# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014











data_dw1269

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H28 Al Li O4'
_chemical_formula_sum            'C12 H28 Al Li O4'
_chemical_formula_weight         270.26

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   15.7387(4)
_cell_length_b                   11.7343(3)
_cell_length_c                   15.7462(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.603(2)
_cell_angle_gamma                90.00
_cell_volume                     2684.68(11)
_cell_formula_units_Z            6
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    8569
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            25789
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_theta_max         20.59
_reflns_number_total             2859
_reflns_number_gt                2749
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'

_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.

 The dataset used for this refinement is the best of THREE datasets collected
 from three different crystals.  In each case the crystal was twinned: the a
 and c axes are very similar in length, the twin law is ...

                            0   0   1
                            0  -1   0
                            1   0   0

 The refined 'BASF' is 0.43.  If the TWIN and BASF commands are not included
 in the SHELXL commands, the final R-factor is ca 28% (!)

 To further complicate matters, the three dioxane rings and two of the six
 tert-butyl groups in the asymmetric unit are disordered. Each disordered
 part was modelled over two sites, each site with 50% occupancy.

 Anisotropic displacement parameters were assigned to the Al and O atoms
 only. Each Li and C atom was assigned one of four common isotropic
 displacement parameters (one for the Li atoms, two for the t-Bu groups
 and one for the dioxane rings), a process which reduced the total number
 of LS parameters to 316 and significantly improved the parameter to data
 ratio.

 Two extra LS parameters (d1 and d2) were used to restrain the geometries
 of ALL t-Bu groups and dioxane rings.  All distances between adjacent atoms
 in these groups were constrained to be d(0.05)A and all distances between
 atoms once-removed were constrained to be 1.633*d(0.05) This process 
 ensured approximately tetrahedral geometry in these groups.

 Despite these problems, the six AL-H hydrogen atoms were all clearly visible
 in the final difference map (6 of the eight largest peaks in this map), and
 their positions were refined satisfactorily with weak bond length restraints
 (each distance restrained to be 1.79(0.05)A).

 2517 Friedel pairs were averaged for the refinement.  The R(merge) without
 Friedel averaging is 0.031 (with averaging is 0.032).
;

_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)+(0.2000P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(8)
_refine_ls_number_reflns         2859
_refine_ls_number_parameters     316
_refine_ls_number_restraints     121
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.1099
_refine_ls_wR_factor_ref         0.3309
_refine_ls_wR_factor_gt          0.3226
_refine_ls_goodness_of_fit_ref   1.742
_refine_ls_restrained_S_all      1.748
_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
Al10 Al 0.3310(2) -0.0046(7) 0.1889(2) 0.0662(11) Uani 1 1 d . . .
H10A H 0.3867 -0.1313 0.1731 0.079 Uiso 1 1 calc R . .
H10B H 0.3871 0.1198 0.1699 0.079 Uiso 1 1 calc R . .
Al30 Al 0.0516(3) -0.5048(7) 0.5188(2) 0.0771(13) Uani 1 1 d . A .
H30A H 0.0427 -0.3835 0.5838 0.093 Uiso 1 1 calc R . .
H30B H 0.0491 -0.6344 0.5777 0.093 Uiso 1 1 calc R . .
Al70 Al 0.2737(2) -0.5030(5) 0.0880(2) 0.0566(10) Uani 1 1 d . B .
H70A H 0.2206 -0.6268 0.1125 0.068 Uiso 1 1 calc R . .
H70B H 0.2199 -0.3759 0.1060 0.068 Uiso 1 1 calc R . .
Li10 Li 0.1826(11) -0.008(2) 0.2364(11) 0.051(2) Uiso 1 1 d . . .
Li30 Li 0.0672(11) -0.499(2) 0.3549(11) 0.051(2) Uiso 1 1 d . . .
Li70 Li 0.4136(11) -0.503(2) 0.0327(11) 0.051(2) Uiso 1 1 d . . .
O10 O 0.2099(4) -0.0047(9) 0.1258(3) 0.0452(16) Uani 1 1 d D . .
C10 C 0.1553(6) -0.0017(11) 0.0276(5) 0.0613(12) Uiso 1 1 d D . .
C11 C 0.1669(16) -0.1083(13) -0.0152(19) 0.1173(16) Uiso 1 1 d D . .
H11A H 0.2324 -0.1208 -0.0017 0.176 Uiso 1 1 calc R . .
H11B H 0.1331 -0.1036 -0.0820 0.176 Uiso 1 1 calc R . .
H11C H 0.1429 -0.1719 0.0093 0.176 Uiso 1 1 calc R . .
C12 C 0.1744(16) 0.0975(14) -0.0188(18) 0.1173(16) Uiso 1 1 d D . .
H12A H 0.2340 0.0875 -0.0240 0.176 Uiso 1 1 calc R . .
H12B H 0.1760 0.1664 0.0169 0.176 Uiso 1 1 calc R . .
H12C H 0.1260 0.1049 -0.0804 0.176 Uiso 1 1 calc R . .
C13 C 0.0571(8) 0.0062(19) 0.0169(12) 0.1173(16) Uiso 1 1 d D . .
H13A H 0.0512 0.0631 0.0599 0.176 Uiso 1 1 calc R . .
H13B H 0.0365 -0.0681 0.0300 0.176 Uiso 1 1 calc R . .
H13C H 0.0191 0.0289 -0.0463 0.176 Uiso 1 1 calc R . .
O20 O 0.3154(4) -0.0019(11) 0.2928(4) 0.0593(19) Uani 1 1 d D . .
C20 C 0.3802(6) 0.0042(11) 0.3877(5) 0.0613(12) Uiso 1 1 d D . .
C21 C 0.4467(13) 0.0960(15) 0.4018(16) 0.1173(16) Uiso 1 1 d D . .
H21A H 0.5061 0.0638 0.4074 0.176 Uiso 1 1 calc R . .
H21B H 0.4541 0.1376 0.4581 0.176 Uiso 1 1 calc R . .
H21C H 0.4247 0.1483 0.3492 0.176 Uiso 1 1 calc R . .
C22 C 0.3298(12) 0.0203(15) 0.4492(12) 0.1173(16) Uiso 1 1 d D . .
H22A H 0.2799 -0.0356 0.4339 0.176 Uiso 1 1 calc R . .
H22B H 0.3040 0.0974 0.4412 0.176 Uiso 1 1 calc R . .
H22C H 0.3722 0.0099 0.5133 0.176 Uiso 1 1 calc R . .
C23 C 0.4280(15) -0.1066(13) 0.4100(17) 0.1173(16) Uiso 1 1 d D . .
H23A H 0.4588 -0.1212 0.3676 0.176 Uiso 1 1 calc R . .
H23B H 0.3831 -0.1672 0.4039 0.176 Uiso 1 1 calc R . .
H23C H 0.4737 -0.1050 0.4733 0.176 Uiso 1 1 calc R . .
O30 O 0.1432(5) -0.4967(13) 0.4822(6) 0.076(2) Uani 1 1 d D A .
C30 C 0.2419(5) -0.5110(10) 0.5342(6) 0.0613(12) Uiso 1 1 d D . .
C31 C 0.2741(16) -0.4248(12) 0.6061(11) 0.1173(16) Uiso 1 1 d D . .
H31A H 0.2592 -0.4484 0.6585 0.176 Uiso 1 1 calc R . .
H31B H 0.2438 -0.3520 0.5821 0.176 Uiso 1 1 calc R . .
H31C H 0.3409 -0.4159 0.6261 0.176 Uiso 1 1 calc R . .
C32 C 0.2859(13) -0.4970(17) 0.4681(10) 0.1173(16) Uiso 1 1 d D . .
H32A H 0.2629 -0.5554 0.4201 0.176 Uiso 1 1 calc R . .
H32B H 0.3527 -0.5051 0.4999 0.176 Uiso 1 1 calc R . .
H32C H 0.2717 -0.4213 0.4400 0.176 Uiso 1 1 calc R . .
C33 C 0.2630(16) -0.6253(10) 0.5752(12) 0.1173(16) Uiso 1 1 d D . .
H33A H 0.2520 -0.6272 0.6324 0.176 Uiso 1 1 calc R . .
H33B H 0.3277 -0.6435 0.5886 0.176 Uiso 1 1 calc R . .
H33C H 0.2235 -0.6816 0.5320 0.176 Uiso 1 1 calc R . .
O40 O -0.0287(4) -0.5025(10) 0.4002(4) 0.0526(17) Uani 1 1 d D A .
C40 C -0.1299(5) -0.5029(12) 0.3619(6) 0.0613(12) Uiso 1 1 d D . .
C41 C -0.159(3) -0.605(2) 0.397(3) 0.1173(16) Uiso 0.50 1 d PD A 1
H41A H -0.1142 -0.6231 0.4588 0.176 Uiso 0.50 1 calc PR A 1
H41B H -0.1644 -0.6696 0.3559 0.176 Uiso 0.50 1 calc PR A 1
H41C H -0.2195 -0.5911 0.4005 0.176 Uiso 0.50 1 calc PR A 1
C42 C -0.170(3) -0.402(2) 0.389(3) 0.1173(16) Uiso 0.50 1 d PD A 1
H42A H -0.1515 -0.4013 0.4558 0.176 Uiso 0.50 1 calc PR A 1
H42B H -0.2368 -0.4042 0.3588 0.176 Uiso 0.50 1 calc PR A 1
H42C H -0.1467 -0.3324 0.3700 0.176 Uiso 0.50 1 calc PR A 1
C43 C -0.160(2) -0.508(4) 0.2625(9) 0.1173(16) Uiso 0.50 1 d PD A 1
H43A H -0.1498 -0.4338 0.2393 0.176 Uiso 0.50 1 calc PR A 1
H43B H -0.2251 -0.5277 0.2350 0.176 Uiso 0.50 1 calc PR A 1
H43C H -0.1238 -0.5663 0.2461 0.176 Uiso 0.50 1 calc PR A 1
C41' C -0.168(3) -0.530(3) 0.4302(19) 0.1173(16) Uiso 0.50 1 d PD A 2
H41D H -0.2179 -0.4762 0.4243 0.176 Uiso 0.50 1 calc PR A 2
H41E H -0.1199 -0.5237 0.4919 0.176 Uiso 0.50 1 calc PR A 2
H41F H -0.1927 -0.6077 0.4203 0.176 Uiso 0.50 1 calc PR A 2
C42' C -0.168(3) -0.396(2) 0.315(2) 0.1173(16) Uiso 0.50 1 d PD A 2
H42D H -0.1279 -0.3326 0.3476 0.176 Uiso 0.50 1 calc PR A 2
H42E H -0.2295 -0.3845 0.3145 0.176 Uiso 0.50 1 calc PR A 2
H42F H -0.1709 -0.3991 0.2517 0.176 Uiso 0.50 1 calc PR A 2
C43' C -0.151(3) -0.596(2) 0.294(2) 0.1173(16) Uiso 0.50 1 d PD A 2
