# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Fabio Marchetti'
_publ_contact_author_email       fabmar@dcci.unipi.it
loop_
_publ_author_name
F.Marchetti
G.Pampaloni
S.Zacchini
N.Guazzelli
M.Bortoluzzi

# Attachment '- 3eB.CIF'

data_p-1
_database_code_depnum_ccdc_archive 'CCDC 876459'
#TrackingRef '- 3eB.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H37 F9 Nb3 O6'
_chemical_formula_weight         1051.42

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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5980(18)
_cell_length_b                   11.661(2)
_cell_length_c                   18.367(3)
_cell_angle_alpha                83.930(2)
_cell_angle_beta                 75.313(2)
_cell_angle_gamma                86.150(2)
_cell_volume                     1975.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1677
_cell_measurement_theta_min      2.188
_cell_measurement_theta_max      19.836

_exptl_crystal_description       plate
_exptl_crystal_colour            orange-yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1046
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8485
_exptl_absorpt_correction_T_max  0.9033
_exptl_absorpt_process_details   
;
Data were corrected for Lorentz polarization and absorption
effects (empirical absorption correction SADABS).
R(int) = 0.0859 (selected reflections only, before parameter refinement)
R(int) = 0.0528 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18800
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_av_sigmaI/netI    0.1483
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.03
_reflns_number_total             6969
_reflns_number_gt                3643
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_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. The following restraints
were applied (given as SHELXL lines):
SIMU .01 $C
SADI .01 O1 C11 O1 C11' O6 C61 O6 C61'
phenyl rings have been fixed with AFIX 66
DFIX 1.53 .01 C101 C102 C102 C103 C103 C104 C104 C105 C105 C106
dfix 2.56 .01 c101 c103 c102 c104 c103 c105 c104 c106
SAME C106 < C101
SIMU .01 C101 > C106
;

_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^)+(0.0661P)^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         6969
_refine_ls_number_parameters     573
_refine_ls_number_restraints     492
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1550
_refine_ls_wR_factor_gt          0.1219
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.957
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.63711(8) 0.37598(7) 0.21799(5) 0.0313(2) Uani 1 1 d . A .
Nb2 Nb 0.40961(8) 0.18950(7) 0.40466(5) 0.0312(2) Uani 1 1 d . . .
Nb3 Nb 0.35491(9) 0.14271(7) 0.19852(5) 0.0391(3) Uani 1 1 d . B .
F1 F 0.5293(5) 0.3092(4) 0.3250(3) 0.0347(12) Uani 1 1 d . . .
F2 F 0.3310(5) 0.1644(4) 0.3115(3) 0.0367(12) Uani 1 1 d . . .
F3 F 0.5162(5) 0.2584(4) 0.1864(3) 0.0436(14) Uani 1 1 d . . .
F4 F 0.4683(5) 0.4691(4) 0.2253(3) 0.0407(13) Uani 1 1 d . . .
F5 F 0.7607(5) 0.2458(4) 0.2257(3) 0.0585(16) Uani 1 1 d . . .
F6 F 0.2724(5) 0.3155(4) 0.4151(3) 0.0361(12) Uani 1 1 d . . .
F7 F 0.5575(5) 0.0874(4) 0.3585(3) 0.0384(13) Uani 1 1 d . . .
F8 F 0.2358(6) 0.2781(4) 0.2041(3) 0.0559(16) Uani 1 1 d . . .
F9 F 0.5010(6) 0.0349(4) 0.2129(3) 0.0576(16) Uani 1 1 d . . .
O1 O 0.7168(6) 0.4165(5) 0.1191(3) 0.0472(18) Uani 1 1 d D . .
O2 O 0.7356(6) 0.4692(5) 0.2603(3) 0.0386(16) Uani 1 1 d . . .
O3 O 0.4930(6) 0.2280(5) 0.4774(3) 0.0369(15) Uani 1 1 d . . .
O4 O 0.2921(6) 0.0783(5) 0.4597(3) 0.0378(15) Uani 1 1 d . . .
O5 O 0.2112(7) 0.0415(5) 0.2211(4) 0.0530(19) Uani 1 1 d . . .
O6 O 0.3923(7) 0.1489(5) 0.0956(4) 0.057(2) Uani 1 1 d D . .
C11 C 0.7494(17) 0.4196(14) 0.0419(4) 0.066(3) Uani 0.496(8) 1 d PGDU A 1
C12 C 0.8466(18) 0.3309(12) 0.0147(7) 0.076(4) Uani 0.496(8) 1 d PGU A 1
H12 H 0.8800 0.2757 0.0490 0.091 Uiso 0.496(8) 1 calc PR A 1
C13 C 0.8948(16) 0.3229(12) -0.0627(8) 0.086(4) Uani 0.496(8) 1 d PGU A 1
H13 H 0.9612 0.2623 -0.0813 0.103 Uiso 0.496(8) 1 calc PR A 1
C14 C 0.8459(18) 0.4036(15) -0.1129(5) 0.087(4) Uani 0.496(8) 1 d PGU A 1
H14 H 0.8789 0.3981 -0.1658 0.104 Uiso 0.496(8) 1 calc PR A 1
C15 C 0.7487(18) 0.4923(12) -0.0857(7) 0.082(4) Uani 0.496(8) 1 d PGU A 1
H15 H 0.7153 0.5474 -0.1200 0.098 Uiso 0.496(8) 1 calc PR A 1
C16 C 0.7005(16) 0.5003(12) -0.0083(8) 0.072(3) Uani 0.496(8) 1 d PGU A 1
H16 H 0.6341 0.5609 0.0103 0.087 Uiso 0.496(8) 1 calc PR A 1
C11' C 0.7619(17) 0.4107(13) 0.0424(4) 0.066(3) Uani 0.504(8) 1 d PGDU A 2
C12' C 0.8998(14) 0.4240(13) -0.0041(7) 0.077(3) Uani 0.504(8) 1 d PGU A 2
H12' H 0.9799 0.4240 0.0174 0.092 Uiso 0.504(8) 1 calc PR A 2
C13' C 0.9205(14) 0.4372(13) -0.0822(7) 0.081(4) Uani 0.504(8) 1 d PGU A 2
H13' H 1.0147 0.4463 -0.1140 0.097 Uiso 0.504(8) 1 calc PR A 2
C14' C 0.8033(19) 0.4371(13) -0.1138(4) 0.085(4) Uani 0.504(8) 1 d PGU A 2
H14' H 0.8175 0.4461 -0.1671 0.102 Uiso 0.504(8) 1 calc PR A 2
C15' C 0.6654(16) 0.4238(13) -0.0673(8) 0.083(4) Uani 0.504(8) 1 d PGU A 2
H15' H 0.5853 0.4237 -0.0888 0.099 Uiso 0.504(8) 1 calc PR A 2
C16' C 0.6447(13) 0.4106(13) 0.0108(7) 0.074(4) Uani 0.504(8) 1 d PGU A 2
H16' H 0.5504 0.4015 0.0426 0.089 Uiso 0.504(8) 1 calc PR A 2
C21 C 0.8269(9) 0.4908(7) 0.3048(5) 0.0282(19) Uani 1 1 d U A .
C22 C 0.9680(9) 0.4458(7) 0.2880(5) 0.0299(19) Uani 1 1 d U . .
H22 H 1.0032 0.4006 0.2465 0.036 Uiso 1 1 calc R A .
C23 C 1.0556(9) 0.4686(7) 0.3336(5) 0.037(2) Uani 1 1 d U A .
H23 H 1.1521 0.4381 0.3235 0.044 Uiso 1 1 calc R . .
C24 C 1.0049(9) 0.5350(7) 0.3935(5) 0.037(2) Uani 1 1 d U . .
H24 H 1.0670 0.5521 0.4234 0.044 Uiso 1 1 calc R A .
C25 C 0.8641(10) 0.5761(7) 0.4096(5) 0.039(2) Uani 1 1 d U A .
H25 H 0.8283 0.6185 0.4524 0.047 Uiso 1 1 calc R . .
C26 C 0.7732(9) 0.5573(7) 0.3648(5) 0.035(2) Uani 1 1 d U . .
H26 H 0.6772 0.5890 0.3748 0.041 Uiso 1 1 calc R A .
C31 C 0.5307(8) 0.2616(7) 0.5399(5) 0.0253(18) Uani 1 1 d U . .
C32 C 0.5936(8) 0.3657(7) 0.5334(5) 0.034(2) Uani 1 1 d U . .
