# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1895241'
loop_
_audit_author_name
_audit_author_address
'Simon Aldridge'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-02-01 deposited with the CCDC.	2019-02-25 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   10.75290(10)
_cell_length_b                   12.94880(10)
_cell_length_c                   26.8741(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.3816(7)
_cell_angle_gamma                90
_cell_volume                     3730.94(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Al 0.2130 0.2455 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886
1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C11 H10 Al0.25 B0.25 N1 
# Dc =      0.29 Fooo =   1312.00 Mu =      1.86 M =    165.66
# Found Formula = C39 H62 Al1 B1 N2 
# Dc =      1.06 FOOO =   1312.00 Mu =      6.60 M =    596.73

_chemical_formula_sum            'C39 H62 Al1 B1 N2'
_chemical_formula_moiety         'C39 H62 Al1 B1 N2'
_chemical_compound_source        ?
_chemical_formula_weight         596.73


_cell_measurement_reflns_used    22125
_cell_measurement_theta_min      3
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_max          0.230

_exptl_crystal_density_diffrn    1.062
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.660

# Sheldrick geometric approximatio 0.92 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_T_max  0.96
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            41741
_reflns_number_total             7777
_diffrn_reflns_av_R_equivalents  0.022
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7777 
# Theoretical number of reflections is about 15603 


_diffrn_reflns_theta_min         3.791
_diffrn_reflns_theta_max         76.108
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        76.108
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              33

_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      0.01

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.22
_refine_diff_density_max         0.32


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         7747
_refine_ls_number_restraints     162
_refine_ls_number_parameters     416
_oxford_refine_ls_R_factor_ref   0.0438
_refine_ls_wR_factor_ref         0.1074
_refine_ls_goodness_of_fit_ref   0.9772
_refine_ls_shift/su_max          0.0023474
_refine_ls_shift/su_mean         0.0000503


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7747
_refine_ls_R_factor_all          0.0438
_refine_ls_wR_factor_all         0.1074

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7098
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_gt          0.1049