H43D H -0.1088 -0.5912 0.2613 0.176 Uiso 0.50 1 calc PR A 2
H43E H -0.2143 -0.5889 0.2498 0.176 Uiso 0.50 1 calc PR A 2
H43F H -0.1424 -0.6694 0.3257 0.176 Uiso 0.50 1 calc PR A 2
O50 O 0.2823(4) -0.5079(11) -0.0184(4) 0.0600(19) Uani 1 1 d D B .
C50 C 0.2126(6) -0.4981(11) -0.1119(5) 0.0613(12) Uiso 1 1 d D . .
C51 C 0.2257(16) -0.3958(13) -0.1594(16) 0.1173(16) Uiso 1 1 d D C .
H51A H 0.2787 -0.4069 -0.1767 0.176 Uiso 1 1 calc R . .
H51B H 0.2368 -0.3299 -0.1183 0.176 Uiso 1 1 calc R . .
H51C H 0.1704 -0.3824 -0.2148 0.176 Uiso 1 1 calc R . .
C52 C 0.2225(17) -0.6015(13) -0.1603(17) 0.1173(16) Uiso 1 1 d D C .
H52A H 0.2787 -0.5960 -0.1729 0.176 Uiso 1 1 calc R . .
H52B H 0.1691 -0.6090 -0.2184 0.176 Uiso 1 1 calc R . .
H52C H 0.2263 -0.6684 -0.1217 0.176 Uiso 1 1 calc R . .
C53 C 0.1212(9) -0.495(2) -0.1083(13) 0.1173(16) Uiso 1 1 d D C .
H53A H 0.1155 -0.4273 -0.0749 0.176 Uiso 1 1 calc R . .
H53B H 0.1125 -0.5636 -0.0767 0.176 Uiso 1 1 calc R . .
H53C H 0.0742 -0.4934 -0.1710 0.176 Uiso 1 1 calc R . .
O60 O 0.3949(4) -0.5020(11) 0.1449(4) 0.0518(17) Uani 1 1 d D B .
C60 C 0.4563(6) -0.5044(12) 0.2418(5) 0.0613(12) Uiso 1 1 d D . .
C61 C 0.5480(14) -0.479(3) 0.244(3) 0.1173(16) Uiso 0.50 1 d PD B 1
H61A H 0.5724 -0.4112 0.2816 0.176 Uiso 0.50 1 calc PR B 1
H61B H 0.5442 -0.4654 0.1812 0.176 Uiso 0.50 1 calc PR B 1
H61C H 0.5889 -0.5440 0.2704 0.176 Uiso 0.50 1 calc PR B 1
C62 C 0.458(2) -0.6109(19) 0.290(3) 0.1173(16) Uiso 0.50 1 d PD B 1
H62A H 0.3948 -0.6337 0.2798 0.176 Uiso 0.50 1 calc PR B 1
H62B H 0.4929 -0.6001 0.3562 0.176 Uiso 0.50 1 calc PR B 1
H62C H 0.4871 -0.6704 0.2671 0.176 Uiso 0.50 1 calc PR B 1
C63 C 0.426(2) -0.411(2) 0.286(3) 0.1173(16) Uiso 0.50 1 d PD B 1
H63A H 0.3639 -0.4275 0.2833 0.176 Uiso 0.50 1 calc PR B 1
H63B H 0.4254 -0.3395 0.2539 0.176 Uiso 0.50 1 calc PR B 1
H63C H 0.4684 -0.4045 0.3505 0.176 Uiso 0.50 1 calc PR B 1
C61' C 0.524(2) -0.596(2) 0.249(3) 0.1173(16) Uiso 0.50 1 d PD B 2
H61D H 0.4905 -0.6668 0.2227 0.176 Uiso 0.50 1 calc PR B 2
H61E H 0.5632 -0.6085 0.3134 0.176 Uiso 0.50 1 calc PR B 2
H61F H 0.5614 -0.5739 0.2144 0.176 Uiso 0.50 1 calc PR B 2
C62' C 0.408(2) -0.535(2) 0.302(2) 0.1173(16) Uiso 0.50 1 d PD B 2
H62D H 0.3505 -0.4915 0.2837 0.176 Uiso 0.50 1 calc PR B 2
H62E H 0.4472 -0.5162 0.3659 0.176 Uiso 0.50 1 calc PR B 2
H62F H 0.3945 -0.6164 0.2968 0.176 Uiso 0.50 1 calc PR B 2
C63' C 0.507(2) -0.397(2) 0.273(3) 0.1173(16) Uiso 0.50 1 d PD B 2
H63D H 0.4797 -0.3543 0.3095 0.176 Uiso 0.50 1 calc PR B 2
H63E H 0.5035 -0.3522 0.2194 0.176 Uiso 0.50 1 calc PR B 2
H63F H 0.5715 -0.4143 0.3108 0.176 Uiso 0.50 1 calc PR B 2
O71 O 0.1245(7) -0.8635(4) 0.2555(7) 0.068(4) Uani 0.50 1 d PD . 1
C72 C 0.0643(13) -0.8431(4) 0.3054(13) 0.0518(12) Uiso 0.50 1 d PD . 1
H72A H 0.0706 -0.9061 0.3492 0.062 Uiso 0.50 1 calc PR . 1
H72B H -0.0006 -0.8399 0.2616 0.062 Uiso 0.50 1 calc PR . 1
C73 C 0.0902(12) -0.7344(7) 0.3557(8) 0.0518(12) Uiso 0.50 1 d PD . 1
H73A H 0.1557 -0.7363 0.3978 0.062 Uiso 0.50 1 calc PR . 1
H73B H 0.0524 -0.7217 0.3927 0.062 Uiso 0.50 1 calc PR . 1
O74 O 0.0744(7) -0.6415(4) 0.2878(8) 0.073(4) Uani 0.50 1 d PD . 1
C75 C 0.1308(13) -0.6621(4) 0.2342(11) 0.0518(12) Uiso 0.50 1 d PD . 1
H75A H 0.1202 -0.6007 0.1881 0.062 Uiso 0.50 1 calc PR . 1
H75B H 0.1967 -0.6609 0.2754 0.062 Uiso 0.50 1 calc PR . 1
C76 C 0.1083(14) -0.7713(8) 0.1877(9) 0.0518(12) Uiso 0.50 1 d PD . 1
H76A H 0.1468 -0.7837 0.1515 0.062 Uiso 0.50 1 calc PR . 1
H76B H 0.0429 -0.7717 0.1449 0.062 Uiso 0.50 1 calc PR . 1
O71' O 0.1245(7) -0.8635(4) 0.2555(7) 0.068(4) Uani 0.50 1 d PD . 2
C72' C 0.1035(15) -0.8358(7) 0.3368(11) 0.0518(12) Uiso 0.50 1 d PD . 2
H72C H 0.1597 -0.8093 0.3878 0.062 Uiso 0.50 1 calc PR . 2
H72D H 0.0801 -0.9043 0.3576 0.062 Uiso 0.50 1 calc PR . 2
C73' C 0.0325(11) -0.7446(7) 0.3100(12) 0.0518(12) Uiso 0.50 1 d PD . 2
H73C H -0.0219 -0.7687 0.2557 0.062 Uiso 0.50 1 calc PR . 2
H73D H 0.0125 -0.7286 0.3612 0.062 Uiso 0.50 1 calc PR . 2
O74' O 0.0744(7) -0.6415(4) 0.2878(8) 0.073(4) Uani 0.50 1 d PD . 2
C75' C 0.0966(13) -0.6691(6) 0.2063(11) 0.0518(12) Uiso 0.50 1 d PD . 2
H75C H 0.1207 -0.6009 0.1860 0.062 Uiso 0.50 1 calc PR . 2
H75D H 0.0408 -0.6956 0.1547 0.062 Uiso 0.50 1 calc PR . 2
C76' C 0.1675(11) -0.7608(8) 0.2351(14) 0.0518(12) Uiso 0.50 1 d PD . 2
H76C H 0.1893 -0.7770 0.1852 0.062 Uiso 0.50 1 calc PR . 2
H76D H 0.2208 -0.7369 0.2904 0.062 Uiso 0.50 1 calc PR . 2
O81 O 0.1255(6) -0.1425(3) 0.2563(7) 0.057(3) Uani 0.50 1 d PD . 1
C82 C 0.0472(12) -0.1622(5) 0.2832(14) 0.0518(12) Uiso 0.50 1 d PD . 1
H82A H 0.0400 -0.0964 0.3191 0.062 Uiso 0.50 1 calc PR . 1
H82B H -0.0099 -0.1696 0.2274 0.062 Uiso 0.50 1 calc PR . 1
C83 C 0.0615(12) -0.2650(7) 0.3380(11) 0.0518(12) Uiso 0.50 1 d PD . 1
H83A H 0.0080 -0.2781 0.3552 0.062 Uiso 0.50 1 calc PR . 1
H83B H 0.1170 -0.2565 0.3952 0.062 Uiso 0.50 1 calc PR . 1
O84 O 0.0730(8) -0.3634(4) 0.2845(9) 0.085(5) Uani 0.50 1 d PD . 1
C85 C 0.1551(11) -0.3432(5) 0.2632(13) 0.0518(12) Uiso 0.50 1 d PD . 1
H85A H 0.2100 -0.3362 0.3212 0.062 Uiso 0.50 1 calc PR . 1
H85B H 0.1647 -0.4087 0.2283 0.062 Uiso 0.50 1 calc PR . 1
C86 C 0.1441(13) -0.2404(7) 0.2098(12) 0.0518(12) Uiso 0.50 1 d PD . 1
H86A H 0.0927 -0.2505 0.1495 0.062 Uiso 0.50 1 calc PR . 1
H86B H 0.2008 -0.2263 0.1985 0.062 Uiso 0.50 1 calc PR . 1
O81' O 0.1255(6) -0.1425(3) 0.2563(7) 0.057(3) Uani 0.50 1 d PD . 2
C82' C 0.0910(14) -0.1669(7) 0.3287(12) 0.0518(12) Uiso 0.50 1 d PD . 2
H82C H 0.0616 -0.0982 0.3417 0.062 Uiso 0.50 1 calc PR . 2
H82D H 0.1424 -0.1900 0.3859 0.062 Uiso 0.50 1 calc PR . 2
C83' C 0.0222(10) -0.2614(7) 0.2953(14) 0.0518(12) Uiso 0.50 1 d PD . 2
H83C H -0.0062 -0.2767 0.3404 0.062 Uiso 0.50 1 calc PR . 2
H83D H -0.0270 -0.2407 0.2357 0.062 Uiso 0.50 1 calc PR . 2
O84' O 0.0730(8) -0.3634(4) 0.2845(9) 0.085(5) Uani 0.50 1 d PD . 2
C85' C 0.1062(14) -0.3383(6) 0.2100(13) 0.0518(12) Uiso 0.50 1 d PD . 2
H85C H 0.1360 -0.4065 0.1966 0.062 Uiso 0.50 1 calc PR . 2
H85D H 0.0540 -0.3159 0.1531 0.062 Uiso 0.50 1 calc PR . 2
C86' C 0.1734(11) -0.2435(8) 0.2423(15) 0.0518(12) Uiso 0.50 1 d PD . 2
H86C H 0.2241 -0.2649 0.3007 0.062 Uiso 0.50 1 calc PR . 2
H86D H 0.2001 -0.2271 0.1960 0.062 Uiso 0.50 1 calc PR . 2
O91 O 0.4655(6) -0.3624(5) 0.0059(8) 0.074(4) Uani 0.50 1 d PD C 1
C92 C 0.5057(12) -0.3388(6) -0.0625(12) 0.0518(12) Uiso 0.50 1 d PD C 1
H92A H 0.4572 -0.3125 -0.1208 0.062 Uiso 0.50 1 calc PR C 1
H92B H 0.5337 -0.4089 -0.0753 0.062 Uiso 0.50 1 calc PR C 1
C93 C 0.5767(9) -0.2493(7) -0.0253(12) 0.0518(12) Uiso 0.50 1 d PD C 1
H93A H 0.6072 -0.2342 -0.0687 0.062 Uiso 0.50 1 calc PR C 1
H93B H 0.6241 -0.2741 0.0342 0.062 Uiso 0.50 1 calc PR C 1
O94 O 0.5300(6) -0.1446(4) -0.0122(7) 0.060(3) Uani 0.50 1 d PD . 1
C95 C 0.4943(11) -0.1703(7) 0.0608(11) 0.0518(12) Uiso 0.50 1 d PD C 1
H95A H 0.5445 -0.1987 0.1169 0.062 Uiso 0.50 1 calc PR C 1
H95B H 0.4680 -0.1008 0.0768 0.062 Uiso 0.50 1 calc PR C 1
C96 C 0.4218(10) -0.2591(8) 0.0229(14) 0.0518(12) Uiso 0.50 1 d PD C 1
H96A H 0.3928 -0.2755 0.0673 0.062 Uiso 0.50 1 calc PR C 1
H96B H 0.3735 -0.2320 -0.0352 0.062 Uiso 0.50 1 calc PR C 1
O91' O 0.4655(6) -0.3624(5) 0.0059(8) 0.074(4) Uani 0.50 1 d PD C 2
C92' C 0.5516(10) -0.3469(5) -0.0061(14) 0.0518(12) Uiso 0.50 1 d PD C 2
H92C H 0.6027 -0.3434 0.0551 0.062 Uiso 0.50 1 calc PR C 2
H92D H 0.5624 -0.4135 -0.0393 0.062 Uiso 0.50 1 calc PR C 2
C93' C 0.5522(10) -0.2454(6) -0.0562(12) 0.0518(12) Uiso 0.50 1 d PD C 2
H93C H 0.5065 -0.2525 -0.1201 0.062 Uiso 0.50 1 calc PR C 2
H93D H 0.6137 -0.2353 -0.0586 0.062 Uiso 0.50 1 calc PR C 2
O94' O 0.5300(6) -0.1446(4) -0.0122(7) 0.060(3) Uani 0.50 1 d PD . 2
C95' C 0.4350(9) -0.1622(6) -0.0143(12) 0.0518(12) Uiso 0.50 1 d PD C 2
H95C H 0.4142 -0.0936 0.0089 0.062 Uiso 0.50 1 calc PR C 2
H95D H 0.3912 -0.1773 -0.0780 0.062 Uiso 0.50 1 calc PR C 2
C96' C 0.4393(11) -0.2614(7) 0.0454(12) 0.0518(12) Uiso 0.50 1 d PD C 2
H96C H 0.4853 -0.2474 0.1083 0.062 Uiso 0.50 1 calc PR C 2
H96D H 0.3787 -0.2737 0.0492 0.062 Uiso 0.50 1 calc PR C 2


