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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_dw0816

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H42 Al2 Ca N6, C7 H8'
_chemical_formula_sum            'C45 H50 Al2 Ca N6'
_chemical_formula_weight         768.95

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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                   9.5264(3)
_cell_length_b                   9.6015(3)
_cell_length_c                   12.4043(5)
_cell_angle_alpha                84.746(2)
_cell_angle_beta                 71.733(2)
_cell_angle_gamma                88.276(2)
_cell_volume                     1072.89(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    6503
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             408
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_T_max  0.982
_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            12584
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_sigmaI/netI    0.1030
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.80
_diffrn_reflns_theta_max         27.58
_reflns_number_total             4867
_reflns_number_gt                2857
_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 -CH2-CH2-CH2-CH3 group (disordered over two sites) and the toluene
 solvent molecule are both poorly resolved (both were modelled with bond
 length restraints and common isotropic displacement parameters for the
 carbon atoms).  Anisotropic displacement parameters were assigned to the
 Al and Ca atoms only.  An all-anisotropic refinement does behave and does
 converge but the resulting extra displacement parameters have no apparent
 physical significance.
;

_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)+(0.0660P)²+4.3793P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4867
_refine_ls_number_parameters     138
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1780
_refine_ls_R_factor_gt           0.1048
_refine_ls_wR_factor_ref         0.2583
_refine_ls_wR_factor_gt          0.2132
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.046
_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
Ca1 Ca 0.5000 0.5000 0.5000 0.0312(4) Uani 1 2 d S . .
Al1 Al 0.66872(16) 0.71579(15) 0.65168(13) 0.0332(4) Uani 1 1 d . . .
N1 N 0.4133(5) 0.7334(4) 0.5671(4) 0.0359(10) Uiso 1 1 d . . .
N2 N 0.7534(5) 0.5936(4) 0.4323(4) 0.0398(10) Uiso 1 1 d . . .
N3 N 0.5389(5) 0.4360(4) 0.6873(3) 0.0345(10) Uiso 1 1 d . . .
C1 C 0.7673(13) 1.0119(12) 0.9948(8) 0.078(3) Uiso 0.75 1 d PD A 1
H1A H 0.8394 1.0724 1.0091 0.116 Uiso 0.75 1 calc PR A 1
H1B H 0.7615 0.9222 1.0406 0.116 Uiso 0.75 1 calc PR A 1
H1C H 0.6700 1.0572 1.0157 0.116 Uiso 0.75 1 calc PR A 1
C2 C 0.8154(10) 0.9867(9) 0.8682(7) 0.056(2) Uiso 0.75 1 d PD A 1
H2A H 0.9187 0.9523 0.8455 0.068 Uiso 0.75 1 calc PR A 1
H2B H 0.8134 1.0769 0.8231 0.068 Uiso 0.75 1 calc PR A 1
C3 C 0.7173(8) 0.8808(7) 0.8392(5) 0.0406(15) Uiso 0.75 1 d PD A 1
H3A H 0.7050 0.7972 0.8943 0.049 Uiso 0.75 1 calc PR A 1
H3B H 0.6183 0.9230 0.8498 0.049 Uiso 0.75 1 calc PR A 1
C4 C 0.7748(8) 0.8341(7) 0.7200(5) 0.0607(11) Uiso 0.75 1 d PD A 1
H4A H 0.8698 0.7860 0.7150 0.073 Uiso 0.75 1 calc PR A 1
H4B H 0.7997 0.9208 0.6682 0.073 Uiso 0.75 1 calc PR A 1
C1A C 0.802(3) 1.014(4) 0.9393(19) 0.078(3) Uiso 0.25 1 d PD A 2
H1D H 0.8440 1.0891 0.9679 0.116 Uiso 0.25 1 calc PR A 2
H1E H 0.7996 0.9272 0.9879 0.116 Uiso 0.25 1 calc PR A 2
H1F H 0.7009 1.0395 0.9404 0.116 Uiso 0.25 1 calc PR A 2
C2A C 0.897(2) 0.993(3) 0.8170(18) 0.056(2) Uiso 0.25 1 d PD A 2
H2C H 0.9564 0.9067 0.8172 0.068 Uiso 0.25 1 calc PR A 2
H2D H 0.9657 1.0726 0.7873 0.068 Uiso 0.25 1 calc PR A 2
C3A C 0.803(2) 0.9812(12) 0.7380(16) 0.0406(15) Uiso 0.25 1 d PD A 2
H3C H 0.7067 1.0280 0.7705 0.049 Uiso 0.25 1 calc PR A 2
H3D H 0.8534 1.0317 0.6632 0.049 Uiso 0.25 1 calc PR A 2
C4A C 0.7748(8) 0.8341(7) 0.7200(5) 0.0607(11) Uiso 0.25 1 d PD A 2
H4C H 0.7441 0.7913 0.7996 0.073 Uiso 0.25 1 calc PR A 2
H4D H 0.8773 0.8006 0.6868 0.073 Uiso 0.25 1 calc PR A 2
C5 C 0.2924(6) 0.7905(6) 0.5481(5) 0.0431(13) Uiso 1 1 d . A .
H5A H 0.2441 0.7401 0.5075 0.052 Uiso 1 1 calc R . .
C6 C 0.2331(7) 0.9179(6) 0.5835(5) 0.0461(14) Uiso 1 1 d . . .
H6A H 0.1469 0.9539 0.5679 0.055 Uiso 1 1 calc R A .
C7 C 0.3032(6) 0.9906(6) 0.6422(5) 0.0468(14) Uiso 1 1 d . A .
H7A H 0.2661 1.0784 0.6687 0.056 Uiso 1 1 calc R . .
C8 C 0.4285(6) 0.9336(6) 0.6617(5) 0.0427(13) Uiso 1 1 d . . .
H8A H 0.4779 0.9841 0.7015 0.051 Uiso 1 1 calc R A .
C9 C 0.4856(5) 0.8038(5) 0.6252(4) 0.0333(11) Uiso 1 1 d . A .
C10 C 0.8444(7) 0.5597(6) 0.3303(5) 0.0536(15) Uiso 1 1 d . A .
H10A H 0.8051 0.5073 0.2850 0.064 Uiso 1 1 calc R . .
C11 C 0.9911(7) 0.5974(7) 0.2888(6) 0.0569(16) Uiso 1 1 d . . .
H11A H 1.0518 0.5712 0.2169 0.068 Uiso 1 1 calc R A .
C12 C 1.0473(7) 0.6735(6) 0.3538(5) 0.0541(15) Uiso 1 1 d . A .
H12A H 1.1480 0.7013 0.3279 0.065 Uiso 1 1 calc R . .
C13 C 0.9544(6) 0.7091(6) 0.4579(5) 0.0425(13) Uiso 1 1 d . . .
H13A H 0.9929 0.7621 0.5033 0.051 Uiso 1 1 calc R A .
C14 C 0.8061(6) 0.6697(5) 0.4984(4) 0.0338(11) Uiso 1 1 d . A .
C15 C 0.4988(6) 0.3081(6) 0.7396(5) 0.0448(13) Uiso 1 1 d . A .
H15A H 0.4543 0.2468 0.7039 0.054 Uiso 1 1 calc R . .
C16 C 0.5184(7) 0.2609(6) 0.8415(5) 0.0494(14) Uiso 1 1 d . . .
H16A H 0.4901 0.1688 0.8748 0.059 Uiso 1 1 calc R A .
C17 C 0.5799(7) 0.3502(6) 0.8943(5) 0.0506(15) Uiso 1 1 d . A .
H17A H 0.5939 0.3215 0.9656 0.061 Uiso 1 1 calc R . .
C18 C 0.6211(6) 0.4820(6) 0.8423(5) 0.0417(13) Uiso 1 1 d . . .
H18A H 0.6636 0.5442 0.8788 0.050 Uiso 1 1 calc R A .
C19 C 0.6022(5) 0.5270(5) 0.7370(4) 0.0335(11) Uiso 1 1 d . A .
C20 C 1.1402(13) 0.6219(12) -0.0804(9) 0.0607(11) Uiso 0.50 1 d PD B -1
H20A H 1.2151 0.6857 -0.1242 0.073 Uiso 0.50 1 calc PR B -1
C21 C 1.1747(14) 0.4859(11) -0.0527(8) 0.0607(11) Uiso 0.50 1 d PD B -1
H21A H 1.2750 0.4565 -0.0781 0.073 Uiso 0.50 1 calc PR B -1
C22 C 1.0678(10) 0.3904(14) 0.0110(8) 0.0607(11) Uiso 0.50 1 d PD B -1
H22A H 1.0945 0.2971 0.0290 0.073 Uiso 0.50 1 calc PR B -1
C23 C 0.9209(12) 0.4329(11) 0.0483(8) 0.0607(11) Uiso 0.50 1 d PD B -1
C24 C 0.8864(15) 0.5702(9) 0.0202(8) 0.0607(11) Uiso 0.50 1 d PD B -1
H24A H 0.7865 0.6006 0.0451 0.073 Uiso 0.50 1 calc PR B -1
C25 C 0.9950(12) 0.6631(13) -0.0433(9) 0.0607(11) Uiso 0.50 1 d PD B -1
H25A H 0.9690 0.7565 -0.0615 0.073 Uiso 0.50 1 calc PR B -1
C26 C 0.8032(14) 0.3342(12) 0.1166(10) 0.0607(11) Uiso 0.50 1 d PD B -1
H26A H 0.7158 0.3870 0.1570 0.091 Uiso 0.50 1 calc PR B -1
H26B H 0.8387 0.2763 0.1720 0.091 Uiso 0.50 1 calc PR B -1
H26C H 0.7771 0.2741 0.0660 0.091 Uiso 0.50 1 calc PR B -1


_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
Ca1 N2 2.462(4) 2_666 ?
Ca1 N2 2.462(4) . ?
Ca1 N3 2.485(4) 2_666 ?
Ca1 N3 2.485(4) . ?
Ca1 N1 2.489(4) . ?
Ca1 N1 2.489(4) 2_666 ?
Ca1 Al1 3.6368(14) 2_666 ?
Ca1 Al1 3.6368(14) . ?
Al1 C4 1.953(7) . ?
Al1 C14 2.020(5) . ?
Al1 C9 2.021(5) . ?
Al1 C19 2.027(5) . ?
N1 C5 1.338(7) . ?
N1 C9 1.371(6) . ?
N2 C10 1.353(7) . ?
N2 C14 1.360(6) . ?
N3 C15 1.343(7) . ?
N3 C19 1.368(6) . ?
C1 C2 1.531(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.541(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.512(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C1A C2A 1.532(10) . ?
C1A H1D 0.9800 . ?
C1A H1E 0.9800 . ?
C1A H1F 0.9800 . ?
C2A C3A 1.532(10) . ?
C2A H2C 0.9900 . ?
C2A H2D 0.9900 . ?
C3A H3C 0.9900 . ?
C3A H3D 0.9900 . ?
C5 C6 1.381(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.375(8) . ?
C6 H6A 0.9500 . ?
C7 C8 1.379(8) . ?
C7 H7A 0.9500 . ?
C8 C9 1.401(7) . ?
C8 H8A 0.9500 . ?
C10 C11 1.377(9) . ?
C10 H10A 0.9500 . ?
C11 C12 1.368(9) . ?
C11 H11A 0.9500 . ?
C12 C13 1.384(8) . ?
C12 H12A 0.9500 . ?
C13 C14 1.394(7) . ?
C13 H13A 0.9500 . ?
C15 C16 1.370(8) . ?
C15 H15A 0.9500 . ?
C16 C17 1.371(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.376(8) . ?
C17 H17A 0.9500 . ?
C18 C19 1.402(7) . ?
C18 H18A 0.9500 . ?
C20 C25 1.372(8) . ?
C20 C21 1.376(8) . ?
C20 H20A 0.9500 . ?
C21 C22 1.386(7) . ?
C21 H21A 0.9500 . ?
C22 C23 1.390(7) . ?
C22 H22A 0.9500 . ?
C23 C24 1.389(7) . ?
C23 C26 1.481(13) . ?
C24 C25 1.379(7) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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
N2 Ca1 N2 180.0(3) 2_666 . ?
N2 Ca1 N3 87.59(14) 2_666 2_666 ?
N2 Ca1 N3 92.41(14) . 2_666 ?
N2 Ca1 N3 92.41(14) 2_666 . ?
N2 Ca1 N3 87.59(14) . . ?
N3 Ca1 N3 180.000(1) 2_666 . ?
N2 Ca1 N1 91.91(14) 2_666 . ?
N2 Ca1 N1 88.09(14) . . ?
N3 Ca1 N1 91.99(13) 2_666 . ?
N3 Ca1 N1 88.01(13) . . ?
N2 Ca1 N1 88.09(14) 2_666 2_666 ?
N2 Ca1 N1 91.91(14) . 2_666 ?
N3 Ca1 N1 88.01(13) 2_666 2_666 ?
N3 Ca1 N1 91.99(13) . 2_666 ?
N1 Ca1 N1 180.00(19) . 2_666 ?
N2 Ca1 Al1 53.29(11) 2_666 2_666 ?
N2 Ca1 Al1 126.71(11) . 2_666 ?
N3 Ca1 Al1 53.23(10) 2_666 2_666 ?
N3 Ca1 Al1 126.77(10) . 2_666 ?
N1 Ca1 Al1 126.73(10) . 2_666 ?
N1 Ca1 Al1 53.27(10) 2_666 2_666 ?
N2 Ca1 Al1 126.71(11) 2_666 . ?
N2 Ca1 Al1 53.29(11) . . ?
N3 Ca1 Al1 126.77(10) 2_666 . ?
N3 Ca1 Al1 53.23(10) . . ?
N1 Ca1 Al1 53.27(10) . . ?
N1 Ca1 Al1 126.73(10) 2_666 . ?
Al1 Ca1 Al1 180.00(4) 2_666 . ?
C4 Al1 C14 108.4(2) . . ?
C4 Al1 C9 114.7(3) . . ?
C14 Al1 C9 107.2(2) . . ?
C4 Al1 C19 116.1(3) . . ?
C14 Al1 C19 104.4(2) . . ?
C9 Al1 C19 105.2(2) . . ?
C4 Al1 Ca1 174.7(2) . . ?
C14 Al1 Ca1 66.31(15) . . ?
C9 Al1 Ca1 67.18(14) . . ?
C19 Al1 Ca1 67.15(15) . . ?
C5 N1 C9 119.2(5) . . ?
C5 N1 Ca1 119.6(4) . . ?
C9 N1 Ca1 121.2(3) . . ?
C10 N2 C14 119.7(5) . . ?
C10 N2 Ca1 118.7(4) . . ?
C14 N2 Ca1 121.5(3) . . ?
C15 N3 C19 119.5(4) . . ?
C15 N3 Ca1 118.9(3) . . ?
C19 N3 Ca1 121.6(3) . . ?
C1 C2 C3 113.4(7) . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 C2 115.3(6) . . ?
C4 C3 H3A 108.4 . . ?
C2 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C2 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C3 C4 Al1 125.5(5) . . ?
C3 C4 H4A 105.9 . . ?
Al1 C4 H4A 105.9 . . ?
C3 C4 H4B 105.9 . . ?
Al1 C4 H4B 105.9 . . ?
H4A C4 H4B 106.3 . . ?
C2A C1A H1D 109.5 . . ?
C2A C1A H1E 109.5 . . ?
H1D C1A H1E 109.5 . . ?
C2A C1A H1F 109.5 . . ?
H1D C1A H1F 109.5 . . ?
H1E C1A H1F 109.5 . . ?
C1A C2A C3A 112.1(16) . . ?
C1A C2A H2C 109.2 . . ?
C3A C2A H2C 109.2 . . ?
C1A C2A H2D 109.2 . . ?
C3A C2A H2D 109.2 . . ?
H2C C2A H2D 107.9 . . ?
C2A C3A H3C 108.8 . . ?
C2A C3A H3D 108.8 . . ?
H3C C3A H3D 107.7 . . ?
N1 C5 C6 124.4(5) . . ?
N1 C5 H5A 117.8 . . ?
C6 C5 H5A 117.8 . . ?
C7 C6 C5 117.7(6) . . ?
C7 C6 H6A 121.1 . . ?
C5 C6 H6A 121.1 . . ?
C6 C7 C8 118.6(6) . . ?
C6 C7 H7A 120.7 . . ?
C8 C7 H7A 120.7 . . ?
C7 C8 C9 122.4(5) . . ?
C7 C8 H8A 118.8 . . ?
C9 C8 H8A 118.8 . . ?
N1 C9 C8 117.8(5) . . ?
N1 C9 Al1 118.3(3) . . ?
C8 C9 Al1 123.9(4) . . ?
N2 C10 C11 123.2(6) . . ?
N2 C10 H10A 118.4 . . ?
C11 C10 H10A 118.4 . . ?
C12 C11 C10 118.3(6) . . ?
C12 C11 H11A 120.8 . . ?
C10 C11 H11A 120.8 . . ?
C11 C12 C13 118.7(6) . . ?
C11 C12 H12A 120.6 . . ?
C13 C12 H12A 120.6 . . ?
C12 C13 C14 122.0(5) . . ?
C12 C13 H13A 119.0 . . ?
C14 C13 H13A 119.0 . . ?
N2 C14 C13 118.0(5) . . ?
N2 C14 Al1 118.9(4) . . ?
C13 C14 Al1 123.1(4) . . ?
N3 C15 C16 123.7(5) . . ?
N3 C15 H15A 118.1 . . ?
C16 C15 H15A 118.1 . . ?
C15 C16 C17 118.2(6) . . ?
C15 C16 H16A 120.9 . . ?
C17 C16 H16A 120.9 . . ?
C16 C17 C18 119.0(6) . . ?
C16 C17 H17A 120.5 . . ?
C18 C17 H17A 120.5 . . ?
C17 C18 C19 121.7(5) . . ?
C17 C18 H18A 119.1 . . ?
C19 C18 H18A 119.1 . . ?
N3 C19 C18 117.9(4) . . ?
N3 C19 Al1 118.0(3) . . ?
C18 C19 Al1 124.1(4) . . ?
C25 C20 C21 118.4(13) . . ?
C25 C20 H20A 120.8 . . ?
C21 C20 H20A 120.8 . . ?
C20 C21 C22 122.1(13) . . ?
C20 C21 H21A 119.0 . . ?
C22 C21 H21A 119.0 . . ?
C21 C22 C23 119.2(12) . . ?
C21 C22 H22A 120.4 . . ?
C23 C22 H22A 120.4 . . ?
C24 C23 C22 118.6(10) . . ?
C24 C23 C26 120.5(7) . . ?
C22 C23 C26 120.9(7) . . ?
C25 C24 C23 121.0(12) . . ?
C25 C24 H24A 119.5 . . ?
C23 C24 H24A 119.5 . . ?
C20 C25 C24 120.7(13) . . ?
C20 C25 H25A 119.7 . . ?
C24 C25 H25A 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.092
_database_code_depnum_ccdc_archive 'CCDC 993333'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw0821

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H42 Al2 Mn N6, C7 H8'
_chemical_formula_sum            'C45 H50 Al2 Mn N6'
_chemical_formula_weight         783.81

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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                   9.4064(5)
_cell_length_b                   9.5770(5)
_cell_length_c                   12.3360(7)
_cell_angle_alpha                86.303(2)
_cell_angle_beta                 72.415(3)
_cell_angle_gamma                89.284(2)
_cell_volume                     1057.13(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    22294
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             413
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_T_max  0.967
_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            11362
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.53
_diffrn_reflns_theta_max         27.55
_reflns_number_total             4710
_reflns_number_gt                3404
_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 -CH2-CH2-CH2-CH3 group and the toluene solvent molecule are both
 poorly resolved (both were modelled as disordered over two sites with
 bond length restraints and common isotropic displacement parameters for
 the carbon atoms).  Anisotropic displacement parameters were assigned to
 the Al and Mn atoms only.  An all-anisotropic refinement does behave and
 does converge but the resulting extra displacement parameters have no
 apparent physical significance.
;