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 1.53P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Al1 Al 0.71115(3) 0.27618(2) 0.656216(11) 0.0218 1.0000 Uani . . . . . .
N2 N 0.83606(9) 0.32826(7) 0.61548(3) 0.0248 1.0000 Uani . . . . . .
C3 C 0.94962(11) 0.34586(9) 0.63791(4) 0.0289 1.0000 Uani . . . . . .
C4 C 0.99136(11) 0.30180(10) 0.68367(5) 0.0317 1.0000 Uani . . . . . .
C5 C 0.93701(11) 0.22005(9) 0.70799(5) 0.0300 1.0000 Uani . . . . . .
N6 N 0.82209(9) 0.18569(7) 0.69474(4) 0.0254 1.0000 Uani . . . . . .
C7 C 0.78237(10) 0.08830(9) 0.71508(5) 0.0293 1.0000 Uani . . . . . .
C8 C 0.71776(12) 0.08744(11) 0.75867(5) 0.0365 1.0000 Uani . . . . . .
C9 C 0.67982(13) -0.00796(13) 0.77643(6) 0.0461 1.0000 Uani . . . . . .
C10 C 0.70292(13) -0.09837(12) 0.75214(6) 0.0486 1.0000 Uani . . . . . .
C11 C 0.76529(13) -0.09616(11) 0.70896(6) 0.0427 1.0000 Uani . . . . . .
C12 C 0.80650(12) -0.00314(10) 0.68967(5) 0.0341 1.0000 Uani . . . . . .
C13 C 0.87925(15) -0.00446(10) 0.64343(6) 0.0428 1.0000 Uani . . . . . .
C14 C 1.01564(17) -0.0329(2) 0.65651(8) 0.0770 1.0000 Uani . . . . . .
C15 C 0.82390(18) -0.07666(13) 0.60284(7) 0.0563 1.0000 Uani . . . . . .
C16 C 0.68742(15) 0.18505(13) 0.78639(5) 0.0439 1.0000 Uani . . . . . .
C17 C 0.7471(2) 0.18625(18) 0.84002(6) 0.0740 1.0000 Uani . . . . . .
C18 C 0.54537(17) 0.19952(17) 0.78639(7) 0.0619 1.0000 Uani . . . . . .
C19 C 1.01457(14) 0.17074(12) 0.75081(6) 0.0463 1.0000 Uani . . . . . .
C20 C 1.04099(14) 0.41498(11) 0.61397(6) 0.0429 1.0000 Uani . . . . . .
C21 C 0.80907(11) 0.36574(9) 0.56483(4) 0.0270 1.0000 Uani . . . . . .
C22 C 0.82346(11) 0.29801(9) 0.52480(4) 0.0281 1.0000 Uani . . . . . .
C23 C 0.80182(14) 0.33677(11) 0.47654(5) 0.0396 1.0000 Uani . . . . . .
C24 C 0.76639(16) 0.43798(12) 0.46779(5) 0.0458 1.0000 Uani . . . . . .
C25 C 0.74930(16) 0.50195(11) 0.50731(5) 0.0449 1.0000 Uani . . . . . .
C26 C 0.76900(14) 0.46735(10) 0.55620(5) 0.0400 1.0000 Uani D . . . . .
C27 C 0.7246(4) 0.53765(18) 0.59711(7) 0.0564 0.622(10) Uani D . P 1 1 .
C28 C 0.7688(6) 0.5485(3) 0.59822(10) 0.0547 0.378(10) Uani D . P 1 2 .
C29 C 0.7983(6) 0.6388(2) 0.60018(14) 0.0691 0.622(10) Uani D . P 1 1 .
C30 C 0.8690(8) 0.6341(3) 0.5918(2) 0.0620 0.378(10) Uani D . P 1 2 .
C31 C 0.6413(8) 0.5950(5) 0.6008(2) 0.0657 0.378(10) Uani D . P 1 2 .
C32 C 0.5836(5) 0.5582(3) 0.58918(14) 0.0655 0.622(10) Uani D . P 1 1 .
C33 C 0.86142(12) 0.18581(10) 0.53321(5) 0.0320 1.0000 Uani . . . . . .
C34 C 0.81284(14) 0.11435(11) 0.49095(5) 0.0417 1.0000 Uani . . . . . .
C35 C 1.00222(13) 0.17332(13) 0.54235(7) 0.0491 1.0000 Uani . . . . . .
C36 C 0.64185(12) 0.38646(10) 0.69627(4) 0.0321 1.0000 Uani . . . . . .
C37 C 0.73171(16) 0.45230(12) 0.73004(5) 0.0458 1.0000 Uani . . . . . .
B38 B 0.54540(12) 0.19762(10) 0.61637(5) 0.0264 1.0000 Uani . . . . . .
C39 C 0.40715(11) 0.23749(10) 0.62512(5) 0.0340 1.0000 Uani . . . . . .
C40 C 0.33485(13) 0.14947(13) 0.64819(6) 0.0444 1.0000 Uani . . . . . .
C41 C 0.33787(14) 0.04485(12) 0.62177(6) 0.0456 1.0000 Uani . . . . . .
C42 C 0.46474(13) 0.01482(10) 0.60326(6) 0.0396 1.0000 Uani . . . . . .
C43 C 0.53384(11) 0.10259(10) 0.57819(5) 0.0311 1.0000 Uani . . . . . .
C44 C 0.46926(13) 0.14071(12) 0.52847(5) 0.0415 1.0000 Uani . . . . . .
C45 C 0.34579(14) 0.19597(13) 0.53244(6) 0.0458 1.0000 Uani . . . . . .
C46 C 0.34736(13) 0.27542(12) 0.57431(6) 0.0445 1.0000 Uani . . . . . .
H41 H 1.0729 0.3258 0.6984 0.0391 1.0000 Uiso R . . . . .
H91 H 0.6348 -0.0099 0.8063 0.0578 1.0000 Uiso R . . . . .
H101 H 0.6743 -0.1635 0.7649 0.0616 1.0000 Uiso R . . . . .
H111 H 0.7808 -0.1615 0.6910 0.0540 1.0000 Uiso R . . . . .
H131 H 0.8777 0.0683 0.6290 0.0529 1.0000 Uiso R . . . . .
H141 H 1.0582 -0.0283 0.6251 0.1218 1.0000 Uiso R . . . . .
H142 H 1.0511 0.0120 0.6804 0.1219 1.0000 Uiso R . . . . .
H143 H 1.0153 -0.1093 0.6684 0.1225 1.0000 Uiso R . . . . .
H151 H 0.8663 -0.0680 0.5715 0.0879 1.0000 Uiso R . . . . .
H152 H 0.8380 -0.1492 0.6147 0.0877 1.0000 Uiso R . . . . .
H153 H 0.7340 -0.0659 0.5950 0.0883 1.0000 Uiso R . . . . .
H161 H 0.7229 0.2462 0.7684 0.0531 1.0000 Uiso R . . . . .
H171 H 0.7261 0.2515 0.8570 0.1171 1.0000 Uiso R . . . . .
H172 H 0.7132 0.1286 0.8580 0.1174 1.0000 Uiso R . . . . .
H173 H 0.8380 0.1803 0.8395 0.1157 1.0000 Uiso R . . . . .
H182 H 0.5286 0.2659 0.8028 0.1012 1.0000 Uiso R . . . . .
H181 H 0.5090 0.1427 0.8052 0.1019 1.0000 Uiso R . . . . .
H183 H 0.5084 0.1999 0.7512 0.1020 1.0000 Uiso R . . . . .
H191 H 0.9988 0.0958 0.7535 0.0747 1.0000 Uiso R . . . . .
H192 H 0.9865 0.2008 0.7813 0.0758 1.0000 Uiso R . . . . .
H193 H 1.1046 0.1849 0.7500 0.0749 1.0000 Uiso R . . . . .
H201 H 1.1232 0.4030 0.6282 0.0689 1.0000 Uiso R . . . . .
H202 H 1.0181 0.4860 0.6188 0.0699 1.0000 Uiso R . . . . .
H203 H 1.0391 0.4006 0.5785 0.0687 1.0000 Uiso R . . . . .
H231 H 0.8106 0.2901 0.4480 0.0493 1.0000 Uiso R . . . . .
H241 H 0.7523 0.4635 0.4338 0.0589 1.0000 Uiso R . . . . .
H251 H 0.7196 0.5730 0.5012 0.0571 1.0000 Uiso R . . . . .
H271 H 0.7415 0.5002 0.6301 0.0663 0.622(10) Uiso R . P 1 1 .
H281 H 0.7941 0.5123 0.6308 0.0640 0.378(10) Uiso R . P 1 2 .
H291 H 0.7657 0.6826 0.6258 0.0968 0.622(10) Uiso R . P 1 1 .
H292 H 0.8862 0.6297 0.6078 0.0975 0.622(10) Uiso R . P 1 1 .
H293 H 0.7842 0.6765 0.5683 0.0964 0.622(10) Uiso R . P 1 1 .
H302 H 0.8806 0.6747 0.6223 0.0851 0.378(10) Uiso R . P 1 2 .
H301 H 0.9510 0.6025 0.5859 0.0848 0.378(10) Uiso R . P 1 2 .
H303 H 0.8445 0.6772 0.5644 0.0848 0.378(10) Uiso R . P 1 2 .
H311 H 0.6426 0.6441 0.6289 0.0881 0.378(10) Uiso R . P 1 2 .
H312 H 0.5792 0.5412 0.6043 0.0883 0.378(10) Uiso R . P 1 2 .
H313 H 0.6195 0.6344 0.5696 0.0880 0.378(10) Uiso R . P 1 2 .
H321 H 0.5504 0.5958 0.6175 0.0872 0.622(10) Uiso R . P 1 1 .
H322 H 0.5388 0.4921 0.5866 0.0864 0.622(10) Uiso R . P 1 1 .
H323 H 0.5632 0.5974 0.5589 0.0867 0.622(10) Uiso R . P 1 1 .
H331 H 0.8208 0.1629 0.5658 0.0411 1.0000 Uiso R . . . . .
H341 H 0.8304 0.0411 0.5016 0.0664 1.0000 Uiso R . . . . .
H342 H 0.8579 0.1273 0.4600 0.0661 1.0000 Uiso R . . . . .
H343 H 0.7218 0.1224 0.4839 0.0673 1.0000 Uiso R . . . . .
H351 H 1.0276 0.0974 0.5433 0.0825 1.0000 Uiso R . . . . .
H352 H 1.0347 0.2105 0.5739 0.0817 1.0000 Uiso R . . . . .
H353 H 1.0404 0.2044 0.5142 0.0795 1.0000 Uiso R . . . . .
H362 H 0.5782 0.3540 0.7168 0.0426 1.0000 Uiso R . . . . .
H361 H 0.5927 0.4320 0.6719 0.0436 1.0000 Uiso R . . . . .
H391 H 0.4095 0.2987 0.6489 0.0446 1.0000 Uiso R . . . . .
H401 H 0.3743 0.1402 0.6821 0.0554 1.0000 Uiso R . . . . .
H402 H 0.2450 0.1696 0.6515 0.0562 1.0000 Uiso R . . . . .
H411 H 0.3140 -0.0122 0.6444 0.0603 1.0000 Uiso R . . . . .
H412 H 0.2734 0.0438 0.5909 0.0596 1.0000 Uiso R . . . . .
H421 H 0.5183 -0.0092 0.6339 0.0526 1.0000 Uiso R . . . . .
H422 H 0.4522 -0.0454 0.5805 0.0506 1.0000 Uiso R . . . . .
H431 H 0.6185 0.0757 0.5707 0.0387 1.0000 Uiso R . . . . .
H441 H 0.5296 0.1914 0.5132 0.0541 1.0000 Uiso R . . . . .
H442 H 0.4551 0.0779 0.5051 0.0550 1.0000 Uiso R . . . . .
H451 H 0.2765 0.1445 0.5372 0.0586 1.0000 Uiso R . . . . .
H452 H 0.3212 0.2320 0.4998 0.0593 1.0000 Uiso R . . . . .
H461 H 0.2602 0.2980 0.5790 0.0567 1.0000 Uiso R . . . . .
H462 H 0.3965 0.3389 0.5646 0.0575 1.0000 Uiso R . . . . .
H382 H 0.6055 0.2679 0.6001 0.0350 1.0000 Uiso R . . . . .
H381 H 0.6020 0.1742 0.6565 0.0358 1.0000 Uiso R . . . . .
H371 H 0.6878 0.5030 0.7475 0.0586 1.0000 Uiso R . . . . .
H372 H 0.7788 0.4102 0.7540 0.0586 1.0000 Uiso R . . . . .
H373 H 0.7900 0.4875 0.7104 0.0586 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          5.08(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 . N2 . 1.9189(10) yes
Al1 . N6 . 1.9182(10) yes
Al1 . C36 . 1.9686(12) yes
Al1 . B38 . 2.2510(13) yes
Al1 . H382 . 1.819 no
Al1 . H381 . 1.768 no
N2 . C3 . 1.3393(15) yes
N2 . C21 . 1.4531(14) yes
C3 . C4 . 1.3983(18) yes
C3 . C20 . 1.5090(16) yes
C4 . C5 . 1.3956(17) yes
C4 . H41 . 0.985 no
C5 . N6 . 1.3359(15) yes
C5 . C19 . 1.5101(17) yes
N6 . C7 . 1.4517(14) yes
C7 . C8 . 1.4068(18) yes
C7 . C12 . 1.4008(19) yes
C8 . C9 . 1.3965(19) yes
C8 . C16 . 1.515(2) yes
C9 . C10 . 1.372(2) yes
C9 . H91 . 0.969 no
C10 . C11 . 1.384(2) yes
C10 . H101 . 0.970 no
C11 . C12 . 1.3968(18) yes
C11 . H111 . 0.994 no
C12 . C13 . 1.518(2) yes
C13 . C14 . 1.527(2) yes
C13 . C15 . 1.523(2) yes
C13 . H131 . 1.018 no
C14 . H141 . 0.992 no
C14 . H142 . 0.926 no
C14 . H143 . 1.040 no
C15 . H151 . 0.994 no
C15 . H152 . 1.000 no
C15 . H153 . 0.984 no
C16 . C17 . 1.532(2) yes
C16 . C18 . 1.539(2) yes
C16 . H161 . 1.017 no
C17 . H171 . 0.994 no
C17 . H172 . 0.975 no
C17 . H173 . 0.981 no
C18 . H182 . 0.989 no
C18 . H181 . 0.989 no
C18 . H183 . 0.998 no
C19 . H191 . 0.988 no
C19 . H192 . 0.976 no
C19 . H193 . 0.987 no
C20 . H201 . 0.949 no
C20 . H202 . 0.963 no
C20 . H203 . 0.970 no
C21 . C22 . 1.4058(16) yes
C21 . C26 . 1.3985(17) yes
C22 . C23 . 1.3935(17) yes
C22 . C33 . 1.5213(17) yes
C23 . C24 . 1.380(2) yes
C23 . H231 . 0.986 no
C24 . C25 . 1.370(2) yes
C24 . H241 . 0.971 no
C25 . C26 . 1.3891(18) yes
C25 . H251 . 0.984 no
C26 . C27 . 1.531(2) yes
C26 . C28 . 1.543(3) yes
C27 . C29 . 1.530(3) yes
C27 . C32 . 1.538(3) yes
C27 . H271 . 1.014 no
C28 . C30 . 1.565(4) yes
C28 . C31 . 1.504(4) yes
C28 . H281 . 1.012 no
C29 . H291 . 0.978 no
C29 . H292 . 0.959 no
C29 . H293 . 0.988 no
C30 . H302 . 0.975 no
C30 . H301 . 0.995 no
C30 . H303 . 0.944 no
C31 . H311 . 0.987 no
C31 . H312 . 0.974 no
C31 . H313 . 0.995 no
C32 . H321 . 0.992 no
C32 . H322 . 0.983 no
C32 . H323 . 0.970 no
C33 . C34 . 1.5257(17) yes
C33 . C35 . 1.5238(18) yes
C33 . H331 . 1.051 no
C34 . H341 . 1.005 no
C34 . H342 . 1.009 no
C34 . H343 . 0.989 no
C35 . H351 . 1.020 no
C35 . H352 . 1.014 no
C35 . H353 . 0.974 no
C36 . C37 . 1.5330(19) yes
C36 . H362 . 1.004 no
C36 . H361 . 1.002 no
C37 . H371 . 0.953 no
C37 . H372 . 0.958 no
C37 . H373 . 0.963 no
B38 . C39 . 1.6078(17) yes
B38 . C43 . 1.6009(18) yes
B38 . H382 . 1.216 no
B38 . H381 . 1.236 no
C39 . C40 . 1.5368(19) yes
C39 . C46 . 1.5442(19) yes
C39 . H391 . 1.018 no
C40 . C41 . 1.531(2) yes
C40 . H401 . 0.982 no
C40 . H402 . 1.011 no
C41 . C42 . 1.537(2) yes
C41 . H411 . 1.002 no
C41 . H412 . 1.041 no
C42 . C43 . 1.5408(18) yes
C42 . H421 . 1.018 no
C42 . H422 . 0.994 no
C43 . C44 . 1.5394(18) yes
C43 . H431 . 1.008 no
C44 . C45 . 1.519(2) yes
C44 . H441 . 1.030 no
C44 . H442 . 1.032 no
C45 . C46 . 1.524(2) yes
C45 . H451 . 1.015 no
C45 . H452 . 1.010 no
C46 . H461 . 0.999 no
C46 . H462 . 1.021 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 . Al1 . N6 . 95.11(4) yes
N2 . Al1 . C36 . 111.58(5) yes
N6 . Al1 . C36 . 113.19(5) yes
N2 . Al1 . B38 . 116.79(5) yes
N6 . Al1 . B38 . 114.70(5) yes
C36 . Al1 . B38 . 105.60(5) yes
N2 . Al1 . H382 . 88.2 no
N6 . Al1 . H382 . 137.2 no
C36 . Al1 . H382 . 104.9 no
B38 . Al1 . H382 . 32.6 no
N2 . Al1 . H381 . 139.4 no
N6 . Al1 . H381 . 85.8 no
C36 . Al1 . H381 . 105.1 no
B38 . Al1 . H381 . 33.1 no
H382 . Al1 . H381 . 65.6 no
Al1 . N2 . C3 . 117.18(8) yes
Al1 . N2 . C21 . 123.60(7) yes
C3 . N2 . C21 . 118.34(9) yes
N2 . C3 . C4 . 123.15(10) yes
N2 . C3 . C20 . 120.66(11) yes
C4 . C3 . C20 . 116.19(11) yes
C3 . C4 . C5 . 127.14(11) yes
C3 . C4 . H41 . 116.2 no
C5 . C4 . H41 . 116.3 no
C4 . C5 . N6 . 122.66(11) yes
C4 . C5 . C19 . 116.80(11) yes
N6 . C5 . C19 . 120.53(11) yes
C5 . N6 . Al1 . 117.70(8) yes
C5 . N6 . C7 . 118.80(9) yes
Al1 . N6 . C7 . 123.04(7) yes
N6 . C7 . C8 . 119.90(11) yes
N6 . C7 . C12 . 118.68(11) yes
C8 . C7 . C12 . 121.39(11) yes
C7 . C8 . C9 . 117.86(14) yes
C7 . C8 . C16 . 122.78(12) yes
C9 . C8 . C16 . 119.36(13) yes
C8 . C9 . C10 . 121.58(14) yes
C8 . C9 . H91 . 118.9 no
C10 . C9 . H91 . 119.5 no
C9 . C10 . C11 . 119.88(13) yes
C9 . C10 . H101 . 119.9 no
C11 . C10 . H101 . 120.2 no
C10 . C11 . C12 . 121.11(15) yes
C10 . C11 . H111 . 120.0 no
C12 . C11 . H111 . 118.9 no
C7 . C12 . C11 . 118.17(13) yes
C7 . C12 . C13 . 122.32(11) yes
C11 . C12 . C13 . 119.47(13) yes
C12 . C13 . C14 . 111.10(14) yes
C12 . C13 . C15 . 113.31(13) yes
C14 . C13 . C15 . 109.45(14) yes
C12 . C13 . H131 . 107.8 no
C14 . C13 . H131 . 107.3 no
C15 . C13 . H131 . 107.6 no
C13 . C14 . H141 . 106.7 no
C13 . C14 . H142 . 110.3 no
H141 . C14 . H142 . 111.0 no
C13 . C14 . H143 . 105.9 no
H141 . C14 . H143 . 109.3 no
H142 . C14 . H143 . 113.3 no
C13 . C15 . H151 . 111.0 no
C13 . C15 . H152 . 107.9 no
H151 . C15 . H152 . 107.9 no
C13 . C15 . H153 . 112.9 no
H151 . C15 . H153 . 108.1 no
H152 . C15 . H153 . 108.9 no
C8 . C16 . C17 . 112.35(14) yes
C8 . C16 . C18 . 110.64(14) yes
C17 . C16 . C18 . 110.08(15) yes
C8 . C16 . H161 . 108.2 no
C17 . C16 . H161 . 107.1 no
C18 . C16 . H161 . 108.3 no
C16 . C17 . H171 . 110.3 no
C16 . C17 . H172 . 108.2 no
H171 . C17 . H172 . 108.4 no
C16 . C17 . H173 . 109.3 no
H171 . C17 . H173 . 109.5 no
H172 . C17 . H173 . 111.0 no
C16 . C18 . H182 . 108.7 no
C16 . C18 . H181 . 109.9 no
H182 . C18 . H181 . 109.0 no
C16 . C18 . H183 . 108.9 no
H182 . C18 . H183 . 110.2 no
H181 . C18 . H183 . 110.0 no
C5 . C19 . H191 . 112.5 no
C5 . C19 . H192 . 106.4 no
H191 . C19 . H192 . 105.3 no
C5 . C19 . H193 . 113.0 no
H191 . C19 . H193 . 110.9 no
H192 . C19 . H193 . 108.1 no
C3 . C20 . H201 . 110.3 no
C3 . C20 . H202 . 109.1 no
H201 . C20 . H202 . 110.0 no
C3 . C20 . H203 . 109.8 no
H201 . C20 . H203 . 108.3 no
H202 . C20 . H203 . 109.3 no
N2 . C21 . C22 . 118.87(10) yes
N2 . C21 . C26 . 120.44(10) yes
C22 . C21 . C26 . 120.70(11) yes
C21 . C22 . C23 . 117.86(12) yes
C21 . C22 . C33 . 121.74(11) yes
C23 . C22 . C33 . 120.40(11) yes
C22 . C23 . C24 . 121.66(12) yes
C22 . C23 . H231 . 118.9 no
C24 . C23 . H231 . 119.4 no
C23 . C24 . C25 . 119.58(13) yes
C23 . C24 . H241 . 120.3 no
C25 . C24 . H241 . 120.1 no
C24 . C25 . C26 . 121.23(13) yes
C24 . C25 . H251 . 119.9 no
C26 . C25 . H251 . 118.9 no
C21 . C26 . C25 . 118.90(12) yes
C21 . C26 . C27 . 123.31(12) yes
C25 . C26 . C27 . 117.00(13) yes
C21 . C26 . C25 . 118.90(12) yes
C21 . C26 . C28 . 122.49(15) yes
C25 . C26 . C28 . 117.65(15) yes
C26 . C27 . C29 . 111.07(6) yes
C26 . C27 . C32 . 111.18(6) yes
C29 . C27 . C32 . 111.09(6) yes
C26 . C27 . H271 . 107.4 no
C29 . C27 . H271 . 107.8 no
C32 . C27 . H271 . 108.2 no
C26 . C28 . C30 . 111.22(6) yes
C26 . C28 . C31 . 111.02(6) yes
C30 . C28 . C31 . 111.09(6) yes
C26 . C28 . H281 . 107.6 no
C30 . C28 . H281 . 106.4 no
C31 . C28 . H281 . 109.3 no
C27 . C29 . H291 . 108.9 no
C27 . C29 . H292 . 113.8 no
H291 . C29 . H292 . 108.8 no
C27 . C29 . H293 . 109.3 no
H291 . C29 . H293 . 106.7 no
H292 . C29 . H293 . 109.2 no
C28 . C30 . H302 . 109.4 no
C28 . C30 . H301 . 110.6 no
H302 . C30 . H301 . 107.2 no
C28 . C30 . H303 . 110.5 no
H302 . C30 . H303 . 110.4 no
H301 . C30 . H303 . 108.6 no
C28 . C31 . H311 . 109.5 no
C28 . C31 . H312 . 110.6 no
H311 . C31 . H312 . 111.0 no
C28 . C31 . H313 . 108.8 no
H311 . C31 . H313 . 107.7 no
H312 . C31 . H313 . 109.2 no
C27 . C32 . H321 . 112.8 no
C27 . C32 . H322 . 109.4 no
H321 . C32 . H322 . 106.1 no
C27 . C32 . H323 . 111.4 no
H321 . C32 . H323 . 108.4 no
H322 . C32 . H323 . 108.5 no
C22 . C33 . C34 . 113.32(11) yes
C22 . C33 . C35 . 112.17(11) yes
C34 . C33 . C35 . 109.58(11) yes
C22 . C33 . H331 . 105.7 no
C34 . C33 . H331 . 108.0 no
C35 . C33 . H331 . 107.9 no
C33 . C34 . H341 . 108.3 no
C33 . C34 . H342 . 110.7 no
H341 . C34 . H342 . 107.5 no
C33 . C34 . H343 . 110.9 no
H341 . C34 . H343 . 108.4 no
H342 . C34 . H343 . 110.8 no
C33 . C35 . H351 . 111.5 no
C33 . C35 . H352 . 111.1 no
H351 . C35 . H352 . 111.3 no
C33 . C35 . H353 . 107.7 no
H351 . C35 . H353 . 106.8 no
H352 . C35 . H353 . 108.3 no
Al1 . C36 . C37 . 118.64(9) yes
Al1 . C36 . H362 . 107.4 no
C37 . C36 . H362 . 109.5 no
Al1 . C36 . H361 . 105.7 no
C37 . C36 . H361 . 109.7 no
H362 . C36 . H361 . 105.0 no
C36 . C37 . H371 . 111.2 no
C36 . C37 . H372 . 111.0 no
H371 . C37 . H372 . 108.5 no
C36 . C37 . H373 . 110.2 no
H371 . C37 . H373 . 108.1 no
H372 . C37 . H373 . 107.7 no
Al1 . B38 . C39 . 119.51(9) yes
Al1 . B38 . C43 . 132.24(8) yes
C39 . B38 . C43 . 108.25(10) yes
Al1 . B38 . H382 . 53.8 no
C39 . B38 . H382 . 109.6 no
C43 . B38 . H382 . 111.3 no
Al1 . B38 . H381 . 51.4 no
C39 . B38 . H381 . 110.5 no
C43 . B38 . H381 . 112.3 no
H382 . B38 . H381 . 104.9 no
B38 . C39 . C40 . 108.83(11) yes
B38 . C39 . C46 . 107.46(10) yes
C40 . C39 . C46 . 113.79(12) yes
B38 . C39 . H391 . 111.3 no
C40 . C39 . H391 . 108.3 no
C46 . C39 . H391 . 107.2 no
C39 . C40 . C41 . 116.09(11) yes
C39 . C40 . H401 . 105.6 no
C41 . C40 . H401 . 107.4 no
C39 . C40 . H402 . 111.1 no
C41 . C40 . H402 . 108.8 no
H401 . C40 . H402 . 107.4 no
C40 . C41 . C42 . 115.13(11) yes
C40 . C41 . H411 . 110.9 no
C42 . C41 . H411 . 106.5 no
C40 . C41 . H412 . 110.2 no
C42 . C41 . H412 . 107.0 no
H411 . C41 . H412 . 106.7 no
C41 . C42 . C43 . 115.11(11) yes
C41 . C42 . H421 . 106.1 no
C43 . C42 . H421 . 108.5 no
C41 . C42 . H422 . 108.4 no
C43 . C42 . H422 . 110.9 no
H421 . C42 . H422 . 107.5 no
C42 . C43 . B38 . 107.64(10) yes
C42 . C43 . C44 . 114.55(11) yes
B38 . C43 . C44 . 108.52(10) yes
C42 . C43 . H431 . 107.8 no
B38 . C43 . H431 . 111.4 no
C44 . C43 . H431 . 107.0 no
C43 . C44 . C45 . 115.38(11) yes
C43 . C44 . H441 . 107.2 no
C45 . C44 . H441 . 108.0 no
C43 . C44 . H442 . 108.1 no
C45 . C44 . H442 . 109.0 no
H441 . C44 . H442 . 109.1 no
C44 . C45 . C46 . 114.17(12) yes
C44 . C45 . H451 . 110.7 no
C46 . C45 . H451 . 108.4 no
C44 . C45 . H452 . 109.2 no
C46 . C45 . H452 . 108.4 no
H451 . C45 . H452 . 105.5 no
C39 . C46 . C45 . 114.74(12) yes
C39 . C46 . H461 . 108.2 no
C45 . C46 . H461 . 109.5 no
C39 . C46 . H462 . 107.0 no
C45 . C46 . H462 . 109.4 no
H461 . C46 . H462 . 107.8 no
B38 . H382 . Al1 . 93.6 no
B38 . H381 . Al1 . 95.4 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C20 . H202 . C30 . 146.60(11) 0.963 2.569 3.415(3) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 16/02/16 at 20:02:08
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE AL  (   1,X'S) H   ( 382,X'S) H   ( 381,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) H   ( 183,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) H   ( 203,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 301,X'S) H   ( 303,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 16/02/16 at 20:02:08
#
#LIST     16                                                                    
REM 
REM DIPP DISORDER 
REM 
SAME  C(28)  C(30)  C(31)  C(26) AND 
CONT  C(28)  C(31)  C(26)  C(30) AND 
CONT  C(28)  C(26)  C(30)  C(31) AND 
CONT  C(27)  C(29)  C(32)  C(26) AND 
CONT  C(27)  C(32)  C(26)  C(29) AND 
CONT  C(27)  C(26)  C(29)  C(32) 
SIMU 0.01 C(28)  C(30)  C(31)  C(26) AND 
CONT  C(28)  C(31)  C(26)  C(30) AND 
CONT  C(28)  C(26)  C(30)  C(31) AND 
CONT  C(27)  C(29)  C(32)  C(26) AND 
CONT  C(27)  C(32)  C(26)  C(29) AND 
CONT  C(27)  C(26)  C(29)  C(32) 
DELU 0.01 C(28)  C(30)  C(31)  C(26) AND 
CONT  C(28)  C(31)  C(26)  C(30) AND 
CONT  C(28)  C(26)  C(30)  C(31) AND 
CONT  C(27)  C(29)  C(32)  C(26) AND 
CONT  C(27)  C(32)  C(26)  C(29) AND 
CONT  C(27)  C(26)  C(29)  C(32) 
END                                                                             
;
####################################################################### 
# 
# 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_global
_database_code_depnum_ccdc_archive 'CCDC 1895242'
loop_
_audit_author_name
_audit_author_address
'Simon Aldridge'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-02-01 deposited with the CCDC.	2019-02-25 downloaded from the CCDC.
;
_audit_creation_date             2017-02-13
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title 191acek17
_chemical_name_systematic        ?
_chemical_melting_point          ?


