# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_I
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H48 Al B Cl6 N3 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         744.18

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.9720(10)
_cell_length_b                   14.1620(12)
_cell_length_c                   18.7531(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.050(5)
_cell_angle_gamma                90
_cell_volume                     3926.8(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560

_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
;
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_T_max  0.91

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            50162
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_full        29.22
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25

_refine_special_details          
;
;

_reflns_number_total             10588
_reflns_number_gt                7691
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1364
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_number_reflns         10588
_refine_ls_number_parameters     400
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0740P)²+0.8082P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.619
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al1 0.74850(4) 0.68969(5) 0.77218(4) 0.02269(15) Uani d . . . 1 . .
B B1 0.35068(15) 0.82197(17) 0.61070(12) 0.0194(5) Uani d . . . 1 . .
C C1 0.28867(12) 0.76706(14) 0.54774(10) 0.0150(4) Uani d . . . 1 . .
C C2 0.36617(12) 0.81815(14) 0.44805(10) 0.0158(4) Uani d . . . 1 . .
C C3 0.44015(13) 0.77428(15) 0.42402(11) 0.0181(4) Uani d . . . 1 . .
C C4 0.45469(14) 0.66844(15) 0.42773(12) 0.0228(4) Uani d . . . 1 . .
H H4 0.4048 0.64 0.4503 0.027 Uiso calc U . R 1 . .
C C5 0.54431(16) 0.64189(18) 0.47438(13) 0.0322(5) Uani d . . . 1 . .
H H5A 0.5945 0.6692 0.4535 0.048 Uiso calc U . R 1 . .
H H5B 0.5504 0.573 0.4762 0.048 Uiso calc U . R 1 . .
H H5C 0.5455 0.6665 0.5234 0.048 Uiso calc U . R 1 . .
C C6 0.44917(17) 0.62711(18) 0.35189(13) 0.0329(5) Uani d . . . 1 . .
H H6A 0.3903 0.6425 0.3235 0.049 Uiso calc U . R 1 . .
H H6B 0.4562 0.5584 0.3551 0.049 Uiso calc U . R 1 . .
H H6C 0.4975 0.6539 0.3284 0.049 Uiso calc U . R 1 . .
C C7 0.50065(13) 0.83230(16) 0.39483(11) 0.0223(4) Uani d . . . 1 . .
H H7 0.552 0.8051 0.3788 0.027 Uiso calc U . R 1 . .
C C8 0.48711(14) 0.92849(16) 0.38892(12) 0.0249(5) Uani d . . . 1 . .
H H8 0.529 0.9667 0.3687 0.03 Uiso calc U . R 1 . .
C C9 0.41297(14) 0.96990(16) 0.41219(12) 0.0245(5) Uani d . . . 1 . .
H H9 0.4047 1.0363 0.4078 0.029 Uiso calc U . R 1 . .
C C10 0.35003(13) 0.91563(14) 0.44204(10) 0.0181(4) Uani d . . . 1 . .
C C11 0.26452(14) 0.96262(15) 0.45960(11) 0.0217(4) Uani d . . . 1 . .
H H11 0.2368 0.919 0.4919 0.026 Uiso calc U . R 1 . .
C C12 0.28294(16) 1.05693(17) 0.49931(14) 0.0319(5) Uani d . . . 1 . .
H H12A 0.3311 1.0486 0.5407 0.048 Uiso calc U . R 1 . .
H H12B 0.2278 1.0785 0.5163 0.048 Uiso calc U . R 1 . .
H H12C 0.3017 1.104 0.4663 0.048 Uiso calc U . R 1 . .
C C13 0.19688(15) 0.97525(17) 0.39035(12) 0.0292(5) Uani d . . . 1 . .
H H13A 0.2224 1.0178 0.3576 0.044 Uiso calc U . R 1 . .
H H13B 0.1407 1.0023 0.4021 0.044 Uiso calc U . R 1 . .
H H13C 0.1841 0.9138 0.367 0.044 Uiso calc U . R 1 . .
C C14 0.15662(12) 0.69881(14) 0.60071(10) 0.0154(4) Uani d . . . 1 . .
C C15 0.06730(13) 0.73162(16) 0.59822(11) 0.0203(4) Uani d . . . 1 . .
C C16 0.02766(14) 0.81028(18) 0.54842(12) 0.0276(5) Uani d . . . 1 . .
H H16 0.0659 0.8161 0.5094 0.033 Uiso calc U . R 1 . .
C C17 0.0336(2) 0.9036(2) 0.58891(17) 0.0532(8) Uani d . . . 1 . .
H H17A -0.0032 0.9003 0.6277 0.08 Uiso calc U . R 1 . .
H H17B 0.0111 0.9545 0.5555 0.08 Uiso calc U . R 1 . .
H H17C 0.0967 0.9162 0.6097 0.08 Uiso calc U . R 1 . .
C C18 -0.0681(2) 0.7913(2) 0.5122(2) 0.0598(10) Uani d . . . 1 . .
H H18A -0.0703 0.7314 0.4859 0.09 Uiso calc U . R 1 . .
H H18B -0.0883 0.8427 0.4785 0.09 Uiso calc U . R 1 . .
H H18C -0.108 0.7877 0.5489 0.09 Uiso calc U . R 1 . .
C C19 0.01687(14) 0.69247(18) 0.64748(12) 0.0271(5) Uani d . . . 1 . .
H H19 -0.0435 0.7132 0.6475 0.033 Uiso calc U . R 1 . .
C C20 0.05294(15) 0.62449(18) 0.69605(12) 0.0290(5) Uani d . . . 1 . .
H H20 0.0168 0.5975 0.7281 0.035 Uiso calc U . R 1 . .
C C21 0.14117(15) 0.59525(16) 0.69853(11) 0.0234(4) Uani d . . . 1 . .
H H21 0.1651 0.5489 0.7329 0.028 Uiso calc U . R 1 . .
C C22 0.19608(13) 0.63218(14) 0.65172(10) 0.0179(4) Uani d . . . 1 . .
C C23 0.29455(14) 0.60233(16) 0.66126(11) 0.0215(4) Uani d . . . 1 . .
H H23 0.3214 0.6281 0.6197 0.026 Uiso calc U . R 1 . .
C C24 0.30703(17) 0.49499(18) 0.66233(13) 0.0341(6) Uani d . . . 1 . .
H H24A 0.2824 0.4683 0.7034 0.051 Uiso calc U . R 1 . .
H H24B 0.3716 0.48 0.667 0.051 Uiso calc U . R 1 . .
H H24C 0.2751 0.468 0.6173 0.051 Uiso calc U . R 1 . .
C C25 0.34562(15) 0.64564(18) 0.73096(12) 0.0292(5) Uani d . . . 1 . .
H H25A 0.3355 0.714 0.7306 0.044 Uiso calc U . R 1 . .
H H25B 0.4105 0.6329 0.7341 0.044 Uiso calc U . R 1 . .