_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)+(0.1425P)²+3.1509P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4710
_refine_ls_number_parameters     130
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1416
_refine_ls_R_factor_gt           0.1095
_refine_ls_wR_factor_ref         0.3071
_refine_ls_wR_factor_gt          0.2775
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_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 0.33556(18) 0.29067(16) 0.34736(13) 0.0440(4) Uani 1 1 d . . .
Mn1 Mn 0.5000 0.5000 0.5000 0.0401(3) Uani 1 2 d S . .
N1 N 0.4744(5) 0.5628(5) 0.3230(4) 0.0451(10) Uiso 1 1 d . . .
N2 N 0.2599(5) 0.4238(4) 0.5630(4) 0.0450(10) Uiso 1 1 d . . .
N3 N 0.5819(5) 0.2799(4) 0.4422(4) 0.0423(9) Uiso 1 1 d . . .
C1 C 0.052(2) -0.008(3) 0.183(3) 0.168(9) Uiso 0.50 1 d PD A 1
H1A H -0.0030 -0.0269 0.1296 0.252 Uiso 0.50 1 calc PR A 1
H1B H 0.0181 0.0796 0.2183 0.252 Uiso 0.50 1 calc PR A 1
H1C H 0.0354 -0.0850 0.2420 0.252 Uiso 0.50 1 calc PR A 1
C2 C 0.217(2) 0.0031(19) 0.1192(16) 0.093(4) Uiso 0.50 1 d PD A 1
H2A H 0.2644 -0.0883 0.1270 0.112 Uiso 0.50 1 calc PR A 1
H2B H 0.2297 0.0246 0.0372 0.112 Uiso 0.50 1 calc PR A 1
C3 C 0.2959(15) 0.1142(14) 0.1613(11) 0.068(2) Uiso 0.50 1 d PD A 1
H3A H 0.3940 0.0757 0.1615 0.081 Uiso 0.50 1 calc PR A 1
H3B H 0.3162 0.1937 0.1033 0.081 Uiso 0.50 1 calc PR A 1
C4 C 0.2299(9) 0.1725(8) 0.2717(7) 0.079(2) Uiso 0.50 1 d PD A 1
H4A H 0.1898 0.0918 0.3264 0.095 Uiso 0.50 1 calc PR A 1
H4B H 0.1426 0.2271 0.2650 0.095 Uiso 0.50 1 calc PR A 1
C1' C 0.228(3) -0.020(4) 0.0421(19) 0.168(9) Uiso 0.50 1 d PD A 2
H1D H 0.1992 -0.1077 0.0176 0.252 Uiso 0.50 1 calc PR A 2
H1E H 0.3342 -0.0233 0.0372 0.252 Uiso 0.50 1 calc PR A 2
H1F H 0.2113 0.0585 -0.0075 0.252 Uiso 0.50 1 calc PR A 2
C2' C 0.140(2) -0.001(2) 0.1593(15) 0.093(4) Uiso 0.50 1 d PD A 2
H2C H 0.0820 -0.0892 0.1857 0.112 Uiso 0.50 1 calc PR A 2
H2D H 0.0658 0.0717 0.1544 0.112 Uiso 0.50 1 calc PR A 2
C3' C 0.1964(16) 0.0360(13) 0.2578(11) 0.068(2) Uiso 0.50 1 d PD A 2
H3C H 0.1207 0.0016 0.3292 0.081 Uiso 0.50 1 calc PR A 2
H3D H 0.2876 -0.0195 0.2520 0.081 Uiso 0.50 1 calc PR A 2
C4' C 0.2299(9) 0.1725(8) 0.2717(7) 0.079(2) Uiso 0.50 1 d PD A 2
H4C H 0.1289 0.2133 0.2959 0.095 Uiso 0.50 1 calc PR A 2
H4D H 0.2727 0.2081 0.1914 0.095 Uiso 0.50 1 calc PR A 2
C5 C 0.4086(6) 0.4776(5) 0.2668(4) 0.0434(11) Uiso 1 1 d . A .
C6 C 0.3923(7) 0.5259(6) 0.1609(5) 0.0541(14) Uiso 1 1 d . . .
H6 H 0.3470 0.4670 0.1216 0.065 Uiso 1 1 calc R A .
C7 C 0.4415(8) 0.6584(7) 0.1133(6) 0.0637(16) Uiso 1 1 d . A .
H7 H 0.4297 0.6907 0.0421 0.076 Uiso 1 1 calc R . .
C8 C 0.5081(8) 0.7427(7) 0.1717(6) 0.0651(16) Uiso 1 1 d . . .
H8 H 0.5422 0.8343 0.1416 0.078 Uiso 1 1 calc R A .
C9 C 0.5240(7) 0.6908(6) 0.2746(5) 0.0548(14) Uiso 1 1 d . A .
H9 H 0.5722 0.7479 0.3133 0.066 Uiso 1 1 calc R . .
C10 C 0.2012(6) 0.3421(5) 0.4993(4) 0.0429(11) Uiso 1 1 d . A .
C11 C 0.0497(7) 0.3032(6) 0.5437(5) 0.0537(13) Uiso 1 1 d . . .
H11 H 0.0071 0.2468 0.5008 0.064 Uiso 1 1 calc R A .
C12 C -0.0384(8) 0.3444(7) 0.6475(6) 0.0609(15) Uiso 1 1 d . A .
H12 H -0.1402 0.3164 0.6760 0.073 Uiso 1 1 calc R . .
C13 C 0.0226(7) 0.4259(7) 0.7087(6) 0.0590(15) Uiso 1 1 d . . .
H13 H -0.0359 0.4570 0.7800 0.071 Uiso 1 1 calc R A .
C14 C 0.1718(7) 0.4622(6) 0.6646(5) 0.0532(13) Uiso 1 1 d . A .
H14 H 0.2145 0.5173 0.7082 0.064 Uiso 1 1 calc R . .
C15 C 0.5158(6) 0.2041(5) 0.3804(4) 0.0415(11) Uiso 1 1 d . A .
C16 C 0.5752(7) 0.0734(6) 0.3469(5) 0.0558(14) Uiso 1 1 d . . .
H16 H 0.5289 0.0193 0.3049 0.067 Uiso 1 1 calc R A .
C17 C 0.6996(7) 0.0205(7) 0.3732(6) 0.0604(15) Uiso 1 1 d . A .
H17 H 0.7396 -0.0677 0.3487 0.072 Uiso 1 1 calc R . .
C18 C 0.7629(7) 0.0987(6) 0.4352(5) 0.0544(14) Uiso 1 1 d . . .
H18 H 0.8472 0.0654 0.4559 0.065 Uiso 1 1 calc R A .
C19 C 0.7024(6) 0.2270(6) 0.4674(5) 0.0499(13) Uiso 1 1 d . A .
H19 H 0.7482 0.2812 0.5097 0.060 Uiso 1 1 calc R . .
C20 C 0.8464(9) 0.5219(7) 0.0433(7) 0.0885(13) Uiso 1 1 d D . .
H20 H 0.7421 0.5369 0.0723 0.106 Uiso 1 1 calc R B 1
C22 C 1.0578(8) 0.3709(8) 0.0111(7) 0.0885(13) Uiso 1 1 d D . .
H22 H 1.0965 0.2801 0.0193 0.106 Uiso 1 1 calc R C 1
C21 C 0.9064(9) 0.3926(8) 0.0542(8) 0.0885(13) Uiso 0.50 1 d PD D 1
C23 C 0.8010(18) 0.2836(16) 0.1143(15) 0.0885(13) Uiso 0.50 1 d PD D 1
H23A H 0.7013 0.3239 0.1426 0.133 Uiso 0.50 1 calc PR D 1
H23B H 0.8312 0.2424 0.1787 0.133 Uiso 0.50 1 calc PR D 1
H23C H 0.7992 0.2110 0.0623 0.133 Uiso 0.50 1 calc PR D 1
C21' C 0.9064(9) 0.3926(8) 0.0542(8) 0.0885(13) Uiso 0.50 1 d P D 2
H21' H 0.8428 0.3167 0.0919 0.133 Uiso 0.50 1 calc PR D 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 C4 1.965(8) . ?
Al1 C10 2.006(5) . ?
Al1 C5 2.013(5) . ?
Al1 C15 2.017(5) . ?
Mn1 N2 2.268(4) . ?
Mn1 N2 2.268(4) 2_666 ?
Mn1 N1 2.309(4) . ?
Mn1 N1 2.309(4) 2_666 ?
Mn1 N3 2.317(4) . ?
Mn1 N3 2.317(4) 2_666 ?
N1 C9 1.352(7) . ?
N1 C5 1.369(7) . ?
N2 C14 1.347(7) . ?
N2 C10 1.374(7) . ?
N3 C19 1.347(7) . ?
N3 C15 1.365(6) . ?
C1 C2 1.511(19) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.509(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.459(13) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C1' C2' 1.456(19) . ?
C1' H1D 0.9800 . ?
C1' H1E 0.9800 . ?
C1' H1F 0.9800 . ?
C2' C3' 1.531(16) . ?
C2' H2C 0.9900 . ?
C2' H2D 0.9900 . ?
C3' H3C 0.9900 . ?
C3' H3D 0.9900 . ?
C5 C6 1.409(8) . ?
C6 C7 1.386(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(9) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.409(8) . ?
C11 C12 1.378(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.363(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(9) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.399(8) . ?
C16 C17 1.388(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.365(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.378(8) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.370(7) . ?
C20 C22 1.373(5) 2_765 ?
C20 H20 0.9500 . ?
C22 C20 1.373(5) 2_765 ?
C22 C21 1.379(7) . ?
C22 H22 0.9500 . ?
C21 C23 1.450(9) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 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
C4 Al1 C10 111.0(3) . . ?
C4 Al1 C5 116.2(3) . . ?
C10 Al1 C5 103.2(2) . . ?
C4 Al1 C15 115.7(3) . . ?
C10 Al1 C15 105.0(2) . . ?
C5 Al1 C15 104.5(2) . . ?
N2 Mn1 N2 180.0 . 2_666 ?
N2 Mn1 N1 90.46(16) . . ?
N2 Mn1 N1 89.54(16) 2_666 . ?
N2 Mn1 N1 89.54(16) . 2_666 ?
N2 Mn1 N1 90.46(16) 2_666 2_666 ?
N1 Mn1 N1 180.000(1) . 2_666 ?
N2 Mn1 N3 91.18(15) . . ?
N2 Mn1 N3 88.82(15) 2_666 . ?
N1 Mn1 N3 90.78(15) . . ?
N1 Mn1 N3 89.22(15) 2_666 . ?
N2 Mn1 N3 88.82(15) . 2_666 ?
N2 Mn1 N3 91.18(15) 2_666 2_666 ?
N1 Mn1 N3 89.22(15) . 2_666 ?
N1 Mn1 N3 90.78(15) 2_666 2_666 ?
N3 Mn1 N3 180.000(1) . 2_666 ?
C9 N1 C5 119.1(5) . . ?
C9 N1 Mn1 118.0(4) . . ?
C5 N1 Mn1 122.9(3) . . ?
C14 N2 C10 119.2(5) . . ?
C14 N2 Mn1 119.1(4) . . ?
C10 N2 Mn1 121.7(3) . . ?
C19 N3 C15 118.9(4) . . ?
C19 N3 Mn1 118.6(3) . . ?
C15 N3 Mn1 122.5(3) . . ?
C3 C2 C1 113.1(14) . . ?
C3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 C2 121.7(11) . . ?
C4 C3 H3A 106.9 . . ?
C2 C3 H3A 106.9 . . ?
C4 C3 H3B 106.9 . . ?
C2 C3 H3B 106.9 . . ?
H3A C3 H3B 106.7 . . ?
C3 C4 Al1 125.1(7) . . ?
C3 C4 H4A 106.0 . . ?
Al1 C4 H4A 106.0 . . ?
C3 C4 H4B 106.0 . . ?
Al1 C4 H4B 106.0 . . ?
H4A C4 H4B 106.3 . . ?
C2' C1' H1D 109.5 . . ?
C2' C1' H1E 109.5 . . ?
H1D C1' H1E 109.5 . . ?
C2' C1' H1F 109.5 . . ?
H1D C1' H1F 109.5 . . ?
H1E C1' H1F 109.5 . . ?
C1' C2' C3' 127.2(18) . . ?
C1' C2' H2C 105.5 . . ?
C3' C2' H2C 105.5 . . ?
C1' C2' H2D 105.5 . . ?
C3' C2' H2D 105.5 . . ?
H2C C2' H2D 106.1 . . ?
C2' C3' H3C 107.0 . . ?
C2' C3' H3D 107.0 . . ?
H3C C3' H3D 106.7 . . ?
N1 C5 C6 119.3(5) . . ?
N1 C5 Al1 115.9(4) . . ?
C6 C5 Al1 124.7(4) . . ?
C7 C6 C5 120.9(6) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C8 118.7(6) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 118.6(6) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
N1 C9 C8 123.3(6) . . ?
N1 C9 H9 118.3 . . ?
C8 C9 H9 118.3 . . ?
N2 C10 C11 117.8(5) . . ?
N2 C10 Al1 117.8(4) . . ?
C11 C10 Al1 124.4(4) . . ?
C12 C11 C10 121.9(6) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C13 C12 C11 119.0(6) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 118.4(6) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
N2 C14 C13 123.7(6) . . ?
N2 C14 H14 118.2 . . ?
C13 C14 H14 118.2 . . ?
N3 C15 C16 118.5(5) . . ?
N3 C15 Al1 116.2(3) . . ?
C16 C15 Al1 125.3(4) . . ?
C17 C16 C15 122.0(6) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C18 C17 C16 118.1(6) . . ?
C18 C17 H17 121.0 . . ?
C16 C17 H17 121.0 . . ?
C17 C18 C19 118.9(6) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
N3 C19 C18 123.6(5) . . ?
N3 C19 H19 118.2 . . ?
C18 C19 H19 118.2 . . ?
C21 C20 C22 117.7(8) . 2_765 ?
C21 C20 H20 121.1 . . ?
C22 C20 H20 121.1 2_765 . ?
C20 C22 C21 121.3(8) 2_765 . ?
C20 C22 H22 119.4 2_765 . ?
C21 C22 H22 119.4 . . ?
C20 C21 C22 121.0(7) . . ?
C20 C21 C23 115.6(10) . . ?
C22 C21 C23 123.4(10) . . ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.108
_database_code_depnum_ccdc_archive 'CCDC 993334'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw0848

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H42 Al2 Ca N6, C7 H8'
_chemical_formula_sum            'C45 H50 Al2 Ca N6'
_chemical_formula_weight         768.95

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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                   9.5380(4)
_cell_length_b                   9.5762(5)
_cell_length_c                   12.4193(7)
_cell_angle_alpha                89.456(2)
_cell_angle_beta                 72.848(2)
_cell_angle_gamma                86.782(3)
_cell_volume                     1082.16(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    11754
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             408
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 Poor crystal, poor data.  The refinement presented several problems
 (see _refine_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            11281
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.77
_diffrn_reflns_theta_max         27.51
_reflns_number_total             4841
_reflns_number_gt                3113
_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 sec-Bu group and the toluene solvent molecule are both
 poorly resolved, the toluene is disordered about an inversion centre.
 Both were modelled with bond length restraints and common
 isotropic displacement parameters for the carbon atoms.  Anisotropic
 displacement parameters were assigned to the Al and Ca atoms only. 
 
;