_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
Al10 O20 1.745(7) . ?
Al10 O10 1.780(7) . ?
Al10 Li10 2.713(17) . ?
Al10 H10A 1.7900 . ?
Al10 H10B 1.7900 . ?
Al30 O30 1.748(7) . ?
Al30 O40 1.808(7) . ?
Al30 Li30 2.686(17) . ?
Al30 H30A 1.7900 . ?
Al30 H30B 1.7900 . ?
Al70 O50 1.733(6) . ?
Al70 O60 1.769(6) . ?
Al70 Li70 2.662(16) . ?
Al70 H70A 1.7900 . ?
Al70 H70B 1.7900 . ?
Li10 O81 1.90(2) . ?
Li10 O20 1.932(16) . ?
Li10 O10 1.948(16) . ?
Li10 O71' 2.00(2) 1_565 ?
Li10 O71 2.00(2) 1_565 ?
Li10 C86' 2.77(3) . ?
Li30 O30 1.899(17) . ?
Li30 O40 1.902(16) . ?
Li30 O84 1.96(2) . ?
Li30 O74 2.01(2) . ?
Li30 C83 2.75(3) . ?
Li70 O60 1.901(15) . ?
Li70 O50 1.909(16) . ?
Li70 O91 1.95(2) . ?
Li70 O94' 1.97(2) 2_645 ?
Li70 O94 1.97(2) 2_645 ?
O10 C10 1.452(8) . ?
C10 C11 1.466(9) . ?
C10 C12 1.466(9) . ?
C10 C13 1.491(9) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
O20 C20 1.452(8) . ?
C20 C21 1.459(9) . ?
C20 C23 1.475(9) . ?
C20 C22 1.480(9) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O30 C30 1.461(8) . ?
C30 C31 1.457(9) . ?
C30 C32 1.465(9) . ?
C30 C33 1.471(9) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O40 C40 1.471(8) . ?
C40 C43 1.452(10) . ?
C40 C41' 1.456(10) . ?
C40 C42' 1.461(10) . ?
C40 C41 1.472(10) . ?
C40 C43' 1.473(10) . ?
C40 C42 1.479(10) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C41' H41D 0.9800 . ?
C41' H41E 0.9800 . ?
C41' H41F 0.9800 . ?
C42' H42D 0.9800 . ?
C42' H42E 0.9800 . ?
C42' H42F 0.9800 . ?
C43' H43D 0.9800 . ?
C43' H43E 0.9800 . ?
C43' H43F 0.9800 . ?
O50 C50 1.464(8) . ?
C50 C53 1.463(9) . ?
C50 C51 1.470(9) . ?
C50 C52 1.472(9) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
O60 C60 1.459(8) . ?
C60 C62 1.458(10) . ?
C60 C61 1.462(10) . ?
C60 C62' 1.467(10) . ?
C60 C63' 1.467(10) . ?
C60 C63 1.471(10) . ?
C60 C61' 1.485(10) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C61' H61D 0.9800 . ?
C61' H61E 0.9800 . ?
C61' H61F 0.9800 . ?
C62' H62D 0.9800 . ?
C62' H62E 0.9800 . ?
C62' H62F 0.9800 . ?
C63' H63D 0.9800 . ?
C63' H63E 0.9800 . ?
C63' H63F 0.9800 . ?
O71 C72 1.465(10) . ?
O71 C76 1.471(10) . ?
O71 Li10 2.00(2) 1_545 ?
C72 C73 1.473(9) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 O74 1.479(9) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
O74 C75 1.462(9) . ?
C75 C76 1.450(9) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C72' C73' 1.486(10) . ?
C72' H72C 0.9900 . ?
C72' H72D 0.9900 . ?
C73' H73C 0.9900 . ?
C73' H73D 0.9900 . ?
C75' C76' 1.490(10) . ?
C75' H75C 0.9900 . ?
C75' H75D 0.9900 . ?
C76' H76C 0.9900 . ?
C76' H76D 0.9900 . ?
O81 C86 1.451(10) . ?
O81 C82 1.467(10) . ?
C82 C83 1.450(9) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 O84 1.480(9) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
O84 C85 1.474(9) . ?
C85 C86 1.442(9) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C82' C83' 1.496(10) . ?
C82' H82C 0.9900 . ?
C82' H82D 0.9900 . ?
C83' H83C 0.9900 . ?
C83' H83D 0.9900 . ?
C85' C86' 1.484(10) . ?
C85' H85C 0.9900 . ?
C85' H85D 0.9900 . ?
C86' H86C 0.9900 . ?
C86' H86D 0.9900 . ?
O91 C96 1.468(10) . ?
O91 C92 1.471(10) . ?
C92 C93 1.481(10) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 O94 1.486(9) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
O94 C95 1.491(9) . ?
O94 Li70 1.97(2) 2_655 ?
C95 C96 1.489(10) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C96 H96A 0.9900 . ?
C96 H96B 0.9900 . ?
C92' C93' 1.431(9) . ?
C92' H92C 0.9900 . ?
C92' H92D 0.9900 . ?
C93' H93C 0.9900 . ?
C93' H93D 0.9900 . ?
C95' C96' 1.481(9) . ?
C95' H95C 0.9900 . ?
C95' H95D 0.9900 . ?
C96' H96C 0.9900 . ?
C96' H96D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O20 Al10 O10 91.0(3) . . ?
O20 Al10 Li10 45.2(4) . . ?
O10 Al10 Li10 45.8(3) . . ?
O20 Al10 H10A 113.5 . . ?
O10 Al10 H10A 113.5 . . ?
Li10 Al10 H10A 123.1 . . ?
O20 Al10 H10B 113.5 . . ?
O10 Al10 H10B 113.5 . . ?
Li10 Al10 H10B 126.1 . . ?
H10A Al10 H10B 110.8 . . ?
O30 Al30 O40 89.8(4) . . ?
O30 Al30 Li30 44.8(4) . . ?
O40 Al30 Li30 45.0(4) . . ?
O30 Al30 H30A 113.7 . . ?
O40 Al30 H30A 113.7 . . ?
Li30 Al30 H30A 125.8 . . ?
O30 Al30 H30B 113.7 . . ?
O40 Al30 H30B 113.7 . . ?
Li30 Al30 H30B 123.3 . . ?
H30A Al30 H30B 110.9 . . ?
O50 Al70 O60 91.2(3) . . ?
O50 Al70 Li70 45.7(4) . . ?
O60 Al70 Li70 45.5(4) . . ?
O50 Al70 H70A 113.4 . . ?
O60 Al70 H70A 113.4 . . ?
Li70 Al70 H70A 125.8 . . ?
O50 Al70 H70B 113.4 . . ?
O60 Al70 H70B 113.4 . . ?
Li70 Al70 H70B 123.5 . . ?
H70A Al70 H70B 110.7 . . ?
O81 Li10 O20 116.8(11) . . ?
O81 Li10 O10 116.3(12) . . ?
O20 Li10 O10 80.7(7) . . ?
O81 Li10 O71' 114.0(8) . 1_565 ?
O20 Li10 O71' 112.1(11) . 1_565 ?
O10 Li10 O71' 112.9(11) . 1_565 ?
O81 Li10 O71 114.0(8) . 1_565 ?
O20 Li10 O71 112.1(11) . 1_565 ?
O10 Li10 O71 112.9(11) . 1_565 ?
O71' Li10 O71 0.0(5) 1_565 1_565 ?
O81 Li10 Al10 124.6(11) . . ?
O20 Li10 Al10 39.8(4) . . ?
O10 Li10 Al10 40.9(4) . . ?
O71' Li10 Al10 121.4(10) 1_565 . ?
O71 Li10 Al10 121.4(10) 1_565 . ?
O81 Li10 C86' 29.8(4) . . ?
O20 Li10 C86' 94.7(9) . . ?
O10 Li10 C86' 94.6(10) . . ?
O71' Li10 C86' 143.8(8) 1_565 . ?
O71 Li10 C86' 143.8(8) 1_565 . ?
Al10 Li10 C86' 94.8(7) . . ?
O30 Li30 O40 82.7(7) . . ?
O30 Li30 O84 116.2(13) . . ?
O40 Li30 O84 116.6(12) . . ?
O30 Li30 O74 115.1(12) . . ?
O40 Li30 O74 113.0(11) . . ?
O84 Li30 O74 110.8(8) . . ?
O30 Li30 Al30 40.4(4) . . ?
O40 Li30 Al30 42.3(4) . . ?
O84 Li30 Al30 127.4(11) . . ?
O74 Li30 Al30 121.8(10) . . ?
O30 Li30 C83 94.3(11) . . ?
O40 Li30 C83 93.4(9) . . ?
O84 Li30 C83 31.2(5) . . ?
O74 Li30 C83 142.0(9) . . ?
Al30 Li30 C83 96.2(7) . . ?
O60 Li70 O50 82.1(6) . . ?
O60 Li70 O91 115.1(13) . . ?
O50 Li70 O91 114.2(12) . . ?
O60 Li70 O94' 113.3(12) . 2_645 ?
O50 Li70 O94' 112.8(13) . 2_645 ?
O91 Li70 O94' 115.1(8) . 2_645 ?
O60 Li70 O94 113.3(12) . 2_645 ?
O50 Li70 O94 112.8(13) . 2_645 ?
O91 Li70 O94 115.1(8) . 2_645 ?
O94' Li70 O94 0.0(5) 2_645 2_645 ?
O60 Li70 Al70 41.6(3) . . ?
O50 Li70 Al70 40.5(4) . . ?
O91 Li70 Al70 122.6(11) . . ?
O94' Li70 Al70 122.3(11) 2_645 . ?
O94 Li70 Al70 122.3(11) 2_645 . ?
C10 O10 Al10 131.6(5) . . ?
C10 O10 Li10 135.1(7) . . ?
Al10 O10 Li10 93.3(5) . . ?
O10 C10 C11 110.0(15) . . ?
O10 C10 C12 113.5(14) . . ?
C11 C10 C12 111.2(8) . . ?
O10 C10 C13 106.6(9) . . ?
C11 C10 C13 107.9(8) . . ?
C12 C10 C13 107.2(8) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C20 O20 Al10 132.1(5) . . ?
C20 O20 Li10 133.0(7) . . ?
Al10 O20 Li10 95.0(6) . . ?
O20 C20 C21 111.8(13) . . ?
O20 C20 C23 107.1(13) . . ?
C21 C20 C23 110.1(8) . . ?
O20 C20 C22 109.8(10) . . ?
C21 C20 C22 109.9(8) . . ?
C23 C20 C22 108.0(8) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C30 O30 Al30 130.0(7) . . ?
C30 O30 Li30 133.9(7) . . ?
Al30 O30 Li30 94.7(6) . . ?
C31 C30 O30 109.5(13) . . ?
C31 C30 C32 110.9(8) . . ?
O30 C30 C32 106.3(10) . . ?
C31 C30 C33 109.9(8) . . ?
O30 C30 C33 111.3(13) . . ?
C32 C30 C33 109.0(8) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C40 O40 Al30 129.9(5) . . ?
C40 O40 Li30 137.4(8) . . ?
Al30 O40 Li30 92.7(6) . . ?
C43 C40 C41' 137(2) . . ?
C43 C40 C42' 65.9(19) . . ?
C41' C40 C42' 110.8(10) . . ?
C43 C40 O40 107.0(15) . . ?
C41' C40 O40 112.9(17) . . ?
C42' C40 O40 112(2) . . ?
C43 C40 C41 110.9(10) . . ?
C41' C40 C41 42.5(15) . . ?
C42' C40 C41 140(2) . . ?
O40 C40 C41 107(2) . . ?
C43 C40 C43' 45.4(18) . . ?
C41' C40 C43' 109.7(10) . . ?
C42' C40 C43' 109.7(9) . . ?
O40 C40 C43' 101.7(19) . . ?
C41 C40 C43' 69.9(16) . . ?
C43 C40 C42 110.3(9) . . ?
C41' C40 C42 67.7(16) . . ?
C42' C40 C42 47.2(17) . . ?
O40 C40 C42 113(2) . . ?
C41 C40 C42 108.4(9) . . ?
C43' C40 C42 143(2) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C40 C41' H41D 109.5 . . ?
C40 C41' H41E 109.5 . . ?
H41D C41' H41E 109.5 . . ?
C40 C41' H41F 109.5 . . ?
H41D C41' H41F 109.5 . . ?
H41E C41' H41F 109.5 . . ?
C40 C42' H42D 109.5 . . ?
C40 C42' H42E 109.5 . . ?
H42D C42' H42E 109.5 . . ?
C40 C42' H42F 109.5 . . ?
H42D C42' H42F 109.5 . . ?
H42E C42' H42F 109.5 . . ?
C40 C43' H43D 109.5 . . ?
C40 C43' H43E 109.5 . . ?
H43D C43' H43E 109.5 . . ?
C40 C43' H43F 109.5 . . ?
H43D C43' H43F 109.5 . . ?
H43E C43' H43F 109.5 . . ?
C50 O50 Al70 131.6(5) . . ?
C50 O50 Li70 133.8(7) . . ?
Al70 O50 Li70 93.8(5) . . ?
C53 C50 O50 109.3(9) . . ?
C53 C50 C51 109.5(8) . . ?
O50 C50 C51 112.2(14) . . ?
C53 C50 C52 109.9(8) . . ?
O50 C50 C52 105.6(14) . . ?
C51 C50 C52 110.3(7) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C60 O60 Al70 132.9(5) . . ?
C60 O60 Li70 134.1(7) . . ?
Al70 O60 Li70 92.9(5) . . ?
C62 C60 O60 115.7(19) . . ?
C62 C60 C61 110.1(10) . . ?
O60 C60 C61 105.7(16) . . ?
C62 C60 C62' 50.6(17) . . ?
O60 C60 C62' 112.4(16) . . ?
C61 C60 C62' 142(2) . . ?
C62 C60 C63' 131(2) . . ?
O60 C60 C63' 112.9(18) . . ?
C61 C60 C63' 54.1(18) . . ?
C62' C60 C63' 109.9(10) . . ?
C62 C60 C63 109.5(9) . . ?
O60 C60 C63 106.0(18) . . ?
C61 C60 C63 109.6(9) . . ?
C62' C60 C63 62.1(17) . . ?
C63' C60 C63 55.9(18) . . ?
C62 C60 C61' 58.1(17) . . ?
O60 C60 C61' 104.9(18) . . ?
C61 C60 C61' 58.3(18) . . ?
C62' C60 C61' 108.0(9) . . ?
C63' C60 C61' 108.4(9) . . ?
C63 C60 C61' 149(2) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 H62A 109.5 . . ?
C60 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C60 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C60 C63 H63A 109.5 . . ?
C60 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C60 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C60 C61' H61D 109.5 . . ?
C60 C61' H61E 109.5 . . ?
H61D C61' H61E 109.5 . . ?
C60 C61' H61F 109.5 . . ?
H61D C61' H61F 109.5 . . ?
H61E C61' H61F 109.5 . . ?
C60 C62' H62D 109.5 . . ?
C60 C62' H62E 109.5 . . ?
H62D C62' H62E 109.5 . . ?
C60 C62' H62F 109.5 . . ?
H62D C62' H62F 109.5 . . ?
H62E C62' H62F 109.5 . . ?
C60 C63' H63D 109.5 . . ?
C60 C63' H63E 109.5 . . ?
H63D C63' H63E 109.5 . . ?
C60 C63' H63F 109.5 . . ?
H63D C63' H63F 109.5 . . ?
H63E C63' H63F 109.5 . . ?
C72 O71 C76 107.6(8) . . ?
C72 O71 Li10 130.2(7) . 1_545 ?
C76 O71 Li10 118.4(7) . 1_545 ?
O71 C72 C73 109.1(7) . . ?
O71 C72 H72A 109.9 . . ?
C73 C72 H72A 109.9 . . ?
O71 C72 H72B 109.9 . . ?
C73 C72 H72B 109.9 . . ?
H72A C72 H72B 108.3 . . ?
C72 C73 O74 108.4(7) . . ?
C72 C73 H73A 110.0 . . ?
O74 C73 H73A 110.0 . . ?
C72 C73 H73B 110.0 . . ?
O74 C73 H73B 110.0 . . ?
H73A C73 H73B 108.4 . . ?
C75 O74 C73 109.0(6) . . ?
C75 O74 Li30 127.7(7) . . ?
C73 O74 Li30 105.3(8) . . ?
C76 C75 O74 110.6(7) . . ?
C76 C75 H75A 109.5 . . ?
O74 C75 H75A 109.5 . . ?
C76 C75 H75B 109.5 . . ?
O74 C75 H75B 109.5 . . ?
H75A C75 H75B 108.1 . . ?
C75 C76 O71 110.1(7) . . ?
C75 C76 H76A 109.6 . . ?
O71 C76 H76A 109.6 . . ?
C75 C76 H76B 109.6 . . ?
O71 C76 H76B 109.6 . . ?
H76A C76 H76B 108.2 . . ?
C73' C72' H72C 110.1 . . ?
C73' C72' H72D 110.1 . . ?
H72C C72' H72D 108.5 . . ?
C72' C73' H73C 110.2 . . ?
C72' C73' H73D 110.2 . . ?
H73C C73' H73D 108.5 . . ?
C76' C75' H75C 110.3 . . ?
C76' C75' H75D 110.3 . . ?
H75C C75' H75D 108.6 . . ?
C75' C76' H76C 110.2 . . ?
C75' C76' H76D 110.2 . . ?
H76C C76' H76D 108.5 . . ?
C86 O81 C82 112.0(7) . . ?
C86 O81 Li10 112.0(7) . . ?
C82 O81 Li10 132.9(7) . . ?
C83 C82 O81 110.4(7) . . ?
C83 C82 H82A 109.6 . . ?
O81 C82 H82A 109.6 . . ?
C83 C82 H82B 109.6 . . ?
O81 C82 H82B 109.6 . . ?
H82A C82 H82B 108.1 . . ?
C82 C83 O84 109.6(7) . . ?
C82 C83 Li30 151.4(9) . . ?
O84 C83 Li30 43.3(5) . . ?
C82 C83 H83A 109.8 . . ?
O84 C83 H83A 109.8 . . ?
Li30 C83 H83A 79.6 . . ?
C82 C83 H83B 109.8 . . ?
O84 C83 H83B 109.8 . . ?
Li30 C83 H83B 91.6 . . ?
H83A C83 H83B 108.2 . . ?
C85 O84 C83 108.2(6) . . ?
C85 O84 Li30 119.7(8) . . ?
C83 O84 Li30 105.5(8) . . ?
C86 C85 O84 110.4(7) . . ?
C86 C85 H85A 109.6 . . ?
O84 C85 H85A 109.6 . . ?
C86 C85 H85B 109.6 . . ?
O84 C85 H85B 109.6 . . ?
H85A C85 H85B 108.1 . . ?
C85 C86 O81 111.8(7) . . ?
C85 C86 H86A 109.3 . . ?
O81 C86 H86A 109.3 . . ?
C85 C86 H86B 109.3 . . ?
O81 C86 H86B 109.3 . . ?
H86A C86 H86B 107.9 . . ?
C83' C82' H82C 110.1 . . ?
C83' C82' H82D 110.1 . . ?
H82C C82' H82D 108.5 . . ?
C82' C83' H83C 110.4 . . ?
C82' C83' H83D 110.4 . . ?
H83C C83' H83D 108.6 . . ?
C86' C85' H85C 110.2 . . ?
C86' C85' H85D 110.2 . . ?
H85C C85' H85D 108.5 . . ?
C85' C86' Li10 140.9(10) . . ?
C85' C86' H86C 110.0 . . ?
Li10 C86' H86C 104.5 . . ?
C85' C86' H86D 110.0 . . ?
Li10 C86' H86D 74.9 . . ?
H86C C86' H86D 108.4 . . ?
C96 O91 C92 109.9(8) . . ?
C96 O91 Li70 113.1(7) . . ?
C92 O91 Li70 130.5(7) . . ?
O91 C92 C93 108.4(7) . . ?
O91 C92 H92A 110.0 . . ?
C93 C92 H92A 110.0 . . ?
O91 C92 H92B 110.0 . . ?
C93 C92 H92B 110.0 . . ?
H92A C92 H92B 108.4 . . ?
C92 C93 O94 107.6(7) . . ?
C92 C93 H93A 110.2 . . ?
O94 C93 H93A 110.2 . . ?
C92 C93 H93B 110.2 . . ?
O94 C93 H93B 110.2 . . ?
H93A C93 H93B 108.5 . . ?
C93 O94 C95 107.1(6) . . ?
C93 O94 Li70 113.4(6) . 2_655 ?
C95 O94 Li70 128.6(6) . 2_655 ?
C96 C95 O94 106.9(7) . . ?
C96 C95 H95A 110.3 . . ?
O94 C95 H95A 110.3 . . ?
C96 C95 H95B 110.3 . . ?
O94 C95 H95B 110.3 . . ?
H95A C95 H95B 108.6 . . ?
O91 C96 C95 108.1(7) . . ?
O91 C96 H96A 110.1 . . ?
C95 C96 H96A 110.1 . . ?
O91 C96 H96B 110.1 . . ?
C95 C96 H96B 110.1 . . ?
H96A C96 H96B 108.4 . . ?
C93' C92' H92C 109.1 . . ?
C93' C92' H92D 109.1 . . ?
H92C C92' H92D 107.9 . . ?
C92' C93' H93C 109.5 . . ?
C92' C93' H93D 109.5 . . ?
H93C C93' H93D 108.1 . . ?
C96' C95' H95C 110.3 . . ?
C96' C95' H95D 110.3 . . ?
H95C C95' H95D 108.6 . . ?
C95' C96' H96C 110.0 . . ?
C95' C96' H96D 110.0 . . ?
H96C C96' H96D 108.4 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        20.59
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.087
_database_code_depnum_ccdc_archive 'CCDC 981533'










