7740 0.061 Uiso 1 1 calc R . .
C41 C 0.0769(3) 0.39062(17) 0.74547(16) 0.0535(10) Uani 1 1 d . . .
H41A H 0.0921 0.4040 0.7109 0.064 Uiso 1 1 calc R . .
H41B H 0.0201 0.4066 0.7557 0.064 Uiso 1 1 calc R . .
C42 C 0.0543(2) 0.32202(17) 0.73277(16) 0.0524(9) Uani 1 1 d . . .
H42A H 0.0431 0.3086 0.7680 0.063 Uiso 1 1 calc R . .
H42B H -0.0054 0.3047 0.7026 0.063 Uiso 1 1 calc R . .
C43 C 0.1139(3) 0.23335(17) 0.69678(18) 0.0600(10) Uani 1 1 d . . .
H43A H 0.0548 0.2169 0.6661 0.072 Uiso 1 1 calc R . .
H43B H 0.1029 0.2165 0.7303 0.072 Uiso 1 1 calc R . .
C44 C 0.1977(3) 0.21387(17) 0.67541(15) 0.0535(9) Uani 1 1 d . . .
H44A H 0.1835 0.1680 0.6610 0.064 Uiso 1 1 calc R . .
H44B H 0.2108 0.2325 0.6432 0.064 Uiso 1 1 calc R . .
C45 C 0.3603(2) 0.20914(16) 0.70858(15) 0.0475(9) Uani 1 1 d . . .
H45A H 0.3827 0.2233 0.6759 0.057 Uiso 1 1 calc R . .
H45B H 0.3419 0.1631 0.6976 0.057 Uiso 1 1 calc R . .
C46 C 0.4388(2) 0.23112(15) 0.76085(15) 0.0455(8) Uani 1 1 d . . .
H46A H 0.4147 0.2199 0.7943 0.055 Uiso 1 1 calc R . .
H46B H 0.4939 0.2112 0.7545 0.055 Uiso 1 1 calc R . .
C47 C 0.5396(2) 0.32330(15) 0.82390(14) 0.0423(8) Uani 1 1 d . . .
H47A H 0.5953 0.3029 0.8235 0.051 Uiso 1 1 calc R . .
H47B H 0.5107 0.3174 0.8575 0.051 Uiso 1 1 calc R . .
C48 C 0.5725(2) 0.39159(15) 0.82803(15) 0.0451(8) Uani 1 1 d . . .
H48A H 0.6254 0.4111 0.8622 0.054 Uiso 1 1 calc R . .
H48B H 0.5972 0.3975 0.7931 0.054 Uiso 1 1 calc R . .
K2 K -0.08470(5) 0.16910(3) 0.93472(3) 0.04234(19) Uani 1 1 d . . .
O15 O -0.1214(2) 0.06072(12) 0.97392(12) 0.0676(8) Uani 1 1 d . . .
O16 O -0.23726(19) 0.14502(11) 0.99749(10) 0.0581(7) Uani 1 1 d . . .
O17 O -0.14772(15) 0.26827(10) 1.00410(9) 0.0421(5) Uani 1 1 d . . .
O18 O -0.12583(16) 0.26708(9) 0.88998(9) 0.0414(5) Uani 1 1 d . . .
O19 O -0.13087(16) 0.15324(10) 0.81372(9) 0.0453(6) Uani 1 1 d . . .
O20 O -0.09238(17) 0.05368(10) 0.85896(11) 0.0539(6) Uani 1 1 d . . .
C49 C -0.2177(3) 0.04120(18) 0.98020(17) 0.0693(12) Uani 1 1 d . . .
H49A H -0.2245 0.0032 0.9948 0.083 Uiso 1 1 calc R . .
H49B H -0.2628 0.0317 0.9425 0.083 Uiso 1 1 calc R . .
C50 C -0.2400(4) 0.09252(19) 1.02163(17) 0.0800(14) Uani 1 1 d . . .
H50A H -0.3052 0.0793 1.0299 0.096 Uiso 1 1 calc R . .
H50B H -0.1920 0.1038 1.0584 0.096 Uiso 1 1 calc R . .
C51 C -0.2542(3) 0.19708(19) 1.03640(16) 0.0624(11) Uani 1 1 d . . .
H51A H -0.2070 0.2072 1.0734 0.075 Uiso 1 1 calc R . .
H51B H -0.3202 0.1869 1.0445 0.075 Uiso 1 1 calc R . .
C52 C -0.2444(2) 0.25147(17) 1.01100(15) 0.0500(9) Uani 1 1 d . . .
H52A H -0.2892 0.2408 0.9731 0.060 Uiso 1 1 calc R . .
H52B H -0.2612 0.2868 1.0367 0.060 Uiso 1 1 calc R . .
C53 C -0.1295(2) 0.32283(14) 0.98401(16) 0.0477(9) Uani 1 1 d . . .
H53A H -0.0586 0.3396 0.9919 0.057 Uiso 1 1 calc R . .
H53B H -0.1586 0.3545 1.0060 0.057 Uiso 1 1 calc R . .
C54 C -0.1688(3) 0.31257(15) 0.92050(16) 0.0486(9) Uani 1 1 d . . .
H54A H -0.2403 0.2979 0.9120 0.058 Uiso 1 1 calc R . .
H54B H -0.1528 0.3520 0.9087 0.058 Uiso 1 1 calc R . .
C55 C -0.1540(3) 0.25560(17) 0.82945(15) 0.0545(10) Uani 1 1 d . . .
H55A H -0.1395 0.2951 0.8176 0.065 Uiso 1 1 calc R . .
H55B H -0.2246 0.2379 0.8174 0.065 Uiso 1 1 calc R . .
C56 C -0.1001(3) 0.21103(16) 0.80113(14) 0.0500(9) Uani 1 1 d . . .
H56A H -0.1135 0.2061 0.7588 0.060 Uiso 1 1 calc R . .
H56B H -0.0295 0.2268 0.8159 0.060 Uiso 1 1 calc R . .
C57 C -0.0880(3) 0.10604(18) 0.78490(16) 0.0594(10) Uani 1 1 d . . .
H57A H -0.0166 0.1179 0.7977 0.071 Uiso 1 1 calc R . .
H57B H -0.1038 0.1010 0.7426 0.071 Uiso 1 1 calc R . .
C58 C -0.1268(3) 0.04675(17) 0.79903(17) 0.0619(11) Uani 1 1 d . . .
H58A H -0.1985 0.0372 0.7901 0.074 Uiso 1 1 calc R . .
H58B H -0.1045 0.0121 0.7758 0.074 Uiso 1 1 calc R . .
C59 C -0.1255(3) -0.00092(16) 0.87700(19) 0.0651(12) Uani 1 1 d . . .
H59A H -0.1021 -0.0363 0.8560 0.078 Uiso 1 1 calc R . .
H59B H -0.1973 -0.0120 0.8690 0.078 Uiso 1 1 calc R . .
C60 C -0.0864(3) 0.01266(19) 0.9406(2) 0.0807(15) Uani 1 1 d . . .
H60A H -0.1041 -0.0258 0.9536 0.097 Uiso 1 1 calc R . .
H60B H -0.0147 0.0248 0.9477 0.097 Uiso 1 1 calc R . .
S2 S 0.73462(5) 0.22707(3) 0.41092(3) 0.02396(16) Uani 1 1 d . . .
O5 O 0.80938(13) 0.18968(8) 0.42408(7) 0.0249(4) Uani 1 1 d . . .
O6 O 0.71463(13) 0.25585(8) 0.47025(7) 0.0255(4) Uani 1 1 d . . .
O7 O 0.77988(14) 0.27477(8) 0.38767(8) 0.0305(5) Uani 1 1 d . . .
O8 O 0.64563(13) 0.18768(8) 0.37732(8) 0.0295(4) Uani 1 1 d . . .
B3 B 0.8025(2) 0.12482(15) 0.43432(14) 0.0277(7) Uani 1 1 d . . .
C61 C 0.7799(2) 0.12766(12) 0.49937(12) 0.0283(7) Uani 1 1 d . . .
C62 C 0.6892(2) 0.12919(12) 0.51132(12) 0.0298(7) Uani 1 1 d . . .
C63 C 0.6667(2) 0.13320(13) 0.56483(14) 0.0377(8) Uani 1 1 d . . .
C64 C 0.7390(3) 0.13735(14) 0.61167(13) 0.0406(8) Uani 1 1 d . . .
C65 C 0.8299(3) 0.13651(14) 0.60279(13) 0.0413(8) Uani 1 1 d . . .
C66 C 0.8498(2) 0.13262(12) 0.54770(12) 0.0321(7) Uani 1 1 d . . .
C67 C 0.9068(2) 0.10692(13) 0.42768(12) 0.0299(7) Uani 1 1 d . . .
C68 C 0.9197(2) 0.04805(15) 0.43166(14) 0.0407(8) Uani 1 1 d . . .
C69 C 0.9979(3) 0.02511(17) 0.42075(16) 0.0556(10) Uani 1 1 d . . .
C70 C 1.0711(3) 0.06063(19) 0.40472(16) 0.0578(11) Uani 1 1 d . . .
C71 C 1.0648(2) 0.11966(17) 0.40123(14) 0.0482(9) Uani 1 1 d . . .
C72 C 0.9841(2) 0.14166(14) 0.41310(13) 0.0357(7) Uani 1 1 d . . .
C73 C 0.7251(2) 0.07188(12) 0.38169(12) 0.0263(6) Uani 1 1 d . . .
C74 C 0.6636(2) 0.01994(13) 0.38694(12) 0.0294(7) Uani 1 1 d . . .
C75 C 0.6098(2) -0.02741(12) 0.34044(13) 0.0324(7) Uani 1 1 d . . .
C76 C 0.6151(2) -0.02397(13) 0.28536(13) 0.0332(7) Uani 1 1 d . . .
C77 C 0.6739(2) 0.02699(13) 0.27754(12) 0.0313(7) Uani 1 1 d . . .
C78 C 0.7271(2) 0.07252(12) 0.32458(12) 0.0276(7) Uani 1 1 d . . .
F31 F 0.61468(12) 0.12612(7) 0.46826(7) 0.0358(4) Uani 1 1 d . . .
F32 F 0.57646(14) 0.13264(9) 0.57298(8) 0.0533(5) Uani 1 1 d . . .
F33 F 0.71954(15) 0.14244(9) 0.66491(7) 0.0611(6) Uani 1 1 d . . .
F34 F 0.90169(15) 0.14099(9) 0.64775(8) 0.0567(5) Uani 1 1 d . . .
F35 F 0.94327(13) 0.13582(8) 0.54463(7) 0.0411(4) Uani 1 1 d . . .
F36 F 0.84999(15) 0.01065(8) 0.44727(9) 0.0550(5) Uani 1 1 d . . .
F37 F 1.00319(18) -0.03287(10) 0.42458(12) 0.0885(8) Uani 1 1 d . . .
F38 F 1.14724(16) 0.03797(12) 0.39069(12) 0.0983(9) Uani 1 1 d . . .
F39 F 1.13593(15) 0.15566(12) 0.38496(10) 0.0741(7) Uani 1 1 d . . .
F40 F 0.98634(13) 0.20101(8) 0.40944(8) 0.0470(5) Uani 1 1 d . . .
F41 F 0.65226(13) 0.01129(7) 0.43921(7) 0.0409(4) Uani 1 1 d . . .
F42 F 0.55180(13) -0.07695(8) 0.34955(8) 0.0462(5) Uani 1 1 d . . .
F43 F 0.56213(14) -0.06928(8) 0.24026(7) 0.0481(5) Uani 1 1 d . . .
F44 F 0.67845(14) 0.03203(8) 0.22310(7) 0.0446(5) Uani 1 1 d . . .
F45 F 0.78714(12) 0.11924(7) 0.31268(7) 0.0370(4) Uani 1 1 d . . .
B4 B 0.7579(2) 0.32054(14) 0.50961(14) 0.0247(7) Uani 1 1 d . . .
C79 C 0.8742(2) 0.33848(12) 0.51008(11) 0.0260(6) Uani 1 1 d . . .
C80 C 0.9203(2) 0.38383(13) 0.48700(12) 0.0293(7) Uani 1 1 d . . .
C81 C 1.0178(2) 0.39687(13) 0.48810(13) 0.0325(7) Uani 1 1 d . . .
C82 C 1.0754(2) 0.36276(15) 0.51153(14) 0.0375(8) Uani 1 1 d . . .
C83 C 1.0344(2) 0.31657(14) 0.53435(13) 0.0359(7) Uani 1 1 d . . .
C84 C 0.9364(2) 0.30571(13) 0.53314(12) 0.0306(7) Uani 1 1 d . . .
C85 C 0.69862(19) 0.37208(12) 0.49181(12) 0.0260(6) Uani 1 1 d . . .
C86 C 0.7222(2) 0.43181(13) 0.52752(13) 0.0344(7) Uani 1 1 d . . .
C87 C 0.6791(2) 0.47913(13) 0.51813(15) 0.0432(8) Uani 1 1 d . . .
C88 C 0.6065(2) 0.46834(14) 0.47105(15) 0.0416(8) Uani 1 1 d . . .
C89 C 0.5786(2) 0.41033(14) 0.43424(13) 0.0336(7) Uani 1 1 d . . .
C90 C 0.6235(2) 0.36357(12) 0.44522(12) 0.0280(7) Uani 1 1 d . . .
C91 C 0.73367(19) 0.31280(12) 0.57281(12) 0.0253(6) Uani 1 1 d . . .
C92 C 0.6428(2) 0.28217(13) 0.57569(12) 0.0299(7) Uani 1 1 d . . .
C93 C 0.6146(2) 0.27173(14) 0.62514(13) 0.0361(7) Uani 1 1 d . . .
C94 C 0.6803(2) 0.29304(16) 0.67645(13) 0.0430(8) Uani 1 1 d . . .
C95 C 0.7706(2) 0.32511(16) 0.67726(13) 0.0405(8) Uani 1 1 d . . .
C96 C 0.7952(2) 0.33511(13) 0.62630(13) 0.0322(7) Uani 1 1 d . . .
F46 F 0.86878(12) 0.41811(8) 0.46019(8) 0.0430(4) Uani 1 1 d . . .
F47 F 1.05784(13) 0.44355(8) 0.46674(8) 0.0491(5) Uani 1 1 d . . .
F48 F 1.17097(13) 0.37540(10) 0.51314(9) 0.0588(5) Uani 1 1 d . . .
F49 F 1.08945(13) 0.28206(9) 0.55775(9) 0.0568(5) Uani 1 1 d . . .
F50 F 0.90143(12) 0.26020(7) 0.55747(7) 0.0380(4) Uani 1 1 d . . .
F51 F 0.79490(14) 0.44576(8) 0.57441(8) 0.0496(5) Uani 1 1 d . . .
F52 F 0.70809(16) 0.53598(8) 0.55501(10) 0.0687(6) Uani 1 1 d . . .
F53 F 0.56348(14) 0.51450(8) 0.46055(9) 0.0573(5) Uani 1 1 d . . .
F54 F 0.50707(12) 0.39981(8) 0.38768(8) 0.0437(4) Uani 1 1 d . . .
F55 F 0.59045(11) 0.30811(7) 0.40680(7) 0.0349(4) Uani 1 1 d . . .
F56 F 0.57285(11) 0.26071(8) 0.52666(7) 0.0396(4) Uani 1 1 d . . .
F57 F 0.52452(13) 0.24198(9) 0.62417(8) 0.0544(5) Uani 1 1 d . . .
F58 F 0.65599(15) 0.28286(11) 0.72585(8) 0.0672(6) Uani 1 1 d . . .
F59 F 0.83511(14) 0.34745(11) 0.72770(8) 0.0629(6) Uani 1 1 d . . .
F60 F 0.88570(12) 0.36891(8) 0.63260(7) 0.0406(4) Uani 1 1 d . . .
K3 K 0.79489(5) 0.33357(3) 0.30554(3) 0.03389(16) Uani 1 1 d . . .
O21 O 0.83576(16) 0.46884(10) 0.32920(9) 0.0445(6) Uani 1 1 d . . .
O22 O 0.64647(16) 0.39815(11) 0.30211(10) 0.0504(6) Uani 1 1 d . . .
O23 O 0.61539(16) 0.27693(11) 0.23144(10) 0.0513(6) Uani 1 1 d . . .
O24 O 0.76605(16) 0.21356(10) 0.23657(9) 0.0449(6) Uani 1 1 d . . .
O25 O 0.95607(15) 0.27950(10) 0.27525(9) 0.0408(5) Uani 1 1 d . . .
O26 O 0.98230(15) 0.40291(10) 0.33612(10) 0.0453(6) Uani 1 1 d . . .
C97 C 0.7614(3) 0.48898(17) 0.35529(17) 0.0577(10) Uani 1 1 d . . .
H97A H 0.7749 0.5351 0.3664 0.069 Uiso 1 1 calc R . .
H97B H 0.7584 0.4739 0.3906 0.069 Uiso 1 1 calc R . .
C98 C 0.6676(3) 0.46408(17) 0.31381(18) 0.0581(10) Uani 1 1 d . . .
H98A H 0.6155 0.4805 0.3304 0.070 Uiso 1 1 calc R . .
H98B H 0.6716 0.4772 0.2776 0.070 Uiso 1 1 calc R . .
C99 C 0.5620(3) 0.3701(2) 0.25886(18) 0.0666(11) Uani 1 1 d . . .
H99A H 0.5725 0.3789 0.2217 0.080 Uiso 1 1 calc R . .
H99B H 0.5068 0.3876 0.2697 0.080 Uiso 1 1 calc R . .
C100 C 0.5399(3) 0.3026(2) 0.25261(17) 0.0622(11) Uani 1 1 d . . .
H10A H 0.5342 0.2938 0.2905 0.075 Uiso 1 1 calc R . .
H10B H 0.4773 0.2832 0.2254 0.075 Uiso 1 1 calc R . .
C101 C 0.5999(3) 0.21129(18) 0.22586(17) 0.0640(11) Uani 1 1 d . . .
H10C H 0.5351 0.1901 0.2019 0.077 Uiso 1 1 calc R . .
H10D H 0.6028 0.2026 0.2644 0.077 Uiso 1 1 calc R . .
C102 C 0.6763(3) 0.18790(16) 0.19838(16) 0.0566(10) Uani 1 1 d . . .
H10E H 0.6628 0.1419 0.1899 0.068 Uiso 1 1 calc R . .
H10F H 0.6776 0.2002 0.1616 0.068 Uiso 1 1 calc R . .
C103 C 0.8429(3) 0.18925(15) 0.21850(15) 0.0506(9) Uani 1 1 d . . .
H10G H 0.8567 0.2020 0.1834 0.061 Uiso 1 1 calc R . .
H10H H 0.8258 0.1432 0.2092 0.061 Uiso 1 1 calc R . .
C104 C 0.9294(3) 0.21355(15) 0.26599(16) 0.0506(9) Uani 1 1 d . . .
H10I H 0.9143 0.2029 0.3017 0.061 Uiso 1 1 calc R . .
H10J H 0.9836 0.1946 0.2556 0.061 Uiso 1 1 calc R . .
C105 C 1.0314(3) 0.30754(17) 0.32398(16) 0.0536(9) Uani 1 1 d . . .
H10K H 1.0874 0.2878 0.3208 0.064 Uiso 1 1 calc R . .
H10L H 1.0086 0.3021 0.3596 0.064 Uiso 1 1 calc R . .
C106 C 1.0606(2) 0.37482(17) 0.32655(17) 0.0544(10) Uani 1 1 d . . .
H10M H 1.1174 0.3948 0.3583 0.065 Uiso 1 1 calc R . .
H10N H 1.0789 0.3801 0.2898 0.065 Uiso 1 1 calc R . .
C107 C 1.0019(3) 0.46721(16) 0.33689(16) 0.0516(9) Uani 1 1 d . . .
H10O H 0.9982 0.4721 0.2970 0.062 Uiso 1 1 calc R . .
H10P H 1.0680 0.4878 0.3593 0.062 Uiso 1 1 calc R . .
C108 C 0.9299(3) 0.49629(15) 0.36361(14) 0.0477(9) Uani 1 1 d . . .
H10Q H 0.9320 0.4901 0.4030 0.057 Uiso 1 1 calc R . .
H10R H 0.9451 0.5416 0.3667 0.057 Uiso 1 1 calc R . .
K4 K 0.45831(5) 0.18896(3) 0.41127(3) 0.03420(17) Uani 1 1 d . . .
O27 O 0.35376(16) 0.09547(9) 0.45711(9) 0.0413(5) Uani 1 1 d . . .
O28 O 0.42440(15) 0.05532(9) 0.35828(9) 0.0385(5) Uani 1 1 d . . .
O29 O 0.41841(15) 0.13965(9) 0.28786(9) 0.0386(5) Uani 1 1 d . . .
O30 O 0.31194(16) 0.22337(10) 0.33015(9) 0.0453(6) Uani 1 1 d . . .
O31 O 0.38659(15) 0.30545(9) 0.43754(9) 0.0379(5) Uani 1 1 d . . .
O32 O 0.35339(15) 0.21963(9) 0.50689(9) 0.0388(5) Uani 1 1 d . . .
C109 C 0.3870(3) 0.03940(15) 0.44751(15) 0.0485(9) Uani 1 1 d . . .
H10S H 0.3507 0.0095 0.4654 0.058 Uiso 1 1 calc R . .
H10T H 0.4567 0.0478 0.4652 0.058 Uiso 1 1 calc R . .
C110 C 0.3721(2) 0.01272(14) 0.38427(15) 0.0446(8) Uani 1 1 d . . .
H11A H 0.3944 -0.0268 0.3768 0.054 Uiso 1 1 calc R . .
H11B H 0.3021 0.0035 0.3669 0.054 Uiso 1 1 calc R . .
C111 C 0.4079(2) 0.03390(14) 0.29764(14) 0.0413(8) Uani 1 1 d . . .
H11C H 0.3374 0.0220 0.2814 0.050 Uiso 1 1 calc R . .
H11D H 0.4356 -0.0032 0.2869 0.050 Uiso 1 1 calc R . .
C112 C 0.4547(2) 0.08465(15) 0.27404(14) 0.0435(8) Uani 1 1 d . . .
H11E H 0.5255 0.0949 0.2895 0.052 Uiso 1 1 calc R . .
H11F H 0.4443 0.0696 0.2315 0.052 Uiso 1 1 calc R . .
C113 C 0.3180(2) 0.13105(15) 0.26523(14) 0.0469(9) Uani 1 1 d . . .
H11G H 0.2791 0.1078 0.2874 0.056 Uiso 1 1 calc R . .
H11H H 0.3020 0.1069 0.2243 0.056 Uiso 1 1 calc R . .
C114 C 0.2958(3) 0.19353(15) 0.26984(14) 0.0497(9) Uani 1 1 d . . .
H11I H 0.3386 0.2182 0.2505 0.060 Uiso 1 1 calc R . .
H11J H 0.2276 0.1895 0.2512 0.060 Uiso 1 1 calc R . .
C115 C 0.3134(3) 0.28712(14) 0.33856(14) 0.0431(8) Uani 1 1 d . . .
H11K H 0.2587 0.2933 0.3116 0.052 Uiso 1 1 calc R . .
H11L H 0.3748 0.3092 0.3311 0.052 Uiso 1 1 calc R . .
C116 C 0.3050(3) 0.31197(16) 0.39925(15) 0.0476(9) Uani 1 1 d . . .
H11M H 0.3023 0.3565 0.4058 0.057 Uiso 1 1 calc R . .
H11N H 0.2445 0.2889 0.4068 0.057 Uiso 1 1 calc R . .
C117 C 0.3787(2) 0.32244(14) 0.49632(14) 0.0420(8) Uani 1 1 d . . .
H11O H 0.3536 0.3610 0.5034 0.050 Uiso 1 1 calc R . .
H11P H 0.4440 0.3315 0.5211 0.050 Uiso 1 1 calc R . .
C118 C 0.3134(3) 0.27273(15) 0.51291(14) 0.0455(8) Uani 1 1 d . . .
H11Q H 0.3066 0.2875 0.5534 0.055 Uiso 1 1 calc R . .
H11R H 0.2483 0.2624 0.4877 0.055 Uiso 1 1 calc R . .
C119 C 0.2925(2) 0.16925(15) 0.51878(14) 0.0422(8) Uani 1 1 d . . .
H11S H 0.2298 0.1573 0.4910 0.051 Uiso 1 1 calc R . .
H11T H 0.2794 0.1820 0.5582 0.051 Uiso 1 1 calc R . .
C120 C 0.3396(3) 0.11482(15) 0.51433(14) 0.0445(8) Uani 1 1 d . . .
H12A H 0.4027 0.1268 0.5417 0.053 Uiso 1 1 calc R . .
H12B H 0.2979 0.0802 0.5243 0.053 Uiso 1 1 calc R . .
C121 C 0.4505(5) 0.3636(3) 0.6659(3) 0.0941(16) Uani 0.866(3) 1 d P . .
H12C H 0.4790 0.3575 0.7036 0.113 Uiso 0.866(3) 1 calc PR . .
H12D H 0.4472 0.3249 0.6362 0.113 Uiso 0.866(3) 1 calc PR . .
Cl1 Cl 0.33136(11) 0.37260(6) 0.66774(5) 0.0755(5) Uani 0.866(3) 1 d P . .
Cl2 Cl 0.52312(14) 0.41928(8) 0.65254(9) 0.1167(7) Uani 0.866(3) 1 d P . .
C122 C 0.9114(3) 0.3388(2) 0.1609(2) 0.0763(13) Uani 1 1 d . . .
H12E H 0.9397 0.3210 0.1918 0.092 Uiso 0.801(6) 1 calc PR A 1
H12F H 0.9038 0.3078 0.1237 0.092 Uiso 0.801(6) 1 calc PR A 1
H12G H 0.9539 0.3415 0.1981 0.092 Uiso 0.199(6) 1 d PR A 2
H12H H 0.9064 0.2975 0.1346 0.092 Uiso 0.199(6) 1 d PR A 2
Cl3 Cl 0.79696(8) 0.34782(5) 0.17108(4) 0.0667(3) Uani 1 1 d . A .