_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)+(0.1920P)²+5.9814P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4841
_refine_ls_number_parameters     68
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1995
_refine_ls_R_factor_gt           0.1434
_refine_ls_wR_factor_ref         0.4026
_refine_ls_wR_factor_gt          0.3512
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
Ca1 Ca 0.5000 0.5000 0.5000 0.0358(5) Uani 1 2 d S . .
Al1 Al 0.3370(2) 0.2770(2) 0.33850(16) 0.0371(5) Uani 1 1 d . . .
C1 C 0.2553(13) 0.1567(11) 0.2439(9) 0.115(2) Uiso 1 1 d D . .
H1 H 0.1783 0.2204 0.2265 0.138 Uiso 1 1 calc R . .
C4 C 0.3644(15) 0.1280(14) 0.1286(10) 0.115(2) Uiso 1 1 d D . .
H4A H 0.3189 0.0731 0.0831 0.173 Uiso 1 1 calc R . .
H4B H 0.4516 0.0755 0.1373 0.173 Uiso 1 1 calc R . .
H4C H 0.3932 0.2169 0.0911 0.173 Uiso 1 1 calc R . .
C2 C 0.1738(14) 0.0258(13) 0.2857(9) 0.115(2) Uiso 1 1 d D . .
H2A H 0.0939 0.0471 0.3562 0.138 Uiso 1 1 calc R . .
H2B H 0.2421 -0.0473 0.3021 0.138 Uiso 1 1 calc R . .
C3 C 0.1098(16) -0.0268(14) 0.1963(11) 0.115(2) Uiso 1 1 d D . .
H3A H 0.0766 -0.1213 0.2154 0.173 Uiso 1 1 calc R . .
H3B H 0.1853 -0.0288 0.1229 0.173 Uiso 1 1 calc R . .
H3C H 0.0264 0.0358 0.1928 0.173 Uiso 1 1 calc R . .
N1 N 0.4667(5) 0.5500(4) 0.3137(3) 0.0416(8) Uiso 1 1 d G . .
C11 C 0.3986(5) 0.4602(3) 0.2602(3) 0.0439(7) Uiso 1 1 d G . .
C12 C 0.3702(5) 0.5003(4) 0.1605(4) 0.0516(8) Uiso 1 1 d G . .
H12 H 0.3236 0.4388 0.1239 0.062 Uiso 1 1 calc R . .
C13 C 0.4098(6) 0.6302(5) 0.1143(3) 0.0569(11) Uiso 1 1 d G . .
H13 H 0.3903 0.6576 0.0461 0.068 Uiso 1 1 calc R . .
C14 C 0.4779(5) 0.7201(4) 0.1678(4) 0.0516(8) Uiso 1 1 d G . .
H14 H 0.5049 0.8089 0.1362 0.062 Uiso 1 1 calc R . .
C15 C 0.5064(5) 0.6800(4) 0.2675(3) 0.0439(7) Uiso 1 1 d G . .
H15 H 0.5529 0.7414 0.3040 0.053 Uiso 1 1 calc R . .
N2 N 0.5867(4) 0.2609(3) 0.4322(3) 0.0416(8) Uiso 1 1 d G . .
C21 C 0.5178(4) 0.1834(4) 0.3705(4) 0.0439(7) Uiso 1 1 d G . .
C22 C 0.5708(5) 0.0479(4) 0.3360(4) 0.0516(8) Uiso 1 1 d G . .
H22 H 0.5238 -0.0051 0.2939 0.062 Uiso 1 1 calc R . .
C23 C 0.6928(5) -0.0101(3) 0.3633(4) 0.0569(11) Uiso 1 1 d G . .
H23 H 0.7290 -0.1027 0.3398 0.068 Uiso 1 1 calc R . .
C24 C 0.7616(4) 0.0674(4) 0.4250(4) 0.0516(8) Uiso 1 1 d G . .
H24 H 0.8450 0.0277 0.4437 0.062 Uiso 1 1 calc R . .
C25 C 0.7086(4) 0.2029(4) 0.4595(4) 0.0439(7) Uiso 1 1 d G . .
H25 H 0.7556 0.2558 0.5017 0.053 Uiso 1 1 calc R . .
N3 N 0.2506(3) 0.4174(4) 0.5576(3) 0.0416(8) Uiso 1 1 d G . .
C31 C 0.1953(4) 0.3345(5) 0.4901(3) 0.0439(7) Uiso 1 1 d G . .
C32 C 0.0505(5) 0.2965(5) 0.5278(4) 0.0516(8) Uiso 1 1 d G . .
H32 H 0.0127 0.2398 0.4816 0.062 Uiso 1 1 calc R . .
C33 C -0.0391(4) 0.3414(5) 0.6329(4) 0.0569(11) Uiso 1 1 d G . .
H33 H -0.1381 0.3154 0.6587 0.068 Uiso 1 1 calc R . .
C34 C 0.0162(4) 0.4243(5) 0.7005(3) 0.0516(8) Uiso 1 1 d G . .
H34 H -0.0450 0.4549 0.7724 0.062 Uiso 1 1 calc R . .
C35 C 0.1611(4) 0.4622(4) 0.6628(3) 0.0439(7) Uiso 1 1 d G . .
H35 H 0.1989 0.5189 0.7090 0.053 Uiso 1 1 calc R . .
C5 C 0.0768(14) 0.3774(14) 0.9950(11) 0.097(2) Uiso 1 1 d . . .
H5 H 0.1315 0.2904 0.9897 0.117 Uiso 1 1 calc R . .
C6 C 0.1481(15) 0.4908(14) 0.9522(11) 0.097(2) Uiso 1 1 d . . .
H6 H 0.2519 0.4814 0.9210 0.117 Uiso 1 1 calc R A 1
C7 C 0.0799(15) 0.6188(14) 0.9511(11) 0.097(2) Uiso 0.50 1 d P . 1
C8 C 0.163(3) 0.725(3) 0.895(2) 0.097(2) Uiso 0.50 1 d P B 1
H8A H 0.2679 0.6981 0.8805 0.146 Uiso 0.50 1 calc PR B 1
H8B H 0.1390 0.8105 0.9417 0.146 Uiso 0.50 1 calc PR B 1
H8C H 0.1423 0.7432 0.8234 0.146 Uiso 0.50 1 calc PR B 1
C7' C 0.0799(15) 0.6188(14) 0.9511(11) 0.097(2) Uiso 0.50 1 d P . 2
H7' H 0.1304 0.6985 0.9180 0.146 Uiso 0.50 1 calc PR . 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
Ca1 N3 2.448(3) 2_666 ?
Ca1 N3 2.448(3) . ?
Ca1 N2 2.459(3) 2_666 ?
Ca1 N2 2.459(3) . ?
Ca1 N1 2.466(3) . ?
Ca1 N1 2.466(3) 2_666 ?
Ca1 Al1 3.6458(18) . ?
Ca1 Al1 3.6458(18) 2_666 ?
Al1 C1 1.995(11) . ?
Al1 C31 2.027(4) . ?
Al1 C11 2.028(4) . ?
Al1 C21 2.039(3) . ?
C1 C2 1.518(7) . ?
C1 C4 1.518(7) . ?
C1 H1 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C2 C3 1.518(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
N1 C11 1.3900 . ?
N1 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 H12 0.9500 . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N2 C21 1.3900 . ?
N2 C25 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22 0.9500 . ?
C23 C24 1.3900 . ?
C23 H23 0.9500 . ?
C24 C25 1.3900 . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
N3 C31 1.3900 . ?
N3 C35 1.3900 . ?
C31 C32 1.3900 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 C35 1.3900 . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C5 C6 1.335(16) . ?
C5 C7' 1.445(18) 2_567 ?
C5 C7 1.445(18) 2_567 ?
C5 H5 0.9500 . ?
C6 C7 1.357(17) . ?
C6 H6 0.9500 . ?
C7 C8 1.38(3) . ?
C7 C5 1.445(18) 2_567 ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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 Ca1 N3 180.00(18) 2_666 . ?
N3 Ca1 N2 87.44(13) 2_666 2_666 ?
N3 Ca1 N2 92.56(13) . 2_666 ?
N3 Ca1 N2 92.56(13) 2_666 . ?
N3 Ca1 N2 87.44(13) . . ?
N2 Ca1 N2 180.0 2_666 . ?
N3 Ca1 N1 92.34(13) 2_666 . ?
N3 Ca1 N1 87.66(13) . . ?
N2 Ca1 N1 92.02(13) 2_666 . ?
N2 Ca1 N1 87.98(13) . . ?
N3 Ca1 N1 87.66(13) 2_666 2_666 ?
N3 Ca1 N1 92.34(13) . 2_666 ?
N2 Ca1 N1 87.98(13) 2_666 2_666 ?
N2 Ca1 N1 92.02(13) . 2_666 ?
N1 Ca1 N1 180.0 . 2_666 ?
N3 Ca1 Al1 127.11(9) 2_666 . ?
N3 Ca1 Al1 52.89(9) . . ?
N2 Ca1 Al1 126.65(9) 2_666 . ?
N2 Ca1 Al1 53.35(9) . . ?
N1 Ca1 Al1 53.13(9) . . ?
N1 Ca1 Al1 126.87(9) 2_666 . ?
N3 Ca1 Al1 52.89(9) 2_666 2_666 ?
N3 Ca1 Al1 127.11(9) . 2_666 ?
N2 Ca1 Al1 53.35(9) 2_666 2_666 ?
N2 Ca1 Al1 126.65(9) . 2_666 ?
N1 Ca1 Al1 126.87(9) . 2_666 ?
N1 Ca1 Al1 53.13(9) 2_666 2_666 ?
Al1 Ca1 Al1 180.00(5) . 2_666 ?
C1 Al1 C31 115.2(3) . . ?
C1 Al1 C11 110.8(4) . . ?
C31 Al1 C11 104.6(2) . . ?
C1 Al1 C21 112.1(4) . . ?
C31 Al1 C21 106.4(2) . . ?
C11 Al1 C21 107.1(2) . . ?
C1 Al1 Ca1 177.4(3) . . ?
C31 Al1 Ca1 67.33(12) . . ?
C11 Al1 Ca1 67.36(12) . . ?
C21 Al1 Ca1 67.17(12) . . ?
C2 C1 C4 109.41(10) . . ?
C2 C1 Al1 124.2(7) . . ?
C4 C1 Al1 111.7(8) . . ?
C2 C1 H1 102.9 . . ?
C4 C1 H1 102.9 . . ?
Al1 C1 H1 102.9 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C2 C3 109.41(10) . . ?
C1 C2 H2A 109.8 . . ?
C3 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
C3 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C11 N1 C15 120.0 . . ?
C11 N1 Ca1 122.68(19) . . ?
C15 N1 Ca1 117.03(19) . . ?
C12 C11 N1 120.0 . . ?
C12 C11 Al1 123.2(2) . . ?
N1 C11 Al1 116.7(2) . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 N1 120.0 . . ?
C14 C15 H15 120.0 . . ?
N1 C15 H15 120.0 . . ?
C21 N2 C25 120.0 . . ?
C21 N2 Ca1 122.77(19) . . ?
C25 N2 Ca1 117.22(19) . . ?
N2 C21 C22 120.0 . . ?
N2 C21 Al1 116.7(2) . . ?
C22 C21 Al1 123.3(2) . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 N2 120.0 . . ?
C24 C25 H25 120.0 . . ?
N2 C25 H25 120.0 . . ?
C31 N3 C35 120.0 . . ?
C31 N3 Ca1 123.74(19) . . ?
C35 N3 Ca1 116.22(19) . . ?
N3 C31 C32 120.0 . . ?
N3 C31 Al1 116.0(2) . . ?
C32 C31 Al1 124.0(2) . . ?
C31 C32 C33 120.0 . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 N3 120.0 . . ?
C34 C35 H35 120.0 . . ?
N3 C35 H35 120.0 . . ?
C6 C5 C7' 122.9(12) . 2_567 ?
C6 C5 C7 122.9(12) . 2_567 ?
C7' C5 C7 0.0(12) 2_567 2_567 ?
C6 C5 H5 118.6 . . ?
C7' C5 H5 118.6 2_567 . ?
C7 C5 H5 118.6 2_567 . ?
C5 C6 C7 123.3(13) . . ?
C5 C6 H6 118.3 . . ?
C7 C6 H6 118.3 . . ?
C6 C7 C8 118.0(16) . . ?
C6 C7 C5 113.8(12) . 2_567 ?
C8 C7 C5 128.1(16) . 2_567 ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.721
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.132
_database_code_depnum_ccdc_archive 'CCDC 993335'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw0854

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H42 Al2 Mn N6, C7 H8'
_chemical_formula_sum            'C45 H50 Al2 Mn N6'
_chemical_formula_weight         783.81

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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                   9.4224(2)
_cell_length_b                   9.4959(2)
_cell_length_c                   12.3300(3)
_cell_angle_alpha                90.491(2)
_cell_angle_beta                 106.116(2)
_cell_angle_gamma                93.0150(10)
_cell_volume                     1058.09(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    10715
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      24.11

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             413
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_T_max  0.965
_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            14981
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         24.12
_reflns_number_total             3332
_reflns_number_gt                2748
_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 sec-Bu group and the toluene solvent molecule are both
 poorly resolved: both were modelled with bond length restraints and common
 isotropic displacement parameters for the carbon atoms.  
;

_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)+(0.0929P)²+3.1819P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3332
_refine_ls_number_parameters     216
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.2000
_refine_ls_wR_factor_gt          0.1872
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.050
_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
Mn1 Mn 0.5000 0.0000 0.0000 0.0303(3) Uani 1 2 d S . .
Al1 Al 0.34241(14) 0.21970(14) 0.16025(11) 0.0333(4) Uani 1 1 d . . .
C1 C 0.2630(8) 0.3432(8) 0.2575(6) 0.0784(13) Uiso 0.623(9) 1 d PD A 1
H1 H 0.1828 0.2797 0.2725 0.094 Uiso 0.623(9) 1 calc PR A 1
C2 C 0.3745(13) 0.3629(14) 0.3802(8) 0.0784(13) Uiso 0.623(9) 1 d PD A 1
H2A H 0.3409 0.4361 0.4223 0.118 Uiso 0.623(9) 1 calc PR A 1
H2B H 0.4735 0.3912 0.3740 0.118 Uiso 0.623(9) 1 calc PR A 1
H2C H 0.3781 0.2737 0.4200 0.118 Uiso 0.623(9) 1 calc PR A 1
C3 C 0.1884(13) 0.4632(12) 0.2215(9) 0.0784(13) Uiso 0.623(9) 1 d PD A 1
H3A H 0.1103 0.4392 0.1506 0.094 Uiso 0.623(9) 1 calc PR A 1
H3B H 0.2587 0.5341 0.2035 0.094 Uiso 0.623(9) 1 calc PR A 1
C4 C 0.1130(13) 0.5342(13) 0.3085(10) 0.0784(13) Uiso 0.623(9) 1 d PD A 1
H4A H 0.1064 0.6354 0.2946 0.118 Uiso 0.623(9) 1 calc PR A 1
H4B H 0.1731 0.5203 0.3860 0.118 Uiso 0.623(9) 1 calc PR A 1
H4C H 0.0135 0.4904 0.2982 0.118 Uiso 0.623(9) 1 calc PR A 1
C1' C 0.2630(8) 0.3432(8) 0.2575(6) 0.0784(13) Uiso 0.377(9) 1 d PD A 2
H1' H 0.2583 0.4302 0.2118 0.094 Uiso 0.377(9) 1 calc PR A 2
C2' C 0.3913(18) 0.400(2) 0.3639(13) 0.0784(13) Uiso 0.377(9) 1 d PD A 2
H2'A H 0.3495 0.4552 0.4137 0.118 Uiso 0.377(9) 1 calc PR A 2
H2'B H 0.4637 0.4593 0.3388 0.118 Uiso 0.377(9) 1 calc PR A 2
H2'C H 0.4402 0.3197 0.4050 0.118 Uiso 0.377(9) 1 calc PR A 2
C3' C 0.1222(15) 0.3414(19) 0.2676(16) 0.0784(13) Uiso 0.377(9) 1 d PD A 2
H3'A H 0.1027 0.2506 0.3010 0.094 Uiso 0.377(9) 1 calc PR A 2
H3'B H 0.0538 0.3417 0.1904 0.094 Uiso 0.377(9) 1 calc PR A 2
C4' C 0.079(2) 0.464(2) 0.3396(16) 0.0784(13) Uiso 0.377(9) 1 d PD A 2
H4'A H 0.0262 0.4229 0.3912 0.118 Uiso 0.377(9) 1 calc PR A 2
H4'B H 0.0142 0.5277 0.2885 0.118 Uiso 0.377(9) 1 calc PR A 2
H4'C H 0.1685 0.5175 0.3833 0.118 Uiso 0.377(9) 1 calc PR A 2
N1 N 0.4753(4) -0.0510(4) 0.1767(3) 0.0354(9) Uani 1 1 d . . .
C11 C 0.4070(5) 0.0358(5) 0.2333(4) 0.0333(10) Uani 1 1 d . A .
C12 C 0.3823(5) -0.0107(5) 0.3345(4) 0.0418(11) Uani 1 1 d . . .
H12 H 0.3353 0.0487 0.3747 0.050 Uiso 1 1 calc R A .
C13 C 0.4244(6) -0.1403(6) 0.3771(4) 0.0492(13) Uani 1 1 d . A .
H13 H 0.4048 -0.1711 0.4449 0.059 Uiso 1 1 calc R . .
C14 C 0.4956(6) -0.2249(5) 0.3196(4) 0.0485(13) Uani 1 1 d . . .
H14 H 0.5276 -0.3142 0.3474 0.058 Uiso 1 1 calc R A .
C15 C 0.5189(6) -0.1761(5) 0.2207(4) 0.0422(11) Uani 1 1 d . A .
H15 H 0.5685 -0.2338 0.1814 0.051 Uiso 1 1 calc R . .
N2 N 0.4132(4) -0.2261(4) -0.0591(3) 0.0350(9) Uani 1 1 d . . .
C21 C 0.4784(5) -0.3067(5) -0.1219(4) 0.0340(10) Uani 1 1 d . . .
C22 C 0.4188(6) -0.4442(5) -0.1523(5) 0.0448(12) Uani 1 1 d . . .
H22 H 0.4630 -0.5014 -0.1961 0.054 Uiso 1 1 calc R A .
C23 C 0.2983(6) -0.4995(5) -0.1210(5) 0.0510(13) Uani 1 1 d . A .
H23 H 0.2595 -0.5930 -0.1428 0.061 Uiso 1 1 calc R . .
C24 C 0.2358(6) -0.4162(5) -0.0577(5) 0.0476(13) Uani 1 1 d . . .
H24 H 0.1530 -0.4508 -0.0340 0.057 Uiso 1 1 calc R A .
C25 C 0.2955(5) -0.2819(5) -0.0292(4) 0.0427(12) Uani 1 1 d . A .
H25 H 0.2512 -0.2245 0.0143 0.051 Uiso 1 1 calc R . .
N3 N 0.7380(4) -0.0703(4) 0.0555(3) 0.0354(9) Uani 1 1 d . . .
C31 C 0.7948(5) -0.1559(5) -0.0094(4) 0.0337(10) Uani 1 1 d . . .
C32 C 0.9417(5) -0.1928(5) 0.0331(4) 0.0422(11) Uani 1 1 d . . .
H32 H 0.9824 -0.2525 -0.0113 0.051 Uiso 1 1 calc R A .
C33 C 1.0286(5) -0.1451(6) 0.1376(4) 0.0477(13) Uani 1 1 d . A .
H33 H 1.1277 -0.1719 0.1652 0.057 Uiso 1 1 calc R . .
C34 C 0.9692(5) -0.0578(6) 0.2011(4) 0.0463(12) Uani 1 1 d . . .
H34 H 1.0267 -0.0224 0.2731 0.056 Uiso 1 1 calc R A .
C35 C 0.8249(5) -0.0232(5) 0.1581(4) 0.0423(11) Uani 1 1 d . A .
H35 H 0.7839 0.0367 0.2022 0.051 Uiso 1 1 calc R . .
C41 C 0.9222(9) -0.1269(8) 0.4915(7) 0.0902(13) Uiso 1 1 d D . .
H41 H 0.8671 -0.2148 0.4844 0.108 Uiso 1 1 calc R . .
C42 C 0.8493(9) -0.0076(7) 0.4540(7) 0.0902(13) Uiso 1 1 d D . .
H42 H 0.7449 -0.0151 0.4232 0.108 Uiso 1 1 calc R B 1
C43 C 0.9229(9) 0.1225(8) 0.4596(7) 0.0902(13) Uiso 0.50 1 d PD . 1
C44 C 0.8406(19) 0.2377(17) 0.4108(14) 0.0902(13) Uiso 0.50 1 d P C 1
H44A H 0.8707 0.2679 0.3443 0.108 Uiso 0.50 1 calc PR C 1
H44B H 0.8592 0.3161 0.4661 0.108 Uiso 0.50 1 calc PR C 1
H44C H 0.7349 0.2090 0.3883 0.108 Uiso 0.50 1 calc PR C 1
C43' C 0.9229(9) 0.1225(8) 0.4596(7) 0.0902(13) Uiso 0.50 1 d P . 2
H43 H 0.8725 0.2047 0.4322 0.108 Uiso 0.50 1 calc PR . 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
Mn1 N3 2.293(4) . ?
Mn1 N3 2.293(4) 2_655 ?
Mn1 N2 2.295(4) 2_655 ?
Mn1 N2 2.295(4) . ?
Mn1 N1 2.308(4) . ?
Mn1 N1 2.308(4) 2_655 ?
Al1 C1 1.986(8) . ?
Al1 C21 2.015(5) 2_655 ?
Al1 C11 2.016(5) . ?
Al1 C31 2.016(5) 2_655 ?
C1 C3 1.381(12) . ?
C1 C2 1.587(11) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.603(13) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C2' H2'A 0.9800 . ?
C2' H2'B 0.9800 . ?
C2' H2'C 0.9800 . ?
C3' C4' 1.598(14) . ?
C3' H3'A 0.9900 . ?
C3' H3'B 0.9900 . ?
C4' H4'A 0.9800 . ?
C4' H4'B 0.9800 . ?
C4' H4'C 0.9800 . ?
N1 C15 1.346(6) . ?
N1 C11 1.369(6) . ?
C11 C12 1.403(7) . ?
C12 C13 1.376(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N2 C25 1.348(6) . ?
N2 C21 1.366(6) . ?
C21 C22 1.399(7) . ?
C21 Al1 2.015(5) 2_655 ?
C22 C23 1.378(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.370(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.368(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
N3 C35 1.359(6) . ?
N3 C31 1.363(6) . ?
C31 C32 1.401(7) . ?
C31 Al1 2.016(5) 2_655 ?
C32 C33 1.379(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.376(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.374(7) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C41 C42 1.372(7) . ?
C41 C43' 1.414(11) 2_756 ?
C41 C43 1.414(11) 2_756 ?
C41 H41 0.9500 . ?
C42 C43 1.376(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.414(17) . ?
C43 C41 1.414(11) 2_756 ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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 Mn1 N3 180.00(19) . 2_655 ?
N3 Mn1 N2 89.38(13) . 2_655 ?
N3 Mn1 N2 90.62(13) 2_655 2_655 ?
N3 Mn1 N2 90.62(13) . . ?
N3 Mn1 N2 89.38(13) 2_655 . ?
N2 Mn1 N2 180.0(2) 2_655 . ?
N3 Mn1 N1 89.52(13) . . ?
N3 Mn1 N1 90.48(13) 2_655 . ?
N2 Mn1 N1 90.85(13) 2_655 . ?
N2 Mn1 N1 89.15(13) . . ?
N3 Mn1 N1 90.48(13) . 2_655 ?
N3 Mn1 N1 89.52(13) 2_655 2_655 ?
N2 Mn1 N1 89.15(13) 2_655 2_655 ?
N2 Mn1 N1 90.85(13) . 2_655 ?
N1 Mn1 N1 180.0(3) . 2_655 ?
C1 Al1 C21 113.5(3) . 2_655 ?
C1 Al1 C11 112.6(3) . . ?
C21 Al1 C11 105.25(18) 2_655 . ?
C1 Al1 C31 117.5(3) . 2_655 ?
C21 Al1 C31 103.98(18) 2_655 2_655 ?
C11 Al1 C31 102.63(18) . 2_655 ?
C3 C1 C2 112.6(8) . . ?
C3 C1 Al1 124.5(7) . . ?
C2 C1 Al1 111.1(7) . . ?
C3 C1 H1 101.5 . . ?
C2 C1 H1 101.5 . . ?
Al1 C1 H1 101.5 . . ?
C1 C3 C4 116.0(9) . . ?
C1 C3 H3A 108.3 . . ?
C4 C3 H3A 108.3 . . ?
C1 C3 H3B 108.3 . . ?
C4 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
H2'A C2' H2'B 109.5 . . ?
H2'A C2' H2'C 109.5 . . ?
H2'B C2' H2'C 109.5 . . ?
C4' C3' H3'A 107.6 . . ?
C4' C3' H3'B 107.6 . . ?
H3'A C3' H3'B 107.0 . . ?
C3' C4' H4'A 109.5 . . ?
C3' C4' H4'B 109.5 . . ?
H4'A C4' H4'B 109.5 . . ?
C3' C4' H4'C 109.5 . . ?
H4'A C4' H4'C 109.5 . . ?
H4'B C4' H4'C 109.5 . . ?
C15 N1 C11 119.3(4) . . ?
C15 N1 Mn1 118.2(3) . . ?
C11 N1 Mn1 122.2(3) . . ?
N1 C11 C12 118.4(4) . . ?
N1 C11 Al1 116.7(3) . . ?
C12 C11 Al1 124.9(4) . . ?
C13 C12 C11 121.6(5) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C14 118.9(5) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 118.1(5) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
N1 C15 C14 123.7(5) . . ?
N1 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
C25 N2 C21 118.9(4) . . ?
C25 N2 Mn1 118.8(3) . . ?
C21 N2 Mn1 122.2(3) . . ?
N2 C21 C22 118.0(4) . . ?
N2 C21 Al1 117.2(3) . 2_655 ?
C22 C21 Al1 124.8(3) . 2_655 ?
C23 C22 C21 122.3(5) . . ?
C23 C22 H22 118.9 . . ?
C21 C22 H22 118.9 . . ?
C24 C23 C22 118.4(5) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C25 C24 C23 118.4(5) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
N2 C25 C24 124.1(5) . . ?
N2 C25 H25 118.0 . . ?
C24 C25 H25 118.0 . . ?
C35 N3 C31 119.4(4) . . ?
C35 N3 Mn1 117.5(3) . . ?
C31 N3 Mn1 123.1(3) . . ?
N3 C31 C32 118.3(4) . . ?
N3 C31 Al1 116.4(3) . 2_655 ?
C32 C31 Al1 125.3(3) . 2_655 ?
C33 C32 C31 121.8(5) . . ?
C33 C32 H32 119.1 . . ?
C31 C32 H32 119.1 . . ?
C34 C33 C32 118.8(5) . . ?
C34 C33 H33 120.6 . . ?
C32 C33 H33 120.6 . . ?
C35 C34 C33 118.5(5) . . ?
C35 C34 H34 120.8 . . ?
C33 C34 H34 120.8 . . ?
N3 C35 C34 123.2(4) . . ?
N3 C35 H35 118.4 . . ?
C34 C35 H35 118.4 . . ?
C42 C41 C43' 121.8(8) . 2_756 ?
C42 C41 C43 121.8(8) . 2_756 ?
C43' C41 C43 0.0(11) 2_756 2_756 ?
C42 C41 H41 119.1 . . ?
C43' C41 H41 119.1 2_756 . ?
C43 C41 H41 119.1 2_756 . ?
C41 C42 C43 122.0(8) . . ?
C41 C42 H42 119.0 . . ?
C43 C42 H42 119.0 . . ?
C42 C43 C44 118.2(10) . . ?
C42 C43 C41 116.1(7) . 2_756 ?
C44 C43 C41 125.6(10) . 2_756 ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        24.12
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 993336'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw0855

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H42 Al2 Fe N6'
_chemical_formula_sum            'C38 H42 Al2 Fe N6'
_chemical_formula_weight         692.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R3
_symmetry_space_group_name_Hall  'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   12.432(2)
_cell_length_b                   12.432(2)
_cell_length_c                   19.172(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2566.0(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    19889
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 The molecule lies on the triad axis (0,0,z) in space group R3.  The
 structure is perhaps best viewed as totally disordered (spinning) about
 this triad axis, a situation which presents several challenging problems
 for the refinement (see _refine_special_details).

