# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4a
_database_code_depnum_ccdc_archive 'CCDC 1489247'
_audit_update_record             
;
2016-07-26 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
# local name mc15023
_audit_creation_date             2016-07-26
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.07.25 svn.r3318 for OlexSys, GUI svn.r5204)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H43 Al N2'
_chemical_formula_sum            'C27 H43 Al N2'
_chemical_formula_weight         422.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C27 H43 Al N2'
_chemical_oxdiff_usercomment     '@ 120 K SU222'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.7729(3)
_cell_length_b                   15.6899(4)
_cell_length_c                   16.0285(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.321(3)
_cell_angle_gamma                90
_cell_volume                     2612.93(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12723
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.0200
_cell_measurement_theta_min      3.6800
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from hexane by slow cooling'
_exptl_crystal_size_max          0.4194
_exptl_crystal_size_mid          0.1993
_exptl_crystal_size_min          0.1131
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46010
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.719
_diffrn_reflns_theta_min         3.122
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -79.00   17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -57.0000  -30.0000 96

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000   30.0000 51

#__ type_ start__ end____ width___ exp.time_
  3 omega  -63.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -77.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
  4 omega  -16.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372   57.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
  5 omega  -63.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -77.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
  6 omega  -21.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372   77.0000 -150.0000 106

#__ type_ start__ end____ width___ exp.time_
  7 omega    2.00   57.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -125.0000  -75.0000 55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0403734000
_diffrn_orient_matrix_UB_12      -0.0363573000
_diffrn_orient_matrix_UB_13      -0.0097716000
_diffrn_orient_matrix_UB_21      -0.0550084000
_diffrn_orient_matrix_UB_22      0.0266807000
_diffrn_orient_matrix_UB_23      -0.0077234000
_diffrn_orient_matrix_UB_31      -0.0001017000
_diffrn_orient_matrix_UB_32      0.0034142000
_diffrn_orient_matrix_UB_33      -0.0441502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5373
_reflns_number_total             6853
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6853
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0459P)²+1.5029P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1278
_refine_special_details          
;
The hydride was located in a difference Fourier map and refined freely.

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
906_ALERT_3_C Large K value in the Analysis of Variance ......      4.634 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Th(Min) ...         10 Report
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          3 Report
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1 Note

Not important

#===============================================================================
069_ALERT_1_G Atom Label without Numerical Part ..............          H Do !
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        557 Note

Not important

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C26(H26A,
 H26B,H26C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.79265(4) 0.33070(3) 0.20056(3) 0.01830(12) Uani 1 1 d . . . . .
H H 0.7716(17) 0.3166(11) 0.1039(11) 0.028(5) Uiso 1 1 d . . . . .
N1 N 0.71249(12) 0.14497(8) 0.20562(8) 0.0195(3) Uani 1 1 d . . . . .
N2 N 0.79560(11) 0.18690(8) 0.33492(8) 0.0179(3) Uani 1 1 d . . . . .
C1 C 0.76780(14) 0.21372(9) 0.25183(9) 0.0179(3) Uani 1 1 d . . . . .
C8 C 0.75675(14) 0.10316(9) 0.34080(10) 0.0201(3) Uani 1 1 d . . . . .
C9 C 0.70497(14) 0.07639(10) 0.25886(10) 0.0215(3) Uani 1 1 d . . . . .
C10 C 0.85727(15) 0.23836(10) 0.41021(9) 0.0234(3) Uani 1 1 d . . . . .
H10A H 0.7976 0.2464 0.4463 0.035 Uiso 1 1 calc GR . . . .
H10B H 0.8807 0.2940 0.3911 0.035 Uiso 1 1 calc GR . . . .
H10C H 0.9349 0.2093 0.4438 0.035 Uiso 1 1 calc GR . . . .
C11 C 0.77533(18) 0.05798(10) 0.42496(10) 0.0287(4) Uani 1 1 d . . . . .
H11A H 0.8674 0.0482 0.4506 0.043 Uiso 1 1 calc GR . . . .
H11B H 0.7301 0.0032 0.4154 0.043 Uiso 1 1 calc GR . . . .
H11C H 0.7407 0.0929 0.4643 0.043 Uiso 1 1 calc GR . . . .
C12 C 0.65032(17) -0.00782(11) 0.22413(11) 0.0315(4) Uani 1 1 d . . . . .
H12A H 0.5657 0.0007 0.1834 0.047 Uiso 1 1 calc GR . . . .
H12B H 0.6413 -0.0441 0.2719 0.047 Uiso 1 1 calc GR . . . .
H12C H 0.7081 -0.0353 0.1943 0.047 Uiso 1 1 calc GR . . . .
C13 C 0.66085(16) 0.14232(11) 0.11178(10) 0.0277(3) Uani 1 1 d . . . . .
H13A H 0.5673 0.1347 0.0975 0.042 Uiso 1 1 calc GR . . . .
H13B H 0.6997 0.0946 0.0882 0.042 Uiso 1 1 calc GR . . . .
H13C H 0.6809 0.1959 0.0867 0.042 Uiso 1 1 calc GR . . . .
C5 C 0.98296(14) 0.37385(10) 0.23392(9) 0.0211(3) Uani 1 1 d . . . . .
C7 C 1.04554(14) 0.28907(10) 0.24205(10) 0.0223(3) Uani 1 1 d . . . . .
C22 C 1.10865(14) 0.27535(10) 0.32674(10) 0.0241(3) Uani 1 1 d . . . . .
C21 C 1.10102(15) 0.35193(11) 0.37554(10) 0.0251(3) Uani 1 1 d . . . . .
C6 C 1.02950(15) 0.41091(10) 0.32122(10) 0.0237(3) Uani 1 1 d . . . . .
C23 C 0.99576(18) 0.43057(12) 0.15877(11) 0.0335(4) Uani 1 1 d . . . . .
H23A H 0.9669 0.3990 0.1043 0.050 Uiso 1 1 calc GR . . . .
H23B H 1.0860 0.4473 0.1676 0.050 Uiso 1 1 calc GR . . . .
H23C H 0.9426 0.4817 0.1563 0.050 Uiso 1 1 calc GR . . . .
C25 C 1.03957(17) 0.23019(12) 0.16710(11) 0.0322(4) Uani 1 1 d . . . . .
H25A H 0.9510 0.2102 0.1438 0.048 Uiso 1 1 calc GR . . . .
H25B H 1.0963 0.1813 0.1867 0.048 Uiso 1 1 calc GR . . . .
H25C H 1.0676 0.2607 0.1219 0.048 Uiso 1 1 calc GR . . . .
C27 C 1.17184(18) 0.19371(12) 0.36568(13) 0.0364(4) Uani 1 1 d . . . . .
H27A H 1.1257 0.1707 0.4058 0.055 Uiso 1 1 calc GR . . . .
H27B H 1.2615 0.2051 0.3970 0.055 Uiso 1 1 calc GR . . . .
H27C H 1.1694 0.1522 0.3196 0.055 Uiso 1 1 calc GR . . . .
C26 C 1.16436(19) 0.36138(14) 0.47054(11) 0.0406(5) Uani 1 1 d . . . . .
H26A H 1.1342 0.3161 0.5025 0.061 Uiso 1 1 calc GR . . . .
H26B H 1.1422 0.4170 0.4904 0.061 Uiso 1 1 calc GR . . . .
H26C H 1.2579 0.3572 0.4807 0.061 Uiso 1 1 calc GR . . . .
C24 C 1.01271(18) 0.50337(11) 0.34013(13) 0.0354(4) Uani 1 1 d . . . . .
H24A H 1.0684 0.5382 0.3143 0.053 Uiso 1 1 calc GR . . . .
H24B H 1.0361 0.5123 0.4029 0.053 Uiso 1 1 calc GR . . . .
H24C H 0.9227 0.5199 0.3156 0.053 Uiso 1 1 calc GR . . . .
C2 C 0.64198(15) 0.40862(10) 0.21350(10) 0.0218(3) Uani 1 1 d . . . . .
C4 C 0.53977(14) 0.35407(10) 0.16120(10) 0.0223(3) Uani 1 1 d . . . . .
C15 C 0.49270(14) 0.30328(10) 0.21574(10) 0.0228(3) Uani 1 1 d . . . . .
C14 C 0.55419(14) 0.32739(10) 0.30388(10) 0.0214(3) Uani 1 1 d . . . . .
C3 C 0.63930(14) 0.39216(10) 0.30369(9) 0.0216(3) Uani 1 1 d . . . . .
C16 C 0.65686(18) 0.49913(11) 0.18281(12) 0.0320(4) Uani 1 1 d . . . . .
H16A H 0.7295 0.5270 0.2236 0.048 Uiso 1 1 calc GR . . . .
H16B H 0.5778 0.5314 0.1797 0.048 Uiso 1 1 calc GR . . . .
H16C H 0.6728 0.4972 0.1254 0.048 Uiso 1 1 calc GR . . . .
C18 C 0.49249(17) 0.35866(12) 0.06428(10) 0.0318(4) Uani 1 1 d . . . . .
H18A H 0.4568 0.4154 0.0472 0.048 Uiso 1 1 calc GR . . . .
H18B H 0.4255 0.3156 0.0437 0.048 Uiso 1 1 calc GR . . . .
H18C H 0.5643 0.3480 0.0388 0.048 Uiso 1 1 calc GR . . . .
C20 C 0.39423(17) 0.23368(12) 0.19243(12) 0.0343(4) Uani 1 1 d . . . . .
H20A H 0.3616 0.2303 0.1294 0.051 Uiso 1 1 calc GR . . . .
H20B H 0.3229 0.2460 0.2179 0.051 Uiso 1 1 calc GR . . . .
H20C H 0.4338 0.1792 0.2148 0.051 Uiso 1 1 calc GR . . . .
C19 C 0.52237(17) 0.28621(12) 0.38017(11) 0.0317(4) Uani 1 1 d . . . . .
H19A H 0.5761 0.3110 0.4337 0.048 Uiso 1 1 calc GR . . . .
H19B H 0.5388 0.2248 0.3795 0.048 Uiso 1 1 calc GR . . . .
H19C H 0.4314 0.2959 0.3771 0.048 Uiso 1 1 calc GR . . . .
C17 C 0.71225(17) 0.44331(11) 0.37998(11) 0.0301(4) Uani 1 1 d . . . . .
H17A H 0.8047 0.4334 0.3895 0.045 Uiso 1 1 calc GR . . . .
H17B H 0.6860 0.4260 0.4315 0.045 Uiso 1 1 calc GR . . . .
H17C H 0.6937 0.5040 0.3688 0.045 Uiso 1 1 calc GR . . . .


