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

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

data_rm15117
_database_code_depnum_ccdc_archive 'CCDC 1499077'
_audit_update_record             
;
2016-08-14 deposited with the CCDC.
2016-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H33 Al B Cl5 N2'
_chemical_formula_sum            'C28 H33 Al B Cl5 N2'
_chemical_formula_weight         612.60

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   9.7882(4)
_cell_length_b                   11.2460(5)
_cell_length_c                   14.7984(6)
_cell_angle_alpha                88.786(4)
_cell_angle_beta                 79.599(4)
_cell_angle_gamma                74.904(4)
_cell_volume                     1546.35(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4941
_cell_measurement_theta_min      3.8010
_cell_measurement_theta_max      29.0170

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_F_000             636
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.236
_exptl_absorpt_coefficient_mu    0.518
_shelx_estimated_absorpt_T_min   0.838
_shelx_estimated_absorpt_T_max   0.888
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  
'Agilent Supernova Dual Atlas with CCD detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12778
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.329
_diffrn_reflns_theta_max         29.820
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7336
_reflns_number_gt                5744
_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, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XSHELL and Mercury'
_computing_publication_material  XCIF

_refine_special_details          
;
Structure was solved by direct methods to reveal all non-H atoms 
which were refined anisotropically. H atoms were added at calculated
positions and refined using a riding model.