_cell_length_a                   8.9708(3)
_cell_length_b                   19.9599(6)
_cell_length_c                   10.2247(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.937(3)
_cell_angle_gamma                90
_cell_volume                     1731.71(10)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z
-x,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Al 0.2130 0.2455 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886
1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C22 H20 Al2 B2 N2 
# Dc =      0.74 Fooo =    624.00 Mu =      7.92 M =    194.00
# Found Formula = C37 H58 Al1 B1 N2 
# Dc =      1.09 FOOO =    624.00 Mu =      6.90 M =    284.34

_chemical_formula_sum            'C37 H58 Al1 B1 N2'
_chemical_formula_moiety         'C37 H58 Al1 B1 N2'
_chemical_compound_source        ?
_chemical_formula_weight         568.67


_cell_measurement_reflns_used    4127
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.210

_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             624
_exptl_absorpt_coefficient_mu    0.690

# Sheldrick geometric approximatio 0.87 0.97 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.97
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            9092
_reflns_number_total             3678
_diffrn_reflns_av_R_equivalents  0.021
# Number of reflections without Friedels Law is 5226 
# Number of reflections with Friedels Law is 3678 
# Theoretical number of reflections is about 3624 


_diffrn_reflns_theta_min         4.430
_diffrn_reflns_theta_max         76.171
_diffrn_measured_fraction_theta_max 0.986

_diffrn_reflns_theta_full        73.886
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -11
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              25
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.26
_refine_diff_density_max         0.28


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3663
_refine_ls_number_restraints     0
_refine_ls_number_parameters     193
_oxford_refine_ls_R_factor_ref   0.0435
_refine_ls_wR_factor_ref         0.1039
_refine_ls_goodness_of_fit_ref   0.9260
_refine_ls_shift/su_max          0.0004862
_refine_ls_shift/su_mean         0.0000279


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3663
_refine_ls_R_factor_all          0.0435
_refine_ls_wR_factor_all         0.1039

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3257
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_gt          0.0995

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 0.80P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Al1 Al 0.24888(6) 0.7500 0.27193(5) 0.0213 1.0000 Uani S T . . . .
N2 N 0.18289(11) 0.67997(5) 0.13987(10) 0.0208 1.0000 Uani . . . . . .
C3 C 0.05024(13) 0.68708(6) 0.03306(12) 0.0231 1.0000 Uani . . . . . .
C4 C -0.01772(19) 0.7500 -0.01013(17) 0.0249 1.0000 Uani S T . . . .
C5 C -0.03126(15) 0.62607(7) -0.04415(14) 0.0305 1.0000 Uani . . . . . .
C6 C 0.25922(14) 0.61520(6) 0.16939(12) 0.0227 1.0000 Uani . . . . . .
C7 C 0.21949(15) 0.57067(6) 0.25865(13) 0.0276 1.0000 Uani . . . . . .
C8 C 0.30385(18) 0.51072(7) 0.29221(16) 0.0372 1.0000 Uani . . . . . .
C9 C 0.42381(18) 0.49595(7) 0.24004(16) 0.0391 1.0000 Uani . . . . . .
C10 C 0.46229(16) 0.54056(7) 0.15247(15) 0.0341 1.0000 Uani . . . . . .
C11 C 0.38198(15) 0.60117(6) 0.11555(13) 0.0266 1.0000 Uani . . . . . .
C12 C 0.42852(17) 0.65111(7) 0.02331(15) 0.0343 1.0000 Uani . . . . . .
C13 C 0.3242(2) 0.64535(10) -0.12776(17) 0.0503 1.0000 Uani . . . . . .
C14 C 0.60170(18) 0.64566(8) 0.03214(17) 0.0415 1.0000 Uani . . . . . .
C15 C 0.09272(16) 0.58572(7) 0.32338(14) 0.0317 1.0000 Uani . . . . . .
C16 C -0.03492(19) 0.53137(8) 0.2894(2) 0.0456 1.0000 Uani . . . . . .
C17 C 0.1662(2) 0.59472(9) 0.48007(16) 0.0432 1.0000 Uani . . . . . .
B18 B 0.5019(2) 0.7500 0.4021(2) 0.0267 1.0000 Uani S T . . . .
C19 C 0.5434(2) 0.7500 0.56695(19) 0.0309 1.0000 Uani S T . . . .
C20 C 0.63409(17) 0.68510(8) 0.62264(14) 0.0387 1.0000 Uani . . . . . .
C21 C 0.78012(17) 0.67254(7) 0.57932(15) 0.0365 1.0000 Uani . . . . . .
C22 C 0.75372(17) 0.68542(8) 0.42536(15) 0.0368 1.0000 Uani . . . . . .
C23 C 0.6633(2) 0.7500 0.36674(18) 0.0306 1.0000 Uani S T . . . .
H41 H -0.1170 0.7500 -0.0810 0.0295 1.0000 Uiso . . . . . .
H52 H -0.1094 0.6372 -0.1292 0.0482 1.0000 Uiso . . . . . .
H51 H 0.0436 0.5945 -0.0585 0.0478 1.0000 Uiso . . . . . .
H53 H -0.0821 0.6037 0.0108 0.0489 1.0000 Uiso . . . . . .
H81 H 0.2798 0.4814 0.3555 0.0448 1.0000 Uiso . . . . . .
H91 H 0.4802 0.4548 0.2649 0.0474 1.0000 Uiso . . . . . .
H101 H 0.5474 0.5298 0.1187 0.0407 1.0000 Uiso . . . . . .
H121 H 0.4143 0.6961 0.0572 0.0403 1.0000 Uiso . . . . . .
H131 H 0.3644 0.6758 -0.1834 0.0748 1.0000 Uiso . . . . . .
H132 H 0.2163 0.6588 -0.1388 0.0746 1.0000 Uiso . . . . . .
H133 H 0.3257 0.5999 -0.1622 0.0753 1.0000 Uiso . . . . . .
H141 H 0.6271 0.6840 -0.0174 0.0616 1.0000 Uiso . . . . . .
H143 H 0.6735 0.6484 0.1284 0.0621 1.0000 Uiso . . . . . .
H142 H 0.6210 0.6040 -0.0120 0.0609 1.0000 Uiso . . . . . .
H151 H 0.0401 0.6283 0.2843 0.0352 1.0000 Uiso . . . . . .
H162 H -0.1175 0.5434 0.3259 0.0679 1.0000 Uiso . . . . . .
H163 H -0.0816 0.5254 0.1892 0.0662 1.0000 Uiso . . . . . .
H161 H 0.0092 0.4892 0.3295 0.0681 1.0000 Uiso . . . . . .
H171 H 0.0854 0.6054 0.5220 0.0650 1.0000 Uiso . . . . . .
H173 H 0.2483 0.6313 0.5027 0.0655 1.0000 Uiso . . . . . .
H172 H 0.2193 0.5532 0.5219 0.0639 1.0000 Uiso . . . . . .
H191 H 0.4468 0.7500 0.5919 0.0374 1.0000 Uiso . . . . . .
H201 H 0.6664 0.6851 0.7241 0.0480 1.0000 Uiso . . . . . .
H202 H 0.5609 0.6477 0.5860 0.0459 1.0000 Uiso . . . . . .
H211 H 0.8128 0.6258 0.6002 0.0442 1.0000 Uiso . . . . . .
H222 H 0.8562 0.6861 0.4093 0.0450 1.0000 Uiso . . . . . .
H223 H 0.6926 0.6478 0.3740 0.0437 1.0000 Uiso . . . . . .
H232 H 0.6405 0.7500 0.2648 0.0378 1.0000 Uiso . . . . . .
H13 H 0.1595 0.7500 0.3755 0.0395 1.0000 Uiso . . . . . .
H182 H 0.4185 0.7031 0.3515 0.0344 1.0000 Uiso . . . . . .
H212 H 0.8680 0.7010 0.6350 0.0430 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          7.8(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 . H182 3_565 1.746 no
Al1 . N2 3_565 1.8997(10) yes
Al1 . N2 . 1.8997(10) yes
Al1 . B18 . 2.228(2) yes
Al1 . H13 . 1.522 no
Al1 . H182 . 1.746 no
N2 . C3 . 1.3361(15) yes
N2 . C6 . 1.4481(15) yes
C3 . C4 . 1.4033(14) yes
C3 . C5 . 1.5053(17) yes
C4 . H41 . 0.948 no
C5 . H52 . 0.949 no
C5 . H51 . 0.967 no
C5 . H53 . 0.944 no
C6 . C7 . 1.4004(17) yes
C6 . C11 . 1.4099(17) yes
C7 . C8 . 1.3978(18) yes
C7 . C15 . 1.5199(17) yes
C8 . C9 . 1.379(2) yes
C8 . H81 . 0.947 no
C9 . C10 . 1.384(2) yes
C9 . H91 . 0.954 no
C10 . C11 . 1.3959(19) yes
C10 . H101 . 0.959 no
C11 . C12 . 1.5209(18) yes
C12 . C13 . 1.529(2) yes
C12 . C14 . 1.531(2) yes
C12 . H121 . 0.986 no
C13 . H131 . 0.977 no
C13 . H132 . 0.975 no
C13 . H133 . 0.974 no
C14 . H141 . 0.984 no
C14 . H143 . 0.988 no
C14 . H142 . 0.988 no
C15 . C16 . 1.533(2) yes
C15 . C17 . 1.532(2) yes
C15 . H151 . 0.991 no
C16 . H162 . 0.962 no
C16 . H163 . 0.980 no
C16 . H161 . 0.963 no
C17 . H171 . 0.978 no
C17 . H173 . 1.010 no
C17 . H172 . 0.981 no
B18 . H182 3_565 1.205 no
B18 . C19 . 1.604(3) yes
B18 . C23 . 1.601(3) yes
B18 . H182 . 1.205 no
C19 . C20 3_565 1.5374(18) yes
C19 . C20 . 1.5374(18) yes
C19 . H191 . 0.979 no
C20 . C21 . 1.534(2) yes
C20 . H201 . 0.982 no
C20 . H202 . 0.984 no
C21 . C22 . 1.536(2) yes
C21 . H211 . 0.981 no
C21 . H212 . 0.989 no
C22 . C23 . 1.5374(17) yes
C22 . H222 . 0.985 no
C22 . H223 . 0.977 no
C23 . H232 . 0.995 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
H182 3_565 Al1 . N2 3_565 87.7 no
H182 3_565 Al1 . N2 . 138.5 no
N2 3_565 Al1 . N2 . 94.75(6) yes
H182 3_565 Al1 . B18 . 32.5 no
N2 3_565 Al1 . B18 . 116.53(5) yes
N2 . Al1 . B18 . 116.53(5) yes
H182 3_565 Al1 . H13 . 104.6 no
N2 3_565 Al1 . H13 . 112.4 no
N2 . Al1 . H13 . 112.4 no
B18 . Al1 . H13 . 104.4 no
H182 3_565 Al1 . H182 . 64.8 no
N2 3_565 Al1 . H182 . 138.5 no
N2 . Al1 . H182 . 87.7 no
B18 . Al1 . H182 . 32.5 no
H13 . Al1 . H182 . 104.6 no
Al1 . N2 . C3 . 119.49(8) yes
Al1 . N2 . C6 . 119.44(7) yes
C3 . N2 . C6 . 120.04(10) yes
N2 . C3 . C4 . 122.21(11) yes
N2 . C3 . C5 . 119.66(11) yes
C4 . C3 . C5 . 118.13(11) yes
C3 . C4 . C3 3_565 127.01(15) yes
C3 . C4 . H41 . 116.4 no
C3 3_565 C4 . H41 . 116.4 no
C3 . C5 . H52 . 112.4 no
C3 . C5 . H51 . 111.4 no
H52 . C5 . H51 . 110.9 no
C3 . C5 . H53 . 108.5 no
H52 . C5 . H53 . 107.4 no
H51 . C5 . H53 . 106.0 no
N2 . C6 . C7 . 119.95(10) yes
N2 . C6 . C11 . 118.19(11) yes
C7 . C6 . C11 . 121.65(11) yes
C6 . C7 . C8 . 118.12(12) yes
C6 . C7 . C15 . 122.89(11) yes
C8 . C7 . C15 . 118.97(12) yes
C7 . C8 . C9 . 121.09(13) yes
C7 . C8 . H81 . 118.1 no
C9 . C8 . H81 . 120.7 no
C8 . C9 . C10 . 120.17(13) yes
C8 . C9 . H91 . 119.6 no
C10 . C9 . H91 . 120.3 no
C9 . C10 . C11 . 121.17(12) yes
C9 . C10 . H101 . 118.9 no
C11 . C10 . H101 . 119.9 no
C6 . C11 . C10 . 117.81(12) yes
C6 . C11 . C12 . 121.22(11) yes
C10 . C11 . C12 . 120.95(11) yes
C11 . C12 . C13 . 112.10(12) yes
C11 . C12 . C14 . 113.23(12) yes
C13 . C12 . C14 . 109.32(12) yes
C11 . C12 . H121 . 106.7 no
C13 . C12 . H121 . 108.5 no
C14 . C12 . H121 . 106.8 no
C12 . C13 . H131 . 108.8 no
C12 . C13 . H132 . 110.8 no
H131 . C13 . H132 . 107.6 no
C12 . C13 . H133 . 111.1 no
H131 . C13 . H133 . 108.5 no
H132 . C13 . H133 . 110.1 no
C12 . C14 . H141 . 108.3 no
C12 . C14 . H143 . 112.1 no
H141 . C14 . H143 . 106.5 no
C12 . C14 . H142 . 111.0 no
H141 . C14 . H142 . 108.4 no
H143 . C14 . H142 . 110.4 no
C7 . C15 . C16 . 111.76(12) yes
C7 . C15 . C17 . 110.48(11) yes
C16 . C15 . C17 . 110.86(12) yes
C7 . C15 . H151 . 108.7 no
C16 . C15 . H151 . 107.0 no
C17 . C15 . H151 . 107.9 no
C15 . C16 . H162 . 110.4 no
C15 . C16 . H163 . 111.0 no
H162 . C16 . H163 . 108.3 no
C15 . C16 . H161 . 110.4 no
H162 . C16 . H161 . 108.3 no
H163 . C16 . H161 . 108.4 no
C15 . C17 . H171 . 110.8 no
C15 . C17 . H173 . 111.0 no
H171 . C17 . H173 . 109.4 no
C15 . C17 . H172 . 109.8 no
H171 . C17 . H172 . 108.5 no
H173 . C17 . H172 . 107.2 no
H182 3_565 B18 . Al1 . 51.2 no
H182 3_565 B18 . C19 . 110.5 no
Al1 . B18 . C19 . 118.12(13) yes
H182 3_565 B18 . C23 . 112.6 no
Al1 . B18 . C23 . 133.29(13) yes
C19 . B18 . C23 . 108.59(14) yes
H182 3_565 B18 . H182 . 101.9 no
Al1 . B18 . H182 . 51.2 no
C19 . B18 . H182 . 110.5 no
C23 . B18 . H182 . 112.6 no
C20 3_565 C19 . B18 . 107.67(10) yes
C20 3_565 C19 . C20 . 114.82(16) yes
B18 . C19 . C20 . 107.67(10) yes
C20 3_565 C19 . H191 . 108.1 no
B18 . C19 . H191 . 110.5 no
C20 . C19 . H191 . 108.1 no
C19 . C20 . C21 . 115.46(12) yes
C19 . C20 . H201 . 109.3 no
C21 . C20 . H201 . 108.6 no
C19 . C20 . H202 . 106.9 no
C21 . C20 . H202 . 107.1 no
H201 . C20 . H202 . 109.4 no
C20 . C21 . C22 . 114.00(11) yes
C20 . C21 . H211 . 108.4 no
C22 . C21 . H211 . 108.5 no
C20 . C21 . H212 . 109.7 no
C22 . C21 . H212 . 108.8 no
H211 . C21 . H212 . 107.2 no
C21 . C22 . C23 . 115.23(13) yes
C21 . C22 . H222 . 109.3 no
C23 . C22 . H222 . 109.1 no
C21 . C22 . H223 . 107.2 no
C23 . C22 . H223 . 107.5 no
H222 . C22 . H223 . 108.2 no
C22 . C23 . C22 3_565 113.96(16) yes
C22 . C23 . B18 . 108.26(10) yes
C22 3_565 C23 . B18 . 108.26(10) yes
C22 . C23 . H232 . 108.1 no
C22 3_565 C23 . H232 . 108.1 no
B18 . C23 . H232 . 110.0 no
Al1 . H182 . B18 . 96.3 no