_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 H 1.522(18) . ?
Al1 C1 2.0571(15) . ?
Al1 C5 2.0901(15) . ?
Al1 C2 2.0857(16) . ?
N1 C1 1.3542(18) . ?
N1 C9 1.3890(19) . ?
N1 C13 1.4598(19) . ?
N2 C1 1.3527(18) . ?
N2 C8 1.3897(18) . ?
N2 C10 1.4581(18) . ?
C8 C9 1.351(2) . ?
C8 C11 1.490(2) . ?
C9 C12 1.493(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C5 C7 1.481(2) . ?
C5 C6 1.475(2) . ?
C5 C23 1.533(2) . ?
C7 C22 1.365(2) . ?
C7 C25 1.503(2) . ?
C22 C21 1.448(2) . ?
C22 C27 1.506(2) . ?
C21 C6 1.361(2) . ?
C21 C26 1.502(2) . ?
C6 C24 1.503(2) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C2 C4 1.470(2) . ?
C2 C3 1.476(2) . ?
C2 C16 1.525(2) . ?
C4 C15 1.375(2) . ?
C4 C18 1.503(2) . ?
C15 C14 1.443(2) . ?
C15 C20 1.499(2) . ?
C14 C3 1.369(2) . ?
C14 C19 1.501(2) . ?
C3 C17 1.500(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 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
C1 Al1 H 106.1(7) . . ?
C1 Al1 C5 114.16(6) . . ?
C1 Al1 C2 107.24(6) . . ?
C5 Al1 H 100.3(7) . . ?
C2 Al1 H 106.0(7) . . ?
C2 Al1 C5 121.42(6) . . ?
C1 N1 C9 111.69(12) . . ?
C1 N1 C13 125.39(13) . . ?
C9 N1 C13 122.87(13) . . ?
C1 N2 C8 111.63(12) . . ?
C1 N2 C10 125.21(12) . . ?
C8 N2 C10 123.16(12) . . ?
N1 C1 Al1 125.24(10) . . ?
N2 C1 Al1 130.73(10) . . ?
N2 C1 N1 103.99(12) . . ?
N2 C8 C11 122.71(13) . . ?
C9 C8 N2 106.40(13) . . ?
C9 C8 C11 130.89(14) . . ?
N1 C9 C12 122.53(14) . . ?
C8 C9 N1 106.28(13) . . ?
C8 C9 C12 131.18(14) . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C5 Al1 97.15(9) . . ?
C7 C5 C23 117.20(13) . . ?
C6 C5 Al1 115.77(10) . . ?
C6 C5 C7 103.75(13) . . ?
C6 C5 C23 115.97(13) . . ?
C23 C5 Al1 105.84(10) . . ?
C5 C7 C25 123.99(14) . . ?
C22 C7 C5 108.94(13) . . ?
C22 C7 C25 127.06(15) . . ?
C7 C22 C21 108.78(14) . . ?
C7 C22 C27 126.72(16) . . ?
C21 C22 C27 124.46(15) . . ?
C22 C21 C26 123.64(16) . . ?
C6 C21 C22 108.78(14) . . ?
C6 C21 C26 127.58(16) . . ?
C5 C6 C24 122.88(15) . . ?
C21 C6 C5 109.37(14) . . ?
C21 C6 C24 127.24(15) . . ?
C5 C23 H23A 109.5 . . ?
C5 C23 H23B 109.5 . . ?
C5 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C7 C25 H25A 109.5 . . ?
C7 C25 H25B 109.5 . . ?
C7 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C6 C24 H24A 109.5 . . ?
C6 C24 H24B 109.5 . . ?
C6 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C2 Al1 95.01(9) . . ?
C4 C2 C3 104.55(12) . . ?
C4 C2 C16 119.02(14) . . ?
C3 C2 Al1 102.23(10) . . ?
C3 C2 C16 120.64(13) . . ?
C16 C2 Al1 111.28(11) . . ?
C2 C4 C18 124.04(14) . . ?
C15 C4 C2 108.75(13) . . ?
C15 C4 C18 127.13(15) . . ?
C4 C15 C14 108.62(14) . . ?
C4 C15 C20 128.26(15) . . ?
C14 C15 C20 123.12(14) . . ?
C15 C14 C19 122.69(14) . . ?
C3 C14 C15 109.08(13) . . ?
C3 C14 C19 128.22(14) . . ?
C2 C3 C17 124.28(14) . . ?
C14 C3 C2 108.56(13) . . ?
C14 C3 C17 127.04(14) . . ?
C2 C16 H16A 109.5 . . ?
C2 C16 H16B 109.5 . . ?
C2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C4 C18 H18A 109.5 . . ?
C4 C18 H18B 109.5 . . ?
C4 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C17 H17A 109.5 . . ?
C3 C17 H17B 109.5 . . ?
C3 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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
Al1 C5 C7 C22 -112.56(11) . . . . ?
Al1 C5 C7 C25 68.24(15) . . . . ?
Al1 C5 C6 C21 100.19(14) . . . . ?
Al1 C5 C6 C24 -87.43(16) . . . . ?
Al1 C2 C4 C15 97.48(12) . . . . ?
Al1 C2 C4 C18 -85.59(15) . . . . ?
Al1 C2 C3 C14 -92.28(12) . . . . ?
Al1 C2 C3 C17 91.52(15) . . . . ?
N2 C8 C9 N1 -0.68(16) . . . . ?
N2 C8 C9 C12 178.18(16) . . . . ?
C1 N1 C9 C8 0.19(17) . . . . ?
C1 N1 C9 C12 -178.79(14) . . . . ?
C1 N2 C8 C9 0.97(16) . . . . ?
C1 N2 C8 C11 -179.72(14) . . . . ?
C8 N2 C1 Al1 176.98(11) . . . . ?
C8 N2 C1 N1 -0.83(15) . . . . ?
C9 N1 C1 Al1 -177.58(10) . . . . ?
C9 N1 C1 N2 0.39(16) . . . . ?
C10 N2 C1 Al1 -2.4(2) . . . . ?
C10 N2 C1 N1 179.80(13) . . . . ?
C10 N2 C8 C9 -179.65(13) . . . . ?
C10 N2 C8 C11 -0.3(2) . . . . ?
C11 C8 C9 N1 -179.90(15) . . . . ?
C11 C8 C9 C12 -1.0(3) . . . . ?
C13 N1 C1 Al1 -0.2(2) . . . . ?
C13 N1 C1 N2 177.76(13) . . . . ?
C13 N1 C9 C8 -177.25(13) . . . . ?
C13 N1 C9 C12 3.8(2) . . . . ?
C5 C7 C22 C21 -5.34(17) . . . . ?
C5 C7 C22 C27 172.26(15) . . . . ?
C7 C5 C6 C21 -4.90(16) . . . . ?
C7 C5 C6 C24 167.47(14) . . . . ?
C7 C22 C21 C6 2.18(18) . . . . ?
C7 C22 C21 C26 -177.49(15) . . . . ?
C22 C21 C6 C5 1.92(17) . . . . ?
C22 C21 C6 C24 -170.03(15) . . . . ?
C6 C5 C7 C22 6.24(16) . . . . ?
C6 C5 C7 C25 -172.96(14) . . . . ?
C23 C5 C7 C22 135.50(14) . . . . ?
C23 C5 C7 C25 -43.7(2) . . . . ?
C23 C5 C6 C21 -134.90(15) . . . . ?
C23 C5 C6 C24 37.5(2) . . . . ?
C25 C7 C22 C21 173.83(15) . . . . ?
C25 C7 C22 C27 -8.6(3) . . . . ?
C27 C22 C21 C6 -175.49(15) . . . . ?
C27 C22 C21 C26 4.8(2) . . . . ?
C26 C21 C6 C5 -178.42(15) . . . . ?
C26 C21 C6 C24 9.6(3) . . . . ?
C2 C4 C15 C14 4.51(17) . . . . ?
C2 C4 C15 C20 -175.61(16) . . . . ?
C4 C2 C3 C14 6.27(16) . . . . ?
C4 C2 C3 C17 -169.93(14) . . . . ?
C4 C15 C14 C3 -0.45(18) . . . . ?
C4 C15 C14 C19 178.29(14) . . . . ?
C15 C14 C3 C2 -3.77(17) . . . . ?
C15 C14 C3 C17 172.29(15) . . . . ?
C3 C2 C4 C15 -6.56(16) . . . . ?
C3 C2 C4 C18 170.37(14) . . . . ?
C16 C2 C4 C15 -144.80(14) . . . . ?
C16 C2 C4 C18 32.1(2) . . . . ?
C16 C2 C3 C14 143.67(15) . . . . ?
C16 C2 C3 C17 -32.5(2) . . . . ?
C18 C4 C15 C14 -172.30(15) . . . . ?
C18 C4 C15 C20 7.6(3) . . . . ?
C20 C15 C14 C3 179.66(15) . . . . ?
C20 C15 C14 C19 -1.6(2) . . . . ?
C19 C14 C3 C2 177.57(15) . . . . ?
C19 C14 C3 C17 -6.4(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
13 9 1 0.0459 12.9884 8.9835 1.0115 -0.8609 -0.4826 -0.0153
-13 -9 -1 0.0672 -12.9884 -8.9835 -1.0115 0.8609 0.4826 0.0153
1 -1 -22 0.1976 1.0084 -0.9940 -21.9771 0.2102 0.0877 0.9668
0 1 22 0.1794 -0.0094 0.9934 21.9779 -0.2505 -0.1427 -0.9669
11 -14 0 0.0656 10.9878 -13.9918 0.0051 0.0650 -0.9778 -0.0491
-11 14 0 0.0656 -10.9878 13.9918 -0.0051 -0.0650 0.9778 0.0491
3 3 -22 0.1990 3.0070 3.0009 -21.9745 -0.0158 0.0844 0.9801
-3 -3 22 0.1990 -3.0070 -3.0009 21.9745 0.0158 -0.0844 -0.9801