H H25C 0.3235 0.6177 0.7727 0.044 Uiso calc U . R 1 . .
C C26 0.20322(14) 0.53793(15) 0.46279(11) 0.0215(4) Uani d . . . 1 . .
H H26 0.2466 0.5595 0.5057 0.026 Uiso calc U . R 1 . .
C C27 0.25546(16) 0.47608(17) 0.41723(13) 0.0309(5) Uani d . . . 1 . .
H H27A 0.2139 0.451 0.376 0.046 Uiso calc U . R 1 . .
H H27B 0.2836 0.4236 0.4467 0.046 Uiso calc U . R 1 . .
H H27C 0.3025 0.5138 0.3998 0.046 Uiso calc U . R 1 . .
C C28 0.12772(16) 0.48329(17) 0.49065(13) 0.0312(5) Uani d . . . 1 . .
H H28A 0.097 0.5248 0.5209 0.047 Uiso calc U . R 1 . .
H H28B 0.1536 0.4292 0.5193 0.047 Uiso calc U . R 1 . .
H H28C 0.0841 0.4608 0.4497 0.047 Uiso calc U . R 1 . .
C C29 0.10628(15) 0.60948(16) 0.35082(12) 0.0252(5) Uani d . . . 1 . .
H H29 0.0996 0.5399 0.3425 0.03 Uiso calc U . R 1 . .
C C30 0.01204(16) 0.6499(2) 0.34978(16) 0.0423(7) Uani d . . . 1 . .
H H30A -0.0149 0.6225 0.3894 0.063 Uiso calc U . R 1 . .
H H30B -0.0257 0.6347 0.3036 0.063 Uiso calc U . R 1 . .
H H30C 0.016 0.7186 0.3557 0.063 Uiso calc U . R 1 . .
C C31 0.15274(19) 0.64970(19) 0.29089(12) 0.0360(6) Uani d . . . 1 . .
H H31A 0.1558 0.7186 0.2951 0.054 Uiso calc U . R 1 . .
H H31B 0.1183 0.6324 0.2439 0.054 Uiso calc U . R 1 . .
H H31C 0.2141 0.624 0.2951 0.054 Uiso calc U . R 1 . .
Cl Cl1 0.46473(3) 0.79841(4) 0.62745(3) 0.02769(13) Uani d . . . 1 . .
Cl Cl2 0.30119(4) 0.90439(4) 0.65842(3) 0.03015(14) Uani d . . . 1 . .
Cl Cl3 0.62264(4) 0.62330(5) 0.73267(4) 0.03905(16) Uani d . . . 1 . .
Cl Cl4 0.74037(4) 0.75664(4) 0.87258(3) 0.03006(13) Uani d . . . 1 . .
Cl Cl5 0.85264(4) 0.58504(4) 0.78944(4) 0.03476(15) Uani d . . . 1 . .
Cl Cl6 0.78175(5) 0.78963(5) 0.69555(4) 0.0504(2) Uani d . . . 1 . .
N N1 0.20603(10) 0.73013(12) 0.54555(8) 0.0155(3) Uani d . . . 1 . .
N N2 0.30433(10) 0.75870(12) 0.47930(9) 0.0151(3) Uani d . . . 1 . .
N N3 0.16514(11) 0.62363(12) 0.42329(9) 0.0180(3) Uani d . . . 1 . .
P P1 0.18324(3) 0.73180(4) 0.44910(3) 0.01525(11) Uani d . . . 1 . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 Cl4 . 2.1287(9) ?
Al1 Cl6 . 2.1310(9) ?
Al1 Cl3 . 2.1318(9) ?
Al1 Cl5 . 2.1387(8) ?
B1 C1 . 1.586(3) ?
B1 Cl2 . 1.709(2) ?
B1 Cl1 . 1.720(2) ?
C1 N1 . 1.338(2) ?
C1 N2 . 1.346(2) ?
C1 P1 . 2.290(2) ?
C2 C10 . 1.403(3) ?
C2 C3 . 1.405(3) ?
C2 N2 . 1.442(2) ?
C3 C7 . 1.397(3) ?
C3 C4 . 1.515(3) ?
C4 C6 . 1.528(3) ?
C4 C5 . 1.529(3) ?
C4 H4 . 1.0 ?
C5 H5A . 0.98 ?
C5 H5B . 0.98 ?
C5 H5C . 0.98 ?
C6 H6A . 0.98 ?
C6 H6B . 0.98 ?
C6 H6C . 0.98 ?
C7 C8 . 1.379(3) ?
C7 H7 . 0.95 ?
C8 C9 . 1.385(3) ?
C8 H8 . 0.95 ?
C9 C10 . 1.399(3) ?
C9 H9 . 0.95 ?
C10 C11 . 1.524(3) ?
C11 C13 . 1.526(3) ?
C11 C12 . 1.533(3) ?
C11 H11 . 1.0 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C14 C22 . 1.406(3) ?
C14 C15 . 1.409(3) ?
C14 N1 . 1.434(2) ?
C15 C19 . 1.397(3) ?
C15 C16 . 1.514(3) ?
C16 C18 . 1.511(3) ?
C16 C17 . 1.520(4) ?
C16 H16 . 1.0 ?
C17 H17A . 0.98 ?
C17 H17B . 0.98 ?
C17 H17C . 0.98 ?
C18 H18A . 0.98 ?
C18 H18B . 0.98 ?
C18 H18C . 0.98 ?
C19 C20 . 1.376(3) ?
C19 H19 . 0.95 ?
C20 C21 . 1.378(3) ?
C20 H20 . 0.95 ?
C21 C22 . 1.395(3) ?
C21 H21 . 0.95 ?
C22 C23 . 1.517(3) ?
C23 C24 . 1.531(3) ?
C23 C25 . 1.535(3) ?
C23 H23 . 1.0 ?
C24 H24A . 0.98 ?
C24 H24B . 0.98 ?
C24 H24C . 0.98 ?
C25 H25A . 0.98 ?
C25 H25B . 0.98 ?
C25 H25C . 0.98 ?
C26 N3 . 1.488(3) ?
C26 C27 . 1.523(3) ?
C26 C28 . 1.528(3) ?
C26 H26 . 1.0 ?
C27 H27A . 0.98 ?
C27 H27B . 0.98 ?
C27 H27C . 0.98 ?
C28 H28A . 0.98 ?
C28 H28B . 0.98 ?
C28 H28C . 0.98 ?
C29 N3 . 1.512(3) ?
C29 C30 . 1.520(3) ?
C29 C31 . 1.522(3) ?
C29 H29 . 1.0 ?
C30 H30A . 0.98 ?
C30 H30B . 0.98 ?
C30 H30C . 0.98 ?
C31 H31A . 0.98 ?
C31 H31B . 0.98 ?
C31 H31C . 0.98 ?
N1 P1 . 1.7873(17) ?
N2 P1 . 1.8520(16) ?
