# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Sergey Troyanov'
_publ_contact_author_address     
;
Chemistry
Moscow State University
Leninkie Gory
Moscow
119992
RUSSIAN FEDERATION
;

_publ_contact_author_email       SERGEJ.TROYANOV@RZ.HU-BERLIN.DE

_publ_section_title              
;
The former C60F16 is actually a double-caged adduct:
(C60F16)(C60)
;
loop_
_publ_author_name
'Sergey Troyanov'
'Stanislav M Avdoshenko'
'Alexey A. Goryunkov'
'Iiya N. Ioffe'
'Pavel A. Khavrel'
;
V.Yu.Markov
;
'Z. Mazej'
'Lev N. Sidorov'

# Attachment 'fgp17d.CIF'

data_fgp17c
_database_code_depnum_ccdc_archive 'CCDC 625333'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C60F16)(C60) 2C7H8 2C6..'
_chemical_formula_sum            'C146 H16 F16'
_chemical_formula_weight         2073.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   11.1816(5)
_cell_length_b                   21.1070(10)
_cell_length_c                   18.2770(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.687(3)
_cell_angle_gamma                90.00
_cell_volume                     4131.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9000
_cell_measurement_theta_min      6
_cell_measurement_theta_max      30

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2072
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.91000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'BL14.2, PSF, BESSY, Berlin, Germany'
_diffrn_radiation_monochromator  Cu(113)
_diffrn_measurement_device_type  MAR345
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12501
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         33.5
_reflns_number_total             4094
_reflns_number_gt                2753
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
Some additional atoms, C72-C77, with very large thermal displacement
parameters probably belong to a strongly disordered molecule which, however,
could not be identified reliably (only toluene was used in the separation and
crystal growing procedures). Therefore, the composition of the compound given
in the paper does not include this not completely identified unit.
The coefficients of the weighting scheme were varied to receive best R1
and esd's values before they were included into final refinement.

;

_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^)+(0.0850P)^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       0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4094
_refine_ls_number_parameters     706
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.1944
_refine_ls_wR_factor_gt          0.1815
_refine_ls_goodness_of_fit_ref   1.355
_refine_ls_restrained_S_all      1.355
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.3753(3) 0.17310(15) 0.4431(2) 0.0748(10) Uani 1 1 d . . .
F2 F 0.5309(3) 0.08663(15) 0.5004(2) 0.0750(10) Uani 1 1 d . . .
F3 F 0.4177(3) 0.02799(16) 0.5776(2) 0.0790(11) Uani 1 1 d . . .
F4 F 0.2184(3) 0.09000(15) 0.5515(2) 0.0791(11) Uani 1 1 d . . .
F5 F 0.1788(3) 0.06220(16) 0.6744(2) 0.0848(12) Uani 1 1 d . . .
F6 F 0.0686(3) 0.16639(16) 0.6526(2) 0.0791(11) Uani 1 1 d . . .
F7 F 0.1018(3) 0.19129(17) 0.7909(2) 0.0871(12) Uani 1 1 d . . .
F8 F 0.3372(3) 0.03538(17) 0.7888(2) 0.0884(12) Uani 1 1 d . . .
C1 C 0.2500(5) 0.2179(3) 0.6436(4) 0.0677(18) Uani 1 1 d . . .
C2 C 0.3133(5) 0.1839(3) 0.6016(4) 0.0664(18) Uani 1 1 d . . .
C3 C 0.3766(5) 0.2167(3) 0.5584(4) 0.0666(18) Uani 1 1 d . . .
C4 C 0.4548(5) 0.1908(3) 0.5141(4) 0.0625(17) Uani 1 1 d . . .
C5 C 0.5151(6) 0.1288(3) 0.5554(4) 0.0696(19) Uani 1 1 d . . .
C6 C 0.4400(6) 0.0896(3) 0.6083(4) 0.071(2) Uani 1 1 d . . .
C7 C 0.3130(6) 0.1161(3) 0.6118(4) 0.0640(17) Uani 1 1 d . . .
C8 C 0.2656(6) 0.1098(3) 0.6865(4) 0.0674(18) Uani 1 1 d . . .
C9 C 0.1955(6) 0.1760(3) 0.6911(4) 0.076(2) Uani 1 1 d . . .
C10 C 0.2032(5) 0.2106(3) 0.7670(4) 0.0698(19) Uani 1 1 d . . .
C11 C 0.3691(6) 0.0936(3) 0.7603(4) 0.075(2) Uani 1 1 d . . .
C12 C 0.3915(6) 0.1422(3) 0.8251(4) 0.0700(19) Uani 1 1 d . . .
C13 C 0.3218(6) 0.1941(4) 0.8258(4) 0.0703(18) Uani 1 1 d . . .
C14 C 0.3780(9) 0.2500 0.8665(6) 0.076(3) Uani 1 2 d S . .
C15 C 0.5038(10) 0.2500 0.9093(5) 0.071(3) Uani 1 2 d S . .
C16 C 0.5798(6) 0.1950(4) 0.9097(4) 0.0717(19) Uani 1 1 d . . .