H32 H 0.6135 0.4130 0.4868 0.041 Uiso 1 1 calc R . .
C33 C 0.6269(9) 0.3994(8) 0.5964(6) 0.039(2) Uani 1 1 d U . .
H33 H 0.6691 0.4716 0.5938 0.047 Uiso 1 1 calc R . .
C34 C 0.5994(9) 0.3294(8) 0.6631(6) 0.041(2) Uani 1 1 d U . .
H34 H 0.6214 0.3535 0.7066 0.050 Uiso 1 1 calc R . .
C35 C 0.5396(9) 0.2240(8) 0.6665(5) 0.039(2) Uani 1 1 d U . .
H35 H 0.5239 0.1747 0.7121 0.047 Uiso 1 1 calc R . .
C36 C 0.5028(9) 0.1894(7) 0.6055(5) 0.0294(19) Uani 1 1 d U . .
H36 H 0.4593 0.1177 0.6083 0.035 Uiso 1 1 calc R . .
C41 C 0.2108(8) -0.0205(7) 0.4848(5) 0.035(2) Uani 1 1 d U . .
C42 C 0.1560(9) -0.0686(7) 0.4344(5) 0.035(2) Uani 1 1 d U . .
H42 H 0.1703 -0.0364 0.3834 0.043 Uiso 1 1 calc R . .
C43 C 0.0786(9) -0.1666(8) 0.4606(6) 0.043(2) Uani 1 1 d U . .
H43 H 0.0383 -0.2023 0.4270 0.052 Uiso 1 1 calc R . .
C44 C 0.0585(10) -0.2137(8) 0.5337(6) 0.045(2) Uani 1 1 d U . .
H44 H 0.0059 -0.2818 0.5499 0.054 Uiso 1 1 calc R . .
C45 C 0.1132(10) -0.1635(8) 0.5833(6) 0.047(2) Uani 1 1 d U . .
H45 H 0.0992 -0.1960 0.6342 0.056 Uiso 1 1 calc R . .
C46 C 0.1897(9) -0.0644(8) 0.5587(5) 0.040(2) Uani 1 1 d U . .
H46 H 0.2273 -0.0272 0.5928 0.048 Uiso 1 1 calc R . .
C51 C 0.0937(10) -0.0266(8) 0.2329(5) 0.040(2) Uani 1 1 d U . .
C52 C 0.1116(10) -0.1425(8) 0.2457(6) 0.047(2) Uani 1 1 d U . .
H52 H 0.2034 -0.1774 0.2469 0.057 Uiso 1 1 calc R . .
C53 C -0.0098(10) -0.2094(8) 0.2570(6) 0.051(2) Uani 1 1 d U . .
H53 H 0.0005 -0.2910 0.2656 0.061 Uiso 1 1 calc R . .
C54 C -0.1400(11) -0.1603(9) 0.2561(6) 0.055(2) Uani 1 1 d U . .
H54 H -0.2217 -0.2064 0.2655 0.066 Uiso 1 1 calc R . .
C55 C -0.1535(11) -0.0443(9) 0.2415(6) 0.061(3) Uani 1 1 d U . .
H55 H -0.2449 -0.0101 0.2386 0.074 Uiso 1 1 calc R . .
C56 C -0.0383(10) 0.0256(8) 0.2307(6) 0.050(2) Uani 1 1 d U . .
H56 H -0.0496 0.1071 0.2221 0.060 Uiso 1 1 calc R . .
C61 C 0.386(2) 0.1918(15) 0.0235(6) 0.074(3) Uani 0.459(10) 1 d PGDU B 1
C62 C 0.4854(19) 0.1483(14) -0.0373(10) 0.081(3) Uani 0.459(10) 1 d PGU B 1
H62 H 0.5613 0.0962 -0.0286 0.097 Uiso 0.459(10) 1 calc PR B 1
C63 C 0.4743(19) 0.1811(16) -0.1106(7) 0.082(4) Uani 0.459(10) 1 d PGU B 1
H63 H 0.5426 0.1515 -0.1522 0.098 Uiso 0.459(10) 1 calc PR B 1
C64 C 0.363(2) 0.2574(15) -0.1233(6) 0.084(3) Uani 0.459(10) 1 d PGU B 1
H64 H 0.3558 0.2798 -0.1734 0.101 Uiso 0.459(10) 1 calc PR B 1
C65 C 0.2636(19) 0.3008(15) -0.0625(10) 0.082(4) Uani 0.459(10) 1 d PGU B 1
H65 H 0.1878 0.3529 -0.0711 0.098 Uiso 0.459(10) 1 calc PR B 1
C66 C 0.2747(19) 0.2680(16) 0.0109(7) 0.076(4) Uani 0.459(10) 1 d PGU B 1
H66 H 0.2064 0.2977 0.0524 0.091 Uiso 0.459(10) 1 calc PR B 1
C61' C 0.3878(18) 0.1814(11) 0.0216(5) 0.073(3) Uani 0.541(10) 1 d PGDU B 2
C62' C 0.5089(14) 0.2200(13) -0.0325(8) 0.078(3) Uani 0.541(10) 1 d PGU B 2
H62' H 0.5990 0.2197 -0.0198 0.094 Uiso 0.541(10) 1 calc PR B 2
C63' C 0.4984(16) 0.2590(13) -0.1052(6) 0.081(3) Uani 0.541(10) 1 d PGU B 2
H63' H 0.5812 0.2854 -0.1421 0.097 Uiso 0.541(10) 1 calc PR B 2
C64' C 0.3667(19) 0.2595(12) -0.1237(5) 0.084(3) Uani 0.541(10) 1 d PGU B 2
H64' H 0.3594 0.2862 -0.1734 0.101 Uiso 0.541(10) 1 calc PR B 2
C65' C 0.2455(15) 0.2209(14) -0.0696(8) 0.084(4) Uani 0.541(10) 1 d PGU B 2
H65' H 0.1554 0.2212 -0.0823 0.101 Uiso 0.541(10) 1 calc PR B 2
C66' C 0.2560(15) 0.1819(13) 0.0030(7) 0.077(4) Uani 0.541(10) 1 d PGU B 2
H66' H 0.1732 0.1555 0.0400 0.092 Uiso 0.541(10) 1 calc PR B 2
C101 C 0.841(4) 0.127(3) 0.051(2) 0.185(15) Uiso 0.50 1 d PDU C -1
H10A H 0.7622 0.1850 0.0652 0.278 Uiso 0.50 1 calc PR C -1
H10B H 0.9290 0.1536 0.0605 0.278 Uiso 0.50 1 calc PR C -1
H10C H 0.8148 0.0540 0.0820 0.278 Uiso 0.50 1 calc PR C -1
C102 C 0.866(5) 0.109(4) -0.033(2) 0.267(16) Uiso 0.50 1 d PDU C -1
H10D H 0.7727 0.0947 -0.0433 0.320 Uiso 0.50 1 calc PR C -1
H10E H 0.9032 0.1804 -0.0637 0.320 Uiso 0.50 1 calc PR C -1
C103 C 0.972(5) 0.008(4) -0.057(2) 0.293(17) Uiso 0.50 1 d PDU C -1
H10F H 0.9188 -0.0639 -0.0483 0.352 Uiso 0.50 1 calc PR C -1
H10G H 1.0178 0.0211 -0.1116 0.352 Uiso 0.50 1 calc PR C -1
C104 C 1.091(6) -0.008(5) -0.0139(19) 0.335(18) Uiso 0.50 1 d PDU C -1
H10H H 1.0760 -0.0810 0.0197 0.402 Uiso 0.50 1 calc PR C -1
H10I H 1.0819 0.0560 0.0183 0.402 Uiso 0.50 1 calc PR C -1
C105 C 1.243(5) -0.012(6) -0.066(3) 0.367(19) Uiso 0.50 1 d PDU C -1
H10J H 1.2826 0.0653 -0.0733 0.440 Uiso 0.50 1 calc PR C -1
H10K H 1.2378 -0.0336 -0.1160 0.440 Uiso 0.50 1 calc PR C -1
C106 C 1.346(5) -0.100(6) -0.034(4) 0.45(3) Uiso 0.50 1 d PDU C -1
H10L H 1.4168 -0.0581 -0.0183 0.672 Uiso 0.50 1 calc PR C -1
H10M H 1.3963 -0.1492 -0.0737 0.672 Uiso 0.50 1 calc PR C -1
