data_2005src0721
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. S. J. Lancaster
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C36 H2 B2 F30 P1, C8 H16 Li O4'
_chemical_formula_sum
 'C44 H18 B2 F30 Li O4 P'
_chemical_formula_weight          1240.11
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Li'  'Li'  -0.0003   0.0001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'B'  'B'   0.0013   0.0007
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 '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
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    12.465(13)
_cell_length_b                    14.37(3)
_cell_length_c                    14.461(14)
_cell_angle_alpha                 62.10(13)
_cell_angle_beta                  84.68(10)
_cell_angle_gamma                 89.27(10)
_cell_volume                      2279(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     9641
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        'Cut Blade'
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.14
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.807
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1224
_exptl_absorpt_coefficient_mu     0.230
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9685
_exptl_absorpt_correction_T_max   0.9954
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             42972
_diffrn_reflns_av_R_equivalents   0.1233
_diffrn_reflns_av_sigmaI/netI     0.1414
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          3.09
_diffrn_reflns_theta_max          27.48
_reflns_number_total              10370
_reflns_number_gt                 5853
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0264P)²+4.4235P] where P=(Fo²+2Fc²)/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          10370
_refine_ls_number_parameters      739
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1822
_refine_ls_R_factor_gt            0.0920
_refine_ls_wR_factor_ref          0.1623
_refine_ls_wR_factor_gt           0.1375
_refine_ls_goodness_of_fit_ref    1.086
_refine_ls_restrained_S_all       1.086
_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 0.7402(3) 0.7021(3) 0.1971(3) 0.0265(10) Uani 1 1 d . . .
C2 C 0.6594(3) 0.7667(3) 0.2064(3) 0.0248(10) Uani 1 1 d . . .
C3 C 0.5816(4) 0.8084(4) 0.1387(4) 0.0317(11) Uani 1 1 d . . .
C4 C 0.5802(4) 0.7859(4) 0.0559(4) 0.0374(12) Uani 1 1 d . . .
C5 C 0.6558(4) 0.7209(4) 0.0439(4) 0.0340(12) Uani 1 1 d . . .
C6 C 0.7322(4) 0.6789(4) 0.1147(3) 0.0281(11) Uani 1 1 d . . .
C7 C 0.7489(3) 0.5571(3) 0.3911(3) 0.0262(10) Uani 1 1 d . . .
C8 C 0.7051(3) 0.5636(4) 0.4796(3) 0.0266(10) Uani 1 1 d . . .
C9 C 0.6335(4) 0.4906(4) 0.5585(4) 0.0304(11) Uani 1 1 d . . .
C10 C 0.6013(4) 0.4039(4) 0.5511(4) 0.0322(11) Uani 1 1 d . . .
C11 C 0.6398(4) 0.3930(4) 0.4642(4) 0.0323(11) Uani 1 1 d . . .
C12 C 0.7104(4) 0.4694(4) 0.3862(3) 0.0294(11) Uani 1 1 d . . .
C13 C 0.8845(3) 0.7322(3) 0.3186(3) 0.0238(10) Uani 1 1 d . . .
C14 C 0.8917(3) 0.8414(3) 0.2572(3) 0.0261(10) Uani 1 1 d . . .
C15 C 0.9463(4) 0.9075(4) 0.2828(4) 0.0294(11) Uani 1 1 d . . .
C16 C 1.0004(4) 0.8654(4) 0.3718(4) 0.0335(12) Uani 1 1 d . . .
C17 C 0.9972(4) 0.7588(4) 0.4349(4) 0.0329(12) Uani 1 1 d . . .
C18 C 0.9401(4) 0.6960(3) 0.4074(3) 0.0275(11) Uani 1 1 d . . .
C19 C 1.0362(3) 0.6867(3) 0.0336(3) 0.0262(10) Uani 1 1 d . . .
C20 C 0.9686(4) 0.7719(3) -0.0034(3) 0.0287(11) Uani 1 1 d . . .
