# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2001
# CCDC Number: 186/2230

data_global
_publ_contact_letter
;
 These are the CIF format data (4 compounds) for the paper 

  "Neutral and cationic organometallic aluminium and
  indium complexes of mono-pendant arm triazacyclononane
  ligands"

  D. A. Robson, S. Y. Bylikin, M. Cantuel, N. A. H. Male, 
  L. H. Rees, P. Mountford and M. Schroeder

;
_publ_contact_author
;
 Dr P. Mountford           
 Inorganic Chemistry Laboratory
 South Parks Road
 Oxford
 OX1 3QR
 UK
;                                           
_publ_contact_author_phone      '+44 1865 272679'
_contact_author_fax             '+44 1865 272690'
_publ_contact_author_email      Philip.Mountford@chem.ox.ac.uk

data_compound_7

#  Local code str28
 
_chemical_name_systematic
;
 [Al2(L-4)2Me4] 
;
 
_audit_creation_method            SHELXL
_chemical_name_common             ?
_chemical_formula_moiety          'C16 H33 Al1 N3 O1'
_chemical_formula_structural      'C16 H33 AL1 N3 O1'
_chemical_formula_analytical      ?
_chemical_formula_sum             'C34 H76 Al2 N6 O2'
_chemical_formula_weight          654.97
_chemical_melting_point           ?
_chemical_compound_source         'synthesis as described'
 
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            monoclinic
_symmetry_space_group_name_H-M    'P 21'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    12.2690(5)
_cell_length_b                    13.4100(6)
_cell_length_c                    12.4290(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  95.998(2)
_cell_angle_gamma                 90.00
_cell_volume                      2033.71(14)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       0
_cell_measurement_theta_max       0
 
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.3
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.3
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.070
_exptl_crystal_density_method     none
_exptl_crystal_F_000              728
_exptl_absorpt_coefficient_mu     0.106
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        ?
_diffrn_measurement_method        ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             4232
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0452
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          1.67
_diffrn_reflns_theta_max          26.49
_reflns_number_total              4232
_reflns_number_observed           4128
_reflns_observed_criterion        >2sigma(I)
 
_computing_data_collection        'Enraf-Nonius DIP2000 Software - XPRESS'
_computing_cell_refinement        DENZO
_computing_data_reduction         'DENZO & SCALEPACK'
_computing_structure_solution     SIR-92
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1998)'
 