H10N H 1.2905 -0.1476 0.0090 0.672 Uiso 0.50 1 calc PR C -1

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
Nb1 0.0263(5) 0.0288(5) 0.0401(6) -0.0031(4) -0.0092(4) -0.0073(4)
Nb2 0.0228(5) 0.0314(5) 0.0407(6) 0.0014(4) -0.0111(4) -0.0050(4)
Nb3 0.0352(5) 0.0362(5) 0.0527(6) -0.0091(4) -0.0196(5) -0.0084(4)
F1 0.028(3) 0.039(3) 0.039(3) -0.002(2) -0.009(2) -0.008(2)
F2 0.025(3) 0.039(3) 0.050(3) -0.001(2) -0.015(2) -0.006(2)
F3 0.042(3) 0.043(3) 0.048(4) -0.016(3) -0.007(3) -0.016(3)
F4 0.040(3) 0.031(3) 0.058(4) -0.007(3) -0.025(3) 0.005(2)
F5 0.034(3) 0.047(3) 0.088(5) -0.002(3) -0.007(3) 0.007(3)
F6 0.027(3) 0.031(3) 0.051(3) -0.001(2) -0.013(2) 0.001(2)
F7 0.028(3) 0.037(3) 0.050(3) -0.004(2) -0.009(2) 0.004(2)
F8 0.055(4) 0.053(4) 0.066(4) -0.006(3) -0.030(3) 0.012(3)
F9 0.057(4) 0.038(3) 0.085(5) -0.017(3) -0.029(3) 0.006(3)
O1 0.045(4) 0.058(4) 0.040(4) -0.007(3) -0.006(3) -0.020(3)
O2 0.036(4) 0.034(3) 0.054(4) 0.000(3) -0.025(3) -0.012(3)
O3 0.024(3) 0.050(4) 0.039(4) -0.006(3) -0.012(3) 0.002(3)
O4 0.026(3) 0.041(4) 0.043(4) 0.007(3) -0.005(3) -0.007(3)
O5 0.052(4) 0.059(4) 0.058(5) -0.003(4) -0.024(4) -0.030(4)
O6 0.062(5) 0.054(4) 0.063(5) -0.013(4) -0.025(4) -0.012(4)
C11 0.083(7) 0.062(6) 0.056(6) -0.004(5) -0.017(5) -0.037(6)
C12 0.093(8) 0.072(7) 0.060(7) -0.006(6) -0.009(6) -0.030(6)
C13 0.103(8) 0.082(7) 0.064(7) -0.005(6) -0.002(6) -0.026(7)
C14 0.109(8) 0.084(7) 0.062(7) -0.003(6) -0.007(6) -0.029(7)
C15 0.107(8) 0.077(7) 0.062(7) -0.002(6) -0.014(6) -0.035(7)
C16 0.095(7) 0.069(7) 0.056(6) -0.004(6) -0.018(6) -0.036(6)
C11' 0.084(7) 0.062(6) 0.056(6) -0.004(5) -0.017(5) -0.037(6)
C12' 0.094(7) 0.072(7) 0.062(6) -0.003(6) -0.008(6) -0.032(6)
C13' 0.101(8) 0.081(7) 0.058(7) -0.003(6) -0.008(6) -0.033(7)
C14' 0.105(8) 0.083(7) 0.061(7) -0.005(6) -0.008(6) -0.029(7)
C15' 0.103(8) 0.082(7) 0.064(7) -0.001(6) -0.016(6) -0.036(6)
C16' 0.093(8) 0.074(7) 0.059(6) -0.003(6) -0.019(6) -0.036(6)
C21 0.026(4) 0.024(4) 0.035(5) 0.008(4) -0.012(4) -0.008(3)
C22 0.030(4) 0.026(4) 0.035(5) 0.001(4) -0.009(4) -0.004(4)
C23 0.025(4) 0.038(4) 0.046(5) 0.008(4) -0.010(4) -0.001(4)
C24 0.026(4) 0.044(5) 0.042(5) -0.001(4) -0.012(4) -0.006(4)
C25 0.036(5) 0.040(5) 0.041(5) -0.007(4) -0.005(4) -0.010(4)
C26 0.027(4) 0.028(4) 0.048(5) -0.006(4) -0.008(4) -0.001(4)
C31 0.014(4) 0.029(4) 0.036(5) -0.001(4) -0.012(3) -0.002(3)
C32 0.019(4) 0.027(4) 0.056(5) 0.005(4) -0.011(4) -0.004(3)
C33 0.019(4) 0.033(4) 0.070(6) -0.013(4) -0.016(4) -0.001(4)
C34 0.029(4) 0.044(5) 0.058(5) -0.020(4) -0.021(4) 0.008(4)
C35 0.025(4) 0.043(5) 0.048(5) 0.000(4) -0.011(4) 0.014(4)
C36 0.025(4) 0.026(4) 0.039(5) 0.004(4) -0.012(4) -0.003(3)
C41 0.014(4) 0.037(5) 0.052(5) 0.007(4) -0.009(4) 0.002(4)
C42 0.022(4) 0.043(5) 0.041(5) -0.002(4) -0.009(4) 0.002(4)
C43 0.023(4) 0.042(5) 0.063(5) -0.011(4) -0.006(4) 0.001(4)
C44 0.030(5) 0.034(5) 0.063(6) 0.006(4) -0.001(4) 0.002(4)
C45 0.036(5) 0.041(5) 0.057(6) 0.012(4) -0.007(4) 0.006(4)
C46 0.023(4) 0.044(5) 0.053(5) 0.004(4) -0.012(4) 0.006(4)
C51 0.028(4) 0.036(4) 0.059(5) -0.006(4) -0.017(4) -0.003(4)
C52 0.032(5) 0.043(5) 0.066(5) -0.004(4) -0.013(4) 0.004(4)
C53 0.040(5) 0.043(5) 0.068(6) -0.004(5) -0.010(5) -0.004(4)
C54 0.033(5) 0.056(5) 0.080(6) -0.011(5) -0.017(5) -0.012(4)
C55 0.031(5) 0.062(5) 0.091(6) -0.001(5) -0.019(5) 0.005(5)
C56 0.035(5) 0.032(5) 0.080(6) -0.005(4) -0.010(5) 0.005(4)
C61 0.098(7) 0.074(7) 0.057(6) -0.016(6) -0.024(6) -0.021(6)
C62 0.106(7) 0.080(7) 0.061(6) -0.015(6) -0.024(6) -0.017(6)
C63 0.109(7) 0.083(7) 0.058(6) -0.012(6) -0.024(6) -0.014(6)
C64 0.108(7) 0.088(7) 0.061(6) -0.011(6) -0.026(6) -0.014(6)
C65 0.107(8) 0.083(7) 0.062(7) -0.011(7) -0.026(6) -0.015(7)
C66 0.102(8) 0.077(7) 0.058(6) -0.016(6) -0.027(6) -0.017(7)
C61' 0.097(7) 0.072(7) 0.056(6) -0.016(6) -0.024(6) -0.020(6)
C62' 0.103(7) 0.079(7) 0.059(6) -0.016(6) -0.023(6) -0.023(6)
C63' 0.106(7) 0.083(7) 0.060(6) -0.013(6) -0.024(6) -0.019(6)
C64' 0.108(7) 0.088(7) 0.062(6) -0.011(6) -0.026(6) -0.014(6)
C65' 0.108(8) 0.090(7) 0.063(6) -0.012(6) -0.029(6) -0.016(7)
C66' 0.103(8) 0.082(7) 0.056(6) -0.016(6) -0.030(6) -0.022(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
Nb1 O1 1.808(6) . ?
Nb1 O2 1.835(5) . ?
Nb1 F4 1.873(5) . ?
Nb1 F5 1.879(5) . ?
Nb1 F3 2.071(4) . ?
Nb1 F1 2.073(5) . ?
Nb2 O4 1.822(5) . ?
Nb2 O3 1.829(5) . ?
Nb2 F7 1.878(5) . ?
Nb2 F6 1.898(4) . ?
Nb2 F1 2.083(4) . ?
Nb2 F2 2.091(4) . ?
Nb3 O5 1.815(6) . ?
Nb3 O6 1.827(6) . ?
Nb3 F9 1.870(5) . ?
Nb3 F8 1.882(5) . ?
Nb3 F2 2.070(5) . ?
Nb3 F3 2.075(5) . ?
O1 C11 1.370(8) . ?