N3 P1 . 1.6164(18) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl4 Al1 Cl6 . . 110.65(4) ?
Cl4 Al1 Cl3 . . 109.48(3) ?
Cl6 Al1 Cl3 . . 110.25(4) ?
Cl4 Al1 Cl5 . . 108.45(4) ?
Cl6 Al1 Cl5 . . 108.67(4) ?
Cl3 Al1 Cl5 . . 109.30(4) ?
C1 B1 Cl2 . . 118.26(15) ?
C1 B1 Cl1 . . 119.28(16) ?
Cl2 B1 Cl1 . . 122.46(14) ?
N1 C1 N2 . . 103.62(16) ?
N1 C1 B1 . . 130.14(16) ?
N2 C1 B1 . . 125.71(17) ?
N1 C1 P1 . . 51.20(10) ?
N2 C1 P1 . . 53.97(10) ?
B1 C1 P1 . . 163.05(14) ?
C10 C2 C3 . . 122.96(17) ?
C10 C2 N2 . . 119.58(16) ?
C3 C2 N2 . . 117.46(17) ?
C7 C3 C2 . . 117.26(19) ?
C7 C3 C4 . . 120.19(17) ?
C2 C3 C4 . . 122.54(17) ?
C3 C4 C6 . . 110.48(18) ?
C3 C4 C5 . . 112.12(18) ?
C6 C4 C5 . . 110.63(18) ?
C3 C4 H4 . . 107.8 ?
C6 C4 H4 . . 107.8 ?
C5 C4 H4 . . 107.8 ?
C4 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
C4 C6 H6A . . 109.5 ?
C4 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C4 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
C8 C7 C3 . . 121.09(19) ?
C8 C7 H7 . . 119.5 ?
C3 C7 H7 . . 119.5 ?
C7 C8 C9 . . 120.51(19) ?
C7 C8 H8 . . 119.7 ?
C9 C8 H8 . . 119.7 ?
C8 C9 C10 . . 121.1(2) ?
C8 C9 H9 . . 119.4 ?
C10 C9 H9 . . 119.4 ?
C9 C10 C2 . . 117.02(18) ?
C9 C10 C11 . . 119.21(19) ?
C2 C10 C11 . . 123.52(17) ?
C10 C11 C13 . . 109.56(17) ?
C10 C11 C12 . . 113.10(18) ?
C13 C11 C12 . . 110.84(18) ?
C10 C11 H11 . . 107.7 ?
C13 C11 H11 . . 107.7 ?
C12 C11 H11 . . 107.7 ?
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 ?
C22 C14 C15 . . 122.60(17) ?
C22 C14 N1 . . 119.29(16) ?
C15 C14 N1 . . 117.95(18) ?
C19 C15 C14 . . 117.1(2) ?
C19 C15 C16 . . 119.99(18) ?
C14 C15 C16 . . 122.76(18) ?
C18 C16 C15 . . 113.5(2) ?
C18 C16 C17 . . 110.8(2) ?
C15 C16 C17 . . 110.20(19) ?
C18 C16 H16 . . 107.3 ?
C15 C16 H16 . . 107.3 ?
C17 C16 H16 . . 107.3 ?
C16 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C16 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C16 C18 H18A . . 109.5 ?
C16 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C16 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C20 C19 C15 . . 121.3(2) ?
C20 C19 H19 . . 119.4 ?
C15 C19 H19 . . 119.4 ?
C19 C20 C21 . . 120.5(2) ?
C19 C20 H20 . . 119.8 ?
C21 C20 H20 . . 119.8 ?
C20 C21 C22 . . 121.5(2) ?
C20 C21 H21 . . 119.2 ?
C22 C21 H21 . . 119.2 ?
C21 C22 C14 . . 116.96(18) ?
C21 C22 C23 . . 118.64(18) ?
C14 C22 C23 . . 124.32(17) ?
C22 C23 C24 . . 113.11(19) ?
C22 C23 C25 . . 109.50(17) ?
C24 C23 C25 . . 110.01(18) ?
C22 C23 H23 . . 108.0 ?
C24 C23 H23 . . 108.0 ?
C25 C23 H23 . . 108.0 ?
C23 C24 H24A . . 109.5 ?
C23 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C23 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C23 C25 H25A . . 109.5 ?
C23 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
C23 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
N3 C26 C27 . . 112.35(17) ?
N3 C26 C28 . . 109.70(17) ?
C27 C26 C28 . . 111.92(19) ?
N3 C26 H26 . . 107.5 ?
C27 C26 H26 . . 107.5 ?
C28 C26 H26 . . 107.5 ?
C26 C27 H27A . . 109.5 ?
C26 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C26 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
C26 C28 H28A . . 109.5 ?
C26 C28 H28B . . 109.5 ?
H28A C28 H28B . . 109.5 ?
C26 C28 H28C . . 109.5 ?
H28A C28 H28C . . 109.5 ?
H28B C28 H28C . . 109.5 ?
N3 C29 C30 . . 111.72(19) ?
N3 C29 C31 . . 110.15(18) ?
C30 C29 C31 . . 112.4(2) ?
N3 C29 H29 . . 107.4 ?
C30 C29 H29 . . 107.4 ?
C31 C29 H29 . . 107.4 ?
C29 C30 H30A . . 109.5 ?
C29 C30 H30B . . 109.5 ?
H30A C30 H30B . . 109.5 ?
C29 C30 H30C . . 109.5 ?
H30A C30 H30C . . 109.5 ?
H30B C30 H30C . . 109.5 ?
C29 C31 H31A . . 109.5 ?
C29 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C29 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C1 N1 C14 . . 132.73(17) ?
C1 N1 P1 . . 93.11(12) ?
C14 N1 P1 . . 134.13(13) ?
C1 N2 C2 . . 123.74(17) ?
C1 N2 P1 . . 90.04(11) ?
C2 N2 P1 . . 130.99(13) ?
C26 N3 C29 . . 117.56(17) ?
C26 N3 P1 . . 126.22(14) ?
C29 N3 P1 . . 116.18(14) ?
N3 P1 N1 . . 106.66(8) ?
N3 P1 N2 . . 113.36(8) ?
N1 P1 N2 . . 70.81(7) ?
N3 P1 C1 . . 120.68(8) ?
N1 P1 C1 . . 35.69(7) ?
N2 P1 C1 . . 35.99(7) ?

_database_code_depnum_ccdc_archive 'CCDC 986260'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dv13

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34.36 H54.29 B Cl3 N3 P'
_chemical_formula_weight         657.52

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.314(4)
_cell_length_b                   18.597(10)
_cell_length_c                   19.160(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.535(19)
_cell_angle_gamma                90.00
_cell_volume                     3624(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    3752
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      24.15

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1410
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_T_max  0.9380
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41400
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_av_sigmaI/netI    0.1216
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         28.01
_reflns_number_total             8489
_reflns_number_gt                5003
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1153P)²+0.3188P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8489
_refine_ls_number_parameters     430
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.1440
_refine_ls_R_factor_gt           0.0797
_refine_ls_wR_factor_ref         0.2370
_refine_ls_wR_factor_gt          0.1909
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B -0.1943(4) 0.2564(3) 0.2764(2) 0.0244(10) Uani 1 1 d . . .