C21 C 0.9182(4) 0.8067(4) -0.0942(4) 0.0300(11) Uani 1 1 d . . .
C22 C 0.9353(4) 0.7569(4) -0.1550(4) 0.0351(12) Uani 1 1 d . . .
C23 C 1.0017(4) 0.6726(4) -0.1231(4) 0.0347(12) Uani 1 1 d . . .
C24 C 1.0494(4) 0.6385(3) -0.0306(4) 0.0295(11) Uani 1 1 d . . .
C25 C 1.1829(4) 0.5610(3) 0.1657(3) 0.0267(10) Uani 1 1 d . . .
C26 C 1.1873(4) 0.4574(4) 0.2429(3) 0.0284(11) Uani 1 1 d . . .
C27 C 1.2740(4) 0.3948(4) 0.2504(4) 0.0322(11) Uani 1 1 d . . .
C28 C 1.3646(4) 0.4344(4) 0.1807(4) 0.0353(12) Uani 1 1 d . . .
C29 C 1.3661(4) 0.5362(4) 0.1024(4) 0.0369(12) Uani 1 1 d . . .
C30 C 1.2767(4) 0.5954(4) 0.0973(4) 0.0323(11) Uani 1 1 d . . .
C31 C 1.1434(3) 0.7436(3) 0.1582(3) 0.0249(10) Uani 1 1 d . . .
C32 C 1.1791(4) 0.8416(4) 0.0747(3) 0.0293(11) Uani 1 1 d . . .
C33 C 1.2357(4) 0.9158(4) 0.0856(4) 0.0323(11) Uani 1 1 d . . .
C34 C 1.2591(4) 0.8970(4) 0.1836(4) 0.0317(11) Uani 1 1 d . . .
C35 C 1.2269(4) 0.8014(4) 0.2700(4) 0.0295(11) Uani 1 1 d . . .
C36 C 1.1732(4) 0.7285(3) 0.2545(3) 0.0280(11) Uani 1 1 d . . .
B1 B 0.8231(4) 0.6505(4) 0.2888(4) 0.0271(12) Uani 1 1 d . . .
B2 B 1.0872(4) 0.6478(4) 0.1465(4) 0.0282(12) Uani 1 1 d . . .
F2 F 0.65690(19) 0.79120(19) 0.28636(19) 0.0307(6) Uani 1 1 d . . .
F3 F 0.5082(2) 0.8726(2) 0.1516(2) 0.0416(7) Uani 1 1 d . . .
F4 F 0.5048(2) 0.8288(2) -0.0128(2) 0.0506(8) Uani 1 1 d . . .
F5 F 0.6557(2) 0.6992(2) -0.0368(2) 0.0455(8) Uani 1 1 d . . .
F6 F 0.8005(2) 0.6121(2) 0.09952(19) 0.0342(6) Uani 1 1 d . . .
F8 F 0.7286(2) 0.6481(2) 0.49392(19) 0.0338(6) Uani 1 1 d . . .
F9 F 0.5947(2) 0.5031(2) 0.6425(2) 0.0417(7) Uani 1 1 d . . .
F10 F 0.5332(2) 0.3305(2) 0.6272(2) 0.0448(8) Uani 1 1 d . . .
F11 F 0.6069(2) 0.3101(2) 0.4543(2) 0.0437(7) Uani 1 1 d . . .
F12 F 0.7398(2) 0.4545(2) 0.3016(2) 0.0374(7) Uani 1 1 d . . .
F14 F 0.8400(2) 0.89140(18) 0.16993(18) 0.0302(6) Uani 1 1 d . . .
F15 F 0.9454(2) 1.0128(2) 0.2224(2) 0.0413(7) Uani 1 1 d . . .
F16 F 1.0557(2) 0.9299(2) 0.3953(2) 0.0482(8) Uani 1 1 d . . .
F17 F 1.0511(2) 0.7173(2) 0.5212(2) 0.0411(7) Uani 1 1 d . . .