data_dw1334

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H22 Al N4 )0.3, C20 H24 Al N4'
_chemical_formula_sum            'C40 H46 Al2 N8 O0.30'
_chemical_formula_weight         697.61

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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                   10.6722(3)
_cell_length_b                   13.5757(4)
_cell_length_c                   13.6681(4)
_cell_angle_alpha                90.244(2)
_cell_angle_beta                 101.867(2)
_cell_angle_gamma                93.413(1)
_cell_volume                     1934.2(1)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    10102
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      22.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             741
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 redetermination of structure DW1325 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            15742
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_theta_max         22.43
_reflns_number_total             4994
_reflns_number_gt                3744
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'

_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.

 The eight -CH2- hydrogen atoms were all clearly visible in the final
 difference maps.

 The site containing atom Al2 is disordered, Al(H2)py4 / AL(OH)2py4
 with occupancies (best estimate) 0.85 : 0.15.  For the refinement, common
 isotropic displacement parameters were assigned to the disordered O
 and H atoms and weak bond length restraints were applied to the Al-H
 and Al-O bonds. 
;

_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)+(0.0383P)²+0.8211P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4994
_refine_ls_number_parameters     467
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1055
_refine_ls_wR_factor_gt          0.0939
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.036
_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
Al1 Al 0.00203(8) 0.24839(6) -0.24491(6) 0.0398(2) Uani 1 1 d . . .
N1 N -0.1013(2) 0.22145(16) -0.36963(16) 0.0412(6) Uani 1 1 d . . .
C11 C -0.0650(3) 0.2535(2) -0.4575(2) 0.0443(7) Uani 1 1 d . . .
H11 H 0.0095 0.2969 -0.4509 0.053 Uiso 1 1 calc R . .
C12 C -0.1269(3) 0.2277(2) -0.5499(2) 0.0496(8) Uani 1 1 d . . .
H12 H -0.0934 0.2531 -0.6046 0.060 Uiso 1 1 calc R . .
C13 C -0.2463(3) 0.1610(2) -0.5719(2) 0.0581(8) Uani 1 1 d . . .
H13A H -0.3183 0.1970 -0.6098 0.070 Uiso 1 1 calc R . .
H13B H -0.2334 0.1039 -0.6132 0.070 Uiso 1 1 calc R . .
C14 C -0.2773(3) 0.1260(2) -0.4757(2) 0.0526(8) Uani 1 1 d . . .
H14A H -0.3487 0.0802 -0.4781 0.063 Uiso 1 1 calc R . .
C15 C -0.2090(3) 0.1563(2) -0.3864(2) 0.0460(7) Uani 1 1 d . . .
H15 H -0.2366 0.1309 -0.3292 0.055 Uiso 1 1 calc R . .
N2 N 0.1047(2) 0.36212(16) -0.24979(16) 0.0413(6) Uani 1 1 d . . .
C21 C 0.2200(3) 0.3651(2) -0.2808(2) 0.0546(8) Uani 1 1 d . . .
H21 H 0.2518 0.3038 -0.2949 0.066 Uiso 1 1 calc R . .
C22 C 0.2905(3) 0.4467(2) -0.2924(2) 0.0637(9) Uani 1 1 d . . .
H22 H 0.3690 0.4399 -0.3136 0.076 Uiso 1 1 calc R . .
C23 C 0.2534(3) 0.5481(2) -0.2742(2) 0.0610(9) Uani 1 1 d . . .
H23A H 0.2505 0.5879 -0.3351 0.073 Uiso 1 1 calc R . .
H23B H 0.3175 0.5807 -0.2191 0.073 Uiso 1 1 calc R . .
C24 C 0.1246(3) 0.5413(2) -0.2473(2) 0.0520(8) Uani 1 1 d . . .
H24 H 0.0858 0.6007 -0.2372 0.062 Uiso 1 1 calc R . .
C25 C 0.0620(3) 0.4558(2) -0.2368(2) 0.0472(7) Uani 1 1 d . . .
H25 H -0.0192 0.4584 -0.2189 0.057 Uiso 1 1 calc R . .
N3 N -0.1042(2) 0.26473(16) -0.15483(16) 0.0409(6) Uani 1 1 d . . .
C31 C -0.2209(3) 0.3072(2) -0.1775(2) 0.0511(8) Uani 1 1 d . . .
H31 H -0.2509 0.3244 -0.2453 0.061 Uiso 1 1 calc R . .
C32 C -0.2956(3) 0.3264(2) -0.1135(2) 0.0549(8) Uani 1 1 d . . .
H32 H -0.3742 0.3559 -0.1379 0.066 Uiso 1 1 calc R . .
C33 C -0.2602(3) 0.3030(2) -0.0045(2) 0.0579(9) Uani 1 1 d . . .
H33A H -0.2600 0.3635 0.0362 0.069 Uiso 1 1 calc R . .
H33B H -0.3239 0.2537 0.0127 0.069 Uiso 1 1 calc R . .
C34 C -0.1302(3) 0.2631(2) 0.0174(2) 0.0501(7) Uani 1 1 d . . .
H34 H -0.0928 0.2488 0.0847 0.060 Uiso 1 1 calc R . .
C35 C -0.0642(3) 0.2466(2) -0.0531(2) 0.0441(7) Uani 1 1 d . . .
H35 H 0.0173 0.2202 -0.0324 0.053 Uiso 1 1 calc R . .
N4 N 0.1078(2) 0.14508(16) -0.20632(16) 0.0401(5) Uani 1 1 d . . .
C41 C 0.0701(3) 0.0484(2) -0.2412(2) 0.0478(7) Uani 1 1 d . . .
H41 H -0.0075 0.0390 -0.2897 0.057 Uiso 1 1 calc R . .
C42 C 0.1335(3) -0.0313(2) -0.2121(2) 0.0505(8) Uani 1 1 d . . .
H42 H 0.0986 -0.0936 -0.2401 0.061 Uiso 1 1 calc R . .
C43 C 0.2570(3) -0.0270(2) -0.1376(2) 0.0601(9) Uani 1 1 d . . .
H43A H 0.3250 -0.0529 -0.1683 0.072 Uiso 1 1 calc R . .
H43B H 0.2479 -0.0686 -0.0799 0.072 Uiso 1 1 calc R . .
C44 C 0.2939(3) 0.0775(2) -0.1027(2) 0.0547(8) Uani 1 1 d . . .
H44 H 0.3716 0.0912 -0.0553 0.066 Uiso 1 1 calc R . .
C45 C 0.2209(3) 0.1521(2) -0.1361(2) 0.0504(8) Uani 1 1 d . . .
H45 H 0.2499 0.2159 -0.1088 0.060 Uiso 1 1 calc R . .
Al2 Al 0.29797(7) 0.26337(6) 0.29410(6) 0.0362(2) Uani 1 1 d D . .
O1 O 0.0801(9) 0.2589(10) 0.2599(9) 0.050(2) Uiso 0.15 1 d PD A 1
H1A H 0.0511 0.2078 0.2841 0.075 Uiso 0.15 1 calc PR A 1
H1 H 0.4313(16) 0.269(2) 0.3153(19) 0.034(5) Uiso 0.85 1 d PD B 1
O2 O 0.5158(9) 0.2778(10) 0.3221(9) 0.050(2) Uiso 0.15 1 d PD A 2
H2A H 0.5431 0.2258 0.3029 0.075 Uiso 0.15 1 calc PR A 2
H2 H 0.1646(16) 0.257(2) 0.2725(19) 0.034(5) Uiso 0.85 1 d PD C 2
N5 N 0.2981(2) 0.12694(15) 0.22383(15) 0.0370(5) Uani 1 1 d . A .
C51 C 0.4042(3) 0.0766(2) 0.2355(2) 0.0481(7) Uani 1 1 d . . .
H51 H 0.4813 0.1048 0.2759 0.058 Uiso 1 1 calc R A .
C52 C 0.4058(3) -0.0148(2) 0.1912(2) 0.0506(8) Uani 1 1 d . A .
H52 H 0.4826 -0.0487 0.2011 0.061 Uiso 1 1 calc R . .
C53 C 0.2954(3) -0.0555(2) 0.1328(2) 0.0505(8) Uani 1 1 d . . .
H53 H 0.2941 -0.1186 0.1021 0.061 Uiso 1 1 calc R A .
C54 C 0.1864(3) -0.0043(2) 0.1191(2) 0.0547(8) Uani 1 1 d . A .
H54 H 0.1089 -0.0308 0.0779 0.066 Uiso 1 1 calc R . .
C55 C 0.1910(3) 0.0863(2) 0.1662(2) 0.0461(7) Uani 1 1 d . . .
H55 H 0.1149 0.1211 0.1572 0.055 Uiso 1 1 calc R A .
N6 N 0.2999(2) 0.19452(15) 0.43087(16) 0.0381(5) Uani 1 1 d . A .
C61 C 0.1935(3) 0.1492(2) 0.4522(2) 0.0452(7) Uani 1 1 d . . .
H61 H 0.1171 0.1450 0.4020 0.054 Uiso 1 1 calc R A .
C62 C 0.1909(3) 0.1086(2) 0.5439(2) 0.0514(8) Uani 1 1 d . A .
H62 H 0.1144 0.0761 0.5559 0.062 Uiso 1 1 calc R . .
C63 C 0.2992(3) 0.1156(2) 0.6173(2) 0.0505(8) Uani 1 1 d . . .
H63 H 0.2986 0.0895 0.6816 0.061 Uiso 1 1 calc R A .
C64 C 0.4091(3) 0.1611(2) 0.5965(2) 0.0535(8) Uani 1 1 d . A .
H64 H 0.4862 0.1660 0.6460 0.064 Uiso 1 1 calc R . .
C65 C 0.4061(3) 0.1994(2) 0.5031(2) 0.0445(7) Uani 1 1 d . . .
H65 H 0.4824 0.2305 0.4892 0.053 Uiso 1 1 calc R A .
N7 N 0.2983(2) 0.40143(15) 0.36294(15) 0.0374(5) Uani 1 1 d . A .
C71 C 0.2021(3) 0.4266(2) 0.4049(2) 0.0503(8) Uani 1 1 d . . .
H71 H 0.1319 0.3800 0.4039 0.060 Uiso 1 1 calc R A .
C72 C 0.2009(3) 0.5177(2) 0.4495(2) 0.0547(8) Uani 1 1 d . A .
H72 H 0.1318 0.5324 0.4801 0.066 Uiso 1 1 calc R . .
C73 C 0.2986(3) 0.5864(2) 0.4495(2) 0.0501(8) Uani 1 1 d . . .
H73 H 0.2986 0.6499 0.4788 0.060 Uiso 1 1 calc R A .
C74 C 0.3975(3) 0.5612(2) 0.4058(2) 0.0575(8) Uani 1 1 d . A .
H74 H 0.4674 0.6076 0.4044 0.069 Uiso 1 1 calc R . .
C75 C 0.3944(3) 0.4687(2) 0.3643(2) 0.0497(8) Uani 1 1 d . . .
H75 H 0.4641 0.4520 0.3352 0.060 Uiso 1 1 calc R A .
N8 N 0.2989(2) 0.33346(15) 0.15862(15) 0.0379(5) Uani 1 1 d . A .
C81 C 0.4013(3) 0.3334(2) 0.1157(2) 0.0489(7) Uani 1 1 d . . .
H81 H 0.4745 0.3011 0.1486 0.059 Uiso 1 1 calc R A .
C82 C 0.4046(3) 0.3782(2) 0.0260(2) 0.0555(8) Uani 1 1 d . A .
H82 H 0.4786 0.3762 -0.0024 0.067 Uiso 1 1 calc R . .
C83 C 0.3004(3) 0.4256(2) -0.0216(2) 0.0529(8) Uani 1 1 d . . .
H83 H 0.3004 0.4566 -0.0838 0.063 Uiso 1 1 calc R A .
C84 C 0.1961(3) 0.4274(2) 0.0218(2) 0.0559(8) Uani 1 1 d . A .
H84 H 0.1230 0.4609 -0.0093 0.067 Uiso 1 1 calc R . .
C85 C 0.1978(3) 0.3805(2) 0.1111(2) 0.0470(7) Uani 1 1 d . . .
H85 H 0.1243 0.3815 0.1401 0.056 Uiso 1 1 calc R A .


