# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1214

data_s12_h

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 1,2,3-Tri-tert.butyl-1,3-2,4-diazaphosphaaluminetidine-
 trimethylamino-donor
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C15 H37 Al N3 P'
_chemical_formula_weight          317.43

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    'Pbca (no.61)'

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

_cell_length_a                    12.8335(4)
_cell_length_b                    16.7315(5)
_cell_length_c                    18.6500(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      4004.6(2)
_cell_formula_units_Z             8
_cell_measurement_temperature     123(2)
_cell_measurement_reflns_used     33067
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        plates
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.45
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       none
_exptl_crystal_density_diffrn     1.053
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1408
_exptl_absorpt_coefficient_mu     0.178
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   '0.9161 (theor.)'
_exptl_absorpt_correction_T_max   '0.9737 (theor.)'

_exptl_special_details
;
 dx = 39.943(5) mm; 2 x 60 sec., 1 deg., 570 frames (phi + omega),
 mos.= 0.879(1)
;

_diffrn_ambient_temperature       123(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   'Nonius KappaCCD'
_diffrn_measurement_method        'rotation in phi and omega, 1 deg.'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             48091
_diffrn_reflns_av_R_equivalents   0.0526
_diffrn_reflns_av_sigmaI/netI     0.0588
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          2.43
_diffrn_reflns_theta_max          28.27
_reflns_number_total              4824
_reflns_number_gt                 3154
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        Collect
_computing_cell_refinement        DENZO-SMN
_computing_data_reduction         DENZO-SMN
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     XP
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'