_olex2_date_sample_submission    2015-11-17
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 'SU 222'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4b
_database_code_depnum_ccdc_archive 'CCDC 1489248'
_audit_update_record             
;
2016-07-26 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
# local name mc15012
_audit_creation_date             2016-07-26
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.07.25 svn.r3318 for OlexSys, GUI svn.r5204)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H51 Al N2'
_chemical_formula_sum            'C31 H51 Al N2'
_chemical_formula_weight         478.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H51 Al N2'
_chemical_oxdiff_usercomment     '@ 120 K SU126'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.8699(7)
_cell_length_b                   16.0945(13)
_cell_length_c                   20.2907(17)
_cell_angle_alpha                90
_cell_angle_beta                 98.473(7)
_cell_angle_gamma                90
_cell_volume                     2865.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3893
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.0810
_cell_measurement_theta_min      3.4270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_recrystallization_method 
'The material was recrystallised from d6-benzene by slow evaporation'
_exptl_crystal_size_max          0.2092
_exptl_crystal_size_mid          0.1046
_exptl_crystal_size_min          0.0495
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22402
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.119
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.8965  -99.0000  -90.0000 52

#__ type_ start__ end____ width___ exp.time_
  2 omega  -39.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.8965   77.0000  120.0000 79

#__ type_ start__ end____ width___ exp.time_
  3 omega  -64.00  -14.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.8965  -38.0000  150.0000 50

#__ type_ start__ end____ width___ exp.time_
  4 omega  -48.00   45.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        9.4590  -19.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        9.4590 -123.0000  178.0000 33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0331722000
_diffrn_orient_matrix_UB_12      0.0149930000
_diffrn_orient_matrix_UB_13      0.0274351000
_diffrn_orient_matrix_UB_21      0.0530089000
_diffrn_orient_matrix_UB_22      -0.0235755000
_diffrn_orient_matrix_UB_23      0.0220516000
_diffrn_orient_matrix_UB_31      0.0512350000
_diffrn_orient_matrix_UB_32      0.0340918000
_diffrn_orient_matrix_UB_33      0.0031556000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4180
_reflns_number_total             5441
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5441
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0602
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0303P)²+2.4805P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1262
_refine_special_details          
;
The hydride ligand was located in a difference Fourier map and refined freely.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
906_ALERT_3_C Large K value in the Analysis of Variance ......      9.230 Check
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.045 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Th(Min) ...         10 Report
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1 Note

Not significant.