Cl4A Cl 0.9932(2) 0.40471(9) 0.16045(16) 0.0782(8) Uani 0.801(6) 1 d P A 1
Cl4B Cl 0.9553(8) 0.3942(4) 0.1309(6) 0.0782(8) Uani 0.199(6) 1 d P A 2
C123 C 0.7788(10) 0.4776(6) 0.7456(6) 0.0941(16) Uani 0.435(5) 1 d P B 1
H90A H 0.8313 0.4716 0.7240 0.113 Uiso 0.435(5) 1 calc PR B 1
H90B H 0.7243 0.4412 0.7277 0.113 Uiso 0.435(5) 1 calc PR B 1
Cl5 Cl 0.8238(3) 0.46982(19) 0.8194(2) 0.1395(18) Uani 0.435(5) 1 d P B 1
Cl6 Cl 0.7449(4) 0.5324(3) 0.7318(3) 0.181(2) Uani 0.435(5) 1 d P B 1
C124 C 0.7513(19) 0.4872(11) 0.7125(10) 0.0941(16) Uani 0.257(4) 1 d P C 2
H90C H 0.8148 0.4872 0.7010 0.113 Uiso 0.257(4) 1 calc PR C 2
H90D H 0.7093 0.4449 0.6969 0.113 Uiso 0.257(4) 1 calc PR C 2
Cl7 Cl 0.6944(7) 0.5449(5) 0.6857(5) 0.181(2) Uani 0.257(4) 1 d P C 2
Cl8 Cl 0.7679(5) 0.5126(3) 0.7971(4) 0.1395(18) Uani 0.257(4) 1 d P 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
S1 0.0349(4) 0.0240(4) 0.0218(4) 0.0019(3) 0.0019(3) 0.0091(3)
O1 0.0326(11) 0.0260(10) 0.0266(11) 0.0038(8) 0.0031(9) 0.0080(8)
O2 0.0303(11) 0.0220(10) 0.0259(11) 0.0013(8) 0.0051(9) 0.0050(8)
O3 0.0463(13) 0.0292(11) 0.0279(11) 0.0105(9) 0.0097(10) 0.0097(9)
O4 0.0389(12) 0.0312(11) 0.0276(11) -0.0007(9) -0.0044(10) 0.0098(9)
B1 0.0338(19) 0.0275(18) 0.0252(19) 0.0070(15) 0.0036(15) 0.0114(15)
C1 0.0363(18) 0.0341(17) 0.0179(15) 0.0004(13) -0.0022(13) 0.0134(14)
C2 0.0376(19) 0.0364(19) 0.0266(17) 0.0028(14) 0.0013(14) 0.0092(15)
C3 0.037(2) 0.065(2) 0.0276(18) 0.0038(16) 0.0025(15) 0.0102(18)
C4 0.040(2) 0.070(3) 0.033(2) -0.0011(18) 0.0020(16) 0.0288(19)
C5 0.056(2) 0.046(2) 0.038(2) 0.0018(16) 0.0030(17) 0.0306(18)
C6 0.045(2) 0.0350(18) 0.0326(18) 0.0037(14) 0.0033(15) 0.0144(16)
C7 0.0394(18) 0.0195(15) 0.0262(17) 0.0027(12) 0.0002(14) 0.0056(13)
C8 0.0403(19) 0.0303(17) 0.0298(19) 0.0060(14) -0.0006(15) 0.0061(14)
C9 0.062(2) 0.0304(18) 0.0228(18) 0.0040(14) -0.0094(17) 0.0061(16)
C10 0.064(2) 0.0277(17) 0.0238(18) 0.0044(13) 0.0104(17) 0.0041(15)
C11 0.043(2) 0.0222(16) 0.040(2) 0.0053(14) 0.0124(16) 0.0029(14)
C12 0.0417(19) 0.0201(15) 0.0192(16) 0.0012(12) -0.0001(14) 0.0034(13)
C13 0.0360(17) 0.0250(16) 0.0264(17) 0.0013(13) 0.0043(13) 0.0129(13)
C14 0.0421(19) 0.0329(18) 0.0243(17) 0.0008(14) 0.0052(14) 0.0113(15)
C15 0.046(2) 0.0309(19) 0.047(2) -0.0054(16) 0.0067(17) 0.0055(16)
C16 0.047(2) 0.042(2) 0.032(2) -0.0185(17) -0.0026(16) 0.0060(17)
C17 0.060(2) 0.049(2) 0.0184(18) -0.0029(15) 0.0034(16) 0.0224(18)
C18 0.0421(19) 0.0297(17) 0.0273(18) 0.0015(14) 0.0056(15) 0.0119(14)
F1 0.0393(11) 0.0420(11) 0.0566(12) 0.0102(9) 0.0074(9) 0.0034(8)
F2 0.0375(11) 0.0889(16) 0.0584(14) 0.0132(12) 0.0147(10) 0.0053(11)
F3 0.0546(13) 0.1074(18) 0.0558(14) 0.0057(12) 0.0150(11) 0.0478(13)
F4 0.0870(17) 0.0596(14) 0.0793(16) 0.0122(12) 0.0159(13) 0.0514(12)
F5 0.0595(13) 0.0361(11) 0.0619(13) 0.0170(9) 0.0130(10) 0.0200(9)
F6 0.0444(12) 0.0660(13) 0.0368(11) 0.0060(9) -0.0064(9) 0.0175(9)
F7 0.0763(15) 0.0740(14) 0.0279(11) 0.0113(10) -0.0118(10) 0.0140(11)
F8 0.0928(16) 0.0578(13) 0.0242(11) 0.0070(9) 0.0176(10) 0.0059(11)
F9 0.0519(12) 0.0430(11) 0.0466(11) 0.0061(9) 0.0227(9) 0.0041(9)
F10 0.0362(10) 0.0326(9) 0.0315(10) 0.0029(7) 0.0039(8) 0.0072(7)
F11 0.0623(12) 0.0290(10) 0.0356(11) 0.0036(8) 0.0074(9) 0.0005(8)
F12 0.0655(14) 0.0340(11) 0.0665(14) -0.0101(10) 0.0123(11) -0.0078(10)
F13 0.0780(16) 0.0632(14) 0.0468(13) -0.0245(11) -0.0119(11) -0.0012(12)
F14 0.0906(17) 0.0679(14) 0.0244(11) -0.0029(10) -0.0002(10) 0.0192(12)
F15 0.0592(12) 0.0415(11) 0.0290(10) 0.0056(8) 0.0129(9) 0.0112(9)
B2 0.0256(17) 0.0187(16) 0.0275(19) 0.0013(14) 0.0027(14) 0.0045(13)
C19 0.0274(16) 0.0255(16) 0.0299(17) 0.0061(13) 0.0086(13) 0.0055(12)
C20 0.0298(16) 0.0270(16) 0.0279(17) 0.0018(13) 0.0035(14) 0.0050(13)
C21 0.0291(17) 0.0416(19) 0.0361(19) 0.0157(15) 0.0058(15) 0.0106(14)
C22 0.045(2) 0.0317(18) 0.052(2) 0.0210(16) 0.0217(17) 0.0207(15)
C23 0.048(2) 0.0253(17) 0.047(2) 0.0069(15) 0.0161(17) 0.0114(15)
C24 0.0346(17) 0.0284(17) 0.0303(18) 0.0049(14) 0.0058(14) 0.0085(13)
C25 0.0284(16) 0.0220(15) 0.0240(16) 0.0011(12) 0.0057(13) 0.0051(12)
C26 0.0318(17) 0.0262(16) 0.0268(17) 0.0004(13) 0.0045(13) 0.0064(13)
C27 0.0349(18) 0.0311(17) 0.0303(17) 0.0028(14) 0.0114(14) 0.0003(14)
C28 0.0228(17) 0.0451(19) 0.0394(19) 0.0030(16) 0.0073(14) 0.0022(14)
C29 0.0307(18) 0.045(2) 0.044(2) 0.0140(16) 0.0052(15) 0.0137(15)
C30 0.0328(17) 0.0262(16) 0.0365(18) 0.0064(14) 0.0074(14) 0.0058(13)
C31 0.0272(16) 0.0175(14) 0.0269(17) 0.0008(12) 0.0035(13) 0.0059(12)
C32 0.0246(16) 0.0246(15) 0.0282(17) -0.0021(13) -0.0005(14) 0.0017(12)
C33 0.0311(17) 0.0329(17) 0.040(2) 0.0064(14) 0.0148(15) 0.0069(14)
C34 0.051(2) 0.046(2) 0.0306(19) 0.0133(15) 0.0215(17) 0.0165(16)
C35 0.041(2) 0.0430(19) 0.0239(18) 0.0001(14) 0.0025(15) 0.0089(15)
C36 0.0289(17) 0.0289(16) 0.0297(18) 0.0020(13) 0.0040(14) 0.0035(13)
F16 0.0416(10) 0.0374(10) 0.0394(11) -0.0014(8) -0.0091(8) 0.0134(8)
F17 0.0425(11) 0.0584(12) 0.0495(12) 0.0201(10) 0.0018(10) 0.0227(9)
F18 0.0647(13) 0.0480(12) 0.0711(14) 0.0265(10) 0.0192(11) 0.0342(10)
F19 0.0811(15) 0.0273(10) 0.0643(14) -0.0018(9) 0.0107(11) 0.0214(10)
F20 0.0520(11) 0.0285(9) 0.0391(11) -0.0047(8) -0.0047(9) 0.0093(8)
F21 0.0378(10) 0.0397(10) 0.0478(11) 0.0226(9) 0.0092(8) 0.0077(8)
F22 0.0412(11) 0.0455(11) 0.0487(12) 0.0134(9) 0.0141(9) -0.0048(9)
F23 0.0272(10) 0.0778(14) 0.0814(15) 0.0286(12) 0.0170(10) 0.0091(10)
F24 0.0366(11) 0.0741(14) 0.0990(17) 0.0455(13) 0.0168(11) 0.0269(10)
F25 0.0365(10) 0.0325(10) 0.0518(11) 0.0163(8) 0.0098(8) 0.0097(8)
F26 0.0257(9) 0.0424(10) 0.0370(10) 0.0026(8) 0.0028(8) 0.0016(7)
F27 0.0352(10) 0.0570(12) 0.0626(13) 0.0171(10) 0.0231(9) 0.0054(9)
F28 0.0629(13) 0.0854(15) 0.0412(12) 0.0276(11) 0.0275(10) 0.0201(11)
F29 0.0574(13) 0.0894(15) 0.0260(11) 0.0122(10) 0.0022(10) 0.0099(11)
F30 0.0324(10) 0.0455(10) 0.0295(10) 0.0011(8) -0.0006(8) -0.0030(8)
K1 0.0342(4) 0.0347(4) 0.0306(4) 0.0078(3) 0.0070(3) 0.0076(3)
O9 0.0338(12) 0.0365(13) 0.0500(14) 0.0071(10) 0.0056(10) 0.0030(10)
O10 0.0411(13) 0.0393(12) 0.0364(13) 0.0068(10) 0.0059(10) 0.0083(10)
O11 0.0343(12) 0.0444(14) 0.0496(14) 0.0188(11) 0.0080(11) 0.0118(10)
O12 0.0325(13) 0.0516(15) 0.0504(15) 0.0088(11) 0.0073(11) 0.0039(10)
O13 0.0443(13) 0.0395(12) 0.0328(12) -0.0001(10) 0.0079(11) 0.0091(10)
O14 0.0405(13) 0.0412(13) 0.0361(13) 0.0081(10) 0.0057(10) 0.0093(10)
C37 0.0377(19) 0.041(2) 0.051(2) 0.0104(17) 0.0008(16) -0.0051(15)
C38 0.048(2) 0.0342(18) 0.041(2) 0.0064(15) 0.0026(17) 0.0041(15)
C39 0.052(2) 0.0381(19) 0.047(2) 0.0107(16) 0.0158(18) 0.0171(16)
C40 0.052(2) 0.050(2) 0.064(3) 0.0261(19) 0.022(2) 0.0235(18)
C41 0.040(2) 0.064(3) 0.061(3) 0.022(2) 0.0079(19) 0.0147(18)
C42 0.0295(19) 0.063(3) 0.061(2) 0.0123(19) 0.0065(17) 0.0075(17)
C43 0.042(2) 0.052(2) 0.070(3) 0.000(2) 0.0037(19) -0.0037(18)
C44 0.050(2) 0.049(2) 0.045(2) -0.0093(17) -0.0025(18) 0.0035(17)
C45 0.051(2) 0.045(2) 0.046(2) 0.0027(16) 0.0201(18) 0.0107(17)
C46 0.044(2) 0.044(2) 0.052(2) 0.0130(17) 0.0124(18) 0.0152(16)
C47 0.041(2) 0.052(2) 0.0331(19) 0.0064(16) 0.0047(16) 0.0161(16)
C48 0.0327(18) 0.056(2) 0.045(2) 0.0103(17) 0.0039(16) 0.0101(16)
K2 0.0547(5) 0.0281(4) 0.0363(4) 0.0045(3) -0.0042(3) 0.0047(3)
O15 0.076(2) 0.0411(15) 0.0663(18) 0.0261(14) -0.0255(15) -0.0175(14)
O16 0.0783(18) 0.0513(15) 0.0383(14) 0.0173(12) 0.0113(13) -0.0090(13)
O17 0.0387(13) 0.0416(13) 0.0444(14) 0.0060(11) 0.0118(11) 0.0077(10)
O18 0.0523(14) 0.0368(12) 0.0383(14) 0.0135(10) 0.0083(11) 0.0143(10)
O19 0.0490(14) 0.0441(14) 0.0382(13) 0.0058(11) 0.0081(11) 0.0048(11)
O20 0.0485(15) 0.0303(13) 0.0657(18) -0.0020(12) -0.0070(13) -0.0026(11)
C49 0.095(3) 0.046(2) 0.052(3) 0.025(2) -0.007(2) -0.018(2)
C50 0.121(4) 0.064(3) 0.043(2) 0.026(2) 0.010(2) -0.018(3)
C51 0.061(3) 0.083(3) 0.040(2) 0.015(2) 0.0171(19) 0.003(2)
C52 0.042(2) 0.066(2) 0.042(2) 0.0094(18) 0.0145(17) 0.0085(17)
C53 0.043(2) 0.0316(19) 0.066(3) 0.0020(17) 0.0165(18) 0.0087(15)
C54 0.048(2) 0.0371(19) 0.068(3) 0.0213(18) 0.0150(19) 0.0160(16)
C55 0.066(3) 0.053(2) 0.047(2) 0.0287(19) 0.0042(19) 0.0071(19)
C56 0.063(2) 0.055(2) 0.0254(18) 0.0112(16) 0.0060(17) -0.0033(19)
C57 0.054(2) 0.066(3) 0.045(2) -0.0066(19) 0.0078(19) 0.006(2)
C58 0.049(2) 0.050(2) 0.066(3) -0.017(2) 0.000(2) 0.0052(18)
C59 0.054(2) 0.030(2) 0.100(4) 0.007(2) 0.001(2) 0.0030(17)
C60 0.061(3) 0.040(2) 0.128(4) 0.039(3) -0.027(3) -0.007(2)
S2 0.0303(4) 0.0211(4) 0.0204(4) 0.0041(3) 0.0037(3) 0.0081(3)
O5 0.0298(11) 0.0215(10) 0.0223(10) 0.0032(8) 0.0023(8) 0.0086(8)
O6 0.0324(11) 0.0217(10) 0.0210(10) 0.0023(8) 0.0050(8) 0.0066(8)
O7 0.0419(12) 0.0257(11) 0.0259(11) 0.0085(9) 0.0079(9) 0.0088(9)
O8 0.0320(11) 0.0270(11) 0.0253(11) 0.0028(9) -0.0024(9) 0.0073(9)
B3 0.0353(19) 0.0261(18) 0.0223(18) 0.0066(14) 0.0033(15) 0.0096(15)
C61 0.0387(18) 0.0196(15) 0.0251(16) 0.0042(12) 0.0032(14) 0.0068(13)
C62 0.0395(18) 0.0207(15) 0.0256(17) 0.0036(12) 0.0016(15) 0.0044(13)
C63 0.048(2) 0.0269(17) 0.037(2) 0.0045(14) 0.0173(17) 0.0021(14)
C64 0.058(2) 0.0348(18) 0.0197(18) 0.0018(14) 0.0093(16) -0.0077(16)
C65 0.059(2) 0.0306(18) 0.0215(18) 0.0033(14) -0.0067(17) -0.0068(16)
C66 0.045(2) 0.0198(15) 0.0268(18) -0.0001(13) 0.0043(15) 0.0046(13)
C67 0.0349(17) 0.0325(17) 0.0199(16) 0.0011(13) -0.0017(13) 0.0137(14)
C68 0.043(2) 0.0388(19) 0.0366(19) 0.0031(15) -0.0036(16) 0.0164(16)
C69 0.054(2) 0.045(2) 0.059(3) -0.0058(18) -0.008(2) 0.0291(19)
C70 0.039(2) 0.069(3) 0.054(2) -0.013(2) -0.0084(18) 0.033(2)
C71 0.0287(19) 0.068(3) 0.036(2) -0.0053(17) 0.0006(15) 0.0073(17)
C72 0.0349(18) 0.0393(19) 0.0281(18) 0.0015(14) -0.0003(14) 0.0101(15)
C73 0.0339(17) 0.0223(15) 0.0251(16) 0.0047(12) 0.0062(13) 0.0136(13)
C74 0.0451(19) 0.0245(16) 0.0202(16) 0.0046(13) 0.0083(14) 0.0120(14)
C75 0.0362(18) 0.0201(16) 0.039(2) 0.0038(14) 0.0088(15) 0.0052(13)
C76 0.0392(18) 0.0270(17) 0.0263(18) -0.0061(14) 0.0009(14) 0.0094(14)
C77 0.0455(19) 0.0313(17) 0.0172(16) 0.0013(13) 0.0077(14) 0.0136(15)
C78 0.0343(17) 0.0244(16) 0.0270(17) 0.0070(13) 0.0104(13) 0.0099(13)
F31 0.0370(10) 0.0383(10) 0.0330(10) 0.0090(8) 0.0073(8) 0.0100(8)
F32 0.0523(12) 0.0588(13) 0.0460(12) 0.0056(9) 0.0250(10) 0.0015(10)
F33 0.0804(15) 0.0634(13) 0.0249(11) 0.0031(9) 0.0147(10) -0.0151(11)
F34 0.0662(13) 0.0646(13) 0.0251(10) 0.0123(9) -0.0086(10) -0.0082(10)
F35 0.0406(11) 0.0469(11) 0.0316(10) 0.0074(8) -0.0034(8) 0.0113(8)
F36 0.0613(13) 0.0370(11) 0.0698(14) 0.0211(10) 0.0041(11) 0.0173(10)
F37 0.0843(17) 0.0520(14) 0.123(2) 0.0054(13) -0.0143(15) 0.0479(12)
F38 0.0455(14) 0.111(2) 0.123(2) -0.0208(16) 0.0061(14) 0.0465(13)
F39 0.0362(12) 0.1099(19) 0.0688(15) 0.0068(13) 0.0171(11) 0.0105(12)
F40 0.0391(11) 0.0513(12) 0.0530(12) 0.0198(9) 0.0113(9) 0.0063(9)
F41 0.0656(12) 0.0288(9) 0.0264(10) 0.0092(7) 0.0103(9) 0.0020(8)
F42 0.0565(12) 0.0298(10) 0.0438(11) 0.0015(8) 0.0097(9) -0.0026(9)
F43 0.0565(12) 0.0416(11) 0.0305(10) -0.0109(8) -0.0012(9) 0.0036(9)
F44 0.0639(13) 0.0464(11) 0.0207(10) 0.0015(8) 0.0090(8) 0.0130(9)
F45 0.0482(11) 0.0335(9) 0.0283(9) 0.0059(7) 0.0126(8) 0.0046(8)
B4 0.0260(17) 0.0212(17) 0.0240(18) 0.0016(14) 0.0015(14) 0.0054(13)
C79 0.0270(16) 0.0261(15) 0.0212(15) -0.0004(12) 0.0024(12) 0.0064(12)
C80 0.0337(17) 0.0254(16) 0.0280(17) 0.0057(13) 0.0025(13) 0.0088(13)
C81 0.0343(18) 0.0305(17) 0.0317(18) 0.0071(14) 0.0112(14) 0.0013(14)
C82 0.0229(17) 0.048(2) 0.0391(19) 0.0039(16) 0.0077(14) 0.0082(15)
C83 0.0315(18) 0.0349(18) 0.0422(19) 0.0082(15) 0.0061(15) 0.0130(14)
C84 0.0330(18) 0.0267(16) 0.0295(17) 0.0015(13) 0.0046(14) 0.0076(13)
C85 0.0241(15) 0.0229(15) 0.0289(17) 0.0025(13) 0.0059(13) 0.0041(12)
C86 0.0318(17) 0.0268(17) 0.0378(19) -0.0006(14) -0.0001(15) 0.0055(13)
C87 0.050(2) 0.0218(17) 0.055(2) 0.0009(16) 0.0113(18) 0.0107(15)
C88 0.042(2) 0.0326(19) 0.060(2) 0.0197(17) 0.0150(18) 0.0193(15)
C89 0.0292(17) 0.0339(18) 0.0413(19) 0.0156(15) 0.0067(15) 0.0090(14)
C90 0.0298(16) 0.0234(16) 0.0314(17) 0.0064(13) 0.0071(14) 0.0068(13)
C91 0.0246(15) 0.0232(15) 0.0261(16) -0.0001(12) 0.0038(13) 0.0086(12)
C92 0.0288(17) 0.0307(16) 0.0250(17) -0.0036(13) 0.0020(14) 0.0094(13)
C93 0.0288(17) 0.0435(19) 0.035(2) 0.0033(15) 0.0131(15) 0.0074(14)
C94 0.047(2) 0.059(2) 0.0254(19) 0.0081(16) 0.0171(16) 0.0126(17)
C95 0.0326(18) 0.063(2) 0.0186(17) 0.0002(15) -0.0006(14) 0.0097(16)
C96 0.0277(17) 0.0346(17) 0.0297(18) 0.0008(14) 0.0056(14) 0.0041(13)
F46 0.0357(10) 0.0449(11) 0.0554(12) 0.0291(9) 0.0069(9) 0.0083(8)
F47 0.0399(11) 0.0536(12) 0.0531(12) 0.0206(10) 0.0135(9) -0.0034(9)
F48 0.0270(10) 0.0774(14) 0.0774(15) 0.0246(12) 0.0200(10) 0.0114(9)
F49 0.0378(11) 0.0660(13) 0.0809(15) 0.0336(11) 0.0135(10) 0.0284(10)
F50 0.0372(10) 0.0325(9) 0.0504(11) 0.0191(8) 0.0102(8) 0.0112(8)
F51 0.0529(12) 0.0315(10) 0.0468(12) -0.0110(8) -0.0120(10) 0.0086(8)
F52 0.0840(16) 0.0280(11) 0.0788(16) -0.0111(10) -0.0020(12) 0.0187(10)
F53 0.0620(13) 0.0351(10) 0.0868(15) 0.0240(10) 0.0176(11) 0.0283(9)
F54 0.0364(10) 0.0482(11) 0.0513(12) 0.0218(9) 0.0023(9) 0.0155(8)
F55 0.0360(10) 0.0271(9) 0.0363(10) 0.0027(8) -0.0047(8) 0.0097(7)
F56 0.0268(9) 0.0504(11) 0.0319(10) -0.0019(8) 0.0023(8) 0.0014(8)
F57 0.0363(11) 0.0727(14) 0.0495(12) 0.0061(10) 0.0224(9) 0.0001(10)
F58 0.0566(13) 0.1140(18) 0.0361(12) 0.0229(12) 0.0238(10) 0.0149(12)
F59 0.0445(12) 0.1108(18) 0.0246(11) 0.0077(11) 0.0023(9) 0.0098(11)
F60 0.0305(10) 0.0506(11) 0.0307(10) 0.0009(8) 0.0015(8) -0.0011(8)
K3 0.0333(4) 0.0379(4) 0.0306(4) 0.0113(3) 0.0063(3) 0.0051(3)
O21 0.0488(14) 0.0431(13) 0.0415(14) 0.0097(11) 0.0105(11) 0.0098(11)
O22 0.0386(14) 0.0627(16) 0.0576(16) 0.0241(13) 0.0104(12) 0.0189(12)
O23 0.0341(13) 0.0671(17) 0.0498(15) 0.0186(12) 0.0064(11) 0.0006(12)
O24 0.0528(15) 0.0405(13) 0.0362(13) 0.0037(10) 0.0058(11) 0.0069(11)
O25 0.0394(13) 0.0451(14) 0.0387(13) 0.0119(10) 0.0079(11) 0.0099(10)
O26 0.0334(13) 0.0437(14) 0.0525(15) 0.0084(11) 0.0051(11) -0.0003(10)
C97 0.076(3) 0.050(2) 0.059(3) 0.0183(19) 0.028(2) 0.026(2)
C98 0.057(2) 0.062(3) 0.076(3) 0.033(2) 0.032(2) 0.033(2)
C99 0.045(2) 0.098(3) 0.062(3) 0.023(2) 0.006(2) 0.026(2)
C100 0.031(2) 0.091(3) 0.059(3) 0.015(2) 0.0061(18) 0.005(2)
C101 0.047(2) 0.068(3) 0.057(3) 0.007(2) -0.006(2) -0.012(2)
C102 0.062(3) 0.041(2) 0.046(2) -0.0051(17) -0.009(2) -0.0046(18)
C103 0.071(3) 0.0341(19) 0.045(2) 0.0065(16) 0.013(2) 0.0091(18)
C104 0.056(2) 0.044(2) 0.060(2) 0.0202(18) 0.019(2) 0.0190(18)
C105 0.044(2) 0.064(3) 0.051(2) 0.0089(19) 0.0053(19) 0.0178(18)
C106 0.0294(19) 0.067(3) 0.058(2) 0.0045(19) 0.0028(17) 0.0071(17)
C107 0.048(2) 0.049(2) 0.045(2) 0.0068(17) 0.0020(18) -0.0085(17)
C108 0.059(2) 0.0354(19) 0.037(2) 0.0048(16) -0.0006(18) -0.0043(17)
K4 0.0406(4) 0.0293(4) 0.0305(4) 0.0035(3) 0.0063(3) 0.0078(3)
O27 0.0580(15) 0.0300(12) 0.0382(13) 0.0100(10) 0.0126(11) 0.0115(10)
O28 0.0397(13) 0.0325(12) 0.0365(13) 0.0024(10) 0.0050(10) 0.0008(10)
O29 0.0387(13) 0.0406(13) 0.0349(12) 0.0043(10) 0.0066(10) 0.0118(10)
O30 0.0563(15) 0.0396(13) 0.0368(13) 0.0012(10) 0.0050(11) 0.0159(11)
O31 0.0395(13) 0.0372(12) 0.0367(13) 0.0057(10) 0.0070(10) 0.0130(10)
O32 0.0396(13) 0.0362(12) 0.0414(13) 0.0101(10) 0.0103(10) 0.0080(10)
C109 0.056(2) 0.038(2) 0.058(2) 0.0215(17) 0.0160(18) 0.0112(17)
C110 0.047(2) 0.0289(18) 0.057(2) 0.0091(16) 0.0173(18) 0.0043(15)
C111 0.0418(19) 0.0344(18) 0.041(2) -0.0040(15) 0.0025(16) 0.0114(15)
C112 0.049(2) 0.046(2) 0.0361(19) 0.0016(16) 0.0115(16) 0.0208(16)
C113 0.047(2) 0.049(2) 0.036(2) -0.0023(16) -0.0050(16) 0.0148(16)
C114 0.056(2) 0.051(2) 0.035(2) 0.0022(16) -0.0049(17) 0.0139(17)
C115 0.047(2) 0.040(2) 0.040(2) 0.0071(16) 0.0011(16) 0.0146(16)
C116 0.050(2) 0.043(2) 0.054(2) 0.0090(17) 0.0088(18) 0.0238(16)
C117 0.049(2) 0.0305(18) 0.039(2) -0.0052(15) 0.0069(16) 0.0093(15)
C118 0.055(2) 0.041(2) 0.040(2) 0.0000(16) 0.0172(17) 0.0148(16)
C119 0.044(2) 0.050(2) 0.0325(19) 0.0090(16) 0.0114(15) 0.0061(16)
C120 0.057(2) 0.045(2) 0.0330(19) 0.0138(16) 0.0106(16) 0.0075(17)
C121 0.120(5) 0.080(3) 0.089(4) 0.019(3) 0.014(3) 0.045(3)
Cl1 0.1044(11) 0.0733(9) 0.0597(8) 0.0190(6) 0.0223(7) 0.0395(7)
Cl2 0.1236(14) 0.0935(12) 0.1538(17) 0.0479(11) 0.0569(12) 0.0316(10)
C122 0.081(3) 0.078(3) 0.082(3) 0.034(3) 0.015(3) 0.031(2)
Cl3 0.0784(7) 0.0791(7) 0.0555(6) 0.0236(5) 0.0213(5) 0.0357(6)
Cl4A 0.0864(16) 0.0673(9) 0.095(2) 0.0294(12) 0.0384(15) 0.0239(10)
Cl4B 0.0864(16) 0.0673(9) 0.095(2) 0.0294(12) 0.0384(15) 0.0239(10)
C123 0.120(5) 0.080(3) 0.089(4) 0.019(3) 0.014(3) 0.045(3)
Cl5 0.124(3) 0.107(3) 0.195(4) 0.050(2) 0.060(3) 0.0060(19)
Cl6 0.151(5) 0.171(4) 0.222(7) 0.068(5) 0.045(4) 0.009(4)
C124 0.120(5) 0.080(3) 0.089(4) 0.019(3) 0.014(3) 0.045(3)
Cl7 0.151(5) 0.171(4) 0.222(7) 0.068(5) 0.045(4) 0.009(4)
Cl8 0.124(3) 0.107(3) 0.195(4) 0.050(2) 0.060(3) 0.0060(19)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
S1 O4 1.422(2) . ?
S1 O3 1.428(2) . ?
S1 O1 1.521(2) . ?
S1 O2 1.5324(19) . ?
O1 B1 1.523(4) . ?
O2 B2 1.524(4) . ?
O3 K1 2.619(2) . ?
B1 C7 1.649(4) . ?
B1 C1 1.650(4) . ?
B1 C13 1.652(4) . ?
C1 C2 1.366(4) . ?
C1 C6 1.384(4) . ?
C2 F1 1.344(3) . ?
C2 C3 1.375(4) . ?
C3 F2 1.340(4) . ?
C3 C4 1.364(5) . ?
C4 F3 1.346(4) . ?
C4 C5 1.357(5) . ?
C5 F4 1.352(4) . ?
C5 C6 1.368(4) . ?
C6 F5 1.351(4) . ?
C7 C12 1.377(4) . ?
C7 C8 1.386(4) . ?
C8 F6 1.345(4) . ?
C8 C9 1.386(4) . ?
C9 C10 1.352(5) . ?
C9 F7 1.353(4) . ?
C10 F8 1.349(3) . ?
C10 C11 1.365(5) . ?
C11 F9 1.340(4) . ?
C11 C12 1.378(4) . ?
C12 F10 1.351(3) . ?
C13 C14 1.372(4) . ?
C13 C18 1.387(4) . ?
C14 F11 1.367(3) . ?
C14 C15 1.372(4) . ?
C15 F12 1.345(4) . ?
C15 C16 1.378(5) . ?
C16 F13 1.337(4) . ?
C16 C17 1.355(5) . ?
C17 F14 1.355(4) . ?
C17 C18 1.370(4) . ?
C18 F15 1.337(3) . ?
F10 K2 3.096(2) . ?
B2 C25 1.626(4) . ?
B2 C19 1.656(4) . ?
B2 C31 1.659(4) . ?
C19 C20 1.378(4) . ?
C19 C24 1.385(4) . ?
C20 F16 1.342(3) . ?
C20 C21 1.378(4) . ?
C21 F17 1.350(3) . ?
C21 C22 1.360(4) . ?
C22 F18 1.344(3) . ?
C22 C23 1.384(5) . ?
C23 F19 1.346(4) . ?
C23 C24 1.361(4) . ?
C24 F20 1.365(3) . ?
C25 C26 1.377(4) . ?
C25 C30 1.389(4) . ?
C26 F21 1.353(3) . ?
C26 C27 1.370(4) . ?
C27 F22 1.337(3) . ?
C27 C28 1.380(4) . ?
C28 F23 1.340(3) . ?
C28 C29 1.363(4) . ?
C29 F24 1.357(3) . ?
C29 C30 1.358(4) . ?
C30 F25 1.351(3) . ?
C31 C32 1.366(4) . ?
C31 C36 1.391(4) . ?
C32 F26 1.359(3) . ?
C32 C33 1.377(4) . ?
C33 F27 1.329(3) . ?
C33 C34 1.376(4) . ?
C34 C35 1.351(4) . ?
C34 F28 1.352(3) . ?
C35 F29 1.353(4) . ?
C35 C36 1.383(4) . ?
C36 F30 1.348(3) . ?
F26 K2 2.758(2) . ?
K1 O9 2.757(2) . ?
K1 O13 2.772(2) . ?
K1 O11 2.776(2) . ?
K1 O12 2.806(3) . ?
K1 O10 2.899(2) . ?
K1 O14 2.916(2) . ?
K1 Cl1 3.3387(17) . ?
K1 C47 3.511(3) . ?
O9 C48 1.411(4) . ?
O9 C37 1.416(4) . ?
O10 C39 1.423(4) . ?
O10 C38 1.426(4) . ?
O11 C41 1.422(4) . ?
O11 C40 1.425(4) . ?
O12 C42 1.413(4) . ?
O12 C43 1.427(4) . ?
O13 C44 1.414(4) . ?
O13 C45 1.420(4) . ?
O14 C47 1.416(4) . ?
O14 C46 1.427(4) . ?
C37 C38 1.491(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.479(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.475(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.476(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.484(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.503(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
K2 O18 2.777(2) . ?
K2 O15 2.801(3) . ?
K2 O20 2.813(3) . ?
K2 O19 2.830(2) . ?
K2 O17 2.863(2) . ?
K2 O16 2.883(3) . ?
O15 C49 1.411(5) . ?
O15 C60 1.420(5) . ?
O16 C51 1.420(4) . ?
O16 C50 1.426(4) . ?
O17 C52 1.413(4) . ?
O17 C53 1.415(4) . ?
O18 C55 1.412(4) . ?
O18 C54 1.419(4) . ?
O19 C56 1.411(4) . ?
O19 C57 1.428(4) . ?
O20 C59 1.420(4) . ?
O20 C58 1.423(4) . ?
C49 C50 1.475(6) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.481(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.506(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.489(5) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.483(5) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.499(6) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
S2 O7 1.420(2) . ?
S2 O8 1.426(2) . ?
S2 O5 1.5150(19) . ?
S2 O6 1.5340(19) . ?
O5 B3 1.524(4) . ?
O6 B4 1.520(4) . ?
O7 K3 2.632(2) . ?
O8 K4 2.924(2) . ?
B3 C67 1.636(4) . ?
B3 C73 1.645(4) . ?
B3 C61 1.645(4) . ?
C61 C62 1.376(4) . ?
C61 C66 1.389(4) . ?
C62 F31 1.353(3) . ?
C62 C63 1.370(4) . ?
C63 F32 1.334(4) . ?
C63 C64 1.387(5) . ?
C64 F33 1.344(3) . ?
C64 C65 1.353(5) . ?
C65 F34 1.350(4) . ?
C65 C66 1.393(4) . ?
C66 F35 1.340(3) . ?
C67 C72 1.374(4) . ?
C67 C68 1.395(4) . ?
C68 F36 1.341(4) . ?
C68 C69 1.352(5) . ?
C69 F37 1.345(4) . ?
C69 C70 1.359(6) . ?
C70 F38 1.343(4) . ?
C70 C71 1.370(5) . ?
C71 F39 1.347(4) . ?
C71 C72 1.381(4) . ?
C72 F40 1.355(3) . ?
C73 C74 1.375(4) . ?
C73 C78 1.390(4) . ?
C74 F41 1.350(3) . ?
C74 C75 1.384(4) . ?
C75 F42 1.347(3) . ?
C75 C76 1.365(4) . ?
C76 F43 1.339(3) . ?
C76 C77 1.363(4) . ?
C77 F44 1.357(3) . ?
C77 C78 1.370(4) . ?
C78 F45 1.346(3) . ?
F31 K4 3.157(2) . ?
B4 C79 1.638(4) . ?
B4 C85 1.648(4) . ?
B4 C91 1.657(4) . ?
C79 C80 1.382(4) . ?
C79 C84 1.383(4) . ?
C80 F46 1.356(3) . ?
C80 C81 1.368(4) . ?
C81 F47 1.346(3) . ?
C81 C82 1.367(4) . ?
C82 F48 1.338(3) . ?
C82 C83 1.365(4) . ?
C83 F49 1.351(3) . ?
C83 C84 1.374(4) . ?
C84 F50 1.348(3) . ?
C85 C86 1.385(4) . ?
C85 C90 1.388(4) . ?
C86 F51 1.355(3) . ?
C86 C87 1.367(4) . ?
C87 F52 1.346(4) . ?
C87 C88 1.365(5) . ?
C88 F53 1.351(3) . ?
C88 C89 1.365(4) . ?
C89 F54 1.348(3) . ?
C89 C90 1.382(4) . ?
C90 F55 1.341(3) . ?
C91 C92 1.378(4) . ?
C91 C96 1.383(4) . ?
C92 F56 1.362(3) . ?
C92 C93 1.373(4) . ?
C93 F57 1.336(3) . ?
C93 C94 1.370(4) . ?
C94 F58 1.349(4) . ?
C94 C95 1.357(5) . ?
C95 F59 1.348(3) . ?
C95 C96 1.386(4) . ?
C96 F60 1.347(3) . ?
F55 K4 3.027(2) . ?
F56 K4 2.964(2) . ?
K3 O26 2.750(2) . ?
K3 O24 2.776(2) . ?
K3 O22 2.784(2) . ?
K3 O23 2.803(3) . ?
K3 O21 2.911(3) . ?
K3 O25 2.913(2) . ?
K3 Cl3 3.3424(16) . ?
K3 C105 3.516(4) . ?
K3 C101 3.519(4) . ?
O21 C97 1.412(4) . ?
O21 C108 1.422(4) . ?
O22 C99 1.417(4) . ?
O22 C98 1.418(4) . ?
O23 C100 1.424(4) . ?