C1 C -0.0411(4) 0.2308(2) 0.29572(18) 0.0182(8) Uani 1 1 d . . .
C2 C 0.0523(4) 0.2927(2) 0.41439(18) 0.0198(8) Uani 1 1 d . . .
C3 C 0.0752(4) 0.3666(2) 0.42023(19) 0.0235(9) Uani 1 1 d . . .
C4 C 0.0807(4) 0.4167(2) 0.3576(2) 0.0273(9) Uani 1 1 d . . .
H4 H 0.0952 0.3872 0.3160 0.033 Uiso 1 1 calc R . .
C5 C 0.1919(5) 0.4724(2) 0.3735(2) 0.0389(11) Uani 1 1 d . . .
H5A H 0.1653 0.5106 0.4035 0.058 Uiso 1 1 calc R . .
H5B H 0.2096 0.4932 0.3291 0.058 Uiso 1 1 calc R . .
H5C H 0.2715 0.4489 0.3982 0.058 Uiso 1 1 calc R . .
C6 C -0.0513(4) 0.4561(2) 0.3392(2) 0.0366(11) Uani 1 1 d . . .
H6A H -0.1227 0.4208 0.3302 0.055 Uiso 1 1 calc R . .
H6B H -0.0511 0.4854 0.2967 0.055 Uiso 1 1 calc R . .
H6C H -0.0644 0.4871 0.3787 0.055 Uiso 1 1 calc R . .
C7 C 0.0822(4) 0.3981(2) 0.4873(2) 0.0304(10) Uani 1 1 d . . .
H7 H 0.0961 0.4485 0.4921 0.036 Uiso 1 1 calc R . .
C8 C 0.0695(5) 0.3582(2) 0.5464(2) 0.0340(11) Uani 1 1 d . . .
H8 H 0.0781 0.3805 0.5915 0.041 Uiso 1 1 calc R . .
C9 C 0.0446(4) 0.2863(2) 0.5393(2) 0.0286(10) Uani 1 1 d . . .
H9 H 0.0338 0.2592 0.5800 0.034 Uiso 1 1 calc R . .
C10 C 0.0344(4) 0.2514(2) 0.47421(19) 0.0216(9) Uani 1 1 d . . .
C11 C 0.0010(4) 0.1726(2) 0.4709(2) 0.0275(10) Uani 1 1 d . . .
H11 H -0.0132 0.1580 0.4200 0.033 Uiso 1 1 calc R . .
C12 C 0.1140(5) 0.1271(2) 0.5100(2) 0.0377(11) Uani 1 1 d . . .
H12A H 0.1953 0.1387 0.4922 0.057 Uiso 1 1 calc R . .
H12B H 0.0936 0.0760 0.5020 0.057 Uiso 1 1 calc R . .
H12C H 0.1254 0.1374 0.5608 0.057 Uiso 1 1 calc R . .
C13 C -0.1271(5) 0.1571(3) 0.4995(2) 0.0396(11) Uani 1 1 d . . .
H13A H -0.1127 0.1651 0.5508 0.059 Uiso 1 1 calc R . .
H13B H -0.1534 0.1071 0.4894 0.059 Uiso 1 1 calc R . .
H13C H -0.1966 0.1893 0.4767 0.059 Uiso 1 1 calc R . .
C14 C -0.0222(4) 0.1250(2) 0.21224(19) 0.0213(9) Uani 1 1 d . . .
C15 C -0.0235(4) 0.1349(2) 0.13942(19) 0.0259(9) Uani 1 1 d . . .
C16 C 0.0170(4) 0.2040(2) 0.1072(2) 0.0297(10) Uani 1 1 d . . .
H16 H 0.0571 0.2367 0.1463 0.036 Uiso 1 1 calc R . .
C17 C -0.1045(5) 0.2415(3) 0.0649(2) 0.0377(11) Uani 1 1 d . . .
H17A H -0.1414 0.2115 0.0245 0.056 Uiso 1 1 calc R . .
H17B H -0.0786 0.2882 0.0479 0.056 Uiso 1 1 calc R . .
H17C H -0.1707 0.2487 0.0955 0.056 Uiso 1 1 calc R . .
C18 C 0.1178(5) 0.1908(3) 0.0583(2) 0.0431(12) Uani 1 1 d . . .
H18A H 0.1922 0.1636 0.0838 0.065 Uiso 1 1 calc R . .
H18B H 0.1490 0.2370 0.0430 0.065 Uiso 1 1 calc R . .
H18C H 0.0767 0.1634 0.0168 0.065 Uiso 1 1 calc R . .
C19 C -0.0664(4) 0.0774(3) 0.0943(2) 0.0331(11) Uani 1 1 d . . .
H19 H -0.0690 0.0830 0.0448 0.040 Uiso 1 1 calc R . .
C20 C -0.1048(5) 0.0133(3) 0.1194(2) 0.0364(11) Uani 1 1 d . . .
H20 H -0.1347 -0.0247 0.0876 0.044 Uiso 1 1 calc R . .
C21 C -0.0995(4) 0.0043(2) 0.1916(2) 0.0266(9) Uani 1 1 d . . .
H21 H -0.1247 -0.0406 0.2089 0.032 Uiso 1 1 calc R . .
C22 C -0.0582(4) 0.0594(2) 0.23933(19) 0.0230(9) Uani 1 1 d . . .
C23 C -0.0551(4) 0.0446(2) 0.3175(2) 0.0253(9) Uani 1 1 d . . .
H23 H -0.0280 0.0900 0.3439 0.030 Uiso 1 1 calc R . .
C24 C 0.0469(5) -0.0134(3) 0.3445(2) 0.0495(14) Uani 1 1 d . . .
H24A H 0.0200 -0.0594 0.3215 0.074 Uiso 1 1 calc R . .
H24B H 0.0530 -0.0186 0.3959 0.074 Uiso 1 1 calc R . .
H24C H 0.1328 0.0006 0.3335 0.074 Uiso 1 1 calc RD . .
C25 C -0.1904(4) 0.0227(3) 0.3344(2) 0.0368(11) Uani 1 1 d . . .
H25A H -0.2551 0.0599 0.3172 0.055 Uiso 1 1 calc R . .
H25B H -0.1848 0.0172 0.3857 0.055 Uiso 1 1 calc R . .
H25C H -0.2175 -0.0231 0.3110 0.055 Uiso 1 1 calc R . .
C26 C 0.2947(4) 0.2872(2) 0.2652(2) 0.0265(9) Uani 1 1 d . . .
H26 H 0.2023 0.3054 0.2538 0.032 Uiso 1 1 calc R . .