O1 C11' 1.374(8) . ?
O2 C21 1.391(9) . ?
O3 C31 1.389(9) . ?
O4 C41 1.404(9) . ?
O5 C51 1.381(9) . ?
O6 C61 1.381(8) . ?
O6 C61' 1.383(8) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C12 H12 0.9500 . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 C16 1.3900 . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C11' C12' 1.3900 . ?
C11' C16' 1.3900 . ?
C12' C13' 1.3900 . ?
C12' H12' 0.9500 . ?
C13' C14' 1.3900 . ?
C13' H13' 0.9500 . ?
C14' C15' 1.3900 . ?
C14' H14' 0.9500 . ?
C15' C16' 1.3900 . ?
C15' H15' 0.9500 . ?
C16' H16' 0.9500 . ?
C21 C26 1.385(11) . ?
C21 C22 1.390(11) . ?
C22 C23 1.382(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.373(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.383(11) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.372(10) . ?
C31 C36 1.372(11) . ?
C32 C33 1.378(12) . ?
C32 H32 0.9500 . ?
C33 C34 1.375(12) . ?
C33 H33 0.9500 . ?
C34 C35 1.380(11) . ?
C34 H34 0.9500 . ?
C35 C36 1.363(11) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.358(11) . ?
C41 C46 1.370(12) . ?
C42 C43 1.381(11) . ?
C42 H42 0.9500 . ?
C43 C44 1.366(12) . ?
C43 H43 0.9500 . ?
C44 C45 1.358(12) . ?
C44 H44 0.9500 . ?
C45 C46 1.384(12) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C52 1.354(12) . ?
C51 C56 1.376(12) . ?
C52 C53 1.405(12) . ?
C52 H52 0.9500 . ?
C53 C54 1.342(13) . ?
C53 H53 0.9500 . ?
C54 C55 1.355(13) . ?
C54 H54 0.9500 . ?
C55 C56 1.380(13) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C62 C63 1.3900 . ?
C62 H62 0.9500 . ?
C63 C64 1.3900 . ?
C63 H63 0.9500 . ?
C64 C65 1.3900 . ?
C64 H64 0.9500 . ?
C65 C66 1.3900 . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C61' C62' 1.3900 . ?
C61' C66' 1.3900 . ?
C62' C63' 1.3900 . ?
C62' H62' 0.9500 . ?
C63' C64' 1.3900 . ?
C63' H63' 0.9500 . ?
C64' C65' 1.3900 . ?
C64' H64' 0.9500 . ?
C65' C66' 1.3900 . ?
C65' H65' 0.9500 . ?
C66' H66' 0.9500 . ?
C101 C102 1.539(9) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C102 C103 1.531(9) . ?
C102 H10D 0.9900 . ?
C102 H10E 0.9900 . ?
C103 C104 1.528(10) . ?
C103 H10F 0.9900 . ?
C103 H10G 0.9900 . ?
C104 C105 1.532(9) . ?
C104 H10H 0.9900 . ?
C104 H10I 0.9900 . ?
C105 C106 1.544(9) . ?
C105 H10J 0.9900 . ?
C105 H10K 0.9900 . ?
C106 H10L 0.9800 . ?
C106 H10M 0.9800 . ?
C106 H10N 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
O1 Nb1 O2 99.4(3) . . ?
O1 Nb1 F4 96.7(3) . . ?
O2 Nb1 F4 98.0(2) . . ?
O1 Nb1 F5 95.5(3) . . ?
O2 Nb1 F5 94.5(2) . . ?
F4 Nb1 F5 160.8(2) . . ?
O1 Nb1 F3 89.0(2) . . ?
O2 Nb1 F3 171.4(2) . . ?
F4 Nb1 F3 82.72(19) . . ?
F5 Nb1 F3 82.8(2) . . ?
O1 Nb1 F1 170.6(2) . . ?
O2 Nb1 F1 89.9(2) . . ?
F4 Nb1 F1 83.0(2) . . ?
F5 Nb1 F1 82.6(2) . . ?
F3 Nb1 F1 81.69(18) . . ?
O4 Nb2 O3 99.5(3) . . ?
O4 Nb2 F7 95.9(2) . . ?
O3 Nb2 F7 97.6(2) . . ?
O4 Nb2 F6 98.0(2) . . ?
O3 Nb2 F6 94.8(2) . . ?
F7 Nb2 F6 159.6(2) . . ?
O4 Nb2 F1 169.3(2) . . ?
O3 Nb2 F1 91.2(2) . . ?
F7 Nb2 F1 82.14(19) . . ?
F6 Nb2 F1 81.39(19) . . ?
O4 Nb2 F2 88.7(2) . . ?
O3 Nb2 F2 171.8(2) . . ?
F7 Nb2 F2 81.97(19) . . ?
F6 Nb2 F2 83.52(19) . . ?
F1 Nb2 F2 80.65(17) . . ?
O5 Nb3 O6 98.0(3) . . ?
O5 Nb3 F9 96.2(3) . . ?
O6 Nb3 F9 98.5(3) . . ?
O5 Nb3 F8 96.7(3) . . ?
O6 Nb3 F8 93.6(3) . . ?
F9 Nb3 F8 160.8(2) . . ?
O5 Nb3 F2 91.9(2) . . ?
O6 Nb3 F2 169.5(2) . . ?
F9 Nb3 F2 84.0(2) . . ?
F8 Nb3 F2 81.5(2) . . ?
O5 Nb3 F3 173.2(2) . . ?
O6 Nb3 F3 88.8(2) . . ?
F9 Nb3 F3 82.5(2) . . ?
F8 Nb3 F3 82.9(2) . . ?
F2 Nb3 F3 81.35(18) . . ?
Nb1 F1 Nb2 155.9(2) . . ?
Nb3 F2 Nb2 153.3(2) . . ?
Nb1 F3 Nb3 157.7(3) . . ?
C11 O1 C11' 6.4(11) . . ?
C11 O1 Nb1 161.4(7) . . ?
C11' O1 Nb1 160.4(7) . . ?
C21 O2 Nb1 154.3(5) . . ?
C31 O3 Nb2 169.5(5) . . ?
C41 O4 Nb2 165.4(6) . . ?
C51 O5 Nb3 173.1(6) . . ?
C61 O6 C61' 5.3(11) . . ?
C61 O6 Nb3 157.4(10) . . ?
C61' O6 Nb3 161.9(8) . . ?
O1 C11 C12 112.3(12) . . ?
O1 C11 C16 127.7(12) . . ?
C12 C11 C16 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 120.0 . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
O1 C11' C12' 128.2(11) . . ?
O1 C11' C16' 110.8(11) . . ?
C12' C11' C16' 120.0 . . ?
C11' C12' C13' 120.0 . . ?
C11' C12' H12' 120.0 . . ?
C13' C12' H12' 120.0 . . ?
C12' C13' C14' 120.0 . . ?
C12' C13' H13' 120.0 . . ?
C14' C13' H13' 120.0 . . ?
C15' C14' C13' 120.0 . . ?
C15' C14' H14' 120.0 . . ?
C13' C14' H14' 120.0 . . ?
C14' C15' C16' 120.0 . . ?
C14' C15' H15' 120.0 . . ?
C16' C15' H15' 120.0 . . ?
C15' C16' C11' 120.0 . . ?
C15' C16' H16' 120.0 . . ?
C11' C16' H16' 120.0 . . ?
C26 C21 C22 122.1(8) . . ?
C26 C21 O2 118.3(7) . . ?
C22 C21 O2 119.5(8) . . ?
C23 C22 C21 118.0(8) . . ?
C23 C22 H22 121.0 . . ?
C21 C22 H22 121.0 . . ?
C24 C23 C22 121.1(8) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C25 C24 C23 119.5(8) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 121.4(9) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C25 C26 C21 117.8(8) . . ?
C25 C26 H26 121.1 . . ?
C21 C26 H26 121.1 . . ?
C32 C31 C36 123.1(8) . . ?
C32 C31 O3 118.4(8) . . ?
C36 C31 O3 118.5(7) . . ?
C31 C32 C33 117.9(9) . . ?
C31 C32 H32 121.1 . . ?
C33 C32 H32 121.1 . . ?
C34 C33 C32 120.5(8) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.6(9) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C36 C35 C34 121.2(9) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C35 C36 C31 117.7(8) . . ?
C35 C36 H36 121.2 . . ?
C31 C36 H36 121.2 . . ?