F18 F 0.9399(2) 0.59140(19) 0.47398(18) 0.0317(6) Uani 1 1 d . . .
F20 F 0.9486(2) 0.82457(19) 0.05225(19) 0.0335(6) Uani 1 1 d . . .
F21 F 0.8527(2) 0.8887(2) -0.1236(2) 0.0412(7) Uani 1 1 d . . .
F22 F 0.8890(3) 0.7905(2) -0.2454(2) 0.0522(8) Uani 1 1 d . . .
F23 F 1.0218(3) 0.6234(2) -0.1827(2) 0.0497(8) Uani 1 1 d . . .
F24 F 1.1118(2) 0.5532(2) -0.0055(2) 0.0379(7) Uani 1 1 d . . .
F26 F 1.1034(2) 0.41002(19) 0.31794(19) 0.0344(7) Uani 1 1 d . . .
F27 F 1.2715(2) 0.2941(2) 0.3281(2) 0.0411(7) Uani 1 1 d . . .
F28 F 1.4509(2) 0.3740(2) 0.1896(2) 0.0506(8) Uani 1 1 d . . .
F29 F 1.4540(2) 0.5782(2) 0.0316(2) 0.0519(8) Uani 1 1 d . . .
F30 F 1.2829(2) 0.6946(2) 0.0141(2) 0.0404(7) Uani 1 1 d . . .
F32 F 1.1644(2) 0.8677(2) -0.02646(19) 0.0366(7) Uani 1 1 d . . .
F33 F 1.2717(2) 1.0068(2) 0.0009(2) 0.0419(7) Uani 1 1 d . . .
F34 F 1.3136(2) 0.9697(2) 0.1966(2) 0.0415(7) Uani 1 1 d . . .
F35 F 1.2503(2) 0.7830(2) 0.3665(2) 0.0387(7) Uani 1 1 d . . .
F36 F 1.1495(2) 0.63474(19) 0.34162(18) 0.0319(6) Uani 1 1 d . . .
P1 P 0.95520(10) 0.58065(9) 0.25480(9) 0.0252(3) Uani 1 1 d . . .
H1A H 0.9155 0.5115 0.2321 0.030 Uiso 1 1 calc R . .
H1B H 0.9952 0.5268 0.3441 0.030 Uiso 1 1 calc R . .
C41 C 0.4880(5) 0.9598(4) 0.3398(4) 0.0451(14) Uani 1 1 d . . .
H41A H 0.4323 0.9114 0.3396 0.054 Uiso 1 1 calc R . .
H41B H 0.5537 0.9574 0.2970 0.054 Uiso 1 1 calc R . .
C42 C 0.4479(5) 1.0701(4) 0.2943(4) 0.0506(15) Uani 1 1 d . . .
H42A H 0.4367 1.0958 0.2194 0.061 Uiso 1 1 calc R . .
H42B H 0.3779 1.0707 0.3325 0.061 Uiso 1 1 calc R . .
C43 C 0.6042(4) 1.1915(4) 0.2145(4) 0.0415(13) Uani 1 1 d . . .
H43A H 0.5693 1.2401 0.1514 0.050 Uiso 1 1 calc R . .
H43B H 0.6457 1.1406 0.1988 0.050 Uiso 1 1 calc R . .
C44 C 0.6765(4) 1.2516(4) 0.2475(4) 0.0441(14) Uani 1 1 d . . .
H44A H 0.7395 1.2826 0.1945 0.053 Uiso 1 1 calc R . .
H44B H 0.6367 1.3098 0.2516 0.053 Uiso 1 1 calc R . .
C45 C 0.8081(4) 1.1276(4) 0.3433(5) 0.0545(16) Uani 1 1 d . . .
H45A H 0.8732 1.1738 0.3258 0.065 Uiso 1 1 calc R . .
H45B H 0.8060 1.1038 0.2894 0.065 Uiso 1 1 calc R . .