_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^
 or flagged by the user for potential systematic errors.  Weighted R-factors
 wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
 are based on F, with F set to zero for negative F^2^. The observed criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+1.6410P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_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    0.09(28)
_refine_ls_number_reflns          4231
_refine_ls_number_parameters      411
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0726
_refine_ls_R_factor_obs           0.0691
_refine_ls_wR_factor_all          0.1740
_refine_ls_wR_factor_obs          0.1677
_refine_ls_goodness_of_fit_all    1.298
_refine_ls_goodness_of_fit_obs    1.311
_refine_ls_restrained_S_all       1.342
_refine_ls_restrained_S_obs       1.310
_refine_ls_shift/esd_max          0.011
_refine_ls_shift/esd_mean         0.001
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Al1 Al 0.71753(11) 0.95307(10) 0.74961(10) 0.0161(3) Uani 1 d . .
Al2 Al 0.71583(10) 1.12201(10) 0.59199(10) 0.0158(3) Uani 1 d . .
N1 N 0.8669(3) 0.8556(3) 0.7579(3) 0.0198(8) Uani 1 d . .
C2 C 0.8583(4) 0.7551(4) 0.8075(4) 0.0227(10) Uani 1 d . .
H2A H 0.9273(4) 0.7206(4) 0.8037(4) 0.027 Uiso 1 calc R .
H2B H 0.8023(4) 0.7178(4) 0.7637(4) 0.027 Uiso 1 calc R .
C3 C 0.8317(4) 0.7519(4) 0.9234(4) 0.0263(11) Uani 1 d . .
H3A H 0.7659(4) 0.7908(4) 0.9290(4) 0.032 Uiso 1 calc R .
H3B H 0.8155(4) 0.6834(4) 0.9414(4) 0.032 Uiso 1 calc R .
N4 N 0.9176(3) 0.7888(3) 1.0025(3) 0.0242(9) Uani 1 d . .
C41 C 0.8778(5) 0.8070(5) 1.1080(4) 0.0337(13) Uani 1 d . .
H41 H 0.8098(5) 0.8454(5) 1.0938(4) 0.040 Uiso 1 calc R .
C42 C 0.9573(6) 0.8726(6) 1.1770(5) 0.045(2) Uani 1 d . .
H42A H 0.9249(17) 0.8929(31) 1.2406(21) 0.067 Uiso 1 calc R .
H42B H 0.9741(33) 0.9305(19) 1.1364(15) 0.067 Uiso 1 calc R .
H42C H 1.0234(17) 0.8361(13) 1.1979(34) 0.067 Uiso 1 calc R .
C43 C 0.8487(6) 0.7132(6) 1.1688(5) 0.047(2) Uani 1 d . .
H43A H 0.8188(39) 0.7319(6) 1.2343(21) 0.071 Uiso 1 calc R .
H43B H 0.9134(9) 0.6738(19) 1.1862(36) 0.071 Uiso 1 calc R .
H43C H 0.7955(31) 0.6749(20) 1.1241(17) 0.071 Uiso 1 calc R .
C5 C 1.0193(4) 0.7309(4) 1.0065(4) 0.0281(11) Uani 1 d . .
H5A H 1.0041(4) 0.6687(4) 0.9678(4) 0.034 Uiso 1 calc R .
H5B H 1.0430(4) 0.7145(4) 1.0813(4) 0.034 Uiso 1 calc R .
C6 C 1.1132(4) 0.7845(5) 0.9579(4) 0.0292(11) Uani 1 d . .
H6A H 1.1169(4) 0.8525(5) 0.9845(4) 0.035 Uiso 1 calc R .
H6B H 1.1815(4) 0.7519(5) 0.9839(4) 0.035 Uiso 1 calc R .
N7 N 1.1039(3) 0.7868(3) 0.8390(3) 0.0254(9) Uani 1 d . .
C71 C 1.1963(5) 0.7400(5) 0.7908(5) 0.0332(12) Uani 1 d . .
H71 H 1.1812(5) 0.7485(5) 0.7124(5) 0.040 Uiso 1 calc R .
C72 C 1.3065(5) 0.7889(7) 0.8229(6) 0.055(2) Uani 1 d . .
H72A H 1.3609(11) 0.7594(31) 0.7826(35) 0.083 Uiso 1 calc R .
H72B H 1.3270(23) 0.7792(38) 0.8988(12) 0.083 Uiso 1 calc R .
H72C H 1.3015(14) 0.8590(10) 0.8075(44) 0.083 Uiso 1 calc R .
C73 C 1.1972(6) 0.6289(6) 0.8115(5) 0.051(2) Uani 1 d . .
H73A H 1.2173(40) 0.6165(6) 0.8871(9) 0.076 Uiso 1 calc R .
H73B H 1.2493(30) 0.5975(8) 0.7700(32) 0.076 Uiso 1 calc R .
H73C H 1.1256(12) 0.6020(9) 0.7907(38) 0.076 Uiso 1 calc R .
C8 C 1.0750(4) 0.8842(4) 0.7939(4) 0.0266(11) Uani 1 d . .
H8A H 1.0836(4) 0.8833(4) 0.7172(4) 0.032 Uiso 1 calc R .
H8B H 1.1258(4) 0.9331(4) 0.8277(4) 0.032 Uiso 1 calc R .
C9 C 0.9590(4) 0.9169(4) 0.8085(4) 0.0208(10) Uani 1 d . .
H9A H 0.9525(4) 0.9200(4) 0.8856(4) 0.025 Uiso 1 calc R .
H9B H 0.9494(4) 0.9842(4) 0.7806(4) 0.025 Uiso 1 calc R .
C10 C 0.8754(4) 0.8398(4) 0.6417(4) 0.0213(10) Uani 1 d . .
H10A H 0.8196(4) 0.7930(4) 0.6129(4) 0.026 Uiso 1 calc R .
H10B H 0.9465(4) 0.8116(4) 0.6320(4) 0.026 Uiso 1 calc R .
C11 C 0.8610(4) 0.9377(4) 0.5807(4) 0.0213(10) Uani 1 d . .
H11 H 0.9286(4) 0.9768(4) 0.5932(4) 0.026 Uiso 1 calc R .
C12 C 0.8362(5) 0.9175(5) 0.4610(4) 0.0326(12) Uani 1 d . .
H12A H 0.8935(19) 0.8772(27) 0.4366(8) 0.049 Uiso 1 calc R .
H12B H 0.8319(34) 0.9796(5) 0.4223(5) 0.049 Uiso 1 calc R .
H12C H 0.7676(18) 0.8829(28) 0.4481(6) 0.049 Uiso 1 calc R .
O13 O 0.7751(3) 0.9893(2) 0.6236(2) 0.0183(7) Uani 1 d . .
C14 C 0.7527(4) 1.0093(4) 0.8961(4) 0.0231(10) Uani 1 d . .
H14A H 0.7981(26) 0.9633(13) 0.9398(10) 0.035 Uiso 1 calc R .
H14B H 0.6861(4) 1.0206(26) 0.9286(12) 0.035 Uiso 1 calc R .
H14C H 0.7910(27) 1.0713(14) 0.8913(4) 0.035 Uiso 1 calc R .
C15 C 0.6090(4) 0.8448(4) 0.7256(5) 0.0273(11) Uani 1 d . .
H15A H 0.5396(9) 0.8721(5) 0.6971(30) 0.041 Uiso 1 calc R .
H15B H 0.6013(24) 0.8118(19) 0.7930(7) 0.041 Uiso 1 calc R .
H15C H 0.6332(16) 0.7977(16) 0.6751(25) 0.041 Uiso 1 calc R .
N16 N 0.6268(3) 1.2606(3) 0.6395(3) 0.0190(8) Uani 1 d . .
C17 C 0.5905(4) 1.3326(4) 0.5514(4) 0.0226(10) Uani 1 d . .
H17A H 0.5460(4) 1.3834(4) 0.5812(4) 0.027 Uiso 1 calc R .
H17B H 0.5438(4) 1.2972(4) 0.4963(4) 0.027 Uiso 1 calc R .
C18 C 0.6797(4) 1.3839(4) 0.4975(4) 0.0241(10) Uani 1 d . .
H18A H 0.7310(4) 1.3339(4) 0.4774(4) 0.029 Uiso 1 calc R .
H18B H 0.6471(4) 1.4152(4) 0.4315(4) 0.029 Uiso 1 calc R .
N19 N 0.7403(3) 1.4594(3) 0.5640(3) 0.0239(9) Uani 1 d . .
C191 C 0.8379(4) 1.4948(4) 0.5177(4) 0.0254(10) Uani 1 d . .
H191 H 0.8772(4) 1.4353(4) 0.4972(4) 0.030 Uiso 1 calc R .
C192 C 0.9137(4) 1.5484(5) 0.6019(5) 0.0315(12) Uani 1 d . .
H19A H 0.9810(14) 1.5638(29) 0.5726(12) 0.047 Uiso 1 calc R .
H19B H 0.9286(28) 1.5064(13) 0.6643(14) 0.047 Uiso 1 calc R .
H19C H 0.8796(15) 1.6090(16) 0.6223(26) 0.047 Uiso 1 calc R .
C193 C 0.8155(5) 1.5577(5) 0.4153(5) 0.0336(13) Uani 1 d . .
H19D H 0.8836(5) 1.5741(28) 0.3880(20) 0.050 Uiso 1 calc R .
H19E H 0.7785(32) 1.6180(15) 0.4320(8) 0.050 Uiso 1 calc R .
H19F H 0.7702(30) 1.5207(13) 0.3617(13) 0.050 Uiso 1 calc R .
C20 C 0.6706(4) 1.5382(4) 0.6011(5) 0.0285(11) Uani 1 d . .
H20A H 0.5988(4) 1.5334(4) 0.5606(5) 0.034 Uiso 1 calc R .
H20B H 0.7014(4) 1.6023(4) 0.5842(5) 0.034 Uiso 1 calc R .
C21 C 0.6563(4) 1.5360(4) 0.7215(4) 0.0289(11) Uani 1 d . .
H21A H 0.7279(4) 1.5266(4) 0.7613(4) 0.035 Uiso 1 calc R .
H21B H 0.6296(4) 1.6008(4) 0.7416(4) 0.035 Uiso 1 calc R .
N22 N 0.5826(3) 1.4598(3) 0.7569(3) 0.0233(8) Uani 1 d . .
C221 C 0.5006(5) 1.5032(4) 0.8230(4) 0.0293(11) Uani 1 d . .
H221 H 0.4699(5) 1.5619(4) 0.7839(4) 0.035 Uiso 1 calc R .
C222 C 0.4064(5) 1.4315(5) 0.8318(5) 0.0379(14) Uani 1 d . .
H22A H 0.3508(18) 1.4636(12) 0.8683(34) 0.057 Uiso 1 calc R .
H22B H 0.4326(9) 1.3736(16) 0.8719(33) 0.057 Uiso 1 calc R .
H22C H 0.3760(25) 1.4118(27) 0.7606(5) 0.057 Uiso 1 calc R .
C223 C 0.5484(6) 1.5390(5) 0.9337(5) 0.046(2) Uani 1 d . .
H22D H 0.4924(12) 1.5717(34) 0.9692(18) 0.068 Uiso 1 calc R .
H22E H 0.6070(29) 1.5850(30) 0.9258(6) 0.068 Uiso 1 calc R .
H22F H 0.5761(38) 1.4830(7) 0.9763(15) 0.068 Uiso 1 calc R .
C23 C 0.6403(4) 1.3749(4) 0.8078(4) 0.0255(10) Uani 1 d . .
H23A H 0.5888(4) 1.3353(4) 0.8439(4) 0.031 Uiso 1 calc R .
H23B H 0.6959(4) 1.3991(4) 0.8627(4) 0.031 Uiso 1 calc R .
C24 C 0.6950(4) 1.3077(3) 0.7306(4) 0.0189(9) Uani 1 d . .
H24A H 0.7510(4) 1.3466(3) 0.7004(4) 0.023 Uiso 1 calc R .
H24B H 0.7321(4) 1.2547(3) 0.7731(4) 0.023 Uiso 1 calc R .
C25 C 0.5279(4) 1.2144(4) 0.6739(4) 0.0201(10) Uani 1 d . .
H25A H 0.4815(4) 1.1907(4) 0.6111(4) 0.024 Uiso 1 calc R .
H25B H 0.4869(4) 1.2633(4) 0.7108(4) 0.024 Uiso 1 calc R .
C26 C 0.5594(4) 1.1280(4) 0.7492(3) 0.0198(9) Uani 1 d . .
H26 H 0.5930(4) 1.1540(4) 0.8186(3) 0.024 Uiso 1 calc R .
C27 C 0.4611(4) 1.0653(4) 0.7683(5) 0.0297(11) Uani 1 d . .
H27A H 0.4094(16) 1.1053(9) 0.8020(30) 0.044 Uiso 1 calc R .
H27B H 0.4841(6) 1.0103(18) 0.8147(27) 0.044 Uiso 1 calc R .
H27C H 0.4274(20) 1.0404(26) 0.7004(6) 0.044 Uiso 1 calc R .
O28 O 0.6384(3) 1.0719(2) 0.6995(3) 0.0179(7) Uani 1 d . .
C29 C 0.6394(4) 1.1074(4) 0.4457(4) 0.0253(11) Uani 1 d . .
H29A H 0.6275(28) 1.0380(4) 0.4299(12) 0.038 Uiso 1 calc R .
H29B H 0.6833(15) 1.1360(26) 0.3940(5) 0.038 Uiso 1 calc R .
H29C H 0.5702(15) 1.1412(25) 0.4419(10) 0.038 Uiso 1 calc R .
C30 C 0.8624(4) 1.1859(4) 0.6065(5) 0.0252(11) Uani 1 d . .
H30A H 0.8542(4) 1.2567(5) 0.5972(31) 0.038 Uiso 1 calc R .
H30B H 0.9050(12) 1.1598(21) 0.5524(20) 0.038 Uiso 1 calc R .
H30C H 0.8990(13) 1.1722(24) 0.6771(12) 0.038 Uiso 1 calc R .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Al1 0.0199(6) 0.0144(6) 0.0138(6) 0.0006(5) 0.0011(5) -0.0012(6)
Al2 0.0160(6) 0.0166(6) 0.0147(6) 0.0018(5) 0.0005(5) -0.0022(5)
N1 0.026(2) 0.015(2) 0.019(2) 0.000(2) 0.003(2) 0.002(2)
C2 0.028(2) 0.018(2) 0.021(2) -0.002(2) 0.000(2) -0.003(2)
C3 0.028(2) 0.021(3) 0.031(3) 0.009(2) 0.007(2) -0.001(2)
N4 0.024(2) 0.027(2) 0.022(2) 0.002(2) 0.005(2) 0.003(2)
C41 0.035(3) 0.045(3) 0.023(2) 0.008(2) 0.012(2) 0.014(3)
C42 0.055(4) 0.055(4) 0.025(3) -0.007(3) 0.007(3) 0.013(3)
C43 0.047(4) 0.063(5) 0.035(3) 0.018(3) 0.018(3) 0.008(3)
C5 0.034(3) 0.033(3) 0.017(2) 0.006(2) 0.004(2) 0.005(2)
C6 0.026(2) 0.037(3) 0.025(2) 0.001(2) 0.000(2) 0.012(2)
N7 0.023(2) 0.029(2) 0.025(2) 0.004(2) 0.003(2) 0.005(2)
C71 0.031(3) 0.039(3) 0.031(3) 0.006(2) 0.008(2) 0.009(2)
C72 0.028(3) 0.075(5) 0.065(4) 0.006(4) 0.014(3) 0.009(3)
C73 0.064(4) 0.051(4) 0.041(3) 0.011(3) 0.022(3) 0.028(4)
C8 0.019(2) 0.032(3) 0.029(3) -0.001(2) 0.002(2) -0.002(2)
C9 0.021(2) 0.020(2) 0.021(2) 0.003(2) -0.001(2) 0.003(2)
C10 0.024(2) 0.018(2) 0.022(2) -0.005(2) 0.002(2) 0.004(2)
C11 0.024(2) 0.022(3) 0.019(2) 0.000(2) 0.008(2) 0.003(2)
C12 0.042(3) 0.033(3) 0.024(3) 0.000(2) 0.008(2) 0.013(2)
O13 0.026(2) 0.014(2) 0.0155(15) 0.0024(12) 0.0049(13) 0.0028(13)
C14 0.029(2) 0.022(3) 0.017(2) -0.004(2) -0.003(2) 0.007(2)
C15 0.022(2) 0.021(3) 0.039(3) 0.003(2) -0.001(2) -0.004(2)
N16 0.016(2) 0.019(2) 0.022(2) 0.003(2) -0.0001(15) -0.002(2)
C17 0.025(2) 0.019(2) 0.022(2) 0.000(2) -0.005(2) 0.002(2)
C18 0.029(2) 0.022(2) 0.020(2) 0.002(2) 0.000(2) 0.006(2)
N19 0.025(2) 0.020(2) 0.027(2) 0.002(2) 0.006(2) 0.007(2)
C191 0.027(2) 0.020(2) 0.030(3) 0.003(2) 0.008(2) 0.003(2)
C192 0.025(2) 0.035(3) 0.036(3) -0.001(2) 0.007(2) -0.002(2)
C193 0.029(3) 0.041(3) 0.033(3) 0.009(2) 0.012(2) 0.003(2)
C20 0.031(3) 0.018(3) 0.039(3) 0.002(2) 0.013(2) 0.003(2)
C21 0.033(3) 0.019(3) 0.036(3) -0.003(2) 0.012(2) 0.002(2)
N22 0.026(2) 0.018(2) 0.027(2) 0.000(2) 0.007(2) 0.001(2)
C221 0.036(3) 0.024(3) 0.030(3) -0.001(2) 0.010(2) 0.010(2)
C222 0.032(3) 0.035(3) 0.049(3) 0.007(3) 0.018(3) 0.009(2)
C223 0.056(4) 0.044(4) 0.040(3) -0.007(3) 0.021(3) 0.009(3)
C23 0.027(2) 0.024(3) 0.025(2) -0.003(2) 0.000(2) 0.000(2)
C24 0.018(2) 0.015(2) 0.023(2) 0.008(2) -0.001(2) 0.008(2)
C25 0.018(2) 0.020(2) 0.021(2) -0.004(2) 0.000(2) 0.002(2)
C26 0.020(2) 0.022(2) 0.016(2) -0.002(2) 0.000(2) -0.003(2)
C27 0.027(2) 0.030(3) 0.033(3) -0.002(2) 0.011(2) 0.000(2)
O28 0.019(2) 0.017(2) 0.018(2) 0.0068(13) 0.0054(13) 0.0036(13)
C29 0.031(2) 0.029(3) 0.015(2) -0.001(2) -0.001(2) -0.001(2)
C30 0.014(2) 0.025(3) 0.037(3) -0.004(2) 0.003(2) -0.004(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
Al1 O13 1.849(3) . ?
Al1 O28 1.935(3) . ?
Al1 C15 1.972(5) . ?
Al1 C14 1.977(5) . ?
Al1 N1 2.245(4) . ?
Al1 Al2 2.994(2) . ?
Al2 O28 1.845(3) . ?
Al2 O13 1.946(3) . ?
Al2 C29 1.966(5) . ?
Al2 C30 1.983(5) . ?
Al2 N16 2.265(4) . ?
N1 C10 1.474(6) . ?
N1 C9 1.484(6) . ?
N1 C2 1.490(6) . ?
C2 C3 1.510(7) . ?
C3 N4 1.452(7) . ?
N4 C5 1.466(7) . ?
N4 C41 1.467(7) . ?
C41 C42 1.512(9) . ?
C41 C43 1.530(9) . ?
C5 C6 1.534(8) . ?
C6 N7 1.471(6) . ?
N7 C8 1.451(7) . ?
N7 C71 1.477(7) . ?
C71 C73 1.512(10) . ?
C71 C72 1.519(9) . ?
C8 C9 1.518(7) . ?
C10 C11 1.517(7) . ?
C11 O13 1.412(5) . ?
C11 C12 1.512(7) . ?
N16 C25 1.466(6) . ?
N16 C24 1.477(6) . ?
N16 C17 1.492(6) . ?
C17 C18 1.508(7) . ?
C18 N19 1.461(7) . ?
N19 C191 1.460(6) . ?
N19 C20 1.464(6) . ?
C191 C192 1.507(8) . ?
C191 C193 1.528(7) . ?
C20 C21 1.525(7) . ?
C21 N22 1.463(7) . ?
N22 C23 1.451(7) . ?
N22 C221 1.482(6) . ?
C221 C223 1.516(9) . ?
C221 C222 1.517(8) . ?
C23 C24 1.522(7) . ?
C25 C26 1.513(7) . ?
C26 O28 1.419(6) . ?
C26 C27 1.509(7) . ?
 