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 13/02/17 at 10:38:22
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 13/02/17 at 10:38:22
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_060acmaf17
_database_code_depnum_ccdc_archive 'CCDC 1895245'
loop_
_audit_author_name
_audit_author_address
'Simon Aldridge'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-02-01 deposited with the CCDC.	2019-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        .
_chemical_name_common            .
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C39 H64 Al B N4'
_chemical_formula_sum            'C39 H64 Al B N4'
_chemical_formula_weight         626.73

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'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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.
;

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

_cell_length_a                   9.01940(10)
_cell_length_b                   21.1266(3)
_cell_length_c                   10.7665(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.865(2)
_cell_angle_gamma                90
_cell_volume                     1876.14(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8122
_cell_measurement_theta_min      4.4630
_cell_measurement_theta_max      75.9490

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.693
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_T_min  0.90443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_reflns_number            13033
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.185
_diffrn_reflns_theta_max         76.114
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3997
_reflns_number_gt                3687
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'SHELXLE (HUbschle, 2017)'
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_refine_special_details          
;
The hydrogen atoms were set at geometric
positions. The exception is the hydrides, 
which were located using the difference Fourier map 
and then refined. 
This resulted with hydrogens and the hydrides 
at sensible positions.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²+0.7161P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   .
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3997
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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_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 0.24594(5) 0.750000 0.77531(4) 0.01700(11) Uani 1 2 d S T P . .
H H 0.209(2) 0.750000 0.899(2) 0.028(5) Uiso 1 2 d S . P . .
H1 H 0.4336(16) 0.7056(7) 0.8247(14) 0.028(3) Uiso 1 1 d . . . . .
N1 N 0.14295(10) 0.68148(4) 0.65634(9) 0.01737(18) Uani 1 1 d . . . . .
N2 N -0.09696(12) 0.63857(5) 0.48985(10) 0.0247(2) Uani 1 1 d . . . . .
C1 C -0.00733(12) 0.69003(5) 0.55709(10) 0.0187(2) Uani 1 1 d . . . . .
C2 C -0.07754(18) 0.750000 0.51927(15) 0.0202(3) Uani 1 2 d S T P . .
H2 H -0.188997 0.750000 0.459242 0.024 Uiso 1 2 calc R U P . .
C3 C -0.10676(16) 0.58148(6) 0.56231(14) 0.0326(3) Uani 1 1 d . . . . .
H3A H -0.219181 0.574831 0.550612 0.049 Uiso 1 1 calc R U . . .
H3B H -0.037416 0.586248 0.659135 0.049 Uiso 1 1 calc R U . . .
H3C H -0.070268 0.545008 0.525887 0.049 Uiso 1 1 calc R U . . .
C4 C -0.23269(15) 0.64670(6) 0.35881(13) 0.0336(3) Uani 1 1 d . . . . .
H4A H -0.204401 0.678215 0.305228 0.050 Uiso 1 1 calc R U . . .
H4B H -0.328035 0.661115 0.372853 0.050 Uiso 1 1 calc R U . . .
H4C H -0.256964 0.606227 0.310171 0.050 Uiso 1 1 calc R U . . .
C5 C 0.23158(13) 0.62343(5) 0.66522(11) 0.0192(2) Uani 1 1 d . . . . .
C6 C 0.27896(13) 0.60601(5) 0.56011(11) 0.0217(2) Uani 1 1 d . . . . .
C7 C 0.38256(15) 0.55430(6) 0.58073(12) 0.0269(3) Uani 1 1 d . . . . .
H7 H 0.414866 0.542118 0.510426 0.032 Uiso 1 1 calc R U . . .
C8 C 0.43932(15) 0.52037(6) 0.70057(13) 0.0303(3) Uani 1 1 d . . . . .
H8 H 0.513291 0.486409 0.714036 0.036 Uiso 1 1 calc R U . . .
C9 C 0.38718(16) 0.53644(6) 0.80056(12) 0.0292(3) Uani 1 1 d . . . . .
H9 H 0.423680 0.512244 0.881850 0.035 Uiso 1 1 calc R U . . .
C10 C 0.28251(14) 0.58714(5) 0.78566(11) 0.0228(2) Uani 1 1 d . . . . .
C11 C 0.22462(15) 0.59928(6) 0.89849(12) 0.0266(3) Uani 1 1 d . . . . .
H11 H 0.141866 0.633851 0.867785 0.032 Uiso 1 1 calc R U . . .
C12 C 0.36232(17) 0.62050(6) 1.03106(12) 0.0328(3) Uani 1 1 d . . . . .
H12A H 0.409528 0.659900 1.015432 0.049 Uiso 1 1 calc R U . . .
H12B H 0.445995 0.587602 1.062241 0.049 Uiso 1 1 calc R U . . .
H12C H 0.319536 0.627580 1.100337 0.049 Uiso 1 1 calc R U . . .
C13 C 0.14402(19) 0.54013(6) 0.92684(14) 0.0385(3) Uani 1 1 d . . . . .
H13A H 0.055760 0.526147 0.842521 0.058 Uiso 1 1 calc R U . . .
H13B H 0.100369 0.550287 0.994323 0.058 Uiso 1 1 calc R U . . .
H13C H 0.224559 0.506249 0.961753 0.058 Uiso 1 1 calc R U . . .
C14 C 0.22203(15) 0.63985(6) 0.42372(12) 0.0269(3) Uani 1 1 d . . . . .
H14 H 0.157095 0.677730 0.426753 0.032 Uiso 1 1 calc R U . . .
C15 C 0.11340(16) 0.59590(7) 0.30967(12) 0.0345(3) Uani 1 1 d . . . . .
H15A H 0.071723 0.618986 0.223344 0.052 Uiso 1 1 calc R U . . .
H15B H 0.022457 0.581287 0.329923 0.052 Uiso 1 1 calc R U . . .
H15C H 0.176684 0.559358 0.302937 0.052 Uiso 1 1 calc R U . . .
C16 C 0.36450(18) 0.66206(7) 0.39221(14) 0.0362(3) Uani 1 1 d . . . . .
H16A H 0.423850 0.625180 0.380991 0.054 Uiso 1 1 calc R U . . .
H16B H 0.437281 0.688258 0.467199 0.054 Uiso 1 1 calc R U . . .
H16C H 0.323648 0.686959 0.308233 0.054 Uiso 1 1 calc R U . . .
C17 C 0.6047(2) 0.750000 0.73808(18) 0.0301(4) Uani 1 2 d S T P . .
H17 H 0.518205 0.750000 0.643669 0.036 Uiso 1 2 calc R U P . .
C18 C 0.7039(2) 0.81115(7) 0.75805(16) 0.0429(3) Uani 1 1 d . . . . .
H18A H 0.763777 0.809393 0.698737 0.051 Uiso 1 1 calc R U . . .
H18B H 0.627896 0.847341 0.727623 0.051 Uiso 1 1 calc R U . . .
C19 C 0.8246(2) 0.82368(10) 0.9030(2) 0.0592(5) Uani 1 1 d . . . . .
H19A H 0.859749 0.868417 0.910119 0.071 Uiso 1 1 calc R U . . .
H19B H 0.921409 0.796866 0.922223 0.071 Uiso 1 1 calc R U . . .
C20 C 0.75873(19) 0.81085(11) 1.01159(17) 0.0653(6) Uani 1 1 d . . . . .
H20A H 0.690259 0.847172 1.013354 0.078 Uiso 1 1 calc R U . . .
H20B H 0.851554 0.809037 1.101237 0.078 Uiso 1 1 calc R U . . .
C21 C 0.6590(2) 0.750000 0.99302(18) 0.0413(5) Uani 1 2 d S T P . .
H21 H 0.607727 0.750000 1.059808 0.050 Uiso 1 2 calc R U P . .
B1 B 0.5189(2) 0.750000 0.84223(19) 0.0235(4) Uani 1 2 d S T P . .


_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 1.9069(9) 4_575 ?
Al1 N1 1.9069(9) . ?
Al1 B1 2.2679(18) . ?
Al1 H 1.49(2) . ?
Al1 H1 1.816(14) . ?
N1 C1 1.3563(14) . ?
N1 C5 1.4458(13) . ?
N2 C1 1.3734(14) . ?
N2 C4 1.4564(15) . ?
N2 C3 1.4584(15) . ?
C1 C2 1.4011(12) . ?
C2 H2 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.4107(15) . ?
C5 C10 1.4136(15) . ?
C6 C7 1.3958(15) . ?
C6 C14 1.5235(15) . ?
C7 C8 1.3807(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.3802(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.3935(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.5256(15) . ?
C11 C12 1.5318(17) . ?
C11 C13 1.5372(17) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.5294(18) . ?
C14 C15 1.5351(17) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.5361(17) 4_575 ?
C17 C18 1.5362(17) . ?
C17 B1 1.600(3) . ?
C17 H17 1.0000 . ?
C18 C19 1.522(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.535(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.535(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 B1 1.604(2) . ?
C21 H21 1.0000 . ?
B1 H1 1.178(14) . ?

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 N1 98.77(6) 4_575 . ?
N1 Al1 B1 112.62(4) 4_575 . ?
N1 Al1 B1 112.62(4) . . ?
N1 Al1 H 112.0(4) 4_575 . ?
N1 Al1 H 112.0(4) . . ?
B1 Al1 H 108.6(8) . . ?
N1 Al1 H1 137.0(4) 4_575 . ?
N1 Al1 H1 87.0(4) . . ?
B1 Al1 H1 31.1(4) . . ?
H Al1 H1 104.7(8) . . ?
C1 N1 C5 120.98(9) . . ?
C1 N1 Al1 119.21(7) . . ?
C5 N1 Al1 119.57(7) . . ?
C1 N2 C4 120.14(10) . . ?
C1 N2 C3 121.53(10) . . ?
C4 N2 C3 113.99(10) . . ?
N1 C1 N2 119.82(10) . . ?
N1 C1 C2 122.65(10) . . ?
N2 C1 C2 117.53(10) . . ?
C1 C2 C1 129.42(14) . 4_575 ?
C1 C2 H2 115.3 . . ?
C1 C2 H2 115.3 4_575 . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 120.19(10) . . ?
C6 C5 N1 120.47(9) . . ?
C10 C5 N1 119.11(9) . . ?
C7 C6 C5 118.50(10) . . ?
C7 C6 C14 117.61(10) . . ?
C5 C6 C14 123.88(10) . . ?
C8 C7 C6 121.75(11) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C9 C8 C7 119.12(11) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 121.87(11) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C9 C10 C5 118.43(10) . . ?
C9 C10 C11 118.15(10) . . ?
C5 C10 C11 123.39(10) . . ?
C10 C11 C12 112.43(10) . . ?
C10 C11 C13 111.29(10) . . ?
C12 C11 C13 108.85(10) . . ?
C10 C11 H11 108.0 . . ?
C12 C11 H11 108.0 . . ?
C13 C11 H11 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6 C14 C16 111.84(10) . . ?
C6 C14 C15 110.14(10) . . ?
C16 C14 C15 109.25(10) . . ?
C6 C14 H14 108.5 . . ?
C16 C14 H14 108.5 . . ?
C15 C14 H14 108.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
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 . . ?
C18 C17 C18 114.47(17) 4_575 . ?
C18 C17 B1 108.75(9) 4_575 . ?
C18 C17 B1 108.75(9) . . ?
C18 C17 H17 108.2 4_575 . ?
C18 C17 H17 108.2 . . ?
B1 C17 H17 108.2 . . ?
C19 C18 C17 115.12(14) . . ?
C19 C18 H18A 108.5 . . ?
C17 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
C17 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C18 C19 C20 114.44(12) . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19B 108.7 . . ?
C20 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 C21 115.83(14) . . ?
C19 C20 H20A 108.3 . . ?
C21 C20 H20A 108.3 . . ?
C19 C20 H20B 108.3 . . ?
C21 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C20 C21 C20 113.8(2) . 4_575 ?
C20 C21 B1 108.19(11) . . ?
C20 C21 B1 108.19(11) 4_575 . ?
C20 C21 H21 108.9 . . ?
C20 C21 H21 108.9 4_575 . ?
B1 C21 H21 108.9 . . ?
C17 B1 C21 107.63(14) . . ?
C17 B1 Al1 123.24(12) . . ?
C21 B1 Al1 129.13(13) . . ?
C17 B1 H1 110.9(7) . . ?
C21 B1 H1 111.0(7) . . ?
Al1 B1 H1 52.8(7) . . ?

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
C5 N1 C1 N2 19.59(14) . . . . ?
Al1 N1 C1 N2 -166.15(8) . . . . ?
C5 N1 C1 C2 -160.69(11) . . . . ?
Al1 N1 C1 C2 13.56(15) . . . . ?
C4 N2 C1 N1 -161.05(10) . . . . ?
C3 N2 C1 N1 43.76(15) . . . . ?
C4 N2 C1 C2 19.22(16) . . . . ?
C3 N2 C1 C2 -135.97(12) . . . . ?
N1 C1 C2 C1 9.6(2) . . . 4_575 ?
N2 C1 C2 C1 -170.66(11) . . . 4_575 ?
C1 N1 C5 C6 63.67(14) . . . . ?
Al1 N1 C5 C6 -110.57(10) . . . . ?
C1 N1 C5 C10 -121.81(11) . . . . ?
Al1 N1 C5 C10 63.95(12) . . . . ?
C10 C5 C6 C7 -2.93(16) . . . . ?
N1 C5 C6 C7 171.52(10) . . . . ?
C10 C5 C6 C14 176.26(11) . . . . ?
N1 C5 C6 C14 -9.28(16) . . . . ?
C5 C6 C7 C8 -0.20(18) . . . . ?
C14 C6 C7 C8 -179.44(11) . . . . ?
C6 C7 C8 C9 2.62(19) . . . . ?
C7 C8 C9 C10 -1.9(2) . . . . ?
C8 C9 C10 C5 -1.15(19) . . . . ?
C8 C9 C10 C11 176.95(12) . . . . ?
C6 C5 C10 C9 3.59(17) . . . . ?
N1 C5 C10 C9 -170.95(10) . . . . ?
C6 C5 C10 C11 -174.40(11) . . . . ?
N1 C5 C10 C11 11.06(16) . . . . ?
C9 C10 C11 C12 67.00(14) . . . . ?
C5 C10 C11 C12 -115.00(12) . . . . ?
C9 C10 C11 C13 -55.41(15) . . . . ?
C5 C10 C11 C13 122.58(12) . . . . ?
C7 C6 C14 C16 -55.53(14) . . . . ?
C5 C6 C14 C16 125.27(12) . . . . ?
C7 C6 C14 C15 66.16(14) . . . . ?
C5 C6 C14 C15 -113.04(12) . . . . ?
C18 C17 C18 C19 -68.1(2) 4_575 . . . ?
B1 C17 C18 C19 53.76(17) . . . . ?
C17 C18 C19 C20 -43.2(2) . . . . ?
C18 C19 C20 C21 43.1(3) . . . . ?
C19 C20 C21 C20 67.5(2) . . . 4_575 ?
C19 C20 C21 B1 -52.7(2) . . . . ?
C18 C17 B1 C21 62.63(11) 4_575 . . . ?
C18 C17 B1 C21 -62.63(11) . . . . ?
C18 C17 B1 Al1 -117.37(11) 4_575 . . . ?
C18 C17 B1 Al1 117.37(11) . . . . ?
C20 C21 B1 C17 61.83(11) . . . . ?
C20 C21 B1 C17 -61.83(11) 4_575 . . . ?
C20 C21 B1 Al1 -118.17(11) . . . . ?
C20 C21 B1 Al1 118.17(11) 4_575 . . . ?