Residual electron density about the main residue is <0.5 e-/A,
slight disorder noted about the AlCl4 counterion, however not great
enough to merit modelling over separate sites
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0436P)²+1.2962P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7336
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1168
_refine_ls_wR_factor_gt          0.1017
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
Cl5 Cl -0.39849(5) 0.79875(6) 0.32167(4) 0.03657(15) Uani 1 1 d . . . . .
Al2 Al 0.47561(7) 0.31271(6) 0.32053(4) 0.02578(14) Uani 1 1 d . . . . .
Cl3 Cl 0.36109(7) 0.28877(8) 0.45306(4) 0.05289(19) Uani 1 1 d . . . . .
Cl2 Cl 0.33452(7) 0.32998(7) 0.22474(4) 0.05007(18) Uani 1 1 d . . . . .
Cl1 Cl 0.65444(7) 0.15468(6) 0.28491(5) 0.05257(19) Uani 1 1 d . . . . .
Cl4 Cl 0.55153(7) 0.47272(7) 0.32098(6) 0.0597(2) Uani 1 1 d . . . . .
B1 B 0.0091(2) 0.77980(19) 0.22933(15) 0.0200(4) Uani 1 1 d . . . . .
C11 C 0.1410(2) 0.74502(18) 0.15093(13) 0.0220(4) Uani 1 1 d . . . . .
C12 C 0.1306(2) 0.7790(2) 0.06018(14) 0.0266(4) Uani 1 1 d . . . . .
H12 H 0.0398 0.8212 0.0459 0.032 Uiso 1 1 calc R U . . .
C16 C 0.2758(2) 0.6825(2) 0.16947(15) 0.0300(5) Uani 1 1 d . . . . .
H16 H 0.2855 0.6595 0.2306 0.036 Uiso 1 1 calc R U . . .
C13 C 0.2517(2) 0.7517(2) -0.00933(15) 0.0330(5) Uani 1 1 d . . . . .
H13 H 0.2438 0.7765 -0.0704 0.040 Uiso 1 1 calc R U . . .
C15 C 0.3960(2) 0.6535(2) 0.09982(17) 0.0391(5) Uani 1 1 d . . . . .
H15 H 0.4868 0.6098 0.1132 0.047 Uiso 1 1 calc R U . . .
C14 C 0.3832(2) 0.6883(2) 0.01093(17) 0.0385(5) Uani 1 1 d . . . . .
H14 H 0.4656 0.6685 -0.0366 0.046 Uiso 1 1 calc R U . . .
C21 C -0.17998(19) 0.71546(18) 0.14406(12) 0.0197(4) Uani 1 1 d . . . . .
C22 C -0.1441(2) 0.58678(18) 0.14077(13) 0.0226(4) Uani 1 1 d . . . . .
C26 C -0.2419(2) 0.79012(18) 0.07820(13) 0.0224(4) Uani 1 1 d . . . . .
C24 C -0.2327(2) 0.6023(2) -0.00222(14) 0.0290(4) Uani 1 1 d . . . . .
H24 H -0.2502 0.5630 -0.0536 0.035 Uiso 1 1 calc R U . . .
C25 C -0.2669(2) 0.7294(2) 0.00407(14) 0.0270(4) Uani 1 1 d . . . . .
H25 H -0.3083 0.7763 -0.0430 0.032 Uiso 1 1 calc R U . . .
C23 C -0.1731(2) 0.5318(2) 0.06585(15) 0.0278(4) Uani 1 1 d . . . . .
H23 H -0.1517 0.4445 0.0611 0.033 Uiso 1 1 calc R U . . .
C31 C 0.0981(2) 0.85432(18) 0.36510(13) 0.0229(4) Uani 1 1 d . . . . .
C36 C 0.1238(2) 0.9702(2) 0.35169(16) 0.0317(5) Uani 1 1 d . . . . .
C32 C 0.1690(2) 0.7681(2) 0.42248(14) 0.0314(5) Uani 1 1 d . . . . .
C34 C 0.2952(2) 0.9148(3) 0.45433(18) 0.0474(7) Uani 1 1 d . . . . .
H34 H 0.3632 0.9358 0.4852 0.057 Uiso 1 1 calc R U . . .
C35 C 0.2244(3) 0.9990(2) 0.39782(19) 0.0447(6) Uani 1 1 d . . . . .
H35 H 0.2441 1.0773 0.3902 0.054 Uiso 1 1 calc R U . . .
C33 C 0.2684(3) 0.8017(3) 0.46618(16) 0.0423(6) Uani 1 1 d . . . . .
H33 H 0.3185 0.7448 0.5050 0.051 Uiso 1 1 calc R U . . .
N1 N -0.14132(16) 0.77108(14) 0.22077(10) 0.0201(3) Uani 1 1 d . . . . .
N2 N -0.00552(17) 0.82205(15) 0.31856(11) 0.0217(3) Uani 1 1 d . . . . .
C1 C -0.2273(2) 0.80486(18) 0.29853(13) 0.0233(4) Uani 1 1 d . . . . .
C2 C -0.1539(2) 0.8441(2) 0.36753(13) 0.0252(4) Uani 1 1 d . . . . .
H2A H -0.1957 0.9323 0.3853 0.030 Uiso 1 1 calc R U . . .
H2B H -0.1598 0.7941 0.4233 0.030 Uiso 1 1 calc R U . . .
C4 C -0.0769(2) 0.51387(19) 0.21603(15) 0.0297(5) Uani 1 1 d . . . . .
H4A H -0.1407 0.5417 0.2758 0.036 Uiso 1 1 calc R U . . .
H4B H 0.0158 0.5332 0.2175 0.036 Uiso 1 1 calc R U . . .
C5 C -0.2839(2) 0.92894(19) 0.08414(15) 0.0309(5) Uani 1 1 d . . . . .
H5A H -0.2528 0.9612 0.0233 0.037 Uiso 1 1 calc R U . . .
H5B H -0.2332 0.9566 0.1285 0.037 Uiso 1 1 calc R U . . .
C3 C -0.0495(3) 0.3751(2) 0.20654(17) 0.0366(5) Uani 1 1 d . . . . .
H3A H -0.0079 0.3359 0.2586 0.055 Uiso 1 1 calc R U . . .
H3B H 0.0175 0.3455 0.1491 0.055 Uiso 1 1 calc R U . . .
H3C H -0.1405 0.3544 0.2058 0.055 Uiso 1 1 calc R U . . .
C9 C 0.1439(3) 0.6417(2) 0.43752(17) 0.0413(6) Uani 1 1 d . . . . .
H9A H 0.0751 0.6308 0.3989 0.050 Uiso 1 1 calc R U . . .
H9B H 0.2359 0.5789 0.4171 0.050 Uiso 1 1 calc R U . . .
C6 C -0.4457(3) 0.9822(2) 0.11425(17) 0.0425(6) Uani 1 1 d . . . . .
H6A H -0.4678 1.0723 0.1174 0.064 Uiso 1 1 calc R U . . .
H6B H -0.4769 0.9516 0.1749 0.064 Uiso 1 1 calc R U . . .
H6C H -0.4964 0.9569 0.0697 0.064 Uiso 1 1 calc R U . . .
C8 C 0.0520(3) 1.0609(2) 0.2878(2) 0.0439(6) Uani 1 1 d . . . . .
H8A H 0.0236 1.1443 0.3168 0.053 Uiso 1 1 calc R U . . .
H8B H -0.0366 1.0401 0.2783 0.053 Uiso 1 1 calc R U . . .