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
O13 Al1 O28 74.56(14) . . ?
O13 Al1 C15 112.2(2) . . ?
O28 Al1 C15 104.5(2) . . ?
O13 Al1 C14 127.9(2) . . ?
O28 Al1 C14 92.1(2) . . ?
C15 Al1 C14 120.0(2) . . ?
O13 Al1 N1 79.05(15) . . ?
O28 Al1 N1 151.0(2) . . ?
C15 Al1 N1 96.5(2) . . ?
C14 Al1 N1 94.7(2) . . ?
O13 Al1 Al2 39.09(11) . . ?
O28 Al1 Al2 36.59(10) . . ?
C15 Al1 Al2 120.0(2) . . ?
C14 Al1 Al2 107.5(2) . . ?
N1 Al1 Al2 114.88(11) . . ?
O28 Al2 O13 74.36(14) . . ?
O28 Al2 C29 113.7(2) . . ?
O13 Al2 C29 103.2(2) . . ?
O28 Al2 C30 128.4(2) . . ?
O13 Al2 C30 93.5(2) . . ?
C29 Al2 C30 117.9(2) . . ?
O28 Al2 N16 79.12(15) . . ?
O13 Al2 N16 151.33(15) . . ?
C29 Al2 N16 97.2(2) . . ?
C30 Al2 N16 94.5(2) . . ?
O28 Al2 Al1 38.68(10) . . ?
O13 Al2 Al1 36.79(10) . . ?
C29 Al2 Al1 120.0(2) . . ?
C30 Al2 Al1 108.8(2) . . ?
N16 Al2 Al1 114.89(11) . . ?
C10 N1 C9 111.5(4) . . ?
C10 N1 C2 106.9(4) . . ?
C9 N1 C2 114.2(4) . . ?
C10 N1 Al1 100.3(3) . . ?
C9 N1 Al1 106.2(3) . . ?
C2 N1 Al1 116.9(3) . . ?
N1 C2 C3 116.9(4) . . ?
N4 C3 C2 115.0(4) . . ?
C3 N4 C5 113.4(4) . . ?
C3 N4 C41 112.1(4) . . ?
C5 N4 C41 114.8(4) . . ?
N4 C41 C42 110.4(5) . . ?
N4 C41 C43 114.9(5) . . ?
C42 C41 C43 111.6(5) . . ?
N4 C5 C6 114.2(4) . . ?
N7 C6 C5 115.0(4) . . ?
C8 N7 C6 113.5(4) . . ?
C8 N7 C71 113.2(4) . . ?
C6 N7 C71 114.6(4) . . ?
N7 C71 C73 110.0(5) . . ?
N7 C71 C72 114.2(5) . . ?
C73 C71 C72 113.0(6) . . ?
N7 C8 C9 114.0(4) . . ?
N1 C9 C8 118.1(4) . . ?
N1 C10 C11 110.4(4) . . ?
O13 C11 C12 112.2(4) . . ?
O13 C11 C10 106.8(4) . . ?
C12 C11 C10 109.8(4) . . ?
C11 O13 Al1 123.9(3) . . ?
C11 O13 Al2 130.6(3) . . ?
Al1 O13 Al2 104.1(2) . . ?
C25 N16 C24 112.1(4) . . ?
C25 N16 C17 107.2(4) . . ?
C24 N16 C17 112.8(4) . . ?
C25 N16 Al2 99.5(3) . . ?
C24 N16 Al2 107.5(3) . . ?
C17 N16 Al2 117.0(3) . . ?
N16 C17 C18 116.5(4) . . ?
N19 C18 C17 114.6(4) . . ?
C191 N19 C18 113.1(4) . . ?
C191 N19 C20 114.8(4) . . ?
C18 N19 C20 113.5(4) . . ?
N19 C191 C192 110.7(4) . . ?
N19 C191 C193 115.1(4) . . ?
C192 C191 C193 111.1(5) . . ?
N19 C20 C21 115.2(4) . . ?
N22 C21 C20 116.5(4) . . ?
C23 N22 C21 113.0(4) . . ?
C23 N22 C221 113.2(4) . . ?
C21 N22 C221 111.7(4) . . ?
N22 C221 C223 114.0(5) . . ?
N22 C221 C222 110.9(5) . . ?
C223 C221 C222 111.2(5) . . ?
N22 C23 C24 114.6(4) . . ?
N16 C24 C23 119.0(4) . . ?
N16 C25 C26 109.8(4) . . ?
O28 C26 C27 111.5(4) . . ?
O28 C26 C25 106.2(3) . . ?
C27 C26 C25 111.5(4) . . ?
C26 O28 Al2 123.3(3) . . ?
C26 O28 Al1 129.7(3) . . ?
Al2 O28 Al1 104.7(2) . . ?
 
_refine_diff_density_max    0.462
_refine_diff_density_min   -0.261
_refine_diff_density_rms    0.068