C42 C41 C46 122.6(9) . . ?
C42 C41 O4 118.4(8) . . ?
C46 C41 O4 119.0(8) . . ?
C41 C42 C43 116.8(9) . . ?
C41 C42 H42 121.6 . . ?
C43 C42 H42 121.6 . . ?
C44 C43 C42 121.8(9) . . ?
C44 C43 H43 119.1 . . ?
C42 C43 H43 119.1 . . ?
C45 C44 C43 120.3(9) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 119.1(10) . . ?
C44 C45 H45 120.5 . . ?
C46 C45 H45 120.5 . . ?
C41 C46 C45 119.3(9) . . ?
C41 C46 H46 120.3 . . ?
C45 C46 H46 120.3 . . ?
C52 C51 C56 121.9(9) . . ?
C52 C51 O5 119.3(8) . . ?
C56 C51 O5 118.9(8) . . ?
C51 C52 C53 117.9(9) . . ?
C51 C52 H52 121.0 . . ?
C53 C52 H52 121.0 . . ?
C54 C53 C52 121.3(9) . . ?
C54 C53 H53 119.4 . . ?
C52 C53 H53 119.4 . . ?
C53 C54 C55 119.3(9) . . ?
C53 C54 H54 120.4 . . ?
C55 C54 H54 120.4 . . ?
C54 C55 C56 121.8(10) . . ?
C54 C55 H55 119.1 . . ?
C56 C55 H55 119.1 . . ?
C51 C56 C55 117.8(9) . . ?
C51 C56 H56 121.1 . . ?
C55 C56 H56 121.1 . . ?
O6 C61 C62 118.2(14) . . ?
O6 C61 C66 121.6(14) . . ?
C62 C61 C66 120.0 . . ?
C63 C62 C61 120.0 . . ?
C63 C62 H62 120.0 . . ?
C61 C62 H62 120.0 . . ?
C62 C63 C64 120.0 . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C65 C64 C63 120.0 . . ?
C65 C64 H64 120.0 . . ?
C63 C64 H64 120.0 . . ?
C64 C65 C66 120.0 . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C65 C66 C61 120.0 . . ?
C65 C66 H66 120.0 . . ?
C61 C66 H66 120.0 . . ?
O6 C61' C62' 121.5(11) . . ?
O6 C61' C66' 118.4(11) . . ?
C62' C61' C66' 120.0 . . ?
C63' C62' C61' 120.0 . . ?
C63' C62' H62' 120.0 . . ?
C61' C62' H62' 120.0 . . ?
C62' C63' C64' 120.0 . . ?
C62' C63' H63' 120.0 . . ?
C64' C63' H63' 120.0 . . ?
C65' C64' C63' 120.0 . . ?
C65' C64' H64' 120.0 . . ?
C63' C64' H64' 120.0 . . ?
C66' C65' C64' 120.0 . . ?
C66' C65' H65' 120.0 . . ?
C64' C65' H65' 120.0 . . ?
C65' C66' C61' 120.0 . . ?
C65' C66' H66' 120.0 . . ?
C61' C66' H66' 120.0 . . ?
C102 C101 H10A 109.5 . . ?
C102 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
C102 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C103 C102 C101 112.9(10) . . ?
C103 C102 H10D 109.0 . . ?
C101 C102 H10D 109.0 . . ?
C103 C102 H10E 109.0 . . ?
C101 C102 H10E 109.0 . . ?
H10D C102 H10E 107.8 . . ?
C104 C103 C102 113.2(10) . . ?
C104 C103 H10F 108.9 . . ?
C102 C103 H10F 108.9 . . ?
C104 C103 H10G 108.9 . . ?
C102 C103 H10G 108.9 . . ?
H10F C103 H10G 107.7 . . ?
C103 C104 C105 113.3(10) . . ?
C103 C104 H10H 108.9 . . ?
C105 C104 H10H 108.9 . . ?
C103 C104 H10I 108.9 . . ?
C105 C104 H10I 108.9 . . ?
H10H C104 H10I 107.7 . . ?
C104 C105 C106 112.7(10) . . ?
C104 C105 H10J 109.1 . . ?
C106 C105 H10J 109.1 . . ?
C104 C105 H10K 109.1 . . ?
C106 C105 H10K 109.1 . . ?
H10J C105 H10K 107.8 . . ?
C105 C106 H10L 109.5 . . ?
C105 C106 H10M 109.5 . . ?
H10L C106 H10M 109.5 . . ?
C105 C106 H10N 109.5 . . ?
H10L C106 H10N 109.5 . . ?
H10M C106 H10N 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
O1 Nb1 F1 Nb2 13.1(19) . . . . ?
O2 Nb1 F1 Nb2 -160.3(6) . . . . ?
F4 Nb1 F1 Nb2 101.6(6) . . . . ?
F5 Nb1 F1 Nb2 -65.8(6) . . . . ?
F3 Nb1 F1 Nb2 18.0(6) . . . . ?
O4 Nb2 F1 Nb1 -27.7(16) . . . . ?
O3 Nb2 F1 Nb1 149.8(6) . . . . ?
F7 Nb2 F1 Nb1 52.4(6) . . . . ?
F6 Nb2 F1 Nb1 -115.5(6) . . . . ?
F2 Nb2 F1 Nb1 -30.7(6) . . . . ?
O5 Nb3 F2 Nb2 143.6(6) . . . . ?
O6 Nb3 F2 Nb2 -56.7(16) . . . . ?
F9 Nb3 F2 Nb2 47.6(5) . . . . ?
F8 Nb3 F2 Nb2 -119.9(6) . . . . ?
F3 Nb3 F2 Nb2 -35.8(5) . . . . ?
O4 Nb2 F2 Nb3 -135.1(6) . . . . ?
O3 Nb2 F2 Nb3 48.4(18) . . . . ?
F7 Nb2 F2 Nb3 -38.9(5) . . . . ?
F6 Nb2 F2 Nb3 126.7(5) . . . . ?
F1 Nb2 F2 Nb3 44.4(5) . . . . ?
O1 Nb1 F3 Nb3 -166.3(8) . . . . ?
O2 Nb1 F3 Nb3 26(2) . . . . ?
F4 Nb1 F3 Nb3 -69.4(7) . . . . ?
F5 Nb1 F3 Nb3 98.0(7) . . . . ?
F1 Nb1 F3 Nb3 14.5(7) . . . . ?
O5 Nb3 F3 Nb1 -15(3) . . . . ?
O6 Nb3 F3 Nb1 166.1(8) . . . . ?
F9 Nb3 F3 Nb1 -95.2(7) . . . . ?
F8 Nb3 F3 Nb1 72.3(7) . . . . ?
F2 Nb3 F3 Nb1 -10.2(7) . . . . ?
O2 Nb1 O1 C11 176(3) . . . . ?
F4 Nb1 O1 C11 -85(3) . . . . ?
F5 Nb1 O1 C11 81(3) . . . . ?
F3 Nb1 O1 C11 -2(3) . . . . ?
F1 Nb1 O1 C11 3(4) . . . . ?
O2 Nb1 O1 C11' 157(2) . . . . ?
F4 Nb1 O1 C11' -104(2) . . . . ?
F5 Nb1 O1 C11' 61(2) . . . . ?
F3 Nb1 O1 C11' -22(2) . . . . ?
F1 Nb1 O1 C11' -17(3) . . . . ?
O1 Nb1 O2 C21 -119.7(13) . . . . ?
F4 Nb1 O2 C21 142.1(13) . . . . ?
F5 Nb1 O2 C21 -23.3(13) . . . . ?
F3 Nb1 O2 C21 48(2) . . . . ?
F1 Nb1 O2 C21 59.2(13) . . . . ?
O4 Nb2 O3 C31 -57(3) . . . . ?
F7 Nb2 O3 C31 -155(3) . . . . ?
F6 Nb2 O3 C31 42(3) . . . . ?
F1 Nb2 O3 C31 123(3) . . . . ?
F2 Nb2 O3 C31 119(3) . . . . ?
O3 Nb2 O4 C41 -144(2) . . . . ?
F7 Nb2 O4 C41 -45(2) . . . . ?
F6 Nb2 O4 C41 120(2) . . . . ?
F1 Nb2 O4 C41 34(3) . . . . ?
F2 Nb2 O4 C41 37(2) . . . . ?
O6 Nb3 O5 C51 -54(5) . . . . ?
F9 Nb3 O5 C51 -154(5) . . . . ?