_refine_diff_density_max         0.248
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.040

####################################################################### 
# 
# 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_138ACE
_database_code_depnum_ccdc_archive 'CCDC 1895263'
loop_
_audit_author_name
_audit_author_address
'Simon Aldridge'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-02-02 deposited with the CCDC.	2019-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H57 Al B F3 N2 O3 S, 2(C7 H8)'
_chemical_formula_sum            'C52 H73 Al B F3 N2 O3 S'
_chemical_formula_weight         900.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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.
;

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

_cell_length_a                   10.193(2)
_cell_length_b                   25.619(5)
_cell_length_c                   19.416(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5070.2(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6328
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27

_exptl_crystal_description       hexagon
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_F_000             1936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.134
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11064
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         5.110
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5897
_reflns_number_gt                4088
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1014P)²+2.4999P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5897
_refine_ls_number_parameters     563
_refine_ls_number_restraints     413
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0638
_refine_ls_wR_factor_ref         0.1868
_refine_ls_wR_factor_gt          0.1664
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.185
_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_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
S1A S 0.57223(9) 0.7578(2) 0.33644(5) 0.0385(11) Uani 0.5 1 d . . P A -1
Al1 Al 0.40186(7) 0.750000 0.47321(4) 0.0246(2) Uani 1 2 d S T P A .
F1 F 0.8131(12) 0.7635(4) 0.2901(4) 0.078(3) Uani 0.25 1 d D U P A -1
F2 F 0.8037(8) 0.7346(3) 0.3937(4) 0.077(3) Uani 0.25 1 d D U P A -1
F3 F 0.7703(10) 0.8147(3) 0.3726(5) 0.083(2) Uani 0.25 1 d D U P A -1
F1A F 0.7985(12) 0.7810(4) 0.2888(4) 0.076(2) Uani 0.25 1 d D U P B -2
F2A F 0.8013(10) 0.7197(4) 0.3634(5) 0.082(2) Uani 0.25 1 d D U P C -2
F3A F 0.7792(11) 0.7983(4) 0.3949(4) 0.078(2) Uani 0.25 1 d D U P D -2
O1 O 0.53246(18) 0.750000 0.41062(9) 0.0355(5) Uani 1 2 d S T P . .
O2 O 0.5529(13) 0.7106(4) 0.2991(6) 0.0475(18) Uani 0.5 1 d . . P A -1
O2A O 0.5300(13) 0.8056(4) 0.3071(7) 0.055(2) Uani 0.5 1 d . . P A -1
N1 N 0.28980(15) 0.69464(6) 0.45103(7) 0.0270(3) Uani 1 1 d . . . . .
C1 C 0.28730(19) 0.64513(7) 0.48777(10) 0.0374(4) Uani 1 1 d D U . . .
C2 C 0.1954(8) 0.6315(3) 0.5373(5) 0.0400(11) Uani 0.398(9) 1 d D U P E 1
C3 C 0.2112(8) 0.5837(3) 0.5704(4) 0.0462(14) Uani 0.398(9) 1 d D U P E 1
H3 H 0.151870 0.574001 0.605942 0.055 Uiso 0.398(9) 1 calc R U P E 1
C4 C 0.3122(9) 0.5497(3) 0.5524(4) 0.0557(14) Uani 0.398(9) 1 d D U P E 1
H4 H 0.322493 0.517678 0.576396 0.067 Uiso 0.398(9) 1 calc R U P E 1
C5 C 0.3975(8) 0.5625(2) 0.4998(5) 0.0584(14) Uani 0.398(9) 1 d D U P E 1
H5 H 0.462660 0.538542 0.484866 0.070 Uiso 0.398(9) 1 calc R U P E 1
C6 C 0.3857(7) 0.6109(3) 0.4693(4) 0.0520(12) Uani 0.398(9) 1 d D U P E 1
C7 C 0.5107(7) 0.6130(4) 0.4305(4) 0.0601(16) Uani 0.398(9) 1 d D U P E 1
H7 H 0.519242 0.649428 0.412414 0.072 Uiso 0.398(9) 1 calc R U P E 1
C8 C 0.5094(11) 0.5766(7) 0.3677(6) 0.074(3) Uani 0.398(9) 1 d D U P E 1
H8A H 0.510769 0.540218 0.383300 0.111 Uiso 0.398(9) 1 calc R U P E 1
H8B H 0.586857 0.583443 0.339196 0.111 Uiso 0.398(9) 1 calc R U P E 1
H8C H 0.429880 0.582893 0.340642 0.111 Uiso 0.398(9) 1 calc R U P E 1
C9 C 0.6307(7) 0.6029(4) 0.4746(5) 0.066(2) Uani 0.398(9) 1 d D U P E 1
H9A H 0.633976 0.628507 0.512161 0.099 Uiso 0.398(9) 1 calc R U P E 1
H9B H 0.709905 0.606141 0.446330 0.099 Uiso 0.398(9) 1 calc R U P E 1
H9C H 0.625879 0.567665 0.493977 0.099 Uiso 0.398(9) 1 calc R U P E 1
C10 C 0.0975(7) 0.6736(3) 0.5583(4) 0.0416(14) Uani 0.398(9) 1 d D U P E 1
H10 H 0.139266 0.708517 0.551655 0.050 Uiso 0.398(9) 1 calc R U P E 1
C11 C 0.0615(8) 0.6674(3) 0.6339(3) 0.0477(18) Uani 0.398(9) 1 d D U P E 1
H11A H 0.022573 0.632890 0.641384 0.072 Uiso 0.398(9) 1 calc R U P E 1
H11B H -0.001798 0.694457 0.646911 0.072 Uiso 0.398(9) 1 calc R U P E 1
H11C H 0.140659 0.670904 0.662238 0.072 Uiso 0.398(9) 1 calc R U P E 1
C12 C -0.0255(8) 0.6707(4) 0.5135(4) 0.056(2) Uani 0.398(9) 1 d D U P E 1
H12A H -0.067550 0.636571 0.519630 0.084 Uiso 0.398(9) 1 calc R U P E 1
H12B H -0.001146 0.675197 0.465033 0.084 Uiso 0.398(9) 1 calc R U P E 1
H12C H -0.086621 0.698318 0.527077 0.084 Uiso 0.398(9) 1 calc R U P E 1
C13 C 0.1617(3) 0.65428(8) 0.35668(12) 0.0479(6) Uani 1 1 d . . . . .
H13A H 0.228015 0.639574 0.325697 0.072 Uiso 1 1 calc R U . . .
H13B H 0.084828 0.665002 0.329891 0.072 Uiso 1 1 calc R U . . .
H13C H 0.135714 0.627885 0.390564 0.072 Uiso 1 1 calc R U . . .
C14 C 0.21801(19) 0.70097(7) 0.39340(9) 0.0311(4) Uani 1 1 d . . . . .
C15 C 0.1947(3) 0.750000 0.36453(13) 0.0325(6) Uani 1 2 d S T P . .
H15 H 0.158295 0.749999 0.319490 0.039 Uiso 1 2 calc R U P . .
C16 C 0.3964(3) 0.7529(3) 0.63746(15) 0.0389(8) Uani 0.5 1 d D U P A -1
H16 H 0.304256 0.754089 0.619812 0.047 Uiso 0.5 1 calc R U P A -1
C17 C 0.4268(6) 0.8043(3) 0.6746(4) 0.0393(13) Uani 0.5 1 d D U P A -1
H17A H 0.409640 0.833795 0.642937 0.047 Uiso 0.5 1 calc R U P A -1
H17B H 0.367309 0.807982 0.714632 0.047 Uiso 0.5 1 calc R U P A -1
C18 C 0.5688(4) 0.80708(19) 0.6995(2) 0.0381(9) Uani 0.5 1 d D U P A -1
H18A H 0.583055 0.780225 0.735351 0.046 Uiso 0.5 1 calc R U P A -1
H18B H 0.584880 0.841691 0.720482 0.046 Uiso 0.5 1 calc R U P A -1
C19 C 0.6665(6) 0.7984(4) 0.6404(4) 0.0426(13) Uani 0.5 1 d D U P A -1
H19A H 0.756936 0.798748 0.659079 0.051 Uiso 0.5 1 calc R U P A -1
H19B H 0.658766 0.827383 0.606941 0.051 Uiso 0.5 1 calc R U P A -1
C20 C 0.6419(3) 0.7462(3) 0.60326(16) 0.0414(9) Uani 0.5 1 d D U P A -1
H20 H 0.705426 0.742197 0.564363 0.050 Uiso 0.5 1 calc R U P A -1
C21 C 0.6540(7) 0.6997(4) 0.6520(6) 0.0583(17) Uani 0.5 1 d D U P A -1
H21A H 0.713742 0.673858 0.630743 0.070 Uiso 0.5 1 calc R U P A -1
H21B H 0.695963 0.711917 0.695098 0.070 Uiso 0.5 1 calc R U P A -1
C22 C 0.5290(6) 0.6725(2) 0.6705(4) 0.0695(14) Uani 0.5 1 d D U P A -1
H22A H 0.545480 0.651142 0.712093 0.083 Uiso 0.5 1 calc R U P A -1
H22B H 0.506886 0.648201 0.632623 0.083 Uiso 0.5 1 calc R U P A -1
C23 C 0.4116(7) 0.7060(3) 0.6841(5) 0.0547(17) Uani 0.5 1 d D U P A -1
H23A H 0.415918 0.718349 0.732302 0.066 Uiso 0.5 1 calc R U P A -1
H23B H 0.332101 0.684031 0.679656 0.066 Uiso 0.5 1 calc R U P A -1
C24 C 0.7470(5) 0.7657(2) 0.3482(3) 0.0760(17) Uani 0.5 1 d D U P A -1
C25 C 0.5367(5) 0.4794(2) 0.2246(3) 0.0890(14) Uani 0.792(7) 1 d D U P F 1
H25 H 0.487677 0.478013 0.266169 0.107 Uiso 0.792(7) 1 calc R U P F 1
C26 C 0.6444(6) 0.44599(19) 0.2163(3) 0.1067(16) Uani 0.792(7) 1 d D U P F 1
H26 H 0.671577 0.423772 0.252739 0.128 Uiso 0.792(7) 1 calc R U P F 1
C27 C 0.7103(5) 0.4459(2) 0.1541(3) 0.1139(18) Uani 0.792(7) 1 d D U P F 1
H27 H 0.781676 0.422691 0.146926 0.137 Uiso 0.792(7) 1 calc R U P F 1
C28 C 0.6725(6) 0.4794(2) 0.1029(3) 0.1103(17) Uani 0.792(7) 1 d D U P F 1
H28 H 0.719056 0.479193 0.060495 0.132 Uiso 0.792(7) 1 calc R U P F 1
C29 C 0.5687(5) 0.51341(16) 0.1111(3) 0.0945(14) Uani 0.792(7) 1 d D U P F 1
H29 H 0.543433 0.536180 0.074845 0.113 Uiso 0.792(7) 1 calc R U P F 1
C30 C 0.5006(4) 0.51372(15) 0.1746(2) 0.0772(12) Uani 0.792(7) 1 d D U P F 1
C31 C 0.3893(5) 0.5501(2) 0.1834(3) 0.1082(19) Uani 0.792(7) 1 d D U P F 1
H31A H 0.318669 0.532565 0.208629 0.162 Uiso 0.792(7) 1 calc R U P F 1
H31B H 0.357069 0.560919 0.138008 0.162 Uiso 0.792(7) 1 calc R U P F 1
H31C H 0.418364 0.580820 0.209201 0.162 Uiso 0.792(7) 1 calc R U P F 1
C2A C 0.1820(5) 0.6390(2) 0.5344(3) 0.0405(9) Uani 0.602(9) 1 d D U P E 2
C3A C 0.1743(6) 0.5938(2) 0.5748(3) 0.0518(11) Uani 0.602(9) 1 d D U P E 2
H3A H 0.100858 0.588202 0.604041 0.062 Uiso 0.602(9) 1 calc R U P E 2
C4A C 0.2733(6) 0.5576(2) 0.5719(3) 0.0622(12) Uani 0.602(9) 1 d D U P E 2
H4A H 0.269327 0.527391 0.600242 0.075 Uiso 0.602(9) 1 calc R U P E 2
C5A C 0.3784(6) 0.56454(18) 0.5281(3) 0.0609(11) Uani 0.602(9) 1 d D U P E 2
H5A H 0.446974 0.539412 0.528499 0.073 Uiso 0.602(9) 1 calc R U P E 2
C6A C 0.3885(5) 0.6074(2) 0.4830(3) 0.0540(10) Uani 0.602(9) 1 d D U P E 2
C7A C 0.4846(5) 0.6172(3) 0.4203(3) 0.0653(13) Uani 0.602(9) 1 d D U P E 2
H7A H 0.458853 0.650303 0.396668 0.078 Uiso 0.602(9) 1 calc R U P E 2
C8A C 0.4714(7) 0.5720(4) 0.3696(4) 0.079(2) Uani 0.602(9) 1 d D U P E 2
H8A1 H 0.530059 0.577839 0.330369 0.118 Uiso 0.602(9) 1 calc R U P E 2
H8A2 H 0.380587 0.569918 0.353331 0.118 Uiso 0.602(9) 1 calc R U P E 2
H8A3 H 0.495193 0.539311 0.392610 0.118 Uiso 0.602(9) 1 calc R U P E 2
C9A C 0.6265(5) 0.6219(3) 0.4450(4) 0.0780(18) Uani 0.602(9) 1 d D U P E 2
H9A1 H 0.651257 0.590117 0.470003 0.117 Uiso 0.602(9) 1 calc R U P E 2
H9A2 H 0.634684 0.652085 0.475683 0.117 Uiso 0.602(9) 1 calc R U P E 2
H9A3 H 0.684591 0.626421 0.405253 0.117 Uiso 0.602(9) 1 calc R U P E 2
C10A C 0.0631(5) 0.6746(2) 0.5411(3) 0.0450(11) Uani 0.602(9) 1 d D U P E 2
H10A H 0.082491 0.707721 0.515932 0.054 Uiso 0.602(9) 1 calc R U P E 2
C11A C 0.0342(5) 0.6883(3) 0.6162(3) 0.0557(14) Uani 0.602(9) 1 d D U P E 2
H11D H 0.006960 0.656762 0.640954 0.084 Uiso 0.602(9) 1 calc R U P E 2
H11E H -0.036268 0.714257 0.618079 0.084 Uiso 0.602(9) 1 calc R U P E 2
H11F H 0.113409 0.702612 0.637662 0.084 Uiso 0.602(9) 1 calc R U P E 2
C12A C -0.0595(6) 0.6503(3) 0.5092(3) 0.0598(14) Uani 0.602(9) 1 d D U P E 2
H12D H -0.042119 0.641572 0.460932 0.090 Uiso 0.602(9) 1 calc R U P E 2
H12E H -0.132257 0.675178 0.511806 0.090 Uiso 0.602(9) 1 calc R U P E 2
H12F H -0.082646 0.618460 0.534490 0.090 Uiso 0.602(9) 1 calc R U P E 2
C25A C 0.4990(17) 0.4836(9) 0.2178(9) 0.092(4) Uani 0.208(7) 1 d D U P F 2
H25A H 0.425245 0.496842 0.242094 0.110 Uiso 0.208(7) 1 calc R U P F 2
C26A C 0.5813(14) 0.4461(6) 0.2483(7) 0.088(4) Uani 0.208(7) 1 d D U P F 2
H26A H 0.558826 0.430752 0.291215 0.106 Uiso 0.208(7) 1 calc R U P F 2
C27A C 0.6959(15) 0.4318(7) 0.2145(9) 0.091(4) Uani 0.208(7) 1 d D U P F 2
H27A H 0.747997 0.404161 0.232142 0.109 Uiso 0.208(7) 1 calc R U P F 2
C28A C 0.7348(15) 0.4577(8) 0.1550(10) 0.097(4) Uani 0.208(7) 1 d D U P F 2
H28A H 0.820144 0.452280 0.136743 0.117 Uiso 0.208(7) 1 calc R U P F 2
C29A C 0.6486(16) 0.4916(8) 0.1226(8) 0.099(4) Uani 0.208(7) 1 d D U P F 2
H29A H 0.672451 0.508135 0.080627 0.119 Uiso 0.208(7) 1 calc R U P F 2
C30A C 0.5268(15) 0.5009(7) 0.1522(8) 0.098(4) Uani 0.208(7) 1 d D U P F 2
C31A C 0.4395(16) 0.5401(6) 0.1179(10) 0.103(5) Uani 0.208(7) 1 d D U P F 2
H31D H 0.348257 0.533821 0.131484 0.154 Uiso 0.208(7) 1 calc R U P F 2
H31E H 0.447627 0.536831 0.067794 0.154 Uiso 0.208(7) 1 calc R U P F 2
H31F H 0.465466 0.575382 0.131968 0.154 Uiso 0.208(7) 1 calc R U P F 2
B1 B 0.4951(3) 0.750000 0.57344(16) 0.0330(7) Uani 1 2 d S T P . .
H1 H 0.477(2) 0.7117(9) 0.5368(11) 0.040 Uiso 1 1 d . U . . .