O23 C101 1.430(4) . ?
O24 C103 1.401(4) . ?
O24 C102 1.406(4) . ?
O25 C105 1.412(4) . ?
O25 C104 1.425(4) . ?
O26 C106 1.408(4) . ?
O26 C107 1.422(4) . ?
C97 C98 1.482(5) . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C99 C100 1.468(6) . ?
C99 H99A 0.9900 . ?
C99 H99B 0.9900 . ?
C100 H10A 0.9900 . ?
C100 H10B 0.9900 . ?
C101 C102 1.481(5) . ?
C101 H10C 0.9900 . ?
C101 H10D 0.9900 . ?
C102 H10E 0.9900 . ?
C102 H10F 0.9900 . ?
C103 C104 1.483(5) . ?
C103 H10G 0.9900 . ?
C103 H10H 0.9900 . ?
C104 H10I 0.9900 . ?
C104 H10J 0.9900 . ?
C105 C106 1.484(5) . ?
C105 H10K 0.9900 . ?
C105 H10L 0.9900 . ?
C106 H10M 0.9900 . ?
C106 H10N 0.9900 . ?
C107 C108 1.475(5) . ?
C107 H10O 0.9900 . ?
C107 H10P 0.9900 . ?
C108 H10Q 0.9900 . ?
C108 H10R 0.9900 . ?
K4 O29 2.879(2) . ?
K4 O27 2.881(2) . ?
K4 O28 2.927(2) . ?
K4 O31 2.968(2) . ?
K4 O32 2.971(2) . ?
K4 O30 2.972(2) . ?
O27 C109 1.415(4) . ?
O27 C120 1.416(4) . ?
O28 C111 1.410(4) . ?
O28 C110 1.423(4) . ?
O29 C113 1.420(4) . ?
O29 C112 1.423(4) . ?
O30 C115 1.403(4) . ?
O30 C114 1.432(4) . ?
O31 C117 1.418(4) . ?
O31 C116 1.427(4) . ?
O32 C118 1.407(4) . ?
O32 C119 1.412(4) . ?
C109 C110 1.485(5) . ?
C109 H10S 0.9900 . ?
C109 H10T 0.9900 . ?
C110 H11A 0.9900 . ?
C110 H11B 0.9900 . ?
C111 C112 1.486(5) . ?
C111 H11C 0.9900 . ?
C111 H11D 0.9900 . ?
C112 H11E 0.9900 . ?
C112 H11F 0.9900 . ?
C113 C114 1.484(4) . ?
C113 H11G 0.9900 . ?
C113 H11H 0.9900 . ?
C114 H11I 0.9900 . ?
C114 H11J 0.9900 . ?
C115 C116 1.486(5) . ?
C115 H11K 0.9900 . ?
C115 H11L 0.9900 . ?
C116 H11M 0.9900 . ?
C116 H11N 0.9900 . ?
C117 C118 1.491(5) . ?
C117 H11O 0.9900 . ?
C117 H11P 0.9900 . ?
C118 H11Q 0.9900 . ?
C118 H11R 0.9900 . ?
C119 C120 1.496(4) . ?
C119 H11S 0.9900 . ?
C119 H11T 0.9900 . ?
C120 H12A 0.9900 . ?
C120 H12B 0.9900 . ?
C121 Cl2 1.603(6) . ?
C121 Cl1 1.760(6) . ?
C121 H12C 0.9900 . ?
C121 H12D 0.9900 . ?
C122 Cl4B 1.653(9) . ?
C122 Cl4A 1.722(5) . ?
C122 Cl3 1.734(4) . ?
C122 H12E 0.9900 . ?
C122 H12F 0.9900 . ?
C122 H12G 0.9900 . ?
C122 H12H 0.9900 . ?
C123 Cl6 1.490(13) . ?
C123 Cl5 1.861(13) . ?
C123 H90A 0.9900 . ?
C123 H90B 0.9900 . ?
C124 Cl7 1.83(2) . ?
C124 Cl8 1.97(3) . ?
C124 H90C 0.9900 . ?
C124 H90D 0.9900 . ?
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 S1 O3 117.12(12) . . ?
O4 S1 O1 111.36(11) . . ?
O3 S1 O1 106.18(12) . . ?
O4 S1 O2 107.88(12) . . ?
O3 S1 O2 109.50(11) . . ?
O1 S1 O2 104.02(11) . . ?
S1 O1 B1 134.58(18) . . ?
B2 O2 S1 128.78(17) . . ?
S1 O3 K1 151.84(12) . . ?
O1 B1 C7 106.1(2) . . ?
O1 B1 C1 105.3(2) . . ?
C7 B1 C1 114.3(2) . . ?
O1 B1 C13 111.0(2) . . ?
C7 B1 C13 114.3(2) . . ?
C1 B1 C13 105.5(2) . . ?
C2 C1 C6 113.3(3) . . ?
C2 C1 B1 127.2(3) . . ?
C6 C1 B1 119.3(3) . . ?
F1 C2 C1 121.5(3) . . ?
F1 C2 C3 114.9(3) . . ?
C1 C2 C3 123.6(3) . . ?
F2 C3 C4 119.5(3) . . ?
F2 C3 C2 120.3(3) . . ?
C4 C3 C2 120.2(3) . . ?
F3 C4 C5 120.9(3) . . ?
F3 C4 C3 120.4(4) . . ?
C5 C4 C3 118.7(3) . . ?
F4 C5 C4 119.8(3) . . ?
F4 C5 C6 121.0(3) . . ?
C4 C5 C6 119.2(3) . . ?
F5 C6 C5 115.8(3) . . ?
F5 C6 C1 119.5(3) . . ?
C5 C6 C1 124.7(3) . . ?
C12 C7 C8 113.7(3) . . ?
C12 C7 B1 120.7(2) . . ?
C8 C7 B1 125.3(3) . . ?
F6 C8 C7 121.1(3) . . ?
F6 C8 C9 115.6(3) . . ?
C7 C8 C9 123.3(3) . . ?
C10 C9 F7 119.7(3) . . ?
C10 C9 C8 119.8(3) . . ?
F7 C9 C8 120.4(3) . . ?
F8 C10 C9 120.5(3) . . ?
F8 C10 C11 119.9(3) . . ?
C9 C10 C11 119.5(3) . . ?
F9 C11 C10 120.6(3) . . ?
F9 C11 C12 120.2(3) . . ?
C10 C11 C12 119.2(3) . . ?
F10 C12 C7 120.2(2) . . ?
F10 C12 C11 115.5(3) . . ?
C7 C12 C11 124.4(3) . . ?
C14 C13 C18 113.4(3) . . ?
C14 C13 B1 125.7(3) . . ?
C18 C13 B1 120.8(3) . . ?
F11 C14 C15 114.4(3) . . ?
F11 C14 C13 121.1(3) . . ?
C15 C14 C13 124.5(3) . . ?
F12 C15 C14 120.8(3) . . ?
F12 C15 C16 119.8(3) . . ?
C14 C15 C16 119.3(3) . . ?
F13 C16 C17 121.6(3) . . ?
F13 C16 C15 119.7(3) . . ?
C17 C16 C15 118.7(3) . . ?
F14 C17 C16 119.3(3) . . ?
F14 C17 C18 120.7(3) . . ?
C16 C17 C18 120.0(3) . . ?
F15 C18 C17 116.2(3) . . ?
F15 C18 C13 119.8(3) . . ?
C17 C18 C13 124.0(3) . . ?
C12 F10 K2 135.17(15) . . ?
O2 B2 C25 108.8(2) . . ?
O2 B2 C19 111.8(2) . . ?
C25 B2 C19 113.2(2) . . ?
O2 B2 C31 103.1(2) . . ?
C25 B2 C31 113.6(2) . . ?
C19 B2 C31 105.9(2) . . ?
C20 C19 C24 113.4(3) . . ?
C20 C19 B2 128.0(2) . . ?
C24 C19 B2 118.5(3) . . ?
F16 C20 C21 115.1(3) . . ?
F16 C20 C19 121.2(2) . . ?
C21 C20 C19 123.7(3) . . ?
F17 C21 C22 118.8(3) . . ?
F17 C21 C20 120.9(3) . . ?
C22 C21 C20 120.3(3) . . ?
F18 C22 C21 121.1(3) . . ?
F18 C22 C23 120.3(3) . . ?
C21 C22 C23 118.6(3) . . ?
F19 C23 C24 121.4(3) . . ?
F19 C23 C22 119.6(3) . . ?
C24 C23 C22 119.0(3) . . ?
C23 C24 F20 116.3(3) . . ?
C23 C24 C19 125.0(3) . . ?
F20 C24 C19 118.6(2) . . ?
C26 C25 C30 113.0(3) . . ?
C26 C25 B2 126.8(3) . . ?
C30 C25 B2 120.1(2) . . ?
F21 C26 C27 115.0(3) . . ?
F21 C26 C25 120.6(3) . . ?
C27 C26 C25 124.4(3) . . ?
F22 C27 C26 121.3(3) . . ?
F22 C27 C28 119.4(3) . . ?
C26 C27 C28 119.3(3) . . ?
F23 C28 C29 121.1(3) . . ?
F23 C28 C27 120.1(3) . . ?
C29 C28 C27 118.8(3) . . ?
F24 C29 C30 120.4(3) . . ?
F24 C29 C28 120.0(3) . . ?
C30 C29 C28 119.6(3) . . ?
F25 C30 C29 115.7(3) . . ?
F25 C30 C25 119.4(3) . . ?
C29 C30 C25 124.8(3) . . ?
C32 C31 C36 112.8(3) . . ?
C32 C31 B2 119.8(2) . . ?
C36 C31 B2 127.3(2) . . ?
F26 C32 C31 119.2(3) . . ?
F26 C32 C33 115.3(2) . . ?
C31 C32 C33 125.5(3) . . ?
F27 C33 C34 119.8(3) . . ?
F27 C33 C32 121.6(3) . . ?
C34 C33 C32 118.6(3) . . ?
C35 C34 F28 120.4(3) . . ?
C35 C34 C33 119.3(3) . . ?
F28 C34 C33 120.3(3) . . ?
C34 C35 F29 119.9(3) . . ?
C34 C35 C36 119.7(3) . . ?
F29 C35 C36 120.4(3) . . ?
F30 C36 C35 114.4(3) . . ?
F30 C36 C31 121.6(3) . . ?
C35 C36 C31 124.0(3) . . ?
C32 F26 K2 146.58(16) . . ?
O3 K1 O9 103.86(7) . . ?
O3 K1 O13 84.63(7) . . ?
O9 K1 O13 116.24(7) . . ?
O3 K1 O11 107.17(7) . . ?
O9 K1 O11 116.96(7) . . ?
O13 K1 O11 120.08(7) . . ?
O3 K1 O12 103.17(7) . . ?
O9 K1 O12 152.12(7) . . ?
O13 K1 O12 59.92(7) . . ?
O11 K1 O12 60.19(7) . . ?
O3 K1 O10 122.62(7) . . ?
O9 K1 O10 58.64(7) . . ?
O13 K1 O10 152.62(7) . . ?
O11 K1 O10 58.36(7) . . ?
O12 K1 O10 110.68(7) . . ?
O3 K1 O14 90.23(7) . . ?
O9 K1 O14 58.24(7) . . ?
O13 K1 O14 58.68(7) . . ?
O11 K1 O14 162.53(7) . . ?
O12 K1 O14 115.09(7) . . ?
O10 K1 O14 113.68(7) . . ?
O3 K1 Cl1 156.80(5) . . ?
O9 K1 Cl1 84.21(6) . . ?
O13 K1 Cl1 72.37(6) . . ?
O11 K1 Cl1 87.56(6) . . ?
O12 K1 Cl1 68.16(6) . . ?
O10 K1 Cl1 80.27(5) . . ?
O14 K1 Cl1 75.41(5) . . ?
O3 K1 C47 81.29(8) . . ?
O9 K1 C47 42.08(7) . . ?
O13 K1 C47 79.29(8) . . ?
O11 K1 C47 158.94(8) . . ?
O12 K1 C47 137.92(7) . . ?
O10 K1 C47 100.71(8) . . ?
O14 K1 C47 23.17(7) . . ?
Cl1 K1 C47 91.23(7) . . ?
C48 O9 C37 113.0(2) . . ?
C48 O9 K1 121.54(18) . . ?
C37 O9 K1 120.88(18) . . ?
C39 O10 C38 111.4(2) . . ?
C39 O10 K1 106.62(17) . . ?
C38 O10 K1 112.87(17) . . ?
C41 O11 C40 111.5(2) . . ?
C41 O11 K1 117.20(19) . . ?
C40 O11 K1 121.12(18) . . ?
C42 O12 C43 112.4(3) . . ?
C42 O12 K1 110.78(19) . . ?
C43 O12 K1 111.39(19) . . ?
C44 O13 C45 113.7(2) . . ?
C44 O13 K1 118.25(18) . . ?
C45 O13 K1 120.98(18) . . ?
C47 O14 C46 112.7(2) . . ?
C47 O14 K1 102.71(17) . . ?
C46 O14 K1 107.00(17) . . ?
O9 C37 C38 108.4(3) . . ?
O9 C37 H37A 110.0 . . ?
C38 C37 H37A 110.0 . . ?
O9 C37 H37B 110.0 . . ?
C38 C37 H37B 110.0 . . ?
H37A C37 H37B 108.4 . . ?
O10 C38 C37 109.0(3) . . ?
O10 C38 H38A 109.9 . . ?
C37 C38 H38A 109.9 . . ?
O10 C38 H38B 109.9 . . ?
C37 C38 H38B 109.9 . . ?
H38A C38 H38B 108.3 . . ?
O10 C39 C40 108.2(3) . . ?
O10 C39 H39A 110.1 . . ?
C40 C39 H39A 110.1 . . ?
O10 C39 H39B 110.1 . . ?
C40 C39 H39B 110.1 . . ?
H39A C39 H39B 108.4 . . ?
O11 C40 C39 108.3(3) . . ?
O11 C40 H40A 110.0 . . ?
C39 C40 H40A 110.0 . . ?
O11 C40 H40B 110.0 . . ?
C39 C40 H40B 110.0 . . ?
H40A C40 H40B 108.4 . . ?
O11 C41 C42 109.3(3) . . ?
O11 C41 H41A 109.8 . . ?
C42 C41 H41A 109.8 . . ?
O11 C41 H41B 109.8 . . ?
C42 C41 H41B 109.8 . . ?
H41A C41 H41B 108.3 . . ?
O12 C42 C41 109.0(3) . . ?
O12 C42 H42A 109.9 . . ?
C41 C42 H42A 109.9 . . ?
O12 C42 H42B 109.9 . . ?
C41 C42 H42B 109.9 . . ?
H42A C42 H42B 108.3 . . ?
O12 C43 C44 109.1(3) . . ?
O12 C43 H43A 109.9 . . ?
C44 C43 H43A 109.9 . . ?
O12 C43 H43B 109.9 . . ?
C44 C43 H43B 109.9 . . ?
H43A C43 H43B 108.3 . . ?
O13 C44 C43 108.7(3) . . ?
O13 C44 H44A 110.0 . . ?
C43 C44 H44A 110.0 . . ?
O13 C44 H44B 110.0 . . ?
C43 C44 H44B 110.0 . . ?
H44A C44 H44B 108.3 . . ?
O13 C45 C46 108.3(3) . . ?
O13 C45 H45A 110.0 . . ?
C46 C45 H45A 110.0 . . ?
O13 C45 H45B 110.0 . . ?
C46 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
O14 C46 C45 108.4(3) . . ?
O14 C46 H46A 110.0 . . ?
C45 C46 H46A 110.0 . . ?
O14 C46 H46B 110.0 . . ?
C45 C46 H46B 110.0 . . ?
H46A C46 H46B 108.4 . . ?
O14 C47 C48 107.5(3) . . ?
O14 C47 K1 54.12(14) . . ?
C48 C47 K1 84.98(18) . . ?
O14 C47 H47A 110.2 . . ?
C48 C47 H47A 110.2 . . ?
K1 C47 H47A 162.0 . . ?
O14 C47 H47B 110.2 . . ?
C48 C47 H47B 110.2 . . ?
K1 C47 H47B 73.4 . . ?
H47A C47 H47B 108.5 . . ?
O9 C48 C47 107.9(3) . . ?
O9 C48 H48A 110.1 . . ?
C47 C48 H48A 110.1 . . ?
O9 C48 H48B 110.1 . . ?
C47 C48 H48B 110.1 . . ?
H48A C48 H48B 108.4 . . ?
F26 K2 O18 80.91(7) . . ?
F26 K2 O15 115.13(7) . . ?
O18 K2 O15 157.75(8) . . ?
F26 K2 O20 134.77(7) . . ?
O18 K2 O20 119.52(8) . . ?
O15 K2 O20 61.02(9) . . ?
F26 K2 O19 122.21(7) . . ?
O18 K2 O19 59.90(7) . . ?
O15 K2 O19 116.21(8) . . ?
O20 K2 O19 59.63(7) . . ?
F26 K2 O17 64.99(6) . . ?
O18 K2 O17 60.01(7) . . ?
O15 K2 O17 111.13(9) . . ?
O20 K2 O17 159.98(7) . . ?
O19 K2 O17 116.35(7) . . ?
F26 K2 O16 108.57(7) . . ?
O18 K2 O16 103.19(8) . . ?
O15 K2 O16 58.20(9) . . ?
O20 K2 O16 105.10(8) . . ?
O19 K2 O16 119.91(7) . . ?
O17 K2 O16 58.37(7) . . ?
F26 K2 F10 68.38(6) . . ?
O18 K2 F10 123.93(6) . . ?
O15 K2 F10 77.76(8) . . ?
O20 K2 F10 66.92(7) . . ?
O19 K2 F10 98.68(6) . . ?
O17 K2 F10 131.63(6) . . ?
O16 K2 F10 130.25(7) . . ?
C49 O15 C60 113.2(3) . . ?
C49 O15 K2 115.1(2) . . ?
C60 O15 K2 110.6(2) . . ?
C51 O16 C50 111.8(3) . . ?
C51 O16 K2 117.0(2) . . ?
C50 O16 K2 116.1(2) . . ?
C52 O17 C53 112.9(2) . . ?
C52 O17 K2 113.51(19) . . ?
C53 O17 K2 110.96(17) . . ?
C55 O18 C54 112.9(3) . . ?
C55 O18 K2 117.78(18) . . ?
C54 O18 K2 121.09(18) . . ?
C56 O19 C57 112.2(3) . . ?
C56 O19 K2 108.84(17) . . ?
C57 O19 K2 110.3(2) . . ?
C59 O20 C58 112.5(3) . . ?
C59 O20 K2 117.4(2) . . ?
C58 O20 K2 117.40(19) . . ?
O15 C49 C50 107.4(3) . . ?
O15 C49 H49A 110.2 . . ?
C50 C49 H49A 110.2 . . ?
O15 C49 H49B 110.2 . . ?
C50 C49 H49B 110.2 . . ?
H49A C49 H49B 108.5 . . ?
O16 C50 C49 109.0(3) . . ?
O16 C50 H50A 109.9 . . ?
C49 C50 H50A 109.9 . . ?
O16 C50 H50B 109.9 . . ?
C49 C50 H50B 109.9 . . ?
H50A C50 H50B 108.3 . . ?
O16 C51 C52 109.8(3) . . ?
O16 C51 H51A 109.7 . . ?
C52 C51 H51A 109.7 . . ?
O16 C51 H51B 109.7 . . ?
C52 C51 H51B 109.7 . . ?
H51A C51 H51B 108.2 . . ?
O17 C52 C51 108.8(3) . . ?
O17 C52 H52A 109.9 . . ?
C51 C52 H52A 109.9 . . ?
O17 C52 H52B 109.9 . . ?
C51 C52 H52B 109.9 . . ?
H52A C52 H52B 108.3 . . ?
O17 C53 C54 113.7(3) . . ?
O17 C53 H53A 108.8 . . ?
C54 C53 H53A 108.8 . . ?
O17 C53 H53B 108.8 . . ?
C54 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
O18 C54 C53 107.7(3) . . ?
O18 C54 H54A 110.2 . . ?
C53 C54 H54A 110.2 . . ?
O18 C54 H54B 110.2 . . ?
C53 C54 H54B 110.2 . . ?
H54A C54 H54B 108.5 . . ?
O18 C55 C56 109.1(3) . . ?
O18 C55 H55A 109.9 . . ?
C56 C55 H55A 109.9 . . ?
O18 C55 H55B 109.9 . . ?
C56 C55 H55B 109.9 . . ?
H55A C55 H55B 108.3 . . ?
O19 C56 C55 108.1(3) . . ?
O19 C56 H56A 110.1 . . ?
C55 C56 H56A 110.1 . . ?
O19 C56 H56B 110.1 . . ?
C55 C56 H56B 110.1 . . ?
H56A C56 H56B 108.4 . . ?
O19 C57 C58 108.5(3) . . ?
O19 C57 H57A 110.0 . . ?
C58 C57 H57A 110.0 . . ?
O19 C57 H57B 110.0 . . ?
C58 C57 H57B 110.0 . . ?
H57A C57 H57B 108.4 . . ?
O20 C58 C57 108.1(3) . . ?
O20 C58 H58A 110.1 . . ?
C57 C58 H58A 110.1 . . ?
O20 C58 H58B 110.1 . . ?
C57 C58 H58B 110.1 . . ?
H58A C58 H58B 108.4 . . ?
O20 C59 C60 107.4(3) . . ?
O20 C59 H59A 110.2 . . ?
C60 C59 H59A 110.2 . . ?
O20 C59 H59B 110.2 . . ?
C60 C59 H59B 110.2 . . ?
H59A C59 H59B 108.5 . . ?
O15 C60 C59 113.4(3) . . ?
O15 C60 H60A 108.9 . . ?
C59 C60 H60A 108.9 . . ?
O15 C60 H60B 108.9 . . ?
C59 C60 H60B 108.9 . . ?
H60A C60 H60B 107.7 . . ?
O7 S2 O8 117.01(12) . . ?
O7 S2 O5 106.74(11) . . ?
O8 S2 O5 111.36(11) . . ?
O7 S2 O6 109.80(11) . . ?
O8 S2 O6 107.06(11) . . ?
O5 S2 O6 104.13(10) . . ?
S2 O5 B3 133.37(18) . . ?
B4 O6 S2 128.70(17) . . ?
S2 O7 K3 152.96(12) . . ?
S2 O8 K4 123.26(10) . . ?
O5 B3 C67 106.4(2) . . ?
O5 B3 C73 111.2(2) . . ?
C67 B3 C73 103.2(2) . . ?
O5 B3 C61 108.0(2) . . ?
C67 B3 C61 112.5(2) . . ?
C73 B3 C61 115.1(2) . . ?
C62 C61 C66 113.6(3) . . ?
C62 C61 B3 122.2(3) . . ?
C66 C61 B3 124.1(3) . . ?
F31 C62 C63 115.5(3) . . ?
F31 C62 C61 119.7(2) . . ?
C63 C62 C61 124.7(3) . . ?
F32 C63 C62 121.5(3) . . ?
F32 C63 C64 119.0(3) . . ?
C62 C63 C64 119.4(3) . . ?
F33 C64 C65 120.5(3) . . ?
F33 C64 C63 120.9(3) . . ?
C65 C64 C63 118.6(3) . . ?
F34 C65 C64 119.8(3) . . ?
F34 C65 C66 120.1(3) . . ?
C64 C65 C66 120.1(3) . . ?
F35 C66 C61 121.6(3) . . ?
F35 C66 C65 114.9(3) . . ?
C61 C66 C65 123.4(3) . . ?
C72 C67 C68 113.2(3) . . ?
C72 C67 B3 127.4(3) . . ?
C68 C67 B3 119.2(3) . . ?
F36 C68 C69 116.6(3) . . ?
F36 C68 C67 118.4(3) . . ?
C69 C68 C67 124.9(4) . . ?
F37 C69 C68 120.8(4) . . ?
F37 C69 C70 119.6(3) . . ?
C68 C69 C70 119.6(3) . . ?
F38 C70 C69 120.9(4) . . ?
F38 C70 C71 120.1(4) . . ?
C69 C70 C71 118.9(3) . . ?
F39 C71 C70 120.1(3) . . ?
F39 C71 C72 120.0(3) . . ?
C70 C71 C72 119.8(3) . . ?
F40 C72 C67 121.6(3) . . ?
F40 C72 C71 114.9(3) . . ?
C67 C72 C71 123.5(3) . . ?
C74 C73 C78 113.0(2) . . ?
C74 C73 B3 126.6(2) . . ?
C78 C73 B3 119.8(2) . . ?
F41 C74 C73 121.4(2) . . ?
F41 C74 C75 114.8(2) . . ?
C73 C74 C75 123.8(3) . . ?
F42 C75 C76 119.9(3) . . ?
F42 C75 C74 119.9(3) . . ?
C76 C75 C74 120.2(3) . . ?
F43 C76 C77 121.2(3) . . ?
F43 C76 C75 120.4(3) . . ?
C77 C76 C75 118.5(3) . . ?
F44 C77 C76 119.4(3) . . ?
F44 C77 C78 120.9(3) . . ?
C76 C77 C78 119.7(3) . . ?
F45 C78 C77 115.5(2) . . ?
F45 C78 C73 119.8(2) . . ?
C77 C78 C73 124.7(3) . . ?
C62 F31 K4 149.73(15) . . ?
O6 B4 C79 109.2(2) . . ?
O6 B4 C85 111.4(2) . . ?
C79 B4 C85 113.8(2) . . ?
O6 B4 C91 102.8(2) . . ?
C79 B4 C91 113.3(2) . . ?
C85 B4 C91 105.9(2) . . ?
C80 C79 C84 113.1(3) . . ?
C80 C79 B4 126.2(2) . . ?
C84 C79 B4 120.6(2) . . ?
F46 C80 C81 115.4(3) . . ?
F46 C80 C79 120.5(3) . . ?
C81 C80 C79 124.1(3) . . ?
F47 C81 C82 119.6(3) . . ?
F47 C81 C80 120.5(3) . . ?
C82 C81 C80 119.9(3) . . ?
F48 C82 C83 120.6(3) . . ?
F48 C82 C81 120.4(3) . . ?
C83 C82 C81 119.0(3) . . ?
F49 C83 C82 120.4(3) . . ?
F49 C83 C84 120.5(3) . . ?
C82 C83 C84 119.1(3) . . ?
F50 C84 C83 115.7(3) . . ?
F50 C84 C79 119.6(3) . . ?
C83 C84 C79 124.7(3) . . ?
C86 C85 C90 113.2(3) . . ?
C86 C85 B4 118.4(2) . . ?
C90 C85 B4 128.4(2) . . ?
F51 C86 C87 116.7(3) . . ?
F51 C86 C85 118.5(3) . . ?
C87 C86 C85 124.7(3) . . ?
F52 C87 C88 120.2(3) . . ?
F52 C87 C86 120.3(3) . . ?
C88 C87 C86 119.6(3) . . ?
F53 C88 C89 120.3(3) . . ?
F53 C88 C87 120.7(3) . . ?
C89 C88 C87 119.0(3) . . ?
F54 C89 C88 119.0(3) . . ?
F54 C89 C90 121.2(3) . . ?
C88 C89 C90 119.8(3) . . ?
F55 C90 C89 115.3(3) . . ?
F55 C90 C85 121.0(2) . . ?
C89 C90 C85 123.7(3) . . ?
C92 C91 C96 112.9(3) . . ?
C92 C91 B4 119.8(2) . . ?
C96 C91 B4 127.4(2) . . ?
F56 C92 C93 115.5(3) . . ?
F56 C92 C91 119.3(3) . . ?
C93 C92 C91 125.1(3) . . ?
F57 C93 C94 119.7(3) . . ?
F57 C93 C92 121.3(3) . . ?
C94 C93 C92 119.0(3) . . ?
F58 C94 C95 120.0(3) . . ?
F58 C94 C93 120.9(3) . . ?
C95 C94 C93 119.2(3) . . ?
F59 C95 C94 119.7(3) . . ?
F59 C95 C96 120.7(3) . . ?
C94 C95 C96 119.6(3) . . ?
F60 C96 C91 121.6(3) . . ?
F60 C96 C95 114.4(3) . . ?
C91 C96 C95 124.1(3) . . ?
C90 F55 K4 132.14(15) . . ?
C92 F56 K4 163.25(15) . . ?
O7 K3 O26 103.81(7) . . ?
O7 K3 O24 82.82(7) . . ?
O26 K3 O24 116.59(8) . . ?
O7 K3 O22 106.66(7) . . ?
O26 K3 O22 117.34(8) . . ?
O24 K3 O22 120.50(8) . . ?
O7 K3 O23 99.58(7) . . ?
O26 K3 O23 155.79(7) . . ?
O24 K3 O23 60.12(8) . . ?
O22 K3 O23 60.38(8) . . ?
O7 K3 O21 122.21(7) . . ?
O26 K3 O21 58.88(7) . . ?
O24 K3 O21 154.85(7) . . ?
O22 K3 O21 58.49(7) . . ?
O23 K3 O21 112.68(8) . . ?
O7 K3 O25 91.80(7) . . ?
O26 K3 O25 58.73(7) . . ?
O24 K3 O25 58.07(7) . . ?
O22 K3 O25 161.34(7) . . ?
O23 K3 O25 114.75(7) . . ?
O21 K3 O25 113.87(7) . . ?
O7 K3 Cl3 156.57(5) . . ?
O26 K3 Cl3 87.56(6) . . ?
O24 K3 Cl3 73.75(6) . . ?
O22 K3 Cl3 85.26(6) . . ?
O23 K3 Cl3 68.33(6) . . ?
O21 K3 Cl3 81.22(6) . . ?
O25 K3 Cl3 76.49(5) . . ?
O7 K3 C105 83.21(8) . . ?
O26 K3 C105 41.93(8) . . ?
O24 K3 C105 78.20(8) . . ?
O22 K3 C105 159.27(8) . . ?
O23 K3 C105 137.24(8) . . ?
O21 K3 C105 100.78(8) . . ?
O25 K3 C105 23.02(7) . . ?
Cl3 K3 C105 92.44(7) . . ?
O7 K3 C101 83.38(9) . . ?
O26 K3 C101 156.87(9) . . ?
O24 K3 C101 41.63(9) . . ?
O22 K3 C101 80.33(9) . . ?
O23 K3 C101 22.74(8) . . ?
O21 K3 C101 135.35(9) . . ?
O25 K3 C101 99.59(9) . . ?
Cl3 K3 C101 78.76(8) . . ?
C105 K3 C101 119.47(10) . . ?
C97 O21 C108 112.8(3) . . ?
C97 O21 K3 107.34(19) . . ?
C108 O21 K3 111.63(18) . . ?
C99 O22 C98 112.4(3) . . ?
C99 O22 K3 116.7(2) . . ?
C98 O22 K3 120.82(19) . . ?
C100 O23 C101 112.3(3) . . ?
C100 O23 K3 110.6(2) . . ?
C101 O23 K3 107.99(19) . . ?
C103 O24 C102 114.0(3) . . ?
C103 O24 K3 121.86(19) . . ?
C102 O24 K3 118.0(2) . . ?
C105 O25 C104 112.4(3) . . ?
C105 O25 K3 103.22(18) . . ?
C104 O25 K3 109.28(18) . . ?
C106 O26 C107 113.2(3) . . ?
C106 O26 K3 120.79(19) . . ?
C107 O26 K3 120.33(19) . . ?
O21 C97 C98 109.1(3) . . ?
O21 C97 H97A 109.9 . . ?
C98 C97 H97A 109.9 . . ?
O21 C97 H97B 109.9 . . ?
C98 C97 H97B 109.9 . . ?
H97A C97 H97B 108.3 . . ?
O22 C98 C97 108.6(3) . . ?
O22 C98 H98A 110.0 . . ?
C97 C98 H98A 110.0 . . ?
O22 C98 H98B 110.0 . . ?
C97 C98 H98B 110.0 . . ?
H98A C98 H98B 108.3 . . ?
O22 C99 C100 109.4(3) . . ?
O22 C99 H99A 109.8 . . ?
C100 C99 H99A 109.8 . . ?
O22 C99 H99B 109.8 . . ?
C100 C99 H99B 109.8 . . ?
H99A C99 H99B 108.2 . . ?
O23 C100 C99 109.3(3) . . ?
O23 C100 H10A 109.8 . . ?