#===============================================================================
066_ALERT_1_G Predicted and Reported Tmin&Tmax Range Identical          ? Check
069_ALERT_1_G Atom Label without Numerical Part ..............          H Do !
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.44779(7) 0.70712(4) 0.26041(3) 0.01381(17) Uani 1 1 d . . . . .
H H 0.454(3) 0.8037(15) 0.2654(12) 0.025(7) Uiso 1 1 d . . . . .
N1 N 0.2252(2) 0.59356(12) 0.32424(9) 0.0144(4) Uani 1 1 d . . . . .
N2 N 0.2484(2) 0.71339(12) 0.37197(9) 0.0154(4) Uani 1 1 d . . . . .
C1 C 0.2935(2) 0.66871(14) 0.32135(11) 0.0135(5) Uani 1 1 d . . . . .
C8 C 0.1399(2) 0.59066(16) 0.37652(11) 0.0178(5) Uani 1 1 d . . . . .
C9 C 0.1543(2) 0.66616(16) 0.40651(11) 0.0178(5) Uani 1 1 d . . . . .
C16 C 0.0500(3) 0.51793(17) 0.39457(13) 0.0246(6) Uani 1 1 d . . . . .
H16A H -0.0318 0.5057 0.3579 0.037 Uiso 1 1 calc GR . . . .
H16B H 0.0057 0.5308 0.4349 0.037 Uiso 1 1 calc GR . . . .
H16C H 0.1171 0.4695 0.4028 0.037 Uiso 1 1 calc GR . . . .
C17 C 0.0851(3) 0.69481(17) 0.46558(12) 0.0262(6) Uani 1 1 d . . . . .
H17A H 0.1659 0.7044 0.5032 0.039 Uiso 1 1 calc GR . . . .
H17B H 0.0151 0.6522 0.4776 0.039 Uiso 1 1 calc GR . . . .
H17C H 0.0290 0.7466 0.4545 0.039 Uiso 1 1 calc GR . . . .
C10 C 0.2373(2) 0.52756(15) 0.27448(12) 0.0175(5) Uani 1 1 d . . . . .
H10 H 0.3055 0.5494 0.2434 0.021 Uiso 1 1 calc R . . . .
C11 C 0.3112(3) 0.44891(16) 0.30552(14) 0.0269(6) Uani 1 1 d . . . . .
H11A H 0.4003 0.4636 0.3380 0.040 Uiso 1 1 calc GR . . . .
H11B H 0.3433 0.4139 0.2706 0.040 Uiso 1 1 calc GR . . . .
H11C H 0.2377 0.4185 0.3280 0.040 Uiso 1 1 calc GR . . . .
C12 C 0.0836(3) 0.51001(17) 0.23281(12) 0.0242(6) Uani 1 1 d . . . . .
H12A H 0.0192 0.4793 0.2597 0.036 Uiso 1 1 calc GR . . . .
H12B H 0.0986 0.4768 0.1938 0.036 Uiso 1 1 calc GR . . . .
H12C H 0.0341 0.5626 0.2181 0.036 Uiso 1 1 calc GR . . . .
C13 C 0.2884(3) 0.80263(15) 0.38263(11) 0.0179(5) Uani 1 1 d . . . . .
H13 H 0.3622 0.8165 0.3515 0.021 Uiso 1 1 calc R . . . .
C15 C 0.3684(3) 0.82055(17) 0.45240(12) 0.0255(6) Uani 1 1 d . . . . .
H15A H 0.2948 0.8172 0.4839 0.038 Uiso 1 1 calc GR . . . .
H15B H 0.4127 0.8764 0.4539 0.038 Uiso 1 1 calc GR . . . .
H15C H 0.4496 0.7796 0.4646 0.038 Uiso 1 1 calc GR . . . .
C14 C 0.1492(3) 0.85800(17) 0.36328(14) 0.0287(6) Uani 1 1 d . . . . .
H14A H 0.0978 0.8421 0.3190 0.043 Uiso 1 1 calc GR . . . .
H14B H 0.1817 0.9162 0.3625 0.043 Uiso 1 1 calc GR . . . .
H14C H 0.0789 0.8513 0.3959 0.043 Uiso 1 1 calc GR . . . .
C5 C 0.3781(3) 0.69399(15) 0.15839(11) 0.0160(5) Uani 1 1 d . . . . .
C6 C 0.3912(3) 0.61343(15) 0.12338(11) 0.0172(5) Uani 1 1 d . . . . .
C25 C 0.2503(3) 0.58572(15) 0.09761(12) 0.0192(5) Uani 1 1 d . . . . .
C26 C 0.1373(3) 0.64627(15) 0.11259(12) 0.0189(5) Uani 1 1 d . . . . .
C7 C 0.2098(3) 0.71057(15) 0.14677(11) 0.0174(5) Uani 1 1 d . . . . .
C27 C 0.4703(3) 0.76354(16) 0.12938(12) 0.0213(6) Uani 1 1 d . . . . .
H27A H 0.4582 0.8158 0.1528 0.032 Uiso 1 1 calc GR . . . .
H27B H 0.4326 0.7705 0.0818 0.032 Uiso 1 1 calc GR . . . .
H27C H 0.5784 0.7482 0.1352 0.032 Uiso 1 1 calc GR . . . .
C28 C 0.5391(3) 0.57754(17) 0.10862(13) 0.0266(6) Uani 1 1 d . . . . .
H28A H 0.5676 0.6043 0.0688 0.040 Uiso 1 1 calc GR . . . .
H28B H 0.5272 0.5177 0.1008 0.040 Uiso 1 1 calc GR . . . .
H28C H 0.6191 0.5873 0.1466 0.040 Uiso 1 1 calc GR . . . .
C30 C 0.2101(3) 0.50986(16) 0.05601(13) 0.0262(6) Uani 1 1 d . . . . .
H30A H 0.1647 0.5265 0.0110 0.039 Uiso 1 1 calc GR . . . .
H30B H 0.1368 0.4762 0.0761 0.039 Uiso 1 1 calc GR . . . .
H30C H 0.3024 0.4772 0.0537 0.039 Uiso 1 1 calc GR . . . .
C31 C -0.0307(3) 0.63737(17) 0.08882(13) 0.0261(6) Uani 1 1 d . . . . .
H31A H -0.0493 0.6384 0.0400 0.039 Uiso 1 1 calc GR . . . .
H31B H -0.0856 0.6834 0.1062 0.039 Uiso 1 1 calc GR . . . .
H31C H -0.0668 0.5845 0.1047 0.039 Uiso 1 1 calc GR . . . .
C29 C 0.1377(3) 0.78894(16) 0.16765(13) 0.0245(6) Uani 1 1 d . . . . .
H29A H 0.1824 0.8032 0.2133 0.037 Uiso 1 1 calc GR . . . .
H29B H 0.0277 0.7804 0.1657 0.037 Uiso 1 1 calc GR . . . .
H29C H 0.1558 0.8343 0.1376 0.037 Uiso 1 1 calc GR . . . .
C2 C 0.6617(2) 0.66786(15) 0.30421(12) 0.0167(5) Uani 1 1 d . . . . .
C3 C 0.6558(2) 0.57834(15) 0.32121(12) 0.0163(5) Uani 1 1 d . . . . .
C18 C 0.6556(3) 0.57054(15) 0.38816(12) 0.0191(5) Uani 1 1 d . . . . .
C19 C 0.6699(2) 0.65216(15) 0.41848(12) 0.0179(5) Uani 1 1 d . . . . .
C4 C 0.6786(2) 0.70998(15) 0.37019(11) 0.0168(5) Uani 1 1 d . . . . .
C20 C 0.7812(3) 0.69381(16) 0.26037(12) 0.0209(6) Uani 1 1 d . . . . .
H20A H 0.7668 0.6612 0.2191 0.031 Uiso 1 1 calc GR . . . .
H20B H 0.8837 0.6837 0.2845 0.031 Uiso 1 1 calc GR . . . .
H20C H 0.7694 0.7530 0.2495 0.031 Uiso 1 1 calc GR . . . .
C21 C 0.6583(3) 0.50930(15) 0.27178(12) 0.0220(6) Uani 1 1 d . . . . .
H21A H 0.5634 0.5100 0.2402 0.033 Uiso 1 1 calc GR . . . .
H21B H 0.6681 0.4559 0.2953 0.033 Uiso 1 1 calc GR . . . .
H21C H 0.7451 0.5169 0.2476 0.033 Uiso 1 1 calc GR . . . .
C23 C 0.6484(3) 0.49226(16) 0.42830(13) 0.0254(6) Uani 1 1 d . . . . .
H23A H 0.5510 0.4901 0.4456 0.038 Uiso 1 1 calc GR . . . .
H23B H 0.7324 0.4920 0.4656 0.038 Uiso 1 1 calc GR . . . .
H23C H 0.6572 0.4438 0.3998 0.038 Uiso 1 1 calc GR . . . .
C24 C 0.6793(3) 0.66567(17) 0.49259(12) 0.0247(6) Uani 1 1 d . . . . .
H24A H 0.5851 0.6462 0.5073 0.037 Uiso 1 1 calc GR . . . .
H24B H 0.6929 0.7250 0.5026 0.037 Uiso 1 1 calc GR . . . .
H24C H 0.7661 0.6346 0.5160 0.037 Uiso 1 1 calc GR . . . .
C22 C 0.7131(3) 0.80086(16) 0.37983(12) 0.0229(6) Uani 1 1 d . . . . .
H22A H 0.8088 0.8138 0.3633 0.034 Uiso 1 1 calc GR . . . .
H22B H 0.7229 0.8145 0.4273 0.034 Uiso 1 1 calc GR . . . .
H22C H 0.6302 0.8336 0.3551 0.034 Uiso 1 1 calc GR . . . .