 Note! IUCr CHECKCIF (March 2014) miss-calculates the sum formula due (?)
 to rounding errors (many atoms have site multiplicity 0.3333333).
 SHELX gets it right: the information in _chemical_formula_sum is that
 calculated by SHELXL.
;

_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            6085
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.93
_diffrn_reflns_theta_max         27.46
_reflns_number_total             1957
_reflns_number_gt                1703
_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.

 Refined as a racemic twin with final BASF=0.41.  Stenuous attempts to
 refine the structure in a higher symmetry rhombohedral group were 
 unsuccessful.

 The two -nBu groups are very poorly resolved, modelled as disordered
 about a triad axis with bond length restraints and common isotropic
 displacement parameters for the carbon atoms.  Anisotropic
 displacement parameters were assigned to the Al and Fe atoms only, common
 isotropic displacement parameters were assigned to the C and N atoms of
 the C5H4N rings.  
;

_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   0.47(9)
_refine_ls_number_reflns         1957
_refine_ls_number_parameters     52
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.1381
_refine_ls_wR_factor_ref         0.4458
_refine_ls_wR_factor_gt          0.4168
_refine_ls_goodness_of_fit_ref   2.112
_refine_ls_restrained_S_all      2.105
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.0000 0.0000 0.2774(4) 0.0470(7) Uani 1 3 d S . .
Al1 Al 1.0000 0.0000 0.1095(3) 0.064(2) Uani 1 3 d SD . .
Al2 Al 1.0000 0.0000 0.4456(3) 0.0558(18) Uani 1 3 d SD . .
N1 N 1.0002(7) -0.1401(6) 0.2198(5) 0.0620(13) Uiso 1 1 d G . .
C11 C 0.9989(8) -0.1331(7) 0.1475(5) 0.0509(10) Uiso 1 1 d G A .
C12 C 0.9990(8) -0.2259(8) 0.1070(5) 0.0662(13) Uiso 1 1 d G A .
H12 H 0.9981 -0.2211 0.0576 0.079 Uiso 1 1 calc R . .
C13 C 1.0004(7) -0.3256(7) 0.1389(5) 0.077(2) Uiso 1 1 d G A .
H13 H 1.0005 -0.3890 0.1113 0.092 Uiso 1 1 calc R . .
C14 C 1.0017(8) -0.3325(6) 0.2112(5) 0.0662(13) Uiso 1 1 d G A .
H14 H 1.0027 -0.4007 0.2330 0.079 Uiso 1 1 calc R . .
C15 C 1.0016(8) -0.2398(7) 0.2517(5) 0.0509(10) Uiso 1 1 d G A .
H15 H 1.0025 -0.2446 0.3011 0.061 Uiso 1 1 calc R . .
N2 N 1.1368(6) -0.0037(7) 0.3319(5) 0.0620(13) Uiso 1 1 d G . .
C21 C 1.1390(6) 0.0029(8) 0.4043(5) 0.0509(10) Uiso 1 1 d G A .
C22 C 1.2355(7) 0.0035(8) 0.4412(5) 0.0662(13) Uiso 1 1 d G A .
H22 H 1.2370 0.0080 0.4907 0.079 Uiso 1 1 calc R . .
C23 C 1.3299(6) -0.0024(8) 0.4058(5) 0.077(2) Uiso 1 1 d G A .
H23 H 1.3959 -0.0020 0.4310 0.092 Uiso 1 1 calc R . .
C24 C 1.3278(6) -0.0089(9) 0.3333(5) 0.0662(13) Uiso 1 1 d G A .
H24 H 1.3923 -0.0130 0.3091 0.079 Uiso 1 1 calc R . .
C25 C 1.2312(7) -0.0096(8) 0.2964(5) 0.0509(10) Uiso 1 1 d G A .
H25 H 1.2298 -0.0140 0.2470 0.061 Uiso 1 1 calc R . .
C1 C 1.0000 0.0000 0.0116(5) 0.126(4) Uiso 1 3 d SD A -1
H1A H 1.0641 -0.0223 0.0002 0.151 Uiso 0.33 1 calc PR A -1
H1B H 0.9199 -0.0750 0.0002 0.151 Uiso 0.33 1 calc PR A -1
C2 C 1.015(5) 0.091(2) -0.0480(6) 0.126(4) Uiso 0.33 1 d PD A -1
H2A H 1.0982 0.1660 -0.0453 0.151 Uiso 0.33 1 calc PR A -1
H2B H 0.9518 0.1166 -0.0430 0.151 Uiso 0.33 1 calc PR A -1
C3 C 0.999(5) 0.026(4) -0.1193(5) 0.126(4) Uiso 0.33 1 d PD A -1
H3A H 1.0767 0.0267 -0.1319 0.151 Uiso 0.33 1 calc PR A -1
H3B H 0.9315 -0.0621 -0.1161 0.151 Uiso 0.33 1 calc PR A -1
C4 C 0.967(7) 0.094(6) -0.1759(11) 0.126(4) Uiso 0.33 1 d PD A -1
H4A H 0.9777 0.0675 -0.2222 0.189 Uiso 0.33 1 calc PR A -1
H4B H 1.0223 0.1839 -0.1711 0.189 Uiso 0.33 1 calc PR A -1
H4C H 0.8806 0.0743 -0.1702 0.189 Uiso 0.33 1 calc PR A -1
C5 C 1.0000 0.0000 0.5434(7) 0.126(4) Uiso 1 3 d SD B -1
H5A H 0.9105 -0.0465 0.5551 0.151 Uiso 0.33 1 calc PR B -1
H5B H 1.0314 -0.0570 0.5551 0.151 Uiso 0.33 1 calc PR B -1
C6 C 1.056(3) 0.099(2) 0.6018(10) 0.126(4) Uiso 0.33 1 d PD B -1
H6A H 1.0072 0.1423 0.6061 0.151 Uiso 0.33 1 calc PR B -1
H6B H 1.1425 0.1620 0.5899 0.151 Uiso 0.33 1 calc PR B -1
C7 C 1.053(2) 0.036(4) 0.6718(6) 0.126(4) Uiso 0.33 1 d PD B -1
H7A H 0.9693 -0.0368 0.6795 0.151 Uiso 0.33 1 calc PR B -1
H7B H 1.0717 0.0947 0.7108 0.151 Uiso 0.33 1 calc PR B -1
C8 C 1.151(6) -0.007(6) 0.670(2) 0.126(4) Uiso 0.33 1 d PD B -1
H8A H 1.1554 -0.0390 0.7158 0.189 Uiso 0.33 1 calc PR B -1
H8B H 1.2321 0.0637 0.6578 0.189 Uiso 0.33 1 calc PR B -1
H8C H 1.1265 -0.0724 0.6348 0.189 Uiso 0.33 1 calc PR B -1


_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
Fe1 N2 2.017(6) 2_645 ?
Fe1 N2 2.017(6) . ?
Fe1 N2 2.017(6) 3_765 ?
Fe1 N1 2.063(6) 2_645 ?
Fe1 N1 2.063(6) . ?
Fe1 N1 2.063(6) 3_765 ?
Al1 C11 1.802(9) 2_645 ?
Al1 C11 1.802(6) . ?
Al1 C11 1.802(9) 3_765 ?
Al1 C1 1.876(11) . ?
Al2 C5 1.876(11) . ?
Al2 C21 1.884(9) 3_765 ?
Al2 C21 1.884(10) 2_645 ?
Al2 C21 1.884(6) . ?
N1 C11 1.3900 . ?
N1 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 H12 0.9500 . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N2 C21 1.3900 . ?
N2 C25 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22 0.9500 . ?
C23 C24 1.3900 . ?
C23 H23 0.9500 . ?
C24 C25 1.3900 . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C1 C2 1.5498(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.5501(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.5500(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.5499(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.5501(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.5501(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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
N2 Fe1 N2 95.5(2) 2_645 . ?
N2 Fe1 N2 95.5(2) 2_645 3_765 ?
N2 Fe1 N2 95.5(2) . 3_765 ?
N2 Fe1 N1 84.3(3) 2_645 2_645 ?
N2 Fe1 N1 86.1(3) . 2_645 ?
N2 Fe1 N1 178.4(3) 3_765 2_645 ?
N2 Fe1 N1 178.4(3) 2_645 . ?
N2 Fe1 N1 84.3(3) . . ?
N2 Fe1 N1 86.1(3) 3_765 . ?
N1 Fe1 N1 94.0(2) 2_645 . ?
N2 Fe1 N1 86.1(3) 2_645 3_765 ?
N2 Fe1 N1 178.4(3) . 3_765 ?
N2 Fe1 N1 84.3(3) 3_765 3_765 ?
N1 Fe1 N1 94.0(2) 2_645 3_765 ?
N1 Fe1 N1 94.0(2) . 3_765 ?
C11 Al1 C11 104.8(5) 2_645 . ?
C11 Al1 C11 104.8(5) 2_645 3_765 ?
C11 Al1 C11 104.8(6) . 3_765 ?
C11 Al1 C1 113.8(5) 2_645 . ?
C11 Al1 C1 113.8(3) . . ?
C11 Al1 C1 113.8(5) 3_765 . ?
C5 Al2 C21 114.8(5) . 3_765 ?
C5 Al2 C21 114.8(5) . 2_645 ?
C21 Al2 C21 103.6(5) 3_765 2_645 ?
C5 Al2 C21 114.8(3) . . ?
C21 Al2 C21 103.6(5) 3_765 . ?
C21 Al2 C21 103.6(5) 2_645 . ?
C11 N1 C15 120.0 . . ?
C11 N1 Fe1 118.5(3) . . ?
C15 N1 Fe1 121.5(3) . . ?
N1 C11 C12 120.0 . . ?
N1 C11 Al1 117.7(4) . . ?
C12 C11 Al1 122.3(4) . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 N1 120.0 . . ?
C14 C15 H15 120.0 . . ?
N1 C15 H15 120.0 . . ?
C21 N2 C25 120.0 . . ?
C21 N2 Fe1 120.6(3) . . ?
C25 N2 Fe1 119.4(3) . . ?
N2 C21 C22 120.0 . . ?
N2 C21 Al2 115.3(4) . . ?
C22 C21 Al2 124.6(4) . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 N2 120.0 . . ?
C24 C25 H25 120.0 . . ?
N2 C25 H25 120.0 . . ?
C2 C1 Al1 137.5(8) . . ?
C2 C1 H1A 102.8 . . ?
Al1 C1 H1A 102.8 . . ?
C2 C1 H1B 102.8 . . ?
Al1 C1 H1B 102.8 . . ?
H1A C1 H1B 105.0 . . ?
C1 C2 C3 109.40(10) . . ?
C1 C2 H2A 109.8 . . ?
C3 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
C3 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C2 109.39(10) . . ?
C4 C3 H3A 109.8 . . ?
C2 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 Al2 136.2(11) . . ?
C6 C5 H5A 103.1 . . ?
Al2 C5 H5A 103.1 . . ?
C6 C5 H5B 103.1 . . ?
Al2 C5 H5B 103.1 . . ?
H5A C5 H5B 105.1 . . ?
C5 C6 C7 109.39(10) . . ?
C5 C6 H6A 109.8 . . ?
C7 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
C7 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
C6 C7 C8 109.38(10) . . ?
C6 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
C6 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.264
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.169
_database_code_depnum_ccdc_archive 'CCDC 993337'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw0861

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H42 Al2 Ca N6'
_chemical_formula_sum            'C38 H42 Al2 Ca N6'
_chemical_formula_weight         676.82

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'
Ca Ca 0.2262 0.3064 '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)/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.2800(8)
_cell_length_b                   10.297(1)
_cell_length_c                   18.271(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.983(3)
_cell_angle_gamma                90.00
_cell_volume                     1884.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    122487
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      32.03

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             716
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_T_max  0.982
_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            9723
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.58
_diffrn_reflns_theta_max         32.25
_reflns_number_total             5475
_reflns_number_gt                4059
_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. 
;