#=== end

data_compound_8

#  Local code STR6_PM 

_audit_creation_method   CRYSTALS

_chemical_name_systematic
;
 [Al2(L-5)2Me4]  
;
_cell_length_a                          22.345(1)
_cell_angle_alpha                       90
_cell_length_b                          13.9720(4)
_cell_angle_beta                        90
_cell_length_c                          10.6340(3)
_cell_angle_gamma                       90
_cell_volume                            3319.9
_symmetry_cell_setting                  Orthorhombic
_symmetry_space_group_name_H-M          'P b c n '
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-x+1/2,y+1/2,z'
 'x+1/2,-y+1/2,-z'
 'x,-y,z+1/2'
 '-x,y,-z+1/2'
 '-x+1/2,-y+1/2,z+1/2'
 'x+1/2,y+1/2,-z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
 'C   '    0.0020    0.0020    2.3100   20.8439
    1.0200   10.2075    1.5886    0.5687    0.8650   51.6512    0.2156
'International_Tables_Vol_IV_Table_2.2B'
 'N   '    0.0040    0.0030   12.2126    0.0057
    3.1322    9.8933    2.0125   28.9975    1.1663    0.5826  -11.5290
'International_Tables_Vol_IV_Table_2.2B'
 'Al  '    0.0560    0.0520    6.4202    3.0387
    1.9002    0.7426    1.5936   31.5472    1.9646   85.0886    1.1151
'International_Tables_Vol_IV_Table_2.2B'
 'O   '    0.0080    0.0060    3.0485   13.2771
    2.2868    5.7011    1.5463    0.3239    0.8670   32.9089    0.2508
'International_Tables_Vol_IV_Table_2.2B'
 'H   '    0.0000    0.0000    0.4930   10.5109
    0.3229   26.1257    0.1402    3.1424    0.0408   57.7997    0.0030
'International_Tables_Vol_IV_Table_2.2B'
_chemical_formula_sum
' C26 H60 Al2 N6 O2 '
_chemical_formula_moiety
' C26 H60 Al2 N6 O2 '
_chemical_compound_source
;
[AlMe3.py] + HL-4 in hexane. 
;
_chemical_formula_weight                        542.76
_cell_measurement_reflns_used                   18308
_cell_measurement_theta_min                     0
_cell_measurement_theta_max                     27
_cell_measurement_temperature                   200
_cell_formula_units_Z                           4
_exptl_crystal_description                      prism
_exptl_crystal_colour                           colourless
_exptl_crystal_size_min                         0.30
_exptl_crystal_size_mid                         0.30
_exptl_crystal_size_max                         0.40
_exptl_crystal_density_diffrn                   1.09
_exptl_crystal_F_000                            1200
_exptl_absorpt_coefficient_mu                   0.11
_exptl_absorpt_correction_type                  'multi-scan'
_exptl_absorpt_correction_T_min                 0.957
_exptl_absorpt_correction_T_max                 0.968
_exptl_crystal_density_method                   none
_exptl_crystal_density_meas                     'not measured'
_diffrn_reflns_av_sigmaI/netI                   0.041
_diffrn_radiation_monochromator                 graphite
_diffrn_measurement_device-type                 'Enraf-nonius DIP2000'
_diffrn_radiation_type                          'Mo K\a'
_diffrn_radiation_wavelength                    0.71069
_diffrn_measurement_method                      \wA
_diffrn_standards_interval_time                 ?
_diffrn_standards_interval_count                ?
_diffrn_standards_number                        0
_diffrn_standards_decay_%                       0.00
_diffrn_ambient_temperature                     200
_diffrn_reflns_number                           18308
_reflns_number_total                            3779
_diffrn_reflns_av_R_equivalents                 0.06
_reflns_number_observed                         1731
_diffrn_reflns_theta_min                        0.00
_diffrn_reflns_theta_max                        26.57
_diffrn_reflns_limit_h_min                      0
_diffrn_reflns_limit_h_max                      27
_diffrn_reflns_limit_k_min                      -17
_diffrn_reflns_limit_k_max                      0
_diffrn_reflns_limit_l_min                      0
_diffrn_reflns_limit_l_max                      13
_reflns_limit_h_min                             0
_reflns_limit_h_max                             27
_reflns_limit_k_min                             0
_reflns_limit_k_max                             17
_reflns_limit_l_min                             0
_reflns_limit_l_max                             13
_atom_sites_solution_primary                    'direct methods'
_atom_sites_solution_hydrogens                  geometric
_refine_ls_hydrogen_treatment                   'riding model'
_refine_ls_matrix_type                          full
_refine_ls_weighting_scheme                     'Chebychev polynomial'
_refine_ls_number_restraints                    0    
_refine_ls_abs_structure_flack                  none 
_refine_ls_extinction_method                    none
_refine_ls_extinction_coef                      none 
_reflns_observed_criterion                      >3\s(I)
_refine_diff_density_min                        -0.39
_refine_diff_density_max                        0.55
_refine_ls_number_reflns                        1731
_refine_ls_number_parameters                    163
_refine_ls_R_factor_obs                         0.054
_refine_ls_wR_factor_obs                        0.066
_refine_ls_goodness_of_fit_obs                  1.06
_refine_ls_shift/esd_max                        0.004
_refine_ls_structure_factor_coef                F

_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)'
 
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)'
_computing_data_reduction
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
 
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
 Al1 0.93336(4) 0.30048(7) 0.23094(9) 0.0294 1.0000 Uani
 N3 0.9022(1) 0.2624(2) 0.0304(3) 0.0319 1.0000 Uani
 N6 0.7766(1) 0.1558(3) 0.0605(3) 0.0532 1.0000 Uani
 N9 0.8594(2) 0.1262(2) -0.1902(3) 0.0567 1.0000 Uani
 O1 1.0044(1) 0.3096(2) 0.1420(2) 0.0316 1.0000 Uani
 C1 0.9149(2) 0.1162(3) -0.1169(4) 0.0520 1.0000 Uani
 C2 0.9112(2) 0.1571(2) 0.0153(3) 0.0392 1.0000 Uani
 C4 0.8413(2) 0.2943(3) -0.0096(3) 0.0418 1.0000 Uani
 C5 0.7898(2) 0.2577(3) 0.0704(4) 0.0519 1.0000 Uani
 C7 0.7612(2) 0.1243(4) -0.0675(5) 0.0701 1.0000 Uani
 C8 0.8095(2) 0.0690(4) -0.1376(4) 0.0704 1.0000 Uani
 C11 0.8958(2) 0.1854(3) 0.3086(3) 0.0409 1.0000 Uani
 C12 0.8913(2) 0.4252(3) 0.2431(4) 0.0440 1.0000 Uani
 C31 0.9463(2) 0.3181(2) -0.0423(3) 0.0365 1.0000 Uani
 C32 1.0085(2) 0.3006(3) 0.0087(3) 0.0353 1.0000 Uani
 C33 1.0528(2) 0.3718(3) -0.0467(4) 0.0468 1.0000 Uani
 C61 0.7300(2) 0.1306(4) 0.1509(5) 0.0721 1.0000 Uani
 C91 0.8715(3) 0.1003(4) -0.3214(4) 0.0799 1.0000 Uani
 H11 0.9460(2) 0.1498(3) -0.1609(4) 0.0680 1.0000 Uiso
 H12 0.9248(2) 0.0495(3) -0.1119(4) 0.0680 1.0000 Uiso
 H21 0.9480(2) 0.1413(2) 0.0572(3) 0.0514 1.0000 Uiso
 H22 0.8785(2) 0.1253(2) 0.0565(3) 0.0514 1.0000 Uiso
 H41 0.8407(2) 0.3630(3) -0.0086(3) 0.0554 1.0000 Uiso
 H42 0.8347(2) 0.2719(3) -0.0938(3) 0.0554 1.0000 Uiso
 H51 0.7995(2) 0.2711(3) 0.1565(4) 0.0677 1.0000 Uiso
 H52 0.7544(2) 0.2925(3) 0.0472(4) 0.0677 1.0000 Uiso
 H71 0.7524(2) 0.1805(4) -0.1161(5) 0.0957 1.0000 Uiso
 H72 0.7263(2) 0.0846(4) -0.0626(5) 0.0957 1.0000 Uiso
 H81 0.8264(2) 0.0238(4) -0.0796(4) 0.0902 1.0000 Uiso
 H82 0.7909(2) 0.0353(4) -0.2059(4) 0.0902 1.0000 Uiso
 H111 0.8590(2) 0.2031(3) 0.3486(3) 0.0554 1.0000 Uiso
 H112 0.9226(2) 0.1589(3) 0.3701(3) 0.0554 1.0000 Uiso
 H113 0.8880(2) 0.1385(3) 0.2447(3) 0.0554 1.0000 Uiso
 H121 0.8549(2) 0.4173(3) 0.2898(4) 0.0595 1.0000 Uiso
 H122 0.9166(2) 0.4706(3) 0.2852(4) 0.0595 1.0000 Uiso
 H123 0.8822(2) 0.4481(3) 0.1601(4) 0.0595 1.0000 Uiso
 H311 0.9371(2) 0.3850(2) -0.0349(3) 0.0496 1.0000 Uiso
 H312 0.9448(2) 0.2997(2) -0.1292(3) 0.0496 1.0000 Uiso
 H321 1.0226(2) 0.2370(3) -0.0089(3) 0.0456 1.0000 Uiso
 H331 1.0549(2) 0.3643(3) -0.1363(4) 0.0641 1.0000 Uiso
 H332 1.0917(2) 0.3612(3) -0.0108(4) 0.0641 1.0000 Uiso
 H333 1.0397(2) 0.4355(3) -0.0270(4) 0.0641 1.0000 Uiso
 H611 0.7212(2) 0.0636(4) 0.1445(5) 0.0879 1.0000 Uiso
 H612 0.7433(2) 0.1449(4) 0.2347(5) 0.0879 1.0000 Uiso
 H613 0.6946(2) 0.1671(4) 0.1326(5) 0.0879 1.0000 Uiso
 H911 0.8355(3) 0.1062(4) -0.3703(4) 0.0974 1.0000 Uiso
 H912 0.9014(3) 0.1427(4) -0.3543(4) 0.0974 1.0000 Uiso
 H913 0.8857(3) 0.0355(4) -0.3256(4) 0.0974 1.0000 Uiso
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
 Al1 0.0255(4) 0.0300(5) 0.0329(5) 0.0031(4) 0.0063(4) 0.0003(4)
 N3 0.033(2) 0.031(1) 0.032(1) 0.003(1) -0.001(1) -0.001(1)
 N6 0.040(2) 0.069(2) 0.051(2) 0.010(2) -0.011(2) -0.014(2)
 N9 0.081(3) 0.051(2) 0.038(2) -0.003(2) -0.012(2) -0.010(2)
 O1 0.029(1) 0.038(1) 0.028(1) 0.001(1) 0.0054(8) 0.001(1)
 C1 0.069(3) 0.040(2) 0.047(2) -0.008(2) 0.001(2) -0.004(2)
 C2 0.042(2) 0.032(2) 0.044(2) 0.000(2) -0.002(2) -0.005(2)
 C4 0.039(2) 0.042(2) 0.045(2) 0.003(2) -0.010(1) 0.004(2)
 C5 0.030(2) 0.063(3) 0.063(3) 0.004(2) -0.006(2) 0.006(2)
 C7 0.058(3) 0.081(3) 0.072(3) 0.006(3) -0.031(3) -0.023(2)
 C8 0.092(4) 0.062(3) 0.057(3) -0.013(2) -0.027(3) -0.026(3)
 C11 0.043(2) 0.040(2) 0.039(2) 0.007(2) -0.002(1) -0.011(2)
 C12 0.047(2) 0.037(2) 0.048(2) 0.004(2) 0.013(2) 0.007(2)
 C31 0.046(2) 0.033(2) 0.030(2) 0.005(1) 0.002(1) -0.003(1)
 C32 0.041(2) 0.039(2) 0.026(2) -0.002(1) 0.008(1) 0.003(2)
 C33 0.049(2) 0.052(2) 0.039(2) 0.005(2) 0.017(2) -0.012(2)
 C61 0.034(2) 0.100(4) 0.083(4) 0.026(3) -0.001(2) -0.017(2)
 C91 0.129(5) 0.070(3) 0.041(3) -0.010(2) -0.010(3) 0.006(3)
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Al1 . Al1 6_755 3.006(2)    yes
Al1 . N3 . 2.306(3)    yes
Al1 . O1 . 1.851(2)    yes
Al1 . O1 6_755 1.944(3)    yes
Al1 . C11 . 1.993(4)    yes
Al1 . C12 . 1.984(4)    yes
N3 . C2 . 1.494(4)    yes
N3 . C4 . 1.493(4)    yes
N3 . C31 . 1.475(4)    yes
N6 . C5 . 1.458(6)    yes
N6 . C7 . 1.471(6)    yes
N6 . C61 . 1.460(5)    yes
N9 . C1 . 1.469(6)    yes
N9 . C8 . 1.482(6)    yes
N9 . C91 . 1.467(6)    yes
O1 . C32 . 1.426(4)    yes
C1 . C2 . 1.519(5)    yes
C4 . C5 . 1.521(6)    yes
C7 . C8 . 1.521(8)    yes
C31 . C32 . 1.512(5)    yes
C32 . C33 . 1.522(5)    yes
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
Al1 6_755 Al1 . N3 . 115.08(8)    yes
Al1 6_755 Al1 . O1 . 38.73(7)    yes
N3 . Al1 . O1 . 78.6(1)    yes
Al1 6_755 Al1 . O1 6_755 36.57(7)    yes
N3 . Al1 . O1 6_755 151.0(1)    yes
O1 . Al1 . O1 6_755 74.8(1)    yes
Al1 6_755 Al1 . C11 . 111.2(1)    yes
N3 . Al1 . C11 . 94.0(1)    yes
O1 . Al1 . C11 . 128.9(1)    yes
O1 6_755 Al1 . C11 . 93.8(1)    yes
Al1 6_755 Al1 . C12 . 117.4(1)    yes
N3 . Al1 . C12 . 96.9(1)    yes
O1 . Al1 . C12 . 112.2(1)    yes
O1 6_755 Al1 . C12 . 103.7(1)    yes
C11 . Al1 . C12 . 118.9(2)    yes
Al1 . N3 . C2 . 106.6(2)    yes
Al1 . N3 . C4 . 118.0(2)    yes
C2 . N3 . C4 . 112.7(3)    yes
Al1 . N3 . C31 . 99.3(2)    yes
C2 . N3 . C31 . 111.9(3)    yes
C4 . N3 . C31 . 107.6(3)    yes
C5 . N6 . C7 . 113.9(4)    yes
C5 . N6 . C61 . 109.4(4)    yes
C7 . N6 . C61 . 111.8(4)    yes
C1 . N9 . C8 . 112.6(3)    yes
C1 . N9 . C91 . 109.1(4)    yes
C8 . N9 . C91 . 111.4(4)    yes
Al1 . O1 . Al1 6_755 104.7(1)    yes
Al1 . O1 . C32 . 123.9(2)    yes
Al1 6_755 O1 . C32 . 129.7(2)    yes
N9 . C1 . C2 . 114.2(4)    yes
N3 . C2 . C1 . 118.4(3)    yes
N3 . C4 . C5 . 115.6(3)    yes
N6 . C5 . C4 . 116.2(4)    yes
N6 . C7 . C8 . 116.1(4)    yes
N9 . C8 . C7 . 116.4(4)    yes
N3 . C31 . C32 . 109.9(3)    yes
O1 . C32 . C31 . 106.4(3)    yes
O1 . C32 . C33 . 111.7(3)    yes
C31 . C32 . C33 . 110.7(3)    yes

