Electronic Supplementary Material for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2008
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_publ_contact_author_name 'Ingo Krossing'
_publ_contact_author_address
;
Institut fuer Anorganische und Analytische Chemie
Universitaet Freiburg
Albertstr. 21
Freiburg i. Br.
79104
GERMANY
;
_publ_contact_author_email KROSSING@UNI-FREIBURG.DE
_publ_section_title
;
Stable CI3+ Salts and Attempts to Prepare CHI2+ and
CH2I+
;
loop_
_publ_author_name
'Ingo Krossing'
'Daniel Himmel'
'M. Kaupp'
'Sonja Muller'
'Ines Raabe'
'Nils Trapp'
data_sonja2
_database_code_depnum_ccdc_archive 'CCDC 646517'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'Ag1 C19 H6 I6 Al1 O4 F36'
_chemical_formula_sum 'C19 H6 Ag Al F36 I6 O4'
_chemical_formula_weight 1878.49
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'
Al Al 0.0645 0.0514 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
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 10.397(2)
_cell_length_b 14.727(3)
_cell_length_c 28.946(6)
_cell_angle_alpha 90.00
_cell_angle_beta 97.13(3)
_cell_angle_gamma 90.00
_cell_volume 4397.8(15)
_cell_formula_units_Z 4
_cell_measurement_temperature 140(2)
_cell_measurement_reflns_used 24282
_cell_measurement_theta_min 6.81
_cell_measurement_theta_max 23.96
_exptl_crystal_description plate
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.7
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.2
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.837
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3416
_exptl_absorpt_coefficient_mu 4.873
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.1589
_exptl_absorpt_correction_T_max 0.7779
_exptl_absorpt_process_details 'X-Shape (STOE)'
_exptl_special_details
;
Crystal moutned in PFE-oil
;
_diffrn_ambient_temperature 140(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 'STOE IPDS II'
_diffrn_measurement_method \f-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 24282
_diffrn_reflns_av_R_equivalents 0.1675
_diffrn_reflns_av_sigmaI/netI 0.1022
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_theta_min 6.81
_diffrn_reflns_theta_max 23.96
_reflns_number_total 6459
_reflns_number_gt 5384
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'XPOSE (STOE, 2003)'
_computing_cell_refinement 'CELL (STOE, 2003)'
_computing_data_reduction 'XRED (STOE, 2003)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Diamond 3.1 (Crystal Impact, 2006)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1344P)^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 SHELXL
_refine_ls_extinction_coef 0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 6459
_refine_ls_number_parameters 605
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0794
_refine_ls_R_factor_gt 0.0720
_refine_ls_wR_factor_ref 0.1980
_refine_ls_wR_factor_gt 0.1883
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_restrained_S_all 1.053
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.12155(7) 0.58800(5) 0.45928(3) 0.0584(3) Uani 1 1 d . . .
I3 I 0.12286(7) 0.59242(5) 0.30055(3) 0.0587(3) Uani 1 1 d . . .
I2 I -0.14269(7) 0.71533(4) 0.40452(3) 0.0558(3) Uani 1 1 d . . .
I6 I 0.17534(8) 0.90977(6) 0.44089(3) 0.0691(3) Uani 1 1 d . . .
I5 I 0.08485(9) 0.88991(5) 0.32063(2) 0.0653(3) Uani 1 1 d . . .
I4 I 0.40326(7) 0.67072(5) 0.37130(2) 0.0573(3) Uani 1 1 d . . .
Ag1 Ag 0.13284(13) 0.73068(7) 0.38184(5) 0.0969(5) Uani 1 1 d . . .
Al1 Al 1.4677(2) 0.72145(14) 0.13367(7) 0.0298(5) Uani 1 1 d . . .
F25 F 1.4559(6) 0.8927(4) 0.0079(2) 0.0591(15) Uani 1 1 d . . .
O2 O 1.5900(6) 0.7031(5) 0.1776(2) 0.0498(15) Uani 1 1 d . . .
F21 F 1.7656(7) 0.7144(4) 0.0181(2) 0.0701(18) Uani 1 1 d . . .