C17 C 0.7010(6) 0.2163(3) 0.9084(4) 0.0721(19) Uani 1 1 d . . .
C18 C 0.7653(6) 0.1830(3) 0.8649(4) 0.0738(19) Uani 1 1 d . . .
C19 C 0.8322(5) 0.2170(3) 0.8191(4) 0.0696(19) Uani 1 1 d . . .
C20 C 0.8146(5) 0.1832(3) 0.7488(5) 0.0706(19) Uani 1 1 d . . .
C21 C 0.7953(6) 0.2159(3) 0.6796(5) 0.0680(19) Uani 1 1 d . . .
C22 C 0.7089(6) 0.1949(3) 0.6118(4) 0.0629(17) Uani 1 1 d . . .
C23 C 0.6372(6) 0.1430(3) 0.6126(4) 0.0633(17) Uani 1 1 d . . .
C24 C 0.6496(6) 0.1107(3) 0.6835(5) 0.0666(18) Uani 1 1 d . . .
C25 C 0.7382(6) 0.1287(3) 0.7491(4) 0.0696(19) Uani 1 1 d . . .
C26 C 0.7089(6) 0.1288(3) 0.8216(4) 0.0727(19) Uani 1 1 d . . .
C27 C 0.5898(7) 0.1085(3) 0.8209(4) 0.0700(19) Uani 1 1 d . . .
C28 C 0.5252(7) 0.1427(3) 0.8656(5) 0.079(2) Uani 1 1 d . . .
C29 C 0.5013(6) 0.0870(3) 0.7517(5) 0.075(2) Uani 1 1 d . . .
C30 C 0.5316(6) 0.0878(3) 0.6852(5) 0.0693(18) Uani 1 1 d . . .
C31 C 0.5367(7) 0.2500 0.5031(5) 0.063(2) Uani 1 2 d S . .
C32 C 0.6715(8) 0.2500 0.5553(6) 0.071(3) Uani 1 2 d S . .
C33 C 0.5832(8) 0.2500 0.4294(6) 0.071(3) Uani 1 2 d S . .
C34 C 0.7245(7) 0.2500 0.4851(5) 0.063(2) Uani 1 2 d S . .
C35 C 0.8054(6) 0.3067(4) 0.4771(4) 0.0715(19) Uani 1 1 d . . .
C36 C 0.9299(6) 0.2845(3) 0.4830(4) 0.0730(19) Uani 1 1 d . . .
C37 C 1.0074(6) 0.3170(4) 0.4485(5) 0.084(2) Uani 1 1 d . . .
C38 C 1.0869(6) 0.2832(3) 0.4108(5) 0.090(2) Uani 1 1 d . . .
C39 C 1.0878(7) 0.3172(5) 0.3433(5) 0.096(2) Uani 1 1 d . . .
C40 C 1.0881(6) 0.2845(4) 0.2783(6) 0.089(2) Uani 1 1 d . . .
C41 C 1.0113(8) 0.3055(4) 0.2048(5) 0.092(2) Uani 1 1 d . . .
C42 C 0.9613(13) 0.2500 0.1583(8) 0.092(3) Uani 1 2 d S . .
C43 C 0.8434(12) 0.2500 0.1094(6) 0.085(3) Uani 1 2 d S . .
C44 C 0.7666(8) 0.3058(4) 0.1045(5) 0.093(2) Uani 1 1 d . . .
C45 C 0.6397(8) 0.2845(3) 0.0946(4) 0.091(2) Uani 1 1 d . . .
C46 C 0.5617(7) 0.3170(4) 0.1285(5) 0.095(2) Uani 1 1 d . . .
C47 C 0.4839(6) 0.2827(3) 0.1658(5) 0.087(2) Uani 1 1 d . . .
C48 C 0.4817(6) 0.3159(4) 0.2351(5) 0.082(2) Uani 1 1 d . . .
C49 C 0.4815(6) 0.2850(3) 0.3000(5) 0.077(2) Uani 1 1 d . . .
C50 C 0.5540(6) 0.3072(3) 0.3745(4) 0.0709(19) Uani 1 1 d . . .
C51 C 0.6313(7) 0.3573(3) 0.3806(4) 0.0705(19) Uani 1 1 d . . .
C52 C 0.7594(6) 0.3578(3) 0.4326(4) 0.075(2) Uani 1 1 d . . .
C53 C 0.8390(7) 0.3917(3) 0.3941(5) 0.076(2) Uani 1 1 d . . .
C54 C 0.9603(7) 0.3721(4) 0.4032(5) 0.084(2) Uani 1 1 d . . .
C55 C 1.0101(8) 0.3729(4) 0.3389(6) 0.091(2) Uani 1 1 d . . .
C56 C 0.9370(8) 0.3922(4) 0.2685(6) 0.086(2) Uani 1 1 d . . .
C57 C 0.9369(8) 0.3587(4) 0.2004(5) 0.090(2) Uani 1 1 d . . .
C58 C 0.8125(9) 0.3584(4) 0.1490(5) 0.087(2) Uani 1 1 d . . .