_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
S1A O2A 1.418(11) . ?
S1A O2 1.422(12) . ?
S1A O1 1.509(2) . ?
S1A C24 1.807(5) . ?
Al1 O1 1.8025(19) . ?
Al1 N1 1.8711(16) 8_575 ?
Al1 N1 1.8712(16) . ?
Al1 B1 2.166(3) . ?
F1 C24 1.315(6) . ?
F2 C24 1.323(6) . ?
F3 C24 1.363(6) . ?
N1 C14 1.347(2) . ?
N1 C1 1.455(2) . ?
C1 C6 1.379(5) . ?
C1 C2 1.388(5) . ?
C1 C2A 1.413(4) . ?
C1 C6A 1.417(4) . ?
C2 C3 1.394(6) . ?
C2 C10 1.523(6) . ?
C3 C4 1.392(6) . ?
C4 C5 1.381(6) . ?
C5 C6 1.378(6) . ?
C6 C7 1.482(7) . ?
C7 C9 1.515(7) . ?
C7 C8 1.536(7) . ?
C10 C11 1.522(6) . ?
C10 C12 1.527(6) . ?
C13 C14 1.506(3) . ?
C14 C15 1.396(2) . ?
C16 C23 1.513(6) . ?
C16 C17 1.532(6) . ?
C16 B1 1.601(4) . ?
C17 C18 1.527(6) . ?
C18 C19 1.535(6) . ?
C19 C20 1.541(6) . ?
C20 C21 1.526(6) . ?
C20 B1 1.608(5) . ?
C21 C22 1.496(6) . ?
C22 C23 1.495(6) . ?
C25 C30 1.360(5) . ?
C25 C26 1.401(6) . ?
C26 C27 1.382(6) . ?
C27 C28 1.368(6) . ?
C28 C29 1.381(5) . ?
C29 C30 1.415(5) . ?
C30 C31 1.477(5) . ?
C2A C3A 1.401(5) . ?
C2A C10A 1.522(5) . ?
C3A C4A 1.372(5) . ?
C4A C5A 1.379(5) . ?
C5A C6A 1.409(5) . ?
C6A C7A 1.582(6) . ?
C7A C8A 1.524(6) . ?
C7A C9A 1.529(5) . ?
C10A C12A 1.527(5) . ?
C10A C11A 1.528(5) . ?
C25A C30A 1.378(7) . ?
C25A C26A 1.406(7) . ?
C26A C27A 1.388(7) . ?
C27A C28A 1.389(7) . ?
C28A C29A 1.386(7) . ?
C29A C30A 1.389(7) . ?
C30A C31A 1.498(6) . ?

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
O2A S1A O2 119.2(2) . . ?
O2A S1A O1 114.5(5) . . ?
O2 S1A O1 109.7(5) . . ?
O2A S1A C24 104.6(7) . . ?
O2 S1A C24 107.2(6) . . ?
O1 S1A C24 99.17(19) . . ?
O1 Al1 N1 107.20(6) . 8_575 ?
O1 Al1 N1 107.20(6) . . ?
N1 Al1 N1 98.57(10) 8_575 . ?
O1 Al1 B1 106.37(11) . . ?
N1 Al1 B1 118.33(7) 8_575 . ?
N1 Al1 B1 118.33(7) . . ?
S1A O1 Al1 147.31(14) . . ?
C14 N1 C1 120.16(15) . . ?
C14 N1 Al1 115.57(12) . . ?
C1 N1 Al1 123.95(12) . . ?
C6 C1 C2 120.7(4) . . ?
C2A C1 C6A 121.3(3) . . ?
C6 C1 N1 114.5(3) . . ?
C2 C1 N1 124.8(3) . . ?
C2A C1 N1 115.1(2) . . ?
C6A C1 N1 123.3(2) . . ?
C1 C2 C3 117.6(4) . . ?
C1 C2 C10 116.7(5) . . ?
C3 C2 C10 125.1(5) . . ?
C4 C3 C2 121.3(5) . . ?
C5 C4 C3 120.2(4) . . ?
C6 C5 C4 118.4(4) . . ?
C5 C6 C1 121.6(4) . . ?
C5 C6 C7 100.1(6) . . ?
C1 C6 C7 137.2(7) . . ?
C6 C7 C9 113.6(6) . . ?
C6 C7 C8 111.9(6) . . ?
C9 C7 C8 110.6(6) . . ?
C11 C10 C2 110.0(5) . . ?
C11 C10 C12 110.3(5) . . ?
C2 C10 C12 110.6(6) . . ?
N1 C14 C15 122.30(18) . . ?
N1 C14 C13 120.31(17) . . ?
C15 C14 C13 117.38(18) . . ?
C14 C15 C14 128.3(2) . 8_575 ?
C23 C16 C17 112.4(3) . . ?
C23 C16 B1 111.3(5) . . ?
C17 C16 B1 106.2(4) . . ?
C18 C17 C16 112.4(4) . . ?
C17 C18 C19 111.9(4) . . ?
C18 C19 C20 111.7(5) . . ?
C21 C20 C19 111.9(3) . . ?
C21 C20 B1 110.3(4) . . ?
C19 C20 B1 105.5(5) . . ?
C22 C21 C20 116.3(6) . . ?
C21 C22 C23 117.2(5) . . ?
C22 C23 C16 115.6(5) . . ?
F1 C24 F2 108.9(6) . . ?
F1 C24 F3 104.4(6) . . ?
F2 C24 F3 104.2(5) . . ?
F1 C24 S1A 113.1(6) . . ?
F2 C24 S1A 116.6(5) . . ?
F3 C24 S1A 108.6(6) . . ?
C30 C25 C26 121.6(4) . . ?
C27 C26 C25 118.9(4) . . ?
C28 C27 C26 119.8(5) . . ?
C27 C28 C29 121.8(5) . . ?
C28 C29 C30 118.7(4) . . ?
C25 C30 C29 119.0(4) . . ?
C25 C30 C31 122.2(5) . . ?
C29 C30 C31 118.7(4) . . ?
C3A C2A C1 119.6(3) . . ?
C3A C2A C10A 113.7(4) . . ?
C1 C2A C10A 126.4(3) . . ?
C4A C3A C2A 119.6(4) . . ?
C3A C4A C5A 120.6(4) . . ?
C4A C5A C6A 122.7(4) . . ?
C5A C6A C1 116.0(3) . . ?
C5A C6A C7A 130.3(5) . . ?
C1 C6A C7A 113.2(4) . . ?
C8A C7A C9A 110.2(4) . . ?
C8A C7A C6A 108.8(5) . . ?
C9A C7A C6A 110.9(5) . . ?
C2A C10A C12A 111.9(4) . . ?
C2A C10A C11A 111.9(4) . . ?
C12A C10A C11A 108.8(4) . . ?
C30A C25A C26A 119.1(6) . . ?
C27A C26A C25A 118.9(6) . . ?
C28A C27A C26A 120.5(6) . . ?
C29A C28A C27A 119.7(6) . . ?
C28A C29A C30A 119.1(6) . . ?
C25A C30A C29A 120.7(6) . . ?
C25A C30A C31A 120.3(7) . . ?
C29A C30A C31A 117.5(7) . . ?
C16 B1 C20 108.0(2) . . ?
C16 B1 Al1 115.0(2) . . ?
C20 B1 Al1 137.1(2) . . ?

_refine_diff_density_max         0.379
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.048

####################################################################### 
# 
# 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_031acjh17_a
_database_code_depnum_ccdc_archive 'CCDC 1895244'
loop_
_audit_author_name
_audit_author_address
'Simon Aldridge'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-02-01 deposited with the CCDC.	2019-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H68 Al B N4, 0.5(C7 H8)'
_chemical_formula_sum            'C44.50 H72 Al B N4'
_chemical_formula_weight         700.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
B B 0.0090 0.0039 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

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

_cell_length_a                   19.0779(5)
_cell_length_b                   11.5597(3)
_cell_length_c                   39.5676(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.891(3)
_cell_angle_gamma                90
_cell_volume                     8568.9(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6894
_cell_measurement_theta_min      3.7450
_cell_measurement_theta_max      76.0430