C7 C 0.1488(3) 1.0626(2) 0.1944(2) 0.0503(7) Uani 1 1 d . . . . .
H7A H 0.0968 1.1229 0.1555 0.076 Uiso 1 1 calc R U . . .
H7B H 0.1758 0.9806 0.1647 0.076 Uiso 1 1 calc R U . . .
H7C H 0.2357 1.0853 0.2032 0.076 Uiso 1 1 calc R U . . .
C10 C 0.0862(4) 0.6198(3) 0.5362(2) 0.0673(9) Uani 1 1 d . . . . .
H10A H 0.0711 0.5369 0.5413 0.101 Uiso 1 1 calc R U . . .
H10B H -0.0055 0.6810 0.5569 0.101 Uiso 1 1 calc R U . . .
H10C H 0.1554 0.6272 0.5747 0.101 Uiso 1 1 calc R 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
Cl5 C1 1.668(2) . ?
Al2 Cl4 2.1187(9) . ?
Al2 Cl2 2.1236(8) . ?
Al2 Cl3 2.1252(9) . ?
Al2 Cl1 2.1416(9) . ?
B1 N2 1.383(3) . ?
B1 N1 1.528(3) . ?
B1 C11 1.544(3) . ?
C11 C16 1.396(3) . ?
C11 C12 1.403(3) . ?
C12 C13 1.393(3) . ?
C12 H12 0.9500 . ?
C16 C15 1.389(3) . ?
C16 H16 0.9500 . ?
C13 C14 1.381(3) . ?
C13 H13 0.9500 . ?
C15 C14 1.383(4) . ?
C15 H15 0.9500 . ?
C14 H14 0.9500 . ?
C21 C26 1.391(3) . ?
C21 C22 1.397(3) . ?
C21 N1 1.460(2) . ?
C22 C23 1.388(3) . ?
C22 C4 1.513(3) . ?
C26 C25 1.395(3) . ?
C26 C5 1.507(3) . ?
C24 C25 1.381(3) . ?
C24 C23 1.386(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C23 H23 0.9500 . ?
C31 C36 1.394(3) . ?
C31 C32 1.403(3) . ?
C31 N2 1.446(2) . ?
C36 C35 1.399(3) . ?
C36 C8 1.501(3) . ?
C32 C33 1.391(3) . ?
C32 C9 1.510(3) . ?
C34 C33 1.367(4) . ?
C34 C35 1.382(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C33 H33 0.9500 . ?
N1 C1 1.296(2) . ?
N2 C2 1.461(2) . ?
C1 C2 1.484(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 C3 1.518(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.526(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C9 C10 1.508(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 C7 1.531(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl4 Al2 Cl2 110.04(4) . . ?
Cl4 Al2 Cl3 110.08(4) . . ?
Cl2 Al2 Cl3 108.47(4) . . ?
Cl4 Al2 Cl1 109.48(4) . . ?
Cl2 Al2 Cl1 109.96(4) . . ?
Cl3 Al2 Cl1 108.78(4) . . ?
N2 B1 N1 104.63(16) . . ?
N2 B1 C11 131.43(18) . . ?
N1 B1 C11 123.94(17) . . ?
C16 C11 C12 118.18(18) . . ?
C16 C11 B1 120.46(18) . . ?
C12 C11 B1 121.32(18) . . ?
C13 C12 C11 120.8(2) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C15 C16 C11 120.9(2) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C14 C13 C12 119.7(2) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C14 C15 C16 119.9(2) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C13 C14 C15 120.5(2) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C26 C21 C22 124.56(18) . . ?
C26 C21 N1 119.81(17) . . ?
C22 C21 N1 115.55(16) . . ?
C23 C22 C21 116.54(18) . . ?
C23 C22 C4 122.99(18) . . ?
C21 C22 C4 120.47(18) . . ?
C21 C26 C25 116.17(18) . . ?
C21 C26 C5 123.92(18) . . ?
C25 C26 C5 119.91(18) . . ?
C25 C24 C23 120.46(19) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 121.28(19) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C24 C23 C22 120.99(19) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C36 C31 C32 122.26(19) . . ?
C36 C31 N2 118.84(18) . . ?
C32 C31 N2 118.91(18) . . ?
C31 C36 C35 117.6(2) . . ?
C31 C36 C8 122.4(2) . . ?
C35 C36 C8 120.0(2) . . ?
C33 C32 C31 117.6(2) . . ?
C33 C32 C9 119.1(2) . . ?
C31 C32 C9 123.2(2) . . ?
C33 C34 C35 120.5(2) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C36 120.8(2) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C34 C33 C32 121.2(2) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C1 N1 C21 123.96(16) . . ?
C1 N1 B1 108.89(16) . . ?
C21 N1 B1 126.46(15) . . ?
B1 N2 C31 130.18(16) . . ?
B1 N2 C2 111.55(16) . . ?
C31 N2 C2 118.09(15) . . ?
N1 C1 C2 112.18(17) . . ?
N1 C1 Cl5 124.62(16) . . ?
C2 C1 Cl5 123.13(14) . . ?
N2 C2 C1 102.67(15) . . ?
N2 C2 H2A 111.2 . . ?
C1 C2 H2A 111.2 . . ?
N2 C2 H2B 111.2 . . ?
C1 C2 H2B 111.2 . . ?
H2A C2 H2B 109.1 . . ?
C22 C4 C3 115.19(19) . . ?
C22 C4 H4A 108.5 . . ?
C3 C4 H4A 108.5 . . ?
C22 C4 H4B 108.5 . . ?
C3 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C26 C5 C6 112.39(19) . . ?
C26 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
C26 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C10 C9 C32 113.5(2) . . ?
C10 C9 H9A 108.9 . . ?
C32 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
C32 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C36 C8 C7 112.8(2) . . ?
C36 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C36 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_refine_diff_density_max         0.656
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.057