C59 C 0.7323(9) 0.3925(4) 0.1855(6) 0.094(2) Uani 1 1 d . . .
C60 C 0.6095(8) 0.3720(4) 0.1748(5) 0.089(2) Uani 1 1 d . . .
C61 C 0.5593(8) 0.3725(4) 0.2391(5) 0.086(2) Uani 1 1 d . . .
C62 C 0.6328(7) 0.3912(3) 0.3110(5) 0.080(2) Uani 1 1 d . . .
C63 C 0.7615(8) 0.4125(3) 0.3213(6) 0.086(2) Uani 1 1 d . . .
C64 C 0.8101(9) 0.4130(3) 0.2593(6) 0.089(2) Uani 1 1 d . . .
C65 C 0.8933(5) 0.0033(3) 0.7724(3) 0.111(3) Uani 1 1 d G . .
C66 C 0.7892(6) -0.0357(2) 0.7607(4) 0.121(3) Uani 1 1 d G . .
H66 H 0.7679 -0.0533 0.8031 0.145 Uiso 1 1 calc R . .
C67 C 0.7165(5) -0.0490(2) 0.6868(5) 0.121(3) Uani 1 1 d G . .
H67 H 0.6454 -0.0756 0.6788 0.146 Uiso 1 1 calc R . .
C68 C 0.7477(5) -0.0233(2) 0.6247(4) 0.113(3) Uani 1 1 d G . .
H68 H 0.6980 -0.0324 0.5742 0.136 Uiso 1 1 calc R . .
C69 C 0.8517(5) 0.0157(2) 0.6365(4) 0.111(3) Uani 1 1 d G . .
C70 C 0.9245(4) 0.0290(2) 0.7103(4) 0.108(3) Uani 1 1 d G . .
H70 H 0.9956 0.0556 0.7184 0.130 Uiso 1 1 calc R . .
C71 C 0.9668(8) 0.0151(4) 0.8486(4) 0.102(5) Uani 0.50 1 d PG . .
H71A H 0.9129 0.0298 0.8790 0.153 Uiso 0.50 1 calc PR . .
H71B H 1.0292 0.0477 0.8485 0.153 Uiso 0.50 1 calc PR . .
H71C H 1.0091 -0.0240 0.8709 0.153 Uiso 0.50 1 calc PR . .
C71A C 0.8901(8) 0.0353(4) 0.5768(4) 0.082(4) Uani 0.50 1 d PG . .
H71D H 0.9606 0.0092 0.5731 0.123 Uiso 0.50 1 calc PR . .
H71E H 0.9163 0.0797 0.5842 0.123 Uiso 0.50 1 calc PR . .
H71F H 0.8214 0.0312 0.5296 0.123 Uiso 0.50 1 calc PR . .
C72 C 0.4500(14) 0.0179(8) 1.0088(10) 0.234(6) Uiso 1 1 d . . .
C73 C 0.315(2) -0.0007(11) 0.9961(11) 0.288(8) Uiso 1 1 d . . .
C74 C 0.256(3) 0.062(2) 1.0086(17) 0.411(15) Uiso 1 1 d . . .
C75 C 0.212(3) 0.1284(17) 1.0053(14) 0.354(12) Uiso 1 1 d . . .
C76 C 0.095(2) 0.1595(12) 1.0078(12) 0.322(10) Uiso 1 1 d . . .
C77 C 0.1432(13) 0.2191(8) 1.0093(8) 0.249(8) 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
F1 0.063(2) 0.072(2) 0.088(3) -0.003(2) 0.020(2) 0.0002(19)
F2 0.073(2) 0.064(2) 0.091(3) -0.006(2) 0.029(2) 0.0023(19)
F3 0.072(2) 0.064(2) 0.103(3) 0.001(2) 0.029(2) 0.0051(19)
F4 0.066(2) 0.065(2) 0.109(3) -0.004(2) 0.029(2) -0.004(2)
F5 0.075(2) 0.069(2) 0.116(3) 0.003(2) 0.037(2) -0.005(2)
F6 0.063(2) 0.075(2) 0.102(3) -0.002(2) 0.029(2) -0.0037(19)
F7 0.073(2) 0.085(3) 0.113(3) 0.004(2) 0.043(2) -0.005(2)
F8 0.087(3) 0.078(3) 0.111(3) 0.013(2) 0.045(2) 0.000(2)
C1 0.058(3) 0.055(4) 0.090(5) 0.003(3) 0.022(4) -0.001(3)
C2 0.059(4) 0.049(4) 0.090(5) -0.001(4) 0.020(4) -0.006(3)
C3 0.049(3) 0.060(4) 0.091(5) -0.003(4) 0.023(4) 0.000(3)
C4 0.053(4) 0.062(4) 0.072(5) -0.010(4) 0.017(4) -0.001(4)
C5 0.072(5) 0.046(4) 0.099(6) -0.006(4) 0.037(4) 0.006(4)
C6 0.073(4) 0.043(4) 0.102(6) -0.005(4) 0.031(5) -0.008(4)