_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 H 1.56(2) . ?
Al1 C1 2.069(2) . ?
Al1 C5 2.082(2) . ?
Al1 C2 2.072(2) . ?
N1 C1 1.358(3) . ?
N1 C8 1.392(3) . ?
N1 C10 1.480(3) . ?
N2 C1 1.361(3) . ?
N2 C9 1.392(3) . ?
N2 C13 1.487(3) . ?
C8 C9 1.357(3) . ?
C8 C16 1.492(3) . ?
C9 C17 1.498(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.519(3) . ?
C10 C12 1.521(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C15 1.515(3) . ?
C13 C14 1.526(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C5 C6 1.491(3) . ?
C5 C7 1.501(3) . ?
C5 C27 1.552(3) . ?
C6 C25 1.358(3) . ?
C6 C28 1.503(3) . ?
C25 C26 1.462(3) . ?
C25 C30 1.497(3) . ?
C26 C7 1.354(3) . ?
C26 C31 1.504(3) . ?
C7 C29 1.503(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C2 C3 1.484(3) . ?
C2 C4 1.488(3) . ?
C2 C20 1.539(3) . ?
C3 C18 1.365(3) . ?
C3 C21 1.499(3) . ?
C18 C19 1.448(3) . ?
C18 C23 1.507(3) . ?
C19 C4 1.362(3) . ?
C19 C24 1.510(3) . ?
C4 C22 1.501(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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
C1 Al1 H 106.2(9) . . ?
C1 Al1 C5 115.99(9) . . ?
C1 Al1 C2 107.27(9) . . ?
C5 Al1 H 99.7(9) . . ?
C2 Al1 H 104.8(9) . . ?
C2 Al1 C5 120.96(10) . . ?
C1 N1 C8 111.03(19) . . ?
C1 N1 C10 122.15(18) . . ?
C8 N1 C10 126.73(19) . . ?
C1 N2 C9 110.8(2) . . ?
C1 N2 C13 121.99(19) . . ?
C9 N2 C13 126.98(19) . . ?
N1 C1 Al1 129.07(16) . . ?
N1 C1 N2 104.81(19) . . ?
N2 C1 Al1 125.92(17) . . ?
N1 C8 C16 125.7(2) . . ?
C9 C8 N1 106.6(2) . . ?
C9 C8 C16 127.7(2) . . ?
N2 C9 C17 125.6(2) . . ?
C8 C9 N2 106.7(2) . . ?
C8 C9 C17 127.7(2) . . ?
C8 C16 H16A 109.5 . . ?
C8 C16 H16B 109.5 . . ?
C8 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C9 C17 H17A 109.5 . . ?
C9 C17 H17B 109.5 . . ?
C9 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C10 H10 106.9 . . ?
N1 C10 C11 112.7(2) . . ?
N1 C10 C12 111.29(19) . . ?
C11 C10 H10 106.9 . . ?
C11 C10 C12 111.9(2) . . ?
C12 C10 H10 106.9 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13 106.7 . . ?
N2 C13 C15 112.9(2) . . ?
N2 C13 C14 111.12(19) . . ?
C15 C13 H13 106.7 . . ?
C15 C13 C14 112.3(2) . . ?
C14 C13 H13 106.7 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C5 Al1 121.96(16) . . ?
C6 C5 C7 103.02(18) . . ?
C6 C5 C27 111.34(19) . . ?
C7 C5 Al1 106.31(15) . . ?
C7 C5 C27 112.31(19) . . ?
C27 C5 Al1 102.01(15) . . ?
C5 C6 C28 124.1(2) . . ?
C25 C6 C5 109.7(2) . . ?
C25 C6 C28 125.3(2) . . ?
C6 C25 C26 108.8(2) . . ?
C6 C25 C30 127.9(2) . . ?
C26 C25 C30 123.2(2) . . ?
C25 C26 C31 123.2(2) . . ?
C7 C26 C25 109.1(2) . . ?
C7 C26 C31 127.6(2) . . ?
C5 C7 C29 124.0(2) . . ?
C26 C7 C5 109.3(2) . . ?
C26 C7 C29 126.6(2) . . ?
C5 C27 H27A 109.5 . . ?
C5 C27 H27B 109.5 . . ?
C5 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C6 C28 H28A 109.5 . . ?
C6 C28 H28B 109.5 . . ?
C6 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C7 C29 H29A 109.5 . . ?
C7 C29 H29B 109.5 . . ?
C7 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C3 C2 Al1 109.54(15) . . ?
C3 C2 C4 103.62(19) . . ?
C3 C2 C20 116.6(2) . . ?
C4 C2 Al1 102.21(15) . . ?
C4 C2 C20 114.2(2) . . ?
C20 C2 Al1 109.55(16) . . ?
C2 C3 C21 124.0(2) . . ?
C18 C3 C2 109.0(2) . . ?
C18 C3 C21 126.9(2) . . ?
C3 C18 C19 109.1(2) . . ?
C3 C18 C23 128.4(2) . . ?
C19 C18 C23 122.5(2) . . ?
C18 C19 C24 122.8(2) . . ?
C4 C19 C18 109.0(2) . . ?
C4 C19 C24 128.1(2) . . ?
C2 C4 C22 123.5(2) . . ?
C19 C4 C2 109.1(2) . . ?
C19 C4 C22 127.2(2) . . ?
C2 C20 H20A 109.5 . . ?
C2 C20 H20B 109.5 . . ?
C2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C3 C21 H21A 109.5 . . ?
C3 C21 H21B 109.5 . . ?
C3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C22 H22A 109.5 . . ?
C4 C22 H22B 109.5 . . ?
C4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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
Al1 C5 C6 C25 116.7(2) . . . . ?
Al1 C5 C6 C28 -73.5(3) . . . . ?
Al1 C5 C7 C26 -126.81(18) . . . . ?
Al1 C5 C7 C29 55.9(3) . . . . ?
Al1 C2 C3 C18 -103.67(18) . . . . ?
Al1 C2 C3 C21 79.3(2) . . . . ?
Al1 C2 C4 C19 109.12(18) . . . . ?
Al1 C2 C4 C22 -75.7(2) . . . . ?
N1 C8 C9 N2 -0.2(2) . . . . ?
N1 C8 C9 C17 -179.7(2) . . . . ?
C1 N1 C8 C9 0.6(2) . . . . ?
C1 N1 C8 C16 -179.9(2) . . . . ?
C1 N1 C10 C11 119.7(2) . . . . ?
C1 N1 C10 C12 -113.7(2) . . . . ?
C1 N2 C9 C8 -0.3(3) . . . . ?
C1 N2 C9 C17 179.2(2) . . . . ?
C1 N2 C13 C15 -125.2(2) . . . . ?
C1 N2 C13 C14 107.6(2) . . . . ?
C8 N1 C1 Al1 174.28(16) . . . . ?
C8 N1 C1 N2 -0.8(2) . . . . ?
C8 N1 C10 C11 -63.9(3) . . . . ?
C8 N1 C10 C12 62.6(3) . . . . ?
C9 N2 C1 Al1 -174.59(15) . . . . ?
C9 N2 C1 N1 0.7(2) . . . . ?
C9 N2 C13 C15 60.1(3) . . . . ?
C9 N2 C13 C14 -67.0(3) . . . . ?
C16 C8 C9 N2 -179.7(2) . . . . ?
C16 C8 C9 C17 0.8(4) . . . . ?
C10 N1 C1 Al1 -8.8(3) . . . . ?
C10 N1 C1 N2 176.11(18) . . . . ?
C10 N1 C8 C9 -176.1(2) . . . . ?
C10 N1 C8 C16 3.4(3) . . . . ?
C13 N2 C1 Al1 9.9(3) . . . . ?
C13 N2 C1 N1 -174.80(18) . . . . ?
C13 N2 C9 C8 174.9(2) . . . . ?
C13 N2 C9 C17 -5.6(4) . . . . ?
C5 C6 C25 C26 1.2(3) . . . . ?
C5 C6 C25 C30 176.9(2) . . . . ?
C6 C5 C7 C26 2.5(3) . . . . ?
C6 C5 C7 C29 -174.8(2) . . . . ?
C6 C25 C26 C7 0.5(3) . . . . ?
C6 C25 C26 C31 177.2(2) . . . . ?
C25 C26 C7 C5 -1.9(3) . . . . ?
C25 C26 C7 C29 175.3(2) . . . . ?
C7 C5 C6 C25 -2.2(3) . . . . ?
C7 C5 C6 C28 167.6(2) . . . . ?
C27 C5 C6 C25 -122.8(2) . . . . ?
C27 C5 C6 C28 47.0(3) . . . . ?
C27 C5 C7 C26 122.4(2) . . . . ?
C27 C5 C7 C29 -54.9(3) . . . . ?
C28 C6 C25 C26 -168.4(2) . . . . ?
C28 C6 C25 C30 7.2(4) . . . . ?
C30 C25 C26 C7 -175.4(2) . . . . ?
C30 C25 C26 C31 1.3(4) . . . . ?
C31 C26 C7 C5 -178.5(2) . . . . ?
C31 C26 C7 C29 -1.2(4) . . . . ?
C2 C3 C18 C19 -3.2(2) . . . . ?
C2 C3 C18 C23 179.1(2) . . . . ?
C3 C2 C4 C19 -4.7(2) . . . . ?
C3 C2 C4 C22 170.5(2) . . . . ?
C3 C18 C19 C4 0.1(3) . . . . ?
C3 C18 C19 C24 -177.6(2) . . . . ?
C18 C19 C4 C2 3.0(3) . . . . ?
C18 C19 C4 C22 -172.0(2) . . . . ?
C4 C2 C3 C18 4.8(2) . . . . ?
C4 C2 C3 C21 -172.2(2) . . . . ?
C20 C2 C3 C18 131.2(2) . . . . ?
C20 C2 C3 C21 -45.8(3) . . . . ?
C20 C2 C4 C19 -132.7(2) . . . . ?
C20 C2 C4 C22 42.5(3) . . . . ?
C21 C3 C18 C19 173.7(2) . . . . ?
C21 C3 C18 C23 -4.0(4) . . . . ?
C23 C18 C19 C4 178.0(2) . . . . ?
C23 C18 C19 C24 0.2(3) . . . . ?
C24 C19 C4 C2 -179.4(2) . . . . ?
C24 C19 C4 C22 5.6(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 22 6 0.0525 0.2397 22.1502 6.0323 0.4896 -0.3765 0.7865
12 -6 -9 0.0971 11.7941 -6.2143 -9.3137 -0.7399 0.5663 0.3630
0 -22 -6 0.0500 0.2687 -22.1226 -6.3512 -0.5148 0.3957 -0.7605
-12 7 9 0.0679 -11.6494 6.9726 9.4325 0.7498 -0.5739 -0.3294
-1 3 -28 0.0295 -1.0062 3.0206 -27.9895 -0.6892 -0.7418 -0.0369
1 -2 28 0.0181 1.0068 -2.0209 27.9891 0.7042 0.7182 0.0710
0 -2 1 0.0446 -0.0008 -2.0000 1.0002 -0.0025 0.0692 -0.0651
1 2 1 0.0933 1.0016 1.9984 0.9993 0.0242 0.0280 0.1226