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2016ncs0437_sq
_database_code_depnum_ccdc_archive 'CCDC 1499078'
_audit_update_record             
;
2016-08-14 deposited with the CCDC.
2016-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H41 B Cl1 N2, Al Cl4'
_chemical_formula_sum            'C32 H41 Al B Cl5 N2'
_chemical_formula_weight         668.71

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

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

_cell_length_a                   18.9942(4)
_cell_length_b                   18.2174(4)
_cell_length_c                   10.5733(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3658.63(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22889
_cell_measurement_theta_min      2.2130
_cell_measurement_theta_max      25.0240

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.444
_shelx_estimated_absorpt_T_min   0.970
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88232
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41108
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.418
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             6461
_reflns_number_gt                5852
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    0.976

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XSHELL and Mercury'
_computing_publication_material  XCIF

_refine_special_details          
;
Structure was solved by direct methods to reveal all non-H atoms. Remaining
non-H atoms were located in subsequent difference map. All non-H atoms were
refined anisotropically with H atoms being added at calculated positions and
refined using a riding model.

OMIT h k l command was used on the follwing low angle reflections 
due in part to weakly diffracting data showing impingement from beamstop:

0   2   0
0   1   1
0   0   1
1   1   0
1   0   1
2   0   0

Due to severely disordered CH2Cl2 solvent molecules which could not be
effectively modelled over several sites, SQUEEZE protocol was implemented
identifying a SAV of 173 A3 containing 69 electrons which is roughly
consistent with the presence of 1-2 CH2Cl2 solvent molecules in the structure.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0448P)²+1.2807P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.025(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6461
_refine_ls_number_parameters     378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0843
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cl1 Cl 0.38636(4) 0.20883(5) 0.81206(9) 0.0365(2) Uani 1 1 d . . . . .
Cl5 Cl 0.16214(5) 0.53982(5) 0.04475(8) 0.0329(2) Uani 1 1 d . . . . .
Cl4 Cl 0.46011(6) 0.21761(6) 1.11397(9) 0.0543(3) Uani 1 1 d . . . . .
Cl3 Cl 0.52859(6) 0.09849(6) 0.89002(12) 0.0551(3) Uani 1 1 d . . . . .
Al1 Al 0.48236(5) 0.20415(6) 0.91854(10) 0.0336(2) Uani 1 1 d . . . . .
Cl2 Cl 0.55047(6) 0.28786(7) 0.85180(13) 0.0687(4) Uani 1 1 d . . . . .
N2 N 0.18009(14) 0.48535(14) 0.4016(2) 0.0248(6) Uani 1 1 d . . . . .
N1 N 0.24198(14) 0.47724(14) 0.2156(2) 0.0230(6) Uani 1 1 d . . . . .
C31 C 0.15176(17) 0.48909(17) 0.5284(3) 0.0254(7) Uani 1 1 d . . . . .
C32 C 0.10555(16) 0.43391(17) 0.5689(3) 0.0268(7) Uani 1 1 d . . . . .
C21 C 0.29747(17) 0.46619(17) 0.1224(3) 0.0245(7) Uani 1 1 d . . . . .
C16 C 0.35813(17) 0.37956(18) 0.3561(3) 0.0298(8) Uani 1 1 d . . . . .
H16 H 0.3585 0.3812 0.2663 0.036 Uiso 1 1 calc R U . . .
C15 C 0.41095(19) 0.34192(19) 0.4177(3) 0.0343(8) Uani 1 1 d . . . . .
H15 H 0.4471 0.3184 0.3706 0.041 Uiso 1 1 calc R U . . .
C11 C 0.30368(17) 0.41566(17) 0.4215(3) 0.0264(7) Uani 1 1 d . . . . .
C33 C 0.07599(17) 0.4409(2) 0.6882(3) 0.0319(8) Uani 1 1 d . . . . .
H33 H 0.0452 0.4038 0.7188 0.038 Uiso 1 1 calc R U . . .
C36 C 0.16890(18) 0.54943(19) 0.6045(3) 0.0317(8) Uani 1 1 d . . . . .
C35 C 0.13615(19) 0.5543(2) 0.7222(3) 0.0349(8) Uani 1 1 d . . . . .
H35 H 0.1455 0.5953 0.7750 0.042 Uiso 1 1 calc R U . . .
C58 C 0.35642(19) 0.57964(18) 0.2159(4) 0.0331(8) Uani 1 1 d . . . . .
H58 H 0.3264 0.5664 0.2901 0.040 Uiso 1 1 calc R U . . .
C22 C 0.35297(17) 0.51548(18) 0.1230(3) 0.0285(7) Uani 1 1 d . . . . .
C55 C 0.08699(19) 0.36784(19) 0.4885(4) 0.0342(8) Uani 1 1 d . . . . .
H55 H 0.1089 0.3747 0.4033 0.041 Uiso 1 1 calc R U . . .
C26 C 0.29252(17) 0.40518(18) 0.0428(3) 0.0285(7) Uani 1 1 d . . . . .
C34 C 0.09055(19) 0.5008(2) 0.7629(3) 0.0363(9) Uani 1 1 d . . . . .
H34 H 0.0688 0.5053 0.8435 0.044 Uiso 1 1 calc R U . . .
C25 C 0.34914(19) 0.3939(2) -0.0373(3) 0.0358(8) Uani 1 1 d . . . . .
H25 H 0.3496 0.3516 -0.0900 0.043 Uiso 1 1 calc R U . . .
C50 C 0.13909(17) 0.52033(18) 0.3024(3) 0.0280(7) Uani 1 1 d . . . . .
H50A H 0.1315 0.5730 0.3209 0.034 Uiso 1 1 calc R U . . .
H50B H 0.0929 0.4960 0.2917 0.034 Uiso 1 1 calc R U . . .
C52 C 0.2212(2) 0.6081(2) 0.5649(4) 0.0405(9) Uani 1 1 d . . . . .
H52 H 0.2422 0.5930 0.4823 0.049 Uiso 1 1 calc R U . . .
C12 C 0.3063(2) 0.4107(2) 0.5537(4) 0.0422(9) Uani 1 1 d . . . . .
H12 H 0.2707 0.4339 0.6026 0.051 Uiso 1 1 calc R U . . .
C61 C 0.23088(19) 0.35189(19) 0.0447(3) 0.0331(8) Uani 1 1 d . . . . .
H61 H 0.1932 0.3732 0.0998 0.040 Uiso 1 1 calc R U . . .
C24 C 0.4052(2) 0.4425(2) -0.0428(3) 0.0392(9) Uani 1 1 d . . . . .
H24 H 0.4428 0.4341 -0.1003 0.047 Uiso 1 1 calc R U . . .
C23 C 0.4061(2) 0.5029(2) 0.0355(3) 0.0370(8) Uani 1 1 d . . . . .
H23 H 0.4440 0.5368 0.0295 0.044 Uiso 1 1 calc R U . . .
C51 C 0.18341(17) 0.51053(17) 0.1899(3) 0.0246(7) Uani 1 1 d . . . . .
C14 C 0.4111(2) 0.3387(2) 0.5471(4) 0.0494(11) Uani 1 1 d . . . . .
H14 H 0.4471 0.3126 0.5903 0.059 Uiso 1 1 calc R U . . .
C63 C 0.2004(2) 0.3418(2) -0.0882(4) 0.0445(10) Uani 1 1 d . . . . .
H63A H 0.1909 0.3900 -0.1256 0.067 Uiso 1 1 calc R U . . .
H63B H 0.1565 0.3137 -0.0831 0.067 Uiso 1 1 calc R U . . .
H63C H 0.2344 0.3153 -0.1410 0.067 Uiso 1 1 calc R U . . .
C62 C 0.2525(2) 0.2775(2) 0.1004(4) 0.0438(10) Uani 1 1 d . . . . .