C27 C 0.3748(4) 0.3421(2) 0.3137(2) 0.0350(11) Uani 1 1 d . . .
H27A H 0.3432 0.3435 0.3592 0.052 Uiso 1 1 calc R . .
H27B H 0.3648 0.3898 0.2917 0.052 Uiso 1 1 calc R . .
H27C H 0.4677 0.3283 0.3215 0.052 Uiso 1 1 calc R . .
C28 C 0.3466(4) 0.2787(3) 0.1960(2) 0.0384(12) Uani 1 1 d . . .
H28A H 0.4424 0.2731 0.2059 0.058 Uiso 1 1 calc R . .
H28B H 0.3239 0.3213 0.1665 0.058 Uiso 1 1 calc R . .
H28C H 0.3071 0.2360 0.1710 0.058 Uiso 1 1 calc R . .
C29 C 0.4199(4) 0.1773(2) 0.3206(2) 0.0235(9) Uani 1 1 d . . .
H29 H 0.4879 0.2065 0.3018 0.028 Uiso 1 1 calc R . .
C30 C 0.4651(4) 0.1698(2) 0.3996(2) 0.0312(10) Uani 1 1 d . . .
H30A H 0.4725 0.2176 0.4215 0.047 Uiso 1 1 calc R . .
H30B H 0.5510 0.1459 0.4084 0.047 Uiso 1 1 calc R . .
H30C H 0.4012 0.1411 0.4201 0.047 Uiso 1 1 calc R . .
C31 C 0.4095(4) 0.1063(3) 0.2816(2) 0.0388(12) Uani 1 1 d . . .
H31A H 0.3483 0.0747 0.3010 0.058 Uiso 1 1 calc R . .
H31B H 0.4963 0.0835 0.2873 0.058 Uiso 1 1 calc R . .
H31C H 0.3773 0.1146 0.2312 0.058 Uiso 1 1 calc R . .
C32 C 0.5853(9) 0.0905(5) 0.6433(5) 0.051(2) Uani 0.644(9) 1 d PDU A 1
H32A H 0.6582 0.0588 0.6629 0.076 Uiso 0.644(9) 1 calc PR A 1
H32B H 0.5406 0.1075 0.6815 0.076 Uiso 0.644(9) 1 calc PR A 1
H32C H 0.6194 0.1317 0.6201 0.076 Uiso 0.644(9) 1 calc PR A 1
C33 C 0.4868(8) 0.0485(4) 0.5885(4) 0.039(2) Uani 0.644(9) 1 d PDU A 1
H33A H 0.4506 0.0078 0.6125 0.047 Uiso 0.644(9) 1 calc PR A 1
H33B H 0.4129 0.0806 0.5692 0.047 Uiso 0.644(9) 1 calc PR A 1
C34 C 0.5503(9) 0.0199(5) 0.5280(4) 0.0296(19) Uani 0.644(9) 1 d PDU . 1
H34A H 0.6221 -0.0136 0.5471 0.035 Uiso 0.644(9) 1 calc PR A 1
H34B H 0.5893 0.0604 0.5052 0.035 Uiso 0.644(9) 1 calc PR A 1
C35 C 0.6278(17) 0.0741(10) 0.6085(10) 0.055(4) Uani 0.356(9) 1 d PU A 2
H35A H 0.5811 0.1190 0.6143 0.082 Uiso 0.356(9) 1 calc PR A 2
H35B H 0.7159 0.0850 0.5986 0.082 Uiso 0.356(9) 1 calc PRD A 2
H35C H 0.6351 0.0457 0.6521 0.082 Uiso 0.356(9) 1 calc PRD A 2
C36 C 0.5639(19) 0.0381(10) 0.5569(9) 0.038(4) Uani 0.356(9) 1 d PU A 2
C37 C 0.6325(13) 0.0046(6) 0.5084(7) 0.033(3) Uani 0.356(9) 1 d PU . 2
H37 H 0.7254 0.0089 0.5138 0.039 Uiso 0.356(9) 1 calc PR A 2
C38 C 0.4340(13) 0.0340(7) 0.5462(7) 0.032(3) Uani 0.356(9) 1 d PU . 2
H38 H 0.3864 0.0584 0.5774 0.039 Uiso 0.356(9) 1 calc PR A 2
Cl1 Cl -0.19297(11) 0.33223(6) 0.21402(5) 0.0364(3) Uani 1 1 d . . .
Cl2 Cl -0.29886(9) 0.18389(6) 0.23249(5) 0.0305(3) Uani 1 1 d . . .
Cl3 Cl -0.25639(9) 0.28615(6) 0.35702(5) 0.0295(3) Uani 1 1 d . . .
N1 N 0.0567(3) 0.25501(17) 0.34771(15) 0.0183(7) Uani 1 1 d . . .
N2 N 0.0243(3) 0.18352(17) 0.26128(15) 0.0184(7) Uani 1 1 d . . .
N3 N 0.2924(3) 0.21790(18) 0.30393(16) 0.0218(7) Uani 1 1 d . . .
P1 P 0.16508(9) 0.18357(6) 0.33182(5) 0.0187(2) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C1 1.633(6) . ?
B1 Cl2 1.841(5) . ?
B1 Cl1 1.850(5) . ?
B1 Cl3 1.852(5) . ?
C1 N2 1.345(5) . ?
C1 N1 1.372(5) . ?
C1 P1 2.299(4) . ?
C2 C3 1.397(6) . ?
C2 C10 1.417(5) . ?
C2 N1 1.464(4) . ?
C3 C7 1.403(5) . ?
C3 C4 1.527(5) . ?
C4 C6 1.535(6) . ?
C4 C5 1.538(6) . ?
C7 C8 1.378(6) . ?
C8 C9 1.365(6) . ?
C9 C10 1.394(5) . ?
C10 C11 1.503(6) . ?
C11 C12 1.533(6) . ?
C11 C13 1.539(6) . ?
C14 C22 1.400(6) . ?
C14 C15 1.405(5) . ?
C14 N2 1.466(5) . ?
C15 C19 1.401(6) . ?
C15 C16 1.514(6) . ?
C16 C18 1.530(6) . ?
C16 C17 1.541(6) . ?
C19 C20 1.368(6) . ?
C20 C21 1.386(5) . ?
C21 C22 1.392(5) . ?
C22 C23 1.519(5) . ?
C23 C24 1.535(6) . ?
C23 C25 1.539(6) . ?
C26 N3 1.490(5) . ?
C26 C28 1.518(5) . ?
C26 C27 1.528(6) . ?
C29 N3 1.504(5) . ?
C29 C31 1.512(6) . ?
C29 C30 1.516(5) . ?
C32 C33 1.545(10) . ?
C33 C34 1.519(9) . ?
C34 C34 1.551(17) 3_656 ?
C35 C36 1.28(2) . ?
C36 C38 1.32(2) . ?
C36 C37 1.40(2) . ?
C37 C38 1.357(19) 3_656 ?
C38 C37 1.357(19) 3_656 ?