_olex2_date_sample_data_collection 2015-07-06
_olex2_date_sample_submission    2015-07-01
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id SU126
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4c
_database_code_depnum_ccdc_archive 'CCDC 1489249'
_audit_update_record             
;
2016-07-26 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
# local name mc16007
_audit_creation_date             2016-07-26
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.07.25 svn.r3318 for OlexSys, GUI svn.r5204)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H41 Al N2'
_chemical_formula_sum            'C27 H41 Al N2'
_chemical_formula_weight         420.60
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C27 H41 Al N2'
_chemical_oxdiff_usercomment     '@ 120 K SU255'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'I 1 a 1'
_space_group_name_Hall           'I -2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'

_cell_length_a                   15.5778(7)
_cell_length_b                   11.6033(4)
_cell_length_c                   15.6858(7)
_cell_angle_alpha                90
_cell_angle_beta                 116.418(5)
_cell_angle_gamma                90
_cell_volume                     2539.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.1760
_cell_measurement_theta_min      3.8090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_recrystallization_method 
'The material was recrystallised from d6-benzene by slow evaporation'
_exptl_crystal_size_max          0.3723
_exptl_crystal_size_mid          0.3253
_exptl_crystal_size_min          0.1679
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22186
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.651
_diffrn_reflns_theta_min         3.140
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  -99.0000 -180.0000 50

#__ type_ start__ end____ width___ exp.time_
  2 omega  -32.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310   38.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
  3 omega  -82.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  -38.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
  4 omega  -63.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935  -77.0000   30.0000 105

#__ type_ start__ end____ width___ exp.time_
  5 omega  -16.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935   57.0000 -180.0000 97

#__ type_ start__ end____ width___ exp.time_
  6 omega  -85.00  -39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  155.0000   60.2380 46

#__ type_ start__ end____ width___ exp.time_
  7 omega  -12.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935   38.0000   60.0000 41

#__ type_ start__ end____ width___ exp.time_
  8 omega  -62.00   34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935  -38.0000   60.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0241283000
_diffrn_orient_matrix_UB_12      -0.0524057000
_diffrn_orient_matrix_UB_13      0.0196172000
_diffrn_orient_matrix_UB_21      -0.0038200000
_diffrn_orient_matrix_UB_22      -0.0161758000
_diffrn_orient_matrix_UB_23      -0.0451710000
_diffrn_orient_matrix_UB_31      0.0445867000
_diffrn_orient_matrix_UB_32      0.0270115000
_diffrn_orient_matrix_UB_33      0.0111315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.825
_reflns_number_gt                5769
_reflns_number_total             6273
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 
;
 Flack x determined using 2388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6273
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0437
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0473P)²+0.9839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1010
_refine_special_details          
;
The Al-bound H atom was located from a difference Fourier map and refined freely.

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 

129_ALERT_4_A Unusual Space group Specified ..................       I1A1 Check

Noted
#===============================================================================
340_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00408 Ang.
910_ALERT_3_C Missing # of FCF Reflection(s) Below Th(Min) ...          5 Report
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1 Note
915_ALERT_3_C Low Friedel Pair Coverage ......................         82 %
923_ALERT_1_C S    values in the CIF and FCF Differ by .......      0.025 Check

Not significant

#===============================================================================
069_ALERT_1_G Atom Label without Numerical Part ..............          H Do !
380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety .....        C20 Check
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        236 Note