H62A H 0.2879 0.2546 0.0456 0.066 Uiso 1 1 calc R U . . .
H62B H 0.2112 0.2455 0.1060 0.066 Uiso 1 1 calc R U . . .
H62C H 0.2724 0.2848 0.1850 0.066 Uiso 1 1 calc R U . . .
C53 C 0.1856(2) 0.6817(2) 0.5459(5) 0.0508(11) Uani 1 1 d . . . . .
H53A H 0.1484 0.6768 0.4821 0.076 Uiso 1 1 calc R U . . .
H53B H 0.2203 0.7178 0.5172 0.076 Uiso 1 1 calc R U . . .
H53C H 0.1649 0.6981 0.6260 0.076 Uiso 1 1 calc R U . . .
C13 C 0.3588(3) 0.3734(3) 0.6140(4) 0.0565(12) Uani 1 1 d . . . . .
H13 H 0.3592 0.3714 0.7038 0.068 Uiso 1 1 calc R U . . .
B1 B 0.2438(2) 0.4571(2) 0.3560(3) 0.0250(8) Uani 1 1 d . . . . .
C54 C 0.2811(2) 0.6150(2) 0.6610(5) 0.0620(14) Uani 1 1 d . . . . .
H54A H 0.2620 0.6311 0.7425 0.093 Uiso 1 1 calc R U . . .
H54B H 0.3155 0.6510 0.6307 0.093 Uiso 1 1 calc R U . . .
H54C H 0.3041 0.5672 0.6713 0.093 Uiso 1 1 calc R U . . .
C57 C 0.1171(3) 0.2974(2) 0.5463(5) 0.0694(14) Uani 1 1 d . . . . .
H57A H 0.1684 0.3016 0.5526 0.104 Uiso 1 1 calc R U . . .
H57B H 0.1050 0.2555 0.4925 0.104 Uiso 1 1 calc R U . . .
H57C H 0.0972 0.2902 0.6309 0.104 Uiso 1 1 calc R U . . .
C56 C 0.0084(2) 0.3608(2) 0.4706(5) 0.0525(11) Uani 1 1 d . . . . .
H56A H -0.0139 0.3513 0.5524 0.079 Uiso 1 1 calc R U . . .
H56B H -0.0015 0.3201 0.4127 0.079 Uiso 1 1 calc R U . . .
H56C H -0.0102 0.4065 0.4349 0.079 Uiso 1 1 calc R U . . .
C59 C 0.4299(2) 0.5939(3) 0.2653(5) 0.0656(14) Uani 1 1 d . . . . .
H59A H 0.4509 0.5476 0.2936 0.098 Uiso 1 1 calc R U . . .
H59B H 0.4275 0.6283 0.3365 0.098 Uiso 1 1 calc R U . . .
H59C H 0.4588 0.6151 0.1978 0.098 Uiso 1 1 calc R U . . .
C60 C 0.3260(3) 0.6486(2) 0.1587(5) 0.0665(14) Uani 1 1 d . . . . .
H60A H 0.3524 0.6614 0.0822 0.100 Uiso 1 1 calc R U . . .
H60B H 0.3294 0.6888 0.2199 0.100 Uiso 1 1 calc R U . . .
H60C H 0.2765 0.6403 0.1369 0.100 Uiso 1 1 calc R 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
Cl1 Al1 2.1446(14) . ?
Cl5 C51 1.674(3) . ?
Cl4 Al1 2.1233(15) . ?
Cl3 Al1 2.1371(14) . ?
Al1 Cl2 2.1208(16) . ?
N2 B1 1.401(5) . ?
N2 C31 1.447(4) . ?
N2 C50 1.454(4) . ?
N1 C51 1.296(4) . ?
N1 C21 1.456(4) . ?
N1 B1 1.530(4) . ?
C31 C36 1.400(5) . ?
C31 C32 1.401(5) . ?
C32 C33 1.387(5) . ?
C32 C55 1.515(5) . ?
C21 C22 1.385(5) . ?
C21 C26 1.397(5) . ?
C16 C15 1.379(5) . ?
C16 C11 1.407(5) . ?
C16 H16 0.9500 . ?
C15 C14 1.369(6) . ?
C15 H15 0.9500 . ?
C11 C12 1.402(5) . ?
C11 B1 1.531(5) . ?
C33 C34 1.376(5) . ?
C33 H33 0.9500 . ?
C36 C35 1.394(5) . ?
C36 C52 1.519(5) . ?
C35 C34 1.373(5) . ?
C35 H35 0.9500 . ?
C58 C60 1.508(6) . ?
C58 C59 1.513(5) . ?
C58 C22 1.528(5) . ?
C58 H58 1.0000 . ?
C22 C23 1.388(5) . ?
C55 C56 1.509(5) . ?
C55 C57 1.532(6) . ?
C55 H55 1.0000 . ?
C26 C25 1.384(5) . ?
C26 C61 1.521(5) . ?
C34 H34 0.9500 . ?
C25 C24 1.386(5) . ?
C25 H25 0.9500 . ?
C50 C51 1.468(5) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C52 C53 1.516(6) . ?
C52 C54 1.529(6) . ?
C52 H52 1.0000 . ?
C12 C13 1.366(6) . ?
C12 H12 0.9500 . ?
C61 C63 1.530(5) . ?
C61 C62 1.534(5) . ?
C61 H61 1.0000 . ?
C24 C23 1.378(5) . ?
C24 H24 0.9500 . ?
C23 H23 0.9500 . ?
C14 C13 1.373(6) . ?
C14 H14 0.9500 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C13 H13 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Al1 Cl4 111.23(7) . . ?
Cl2 Al1 Cl3 110.49(7) . . ?
Cl4 Al1 Cl3 108.85(7) . . ?
Cl2 Al1 Cl1 108.39(6) . . ?
Cl4 Al1 Cl1 109.70(6) . . ?
Cl3 Al1 Cl1 108.12(6) . . ?
B1 N2 C31 131.1(3) . . ?
B1 N2 C50 112.1(3) . . ?
C31 N2 C50 116.7(3) . . ?
C51 N1 C21 123.0(3) . . ?
C51 N1 B1 109.6(3) . . ?
C21 N1 B1 127.3(3) . . ?
C36 C31 C32 122.3(3) . . ?
C36 C31 N2 118.9(3) . . ?
C32 C31 N2 118.8(3) . . ?
C33 C32 C31 117.7(3) . . ?
C33 C32 C55 119.3(3) . . ?
C31 C32 C55 123.0(3) . . ?
C22 C21 C26 124.7(3) . . ?
C22 C21 N1 117.3(3) . . ?
C26 C21 N1 117.9(3) . . ?
C15 C16 C11 122.4(3) . . ?
C15 C16 H16 118.8 . . ?
C11 C16 H16 118.8 . . ?
C14 C15 C16 119.6(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C12 C11 C16 115.7(3) . . ?
C12 C11 B1 120.6(3) . . ?
C16 C11 B1 123.6(3) . . ?
C34 C33 C32 120.9(3) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C35 C36 C31 117.3(3) . . ?
C35 C36 C52 119.5(3) . . ?
C31 C36 C52 123.1(3) . . ?
C34 C35 C36 121.1(3) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C60 C58 C59 110.4(4) . . ?
C60 C58 C22 111.3(3) . . ?
C59 C58 C22 113.2(3) . . ?
C60 C58 H58 107.2 . . ?
C59 C58 H58 107.2 . . ?
C22 C58 H58 107.2 . . ?
C21 C22 C23 116.3(3) . . ?
C21 C22 C58 122.1(3) . . ?
C23 C22 C58 121.5(3) . . ?
C56 C55 C32 111.6(3) . . ?
C56 C55 C57 110.4(3) . . ?
C32 C55 C57 110.7(3) . . ?
C56 C55 H55 108.0 . . ?
C32 C55 H55 108.0 . . ?
C57 C55 H55 108.0 . . ?
C25 C26 C21 115.8(3) . . ?
C25 C26 C61 120.8(3) . . ?
C21 C26 C61 123.5(3) . . ?
C35 C34 C33 120.6(3) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C26 C25 C24 121.9(3) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
N2 C50 C51 103.0(3) . . ?
N2 C50 H50A 111.2 . . ?
C51 C50 H50A 111.2 . . ?
N2 C50 H50B 111.2 . . ?
C51 C50 H50B 111.2 . . ?
H50A C50 H50B 109.1 . . ?
C53 C52 C36 111.5(3) . . ?
C53 C52 C54 110.4(3) . . ?
C36 C52 C54 111.2(3) . . ?
C53 C52 H52 107.9 . . ?
C36 C52 H52 107.9 . . ?
C54 C52 H52 107.9 . . ?
C13 C12 C11 121.6(4) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C26 C61 C63 110.8(3) . . ?
C26 C61 C62 111.3(3) . . ?
C63 C61 C62 110.3(3) . . ?
C26 C61 H61 108.1 . . ?
C63 C61 H61 108.1 . . ?
C62 C61 H61 108.1 . . ?
C23 C24 C25 119.7(3) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C23 C22 121.5(3) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
N1 C51 C50 112.3(3) . . ?
N1 C51 Cl5 123.2(3) . . ?
C50 C51 Cl5 124.4(2) . . ?
C15 C14 C13 119.6(4) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C12 C13 C14 121.1(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
N2 B1 N1 103.1(3) . . ?
N2 B1 C11 131.8(3) . . ?
N1 B1 C11 125.1(3) . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