C7 0.058(4) 0.065(5) 0.071(5) -0.014(4) 0.021(4) -0.005(4)
C8 0.053(4) 0.063(4) 0.084(5) -0.004(4) 0.017(4) -0.018(4)
C9 0.052(4) 0.081(5) 0.095(6) -0.005(5) 0.022(4) -0.011(4)
C10 0.052(4) 0.064(4) 0.104(6) 0.002(4) 0.040(4) -0.005(3)
C11 0.075(5) 0.065(5) 0.095(6) 0.004(5) 0.041(5) -0.010(4)
C12 0.072(5) 0.059(5) 0.085(5) 0.008(4) 0.033(4) -0.004(4)
C13 0.059(4) 0.072(5) 0.086(5) 0.003(4) 0.031(4) 0.000(4)
C14 0.065(7) 0.082(8) 0.089(8) 0.000 0.037(6) 0.000
C15 0.085(7) 0.070(7) 0.058(7) 0.000 0.023(6) 0.000
C16 0.074(5) 0.077(5) 0.066(5) 0.014(4) 0.023(4) 0.000(4)
C17 0.064(4) 0.076(4) 0.072(5) 0.007(3) 0.014(4) 0.006(3)
C18 0.062(4) 0.071(5) 0.082(5) 0.002(4) 0.010(4) 0.002(4)
C19 0.058(4) 0.077(5) 0.077(5) 0.004(4) 0.024(4) 0.006(3)
C20 0.049(4) 0.076(5) 0.086(6) -0.005(5) 0.019(4) 0.000(4)
C21 0.055(4) 0.070(4) 0.086(5) -0.001(4) 0.032(4) 0.004(3)
C22 0.058(4) 0.064(4) 0.065(5) 0.003(4) 0.014(4) -0.003(4)
C23 0.054(4) 0.063(5) 0.075(5) -0.001(4) 0.023(4) 0.003(4)
C24 0.058(4) 0.063(5) 0.079(6) 0.001(4) 0.021(4) 0.009(4)
C25 0.065(4) 0.073(5) 0.073(5) 0.008(4) 0.023(4) 0.008(4)
C26 0.066(5) 0.065(5) 0.081(6) 0.011(4) 0.012(4) 0.007(4)
C27 0.072(5) 0.070(5) 0.074(5) 0.010(4) 0.030(5) 0.004(4)
C28 0.078(5) 0.065(5) 0.101(6) 0.013(5) 0.037(5) 0.008(4)
C29 0.073(5) 0.061(5) 0.088(6) 0.012(4) 0.021(5) 0.003(4)
C30 0.067(5) 0.067(5) 0.071(5) 0.004(4) 0.014(5) 0.001(4)
C31 0.055(5) 0.050(5) 0.081(7) 0.000 0.015(5) 0.000
C32 0.067(6) 0.072(7) 0.076(7) 0.000 0.023(6) 0.000
C33 0.059(6) 0.069(7) 0.089(7) 0.000 0.029(6) 0.000
C34 0.058(5) 0.065(6) 0.067(6) 0.000 0.021(5) 0.000
C35 0.058(4) 0.075(5) 0.084(5) -0.009(4) 0.024(4) -0.001(4)
C36 0.065(4) 0.079(4) 0.074(5) -0.003(3) 0.017(4) -0.010(3)
C37 0.061(4) 0.081(5) 0.109(6) -0.006(5) 0.023(5) -0.022(4)
C38 0.051(4) 0.109(6) 0.114(6) -0.002(5) 0.033(4) -0.006(4)
C39 0.075(5) 0.121(8) 0.100(7) -0.015(6) 0.039(5) -0.024(5)
C40 0.075(5) 0.100(6) 0.099(6) -0.002(5) 0.035(5) -0.012(4)
C41 0.094(6) 0.092(6) 0.107(8) 0.005(6) 0.054(6) -0.001(6)
C42 0.107(10) 0.093(10) 0.084(9) 0.000 0.041(8) 0.000
C43 0.100(9) 0.087(9) 0.069(8) 0.000 0.025(7) 0.000
C44 0.101(6) 0.080(6) 0.104(7) 0.011(5) 0.041(5) 0.006(6)
C45 0.108(6) 0.098(6) 0.066(5) 0.002(4) 0.024(5) -0.005(5)
C46 0.106(6) 0.094(6) 0.091(6) 0.004(6) 0.039(5) 0.018(5)
C47 0.079(4) 0.100(6) 0.077(5) 0.007(4) 0.013(4) 0.007(4)
C48 0.071(5) 0.101(6) 0.072(6) 0.014(5) 0.015(4) 0.023(5)
C49 0.063(4) 0.085(5) 0.081(6) 0.005(4) 0.018(4) 0.010(3)
C50 0.069(4) 0.069(5) 0.080(6) 0.012(5) 0.032(4) 0.012(4)
C51 0.083(5) 0.052(4) 0.083(5) 0.005(4) 0.034(5) 0.007(4)
C52 0.067(5) 0.057(5) 0.100(6) -0.005(4) 0.022(5) 0.006(4)
C53 0.088(5) 0.055(4) 0.094(6) -0.007(4) 0.039(5) -0.021(4)