#===end

data_compound_9

# Local code STR24

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 [Al2{(L-4).AlMe3}Me2]
;
_chemical_name_common             ?
_chemical_formula_moiety          'C20 H47 Al1 N3 O1'
_chemical_formula_structural      'C20 H47 AL1 N3 O1'
_chemical_formula_analytical      ?
_chemical_formula_sum             'C20 H47 Al2 N3 O'
_chemical_formula_weight          399.57
_chemical_melting_point           ?
_chemical_compound_source         'synthesis as described'
 
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'
 'Al'  'Al'   0.0645   0.0514
 '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'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P -1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    7.6670(6)
_cell_length_b                    11.4630(15)
_cell_length_c                    15.1650(13)
_cell_angle_alpha                 70.965(5)
_cell_angle_beta                  88.397(5)
_cell_angle_gamma                 78.458(6)
_cell_volume                      1233.4(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       0
_cell_measurement_theta_max       0
 
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.6
_exptl_crystal_size_mid           0.5
_exptl_crystal_size_min           0.5
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.076
_exptl_crystal_density_method     none
_exptl_crystal_F_000              444
_exptl_absorpt_coefficient_mu     0.131
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        ?
_diffrn_measurement_method        ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             3762
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0442
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.98
_diffrn_reflns_theta_max          26.81
_reflns_number_total              3762
_reflns_number_observed           3296
_reflns_observed_criterion        >2sigma(I)
 
_computing_data_collection        'Enraf Nonius DIP2000 Software - XPRESS'
_computing_cell_refinement        DENZO
_computing_data_reduction         'DENZO & SCALEPACK'
_computing_structure_solution     SHELXS
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1998)'
 