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_F_000             3080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.654
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.99494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_reflns_number            25090
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         3.990
_diffrn_reflns_theta_max         76.297
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8889
_reflns_number_gt                6997
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1089P)²+9.3581P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8889
_refine_ls_number_parameters     662
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.2100
_refine_ls_wR_factor_gt          0.1917
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.054
_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_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 0.50962(4) 0.31826(6) 0.62106(2) 0.0448(2) Uani 1 1 d . . . . .
N1 N 0.51525(13) 0.1921(2) 0.58995(4) 0.0573(6) Uani 1 1 d . . . . .
N2 N 0.59287(9) 0.28415(14) 0.65518(4) 0.0359(4) Uani 1 1 d . . . . .
N3 N 0.5822(5) 0.0816(8) 0.55899(17) 0.0526(15) Uani 0.543(18) 1 d . . P A 1
N4 N 0.71629(11) 0.24345(19) 0.66345(6) 0.0565(6) Uani 1 1 d . . . . .
N3A N 0.6057(5) 0.1115(8) 0.55944(18) 0.0439(16) Uani 0.457(18) 1 d . . P A 2
C1 C 0.4633(3) 0.1457(6) 0.56973(12) 0.0299(11) Uani 0.505(5) 1 d . . P B 1
C2 C 0.4165(3) 0.2104(6) 0.54422(11) 0.0394(11) Uani 0.505(5) 1 d . . P B 1
C3 C 0.3556(3) 0.1540(7) 0.52704(12) 0.0469(13) Uani 0.505(5) 1 d . . P B 1
H3 H 0.3234 0.1954 0.5101 0.056 Uiso 0.505(5) 1 calc R U P B 1
C4 C 0.3399(6) 0.0411(8) 0.5335(3) 0.041(2) Uani 0.505(5) 1 d . . P B 1
H4 H 0.2968 0.0063 0.5220 0.050 Uiso 0.505(5) 1 calc R U P B 1
C5 C 0.3882(3) -0.0205(6) 0.55713(13) 0.0411(11) Uani 0.505(5) 1 d . . P B 1
H5 H 0.3795 -0.1003 0.5604 0.049 Uiso 0.505(5) 1 calc R U P B 1
C6 C 0.4490(3) 0.0302(6) 0.57624(17) 0.0310(13) Uani 0.505(5) 1 d D . P B 1
C7 C 0.4895(9) -0.0491(15) 0.6045(4) 0.054(2) Uani 0.505(5) 1 d D . P B 1
H7 H 0.5253 0.0037 0.6184 0.064 Uiso 0.505(5) 1 calc R U P B 1
C8 C 0.5396(6) -0.1344(9) 0.5838(3) 0.069(3) Uani 0.505(5) 1 d . . P B 1
H8A H 0.5093 -0.1943 0.5709 0.103 Uiso 0.505(5) 1 calc R U P B 1
H8B H 0.5773 -0.1710 0.6006 0.103 Uiso 0.505(5) 1 calc R U P B 1
H8C H 0.5611 -0.0875 0.5678 0.103 Uiso 0.505(5) 1 calc R U P B 1
C9 C 0.4608(11) -0.1225(14) 0.6327(6) 0.105(7) Uani 0.505(5) 1 d . . P B 1
H9A H 0.4310 -0.1860 0.6215 0.157 Uiso 0.505(5) 1 calc R U P B 1
H9B H 0.4323 -0.0728 0.6449 0.157 Uiso 0.505(5) 1 calc R U P B 1
H9C H 0.5012 -0.1543 0.6490 0.157 Uiso 0.505(5) 1 calc R U P B 1
C10 C 0.4300(3) 0.3320(5) 0.53361(11) 0.0522(13) Uani 0.505(5) 1 d . . P B 1
H10 H 0.4777 0.3568 0.5467 0.063 Uiso 0.505(5) 1 calc R U P B 1
C11 C 0.3736(3) 0.4173(5) 0.54197(14) 0.0636(16) Uani 0.505(5) 1 d . . P B 1
H11A H 0.3269 0.3981 0.5281 0.095 Uiso 0.505(5) 1 calc R U P B 1
H11B H 0.3868 0.4963 0.5367 0.095 Uiso 0.505(5) 1 calc R U P B 1
H11C H 0.3714 0.4117 0.5665 0.095 Uiso 0.505(5) 1 calc R U P B 1
C12 C 0.4310(4) 0.3423(7) 0.49493(13) 0.075(2) Uani 0.505(5) 1 d . . P B 1
H12D H 0.4646 0.2858 0.4886 0.113 Uiso 0.505(5) 1 calc R U P B 1
H12E H 0.4460 0.4205 0.4899 0.113 Uiso 0.505(5) 1 calc R U P B 1
H12F H 0.3831 0.3272 0.4817 0.113 Uiso 0.505(5) 1 calc R U P B 1
C13 C 0.58260(17) 0.1617(2) 0.58691(6) 0.0570(7) Uani 1 1 d . . . . .
C14 C 0.64338(15) 0.1961(2) 0.61000(6) 0.0493(6) Uani 1 1 d . . . . .
H14 H 0.6870 0.1874 0.6020 0.059 Uiso 1 1 calc R U . . .
C15 C 0.64990(12) 0.24196(17) 0.64343(6) 0.0420(5) Uani 1 1 d . . . . .
C16 C 0.5394(6) 0.0970(9) 0.52468(14) 0.086(3) Uani 0.543(18) 1 d . . P A 1
H16A H 0.5185 0.1747 0.5227 0.129 Uiso 0.543(18) 1 calc R U P A 1
H16B H 0.5012 0.0391 0.5208 0.129 Uiso 0.543(18) 1 calc R U P A 1
H16C H 0.5698 0.0875 0.5075 0.129 Uiso 0.543(18) 1 calc R U P A 1
C17 C 0.6593(10) 0.0223(14) 0.5634(4) 0.083(4) Uani 0.543(18) 1 d . U P A 1
H17D H 0.6930 0.0767 0.5562 0.124 Uiso 0.543(18) 1 calc R U P A 1
H17E H 0.6560 -0.0475 0.5491 0.124 Uiso 0.543(18) 1 calc R U P A 1
H17F H 0.6759 0.0013 0.5876 0.124 Uiso 0.543(18) 1 calc R U P A 1
C18 C 0.77408(16) 0.1730(3) 0.65515(11) 0.0812(11) Uani 1 1 d . . . . .
H18A H 0.7554 0.0973 0.6467 0.122 Uiso 1 1 calc R U . . .
H18B H 0.8109 0.1627 0.6758 0.122 Uiso 1 1 calc R U . . .
H18C H 0.7949 0.2118 0.6373 0.122 Uiso 1 1 calc R U . . .
C19 C 0.74064(15) 0.3372(3) 0.68729(11) 0.0826(12) Uani 1 1 d . . . . .
H19A H 0.7073 0.4022 0.6826 0.124 Uiso 1 1 calc R U . . .
H19B H 0.7882 0.3623 0.6843 0.124 Uiso 1 1 calc R U . . .
H19C H 0.7429 0.3102 0.7109 0.124 Uiso 1 1 calc R U . . .
C20 C 0.59393(10) 0.29064(18) 0.69181(5) 0.0350(4) Uani 1 1 d . . . . .
C21 C 0.60063(10) 0.1893(2) 0.71181(5) 0.0382(4) Uani 1 1 d . . . . .
C22 C 0.59286(13) 0.1966(3) 0.74619(6) 0.0527(6) Uani 1 1 d . . . . .
H22 H 0.5973 0.1284 0.7599 0.063 Uiso 1 1 calc R U . . .
C23 C 0.57885(14) 0.3005(3) 0.76068(6) 0.0606(7) Uani 1 1 d . . . . .
H23 H 0.5714 0.3033 0.7837 0.073 Uiso 1 1 calc R U . . .
C24 C 0.57579(12) 0.3994(3) 0.74153(7) 0.0567(7) Uani 1 1 d . . . . .
H24 H 0.5677 0.4710 0.7519 0.068 Uiso 1 1 calc R U . . .
C25 C 0.58423(11) 0.39864(19) 0.70706(6) 0.0450(5) Uani 1 1 d D . . . .
C26 C 0.5801(5) 0.5108(6) 0.6861(2) 0.064(3) Uani 0.65 1 d D . P C 1
H26 H 0.5880 0.4989 0.6621 0.077 Uiso 0.65 1 calc R U P C 1
C27 C 0.6505(3) 0.5855(5) 0.71260(15) 0.0516(12) Uani 0.65 1 d . . P C 1
H27A H 0.6378 0.6002 0.7351 0.077 Uiso 0.65 1 calc R U P C 1
H27B H 0.6588 0.6593 0.7018 0.077 Uiso 0.65 1 calc R U P C 1
H27C H 0.6940 0.5385 0.7156 0.077 Uiso 0.65 1 calc R U P C 1
C28 C 0.5192(7) 0.5766(11) 0.6877(3) 0.051(2) Uani 0.65 1 d . . P C 1
H28A H 0.4766 0.5347 0.6763 0.077 Uiso 0.65 1 calc R U P C 1
H28B H 0.5222 0.6509 0.6762 0.077 Uiso 0.65 1 calc R U P C 1
H28C H 0.5163 0.5901 0.7119 0.077 Uiso 0.65 1 calc R U P C 1
C29 C 0.61631(12) 0.0703(2) 0.69865(5) 0.0421(5) Uani 1 1 d . . . . .
H29 H 0.6145 0.0759 0.6733 0.051 Uiso 1 1 calc R U . . .
C30 C 0.56174(15) -0.0201(2) 0.70492(7) 0.0568(6) Uani 1 1 d . . . . .
H30A H 0.5629 -0.0273 0.7297 0.085 Uiso 1 1 calc R U . . .
H30B H 0.5734 -0.0949 0.6957 0.085 Uiso 1 1 calc R U . . .
H30C H 0.5139 0.0040 0.6934 0.085 Uiso 1 1 calc R U . . .
C31 C 0.69123(15) 0.0295(3) 0.71567(7) 0.0641(7) Uani 1 1 d . . . . .
H31A H 0.7264 0.0883 0.7124 0.096 Uiso 1 1 calc R U . . .
H31B H 0.7022 -0.0433 0.7051 0.096 Uiso 1 1 calc R U . . .
H31C H 0.6930 0.0177 0.7403 0.096 Uiso 1 1 calc R U . . .
C32 C 0.5282(3) 0.4788(4) 0.60334(13) 0.0508(11) Uani 0.65 1 d . . P D 1
H32A H 0.4877 0.4991 0.5847 0.061 Uiso 0.65 1 calc R U P D 1
H32B H 0.5282 0.5348 0.6223 0.061 Uiso 0.65 1 calc R U P D 1
C33 C 0.5974(3) 0.4959(5) 0.58957(14) 0.0653(13) Uani 0.65 1 d . . P D 1
H33A H 0.6385 0.4814 0.6080 0.098 Uiso 0.65 1 calc R U P D 1
H33B H 0.5995 0.5755 0.5812 0.098 Uiso 0.65 1 calc R U P D 1
H33C H 0.5984 0.4418 0.5706 0.098 Uiso 0.65 1 calc R U P D 1
C34 C 0.35003(12) 0.3914(2) 0.65060(6) 0.0468(5) Uani 1 1 d . . . . .
H34 H 0.3637 0.4704 0.6438 0.056 Uiso 1 1 calc R U . . .
C35 C 0.35359(13) 0.3890(2) 0.68976(6) 0.0470(5) Uani 1 1 d . . . . .
H35A H 0.4006 0.4197 0.7011 0.056 Uiso 1 1 calc R U . . .
H35B H 0.3166 0.4420 0.6953 0.056 Uiso 1 1 calc R U . . .
C36 C 0.34326(15) 0.2710(2) 0.70494(7) 0.0580(6) Uani 1 1 d . . . . .
H36A H 0.2921 0.2502 0.6992 0.070 Uiso 1 1 calc R U . . .
H36B H 0.3569 0.2757 0.7303 0.070 Uiso 1 1 calc R U . . .
C37 C 0.38707(17) 0.1753(2) 0.69197(8) 0.0635(7) Uani 1 1 d . . . . .
H37A H 0.4371 0.1817 0.7044 0.076 Uiso 1 1 calc R U . . .
H37B H 0.3686 0.0996 0.6981 0.076 Uiso 1 1 calc R U . . .
C38 C 0.38718(15) 0.1756(2) 0.65337(8) 0.0576(6) Uani 1 1 d . . . . .
H38 H 0.4236 0.1189 0.6484 0.069 Uiso 1 1 calc R U . . .
C39 C 0.3140(2) 0.1469(3) 0.63029(11) 0.0898(11) Uani 1 1 d . . . . .
H39A H 0.3209 0.1382 0.6063 0.108 Uiso 1 1 calc R U . . .
H39B H 0.2974 0.0715 0.6376 0.108 Uiso 1 1 calc R U . . .
C40 C 0.2562(2) 0.2358(5) 0.63101(15) 0.1226(19) Uani 1 1 d . . . . .
H40A H 0.2171 0.2206 0.6112 0.147 Uiso 1 1 calc R U . . .
H40B H 0.2368 0.2234 0.6522 0.147 Uiso 1 1 calc R U . . .
C41 C 0.27698(16) 0.3615(3) 0.62980(9) 0.0787(10) Uani 1 1 d . . . . .
H41A H 0.2407 0.4089 0.6383 0.094 Uiso 1 1 calc R U . . .
H41B H 0.2758 0.3833 0.6055 0.094 Uiso 1 1 calc R U . . .
C42 C 0.2290(3) 0.6541(6) 0.51275(14) 0.0608(15) Uiso 0.5 1 d D . P E -1
H42 H 0.1794 0.6448 0.5040 0.073 Uiso 0.5 1 calc R U P E -1
C43 C 0.2537(4) 0.6506(9) 0.54768(17) 0.096(3) Uiso 0.5 1 d D . P E -1
H43 H 0.2211 0.6471 0.5631 0.115 Uiso 0.5 1 calc R U P E -1
C44 C 0.3267(4) 0.6521(11) 0.56025(19) 0.147(4) Uiso 0.5 1 d D . P E -1
H44 H 0.3447 0.6491 0.5843 0.176 Uiso 0.5 1 calc R U P E -1
C45 C 0.3734(4) 0.6581(9) 0.5369(2) 0.107(3) Uiso 0.5 1 d D . P E -1
H45 H 0.4234 0.6599 0.5454 0.129 Uiso 0.5 1 calc R U P E -1
C46 C 0.3482(4) 0.6612(10) 0.5021(2) 0.123(3) Uiso 0.5 1 d D . P E -1
H46 H 0.3802 0.6570 0.4864 0.148 Uiso 0.5 1 calc R U P E -1
C47 C 0.2749(5) 0.6709(18) 0.4901(2) 0.234(12) Uiso 0.5 1 d D . P E -1
C48 C 0.2472(8) 0.653(3) 0.4528(2) 0.319(19) Uiso 0.5 1 d D . P E -1
H48A H 0.2854 0.6680 0.4399 0.478 Uiso 0.5 1 calc R U P E -1
H48B H 0.2304 0.5733 0.4488 0.478 Uiso 0.5 1 calc R U P E -1
H48C H 0.2075 0.7066 0.4451 0.478 Uiso 0.5 1 calc R U P E -1
C1A C 0.4457(3) 0.1040(7) 0.57394(13) 0.0297(12) Uani 0.495(5) 1 d . . P B 2
C2A C 0.3907(3) 0.1544(5) 0.54781(11) 0.0363(11) Uani 0.495(5) 1 d . . P B 2
C3A C 0.3362(6) 0.0854(7) 0.5324(3) 0.0361(19) Uani 0.495(5) 1 d . . P B 2
H3A H 0.3000 0.1177 0.5152 0.043 Uiso 0.495(5) 1 calc R U P B 2
C4A C 0.3314(2) -0.0294(6) 0.54076(12) 0.0402(12) Uani 0.495(5) 1 d . . P B 2
H4A H 0.2928 -0.0755 0.5294 0.048 Uiso 0.495(5) 1 calc R U P B 2
C5A C 0.3841(2) -0.0770(5) 0.56616(14) 0.0382(10) Uani 0.495(5) 1 d . . P B 2
H5A H 0.3810 -0.1561 0.5722 0.046 Uiso 0.495(5) 1 calc R U P B 2
C6A C 0.4413(3) -0.0107(6) 0.58282(17) 0.0309(13) Uani 0.495(5) 1 d D . P B 2
C7A C 0.5010(11) -0.067(2) 0.6090(6) 0.068(4) Uani 0.495(5) 1 d D . P B 2
H7A H 0.5336 -0.0089 0.6227 0.081 Uiso 0.495(5) 1 calc R U P B 2
C8A C 0.5381(7) -0.1595(11) 0.5970(3) 0.067(3) Uani 0.495(5) 1 d . . P B 2
H8A1 H 0.5736 -0.1903 0.6161 0.101 Uiso 0.495(5) 1 calc R U P B 2
H8A2 H 0.5622 -0.1316 0.5788 0.101 Uiso 0.495(5) 1 calc R U P B 2
H8A3 H 0.5042 -0.2206 0.5879 0.101 Uiso 0.495(5) 1 calc R U P B 2
C9A C 0.4497(8) -0.1236(14) 0.6300(5) 0.071(4) Uani 0.495(5) 1 d . . P B 2
H9A1 H 0.4195 -0.0640 0.6375 0.106 Uiso 0.495(5) 1 calc R U P B 2
H9A2 H 0.4774 -0.1625 0.6502 0.106 Uiso 0.495(5) 1 calc R U P B 2
H9A3 H 0.4196 -0.1803 0.6156 0.106 Uiso 0.495(5) 1 calc R U P B 2
C10A C 0.3901(3) 0.2778(5) 0.53429(12) 0.0497(14) Uani 0.495(5) 1 d . . P B 2
H10A H 0.4348 0.3176 0.5458 0.060 Uiso 0.495(5) 1 calc R U P B 2
C11A C 0.3864(5) 0.2806(7) 0.49471(15) 0.085(2) Uani 0.495(5) 1 d . . P B 2
H11D H 0.4273 0.2386 0.4891 0.128 Uiso 0.495(5) 1 calc R U P B 2
H11E H 0.3876 0.3610 0.4870 0.128 Uiso 0.495(5) 1 calc R U P B 2
H11F H 0.3421 0.2438 0.4831 0.128 Uiso 0.495(5) 1 calc R U P B 2
C12A C 0.3256(4) 0.3457(5) 0.54177(14) 0.0651(18) Uani 0.495(5) 1 d . . P B 2
H12A H 0.2815 0.3094 0.5297 0.098 Uiso 0.495(5) 1 calc R U P B 2
H12B H 0.3279 0.4256 0.5338 0.098 Uiso 0.495(5) 1 calc R U P B 2
H12C H 0.3263 0.3455 0.5666 0.098 Uiso 0.495(5) 1 calc R U P B 2
C16A C 0.5708(5) 0.1507(11) 0.52469(14) 0.067(3) Uani 0.457(18) 1 d . . P A 2
H16D H 0.6054 0.1489 0.5093 0.100 Uiso 0.457(18) 1 calc R U P A 2
H16E H 0.5531 0.2298 0.5261 0.100 Uiso 0.457(18) 1 calc R U P A 2
H16F H 0.5307 0.0992 0.5157 0.100 Uiso 0.457(18) 1 calc R U P A 2
C17A C 0.6651(12) 0.0531(14) 0.5577(4) 0.069(3) Uani 0.457(18) 1 d . U P A 2
H17A H 0.7000 0.1055 0.5505 0.104 Uiso 0.457(18) 1 calc R U P A 2
H17B H 0.6540 -0.0097 0.5408 0.104 Uiso 0.457(18) 1 calc R U P A 2
H17C H 0.6851 0.0205 0.5803 0.104 Uiso 0.457(18) 1 calc R U P A 2
C26A C 0.5944(7) 0.5182(7) 0.6929(3) 0.027(2) Uani 0.35 1 d D U P C 2
H26A H 0.6040 0.4944 0.6699 0.033 Uiso 0.35 1 calc R U P C 2
C27A C 0.6343(7) 0.6066(11) 0.6974(3) 0.061(3) Uani 0.35 1 d . . P C 2
H27D H 0.6226 0.6578 0.6774 0.092 Uiso 0.35 1 calc R U P C 2
H27E H 0.6843 0.5825 0.7003 0.092 Uiso 0.35 1 calc R U P C 2
H27F H 0.6268 0.6480 0.7181 0.092 Uiso 0.35 1 calc R U P C 2
C28A C 0.5040(13) 0.582(2) 0.6782(6) 0.064(6) Uani 0.35 1 d . . P C 2
H28D H 0.4863 0.6130 0.6981 0.096 Uiso 0.35 1 calc R U P C 2
H28E H 0.4713 0.5219 0.6671 0.096 Uiso 0.35 1 calc R U P C 2
H28F H 0.5068 0.6444 0.6618 0.096 Uiso 0.35 1 calc R U P C 2
C32A C 0.4975(4) 0.4588(7) 0.5952(2) 0.0394(17) Uani 0.35 1 d . . P D 2
H32C H 0.4521 0.4550 0.5783 0.047 Uiso 0.35 1 calc R U P D 2
H32D H 0.4941 0.5241 0.6110 0.047 Uiso 0.35 1 calc R U P D 2
C33A C 0.5580(7) 0.4812(10) 0.5763(4) 0.083(3) Uani 0.35 1 d . . P D 2
H33D H 0.6013 0.5008 0.5930 0.125 Uiso 0.35 1 calc R U P D 2
H33E H 0.5454 0.5458 0.5603 0.125 Uiso 0.35 1 calc R U P D 2
H33F H 0.5667 0.4118 0.5635 0.125 Uiso 0.35 1 calc R U P D 2
B1 B 0.40734(14) 0.2997(2) 0.64192(6) 0.0413(5) Uani 1 1 d . . . . .
H1A H 0.4163(14) 0.302(2) 0.6136(7) 0.050 Uiso 1 1 d . U . . .
H1B H 0.4680(14) 0.330(2) 0.6564(7) 0.050 Uiso 1 1 d . U . . .


_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 C32A 1.911(8) . ?
Al1 N2 1.921(2) . ?
Al1 N1 1.924(2) . ?
Al1 C32 2.039(5) . ?
Al1 B1 2.268(3) . ?
N1 C1 1.269(6) . ?
N1 C13 1.359(4) . ?
N1 C1A 1.697(8) . ?
N2 C15 1.352(3) . ?
N2 C20 1.448(2) . ?
N3 C13 1.440(7) . ?
N3 C16 1.456(10) . ?
N3 C17 1.60(2) . ?
N4 C15 1.361(3) . ?
N4 C19 1.454(3) . ?
N4 C18 1.457(3) . ?
N3A C17A 1.33(2) . ?
N3A C13 1.376(7) . ?
N3A C16A 1.481(10) . ?
C1 C6 1.396(7) . ?
C1 C2 1.427(8) . ?
C2 C3 1.393(7) . ?
C2 C10 1.503(8) . ?
C3 C4 1.374(9) . ?
C4 C5 1.380(11) . ?
C5 C6 1.390(8) . ?
C6 C7 1.536(7) . ?
C7 C9 1.58(3) . ?
C7 C8 1.69(2) . ?
C10 C12 1.539(7) . ?
C10 C11 1.540(8) . ?
C13 C14 1.392(4) . ?
C14 C15 1.408(3) . ?
C20 C21 1.406(3) . ?
C20 C25 1.414(3) . ?
C21 C22 1.398(3) . ?
C21 C29 1.521(3) . ?
C22 C23 1.378(4) . ?
C23 C24 1.367(4) . ?
C24 C25 1.403(3) . ?
C25 C26A 1.519(6) . ?
C25 C26 1.534(6) . ?
C26 C28 1.399(17) . ?
C26 C27 1.767(10) . ?
C29 C30 1.528(3) . ?
C29 C31 1.534(3) . ?
C32 C33 1.532(7) . ?
C34 C41 1.518(4) . ?
C34 C35 1.538(3) . ?
C34 B1 1.605(3) . ?
C35 C36 1.518(3) . ?
C36 C37 1.533(4) . ?
C37 C38 1.528(4) . ?
C38 C39 1.553(5) . ?
C38 B1 1.574(4) . ?
C39 C40 1.511(6) . ?
C40 C41 1.509(6) . ?
C42 C43 1.374(6) . ?
C42 C47 1.380(6) . ?
C43 C44 1.388(6) . ?
C44 C45 1.400(6) . ?
C45 C46 1.372(6) . ?
C46 C47 1.393(7) . ?
C47 C48 1.485(7) . ?
C1A C6A 1.379(8) . ?
C1A C2A 1.450(7) . ?
C2A C3A 1.360(12) . ?
C2A C10A 1.523(7) . ?
C3A C4A 1.375(8) . ?
C4A C5A 1.394(7) . ?
C5A C6A 1.393(8) . ?
C6A C7A 1.532(7) . ?
C7A C8A 1.41(3) . ?
C7A C9A 1.54(3) . ?
C10A C12A 1.535(9) . ?
C10A C11A 1.554(8) . ?
C26A C27A 1.267(17) . ?
C26A C28A 1.86(3) . ?
C32A C33A 1.512(13) . ?