C54 0.077(5) 0.077(6) 0.109(7) -0.021(5) 0.043(5) -0.033(5)
C55 0.089(6) 0.083(6) 0.114(8) -0.008(6) 0.047(6) -0.022(5)
C56 0.097(6) 0.079(6) 0.094(7) 0.000(5) 0.048(6) -0.015(5)
C57 0.095(6) 0.086(6) 0.103(7) 0.012(6) 0.048(6) -0.008(5)
C58 0.112(7) 0.063(5) 0.098(6) 0.014(5) 0.051(6) 0.003(5)
C59 0.120(7) 0.063(5) 0.113(8) 0.023(5) 0.056(7) 0.021(5)
C60 0.106(6) 0.093(6) 0.076(6) 0.009(5) 0.041(5) 0.030(5)
C61 0.093(5) 0.078(6) 0.089(7) 0.010(5) 0.028(6) 0.026(5)
C62 0.090(6) 0.057(5) 0.100(7) 0.004(5) 0.037(5) 0.015(4)
C63 0.109(6) 0.051(4) 0.106(7) -0.007(5) 0.045(6) -0.008(4)
C64 0.117(7) 0.062(5) 0.100(7) 0.008(5) 0.051(7) -0.002(5)
C65 0.083(6) 0.092(7) 0.155(10) -0.009(7) 0.030(6) 0.016(5)
C66 0.131(8) 0.091(7) 0.147(10) -0.001(6) 0.049(7) 0.046(6)
C67 0.118(7) 0.073(6) 0.191(11) -0.003(7) 0.071(9) 0.020(5)
C68 0.113(7) 0.094(7) 0.129(8) -0.023(6) 0.027(6) 0.030(6)
C69 0.124(8) 0.103(7) 0.131(9) 0.009(7) 0.076(7) 0.031(6)
C70 0.087(6) 0.087(6) 0.162(9) -0.005(7) 0.054(7) 0.019(5)
C71 0.100(11) 0.101(12) 0.078(11) -0.029(10) -0.016(9) 0.040(9)
C71A 0.071(8) 0.048(8) 0.137(14) 0.019(9) 0.044(9) 0.019(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
F1 C4 1.397(7) . ?
F2 C5 1.391(7) . ?
F3 C6 1.409(6) . ?
F4 C7 1.402(6) . ?
F5 C8 1.370(6) . ?
F6 C9 1.406(6) . ?
F7 C10 1.387(6) . ?
F8 C11 1.420(7) . ?
C1 C1 1.356(11) 4_565 ?
C1 C2 1.383(8) . ?
C1 C9 1.487(8) . ?
C2 C3 1.387(8) . ?
C2 C7 1.444(8) . ?
C3 C3 1.406(11) 4_565 ?
C3 C4 1.458(8) . ?
C4 C5 1.565(8) . ?
C4 C31 1.595(8) . ?
C5 C23 1.492(8) . ?
C5 C6 1.670(8) . ?
C6 C30 1.483(9) . ?
C6 C7 1.546(8) . ?
C7 C8 1.605(8) . ?
C8 C11 1.543(9) . ?
C8 C9 1.615(9) . ?
C9 C10 1.549(9) . ?
C10 C13 1.489(9) . ?
C10 C10 1.664(12) 4_565 ?
C11 C12 1.532(9) . ?
C11 C29 1.537(9) . ?
C12 C13 1.348(8) . ?
C12 C28 1.465(9) . ?
C13 C14 1.439(8) . ?
C14 C15 1.399(13) . ?
C14 C13 1.439(8) 4_565 ?
C15 C16 1.438(8) 4_565 ?
C15 C16 1.438(8) . ?
C16 C28 1.398(9) . ?
C16 C17 1.435(8) . ?
C17 C18 1.405(8) . ?
C17 C17 1.423(12) 4_565 ?
C18 C26 1.430(9) . ?
C18 C19 1.460(8) . ?
C19 C19 1.395(12) 4_565 ?
C19 C20 1.432(9) . ?
C20 C21 1.403(9) . ?
C20 C25 1.433(9) . ?
C21 C22 1.407(8) . ?
C21 C21 1.439(12) 4_565 ?
C22 C23 1.361(8) . ?
C22 C32 1.532(8) . ?
C23 C24 1.435(8) . ?
C24 C25 1.371(9) . ?
C24 C30 1.414(9) . ?
C25 C26 1.455(9) . ?
C26 C27 1.395(9) . ?
C27 C28 1.432(9) . ?
C27 C29 1.438(9) . ?
C29 C30 1.352(9) . ?
C31 C32 1.535(11) . ?
C31 C33 1.578(12) . ?
C31 C4 1.595(7) 4_565 ?
C32 C22 1.532(8) 4_565 ?
C32 C34 1.561(12) . ?
C33 C50 1.543(8) 4_565 ?
C33 C50 1.543(8) . ?
C33 C34 1.616(12) . ?
C34 C35 1.532(8) 4_565 ?
C34 C35 1.532(8) . ?
C35 C52 1.358(9) . ?
C35 C36 1.444(8) . ?
C36 C37 1.390(8) . ?