F24 F 1.5258(8) 0.6233(4) 0.0226(2) 0.0690(18) Uani 1 1 d . . .
F23 F 1.3726(7) 0.7197(5) 0.0122(2) 0.0710(18) Uani 1 1 d . . .
O1 O 1.4084(8) 0.6186(4) 0.1139(3) 0.0568(18) Uani 1 1 d . . .
F22 F 1.5260(8) 0.7238(4) -0.03146(19) 0.0701(18) Uani 1 1 d . . .
F26 F 1.6070(7) 0.9324(4) 0.0590(2) 0.0611(16) Uani 1 1 d . . .
F12 F 1.8688(9) 0.7141(8) 0.1860(3) 0.108(3) Uani 1 1 d . . .
O3 O 1.5209(6) 0.7774(4) 0.08725(19) 0.0375(13) Uani 1 1 d . . .
O4 O 1.3481(7) 0.7847(4) 0.1536(2) 0.0495(15) Uani 1 1 d . . .
F3 F 1.3161(8) 0.4835(4) 0.0454(2) 0.079(2) Uani 1 1 d . . .
C01 C -0.0799(11) 0.6165(7) 0.4551(4) 0.056(2) Uani 1 1 d . . .
H01A H -0.1281 0.5609 0.4478 0.067 Uiso 1 1 calc R . .
H01B H -0.0992 0.6375 0.4853 0.067 Uiso 1 1 calc R . .
F2 F 1.1729(7) 0.4477(4) 0.0893(3) 0.083(2) Uani 1 1 d . . .
F11 F 1.7459(11) 0.8440(6) 0.1725(3) 0.111(3) Uani 1 1 d . . .
C1 C 1.3537(9) 0.5371(5) 0.1234(3) 0.0404(19) Uani 1 1 d . . .
F6 F 1.5173(8) 0.4652(6) 0.1737(3) 0.087(2) Uani 1 1 d . . .
F1 F 1.1826(8) 0.5843(4) 0.0644(3) 0.076(2) Uani 1 1 d . . .
F20 F 1.7257(7) 0.6711(4) 0.0865(2) 0.0710(19) Uani 1 1 d . . .
F27 F 1.6519(6) 0.8801(4) -0.0061(2) 0.0641(16) Uani 1 1 d . . .
F19 F 1.7956(6) 0.8062(5) 0.0775(3) 0.0753(19) Uani 1 1 d . . .
F5 F 1.4050(8) 0.3798(4) 0.1244(3) 0.0730(19) Uani 1 1 d . . .
C5 C 1.6680(9) 0.7257(6) 0.2157(3) 0.042(2) Uani 1 1 d . . .
C12 C 1.5722(10) 0.8709(6) 0.0274(4) 0.048(2) Uani 1 1 d . . .
C3 C 1.4553(11) 0.4604(7) 0.1313(5) 0.064(3) Uani 1 1 d . . .
F10 F 1.8433(11) 0.8221(9) 0.2412(4) 0.141(5) Uani 1 1 d . . .
C11 C 1.4994(11) 0.7084(7) 0.0127(3) 0.052(2) Uani 1 1 d . . .
F4 F 1.5429(8) 0.4705(5) 0.1011(3) 0.087(2) Uani 1 1 d . . .
C6 C 1.785(2) 0.7749(17) 0.2040(5) 0.121(8) Uani 1 1 d . . .
C9 C 1.5772(9) 0.7740(5) 0.0478(3) 0.0380(18) Uani 1 1 d . . .
C10 C 1.7181(10) 0.7403(7) 0.0577(3) 0.050(2) Uani 1 1 d . . .
C2 C 1.2569(13) 0.5137(7) 0.0805(4) 0.068(3) Uani 1 1 d . . .
F36 F 1.3239(7) 0.9420(4) 0.0881(2) 0.0639(16) Uani 1 1 d . . .
F9 F 1.1684(7) 0.5891(4) 0.1563(3) 0.0659(17) Uani 1 1 d . . .
F30 F 1.1806(7) 0.7813(4) 0.2140(2) 0.0708(18) Uani 1 1 d . . .
F33 F 1.0694(7) 0.8925(4) 0.0947(3) 0.0739(19) Uani 1 1 d . . .