_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)+(0.0501P)²+0.9673P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5475
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1382
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_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
Ca1 Ca 1.0000 0.0000 1.0000 0.02429(12) Uani 1 2 d S . .
Al1 Al 0.75257(6) -0.20237(5) 0.88315(3) 0.02813(14) Uani 1 1 d . . .
N1 N 0.99818(16) -0.06822(17) 0.86952(9) 0.0328(4) Uani 1 1 d . . .
N2 N 0.94111(16) -0.22593(15) 1.02757(9) 0.0310(3) Uani 1 1 d . . .
N3 N 0.75941(15) 0.04837(16) 0.96051(9) 0.0313(3) Uani 1 1 d . . .
C21 C 0.84543(18) -0.29265(18) 0.97818(10) 0.0277(4) Uani 1 1 d . . .
C11 C 0.90039(19) -0.14843(18) 0.83181(10) 0.0295(4) Uani 1 1 d . . .
C32 C 0.53989(19) -0.0044(2) 0.89819(11) 0.0333(4) Uani 1 1 d . . .
H32 H 0.4787 -0.0619 0.8674 0.040 Uiso 1 1 calc R . .
C31 C 0.67533(18) -0.03684(18) 0.91637(10) 0.0286(4) Uani 1 1 d . . .
C35 C 0.71097(19) 0.15841(19) 0.98440(11) 0.0342(4) Uani 1 1 d . . .
H35 H 0.7729 0.2154 1.0151 0.041 Uiso 1 1 calc R . .
C25 C 1.00676(19) -0.28427(19) 1.09050(10) 0.0325(4) Uani 1 1 d . . .
H25 H 1.0727 -0.2351 1.1239 0.039 Uiso 1 1 calc R . .
C34 C 0.57829(19) 0.19449(19) 0.96768(11) 0.0317(4) Uani 1 1 d . . .
C24 C 0.98574(19) -0.41087(19) 1.11062(10) 0.0301(4) Uani 1 1 d . . .
C15 C 1.0975(2) -0.0300(2) 0.83669(11) 0.0393(5) Uani 1 1 d . . .
H15 H 1.1632 0.0270 0.8644 0.047 Uiso 1 1 calc R . .
C22 C 0.82017(19) -0.42143(19) 0.99671(11) 0.0316(4) Uani 1 1 d . . .
H22 H 0.7535 -0.4696 0.9632 0.038 Uiso 1 1 calc R . .
C26 C 1.0665(2) -0.4713(2) 1.18089(12) 0.0414(5) Uani 1 1 d . . .
H26A H 1.1299 -0.4073 1.2081 0.062 Uiso 1 1 calc R . .
H26B H 1.1156 -0.5461 1.1678 0.062 Uiso 1 1 calc R . .
H26C H 1.0069 -0.4999 1.2127 0.062 Uiso 1 1 calc R . .
C12 C 0.9104(2) -0.1897(2) 0.75968(10) 0.0357(4) Uani 1 1 d . . .
H12 H 0.8442 -0.2464 0.7322 0.043 Uiso 1 1 calc R . .
C1 C 0.6148(2) -0.3126(2) 0.82034(12) 0.0403(5) Uani 1 1 d . . .
H1A H 0.5721 -0.2652 0.7748 0.061 Uiso 1 1 calc R . .
H1B H 0.5475 -0.3356 0.8485 0.061 Uiso 1 1 calc R . .
H1C H 0.6562 -0.3919 0.8065 0.061 Uiso 1 1 calc R . .
C14 C 1.1110(2) -0.0673(2) 0.76582(11) 0.0418(5) Uani 1 1 d . . .
C36 C 0.5320(2) 0.3190(2) 0.99728(14) 0.0458(5) Uani 1 1 d . . .
H36A H 0.6092 0.3654 1.0272 0.069 Uiso 1 1 calc R . .
H36B H 0.4691 0.2988 1.0288 0.069 Uiso 1 1 calc R . .
H36C H 0.4878 0.3736 0.9551 0.069 Uiso 1 1 calc R . .
C33 C 0.49172(19) 0.1091(2) 0.92360(11) 0.0358(4) Uani 1 1 d . . .
H33 H 0.3989 0.1277 0.9105 0.043 Uiso 1 1 calc R . .
C23 C 0.8886(2) -0.47987(19) 1.06163(11) 0.0332(4) Uani 1 1 d . . .
H23 H 0.8692 -0.5669 1.0726 0.040 Uiso 1 1 calc R . .
C13 C 1.0143(2) -0.1499(2) 0.72740(11) 0.0417(5) Uani 1 1 d . . .
H13 H 1.0184 -0.1799 0.6788 0.050 Uiso 1 1 calc R . .
C16 C 1.2234(3) -0.0162(4) 0.73217(15) 0.0667(8) Uani 1 1 d . . .
H16A H 1.2809 0.0412 0.7684 0.100 Uiso 1 1 calc R . .
H16B H 1.1857 0.0324 0.6862 0.100 Uiso 1 1 calc R . .
H16C H 1.2762 -0.0893 0.7202 0.100 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
Ca1 N3 2.4665(15) 3_757 ?
Ca1 N3 2.4665(15) . ?
Ca1 N1 2.4814(15) . ?
Ca1 N1 2.4814(15) 3_757 ?
Ca1 N2 2.4838(16) 3_757 ?
Ca1 N2 2.4838(16) . ?
Ca1 Al1 3.5959(6) 3_757 ?
Ca1 Al1 3.5959(6) . ?
Al1 C1 1.970(2) . ?
Al1 C21 2.0114(19) . ?
Al1 C31 2.030(2) . ?
Al1 C11 2.034(2) . ?
N1 C15 1.354(3) . ?
N1 C11 1.362(2) . ?
N2 C25 1.338(2) . ?
N2 C21 1.362(2) . ?
N3 C35 1.349(2) . ?
N3 C31 1.362(2) . ?
C21 C22 1.407(3) . ?
C11 C12 1.410(3) . ?
C32 C33 1.389(3) . ?
C32 C31 1.397(3) . ?
C32 H32 0.9500 . ?
C35 C34 1.380(3) . ?
C35 H35 0.9500 . ?
C25 C24 1.385(3) . ?
C25 H25 0.9500 . ?
C34 C33 1.375(3) . ?
C34 C36 1.509(3) . ?
C24 C23 1.379(3) . ?
C24 C26 1.498(3) . ?
C15 C14 1.387(3) . ?
C15 H15 0.9500 . ?
C22 C23 1.374(3) . ?
C22 H22 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C12 C13 1.392(3) . ?
C12 H12 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C14 C13 1.375(3) . ?
C14 C16 1.520(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C33 H33 0.9500 . ?
C23 H23 0.9500 . ?
C13 H13 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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 Ca1 N3 180.000(1) 3_757 . ?
N3 Ca1 N1 90.83(5) 3_757 . ?
N3 Ca1 N1 89.17(5) . . ?
N3 Ca1 N1 89.17(5) 3_757 3_757 ?
N3 Ca1 N1 90.83(5) . 3_757 ?
N1 Ca1 N1 180.000(1) . 3_757 ?
N3 Ca1 N2 88.53(5) 3_757 3_757 ?
N3 Ca1 N2 91.47(5) . 3_757 ?
N1 Ca1 N2 91.14(5) . 3_757 ?
N1 Ca1 N2 88.86(5) 3_757 3_757 ?
N3 Ca1 N2 91.47(5) 3_757 . ?
N3 Ca1 N2 88.53(5) . . ?
N1 Ca1 N2 88.86(5) . . ?
N1 Ca1 N2 91.14(5) 3_757 . ?
N2 Ca1 N2 180.0 3_757 . ?
N3 Ca1 Al1 54.15(4) 3_757 3_757 ?
N3 Ca1 Al1 125.85(4) . 3_757 ?
N1 Ca1 Al1 125.88(4) . 3_757 ?
N1 Ca1 Al1 54.12(4) 3_757 3_757 ?
N2 Ca1 Al1 53.52(4) 3_757 3_757 ?
N2 Ca1 Al1 126.48(4) . 3_757 ?
N3 Ca1 Al1 125.85(4) 3_757 . ?
N3 Ca1 Al1 54.15(4) . . ?
N1 Ca1 Al1 54.12(4) . . ?
N1 Ca1 Al1 125.88(4) 3_757 . ?
N2 Ca1 Al1 126.48(4) 3_757 . ?
N2 Ca1 Al1 53.52(4) . . ?
Al1 Ca1 Al1 180.0 3_757 . ?
C1 Al1 C21 112.10(9) . . ?
C1 Al1 C31 112.31(9) . . ?
C21 Al1 C31 105.76(7) . . ?
C1 Al1 C11 113.74(9) . . ?
C21 Al1 C11 105.39(8) . . ?
C31 Al1 C11 106.95(8) . . ?
C1 Al1 Ca1 178.96(7) . . ?
C21 Al1 Ca1 67.67(5) . . ?
C31 Al1 Ca1 66.92(5) . . ?
C11 Al1 Ca1 67.26(5) . . ?
C15 N1 C11 119.78(17) . . ?
C15 N1 Ca1 119.97(13) . . ?
C11 N1 Ca1 120.20(12) . . ?
C25 N2 C21 119.52(17) . . ?
C25 N2 Ca1 119.74(12) . . ?
C21 N2 Ca1 120.72(12) . . ?
C35 N3 C31 120.10(16) . . ?
C35 N3 Ca1 119.58(12) . . ?
C31 N3 Ca1 120.30(12) . . ?
N2 C21 C22 117.44(16) . . ?
N2 C21 Al1 118.09(13) . . ?
C22 C21 Al1 124.46(14) . . ?
N1 C11 C12 117.03(17) . . ?
N1 C11 Al1 118.36(13) . . ?
C12 C11 Al1 124.60(15) . . ?
C33 C32 C31 122.18(18) . . ?
C33 C32 H32 118.9 . . ?
C31 C32 H32 118.9 . . ?
N3 C31 C32 116.92(17) . . ?
N3 C31 Al1 118.64(13) . . ?
C32 C31 Al1 124.43(14) . . ?
N3 C35 C34 124.94(18) . . ?
N3 C35 H35 117.5 . . ?
C34 C35 H35 117.5 . . ?
N2 C25 C24 124.91(18) . . ?
N2 C25 H25 117.5 . . ?
C24 C25 H25 117.5 . . ?
C33 C34 C35 115.77(18) . . ?
C33 C34 C36 122.58(18) . . ?
C35 C34 C36 121.64(19) . . ?
C23 C24 C25 116.50(17) . . ?
C23 C24 C26 121.56(18) . . ?
C25 C24 C26 121.92(18) . . ?
N1 C15 C14 125.2(2) . . ?
N1 C15 H15 117.4 . . ?
C14 C15 H15 117.4 . . ?
C23 C22 C21 122.27(18) . . ?
C23 C22 H22 118.9 . . ?
C21 C22 H22 118.9 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C13 C12 C11 122.10(19) . . ?
C13 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C14 C15 115.8(2) . . ?
C13 C14 C16 122.4(2) . . ?
C15 C14 C16 121.8(2) . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C33 C32 120.08(17) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C22 C23 C24 119.35(18) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C14 C13 C12 120.06(18) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Ca1 Al1 C1 137(4) 3_757 . . . ?
N3 Ca1 Al1 C1 -43(4) . . . . ?
N1 Ca1 Al1 C1 -163(4) . . . . ?
N1 Ca1 Al1 C1 17(4) 3_757 . . . ?
N2 Ca1 Al1 C1 -103(4) 3_757 . . . ?
N2 Ca1 Al1 C1 77(4) . . . . ?
Al1 Ca1 Al1 C1 29(100) 3_757 . . . ?
N3 Ca1 Al1 C21 60.12(7) 3_757 . . . ?
N3 Ca1 Al1 C21 -119.88(7) . . . . ?
N1 Ca1 Al1 C21 120.07(7) . . . . ?
N1 Ca1 Al1 C21 -59.93(7) 3_757 . . . ?
N2 Ca1 Al1 C21 179.78(7) 3_757 . . . ?
N2 Ca1 Al1 C21 -0.22(7) . . . . ?
Al1 Ca1 Al1 C21 -49(100) 3_757 . . . ?
N3 Ca1 Al1 C31 179.74(7) 3_757 . . . ?
N3 Ca1 Al1 C31 -0.26(7) . . . . ?
N1 Ca1 Al1 C31 -120.31(8) . . . . ?
N1 Ca1 Al1 C31 59.69(8) 3_757 . . . ?
N2 Ca1 Al1 C31 -60.60(7) 3_757 . . . ?
N2 Ca1 Al1 C31 119.40(7) . . . . ?
Al1 Ca1 Al1 C31 71(100) 3_757 . . . ?
N3 Ca1 Al1 C11 -58.78(8) 3_757 . . . ?
N3 Ca1 Al1 C11 121.22(8) . . . . ?
N1 Ca1 Al1 C11 1.17(7) . . . . ?
N1 Ca1 Al1 C11 -178.83(7) 3_757 . . . ?
N2 Ca1 Al1 C11 60.89(7) 3_757 . . . ?
N2 Ca1 Al1 C11 -119.11(7) . . . . ?
Al1 Ca1 Al1 C11 -168(100) 3_757 . . . ?
N3 Ca1 N1 C15 -43.77(16) 3_757 . . . ?
N3 Ca1 N1 C15 136.23(16) . . . . ?
N1 Ca1 N1 C15 163(100) 3_757 . . . ?
N2 Ca1 N1 C15 44.78(16) 3_757 . . . ?
N2 Ca1 N1 C15 -135.22(16) . . . . ?
Al1 Ca1 N1 C15 0.80(18) 3_757 . . . ?
Al1 Ca1 N1 C15 -179.20(18) . . . . ?
N3 Ca1 N1 C11 133.57(14) 3_757 . . . ?
N3 Ca1 N1 C11 -46.43(14) . . . . ?
N1 Ca1 N1 C11 -20(100) 3_757 . . . ?
N2 Ca1 N1 C11 -137.88(14) 3_757 . . . ?
N2 Ca1 N1 C11 42.12(14) . . . . ?
Al1 Ca1 N1 C11 178.13(12) 3_757 . . . ?
Al1 Ca1 N1 C11 -1.87(12) . . . . ?
N3 Ca1 N2 C25 43.10(15) 3_757 . . . ?
N3 Ca1 N2 C25 -136.90(15) . . . . ?
N1 Ca1 N2 C25 133.90(15) . . . . ?
N1 Ca1 N2 C25 -46.10(15) 3_757 . . . ?
N2 Ca1 N2 C25 -133(100) 3_757 . . . ?
Al1 Ca1 N2 C25 -1.69(16) 3_757 . . . ?
Al1 Ca1 N2 C25 178.31(16) . . . . ?
N3 Ca1 N2 C21 -134.87(14) 3_757 . . . ?
N3 Ca1 N2 C21 45.13(14) . . . . ?
N1 Ca1 N2 C21 -44.07(14) . . . . ?
N1 Ca1 N2 C21 135.93(14) 3_757 . . . ?
N2 Ca1 N2 C21 49(100) 3_757 . . . ?
Al1 Ca1 N2 C21 -179.66(12) 3_757 . . . ?
Al1 Ca1 N2 C21 0.34(12) . . . . ?
N3 Ca1 N3 C35 80(100) 3_757 . . . ?
N1 Ca1 N3 C35 -136.63(15) . . . . ?
N1 Ca1 N3 C35 43.37(15) 3_757 . . . ?
N2 Ca1 N3 C35 -45.51(15) 3_757 . . . ?
N2 Ca1 N3 C35 134.49(15) . . . . ?
Al1 Ca1 N3 C35 -1.17(17) 3_757 . . . ?
Al1 Ca1 N3 C35 178.83(17) . . . . ?
N3 Ca1 N3 C31 -99(100) 3_757 . . . ?
N1 Ca1 N3 C31 44.96(14) . . . . ?
N1 Ca1 N3 C31 -135.04(14) 3_757 . . . ?
N2 Ca1 N3 C31 136.08(14) 3_757 . . . ?
N2 Ca1 N3 C31 -43.92(14) . . . . ?
Al1 Ca1 N3 C31 -179.58(12) 3_757 . . . ?
Al1 Ca1 N3 C31 0.42(12) . . . . ?
C25 N2 C21 C22 0.3(3) . . . . ?
Ca1 N2 C21 C22 178.27(13) . . . . ?
C25 N2 C21 Al1 -178.53(14) . . . . ?
Ca1 N2 C21 Al1 -0.56(19) . . . . ?
C1 Al1 C21 N2 -178.55(14) . . . . ?
C31 Al1 C21 N2 -55.84(15) . . . . ?
C11 Al1 C21 N2 57.23(15) . . . . ?
Ca1 Al1 C21 N2 0.36(12) . . . . ?
C1 Al1 C21 C22 2.72(19) . . . . ?
C31 Al1 C21 C22 125.43(16) . . . . ?
C11 Al1 C21 C22 -121.50(16) . . . . ?
Ca1 Al1 C21 C22 -178.38(17) . . . . ?
C15 N1 C11 C12 1.2(3) . . . . ?
Ca1 N1 C11 C12 -176.11(13) . . . . ?
C15 N1 C11 Al1 -179.62(15) . . . . ?
Ca1 N1 C11 Al1 3.04(19) . . . . ?
C1 Al1 C11 N1 177.72(14) . . . . ?
C21 Al1 C11 N1 -59.10(16) . . . . ?
C31 Al1 C11 N1 53.13(16) . . . . ?
Ca1 Al1 C11 N1 -1.97(12) . . . . ?
C1 Al1 C11 C12 -3.2(2) . . . . ?
C21 Al1 C11 C12 119.98(16) . . . . ?
C31 Al1 C11 C12 -127.78(16) . . . . ?
Ca1 Al1 C11 C12 177.12(18) . . . . ?
C35 N3 C31 C32 -0.2(3) . . . . ?
Ca1 N3 C31 C32 178.16(13) . . . . ?
C35 N3 C31 Al1 -179.09(14) . . . . ?
Ca1 N3 C31 Al1 -0.69(19) . . . . ?
C33 C32 C31 N3 -0.1(3) . . . . ?
C33 C32 C31 Al1 178.71(15) . . . . ?
C1 Al1 C31 N3 179.68(14) . . . . ?
C21 Al1 C31 N3 57.11(16) . . . . ?
C11 Al1 C31 N3 -54.87(16) . . . . ?
Ca1 Al1 C31 N3 0.44(12) . . . . ?
C1 Al1 C31 C32 0.93(19) . . . . ?
C21 Al1 C31 C32 -121.64(16) . . . . ?
C11 Al1 C31 C32 126.38(16) . . . . ?
Ca1 Al1 C31 C32 -178.31(18) . . . . ?
C31 N3 C35 C34 0.1(3) . . . . ?
Ca1 N3 C35 C34 -178.35(16) . . . . ?
C21 N2 C25 C24 0.2(3) . . . . ?
Ca1 N2 C25 C24 -177.83(15) . . . . ?
N3 C35 C34 C33 0.4(3) . . . . ?
N3 C35 C34 C36 179.5(2) . . . . ?
N2 C25 C24 C23 -0.6(3) . . . . ?
N2 C25 C24 C26 177.86(19) . . . . ?
C11 N1 C15 C14 -0.9(3) . . . . ?
Ca1 N1 C15 C14 176.47(17) . . . . ?
N2 C21 C22 C23 -0.3(3) . . . . ?
Al1 C21 C22 C23 178.43(15) . . . . ?
N1 C11 C12 C13 -0.7(3) . . . . ?
Al1 C11 C12 C13 -179.75(16) . . . . ?
N1 C15 C14 C13 -0.1(3) . . . . ?
N1 C15 C14 C16 178.0(2) . . . . ?
C35 C34 C33 C32 -0.7(3) . . . . ?
C36 C34 C33 C32 -179.73(19) . . . . ?
C31 C32 C33 C34 0.6(3) . . . . ?
C21 C22 C23 C24 -0.1(3) . . . . ?
C25 C24 C23 C22 0.6(3) . . . . ?
C26 C24 C23 C22 -177.91(19) . . . . ?
C15 C14 C13 C12 0.7(3) . . . . ?
C16 C14 C13 C12 -177.4(2) . . . . ?
C11 C12 C13 C14 -0.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.817
_diffrn_reflns_theta_full        32.25
_diffrn_measured_fraction_theta_full 0.817
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 993338'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw1420

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H31 Al Li N3 O'
_chemical_formula_sum            'C24 H31 Al Li N3 O'
_chemical_formula_weight         411.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 '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)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.7216(3)
_cell_length_b                   16.9280(5)
_cell_length_c                   13.0438(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.930(1)
_cell_angle_gamma                90.00
_cell_volume                     2324.44(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9881
_cell_measurement_theta_min      4.20
_cell_measurement_theta_max      72.05

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            19156
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.20
_diffrn_reflns_theta_max         72.05
_reflns_number_total             4463
_reflns_number_gt                4033
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_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. 
;

_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+0.8818P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4463
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.1008
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.006
_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 0.80247(4) 0.51957(2) 0.28252(3) 0.02826(12) Uani 1 1 d . . .
Li1 Li 0.8427(2) 0.39228(13) 0.12887(17) 0.0311(5) Uani 1 1 d . . .
N1 N 0.72758(10) 0.48966(6) 0.06004(8) 0.0286(2) Uani 1 1 d . . .
N2 N 0.72124(10) 0.35835(6) 0.22957(8) 0.0274(2) Uani 1 1 d . . .
N3 N 1.01256(10) 0.42377(6) 0.23795(8) 0.0285(2) Uani 1 1 d . . .
C1 C 0.78900(15) 0.60415(8) 0.38515(11) 0.0389(3) Uani 1 1 d . . .
H1A H 0.8357 0.5861 0.4540 0.047 Uiso 1 1 calc R . .
H1B H 0.8345 0.6510 0.3655 0.047 Uiso 1 1 calc R . .
C2 C 0.65782(19) 0.63139(11) 0.39959(15) 0.0595(5) Uani 1 1 d . . .
H2A H 0.6669 0.6757 0.4489 0.089 Uiso 1 1 calc R . .
H2B H 0.6140 0.5876 0.4270 0.089 Uiso 1 1 calc R . .
H2C H 0.6083 0.6484 0.3322 0.089 Uiso 1 1 calc R . .
C11 C 0.73084(12) 0.54877(8) 0.13247(10) 0.0297(3) Uani 1 1 d . . .
C12 C 0.67465(14) 0.62154(9) 0.10068(12) 0.0373(3) Uani 1 1 d . . .
H12 H 0.6792 0.6633 0.1498 0.045 Uiso 1 1 calc R . .
C13 C 0.61256(15) 0.63361(9) -0.00112(12) 0.0438(4) Uani 1 1 d . . .
H13 H 0.5760 0.6835 -0.0224 0.053 Uiso 1 1 calc R . .
C14 C 0.60477(14) 0.57197(9) -0.07101(11) 0.0403(3) Uani 1 1 d . . .
H14 H 0.5597 0.5781 -0.1406 0.048 Uiso 1 1 calc R . .
C15 C 0.66371(12) 0.50077(9) -0.03835(10) 0.0323(3) Uani 1 1 d . . .
C16 C 0.65490(16) 0.43264(9) -0.11290(12) 0.0428(4) Uani 1 1 d . . .
H16A H 0.6683 0.3831 -0.0735 0.064 Uiso 1 1 calc R . .
H16B H 0.7200 0.4382 -0.1560 0.064 Uiso 1 1 calc R . .
H16C H 0.5706 0.4321 -0.1579 0.064 Uiso 1 1 calc R . .
C21 C 0.70721(12) 0.41793(8) 0.29764(10) 0.0292(3) Uani 1 1 d . . .
C22 C 0.62381(13) 0.40620(9) 0.36709(10) 0.0340(3) Uani 1 1 d . . .
H22 H 0.6132 0.4470 0.4147 0.041 Uiso 1 1 calc R . .
C23 C 0.55668(13) 0.33645(9) 0.36765(11) 0.0370(3) Uani 1 1 d . . .
H23 H 0.5008 0.3290 0.4153 0.044 Uiso 1 1 calc R . .
C24 C 0.57237(13) 0.27785(9) 0.29766(11) 0.0351(3) Uani 1 1 d . . .
H24 H 0.5271 0.2295 0.2961 0.042 Uiso 1 1 calc R . .
C25 C 0.65545(12) 0.29079(8) 0.22953(10) 0.0296(3) Uani 1 1 d . . .
C26 C 0.67458(15) 0.22965(9) 0.15036(12) 0.0398(3) Uani 1 1 d . . .
H26A H 0.7647 0.2153 0.1609 0.060 Uiso 1 1 calc R . .
H26B H 0.6475 0.2512 0.0799 0.060 Uiso 1 1 calc R . .
H26C H 0.6241 0.1826 0.1586 0.060 Uiso 1 1 calc R . .
C31 C 0.98587(13) 0.48911(8) 0.29147(10) 0.0294(3) Uani 1 1 d . . .
C32 C 1.08532(14) 0.53037(9) 0.35389(11) 0.0378(3) Uani 1 1 d . . .
H32 H 1.0669 0.5753 0.3920 0.045 Uiso 1 1 calc R . .
C33 C 1.20993(15) 0.50662(10) 0.36086(12) 0.0435(4) Uani 1 1 d . . .
H33 H 1.2775 0.5363 0.4004 0.052 Uiso 1 1 calc R . .
C34 C 1.23417(13) 0.43925(9) 0.30950(11) 0.0396(3) Uani 1 1 d . . .
H34 H 1.3189 0.4209 0.3147 0.048 Uiso 1 1 calc R . .
C35 C 1.13394(13) 0.39817(8) 0.24990(10) 0.0318(3) Uani 1 1 d . . .
C36 C 1.15828(15) 0.32122(9) 0.20004(13) 0.0422(3) Uani 1 1 d . . .
H36A H 1.0816 0.2885 0.1908 0.063 Uiso 1 1 calc R . .
H36B H 1.2284 0.2935 0.2449 0.063 Uiso 1 1 calc R . .
H36C H 1.1808 0.3314 0.1319 0.063 Uiso 1 1 calc R . .
O1 O 0.90645(9) 0.33593(6) 0.01514(8) 0.0359(2) Uani 1 1 d . . .
C41 C 0.90621(15) 0.25372(9) -0.01442(12) 0.0382(3) Uani 1 1 d . . .
H41A H 0.8193 0.2365 -0.0465 0.046 Uiso 1 1 calc R . .
H41B H 0.9372 0.2203 0.0474 0.046 Uiso 1 1 calc R . .
C42 C 0.99396(16) 0.24722(9) -0.09227(13) 0.0428(4) Uani 1 1 d . . .
H42A H 0.9654 0.2054 -0.1446 0.051 Uiso 1 1 calc R . .
H42B H 1.0824 0.2362 -0.0570 0.051 Uiso 1 1 calc R . .
C43 C 0.98215(15) 0.32861(10) -0.14194(12) 0.0426(4) Uani 1 1 d . . .
H43A H 1.0568 0.3412 -0.1734 0.051 Uiso 1 1 calc R . .
H43B H 0.9040 0.3331 -0.1960 0.051 Uiso 1 1 calc R . .
C44 C 0.97611(15) 0.38119(9) -0.04972(12) 0.0403(3) Uani 1 1 d . . .
H44A H 1.0625 0.3938 -0.0112 0.048 Uiso 1 1 calc R . .
H44B H 0.9314 0.4311 -0.0727 0.048 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 C1 1.9840(14) . ?
Al1 C31 2.0147(14) . ?
Al1 C11 2.0237(14) . ?
Al1 C21 2.0295(14) . ?
Al1 Li1 3.029(2) . ?
Li1 O1 1.990(2) . ?
Li1 N2 2.098(2) . ?
Li1 N1 2.151(3) . ?
Li1 N3 2.154(3) . ?
N1 C15 1.3483(17) . ?
N1 C11 1.3720(17) . ?
N2 C25 1.3436(17) . ?
N2 C21 1.3708(17) . ?
N3 C35 1.3523(17) . ?
N3 C31 1.3668(17) . ?
C1 C2 1.525(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C11 C12 1.3990(19) . ?
C12 C13 1.383(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.390(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.500(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 C22 1.4023(19) . ?
C22 C23 1.384(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.3898(19) . ?
C24 H24 0.9500 . ?
C25 C26 1.5033(19) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C31 C32 1.3995(19) . ?
C32 C33 1.382(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.372(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.388(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.501(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O1 C41 1.4439(17) . ?
O1 C44 1.4492(17) . ?
C41 C42 1.514(2) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.518(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.508(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 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
C1 Al1 C31 109.93(6) . . ?
C1 Al1 C11 114.43(6) . . ?
C31 Al1 C11 107.81(5) . . ?
C1 Al1 C21 116.35(6) . . ?
C31 Al1 C21 106.32(5) . . ?
C11 Al1 C21 101.27(5) . . ?
C1 Al1 Li1 176.03(7) . . ?
C31 Al1 Li1 66.18(6) . . ?
C11 Al1 Li1 67.01(6) . . ?
C21 Al1 Li1 66.34(6) . . ?
O1 Li1 N2 132.62(12) . . ?
O1 Li1 N1 107.89(11) . . ?
N2 Li1 N1 95.49(10) . . ?
O1 Li1 N3 104.14(11) . . ?
N2 Li1 N3 101.63(10) . . ?
N1 Li1 N3 115.62(11) . . ?
O1 Li1 Al1 161.13(11) . . ?
N2 Li1 Al1 66.24(6) . . ?
N1 Li1 Al1 65.70(6) . . ?
N3 Li1 Al1 66.15(6) . . ?
C15 N1 C11 119.71(12) . . ?
C15 N1 Li1 130.68(11) . . ?
C11 N1 Li1 109.50(10) . . ?
C25 N2 C21 120.30(11) . . ?
C25 N2 Li1 128.39(11) . . ?
C21 N2 Li1 111.20(10) . . ?
C35 N3 C31 119.37(12) . . ?
C35 N3 Li1 132.16(11) . . ?
C31 N3 Li1 107.76(10) . . ?
C2 C1 Al1 119.23(12) . . ?
C2 C1 H1A 107.5 . . ?
Al1 C1 H1A 107.5 . . ?
C2 C1 H1B 107.5 . . ?
Al1 C1 H1B 107.5 . . ?
H1A C1 H1B 107.0 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C11 C12 118.99(12) . . ?
N1 C11 Al1 116.31(9) . . ?
C12 C11 Al1 124.39(10) . . ?
C13 C12 C11 121.10(14) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C12 118.75(14) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 119.15(13) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
N1 C15 C14 122.15(13) . . ?
N1 C15 C16 117.91(12) . . ?
C14 C15 C16 119.93(13) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C21 C22 118.42(12) . . ?
N2 C21 Al1 116.22(9) . . ?
C22 C21 Al1 125.25(10) . . ?
C23 C22 C21 121.36(13) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C24 C23 C22 118.76(13) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C23 C24 C25 118.89(13) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
N2 C25 C24 122.27(13) . . ?
N2 C25 C26 116.51(12) . . ?
C24 C25 C26 121.21(12) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C31 C32 119.39(12) . . ?
N3 C31 Al1 118.30(9) . . ?
C32 C31 Al1 122.24(10) . . ?
C33 C32 C31 120.91(14) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C34 C33 C32 118.69(14) . . ?
C34 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
C33 C34 C35 119.45(13) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
N3 C35 C34 122.01(13) . . ?
N3 C35 C36 118.09(12) . . ?
C34 C35 C36 119.86(13) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C41 O1 C44 109.19(10) . . ?
C41 O1 Li1 132.64(11) . . ?
C44 O1 Li1 118.00(11) . . ?
O1 C41 C42 106.22(11) . . ?
O1 C41 H41A 110.5 . . ?
C42 C41 H41A 110.5 . . ?
O1 C41 H41B 110.5 . . ?
C42 C41 H41B 110.5 . . ?
H41A C41 H41B 108.7 . . ?
C41 C42 C43 102.02(12) . . ?
C41 C42 H42A 111.4 . . ?
C43 C42 H42A 111.4 . . ?
C41 C42 H42B 111.4 . . ?
C43 C42 H42B 111.4 . . ?
H42A C42 H42B 109.2 . . ?
C44 C43 C42 102.01(12) . . ?
C44 C43 H43A 111.4 . . ?
C42 C43 H43A 111.4 . . ?
C44 C43 H43B 111.4 . . ?
C42 C43 H43B 111.4 . . ?
H43A C43 H43B 109.2 . . ?
O1 C44 C43 104.98(11) . . ?
O1 C44 H44A 110.8 . . ?
C43 C44 H44A 110.8 . . ?
O1 C44 H44B 110.8 . . ?
C43 C44 H44B 110.8 . . ?
H44A C44 H44B 108.8 . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        72.05
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.043
_database_code_depnum_ccdc_archive 'CCDC 993339'
#######################################################################
#
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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data_dw1443