_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
Al1 N2 1.849(2) . ?
Al1 N1 1.852(2) . ?
Al1 N3 1.858(2) . ?
Al1 N4 1.863(2) . ?
N1 C15 1.388(4) . ?
N1 C11 1.399(3) . ?
C11 C12 1.333(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.496(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.494(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.336(4) . ?
C14 H14A 0.9500 . ?
C15 H15 0.9500 . ?
N2 C21 1.380(4) . ?
N2 C25 1.398(3) . ?
C21 C22 1.330(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.488(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.492(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.328(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
N3 C31 1.382(3) . ?
N3 C35 1.395(3) . ?
C31 C32 1.334(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.500(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.493(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.330(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
N4 C45 1.377(4) . ?
N4 C41 1.402(4) . ?
C41 C42 1.329(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.489(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.498(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.339(4) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
Al2 N5 2.083(2) . ?
Al2 N8 2.087(2) . ?
Al2 N6 2.091(2) . ?
Al2 N7 2.093(2) . ?
Al2 O1 2.273(9) . ?
Al2 O2 2.273(9) . ?
Al2 H1 1.390(17) . ?
Al2 H2 1.390(17) . ?
O1 H1A 0.8400 . ?
O1 H2 0.885(16) . ?
O2 H1 0.887(16) . ?
O2 H2A 0.8400 . ?
N5 C55 1.336(3) . ?
N5 C51 1.339(3) . ?
C51 C52 1.380(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.365(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.371(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.379(4) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
N6 C65 1.339(3) . ?
N6 C61 1.344(3) . ?
C61 C62 1.376(4) . ?
C61 H61 0.9500 . ?
C62 C63 1.364(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.376(4) . ?
C63 H63 0.9500 . ?
C64 C65 1.375(4) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
N7 C75 1.330(3) . ?
N7 C71 1.334(3) . ?
C71 C72 1.379(4) . ?
C71 H71 0.9500 . ?
C72 C73 1.356(4) . ?
C72 H72 0.9500 . ?
C73 C74 1.373(4) . ?
C73 H73 0.9500 . ?
C74 C75 1.372(4) . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?
N8 C85 1.338(3) . ?
N8 C81 1.343(3) . ?
C81 C82 1.377(4) . ?
C81 H81 0.9500 . ?
C82 C83 1.366(4) . ?
C82 H82 0.9500 . ?
C83 C84 1.367(4) . ?
C83 H83 0.9500 . ?
C84 C85 1.376(4) . ?
C84 H84 0.9500 . ?
C85 H85 0.9500 . ?

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
N2 Al1 N1 109.70(10) . . ?
N2 Al1 N3 110.31(10) . . ?
N1 Al1 N3 107.86(10) . . ?
N2 Al1 N4 108.33(10) . . ?
N1 Al1 N4 110.23(10) . . ?
N3 Al1 N4 110.42(10) . . ?
C15 N1 C11 113.5(2) . . ?
C15 N1 Al1 123.99(18) . . ?
C11 N1 Al1 121.75(19) . . ?
C12 C11 N1 125.1(3) . . ?
C12 C11 H11 117.5 . . ?
N1 C11 H11 117.5 . . ?
C11 C12 C13 123.4(3) . . ?
C11 C12 H12 118.3 . . ?
C13 C12 H12 118.3 . . ?
C14 C13 C12 109.1(2) . . ?
C14 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C15 C14 C13 122.9(3) . . ?
C15 C14 H14A 118.5 . . ?
C13 C14 H14A 118.5 . . ?
C14 C15 N1 125.9(3) . . ?
C14 C15 H15 117.1 . . ?
N1 C15 H15 117.1 . . ?
C21 N2 C25 113.2(2) . . ?
C21 N2 Al1 124.30(19) . . ?
C25 N2 Al1 121.85(19) . . ?
C22 C21 N2 125.3(3) . . ?
C22 C21 H21 117.3 . . ?
N2 C21 H21 117.3 . . ?
C21 C22 C23 123.8(3) . . ?
C21 C22 H22 118.1 . . ?
C23 C22 H22 118.1 . . ?
C22 C23 C24 108.9(3) . . ?
C22 C23 H23A 109.9 . . ?
C24 C23 H23A 109.9 . . ?
C22 C23 H23B 109.9 . . ?
C24 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
C25 C24 C23 122.7(3) . . ?
C25 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
C24 C25 N2 125.9(3) . . ?
C24 C25 H25 117.0 . . ?
N2 C25 H25 117.0 . . ?
C31 N3 C35 113.1(2) . . ?
C31 N3 Al1 124.49(18) . . ?
C35 N3 Al1 121.85(18) . . ?
C32 C31 N3 126.2(3) . . ?
C32 C31 H31 116.9 . . ?
N3 C31 H31 116.9 . . ?
C31 C32 C33 122.5(3) . . ?
C31 C32 H32 118.8 . . ?
C33 C32 H32 118.8 . . ?
C34 C33 C32 109.2(2) . . ?
C34 C33 H33A 109.8 . . ?
C32 C33 H33A 109.8 . . ?
C34 C33 H33B 109.8 . . ?
C32 C33 H33B 109.8 . . ?
H33A C33 H33B 108.3 . . ?
C35 C34 C33 122.9(3) . . ?
C35 C34 H34 118.5 . . ?
C33 C34 H34 118.5 . . ?
C34 C35 N3 125.8(3) . . ?
C34 C35 H35 117.1 . . ?
N3 C35 H35 117.1 . . ?
C45 N4 C41 113.5(2) . . ?
C45 N4 Al1 125.29(19) . . ?
C41 N4 Al1 120.97(19) . . ?
C42 C41 N4 125.6(3) . . ?
C42 C41 H41 117.2 . . ?
N4 C41 H41 117.2 . . ?
C41 C42 C43 122.8(3) . . ?
C41 C42 H42 118.6 . . ?
C43 C42 H42 118.6 . . ?
C42 C43 C44 109.9(2) . . ?
C42 C43 H43A 109.7 . . ?
C44 C43 H43A 109.7 . . ?
C42 C43 H43B 109.7 . . ?
C44 C43 H43B 109.7 . . ?
H43A C43 H43B 108.2 . . ?
C45 C44 C43 122.2(3) . . ?
C45 C44 H44 118.9 . . ?
C43 C44 H44 118.9 . . ?
C44 C45 N4 126.1(3) . . ?
C44 C45 H45 116.9 . . ?
N4 C45 H45 116.9 . . ?
N5 Al2 N8 89.88(8) . . ?
N5 Al2 N6 90.63(8) . . ?
N8 Al2 N6 179.05(10) . . ?
N5 Al2 N7 179.21(9) . . ?
N8 Al2 N7 89.34(8) . . ?
N6 Al2 N7 90.15(8) . . ?
N5 Al2 O1 92.0(3) . . ?
N8 Al2 O1 89.6(3) . . ?
N6 Al2 O1 91.2(3) . . ?
N7 Al2 O1 88.2(3) . . ?
N5 Al2 O2 90.1(3) . . ?
N8 Al2 O2 86.9(3) . . ?
N6 Al2 O2 92.3(3) . . ?
N7 Al2 O2 89.7(3) . . ?
O1 Al2 O2 176.0(5) . . ?
N5 Al2 H1 89.8(11) . . ?
N8 Al2 H1 89.7(11) . . ?
N6 Al2 H1 89.5(11) . . ?
N7 Al2 H1 90.1(11) . . ?
O1 Al2 H1 178.1(12) . . ?
O2 Al2 H1 2.8(12) . . ?
N5 Al2 H2 90.1(11) . . ?
N8 Al2 H2 90.1(11) . . ?
N6 Al2 H2 90.7(11) . . ?
N7 Al2 H2 90.0(11) . . ?
O1 Al2 H2 1.9(12) . . ?
O2 Al2 H2 177.1(11) . . ?
H1 Al2 H2 179.8(16) . . ?
Al2 O1 H1A 109.5 . . ?
Al2 O1 H2 3(2) . . ?
H1A O1 H2 107.2 . . ?
Al2 O2 H1 4.4(18) . . ?
Al2 O2 H2A 109.5 . . ?
H1 O2 H2A 108.6 . . ?
C55 N5 C51 117.8(2) . . ?
C55 N5 Al2 120.62(18) . . ?
C51 N5 Al2 121.60(18) . . ?
N5 C51 C52 122.6(3) . . ?
N5 C51 H51 118.7 . . ?
C52 C51 H51 118.7 . . ?
C53 C52 C51 119.0(3) . . ?
C53 C52 H52 120.5 . . ?
C51 C52 H52 120.5 . . ?
C52 C53 C54 119.1(3) . . ?
C52 C53 H53 120.4 . . ?
C54 C53 H53 120.4 . . ?
C53 C54 C55 119.0(3) . . ?
C53 C54 H54 120.5 . . ?
C55 C54 H54 120.5 . . ?
N5 C55 C54 122.6(3) . . ?
N5 C55 H55 118.7 . . ?
C54 C55 H55 118.7 . . ?
C65 N6 C61 117.4(2) . . ?
C65 N6 Al2 120.79(18) . . ?
C61 N6 Al2 121.68(18) . . ?
N6 C61 C62 122.5(3) . . ?
N6 C61 H61 118.7 . . ?
C62 C61 H61 118.7 . . ?
C63 C62 C61 119.5(3) . . ?
C63 C62 H62 120.3 . . ?
C61 C62 H62 120.3 . . ?
C62 C63 C64 118.7(3) . . ?
C62 C63 H63 120.6 . . ?
C64 C63 H63 120.6 . . ?
C65 C64 C63 119.1(3) . . ?
C65 C64 H64 120.4 . . ?
C63 C64 H64 120.4 . . ?
N6 C65 C64 122.7(3) . . ?
N6 C65 H65 118.6 . . ?
C64 C65 H65 118.6 . . ?
C75 N7 C71 117.3(2) . . ?
C75 N7 Al2 120.60(18) . . ?
C71 N7 Al2 122.06(19) . . ?
N7 C71 C72 122.5(3) . . ?
N7 C71 H71 118.8 . . ?
C72 C71 H71 118.8 . . ?
C73 C72 C71 119.8(3) . . ?
C73 C72 H72 120.1 . . ?
C71 C72 H72 120.1 . . ?
C72 C73 C74 118.0(3) . . ?
C72 C73 H73 121.0 . . ?
C74 C73 H73 121.0 . . ?
C75 C74 C73 119.4(3) . . ?
C75 C74 H74 120.3 . . ?
C73 C74 H74 120.3 . . ?
N7 C75 C74 122.9(3) . . ?
N7 C75 H75 118.5 . . ?
C74 C75 H75 118.5 . . ?
C85 N8 C81 117.2(2) . . ?
C85 N8 Al2 121.49(18) . . ?
C81 N8 Al2 121.26(18) . . ?
N8 C81 C82 122.7(3) . . ?
N8 C81 H81 118.6 . . ?
C82 C81 H81 118.6 . . ?
C83 C82 C81 119.2(3) . . ?
C83 C82 H82 120.4 . . ?
C81 C82 H82 120.4 . . ?
C82 C83 C84 118.7(3) . . ?
C82 C83 H83 120.6 . . ?
C84 C83 H83 120.6 . . ?
C83 C84 C85 119.4(3) . . ?
C83 C84 H84 120.3 . . ?
C85 C84 H84 120.3 . . ?
N8 C85 C84 122.6(3) . . ?
N8 C85 H85 118.7 . . ?
C84 C85 H85 118.7 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        22.43
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.040
_database_code_depnum_ccdc_archive 'CCDC 981534'










data_dw1336

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H25 Al N3 1+, C2 H12 B2 N 1-'
_chemical_formula_sum            'C11 H37 Al B2 N4'
_chemical_formula_weight         274.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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                   6.0538(4)
_cell_length_b                   12.6086(6)
_cell_length_c                   13.3970(9)
_cell_angle_alpha                114.250(2)
_cell_angle_beta                 93.497(2)
_cell_angle_gamma                99.234(3)
_cell_volume                     911.08(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    8465
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             308
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            8576
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_sigmaI/netI    0.1377
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.75
_diffrn_reflns_theta_max         27.62
_reflns_number_total             4054
_reflns_number_gt                2156
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'

_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.