F32 F 1.1933(7) 0.7856(4) 0.0730(2) 0.0655(16) Uani 1 1 d . . .
F8 F 1.3471(7) 0.5893(4) 0.2000(2) 0.0660(16) Uani 1 1 d . . .
F31 F 1.0695(7) 0.7586(4) 0.1266(3) 0.0754(19) Uani 1 1 d . . .
F29 F 1.2890(9) 0.9071(5) 0.2244(3) 0.082(2) Uani 1 1 d . . .
F7 F 1.2512(7) 0.4628(4) 0.1822(3) 0.0736(19) Uani 1 1 d . . .
F15 F 1.6594(9) 0.7780(5) 0.2939(2) 0.087(2) Uani 1 1 d . . .
F35 F 1.4307(8) 0.9520(5) 0.1560(3) 0.085(2) Uani 1 1 d . . .
F34 F 1.2416(8) 1.0116(4) 0.1431(3) 0.082(2) Uani 1 1 d . . .
F14 F 1.4774(8) 0.7498(5) 0.2524(2) 0.0722(18) Uani 1 1 d . . .
F18 F 1.7450(8) 0.5745(5) 0.2116(3) 0.086(2) Uani 1 1 d . . .
F28 F 1.0892(8) 0.9074(5) 0.1908(3) 0.087(2) Uani 1 1 d . . .
F13 F 1.5867(11) 0.8684(5) 0.2351(3) 0.109(3) Uani 1 1 d . . .
F17 F 1.6088(9) 0.5995(5) 0.2615(3) 0.085(2) Uani 1 1 d . . .
C16 C 1.3147(11) 0.9396(7) 0.1331(4) 0.060(3) Uani 1 1 d . . .
C4 C 1.2791(11) 0.5442(6) 0.1659(4) 0.053(2) Uani 1 1 d . . .
F16 F 1.8107(9) 0.6427(7) 0.2738(3) 0.108(3) Uani 1 1 d . . .
C15 C 1.1449(11) 0.8208(7) 0.1099(4) 0.059(3) Uani 1 1 d . . .
C13 C 1.2578(9) 0.8498(6) 0.1474(3) 0.043(2) Uani 1 1 d . . .
C8 C 1.7118(14) 0.6326(9) 0.2414(5) 0.075(3) Uani 1 1 d . . .
C14 C 1.2018(13) 0.8591(9) 0.1957(4) 0.067(3) Uani 1 1 d . . .
C03 C 0.1311(11) 0.9785(8) 0.3768(4) 0.059(3) Uani 1 1 d . . .
H03A H 0.0586 1.0191 0.3788 0.070 Uiso 1 1 calc R . .
H03B H 0.2050 1.0153 0.3710 0.070 Uiso 1 1 calc R . .
C7 C 1.5900(17) 0.7817(8) 0.2510(4) 0.076(4) Uani 1 1 d . . .
C02 C 0.3263(13) 0.5829(12) 0.3166(6) 0.097(5) Uani 1 1 d . . .
H02A H 0.3663 0.5971 0.2890 0.117 Uiso 1 1 calc R . .