C99 C100 H10A 109.8 . . ?
O23 C100 H10B 109.8 . . ?
C99 C100 H10B 109.8 . . ?
H10A C100 H10B 108.3 . . ?
O23 C101 C102 108.4(3) . . ?
O23 C101 K3 49.27(15) . . ?
C102 C101 K3 83.2(2) . . ?
O23 C101 H10C 110.0 . . ?
C102 C101 H10C 110.0 . . ?
K3 C101 H10C 159.1 . . ?
O23 C101 H10D 110.0 . . ?
C102 C101 H10D 110.0 . . ?
K3 C101 H10D 80.6 . . ?
H10C C101 H10D 108.4 . . ?
O24 C102 C101 108.4(3) . . ?
O24 C102 H10E 110.0 . . ?
C101 C102 H10E 110.0 . . ?
O24 C102 H10F 110.0 . . ?
C101 C102 H10F 110.0 . . ?
H10E C102 H10F 108.4 . . ?
O24 C103 C104 108.2(3) . . ?
O24 C103 H10G 110.1 . . ?
C104 C103 H10G 110.1 . . ?
O24 C103 H10H 110.1 . . ?
C104 C103 H10H 110.1 . . ?
H10G C103 H10H 108.4 . . ?
O25 C104 C103 108.4(3) . . ?
O25 C104 H10I 110.0 . . ?
C103 C104 H10I 110.0 . . ?
O25 C104 H10J 110.0 . . ?
C103 C104 H10J 110.0 . . ?
H10I C104 H10J 108.4 . . ?
O25 C105 C106 108.3(3) . . ?
O25 C105 K3 53.76(15) . . ?
C106 C105 K3 84.19(19) . . ?
O25 C105 H10K 110.0 . . ?
C106 C105 H10K 110.0 . . ?
K3 C105 H10K 162.2 . . ?
O25 C105 H10L 110.0 . . ?
C106 C105 H10L 110.0 . . ?
K3 C105 H10L 74.9 . . ?
H10K C105 H10L 108.4 . . ?
O26 C106 C105 108.9(3) . . ?
O26 C106 H10M 109.9 . . ?
C105 C106 H10M 109.9 . . ?
O26 C106 H10N 109.9 . . ?
C105 C106 H10N 109.9 . . ?
H10M C106 H10N 108.3 . . ?
O26 C107 C108 108.9(3) . . ?
O26 C107 H10O 109.9 . . ?
C108 C107 H10O 109.9 . . ?
O26 C107 H10P 109.9 . . ?
C108 C107 H10P 109.9 . . ?
H10O C107 H10P 108.3 . . ?
O21 C108 C107 109.4(3) . . ?
O21 C108 H10Q 109.8 . . ?
C107 C108 H10Q 109.8 . . ?
O21 C108 H10R 109.8 . . ?
C107 C108 H10R 109.8 . . ?
H10Q C108 H10R 108.3 . . ?
O29 K4 O27 106.22(7) . . ?
O29 K4 O8 73.27(6) . . ?
O27 K4 O8 125.23(6) . . ?
O29 K4 O28 58.09(6) . . ?
O27 K4 O28 57.04(6) . . ?
O8 K4 O28 81.84(6) . . ?
O29 K4 F56 157.16(6) . . ?
O27 K4 F56 93.07(7) . . ?
O8 K4 F56 85.72(6) . . ?
O28 K4 F56 128.62(6) . . ?
O29 K4 O31 108.61(6) . . ?
O27 K4 O31 110.56(7) . . ?
O8 K4 O31 121.56(6) . . ?
O28 K4 O31 150.64(6) . . ?
F56 K4 O31 74.63(6) . . ?
O29 K4 O32 139.75(6) . . ?
O27 K4 O32 57.13(6) . . ?
O8 K4 O32 146.98(6) . . ?
O28 K4 O32 113.70(6) . . ?
F56 K4 O32 61.64(6) . . ?
O31 K4 O32 57.30(6) . . ?
O29 K4 O30 56.22(6) . . ?
O27 K4 O30 106.60(7) . . ?
O8 K4 O30 115.51(6) . . ?
O28 K4 O30 99.93(7) . . ?
F56 K4 O30 130.08(6) . . ?
O31 K4 O30 55.60(6) . . ?
O32 K4 O30 91.27(7) . . ?
O29 K4 F55 93.42(6) . . ?
O27 K4 F55 160.33(6) . . ?
O8 K4 F55 59.07(5) . . ?
O28 K4 F55 137.90(6) . . ?
F56 K4 F55 67.53(6) . . ?
O31 K4 F55 62.54(6) . . ?
O32 K4 F55 107.90(6) . . ?
O30 K4 F55 85.01(6) . . ?
O29 K4 F31 109.02(6) . . ?
O27 K4 F31 73.73(6) . . ?
O8 K4 F31 56.65(5) . . ?
O28 K4 F31 67.36(6) . . ?
F56 K4 F31 64.25(5) . . ?
O31 K4 F31 138.87(6) . . ?
O32 K4 F31 100.94(6) . . ?
O30 K4 F31 165.06(5) . . ?
F55 K4 F31 99.19(5) . . ?
C109 O27 C120 112.3(2) . . ?
C109 O27 K4 113.10(18) . . ?
C120 O27 K4 116.80(17) . . ?
C111 O28 C110 112.7(2) . . ?
C111 O28 K4 119.50(17) . . ?
C110 O28 K4 118.77(17) . . ?
C113 O29 C112 113.9(2) . . ?
C113 O29 K4 110.06(17) . . ?
C112 O29 K4 109.70(17) . . ?
C115 O30 C114 110.7(2) . . ?
C115 O30 K4 116.51(18) . . ?
C114 O30 K4 118.43(18) . . ?
C117 O31 C116 112.6(2) . . ?
C117 O31 K4 111.19(16) . . ?
C116 O31 K4 119.00(17) . . ?
C118 O32 C119 112.0(2) . . ?
C118 O32 K4 119.08(17) . . ?
C119 O32 K4 116.79(17) . . ?
O27 C109 C110 108.6(3) . . ?
O27 C109 H10S 110.0 . . ?
C110 C109 H10S 110.0 . . ?
O27 C109 H10T 110.0 . . ?
C110 C109 H10T 110.0 . . ?
H10S C109 H10T 108.3 . . ?
O28 C110 C109 110.3(3) . . ?
O28 C110 H11A 109.6 . . ?
C109 C110 H11A 109.6 . . ?
O28 C110 H11B 109.6 . . ?
C109 C110 H11B 109.6 . . ?
H11A C110 H11B 108.1 . . ?
O28 C111 C112 108.6(2) . . ?
O28 C111 H11C 110.0 . . ?
C112 C111 H11C 110.0 . . ?
O28 C111 H11D 110.0 . . ?
C112 C111 H11D 110.0 . . ?
H11C C111 H11D 108.3 . . ?
O29 C112 C111 113.1(3) . . ?
O29 C112 H11E 109.0 . . ?
C111 C112 H11E 109.0 . . ?
O29 C112 H11F 109.0 . . ?
C111 C112 H11F 109.0 . . ?
H11E C112 H11F 107.8 . . ?
O29 C113 C114 107.8(3) . . ?
O29 C113 H11G 110.1 . . ?
C114 C113 H11G 110.1 . . ?
O29 C113 H11H 110.1 . . ?
C114 C113 H11H 110.1 . . ?
H11G C113 H11H 108.5 . . ?
O30 C114 C113 107.0(3) . . ?
O30 C114 H11I 110.3 . . ?
C113 C114 H11I 110.3 . . ?
O30 C114 H11J 110.3 . . ?
C113 C114 H11J 110.3 . . ?
H11I C114 H11J 108.6 . . ?
O30 C115 C116 108.1(3) . . ?
O30 C115 H11K 110.1 . . ?
C116 C115 H11K 110.1 . . ?
O30 C115 H11L 110.1 . . ?
C116 C115 H11L 110.1 . . ?
H11K C115 H11L 108.4 . . ?
O31 C116 C115 109.4(3) . . ?
O31 C116 H11M 109.8 . . ?
C115 C116 H11M 109.8 . . ?
O31 C116 H11N 109.8 . . ?
C115 C116 H11N 109.8 . . ?
H11M C116 H11N 108.2 . . ?
O31 C117 C118 112.5(2) . . ?
O31 C117 H11O 109.1 . . ?
C118 C117 H11O 109.1 . . ?
O31 C117 H11P 109.1 . . ?
C118 C117 H11P 109.1 . . ?
H11O C117 H11P 107.8 . . ?
O32 C118 C117 108.8(3) . . ?
O32 C118 H11Q 109.9 . . ?
C117 C118 H11Q 109.9 . . ?
O32 C118 H11R 109.9 . . ?
C117 C118 H11R 109.9 . . ?
H11Q C118 H11R 108.3 . . ?
O32 C119 C120 110.1(3) . . ?
O32 C119 H11S 109.6 . . ?
C120 C119 H11S 109.6 . . ?
O32 C119 H11T 109.6 . . ?
C120 C119 H11T 109.6 . . ?
H11S C119 H11T 108.1 . . ?
O27 C120 C119 108.9(3) . . ?
O27 C120 H12A 109.9 . . ?
C119 C120 H12A 109.9 . . ?
O27 C120 H12B 109.9 . . ?
C119 C120 H12B 109.9 . . ?
H12A C120 H12B 108.3 . . ?
Cl2 C121 Cl1 116.8(3) . . ?
Cl2 C121 H12C 108.1 . . ?
Cl1 C121 H12C 108.1 . . ?
Cl2 C121 H12D 108.1 . . ?
Cl1 C121 H12D 108.1 . . ?
H12C C121 H12D 107.3 . . ?
C121 Cl1 K1 102.1(2) . . ?
Cl4B C122 Cl4A 27.0(4) . . ?
Cl4B C122 Cl3 107.2(4) . . ?
Cl4A C122 Cl3 116.8(2) . . ?
Cl4B C122 H12E 133.6 . . ?
Cl4A C122 H12E 108.1 . . ?
Cl3 C122 H12E 108.1 . . ?
Cl4B C122 H12F 89.1 . . ?
Cl4A C122 H12F 108.1 . . ?
Cl3 C122 H12F 108.1 . . ?
H12E C122 H12F 107.3 . . ?
Cl4B C122 H12G 111.2 . . ?
Cl4A C122 H12G 84.3 . . ?
Cl3 C122 H12G 110.7 . . ?
H12E C122 H12G 26.4 . . ?
H12F C122 H12G 127.4 . . ?
Cl4B C122 H12H 109.5 . . ?
Cl4A C122 H12H 123.0 . . ?
Cl3 C122 H12H 109.8 . . ?
H12E C122 H12H 85.6 . . ?
H12F C122 H12H 22.8 . . ?
H12G C122 H12H 108.5 . . ?
C122 Cl3 K3 103.78(16) . . ?
Cl6 C123 Cl5 125.5(9) . . ?
Cl6 C123 H90A 105.9 . . ?
Cl5 C123 H90A 105.9 . . ?
Cl6 C123 H90B 106.0 . . ?
Cl5 C123 H90B 106.0 . . ?
H90A C123 H90B 106.3 . . ?
Cl7 C124 Cl8 105.5(12) . . ?
Cl7 C124 H90C 110.6 . . ?
Cl8 C124 H90C 110.6 . . ?
Cl7 C124 H90D 110.6 . . ?
Cl8 C124 H90D 110.6 . . ?
H90C C124 H90D 108.8 . . ?
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
O4 S1 O1 B1 -31.9(3) . . . . ?
O3 S1 O1 B1 -160.4(2) . . . . ?
O2 S1 O1 B1 84.1(3) . . . . ?
O4 S1 O2 B2 -142.5(2) . . . . ?
O3 S1 O2 B2 -14.0(2) . . . . ?
O1 S1 O2 B2 99.1(2) . . . . ?
O4 S1 O3 K1 -6.4(3) . . . . ?
O1 S1 O3 K1 118.7(2) . . . . ?
O2 S1 O3 K1 -129.6(2) . . . . ?
S1 O1 B1 C7 -77.1(3) . . . . ?
S1 O1 B1 C1 161.34(19) . . . . ?
S1 O1 B1 C13 47.6(3) . . . . ?
O1 B1 C1 C2 1.4(4) . . . . ?
C7 B1 C1 C2 -114.6(3) . . . . ?
C13 B1 C1 C2 118.9(3) . . . . ?
O1 B1 C1 C6 -173.0(2) . . . . ?
C7 B1 C1 C6 71.0(3) . . . . ?
C13 B1 C1 C6 -55.4(3) . . . . ?
C6 C1 C2 F1 -175.7(3) . . . . ?
B1 C1 C2 F1 9.7(4) . . . . ?
C6 C1 C2 C3 4.8(4) . . . . ?
B1 C1 C2 C3 -169.9(3) . . . . ?
F1 C2 C3 F2 -3.1(4) . . . . ?
C1 C2 C3 F2 176.5(3) . . . . ?
F1 C2 C3 C4 177.8(3) . . . . ?
C1 C2 C3 C4 -2.6(5) . . . . ?
F2 C3 C4 F3 -1.5(5) . . . . ?
C2 C3 C4 F3 177.6(3) . . . . ?
F2 C3 C4 C5 179.4(3) . . . . ?
C2 C3 C4 C5 -1.5(5) . . . . ?
F3 C4 C5 F4 1.3(5) . . . . ?
C3 C4 C5 F4 -179.6(3) . . . . ?
F3 C4 C5 C6 -176.2(3) . . . . ?
C3 C4 C5 C6 2.9(5) . . . . ?
F4 C5 C6 F5 2.3(4) . . . . ?
C4 C5 C6 F5 179.9(3) . . . . ?
F4 C5 C6 C1 -177.9(3) . . . . ?
C4 C5 C6 C1 -0.4(5) . . . . ?
C2 C1 C6 F5 176.4(3) . . . . ?
B1 C1 C6 F5 -8.4(4) . . . . ?
C2 C1 C6 C5 -3.3(4) . . . . ?
B1 C1 C6 C5 171.8(3) . . . . ?
O1 B1 C7 C12 73.2(3) . . . . ?
C1 B1 C7 C12 -171.3(2) . . . . ?
C13 B1 C7 C12 -49.5(3) . . . . ?
O1 B1 C7 C8 -100.3(3) . . . . ?
C1 B1 C7 C8 15.3(4) . . . . ?
C13 B1 C7 C8 137.1(3) . . . . ?
C12 C7 C8 F6 -178.6(2) . . . . ?
B1 C7 C8 F6 -4.7(4) . . . . ?
C12 C7 C8 C9 -0.3(4) . . . . ?
B1 C7 C8 C9 173.6(3) . . . . ?
F6 C8 C9 C10 177.2(3) . . . . ?
C7 C8 C9 C10 -1.2(5) . . . . ?
F6 C8 C9 F7 -0.6(4) . . . . ?
C7 C8 C9 F7 -179.0(3) . . . . ?
F7 C9 C10 F8 -2.0(4) . . . . ?
C8 C9 C10 F8 -179.8(3) . . . . ?
F7 C9 C10 C11 180.0(3) . . . . ?
C8 C9 C10 C11 2.2(5) . . . . ?
F8 C10 C11 F9 -2.2(4) . . . . ?
C9 C10 C11 F9 175.8(3) . . . . ?
F8 C10 C11 C12 -179.7(2) . . . . ?
C9 C10 C11 C12 -1.6(4) . . . . ?
C8 C7 C12 F10 -178.9(2) . . . . ?
B1 C7 C12 F10 6.9(4) . . . . ?
C8 C7 C12 C11 0.8(4) . . . . ?
B1 C7 C12 C11 -173.3(3) . . . . ?
F9 C11 C12 F10 2.4(4) . . . . ?
C10 C11 C12 F10 179.9(2) . . . . ?
F9 C11 C12 C7 -177.4(2) . . . . ?
C10 C11 C12 C7 0.1(4) . . . . ?
O1 B1 C13 C14 -143.0(3) . . . . ?
C7 B1 C13 C14 -23.2(4) . . . . ?
C1 B1 C13 C14 103.3(3) . . . . ?
O1 B1 C13 C18 42.2(3) . . . . ?
C7 B1 C13 C18 162.1(2) . . . . ?
C1 B1 C13 C18 -71.4(3) . . . . ?
C18 C13 C14 F11 178.2(2) . . . . ?
B1 C13 C14 F11 3.1(4) . . . . ?
C18 C13 C14 C15 -0.4(4) . . . . ?
B1 C13 C14 C15 -175.5(3) . . . . ?
F11 C14 C15 F12 0.1(4) . . . . ?
C13 C14 C15 F12 178.8(3) . . . . ?
F11 C14 C15 C16 -179.7(3) . . . . ?
C13 C14 C15 C16 -1.0(5) . . . . ?
F12 C15 C16 F13 1.2(5) . . . . ?
C14 C15 C16 F13 -178.9(3) . . . . ?
F12 C15 C16 C17 -178.9(3) . . . . ?
C14 C15 C16 C17 1.0(5) . . . . ?
F13 C16 C17 F14 -0.9(5) . . . . ?
C15 C16 C17 F14 179.2(3) . . . . ?
F13 C16 C17 C18 -179.6(3) . . . . ?
C15 C16 C17 C18 0.5(5) . . . . ?
F14 C17 C18 F15 -2.5(4) . . . . ?
C16 C17 C18 F15 176.2(3) . . . . ?
F14 C17 C18 C13 179.2(3) . . . . ?
C16 C17 C18 C13 -2.2(5) . . . . ?
C14 C13 C18 F15 -176.2(3) . . . . ?
B1 C13 C18 F15 -0.9(4) . . . . ?
C14 C13 C18 C17 2.0(4) . . . . ?
B1 C13 C18 C17 177.4(3) . . . . ?
C7 C12 F10 K2 -160.47(17) . . . . ?
C11 C12 F10 K2 19.8(3) . . . . ?
S1 O2 B2 C25 -43.7(3) . . . . ?
S1 O2 B2 C19 82.1(3) . . . . ?
S1 O2 B2 C31 -164.58(17) . . . . ?
O2 B2 C19 C20 -3.9(4) . . . . ?
C25 B2 C19 C20 119.5(3) . . . . ?
C31 B2 C19 C20 -115.4(3) . . . . ?
O2 B2 C19 C24 171.7(2) . . . . ?
C25 B2 C19 C24 -65.0(3) . . . . ?
C31 B2 C19 C24 60.1(3) . . . . ?
C24 C19 C20 F16 -179.9(2) . . . . ?
B2 C19 C20 F16 -4.1(5) . . . . ?
C24 C19 C20 C21 1.0(4) . . . . ?
B2 C19 C20 C21 176.8(3) . . . . ?
F16 C20 C21 F17 0.7(4) . . . . ?
C19 C20 C21 F17 179.8(3) . . . . ?
F16 C20 C21 C22 -179.8(3) . . . . ?
C19 C20 C21 C22 -0.7(5) . . . . ?
F17 C21 C22 F18 0.1(4) . . . . ?
C20 C21 C22 F18 -179.5(3) . . . . ?
F17 C21 C22 C23 179.9(3) . . . . ?
C20 C21 C22 C23 0.4(5) . . . . ?
F18 C22 C23 F19 -0.1(5) . . . . ?
C21 C22 C23 F19 -180.0(3) . . . . ?
F18 C22 C23 C24 179.3(3) . . . . ?
C21 C22 C23 C24 -0.6(5) . . . . ?
F19 C23 C24 F20 -1.0(4) . . . . ?
C22 C23 C24 F20 179.6(3) . . . . ?
F19 C23 C24 C19 -179.5(3) . . . . ?
C22 C23 C24 C19 1.1(5) . . . . ?
C20 C19 C24 C23 -1.3(4) . . . . ?
B2 C19 C24 C23 -177.4(3) . . . . ?
C20 C19 C24 F20 -179.7(2) . . . . ?
B2 C19 C24 F20 4.1(4) . . . . ?
O2 B2 C25 C26 110.7(3) . . . . ?
C19 B2 C25 C26 -14.3(4) . . . . ?
C31 B2 C25 C26 -135.1(3) . . . . ?
O2 B2 C25 C30 -66.0(3) . . . . ?
C19 B2 C25 C30 169.0(2) . . . . ?
C31 B2 C25 C30 48.2(3) . . . . ?
C30 C25 C26 F21 176.3(2) . . . . ?
B2 C25 C26 F21 -0.6(4) . . . . ?
C30 C25 C26 C27 -2.9(4) . . . . ?
B2 C25 C26 C27 -179.8(3) . . . . ?
F21 C26 C27 F22 2.8(4) . . . . ?
C25 C26 C27 F22 -178.0(2) . . . . ?
F21 C26 C27 C28 -177.4(3) . . . . ?
C25 C26 C27 C28 1.9(4) . . . . ?
F22 C27 C28 F23 0.7(4) . . . . ?
C26 C27 C28 F23 -179.2(3) . . . . ?
F22 C27 C28 C29 179.1(3) . . . . ?
C26 C27 C28 C29 -0.8(5) . . . . ?
F23 C28 C29 F24 -0.5(5) . . . . ?
C27 C28 C29 F24 -178.9(3) . . . . ?
F23 C28 C29 C30 179.4(3) . . . . ?
C27 C28 C29 C30 1.0(5) . . . . ?
F24 C29 C30 F25 0.1(4) . . . . ?
C28 C29 C30 F25 -179.7(3) . . . . ?
F24 C29 C30 C25 177.5(3) . . . . ?
C28 C29 C30 C25 -2.3(5) . . . . ?
C26 C25 C30 F25 -179.6(2) . . . . ?
B2 C25 C30 F25 -2.4(4) . . . . ?
C26 C25 C30 C29 3.1(4) . . . . ?
B2 C25 C30 C29 -179.8(3) . . . . ?
O2 B2 C31 C32 -46.6(3) . . . . ?
C25 B2 C31 C32 -164.2(2) . . . . ?
C19 B2 C31 C32 70.9(3) . . . . ?
O2 B2 C31 C36 134.9(3) . . . . ?
C25 B2 C31 C36 17.3(4) . . . . ?
C19 B2 C31 C36 -107.6(3) . . . . ?
C36 C31 C32 F26 177.1(2) . . . . ?
B2 C31 C32 F26 -1.6(4) . . . . ?
C36 C31 C32 C33 -2.2(4) . . . . ?
B2 C31 C32 C33 179.1(3) . . . . ?
F26 C32 C33 F27 1.9(4) . . . . ?
C31 C32 C33 F27 -178.8(3) . . . . ?
F26 C32 C33 C34 -179.6(2) . . . . ?
C31 C32 C33 C34 -0.2(4) . . . . ?
F27 C33 C34 C35 -179.8(3) . . . . ?
C32 C33 C34 C35 1.6(4) . . . . ?
F27 C33 C34 F28 -0.4(4) . . . . ?
C32 C33 C34 F28 -179.0(3) . . . . ?
F28 C34 C35 F29 0.2(5) . . . . ?
C33 C34 C35 F29 179.7(3) . . . . ?
F28 C34 C35 C36 -179.8(3) . . . . ?
C33 C34 C35 C36 -0.4(5) . . . . ?
C34 C35 C36 F30 177.8(3) . . . . ?
F29 C35 C36 F30 -2.2(4) . . . . ?
C34 C35 C36 C31 -2.3(5) . . . . ?
F29 C35 C36 C31 177.6(3) . . . . ?
C32 C31 C36 F30 -176.7(2) . . . . ?
B2 C31 C36 F30 1.9(4) . . . . ?
C32 C31 C36 C35 3.4(4) . . . . ?
B2 C31 C36 C35 -177.9(3) . . . . ?
C31 C32 F26 K2 137.7(2) . . . . ?
C33 C32 F26 K2 -42.9(4) . . . . ?
S1 O3 K1 O9 -161.7(2) . . . . ?
S1 O3 K1 O13 -45.9(3) . . . . ?
S1 O3 K1 O11 73.9(3) . . . . ?
S1 O3 K1 O12 11.4(3) . . . . ?
S1 O3 K1 O10 136.9(2) . . . . ?
S1 O3 K1 O14 -104.4(3) . . . . ?
S1 O3 K1 Cl1 -53.5(3) . . . . ?
S1 O3 K1 C47 -125.9(3) . . . . ?
O3 K1 O9 C48 72.7(2) . . . . ?
O13 K1 O9 C48 -18.2(2) . . . . ?
O11 K1 O9 C48 -169.5(2) . . . . ?
O12 K1 O9 C48 -92.9(3) . . . . ?
O10 K1 O9 C48 -167.4(2) . . . . ?
O14 K1 O9 C48 -8.8(2) . . . . ?
Cl1 K1 O9 C48 -85.2(2) . . . . ?
C47 K1 O9 C48 13.1(2) . . . . ?
O3 K1 O9 C37 -133.0(2) . . . . ?
O13 K1 O9 C37 136.2(2) . . . . ?
O11 K1 O9 C37 -15.2(2) . . . . ?
O12 K1 O9 C37 61.5(3) . . . . ?
O10 K1 O9 C37 -13.0(2) . . . . ?
O14 K1 O9 C37 145.5(2) . . . . ?
Cl1 K1 O9 C37 69.1(2) . . . . ?
C47 K1 O9 C37 167.4(3) . . . . ?
O3 K1 O10 C39 -56.7(2) . . . . ?
O9 K1 O10 C39 -143.5(2) . . . . ?
O13 K1 O10 C39 129.5(2) . . . . ?
O11 K1 O10 C39 34.26(17) . . . . ?
O12 K1 O10 C39 65.32(19) . . . . ?
O14 K1 O10 C39 -163.34(17) . . . . ?
Cl1 K1 O10 C39 127.41(18) . . . . ?
C47 K1 O10 C39 -143.18(18) . . . . ?
O3 K1 O10 C38 65.9(2) . . . . ?
O9 K1 O10 C38 -20.83(18) . . . . ?
O13 K1 O10 C38 -107.9(2) . . . . ?
O11 K1 O10 C38 156.9(2) . . . . ?
O12 K1 O10 C38 -172.03(18) . . . . ?
O14 K1 O10 C38 -40.7(2) . . . . ?
Cl1 K1 O10 C38 -109.95(19) . . . . ?
C47 K1 O10 C38 -20.5(2) . . . . ?
O3 K1 O11 C41 -102.0(2) . . . . ?
O9 K1 O11 C41 142.0(2) . . . . ?
O13 K1 O11 C41 -8.2(2) . . . . ?
O12 K1 O11 C41 -6.4(2) . . . . ?
O10 K1 O11 C41 139.8(2) . . . . ?
O14 K1 O11 C41 72.5(3) . . . . ?
Cl1 K1 O11 C41 59.7(2) . . . . ?
C47 K1 O11 C41 146.8(2) . . . . ?
O3 K1 O11 C40 115.7(2) . . . . ?
O9 K1 O11 C40 -0.4(2) . . . . ?
O13 K1 O11 C40 -150.6(2) . . . . ?
O12 K1 O11 C40 -148.7(2) . . . . ?
O10 K1 O11 C40 -2.5(2) . . . . ?
O14 K1 O11 C40 -69.8(3) . . . . ?
Cl1 K1 O11 C40 -82.6(2) . . . . ?
C47 K1 O11 C40 4.5(3) . . . . ?
O3 K1 O12 C42 75.6(2) . . . . ?
O9 K1 O12 C42 -118.8(2) . . . . ?
O13 K1 O12 C42 151.3(2) . . . . ?
O11 K1 O12 C42 -26.85(19) . . . . ?
O10 K1 O12 C42 -57.3(2) . . . . ?
O14 K1 O12 C42 172.14(19) . . . . ?
Cl1 K1 O12 C42 -127.0(2) . . . . ?
C47 K1 O12 C42 167.14(19) . . . . ?
O3 K1 O12 C43 -50.3(2) . . . . ?
O9 K1 O12 C43 115.3(2) . . . . ?
O13 K1 O12 C43 25.4(2) . . . . ?
O11 K1 O12 C43 -152.7(2) . . . . ?
O10 K1 O12 C43 176.8(2) . . . . ?
O14 K1 O12 C43 46.2(2) . . . . ?
Cl1 K1 O12 C43 107.1(2) . . . . ?
C47 K1 O12 C43 41.2(2) . . . . ?
O3 K1 O13 C44 116.5(2) . . . . ?
O9 K1 O13 C44 -140.7(2) . . . . ?
O11 K1 O13 C44 9.7(2) . . . . ?
O12 K1 O13 C44 7.9(2) . . . . ?
O10 K1 O13 C44 -68.7(3) . . . . ?
O14 K1 O13 C44 -150.0(2) . . . . ?
Cl1 K1 O13 C44 -66.6(2) . . . . ?
C47 K1 O13 C44 -161.4(2) . . . . ?
O3 K1 O13 C45 -94.8(2) . . . . ?
O9 K1 O13 C45 8.0(2) . . . . ?
O11 K1 O13 C45 158.4(2) . . . . ?
O12 K1 O13 C45 156.6(2) . . . . ?
O10 K1 O13 C45 79.9(3) . . . . ?
O14 K1 O13 C45 -1.3(2) . . . . ?
Cl1 K1 O13 C45 82.1(2) . . . . ?
C47 K1 O13 C45 -12.7(2) . . . . ?
O3 K1 O14 C47 -66.77(18) . . . . ?
O9 K1 O14 C47 39.45(17) . . . . ?
O13 K1 O14 C47 -150.35(19) . . . . ?
O11 K1 O14 C47 118.4(3) . . . . ?
O12 K1 O14 C47 -171.46(17) . . . . ?
O10 K1 O14 C47 59.41(18) . . . . ?
Cl1 K1 O14 C47 131.66(18) . . . . ?
O3 K1 O14 C46 52.08(18) . . . . ?
O9 K1 O14 C46 158.3(2) . . . . ?
O13 K1 O14 C46 -31.49(17) . . . . ?
O11 K1 O14 C46 -122.7(3) . . . . ?
O12 K1 O14 C46 -52.61(19) . . . . ?
O10 K1 O14 C46 178.26(17) . . . . ?
Cl1 K1 O14 C46 -109.49(18) . . . . ?
C47 K1 O14 C46 118.9(3) . . . . ?
C48 O9 C37 C38 -160.1(3) . . . . ?
K1 O9 C37 C38 43.6(3) . . . . ?
C39 O10 C38 C37 170.8(3) . . . . ?
K1 O10 C38 C37 50.9(3) . . . . ?
O9 C37 C38 O10 -61.8(3) . . . . ?
C38 O10 C39 C40 171.0(3) . . . . ?
K1 O10 C39 C40 -65.5(3) . . . . ?
C41 O11 C40 C39 -172.7(3) . . . . ?
K1 O11 C40 C39 -28.4(3) . . . . ?
O10 C39 C40 O11 63.9(3) . . . . ?
C40 O11 C41 C42 -176.7(3) . . . . ?
K1 O11 C41 C42 37.5(3) . . . . ?
C43 O12 C42 C41 -176.4(3) . . . . ?
K1 O12 C42 C41 58.3(3) . . . . ?
O11 C41 C42 O12 -64.6(4) . . . . ?
C42 O12 C43 C44 178.2(3) . . . . ?
K1 O12 C43 C44 -56.8(3) . . . . ?
C45 O13 C44 C43 170.2(3) . . . . ?
K1 O13 C44 C43 -38.9(4) . . . . ?
O12 C43 C44 O13 63.8(4) . . . . ?
C44 O13 C45 C46 -177.2(3) . . . . ?
K1 O13 C45 C46 32.8(3) . . . . ?
C47 O14 C46 C45 175.3(3) . . . . ?
K1 O14 C46 C45 63.1(3) . . . . ?
O13 C45 C46 O14 -65.3(3) . . . . ?
C46 O14 C47 C48 175.2(2) . . . . ?
K1 O14 C47 C48 -70.1(2) . . . . ?
C46 O14 C47 K1 -114.8(2) . . . . ?
O3 K1 C47 O14 111.62(18) . . . . ?
O9 K1 C47 O14 -126.3(2) . . . . ?
O13 K1 C47 O14 25.48(16) . . . . ?
O11 K1 C47 O14 -132.7(2) . . . . ?
O12 K1 C47 O14 11.6(2) . . . . ?
O10 K1 C47 O14 -126.64(17) . . . . ?
Cl1 K1 C47 O14 -46.32(17) . . . . ?
O3 K1 C47 C48 -132.56(19) . . . . ?
O9 K1 C47 C48 -10.46(16) . . . . ?