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
C32A Al1 N2 123.5(2) . . ?
C32A Al1 N1 108.5(3) . . ?
N2 Al1 N1 98.93(8) . . ?
N2 Al1 C32 104.71(17) . . ?
N1 Al1 C32 115.81(16) . . ?
C32A Al1 B1 104.4(3) . . ?
N2 Al1 B1 112.27(8) . . ?
N1 Al1 B1 108.49(11) . . ?
C32 Al1 B1 115.40(16) . . ?
C1 N1 C13 118.3(3) . . ?
C13 N1 C1A 119.8(3) . . ?
C1 N1 Al1 126.3(3) . . ?
C13 N1 Al1 114.9(2) . . ?
C1A N1 Al1 124.0(2) . . ?
C15 N2 C20 120.20(19) . . ?
C15 N2 Al1 116.40(15) . . ?
C20 N2 Al1 123.10(13) . . ?
C13 N3 C16 123.9(6) . . ?
C13 N3 C17 108.6(8) . . ?
C16 N3 C17 119.6(8) . . ?
C15 N4 C19 122.4(2) . . ?
C15 N4 C18 121.5(2) . . ?
C19 N4 C18 113.6(2) . . ?
C17A N3A C13 131.1(9) . . ?
C17A N3A C16A 110.1(8) . . ?
C13 N3A C16A 116.7(6) . . ?
N1 C1 C6 116.3(5) . . ?
N1 C1 C2 122.3(6) . . ?
C6 C1 C2 120.9(5) . . ?
C3 C2 C1 116.9(6) . . ?
C3 C2 C10 118.3(5) . . ?
C1 C2 C10 124.8(5) . . ?
C4 C3 C2 123.1(7) . . ?
C3 C4 C5 118.4(8) . . ?
C4 C5 C6 122.2(7) . . ?
C5 C6 C1 118.4(6) . . ?
C5 C6 C7 113.4(9) . . ?
C1 C6 C7 128.1(9) . . ?
C6 C7 C9 129.8(14) . . ?
C6 C7 C8 104.4(11) . . ?
C9 C7 C8 109.4(11) . . ?
C2 C10 C12 112.7(5) . . ?
C2 C10 C11 112.0(5) . . ?
C12 C10 C11 107.7(5) . . ?
N1 C13 N3A 128.9(5) . . ?
N1 C13 C14 123.5(2) . . ?
N3A C13 C14 106.7(5) . . ?
N1 C13 N3 111.4(4) . . ?
C14 C13 N3 124.8(4) . . ?
C13 C14 C15 129.7(2) . . ?
N2 C15 N4 121.06(19) . . ?
N2 C15 C14 121.6(2) . . ?
N4 C15 C14 117.3(2) . . ?
C21 C20 C25 120.05(19) . . ?
C21 C20 N2 120.19(17) . . ?
C25 C20 N2 119.66(19) . . ?
C22 C21 C20 118.8(2) . . ?
C22 C21 C29 116.8(2) . . ?
C20 C21 C29 124.33(17) . . ?
C23 C22 C21 121.4(3) . . ?
C24 C23 C22 119.3(2) . . ?
C23 C24 C25 122.2(2) . . ?
C24 C25 C20 117.9(2) . . ?
C24 C25 C26A 113.6(5) . . ?
C20 C25 C26A 127.6(5) . . ?
C24 C25 C26 121.2(4) . . ?
C20 C25 C26 120.9(4) . . ?
C28 C26 C25 113.1(8) . . ?
C28 C26 C27 104.6(7) . . ?
C25 C26 C27 97.8(5) . . ?
C21 C29 C30 112.24(19) . . ?
C21 C29 C31 110.8(2) . . ?
C30 C29 C31 109.0(2) . . ?
C33 C32 Al1 117.2(4) . . ?
C41 C34 C35 113.8(2) . . ?
C41 C34 B1 109.1(2) . . ?
C35 C34 B1 107.55(17) . . ?
C36 C35 C34 115.5(2) . . ?
C35 C36 C37 113.4(2) . . ?
C38 C37 C36 115.9(2) . . ?
C37 C38 C39 114.6(3) . . ?
C37 C38 B1 109.7(2) . . ?
C39 C38 B1 105.5(2) . . ?
C40 C39 C38 114.9(3) . . ?
C41 C40 C39 117.3(4) . . ?
C40 C41 C34 114.9(3) . . ?
C43 C42 C47 121.2(5) . . ?
C42 C43 C44 119.4(5) . . ?
C43 C44 C45 119.0(5) . . ?
C46 C45 C44 121.2(5) . . ?
C45 C46 C47 118.7(5) . . ?
C42 C47 C46 119.2(6) . . ?
C42 C47 C48 118.3(8) . . ?
C46 C47 C48 118.2(7) . . ?
C6A C1A C2A 119.8(6) . . ?
C6A C1A N1 124.3(5) . . ?
C2A C1A N1 115.8(6) . . ?
C3A C2A C1A 118.2(6) . . ?
C3A C2A C10A 116.0(6) . . ?
C1A C2A C10A 125.7(6) . . ?
C2A C3A C4A 122.6(8) . . ?
C3A C4A C5A 118.8(6) . . ?
C6A C5A C4A 121.2(6) . . ?
C1A C6A C5A 119.3(6) . . ?
C1A C6A C7A 120.4(12) . . ?
C5A C6A C7A 120.2(12) . . ?
C8A C7A C6A 116.6(17) . . ?
C8A C7A C9A 105.5(17) . . ?
C6A C7A C9A 94.5(14) . . ?
C2A C10A C12A 111.4(5) . . ?
C2A C10A C11A 111.7(5) . . ?
C12A C10A C11A 107.4(5) . . ?
C27A C26A C25 142.9(10) . . ?
C27A C26A C28A 102.8(12) . . ?
C25 C26A C28A 107.4(11) . . ?
C33A C32A Al1 112.6(7) . . ?
C38 B1 C34 109.1(2) . . ?
C38 B1 Al1 117.68(16) . . ?
C34 B1 Al1 133.09(18) . . ?

_refine_diff_density_max         0.627
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_p21m_jh_a
_database_code_depnum_ccdc_archive 'CCDC 1895243'
loop_
_audit_author_name
_audit_author_address
'Simon Aldridge'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-02-01 deposited with the CCDC.	2019-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H60 Al B N2'
_chemical_formula_sum            'C38 H60 Al B N2'
_chemical_formula_weight         582.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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.
;

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

_cell_length_a                   9.1574(18)
_cell_length_b                   20.084(4)
_cell_length_c                   10.311(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.98(3)
_cell_angle_gamma                90
_cell_volume                     1782.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6328
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_F_000             640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    0.084
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13582
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         5.151
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             4180
_reflns_number_gt                3181
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0597P)²+0.6163P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4180
_refine_ls_number_parameters     207
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1339
_refine_ls_wR_factor_gt          0.1218
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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_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 0.74735(7) 0.250000 0.72123(6) 0.02360(17) Uani 1 2 d S T P . .
N1 N 0.81225(13) 0.32042(6) 0.85331(12) 0.0245(3) Uani 1 1 d . . . . .
C1 C 0.73679(16) 0.38503(7) 0.82837(15) 0.0264(3) Uani 1 1 d . . . . .
C2 C 0.61643(18) 0.39718(8) 0.88211(16) 0.0322(3) Uani 1 1 d . . . . .
C3 C 0.5381(2) 0.45783(8) 0.85071(19) 0.0406(4) Uani 1 1 d . . . . .
H3 H 0.457149 0.467096 0.886123 0.049 Uiso 1 1 calc R U . . .
C4 C 0.5757(2) 0.50477(9) 0.7692(2) 0.0451(4) Uani 1 1 d . . . . .
H4 H 0.519807 0.545511 0.747889 0.054 Uiso 1 1 calc R U . . .
C5 C 0.6935(2) 0.49238(8) 0.71920(19) 0.0418(4) Uani 1 1 d . . . . .
H5 H 0.719673 0.525310 0.664716 0.050 Uiso 1 1 calc R U . . .
C6 C 0.77653(18) 0.43243(8) 0.74626(16) 0.0309(3) Uani 1 1 d . . . . .
C7 C 0.90291(19) 0.42177(8) 0.68413(18) 0.0371(4) Uani 1 1 d . . . . .
H7 H 0.947895 0.376393 0.711331 0.044 Uiso 1 1 calc R U . . .
C8 C 0.8349(3) 0.42462(11) 0.5259(2) 0.0532(5) Uani 1 1 d . . . . .
H8A H 0.750152 0.392253 0.492522 0.080 Uiso 1 1 calc R U . . .
H8B H 0.916243 0.413970 0.487417 0.080 Uiso 1 1 calc R U . . .
H8C H 0.794802 0.469456 0.496760 0.080 Uiso 1 1 calc R U . . .
C9 C 1.0349(2) 0.47299(10) 0.7378(2) 0.0528(5) Uani 1 1 d . . . . .
H9A H 0.994083 0.517767 0.709107 0.079 Uiso 1 1 calc R U . . .
H9B H 1.116849 0.462942 0.699618 0.079 Uiso 1 1 calc R U . . .
H9C H 1.077801 0.470867 0.838726 0.079 Uiso 1 1 calc R U . . .
C10 C 0.5736(2) 0.34639(9) 0.9717(2) 0.0435(4) Uani 1 1 d . . . . .
H10 H 0.590315 0.301250 0.938351 0.052 Uiso 1 1 calc R U . . .
C11 C 0.4035(2) 0.35033(10) 0.9626(2) 0.0534(5) Uani 1 1 d . . . . .
H11A H 0.386264 0.391761 1.005502 0.080 Uiso 1 1 calc R U . . .
H11B H 0.378969 0.312237 1.010927 0.080 Uiso 1 1 calc R U . . .
H11C H 0.336189 0.349525 0.865510 0.080 Uiso 1 1 calc R U . . .
C12 C 0.6786(3) 0.35185(13) 1.1227(2) 0.0652(6) Uani 1 1 d . . . . .
H12A H 0.676112 0.397597 1.154925 0.098 Uiso 1 1 calc R U . . .
H12B H 0.785263 0.340119 1.131001 0.098 Uiso 1 1 calc R U . . .
H12C H 0.641606 0.321323 1.178901 0.098 Uiso 1 1 calc R U . . .
C13 C 1.0277(2) 0.37221(8) 1.04020(17) 0.0382(4) Uani 1 1 d . . . . .
H13A H 1.099391 0.390296 0.997009 0.057 Uiso 1 1 calc R U . . .
H13B H 1.086315 0.358768 1.135163 0.057 Uiso 1 1 calc R U . . .
H13C H 0.951509 0.406327 1.040893 0.057 Uiso 1 1 calc R U . . .
C14 C 0.94474(17) 0.31259(7) 0.95951(15) 0.0280(3) Uani 1 1 d . . . . .
C15 C 1.0125(2) 0.250000 1.0012(2) 0.0300(5) Uani 1 2 d S T P . .
H15 H 1.115829 0.250000 1.064894 0.036 Uiso 1 2 calc R U P . .
C16 C 0.8653(3) 0.250000 0.5974(3) 0.0389(5) Uani 1 2 d S T P . .
H16A H 0.829678 0.286516 0.531024 0.058 Uiso 0.5 1 calc R U P . .
H16B H 0.975848 0.255976 0.650652 0.058 Uiso 0.5 1 calc R U P . .
H16C H 0.850235 0.207509 0.547848 0.058 Uiso 0.5 1 calc R U P . .
C17 C 0.3389(3) 0.250000 0.6251(2) 0.0316(5) Uani 1 2 d S T P . .
H17 H 0.365868 0.250000 0.727654 0.038 Uiso 1 2 calc R U P . .
C18 C 0.2509(2) 0.31487(8) 0.56630(18) 0.0381(4) Uani 1 1 d . . . . .
H18A H 0.149570 0.314032 0.580897 0.046 Uiso 1 1 calc R U . . .
H18B H 0.310978 0.352864 0.619589 0.046 Uiso 1 1 calc R U . . .
C19 C 0.2216(2) 0.32721(9) 0.41333(19) 0.0425(4) Uani 1 1 d . . . . .
H19A H 0.187530 0.373915 0.391339 0.051 Uiso 1 1 calc R U . . .
H19B H 0.135590 0.298039 0.358279 0.051 Uiso 1 1 calc R U . . .
C20 C 0.3629(2) 0.31465(10) 0.36970(18) 0.0431(4) Uani 1 1 d . . . . .
H20A H 0.435145 0.352708 0.400827 0.052 Uiso 1 1 calc R U . . .
H20B H 0.327769 0.313529 0.267642 0.052 Uiso 1 1 calc R U . . .
C21 C 0.4529(3) 0.250000 0.4256(2) 0.0347(5) Uani 1 2 d S T P . .
H21 H 0.551124 0.250000 0.403641 0.042 Uiso 1 2 calc R U P . .
B1 B 0.4961(3) 0.250000 0.5899(3) 0.0285(5) Uani 1 2 d S T P . .
H1 H 0.5798(19) 0.2954(9) 0.6431(17) 0.034 Uiso 1 1 d . U . . .


_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 1.9119(13) 4_565 ?
Al1 N1 1.9119(13) . ?
Al1 C16 1.934(2) . ?
Al1 B1 2.235(3) . ?
N1 C14 1.3371(19) . ?
N1 C1 1.4511(18) . ?
C1 C6 1.402(2) . ?
C1 C2 1.414(2) . ?
C2 C3 1.394(2) . ?
C2 C10 1.515(2) . ?
C3 C4 1.383(3) . ?
C4 C5 1.368(3) . ?
C5 C6 1.400(2) . ?
C6 C7 1.517(2) . ?
C7 C8 1.536(3) . ?
C7 C9 1.539(3) . ?
C10 C12 1.529(3) . ?
C10 C11 1.530(3) . ?
C13 C14 1.507(2) . ?
C14 C15 1.4026(18) . ?
C17 C18 1.543(2) . ?
C17 C18 1.543(2) 4_565 ?
C17 B1 1.601(3) . ?
C18 C19 1.527(3) . ?
C19 C20 1.529(3) . ?
C20 C21 1.540(2) . ?
C21 B1 1.603(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Al1 N1 95.43(8) 4_565 . ?
N1 Al1 C16 111.25(6) 4_565 . ?
N1 Al1 C16 111.25(6) . . ?
N1 Al1 B1 115.88(6) 4_565 . ?
N1 Al1 B1 115.88(6) . . ?
C16 Al1 B1 106.96(11) . . ?
C14 N1 C1 119.62(12) . . ?
C14 N1 Al1 118.07(10) . . ?
C1 N1 Al1 121.46(9) . . ?
C6 C1 C2 121.16(14) . . ?
C6 C1 N1 120.53(13) . . ?
C2 C1 N1 118.21(13) . . ?
C3 C2 C1 117.90(15) . . ?
C3 C2 C10 120.65(14) . . ?
C1 C2 C10 121.45(14) . . ?
C4 C3 C2 121.45(16) . . ?
C5 C4 C3 119.80(16) . . ?
C4 C5 C6 121.73(16) . . ?
C5 C6 C1 117.96(14) . . ?
C5 C6 C7 118.54(14) . . ?
C1 C6 C7 123.50(14) . . ?
C6 C7 C8 110.62(14) . . ?
C6 C7 C9 111.88(15) . . ?
C8 C7 C9 109.91(16) . . ?
C2 C10 C12 111.64(16) . . ?
C2 C10 C11 113.45(16) . . ?
C12 C10 C11 109.38(16) . . ?
N1 C14 C15 122.61(14) . . ?
N1 C14 C13 120.26(13) . . ?
C15 C14 C13 117.13(14) . . ?
C14 C15 C14 127.33(19) . 4_565 ?
C18 C17 C18 115.24(19) . 4_565 ?
C18 C17 B1 107.46(12) . . ?
C18 C17 B1 107.46(12) 4_565 . ?
C19 C18 C17 115.30(15) . . ?
C18 C19 C20 114.15(14) . . ?
C19 C20 C21 115.30(15) . . ?
C20 C21 C20 114.89(19) 4_565 . ?
C20 C21 B1 107.64(13) 4_565 . ?
C20 C21 B1 107.64(13) . . ?
C17 B1 C21 108.85(18) . . ?
C17 B1 Al1 133.01(16) . . ?
C21 B1 Al1 118.14(16) . . ?

_refine_diff_density_max         0.527
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.042