C36 C36 1.457(12) 4_565 ?
C37 C54 1.437(9) . ?
C37 C38 1.459(9) . ?
C38 C38 1.401(14) 4_565 ?
C38 C39 1.431(10) . ?
C39 C40 1.375(10) . ?
C39 C55 1.450(10) . ?
C40 C41 1.441(10) . ?
C40 C40 1.456(15) 4_565 ?
C41 C57 1.385(10) . ?
C41 C42 1.461(10) . ?
C42 C43 1.364(14) . ?
C42 C41 1.461(10) 4_565 ?
C43 C44 1.444(9) 4_565 ?
C43 C44 1.444(9) . ?
C44 C58 1.385(10) . ?
C44 C45 1.449(10) . ?
C45 C46 1.388(9) . ?
C45 C45 1.458(14) 4_565 ?
C46 C60 1.445(10) . ?
C46 C47 1.445(9) . ?
C47 C47 1.381(14) 4_565 ?
C47 C48 1.453(9) . ?
C48 C49 1.354(9) . ?
C48 C61 1.466(10) . ?
C49 C50 1.449(9) . ?
C49 C49 1.478(13) 4_565 ?
C50 C51 1.349(8) . ?
C51 C62 1.464(9) . ?
C51 C52 1.474(9) . ?
C52 C53 1.469(9) . ?
C53 C54 1.381(9) . ?
C53 C63 1.433(10) . ?
C54 C55 1.438(10) . ?
C55 C56 1.373(10) . ?
C56 C57 1.431(10) . ?
C56 C64 1.448(10) . ?
C57 C58 1.438(10) . ?
C58 C59 1.453(10) . ?
C59 C60 1.398(10) . ?
C59 C64 1.446(10) . ?
C60 C61 1.441(9) . ?
C61 C62 1.391(9) . ?
C62 C63 1.467(10) . ?
C63 C64 1.390(10) . ?
C65 C66 1.3900 . ?
C65 C70 1.3900 . ?
C65 C71 1.4208 . ?
C66 C67 1.3900 . ?
C67 C68 1.3900 . ?
C68 C69 1.3900 . ?
C69 C71A 1.3471 . ?
C69 C70 1.3900 . ?
C72 C72 1.46(3) 3_657 ?
C72 C73 1.51(2) . ?
C73 C74 1.52(4) . ?
C74 C75 1.49(4) . ?
C75 C76 1.48(3) . ?
C76 C77 1.37(2) . ?
C77 C77 1.31(3) 4_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 C2 121.2(4) 4_565 . ?
C1 C1 C9 126.5(4) 4_565 . ?
C2 C1 C9 112.1(5) . . ?
C1 C2 C3 118.9(6) . . ?
C1 C2 C7 115.0(6) . . ?
C3 C2 C7 126.0(6) . . ?
C2 C3 C3 119.9(4) . 4_565 ?
C2 C3 C4 128.0(6) . . ?
C3 C3 C4 112.0(3) 4_565 . ?
F1 C4 C3 107.1(5) . . ?
F1 C4 C5 107.2(5) . . ?
C3 C4 C5 106.8(5) . . ?
F1 C4 C31 109.1(6) . . ?
C3 C4 C31 103.6(5) . . ?
C5 C4 C31 122.2(5) . . ?
F2 C5 C23 110.7(5) . . ?
F2 C5 C4 108.2(5) . . ?
C23 C5 C4 110.5(5) . . ?
F2 C5 C6 106.9(5) . . ?
C23 C5 C6 101.8(5) . . ?
C4 C5 C6 118.4(5) . . ?
F3 C6 C30 110.4(5) . . ?
F3 C6 C7 106.9(5) . . ?
C30 C6 C7 111.2(6) . . ?
F3 C6 C5 106.8(5) . . ?
C30 C6 C5 103.7(5) . . ?
C7 C6 C5 117.7(5) . . ?
F4 C7 C2 108.5(5) . . ?
F4 C7 C6 108.6(5) . . ?
C2 C7 C6 108.5(5) . . ?
F4 C7 C8 106.0(5) . . ?
C2 C7 C8 101.9(5) . . ?
C6 C7 C8 122.5(6) . . ?
F5 C8 C11 107.3(5) . . ?
F5 C8 C7 108.4(5) . . ?
C11 C8 C7 114.5(5) . . ?
F5 C8 C9 108.1(5) . . ?
C11 C8 C9 113.6(6) . . ?
C7 C8 C9 104.8(5) . . ?
F6 C9 C1 108.6(5) . . ?
F6 C9 C10 107.7(5) . . ?
C1 C9 C10 108.4(5) . . ?
F6 C9 C8 106.6(5) . . ?
C1 C9 C8 101.4(5) . . ?
C10 C9 C8 123.5(6) . . ?
F7 C10 C13 110.1(5) . . ?
F7 C10 C9 107.7(5) . . ?
C13 C10 C9 110.2(5) . . ?
F7 C10 C10 107.1(3) . 4_565 ?
C13 C10 C10 103.5(4) . 4_565 ?
C9 C10 C10 118.1(4) . 4_565 ?