C46 C 0.8092(4) 1.0350(5) 0.4506(5) 0.0538(16) Uani 1 1 d . . .
H46A H 0.8698 0.9899 0.4501 0.065 Uiso 1 1 calc R . .
H46B H 0.8210 1.0603 0.5020 0.065 Uiso 1 1 calc R . .
C47 C 0.7043(4) 0.8980(4) 0.4446(4) 0.0397(13) Uani 1 1 d . . .
H47A H 0.7597 0.8446 0.4733 0.048 Uiso 1 1 calc R . .
H47B H 0.7160 0.9331 0.3669 0.048 Uiso 1 1 calc R . .
C48 C 0.5932(4) 0.8478(4) 0.4819(4) 0.0361(12) Uani 1 1 d . . .
H48A H 0.5826 0.7978 0.4540 0.043 Uiso 1 1 calc R . .
H48B H 0.5851 0.8078 0.5596 0.043 Uiso 1 1 calc R . .
Li41 Li 0.5914(7) 1.0778(7) 0.4373(6) 0.037(2) Uani 1 1 d . . .
O41 O 0.5120(2) 0.9276(2) 0.4469(2) 0.0352(8) Uani 1 1 d . . .
O42 O 0.5252(3) 1.1378(3) 0.3032(3) 0.0463(9) Uani 1 1 d . . .
O43 O 0.7125(3) 1.1825(3) 0.3481(3) 0.0458(9) Uani 1 1 d . . .
O44 O 0.7096(3) 0.9736(3) 0.4828(3) 0.0433(9) Uani 1 1 d . . .
 
 
_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 C6 1.392(6) . ?
C1 C2 1.401(6) . ?
C1 B1 1.641(7) . ?
C2 F2 1.355(5) . ?
C2 C3 1.368(6) . ?
C3 F3 1.352(6) . ?
C3 C4 1.381(7) . ?
C4 F4 1.355(6) . ?
C4 C5 1.375(7) . ?
C5 F5 1.342(5) . ?
C5 C6 1.380(7) . ?
C6 F6 1.355(5) . ?
C7 C8 1.388(6) . ?
C7 C12 1.389(7) . ?
C7 B1 1.663(7) . ?
C8 F8 1.364(6) . ?
C8 C9 1.383(7) . ?
C9 F9 1.354(5) . ?
C9 C10 1.368(7) . ?
C10 F10 1.344(6) . ?
C10 C11 1.381(7) . ?
C11 F11 1.337(6) . ?
C11 C12 1.391(7) . ?
C12 F12 1.355(5) . ?
C13 C18 1.389(6) . ?
C13 C14 1.394(7) . ?
C13 B1 1.646(7) . ?
C14 F14 1.347(5) . ?
C14 C15 1.376(7) . ?
C15 F15 1.349(6) . ?
C15 C16 1.378(7) . ?
C16 F16 1.344(5) . ?
C16 C17 1.367(7) . ?
C17 F17 1.347(5) . ?
C17 C18 1.373(7) . ?
C18 F18 1.353(6) . ?
C19 C24 1.392(7) . ?
C19 C20 1.393(7) . ?
C19 B2 1.647(7) . ?
C20 F20 1.347(5) . ?
C20 C21 1.377(7) . ?
C21 F21 1.344(5) . ?
C21 C22 1.373(7) . ?
C22 F22 1.348(5) . ?
C22 C23 1.375(7) . ?
C23 F23 1.352(6) . ?
C23 C24 1.382(7) . ?
C24 F24 1.361(6) . ?
C25 C26 1.386(7) . ?
C25 C30 1.390(7) . ?
C25 B2 1.661(7) . ?
C26 F26 1.361(5) . ?
C26 C27 1.376(7) . ?
C27 F27 1.353(6) . ?
C27 C28 1.373(7) . ?
C28 F28 1.350(5) . ?
C28 C29 1.367(7) . ?
C29 F29 1.357(6) . ?
C29 C30 1.380(7) . ?
C30 F30 1.367(6) . ?