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H46 Al2 Cl Li Mn N6'
_chemical_formula_sum            'C40 H46 Al2 Cl Li Mn N6'
_chemical_formula_weight         762.12
_chemical_absolute_configuration 
;
 The absolute structure was NOT determined. 1850 Friedel pairs were
 averaged for the refinement.  Without Friedel averaging, the Flack
 parameter is ambiguous (ca 0.45) and attempts to refine as a twin
 did not improve matters.  Not too surprising, considering the problems
 of poor data and disorder (see _refine_special_details).
;

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P3(1)
_symmetry_space_group_name_Hall  'P 31'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'

_cell_length_a                   12.457(2)
_cell_length_b                   12.457(2)
_cell_length_c                   22.235(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2988.1(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    138880
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      25.35

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1197
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
; 
 Low temperature trigonal form.  Poor (poorly diffracting) crystal, 
 poor data.  The Mn, CL anf Li atoms are disordered according to the
 following pattern ...

            Mn---Cl------Li       occupancy 0.89
            Li------Cl---Mn       occupancy 0.11

 Best of FOUR datasets collected from four different crystals.  All
 crystals exhibit the same disorder pattern.  For refinement details,
 see '_refine_special_details'.

 The unusually large number of reflections (138880) reflects the poor quality
 of the crystal.  With a mosaic spread of more than 2 degrees, a large number
 of extra frames were collected but no 'full' reflections were recorded.
 There were 189444 'partial' reflections and the algorithm used to determine
 the cell dimensions used most of them.
;

_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            10346
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_sigmaI/netI    0.1357
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.75
_diffrn_reflns_theta_max         25.37
_reflns_number_total             3476
_reflns_number_gt                1825
_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  Mn(1)---CL(1)-----Li(1)  fragment (occupancy 0.89) and the
      Li(2)-----CL(2)---Mn(2)  fragment (occupancy 0.11) were restrained
 to have the same geometry. The Mn and Li atoms were assigned a common isotropic
 displacement parameter, the Cl atoms another.  The final result seems reasonable 
 (Mn-CL distances 2.34A, Li-Cl distances 2.88A, U(iso)=0.05 for Mn/Li, U(iso) =
 0.07 for Cl), very similar to that obtained for the rhombohedral form.
 Except for the Al atoms (which were assigned anisotropic displacement
 parameters) all other non-H atoms were assigned common isotropic parameters. 
 So, with the Mn/Li occupancy factor etc.,  12 extra LS parameters (SHELXL
 'free variables') were  used for this refinement giving a total of 192 LS
 parameters and a respectable parameter/data ratio of 18:1. 
;

_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)+(0.0800P)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   0.13(4)
_refine_ls_number_reflns         3476
_refine_ls_number_parameters     192
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.1655
_refine_ls_wR_factor_gt          0.1468
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.6724(6) -0.0045(6) 0.2912(2) 0.0460(4) Uiso 0.887(3) 1 d PD A 1
Mn1 Mn 0.67797(14) 0.02206(12) 0.52532(13) 0.0460(4) Uiso 0.887(3) 1 d PD A 1
Cl1 Cl 0.6649(2) 0.0125(3) 0.4201(2) 0.0680(9) Uiso 0.887(3) 1 d PD A 1
Li2 Li 0.67797(14) 0.02206(12) 0.52532(13) 0.0460(4) Uiso 0.113(3) 1 d PD A 2
Mn2 Mn 0.6724(6) -0.0045(6) 0.2912(2) 0.0460(4) Uiso 0.113(3) 1 d PD A 2
Cl2 Cl 0.6881(13) 0.012(2) 0.3963(3) 0.0680(9) Uiso 0.113(3) 1 d PD A 2
Al1 Al 0.6824(2) -0.0178(2) 0.1531(2) 0.0475(8) Uani 1 1 d . . .
Al2 Al 0.6919(2) 0.0299(3) 0.66778(18) 0.0472(8) Uani 1 1 d . . .
C1 C 0.6981(8) -0.0285(9) 0.0663(5) 0.071(3) Uiso 1 1 d . A .
H1A H 0.7822 0.0379 0.0548 0.085 Uiso 1 1 calc R . .
H1B H 0.6942 -0.1084 0.0580 0.085 Uiso 1 1 calc R . .
C2 C 0.6066(10) -0.0194(9) 0.0241(5) 0.083(3) Uiso 1 1 d . . .
H2A H 0.6300 -0.0223 -0.0177 0.124 Uiso 1 1 calc R A .
H2B H 0.6079 0.0589 0.0313 0.124 Uiso 1 1 calc R . .
H2C H 0.5230 -0.0889 0.0316 0.124 Uiso 1 1 calc R . .
C3 C 0.7118(8) 0.0435(8) 0.7566(4) 0.054(3) Uiso 1 1 d . A .
H3A H 0.7872 0.0397 0.7668 0.065 Uiso 1 1 calc R . .
H3B H 0.7274 0.1267 0.7685 0.065 Uiso 1 1 calc R . .
C4 C 0.6066(10) -0.0513(10) 0.7951(5) 0.088(3) Uiso 1 1 d . . .
H4A H 0.6283 -0.0328 0.8377 0.132 Uiso 1 1 calc R A .
H4B H 0.5923 -0.1343 0.7858 0.132 Uiso 1 1 calc R . .
H4C H 0.5311 -0.0479 0.7866 0.132 Uiso 1 1 calc R . .
N1 N 0.6780(6) 0.1470(6) 0.2441(3) 0.0446(7) Uiso 1 1 d . . .
C11 C 0.6906(7) 0.1387(7) 0.1847(4) 0.0448(8) Uiso 1 1 d . A .
C12 C 0.7090(7) 0.2361(8) 0.1475(4) 0.0542(9) Uiso 1 1 d . . .
H12 H 0.7173 0.2303 0.1053 0.065 Uiso 1 1 calc R A .
C13 C 0.7155(8) 0.3407(8) 0.1714(4) 0.0612(9) Uiso 1 1 d . A .
H13 H 0.7299 0.4085 0.1464 0.073 Uiso 1 1 calc R . .
C14 C 0.7006(8) 0.3448(8) 0.2314(4) 0.0574(9) Uiso 1 1 d . . .
H14 H 0.7044 0.4162 0.2488 0.069 Uiso 1 1 calc R A .
C15 C 0.6802(7) 0.2470(7) 0.2674(4) 0.0475(8) Uiso 1 1 d . A .
C16 C 0.6627(8) 0.2512(8) 0.3339(4) 0.0638(10) Uiso 1 1 d . . .
H16A H 0.5984 0.1694 0.3479 0.096 Uiso 1 1 calc R A .
H16B H 0.6375 0.3125 0.3427 0.096 Uiso 1 1 calc R . .
H16C H 0.7409 0.2745 0.3546 0.096 Uiso 1 1 calc R . .
N2 N 0.8305(6) -0.0118(6) 0.2565(3) 0.0446(7) Uiso 1 1 d . . .
C21 C 0.8216(7) -0.0271(7) 0.1953(4) 0.0448(8) Uiso 1 1 d . A .
C22 C 0.9066(7) -0.0484(7) 0.1647(4) 0.0542(9) Uiso 1 1 d . . .
H22 H 0.9010 -0.0583 0.1223 0.065 Uiso 1 1 calc R A .
C23 C 0.9998(8) -0.0554(8) 0.1959(4) 0.0612(9) Uiso 1 1 d . A .
H23 H 1.0564 -0.0724 0.1751 0.073 Uiso 1 1 calc R . .
C24 C 1.0086(8) -0.0375(8) 0.2567(4) 0.0574(9) Uiso 1 1 d . . .
H24 H 1.0727 -0.0399 0.2789 0.069 Uiso 1 1 calc R A .
C25 C 0.9221(7) -0.0157(7) 0.2858(4) 0.0475(8) Uiso 1 1 d . A .
C26 C 0.9303(8) 0.0050(8) 0.3523(4) 0.0638(10) Uiso 1 1 d . . .
H26A H 0.8852 0.0478 0.3633 0.096 Uiso 1 1 calc R A .
H26B H 1.0175 0.0558 0.3640 0.096 Uiso 1 1 calc R . .
H26C H 0.8937 -0.0751 0.3730 0.096 Uiso 1 1 calc R . .
N3 N 0.5253(6) -0.1667(5) 0.2521(3) 0.0446(7) Uiso 1 1 d . . .
C31 C 0.5282(7) -0.1570(7) 0.1906(4) 0.0448(8) Uiso 1 1 d . A .
C32 C 0.4296(8) -0.2477(7) 0.1576(4) 0.0542(9) Uiso 1 1 d . . .
H32 H 0.4318 -0.2438 0.1149 0.065 Uiso 1 1 calc R A .
C33 C 0.3274(9) -0.3442(8) 0.1863(5) 0.0612(9) Uiso 1 1 d . A .
H33 H 0.2585 -0.4034 0.1636 0.073 Uiso 1 1 calc R . .
C34 C 0.3278(8) -0.3523(8) 0.2467(4) 0.0574(9) Uiso 1 1 d . . .
H34 H 0.2600 -0.4190 0.2668 0.069 Uiso 1 1 calc R A .
C35 C 0.4279(7) -0.2626(7) 0.2797(4) 0.0475(8) Uiso 1 1 d . A .
C36 C 0.4322(8) -0.2682(8) 0.3457(4) 0.0638(10) Uiso 1 1 d . . .
H36A H 0.4271 -0.1986 0.3632 0.096 Uiso 1 1 calc R A .
H36B H 0.5101 -0.2632 0.3580 0.096 Uiso 1 1 calc R . .
H36C H 0.3622 -0.3464 0.3599 0.096 Uiso 1 1 calc R . .
N4 N 0.8363(6) 0.1808(6) 0.5652(3) 0.0446(7) Uiso 1 1 d . . .
C41 C 0.8381(7) 0.1696(7) 0.6259(4) 0.0448(8) Uiso 1 1 d . A .
C42 C 0.9426(8) 0.2583(8) 0.6580(4) 0.0542(9) Uiso 1 1 d . . .
H42 H 0.9451 0.2511 0.7005 0.065 Uiso 1 1 calc R A .
C43 C 1.0416(8) 0.3553(8) 0.6289(4) 0.0612(9) Uiso 1 1 d . A .
H43 H 1.1118 0.4143 0.6510 0.073 Uiso 1 1 calc R . .
C44 C 1.0366(8) 0.3650(8) 0.5679(4) 0.0574(9) Uiso 1 1 d . . .
H44 H 1.1042 0.4298 0.5468 0.069 Uiso 1 1 calc R A .
C45 C 0.9333(7) 0.2803(7) 0.5377(4) 0.0475(8) Uiso 1 1 d . A .
C46 C 0.9227(8) 0.2856(9) 0.4706(4) 0.0638(10) Uiso 1 1 d . . .
H46A H 0.8412 0.2744 0.4603 0.096 Uiso 1 1 calc R A .
H46B H 0.9322 0.2196 0.4520 0.096 Uiso 1 1 calc R . .
H46C H 0.9877 0.3663 0.4558 0.096 Uiso 1 1 calc R . .
N5 N 0.5262(6) 0.0248(6) 0.5730(3) 0.0446(7) Uiso 1 1 d . . .
C51 C 0.5479(7) 0.0403(7) 0.6335(4) 0.0448(8) Uiso 1 1 d . A .
C52 C 0.4641(8) 0.0558(7) 0.6696(4) 0.0542(9) Uiso 1 1 d . . .
H52 H 0.4765 0.0652 0.7119 0.065 Uiso 1 1 calc R A .
C53 C 0.3642(8) 0.0576(8) 0.6443(4) 0.0612(9) Uiso 1 1 d . A .
H53 H 0.3085 0.0688 0.6691 0.073 Uiso 1 1 calc R . .
C54 C 0.3449(8) 0.0436(8) 0.5842(4) 0.0574(9) Uiso 1 1 d . . .
H54 H 0.2763 0.0456 0.5667 0.069 Uiso 1 1 calc R A .
C55 C 0.4258(7) 0.0264(8) 0.5486(4) 0.0475(8) Uiso 1 1 d . A .
C56 C 0.4080(8) 0.0121(8) 0.4821(4) 0.0638(10) Uiso 1 1 d . . .
H56A H 0.3224 -0.0112 0.4721 0.096 Uiso 1 1 calc R A .
H56B H 0.4248 -0.0527 0.4680 0.096 Uiso 1 1 calc R . .
H56C H 0.4651 0.0907 0.4624 0.096 Uiso 1 1 calc R . .
N6 N 0.6834(6) -0.1315(6) 0.5688(3) 0.0446(7) Uiso 1 1 d . . .
C61 C 0.6769(7) -0.1236(7) 0.6298(4) 0.0448(8) Uiso 1 1 d . A .
C62 C 0.6650(8) -0.2248(8) 0.6642(4) 0.0542(9) Uiso 1 1 d . . .
H62 H 0.6627 -0.2199 0.7068 0.065 Uiso 1 1 calc R A .
C63 C 0.6567(8) -0.3270(8) 0.6398(4) 0.0612(9) Uiso 1 1 d . A .
H63 H 0.6445 -0.3950 0.6641 0.073 Uiso 1 1 calc R . .
C64 C 0.6666(8) -0.3295(8) 0.5783(4) 0.0574(9) Uiso 1 1 d . . .
H64 H 0.6642 -0.3994 0.5598 0.069 Uiso 1 1 calc R A .
C65 C 0.6800(7) -0.2320(7) 0.5427(4) 0.0475(8) Uiso 1 1 d . A .
C66 C 0.6965(8) -0.2307(9) 0.4772(4) 0.0638(10) Uiso 1 1 d . . .
H66A H 0.7716 -0.1541 0.4655 0.096 Uiso 1 1 calc R A .
H66B H 0.6246 -0.2348 0.4570 0.096 Uiso 1 1 calc R . .
H66C H 0.7043 -0.3022 0.4653 0.096 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
Li1 N3 2.120(9) . ?
Li1 N1 2.129(9) . ?
Li1 N2 2.160(9) . ?
Li1 Cl1 2.878(8) . ?
Li1 Al1 3.082(8) . ?
Mn1 N4 2.165(7) . ?
Mn1 N6 2.175(6) . ?
Mn1 N5 2.182(6) . ?
Mn1 Cl1 2.344(3) . ?
Al1 C1 1.951(11) . ?
Al1 C31 2.015(8) . ?
Al1 C21 2.024(8) . ?
Al1 C11 2.026(8) . ?
Al2 C3 1.986(9) . ?
Al2 C51 2.012(8) . ?
Al2 C41 2.010(8) . ?
Al2 C61 2.012(8) . ?
C1 C2 1.523(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.516(14) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N1 C15 1.336(9) . ?
N1 C11 1.340(9) . ?
C11 C12 1.389(11) . ?
C12 C13 1.372(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.350(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.371(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.500(11) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N2 C25 1.336(9) . ?
N2 C21 1.370(9) . ?
C21 C22 1.391(11) . ?
C22 C23 1.392(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.367(10) . ?
C23 H23 0.9500 . ?
C24 C25 1.395(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.495(11) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
N3 C35 1.352(9) . ?
N3 C31 1.372(9) . ?
C31 C32 1.391(10) . ?
C32 C33 1.394(11) . ?
C32 H32 0.9500 . ?
C33 C34 1.347(12) . ?
C33 H33 0.9500 . ?
C34 C35 1.396(11) . ?
C34 H34 0.9500 . ?
C35 C36 1.471(10) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N4 C41 1.359(9) . ?
N4 C45 1.369(10) . ?
C41 C42 1.409(11) . ?
C42 C43 1.382(11) . ?
C42 H42 0.9500 . ?
C43 C44 1.366(11) . ?
C43 H43 0.9500 . ?
C44 C45 1.365(11) . ?
C44 H44 0.9500 . ?
C45 C46 1.502(11) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N5 C51 1.366(9) . ?
N5 C55 1.373(9) . ?
C51 C52 1.406(11) . ?
C52 C53 1.375(11) . ?
C52 H52 0.9500 . ?
C53 C54 1.353(11) . ?
C53 H53 0.9500 . ?
C54 C55 1.381(11) . ?
C54 H54 0.9500 . ?
C55 C56 1.493(11) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
N6 C65 1.362(9) . ?
N6 C61 1.364(9) . ?
C61 C62 1.418(11) . ?
C62 C63 1.339(11) . ?
C62 H62 0.9500 . ?
C63 C64 1.375(11) . ?
C63 H63 0.9500 . ?
C64 C65 1.388(11) . ?
C64 H64 0.9500 . ?
C65 C66 1.471(10) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 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 Li1 N1 105.8(4) . . ?
N3 Li1 N2 100.6(4) . . ?
N1 Li1 N2 103.6(4) . . ?
N3 Li1 Cl1 115.7(3) . . ?
N1 Li1 Cl1 114.4(3) . . ?
N2 Li1 Cl1 115.0(3) . . ?
N3 Li1 Al1 65.1(3) . . ?
N1 Li1 Al1 64.7(3) . . ?
N2 Li1 Al1 65.1(3) . . ?
Cl1 Li1 Al1 179.0(3) . . ?
N4 Mn1 N6 101.9(2) . . ?
N4 Mn1 N5 100.8(2) . . ?
N6 Mn1 N5 101.9(2) . . ?
N4 Mn1 Cl1 117.65(19) . . ?
N6 Mn1 Cl1 115.5(2) . . ?
N5 Mn1 Cl1 116.54(18) . . ?
Mn1 Cl1 Li1 173.41(19) . . ?
C1 Al1 C31 115.8(4) . . ?
C1 Al1 C21 109.7(4) . . ?
C31 Al1 C21 103.6(3) . . ?
C1 Al1 C11 116.8(4) . . ?
C31 Al1 C11 104.6(3) . . ?
C21 Al1 C11 105.2(3) . . ?
C1 Al1 Li1 176.1(3) . . ?
C31 Al1 Li1 65.7(3) . . ?
C21 Al1 Li1 66.4(3) . . ?
C11 Al1 Li1 65.6(3) . . ?
C3 Al2 C51 116.7(3) . . ?
C3 Al2 C41 111.4(4) . . ?
C51 Al2 C41 102.7(3) . . ?
C3 Al2 C61 116.5(3) . . ?
C51 Al2 C61 103.9(3) . . ?
C41 Al2 C61 104.0(3) . . ?
C2 C1 Al1 120.0(7) . . ?
C2 C1 H1A 107.3 . . ?
Al1 C1 H1A 107.3 . . ?
C2 C1 H1B 107.3 . . ?
Al1 C1 H1B 107.3 . . ?
H1A C1 H1B 106.9 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 Al2 118.2(7) . . ?
C4 C3 H3A 107.8 . . ?
Al2 C3 H3A 107.8 . . ?
C4 C3 H3B 107.8 . . ?
Al2 C3 H3B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C15 N1 C11 120.3(7) . . ?
C15 N1 Li1 127.7(6) . . ?
C11 N1 Li1 111.7(5) . . ?
N1 C11 C12 119.6(7) . . ?
N1 C11 Al1 117.7(5) . . ?
C12 C11 Al1 122.7(6) . . ?
C13 C12 C11 120.3(8) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 118.3(9) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C13 C14 C15 120.8(9) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
N1 C15 C14 120.7(8) . . ?
N1 C15 C16 118.6(7) . . ?
C14 C15 C16 120.7(8) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C25 N2 C21 119.4(6) . . ?
C25 N2 Li1 129.8(6) . . ?
C21 N2 Li1 110.4(5) . . ?
N2 C21 C22 119.6(7) . . ?
N2 C21 Al1 117.7(5) . . ?
C22 C21 Al1 122.7(6) . . ?
C21 C22 C23 120.5(8) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 119.0(9) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C23 C24 C25 118.9(8) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
N2 C25 C24 122.6(8) . . ?
N2 C25 C26 117.5(7) . . ?
C24 C25 C26 119.9(7) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C35 N3 C31 120.2(6) . . ?
C35 N3 Li1 128.4(6) . . ?
C31 N3 Li1 110.7(5) . . ?
N3 C31 C32 118.8(7) . . ?
N3 C31 Al1 117.3(5) . . ?
C32 C31 Al1 123.8(6) . . ?
C31 C32 C33 120.8(8) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 119.1(9) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C33 C34 C35 119.9(8) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
N3 C35 C34 121.1(8) . . ?
N3 C35 C36 117.2(7) . . ?
C34 C35 C36 121.7(8) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C41 N4 C45 119.0(7) . . ?
C41 N4 Mn1 111.6(5) . . ?
C45 N4 Mn1 129.3(5) . . ?
N4 C41 C42 118.6(7) . . ?
N4 C41 Al2 119.6(6) . . ?
C42 C41 Al2 121.7(6) . . ?
C43 C42 C41 121.2(8) . . ?
C43 C42 H42 119.4 . . ?
C41 C42 H42 119.4 . . ?
C44 C43 C42 118.8(9) . . ?
C44 C43 H43 120.6 . . ?
C42 C43 H43 120.6 . . ?
C45 C44 C43 119.2(9) . . ?
C45 C44 H44 120.4 . . ?
C43 C44 H44 120.4 . . ?
C44 C45 N4 123.0(8) . . ?
C44 C45 C46 121.7(8) . . ?
N4 C45 C46 115.2(7) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C51 N5 C55 120.3(6) . . ?
C51 N5 Mn1 111.6(5) . . ?
C55 N5 Mn1 127.7(5) . . ?
N5 C51 C52 118.3(7) . . ?
N5 C51 Al2 119.0(5) . . ?
C52 C51 Al2 122.6(6) . . ?
C53 C52 C51 120.5(8) . . ?
C53 C52 H52 119.7 . . ?
C51 C52 H52 119.7 . . ?
C54 C53 C52 120.4(9) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C53 C54 C55 119.3(9) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
N5 C55 C54 121.1(8) . . ?
N5 C55 C56 118.2(7) . . ?
C54 C55 C56 120.7(8) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C65 N6 C61 121.0(7) . . ?
C65 N6 Mn1 128.2(5) . . ?
C61 N6 Mn1 110.4(5) . . ?
N6 C61 C62 117.1(7) . . ?
N6 C61 Al2 120.4(6) . . ?
C62 C61 Al2 122.5(6) . . ?
C63 C62 C61 123.4(9) . . ?
C63 C62 H62 118.3 . . ?
C61 C62 H62 118.3 . . ?
C62 C63 C64 117.3(9) . . ?
C62 C63 H63 121.3 . . ?
C64 C63 H63 121.3 . . ?
C63 C64 C65 121.4(9) . . ?
C63 C64 H64 119.3 . . ?
C65 C64 H64 119.3 . . ?
N6 C65 C64 119.7(7) . . ?
N6 C65 C66 118.2(7) . . ?
C64 C65 C66 122.1(8) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        25.37
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 1015853'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw1444