_refine_diff_density_max         0.333
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.040

_shelxl_version_number           2013-3



####################################################################### 
# 
# 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_2016ncs0250z_sq_sq
_database_code_depnum_ccdc_archive 'CCDC 1499079'
_audit_update_record             
;
2016-08-14 deposited with the CCDC.
2016-09-28 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_DIFMX01_2016ncs0250z_sq_sq  
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: Disorder noted about one of the phenyl rings of the boronium species.
Despite attempts to split and model this disorder, they were unsuccessful
and a slightly enlarged residual eletron denisty remains.
;
_vrf_DIFMX02_2016ncs0250z_sq_sq  
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: See above.
;
_vrf_PLAT097_2016ncs0250z_sq_sq  
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       1.35 eA-3  
RESPONSE: See above.
;
_vrf_PLAT220_2016ncs0250z_sq_sq  
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        3.6 Ratio 
RESPONSE: As mentioned above, difference in Ueq as a result of
unmodelled disorder about phenyl group.
;
_vrf_PLAT222_2016ncs0250z_sq_sq  
;
PROBLEM: Non-Solvent Resd 1   H Uiso(max)/Uiso(min) Range        4.5 Ratio 
RESPONSE: As mentioned above, difference in Ueq as a result of
unmodelled disorder about phenyl group.
;
_vrf_PLAT241_2016ncs0250z_sq_sq  
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C00M Check 
RESPONSE: As mentioned above, difference in Ueq as a result of
unmodelled disorder about phenyl group.
;
_vrf_PLAT242_2016ncs0250z_sq_sq  
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       C00H Check 
RESPONSE: As mentioned above, difference in Ueq as a result of
unmodelled disorder about phenyl group.
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H28 B Cl2 N2, Al Cl4'
_chemical_formula_sum            'C22 H28 Al B Cl6 N2'
_chemical_formula_weight         570.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   21.5021(5)
_cell_length_b                   12.4712(3)
_cell_length_c                   22.7768(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.399(3)
_cell_angle_gamma                90
_cell_volume                     6025.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    12621
_cell_measurement_theta_min      2.1120
_cell_measurement_theta_max      29.8530

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_F_000             2352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.612
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90586
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19354
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.920
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6881
_reflns_number_gt                5853
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XSHELL and Mercury'
_computing_publication_material  XCIF

_refine_special_details          
;
Structure was solved using direct methods to reveal non-H atoms. 
Subsequent non-H atoms were located using difference maps. H atoms
were added at calculated positions using riding model. 