F8 Nb3 O5 C51 40(5) . . . . ?
F2 Nb3 O5 C51 122(5) . . . . ?
F3 Nb3 O5 C51 127(5) . . . . ?
O5 Nb3 O6 C61 98(2) . . . . ?
F9 Nb3 O6 C61 -165(2) . . . . ?
F8 Nb3 O6 C61 0(2) . . . . ?
F2 Nb3 O6 C61 -62(3) . . . . ?
F3 Nb3 O6 C61 -82(2) . . . . ?
O5 Nb3 O6 C61' 90(3) . . . . ?
F9 Nb3 O6 C61' -173(2) . . . . ?
F8 Nb3 O6 C61' -8(3) . . . . ?
F2 Nb3 O6 C61' -70(3) . . . . ?
F3 Nb3 O6 C61' -91(3) . . . . ?
C11' O1 C11 C12 12(9) . . . . ?
Nb1 O1 C11 C12 -79(3) . . . . ?
C11' O1 C11 C16 -166(10) . . . . ?
Nb1 O1 C11 C16 103(3) . . . . ?
O1 C11 C12 C13 -178.1(12) . . . . ?
C16 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C14 C15 C16 C11 0.0 . . . . ?
O1 C11 C16 C15 177.8(14) . . . . ?
C12 C11 C16 C15 0.0 . . . . ?
C11 O1 C11' C12' 128(9) . . . . ?
Nb1 O1 C11' C12' -125(2) . . . . ?
C11 O1 C11' C16' -41(9) . . . . ?
Nb1 O1 C11' C16' 67(3) . . . . ?
O1 C11' C12' C13' -167.7(14) . . . . ?
C16' C11' C12' C13' 0.0 . . . . ?
C11' C12' C13' C14' 0.0 . . . . ?
C12' C13' C14' C15' 0.0 . . . . ?
C13' C14' C15' C16' 0.0 . . . . ?
C14' C15' C16' C11' 0.0 . . . . ?
O1 C11' C16' C15' 169.7(12) . . . . ?
C12' C11' C16' C15' 0.0 . . . . ?
Nb1 O2 C21 C26 -120.3(12) . . . . ?
Nb1 O2 C21 C22 59.7(16) . . . . ?
C26 C21 C22 C23 0.3(12) . . . . ?
O2 C21 C22 C23 -179.7(7) . . . . ?
C21 C22 C23 C24 -0.6(12) . . . . ?
C22 C23 C24 C25 2.0(13) . . . . ?
C23 C24 C25 C26 -3.2(14) . . . . ?
C24 C25 C26 C21 2.9(13) . . . . ?
C22 C21 C26 C25 -1.4(12) . . . . ?
O2 C21 C26 C25 178.6(7) . . . . ?
Nb2 O3 C31 C32 -108(3) . . . . ?
Nb2 O3 C31 C36 72(3) . . . . ?
C36 C31 C32 C33 -1.5(12) . . . . ?
O3 C31 C32 C33 178.3(7) . . . . ?
C31 C32 C33 C34 1.0(12) . . . . ?
C32 C33 C34 C35 0.8(13) . . . . ?
C33 C34 C35 C36 -2.2(13) . . . . ?
C34 C35 C36 C31 1.7(12) . . . . ?
C32 C31 C36 C35 0.2(12) . . . . ?
O3 C31 C36 C35 -179.6(7) . . . . ?
Nb2 O4 C41 C42 -31(3) . . . . ?
Nb2 O4 C41 C46 149.0(18) . . . . ?
C46 C41 C42 C43 -1.0(13) . . . . ?
O4 C41 C42 C43 179.0(7) . . . . ?
C41 C42 C43 C44 -0.4(13) . . . . ?
C42 C43 C44 C45 0.9(14) . . . . ?
C43 C44 C45 C46 -0.1(14) . . . . ?
C42 C41 C46 C45 1.8(13) . . . . ?
O4 C41 C46 C45 -178.2(7) . . . . ?
C44 C45 C46 C41 -1.2(13) . . . . ?
Nb3 O5 C51 C52 150(5) . . . . ?
Nb3 O5 C51 C56 -30(6) . . . . ?
C56 C51 C52 C53 -0.1(15) . . . . ?
O5 C51 C52 C53 -179.7(9) . . . . ?
C51 C52 C53 C54 -0.7(16) . . . . ?
C52 C53 C54 C55 2.1(17) . . . . ?
C53 C54 C55 C56 -2.8(18) . . . . ?
C52 C51 C56 C55 -0.5(16) . . . . ?
O5 C51 C56 C55 179.0(9) . . . . ?
C54 C55 C56 C51 2.0(17) . . . . ?
C61' O6 C61 C62 -42(13) . . . . ?
Nb3 O6 C61 C62 165.6(17) . . . . ?
C61' O6 C61 C66 132(13) . . . . ?
Nb3 O6 C61 C66 -20(3) . . . . ?
O6 C61 C62 C63 174.0(15) . . . . ?
C66 C61 C62 C63 0.0 . . . . ?
C61 C62 C63 C64 0.0 . . . . ?
C62 C63 C64 C65 0.0 . . . . ?
C63 C64 C65 C66 0.0 . . . . ?
C64 C65 C66 C61 0.0 . . . . ?
O6 C61 C66 C65 -173.8(15) . . . . ?
C62 C61 C66 C65 0.0 . . . . ?
C61 O6 C61' C62' 84(13) . . . . ?
Nb3 O6 C61' C62' 120(2) . . . . ?
C61 O6 C61' C66' -91(13) . . . . ?
Nb3 O6 C61' C66' -56(3) . . . . ?
O6 C61' C62' C63' -175.8(12) . . . . ?
C66' C61' C62' C63' 0.0 . . . . ?
C61' C62' C63' C64' 0.0 . . . . ?
C62' C63' C64' C65' 0.0 . . . . ?
C63' C64' C65' C66' 0.0 . . . . ?
C64' C65' C66' C61' 0.0 . . . . ?
O6 C61' C66' C65' 176.0(12) . . . . ?
C62' C61' C66' C65' 0.0 . . . . ?
C101 C102 C103 C104 -33(5) . . . . ?
C102 C103 C104 C105 -127(6) . . . . ?
C103 C104 C105 C106 -143(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.135

# Attachment '- 5A.CIF'

data_p1
_database_code_depnum_ccdc_archive 'CCDC 876460'
#TrackingRef '- 5A.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H40 F2 O8 Ta2'
_chemical_formula_weight         1144.70

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'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.940(4)
_cell_length_b                   10.003(4)
_cell_length_c                   12.384(5)
_cell_angle_alpha                68.033(4)
_cell_angle_beta                 86.135(4)
_cell_angle_gamma                68.477(4)
_cell_volume                     1058.8(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2919
_cell_measurement_theta_min      2.210
_cell_measurement_theta_max      24.8905

_exptl_crystal_description       'prism irregular'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_absorpt_coefficient_mu    5.227
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4885
_exptl_absorpt_correction_T_max  0.5727
_exptl_absorpt_process_details   
;
Data were corrected for Lorentz polarization and absorption
effects (empirical absorption correction SADABS).
R(int) = 0.0981 (selected reflections only, before parameter refinement)
R(int) = 0.0588 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9079
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3583
_reflns_number_gt                2957
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPIII (johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_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. The following restraints
were applied (given as SHELXL lines):
SIMU 0.01 $C
;

_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^)+(0.0913P)^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         3583
_refine_ls_number_parameters     271
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1354
_refine_ls_wR_factor_gt          0.1257
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1598(10) -0.6558(11) 0.0018(9) 0.0238(19) Uani 1 1 d U . .
C2 C -0.2912(10) -0.6242(10) 0.0474(8) 0.0233(19) Uani 1 1 d U . .
H2 H -0.3252 -0.5441 0.0775 0.028 Uiso 1 1 calc R . .
C3 C -0.3748(11) -0.7092(12) 0.0498(10) 0.033(2) Uani 1 1 d U . .
H3 H -0.4654 -0.6892 0.0831 0.040 Uiso 1 1 calc R . .
C4 C -0.3260(12) -0.8242(12) 0.0032(10) 0.033(2) Uani 1 1 d U . .
H4 H -0.3849 -0.8799 0.0018 0.040 Uiso 1 1 calc R . .
C5 C -0.1910(11) -0.8568(11) -0.0411(9) 0.031(2) Uani 1 1 d U . .