Not significant

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C7(H7), C8(H8), C10(H10)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C18(H18A,
 H18B,H18C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C),
 C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.67552(5) 0.31804(6) 0.61679(5) 0.01844(17) Uani 1 1 d . . . . .
N1 N 0.57827(15) 0.31571(18) 0.48515(15) 0.0191(4) Uani 1 1 d . . . . .
N2 N 0.35603(17) 0.2981(2) 0.20891(16) 0.0281(5) Uani 1 1 d . . . . .
C11 C 0.48657(19) 0.3390(2) 0.46504(19) 0.0227(5) Uani 1 1 d . . . . .
H11 H 0.4729 0.3593 0.5164 0.027 Uiso 1 1 calc R . . . .
C7 C 0.59520(18) 0.2897(2) 0.40961(18) 0.0222(5) Uani 1 1 d . . . . .
H7 H 0.6594 0.2745 0.4213 0.027 Uiso 1 1 calc R . . . .
C4 C 0.74812(18) 0.4722(2) 0.63455(17) 0.0206(5) Uani 1 1 d . . . . .
C6 C 0.66680(19) 0.5473(2) 0.62155(19) 0.0221(5) Uani 1 1 d . . . . .
C5 C 0.75722(17) 0.4857(2) 0.54491(17) 0.0207(5) Uani 1 1 d . . . . .
C1 C 0.74576(19) 0.1600(2) 0.65439(18) 0.0223(5) Uani 1 1 d . . . . .
C2 C 0.81376(19) 0.1506(2) 0.61290(19) 0.0243(6) Uani 1 1 d . . . . .
C3 C 0.66363(19) 0.0872(2) 0.59178(18) 0.0228(6) Uani 1 1 d . . . . .
C8 C 0.52564(19) 0.2841(2) 0.31805(18) 0.0242(5) Uani 1 1 d . . . . .
H8 H 0.5421 0.2656 0.2682 0.029 Uiso 1 1 calc R . . . .
C9 C 0.42851(19) 0.3057(2) 0.29703(19) 0.0218(5) Uani 1 1 d . . . . .
C10 C 0.41200(19) 0.3355(2) 0.3761(2) 0.0249(6) Uani 1 1 d . . . . .
H10 H 0.3489 0.3531 0.3670 0.030 Uiso 1 1 calc R . . . .
C12 C 0.3714(2) 0.2715(3) 0.1259(2) 0.0388(7) Uani 1 1 d . . . . .
H12A H 0.3779 0.3433 0.0965 0.058 Uiso 1 1 calc GR . . . .
H12B H 0.3167 0.2275 0.0799 0.058 Uiso 1 1 calc GR . . . .
H12C H 0.4301 0.2257 0.1457 0.058 Uiso 1 1 calc GR . . . .
C13 C 0.2587(2) 0.3282(3) 0.1902(2) 0.0342(7) Uani 1 1 d . . . . .
H13A H 0.2399 0.2834 0.2322 0.051 Uiso 1 1 calc GR . . . .
H13B H 0.2150 0.3108 0.1237 0.051 Uiso 1 1 calc GR . . . .
H13C H 0.2555 0.4106 0.2021 0.051 Uiso 1 1 calc GR . . . .
C21 C 0.68276(17) 0.5517(2) 0.48347(18) 0.0210(5) Uani 1 1 d . . . . .
C22 C 0.62621(18) 0.5900(2) 0.53041(18) 0.0219(5) Uani 1 1 d . . . . .
C24 C 0.83597(19) 0.4351(3) 0.5264(2) 0.0263(6) Uani 1 1 d . . . . .
H24A H 0.8982 0.4549 0.5790 0.039 Uiso 1 1 calc GR . . . .
H24B H 0.8322 0.4663 0.4668 0.039 Uiso 1 1 calc GR . . . .
H24C H 0.8290 0.3511 0.5214 0.039 Uiso 1 1 calc GR . . . .
C26 C 0.6576(2) 0.5798(3) 0.38129(19) 0.0282(6) Uani 1 1 d . . . . .
H26A H 0.6569 0.6636 0.3733 0.042 Uiso 1 1 calc GR . . . .
H26B H 0.5942 0.5484 0.3398 0.042 Uiso 1 1 calc GR . . . .
H26C H 0.7055 0.5457 0.3643 0.042 Uiso 1 1 calc GR . . . .
C27 C 0.5377(2) 0.6626(3) 0.4833(2) 0.0315(6) Uani 1 1 d . . . . .
H27A H 0.4868 0.6175 0.4336 0.047 Uiso 1 1 calc GR . . . .
H27B H 0.5519 0.7306 0.4547 0.047 Uiso 1 1 calc GR . . . .
H27C H 0.5167 0.6872 0.5308 0.047 Uiso 1 1 calc GR . . . .
C25 C 0.6358(2) 0.5725(3) 0.6980(2) 0.0322(6) Uani 1 1 d . . . . .
H25A H 0.6004 0.5063 0.7051 0.048 Uiso 1 1 calc GR . . . .
H25B H 0.5944 0.6407 0.6803 0.048 Uiso 1 1 calc GR . . . .
H25C H 0.6924 0.5868 0.7585 0.048 Uiso 1 1 calc GR . . . .
C23 C 0.83872(19) 0.4782(3) 0.72925(19) 0.0260(6) Uani 1 1 d . . . . .
H23A H 0.8237 0.4538 0.7809 0.039 Uiso 1 1 calc GR . . . .
H23B H 0.8628 0.5576 0.7407 0.039 Uiso 1 1 calc GR . . . .
H23C H 0.8877 0.4272 0.7269 0.039 Uiso 1 1 calc GR . . . .
C14 C 0.7708(2) 0.0915(2) 0.52869(19) 0.0265(6) Uani 1 1 d . . . . .
C15 C 0.6777(2) 0.0524(2) 0.51591(19) 0.0261(6) Uani 1 1 d . . . . .
C18 C 0.5783(2) 0.0611(3) 0.6090(2) 0.0311(6) Uani 1 1 d . . . . .
H18A H 0.5975 0.0623 0.6776 0.047 Uiso 1 1 calc GR . . . .
H18B H 0.5532 -0.0153 0.5834 0.047 Uiso 1 1 calc GR . . . .
H18C H 0.5286 0.1192 0.5772 0.047 Uiso 1 1 calc GR . . . .
C20 C 0.6087(2) -0.0142(3) 0.4303(2) 0.0380(7) Uani 1 1 d . . . . .
H20A H 0.5518 -0.0343 0.4386 0.057 Uiso 1 1 calc GR . . . .
H20B H 0.6397 -0.0848 0.4237 0.057 Uiso 1 1 calc GR . . . .
H20C H 0.5897 0.0332 0.3731 0.057 Uiso 1 1 calc GR . . . .
C19 C 0.8091(2) 0.0695(3) 0.4574(2) 0.0388(7) Uani 1 1 d . . . . .
H19A H 0.8739 0.1015 0.4813 0.058 Uiso 1 1 calc GR . . . .
H19B H 0.7672 0.1063 0.3968 0.058 Uiso 1 1 calc GR . . . .
H19C H 0.8113 -0.0137 0.4478 0.058 Uiso 1 1 calc GR . . . .
C17 C 0.9170(2) 0.1857(3) 0.6634(2) 0.0331(7) Uani 1 1 d . . . . .
H17A H 0.9216 0.2641 0.6882 0.050 Uiso 1 1 calc GR . . . .
H17B H 0.9454 0.1833 0.6188 0.050 Uiso 1 1 calc GR . . . .
H17C H 0.9516 0.1325 0.7163 0.050 Uiso 1 1 calc GR . . . .
C16 C 0.7849(2) 0.1525(3) 0.76259(19) 0.0294(6) Uani 1 1 d . . . . .
H16A H 0.8294 0.2164 0.7923 0.044 Uiso 1 1 calc GR . . . .
H16B H 0.8187 0.0792 0.7850 0.044 Uiso 1 1 calc GR . . . .
H16C H 0.7317 0.1571 0.7798 0.044 Uiso 1 1 calc GR . . . .
H H 0.618(3) 0.319(3) 0.678(3) 0.043(10) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 N1 1.943(2) . ?
Al1 C4 2.067(3) . ?
Al1 C1 2.081(3) . ?
Al1 H 1.58(4) . ?
N1 C11 1.346(3) . ?
N1 C7 1.358(3) . ?
N2 C9 1.343(3) . ?
N2 C12 1.458(4) . ?
N2 C13 1.453(4) . ?
C11 H11 0.9500 . ?
C11 C10 1.363(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.362(4) . ?
C4 C6 1.476(4) . ?
C4 C5 1.483(3) . ?
C4 C23 1.529(3) . ?
C6 C22 1.373(4) . ?
C6 C25 1.508(4) . ?
C5 C21 1.366(4) . ?
C5 C24 1.500(4) . ?
C1 C2 1.473(4) . ?
C1 C3 1.482(4) . ?
C1 C16 1.529(4) . ?
C2 C14 1.370(4) . ?
C2 C17 1.499(4) . ?
C3 C15 1.364(4) . ?
C3 C18 1.500(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.420(4) . ?
C9 C10 1.416(4) . ?
C10 H10 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C21 C22 1.446(4) . ?
C21 C26 1.507(4) . ?
C22 C27 1.500(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C14 C15 1.445(4) . ?
C14 C19 1.506(4) . ?
C15 C20 1.507(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
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 Al1 C4 106.04(10) . . ?
N1 Al1 C1 110.61(10) . . ?
N1 Al1 H 105.1(13) . . ?
C4 Al1 C1 122.45(11) . . ?
C4 Al1 H 109.7(13) . . ?
C1 Al1 H 101.7(13) . . ?