H02B H 0.3489 0.5208 0.3254 0.117 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
I1 0.0460(5) 0.0803(5) 0.0496(5) 0.0134(3) 0.0089(3) 0.0028(3)
I3 0.0487(5) 0.0706(4) 0.0556(5) -0.0093(3) 0.0028(3) -0.0053(3)
I2 0.0594(5) 0.0521(4) 0.0566(5) 0.0093(3) 0.0102(3) 0.0060(3)
I6 0.0668(6) 0.0976(6) 0.0407(5) 0.0072(3) -0.0027(4) -0.0070(4)
I5 0.0837(6) 0.0739(5) 0.0384(4) -0.0027(3) 0.0075(4) -0.0147(3)
I4 0.0526(5) 0.0770(5) 0.0427(4) -0.0094(3) 0.0069(3) -0.0113(3)
Ag1 0.1168(10) 0.0710(6) 0.1191(10) 0.0291(6) 0.0797(9) 0.0199(5)
Al1 0.0327(14) 0.0381(11) 0.0186(11) 0.0015(8) 0.0033(9) -0.0026(9)
F25 0.057(4) 0.074(3) 0.048(3) 0.020(3) 0.011(3) 0.011(3)
O2 0.043(4) 0.082(4) 0.023(3) 0.000(3) 0.001(3) 0.009(3)
F21 0.066(5) 0.090(4) 0.061(4) 0.016(3) 0.035(3) 0.025(3)
F24 0.114(6) 0.050(3) 0.046(3) -0.011(3) 0.021(3) -0.004(3)
F23 0.061(5) 0.089(4) 0.061(4) -0.015(3) 0.000(3) -0.016(3)
O1 0.077(5) 0.050(3) 0.048(4) -0.007(3) 0.027(4) -0.026(3)
F22 0.102(5) 0.087(4) 0.022(3) -0.005(3) 0.011(3) -0.006(3)
F26 0.077(4) 0.053(3) 0.054(4) 0.003(3) 0.012(3) -0.020(3)
F12 0.061(6) 0.195(10) 0.072(5) -0.001(6) 0.028(4) -0.010(5)
O3 0.039(4) 0.050(3) 0.025(3) 0.007(2) 0.011(2) 0.000(2)
O4 0.047(4) 0.069(4) 0.035(3) 0.012(3) 0.013(3) 0.019(3)
F3 0.125(6) 0.070(4) 0.042(3) -0.021(3) 0.010(4) 0.001(4)
C01 0.048(6) 0.072(6) 0.051(6) -0.001(5) 0.017(5) -0.002(4)
F2 0.067(5) 0.070(4) 0.110(6) -0.022(4) 0.001(4) -0.022(3)
F11 0.164(9) 0.102(6) 0.068(5) 0.013(4) 0.017(5) -0.055(6)
C1 0.051(6) 0.037(4) 0.035(5) 0.003(3) 0.012(4) -0.009(3)
F6 0.079(5) 0.122(6) 0.056(4) 0.009(4) -0.011(4) 0.027(4)
F1 0.097(6) 0.070(4) 0.056(4) -0.004(3) -0.010(4) 0.012(3)
F20 0.071(5) 0.082(4) 0.064(4) 0.028(3) 0.023(3) 0.034(3)
F27 0.065(4) 0.077(3) 0.056(4) 0.026(3) 0.028(3) 0.001(3)
F19 0.031(4) 0.111(5) 0.081(5) 0.015(4) -0.003(3) -0.007(3)
F5 0.092(5) 0.049(3) 0.083(5) 0.008(3) 0.030(4) 0.012(3)
C5 0.048(6) 0.052(4) 0.025(4) -0.006(3) -0.003(4) 0.004(4)
C12 0.045(6) 0.056(5) 0.046(6) 0.016(4) 0.021(4) -0.003(4)
C3 0.050(7) 0.070(6) 0.075(8) 0.006(6) 0.023(6) -0.002(5)
F10 0.122(9) 0.211(11) 0.088(7) -0.028(7) 0.002(6) -0.104(8)
C11 0.057(7) 0.072(6) 0.028(5) 0.001(4) 0.013(4) -0.005(5)
F4 0.067(5) 0.099(5) 0.103(6) -0.011(4) 0.043(4) 0.002(4)
C6 0.118(16) 0.20(2) 0.044(7) 0.014(10) -0.014(9) -0.080(14)
C9 0.043(5) 0.051(4) 0.020(4) 0.004(3) 0.005(3) 0.004(3)
C10 0.046(6) 0.068(5) 0.037(5) 0.014(4) 0.008(4) 0.011(4)