F8 C11 C12 107.3(5) . . ?
F8 C11 C29 108.0(5) . . ?
C12 C11 C29 101.0(6) . . ?
F8 C11 C8 108.0(5) . . ?
C12 C11 C8 116.3(6) . . ?
C29 C11 C8 115.7(6) . . ?
C13 C12 C28 119.9(7) . . ?
C13 C12 C11 125.8(7) . . ?
C28 C12 C11 108.2(6) . . ?
C12 C13 C14 120.2(6) . . ?
C12 C13 C10 125.5(7) . . ?
C14 C13 C10 110.4(7) . . ?
C15 C14 C13 120.6(5) . 4_565 ?
C15 C14 C13 120.6(5) . . ?
C13 C14 C13 110.1(9) 4_565 . ?
C14 C15 C16 120.0(5) . 4_565 ?
C14 C15 C16 120.0(5) . . ?
C16 C15 C16 107.7(9) 4_565 . ?
C28 C16 C17 119.8(6) . . ?
C28 C16 C15 118.3(6) . . ?
C17 C16 C15 107.8(7) . . ?
C18 C17 C17 120.1(4) . 4_565 ?
C18 C17 C16 119.4(6) . . ?
C17 C17 C16 108.3(4) 4_565 . ?
C17 C18 C26 119.8(6) . . ?
C17 C18 C19 120.5(6) . . ?
C26 C18 C19 107.1(6) . . ?
C19 C19 C20 119.9(4) 4_565 . ?
C19 C19 C18 119.4(4) 4_565 . ?
C20 C19 C18 107.9(6) . . ?
C21 C20 C19 120.6(7) . . ?
C21 C20 C25 117.4(6) . . ?
C19 C20 C25 109.0(6) . . ?
C20 C21 C22 121.9(6) . . ?
C20 C21 C21 119.5(4) . 4_565 ?
C22 C21 C21 108.4(4) . 4_565 ?
C23 C22 C21 120.1(6) . . ?
C23 C22 C32 124.9(6) . . ?
C21 C22 C32 109.9(6) . . ?
C22 C23 C24 119.2(6) . . ?
C22 C23 C5 125.2(6) . . ?
C24 C23 C5 111.7(6) . . ?
C25 C24 C30 121.4(7) . . ?
C25 C24 C23 121.0(6) . . ?
C30 C24 C23 109.4(6) . . ?
C24 C25 C20 120.1(7) . . ?
C24 C25 C26 120.1(6) . . ?
C20 C25 C26 107.0(7) . . ?
C27 C26 C18 121.3(7) . . ?
C27 C26 C25 117.1(7) . . ?
C18 C26 C25 109.0(6) . . ?
C26 C27 C28 118.5(7) . . ?
C26 C27 C29 121.3(6) . . ?
C28 C27 C29 109.2(6) . . ?
C16 C28 C27 121.2(7) . . ?
C16 C28 C12 120.7(6) . . ?
C27 C28 C12 108.4(7) . . ?
C30 C29 C27 120.0(6) . . ?
C30 C29 C11 125.9(7) . . ?
C27 C29 C11 108.7(7) . . ?
C29 C30 C24 120.0(7) . . ?
C29 C30 C6 124.7(6) . . ?
C24 C30 C6 111.4(7) . . ?
C32 C31 C33 91.5(6) . . ?
C32 C31 C4 114.7(5) . . ?
C33 C31 C4 116.7(5) . . ?
C32 C31 C4 114.7(5) . 4_565 ?
C33 C31 C4 116.7(5) . 4_565 ?
C4 C31 C4 103.1(6) . 4_565 ?
C22 C32 C22 98.8(8) 4_565 . ?
C22 C32 C31 116.7(5) 4_565 . ?
C22 C32 C31 116.7(5) . . ?
C22 C32 C34 117.4(5) 4_565 . ?
C22 C32 C34 117.4(5) . . ?
C31 C32 C34 91.5(7) . . ?
C50 C33 C50 103.0(8) 4_565 . ?
C50 C33 C31 119.6(4) 4_565 . ?
C50 C33 C31 119.6(4) . . ?
C50 C33 C34 113.3(5) 4_565 . ?
C50 C33 C34 113.3(5) . . ?
C31 C33 C34 87.9(6) . . ?
C35 C34 C35 102.8(7) 4_565 . ?
C35 C34 C32 116.9(5) 4_565 . ?
C35 C34 C32 116.9(5) . . ?
C35 C34 C33 115.9(5) 4_565 . ?
C35 C34 C33 115.9(5) . . ?
C32 C34 C33 89.1(6) . . ?
C52 C35 C36 119.5(6) . . ?
C52 C35 C34 123.0(6) . . ?
C36 C35 C34 108.8(6) . . ?
C37 C36 C35 121.3(6) . . ?
C37 C36 C36 119.6(4) . 4_565 ?
C35 C36 C36 109.0(4) . 4_565 ?
C36 C37 C54 119.2(6) . . ?
C36 C37 C38 121.1(7) . . ?
C54 C37 C38 107.2(7) . . ?
C38 C38 C39 120.1(5) 4_565 . ?