C31 C36 1.392(6) . ?
C31 C32 1.403(7) . ?
C31 B2 1.637(8) . ?
C32 F32 1.359(5) . ?
C32 C33 1.362(7) . ?
C33 F33 1.351(6) . ?
C33 C34 1.373(7) . ?
C34 F34 1.347(6) . ?
C34 C35 1.388(7) . ?
C35 F35 1.353(5) . ?
C35 C36 1.363(7) . ?
C36 F36 1.358(6) . ?
B1 P1 2.057(6) . ?
B2 P1 2.058(6) . ?
P1 H1A 1.3000 . ?
P1 H1B 1.3000 . ?
C41 O41 1.455(6) . ?
C41 C42 1.504(8) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 O42 1.435(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 O42 1.439(6) . ?
C43 C44 1.507(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 O43 1.437(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 O43 1.436(6) . ?
C45 C46 1.500(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 O44 1.440(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O44 1.435(6) . ?
C47 C48 1.501(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O41 1.455(6) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
Li41 O42 1.974(9) . ?
Li41 O41 1.988(9) 2_676 ?
Li41 O44 2.011(9) . ?
Li41 O43 2.022(10) . ?
Li41 O41 2.325(10) . ?
Li41 Li41 3.008(18) 2_676 ?
O41 Li41 1.988(9) 2_676 ?
 
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
C6 C1 C2 114.1(4) . . ?
C6 C1 B1 126.5(4) . . ?
C2 C1 B1 118.9(4) . . ?
F2 C2 C3 116.7(4) . . ?
F2 C2 C1 119.2(4) . . ?
C3 C2 C1 124.2(4) . . ?
F3 C3 C2 120.4(4) . . ?
F3 C3 C4 120.5(4) . . ?
C2 C3 C4 119.1(5) . . ?
F4 C4 C5 121.0(5) . . ?
F4 C4 C3 119.4(5) . . ?
C5 C4 C3 119.6(5) . . ?
F5 C5 C4 120.0(4) . . ?
F5 C5 C6 120.3(5) . . ?
C4 C5 C6 119.7(5) . . ?
F6 C6 C5 115.7(4) . . ?
F6 C6 C1 121.0(4) . . ?
C5 C6 C1 123.3(4) . . ?
C8 C7 C12 112.9(4) . . ?
C8 C7 B1 126.1(4) . . ?
C12 C7 B1 120.3(4) . . ?
F8 C8 C9 113.6(4) . . ?
F8 C8 C7 120.8(4) . . ?
C9 C8 C7 125.5(5) . . ?
F9 C9 C10 119.4(4) . . ?
F9 C9 C8 121.6(4) . . ?
C10 C9 C8 119.0(4) . . ?
F10 C10 C9 120.6(5) . . ?
F10 C10 C11 120.4(5) . . ?
C9 C10 C11 118.9(4) . . ?
F11 C11 C10 119.8(4) . . ?
F11 C11 C12 120.4(5) . . ?
C10 C11 C12 119.8(5) . . ?
F12 C12 C7 120.5(4) . . ?
F12 C12 C11 115.6(4) . . ?
C7 C12 C11 123.8(5) . . ?
C18 C13 C14 113.4(4) . . ?
C18 C13 B1 121.6(4) . . ?
C14 C13 B1 124.9(4) . . ?
F14 C14 C15 114.3(4) . . ?
F14 C14 C13 122.0(4) . . ?
C15 C14 C13 123.6(4) . . ?
F15 C15 C14 120.4(4) . . ?
F15 C15 C16 120.0(4) . . ?
C14 C15 C16 119.6(4) . . ?
F16 C16 C17 120.9(5) . . ?
F16 C16 C15 119.5(4) . . ?
C17 C16 C15 119.6(5) . . ?
F17 C17 C16 119.8(5) . . ?
F17 C17 C18 121.3(4) . . ?
C16 C17 C18 118.8(4) . . ?
F18 C18 C17 115.5(4) . . ?