C2 0.084(9) 0.058(6) 0.060(7) -0.007(5) 0.002(6) 0.006(5)
F36 0.071(4) 0.071(3) 0.051(4) 0.019(3) 0.017(3) 0.007(3)
F9 0.058(4) 0.061(3) 0.083(5) 0.003(3) 0.025(3) 0.007(3)
F30 0.083(5) 0.080(4) 0.058(4) 0.016(3) 0.039(4) 0.012(3)
F33 0.055(4) 0.075(4) 0.088(5) 0.014(4) -0.006(4) 0.016(3)
F32 0.085(5) 0.065(3) 0.043(3) -0.009(3) -0.003(3) 0.003(3)
F8 0.078(5) 0.090(4) 0.031(3) 0.000(3) 0.009(3) -0.013(3)
F31 0.055(4) 0.072(4) 0.098(5) 0.025(4) 0.005(4) -0.008(3)
F29 0.116(6) 0.085(4) 0.045(4) -0.014(3) 0.012(4) 0.006(4)
F7 0.080(5) 0.062(3) 0.086(5) 0.024(3) 0.037(4) -0.007(3)
F15 0.131(7) 0.099(5) 0.027(3) -0.020(3) -0.007(4) 0.002(4)
F35 0.072(5) 0.102(5) 0.075(5) 0.019(4) -0.014(4) -0.028(4)
F34 0.113(6) 0.055(3) 0.079(5) -0.002(3) 0.021(4) 0.007(3)
F14 0.068(5) 0.104(5) 0.048(4) 0.004(3) 0.019(3) 0.022(4)
F18 0.102(6) 0.083(4) 0.074(5) -0.013(4) 0.021(4) 0.039(4)
F28 0.090(6) 0.093(4) 0.091(6) 0.016(4) 0.056(5) 0.042(4)
F13 0.166(9) 0.075(5) 0.079(5) -0.025(4) -0.017(6) 0.047(5)
F17 0.092(6) 0.100(5) 0.066(5) 0.019(4) 0.013(4) -0.005(4)
C16 0.057(7) 0.064(6) 0.056(7) -0.008(5) 0.000(5) 0.006(5)
C4 0.055(7) 0.055(5) 0.051(6) 0.013(4) 0.012(5) -0.011(4)
F16 0.087(6) 0.156(8) 0.074(5) 0.015(5) -0.023(5) 0.050(5)
C15 0.049(7) 0.064(6) 0.063(7) 0.011(5) 0.008(5) 0.009(4)
C13 0.039(5) 0.054(4) 0.038(5) 0.004(4) 0.016(4) 0.011(4)
C8 0.077(9) 0.081(7) 0.071(8) -0.007(6) 0.022(7) 0.003(6)
C14 0.068(8) 0.091(8) 0.044(6) 0.002(6) 0.021(6) 0.010(6)
C03 0.052(7) 0.077(6) 0.043(6) -0.005(5) -0.008(5) 0.000(5)
C7 0.113(13) 0.077(7) 0.036(6) 0.007(5) -0.003(7) 0.003(7)
C02 0.050(8) 0.145(13) 0.097(12) -0.065(10) 0.006(7) -0.004(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C01 2.125(11) . ?
I1 Ag1 3.0853(13) . ?
I3 C02 2.114(14) . ?
I3 Ag1 3.1037(16) . ?
I2 C01 2.110(11) . ?
I2 Ag1 3.0257(15) . ?
I6 C03 2.115(11) . ?
I6 Ag1 3.1442(16) . ?
I5 C03 2.093(11) . ?
I5 Ag1 2.9441(13) . ?
I4 C02 2.122(13) . ?
I4 Ag1 2.9984(14) . ?
Al1 O2 1.705(6) . ?
Al1 O1 1.707(6) . ?
Al1 O4 1.709(6) . ?
Al1 O3 1.725(6) . ?
F25 C12 1.310(12) . ?
O2 C5 1.327(11) . ?
F21 C10 1.358(12) . ?
F24 C11 1.308(12) . ?
F23 C11 1.327(13) . ?
O1 C1 1.371(10) . ?
F22 C11 1.360(11) . ?
F26 C12 1.306(12) . ?
F12 C6 1.40(3) . ?
O3 C9 1.348(10) . ?
O4 C13 1.339(11) . ?
F3 C2 1.328(14) . ?
F2 C2 1.353(15) . ?
F11 C6 1.39(2) . ?
C1 C4 1.537(13) . ?
C1 C2 1.539(15) . ?
C1 C3 1.544(14) . ?
F6 C3 1.314(15) . ?
F1 C2 1.343(13) . ?
F20 C10 1.312(11) . ?