H5 H -0.1561 -0.9378 -0.0702 0.037 Uiso 1 1 calc R . .
C6 C -0.1064(11) -0.7728(11) -0.0433(9) 0.027(2) Uani 1 1 d U . .
H6 H -0.0145 -0.7939 -0.0747 0.033 Uiso 1 1 calc R . .
C7 C 0.0426(11) -0.9450(11) 0.2745(9) 0.029(2) Uani 1 1 d U . .
C8 C -0.0779(11) -0.9849(12) 0.2656(9) 0.032(2) Uani 1 1 d U . .
H8 H -0.1709 -0.9073 0.2349 0.039 Uiso 1 1 calc R . .
C9 C -0.0553(12) -1.1414(12) 0.3034(9) 0.033(2) Uani 1 1 d U . .
H9 H -0.1348 -1.1719 0.3018 0.040 Uiso 1 1 calc R . .
C10 C 0.0814(12) -1.2527(12) 0.3432(9) 0.032(2) Uani 1 1 d U . .
H10 H 0.0966 -1.3592 0.3649 0.038 Uiso 1 1 calc R . .
C11 C 0.1953(13) -1.2101(13) 0.3515(10) 0.040(2) Uani 1 1 d U . .
H11 H 0.2887 -1.2880 0.3806 0.048 Uiso 1 1 calc R . .
C12 C 0.1773(12) -1.0575(12) 0.3189(10) 0.036(2) Uani 1 1 d U . .
H12 H 0.2567 -1.0296 0.3267 0.043 Uiso 1 1 calc R . .
C13 C 0.3430(10) -0.6541(11) 0.2763(8) 0.0250(19) Uani 1 1 d U . .
C14 C 0.4304(11) -0.8105(13) 0.3317(9) 0.033(2) Uani 1 1 d U . .
H14 H 0.3953 -0.8900 0.3398 0.039 Uiso 1 1 calc R . .
C15 C 0.5678(12) -0.8455(13) 0.3738(10) 0.038(2) Uani 1 1 d U . .
H15 H 0.6283 -0.9514 0.4114 0.046 Uiso 1 1 calc R . .
C16 C 0.6219(12) -0.7337(13) 0.3639(10) 0.037(2) Uani 1 1 d U . .
H16 H 0.7179 -0.7614 0.3939 0.044 Uiso 1 1 calc R . .
C17 C 0.5308(11) -0.5762(12) 0.3081(9) 0.031(2) Uani 1 1 d U . .
H17 H 0.5646 -0.4962 0.3012 0.037 Uiso 1 1 calc R . .
C18 C 0.3926(12) -0.5396(12) 0.2636(9) 0.030(2) Uani 1 1 d U . .
H18 H 0.3320 -0.4342 0.2240 0.036 Uiso 1 1 calc R . .
C19 C -0.1962(10) -0.3982(11) 0.2466(9) 0.028(2) Uani 1 1 d U . .
C20 C -0.1898(11) -0.4481(12) 0.3659(10) 0.032(2) Uani 1 1 d U . .
H20 H -0.1116 -0.5382 0.4119 0.039 Uiso 1 1 calc R . .
C21 C -0.2986(12) -0.3664(12) 0.4199(10) 0.032(2) Uani 1 1 d U . .
H21 H -0.2976 -0.4044 0.5027 0.038 Uiso 1 1 calc R . .
C22 C -0.4075(11) -0.2308(11) 0.3535(9) 0.029(2) Uani 1 1 d U . .
H22 H -0.4783 -0.1712 0.3897 0.035 Uiso 1 1 calc R . .
C23 C -0.4121(11) -0.1832(12) 0.2342(9) 0.031(2) Uani 1 1 d U . .
H23 H -0.4888 -0.0913 0.1884 0.037 Uiso 1 1 calc R . .
C24 C -0.3093(10) -0.2641(11) 0.1791(9) 0.027(2) Uani 1 1 d U . .
H24 H -0.3150 -0.2294 0.0962 0.032 Uiso 1 1 calc R . .
F1 F 0.2094(7) -0.7458(7) 0.0843(5) 0.0401(15) Uani 1 1 d . . .
O1 O -0.0742(7) -0.5706(7) 0.0010(6) 0.0277(16) Uani 1 1 d . . .
O3 O 0.0209(8) -0.7916(7) 0.2397(6) 0.0277(15) Uani 1 1 d . . .
O4 O 0.2032(8) -0.6139(8) 0.2361(6) 0.0326(17) Uani 1 1 d . . .
O5 O -0.0932(7) -0.4789(8) 0.1953(6) 0.0288(15) Uani 1 1 d . . .
Ta1 Ta 0.06067(4) -0.61617(4) 0.14530(4) 0.02281(17) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.018(4) 0.019(4) 0.029(4) -0.005(3) -0.007(3) -0.004(3)
C2 0.022(4) 0.016(4) 0.025(4) -0.004(3) -0.003(3) -0.002(3)
C3 0.020(4) 0.028(4) 0.042(5) 0.000(4) -0.006(4) -0.009(4)
C4 0.031(5) 0.022(4) 0.041(5) -0.004(4) -0.008(4) -0.010(4)
C5 0.031(4) 0.020(4) 0.039(5) -0.011(4) -0.013(4) -0.004(4)
C6 0.026(4) 0.021(4) 0.027(4) -0.004(4) -0.004(4) -0.003(3)
C7 0.022(4) 0.024(4) 0.035(5) -0.004(4) -0.001(4) -0.009(4)
C8 0.023(4) 0.030(4) 0.037(5) -0.002(4) 0.003(4) -0.013(4)
C9 0.032(5) 0.026(4) 0.034(5) -0.003(4) -0.002(4) -0.011(4)
C10 0.036(5) 0.022(4) 0.032(5) -0.006(4) -0.002(4) -0.008(4)
C11 0.037(5) 0.027(4) 0.045(5) -0.006(4) -0.005(4) -0.007(4)
C12 0.026(5) 0.028(4) 0.049(5) -0.008(4) -0.001(4) -0.013(4)
C13 0.022(4) 0.026(4) 0.024(4) -0.009(3) -0.001(3) -0.006(3)
C14 0.031(5) 0.029(4) 0.035(5) -0.010(4) 0.000(4) -0.010(4)
C15 0.027(5) 0.034(5) 0.043(5) -0.007(4) -0.002(4) -0.006(4)
C16 0.030(5) 0.035(5) 0.045(5) -0.012(4) -0.002(4) -0.012(4)
C17 0.029(4) 0.032(4) 0.036(5) -0.014(4) 0.001(4) -0.015(4)
C18 0.035(5) 0.025(4) 0.030(5) -0.009(4) 0.000(4) -0.011(4)
C19 0.017(4) 0.024(4) 0.040(5) -0.007(4) -0.001(4) -0.008(3)
C20 0.022(4) 0.021(4) 0.040(5) -0.001(4) -0.002(4) -0.003(4)
C21 0.033(5) 0.023(4) 0.036(5) -0.006(4) -0.001(4) -0.010(4)
C22 0.027(4) 0.023(4) 0.036(5) -0.012(4) 0.000(4) -0.008(4)
C23 0.025(4) 0.027(4) 0.035(5) -0.002(4) -0.011(4) -0.010(4)
C24 0.018(4) 0.023(4) 0.033(5) -0.005(4) -0.004(4) -0.005(3)
F1 0.036(4) 0.030(3) 0.036(4) -0.006(3) 0.002(3) 0.001(3)
O1 0.030(4) 0.016(3) 0.033(4) -0.002(3) -0.005(3) -0.011(3)
O3 0.033(4) 0.018(3) 0.025(4) 0.002(3) -0.007(3) -0.010(3)
O4 0.026(4) 0.024(4) 0.037(4) 0.000(3) -0.012(3) -0.008(3)
O5 0.027(4) 0.022(3) 0.032(4) -0.008(3) -0.001(3) -0.007(3)
Ta1 0.0173(2) 0.0145(2) 0.0308(3) -0.00417(16) -0.00358(15) -0.00309(15)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.362(14) . ?
C1 C6 1.399(14) . ?
C1 O1 1.406(11) . ?
C2 C3 1.382(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(16) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(14) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O3 1.364(12) . ?
C7 C12 1.375(14) . ?
C7 C8 1.417(14) . ?
C8 C9 1.388(15) . ?
C8 H8 0.9500 . ?
C9 C10 1.377(15) . ?
C9 H9 0.9500 . ?