_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^
 or flagged by the user for potential systematic errors.  Weighted R-factors
 wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
 are based on F, with F set to zero for negative F^2^. The observed criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.1977P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          3759
_refine_ls_number_parameters      245
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0485
_refine_ls_R_factor_obs           0.0409
_refine_ls_wR_factor_all          0.1310
_refine_ls_wR_factor_obs          0.1179
_refine_ls_goodness_of_fit_all    1.092
_refine_ls_goodness_of_fit_obs    1.136
_refine_ls_restrained_S_all       1.176
_refine_ls_restrained_S_obs       1.136
_refine_ls_shift/esd_max          0.027
_refine_ls_shift/esd_mean         0.001
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Al1 Al 0.59358(6) 0.60194(5) 0.17161(3) 0.0316(2) Uani 1 d . .
Al2 Al 0.36001(6) 0.69099(5) 0.32491(3) 0.0321(2) Uani 1 d . .
N1 N 0.8114(2) 0.47732(13) 0.23071(8) 0.0289(3) Uani 1 d . .
C2 C 0.7586(2) 0.3668(2) 0.30049(10) 0.0299(3) Uani 1 d . .
H2A H 0.7258(2) 0.3127(2) 0.26696(10) 0.036 Uiso 1 calc R .
H2B H 0.6503(2) 0.3972(2) 0.33022(10) 0.036 Uiso 1 calc R .
C3 C 0.8940(2) 0.2870(2) 0.37577(11) 0.0365(4) Uani 1 d . .
H3A H 0.9207(2) 0.3390(2) 0.41254(11) 0.044 Uiso 1 calc R .
H3B H 0.8416(2) 0.2181(2) 0.41822(11) 0.044 Uiso 1 calc R .
N4 N 1.0589(2) 0.23221(13) 0.34374(9) 0.0317(3) Uani 1 d . .
C5 C 1.0415(2) 0.1310(2) 0.30900(11) 0.0349(4) Uani 1 d . .
H5A H 0.9299(2) 0.1024(2) 0.33160(11) 0.042 Uiso 1 calc R .
H5B H 1.1418(2) 0.0591(2) 0.33560(11) 0.042 Uiso 1 calc R .
C6 C 1.0392(2) 0.1660(2) 0.20521(11) 0.0370(4) Uani 1 d . .
H6A H 1.1382(2) 0.2100(2) 0.18141(11) 0.044 Uiso 1 calc R .
H6B H 1.0604(2) 0.0881(2) 0.18826(11) 0.044 Uiso 1 calc R .
N7 N 0.8744(2) 0.24585(15) 0.15998(9) 0.0353(3) Uani 1 d . .
C8 C 0.8897(2) 0.3725(2) 0.10920(11) 0.0381(4) Uani 1 d . .
H8A H 0.7730(2) 0.4189(2) 0.07761(11) 0.046 Uiso 1 calc R .
H8B H 0.9769(2) 0.3704(2) 0.06006(11) 0.046 Uiso 1 calc R .
C9 C 0.9458(2) 0.4443(2) 0.16613(11) 0.0342(4) Uani 1 d . .
H9A H 1.0557(2) 0.3937(2) 0.20304(11) 0.041 Uiso 1 calc R .
H9B H 0.9753(2) 0.5231(2) 0.12318(11) 0.041 Uiso 1 calc R .
C10 C 0.8831(2) 0.5547(2) 0.27476(11) 0.0341(4) Uani 1 d . .
H10A H 0.9267(2) 0.6230(2) 0.22634(11) 0.041 Uiso 1 calc R .
H10B H 0.9850(2) 0.5023(2) 0.31771(11) 0.041 Uiso 1 calc R .
C11 C 0.7417(2) 0.6103(2) 0.32795(12) 0.0367(4) Uani 1 d . .
H11 H 0.7271(2) 0.5444(2) 0.38837(12) 0.044 Uiso 1 calc R .
C12 C 0.7948(3) 0.7178(3) 0.3478(2) 0.0599(6) Uani 1 d . .
H12A H 0.9133(11) 0.6899(5) 0.3789(12) 0.090 Uiso 1 calc R .
H12B H 0.7084(14) 0.7478(12) 0.3884(11) 0.090 Uiso 1 calc R .
H12C H 0.7975(25) 0.7863(7) 0.2890(2) 0.090 Uiso 1 calc R .
O13 O 0.57860(15) 0.64955(11) 0.27372(8) 0.0318(3) Uani 1 d . .
C14 C 0.4130(3) 0.5147(2) 0.15445(13) 0.0445(4) Uani 1 d . .
H14A H 0.4672(4) 0.4462(10) 0.1309(11) 0.067 Uiso 1 calc R .
H14B H 0.3206(11) 0.5738(4) 0.1094(9) 0.067 Uiso 1 calc R .
H14C H 0.3596(16) 0.4797(13) 0.2143(3) 0.067 Uiso 1 calc R .
C15 C 0.6594(3) 0.7291(2) 0.06581(13) 0.0523(5) Uani 1 d . .
H15A H 0.5582(8) 0.8002(7) 0.0442(7) 0.078 Uiso 1 calc R .
H15B H 0.6930(22) 0.6938(5) 0.0155(4) 0.078 Uiso 1 calc R .
H15C H 0.7605(15) 0.7582(12) 0.0837(3) 0.078 Uiso 1 calc R .
C16 C 0.3092(3) 0.5274(2) 0.39837(12) 0.0410(4) Uani 1 d . .
H16A H 0.2963(19) 0.4794(6) 0.3569(2) 0.061 Uiso 1 calc R .
H16B H 0.1984(10) 0.5400(2) 0.4310(8) 0.061 Uiso 1 calc R .
H16C H 0.4073(9) 0.4808(5) 0.4442(7) 0.061 Uiso 1 calc R .
C17 C 0.3745(3) 0.7953(2) 0.40166(14) 0.0484(5) Uani 1 d . .
H17A H 0.4505(20) 0.7457(5) 0.4575(6) 0.073 Uiso 1 calc R .
H17B H 0.2549(4) 0.8251(14) 0.4203(11) 0.073 Uiso 1 calc R .
H17C H 0.4255(23) 0.8677(9) 0.3660(4) 0.073 Uiso 1 calc R .
C18 C 0.2121(3) 0.7887(2) 0.21417(13) 0.0481(5) Uani 1 d . .
H18A H 0.1007(9) 0.8328(12) 0.2319(2) 0.072 Uiso 1 calc R .
H18B H 0.1856(18) 0.7325(3) 0.1819(6) 0.072 Uiso 1 calc R .
H18C H 0.2752(9) 0.8504(10) 0.1726(5) 0.072 Uiso 1 calc R .
C41 C 1.2064(2) 0.1985(2) 0.41121(11) 0.0350(4) Uani 1 d . .
H41 H 1.2037(2) 0.2735(2) 0.43162(11) 0.042 Uiso 1 calc R .
C42 C 1.1919(3) 0.0908(2) 0.49743(11) 0.0413(4) Uani 1 d . .
H42A H 1.2890(11) 0.0787(9) 0.5422(4) 0.062 Uiso 1 calc R .
H42B H 1.1999(19) 0.0140(3) 0.4811(2) 0.062 Uiso 1 calc R .
H42C H 1.0772(8) 0.1093(6) 0.5254(6) 0.062 Uiso 1 calc R .
C43 C 1.3819(3) 0.1758(2) 0.36721(14) 0.0463(4) Uani 1 d . .
H43A H 1.3954(10) 0.0981(8) 0.3515(10) 0.069 Uiso 1 calc R .
H43B H 1.4786(3) 0.1675(15) 0.4111(4) 0.069 Uiso 1 calc R .
H43C H 1.3863(9) 0.2468(7) 0.3103(6) 0.069 Uiso 1 calc R .
C71 C 0.7778(3) 0.1900(2) 0.10891(12) 0.0444(4) Uani 1 d . .
H71 H 0.6709(3) 0.2554(2) 0.07808(12) 0.053 Uiso 1 calc R .
C72 C 0.8821(3) 0.1552(3) 0.03259(15) 0.0618(7) Uani 1 d . .
H72A H 0.8076(10) 0.1226(20) -0.0014(10) 0.093 Uiso 1 calc R .
H72B H 0.9881(16) 0.0904(14) 0.0600(2) 0.093 Uiso 1 calc R .
H72C H 0.9186(25) 0.2300(5) -0.0105(8) 0.093 Uiso 1 calc R .
C73 C 0.7104(4) 0.0806(3) 0.1733(2) 0.0615(6) Uani 1 d . .
H73A H 0.6326(21) 0.0520(12) 0.1381(3) 0.092 Uiso 1 calc R .
H73B H 0.6431(21) 0.1062(5) 0.2222(8) 0.092 Uiso 1 calc R .
H73C H 0.8113(4) 0.0119(7) 0.2021(10) 0.092 Uiso 1 calc R .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Al1 0.0277(3) 0.0307(3) 0.0316(2) -0.0070(2) -0.0011(2) -0.0004(2)
Al2 0.0286(3) 0.0299(3) 0.0329(2) -0.0083(2) 0.0007(2) 0.0017(2)
N1 0.0262(7) 0.0275(7) 0.0306(6) -0.0084(5) 0.0021(5) -0.0021(5)
C2 0.0288(8) 0.0285(8) 0.0298(7) -0.0078(6) 0.0055(6) -0.0033(6)
C3 0.0399(10) 0.0350(9) 0.0286(7) -0.0071(6) 0.0014(6) 0.0002(7)
N4 0.0348(8) 0.0263(7) 0.0297(6) -0.0078(5) -0.0035(5) 0.0020(6)
C5 0.0410(9) 0.0274(9) 0.0335(7) -0.0089(6) -0.0054(6) -0.0014(7)
C6 0.0404(10) 0.0340(9) 0.0343(7) -0.0134(7) -0.0013(7) 0.0022(7)
N7 0.0387(8) 0.0354(8) 0.0297(6) -0.0118(6) -0.0030(5) -0.0002(6)
C8 0.0412(10) 0.0383(10) 0.0282(7) -0.0082(7) 0.0025(6) 0.0023(7)
C9 0.0316(9) 0.0326(9) 0.0331(7) -0.0072(6) 0.0064(6) -0.0007(7)
C10 0.0256(8) 0.0335(9) 0.0431(8) -0.0137(7) -0.0015(6) -0.0036(6)
C11 0.0269(8) 0.0398(10) 0.0461(8) -0.0207(8) -0.0034(7) -0.0011(7)
C12 0.0382(11) 0.066(2) 0.095(2) -0.0539(14) -0.0003(11) -0.0095(10)
O13 0.0249(6) 0.0306(6) 0.0384(5) -0.0121(5) -0.0009(4) -0.0006(4)
C14 0.0375(10) 0.0516(12) 0.0456(9) -0.0185(8) -0.0052(8) -0.0062(8)
C15 0.0491(12) 0.0458(12) 0.0458(9) 0.0011(8) 0.0030(8) -0.0005(9)
C16 0.0354(10) 0.0417(10) 0.0397(8) -0.0044(7) -0.0025(7) -0.0086(8)
C17 0.0489(12) 0.0474(12) 0.0510(10) -0.0245(9) 0.0070(9) -0.0012(9)
C18 0.0386(10) 0.0499(12) 0.0419(9) -0.0049(8) -0.0030(8) 0.0058(8)
C41 0.0373(9) 0.0296(9) 0.0364(7) -0.0096(6) -0.0057(7) -0.0041(7)
C42 0.0511(11) 0.0344(10) 0.0336(8) -0.0060(7) -0.0115(7) -0.0046(8)
C43 0.0383(10) 0.0414(11) 0.0537(10) -0.0099(8) -0.0028(8) -0.0046(8)
C71 0.0459(11) 0.0488(12) 0.0397(8) -0.0209(8) -0.0076(8) 0.0001(9)
C72 0.070(2) 0.076(2) 0.0447(10) -0.0352(11) -0.0075(10) -0.0005(13)
C73 0.069(2) 0.060(2) 0.0636(12) -0.0255(11) -0.0009(11) -0.0222(12)
 
_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 O13 1.7959(11) . ?
Al1 C15 1.917(2) . ?
Al1 C14 1.931(2) . ?
Al1 N1 1.9819(14) . ?
Al2 O13 1.8671(12) . ?
Al2 C18 1.932(2) . ?
Al2 C17 1.940(2) . ?
Al2 C16 1.953(2) . ?
N1 C10 1.462(2) . ?
N1 C9 1.480(2) . ?
N1 C2 1.482(2) . ?
C2 C3 1.491(2) . ?
C3 N4 1.441(2) . ?
N4 C41 1.452(2) . ?
N4 C5 1.451(2) . ?
C5 C6 1.492(2) . ?
C6 N7 1.442(2) . ?
N7 C8 1.431(2) . ?
N7 C71 1.450(2) . ?
C8 C9 1.495(2) . ?
C10 C11 1.498(2) . ?
C11 O13 1.426(2) . ?
C11 C12 1.491(3) . ?
C41 C42 1.497(2) . ?
C41 C43 1.499(3) . ?
C71 C73 1.492(3) . ?
C71 C72 1.503(3) . ?
 
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
O13 Al1 C15 111.25(8) . . ?
O13 Al1 C14 116.15(7) . . ?
C15 Al1 C14 118.83(9) . . ?
O13 Al1 N1 87.76(5) . . ?
C15 Al1 N1 108.78(8) . . ?
C14 Al1 N1 109.43(8) . . ?
O13 Al2 C18 101.56(7) . . ?
O13 Al2 C17 111.46(7) . . ?
C18 Al2 C17 109.64(10) . . ?
O13 Al2 C16 103.58(7) . . ?
C18 Al2 C16 118.06(9) . . ?
C17 Al2 C16 111.84(9) . . ?
C10 N1 C9 107.31(13) . . ?
C10 N1 C2 112.02(12) . . ?
C9 N1 C2 113.90(13) . . ?
C10 N1 Al1 97.58(10) . . ?
C9 N1 Al1 116.03(10) . . ?
C2 N1 Al1 108.87(10) . . ?
N1 C2 C3 116.54(14) . . ?
N4 C3 C2 115.00(12) . . ?
C3 N4 C41 112.72(12) . . ?
C3 N4 C5 112.90(14) . . ?
C41 N4 C5 113.38(13) . . ?
N4 C5 C6 114.3(2) . . ?
N7 C6 C5 113.59(14) . . ?
C8 N7 C6 113.8(2) . . ?
C8 N7 C71 113.93(13) . . ?
C6 N7 C71 114.32(14) . . ?
N7 C8 C9 115.49(13) . . ?
N1 C9 C8 114.95(14) . . ?
N1 C10 C11 110.05(13) . . ?
O13 C11 C12 111.5(2) . . ?
O13 C11 C10 108.18(12) . . ?
C12 C11 C10 109.9(2) . . ?
C11 O13 Al1 113.03(10) . . ?
C11 O13 Al2 121.71(10) . . ?
Al1 O13 Al2 121.72(6) . . ?
N4 C41 C42 113.88(15) . . ?
N4 C41 C43 111.31(13) . . ?
C42 C41 C43 111.4(2) . . ?
N7 C71 C73 111.25(15) . . ?
N7 C71 C72 113.4(2) . . ?
C73 C71 C72 111.4(2) . . ?
 