C38 C38 C37 119.3(4) 4_565 . ?
C39 C38 C37 108.6(7) . . ?
C40 C39 C38 119.7(9) . . ?
C40 C39 C55 120.7(9) . . ?
C38 C39 C55 107.6(8) . . ?
C39 C40 C41 120.1(8) . . ?
C39 C40 C40 120.2(5) . 4_565 ?
C41 C40 C40 107.9(5) . 4_565 ?
C57 C41 C40 119.3(8) . . ?
C57 C41 C42 119.5(8) . . ?
C40 C41 C42 108.7(9) . . ?
C43 C42 C41 121.2(6) . . ?
C43 C42 C41 121.2(6) . 4_565 ?
C41 C42 C41 106.7(12) . 4_565 ?
C42 C43 C44 119.1(6) . 4_565 ?
C42 C43 C44 119.1(6) . . ?
C44 C43 C44 109.2(11) 4_565 . ?
C58 C44 C43 120.2(8) . . ?
C58 C44 C45 120.4(8) . . ?
C43 C44 C45 107.4(9) . . ?
C46 C45 C44 120.7(7) . . ?
C46 C45 C45 119.6(5) . 4_565 ?
C44 C45 C45 108.0(5) . 4_565 ?
C45 C46 C60 119.0(7) . . ?
C45 C46 C47 120.3(8) . . ?
C60 C46 C47 107.3(7) . . ?
C47 C47 C46 120.1(5) 4_565 . ?
C47 C47 C48 118.8(5) 4_565 . ?
C46 C47 C48 109.4(7) . . ?
C49 C48 C47 122.4(8) . . ?
C49 C48 C61 119.9(7) . . ?
C47 C48 C61 106.2(7) . . ?
C48 C49 C50 121.8(7) . . ?
C48 C49 C49 118.8(5) . 4_565 ?
C50 C49 C49 108.8(4) . 4_565 ?
C51 C50 C49 120.1(6) . . ?
C51 C50 C33 123.3(7) . . ?
C49 C50 C33 108.4(7) . . ?
C50 C51 C62 118.6(7) . . ?
C50 C51 C52 122.6(7) . . ?
C62 C51 C52 107.8(7) . . ?
C35 C52 C53 119.7(6) . . ?
C35 C52 C51 120.7(6) . . ?
C53 C52 C51 107.7(7) . . ?
C54 C53 C63 120.9(7) . . ?
C54 C53 C52 120.4(7) . . ?
C63 C53 C52 107.8(7) . . ?
C53 C54 C37 119.7(7) . . ?
C53 C54 C55 119.7(8) . . ?
C37 C54 C55 108.5(7) . . ?
C56 C55 C54 120.2(8) . . ?
C56 C55 C39 118.5(9) . . ?
C54 C55 C39 108.2(8) . . ?
C55 C56 C57 121.3(8) . . ?
C55 C56 C64 119.9(8) . . ?
C57 C56 C64 107.0(9) . . ?
C41 C57 C56 120.0(9) . . ?
C41 C57 C58 119.1(8) . . ?
C56 C57 C58 109.3(8) . . ?
C44 C58 C57 120.9(8) . . ?
C44 C58 C59 119.5(8) . . ?
C57 C58 C59 107.9(8) . . ?
C60 C59 C64 121.8(8) . . ?
C60 C59 C58 119.6(9) . . ?
C64 C59 C58 106.9(8) . . ?
C59 C60 C61 118.7(8) . . ?
C59 C60 C46 120.9(8) . . ?
C61 C60 C46 108.6(8) . . ?
C62 C61 C60 120.7(8) . . ?
C62 C61 C48 117.3(7) . . ?
C60 C61 C48 108.4(8) . . ?
C61 C62 C51 122.0(7) . . ?
C61 C62 C63 119.9(8) . . ?
C51 C62 C63 107.1(7) . . ?
C64 C63 C53 119.1(8) . . ?
C64 C63 C62 119.8(8) . . ?
C53 C63 C62 109.5(7) . . ?
C63 C64 C59 119.1(8) . . ?
C63 C64 C56 120.2(9) . . ?
C59 C64 C56 109.0(8) . . ?
C66 C65 C70 120.0 . . ?
C66 C65 C71 118.6 . . ?
C70 C65 C71 121.4 . . ?
C65 C66 C67 120.0 . . ?
C66 C67 C68 120.0 . . ?
C67 C68 C69 120.0 . . ?
C71A C69 C68 120.2 . . ?
C71A C69 C70 119.4 . . ?
C68 C69 C70 120.0 . . ?
C69 C70 C65 120.0 . . ?
C72 C72 C73 129(2) 3_657 . ?
C72 C73 C74 101.9(19) . . ?
C75 C74 C73 165(3) . . ?
C76 C75 C74 135(3) . . ?
C77 C76 C75 94(2) . . ?
C77 C77 C76 157.1(13) 4_565 . ?

_diffrn_measured_fraction_theta_max 0.513
_diffrn_reflns_theta_full        33.55
_diffrn_measured_fraction_theta_full 0.513
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.078