N1 P1 1.794(3) . ?
N2 P1 1.813(3) . ?
N3 P1 1.628(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
C1 B1 Cl2 111.2(3) . . ?
C1 B1 Cl1 105.0(3) . . ?
Cl2 B1 Cl1 109.3(2) . . ?
C1 B1 Cl3 110.7(3) . . ?
Cl2 B1 Cl3 110.1(2) . . ?
Cl1 B1 Cl3 110.6(3) . . ?
N2 C1 N1 101.7(3) . . ?
N2 C1 B1 128.6(3) . . ?
N1 C1 B1 129.5(3) . . ?
N2 C1 P1 51.99(18) . . ?
N1 C1 P1 51.26(18) . . ?
B1 C1 P1 172.7(3) . . ?
C3 C2 C10 120.8(3) . . ?
C3 C2 N1 120.8(3) . . ?
C10 C2 N1 118.3(3) . . ?
C2 C3 C7 117.8(3) . . ?
C2 C3 C4 124.4(3) . . ?
C7 C3 C4 117.5(4) . . ?
C3 C4 C6 109.0(3) . . ?
C3 C4 C5 112.2(3) . . ?
C6 C4 C5 109.1(4) . . ?
C8 C7 C3 122.0(4) . . ?
C9 C8 C7 119.2(4) . . ?
C8 C9 C10 122.0(4) . . ?
C9 C10 C2 118.1(4) . . ?
C9 C10 C11 118.3(3) . . ?
C2 C10 C11 123.6(3) . . ?
C10 C11 C12 111.5(4) . . ?
C10 C11 C13 111.8(3) . . ?
C12 C11 C13 110.5(3) . . ?
C22 C14 C15 121.5(4) . . ?
C22 C14 N2 119.2(3) . . ?
C15 C14 N2 119.2(3) . . ?
C19 C15 C14 117.5(4) . . ?
C19 C15 C16 118.5(3) . . ?
C14 C15 C16 124.0(4) . . ?
C15 C16 C18 112.0(4) . . ?
C15 C16 C17 110.1(4) . . ?
C18 C16 C17 109.1(3) . . ?
C20 C19 C15 122.0(4) . . ?
C19 C20 C21 119.3(4) . . ?
C20 C21 C22 121.7(4) . . ?
C21 C22 C14 117.9(3) . . ?
C21 C22 C23 118.0(4) . . ?
C14 C22 C23 124.1(3) . . ?
C22 C23 C24 111.2(3) . . ?
C22 C23 C25 112.5(3) . . ?
C24 C23 C25 109.7(4) . . ?
N3 C26 C28 112.4(4) . . ?
N3 C26 C27 109.0(3) . . ?
C28 C26 C27 111.6(3) . . ?
N3 C29 C31 110.2(3) . . ?
N3 C29 C30 111.8(3) . . ?
C31 C29 C30 113.4(4) . . ?
C34 C33 C32 112.2(8) . . ?
C33 C34 C34 111.9(9) . 3_656 ?
C35 C36 C38 121.8(19) . . ?
C35 C36 C37 119.5(17) . . ?
C38 C36 C37 118.6(16) . . ?
C38 C37 C36 120.0(13) 3_656 . ?
C36 C38 C37 121.3(14) . 3_656 ?
C1 N1 C2 131.7(3) . . ?
C1 N1 P1 92.1(2) . . ?
C2 N1 P1 127.8(2) . . ?
C1 N2 C14 131.5(3) . . ?
C1 N2 P1 92.2(2) . . ?
C14 N2 P1 127.9(2) . . ?
C26 N3 C29 117.0(3) . . ?
C26 N3 P1 125.7(3) . . ?
C29 N3 P1 117.3(3) . . ?
N3 P1 N1 108.92(16) . . ?
N3 P1 N2 110.23(15) . . ?
N1 P1 N2 71.48(14) . . ?
N3 P1 C1 120.53(15) . . ?
N1 P1 C1 36.60(13) . . ?
N2 P1 C1 35.78(13) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.220
_database_code_depnum_ccdc_archive 'CCDC 986261'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_dv52

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H48 B Br2 N3 P, Al Br4 '
_chemical_formula_sum            'C31 H48 Al B Br6 N3 P'
_chemical_formula_weight         1010.94

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   14.8229(10)
_cell_length_b                   14.8271(10)
_cell_length_c                   19.1205(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.137(2)
_cell_angle_gamma                90.00
_cell_volume                     4092.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    2086
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      22.82

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1992
_exptl_absorpt_coefficient_mu    5.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3814
_exptl_absorpt_correction_T_max  0.5343
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31555
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_sigmaI/netI    0.1610
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         29.16
_reflns_number_total             11018
_reflns_number_gt                5161
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0771P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11018
_refine_ls_number_parameters     400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1727
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1848
_refine_ls_wR_factor_gt          0.1260
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.25816(15) 0.68525(15) 0.24047(12) 0.0240(5) Uani 1 1 d . . .
B1 B 0.6521(6) 0.8245(5) 0.3913(5) 0.0214(18) Uani 1 1 d . . .
Br1 Br 0.52339(5) 0.80831(6) 0.36684(4) 0.0313(2) Uani 1 1 d . . .
Br2 Br 0.71154(6) 0.90708(6) 0.34238(4) 0.0352(2) Uani 1 1 d . . .
Br3 Br 0.38792(6) 0.59954(6) 0.28194(5) 0.0378(2) Uani 1 1 d . . .
Br4 Br 0.27777(6) 0.77011(6) 0.14552(5) 0.0423(3) Uani 1 1 d . . .
Br5 Br 0.13199(5) 0.59181(5) 0.20417(5) 0.0321(2) Uani 1 1 d . . .
Br6 Br 0.23528(7) 0.77718(7) 0.33171(6) 0.0523(3) Uani 1 1 d . . .
C1 C 0.7142(5) 0.7708(4) 0.4552(4) 0.0164(15) Uani 1 1 d . . .
C2 C 0.8429(5) 0.6987(5) 0.4055(4) 0.0180(15) Uani 1 1 d . . .
C3 C 0.7992(5) 0.6368(5) 0.3538(4) 0.0209(16) Uani 1 1 d . . .
C4 C 0.6977(5) 0.6115(5) 0.3406(4) 0.0249(17) Uani 1 1 d . . .
H4 H 0.6715 0.6394 0.3793 0.030 Uiso 1 1 calc R . .
C5 C 0.6806(6) 0.5108(5) 0.3407(5) 0.037(2) Uani 1 1 d . . .
H5A H 0.7019 0.4827 0.3009 0.055 Uiso 1 1 calc R . .
H5B H 0.6142 0.4994 0.3351 0.055 Uiso 1 1 calc R . .
H5C H 0.7147 0.4850 0.3863 0.055 Uiso 1 1 calc R . .
C6 C 0.6466(5) 0.6518(6) 0.2679(4) 0.0320(19) Uani 1 1 d . . .