C10 C11 1.371(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.368(15) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.359(14) . ?
C13 O4 1.369(12) . ?
C13 C14 1.397(14) . ?
C14 C15 1.367(15) . ?
C14 H14 0.9500 . ?
C15 C16 1.373(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.415(15) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(15) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 O5 1.339(12) . ?
C19 C20 1.369(15) . ?
C19 C24 1.394(13) . ?
C20 C21 1.396(15) . ?
C20 H20 0.9500 . ?
C21 C22 1.377(14) . ?
C21 H21 0.9500 . ?
C22 C23 1.370(15) . ?
C22 H22 0.9500 . ?
C23 C24 1.371(15) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
F1 Ta1 1.901(6) . ?
O1 Ta1 2.100(6) 2_545 ?
O1 Ta1 2.113(7) . ?
O3 Ta1 1.875(6) . ?
O4 Ta1 1.879(7) . ?
O5 Ta1 1.891(7) . ?
Ta1 O1 2.100(6) 2_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 121.7(9) . . ?
C2 C1 O1 119.6(9) . . ?
C6 C1 O1 118.7(9) . . ?
C1 C2 C3 119.7(9) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C4 120.0(10) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.6(10) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 120.7(10) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 118.3(10) . . ?
C5 C6 H6 120.9 . . ?
C1 C6 H6 120.9 . . ?
O3 C7 C12 120.8(9) . . ?
O3 C7 C8 118.1(9) . . ?
C12 C7 C8 121.1(9) . . ?
C9 C8 C7 117.7(10) . . ?
C9 C8 H8 121.2 . . ?
C7 C8 H8 121.2 . . ?
C10 C9 C8 120.6(10) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 120.1(10) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C12 C11 C10 121.3(11) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C7 119.1(10) . . ?
C11 C12 H12 120.5 . . ?
C7 C12 H12 120.5 . . ?
C18 C13 O4 118.8(9) . . ?
C18 C13 C14 121.4(9) . . ?
O4 C13 C14 119.8(9) . . ?
C15 C14 C13 117.9(10) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
C14 C15 C16 122.6(11) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C15 C16 C17 118.3(10) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
C18 C17 C16 119.5(10) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C13 C18 C17 120.2(10) . . ?
C13 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
O5 C19 C20 119.6(9) . . ?
O5 C19 C24 120.3(9) . . ?
C20 C19 C24 120.1(10) . . ?
C19 C20 C21 119.8(9) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.1(10) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 119.0(10) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 122.0(9) . . ?
C22 C23 H23 119.0 . . ?
C24 C23 H23 119.0 . . ?
C23 C24 C19 118.8(10) . . ?
C23 C24 H24 120.6 . . ?
C19 C24 H24 120.6 . . ?
C1 O1 Ta1 124.3(6) . 2_545 ?
C1 O1 Ta1 124.5(6) . . ?
Ta1 O1 Ta1 111.2(3) 2_545 . ?
C7 O3 Ta1 151.4(7) . . ?
C13 O4 Ta1 153.9(7) . . ?
C19 O5 Ta1 171.5(7) . . ?
O3 Ta1 O4 103.9(3) . . ?
O3 Ta1 O5 93.8(3) . . ?
O4 Ta1 O5 93.4(3) . . ?
O3 Ta1 F1 88.2(3) . . ?
O4 Ta1 F1 89.3(3) . . ?
O5 Ta1 F1 176.0(3) . . ?
O3 Ta1 O1 161.9(3) . 2_545 ?
O4 Ta1 O1 93.3(3) . 2_545 ?
O5 Ta1 O1 90.7(3) . 2_545 ?
F1 Ta1 O1 86.3(3) . 2_545 ?
O3 Ta1 O1 93.6(3) . . ?
O4 Ta1 O1 161.7(3) . . ?
O5 Ta1 O1 90.7(3) . . ?
F1 Ta1 O1 85.8(3) . . ?
O1 Ta1 O1 68.8(3) 2_545 . ?

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
C6 C1 C2 C3 0.1(14) . . . . ?
O1 C1 C2 C3 -179.1(9) . . . . ?
C1 C2 C3 C4 -1.4(15) . . . . ?
C2 C3 C4 C5 2.6(15) . . . . ?
C3 C4 C5 C6 -2.3(16) . . . . ?
C4 C5 C6 C1 1.0(15) . . . . ?
C2 C1 C6 C5 0.2(14) . . . . ?
O1 C1 C6 C5 179.4(9) . . . . ?
O3 C7 C8 C9 -178.7(9) . . . . ?
C12 C7 C8 C9 0.1(16) . . . . ?
C7 C8 C9 C10 -2.8(16) . . . . ?
C8 C9 C10 C11 3.4(17) . . . . ?
C9 C10 C11 C12 -1.3(18) . . . . ?
C10 C11 C12 C7 -1.4(18) . . . . ?
O3 C7 C12 C11 -179.2(10) . . . . ?
C8 C7 C12 C11 2.0(17) . . . . ?
C18 C13 C14 C15 0.5(16) . . . . ?
O4 C13 C14 C15 -178.0(10) . . . . ?
C13 C14 C15 C16 0.2(17) . . . . ?
C14 C15 C16 C17 0.1(18) . . . . ?
C15 C16 C17 C18 -1.1(16) . . . . ?
O4 C13 C18 C17 177.0(10) . . . . ?
C14 C13 C18 C17 -1.5(16) . . . . ?
C16 C17 C18 C13 1.8(16) . . . . ?
O5 C19 C20 C21 -178.6(9) . . . . ?
C24 C19 C20 C21 1.5(15) . . . . ?
C19 C20 C21 C22 -3.9(16) . . . . ?
C20 C21 C22 C23 4.0(15) . . . . ?
C21 C22 C23 C24 -1.9(15) . . . . ?
C22 C23 C24 C19 -0.5(15) . . . . ?
O5 C19 C24 C23 -179.3(9) . . . . ?
C20 C19 C24 C23 0.7(14) . . . . ?
C2 C1 O1 Ta1 -99.7(9) . . . 2_545 ?
C6 C1 O1 Ta1 81.0(10) . . . 2_545 ?
C2 C1 O1 Ta1 81.5(10) . . . . ?
C6 C1 O1 Ta1 -97.7(9) . . . . ?
C12 C7 O3 Ta1 59.9(18) . . . . ?
C8 C7 O3 Ta1 -121.3(12) . . . . ?
C18 C13 O4 Ta1 123.6(13) . . . . ?
C14 C13 O4 Ta1 -57.9(19) . . . . ?
C20 C19 O5 Ta1 12(5) . . . . ?
C24 C19 O5 Ta1 -168(4) . . . . ?
C7 O3 Ta1 O4 -94.0(13) . . . . ?
C7 O3 Ta1 O5 171.5(13) . . . . ?
C7 O3 Ta1 F1 -5.1(13) . . . . ?
C7 O3 Ta1 O1 67.4(17) . . . 2_545 ?
C7 O3 Ta1 O1 80.6(13) . . . . ?
C13 O4 Ta1 O3 87.4(15) . . . . ?
C13 O4 Ta1 O5 -177.7(14) . . . . ?
C13 O4 Ta1 F1 -0.6(15) . . . . ?
C13 O4 Ta1 O1 -86.8(15) . . . 2_545 ?
C13 O4 Ta1 O1 -75.2(17) . . . . ?
C19 O5 Ta1 O3 41(4) . . . . ?
C19 O5 Ta1 O4 -63(4) . . . . ?
C19 O5 Ta1 F1 163(4) . . . . ?
C19 O5 Ta1 O1 -156(4) . . . 2_545 ?
C19 O5 Ta1 O1 135(4) . . . . ?
C1 O1 Ta1 O3 3.3(7) . . . . ?
Ta1 O1 Ta1 O3 -175.6(3) 2_545 . . . ?
C1 O1 Ta1 O4 166.4(9) . . . . ?
Ta1 O1 Ta1 O4 -12.5(11) 2_545 . . . ?
C1 O1 Ta1 O5 -90.6(7) . . . . ?
Ta1 O1 Ta1 O5 90.5(3) 2_545 . . . ?
C1 O1 Ta1 F1 91.3(7) . . . . ?
Ta1 O1 Ta1 F1 -87.6(3) 2_545 . . . ?
C1 O1 Ta1 O1 178.9(9) . . . 2_545 ?
Ta1 O1 Ta1 O1 0.0 2_545 . . 2_545 ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         5.382
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.238