O13 K1 C47 C48 141.30(19) . . . . ?
O11 K1 C47 C48 -16.9(3) . . . . ?
O12 K1 C47 C48 127.40(18) . . . . ?
O10 K1 C47 C48 -10.82(19) . . . . ?
O14 K1 C47 C48 115.8(3) . . . . ?
Cl1 K1 C47 C48 69.50(18) . . . . ?
C37 O9 C48 C47 -178.0(3) . . . . ?
K1 O9 C48 C47 -21.8(3) . . . . ?
O14 C47 C48 O9 64.3(3) . . . . ?
K1 C47 C48 O9 14.5(2) . . . . ?
C32 F26 K2 O18 160.4(3) . . . . ?
C32 F26 K2 O15 -3.4(3) . . . . ?
C32 F26 K2 O20 -76.6(3) . . . . ?
C32 F26 K2 O19 -154.1(3) . . . . ?
C32 F26 K2 O17 99.4(3) . . . . ?
C32 F26 K2 O16 59.5(3) . . . . ?
C32 F26 K2 F10 -67.4(3) . . . . ?
C12 F10 K2 F26 48.5(2) . . . . ?
C12 F10 K2 O18 110.4(2) . . . . ?
C12 F10 K2 O15 -75.1(2) . . . . ?
C12 F10 K2 O20 -138.6(2) . . . . ?
C12 F10 K2 O19 169.8(2) . . . . ?
C12 F10 K2 O17 32.4(2) . . . . ?
C12 F10 K2 O16 -48.0(2) . . . . ?
F26 K2 O15 C49 123.9(2) . . . . ?
O18 K2 O15 C49 -9.5(4) . . . . ?
O20 K2 O15 C49 -107.1(2) . . . . ?
O19 K2 O15 C49 -83.6(3) . . . . ?
O17 K2 O15 C49 52.5(3) . . . . ?
O16 K2 O15 C49 26.8(2) . . . . ?
F10 K2 O15 C49 -177.4(3) . . . . ?
F26 K2 O15 C60 -106.3(2) . . . . ?
O18 K2 O15 C60 120.4(3) . . . . ?
O20 K2 O15 C60 22.7(2) . . . . ?
O19 K2 O15 C60 46.2(2) . . . . ?
O17 K2 O15 C60 -177.7(2) . . . . ?
O16 K2 O15 C60 156.6(2) . . . . ?
F10 K2 O15 C60 -47.6(2) . . . . ?
F26 K2 O16 C51 35.0(2) . . . . ?
O18 K2 O16 C51 -49.7(2) . . . . ?
O15 K2 O16 C51 143.6(3) . . . . ?
O20 K2 O16 C51 -175.6(2) . . . . ?
O19 K2 O16 C51 -112.3(2) . . . . ?
O17 K2 O16 C51 -8.0(2) . . . . ?
F10 K2 O16 C51 112.0(2) . . . . ?
F26 K2 O16 C50 -100.5(2) . . . . ?
O18 K2 O16 C50 174.8(2) . . . . ?
O15 K2 O16 C50 8.1(2) . . . . ?
O20 K2 O16 C50 48.8(2) . . . . ?
O19 K2 O16 C50 112.1(2) . . . . ?
O17 K2 O16 C50 -143.5(3) . . . . ?
F10 K2 O16 C50 -23.5(3) . . . . ?
F26 K2 O17 C52 -160.1(2) . . . . ?
O18 K2 O17 C52 106.0(2) . . . . ?
O15 K2 O17 C52 -51.3(2) . . . . ?
O20 K2 O17 C52 11.5(3) . . . . ?
O19 K2 O17 C52 84.7(2) . . . . ?
O16 K2 O17 C52 -25.70(19) . . . . ?
F10 K2 O17 C52 -143.60(19) . . . . ?
F26 K2 O17 C53 71.47(19) . . . . ?
O18 K2 O17 C53 -22.44(18) . . . . ?
O15 K2 O17 C53 -179.74(19) . . . . ?
O20 K2 O17 C53 -116.9(3) . . . . ?
O19 K2 O17 C53 -43.7(2) . . . . ?
O16 K2 O17 C53 -154.1(2) . . . . ?
F10 K2 O17 C53 88.0(2) . . . . ?
F26 K2 O18 C55 139.4(2) . . . . ?
O15 K2 O18 C55 -82.4(3) . . . . ?
O20 K2 O18 C55 2.6(2) . . . . ?
O19 K2 O18 C55 3.7(2) . . . . ?
O17 K2 O18 C55 -154.3(2) . . . . ?
O16 K2 O18 C55 -113.5(2) . . . . ?
F10 K2 O18 C55 83.3(2) . . . . ?
F26 K2 O18 C54 -74.4(2) . . . . ?
O15 K2 O18 C54 63.7(3) . . . . ?
O20 K2 O18 C54 148.8(2) . . . . ?
O19 K2 O18 C54 149.8(2) . . . . ?
O17 K2 O18 C54 -8.1(2) . . . . ?
O16 K2 O18 C54 32.7(2) . . . . ?
F10 K2 O18 C54 -130.6(2) . . . . ?
F26 K2 O19 C56 -24.4(2) . . . . ?
O18 K2 O19 C56 30.10(19) . . . . ?
O15 K2 O19 C56 -174.8(2) . . . . ?
O20 K2 O19 C56 -150.9(2) . . . . ?
O17 K2 O19 C56 51.4(2) . . . . ?
O16 K2 O19 C56 118.4(2) . . . . ?
F10 K2 O19 C56 -94.2(2) . . . . ?
F26 K2 O19 C57 99.2(2) . . . . ?
O18 K2 O19 C57 153.7(2) . . . . ?
O15 K2 O19 C57 -51.2(2) . . . . ?
O20 K2 O19 C57 -27.4(2) . . . . ?
O17 K2 O19 C57 175.0(2) . . . . ?
O16 K2 O19 C57 -118.0(2) . . . . ?
F10 K2 O19 C57 29.3(2) . . . . ?
F26 K2 O20 C59 107.1(2) . . . . ?
O18 K2 O20 C59 -145.1(2) . . . . ?
O15 K2 O20 C59 9.4(2) . . . . ?
O19 K2 O20 C59 -146.1(2) . . . . ?
O17 K2 O20 C59 -62.2(3) . . . . ?
O16 K2 O20 C59 -30.0(2) . . . . ?
F10 K2 O20 C59 97.8(2) . . . . ?
F26 K2 O20 C58 -113.8(2) . . . . ?
O18 K2 O20 C58 -6.0(2) . . . . ?
O15 K2 O20 C58 148.4(2) . . . . ?
O19 K2 O20 C58 -7.0(2) . . . . ?
O17 K2 O20 C58 76.9(3) . . . . ?
O16 K2 O20 C58 109.1(2) . . . . ?
F10 K2 O20 C58 -123.1(2) . . . . ?
C60 O15 C49 C50 172.6(3) . . . . ?
K2 O15 C49 C50 -58.9(3) . . . . ?
C51 O16 C50 C49 -177.5(4) . . . . ?
K2 O16 C50 C49 -39.8(4) . . . . ?
O15 C49 C50 O16 64.5(4) . . . . ?
C50 O16 C51 C52 176.4(3) . . . . ?
K2 O16 C51 C52 39.0(4) . . . . ?
C53 O17 C52 C51 -175.6(3) . . . . ?
K2 O17 C52 C51 57.0(3) . . . . ?
O16 C51 C52 O17 -63.9(4) . . . . ?
C52 O17 C53 C54 -76.5(3) . . . . ?
K2 O17 C53 C54 52.2(3) . . . . ?
C55 O18 C54 C53 -177.2(3) . . . . ?
K2 O18 C54 C53 35.1(3) . . . . ?
O17 C53 C54 O18 -58.6(3) . . . . ?
C54 O18 C55 C56 175.9(3) . . . . ?
K2 O18 C55 C56 -35.3(3) . . . . ?
C57 O19 C56 C55 175.8(3) . . . . ?
K2 O19 C56 C55 -61.7(3) . . . . ?
O18 C55 C56 O19 66.0(3) . . . . ?
C56 O19 C57 C58 -178.2(3) . . . . ?
K2 O19 C57 C58 60.3(3) . . . . ?
C59 O20 C58 C57 -180.0(3) . . . . ?
K2 O20 C58 C57 39.1(3) . . . . ?
O19 C57 C58 O20 -66.7(4) . . . . ?
C58 O20 C59 C60 -178.9(3) . . . . ?
K2 O20 C59 C60 -37.9(4) . . . . ?
C49 O15 C60 C59 75.9(4) . . . . ?
K2 O15 C60 C59 -54.9(4) . . . . ?
O20 C59 C60 O15 63.2(4) . . . . ?
O7 S2 O5 B3 -161.4(2) . . . . ?
O8 S2 O5 B3 -32.5(3) . . . . ?
O6 S2 O5 B3 82.5(2) . . . . ?
O7 S2 O6 B4 -17.0(2) . . . . ?
O8 S2 O6 B4 -144.9(2) . . . . ?
O5 S2 O6 B4 97.0(2) . . . . ?
O8 S2 O7 K3 -5.7(3) . . . . ?
O5 S2 O7 K3 119.8(2) . . . . ?
O6 S2 O7 K3 -127.9(2) . . . . ?
O7 S2 O8 K4 -111.15(13) . . . . ?
O5 S2 O8 K4 125.72(11) . . . . ?
O6 S2 O8 K4 12.50(14) . . . . ?
S2 O5 B3 C67 164.08(17) . . . . ?
S2 O5 B3 C73 52.4(3) . . . . ?
S2 O5 B3 C61 -74.9(3) . . . . ?
O5 B3 C61 C62 76.5(3) . . . . ?
C67 B3 C61 C62 -166.5(2) . . . . ?
C73 B3 C61 C62 -48.5(3) . . . . ?
O5 B3 C61 C66 -99.4(3) . . . . ?
C67 B3 C61 C66 17.7(4) . . . . ?
C73 B3 C61 C66 135.6(3) . . . . ?
C66 C61 C62 F31 178.6(2) . . . . ?
B3 C61 C62 F31 2.4(4) . . . . ?
C66 C61 C62 C63 -2.0(4) . . . . ?
B3 C61 C62 C63 -178.2(3) . . . . ?
F31 C62 C63 F32 1.4(4) . . . . ?
C61 C62 C63 F32 -178.0(3) . . . . ?
F31 C62 C63 C64 -179.2(2) . . . . ?
C61 C62 C63 C64 1.4(4) . . . . ?
F32 C63 C64 F33 -1.8(4) . . . . ?
C62 C63 C64 F33 178.8(3) . . . . ?
F32 C63 C64 C65 178.6(3) . . . . ?
C62 C63 C64 C65 -0.8(4) . . . . ?
F33 C64 C65 F34 -0.2(4) . . . . ?
C63 C64 C65 F34 179.5(3) . . . . ?
F33 C64 C65 C66 -178.6(3) . . . . ?
C63 C64 C65 C66 1.1(5) . . . . ?
C62 C61 C66 F35 -175.8(2) . . . . ?
B3 C61 C66 F35 0.3(4) . . . . ?
C62 C61 C66 C65 2.2(4) . . . . ?
B3 C61 C66 C65 178.4(3) . . . . ?
F34 C65 C66 F35 -2.1(4) . . . . ?
C64 C65 C66 F35 176.3(3) . . . . ?
F34 C65 C66 C61 179.7(3) . . . . ?
C64 C65 C66 C61 -1.9(5) . . . . ?
O5 B3 C67 C72 -2.8(4) . . . . ?
C73 B3 C67 C72 114.4(3) . . . . ?
C61 B3 C67 C72 -120.9(3) . . . . ?
O5 B3 C67 C68 -176.4(2) . . . . ?
C73 B3 C67 C68 -59.2(3) . . . . ?
C61 B3 C67 C68 65.5(3) . . . . ?
C72 C67 C68 F36 178.1(3) . . . . ?
B3 C67 C68 F36 -7.4(4) . . . . ?
C72 C67 C68 C69 -2.1(5) . . . . ?
B3 C67 C68 C69 172.4(3) . . . . ?
F36 C68 C69 F37 1.2(5) . . . . ?
C67 C68 C69 F37 -178.6(3) . . . . ?
F36 C68 C69 C70 180.0(3) . . . . ?
C67 C68 C69 C70 0.2(5) . . . . ?
F37 C69 C70 F38 2.3(5) . . . . ?
C68 C69 C70 F38 -176.5(3) . . . . ?
F37 C69 C70 C71 -179.8(3) . . . . ?
C68 C69 C70 C71 1.4(5) . . . . ?
F38 C70 C71 F39 -1.5(5) . . . . ?
C69 C70 C71 F39 -179.4(3) . . . . ?
F38 C70 C71 C72 177.0(3) . . . . ?
C69 C70 C71 C72 -1.0(5) . . . . ?
C68 C67 C72 F40 -177.4(3) . . . . ?
B3 C67 C72 F40 8.7(4) . . . . ?
C68 C67 C72 C71 2.5(4) . . . . ?
B3 C67 C72 C71 -171.4(3) . . . . ?
F39 C71 C72 F40 -2.8(4) . . . . ?
C70 C71 C72 F40 178.8(3) . . . . ?
F39 C71 C72 C67 177.3(3) . . . . ?
C70 C71 C72 C67 -1.2(5) . . . . ?
O5 B3 C73 C74 -143.7(3) . . . . ?
C67 B3 C73 C74 102.6(3) . . . . ?
C61 B3 C73 C74 -20.4(4) . . . . ?
O5 B3 C73 C78 45.5(3) . . . . ?
C67 B3 C73 C78 -68.2(3) . . . . ?
C61 B3 C73 C78 168.8(2) . . . . ?
C78 C73 C74 F41 179.9(2) . . . . ?
B3 C73 C74 F41 8.6(4) . . . . ?
C78 C73 C74 C75 0.7(4) . . . . ?
B3 C73 C74 C75 -170.6(3) . . . . ?
F41 C74 C75 F42 0.2(4) . . . . ?
C73 C74 C75 F42 179.5(3) . . . . ?
F41 C74 C75 C76 180.0(3) . . . . ?
C73 C74 C75 C76 -0.8(5) . . . . ?
F42 C75 C76 F43 0.7(4) . . . . ?
C74 C75 C76 F43 -179.1(2) . . . . ?
F42 C75 C76 C77 179.5(3) . . . . ?
C74 C75 C76 C77 -0.2(4) . . . . ?
F43 C76 C77 F44 0.4(4) . . . . ?
C75 C76 C77 F44 -178.4(3) . . . . ?
F43 C76 C77 C78 180.0(2) . . . . ?
C75 C76 C77 C78 1.1(4) . . . . ?
F44 C77 C78 F45 -4.0(4) . . . . ?
C76 C77 C78 F45 176.4(3) . . . . ?
F44 C77 C78 C73 178.4(3) . . . . ?
C76 C77 C78 C73 -1.2(4) . . . . ?
C74 C73 C78 F45 -177.3(2) . . . . ?
B3 C73 C78 F45 -5.3(4) . . . . ?
C74 C73 C78 C77 0.3(4) . . . . ?
B3 C73 C78 C77 172.3(3) . . . . ?
C63 C62 F31 K4 66.1(4) . . . . ?
C61 C62 F31 K4 -114.4(3) . . . . ?
S2 O6 B4 C79 -41.9(3) . . . . ?
S2 O6 B4 C85 84.6(3) . . . . ?
S2 O6 B4 C91 -162.43(17) . . . . ?
O6 B4 C79 C80 111.8(3) . . . . ?
C85 B4 C79 C80 -13.3(4) . . . . ?
C91 B4 C79 C80 -134.3(3) . . . . ?
O6 B4 C79 C84 -65.6(3) . . . . ?
C85 B4 C79 C84 169.3(2) . . . . ?
C91 B4 C79 C84 48.2(3) . . . . ?
C84 C79 C80 F46 176.8(2) . . . . ?
B4 C79 C80 F46 -0.8(4) . . . . ?
C84 C79 C80 C81 -1.9(4) . . . . ?
B4 C79 C80 C81 -179.5(3) . . . . ?
F46 C80 C81 F47 3.9(4) . . . . ?
C79 C80 C81 F47 -177.3(3) . . . . ?
F46 C80 C81 C82 -176.7(3) . . . . ?
C79 C80 C81 C82 2.1(5) . . . . ?
F47 C81 C82 F48 -0.2(4) . . . . ?
C80 C81 C82 F48 -179.6(3) . . . . ?
F47 C81 C82 C83 178.4(3) . . . . ?
C80 C81 C82 C83 -1.0(5) . . . . ?
F48 C82 C83 F49 -1.5(5) . . . . ?
C81 C82 C83 F49 179.9(3) . . . . ?
F48 C82 C83 C84 178.6(3) . . . . ?
C81 C82 C83 C84 0.0(5) . . . . ?
F49 C83 C84 F50 1.3(4) . . . . ?
C82 C83 C84 F50 -178.8(3) . . . . ?
F49 C83 C84 C79 -179.9(3) . . . . ?
C82 C83 C84 C79 0.1(5) . . . . ?
C80 C79 C84 F50 179.6(2) . . . . ?
B4 C79 C84 F50 -2.6(4) . . . . ?
C80 C79 C84 C83 0.9(4) . . . . ?
B4 C79 C84 C83 178.6(3) . . . . ?
O6 B4 C85 C86 172.8(2) . . . . ?
C79 B4 C85 C86 -63.3(3) . . . . ?
C91 B4 C85 C86 61.8(3) . . . . ?
O6 B4 C85 C90 -5.0(4) . . . . ?
C79 B4 C85 C90 118.9(3) . . . . ?
C91 B4 C85 C90 -116.0(3) . . . . ?
C90 C85 C86 F51 -179.7(3) . . . . ?
B4 C85 C86 F51 2.1(4) . . . . ?
C90 C85 C86 C87 -1.9(5) . . . . ?
B4 C85 C86 C87 180.0(3) . . . . ?
F51 C86 C87 F52 -1.1(5) . . . . ?
C85 C86 C87 F52 -179.0(3) . . . . ?
F51 C86 C87 C88 178.9(3) . . . . ?
C85 C86 C87 C88 1.0(5) . . . . ?
F52 C87 C88 F53 0.7(5) . . . . ?
C86 C87 C88 F53 -179.4(3) . . . . ?
F52 C87 C88 C89 179.9(3) . . . . ?
C86 C87 C88 C89 -0.2(5) . . . . ?
F53 C88 C89 F54 -0.6(4) . . . . ?
C87 C88 C89 F54 -179.8(3) . . . . ?
F53 C88 C89 C90 179.6(3) . . . . ?
C87 C88 C89 C90 0.4(5) . . . . ?
F54 C89 C90 F55 -0.3(4) . . . . ?
C88 C89 C90 F55 179.5(3) . . . . ?
F54 C89 C90 C85 178.7(3) . . . . ?
C88 C89 C90 C85 -1.5(5) . . . . ?
C86 C85 C90 F55 -178.9(2) . . . . ?
B4 C85 C90 F55 -1.0(4) . . . . ?
C86 C85 C90 C89 2.1(4) . . . . ?
B4 C85 C90 C89 -180.0(3) . . . . ?
O6 B4 C91 C92 -45.0(3) . . . . ?
C79 B4 C91 C92 -162.7(2) . . . . ?
C85 B4 C91 C92 72.0(3) . . . . ?
O6 B4 C91 C96 136.3(3) . . . . ?
C79 B4 C91 C96 18.7(4) . . . . ?
C85 B4 C91 C96 -106.7(3) . . . . ?
C96 C91 C92 F56 176.4(2) . . . . ?
B4 C91 C92 F56 -2.5(4) . . . . ?
C96 C91 C92 C93 -2.5(4) . . . . ?
B4 C91 C92 C93 178.6(3) . . . . ?
F56 C92 C93 F57 0.5(4) . . . . ?
C91 C92 C93 F57 179.4(3) . . . . ?
F56 C92 C93 C94 -178.7(3) . . . . ?
C91 C92 C93 C94 0.2(5) . . . . ?
F57 C93 C94 F58 1.9(5) . . . . ?
C92 C93 C94 F58 -178.9(3) . . . . ?
F57 C93 C94 C95 -177.7(3) . . . . ?
C92 C93 C94 C95 1.5(5) . . . . ?
F58 C94 C95 F59 -1.0(5) . . . . ?
C93 C94 C95 F59 178.6(3) . . . . ?
F58 C94 C95 C96 179.7(3) . . . . ?
C93 C94 C95 C96 -0.7(5) . . . . ?
C92 C91 C96 F60 -176.8(2) . . . . ?
B4 C91 C96 F60 1.9(4) . . . . ?
C92 C91 C96 C95 3.3(4) . . . . ?
B4 C91 C96 C95 -177.9(3) . . . . ?
F59 C95 C96 F60 -1.0(4) . . . . ?
C94 C95 C96 F60 178.3(3) . . . . ?
F59 C95 C96 C91 178.8(3) . . . . ?
C94 C95 C96 C91 -1.9(5) . . . . ?
C89 C90 F55 K4 -103.3(3) . . . . ?
C85 C90 F55 K4 77.7(3) . . . . ?
C93 C92 F56 K4 -112.4(5) . . . . ?
C91 C92 F56 K4 68.6(7) . . . . ?
S2 O7 K3 O26 -162.6(2) . . . . ?
S2 O7 K3 O24 -46.9(3) . . . . ?
S2 O7 K3 O22 72.9(3) . . . . ?
S2 O7 K3 O23 11.1(3) . . . . ?
S2 O7 K3 O21 135.7(2) . . . . ?
S2 O7 K3 O25 -104.4(3) . . . . ?
S2 O7 K3 Cl3 -45.4(3) . . . . ?
S2 O7 K3 C105 -125.8(3) . . . . ?
S2 O7 K3 C101 -4.9(3) . . . . ?
O7 K3 O21 C97 -58.6(2) . . . . ?
O26 K3 O21 C97 -145.7(2) . . . . ?
O24 K3 O21 C97 127.5(2) . . . . ?
O22 K3 O21 C97 32.1(2) . . . . ?
O23 K3 O21 C97 59.9(2) . . . . ?
O25 K3 O21 C97 -167.2(2) . . . . ?
Cl3 K3 O21 C97 121.9(2) . . . . ?
C105 K3 O21 C97 -147.3(2) . . . . ?
C101 K3 O21 C97 57.8(2) . . . . ?
O7 K3 O21 C108 65.6(2) . . . . ?
O26 K3 O21 C108 -21.52(19) . . . . ?
O24 K3 O21 C108 -108.3(2) . . . . ?
O22 K3 O21 C108 156.2(2) . . . . ?
O23 K3 O21 C108 -175.99(19) . . . . ?
O25 K3 O21 C108 -43.1(2) . . . . ?
Cl3 K3 O21 C108 -113.99(19) . . . . ?
C105 K3 O21 C108 -23.2(2) . . . . ?
C101 K3 O21 C108 -178.1(2) . . . . ?
O7 K3 O22 C99 -99.2(2) . . . . ?
O26 K3 O22 C99 145.0(2) . . . . ?
O24 K3 O22 C99 -7.8(3) . . . . ?
O23 K3 O22 C99 -7.5(2) . . . . ?
O21 K3 O22 C99 142.8(3) . . . . ?
O25 K3 O22 C99 72.2(3) . . . . ?
Cl3 K3 O22 C99 60.2(2) . . . . ?
C105 K3 O22 C99 144.5(3) . . . . ?
C101 K3 O22 C99 -19.2(2) . . . . ?
O7 K3 O22 C98 117.9(2) . . . . ?
O26 K3 O22 C98 2.1(3) . . . . ?
O24 K3 O22 C98 -150.7(2) . . . . ?
O23 K3 O22 C98 -150.4(3) . . . . ?
O21 K3 O22 C98 -0.1(2) . . . . ?
O25 K3 O22 C98 -70.7(3) . . . . ?
Cl3 K3 O22 C98 -82.7(2) . . . . ?
C105 K3 O22 C98 1.7(4) . . . . ?
C101 K3 O22 C98 -162.0(2) . . . . ?
O7 K3 O23 C100 78.1(2) . . . . ?
O26 K3 O23 C100 -117.0(3) . . . . ?
O24 K3 O23 C100 154.1(2) . . . . ?
O22 K3 O23 C100 -25.7(2) . . . . ?
O21 K3 O23 C100 -52.9(2) . . . . ?
O25 K3 O23 C100 174.6(2) . . . . ?
Cl3 K3 O23 C100 -122.8(2) . . . . ?
C105 K3 O23 C100 168.5(2) . . . . ?
C101 K3 O23 C100 123.3(3) . . . . ?
O7 K3 O23 C101 -45.2(2) . . . . ?
O26 K3 O23 C101 119.7(2) . . . . ?
O24 K3 O23 C101 30.8(2) . . . . ?
O22 K3 O23 C101 -149.0(2) . . . . ?
O21 K3 O23 C101 -176.2(2) . . . . ?
O25 K3 O23 C101 51.3(2) . . . . ?
Cl3 K3 O23 C101 113.9(2) . . . . ?
C105 K3 O23 C101 45.2(3) . . . . ?
O7 K3 O24 C103 -101.5(2) . . . . ?
O26 K3 O24 C103 0.4(2) . . . . ?
O22 K3 O24 C103 153.4(2) . . . . ?
O23 K3 O24 C103 153.1(2) . . . . ?
O21 K3 O24 C103 73.3(3) . . . . ?
O25 K3 O24 C103 -4.8(2) . . . . ?
Cl3 K3 O24 C103 79.2(2) . . . . ?
C105 K3 O24 C103 -16.9(2) . . . . ?
C101 K3 O24 C103 170.4(3) . . . . ?
O7 K3 O24 C102 107.9(2) . . . . ?
O26 K3 O24 C102 -150.2(2) . . . . ?
O22 K3 O24 C102 2.8(2) . . . . ?
O23 K3 O24 C102 2.5(2) . . . . ?
O21 K3 O24 C102 -77.3(3) . . . . ?
O25 K3 O24 C102 -155.5(2) . . . . ?
Cl3 K3 O24 C102 -71.5(2) . . . . ?
C105 K3 O24 C102 -167.6(2) . . . . ?
C101 K3 O24 C102 19.8(2) . . . . ?
O7 K3 O25 C105 -67.9(2) . . . . ?
O26 K3 O25 C105 37.20(19) . . . . ?
O24 K3 O25 C105 -148.3(2) . . . . ?
O22 K3 O25 C105 120.4(3) . . . . ?
O23 K3 O25 C105 -169.29(19) . . . . ?
O21 K3 O25 C105 58.8(2) . . . . ?
Cl3 K3 O25 C105 132.63(19) . . . . ?
C101 K3 O25 C105 -151.5(2) . . . . ?
O7 K3 O25 C104 51.9(2) . . . . ?
O26 K3 O25 C104 157.0(2) . . . . ?
O24 K3 O25 C104 -28.50(19) . . . . ?
O22 K3 O25 C104 -119.9(3) . . . . ?
O23 K3 O25 C104 -49.5(2) . . . . ?
O21 K3 O25 C104 178.56(19) . . . . ?
Cl3 K3 O25 C104 -107.58(19) . . . . ?
C105 K3 O25 C104 119.8(3) . . . . ?
C101 K3 O25 C104 -31.7(2) . . . . ?
O7 K3 O26 C106 77.0(2) . . . . ?
O24 K3 O26 C106 -11.8(2) . . . . ?
O22 K3 O26 C106 -165.6(2) . . . . ?
O23 K3 O26 C106 -87.6(3) . . . . ?
O21 K3 O26 C106 -163.4(3) . . . . ?
O25 K3 O26 C106 -6.6(2) . . . . ?
Cl3 K3 O26 C106 -82.2(2) . . . . ?
C105 K3 O26 C106 14.2(2) . . . . ?
C101 K3 O26 C106 -28.8(4) . . . . ?
O7 K3 O26 C107 -131.5(2) . . . . ?
O24 K3 O26 C107 139.7(2) . . . . ?
O22 K3 O26 C107 -14.1(2) . . . . ?
O23 K3 O26 C107 63.9(3) . . . . ?
O21 K3 O26 C107 -11.9(2) . . . . ?
O25 K3 O26 C107 145.0(2) . . . . ?
Cl3 K3 O26 C107 69.3(2) . . . . ?
C105 K3 O26 C107 165.7(3) . . . . ?
C101 K3 O26 C107 122.7(3) . . . . ?
C108 O21 C97 C98 173.4(3) . . . . ?
K3 O21 C97 C98 -63.2(3) . . . . ?
C99 O22 C98 C97 -174.8(3) . . . . ?
K3 O22 C98 C97 -30.5(4) . . . . ?
O21 C97 C98 O22 64.0(4) . . . . ?
C98 O22 C99 C100 -175.1(3) . . . . ?
K3 O22 C99 C100 39.0(4) . . . . ?
C101 O23 C100 C99 178.3(3) . . . . ?
K3 O23 C100 C99 57.6(3) . . . . ?
O22 C99 C100 O23 -65.3(4) . . . . ?
C100 O23 C101 C102 174.5(3) . . . . ?
K3 O23 C101 C102 -63.2(3) . . . . ?
C100 O23 C101 K3 -122.3(3) . . . . ?
O7 K3 C101 O23 135.2(2) . . . . ?
O26 K3 C101 O23 -114.9(3) . . . . ?
O24 K3 C101 O23 -138.1(3) . . . . ?
O22 K3 C101 O23 27.0(2) . . . . ?
O21 K3 C101 O23 5.0(3) . . . . ?
O25 K3 C101 O23 -134.0(2) . . . . ?
Cl3 K3 C101 O23 -60.0(2) . . . . ?
C105 K3 C101 O23 -146.43(19) . . . . ?
O7 K3 C101 C102 -103.2(2) . . . . ?
O26 K3 C101 C102 6.6(4) . . . . ?
O24 K3 C101 C102 -16.62(19) . . . . ?
O22 K3 C101 C102 148.5(2) . . . . ?
O23 K3 C101 C102 121.5(3) . . . . ?
O21 K3 C101 C102 126.5(2) . . . . ?
O25 K3 C101 C102 -12.5(2) . . . . ?
Cl3 K3 C101 C102 61.5(2) . . . . ?
C105 K3 C101 C102 -24.9(3) . . . . ?
C103 O24 C102 C101 172.8(3) . . . . ?
K3 O24 C102 C101 -34.3(4) . . . . ?
O23 C101 C102 O24 66.2(4) . . . . ?
K3 C101 C102 O24 23.3(2) . . . . ?
C102 O24 C103 C104 -172.3(3) . . . . ?
K3 O24 C103 C104 36.0(3) . . . . ?
C105 O25 C104 C103 173.5(3) . . . . ?
K3 O25 C104 C103 59.5(3) . . . . ?
O24 C103 C104 O25 -63.9(3) . . . . ?
C104 O25 C105 C106 174.4(3) . . . . ?
K3 O25 C105 C106 -68.0(3) . . . . ?
C104 O25 C105 K3 -117.6(2) . . . . ?
O7 K3 C105 O25 111.17(19) . . . . ?
O26 K3 C105 O25 -129.3(2) . . . . ?
O24 K3 C105 O25 27.12(18) . . . . ?
O22 K3 C105 O25 -128.8(2) . . . . ?
O23 K3 C105 O25 14.4(3) . . . . ?
O21 K3 C105 O25 -127.24(18) . . . . ?
Cl3 K3 C105 O25 -45.73(19) . . . . ?
C101 K3 C105 O25 32.7(2) . . . . ?
O7 K3 C105 C106 -131.0(2) . . . . ?
O26 K3 C105 C106 -11.56(18) . . . . ?
O24 K3 C105 C106 144.9(2) . . . . ?
O22 K3 C105 C106 -11.0(4) . . . . ?
O23 K3 C105 C106 132.2(2) . . . . ?
O21 K3 C105 C106 -9.5(2) . . . . ?
O25 K3 C105 C106 117.8(3) . . . . ?
Cl3 K3 C105 C106 72.1(2) . . . . ?
C101 K3 C105 C106 150.5(2) . . . . ?
C107 O26 C106 C105 -177.5(3) . . . . ?
K3 O26 C106 C105 -24.1(4) . . . . ?
O25 C105 C106 O26 64.8(4) . . . . ?
K3 C105 C106 O26 16.0(2) . . . . ?
C106 O26 C107 C108 -163.5(3) . . . . ?
K3 O26 C107 C108 43.0(3) . . . . ?