 The two Al-H hydrogen atoms were clearly visible in the final difference
 map (being the two highest peaks in the map).
;

_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)+(0.0504P)²+0.4507P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4054
_refine_ls_number_parameters     179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.0746
_refine_ls_wR_factor_ref         0.1699
_refine_ls_wR_factor_gt          0.1449
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Al1 Al 0.02422(15) 0.79587(7) 0.87054(7) 0.0332(3) Uani 1 1 d . . .
H1 H -0.229(5) 0.792(3) 0.862(2) 0.051(6) Uiso 1 1 d . . .
H2 H 0.196(5) 0.875(3) 0.965(2) 0.051(6) Uiso 1 1 d . . .
N2 N 0.1328(4) 0.9032(2) 0.78617(19) 0.0336(6) Uani 1 1 d . . .
N3 N 0.0957(4) 0.6652(2) 0.73487(19) 0.0328(6) Uani 1 1 d . . .
N4 N 0.0096(4) 0.6645(2) 0.93503(19) 0.0343(6) Uani 1 1 d . . .
C3 C 0.3425(6) 0.9910(3) 0.8511(3) 0.0514(9) Uani 1 1 d . . .
H3A H 0.3914 1.0414 0.8137 0.077 Uiso 1 1 calc R . .
H3B H 0.4618 0.9489 0.8569 0.077 Uiso 1 1 calc R . .
H3C H 0.3123 1.0406 0.9252 0.077 Uiso 1 1 calc R . .
C4 C -0.0416(6) 0.9689(3) 0.7741(3) 0.0492(9) Uani 1 1 d . . .
H4A H 0.0190 1.0235 0.7427 0.074 Uiso 1 1 calc R . .
H4B H -0.0840 1.0142 0.8467 0.074 Uiso 1 1 calc R . .
H4C H -0.1751 0.9124 0.7247 0.074 Uiso 1 1 calc R . .
C5 C 0.1828(5) 0.8247(3) 0.6758(2) 0.0414(8) Uani 1 1 d . . .
H5A H 0.3021 0.8693 0.6523 0.050 Uiso 1 1 calc R . .
H5B H 0.0454 0.7967 0.6206 0.050 Uiso 1 1 calc R . .
C6 C 0.2614(5) 0.7191(3) 0.6830(3) 0.0441(8) Uani 1 1 d . . .
H6A H 0.2727 0.6597 0.6081 0.053 Uiso 1 1 calc R . .
H6B H 0.4125 0.7455 0.7280 0.053 Uiso 1 1 calc R . .
C7 C -0.1130(6) 0.5978(3) 0.6536(3) 0.0521(9) Uani 1 1 d . . .
H7A H -0.0772 0.5301 0.5920 0.078 Uiso 1 1 calc R . .
H7B H -0.1705 0.6502 0.6255 0.078 Uiso 1 1 calc R . .
H7C H -0.2281 0.5691 0.6900 0.078 Uiso 1 1 calc R . .
C8 C 0.1935(6) 0.5836(3) 0.7708(3) 0.0470(8) Uani 1 1 d . . .
H8A H 0.3479 0.6225 0.8113 0.056 Uiso 1 1 calc R . .
H8B H 0.2032 0.5105 0.7055 0.056 Uiso 1 1 calc R . .
C9 C 0.0433(6) 0.5526(3) 0.8454(3) 0.0460(8) Uani 1 1 d . . .
H9A H -0.1043 0.5037 0.8023 0.055 Uiso 1 1 calc R . .
H9B H 0.1150 0.5063 0.8775 0.055 Uiso 1 1 calc R . .
C10 C -0.2109(5) 0.6444(3) 0.9749(3) 0.0492(9) Uani 1 1 d . . .
H10A H -0.2090 0.5880 1.0078 0.074 Uiso 1 1 calc R . .
H10B H -0.3332 0.6121 0.9126 0.074 Uiso 1 1 calc R . .
H10C H -0.2353 0.7200 1.0306 0.074 Uiso 1 1 calc R . .
C11 C 0.1907(6) 0.7041(3) 1.0296(3) 0.0537(9) Uani 1 1 d . . .
H11A H 0.1912 0.6406 1.0538 0.081 Uiso 1 1 calc R . .
H11B H 0.1634 0.7750 1.0907 0.081 Uiso 1 1 calc R . .
H11C H 0.3372 0.7229 1.0069 0.081 Uiso 1 1 calc R . .
N1 N -0.4024(4) 0.7676(2) 0.37832(19) 0.0339(6) Uani 1 1 d . . .
B1 B -0.3572(7) 0.7045(4) 0.2530(3) 0.0490(10) Uani 1 1 d . . .
H98A H -0.3942 0.7511 0.2135 0.074 Uiso 1 1 calc R . .
H98B H -0.4520 0.6245 0.2171 0.074 Uiso 1 1 calc R . .
H98C H -0.1976 0.6991 0.2516 0.074 Uiso 1 1 calc R . .
B2 B -0.3530(6) 0.6975(3) 0.4488(3) 0.0448(9) Uani 1 1 d . . .
H99A H -0.3764 0.7427 0.5254 0.067 Uiso 1 1 calc R . .
H99B H -0.1963 0.6867 0.4473 0.067 Uiso 1 1 calc R . .
H99C H -0.4558 0.6196 0.4175 0.067 Uiso 1 1 calc R . .
C1 C -0.2559(6) 0.8866(3) 0.4308(3) 0.0525(9) Uani 1 1 d . . .
H1A H -0.2821 0.9268 0.5077 0.079 Uiso 1 1 calc R . .
H1B H -0.2907 0.9330 0.3906 0.079 Uiso 1 1 calc R . .
H1C H -0.0973 0.8794 0.4291 0.079 Uiso 1 1 calc R . .
C2 C -0.6388(5) 0.7824(3) 0.3796(3) 0.0541(9) Uani 1 1 d . . .
H2A H -0.6650 0.8253 0.4561 0.081 Uiso 1 1 calc R . .
H2B H -0.7401 0.7041 0.3460 0.081 Uiso 1 1 calc R . .
H2C H -0.6687 0.8275 0.3374 0.081 Uiso 1 1 calc R . .


_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
Al1 N3 2.018(2) . ?
Al1 N2 2.145(2) . ?
Al1 N4 2.153(2) . ?
Al1 H1 1.52(3) . ?
Al1 H2 1.46(3) . ?
N2 C4 1.482(4) . ?
N2 C5 1.485(4) . ?
N2 C3 1.489(4) . ?
N3 C6 1.485(4) . ?
N3 C8 1.486(4) . ?
N3 C7 1.494(4) . ?
N4 C11 1.481(4) . ?
N4 C9 1.485(4) . ?
N4 C10 1.490(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.521(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.515(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
N1 C1 1.470(4) . ?
N1 C2 1.473(4) . ?
N1 B2 1.581(4) . ?
N1 B1 1.598(4) . ?
B1 H98A 0.9800 . ?
B1 H98B 0.9800 . ?
B1 H98C 0.9800 . ?
B2 H99A 0.9800 . ?
B2 H99B 0.9800 . ?
B2 H99C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 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
N3 Al1 N2 82.88(9) . . ?
N3 Al1 N4 83.02(10) . . ?
N2 Al1 N4 161.19(10) . . ?
N3 Al1 H1 109.9(11) . . ?
N2 Al1 H1 101.7(11) . . ?
N4 Al1 H1 94.7(11) . . ?
N3 Al1 H2 122.8(12) . . ?
N2 Al1 H2 89.1(11) . . ?
N4 Al1 H2 88.1(11) . . ?
H1 Al1 H2 127.1(16) . . ?
C4 N2 C5 110.3(2) . . ?
C4 N2 C3 108.4(3) . . ?
C5 N2 C3 109.1(2) . . ?
C4 N2 Al1 111.41(18) . . ?
C5 N2 Al1 108.51(17) . . ?
C3 N2 Al1 109.03(18) . . ?
C6 N3 C8 110.5(2) . . ?
C6 N3 C7 109.5(2) . . ?
C8 N3 C7 109.5(2) . . ?
C6 N3 Al1 108.72(17) . . ?
C8 N3 Al1 107.76(18) . . ?
C7 N3 Al1 110.89(18) . . ?
C11 N4 C9 109.2(3) . . ?
C11 N4 C10 107.7(2) . . ?
C9 N4 C10 110.4(2) . . ?
C11 N4 Al1 110.27(19) . . ?
C9 N4 Al1 107.91(18) . . ?
C10 N4 Al1 111.36(18) . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 108.9(2) . . ?
N2 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N2 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N3 C6 C5 108.7(2) . . ?
N3 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
N3 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C9 108.7(2) . . ?
N3 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
N3 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N4 C9 C8 108.6(2) . . ?
N4 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
N4 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
N4 C10 H10A 109.5 . . ?
N4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C1 N1 C2 107.9(3) . . ?
C1 N1 B2 108.4(2) . . ?
C2 N1 B2 109.4(2) . . ?
C1 N1 B1 108.4(2) . . ?
C2 N1 B1 109.1(2) . . ?
B2 N1 B1 113.5(2) . . ?
N1 B1 H98A 109.5 . . ?
N1 B1 H98B 109.5 . . ?
H98A B1 H98B 109.5 . . ?
N1 B1 H98C 109.5 . . ?
H98A B1 H98C 109.5 . . ?
H98B B1 H98C 109.5 . . ?
N1 B2 H99A 109.5 . . ?
N1 B2 H99B 109.5 . . ?
H99A B2 H99B 109.5 . . ?
N1 B2 H99C 109.5 . . ?
H99A B2 H99C 109.5 . . ?
H99B B2 H99C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.050
_database_code_depnum_ccdc_archive 'CCDC 981535'










data_dw1339

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H96 Al4 Li4 O10'
_chemical_formula_sum            'C40 H96 Al4 Li4 O10'
_chemical_formula_weight         872.85

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna2(1)
_symmetry_space_group_name_Hall  'P 2c -2n'

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

_cell_length_a                   17.6391(2)
_cell_length_b                   20.0133(2)
_cell_length_c                   16.0589(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5669.06(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    23634
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.88

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 5920 Friedel pairs were averaged for the refinement. 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            35011
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.58
_diffrn_reflns_theta_max         27.86
_reflns_number_total             6952
_reflns_number_gt                5416
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'

_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.

 The seven Al-H hydrogen atomns were all clearly visible in the final
 difference map (being amongst the 12 highest peaks in the map).
;