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H46 Al2 Cl Li Mn N6'
_chemical_formula_sum            'C40 H46 Al2 Cl Li Mn N6'
_chemical_formula_weight         762.12
_chemical_absolute_configuration 
;
 The absolute structure was NOT determined. 439 Friedel pairs were
 averaged for the refinement.  Without Friedel averaging, the Flack
 parameter is ambiguous (ca 0.43) and attempts to refine as a twin
 did not improve matters.  Not too surprising, considering the problems
 of poor data and disorder (see _refine_special_details).
;

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R3
_symmetry_space_group_name_Hall  'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   12.543(1)
_cell_length_b                   12.543(1)
_cell_length_c                   22.339(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3043.7(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    2280
_cell_measurement_theta_min      4.53
_cell_measurement_theta_max      41.20

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1197
_exptl_absorpt_coefficient_mu    3.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;

_exptl_special_details           
; 
  High temperature rhombohedral form.  Poor (poorly diffracting) crystal, 
 very poor data.  The two terminal -Et groups are each disordered about the 
 triad axis Mn---Cl------Li and the Mn,Cl and Li atoms are themselves
 disordered along this triad ...

            Mn---Cl------Li       occupancy 0.29000
            Li------Cl---Mn       occupancy 0.04333

 This is the best of three datasets collected from three different crystals.  
 All crystals exhibit the same disorder pattern.  For refinement details,
 see '_refine_special_details'.    
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            2317
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.53
_diffrn_reflns_theta_max         41.20
_reflns_number_total             881
_reflns_number_gt                879
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_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  Mn(1)---CL(1)-----Li(1)  fragment (occupancy 0.29000) and the
      Li(2)-----CL(2)---Mn(2)  fragment (occupancy 0.04333) were restrained
 to have the same geometry, all Mn, Cl and Li atoms were assigned a common
 isotropic displacement parameter.  Happily, the result seems reasonable (Mn-CL
 distances 2.35A, Li-Cl distances 2.80A, U(iso)=0.07), consistent with that
 observed for the low-temperature trigonal form.

 The terminal -Ethyl groups M-C(1)-C(2) are not well resolved, each was modelled with 
 three distance restraints d1=M-C(1),d2= M-C(2), d3=C(1)-C(2) where d1, d2 and d3
 were estimated from the better-resolved refinement of the low temperature trigonal
 form.

 Despite this refinement strategy, the parameter-data ratio is still poor (5:1), 
 reflecting the very poor quality of this dataset (the best of three datasets from 
 three different crystals).   
;

_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)+(0.1123P)²+65.9986P] 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   0.47(4)
_refine_ls_number_reflns         881
_refine_ls_number_parameters     79
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0962
_refine_ls_wR_factor_ref         0.2389
_refine_ls_wR_factor_gt          0.2387
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_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_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
Mn1 Mn 0.0000 0.0000 -0.1079(2) 0.0705(15) Uiso 0.87 .33333 d SPD . 1
Li1 Li 0.0000 0.0000 0.1230(10) 0.0705(15) Uiso 0.87 .33333 d SPD . 1
Cl1 Cl 0.0000 0.0000 -0.0025(4) 0.0705(15) Uiso 0.87 .33333 d SPD A 1
Mn2 Mn 0.0000 0.0000 0.1230(10) 0.0705(15) Uiso 0.13 .33333 d SPD . 2
Li2 Li 0.0000 0.0000 -0.1079(2) 0.0705(15) Uiso 0.13 .33333 d SPD . 2
Cl2 Cl 0.0000 0.0000 0.0178(13) 0.0705(15) Uiso 0.13 .33333 d SPD B 2
Al1 Al 0.0000 0.0000 -0.2495(3) 0.079(3) Uani 1 .33333 d SD . .
Al2 Al 0.0000 0.0000 0.2663(3) 0.073(3) Uani 1 .33333 d SD . .
N1 N 0.1555(12) -0.0005(11) -0.1502(6) 0.058(4) Uiso 1 1 d . . .
C1 C 0.1552(14) 0.0110(14) -0.2087(8) 0.060(5) Uiso 1 1 d . . .
C2 C 0.2520(18) 0.0260(18) -0.2470(9) 0.087(6) Uiso 1 1 d . . .
H2 H 0.2499 0.0329 -0.2893 0.105 Uiso 1 1 calc R . .
C3 C 0.348(2) 0.0297(18) -0.2169(9) 0.094(6) Uiso 1 1 d . . .
H3 H 0.4185 0.0434 -0.2392 0.112 Uiso 1 1 calc R . .
C4 C 0.3496(17) 0.0149(15) -0.1563(8) 0.080(6) Uiso 1 1 d . . .
H4 H 0.4172 0.0136 -0.1379 0.096 Uiso 1 1 calc R . .
C5 C 0.2514(16) 0.0017(15) -0.1219(7) 0.065(5) Uiso 1 1 d . . .
C6 C 0.2495(18) -0.0170(18) -0.0567(8) 0.091(6) Uiso 1 1 d . . .
H6A H 0.2580 0.0557 -0.0359 0.136 Uiso 1 1 calc R . .
H6B H 0.3179 -0.0297 -0.0454 0.136 Uiso 1 1 calc R . .
H6C H 0.1714 -0.0895 -0.0453 0.136 Uiso 1 1 calc R . .
N2 N 0.1538(11) 0.1535(12) 0.1673(6) 0.061(4) Uiso 1 1 d . . .
C7 C 0.1340(16) 0.1438(15) 0.2292(7) 0.062(5) Uiso 1 1 d . . .
C8 C 0.2267(19) 0.2516(19) 0.2596(10) 0.099(7) Uiso 1 1 d . . .
H8 H 0.2190 0.2519 0.3019 0.119 Uiso 1 1 calc R . .
C9 C 0.3251(19) 0.354(2) 0.2351(10) 0.096(7) Uiso 1 1 d . . .
H9 H 0.3814 0.4211 0.2593 0.116 Uiso 1 1 calc R . .
C10 C 0.3374(18) 0.3557(18) 0.1776(9) 0.082(6) Uiso 1 1 d . . .
H10 H 0.4027 0.4250 0.1582 0.099 Uiso 1 1 calc R . .
C11 C 0.2489(16) 0.2488(16) 0.1428(7) 0.062(5) Uiso 1 1 d . . .
C12 C 0.2624(17) 0.2506(17) 0.0772(9) 0.090(6) Uiso 1 1 d . . .
H12A H 0.2889 0.1922 0.0655 0.135 Uiso 1 1 calc R . .
H12B H 0.3241 0.3336 0.0643 0.135 Uiso 1 1 calc R . .
H12C H 0.1832 0.2273 0.0583 0.135 Uiso 1 1 calc R . .
C13 C 0.0000 0.0000 -0.3389(5) 0.150 Uiso 0.33333 0.33333 d SD . -1
H13A H 0.0864 0.0497 -0.3525 0.180 Uiso 0.33333 1 calc PR . -1
H13B H -0.0304 -0.0855 -0.3525 0.180 Uiso 0.33333 1 calc PR . -1
C14 C -0.074(6) 0.048(7) -0.3700(8) 0.150 Uiso 0.33333 1 d PD . -1
H14A H -0.0678 0.0416 -0.4135 0.225 Uiso 0.33333 1 calc PR . -1
H14B H -0.0430 0.1338 -0.3589 0.225 Uiso 0.33333 1 calc PR . -1
H14C H -0.1609 -0.0016 -0.3580 0.225 Uiso 0.33333 1 calc PR . -1
C15 C 0.0000 0.0000 0.3561(5) 0.150 Uiso 0.33333 0.33333 d SD . -1
H15A H -0.0418 -0.0867 0.3698 0.180 Uiso 0.33333 1 calc PR . -1
H15B H 0.0866 0.0391 0.3698 0.180 Uiso 0.3333 1 calc PR . -1
C16 C -0.060(7) 0.063(7) 0.3869(8) 0.150 Uiso 0.33333 1 d PD . -1
H16A H -0.0508 0.0598 0.4304 0.225 Uiso 0.33333 1 calc PR . -1
H16B H -0.1472 0.0221 0.3765 0.225 Uiso 0.33333 1 calc PR . -1
H16C H -0.0196 0.1495 0.3741 0.225 Uiso 0.33333 1 calc PR . -1


_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
Mn1 N1 2.170(13) 3 ?
Mn1 N1 2.170(13) 2 ?
Mn1 N1 2.170(13) . ?
Mn1 Cl1 2.354(9) . ?
Li1 N2 2.166(17) . ?
Li1 N2 2.166(17) 3 ?
Li1 N2 2.166(17) 2 ?
Li1 Cl1 2.80(3) . ?
Li1 Al2 3.20(3) . ?
Al1 C13 1.997(10) . ?
Al1 C1 2.090(16) . ?
Al1 C1 2.090(16) 2 ?
Al1 C1 2.090(16) 3 ?
Al2 C7 1.932(17) 2 ?
Al2 C7 1.932(17) 3 ?
Al2 C7 1.932(17) . ?
Al2 C15 2.006(10) . ?
N1 C1 1.315(17) . ?
N1 C5 1.346(19) . ?
C1 C2 1.42(2) . ?
C2 C3 1.36(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.37(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.39(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.48(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N2 C11 1.314(19) . ?
N2 C7 1.401(18) . ?
C7 C8 1.44(3) . ?
C8 C9 1.38(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.29(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.46(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.47(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.507(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.503(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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
N1 Mn1 N1 102.5(4) 3 2 ?
N1 Mn1 N1 102.5(4) 3 . ?
N1 Mn1 N1 102.5(4) 2 . ?
N1 Mn1 Cl1 115.8(4) 3 . ?
N1 Mn1 Cl1 115.8(4) 2 . ?
N1 Mn1 Cl1 115.8(4) . . ?
N2 Li1 N2 100.8(8) . 3 ?
N2 Li1 N2 100.8(8) . 2 ?
N2 Li1 N2 100.8(8) 3 2 ?
N2 Li1 Cl1 117.2(7) . . ?
N2 Li1 Cl1 117.2(7) 3 . ?
N2 Li1 Cl1 117.2(7) 2 . ?
N2 Li1 Al2 62.8(7) . . ?
N2 Li1 Al2 62.8(7) 3 . ?
N2 Li1 Al2 62.8(7) 2 . ?
Cl1 Li1 Al2 180.0 . . ?
Mn1 Cl1 Li1 180.0 . . ?
C13 Al1 C1 115.8(5) . . ?
C13 Al1 C1 115.8(5) . 2 ?
C1 Al1 C1 102.4(6) . 2 ?
C13 Al1 C1 115.8(5) . 3 ?
C1 Al1 C1 102.4(6) . 3 ?
C1 Al1 C1 102.4(6) 2 3 ?
C7 Al2 C7 103.0(6) 2 3 ?
C7 Al2 C7 103.0(6) 2 . ?
C7 Al2 C7 103.0(6) 3 . ?
C7 Al2 C15 115.4(5) 2 . ?
C7 Al2 C15 115.4(5) 3 . ?
C7 Al2 C15 115.4(5) . . ?
C7 Al2 Li1 64.6(5) 2 . ?
C7 Al2 Li1 64.6(5) 3 . ?
C7 Al2 Li1 64.6(5) . . ?
C15 Al2 Li1 180.000(2) . . ?
C1 N1 C5 121.0(14) . . ?
C1 N1 Mn1 112.3(10) . . ?
C5 N1 Mn1 126.2(11) . . ?
N1 C1 C2 124.4(16) . . ?
N1 C1 Al1 118.7(12) . . ?
C2 C1 Al1 116.9(13) . . ?
C3 C2 C1 113.0(19) . . ?
C3 C2 H2 123.5 . . ?
C1 C2 H2 123.5 . . ?
C4 C3 C2 124(2) . . ?
C4 C3 H3 118.1 . . ?
C2 C3 H3 118.1 . . ?
C3 C4 C5 119.5(19) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 118.2(15) . . ?
N1 C5 C6 121.1(16) . . ?
C4 C5 C6 120.5(17) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C11 N2 C7 122.2(14) . . ?
C11 N2 Li1 128.2(13) . . ?
C7 N2 Li1 109.5(12) . . ?
N2 C7 C8 111.1(15) . . ?
N2 C7 Al2 122.6(12) . . ?
C8 C7 Al2 126.4(13) . . ?
C9 C8 C7 128.1(19) . . ?
C9 C8 H8 115.9 . . ?
C7 C8 H8 115.9 . . ?
C10 C9 C8 117(2) . . ?
C10 C9 H9 121.5 . . ?
C8 C9 H9 121.5 . . ?
C9 C10 C11 119(2) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
N2 C11 C10 122.6(15) . . ?
N2 C11 C12 118.3(15) . . ?
C10 C11 C12 119.0(16) . . ?
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 . . ?
C14 C13 Al1 117.5(10) . . ?
C14 C13 H13A 107.9 . . ?
Al1 C13 H13A 107.9 . . ?
C14 C13 H13B 107.9 . . ?
Al1 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 Al2 117.3(10) . . ?
C16 C15 H15A 108.0 . . ?
Al2 C15 H15A 108.0 . . ?
C16 C15 H15B 108.0 . . ?
Al2 C15 H15B 108.0 . . ?
H15A C15 H15B 107.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        41.20
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.083
_database_code_depnum_ccdc_archive 'CCDC 1015854'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dw1426