C97 O21 C108 C107 173.1(3) . . . . ?
K3 O21 C108 C107 52.1(3) . . . . ?
O26 C107 C108 O21 -63.0(3) . . . . ?
S2 O8 K4 O29 156.73(13) . . . . ?
S2 O8 K4 O27 -104.95(13) . . . . ?
S2 O8 K4 O28 -144.23(13) . . . . ?
S2 O8 K4 F56 -14.21(12) . . . . ?
S2 O8 K4 O31 54.82(14) . . . . ?
S2 O8 K4 O32 -22.58(18) . . . . ?
S2 O8 K4 O30 118.61(12) . . . . ?
S2 O8 K4 F55 52.08(11) . . . . ?
S2 O8 K4 F31 -76.03(12) . . . . ?
C92 F56 K4 O29 -60.0(6) . . . . ?
C92 F56 K4 O27 88.0(6) . . . . ?
C92 F56 K4 O8 -37.1(6) . . . . ?
C92 F56 K4 O28 38.9(6) . . . . ?
C92 F56 K4 O31 -161.5(6) . . . . ?
C92 F56 K4 O32 137.7(6) . . . . ?
C92 F56 K4 O30 -157.2(6) . . . . ?
C92 F56 K4 F55 -95.4(6) . . . . ?
C92 F56 K4 F31 17.7(6) . . . . ?
C90 F55 K4 O29 162.5(2) . . . . ?
C90 F55 K4 O27 -20.6(3) . . . . ?
C90 F55 K4 O8 -129.3(2) . . . . ?
C90 F55 K4 O28 -153.84(19) . . . . ?
C90 F55 K4 F56 -30.49(19) . . . . ?
C90 F55 K4 O31 53.3(2) . . . . ?
C90 F55 K4 O32 17.2(2) . . . . ?
C90 F55 K4 O30 106.9(2) . . . . ?
C90 F55 K4 F31 -87.6(2) . . . . ?
C62 F31 K4 O29 149.9(3) . . . . ?
C62 F31 K4 O27 -108.1(3) . . . . ?
C62 F31 K4 O8 96.2(3) . . . . ?
C62 F31 K4 O28 -168.6(3) . . . . ?
C62 F31 K4 F56 -6.4(3) . . . . ?
C62 F31 K4 O31 -5.3(3) . . . . ?
C62 F31 K4 O32 -57.3(3) . . . . ?
C62 F31 K4 O30 158.4(3) . . . . ?
C62 F31 K4 F55 53.0(3) . . . . ?
O29 K4 O27 C109 64.3(2) . . . . ?
O8 K4 O27 C109 -16.4(2) . . . . ?
O28 K4 O27 C109 31.92(19) . . . . ?
F56 K4 O27 C109 -103.3(2) . . . . ?
O31 K4 O27 C109 -178.07(19) . . . . ?
O32 K4 O27 C109 -156.4(2) . . . . ?
O30 K4 O27 C109 123.1(2) . . . . ?
F55 K4 O27 C109 -112.5(2) . . . . ?
F31 K4 O27 C109 -41.3(2) . . . . ?
O29 K4 O27 C120 -163.1(2) . . . . ?
O8 K4 O27 C120 116.2(2) . . . . ?
O28 K4 O27 C120 164.6(2) . . . . ?
F56 K4 O27 C120 29.3(2) . . . . ?
O31 K4 O27 C120 -45.4(2) . . . . ?
O32 K4 O27 C120 -23.74(19) . . . . ?
O30 K4 O27 C120 -104.2(2) . . . . ?
F55 K4 O27 C120 20.1(3) . . . . ?
F31 K4 O27 C120 91.3(2) . . . . ?
O29 K4 O28 C111 1.80(19) . . . . ?
O27 K4 O28 C111 144.5(2) . . . . ?
O8 K4 O28 C111 -73.5(2) . . . . ?
F56 K4 O28 C111 -151.34(19) . . . . ?
O31 K4 O28 C111 71.9(2) . . . . ?
O32 K4 O28 C111 136.92(19) . . . . ?
O30 K4 O28 C111 41.1(2) . . . . ?
F55 K4 O28 C111 -52.5(2) . . . . ?
F31 K4 O28 C111 -130.7(2) . . . . ?
O29 K4 O28 C110 -142.9(2) . . . . ?
O27 K4 O28 C110 -0.1(2) . . . . ?
O8 K4 O28 C110 141.8(2) . . . . ?
F56 K4 O28 C110 64.0(2) . . . . ?
O31 K4 O28 C110 -72.7(2) . . . . ?
O32 K4 O28 C110 -7.8(2) . . . . ?
O30 K4 O28 C110 -103.6(2) . . . . ?
F55 K4 O28 C110 162.87(19) . . . . ?
F31 K4 O28 C110 84.6(2) . . . . ?
O27 K4 O29 C113 63.28(19) . . . . ?
O8 K4 O29 C113 -174.05(19) . . . . ?
O28 K4 O29 C113 95.23(19) . . . . ?
F56 K4 O29 C113 -150.19(19) . . . . ?
O31 K4 O29 C113 -55.66(19) . . . . ?
O32 K4 O29 C113 5.4(2) . . . . ?
O30 K4 O29 C113 -36.13(18) . . . . ?
F55 K4 O29 C113 -117.80(19) . . . . ?
F31 K4 O29 C113 141.25(18) . . . . ?
O27 K4 O29 C112 -62.76(19) . . . . ?
O8 K4 O29 C112 59.92(18) . . . . ?
O28 K4 O29 C112 -30.81(18) . . . . ?
F56 K4 O29 C112 83.8(2) . . . . ?
O31 K4 O29 C112 178.31(18) . . . . ?
O32 K4 O29 C112 -120.66(19) . . . . ?
O30 K4 O29 C112 -162.2(2) . . . . ?
F55 K4 O29 C112 116.17(19) . . . . ?
F31 K4 O29 C112 15.22(19) . . . . ?
O29 K4 O30 C115 -133.3(2) . . . . ?
O27 K4 O30 C115 128.0(2) . . . . ?
O8 K4 O30 C115 -87.9(2) . . . . ?
O28 K4 O30 C115 -173.6(2) . . . . ?
F56 K4 O30 C115 19.1(2) . . . . ?
O31 K4 O30 C115 24.15(19) . . . . ?
O32 K4 O30 C115 72.1(2) . . . . ?
F55 K4 O30 C115 -35.8(2) . . . . ?
F31 K4 O30 C115 -142.9(2) . . . . ?
O29 K4 O30 C114 2.7(2) . . . . ?
O27 K4 O30 C114 -96.0(2) . . . . ?
O8 K4 O30 C114 48.0(2) . . . . ?
O28 K4 O30 C114 -37.6(2) . . . . ?
F56 K4 O30 C114 155.1(2) . . . . ?
O31 K4 O30 C114 160.1(2) . . . . ?
O32 K4 O30 C114 -152.0(2) . . . . ?
F55 K4 O30 C114 100.2(2) . . . . ?
F31 K4 O30 C114 -6.9(4) . . . . ?
O29 K4 O31 C117 163.43(18) . . . . ?
O27 K4 O31 C117 47.27(19) . . . . ?
O8 K4 O31 C117 -115.18(18) . . . . ?
O28 K4 O31 C117 106.0(2) . . . . ?
F56 K4 O31 C117 -40.23(18) . . . . ?
O32 K4 O31 C117 25.63(17) . . . . ?
O30 K4 O31 C117 143.8(2) . . . . ?
F55 K4 O31 C117 -112.53(19) . . . . ?
F31 K4 O31 C117 -41.3(2) . . . . ?
O29 K4 O31 C116 30.1(2) . . . . ?
O27 K4 O31 C116 -86.1(2) . . . . ?
O8 K4 O31 C116 111.5(2) . . . . ?
O28 K4 O31 C116 -27.3(3) . . . . ?
F56 K4 O31 C116 -173.6(2) . . . . ?
O32 K4 O31 C116 -107.7(2) . . . . ?
O30 K4 O31 C116 10.4(2) . . . . ?
F55 K4 O31 C116 114.1(2) . . . . ?
F31 K4 O31 C116 -174.62(19) . . . . ?
O29 K4 O32 C118 -73.9(2) . . . . ?
O27 K4 O32 C118 -149.5(2) . . . . ?
O8 K4 O32 C118 105.1(2) . . . . ?
O28 K4 O32 C118 -141.9(2) . . . . ?
F56 K4 O32 C118 95.6(2) . . . . ?
O31 K4 O32 C118 6.2(2) . . . . ?
O30 K4 O32 C118 -40.5(2) . . . . ?
F55 K4 O32 C118 44.7(2) . . . . ?
F31 K4 O32 C118 148.2(2) . . . . ?
O29 K4 O32 C119 65.6(2) . . . . ?
O27 K4 O32 C119 -10.00(19) . . . . ?
O8 K4 O32 C119 -115.4(2) . . . . ?
O28 K4 O32 C119 -2.4(2) . . . . ?
F56 K4 O32 C119 -124.9(2) . . . . ?
O31 K4 O32 C119 145.7(2) . . . . ?
O30 K4 O32 C119 99.0(2) . . . . ?
F55 K4 O32 C119 -175.81(19) . . . . ?
F31 K4 O32 C119 -72.3(2) . . . . ?
C120 O27 C109 C110 163.3(3) . . . . ?
K4 O27 C109 C110 -61.9(3) . . . . ?
C111 O28 C110 C109 -176.3(3) . . . . ?
K4 O28 C110 C109 -29.4(3) . . . . ?
O27 C109 C110 O28 59.9(4) . . . . ?
C110 O28 C111 C112 172.6(3) . . . . ?
K4 O28 C111 C112 25.9(3) . . . . ?
C113 O29 C112 C111 -61.6(3) . . . . ?
K4 O29 C112 C111 62.2(3) . . . . ?
O28 C111 C112 O29 -59.6(3) . . . . ?
C112 O29 C113 C114 -166.0(3) . . . . ?
K4 O29 C113 C114 70.4(3) . . . . ?
C115 O30 C114 C113 167.1(3) . . . . ?
K4 O30 C114 C113 28.8(3) . . . . ?
O29 C113 C114 O30 -65.1(4) . . . . ?
C114 O30 C115 C116 165.8(3) . . . . ?
K4 O30 C115 C116 -55.0(3) . . . . ?
C117 O31 C116 C115 -174.1(3) . . . . ?
K4 O31 C116 C115 -41.3(3) . . . . ?
O30 C115 C116 O31 62.5(3) . . . . ?
C116 O31 C117 C118 78.6(3) . . . . ?
K4 O31 C117 C118 -57.8(3) . . . . ?
C119 O32 C118 C117 -176.7(3) . . . . ?
K4 O32 C118 C117 -35.4(3) . . . . ?
O31 C117 C118 O32 63.2(4) . . . . ?
C118 O32 C119 C120 -177.6(3) . . . . ?
K4 O32 C119 C120 40.1(3) . . . . ?
C109 O27 C120 C119 -172.7(3) . . . . ?
K4 O27 C120 C119 54.3(3) . . . . ?
O32 C119 C120 O27 -61.9(3) . . . . ?
Cl2 C121 Cl1 K1 -126.3(3) . . . . ?
O3 K1 Cl1 C121 -71.3(3) . . . . ?
O9 K1 Cl1 C121 40.7(2) . . . . ?
O13 K1 Cl1 C121 -79.2(2) . . . . ?
O11 K1 Cl1 C121 158.1(2) . . . . ?
O12 K1 Cl1 C121 -143.2(2) . . . . ?
O10 K1 Cl1 C121 99.8(2) . . . . ?
O14 K1 Cl1 C121 -18.0(2) . . . . ?
C47 K1 Cl1 C121 -0.9(2) . . . . ?
Cl4B C122 Cl3 K3 -134.5(5) . . . . ?
Cl4A C122 Cl3 K3 -107.3(3) . . . . ?
O7 K3 Cl3 C122 -79.5(2) . . . . ?
O26 K3 Cl3 C122 40.66(17) . . . . ?
O24 K3 Cl3 C122 -77.96(17) . . . . ?
O22 K3 Cl3 C122 158.36(17) . . . . ?
O23 K3 Cl3 C122 -141.69(17) . . . . ?
O21 K3 Cl3 C122 99.54(17) . . . . ?
O25 K3 Cl3 C122 -17.73(16) . . . . ?
C105 K3 Cl3 C122 -1.00(17) . . . . ?
C101 K3 Cl3 C122 -120.58(17) . . . . ?
_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full 24.51
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max 1.012
_refine_diff_density_min -0.710
_refine_diff_density_rms 0.072
#=============================================================================
data_KV70
_database_code_depnum_ccdc_archive 'CCDC 817750'
#TrackingRef '- boran-sauerstoff.cif'
_audit_author_name 'Voss, K.'
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C28 H20 B F15 O4'
_chemical_formula_sum 'C28 H20 B F15 O4'
_chemical_formula_weight 716.25
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'
B B 0.0013 0.0007 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.110(2)
_cell_length_b 10.950(4)
_cell_length_c 13.482(4)
_cell_angle_alpha 75.23(3)
_cell_angle_beta 81.81(2)
_cell_angle_gamma 82.94(2)
_cell_volume 1422.6(7)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 29445
_cell_measurement_theta_min 8.62
_cell_measurement_theta_max 66.00
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.44
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.19
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.672
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 720
_exptl_absorpt_coefficient_mu 0.175
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9270
_exptl_absorpt_correction_T_max 0.9675
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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 Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and psi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 29445
_diffrn_reflns_av_R_equivalents 0.0332
_diffrn_reflns_av_sigmaI/netI 0.0339
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 4.31
_diffrn_reflns_theta_max 33.00
_reflns_number_total 10676
_reflns_number_gt 8229
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex v2.0-2'
_computing_cell_refinement 'Bruker Apex v2.0-2'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a
riding model , with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_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^)+(0.0746P)^2^+0.0592P] 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 10676
_refine_ls_number_parameters 433
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0575
_refine_ls_R_factor_gt 0.0415
_refine_ls_wR_factor_ref 0.1235
_refine_ls_wR_factor_gt 0.1150
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_restrained_S_all 1.050
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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
O1 O 0.87428(6) 0.67606(6) 0.19523(5) 0.01891(12) Uani 1 1 d . . .
B1 B 0.75163(9) 0.75180(9) 0.14022(7) 0.01687(16) Uani 1 1 d . . .
C1 C 0.64129(8) 0.65310(8) 0.14108(7) 0.01905(15) Uani 1 1 d . . .
C2 C 0.65505(10) 0.52219(9) 0.17328(7) 0.02340(17) Uani 1 1 d . . .
C3 C 0.55891(11) 0.44616(10) 0.16382(8) 0.02846(19) Uani 1 1 d . . .
C4 C 0.44471(10) 0.50095(11) 0.11998(8) 0.0289(2) Uani 1 1 d . . .
C5 C 0.42711(9) 0.63042(10) 0.08434(8) 0.02711(19) Uani 1 1 d . . .
C6 C 0.52467(9) 0.70273(9) 0.09483(7) 0.02227(16) Uani 1 1 d . . .
C7 C 0.80058(8) 0.81077(8) 0.01795(6) 0.01774(14) Uani 1 1 d . . .
C8 C 0.84711(9) 0.72997(9) -0.04702(7) 0.02070(16) Uani 1 1 d . . .
C9 C 0.87244(10) 0.76933(11) -0.15337(7) 0.02750(19) Uani 1 1 d . . .
C10 C 0.84997(11) 0.89597(11) -0.20053(7) 0.0298(2) Uani 1 1 d . . .
C11 C 0.80403(10) 0.98035(10) -0.14085(8) 0.02722(19) Uani 1 1 d . . .
C12 C 0.78076(9) 0.93732(9) -0.03441(7) 0.02219(16) Uani 1 1 d . . .
C13 C 0.69861(8) 0.85748(8) 0.20734(7) 0.01913(15) Uani 1 1 d . . .
C14 C 0.57437(9) 0.86996(9) 0.26449(7) 0.02237(16) Uani 1 1 d . . .
C15 C 0.53838(10) 0.96087(9) 0.32126(8) 0.02664(19) Uani 1 1 d . . .
C16 C 0.62918(11) 1.04299(9) 0.32461(8) 0.02758(19) Uani 1 1 d . . .
C17 C 0.75496(10) 1.03414(9) 0.27046(8) 0.02706(19) Uani 1 1 d . . .
C18 C 0.78633(9) 0.94267(9) 0.21465(7) 0.02265(17) Uani 1 1 d . . .
C19 C 0.86334(10) 0.63475(9) 0.30965(7) 0.02436(17) Uani 1 1 d . . .
H19A H 0.7824 0.5890 0.3378 0.029 Uiso 1 1 calc R . .
H19B H 0.8598 0.7081 0.3406 0.029 Uiso 1 1 calc R . .
C20 C 0.98908(10) 0.54810(9) 0.32986(7) 0.02688(19) Uani 1 1 d . . .
H20A H 0.9785 0.4616 0.3241 0.032 Uiso 1 1 calc R . .
H20B H 1.0146 0.5435 0.3990 0.032 Uiso 1 1 calc R . .
C21 C 1.09130(10) 0.61231(10) 0.24466(8) 0.0292(2) Uani 1 1 d . . .
H21A H 1.1229 0.6853 0.2624 0.035 Uiso 1 1 calc R . .
H21B H 1.1695 0.5520 0.2323 0.035 Uiso 1 1 calc R . .
C22 C 1.01498(9) 0.65577(10) 0.15095(7) 0.02586(18) Uani 1 1 d . . .
H22A H 1.0466 0.7354 0.1052 0.031 Uiso 1 1 calc R . .
H22B H 1.0253 0.5901 0.1110 0.031 Uiso 1 1 calc R . .
F1 F 0.76496(7) 0.45950(6) 0.21514(6) 0.03439(15) Uani 1 1 d . . .
F2 F 0.57791(8) 0.32000(6) 0.19643(6) 0.04346(18) Uani 1 1 d . . .
F3 F 0.35132(7) 0.42869(8) 0.11066(6) 0.04339(19) Uani 1 1 d . . .
F4 F 0.31729(6) 0.68429(7) 0.03922(6) 0.03923(17) Uani 1 1 d . . .
F5 F 0.50420(6) 0.82862(6) 0.05782(5) 0.02975(13) Uani 1 1 d . . .
F6 F 0.86777(6) 0.60437(5) -0.00670(5) 0.02669(12) Uani 1 1 d . . .
F7 F 0.91742(8) 0.68556(8) -0.21008(5) 0.04196(17) Uani 1 1 d . . .
F8 F 0.87340(8) 0.93652(8) -0.30322(5) 0.04581(19) Uani 1 1 d . . .
F9 F 0.78308(8) 1.10370(7) -0.18555(6) 0.04207(17) Uani 1 1 d . . .
F10 F 0.73420(7) 1.02755(6) 0.01628(5) 0.03221(14) Uani 1 1 d . . .
F11 F 0.47992(6) 0.79135(6) 0.27007(5) 0.03322(14) Uani 1 1 d . . .
F12 F 0.41594(7) 0.96746(7) 0.37431(6) 0.04293(18) Uani 1 1 d . . .
F13 F 0.59726(8) 1.12751(7) 0.38225(6) 0.04038(17) Uani 1 1 d . . .
F14 F 0.84464(7) 1.11287(7) 0.27311(7) 0.04261(18) Uani 1 1 d . . .
F15 F 0.91157(6) 0.93782(6) 0.16469(6) 0.03185(14) Uani 1 1 d . . .
O2 O 0.11487(7) 0.27343(6) 0.46434(6) 0.02772(15) Uani 1 1 d . . .
O3 O 0.29966(8) 0.44340(7) 0.47143(6) 0.02889(15) Uani 1 1 d . . .
O4 O 0.16447(7) 0.69420(7) 0.46240(6) 0.02765(15) Uani 1 1 d . . .
C23 C 0.25419(11) 0.23812(9) 0.46575(8) 0.02858(19) Uani 1 1 d . . .
H23A H 0.2817 0.1691 0.4298 0.034 Uiso 1 1 calc R . .
H23B H 0.2751 0.2071 0.5379 0.034 Uiso 1 1 calc R . .
C24 C 0.32891(10) 0.35175(10) 0.41251(8) 0.0286(2) Uani 1 1 d . . .
H24A H 0.4266 0.3266 0.4055 0.034 Uiso 1 1 calc R . .
H24B H 0.3015 0.3876 0.3425 0.034 Uiso 1 1 calc R . .
C25 C 0.35626(10) 0.55876(10) 0.42236(8) 0.02706(19) Uani 1 1 d . . .
H25A H 0.3343 0.5877 0.3503 0.032 Uiso 1 1 calc R . .
H25B H 0.4551 0.5463 0.4209 0.032 Uiso 1 1 calc R . .
C26 C 0.29972(10) 0.65649(10) 0.48172(8) 0.02727(19) Uani 1 1 d . . .
H26A H 0.3038 0.6203 0.5565 0.033 Uiso 1 1 calc R . .
H26B H 0.3530 0.7308 0.4596 0.033 Uiso 1 1 calc R . .
C27 C 0.10632(11) 0.78993(10) 0.51261(8) 0.0294(2) Uani 1 1 d . . .
H27A H 0.1592 0.8645 0.4894 0.035 Uiso 1 1 calc R . .
H27B H 0.1066 0.7580 0.5882 0.035 Uiso 1 1 calc R . .
C28 C 0.03558(11) 0.17224(9) 0.51270(8) 0.0289(2) Uani 1 1 d . . .
H28A H 0.0373 0.1521 0.5884 0.035 Uiso 1 1 calc R . .
H28B H 0.0720 0.0957 0.4880 0.035 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0181(3) 0.0225(3) 0.0151(3) -0.0042(2) -0.0026(2) 0.0025(2)
B1 0.0176(4) 0.0157(4) 0.0174(4) -0.0047(3) -0.0023(3) 0.0000(3)
C1 0.0195(4) 0.0186(4) 0.0189(4) -0.0050(3) -0.0008(3) -0.0021(3)
C2 0.0272(4) 0.0201(4) 0.0226(4) -0.0046(3) -0.0019(3) -0.0035(3)
C3 0.0376(5) 0.0220(4) 0.0269(4) -0.0074(3) 0.0032(4) -0.0117(4)
C4 0.0278(4) 0.0356(5) 0.0280(5) -0.0142(4) 0.0051(4) -0.0165(4)
C5 0.0199(4) 0.0367(5) 0.0274(4) -0.0112(4) -0.0017(3) -0.0070(4)
C6 0.0203(4) 0.0234(4) 0.0235(4) -0.0059(3) -0.0019(3) -0.0035(3)
C7 0.0171(3) 0.0182(4) 0.0177(3) -0.0034(3) -0.0027(3) -0.0016(3)
C8 0.0219(4) 0.0217(4) 0.0191(4) -0.0057(3) -0.0025(3) -0.0028(3)
C9 0.0295(5) 0.0362(5) 0.0191(4) -0.0108(4) -0.0001(3) -0.0063(4)
C10 0.0296(5) 0.0409(6) 0.0163(4) 0.0003(4) -0.0021(3) -0.0089(4)
C11 0.0260(4) 0.0263(5) 0.0246(4) 0.0048(3) -0.0046(3) -0.0051(3)
C12 0.0219(4) 0.0198(4) 0.0236(4) -0.0025(3) -0.0039(3) -0.0011(3)
C13 0.0194(4) 0.0176(4) 0.0205(4) -0.0061(3) -0.0028(3) 0.0017(3)
C14 0.0228(4) 0.0206(4) 0.0226(4) -0.0061(3) 0.0011(3) -0.0001(3)
C15 0.0283(4) 0.0241(4) 0.0246(4) -0.0078(3) 0.0039(3) 0.0051(3)
C16 0.0388(5) 0.0198(4) 0.0246(4) -0.0100(3) -0.0048(4) 0.0070(4)
C17 0.0310(5) 0.0223(4) 0.0320(5) -0.0128(4) -0.0081(4) 0.0004(3)
C18 0.0208(4) 0.0224(4) 0.0266(4) -0.0102(3) -0.0030(3) 0.0002(3)
C19 0.0307(4) 0.0261(4) 0.0146(4) -0.0039(3) -0.0033(3) 0.0030(3)
C20 0.0345(5) 0.0229(4) 0.0215(4) -0.0026(3) -0.0092(4) 0.0050(4)
C21 0.0243(4) 0.0329(5) 0.0286(5) -0.0032(4) -0.0103(4) 0.0033(4)
C22 0.0178(4) 0.0351(5) 0.0217(4) -0.0055(4) -0.0018(3) 0.0055(3)
F1 0.0390(3) 0.0196(3) 0.0440(4) -0.0028(3) -0.0156(3) 0.0018(2)
F2 0.0609(5) 0.0206(3) 0.0490(4) -0.0051(3) -0.0035(4) -0.0144(3)
F3 0.0399(4) 0.0518(5) 0.0477(4) -0.0223(4) 0.0035(3) -0.0280(3)
F4 0.0230(3) 0.0527(4) 0.0456(4) -0.0133(3) -0.0111(3) -0.0060(3)
F5 0.0242(3) 0.0249(3) 0.0378(3) -0.0019(2) -0.0093(2) 0.0012(2)
F6 0.0354(3) 0.0203(3) 0.0254(3) -0.0090(2) -0.0025(2) 0.0000(2)
F7 0.0556(4) 0.0486(4) 0.0252(3) -0.0200(3) 0.0044(3) -0.0057(3)
F8 0.0529(4) 0.0615(5) 0.0169(3) 0.0032(3) -0.0009(3) -0.0120(4)
F9 0.0497(4) 0.0289(3) 0.0370(4) 0.0124(3) -0.0074(3) -0.0029(3)
F10 0.0436(4) 0.0181(3) 0.0319(3) -0.0043(2) -0.0047(3) 0.0061(2)
F11 0.0275(3) 0.0349(3) 0.0385(3) -0.0158(3) 0.0116(2) -0.0105(3)
F12 0.0384(4) 0.0407(4) 0.0468(4) -0.0204(3) 0.0188(3) 0.0008(3)
F13 0.0579(4) 0.0299(3) 0.0369(4) -0.0217(3) -0.0022(3) 0.0073(3)
F14 0.0409(4) 0.0384(4) 0.0607(5) -0.0311(4) -0.0073(3) -0.0086(3)
F15 0.0198(3) 0.0344(3) 0.0471(4) -0.0216(3) 0.0010(2) -0.0052(2)
O2 0.0292(3) 0.0180(3) 0.0333(4) -0.0037(3) -0.0032(3) 0.0023(3)
O3 0.0336(4) 0.0266(3) 0.0241(3) -0.0065(3) 0.0054(3) -0.0029(3)
O4 0.0283(3) 0.0274(3) 0.0319(4) -0.0145(3) -0.0058(3) -0.0020(3)
C23 0.0319(5) 0.0223(4) 0.0292(5) -0.0076(4) -0.0026(4) 0.0085(4)
C24 0.0274(5) 0.0297(5) 0.0261(4) -0.0085(4) 0.0026(4) 0.0053(4)
C25 0.0214(4) 0.0323(5) 0.0253(4) -0.0034(4) -0.0006(3) -0.0044(3)
C26 0.0266(4) 0.0301(5) 0.0268(4) -0.0060(4) -0.0045(3) -0.0095(4)
C27 0.0385(5) 0.0225(4) 0.0310(5) -0.0118(4) -0.0032(4) -0.0072(4)
C28 0.0384(5) 0.0173(4) 0.0305(5) -0.0068(3) -0.0020(4) -0.0012(4)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
O1 C22 1.4755(12) . ?
O1 C19 1.4847(11) . ?
O1 B1 1.5721(12) . ?
B1 C7 1.6379(14) . ?
B1 C13 1.6396(13) . ?
B1 C1 1.6427(13) . ?
C1 C2 1.3833(13) . ?
C1 C6 1.3977(13) . ?
C2 F1 1.3484(12) . ?
C2 C3 1.3937(13) . ?
C3 F2 1.3371(13) . ?
C3 C4 1.3732(16) . ?
C4 F3 1.3421(11) . ?
C4 C5 1.3739(16) . ?
C5 F4 1.3415(12) . ?
C5 C6 1.3815(13) . ?
C6 F5 1.3418(12) . ?
C7 C12 1.3899(13) . ?
C7 C8 1.3952(12) . ?
C8 F6 1.3458(12) . ?
C8 C9 1.3837(14) . ?
C9 F7 1.3374(12) . ?
C9 C10 1.3759(16) . ?
C10 F8 1.3375(12) . ?
C10 C11 1.3725(16) . ?
C11 F9 1.3354(13) . ?
C11 C12 1.3868(14) . ?
C12 F10 1.3427(11) . ?
C13 C14 1.3878(13) . ?
C13 C18 1.3933(13) . ?
C14 F11 1.3442(11) . ?
C14 C15 1.3888(13) . ?
C15 F12 1.3421(12) . ?
C15 C16 1.3743(16) . ?
C16 F13 1.3365(11) . ?
C16 C17 1.3786(16) . ?
C17 F14 1.3355(12) . ?
C17 C18 1.3812(13) . ?
C18 F15 1.3485(12) . ?
C19 C20 1.5037(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.5199(16) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.5163(14) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
O2 C28 1.4129(13) . ?
O2 C23 1.4156(13) . ?
O3 C24 1.4114(13) . ?
O3 C25 1.4158(13) . ?
O4 C27 1.4141(13) . ?
O4 C26 1.4199(13) . ?
C23 C24 1.5016(16) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.5060(15) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.5058(16) 2_566 ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C27 1.5058(16) 2_566 ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
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
C22 O1 C19 110.03(7) . . ?
C22 O1 B1 128.87(7) . . ?
C19 O1 B1 120.19(7) . . ?
O1 B1 C7 109.63(7) . . ?
O1 B1 C13 103.27(7) . . ?
C7 B1 C13 114.87(7) . . ?
O1 B1 C1 109.26(7) . . ?
C7 B1 C1 105.18(7) . . ?
C13 B1 C1 114.57(7) . . ?
C2 C1 C6 114.25(8) . . ?
C2 C1 B1 127.53(8) . . ?
C6 C1 B1 117.87(8) . . ?
F1 C2 C1 121.47(8) . . ?
F1 C2 C3 115.47(9) . . ?
C1 C2 C3 123.05(9) . . ?
F2 C3 C4 119.84(9) . . ?
F2 C3 C2 120.28(10) . . ?
C4 C3 C2 119.88(10) . . ?
F3 C4 C3 120.40(10) . . ?
F3 C4 C5 119.97(10) . . ?
C3 C4 C5 119.63(9) . . ?
F4 C5 C4 119.92(9) . . ?
F4 C5 C6 121.20(10) . . ?
C4 C5 C6 118.88(9) . . ?
F5 C6 C5 116.88(8) . . ?
F5 C6 C1 118.85(8) . . ?
C5 C6 C1 124.27(9) . . ?
C12 C7 C8 113.48(8) . . ?
C12 C7 B1 125.64(8) . . ?
C8 C7 B1 120.04(8) . . ?
F6 C8 C9 115.83(8) . . ?
F6 C8 C7 119.75(8) . . ?
C9 C8 C7 124.41(9) . . ?
F7 C9 C10 120.14(9) . . ?
F7 C9 C8 120.64(10) . . ?
C10 C9 C8 119.22(9) . . ?
F8 C10 C11 120.38(10) . . ?
F8 C10 C9 120.44(10) . . ?
C11 C10 C9 119.19(9) . . ?
F9 C11 C10 119.80(9) . . ?
F9 C11 C12 120.32(10) . . ?
C10 C11 C12 119.88(9) . . ?
F10 C12 C11 114.93(9) . . ?
F10 C12 C7 121.24(8) . . ?
C11 C12 C7 123.82(9) . . ?
C14 C13 C18 113.57(8) . . ?
C14 C13 B1 127.31(8) . . ?
C18 C13 B1 119.04(8) . . ?
F11 C14 C13 121.40(8) . . ?
F11 C14 C15 114.93(8) . . ?
C13 C14 C15 123.66(9) . . ?
F12 C15 C16 119.83(9) . . ?
F12 C15 C14 120.23(10) . . ?
C16 C15 C14 119.93(9) . . ?
F13 C16 C15 120.35(10) . . ?
F13 C16 C17 120.53(10) . . ?
C15 C16 C17 119.09(9) . . ?
F14 C17 C16 119.91(9) . . ?
F14 C17 C18 121.03(10) . . ?