F18 C18 C13 119.6(4) . . ?
C17 C18 C13 124.9(4) . . ?
C24 C19 C20 113.5(4) . . ?
C24 C19 B2 126.0(4) . . ?
C20 C19 B2 120.5(4) . . ?
F20 C20 C21 116.3(4) . . ?
F20 C20 C19 119.2(4) . . ?
C21 C20 C19 124.5(5) . . ?
F21 C21 C22 119.8(4) . . ?
F21 C21 C20 120.8(4) . . ?
C22 C21 C20 119.4(4) . . ?
F22 C22 C21 120.8(4) . . ?
F22 C22 C23 120.2(5) . . ?
C21 C22 C23 119.0(4) . . ?
F23 C23 C22 120.2(4) . . ?
F23 C23 C24 119.7(4) . . ?
C22 C23 C24 120.0(5) . . ?
F24 C24 C23 115.2(4) . . ?
F24 C24 C19 121.3(4) . . ?
C23 C24 C19 123.6(4) . . ?
C26 C25 C30 112.4(4) . . ?
C26 C25 B2 130.4(4) . . ?
C30 C25 B2 117.2(4) . . ?
F26 C26 C27 115.0(4) . . ?
F26 C26 C25 121.0(4) . . ?
C27 C26 C25 124.0(5) . . ?
F27 C27 C28 119.3(4) . . ?
F27 C27 C26 120.2(4) . . ?
C28 C27 C26 120.5(4) . . ?
F28 C28 C29 120.6(5) . . ?
F28 C28 C27 120.6(4) . . ?
C29 C28 C27 118.8(4) . . ?
F29 C29 C28 120.7(4) . . ?
F29 C29 C30 120.8(4) . . ?
C28 C29 C30 118.6(5) . . ?
F30 C30 C29 114.8(4) . . ?
F30 C30 C25 119.4(4) . . ?
C29 C30 C25 125.8(4) . . ?
C36 C31 C32 112.9(4) . . ?
C36 C31 B2 121.2(4) . . ?
C32 C31 B2 125.5(4) . . ?
F32 C32 C33 114.2(4) . . ?
F32 C32 C31 121.5(4) . . ?
C33 C32 C31 124.2(4) . . ?
F33 C33 C32 121.0(4) . . ?
F33 C33 C34 119.2(4) . . ?
C32 C33 C34 119.7(4) . . ?
F34 C34 C33 120.9(4) . . ?
F34 C34 C35 119.8(4) . . ?
C33 C34 C35 119.3(5) . . ?
F35 C35 C36 122.1(4) . . ?
F35 C35 C34 119.2(4) . . ?
C36 C35 C34 118.7(4) . . ?
F36 C36 C35 115.4(4) . . ?
F36 C36 C31 119.5(4) . . ?
C35 C36 C31 125.1(4) . . ?
C1 B1 C13 116.7(4) . . ?
C1 B1 C7 104.3(4) . . ?
C13 B1 C7 112.8(4) . . ?
C1 B1 P1 115.8(3) . . ?
C13 B1 P1 99.5(3) . . ?
C7 B1 P1 107.7(3) . . ?
C31 B2 C19 113.6(4) . . ?
C31 B2 C25 105.1(4) . . ?
C19 B2 C25 112.8(4) . . ?
C31 B2 P1 111.7(3) . . ?
C19 B2 P1 102.8(3) . . ?
C25 B2 P1 110.9(3) . . ?
B1 P1 B2 129.8(2) . . ?
B1 P1 H1A 104.8 . . ?
B2 P1 H1A 104.8 . . ?
B1 P1 H1B 104.8 . . ?
B2 P1 H1B 104.8 . . ?
H1A P1 H1B 105.8 . . ?
O41 C41 C42 108.4(4) . . ?
O41 C41 H41A 110.0 . . ?
C42 C41 H41A 110.0 . . ?
O41 C41 H41B 110.0 . . ?
C42 C41 H41B 110.0 . . ?