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

 Large rest electron density (1.54) 200 pm from AL inicates probably
 an OH-group with is disordered with the H(Al). A suitable model would
 be H(Al) : OH(Al) 0.85:0.15 (U(O) around 1.5 times U(Al)).
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4824
_refine_ls_number_parameters      184
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0746
_refine_ls_R_factor_gt            0.0500
_refine_ls_wR_factor_ref          0.1535
_refine_ls_wR_factor_gt           0.1457
_refine_ls_goodness_of_fit_ref    1.004
_refine_ls_restrained_S_all       1.007
_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_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
P1 P 0.30036(4) 0.16985(3) 0.38798(2) 0.02008(16) Uani 1 d . . .
Al1 Al 0.30651(4) 0.02632(3) 0.33667(3) 0.02228(18) Uani 1 d D . .
H1AL H 0.2235(11) -0.0209(10) 0.3018(7) 0.033 Uiso 1 d D . .
N1 N 0.28969(11) 0.07509(9) 0.42467(8) 0.0211(3) Uani 1 d D . .
N2 N 0.33729(12) 0.12763(9) 0.30711(7) 0.0216(3) Uani 1 d D . .
C1 C 0.42341(16) 0.21364(12) 0.42901(9) 0.0272(4) Uani 1 d . . .
C2 C 0.39759(19) 0.23959(14) 0.50597(11) 0.0408(6) Uani 1 d . . .
H2A H 0.3380 0.2762 0.5053 0.061 Uiso 1 calc R . .
H2B H 0.4580 0.2667 0.5269 0.061 Uiso 1 calc R . .
H2C H 0.3803 0.1924 0.5348 0.061 Uiso 1 calc R . .
C3 C 0.45006(19) 0.28869(13) 0.38657(11) 0.0403(6) Uani 1 d . . .
H3A H 0.3899 0.3247 0.3862 0.060 Uiso 1 calc R . .
H3B H 0.4679 0.2740 0.3372 0.060 Uiso 1 calc R . .
H3C H 0.5095 0.3157 0.4089 0.060 Uiso 1 calc R . .
C4 C 0.51572(16) 0.15745(14) 0.42981(12) 0.0382(5) Uani 1 d . . .
H4A H 0.4982 0.1096 0.4576 0.057 Uiso 1 calc R . .
H4B H 0.5756 0.1843 0.4517 0.057 Uiso 1 calc R . .
H4C H 0.5331 0.1420 0.3806 0.057 Uiso 1 calc R . .
C5 C 0.20341(14) 0.05543(12) 0.47480(10) 0.0262(4) Uani 1 d . . .
C6 C 0.21239(16) -0.03362(12) 0.49220(12) 0.0351(5) Uani 1 d . . .
H6A H 0.2080 -0.0647 0.4478 0.053 Uiso 1 calc R . .
H6B H 0.1556 -0.0492 0.5244 0.053 Uiso 1 calc R . .
H6C H 0.2794 -0.0440 0.5156 0.053 Uiso 1 calc R . .
C7 C 0.21067(17) 0.10181(15) 0.54505(11) 0.0382(5) Uani 1 d . . .
H7A H 0.2787 0.0922 0.5672 0.057 Uiso 1 calc R . .
H7B H 0.1554 0.0840 0.5776 0.057 Uiso 1 calc R . .
H7C H 0.2025 0.1590 0.5354 0.057 Uiso 1 calc R . .
C8 C 0.09712(15) 0.07200(15) 0.44089(12) 0.0406(6) Uani 1 d . . .
H8A H 0.0914 0.0427 0.3956 0.061 Uiso 1 calc R . .
H8B H 0.0900 0.1294 0.4318 0.061 Uiso 1 calc R . .
H8C H 0.0419 0.0545 0.4736 0.061 Uiso 1 calc R . .
C9 C 0.33236(18) 0.16607(12) 0.23600(10) 0.0318(5) Uani 1 d . . .
C10 C 0.2818(2) 0.24678(15) 0.23582(12) 0.0467(6) Uani 1 d . . .
H10A H 0.3185 0.2821 0.2693 0.070 Uiso 1 calc R . .
H10B H 0.2088 0.2416 0.2506 0.070 Uiso 1 calc R . .
H10C H 0.2849 0.2695 0.1874 0.070 Uiso 1 calc R . .
C11 C 0.2760(3) 0.11117(16) 0.18434(12) 0.0568(7) Uani 1 d . . .
H11A H 0.3094 0.0585 0.1846 0.085 Uiso 1 calc R . .
H11B H 0.2792 0.1337 0.1359 0.085 Uiso 1 calc R . .
H11C H 0.2031 0.1058 0.1991 0.085 Uiso 1 calc R . .
C12 C 0.4466(2) 0.17503(16) 0.20735(13) 0.0529(7) Uani 1 d . . .
H12A H 0.4807 0.1226 0.2072 0.079 Uiso 1 calc R . .
H12B H 0.4855 0.2116 0.2385 0.079 Uiso 1 calc R . .
H12C H 0.4451 0.1965 0.1585 0.079 Uiso 1 calc R . .
N3 N 0.42164(13) -0.05585(10) 0.32590(9) 0.0318(4) Uani 1 d . . .
C13 C 0.3920(2) -0.12885(13) 0.36658(12) 0.0417(6) Uani 1 d . . .
H13A H 0.3232 -0.1472 0.3507 0.063 Uiso 1 calc R . .
H13B H 0.3897 -0.1165 0.4179 0.063 Uiso 1 calc R . .
H13C H 0.4436 -0.1710 0.3579 0.063 Uiso 1 calc R . .
C14 C 0.4288(2) -0.07703(15) 0.24857(12) 0.0519(7) Uani 1 d . . .
H14A H 0.4482 -0.0295 0.2209 0.078 Uiso 1 calc R . .
H14B H 0.3612 -0.0969 0.2319 0.078 Uiso 1 calc R . .
H14C H 0.4817 -0.1186 0.2420 0.078 Uiso 1 calc R . .
C15 C 0.52528(18) -0.02967(15) 0.35076(16) 0.0548(7) Uani 1 d . . .
H15A H 0.5462 0.0184 0.3244 0.082 Uiso 1 calc R . .
H15B H 0.5762 -0.0723 0.3422 0.082 Uiso 1 calc R . .
H15C H 0.5223 -0.0177 0.4022 0.082 Uiso 1 calc R . .