C11 N1 Al1 119.38(18) . . ?
C11 N1 C7 116.0(2) . . ?
C7 N1 Al1 124.62(17) . . ?
C9 N2 C12 122.4(2) . . ?
C9 N2 C13 121.0(2) . . ?
C13 N2 C12 116.3(2) . . ?
N1 C11 H11 117.8 . . ?
N1 C11 C10 124.5(2) . . ?
C10 C11 H11 117.8 . . ?
N1 C7 H7 118.0 . . ?
N1 C7 C8 123.9(2) . . ?
C8 C7 H7 118.0 . . ?
C6 C4 Al1 96.21(16) . . ?
C6 C4 C5 104.2(2) . . ?
C6 C4 C23 118.1(2) . . ?
C5 C4 Al1 103.96(17) . . ?
C5 C4 C23 118.7(2) . . ?
C23 C4 Al1 112.58(18) . . ?
C4 C6 C25 124.3(2) . . ?
C22 C6 C4 109.0(2) . . ?
C22 C6 C25 126.6(3) . . ?
C4 C5 C24 125.0(2) . . ?
C21 C5 C4 108.6(2) . . ?
C21 C5 C24 126.4(2) . . ?
C2 C1 Al1 109.32(18) . . ?
C2 C1 C3 104.1(2) . . ?
C2 C1 C16 118.4(2) . . ?
C3 C1 Al1 97.15(17) . . ?
C3 C1 C16 120.2(2) . . ?
C16 C1 Al1 105.35(18) . . ?
C1 C2 C17 124.0(3) . . ?
C14 C2 C1 108.9(2) . . ?
C14 C2 C17 126.5(3) . . ?
C1 C3 C18 124.6(2) . . ?
C15 C3 C1 108.7(2) . . ?
C15 C3 C18 126.6(2) . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.1(2) . . ?
C9 C8 H8 119.9 . . ?
N2 C9 C8 123.2(2) . . ?
N2 C9 C10 121.3(2) . . ?
C10 C9 C8 115.4(2) . . ?
C11 C10 C9 120.0(2) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 C21 C22 109.3(2) . . ?
C5 C21 C26 127.5(2) . . ?
C22 C21 C26 123.1(2) . . ?
C6 C22 C21 108.5(2) . . ?
C6 C22 C27 127.8(2) . . ?
C21 C22 C27 123.8(2) . . ?
C5 C24 H24A 109.5 . . ?
C5 C24 H24B 109.5 . . ?
C5 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C6 C25 H25A 109.5 . . ?
C6 C25 H25B 109.5 . . ?
C6 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C4 C23 H23A 109.5 . . ?
C4 C23 H23B 109.5 . . ?
C4 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C2 C14 C15 108.7(2) . . ?
C2 C14 C19 128.0(3) . . ?
C15 C14 C19 123.3(3) . . ?
C3 C15 C14 109.1(2) . . ?
C3 C15 C20 126.9(3) . . ?
C14 C15 C20 124.0(3) . . ?
C3 C18 H18A 109.5 . . ?
C3 C18 H18B 109.5 . . ?
C3 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C2 C17 H17A 109.5 . . ?
C2 C17 H17B 109.5 . . ?
C2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 C16 H16A 109.5 . . ?
C1 C16 H16B 109.5 . . ?
C1 C16 H16C 109.5 . . ?
H16A C16 H16B 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
Al1 N1 C11 C10 -177.3(2) . . . . ?
Al1 N1 C7 C8 177.3(2) . . . . ?
Al1 C4 C6 C22 -100.1(2) . . . . ?
Al1 C4 C6 C25 80.4(3) . . . . ?
Al1 C4 C5 C21 94.4(2) . . . . ?
Al1 C4 C5 C24 -85.9(3) . . . . ?
Al1 C1 C2 C14 -95.8(2) . . . . ?
Al1 C1 C2 C17 92.3(3) . . . . ?
Al1 C1 C3 C15 104.9(2) . . . . ?
Al1 C1 C3 C18 -73.0(3) . . . . ?
N1 C11 C10 C9 0.1(4) . . . . ?
N1 C7 C8 C9 -0.2(4) . . . . ?
N2 C9 C10 C11 177.9(3) . . . . ?
C11 N1 C7 C8 -1.4(4) . . . . ?
C7 N1 C11 C10 1.5(4) . . . . ?
C7 C8 C9 N2 -177.9(2) . . . . ?
C7 C8 C9 C10 1.7(4) . . . . ?
C4 C6 C22 C21 -4.1(3) . . . . ?
C4 C6 C22 C27 175.1(3) . . . . ?
C4 C5 C21 C22 3.6(3) . . . . ?
C4 C5 C21 C26 -174.3(3) . . . . ?
C6 C4 C5 C21 -5.8(3) . . . . ?
C6 C4 C5 C24 173.9(2) . . . . ?
C5 C4 C6 C22 6.0(3) . . . . ?
C5 C4 C6 C25 -173.4(2) . . . . ?
C5 C21 C22 C6 0.3(3) . . . . ?
C5 C21 C22 C27 -178.9(2) . . . . ?
C1 C2 C14 C15 -4.6(3) . . . . ?
C1 C2 C14 C19 174.5(3) . . . . ?
C1 C3 C15 C14 4.6(3) . . . . ?
C1 C3 C15 C20 -174.3(3) . . . . ?
C2 C1 C3 C15 -7.1(3) . . . . ?
C2 C1 C3 C18 174.9(2) . . . . ?
C2 C14 C15 C3 0.0(3) . . . . ?
C2 C14 C15 C20 178.9(3) . . . . ?
C3 C1 C2 C14 7.1(3) . . . . ?
C3 C1 C2 C17 -164.8(3) . . . . ?
C8 C9 C10 C11 -1.6(4) . . . . ?
C12 N2 C9 C8 -2.6(4) . . . . ?
C12 N2 C9 C10 177.8(3) . . . . ?
C13 N2 C9 C8 -176.1(3) . . . . ?
C13 N2 C9 C10 4.4(4) . . . . ?
C24 C5 C21 C22 -176.1(2) . . . . ?
C24 C5 C21 C26 6.0(4) . . . . ?
C26 C21 C22 C6 178.3(2) . . . . ?
C26 C21 C22 C27 -0.9(4) . . . . ?
C25 C6 C22 C21 175.3(3) . . . . ?
C25 C6 C22 C27 -5.5(5) . . . . ?
C23 C4 C6 C22 140.1(2) . . . . ?
C23 C4 C6 C25 -39.3(4) . . . . ?
C23 C4 C5 C21 -139.6(2) . . . . ?
C23 C4 C5 C24 40.1(4) . . . . ?
C18 C3 C15 C14 -177.5(3) . . . . ?
C18 C3 C15 C20 3.6(5) . . . . ?
C19 C14 C15 C3 -179.1(3) . . . . ?
C19 C14 C15 C20 -0.2(4) . . . . ?
C17 C2 C14 C15 167.0(3) . . . . ?
C17 C2 C14 C19 -13.9(5) . . . . ?
C16 C1 C2 C14 143.6(2) . . . . ?
C16 C1 C2 C17 -28.3(4) . . . . ?
C16 C1 C3 C15 -142.6(2) . . . . ?
C16 C1 C3 C18 39.4(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-16 10 13 0.1115 -16.0017 9.9834 12.9854 -0.6545 -0.6869 -0.2993
-19 -7 4 0.1836 -18.9813 -7.0084 3.9994 -0.0123 0.0052 -0.9911
-9 -13 -4 0.1623 -8.9805 -12.9982 -3.9917 0.3862 0.4249 -0.7959
5 -14 -11 0.1115 5.0127 -13.9884 -10.9856 0.6385 0.7034 -0.2766
17 -9 -13 0.1507 17.0001 -8.9834 -12.9858 0.6262 0.6670 0.3708
13 12 1 0.1072 12.9796 12.0012 0.9943 -0.2962 -0.2886 0.9140
11 -14 -2 0.0674 10.5042 -13.9808 -2.4886 0.9373 0.2984 0.0630
-11 14 2 0.0972 -11.0035 13.9802 1.9888 -0.9591 -0.2739 -0.0908
-14 -13 3 0.1599 -13.9800 -12.9997 3.0043 0.4029 0.1280 -0.9410
14 12 -4 0.1318 14.4806 12.0008 -3.5034 -0.3482 -0.0912 0.9308
0 16 0 0.1041 -0.0129 15.9868 -0.0098 -0.8383 -0.2581 0.4311
-5 -12 15 0.1491 -5.4936 -11.9889 15.4993 0.7998 -0.4852 -0.3962
-18 -9 7 0.1670 -18.4818 -9.0050 7.4991 0.1731 -0.1225 -0.9838
-18 -2 -3 0.1928 -17.9827 -2.0143 -3.0003 -0.3872 0.2368 -0.8896
-3 9 -14 0.1199 -3.4974 8.9844 -14.4994 -0.8397 0.5230 -0.0747
8 12 -15 0.1293 7.9913 11.9912 -14.9992 -0.7298 0.4530 0.5132
0 -4 -19 0.1420 0.0125 -4.0037 -18.9889 -0.1624 0.9225 -0.3190
15 2 -20 0.1842 15.4961 2.0035 -20.4893 -0.1330 0.8339 0.5170
-16 3 20 0.1160 -15.5002 2.9924 20.4863 -0.1289 -0.9146 -0.3822
-2 -9 -15 0.1397 -2.4832 -9.0004 -15.4878 0.1079 0.8547 -0.5262
3 15 7 0.1177 3.4815 14.9933 7.4880 -0.5548 -0.5941 0.6436

_olex2_date_sample_submission    2016-01-11
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id SU255
_olex2_submission_special_instructions 'No special instructions were received'


# start Validation Reply Form
_vrf_PLAT129_4c                  
;
PROBLEM: Unusual Space group Specified ..................       I1A1 Check 
RESPONSE: Non-standard setting.  This is not a problem.
;
# end Validation Reply Form