H6A H 0.6680 0.6219 0.2289 0.048 Uiso 1 1 calc R . .
H6B H 0.6597 0.7165 0.2672 0.048 Uiso 1 1 calc R . .
H6C H 0.5798 0.6425 0.2615 0.048 Uiso 1 1 calc R . .
C7 C 0.8520(5) 0.6012(5) 0.3089(4) 0.0258(17) Uani 1 1 d . . .
H7 H 0.8246 0.5580 0.2738 0.031 Uiso 1 1 calc R . .
C8 C 0.9414(5) 0.6261(6) 0.3136(4) 0.0310(19) Uani 1 1 d . . .
H8 H 0.9756 0.5990 0.2827 0.037 Uiso 1 1 calc R . .
C9 C 0.9827(5) 0.6901(5) 0.3625(4) 0.0294(18) Uani 1 1 d . . .
H9 H 1.0446 0.7083 0.3642 0.035 Uiso 1 1 calc R . .
C10 C 0.9345(5) 0.7284(5) 0.4094(4) 0.0253(17) Uani 1 1 d . . .
C11 C 0.9817(5) 0.8017(6) 0.4628(4) 0.035(2) Uani 1 1 d . . .
H11 H 0.9414 0.8142 0.4971 0.042 Uiso 1 1 calc R . .
C12 C 0.9911(7) 0.8894(6) 0.4216(6) 0.057(3) Uani 1 1 d . . .
H12A H 1.0169 0.9370 0.4559 0.085 Uiso 1 1 calc R . .
H12B H 0.9300 0.9079 0.3938 0.085 Uiso 1 1 calc R . .
H12C H 1.0325 0.8790 0.3891 0.085 Uiso 1 1 calc R . .
C13 C 1.0766(7) 0.7732(6) 0.5056(6) 0.057(3) Uani 1 1 d . . .
H13A H 1.1184 0.7650 0.4730 0.086 Uiso 1 1 calc R . .
H13B H 1.0712 0.7163 0.5304 0.086 Uiso 1 1 calc R . .
H13C H 1.1015 0.8199 0.5410 0.086 Uiso 1 1 calc R . .
C14 C 0.6394(5) 0.8224(5) 0.5505(4) 0.0187(15) Uani 1 1 d . . .
C15 C 0.5619(5) 0.7828(5) 0.5693(4) 0.0219(17) Uani 1 1 d . . .
C16 C 0.5457(5) 0.6821(5) 0.5647(4) 0.0268(18) Uani 1 1 d . . .
H16 H 0.5950 0.6541 0.5436 0.032 Uiso 1 1 calc R . .
C17 C 0.4509(6) 0.6574(6) 0.5167(5) 0.039(2) Uani 1 1 d . . .
H17A H 0.4018 0.6878 0.5345 0.058 Uiso 1 1 calc R . .
H17B H 0.4419 0.5920 0.5177 0.058 Uiso 1 1 calc R . .
H17C H 0.4485 0.6767 0.4673 0.058 Uiso 1 1 calc R . .
C18 C 0.5526(6) 0.6418(5) 0.6393(4) 0.035(2) Uani 1 1 d . . .
H18A H 0.6135 0.6557 0.6700 0.053 Uiso 1 1 calc R . .
H18B H 0.5446 0.5762 0.6353 0.053 Uiso 1 1 calc R . .
H18C H 0.5040 0.6676 0.6604 0.053 Uiso 1 1 calc R . .
C19 C 0.5024(5) 0.8401(5) 0.5936(4) 0.0220(17) Uani 1 1 d . . .
H19 H 0.4490 0.8158 0.6063 0.026 Uiso 1 1 calc R . .
C20 C 0.5182(5) 0.9311(5) 0.6001(4) 0.0292(19) Uani 1 1 d . . .
H20 H 0.4754 0.9689 0.6163 0.035 Uiso 1 1 calc R . .
C21 C 0.5956(5) 0.9679(5) 0.5832(4) 0.0243(17) Uani 1 1 d . . .
H21 H 0.6061 1.0310 0.5885 0.029 Uiso 1 1 calc R . .
C22 C 0.6588(5) 0.9145(5) 0.5583(4) 0.0206(16) Uani 1 1 d . . .
C23 C 0.7482(5) 0.9566(5) 0.5467(4) 0.0248(17) Uani 1 1 d . . .
H23 H 0.7754 0.9142 0.5164 0.030 Uiso 1 1 calc R . .
C24 C 0.7335(6) 1.0472(5) 0.5080(4) 0.0303(19) Uani 1 1 d . . .
H24A H 0.6859 1.0408 0.4634 0.045 Uiso 1 1 calc R . .
H24B H 0.7917 1.0669 0.4968 0.045 Uiso 1 1 calc R . .
H24C H 0.7133 1.0920 0.5389 0.045 Uiso 1 1 calc R . .
C25 C 0.8171(5) 0.9654(5) 0.6192(4) 0.0299(19) Uani 1 1 d . . .
H25A H 0.8778 0.9830 0.6115 0.045 Uiso 1 1 calc R . .
H25B H 0.8225 0.9074 0.6444 0.045 Uiso 1 1 calc R . .
H25C H 0.7952 1.0115 0.6482 0.045 Uiso 1 1 calc R . .
C26 C 0.7990(5) 0.5481(5) 0.5397(4) 0.0240(17) Uani 1 1 d . . .
H26 H 0.7547 0.5706 0.4957 0.029 Uiso 1 1 calc R . .
C27 C 0.7457(6) 0.4906(5) 0.5805(5) 0.038(2) Uani 1 1 d . . .
H27A H 0.7873 0.4688 0.6246 0.058 Uiso 1 1 calc R . .
H27B H 0.7191 0.4391 0.5508 0.058 Uiso 1 1 calc R . .
H27C H 0.6958 0.5263 0.5927 0.058 Uiso 1 1 calc R . .
C28 C 0.8739(6) 0.4945(6) 0.5155(5) 0.039(2) Uani 1 1 d . . .
H28A H 0.9054 0.5333 0.4871 0.058 Uiso 1 1 calc R . .
H28B H 0.8457 0.4432 0.4862 0.058 Uiso 1 1 calc R . .
H28C H 0.9190 0.4723 0.5577 0.058 Uiso 1 1 calc R . .
C29 C 0.9006(5) 0.6115(5) 0.6541(4) 0.0296(19) Uani 1 1 d . . .
H29 H 0.9043 0.5448 0.6616 0.036 Uiso 1 1 calc R . .
C30 C 0.9994(6) 0.6461(7) 0.6613(5) 0.052(3) Uani 1 1 d . . .
H30A H 1.0251 0.6208 0.6226 0.078 Uiso 1 1 calc R . .
H30B H 1.0378 0.6276 0.7078 0.078 Uiso 1 1 calc R . .
H30C H 0.9988 0.7120 0.6580 0.078 Uiso 1 1 calc R . .