C16 C17 C18 119.06(9) . . ?
F15 C18 C17 116.10(8) . . ?
F15 C18 C13 119.23(8) . . ?
C17 C18 C13 124.67(9) . . ?
O1 C19 C20 103.51(8) . . ?
O1 C19 H19A 111.1 . . ?
C20 C19 H19A 111.1 . . ?
O1 C19 H19B 111.1 . . ?
C20 C19 H19B 111.1 . . ?
H19A C19 H19B 109.0 . . ?
C19 C20 C21 102.17(8) . . ?
C19 C20 H20A 111.3 . . ?
C21 C20 H20A 111.3 . . ?
C19 C20 H20B 111.3 . . ?
C21 C20 H20B 111.3 . . ?
H20A C20 H20B 109.2 . . ?
C22 C21 C20 103.97(8) . . ?
C22 C21 H21A 111.0 . . ?
C20 C21 H21A 111.0 . . ?
C22 C21 H21B 111.0 . . ?
C20 C21 H21B 111.0 . . ?
H21A C21 H21B 109.0 . . ?
O1 C22 C21 103.87(8) . . ?
O1 C22 H22A 111.0 . . ?
C21 C22 H22A 111.0 . . ?
O1 C22 H22B 111.0 . . ?
C21 C22 H22B 111.0 . . ?
H22A C22 H22B 109.0 . . ?
C28 O2 C23 113.05(8) . . ?
C24 O3 C25 112.87(8) . . ?
C27 O4 C26 111.81(8) . . ?
O2 C23 C24 108.75(8) . . ?
O2 C23 H23A 109.9 . . ?
C24 C23 H23A 109.9 . . ?
O2 C23 H23B 109.9 . . ?
C24 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
O3 C24 C23 108.91(8) . . ?
O3 C24 H24A 109.9 . . ?
C23 C24 H24A 109.9 . . ?
O3 C24 H24B 109.9 . . ?
C23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
O3 C25 C26 108.54(8) . . ?
O3 C25 H25A 110.0 . . ?
C26 C25 H25A 110.0 . . ?
O3 C25 H25B 110.0 . . ?
C26 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
O4 C26 C25 108.68(8) . . ?
O4 C26 H26A 110.0 . . ?
C25 C26 H26A 110.0 . . ?
O4 C26 H26B 110.0 . . ?
C25 C26 H26B 110.0 . . ?
H26A C26 H26B 108.3 . . ?
O4 C27 C28 109.26(8) . 2_566 ?
O4 C27 H27A 109.8 . . ?
C28 C27 H27A 109.8 2_566 . ?
O4 C27 H27B 109.8 . . ?
C28 C27 H27B 109.8 2_566 . ?
H27A C27 H27B 108.3 . . ?
O2 C28 C27 109.04(9) . 2_566 ?
O2 C28 H28A 109.9 . . ?
C27 C28 H28A 109.9 2_566 . ?
O2 C28 H28B 109.9 . . ?
C27 C28 H28B 109.9 2_566 . ?
H28A C28 H28B 108.3 . . ?
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
C22 O1 B1 C7 0.10(11) . . . . ?
C19 O1 B1 C7 167.99(7) . . . . ?
C22 O1 B1 C13 -122.78(9) . . . . ?
C19 O1 B1 C13 45.11(9) . . . . ?
C22 O1 B1 C1 114.88(9) . . . . ?
C19 O1 B1 C1 -77.24(9) . . . . ?
O1 B1 C1 C2 -6.82(12) . . . . ?
C7 B1 C1 C2 110.79(10) . . . . ?
C13 B1 C1 C2 -122.11(10) . . . . ?
O1 B1 C1 C6 -179.61(7) . . . . ?
C7 B1 C1 C6 -62.00(10) . . . . ?
C13 B1 C1 C6 65.10(10) . . . . ?
C6 C1 C2 F1 176.99(8) . . . . ?
B1 C1 C2 F1 3.98(14) . . . . ?
C6 C1 C2 C3 -2.12(14) . . . . ?
B1 C1 C2 C3 -175.13(9) . . . . ?
F1 C2 C3 F2 0.86(14) . . . . ?
C1 C2 C3 F2 -179.98(9) . . . . ?
F1 C2 C3 C4 -178.55(9) . . . . ?
C1 C2 C3 C4 0.60(15) . . . . ?
F2 C3 C4 F3 0.71(15) . . . . ?
C2 C3 C4 F3 -179.87(9) . . . . ?
F2 C3 C4 C5 -178.45(9) . . . . ?
C2 C3 C4 C5 0.97(15) . . . . ?
F3 C4 C5 F4 -0.75(15) . . . . ?
C3 C4 C5 F4 178.41(9) . . . . ?
F3 C4 C5 C6 180.00(9) . . . . ?
C3 C4 C5 C6 -0.83(15) . . . . ?
F4 C5 C6 F5 -0.04(14) . . . . ?
C4 C5 C6 F5 179.20(9) . . . . ?
F4 C5 C6 C1 179.88(9) . . . . ?
C4 C5 C6 C1 -0.88(15) . . . . ?
C2 C1 C6 F5 -177.79(8) . . . . ?
B1 C1 C6 F5 -4.06(12) . . . . ?
C2 C1 C6 C5 2.28(14) . . . . ?
B1 C1 C6 C5 176.01(9) . . . . ?
O1 B1 C7 C12 -126.58(8) . . . . ?
C13 B1 C7 C12 -10.86(12) . . . . ?
C1 B1 C7 C12 116.06(9) . . . . ?
O1 B1 C7 C8 64.62(10) . . . . ?
C13 B1 C7 C8 -179.66(7) . . . . ?
C1 B1 C7 C8 -52.74(10) . . . . ?
C12 C7 C8 F6 -178.53(7) . . . . ?
B1 C7 C8 F6 -8.44(12) . . . . ?
C12 C7 C8 C9 0.25(13) . . . . ?
B1 C7 C8 C9 170.34(8) . . . . ?
F6 C8 C9 F7 -1.41(13) . . . . ?
C7 C8 C9 F7 179.78(8) . . . . ?
F6 C8 C9 C10 178.17(8) . . . . ?
C7 C8 C9 C10 -0.65(15) . . . . ?
F7 C9 C10 F8 -0.30(15) . . . . ?
C8 C9 C10 F8 -179.88(9) . . . . ?
F7 C9 C10 C11 -179.89(9) . . . . ?
C8 C9 C10 C11 0.54(15) . . . . ?
F8 C10 C11 F9 -0.25(15) . . . . ?
C9 C10 C11 F9 179.33(9) . . . . ?
F8 C10 C11 C12 -179.66(9) . . . . ?
C9 C10 C11 C12 -0.08(15) . . . . ?
F9 C11 C12 F10 1.49(13) . . . . ?
C10 C11 C12 F10 -179.10(8) . . . . ?
F9 C11 C12 C7 -179.74(8) . . . . ?
C10 C11 C12 C7 -0.34(15) . . . . ?
C8 C7 C12 F10 178.94(8) . . . . ?
B1 C7 C12 F10 9.50(13) . . . . ?
C8 C7 C12 C11 0.25(13) . . . . ?
B1 C7 C12 C11 -169.19(8) . . . . ?
O1 B1 C13 C14 -117.54(10) . . . . ?
C7 B1 C13 C14 123.14(10) . . . . ?
C1 B1 C13 C14 1.18(13) . . . . ?
O1 B1 C13 C18 58.94(10) . . . . ?
C7 B1 C13 C18 -60.38(11) . . . . ?
C1 B1 C13 C18 177.66(8) . . . . ?
C18 C13 C14 F11 -176.82(8) . . . . ?
B1 C13 C14 F11 -0.17(15) . . . . ?
C18 C13 C14 C15 1.88(14) . . . . ?
B1 C13 C14 C15 178.52(9) . . . . ?
F11 C14 C15 F12 -1.53(14) . . . . ?
C13 C14 C15 F12 179.70(9) . . . . ?
F11 C14 C15 C16 177.34(9) . . . . ?
C13 C14 C15 C16 -1.43(15) . . . . ?
F12 C15 C16 F13 1.49(15) . . . . ?
C14 C15 C16 F13 -177.38(9) . . . . ?
F12 C15 C16 C17 179.38(9) . . . . ?
C14 C15 C16 C17 0.50(15) . . . . ?
F13 C16 C17 F14 -1.89(15) . . . . ?
C15 C16 C17 F14 -179.77(9) . . . . ?
F13 C16 C17 C18 177.66(9) . . . . ?
C15 C16 C17 C18 -0.22(15) . . . . ?
F14 C17 C18 F15 0.48(14) . . . . ?
C16 C17 C18 F15 -179.06(9) . . . . ?
F14 C17 C18 C13 -179.61(9) . . . . ?
C16 C17 C18 C13 0.85(16) . . . . ?
C14 C13 C18 F15 178.30(8) . . . . ?
B1 C13 C18 F15 1.35(13) . . . . ?
C14 C13 C18 C17 -1.61(14) . . . . ?
B1 C13 C18 C17 -178.55(9) . . . . ?
C22 O1 C19 C20 -19.59(10) . . . . ?
B1 O1 C19 C20 170.42(7) . . . . ?
O1 C19 C20 C21 36.32(9) . . . . ?
C19 C20 C21 C22 -40.33(10) . . . . ?
C19 O1 C22 C21 -5.48(10) . . . . ?
B1 O1 C22 C21 163.39(8) . . . . ?
C20 C21 C22 O1 28.24(10) . . . . ?
C28 O2 C23 C24 179.86(8) . . . . ?
C25 O3 C24 C23 -174.63(8) . . . . ?
O2 C23 C24 O3 66.12(11) . . . . ?
C24 O3 C25 C26 170.15(8) . . . . ?
C27 O4 C26 C25 -177.66(8) . . . . ?
O3 C25 C26 O4 -73.18(10) . . . . ?
C26 O4 C27 C28 178.75(8) . . . 2_566 ?
C23 O2 C28 C27 -167.76(8) . . . 2_566 ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 33.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.505
_refine_diff_density_min -0.301
_refine_diff_density_rms 0.085
#=============================================================================
data_kv86
_database_code_depnum_ccdc_archive 'CCDC 817751'
#TrackingRef '- boran-sauerstoff.cif'
# start Validation Reply Form
_vrf_PLAT410_kv86
;
PROBLEM: Short Intra H...H Contact H25A .. H24C .. 1.49 Ang.
RESPONSE: Atoms belong to a disordered diethylether molecule.
;
# end Validation Reply Form
_audit_author_name 'Voss, K., Villinger, A.'
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C26 H20 B F15 K N O5'
_chemical_formula_sum 'C26 H20 B F15 K N O5'
_chemical_formula_weight 761.34
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'
B B 0.0013 0.0007 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 13.0444(5)
_cell_length_b 14.1638(6)
_cell_length_c 16.8260(7)
_cell_angle_alpha 90.00
_cell_angle_beta 90.394(2)
_cell_angle_gamma 90.00
_cell_volume 3108.7(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9828
_cell_measurement_theta_min 5.632
_cell_measurement_theta_max 63.186
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.73
_exptl_crystal_size_mid 0.60
_exptl_crystal_size_min 0.45
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.627
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1528
_exptl_absorpt_coefficient_mu 0.299
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8114
_exptl_absorpt_correction_T_max 0.8772
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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 Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and psi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 77557
_diffrn_reflns_av_R_equivalents 0.0240
_diffrn_reflns_av_sigmaI/netI 0.0174
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 2.42
_diffrn_reflns_theta_max 32.00
_reflns_number_total 10777
_reflns_number_gt 7691
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex v2.0-2'
_computing_cell_refinement 'Bruker Apex v2.0-2'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a
riding model , with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with U~iso~(H) =
1.5 times U~eq~(C) (methyl groups) or with U~iso~(H) = 1.2 times
U~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_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^)+(0.0594P)^2^+0.7188P] 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 10777
_refine_ls_number_parameters 504
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0672
_refine_ls_R_factor_gt 0.0416
_refine_ls_wR_factor_ref 0.1267
_refine_ls_wR_factor_gt 0.1143
_refine_ls_goodness_of_fit_ref 1.080
_refine_ls_restrained_S_all 1.080
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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
N1 N 1.07862(11) 0.47209(8) 0.86679(7) 0.0410(3) Uani 1 1 d . A .
O1 O 1.05898(7) 0.38374(6) 0.84269(5) 0.03412(19) Uani 1 1 d . A .
O2 O 1.14503(10) 0.51852(7) 0.83616(6) 0.0478(3) Uani 1 1 d . . .
O3 O 1.02407(12) 0.49781(9) 0.92194(7) 0.0618(4) Uani 1 1 d . . .
B1 B 1.11935(10) 0.34526(9) 0.77003(8) 0.0279(2) Uani 1 1 d . . .
C1 C 1.09912(9) 0.42077(8) 0.69844(7) 0.0288(2) Uani 1 1 d . . .
C2 C 1.17202(10) 0.47938(9) 0.66464(7) 0.0325(2) Uani 1 1 d . . .
C3 C 1.14885(12) 0.54779(9) 0.60837(8) 0.0393(3) Uani 1 1 d . . .
C4 C 1.04943(13) 0.56051(9) 0.58382(8) 0.0419(3) Uani 1 1 d . . .
C5 C 0.97365(12) 0.50517(10) 0.61605(9) 0.0401(3) Uani 1 1 d . . .
C6 C 0.99959(10) 0.43774(9) 0.67211(8) 0.0341(2) Uani 1 1 d . . .
C7 C 1.06764(9) 0.24093(8) 0.75630(7) 0.0285(2) Uani 1 1 d . . .
C8 C 1.04309(10) 0.20193(9) 0.68282(8) 0.0334(2) Uani 1 1 d . . .
C9 C 1.01150(11) 0.10899(10) 0.67290(9) 0.0402(3) Uani 1 1 d . . .
C10 C 1.00260(11) 0.05141(9) 0.73780(10) 0.0436(3) Uani 1 1 d . . .
C11 C 1.02650(11) 0.08591(9) 0.81217(9) 0.0406(3) Uani 1 1 d . . .
C12 C 1.05808(10) 0.17855(9) 0.81941(8) 0.0326(2) Uani 1 1 d . . .
C13 C 1.23900(9) 0.32418(8) 0.79268(7) 0.0300(2) Uani 1 1 d . . .
C14 C 1.30110(10) 0.28237(9) 0.73577(8) 0.0328(2) Uani 1 1 d . . .
C15 C 1.40185(10) 0.25722(10) 0.74852(9) 0.0396(3) Uani 1 1 d . . .
C16 C 1.44564(11) 0.27276(11) 0.82200(10) 0.0450(3) Uani 1 1 d . . .
C17 C 1.38818(12) 0.31243(11) 0.88081(10) 0.0450(3) Uani 1 1 d . . .
C18 C 1.28683(11) 0.33638(10) 0.86581(8) 0.0370(3) Uani 1 1 d . . .
F1 F 1.27085(6) 0.47450(6) 0.68695(5) 0.04322(19) Uani 1 1 d . . .
F2 F 1.22335(8) 0.60262(7) 0.57874(6) 0.0556(2) Uani 1 1 d . . .
F3 F 1.02608(9) 0.62582(7) 0.52904(6) 0.0584(3) Uani 1 1 d . . .
F4 F 0.87612(8) 0.51584(7) 0.59229(7) 0.0587(3) Uani 1 1 d . . .
F5 F 0.92149(6) 0.38653(6) 0.70199(6) 0.0449(2) Uani 1 1 d . . .
F6 F 1.04972(7) 0.25314(6) 0.61570(5) 0.0441(2) Uani 1 1 d . . .
F7 F 0.99004(8) 0.07545(7) 0.60015(6) 0.0571(3) Uani 1 1 d . . .
F8 F 0.97090(9) -0.03821(6) 0.72901(8) 0.0642(3) Uani 1 1 d . . .
F9 F 1.02073(9) 0.02964(6) 0.87601(6) 0.0581(3) Uani 1 1 d . . .
F10 F 1.08374(7) 0.20682(6) 0.89399(5) 0.04109(19) Uani 1 1 d . A .
F11 F 1.26238(6) 0.26618(6) 0.66267(5) 0.04040(18) Uani 1 1 d . . .
F12 F 1.45773(7) 0.21897(8) 0.68963(6) 0.0559(3) Uani 1 1 d . . .
F13 F 1.54414(7) 0.24971(8) 0.83498(8) 0.0657(3) Uani 1 1 d . . .
F14 F 1.42910(9) 0.32817(8) 0.95298(7) 0.0661(3) Uani 1 1 d . . .
F15 F 1.23487(8) 0.37220(7) 0.92829(5) 0.0501(2) Uani 1 1 d . A .
K1 K 1.00669(3) 0.32602(2) 1.013413(19) 0.04175(8) Uani 1 1 d . . .
C19 C 0.8503(2) 0.11615(14) 1.00541(14) 0.0786(7) Uani 1 1 d . A .
H19A H 0.9146 0.1131 0.9758 0.118 Uiso 1 1 calc R . .
H19B H 0.8195 0.0531 1.0079 0.118 Uiso 1 1 calc R . .
H19C H 0.8641 0.1389 1.0594 0.118 Uiso 1 1 calc R . .
O5A O 1.1694(4) 0.3028(4) 1.1048(4) 0.0430(7) Uani 0.832(10) 1 d P A 1
C23A C 1.2088(6) 0.4102(5) 1.2138(4) 0.120(3) Uani 0.832(10) 1 d P A 1
H23A H 1.2366 0.4730 1.2253 0.180 Uiso 0.832(10) 1 calc PR A 1
H23B H 1.2458 0.3629 1.2453 0.180 Uiso 0.832(10) 1 calc PR A 1
H23C H 1.1359 0.4086 1.2274 0.180 Uiso 0.832(10) 1 calc PR A 1
C24A C 1.2213(2) 0.38858(19) 1.1260(2) 0.0620(9) Uani 0.832(10) 1 d P A 1
H24A H 1.1931 0.4414 1.0942 0.074 Uiso 0.832(10) 1 calc PR A 1
H24B H 1.2951 0.3826 1.1137 0.074 Uiso 0.832(10) 1 calc PR A 1
O5B O 1.171(3) 0.310(2) 1.1221(18) 0.061(7) Uani 0.168(10) 1 d P A 2
C23B C 1.2265(14) 0.4252(17) 1.2056(15) 0.058(5) Uani 0.168(10) 1 d P A 2
H23D H 1.2960 0.4514 1.2047 0.086 Uiso 0.168(10) 1 calc PR A 2
H23E H 1.2025 0.4221 1.2606 0.086 Uiso 0.168(10) 1 calc PR A 2
H23F H 1.1805 0.4657 1.1744 0.086 Uiso 0.168(10) 1 calc PR A 2
C24B C 1.2270(16) 0.350(3) 1.1783(18) 0.136(13) Uani 0.168(10) 1 d P A 2
H24C H 1.2189 0.3073 1.2247 0.163 Uiso 0.168(10) 1 calc PR A 2
H24D H 1.2986 0.3407 1.1606 0.163 Uiso 0.168(10) 1 calc PR A 2
C25 C 1.22394(19) 0.21993(18) 1.1224(2) 0.0896(8) Uani 1 1 d . . .
H25A H 1.2429 0.2193 1.1795 0.107 Uiso 1 1 calc R A 1
H25B H 1.2879 0.2183 1.0911 0.107 Uiso 1 1 calc R A 1
C26 C 1.1621(2) 0.13686(15) 1.10390(17) 0.0793(7) Uani 1 1 d . A .
H26A H 1.0961 0.1414 1.1311 0.119 Uiso 1 1 calc R . .
H26B H 1.1982 0.0800 1.1218 0.119 Uiso 1 1 calc R . .
H26C H 1.1504 0.1334 1.0464 0.119 Uiso 1 1 calc R . .
C20 C 0.7791(2) 0.18122(17) 0.96507(15) 0.0817(7) Uani 1 1 d . . .
H20A H 0.7579 0.1550 0.9129 0.098 Uiso 1 1 calc R A 1
H20B H 0.7171 0.1907 0.9977 0.098 Uiso 1 1 calc R A 1
O4A O 0.8321(2) 0.26982(17) 0.9543(2) 0.0620(8) Uani 0.800(10) 1 d P A 1
C21A C 0.7717(3) 0.3404(3) 0.9156(3) 0.0836(15) Uani 0.800(10) 1 d P A 1
H21A H 0.7344 0.3115 0.8703 0.100 Uiso 0.800(10) 1 calc PR A 1
H21B H 0.8175 0.3898 0.8942 0.100 Uiso 0.800(10) 1 calc PR A 1
C22A C 0.6964(4) 0.3849(4) 0.9703(4) 0.105(2) Uani 0.800(10) 1 d P A 1
H22A H 0.6486 0.3368 0.9895 0.157 Uiso 0.800(10) 1 calc PR A 1
H22B H 0.6583 0.4341 0.9418 0.157 Uiso 0.800(10) 1 calc PR A 1
H22C H 0.7329 0.4130 1.0156 0.157 Uiso 0.800(10) 1 calc PR A 1
C21B C 0.7206(16) 0.3320(18) 0.9581(10) 0.099(7) Uani 0.200(10) 1 d P A 2
H21C H 0.7184 0.3362 0.8993 0.118 Uiso 0.200(10) 1 calc PR A 2
H21D H 0.6539 0.3070 0.9764 0.118 Uiso 0.200(10) 1 calc PR A 2
O4B O 0.8056(11) 0.2665(10) 0.9836(7) 0.076(3) Uani 0.200(10) 1 d P A 2
C22B C 0.7368(14) 0.4199(17) 0.9898(15) 0.131(10) Uani 0.200(10) 1 d P A 2
H22D H 0.7383 0.4156 1.0479 0.196 Uiso 0.200(10) 1 calc PR A 2
H22E H 0.6812 0.4623 0.9731 0.196 Uiso 0.200(10) 1 calc PR A 2
H22F H 0.8024 0.4448 0.9710 0.196 Uiso 0.200(10) 1 calc PR 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
N1 0.0631(8) 0.0283(5) 0.0316(5) -0.0034(4) 0.0029(5) 0.0063(5)
O1 0.0432(5) 0.0264(4) 0.0329(4) -0.0040(3) 0.0070(4) 0.0007(3)
O2 0.0713(7) 0.0317(5) 0.0404(5) -0.0034(4) 0.0008(5) -0.0110(5)
O3 0.0980(10) 0.0434(6) 0.0444(6) -0.0097(5) 0.0242(6) 0.0119(6)
B1 0.0304(6) 0.0260(6) 0.0274(5) -0.0018(4) 0.0019(5) -0.0007(5)
C1 0.0325(5) 0.0257(5) 0.0282(5) -0.0025(4) -0.0003(4) -0.0004(4)
C2 0.0361(6) 0.0287(5) 0.0329(5) -0.0013(4) 0.0011(5) -0.0017(5)
C3 0.0551(8) 0.0274(6) 0.0354(6) 0.0004(5) 0.0056(6) -0.0026(5)
C4 0.0675(9) 0.0258(6) 0.0323(6) -0.0006(5) -0.0084(6) 0.0054(6)
C5 0.0456(7) 0.0333(6) 0.0411(7) -0.0050(5) -0.0133(6) 0.0092(5)
C6 0.0343(6) 0.0291(6) 0.0389(6) -0.0028(5) -0.0031(5) 0.0002(5)
C7 0.0259(5) 0.0253(5) 0.0344(5) -0.0014(4) 0.0013(4) 0.0015(4)
C8 0.0330(6) 0.0301(6) 0.0371(6) -0.0038(5) -0.0023(5) 0.0009(5)
C9 0.0371(6) 0.0322(6) 0.0512(8) -0.0131(5) -0.0024(6) 0.0014(5)
C10 0.0400(7) 0.0234(6) 0.0675(9) -0.0093(6) 0.0104(6) -0.0020(5)
C11 0.0415(7) 0.0271(6) 0.0534(8) 0.0021(5) 0.0164(6) 0.0030(5)
C12 0.0329(6) 0.0280(5) 0.0369(6) -0.0013(4) 0.0074(5) 0.0028(4)
C13 0.0313(5) 0.0274(5) 0.0312(5) 0.0013(4) -0.0025(4) -0.0034(4)
C14 0.0311(6) 0.0315(6) 0.0358(6) 0.0027(5) 0.0000(5) -0.0023(5)
C15 0.0312(6) 0.0343(6) 0.0533(8) 0.0068(6) 0.0040(5) -0.0008(5)
C16 0.0312(6) 0.0384(7) 0.0654(9) 0.0140(7) -0.0107(6) -0.0041(5)
C17 0.0484(8) 0.0373(7) 0.0490(8) 0.0065(6) -0.0209(6) -0.0076(6)
C18 0.0451(7) 0.0316(6) 0.0343(6) 0.0000(5) -0.0066(5) -0.0027(5)
F1 0.0332(4) 0.0409(4) 0.0555(5) 0.0078(4) 0.0019(3) -0.0075(3)
F2 0.0703(6) 0.0386(5) 0.0581(5) 0.0129(4) 0.0143(5) -0.0090(4)
F3 0.0962(8) 0.0353(5) 0.0435(5) 0.0081(4) -0.0158(5) 0.0089(5)
F4 0.0532(6) 0.0516(5) 0.0708(6) 0.0012(5) -0.0267(5) 0.0122(4)
F5 0.0304(4) 0.0408(4) 0.0634(5) 0.0036(4) -0.0033(4) -0.0015(3)
F6 0.0616(5) 0.0374(4) 0.0333(4) -0.0035(3) -0.0091(4) -0.0007(4)
F7 0.0675(6) 0.0441(5) 0.0595(6) -0.0215(4) -0.0120(5) -0.0041(4)
F8 0.0746(7) 0.0263(4) 0.0918(8) -0.0139(5) 0.0184(6) -0.0102(4)
F9 0.0795(7) 0.0312(4) 0.0640(6) 0.0098(4) 0.0277(5) 0.0022(4)
F10 0.0551(5) 0.0345(4) 0.0337(4) 0.0029(3) 0.0061(3) 0.0037(3)
F11 0.0395(4) 0.0492(5) 0.0326(4) -0.0047(3) 0.0025(3) 0.0026(3)
F12 0.0361(4) 0.0605(6) 0.0712(6) 0.0038(5) 0.0156(4) 0.0083(4)
F13 0.0328(4) 0.0662(7) 0.0980(8) 0.0161(6) -0.0182(5) -0.0001(4)
F14 0.0730(7) 0.0639(7) 0.0610(6) 0.0005(5) -0.0399(6) -0.0033(5)
F15 0.0663(6) 0.0524(5) 0.0314(4) -0.0076(4) -0.0097(4) 0.0057(4)
K1 0.04726(17) 0.03587(15) 0.04203(15) -0.00515(11) -0.00678(12) 0.00244(12)
C19 0.1151(19) 0.0436(10) 0.0778(13) -0.0098(9) 0.0461(13) -0.0127(11)
O5A 0.0366(12) 0.0437(11) 0.049(2) 0.0031(12) -0.0023(13) -0.0020(8)
C23A 0.163(6) 0.099(3) 0.099(4) -0.044(3) 0.023(3) -0.058(4)
C24A 0.0499(12) 0.0609(15) 0.075(2) 0.0018(12) -0.0063(11) -0.0162(10)
O5B 0.051(7) 0.080(11) 0.052(12) -0.002(7) -0.021(7) 0.005(6)
C23B 0.043(6) 0.069(11) 0.060(8) 0.013(8) 0.007(6) 0.012(7)
C24B 0.072(11) 0.23(4) 0.102(19) -0.06(2) -0.028(11) 0.040(16)
C25 0.0661(13) 0.0687(14) 0.134(2) 0.0103(14) -0.0214(14) 0.0225(11)
C26 0.0922(16) 0.0498(11) 0.0962(17) 0.0009(11) 0.0197(13) 0.0150(11)
C20 0.1013(18) 0.0688(14) 0.0750(14) 0.0007(11) -0.0062(13) -0.0451(13)
O4A 0.0563(13) 0.0566(11) 0.0729(18) 0.0195(11) -0.0183(11) -0.0244(9)
C21A 0.0543(16) 0.089(2) 0.107(3) 0.047(2) -0.0258(18) -0.0222(15)
C22A 0.059(2) 0.086(3) 0.170(5) 0.044(3) -0.023(3) -0.009(2)
C21B 0.078(11) 0.150(19) 0.067(9) 0.037(11) -0.035(8) -0.014(12)
O4B 0.084(7) 0.100(7) 0.043(5) 0.017(4) -0.006(4) -0.047(5)
C22B 0.072(10) 0.122(16) 0.20(2) 0.025(15) -0.083(12) -0.026(10)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
N1 O2 1.2060(17) . ?
N1 O3 1.2285(16) . ?
N1 O1 1.3396(14) . ?
N1 K1 3.3585(12) . ?
O1 B1 1.5574(15) . ?
O1 K1 3.0679(9) . ?
O3 K1 2.7524(12) 3_767 ?
O3 K1 2.8889(13) . ?
B1 C1 1.6309(18) . ?
B1 C13 1.6317(18) . ?
B1 C7 1.6401(18) . ?
C1 C2 1.3873(17) . ?
C1 C6 1.3899(18) . ?
C2 F1 1.3421(15) . ?
C2 C3 1.3866(19) . ?
C3 F2 1.3426(16) . ?
C3 C4 1.370(2) . ?
C4 F3 1.3395(16) . ?
C4 C5 1.376(2) . ?
C5 F4 1.3395(17) . ?
C5 C6 1.3827(19) . ?
C6 F5 1.3505(15) . ?
C7 C12 1.3876(17) . ?
C7 C8 1.3895(17) . ?
C8 F6 1.3455(16) . ?
C8 C9 1.3891(19) . ?
C9 F7 1.3408(17) . ?
C9 C10 1.368(2) . ?
C10 F8 1.3429(16) . ?
C10 C11 1.377(2) . ?
C11 F9 1.3401(17) . ?
C11 C12 1.3804(19) . ?
C12 F10 1.3569(16) . ?
C13 C18 1.3866(17) . ?
C13 C14 1.3909(17) . ?
C14 F11 1.3462(15) . ?
C14 C15 1.3771(18) . ?
C15 F12 1.3479(17) . ?
C15 C16 1.376(2) . ?
C16 F13 1.3422(17) . ?
C16 C17 1.366(2) . ?
C17 F14 1.3417(17) . ?
C17 C18 1.386(2) . ?
C18 F15 1.3534(16) . ?
F10 K1 2.8154(9) . ?
F12 K1 3.1035(11) 4_665 ?
F15 K1 3.3760(11) . ?
K1 O4A 2.604(2) . ?
K1 O5A 2.634(6) . ?
K1 O3 2.7524(12) 3_767 ?
K1 O4B 2.797(13) . ?
K1 O5B 2.82(3) . ?
K1 F12 3.1035(11) 4_566 ?
K1 C21A 3.475(3) . ?
C19 C20 1.471(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O5A C25 1.402(6) . ?
O5A C24A 1.435(6) . ?
C23A C24A 1.518(8) . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
O5B C24B 1.32(4) . ?
O5B C25 1.44(4) . ?
C23B C24B 1.16(4) . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C25 C26 1.459(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C20 O4B 1.294(13) . ?
C20 O4A 1.444(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O4A C21A 1.427(4) . ?
C21A C22A 1.489(8) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C21B C22B 1.37(4) . ?
C21B O4B 1.51(3) . ?
C21B H21C 0.9900 . ?
C21B H21D 0.9900 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 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
O2 N1 O3 125.63(13) . . ?
O2 N1 O1 121.09(11) . . ?
O3 N1 O1 113.27(12) . . ?
O2 N1 K1 148.75(10) . . ?
O3 N1 K1 57.42(8) . . ?
O1 N1 K1 65.99(6) . . ?
N1 O1 B1 117.90(9) . . ?
N1 O1 K1 90.51(6) . . ?
B1 O1 K1 139.35(7) . . ?
N1 O3 K1 130.85(10) . 3_767 ?
N1 O3 K1 101.58(9) . . ?
K1 O3 K1 122.74(4) 3_767 . ?
O1 B1 C1 105.68(9) . . ?
O1 B1 C13 111.63(10) . . ?
C1 B1 C13 116.24(10) . . ?
O1 B1 C7 102.49(9) . . ?
C1 B1 C7 115.00(10) . . ?
C13 B1 C7 105.07(9) . . ?
C2 C1 C6 114.02(11) . . ?