_refine_diff_density_max    0.163
_refine_diff_density_min   -0.256
_refine_diff_density_rms    0.037

#===end


data_compound_10

#  Local code STR35

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 [Al(L-2)Me2]   
;
_chemical_name_common             ?
_chemical_formula_moiety          'C29 H54 Al N3 O'
_chemical_formula_structural      'C29 H54 AL N3 O'
_chemical_formula_analytical      ?
_chemical_formula_sum             'C29 H54 Al N3 O'
_chemical_formula_weight          487.73
_chemical_melting_point           ?
_chemical_compound_source         'synthesis as described'
 
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            orthorhombic
_symmetry_space_group_name_H-M    'P 21 21 21'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 
_cell_length_a                    10.3380(6)
_cell_length_b                    13.9560(7)
_cell_length_c                    20.8520(11)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      3008.5(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     130
_cell_measurement_theta_min       0
_cell_measurement_theta_max       0
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.3
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.3
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.077
_exptl_crystal_density_method     none
_exptl_crystal_F_000              1080
_exptl_absorpt_coefficient_mu     0.091
_exptl_absorpt_correction_type    'none'
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        
;
Enraf-Nonius DIP2000 Image Plate Diffractometer
;
_diffrn_measurement_method        'Omega scans'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             7450
_diffrn_reflns_av_R_equivalents   0.0338
_diffrn_reflns_av_sigmaI/netI     0.0475
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          1.76
_diffrn_reflns_theta_max          22.50
_reflns_number_total              3926
_reflns_number_observed           3832
_reflns_observed_criterion        >2sigma(I)
 
_computing_data_collection        'Enraf-Nonius DIP2000 Software - XPRESS'
_computing_cell_refinement        DENZO
_computing_data_reduction         'DENZO & SCALEPACK'
_computing_structure_solution     SIR-92
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1998)'
 
_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^
 or flagged by the user for potential systematic errors.  Weighted R-factors
 wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
 are based on F, with F set to zero for negative F^2^. The observed criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+3.4590P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_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    0.59(36)
_refine_ls_number_reflns          3924
_refine_ls_number_parameters      319
_refine_ls_number_restraints      6
_refine_ls_R_factor_all           0.0746
_refine_ls_R_factor_obs           0.0715
_refine_ls_wR_factor_all          0.1466
_refine_ls_wR_factor_obs          0.1446
_refine_ls_goodness_of_fit_all    1.410
_refine_ls_goodness_of_fit_obs    1.421
_refine_ls_restrained_S_all       1.421
_refine_ls_restrained_S_obs       1.420
_refine_ls_shift/esd_max          -0.017
_refine_ls_shift/esd_mean         0.002
 
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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Al1 Al 0.31200(13) 0.11801(10) 0.17284(7) 0.0223(3) Uani 1 d . .
O17 O 0.3899(3) 0.0138(2) 0.1453(2) 0.0311(9) Uani 1 d . .
N7 N 0.6626(4) 0.3524(3) 0.1117(2) 0.0248(10) Uani 1 d . .
N1 N 0.4716(3) 0.2003(3) 0.1701(2) 0.0194(8) Uani 1 d . .
N4 N 0.3603(4) 0.4004(3) 0.1251(2) 0.0235(9) Uani 1 d . .
C10 C 0.5720(4) 0.1409(3) 0.2037(2) 0.0216(11) Uani 1 d . .
H10A H 0.6496(4) 0.1793(3) 0.2085(2) 0.026 Uiso 1 calc R .
H10B H 0.5407(4) 0.1260(3) 0.2464(2) 0.026 Uiso 1 calc R .
C3 C 0.3471(5) 0.3567(3) 0.1877(2) 0.0236(11) Uani 1 d . .
H3A H 0.2674(5) 0.3201(3) 0.1885(2) 0.028 Uiso 1 calc R .
H3B H 0.3392(5) 0.4073(3) 0.2194(2) 0.028 Uiso 1 calc R .
C12 C 0.7368(4) 0.0226(3) 0.1709(2) 0.0233(11) Uani 1 d . .
H12 H 0.7975(4) 0.0650(3) 0.1875(2) 0.028 Uiso 1 calc R .
C13 C 0.7791(4) -0.0636(3) 0.1472(2) 0.0214(11) Uani 1 d . .
C14 C 0.6840(5) -0.1226(3) 0.1215(2) 0.0271(11) Uani 1 d . .
H14 H 0.7095(5) -0.1812(3) 0.1046(2) 0.033 Uiso 1 calc R .
C15 C 0.5535(5) -0.0998(3) 0.1195(2) 0.0219(11) Uani 1 d . .
C5 C 0.4714(5) 0.4641(3) 0.1193(3) 0.0315(13) Uani 1 d . .
H5A H 0.5030(5) 0.4787(3) 0.1620(3) 0.038 Uiso 1 calc R .
H5B H 0.4428(5) 0.5237(3) 0.1001(3) 0.038 Uiso 1 calc R .
C8 C 0.6403(4) 0.2554(3) 0.0875(2) 0.0224(11) Uani 1 d . .
H8A H 0.7042(4) 0.2129(3) 0.1062(2) 0.027 Uiso 1 calc R .
H8B H 0.6534(4) 0.2554(3) 0.0414(2) 0.027 Uiso 1 calc R .
C71 C 0.8005(4) 0.3768(4) 0.1155(2) 0.0312(12) Uani 1 d . .
H71 H 0.8048(4) 0.4451(4) 0.1261(2) 0.037 Uiso 1 calc R .
C9 C 0.5073(4) 0.2162(3) 0.1016(2) 0.0210(11) Uani 1 d . .
H9A H 0.4443(4) 0.2598(3) 0.0832(2) 0.025 Uiso 1 calc R .
H9B H 0.4986(4) 0.1556(3) 0.0793(2) 0.025 Uiso 1 calc R .
C11 C 0.6079(4) 0.0491(3) 0.1712(2) 0.0174(10) Uani 1 d . .
C2 C 0.4565(5) 0.2916(3) 0.2075(2) 0.0217(11) Uani 1 d U .
H2A H 0.5367(5) 0.3274(3) 0.2042(2) 0.026 Uiso 1 calc R .
H2B H 0.4447(5) 0.2751(3) 0.2523(2) 0.026 Uiso 1 calc R .
C6 C 0.5835(5) 0.4248(3) 0.0797(2) 0.0297(13) Uani 1 d . .
H6A H 0.5489(5) 0.3973(3) 0.0406(2) 0.036 Uiso 1 calc R .
H6B H 0.6390(5) 0.4779(3) 0.0676(2) 0.036 Uiso 1 calc R .
C131 C 0.9217(5) -0.0938(4) 0.1469(2) 0.0290(12) Uani 1 d . .
C16 C 0.5155(5) -0.0120(3) 0.1460(2) 0.0239(11) Uani 1 d . .
C151 C 0.4541(5) -0.1681(3) 0.0886(2) 0.0296(12) Uani 1 d . .
C43 C 0.2428(5) 0.4578(4) 0.0303(3) 0.045(2) Uani 1 d . .
H43A H 0.2995(29) 0.5106(18) 0.0214(3) 0.068 Uiso 1 calc R .
H43B H 0.1576(8) 0.4723(26) 0.0147(4) 0.068 Uiso 1 calc R .
H43C H 0.2746(34) 0.4013(10) 0.0093(3) 0.068 Uiso 1 calc R .
C153 C 0.3479(5) -0.1947(4) 0.1351(3) 0.0372(14) Uani 1 d . .
H15A H 0.2826(16) -0.2309(21) 0.1130(4) 0.056 Uiso 1 calc R .
H15B H 0.3102(22) -0.1374(4) 0.1525(12) 0.056 Uiso 1 calc R .
H15C H 0.3834(8) -0.2326(20) 0.1692(9) 0.056 Uiso 1 calc R .
C132 C 1.0032(5) -0.0308(4) 0.1916(3) 0.046(2) Uani 1 d . .
H13A H 1.0914(9) -0.0523(17) 0.1909(14) 0.069 Uiso 1 calc R .
H13B H 0.9700(22) -0.0352(21) 0.2345(4) 0.069 Uiso 1 calc R .
H13C H 0.9991(29) 0.0346(6) 0.1773(10) 0.069 Uiso 1 calc R .
C42 C 0.1922(6) 0.5291(4) 0.1372(3) 0.046(2) Uani 1 d . .
H42A H 0.1058(15) 0.5447(16) 0.1240(13) 0.069 Uiso 1 calc R .
H42B H 0.2488(22) 0.5817(8) 0.1276(14) 0.069 Uiso 1 calc R .
H42C H 0.1934(34) 0.5169(10) 0.1825(3) 0.069 Uiso 1 calc R .
C41 C 0.2373(4) 0.4409(4) 0.1018(2) 0.0277(12) Uani 1 d . .
H41 H 0.1712(4) 0.3917(4) 0.1088(2) 0.033 Uiso 1 calc R .
C19 C 0.1863(5) 0.1634(3) 0.1099(2) 0.0308(12) Uani 1 d . .
H19A H 0.2255(10) 0.2115(16) 0.0833(10) 0.046 Uiso 1 calc R .
H19B H 0.1130(14) 0.1903(20) 0.1317(2) 0.046 Uiso 1 calc R .
H19C H 0.1586(23) 0.1107(5) 0.0837(10) 0.046 Uiso 1 calc R .
C72 C 0.8735(5) 0.3646(4) 0.0528(2) 0.0366(14) Uani 1 d . .
H72A H 0.8810(28) 0.2977(4) 0.0430(8) 0.055 Uiso 1 calc R .
H72B H 0.9583(13) 0.3920(21) 0.0569(6) 0.055 Uiso 1 calc R .
H72C H 0.8274(18) 0.3965(21) 0.0190(4) 0.055 Uiso 1 calc R .
C73 C 0.8664(5) 0.3246(4) 0.1693(3) 0.0424(14) Uani 1 d . .
H73A H 0.9537(12) 0.3471(18) 0.1733(11) 0.064 Uiso 1 calc R .
H73B H 0.8668(29) 0.2571(5) 0.1604(8) 0.064 Uiso 1 calc R .
H73C H 0.8207(20) 0.3363(20) 0.2086(4) 0.064 Uiso 1 calc R .
C154 C 0.3937(6) -0.1183(4) 0.0304(3) 0.0459(15) Uani 1 d . .
H15D H 0.3487(32) -0.0618(16) 0.0442(3) 0.069 Uiso 1 calc R .
H15E H 0.3340(29) -0.1611(11) 0.0099(11) 0.069 Uiso 1 calc R .
H15F H 0.4606(7) -0.1008(25) 0.0007(9) 0.069 Uiso 1 calc R .
C133 C 0.9762(6) -0.0822(6) 0.0806(3) 0.062(2) Uani 1 d . .
H13D H 1.0663(12) -0.0987(31) 0.0808(5) 0.093 Uiso 1 calc R .
H13E H 0.9661(38) -0.0169(9) 0.0670(9) 0.093 Uiso 1 calc R .
H13F H 0.9308(29) -0.1237(23) 0.0515(5) 0.093 Uiso 1 calc R .
C18 C 0.2616(5) 0.1061(4) 0.2634(2) 0.0388(13) Uani 1 d . .
H18A H 0.1698(7) 0.1148(24) 0.2673(3) 0.058 Uiso 1 calc R .
H18B H 0.3055(26) 0.1540(16) 0.2882(3) 0.058 Uiso 1 calc R .
H18C H 0.2848(30) 0.0436(10) 0.2788(5) 0.058 Uiso 1 calc R .
C152 C 0.5155(6) -0.2603(4) 0.0653(3) 0.050(2) Uani 1 d . .
H15G H 0.5782(28) -0.2460(4) 0.0327(14) 0.075 Uiso 1 calc R .
H15H H 0.4499(8) -0.3015(12) 0.0479(17) 0.075 Uiso 1 calc R .
H15I H 0.5574(33) -0.2919(15) 0.1006(5) 0.075 Uiso 1 calc R .
C134 C 0.9363(6) -0.1959(4) 0.1704(4) 0.062(2) Uani 1 d . .
H13G H 0.8964(37) -0.2021(9) 0.2118(10) 0.093 Uiso 1 calc R .
H13H H 1.0265(6) -0.2115(11) 0.1737(20) 0.093 Uiso 1 calc R .
H13I H 0.8953(37) -0.2388(5) 0.1407(11) 0.093 Uiso 1 calc R .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Al1 0.0229(7) 0.0201(8) 0.0238(7) 0.0038(7) 0.0001(6) -0.0010(7)
O17 0.018(2) 0.026(2) 0.049(2) -0.003(2) -0.005(2) -0.005(2)
N7 0.023(2) 0.025(2) 0.026(2) -0.002(2) -0.001(2) -0.003(2)
N1 0.026(2) 0.017(2) 0.015(2) 0.001(2) -0.005(2) -0.002(2)
N4 0.026(2) 0.016(2) 0.029(2) 0.003(2) 0.005(2) -0.002(2)
C10 0.023(3) 0.021(3) 0.020(3) 0.000(2) -0.003(2) 0.001(2)
C3 0.035(3) 0.017(3) 0.019(3) -0.003(2) 0.003(2) 0.001(2)
C12 0.028(3) 0.019(2) 0.023(3) -0.003(2) -0.003(2) -0.007(2)
C13 0.026(3) 0.023(3) 0.015(2) 0.005(2) 0.000(2) -0.001(2)
C14 0.035(3) 0.021(3) 0.025(3) -0.002(2) 0.011(2) 0.004(3)
C15 0.035(3) 0.012(2) 0.019(2) 0.001(2) -0.002(2) 0.001(2)
C5 0.032(3) 0.015(2) 0.048(3) 0.003(2) -0.005(3) -0.004(2)
C8 0.023(3) 0.024(3) 0.020(3) -0.001(2) 0.001(2) 0.000(2)
C71 0.025(3) 0.029(3) 0.040(3) -0.008(3) 0.007(2) -0.008(3)
C9 0.026(3) 0.017(2) 0.020(3) -0.008(2) -0.002(2) 0.002(2)
C11 0.018(2) 0.015(2) 0.019(2) 0.005(2) -0.001(2) 0.004(2)
C2 0.033(3) 0.018(2) 0.013(2) 0.003(2) 0.001(2) 0.000(2)
C6 0.029(3) 0.026(3) 0.034(3) 0.006(2) 0.003(2) -0.008(2)
C131 0.025(3) 0.031(3) 0.031(3) -0.004(2) 0.005(2) 0.004(2)
C16 0.027(3) 0.022(3) 0.023(3) 0.003(2) 0.002(2) -0.005(2)
C151 0.038(3) 0.023(3) 0.027(3) -0.003(2) -0.008(3) -0.007(2)
C43 0.040(3) 0.056(4) 0.040(3) 0.018(3) -0.007(3) -0.003(3)
C153 0.043(3) 0.027(3) 0.042(3) 0.006(3) -0.013(3) -0.010(3)
C132 0.033(3) 0.058(4) 0.048(4) -0.003(3) -0.004(3) 0.010(3)
C42 0.039(3) 0.040(3) 0.058(4) 0.011(3) 0.013(3) 0.012(3)
C41 0.018(3) 0.028(3) 0.037(3) 0.015(2) 0.000(2) 0.003(2)
C19 0.030(3) 0.028(3) 0.035(3) 0.003(2) 0.000(3) -0.004(2)
C72 0.023(3) 0.051(4) 0.035(3) -0.002(3) -0.001(2) -0.009(3)
C73 0.032(3) 0.058(4) 0.037(3) -0.011(3) -0.008(3) -0.004(3)
C154 0.057(4) 0.042(3) 0.039(3) -0.005(3) -0.015(3) -0.016(3)
C133 0.033(3) 0.108(6) 0.043(4) 0.003(4) 0.002(3) 0.018(4)
C18 0.039(3) 0.042(3) 0.036(3) 0.001(3) 0.002(2) -0.001(3)
C152 0.055(4) 0.027(3) 0.069(4) -0.013(3) -0.013(3) -0.001(3)
C134 0.036(3) 0.044(4) 0.104(6) 0.012(4) -0.012(4) 0.012(3)
 