_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)+(0.0762P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(12)
_refine_ls_number_reflns         6952
_refine_ls_number_parameters     572
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1068
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.977
_refine_ls_shift/su_max          0.004
_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
Al1 Al 0.45231(4) 0.58721(4) 0.41702(5) 0.02664(17) Uani 1 1 d . . .
Al2 Al -0.03427(4) 0.41479(3) 0.51431(5) 0.02669(17) Uani 1 1 d . . .
Al3 Al 0.18435(4) 0.47227(4) 0.28438(6) 0.0377(2) Uani 1 1 d . . .
H31 H 0.1276(18) 0.4974(17) 0.221(2) 0.060(3) Uiso 1 1 d . . .
H32 H 0.2360(19) 0.4177(15) 0.236(2) 0.060(3) Uiso 1 1 d . . .
H33 H 0.1391(18) 0.4431(17) 0.353(2) 0.060(3) Uiso 1 1 d . . .
H34 H 0.2345(18) 0.5305(17) 0.321(2) 0.060(3) Uiso 1 1 d . . .
Al4 Al 0.66440(4) 0.47340(4) 0.60753(6) 0.0374(2) Uani 1 1 d . . .
H41 H 0.6366(19) 0.4723(16) 0.697(2) 0.060(3) Uiso 1 1 d . . .
H42 H 0.7519(17) 0.4786(17) 0.608(2) 0.060(3) Uiso 1 1 d . . .
H43 H 0.643(2) 0.4194(16) 0.553(2) 0.060(3) Uiso 1 1 d . . .
H44 H 0.6401(19) 0.5383(16) 0.554(2) 0.060(3) Uiso 1 1 d . . .
Li1 Li 0.5749(3) 0.6075(3) 0.5128(3) 0.0412(11) Uani 1 1 d . . .
Li2 Li 0.3403(2) 0.5480(2) 0.3143(3) 0.0389(11) Uani 1 1 d . . .
Li3 Li 0.0872(2) 0.3787(2) 0.4239(3) 0.0407(11) Uani 1 1 d . . .
Li4 Li -0.1449(2) 0.4630(2) 0.6113(3) 0.0388(10) Uani 1 1 d . . .
O0 O 0.13939(13) 0.29375(11) 0.40514(16) 0.0578(6) Uani 1 1 d . . .
O1 O 0.54988(9) 0.58968(9) 0.39700(12) 0.0312(4) Uani 1 1 d . . .
O2 O 0.40414(9) 0.51180(8) 0.40092(11) 0.0319(4) Uani 1 1 d . . .
O3 O 0.39079(9) 0.63011(8) 0.35091(12) 0.0314(4) Uani 1 1 d . . .
O4 O 0.46538(10) 0.61577(9) 0.51881(12) 0.0343(4) Uani 1 1 d . . .
O5 O 0.06301(9) 0.41001(9) 0.53503(12) 0.0323(4) Uani 1 1 d . . .
O6 O -0.07823(10) 0.49281(8) 0.52337(12) 0.0337(4) Uani 1 1 d . . .
O7 O -0.02316(10) 0.37912(9) 0.41599(12) 0.0334(4) Uani 1 1 d . . .
O8 O -0.09713(9) 0.37836(8) 0.58553(12) 0.0331(4) Uani 1 1 d . . .
O9 O 0.63501(13) 0.68435(12) 0.54532(18) 0.0666(7) Uani 1 1 d . . .
C01 C 0.1897(3) 0.2754(2) 0.3398(3) 0.0823(14) Uani 1 1 d . . .
H01A H 0.1817 0.3043 0.2906 0.099 Uiso 1 1 calc R . .
H01B H 0.2430 0.2799 0.3582 0.099 Uiso 1 1 calc R . .
C02 C 0.1740(2) 0.21106(15) 0.3209(2) 0.0596(10) Uani 1 1 d . . .
H02A H 0.2199 0.1886 0.2991 0.072 Uiso 1 1 calc R . .
H02B H 0.1340 0.2090 0.2778 0.072 Uiso 1 1 calc R . .
C03 C 0.1498(2) 0.17981(19) 0.3926(3) 0.0713(11) Uani 1 1 d . . .
H03A H 0.1916 0.1538 0.4178 0.086 Uiso 1 1 calc R . .
H03B H 0.1073 0.1491 0.3802 0.086 Uiso 1 1 calc R . .
C04 C 0.1246(2) 0.23353(17) 0.4501(3) 0.0637(10) Uani 1 1 d . . .
H04A H 0.0700 0.2292 0.4631 0.076 Uiso 1 1 calc R . .
H04B H 0.1539 0.2323 0.5027 0.076 Uiso 1 1 calc R . .
C11 C 0.60003(14) 0.57877(14) 0.32871(19) 0.0353(6) Uani 1 1 d . . .
C12 C 0.55693(19) 0.58089(18) 0.2472(2) 0.0523(8) Uani 1 1 d . . .
H12A H 0.5364 0.6258 0.2386 0.079 Uiso 1 1 calc R . .
H12B H 0.5153 0.5485 0.2489 0.079 Uiso 1 1 calc R . .
H12C H 0.5913 0.5697 0.2013 0.079 Uiso 1 1 calc R . .
C13 C 0.63863(18) 0.51094(16) 0.3400(2) 0.0527(8) Uani 1 1 d . . .
H13A H 0.6003 0.4755 0.3391 0.079 Uiso 1 1 calc R . .
H13B H 0.6655 0.5101 0.3934 0.079 Uiso 1 1 calc R . .
H13C H 0.6749 0.5037 0.2946 0.079 Uiso 1 1 calc R . .
C14 C 0.66047(18) 0.63352(18) 0.3311(3) 0.0593(9) Uani 1 1 d . . .
H14A H 0.6361 0.6774 0.3264 0.089 Uiso 1 1 calc R . .
H14B H 0.6958 0.6273 0.2846 0.089 Uiso 1 1 calc R . .
H14C H 0.6883 0.6310 0.3838 0.089 Uiso 1 1 calc R . .
C21 C 0.41209(14) 0.44398(13) 0.42681(18) 0.0334(6) Uani 1 1 d . . .
C22 C 0.47557(17) 0.43766(16) 0.4905(2) 0.0489(8) Uani 1 1 d . . .
H22A H 0.5228 0.4551 0.4667 0.073 Uiso 1 1 calc R . .
H22B H 0.4824 0.3905 0.5053 0.073 Uiso 1 1 calc R . .
H22C H 0.4625 0.4633 0.5404 0.073 Uiso 1 1 calc R . .
C23 C 0.4302(2) 0.40343(16) 0.3498(2) 0.0554(9) Uani 1 1 d . . .
H23A H 0.4766 0.4207 0.3240 0.083 Uiso 1 1 calc R . .
H23B H 0.3881 0.4068 0.3103 0.083 Uiso 1 1 calc R . .
H23C H 0.4377 0.3565 0.3654 0.083 Uiso 1 1 calc R . .
C24 C 0.33724(16) 0.42133(17) 0.4651(3) 0.0524(9) Uani 1 1 d . . .
H24A H 0.2964 0.4269 0.4243 0.079 Uiso 1 1 calc R . .
H24B H 0.3262 0.4484 0.5145 0.079 Uiso 1 1 calc R . .
H24C H 0.3410 0.3742 0.4810 0.079 Uiso 1 1 calc R . .
C31 C 0.37733(15) 0.69728(13) 0.32412(19) 0.0373(6) Uani 1 1 d . . .
C32 C 0.3668(2) 0.69627(16) 0.2300(2) 0.0550(9) Uani 1 1 d . . .
H32A H 0.4108 0.6750 0.2039 0.082 Uiso 1 1 calc R . .
H32B H 0.3619 0.7422 0.2094 0.082 Uiso 1 1 calc R . .
H32C H 0.3209 0.6710 0.2161 0.082 Uiso 1 1 calc R . .
C33 C 0.44356(17) 0.74204(15) 0.3482(2) 0.0489(8) Uani 1 1 d . . .
H33A H 0.4905 0.7242 0.3242 0.073 Uiso 1 1 calc R . .
H33B H 0.4481 0.7435 0.4090 0.073 Uiso 1 1 calc R . .
H33C H 0.4348 0.7873 0.3269 0.073 Uiso 1 1 calc R . .
C34 C 0.30427(17) 0.72154(18) 0.3657(3) 0.0590(10) Uani 1 1 d . . .
H34A H 0.3112 0.7224 0.4262 0.089 Uiso 1 1 calc R . .
H34B H 0.2626 0.6912 0.3515 0.089 Uiso 1 1 calc R . .
H34C H 0.2922 0.7666 0.3459 0.089 Uiso 1 1 calc R . .
C41 C 0.41918(16) 0.63174(14) 0.58930(19) 0.0394(6) Uani 1 1 d . . .
C42 C 0.4610(3) 0.6062(2) 0.6662(3) 0.0771(12) Uani 1 1 d . . .
H42A H 0.5109 0.6276 0.6697 0.116 Uiso 1 1 calc R . .
H42B H 0.4673 0.5577 0.6622 0.116 Uiso 1 1 calc R . .
H42C H 0.4315 0.6170 0.7162 0.116 Uiso 1 1 calc R . .
C43 C 0.4097(2) 0.70608(18) 0.5956(3) 0.0648(10) Uani 1 1 d . . .
H43A H 0.3885 0.7233 0.5434 0.097 Uiso 1 1 calc R . .
H43B H 0.4591 0.7269 0.6058 0.097 Uiso 1 1 calc R . .
H43C H 0.3753 0.7166 0.6417 0.097 Uiso 1 1 calc R . .
C44 C 0.34277(19) 0.5976(2) 0.5828(3) 0.0693(11) Uani 1 1 d . . .
H44A H 0.3169 0.6125 0.5321 0.104 Uiso 1 1 calc R . .
H44B H 0.3119 0.6091 0.6315 0.104 Uiso 1 1 calc R . .
H44C H 0.3500 0.5491 0.5807 0.104 Uiso 1 1 calc R . .
C51 C 0.11326(14) 0.42857(14) 0.60099(19) 0.0374(6) Uani 1 1 d . . .
C52 C 0.17515(16) 0.37486(16) 0.6043(2) 0.0509(8) Uani 1 1 d . . .
H52A H 0.1517 0.3309 0.6124 0.076 Uiso 1 1 calc R . .
H52B H 0.2096 0.3843 0.6507 0.076 Uiso 1 1 calc R . .
H52C H 0.2037 0.3750 0.5519 0.076 Uiso 1 1 calc R . .
C53 C 0.14879(18) 0.49582(17) 0.5809(3) 0.0560(9) Uani 1 1 d . . .
H53A H 0.1094 0.5304 0.5807 0.084 Uiso 1 1 calc R . .
H53B H 0.1729 0.4938 0.5260 0.084 Uiso 1 1 calc R . .
H53C H 0.1870 0.5067 0.6232 0.084 Uiso 1 1 calc R . .
C54 C 0.07078(19) 0.4310(2) 0.6828(2) 0.0568(9) Uani 1 1 d . . .
H54A H 0.0306 0.4648 0.6795 0.085 Uiso 1 1 calc R . .
H54B H 0.1060 0.4427 0.7278 0.085 Uiso 1 1 calc R . .
H54C H 0.0482 0.3872 0.6942 0.085 Uiso 1 1 calc R . .
C61 C -0.07236(16) 0.55787(13) 0.48763(19) 0.0378(6) Uani 1 1 d . . .
C62 C -0.01098(17) 0.55858(16) 0.4208(2) 0.0483(7) Uani 1 1 d . . .
H62A H 0.0377 0.5460 0.4456 0.072 Uiso 1 1 calc R . .
H62B H -0.0071 0.6035 0.3969 0.072 Uiso 1 1 calc R . .
H62C H -0.0241 0.5267 0.3768 0.072 Uiso 1 1 calc R . .
C63 C -0.14852(19) 0.57576(18) 0.4499(3) 0.0603(10) Uani 1 1 d . . .
H63A H -0.1870 0.5773 0.4938 0.090 Uiso 1 1 calc R . .
H63B H -0.1626 0.5420 0.4085 0.090 Uiso 1 1 calc R . .
H63C H -0.1451 0.6196 0.4229 0.090 Uiso 1 1 calc R . .
C64 C -0.0531(2) 0.60673(17) 0.5558(3) 0.0601(9) Uani 1 1 d . . .
H64A H -0.0919 0.6046 0.5994 0.090 Uiso 1 1 calc R . .
H64B H -0.0513 0.6520 0.5327 0.090 Uiso 1 1 calc R . .
H64C H -0.0036 0.5953 0.5796 0.090 Uiso 1 1 calc R . .
C71 C -0.06960(16) 0.35978(15) 0.3472(2) 0.0429(7) Uani 1 1 d . . .
C72 C -0.0298(3) 0.3805(2) 0.2688(2) 0.0744(12) Uani 1 1 d . . .
H72A H 0.0180 0.3558 0.2636 0.112 Uiso 1 1 calc R . .
H72B H -0.0192 0.4286 0.2707 0.112 Uiso 1 1 calc R . .
H72C H -0.0621 0.3707 0.2207 0.112 Uiso 1 1 calc R . .
C73 C -0.0785(2) 0.28456(17) 0.3484(3) 0.0640(10) Uani 1 1 d . . .
H73A H -0.0286 0.2636 0.3538 0.096 Uiso 1 1 calc R . .
H73B H -0.1024 0.2699 0.2964 0.096 Uiso 1 1 calc R . .
H73C H -0.1104 0.2715 0.3956 0.096 Uiso 1 1 calc R . .
C74 C -0.1469(2) 0.3943(2) 0.3539(3) 0.0761(12) Uani 1 1 d . . .
H74A H -0.1404 0.4427 0.3481 0.114 Uiso 1 1 calc R . .
H74B H -0.1696 0.3843 0.4082 0.114 Uiso 1 1 calc R . .
H74C H -0.1803 0.3778 0.3096 0.114 Uiso 1 1 calc R . .
C81 C -0.11209(15) 0.31455(14) 0.6209(2) 0.0403(7) Uani 1 1 d . . .
C82 C -0.04730(17) 0.26635(15) 0.6016(3) 0.0531(9) Uani 1 1 d . . .
H82A H -0.0408 0.2629 0.5411 0.080 Uiso 1 1 calc R . .
H82B H -0.0592 0.2222 0.6245 0.080 Uiso 1 1 calc R . .
H82C H -0.0004 0.2830 0.6267 0.080 Uiso 1 1 calc R . .
C83 C -0.18548(17) 0.28817(17) 0.5834(3) 0.0538(9) Uani 1 1 d . . .
H83A H -0.2253 0.3220 0.5889 0.081 Uiso 1 1 calc R . .
H83B H -0.2009 0.2474 0.6127 0.081 Uiso 1 1 calc R . .
H83C H -0.1775 0.2780 0.5243 0.081 Uiso 1 1 calc R . .
C84 C -0.12064(19) 0.32393(17) 0.7147(2) 0.0549(9) Uani 1 1 d . . .
H84A H -0.1598 0.3575 0.7257 0.082 Uiso 1 1 calc R . .
H84B H -0.0723 0.3389 0.7383 0.082 Uiso 1 1 calc R . .
H84C H -0.1353 0.2814 0.7403 0.082 Uiso 1 1 calc R . .
C91 C 0.6896(3) 0.6883(3) 0.6106(4) 0.1053(18) Uani 1 1 d . . .
H91A H 0.6744 0.6594 0.6578 0.126 Uiso 1 1 calc R . .
H91B H 0.7399 0.6735 0.5904 0.126 Uiso 1 1 calc R . .
C92 C 0.6925(3) 0.7527(3) 0.6351(4) 0.110(2) Uani 1 1 d . . .
H92A H 0.6712 0.7568 0.6918 0.132 Uiso 1 1 calc R . .
H92B H 0.7460 0.7676 0.6370 0.132 Uiso 1 1 calc R . .
C93 C 0.6535(4) 0.7921(3) 0.5828(5) 0.123(2) Uani 1 1 d . . .
H93A H 0.6872 0.8270 0.5596 0.148 Uiso 1 1 calc R . .
H93B H 0.6116 0.8144 0.6130 0.148 Uiso 1 1 calc R . .
C94 C 0.6233(2) 0.75111(18) 0.5162(3) 0.0781(13) Uani 1 1 d . . .
H94A H 0.5688 0.7602 0.5073 0.094 Uiso 1 1 calc R . .
H94B H 0.6510 0.7591 0.4635 0.094 Uiso 1 1 calc R . .