OMIT command was used on reflection -1 1 1 due to Fo<Fc due to beamstop
impingement. SQUEEZE protocols were implemented due to severely disordered
toluene molecule. Attempts to model this disorder over multiple sites using
PART and FVAR commands were unsuccessful.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+16.1305P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6881
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1166
_refine_ls_wR_factor_gt          0.1119
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
Cl01 Cl 0.53838(2) 0.61656(4) 0.46757(2) 0.02382(12) Uani 1 1 d . . . . .
Cl02 Cl 0.52139(3) 0.63352(5) 0.61677(3) 0.03020(14) Uani 1 1 d . . . . .
Cl03 Cl 0.39379(3) 0.68869(5) 0.50295(3) 0.03250(15) Uani 1 1 d . . . . .
Cl04 Cl 0.76262(3) 0.34060(5) 0.67461(3) 0.03546(16) Uani 1 1 d . . . . .
Cl05 Cl 0.73881(3) 0.55175(6) 0.72997(3) 0.03770(16) Uani 1 1 d . . . . .
Cl06 Cl 0.52246(4) 0.86598(5) 0.53181(3) 0.04234(18) Uani 1 1 d . . . . .
Al07 Al 0.49338(3) 0.70413(5) 0.53079(3) 0.02423(16) Uani 1 1 d . . . . .
N008 N 0.69745(8) 0.51099(15) 0.60966(8) 0.0221(4) Uani 1 1 d . . . . .
N009 N 0.64055(8) 0.41536(16) 0.67370(9) 0.0243(4) Uani 1 1 d . . . . .
C00A C 0.63999(10) 0.49915(17) 0.58508(10) 0.0224(4) Uani 1 1 d . . . . .
H00A H 0.6222 0.5265 0.5471 0.027 Uiso 1 1 calc R U . . .
C00B C 0.60534(10) 0.43675(18) 0.62444(10) 0.0231(4) Uani 1 1 d . . . . .
H00B H 0.5625 0.4154 0.6144 0.028 Uiso 1 1 calc R U . . .
C00C C 0.74311(11) 0.5748(2) 0.58347(11) 0.0278(5) Uani 1 1 d . . . . .
C00D C 0.78430(12) 0.5221(2) 0.55217(12) 0.0331(6) Uani 1 1 d . . . . .
C00E C 0.61795(11) 0.3535(3) 0.72018(11) 0.0357(6) Uani 1 1 d . . . . .
C00F C 0.74319(13) 0.6859(2) 0.59339(12) 0.0344(6) Uani 1 1 d . . . . .
C00G C 0.77751(13) 0.4065(2) 0.53290(13) 0.0374(6) Uani 1 1 d . . . . .
H00C H 0.7441 0.3721 0.5516 0.045 Uiso 1 1 calc R U . . .
H00D H 0.8175 0.3681 0.5468 0.045 Uiso 1 1 calc R U . . .
C00H C 0.69234(15) 0.7420(2) 0.62047(14) 0.0409(6) Uani 1 1 d . . . . .
H00E H 0.6562 0.7562 0.5885 0.049 Uiso 1 1 calc R U . . .
H00F H 0.6775 0.6926 0.6493 0.049 Uiso 1 1 calc R U . . .
C00I C 0.83136(13) 0.5854(3) 0.53367(13) 0.0439(7) Uani 1 1 d . . . . .
H00I H 0.8611 0.5530 0.5126 0.053 Uiso 1 1 calc R U . . .
C00J C 0.79111(15) 0.7434(3) 0.57336(14) 0.0452(7) Uani 1 1 d . . . . .
H00J H 0.7935 0.8188 0.5791 0.054 Uiso 1 1 calc R U . . .
C00K C 0.59865(12) 0.4090(4) 0.76775(13) 0.0531(10) Uani 1 1 d . . . . .
C00L C 0.63017(15) 0.1819(2) 0.66010(15) 0.0485(8) Uani 1 1 d . . . . .
H00G H 0.6599 0.1227 0.6733 0.058 Uiso 1 1 calc R U . . .
H00H H 0.6509 0.2310 0.6352 0.058 Uiso 1 1 calc R U . . .
C00M C 0.61608(17) 0.2414(4) 0.71352(15) 0.0751(7) Uani 1 1 d . . . . .
C00N C 0.83520(14) 0.6929(3) 0.54535(14) 0.0494(8) Uani 1 1 d . . . . .
H00N H 0.8687 0.7335 0.5340 0.059 Uiso 1 1 calc R U . . .
C00O C 0.76090(16) 0.3966(3) 0.46535(14) 0.0479(7) Uani 1 1 d . . . . .
H00K H 0.7944 0.4291 0.4468 0.072 Uiso 1 1 calc R U . . .
H00L H 0.7210 0.4336 0.4516 0.072 Uiso 1 1 calc R U . . .
H00M H 0.7567 0.3207 0.4543 0.072 Uiso 1 1 calc R U . . .
B00P B 0.71114(12) 0.4550(2) 0.67339(12) 0.0256(5) Uani 1 1 d . . . . .
C00Q C 0.59627(14) 0.5294(4) 0.77242(15) 0.0643(12) Uani 1 1 d . . . . .
H00O H 0.5517 0.5520 0.7694 0.077 Uiso 1 1 calc R U . . .
H00P H 0.6131 0.5612 0.7384 0.077 Uiso 1 1 calc R U . . .
C00R C 0.57061(17) 0.1356(3) 0.62262(17) 0.0618(10) Uani 1 1 d . . . . .
H00Q H 0.5822 0.0939 0.5896 0.093 Uiso 1 1 calc R U . . .
H00R H 0.5425 0.1944 0.6068 0.093 Uiso 1 1 calc R U . . .
H00S H 0.5490 0.0891 0.6475 0.093 Uiso 1 1 calc R U . . .
C00S C 0.63356(16) 0.5739(4) 0.83020(16) 0.0748(14) Uani 1 1 d . . . . .
H00T H 0.6786 0.5606 0.8311 0.112 Uiso 1 1 calc R U . . .
H00U H 0.6198 0.5384 0.8643 0.112 Uiso 1 1 calc R U . . .
H00V H 0.6262 0.6513 0.8323 0.112 Uiso 1 1 calc R U . . .
C00T C 0.57830(17) 0.3461(4) 0.81141(15) 0.0751(7) Uani 1 1 d . . . . .
H00W H 0.5648 0.3799 0.8445 0.090 Uiso 1 1 calc R U . . .
C00U C 0.57737(17) 0.2384(4) 0.80761(15) 0.0751(7) Uani 1 1 d . . . . .
H00X H 0.5636 0.1984 0.8386 0.090 Uiso 1 1 calc R U . . .
C00V C 0.59584(17) 0.1830(4) 0.75983(15) 0.0751(7) Uani 1 1 d . . . . .
H00Y H 0.5947 0.1069 0.7587 0.090 Uiso 1 1 calc R U . . .
C00W C 0.7115(2) 0.8455(3) 0.6516(2) 0.0807(14) Uani 1 1 d . . . . .
H00$ H 0.6756 0.8756 0.6675 0.121 Uiso 1 1 calc R U . . .
H00 H 0.7251 0.8962 0.6233 0.121 Uiso 1 1 calc R U . . .
H002 H 0.7464 0.8324 0.6843 0.121 Uiso 1 1 calc R 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
Cl01 Al07 2.1581(9) . ?
Cl02 Al07 2.1421(10) . ?
Cl03 Al07 2.1403(9) . ?
Cl04 B00P 1.803(3) . ?
Cl05 B00P 1.794(3) . ?
Cl06 Al07 2.1121(9) . ?
N008 C00A 1.279(3) . ?
N008 C00C 1.464(3) . ?
N008 B00P 1.594(3) . ?
N009 C00B 1.275(3) . ?
N009 C00E 1.456(3) . ?
N009 B00P 1.597(3) . ?
C00A C00B 1.477(3) . ?
C00A H00A 0.9500 . ?
C00B H00B 0.9500 . ?
C00C C00D 1.390(4) . ?
C00C C00F 1.403(4) . ?
C00D C00I 1.402(4) . ?
C00D C00G 1.507(4) . ?
C00E C00K 1.404(4) . ?
C00E C00M 1.406(6) . ?
C00F C00J 1.392(4) . ?
C00F C00H 1.512(4) . ?
C00G C00O 1.527(4) . ?
C00G H00C 0.9900 . ?
C00G H00D 0.9900 . ?
C00H C00W 1.498(4) . ?
C00H H00E 0.9900 . ?
C00H H00F 0.9900 . ?
C00I C00N 1.367(5) . ?
C00I H00I 0.9500 . ?
C00J C00N 1.378(5) . ?
C00J H00J 0.9500 . ?
C00K C00T 1.391(4) . ?
C00K C00Q 1.507(6) . ?
C00L C00M 1.498(6) . ?
C00L C00R 1.531(4) . ?
C00L H00G 0.9900 . ?
C00L H00H 0.9900 . ?
C00M C00V 1.408(4) . ?
C00N H00N 0.9500 . ?
C00O H00K 0.9800 . ?
C00O H00L 0.9800 . ?
C00O H00M 0.9800 . ?
C00Q C00S 1.529(5) . ?
C00Q H00O 0.9900 . ?
C00Q H00P 0.9900 . ?
C00R H00Q 0.9800 . ?
C00R H00R 0.9800 . ?
C00R H00S 0.9800 . ?
C00S H00T 0.9800 . ?
C00S H00U 0.9800 . ?
C00S H00V 0.9800 . ?
C00T C00U 1.346(7) . ?
C00T H00W 0.9500 . ?
C00U C00V 1.401(6) . ?