C31 C 0.8561(7) 0.6510(6) 0.7110(4) 0.052(3) Uani 1 1 d . . .
H31A H 0.8489 0.7163 0.7038 0.078 Uiso 1 1 calc R . .
H31B H 0.8955 0.6390 0.7586 0.078 Uiso 1 1 calc R . .
H31C H 0.7952 0.6234 0.7074 0.078 Uiso 1 1 calc R . .
N1 N 0.7970(4) 0.7307(4) 0.4596(3) 0.0159(12) Uani 1 1 d . . .
N2 N 0.7008(4) 0.7632(4) 0.5217(3) 0.0161(12) Uani 1 1 d . . .
N3 N 0.8416(4) 0.6282(4) 0.5815(3) 0.0179(13) Uani 1 1 d . . .
P1 P 0.82487(13) 0.73248(13) 0.55543(10) 0.0185(4) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 Br4 2.281(2) . ?
Al1 Br3 2.291(2) . ?
Al1 Br6 2.299(2) . ?
Al1 Br5 2.304(2) . ?
B1 C1 1.570(11) . ?
B1 Br1 1.874(8) . ?
B1 Br2 1.877(8) . ?
C1 N2 1.335(8) . ?
C1 N1 1.349(8) . ?
C1 P1 2.293(7) . ?
C2 C3 1.395(10) . ?
C2 C10 1.413(10) . ?
C2 N1 1.442(8) . ?
C3 C7 1.391(10) . ?
C3 C4 1.514(10) . ?
C4 C5 1.515(10) . ?
C4 C6 1.544(10) . ?
C4 H4 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.359(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.375(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.545(11) . ?
C11 C13 1.518(12) . ?
C11 C12 1.542(12) . ?
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 C22 1.398(9) . ?
C14 C15 1.409(9) . ?
C14 N2 1.459(8) . ?
C15 C19 1.379(9) . ?
C15 C16 1.511(10) . ?
C16 C18 1.529(10) . ?
C16 C17 1.538(11) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.370(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.374(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.525(10) . ?
C23 C24 1.525(10) . ?
C23 C25 1.529(10) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 N3 1.488(9) . ?
C26 C27 1.496(10) . ?
C26 C28 1.521(10) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 N3 1.485(9) . ?
C29 C31 1.512(12) . ?
C29 C30 1.528(11) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N1 P1 1.785(6) . ?
N2 P1 1.862(6) . ?
N3 P1 1.626(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
Br4 Al1 Br3 109.42(10) . . ?
Br4 Al1 Br6 110.14(10) . . ?
Br3 Al1 Br6 108.86(10) . . ?
Br4 Al1 Br5 109.48(10) . . ?
Br3 Al1 Br5 109.32(10) . . ?
Br6 Al1 Br5 109.60(9) . . ?
C1 B1 Br1 120.8(5) . . ?
C1 B1 Br2 117.4(5) . . ?
Br1 B1 Br2 121.7(5) . . ?
N2 C1 N1 103.5(6) . . ?
N2 C1 B1 126.6(6) . . ?
N1 C1 B1 129.5(6) . . ?
N2 C1 P1 54.3(3) . . ?
N1 C1 P1 51.0(3) . . ?
B1 C1 P1 163.3(5) . . ?
C3 C2 C10 122.0(6) . . ?
C3 C2 N1 120.4(6) . . ?
C10 C2 N1 117.6(6) . . ?
C7 C3 C2 116.7(6) . . ?
C7 C3 C4 118.7(7) . . ?
C2 C3 C4 124.4(6) . . ?
C3 C4 C5 113.8(7) . . ?
C3 C4 C6 108.7(6) . . ?
C5 C4 C6 109.6(6) . . ?
C3 C4 H4 108.2 . . ?
C5 C4 H4 108.2 . . ?
C6 C4 H4 108.2 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C3 122.3(7) . . ?
C8 C7 H7 118.8 . . ?
C3 C7 H7 118.8 . . ?
C7 C8 C9 120.6(7) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C10 120.5(7) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C2 117.8(7) . . ?
C9 C10 C11 119.5(7) . . ?
C2 C10 C11 122.7(6) . . ?
C13 C11 C12 109.2(7) . . ?
C13 C11 C10 112.7(7) . . ?
C12 C11 C10 109.7(7) . . ?
C13 C11 H11 108.4 . . ?
C12 C11 H11 108.4 . . ?
C10 C11 H11 108.4 . . ?
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 . . ?
C22 C14 C15 122.7(6) . . ?
C22 C14 N2 119.9(6) . . ?
C15 C14 N2 117.4(6) . . ?
C19 C15 C14 116.8(7) . . ?
C19 C15 C16 121.6(6) . . ?
C14 C15 C16 121.6(6) . . ?
C15 C16 C18 110.8(6) . . ?
C15 C16 C17 112.4(7) . . ?
C18 C16 C17 108.7(6) . . ?
C15 C16 H16 108.3 . . ?
C18 C16 H16 108.3 . . ?
C17 C16 H16 108.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C15 121.9(7) . . ?
C20 C19 H19 119.1 . . ?
C15 C19 H19 119.1 . . ?
C19 C20 C21 120.3(7) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C20 C21 C22 121.2(7) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
C21 C22 C14 117.1(6) . . ?
C21 C22 C23 119.5(6) . . ?
C14 C22 C23 123.2(7) . . ?
C24 C23 C22 113.4(6) . . ?
C24 C23 C25 110.9(6) . . ?
C22 C23 C25 109.1(6) . . ?
C24 C23 H23 107.7 . . ?
C22 C23 H23 107.7 . . ?
C25 C23 H23 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 C27 112.6(6) . . ?
N3 C26 C28 109.3(6) . . ?
C27 C26 C28 111.6(7) . . ?
N3 C26 H26 107.7 . . ?
C27 C26 H26 107.7 . . ?
C28 C26 H26 107.7 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 C31 110.3(6) . . ?
N3 C29 C30 112.2(6) . . ?
C31 C29 C30 111.9(7) . . ?
N3 C29 H29 107.4 . . ?
C31 C29 H29 107.4 . . ?
C30 C29 H29 107.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 N1 C2 132.2(6) . . ?
C1 N1 P1 93.0(4) . . ?
C2 N1 P1 134.8(5) . . ?
C1 N2 C14 123.3(6) . . ?
C1 N2 P1 90.1(4) . . ?
C14 N2 P1 131.9(4) . . ?
C29 N3 C26 117.2(6) . . ?
C29 N3 P1 117.4(5) . . ?
C26 N3 P1 125.3(5) . . ?
N3 P1 N1 106.5(3) . . ?
N3 P1 N2 114.1(3) . . ?
N1 P1 N2 70.6(3) . . ?
N3 P1 C1 121.4(3) . . ?
N1 P1 C1 36.0(2) . . ?
N2 P1 C1 35.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        29.16
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.065
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.213
_database_code_depnum_ccdc_archive 'CCDC 986262'