_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 O17 1.759(4) . ?
Al1 C19 1.953(5) . ?
Al1 C18 1.965(5) . ?
Al1 N1 2.011(4) . ?
O17 C16 1.348(6) . ?
N7 C6 1.461(6) . ?
N7 C8 1.463(6) . ?
N7 C71 1.468(6) . ?
N1 C9 1.492(6) . ?
N1 C2 1.501(6) . ?
N1 C10 1.502(5) . ?
N4 C3 1.447(6) . ?
N4 C5 1.458(6) . ?
N4 C41 1.473(6) . ?
C10 C11 1.495(6) . ?
C3 C2 1.508(6) . ?
C12 C13 1.371(6) . ?
C12 C11 1.383(6) . ?
C13 C14 1.390(6) . ?
C13 C131 1.533(7) . ?
C14 C15 1.386(7) . ?
C15 C16 1.401(6) . ?
C15 C151 1.543(7) . ?
C5 C6 1.524(7) . ?
C8 C9 1.509(6) . ?
C71 C73 1.501(7) . ?
C71 C72 1.518(7) . ?
C11 C16 1.384(6) . ?
C131 C133 1.502(7) . ?
C131 C134 1.515(8) . ?
C131 C132 1.533(7) . ?
C151 C153 1.510(7) . ?
C151 C152 1.515(7) . ?
C151 C154 1.532(7) . ?
C43 C41 1.511(7) . ?
C42 C41 1.509(7) . ?
 
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
O17 Al1 C19 110.7(2) . . ?
O17 Al1 C18 111.4(2) . . ?
C19 Al1 C18 119.8(2) . . ?
O17 Al1 N1 95.0(2) . . ?
C19 Al1 N1 110.0(2) . . ?
C18 Al1 N1 107.0(2) . . ?
C16 O17 Al1 131.2(3) . . ?
C6 N7 C8 113.2(4) . . ?
C6 N7 C71 114.0(4) . . ?
C8 N7 C71 112.7(4) . . ?
C9 N1 C2 113.3(3) . . ?
C9 N1 C10 110.9(3) . . ?
C2 N1 C10 107.4(3) . . ?
C9 N1 Al1 108.4(3) . . ?
C2 N1 Al1 112.7(3) . . ?
C10 N1 Al1 103.8(3) . . ?
C3 N4 C5 114.0(4) . . ?
C3 N4 C41 112.2(4) . . ?
C5 N4 C41 114.7(4) . . ?
C11 C10 N1 115.7(4) . . ?
N4 C3 C2 115.4(4) . . ?
C13 C12 C11 123.0(4) . . ?
C12 C13 C14 115.6(4) . . ?
C12 C13 C131 123.3(4) . . ?
C14 C13 C131 121.1(4) . . ?
C15 C14 C13 124.4(4) . . ?
C14 C15 C16 117.5(4) . . ?
C14 C15 C151 121.3(4) . . ?
C16 C15 C151 121.2(4) . . ?
N4 C5 C6 115.2(4) . . ?
N7 C8 C9 114.3(4) . . ?
N7 C71 C73 111.6(4) . . ?
N7 C71 C72 114.3(4) . . ?
C73 C71 C72 111.3(4) . . ?
N1 C9 C8 117.8(4) . . ?
C12 C11 C16 119.8(4) . . ?
C12 C11 C10 118.1(4) . . ?
C16 C11 C10 121.9(4) . . ?
N1 C2 C3 116.6(4) . . ?
N7 C6 C5 115.3(4) . . ?
C133 C131 C134 111.2(5) . . ?
C133 C131 C132 107.0(5) . . ?
C134 C131 C132 106.7(5) . . ?
C133 C131 C13 109.6(4) . . ?
C134 C131 C13 110.7(4) . . ?
C132 C131 C13 111.6(4) . . ?
O17 C16 C11 120.3(4) . . ?
O17 C16 C15 119.9(4) . . ?
C11 C16 C15 119.7(4) . . ?
C153 C151 C152 107.6(4) . . ?
C153 C151 C154 108.9(4) . . ?
C152 C151 C154 107.6(5) . . ?
C153 C151 C15 111.6(4) . . ?
C152 C151 C15 112.3(4) . . ?
C154 C151 C15 108.8(4) . . ?
N4 C41 C42 114.7(4) . . ?
N4 C41 C43 110.7(4) . . ?
C42 C41 C43 111.5(4) . . ?
 
_refine_diff_density_max    0.302
_refine_diff_density_min   -0.226
_refine_diff_density_rms    0.056

#===end