_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
Al1 O3 1.7441(18) . ?
Al1 O4 1.747(2) . ?
Al1 O1 1.7516(17) . ?
Al1 O2 1.7511(18) . ?
Al1 Li1 2.684(5) . ?
Al1 Li2 2.691(4) . ?
Al2 O7 1.744(2) . ?
Al2 O6 1.7495(18) . ?
Al2 O5 1.7506(18) . ?
Al2 O8 1.7519(18) . ?
Al2 Li4 2.677(4) . ?
Al2 Li3 2.686(4) . ?
Al3 Li4 3.145(5) 2_564 ?
Al3 Li2 3.177(4) . ?
Al3 H31 1.51(4) . ?
Al3 H32 1.62(3) . ?
Al3 H33 1.48(4) . ?
Al3 H34 1.58(3) . ?
Al4 H41 1.52(4) . ?
Al4 H42 1.55(3) . ?
Al4 H43 1.45(4) . ?
Al4 H44 1.62(3) . ?
Li1 O9 1.941(5) . ?
Li1 O4 1.941(5) . ?
Li1 O1 1.944(5) . ?
Li1 H44 1.92(3) . ?
Li2 O2 1.930(5) . ?
Li2 O3 1.960(5) . ?
Li2 H34 1.90(3) . ?
Li3 O5 1.938(5) . ?
Li3 O7 1.950(5) . ?
Li3 O0 1.958(5) . ?
Li3 H33 1.95(4) . ?
Li4 O6 1.933(5) . ?
Li4 O8 1.936(5) . ?
Li4 Al3 3.145(5) 2_565 ?
O0 C01 1.422(4) . ?
O0 C04 1.429(4) . ?
O1 C11 1.426(3) . ?
O2 C21 1.426(3) . ?
O3 C31 1.431(3) . ?
O4 C41 1.431(3) . ?
O5 C51 1.430(3) . ?
O6 C61 1.427(3) . ?
O7 C71 1.428(3) . ?
O8 C81 1.422(3) . ?
O9 C91 1.426(5) . ?
O9 C94 1.430(5) . ?
C01 C02 1.352(5) . ?
C01 H01A 0.9900 . ?
C01 H01B 0.9900 . ?
C02 C03 1.377(5) . ?
C02 H02A 0.9900 . ?
C02 H02B 0.9900 . ?
C03 C04 1.485(5) . ?
C03 H03A 0.9900 . ?
C03 H03B 0.9900 . ?
C04 H04A 0.9900 . ?
C04 H04B 0.9900 . ?
C11 C12 1.515(4) . ?
C11 C14 1.529(4) . ?
C11 C13 1.529(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 C23 1.513(5) . ?
C21 C22 1.521(4) . ?
C21 C24 1.525(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C33 1.522(4) . ?
C31 C32 1.523(5) . ?
C31 C34 1.530(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C41 C43 1.501(5) . ?
C41 C44 1.515(4) . ?
C41 C42 1.526(5) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C51 C54 1.514(5) . ?
C51 C53 1.519(4) . ?
C51 C52 1.533(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C61 C64 1.506(5) . ?
C61 C63 1.517(4) . ?
C61 C62 1.525(4) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C71 C72 1.501(5) . ?
C71 C73 1.514(5) . ?
C71 C74 1.532(5) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C81 C83 1.523(4) . ?
C81 C84 1.525(5) . ?
C81 C82 1.527(4) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C91 C92 1.348(7) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 C93 1.341(8) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 C94 1.449(7) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Al1 O4 119.38(9) . . ?
O3 Al1 O1 119.06(9) . . ?
O4 Al1 O1 91.88(9) . . ?
O3 Al1 O2 91.87(8) . . ?
O4 Al1 O2 118.95(10) . . ?
O1 Al1 O2 118.29(9) . . ?
O3 Al1 Li1 140.87(13) . . ?
O4 Al1 Li1 46.22(13) . . ?
O1 Al1 Li1 46.32(13) . . ?
O2 Al1 Li1 127.26(13) . . ?
O3 Al1 Li2 46.67(12) . . ?
O4 Al1 Li2 139.99(13) . . ?
O1 Al1 Li2 128.12(13) . . ?
O2 Al1 Li2 45.71(12) . . ?
Li1 Al1 Li2 170.66(15) . . ?
O7 Al2 O6 119.38(10) . . ?
O7 Al2 O5 92.27(9) . . ?
O6 Al2 O5 117.87(9) . . ?
O7 Al2 O8 119.46(10) . . ?
O6 Al2 O8 92.10(9) . . ?
O5 Al2 O8 118.27(10) . . ?
O7 Al2 Li4 139.14(13) . . ?
O6 Al2 Li4 46.13(12) . . ?
O5 Al2 Li4 128.59(13) . . ?
O8 Al2 Li4 46.25(11) . . ?
O7 Al2 Li3 46.47(12) . . ?
O6 Al2 Li3 129.66(12) . . ?
O5 Al2 Li3 46.08(13) . . ?
O8 Al2 Li3 138.21(12) . . ?
Li4 Al2 Li3 173.04(15) . . ?
Li4 Al3 Li2 97.39(12) 2_564 . ?
Li4 Al3 H31 28.6(13) 2_564 . ?
Li2 Al3 H31 121.1(13) . . ?
Li4 Al3 H32 88.8(13) 2_564 . ?
Li2 Al3 H32 84.7(12) . . ?
H31 Al3 H32 105.9(19) . . ?
Li4 Al3 H33 134.6(13) 2_564 . ?
Li2 Al3 H33 122.7(14) . . ?
H31 Al3 H33 106.0(18) . . ?
H32 Al3 H33 113.2(18) . . ?
Li4 Al3 H34 98.7(13) 2_564 . ?
Li2 Al3 H34 26.6(12) . . ?
H31 Al3 H34 112.2(18) . . ?
H32 Al3 H34 111.3(17) . . ?
H33 Al3 H34 108.2(19) . . ?
H41 Al4 H42 108(2) . . ?
H41 Al4 H43 119(2) . . ?
H42 Al4 H43 108(2) . . ?
H41 Al4 H44 115.6(18) . . ?
H42 Al4 H44 102.4(18) . . ?
H43 Al4 H44 101.9(19) . . ?
O9 Li1 O4 117.5(3) . . ?
O9 Li1 O1 121.8(3) . . ?
O4 Li1 O1 80.65(19) . . ?
O9 Li1 Al1 135.6(2) . . ?
O4 Li1 Al1 40.53(10) . . ?
O1 Li1 Al1 40.67(10) . . ?
O9 Li1 H44 98.8(10) . . ?
O4 Li1 H44 130.0(11) . . ?
O1 Li1 H44 109.4(11) . . ?
Al1 Li1 H44 124.8(11) . . ?
O2 Li2 O3 80.41(18) . . ?
O2 Li2 Al1 40.49(10) . . ?
O3 Li2 Al1 40.34(10) . . ?
O2 Li2 Al3 115.8(2) . . ?
O3 Li2 Al3 147.0(2) . . ?
Al1 Li2 Al3 150.19(19) . . ?
O2 Li2 H34 117.4(11) . . ?
O3 Li2 H34 125.6(11) . . ?
Al1 Li2 H34 137.5(12) . . ?
Al3 Li2 H34 21.8(11) . . ?
O5 Li3 O7 80.78(18) . . ?
O5 Li3 O0 121.7(3) . . ?
O7 Li3 O0 117.6(3) . . ?
O5 Li3 Al2 40.59(10) . . ?
O7 Li3 Al2 40.41(10) . . ?
O0 Li3 Al2 133.8(2) . . ?
O5 Li3 H33 115.3(11) . . ?
O7 Li3 H33 115.4(10) . . ?
O0 Li3 H33 105.3(10) . . ?
Al2 Li3 H33 120.9(10) . . ?
O6 Li4 O8 81.32(19) . . ?
O6 Li4 Al2 40.74(10) . . ?
O8 Li4 Al2 40.82(10) . . ?
O6 Li4 Al3 130.8(2) . 2_565 ?
O8 Li4 Al3 130.2(2) . 2_565 ?
Al2 Li4 Al3 145.50(18) . 2_565 ?
C01 O0 C04 105.6(3) . . ?
C01 O0 Li3 129.2(3) . . ?
C04 O0 Li3 124.7(2) . . ?
C11 O1 Al1 138.28(17) . . ?
C11 O1 Li1 128.6(2) . . ?
Al1 O1 Li1 93.01(17) . . ?
C21 O2 Al1 136.84(15) . . ?
C21 O2 Li2 128.6(2) . . ?
Al1 O2 Li2 93.80(16) . . ?
C31 O3 Al1 138.46(16) . . ?
C31 O3 Li2 128.5(2) . . ?
Al1 O3 Li2 92.99(15) . . ?
C41 O4 Al1 137.57(16) . . ?
C41 O4 Li1 128.7(2) . . ?
Al1 O4 Li1 93.26(18) . . ?
C51 O5 Al2 137.23(17) . . ?
C51 O5 Li3 129.0(2) . . ?
Al2 O5 Li3 93.33(17) . . ?
C61 O6 Al2 138.50(17) . . ?
C61 O6 Li4 128.3(2) . . ?
Al2 O6 Li4 93.13(16) . . ?
C71 O7 Al2 138.28(17) . . ?
C71 O7 Li3 128.4(2) . . ?
Al2 O7 Li3 93.12(17) . . ?
C81 O8 Al2 138.75(16) . . ?
C81 O8 Li4 128.2(2) . . ?
Al2 O8 Li4 92.94(16) . . ?
C91 O9 C94 106.6(3) . . ?
C91 O9 Li1 127.7(3) . . ?
C94 O9 Li1 125.0(3) . . ?
C02 C01 O0 106.5(3) . . ?
C02 C01 H01A 110.4 . . ?
O0 C01 H01A 110.4 . . ?
C02 C01 H01B 110.4 . . ?
O0 C01 H01B 110.4 . . ?
H01A C01 H01B 108.6 . . ?
C01 C02 C03 108.0(3) . . ?
C01 C02 H02A 110.1 . . ?
C03 C02 H02A 110.1 . . ?
C01 C02 H02B 110.1 . . ?
C03 C02 H02B 110.1 . . ?
H02A C02 H02B 108.4 . . ?
C02 C03 C04 106.5(3) . . ?
C02 C03 H03A 110.4 . . ?
C04 C03 H03A 110.4 . . ?
C02 C03 H03B 110.4 . . ?
C04 C03 H03B 110.4 . . ?
H03A C03 H03B 108.6 . . ?
O0 C04 C03 104.0(3) . . ?
O0 C04 H04A 111.0 . . ?
C03 C04 H04A 111.0 . . ?
O0 C04 H04B 111.0 . . ?
C03 C04 H04B 111.0 . . ?
H04A C04 H04B 109.0 . . ?
O1 C11 C12 110.4(2) . . ?
O1 C11 C14 107.7(2) . . ?
C12 C11 C14 110.6(3) . . ?
O1 C11 C13 108.7(2) . . ?
C12 C11 C13 110.5(3) . . ?
C14 C11 C13 108.8(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C21 C23 107.1(2) . . ?
O2 C21 C22 110.3(2) . . ?
C23 C21 C22 110.4(3) . . ?
O2 C21 C24 108.4(2) . . ?
C23 C21 C24 110.6(3) . . ?
C22 C21 C24 110.0(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C31 C33 110.4(2) . . ?
O3 C31 C32 107.8(2) . . ?
C33 C31 C32 110.7(3) . . ?
O3 C31 C34 107.9(2) . . ?
C33 C31 C34 110.4(3) . . ?
C32 C31 C34 109.5(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O4 C41 C43 109.8(3) . . ?
O4 C41 C44 110.6(3) . . ?
C43 C41 C44 110.7(3) . . ?
O4 C41 C42 106.9(2) . . ?
C43 C41 C42 109.3(3) . . ?
C44 C41 C42 109.5(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O5 C51 C54 110.2(2) . . ?
O5 C51 C53 109.2(2) . . ?
C54 C51 C53 111.1(3) . . ?
O5 C51 C52 106.5(2) . . ?
C54 C51 C52 110.2(3) . . ?
C53 C51 C52 109.6(2) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O6 C61 C64 108.4(3) . . ?
O6 C61 C63 108.2(2) . . ?
C64 C61 C63 109.7(3) . . ?
O6 C61 C62 110.1(2) . . ?
C64 C61 C62 110.2(3) . . ?
C63 C61 C62 110.2(3) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O7 C71 C72 107.8(2) . . ?
O7 C71 C73 108.7(3) . . ?
C72 C71 C73 109.5(3) . . ?
O7 C71 C74 109.5(3) . . ?
C72 C71 C74 110.5(3) . . ?
C73 C71 C74 110.7(3) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O8 C81 C83 108.1(2) . . ?
O8 C81 C84 107.6(3) . . ?
C83 C81 C84 110.5(3) . . ?
O8 C81 C82 110.3(2) . . ?
C83 C81 C82 109.7(3) . . ?
C84 C81 C82 110.6(3) . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C81 C84 H84A 109.5 . . ?
C81 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C81 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C92 C91 O9 107.0(4) . . ?
C92 C91 H91A 110.3 . . ?
O9 C91 H91A 110.3 . . ?
C92 C91 H91B 110.3 . . ?
O9 C91 H91B 110.3 . . ?
H91A C91 H91B 108.6 . . ?
C93 C92 C91 111.1(5) . . ?
C93 C92 H92A 109.4 . . ?
C91 C92 H92A 109.4 . . ?
C93 C92 H92B 109.4 . . ?
C91 C92 H92B 109.4 . . ?
H92A C92 H92B 108.0 . . ?
C92 C93 C94 108.5(4) . . ?
C92 C93 H93A 110.0 . . ?
C94 C93 H93A 110.0 . . ?
C92 C93 H93B 110.0 . . ?
C94 C93 H93B 110.0 . . ?
H93A C93 H93B 108.4 . . ?
O9 C94 C93 103.5(5) . . ?
O9 C94 H94A 111.1 . . ?
C93 C94 H94A 111.1 . . ?
O9 C94 H94B 111.1 . . ?
C93 C94 H94B 111.1 . . ?
H94A C94 H94B 109.0 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.86
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.042
_database_code_depnum_ccdc_archive 'CCDC 981536'