C2 C1 B1 125.98(11) . . ?
C6 C1 B1 119.66(11) . . ?
F1 C2 C3 115.56(11) . . ?
F1 C2 C1 120.95(11) . . ?
C3 C2 C1 123.46(13) . . ?
F2 C3 C4 119.87(12) . . ?
F2 C3 C2 120.18(14) . . ?
C4 C3 C2 119.94(13) . . ?
F3 C4 C3 120.57(14) . . ?
F3 C4 C5 120.27(14) . . ?
C3 C4 C5 119.17(12) . . ?
F4 C5 C4 120.10(13) . . ?
F4 C5 C6 120.60(14) . . ?
C4 C5 C6 119.29(13) . . ?
F5 C6 C5 116.31(12) . . ?
F5 C6 C1 119.59(11) . . ?
C5 C6 C1 124.10(13) . . ?
C12 C7 C8 113.99(11) . . ?
C12 C7 B1 120.32(11) . . ?
C8 C7 B1 125.13(11) . . ?
F6 C8 C9 115.51(12) . . ?
F6 C8 C7 121.13(11) . . ?
C9 C8 C7 123.36(13) . . ?
F7 C9 C10 119.93(13) . . ?
F7 C9 C8 120.36(14) . . ?
C10 C9 C8 119.71(13) . . ?
F8 C10 C9 120.22(14) . . ?
F8 C10 C11 120.20(14) . . ?
C9 C10 C11 119.58(12) . . ?
F9 C11 C10 120.24(13) . . ?
F9 C11 C12 120.86(14) . . ?
C10 C11 C12 118.88(13) . . ?
F10 C12 C11 115.70(12) . . ?
F10 C12 C7 119.80(11) . . ?
C11 C12 C7 124.47(13) . . ?
C18 C13 C14 113.79(12) . . ?
C18 C13 B1 127.47(11) . . ?
C14 C13 B1 118.53(10) . . ?
F11 C14 C15 116.74(12) . . ?
F11 C14 C13 119.02(11) . . ?
C15 C14 C13 124.23(13) . . ?
F12 C15 C16 120.10(13) . . ?
F12 C15 C14 120.66(13) . . ?
C16 C15 C14 119.24(14) . . ?
F13 C16 C17 120.76(15) . . ?
F13 C16 C15 119.89(15) . . ?
C17 C16 C15 119.35(13) . . ?
F14 C17 C16 120.46(14) . . ?
F14 C17 C18 119.81(15) . . ?
C16 C17 C18 119.73(13) . . ?
F15 C18 C17 115.61(12) . . ?
F15 C18 C13 120.76(12) . . ?
C17 C18 C13 123.62(13) . . ?
C12 F10 K1 138.59(7) . . ?
C15 F12 K1 154.26(9) . 4_665 ?
C18 F15 K1 134.80(8) . . ?
O4A K1 O5A 152.17(11) . . ?
O4A K1 O3 107.38(8) . 3_767 ?
O5A K1 O3 90.10(13) . 3_767 ?
O4A K1 O4B 12.2(2) . . ?
O5A K1 O4B 144.9(3) . . ?
O3 K1 O4B 101.8(3) 3_767 . ?
O4A K1 F10 81.93(9) . . ?
O5A K1 F10 92.95(13) . . ?
O3 K1 F10 151.57(3) 3_767 . ?
O4B K1 F10 91.7(3) . . ?
O4A K1 O5B 152.0(7) . . ?
O5A K1 O5B 5.1(8) . . ?
O3 K1 O5B 86.1(7) 3_767 . ?
O4B K1 O5B 143.2(7) . . ?
F10 K1 O5B 98.0(7) . . ?
O4A K1 O3 97.21(7) . . ?
O5A K1 O3 110.53(10) . . ?
O3 K1 O3 57.26(4) 3_767 . ?
O4B K1 O3 103.6(3) . . ?
F10 K1 O3 95.46(3) . . ?
O5B K1 O3 110.6(6) . . ?
O4A K1 O1 85.60(9) . . ?
O5A K1 O1 113.37(11) . . ?
O3 K1 O1 99.35(3) 3_767 . ?
O4B K1 O1 97.3(2) . . ?
F10 K1 O1 53.75(2) . . ?
O5B K1 O1 117.1(7) . . ?
O3 K1 O1 42.09(3) . . ?
O4A K1 F12 96.73(10) . 4_566 ?
O5A K1 F12 65.58(12) . 4_566 ?
O3 K1 F12 77.12(3) 3_767 4_566 ?
O4B K1 F12 84.9(2) . 4_566 ?
F10 K1 F12 129.46(3) . 4_566 ?
O5B K1 F12 61.6(7) . 4_566 ?
O3 K1 F12 134.38(3) . 4_566 ?
O1 K1 F12 176.21(3) . 4_566 ?
O4A K1 N1 98.96(8) . . ?
O5A K1 N1 106.14(10) . . ?
O3 K1 N1 76.94(3) 3_767 . ?
O4B K1 N1 108.7(2) . . ?
F10 K1 N1 75.06(3) . . ?
O5B K1 N1 108.2(6) . . ?
O3 K1 N1 21.00(3) . . ?
O1 K1 N1 23.51(3) . . ?
F12 K1 N1 152.71(3) 4_566 . ?
O4A K1 F15 131.96(10) . . ?
O5A K1 F15 64.06(11) . . ?
O3 K1 F15 97.09(4) 3_767 . ?
O4B K1 F15 144.2(3) . . ?
F10 K1 F15 59.55(2) . . ?
O5B K1 F15 67.7(7) . . ?
O3 K1 F15 62.49(3) . . ?
O1 K1 F15 49.37(2) . . ?
F12 K1 F15 129.26(2) 4_566 . ?
N1 K1 F15 46.95(3) . . ?
O4A K1 C21A 21.65(8) . . ?
O5A K1 C21A 171.38(13) . . ?
O3 K1 C21A 90.19(8) 3_767 . ?
O4B K1 C21A 27.1(2) . . ?
F10 K1 C21A 90.88(9) . . ?
O5B K1 C21A 167.7(7) . . ?
O3 K1 C21A 76.74(6) . . ?
O1 K1 C21A 75.07(8) . . ?
F12 K1 C21A 106.12(8) 4_566 . ?
N1 K1 C21A 82.31(7) . . ?
F15 K1 C21A 124.43(8) . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 O5A C24A 114.8(4) . . ?
C25 O5A K1 129.3(3) . . ?
C24A O5A K1 114.6(3) . . ?
O5A C24A C23A 111.0(4) . . ?
O5A C24A K1 43.4(2) . . ?
C23A C24A K1 119.3(3) . . ?
O5A C24A H24A 109.4 . . ?
C23A C24A H24A 109.4 . . ?
K1 C24A H24A 66.6 . . ?
O5A C24A H24B 109.4 . . ?
C23A C24A H24B 109.4 . . ?
K1 C24A H24B 130.0 . . ?
H24A C24A H24B 108.0 . . ?
C24B O5B C25 97(3) . . ?
C24B O5B K1 148(3) . . ?
C25 O5B K1 115.7(16) . . ?
C24B C23B H23D 109.5 . . ?
C24B C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C24B C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23B C24B O5B 132(3) . . ?
C23B C24B H24C 104.1 . . ?
O5B C24B H24C 104.1 . . ?
C23B C24B H24D 104.1 . . ?
O5B C24B H24D 104.1 . . ?
H24C C24B H24D 105.5 . . ?
O5A C25 O5B 12.3(14) . . ?
O5A C25 C26 110.5(3) . . ?
O5B C25 C26 116.6(13) . . ?
O5A C25 H25A 109.5 . . ?
O5B C25 H25A 97.3 . . ?
C26 C25 H25A 109.5 . . ?
O5A C25 H25B 109.5 . . ?
O5B C25 H25B 114.8 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O4B C20 O4A 24.8(5) . . ?
O4B C20 C19 107.9(6) . . ?
O4A C20 C19 107.6(2) . . ?
O4B C20 H20A 129.5 . . ?
O4A C20 H20A 110.2 . . ?
C19 C20 H20A 110.2 . . ?
O4B C20 H20B 87.6 . . ?
O4A C20 H20B 110.2 . . ?
C19 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
C21A O4A C20 113.8(2) . . ?
C21A O4A K1 116.02(17) . . ?
C20 O4A K1 129.44(18) . . ?
O4A C21A C22A 112.3(3) . . ?
O4A C21A K1 42.33(12) . . ?
C22A C21A K1 108.4(3) . . ?
O4A C21A H21A 109.1 . . ?
C22A C21A H21A 109.1 . . ?
K1 C21A H21A 140.1 . . ?
O4A C21A H21B 109.1 . . ?
C22A C21A H21B 109.1 . . ?
K1 C21A H21B 71.4 . . ?
H21A C21A H21B 107.9 . . ?
C22B C21B O4B 109.7(13) . . ?
C22B C21B H21C 109.7 . . ?
O4B C21B H21C 109.7 . . ?
C22B C21B H21D 109.7 . . ?
O4B C21B H21D 109.7 . . ?
H21C C21B H21D 108.2 . . ?
C20 O4B C21B 108.1(11) . . ?
C20 O4B K1 125.0(9) . . ?
C21B O4B K1 123.6(10) . . ?
C21B C22B H22D 109.5 . . ?
C21B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C21B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
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
O2 N1 O1 B1 -4.17(19) . . . . ?
O3 N1 O1 B1 176.75(12) . . . . ?
K1 N1 O1 B1 -149.68(10) . . . . ?
O2 N1 O1 K1 145.51(13) . . . . ?
O3 N1 O1 K1 -33.58(12) . . . . ?
O2 N1 O3 K1 12.9(2) . . . 3_767 ?
O1 N1 O3 K1 -168.09(10) . . . 3_767 ?
K1 N1 O3 K1 155.08(17) . . . 3_767 ?
O2 N1 O3 K1 -142.21(13) . . . . ?
O1 N1 O3 K1 36.83(13) . . . . ?
N1 O1 B1 C1 -55.18(13) . . . . ?
K1 O1 B1 C1 175.62(7) . . . . ?
N1 O1 B1 C13 72.07(13) . . . . ?
K1 O1 B1 C13 -57.13(14) . . . . ?
N1 O1 B1 C7 -175.96(10) . . . . ?
K1 O1 B1 C7 54.85(14) . . . . ?
O1 B1 C1 C2 113.08(12) . . . . ?
C13 B1 C1 C2 -11.34(17) . . . . ?
C7 B1 C1 C2 -134.67(12) . . . . ?
O1 B1 C1 C6 -59.85(14) . . . . ?
C13 B1 C1 C6 175.73(11) . . . . ?
C7 B1 C1 C6 52.40(14) . . . . ?
C6 C1 C2 F1 176.83(11) . . . . ?
B1 C1 C2 F1 3.55(19) . . . . ?
C6 C1 C2 C3 -1.22(18) . . . . ?
B1 C1 C2 C3 -174.49(12) . . . . ?
F1 C2 C3 F2 1.25(18) . . . . ?
C1 C2 C3 F2 179.39(12) . . . . ?
F1 C2 C3 C4 -177.73(12) . . . . ?
C1 C2 C3 C4 0.4(2) . . . . ?
F2 C3 C4 F3 1.6(2) . . . . ?
C2 C3 C4 F3 -179.47(12) . . . . ?
F2 C3 C4 C5 -178.56(12) . . . . ?
C2 C3 C4 C5 0.4(2) . . . . ?
F3 C4 C5 F4 0.5(2) . . . . ?
C3 C4 C5 F4 -179.34(13) . . . . ?
F3 C4 C5 C6 179.55(12) . . . . ?
C3 C4 C5 C6 -0.3(2) . . . . ?
F4 C5 C6 F5 -1.68(19) . . . . ?
C4 C5 C6 F5 179.31(12) . . . . ?
F4 C5 C6 C1 178.42(12) . . . . ?
C4 C5 C6 C1 -0.6(2) . . . . ?
C2 C1 C6 F5 -178.58(11) . . . . ?
B1 C1 C6 F5 -4.84(17) . . . . ?
C2 C1 C6 C5 1.32(18) . . . . ?
B1 C1 C6 C5 175.06(12) . . . . ?
O1 B1 C7 C12 -50.53(14) . . . . ?
C1 B1 C7 C12 -164.65(10) . . . . ?
C13 B1 C7 C12 66.25(13) . . . . ?
O1 B1 C7 C8 138.56(11) . . . . ?
C1 B1 C7 C8 24.45(16) . . . . ?
C13 B1 C7 C8 -104.65(13) . . . . ?
C12 C7 C8 F6 -179.20(11) . . . . ?
B1 C7 C8 F6 -7.78(19) . . . . ?
C12 C7 C8 C9 0.16(18) . . . . ?
B1 C7 C8 C9 171.57(12) . . . . ?
F6 C8 C9 F7 0.13(19) . . . . ?
C7 C8 C9 F7 -179.26(12) . . . . ?
F6 C8 C9 C10 179.93(12) . . . . ?
C7 C8 C9 C10 0.5(2) . . . . ?
F7 C9 C10 F8 -1.0(2) . . . . ?
C8 C9 C10 F8 179.17(13) . . . . ?
F7 C9 C10 C11 178.87(13) . . . . ?
C8 C9 C10 C11 -0.9(2) . . . . ?
F8 C10 C11 F9 1.7(2) . . . . ?
C9 C10 C11 F9 -178.25(13) . . . . ?
F8 C10 C11 C12 -179.48(13) . . . . ?
C9 C10 C11 C12 0.6(2) . . . . ?
F9 C11 C12 F10 1.04(18) . . . . ?
C10 C11 C12 F10 -177.81(12) . . . . ?
F9 C11 C12 C7 178.98(12) . . . . ?
C10 C11 C12 C7 0.1(2) . . . . ?
C8 C7 C12 F10 177.36(11) . . . . ?
B1 C7 C12 F10 5.50(17) . . . . ?
C8 C7 C12 C11 -0.49(18) . . . . ?
B1 C7 C12 C11 -172.36(12) . . . . ?
O1 B1 C13 C18 0.41(17) . . . . ?
C1 B1 C13 C18 121.71(13) . . . . ?
C7 B1 C13 C18 -109.93(13) . . . . ?
O1 B1 C13 C14 174.95(10) . . . . ?
C1 B1 C13 C14 -63.75(14) . . . . ?
C7 B1 C13 C14 64.60(13) . . . . ?
C18 C13 C14 F11 179.35(11) . . . . ?
B1 C13 C14 F11 4.09(17) . . . . ?
C18 C13 C14 C15 -1.80(19) . . . . ?
B1 C13 C14 C15 -177.06(12) . . . . ?
F11 C14 C15 F12 0.45(19) . . . . ?
C13 C14 C15 F12 -178.43(12) . . . . ?
F11 C14 C15 C16 179.57(12) . . . . ?
C13 C14 C15 C16 0.7(2) . . . . ?
F12 C15 C16 F13 0.0(2) . . . . ?
C14 C15 C16 F13 -179.15(13) . . . . ?
F12 C15 C16 C17 179.38(13) . . . . ?
C14 C15 C16 C17 0.3(2) . . . . ?
F13 C16 C17 F14 -0.7(2) . . . . ?
C15 C16 C17 F14 179.92(13) . . . . ?
F13 C16 C17 C18 179.45(13) . . . . ?
C15 C16 C17 C18 0.0(2) . . . . ?
F14 C17 C18 F15 -2.1(2) . . . . ?
C16 C17 C18 F15 177.78(13) . . . . ?
F14 C17 C18 C13 178.79(13) . . . . ?
C16 C17 C18 C13 -1.3(2) . . . . ?
C14 C13 C18 F15 -176.97(12) . . . . ?
B1 C13 C18 F15 -2.2(2) . . . . ?
C14 C13 C18 C17 2.11(19) . . . . ?
B1 C13 C18 C17 176.86(13) . . . . ?
C11 C12 F10 K1 -109.60(12) . . . . ?
C7 C12 F10 K1 72.36(15) . . . . ?
C16 C15 F12 K1 -159.80(14) . . . 4_665 ?
C14 C15 F12 K1 19.3(3) . . . 4_665 ?
C17 C18 F15 K1 -130.22(11) . . . . ?
C13 C18 F15 K1 48.93(17) . . . . ?
C12 F10 K1 O4A 33.23(13) . . . . ?
C12 F10 K1 O5A -174.26(14) . . . . ?
C12 F10 K1 O3 -78.59(14) . . . 3_767 ?
C12 F10 K1 O4B 40.5(3) . . . . ?
C12 F10 K1 O5B -175.1(7) . . . . ?
C12 F10 K1 O3 -63.31(11) . . . . ?
C12 F10 K1 O1 -57.22(11) . . . . ?
C12 F10 K1 F12 125.32(11) . . . 4_566 ?
C12 F10 K1 N1 -68.34(11) . . . . ?
C12 F10 K1 F15 -116.84(11) . . . . ?
C12 F10 K1 C21A 13.46(12) . . . . ?
N1 O3 K1 O4A -96.22(14) . . . . ?
K1 O3 K1 O4A 106.05(11) 3_767 . . . ?
N1 O3 K1 O5A 81.53(18) . . . . ?
K1 O3 K1 O5A -76.20(16) 3_767 . . . ?
N1 O3 K1 O3 157.73(16) . . . 3_767 ?
K1 O3 K1 O3 0.0 3_767 . . 3_767 ?
N1 O3 K1 O4B -106.8(3) . . . . ?
K1 O3 K1 O4B 95.5(3) 3_767 . . . ?
N1 O3 K1 F10 -13.69(11) . . . . ?
K1 O3 K1 F10 -171.42(6) 3_767 . . . ?
N1 O3 K1 O5B 87.0(8) . . . . ?
K1 O3 K1 O5B -70.7(8) 3_767 . . . ?
N1 O3 K1 O1 -21.02(9) . . . . ?
K1 O3 K1 O1 -178.75(10) 3_767 . . . ?
N1 O3 K1 F12 156.98(9) . . . 4_566 ?
K1 O3 K1 F12 -0.75(10) 3_767 . . 4_566 ?
K1 O3 K1 N1 -157.73(16) 3_767 . . . ?
N1 O3 K1 F15 37.72(10) . . . . ?
K1 O3 K1 F15 -120.01(7) 3_767 . . . ?
N1 O3 K1 C21A -103.32(14) . . . . ?
K1 O3 K1 C21A 98.95(11) 3_767 . . . ?
N1 O1 K1 O4A 124.65(10) . . . . ?
B1 O1 K1 O4A -98.58(13) . . . . ?
N1 O1 K1 O5A -76.45(15) . . . . ?
B1 O1 K1 O5A 60.32(17) . . . . ?
N1 O1 K1 O3 17.74(8) . . . 3_767 ?
B1 O1 K1 O3 154.51(11) . . . 3_767 ?
N1 O1 K1 O4B 121.1(3) . . . . ?
B1 O1 K1 O4B -102.2(3) . . . . ?
N1 O1 K1 F10 -152.13(8) . . . . ?
B1 O1 K1 F10 -15.37(10) . . . . ?
N1 O1 K1 O5B -72.6(8) . . . . ?
B1 O1 K1 O5B 64.2(8) . . . . ?
N1 O1 K1 O3 18.80(8) . . . . ?
B1 O1 K1 O3 155.57(13) . . . . ?
N1 O1 K1 F12 -3.3(5) . . . 4_566 ?
B1 O1 K1 F12 133.5(4) . . . 4_566 ?
B1 O1 K1 N1 136.77(15) . . . . ?
N1 O1 K1 F15 -73.61(8) . . . . ?
B1 O1 K1 F15 63.16(11) . . . . ?
N1 O1 K1 C21A 105.43(10) . . . . ?
B1 O1 K1 C21A -117.81(13) . . . . ?
O2 N1 K1 O4A -166.97(18) . . . . ?
O3 N1 K1 O4A 86.79(13) . . . . ?
O1 N1 K1 O4A -56.13(11) . . . . ?
O2 N1 K1 O5A 0.9(2) . . . . ?
O3 N1 K1 O5A -105.36(17) . . . . ?
O1 N1 K1 O5A 111.72(15) . . . . ?
O2 N1 K1 O3 87.14(17) . . . 3_767 ?
O3 N1 K1 O3 -19.10(13) . . . 3_767 ?
O1 N1 K1 O3 -162.02(8) . . . 3_767 ?
O2 N1 K1 O4B -174.6(4) . . . . ?
O3 N1 K1 O4B 79.2(3) . . . . ?
O1 N1 K1 O4B -63.8(3) . . . . ?
O2 N1 K1 F10 -87.87(16) . . . . ?
O3 N1 K1 F10 165.88(11) . . . . ?
O1 N1 K1 F10 22.96(7) . . . . ?
O2 N1 K1 O5B 5.8(8) . . . . ?
O3 N1 K1 O5B -100.4(8) . . . . ?
O1 N1 K1 O5B 116.6(8) . . . . ?
O2 N1 K1 O3 106.2(2) . . . . ?
O1 N1 K1 O3 -142.92(15) . . . . ?
O2 N1 K1 O1 -110.83(19) . . . . ?
O3 N1 K1 O1 142.92(15) . . . . ?
O2 N1 K1 F12 68.69(19) . . . 4_566 ?
O3 N1 K1 F12 -37.55(14) . . . 4_566 ?
O1 N1 K1 F12 179.53(7) . . . 4_566 ?
O2 N1 K1 F15 -25.81(15) . . . . ?
O3 N1 K1 F15 -132.05(12) . . . . ?
O1 N1 K1 F15 85.03(7) . . . . ?
O2 N1 K1 C21A 179.14(18) . . . . ?
O3 N1 K1 C21A 72.90(14) . . . . ?
O1 N1 K1 C21A -70.03(11) . . . . ?
C18 F15 K1 O4A -33.29(14) . . . . ?
C18 F15 K1 O5A 118.97(17) . . . . ?
C18 F15 K1 O3 -154.39(11) . . . 3_767 ?
C18 F15 K1 O4B -32.7(5) . . . . ?
C18 F15 K1 F10 8.34(10) . . . . ?
C18 F15 K1 O5B 122.8(8) . . . . ?
C18 F15 K1 O3 -107.16(11) . . . . ?
C18 F15 K1 O1 -58.13(10) . . . . ?
C18 F15 K1 F12 126.48(11) . . . 4_566 ?
C18 F15 K1 N1 -89.70(11) . . . . ?
C18 F15 K1 C21A -59.26(14) . . . . ?
O4A K1 O5A C25 35.4(7) . . . . ?
O3 K1 O5A C25 165.4(4) 3_767 . . . ?
O4B K1 O5A C25 54.4(8) . . . . ?
F10 K1 O5A C25 -42.8(4) . . . . ?
O5B K1 O5A C25 128(8) . . . . ?
O3 K1 O5A C25 -139.8(4) . . . . ?
O1 K1 O5A C25 -94.3(4) . . . . ?
F12 K1 O5A C25 89.7(4) 4_566 . . . ?
N1 K1 O5A C25 -118.1(4) . . . . ?
F15 K1 O5A C25 -96.7(4) . . . . ?
C21A K1 O5A C25 73.5(12) . . . . ?
O4A K1 O5A C24A -158.8(3) . . . . ?
O3 K1 O5A C24A -28.8(3) 3_767 . . . ?
O4B K1 O5A C24A -139.8(6) . . . . ?
F10 K1 O5A C24A 122.9(3) . . . . ?
O5B K1 O5A C24A -66(8) . . . . ?
O3 K1 O5A C24A 26.0(4) . . . . ?
O1 K1 O5A C24A 71.5(4) . . . . ?
F12 K1 O5A C24A -104.6(4) 4_566 . . . ?
N1 K1 O5A C24A 47.7(4) . . . . ?
F15 K1 O5A C24A 69.1(3) . . . . ?
C21A K1 O5A C24A -120.7(9) . . . . ?
C25 O5A C24A C23A -81.2(5) . . . . ?
K1 O5A C24A C23A 110.8(4) . . . . ?
C25 O5A C24A K1 167.9(6) . . . . ?
O4A K1 C24A O5A 66.8(6) . . . . ?
O3 K1 C24A O5A 149.4(4) 3_767 . . . ?
O4B K1 C24A O5A 74.8(9) . . . . ?
F10 K1 C24A O5A -60.0(3) . . . . ?
O5B K1 C24A O5A 13(2) . . . . ?
O3 K1 C24A O5A -155.8(3) . . . . ?
O1 K1 C24A O5A -115.7(3) . . . . ?
F12 K1 C24A O5A 67.4(3) 4_566 . . . ?
N1 K1 C24A O5A -134.8(3) . . . . ?
F15 K1 C24A O5A -99.1(3) . . . . ?
C21A K1 C24A O5A 156.7(4) . . . . ?
O4A K1 C24A C23A -23.6(6) . . . . ?
O5A K1 C24A C23A -90.4(5) . . . . ?
O3 K1 C24A C23A 59.0(4) 3_767 . . . ?
O4B K1 C24A C23A -15.6(9) . . . . ?
F10 K1 C24A C23A -150.4(4) . . . . ?
O5B K1 C24A C23A -77(2) . . . . ?
O3 K1 C24A C23A 113.9(4) . . . . ?
O1 K1 C24A C23A 153.9(4) . . . . ?
F12 K1 C24A C23A -23.0(4) 4_566 . . . ?
N1 K1 C24A C23A 134.9(4) . . . . ?
F15 K1 C24A C23A 170.6(4) . . . . ?
C21A K1 C24A C23A 66.3(5) . . . . ?
O4A K1 O5B C24B -123(4) . . . . ?
O5A K1 O5B C24B 140(11) . . . . ?
O3 K1 O5B C24B -3(4) 3_767 . . . ?
O4B K1 O5B C24B -107(4) . . . . ?
F10 K1 O5B C24B 149(4) . . . . ?
O3 K1 O5B C24B 50(5) . . . . ?
O1 K1 O5B C24B 96(5) . . . . ?
F12 K1 O5B C24B -80(4) 4_566 . . . ?
N1 K1 O5B C24B 72(5) . . . . ?
F15 K1 O5B C24B 97(5) . . . . ?
C21A K1 O5B C24B -75(6) . . . . ?
O4A K1 O5B C25 56(3) . . . . ?
O5A K1 O5B C25 -41(7) . . . . ?
O3 K1 O5B C25 176.4(18) 3_767 . . . ?
O4B K1 O5B C25 72(2) . . . . ?
F10 K1 O5B C25 -31.9(18) . . . . ?
O3 K1 O5B C25 -130.8(16) . . . . ?
O1 K1 O5B C25 -85.1(18) . . . . ?
F12 K1 O5B C25 98.9(18) 4_566 . . . ?
N1 K1 O5B C25 -108.7(17) . . . . ?
F15 K1 O5B C25 -84.3(18) . . . . ?
C21A K1 O5B C25 104(3) . . . . ?
C25 O5B C24B C23B 177(4) . . . . ?
K1 O5B C24B C23B -4(8) . . . . ?
C24A O5A C25 O5B 54(7) . . . . ?
K1 O5A C25 O5B -140(7) . . . . ?
C24A O5A C25 C26 176.0(3) . . . . ?
K1 O5A C25 C26 -18.2(5) . . . . ?
C24B O5B C25 O5A -149(8) . . . . ?
K1 O5B C25 O5A 31(6) . . . . ?
C24B O5B C25 C26 147.5(19) . . . . ?
K1 O5B C25 C26 -31.9(19) . . . . ?
O4B C20 O4A C21A -85.1(15) . . . . ?
C19 C20 O4A C21A -179.9(3) . . . . ?
O4B C20 O4A K1 84.3(16) . . . . ?
C19 C20 O4A K1 -10.5(4) . . . . ?
O5A K1 O4A C21A 165.5(4) . . . . ?
O3 K1 O4A C21A 38.9(3) 3_767 . . . ?
O4B K1 O4A C21A 103.3(16) . . . . ?
F10 K1 O4A C21A -113.5(3) . . . . ?
O5B K1 O4A C21A 154.6(15) . . . . ?
O3 K1 O4A C21A -19.0(3) . . . . ?
O1 K1 O4A C21A -59.6(3) . . . . ?
F12 K1 O4A C21A 117.4(3) 4_566 . . . ?
N1 K1 O4A C21A -40.2(3) . . . . ?
F15 K1 O4A C21A -78.2(3) . . . . ?
O5A K1 O4A C20 -3.7(6) . . . . ?
O3 K1 O4A C20 -130.3(3) 3_767 . . . ?
O4B K1 O4A C20 -65.9(15) . . . . ?
F10 K1 O4A C20 77.3(3) . . . . ?
O5B K1 O4A C20 -14.6(16) . . . . ?
O3 K1 O4A C20 171.8(3) . . . . ?
O1 K1 O4A C20 131.2(3) . . . . ?
F12 K1 O4A C20 -51.8(3) 4_566 . . . ?
N1 K1 O4A C20 150.6(3) . . . . ?
F15 K1 O4A C20 112.6(3) . . . . ?
C21A K1 O4A C20 -169.2(5) . . . . ?
C20 O4A C21A C22A 77.7(5) . . . . ?
K1 O4A C21A C22A -93.2(3) . . . . ?
C20 O4A C21A K1 170.9(4) . . . . ?
O5A K1 C21A O4A -51.3(11) . . . . ?
O3 K1 C21A O4A -143.2(3) 3_767 . . . ?
O4B K1 C21A O4A -26.9(6) . . . . ?
F10 K1 C21A O4A 65.2(3) . . . . ?
O5B K1 C21A O4A -71(3) . . . . ?
O3 K1 C21A O4A 160.6(3) . . . . ?
O1 K1 C21A O4A 117.2(3) . . . . ?
F12 K1 C21A O4A -66.6(3) 4_566 . . . ?
N1 K1 C21A O4A 140.0(3) . . . . ?
F15 K1 C21A O4A 118.1(3) . . . . ?
O4A K1 C21A C22A 103.2(4) . . . . ?
O5A K1 C21A C22A 51.9(10) . . . . ?
O3 K1 C21A C22A -40.0(3) 3_767 . . . ?
O4B K1 C21A C22A 76.3(7) . . . . ?
F10 K1 C21A C22A 168.4(3) . . . . ?
O5B K1 C21A C22A 32(3) . . . . ?
O3 K1 C21A C22A -96.2(3) . . . . ?
O1 K1 C21A C22A -139.6(3) . . . . ?
F12 K1 C21A C22A 36.6(3) 4_566 . . . ?
N1 K1 C21A C22A -116.8(3) . . . . ?
F15 K1 C21A C22A -138.7(2) . . . . ?
O4A C20 O4B C21B 99.2(16) . . . . ?
C19 C20 O4B C21B -167.5(9) . . . . ?
O4A C20 O4B K1 -60.8(15) . . . . ?
C19 C20 O4B K1 32.4(9) . . . . ?
C22B C21B O4B C20 169(2) . . . . ?
C22B C21B O4B K1 -31(2) . . . . ?
O4A K1 O4B C20 73.7(17) . . . . ?
O5A K1 O4B C20 -60.5(11) . . . . ?
O3 K1 O4B C20 -168.0(8) 3_767 . . . ?
F10 K1 O4B C20 37.2(8) . . . . ?
O5B K1 O4B C20 -68.6(16) . . . . ?
O3 K1 O4B C20 133.2(8) . . . . ?
O1 K1 O4B C20 90.8(8) . . . . ?
F12 K1 O4B C20 -92.3(8) 4_566 . . . ?
N1 K1 O4B C20 112.0(8) . . . . ?
F15 K1 O4B C20 71.7(10) . . . . ?
C21A K1 O4B C20 125.7(12) . . . . ?
O4A K1 O4B C21B -83.4(17) . . . . ?
O5A K1 O4B C21B 142.5(10) . . . . ?
O3 K1 O4B C21B 34.9(11) 3_767 . . . ?
F10 K1 O4B C21B -119.9(11) . . . . ?
O5B K1 O4B C21B 134.3(16) . . . . ?
O3 K1 O4B C21B -23.9(12) . . . . ?
O1 K1 O4B C21B -66.2(11) . . . . ?
F12 K1 O4B C21B 110.6(11) 4_566 . . . ?
N1 K1 O4B C21B -45.1(12) . . . . ?
F15 K1 O4B C21B -85.4(13) . . . . ?
C21A K1 O4B C21B -31.3(10) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 32.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.582
_refine_diff_density_min -0.425
_refine_diff_density_rms 0.051
#===================== End of CIF submission =================================