F27 C12 1.360(11) . ?
F19 C10 1.343(13) . ?
F5 C3 1.301(13) . ?
C5 C6 1.49(2) . ?
C5 C8 1.600(16) . ?
C5 C7 1.609(17) . ?
C12 C9 1.542(12) . ?
C3 F4 1.347(13) . ?
F10 C6 1.360(19) . ?
C11 C9 1.554(13) . ?
C9 C10 1.539(14) . ?
F36 C16 1.318(14) . ?
F9 C4 1.327(13) . ?
F30 C14 1.292(14) . ?
F33 C15 1.357(12) . ?
F32 C15 1.340(14) . ?
F8 C4 1.318(13) . ?
F31 C15 1.334(13) . ?
F29 C14 1.352(16) . ?
F7 C4 1.332(11) . ?
F15 C7 1.359(14) . ?
F35 C16 1.315(13) . ?
F34 C16 1.357(13) . ?
F14 C7 1.267(17) . ?
F18 C8 1.292(15) . ?
F28 C14 1.363(14) . ?
F13 C7 1.355(15) . ?
F17 C8 1.370(16) . ?
C16 C13 1.526(15) . ?
F16 C8 1.310(17) . ?
C15 C13 1.556(15) . ?
C13 C14 1.586(13) . ?
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
C01 I1 Ag1 87.2(3) . . ?
C02 I3 Ag1 86.5(4) . . ?
C01 I2 Ag1 89.0(3) . . ?
C03 I6 Ag1 85.6(3) . . ?
C03 I5 Ag1 91.4(3) . . ?
C02 I4 Ag1 89.1(4) . . ?
I5 Ag1 I4 105.33(4) . . ?
I5 Ag1 I2 95.50(4) . . ?
I4 Ag1 I2 157.68(4) . . ?
I5 Ag1 I1 163.91(4) . . ?
I4 Ag1 I1 89.66(4) . . ?
I2 Ag1 I1 70.67(3) . . ?
I5 Ag1 I3 94.54(5) . . ?
I4 Ag1 I3 70.92(4) . . ?
I2 Ag1 I3 99.91(5) . . ?
I1 Ag1 I3 95.93(4) . . ?
I5 Ag1 I6 70.18(3) . . ?
I4 Ag1 I6 103.42(5) . . ?
I2 Ag1 I6 91.01(4) . . ?
I1 Ag1 I6 101.05(5) . . ?
I3 Ag1 I6 162.12(4) . . ?
O2 Al1 O1 108.3(4) . . ?
O2 Al1 O4 109.9(3) . . ?
O1 Al1 O4 110.4(4) . . ?
O2 Al1 O3 112.1(3) . . ?
O1 Al1 O3 107.5(3) . . ?
O4 Al1 O3 108.6(3) . . ?
C5 O2 Al1 154.4(6) . . ?
C1 O1 Al1 148.4(6) . . ?
C9 O3 Al1 149.0(5) . . ?
C13 O4 Al1 150.7(6) . . ?
I2 C01 I1 113.2(5) . . ?
O1 C1 C4 111.4(7) . . ?
O1 C1 C2 106.2(8) . . ?
C4 C1 C2 108.5(9) . . ?
O1 C1 C3 112.2(8) . . ?
C4 C1 C3 109.6(8) . . ?
C2 C1 C3 108.8(8) . . ?
O2 C5 C6 111.4(9) . . ?
O2 C5 C8 106.3(8) . . ?
C6 C5 C8 109.3(13) . . ?
O2 C5 C7 110.6(9) . . ?
C6 C5 C7 112.6(13) . . ?
C8 C5 C7 106.3(8) . . ?
F26 C12 F25 107.0(8) . . ?
F26 C12 F27 106.9(7) . . ?
F25 C12 F27 106.2(8) . . ?
F26 C12 C9 112.4(8) . . ?
F25 C12 C9 112.2(7) . . ?
F27 C12 C9 111.8(8) . . ?
F5 C3 F6 109.5(10) . . ?
F5 C3 F4 107.0(9) . . ?
F6 C3 F4 107.8(10) . . ?