C00U H00X 0.9500 . ?
C00V H00Y 0.9500 . ?
C00W H00$ 0.9800 . ?
C00W H00 0.9800 . ?
C00W H002 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl06 Al07 Cl03 111.68(4) . . ?
Cl06 Al07 Cl02 110.14(4) . . ?
Cl03 Al07 Cl02 110.62(4) . . ?
Cl06 Al07 Cl01 109.07(4) . . ?
Cl03 Al07 Cl01 107.02(4) . . ?
Cl02 Al07 Cl01 108.19(4) . . ?
C00A N008 C00C 123.3(2) . . ?
C00A N008 B00P 111.68(18) . . ?
C00C N008 B00P 124.93(18) . . ?
C00B N009 C00E 122.00(19) . . ?
C00B N009 B00P 111.07(19) . . ?
C00E N009 B00P 126.68(19) . . ?
N008 C00A C00B 110.0(2) . . ?
N008 C00A H00A 125.0 . . ?
C00B C00A H00A 125.0 . . ?
N009 C00B C00A 110.99(19) . . ?
N009 C00B H00B 124.5 . . ?
C00A C00B H00B 124.5 . . ?
C00D C00C C00F 124.5(2) . . ?
C00D C00C N008 118.5(2) . . ?
C00F C00C N008 117.0(2) . . ?
C00C C00D C00I 116.0(3) . . ?
C00C C00D C00G 124.3(2) . . ?
C00I C00D C00G 119.5(2) . . ?
C00K C00E C00M 124.5(3) . . ?
C00K C00E N009 118.4(3) . . ?
C00M C00E N009 117.1(3) . . ?
C00J C00F C00C 115.9(3) . . ?
C00J C00F C00H 121.2(3) . . ?
C00C C00F C00H 122.7(2) . . ?
C00D C00G C00O 111.5(2) . . ?
C00D C00G H00C 109.3 . . ?
C00O C00G H00C 109.3 . . ?
C00D C00G H00D 109.3 . . ?
C00O C00G H00D 109.3 . . ?
H00C C00G H00D 108.0 . . ?
C00W C00H C00F 115.5(3) . . ?
C00W C00H H00E 108.4 . . ?
C00F C00H H00E 108.4 . . ?
C00W C00H H00F 108.4 . . ?
C00F C00H H00F 108.4 . . ?
H00E C00H H00F 107.5 . . ?
C00N C00I C00D 121.2(3) . . ?
C00N C00I H00I 119.4 . . ?
C00D C00I H00I 119.4 . . ?
C00N C00J C00F 121.2(3) . . ?
C00N C00J H00J 119.4 . . ?
C00F C00J H00J 119.4 . . ?
C00T C00K C00E 116.2(4) . . ?
C00T C00K C00Q 119.5(4) . . ?
C00E C00K C00Q 124.3(3) . . ?
C00M C00L C00R 112.2(3) . . ?
C00M C00L H00G 109.2 . . ?
C00R C00L H00G 109.2 . . ?
C00M C00L H00H 109.2 . . ?
C00R C00L H00H 109.2 . . ?
H00G C00L H00H 107.9 . . ?
C00E C00M C00V 116.1(4) . . ?
C00E C00M C00L 125.1(3) . . ?
C00V C00M C00L 118.7(4) . . ?
C00I C00N C00J 120.9(3) . . ?
C00I C00N H00N 119.5 . . ?
C00J C00N H00N 119.5 . . ?
C00G C00O H00K 109.5 . . ?
C00G C00O H00L 109.5 . . ?
H00K C00O H00L 109.5 . . ?
C00G C00O H00M 109.5 . . ?
H00K C00O H00M 109.5 . . ?
H00L C00O H00M 109.5 . . ?
N008 B00P N009 96.05(17) . . ?
N008 B00P Cl05 110.47(17) . . ?
N009 B00P Cl05 114.13(17) . . ?
N008 B00P Cl04 112.46(17) . . ?
N009 B00P Cl04 109.65(17) . . ?
Cl05 B00P Cl04 112.97(14) . . ?
C00K C00Q C00S 113.8(3) . . ?
C00K C00Q H00O 108.8 . . ?
C00S C00Q H00O 108.8 . . ?
C00K C00Q H00P 108.8 . . ?
C00S C00Q H00P 108.8 . . ?
H00O C00Q H00P 107.7 . . ?
C00L C00R H00Q 109.5 . . ?
C00L C00R H00R 109.5 . . ?
H00Q C00R H00R 109.5 . . ?
C00L C00R H00S 109.5 . . ?
H00Q C00R H00S 109.5 . . ?
H00R C00R H00S 109.5 . . ?
C00Q C00S H00T 109.5 . . ?
C00Q C00S H00U 109.5 . . ?
H00T C00S H00U 109.5 . . ?
C00Q C00S H00V 109.5 . . ?
H00T C00S H00V 109.5 . . ?
H00U C00S H00V 109.5 . . ?
C00U C00T C00K 121.3(4) . . ?
C00U C00T H00W 119.4 . . ?
C00K C00T H00W 119.4 . . ?
C00T C00U C00V 122.6(3) . . ?
C00T C00U H00X 118.7 . . ?
C00V C00U H00X 118.7 . . ?
C00U C00V C00M 119.2(5) . . ?
C00U C00V H00Y 120.4 . . ?
C00M C00V H00Y 120.4 . . ?
C00H C00W H00$ 109.5 . . ?
C00H C00W H00 109.5 . . ?
H00$ C00W H00 109.5 . . ?
C00H C00W H002 109.5 . . ?
H00$ C00W H002 109.5 . . ?
H00 C00W H002 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C00C N008 C00A C00B -176.1(2) . . . . ?
B00P N008 C00A C00B -0.1(3) . . . . ?
C00E N009 C00B C00A -179.3(2) . . . . ?
B00P N009 C00B C00A -4.7(3) . . . . ?
N008 C00A C00B N009 3.2(3) . . . . ?
C00A N008 C00C C00D -98.6(3) . . . . ?
B00P N008 C00C C00D 85.9(3) . . . . ?
C00A N008 C00C C00F 83.1(3) . . . . ?
B00P N008 C00C C00F -92.4(3) . . . . ?
C00F C00C C00D C00I 4.8(4) . . . . ?
N008 C00C C00D C00I -173.3(2) . . . . ?
C00F C00C C00D C00G -169.5(3) . . . . ?
N008 C00C C00D C00G 12.4(4) . . . . ?
C00B N009 C00E C00K -98.9(3) . . . . ?
B00P N009 C00E C00K 87.4(3) . . . . ?
C00B N009 C00E C00M 80.0(3) . . . . ?
B00P N009 C00E C00M -93.7(3) . . . . ?
C00D C00C C00F C00J -4.5(4) . . . . ?
N008 C00C C00F C00J 173.7(2) . . . . ?
C00D C00C C00F C00H 171.7(3) . . . . ?
N008 C00C C00F C00H -10.2(4) . . . . ?
C00C C00D C00G C00O 111.8(3) . . . . ?
C00I C00D C00G C00O -62.3(3) . . . . ?
C00J C00F C00H C00W -29.2(4) . . . . ?
C00C C00F C00H C00W 154.8(3) . . . . ?
C00C C00D C00I C00N -0.9(4) . . . . ?
C00G C00D C00I C00N 173.6(3) . . . . ?
C00C C00F C00J C00N 0.3(4) . . . . ?
C00H C00F C00J C00N -175.9(3) . . . . ?
C00M C00E C00K C00T 2.0(4) . . . . ?
N009 C00E C00K C00T -179.1(2) . . . . ?
C00M C00E C00K C00Q -175.3(3) . . . . ?
N009 C00E C00K C00Q 3.6(4) . . . . ?
C00K C00E C00M C00V -2.9(5) . . . . ?
N009 C00E C00M C00V 178.2(3) . . . . ?
C00K C00E C00M C00L 173.4(3) . . . . ?
N009 C00E C00M C00L -5.5(5) . . . . ?
C00R C00L C00M C00E -107.2(3) . . . . ?
C00R C00L C00M C00V 69.0(4) . . . . ?
C00D C00I C00N C00J -3.0(5) . . . . ?
C00F C00J C00N C00I 3.3(5) . . . . ?
C00A N008 B00P N009 -2.2(2) . . . . ?
C00C N008 B00P N009 173.7(2) . . . . ?
C00A N008 B00P Cl05 -120.83(18) . . . . ?
C00C N008 B00P Cl05 55.1(3) . . . . ?
C00A N008 B00P Cl04 111.94(19) . . . . ?
C00C N008 B00P Cl04 -72.1(3) . . . . ?
C00B N009 B00P N008 4.2(2) . . . . ?
C00E N009 B00P N008 178.5(2) . . . . ?
C00B N009 B00P Cl05 119.9(2) . . . . ?
C00E N009 B00P Cl05 -65.9(3) . . . . ?
C00B N009 B00P Cl04 -112.3(2) . . . . ?
C00E N009 B00P Cl04 62.0(3) . . . . ?
C00T C00K C00Q C00S 57.5(4) . . . . ?
C00E C00K C00Q C00S -125.2(3) . . . . ?
C00E C00K C00T C00U -0.1(5) . . . . ?
C00Q C00K C00T C00U 177.4(3) . . . . ?
C00K C00T C00U C00V -0.8(6) . . . . ?
C00T C00U C00V C00M -0.2(5) . . . . ?
C00E C00M C00V C00U 1.9(5) . . . . ?
C00L C00M C00V C00U -174.6(3) . . . . ?

_refine_diff_density_max         1.352
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.069

_shelxl_version_number           2013-3