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H46 Al2 Ca N6'
_chemical_formula_sum            'C40 H46 Al2 Ca N6'
_chemical_formula_weight         704.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 '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)/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.7465(6)
_cell_length_b                   19.5696(9)
_cell_length_c                   16.2852(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.215(2)
_cell_angle_gamma                90.00
_cell_volume                     3721.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      47.24

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_absorpt_coefficient_mu    2.193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            19391
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         47.22
_reflns_number_total             3315
_reflns_number_gt                2976
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_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. 
;

_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)+(0.0832P)²+2.3293P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3315
_refine_ls_number_parameters     449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1259
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_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
Ca1 Ca 0.20033(5) 0.80347(3) 0.32437(4) 0.0275(3) Uani 1 1 d . . .
Al1 Al 0.26801(8) 0.91294(5) 0.17018(6) 0.0297(3) Uani 1 1 d . . .
Al2 Al 0.14015(8) 0.69882(5) 0.48589(6) 0.0270(3) Uani 1 1 d . . .
C1 C 0.3074(3) 0.97611(17) 0.0821(2) 0.0374(9) Uani 1 1 d . . .
H1A H 0.3083 1.0229 0.1051 0.045 Uiso 1 1 calc R . .
H1B H 0.3869 0.9655 0.0713 0.045 Uiso 1 1 calc R . .
C2 C 0.2338(3) 0.97803(18) -0.0020(2) 0.0395(10) Uani 1 1 d . . .
H2A H 0.2655 1.0117 -0.0378 0.059 Uiso 1 1 calc R . .
H2B H 0.1552 0.9908 0.0062 0.059 Uiso 1 1 calc R . .
H2C H 0.2340 0.9328 -0.0278 0.059 Uiso 1 1 calc R . .
C3 C 0.1021(3) 0.64273(17) 0.5803(2) 0.0348(9) Uani 1 1 d . . .
H3A H 0.0210 0.6520 0.5878 0.042 Uiso 1 1 calc R . .
H3B H 0.1064 0.5943 0.5636 0.042 Uiso 1 1 calc R . .
C4 C 0.1712(3) 0.6496(2) 0.6655(2) 0.0463(10) Uani 1 1 d . . .
H4A H 0.1322 0.6249 0.7066 0.069 Uiso 1 1 calc R . .
H4B H 0.1777 0.6980 0.6808 0.069 Uiso 1 1 calc R . .
H4C H 0.2479 0.6304 0.6634 0.069 Uiso 1 1 calc R . .
N1 N 0.0617(2) 0.89649(13) 0.26311(16) 0.0292(7) Uani 1 1 d . . .
C11 C 0.1132(3) 0.93607(17) 0.20779(19) 0.0299(9) Uani 1 1 d . . .
C12 C 0.0562(3) 0.99469(17) 0.1762(2) 0.0331(9) Uani 1 1 d . . .
H12 H 0.0919 1.0231 0.1392 0.040 Uiso 1 1 calc R . .
C13 C -0.0500(3) 1.01223(18) 0.1972(2) 0.0364(9) Uani 1 1 d . . .
H13 H -0.0881 1.0519 0.1746 0.044 Uiso 1 1 calc R . .
C14 C -0.1001(3) 0.97111(17) 0.2518(2) 0.0339(9) Uani 1 1 d . . .
H14 H -0.1738 0.9821 0.2670 0.041 Uiso 1 1 calc R . .
C15 C -0.0431(3) 0.91406(16) 0.28435(19) 0.0287(9) Uani 1 1 d . . .
C16 C -0.0976(3) 0.86971(17) 0.3446(2) 0.0370(9) Uani 1 1 d . . .
H16A H -0.0677 0.8231 0.3424 0.056 Uiso 1 1 calc R . .
H16B H -0.1808 0.8692 0.3302 0.056 Uiso 1 1 calc R . .
H16C H -0.0798 0.8880 0.4006 0.056 Uiso 1 1 calc R . .
N2 N 0.2408(2) 0.75975(15) 0.18393(16) 0.0332(7) Uani 1 1 d . . .
C21 C 0.2642(3) 0.81337(17) 0.1339(2) 0.0291(9) Uani 1 1 d . . .
C22 C 0.2881(3) 0.79910(18) 0.0533(2) 0.0332(9) Uani 1 1 d . . .
H22 H 0.3057 0.8357 0.0185 0.040 Uiso 1 1 calc R . .
C23 C 0.2868(3) 0.7334(2) 0.0236(2) 0.0398(10) Uani 1 1 d . . .
H23 H 0.3026 0.7245 -0.0314 0.048 Uiso 1 1 calc R . .
C24 C 0.2622(3) 0.68097(19) 0.0748(2) 0.0406(10) Uani 1 1 d . . .
H24 H 0.2596 0.6352 0.0552 0.049 Uiso 1 1 calc R . .
C25 C 0.2412(3) 0.69496(17) 0.1550(2) 0.0330(9) Uani 1 1 d . . .
C26 C 0.2199(4) 0.63695(18) 0.2116(2) 0.0551(11) Uani 1 1 d . . .
H26A H 0.2366 0.6518 0.2691 0.083 Uiso 1 1 calc R . .
H26B H 0.2696 0.5984 0.2012 0.083 Uiso 1 1 calc R . .
H26C H 0.1396 0.6228 0.2016 0.083 Uiso 1 1 calc R . .
N3 N 0.3760(2) 0.88614(13) 0.34216(18) 0.0326(7) Uani 1 1 d . . .
C31 C 0.3824(3) 0.92352(17) 0.2712(2) 0.0310(9) Uani 1 1 d . . .
C32 C 0.4695(3) 0.97261(18) 0.2704(2) 0.0386(10) Uani 1 1 d . . .
H32 H 0.4747 0.9988 0.2219 0.046 Uiso 1 1 calc R . .
C33 C 0.5476(3) 0.98353(19) 0.3387(2) 0.0467(10) Uani 1 1 d . . .
H33 H 0.6064 1.0167 0.3375 0.056 Uiso 1 1 calc R . .
C34 C 0.5385(3) 0.94545(19) 0.4081(2) 0.0426(10) Uani 1 1 d . . .
H34 H 0.5911 0.9523 0.4559 0.051 Uiso 1 1 calc R . .
C35 C 0.4524(3) 0.89674(17) 0.4090(2) 0.0339(9) Uani 1 1 d . . .
C36 C 0.4442(3) 0.85634(19) 0.4859(2) 0.0453(10) Uani 1 1 d . . .
H36A H 0.3667 0.8376 0.4853 0.068 Uiso 1 1 calc R . .
H36B H 0.4607 0.8861 0.5342 0.068 Uiso 1 1 calc R . .
H36C H 0.4998 0.8188 0.4888 0.068 Uiso 1 1 calc R . .
N4 N 0.3416(2) 0.71620(13) 0.38875(16) 0.0296(7) Uani 1 1 d . . .
C41 C 0.3025(3) 0.68639(16) 0.4566(2) 0.0269(9) Uani 1 1 d . . .
C42 C 0.3774(3) 0.64667(16) 0.5083(2) 0.0313(9) Uani 1 1 d . . .
H42 H 0.3500 0.6246 0.5542 0.038 Uiso 1 1 calc R . .
C43 C 0.4908(3) 0.63829(17) 0.4947(2) 0.0376(9) Uani 1 1 d . . .
H43 H 0.5420 0.6126 0.5319 0.045 Uiso 1 1 calc R . .
C44 C 0.5272(3) 0.66821(17) 0.4260(2) 0.0322(9) Uani 1 1 d . . .
H44 H 0.6043 0.6630 0.4146 0.039 Uiso 1 1 calc R . .
C45 C 0.4512(3) 0.70605(16) 0.3734(2) 0.0315(9) Uani 1 1 d . . .
C46 C 0.4920(3) 0.7367(2) 0.2971(2) 0.0521(11) Uani 1 1 d . . .
H46A H 0.4651 0.7840 0.2909 0.078 Uiso 1 1 calc R . .
H46B H 0.4615 0.7101 0.2486 0.078 Uiso 1 1 calc R . .
H46C H 0.5759 0.7359 0.3020 0.078 Uiso 1 1 calc R . .
N5 N 0.0293(2) 0.71778(13) 0.31480(17) 0.0292(7) Uani 1 1 d . . .
C51 C 0.0302(3) 0.67871(16) 0.3847(2) 0.0274(8) Uani 1 1 d . . .
C52 C -0.0498(3) 0.62574(17) 0.3864(2) 0.0342(9) Uani 1 1 d . . .
H52 H -0.0480 0.5974 0.4339 0.041 Uiso 1 1 calc R . .
C53 C -0.1314(3) 0.61414(19) 0.3199(2) 0.0410(10) Uani 1 1 d . . .
H53 H -0.1862 0.5787 0.3217 0.049 Uiso 1 1 calc R . .
C54 C -0.1314(3) 0.65474(18) 0.2514(2) 0.0386(10) Uani 1 1 d . . .
H54 H -0.1872 0.6480 0.2054 0.046 Uiso 1 1 calc R . .
C55 C -0.0495(3) 0.70596(16) 0.2495(2) 0.0321(9) Uani 1 1 d . . .
C56 C -0.0474(3) 0.74842(18) 0.1732(2) 0.0416(10) Uani 1 1 d . . .
H56A H -0.0396 0.7967 0.1886 0.062 Uiso 1 1 calc R . .
H56B H -0.1189 0.7417 0.1371 0.062 Uiso 1 1 calc R . .
H56C H 0.0176 0.7346 0.1440 0.062 Uiso 1 1 calc R . .
N6 N 0.1555(2) 0.85168(14) 0.46271(16) 0.0298(7) Uani 1 1 d . . .
C61 C 0.1215(3) 0.79963(16) 0.5114(2) 0.0293(9) Uani 1 1 d . . .
C62 C 0.0729(3) 0.81659(19) 0.5839(2) 0.0373(10) Uani 1 1 d . . .
H62 H 0.0478 0.7811 0.6174 0.045 Uiso 1 1 calc R . .
C63 C 0.0609(3) 0.8832(2) 0.6074(2) 0.0458(10) Uani 1 1 d . . .
H63 H 0.0270 0.8941 0.6561 0.055 Uiso 1 1 calc R . .
C64 C 0.0989(3) 0.93386(19) 0.5590(2) 0.0407(10) Uani 1 1 d . . .
H64 H 0.0937 0.9803 0.5751 0.049 Uiso 1 1 calc R . .
C65 C 0.1448(3) 0.91747(18) 0.4870(2) 0.0320(9) Uani 1 1 d . . .
C66 C 0.1859(3) 0.97362(17) 0.4346(2) 0.0419(10) Uani 1 1 d . . .
H66A H 0.1648 0.9630 0.3761 0.063 Uiso 1 1 calc R . .
H66B H 0.2694 0.9776 0.4453 0.063 Uiso 1 1 calc R . .
H66C H 0.1505 1.0169 0.4481 0.063 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
Ca1 N4 2.528(3) . ?
Ca1 N2 2.535(3) . ?
Ca1 N6 2.549(3) . ?
Ca1 N1 2.571(3) . ?
Ca1 N5 2.608(3) . ?
Ca1 N3 2.613(3) . ?
Ca1 Al1 3.4581(11) . ?
Ca1 Al2 3.4664(11) . ?
Al1 C1 1.986(3) . ?
Al1 C31 2.019(3) . ?
Al1 C11 2.032(3) . ?
Al1 C21 2.035(3) . ?
Al2 C3 1.980(3) . ?
Al2 C51 2.019(3) . ?
Al2 C41 2.030(3) . ?
Al2 C61 2.033(3) . ?
C1 C2 1.538(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.535(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N1 C15 1.359(4) . ?
N1 C11 1.377(4) . ?
C11 C12 1.398(5) . ?
C12 C13 1.372(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.504(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N2 C25 1.353(4) . ?
N2 C21 1.375(4) . ?
C21 C22 1.399(5) . ?
C22 C23 1.373(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.500(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
N3 C35 1.350(4) . ?
N3 C31 1.377(4) . ?
C31 C32 1.404(5) . ?
C32 C33 1.380(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.368(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.390(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.493(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N4 C45 1.353(4) . ?
N4 C41 1.372(4) . ?
C41 C42 1.387(5) . ?
C42 C43 1.384(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.372(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.383(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.504(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N5 C55 1.352(4) . ?
N5 C51 1.371(4) . ?
C51 C52 1.401(5) . ?
C52 C53 1.385(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.369(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.393(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.496(5) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
N6 C65 1.357(4) . ?
N6 C61 1.376(4) . ?
C61 C62 1.407(5) . ?
C62 C63 1.370(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.370(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.381(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.503(5) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 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
N4 Ca1 N2 88.14(9) . . ?
N4 Ca1 N6 94.15(9) . . ?
N2 Ca1 N6 177.65(9) . . ?
N4 Ca1 N1 177.34(8) . . ?
N2 Ca1 N1 93.53(9) . . ?
N6 Ca1 N1 84.16(8) . . ?
N4 Ca1 N5 93.27(9) . . ?
N2 Ca1 N5 86.99(9) . . ?
N6 Ca1 N5 93.40(9) . . ?
N1 Ca1 N5 88.89(9) . . ?
N4 Ca1 N3 84.11(9) . . ?
N2 Ca1 N3 94.94(9) . . ?
N6 Ca1 N3 84.78(9) . . ?
N1 Ca1 N3 93.68(9) . . ?
N5 Ca1 N3 176.68(9) . . ?
N4 Ca1 Al1 121.83(7) . . ?
N2 Ca1 Al1 58.24(7) . . ?
N6 Ca1 Al1 119.88(7) . . ?
N1 Ca1 Al1 57.68(7) . . ?
N5 Ca1 Al1 126.23(7) . . ?
N3 Ca1 Al1 57.06(7) . . ?
N4 Ca1 Al2 57.64(7) . . ?
N2 Ca1 Al2 123.97(7) . . ?
N6 Ca1 Al2 57.96(6) . . ?
N1 Ca1 Al2 122.69(7) . . ?
N5 Ca1 Al2 56.39(6) . . ?
N3 Ca1 Al2 120.33(7) . . ?
Al1 Ca1 Al2 177.20(3) . . ?
C1 Al1 C31 109.75(15) . . ?
C1 Al1 C11 111.43(15) . . ?
C31 Al1 C11 105.67(13) . . ?
C1 Al1 C21 112.69(14) . . ?
C31 Al1 C21 109.06(14) . . ?
C11 Al1 C21 107.98(13) . . ?
C1 Al1 Ca1 179.68(12) . . ?
C31 Al1 Ca1 69.95(10) . . ?
C11 Al1 Ca1 68.62(10) . . ?
C21 Al1 Ca1 67.56(10) . . ?
C3 Al2 C51 110.34(14) . . ?
C3 Al2 C41 114.39(14) . . ?
C51 Al2 C41 108.62(13) . . ?
C3 Al2 C61 109.94(15) . . ?
C51 Al2 C61 106.39(14) . . ?
C41 Al2 C61 106.80(13) . . ?
C3 Al2 Ca1 177.30(11) . . ?
C51 Al2 Ca1 70.18(10) . . ?
C41 Al2 Ca1 67.58(10) . . ?
C61 Al2 Ca1 67.47(10) . . ?
C2 C1 Al1 120.4(2) . . ?
C2 C1 H1A 107.2 . . ?
Al1 C1 H1A 107.2 . . ?
C2 C1 H1B 107.2 . . ?
Al1 C1 H1B 107.2 . . ?
H1A C1 H1B 106.9 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 Al2 120.7(2) . . ?
C4 C3 H3A 107.1 . . ?
Al2 C3 H3A 107.1 . . ?
C4 C3 H3B 107.1 . . ?
Al2 C3 H3B 107.1 . . ?
H3A C3 H3B 106.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C15 N1 C11 119.9(3) . . ?
C15 N1 Ca1 129.3(2) . . ?
C11 N1 Ca1 110.3(2) . . ?
N1 C11 C12 118.4(3) . . ?
N1 C11 Al1 122.9(2) . . ?
C12 C11 Al1 118.7(3) . . ?
C13 C12 C11 121.7(3) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C14 118.6(3) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
N1 C15 C14 121.5(3) . . ?
N1 C15 C16 118.8(3) . . ?
C14 C15 C16 119.7(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C25 N2 C21 120.0(3) . . ?
C25 N2 Ca1 129.7(2) . . ?
C21 N2 Ca1 110.3(2) . . ?
N2 C21 C22 118.5(3) . . ?
N2 C21 Al1 123.9(2) . . ?
C22 C21 Al1 117.6(3) . . ?
C23 C22 C21 121.5(3) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C24 118.7(3) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C23 C24 C25 119.8(3) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
N2 C25 C24 121.5(3) . . ?
N2 C25 C26 119.2(3) . . ?
C24 C25 C26 119.3(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C35 N3 C31 120.2(3) . . ?
C35 N3 Ca1 129.3(2) . . ?
C31 N3 Ca1 110.5(2) . . ?
N3 C31 C32 118.5(3) . . ?
N3 C31 Al1 122.5(2) . . ?
C32 C31 Al1 119.0(3) . . ?
C33 C32 C31 121.4(3) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C34 C33 C32 118.5(3) . . ?
C34 C33 H33 120.8 . . ?
C32 C33 H33 120.8 . . ?
C33 C34 C35 120.3(3) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
N3 C35 C34 121.2(3) . . ?
N3 C35 C36 119.8(3) . . ?
C34 C35 C36 119.0(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C45 N4 C41 119.6(3) . . ?
C45 N4 Ca1 128.1(2) . . ?
C41 N4 Ca1 111.1(2) . . ?
N4 C41 C42 118.8(3) . . ?
N4 C41 Al2 122.9(2) . . ?
C42 C41 Al2 118.3(2) . . ?
C43 C42 C41 121.9(3) . . ?
C43 C42 H42 119.1 . . ?
C41 C42 H42 119.1 . . ?
C44 C43 C42 118.0(3) . . ?
C44 C43 H43 121.0 . . ?
C42 C43 H43 121.0 . . ?
C43 C44 C45 119.8(3) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
N4 C45 C44 121.8(3) . . ?
N4 C45 C46 119.3(3) . . ?
C44 C45 C46 118.9(3) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C55 N5 C51 120.1(3) . . ?
C55 N5 Ca1 127.9(2) . . ?
C51 N5 Ca1 111.9(2) . . ?
N5 C51 C52 118.9(3) . . ?
N5 C51 Al2 121.1(2) . . ?
C52 C51 Al2 120.0(3) . . ?
C53 C52 C51 121.0(3) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
C54 C53 C52 118.8(3) . . ?
C54 C53 H53 120.6 . . ?
C52 C53 H53 120.6 . . ?
C53 C54 C55 119.8(3) . . ?
C53 C54 H54 120.1 . . ?
C55 C54 H54 120.1 . . ?
N5 C55 C54 121.4(3) . . ?
N5 C55 C56 119.1(3) . . ?
C54 C55 C56 119.5(3) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C65 N6 C61 119.5(3) . . ?
C65 N6 Ca1 130.0(2) . . ?
C61 N6 Ca1 109.6(2) . . ?
N6 C61 C62 118.6(3) . . ?
N6 C61 Al2 123.8(2) . . ?
C62 C61 Al2 117.6(3) . . ?
C63 C62 C61 121.5(3) . . ?
C63 C62 H62 119.3 . . ?
C61 C62 H62 119.3 . . ?
C62 C63 C64 118.6(3) . . ?
C62 C63 H63 120.7 . . ?
C64 C63 H63 120.7 . . ?
C63 C64 C65 120.1(3) . . ?
C63 C64 H64 120.0 . . ?
C65 C64 H64 120.0 . . ?
N6 C65 C64 121.7(3) . . ?
N6 C65 C66 118.8(3) . . ?
C64 C65 C66 119.5(3) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        47.22
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 993341'