H41A C41 H41B 108.4 . . ?
O42 C42 C41 109.5(5) . . ?
O42 C42 H42A 109.8 . . ?
C41 C42 H42A 109.8 . . ?
O42 C42 H42B 109.8 . . ?
C41 C42 H42B 109.8 . . ?
H42A C42 H42B 108.2 . . ?
O42 C43 C44 104.7(4) . . ?
O42 C43 H43A 110.8 . . ?
C44 C43 H43A 110.8 . . ?
O42 C43 H43B 110.8 . . ?
C44 C43 H43B 110.8 . . ?
H43A C43 H43B 108.9 . . ?
O43 C44 C43 110.1(4) . . ?
O43 C44 H44A 109.6 . . ?
C43 C44 H44A 109.6 . . ?
O43 C44 H44B 109.6 . . ?
C43 C44 H44B 109.6 . . ?
H44A C44 H44B 108.2 . . ?
O43 C45 C46 105.6(5) . . ?
O43 C45 H45A 110.6 . . ?
C46 C45 H45A 110.6 . . ?
O43 C45 H45B 110.6 . . ?
C46 C45 H45B 110.6 . . ?
H45A C45 H45B 108.7 . . ?
O44 C46 C45 111.5(5) . . ?
O44 C46 H46A 109.3 . . ?
C45 C46 H46A 109.3 . . ?
O44 C46 H46B 109.3 . . ?
C45 C46 H46B 109.3 . . ?
H46A C46 H46B 108.0 . . ?
O44 C47 C48 105.5(4) . . ?
O44 C47 H47A 110.6 . . ?
C48 C47 H47A 110.6 . . ?
O44 C47 H47B 110.6 . . ?
C48 C47 H47B 110.6 . . ?
H47A C47 H47B 108.8 . . ?
O41 C48 C47 110.5(4) . . ?
O41 C48 H48A 109.6 . . ?
C47 C48 H48A 109.6 . . ?
O41 C48 H48B 109.6 . . ?
C47 C48 H48B 109.6 . . ?
H48A C48 H48B 108.1 . . ?
O42 Li41 O41 111.1(4) . 2_676 ?
O42 Li41 O44 127.9(4) . . ?
O41 Li41 O44 115.3(4) 2_676 . ?
O42 Li41 O43 82.9(4) . . ?
O41 Li41 O43 130.9(5) 2_676 . ?
O44 Li41 O43 84.3(4) . . ?
O42 Li41 O41 79.0(3) . . ?
O41 Li41 O41 91.9(4) 2_676 . ?
O44 Li41 O41 77.1(3) . . ?
O43 Li41 O41 137.2(4) . . ?
O42 Li41 Li41 95.2(4) . 2_676 ?
O41 Li41 Li41 50.6(3) 2_676 2_676 ?
O44 Li41 Li41 96.3(4) . 2_676 ?
O43 Li41 Li41 177.9(5) . 2_676 ?
O41 Li41 Li41 41.3(2) . 2_676 ?
C41 O41 C48 112.9(4) . . ?
C41 O41 Li41 125.8(4) . 2_676 ?
C48 O41 Li41 113.9(4) . 2_676 ?
C41 O41 Li41 104.0(4) . . ?
C48 O41 Li41 105.7(3) . . ?
Li41 O41 Li41 88.1(4) 2_676 . ?
C42 O42 C43 116.4(4) . . ?
C42 O42 Li41 115.5(4) . . ?
C43 O42 Li41 111.6(4) . . ?
C45 O43 C44 114.4(4) . . ?
C45 O43 Li41 109.8(4) . . ?
C44 O43 Li41 108.7(4) . . ?
C47 O44 C46 114.4(4) . . ?
C47 O44 Li41 112.9(4) . . ?
C46 O44 Li41 106.1(4) . . ?
 
_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.993
_refine_diff_density_max    0.631
_refine_diff_density_min   -0.355
_refine_diff_density_rms    0.077