F5 C3 C1 113.0(9) . . ?
F6 C3 C1 110.2(9) . . ?
F4 C3 C1 109.2(9) . . ?
F24 C11 F23 107.7(8) . . ?
F24 C11 F22 107.7(8) . . ?
F23 C11 F22 106.7(9) . . ?
F24 C11 C9 112.0(8) . . ?
F23 C11 C9 111.4(8) . . ?
F22 C11 C9 111.1(8) . . ?
F10 C6 F11 102.1(17) . . ?
F10 C6 F12 112.6(18) . . ?
F11 C6 F12 111.7(13) . . ?
F10 C6 C5 111.4(14) . . ?
F11 C6 C5 109.0(16) . . ?
F12 C6 C5 109.7(16) . . ?
O3 C9 C10 110.9(7) . . ?
O3 C9 C12 106.9(7) . . ?
C10 C9 C12 110.9(7) . . ?
O3 C9 C11 109.4(7) . . ?
C10 C9 C11 109.2(8) . . ?
C12 C9 C11 109.6(7) . . ?
F20 C10 F19 107.8(8) . . ?
F20 C10 F21 108.5(8) . . ?
F19 C10 F21 107.4(9) . . ?
F20 C10 C9 110.5(8) . . ?
F19 C10 C9 110.7(8) . . ?
F21 C10 C9 111.7(8) . . ?
F3 C2 F1 107.2(10) . . ?
F3 C2 F2 106.0(9) . . ?
F1 C2 F2 105.4(10) . . ?
F3 C2 C1 112.0(10) . . ?
F1 C2 C1 113.4(8) . . ?
F2 C2 C1 112.3(10) . . ?
F35 C16 F36 108.7(10) . . ?
F35 C16 F34 106.6(9) . . ?
F36 C16 F34 107.6(9) . . ?
F35 C16 C13 110.3(9) . . ?
F36 C16 C13 111.6(8) . . ?
F34 C16 C13 111.9(10) . . ?
F8 C4 F9 106.1(9) . . ?
F8 C4 F7 108.0(9) . . ?
F9 C4 F7 107.6(8) . . ?
F8 C4 C1 110.8(8) . . ?
F9 C4 C1 112.1(9) . . ?
F7 C4 C1 112.0(8) . . ?
F31 C15 F32 108.6(9) . . ?
F31 C15 F33 108.1(9) . . ?
F32 C15 F33 107.5(9) . . ?
F31 C15 C13 111.3(9) . . ?
F32 C15 C13 109.6(9) . . ?
F33 C15 C13 111.7(9) . . ?
O4 C13 C16 111.6(8) . . ?
O4 C13 C15 110.7(8) . . ?
C16 C13 C15 109.5(8) . . ?
O4 C13 C14 105.8(8) . . ?
C16 C13 C14 111.2(8) . . ?
C15 C13 C14 108.0(9) . . ?
F18 C8 F16 107.6(12) . . ?
F18 C8 F17 109.6(11) . . ?
F16 C8 F17 108.8(12) . . ?
F18 C8 C5 110.0(11) . . ?
F16 C8 C5 112.8(10) . . ?
F17 C8 C5 108.1(10) . . ?
F30 C14 F29 110.3(10) . . ?
F30 C14 F28 108.5(10) . . ?
F29 C14 F28 107.0(10) . . ?
F30 C14 C13 112.6(9) . . ?
F29 C14 C13 107.2(9) . . ?
F28 C14 C13 111.0(9) . . ?
I5 C03 I6 112.8(5) . . ?
F14 C7 F13 112.1(13) . . ?
F14 C7 F15 110.1(11) . . ?
F13 C7 F15 109.7(10) . . ?
F14 C7 C5 111.7(10) . . ?
F13 C7 C5 105.1(10) . . ?
F15 C7 C5 107.9(11) . . ?
I3 C02 I4 113.4(6) . . ?
_diffrn_measured_fraction_theta_max 0.940
_diffrn_reflns_theta_full 23.96
_diffrn_measured_fraction_theta_full 0.940
_refine_diff_density_max 1.617
_refine_diff_density_min -2.174
_refine_diff_density_rms 0.249