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
P1 0.0243(3) 0.0190(3) 0.0169(3) -0.00045(19) 0.00166(19) 0.00091(19)
Al1 0.0262(3) 0.0191(3) 0.0215(3) -0.0013(2) -0.0022(2) 0.0001(2)
N1 0.0232(8) 0.0203(8) 0.0199(8) 0.0034(6) 0.0037(6) -0.0007(6)
N2 0.0275(8) 0.0228(8) 0.0144(7) -0.0001(6) 0.0015(6) 0.0025(7)
C1 0.0350(10) 0.0254(10) 0.0212(10) -0.0033(8) -0.0011(8) -0.0072(8)
C2 0.0568(15) 0.0401(13) 0.0256(11) -0.0096(9) -0.0019(10) -0.0102(11)
C3 0.0509(14) 0.0323(12) 0.0376(12) -0.0001(10) -0.0031(11) -0.0176(11)
C4 0.0307(11) 0.0429(13) 0.0410(12) -0.0051(10) -0.0089(10) -0.0069(10)
C5 0.0226(10) 0.0298(11) 0.0262(10) 0.0090(9) 0.0059(8) 0.0002(8)
C6 0.0351(11) 0.0325(12) 0.0377(12) 0.0134(9) 0.0044(10) -0.0016(9)
C7 0.0387(12) 0.0487(14) 0.0273(11) 0.0043(10) 0.0121(9) 0.0061(10)
C8 0.0253(11) 0.0506(15) 0.0459(13) 0.0186(11) 0.0027(10) 0.0011(10)
C9 0.0499(12) 0.0295(11) 0.0159(9) 0.0017(8) -0.0019(9) -0.0019(9)
C10 0.0706(16) 0.0382(13) 0.0314(12) 0.0055(10) -0.0054(11) 0.0079(12)
C11 0.098(2) 0.0445(15) 0.0283(12) -0.0002(11) -0.0179(13) 0.0002(14)
C12 0.0652(17) 0.0542(16) 0.0393(13) 0.0082(12) 0.0210(12) 0.0024(13)
N3 0.0395(10) 0.0248(9) 0.0310(9) -0.0057(7) -0.0003(8) 0.0055(8)
C13 0.0617(16) 0.0251(11) 0.0384(12) 0.0008(9) -0.0019(11) 0.0122(11)
C14 0.0834(19) 0.0398(14) 0.0325(12) -0.0070(11) 0.0121(12) 0.0213(13)
C15 0.0334(13) 0.0442(15) 0.087(2) -0.0141(14) -0.0052(13) 0.0119(11)

_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
P1 N2 1.7316(14) . ?
P1 N1 1.7324(15) . ?
P1 C1 1.902(2) . ?
P1 Al1 2.5864(7) . ?
Al1 N2 1.8256(16) . ?
Al1 N1 1.8456(16) . ?
Al1 N3 2.0283(18) . ?
N1 C5 1.486(2) . ?
N2 C9 1.475(2) . ?
C1 C4 1.513(3) . ?
C1 C3 1.523(3) . ?
C1 C2 1.536(3) . ?
C5 C7 1.526(3) . ?
C5 C8 1.529(3) . ?
C5 C6 1.529(3) . ?
C9 C10 1.498(3) . ?
C9 C11 1.515(3) . ?
C9 C12 1.568(3) . ?
N3 C15 1.475(3) . ?
N3 C13 1.487(3) . ?
N3 C14 1.488(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
N2 P1 N1 89.56(7) . . ?
N2 P1 C1 106.29(8) . . ?
N1 P1 C1 105.03(8) . . ?
N2 P1 Al1 44.81(5) . . ?
N1 P1 Al1 45.47(5) . . ?
C1 P1 Al1 118.77(7) . . ?
N2 Al1 N1 83.30(7) . . ?
N2 Al1 N3 116.22(7) . . ?
N1 Al1 N3 118.22(7) . . ?
N2 Al1 P1 41.95(5) . . ?
N1 Al1 P1 42.00(5) . . ?
N3 Al1 P1 133.49(5) . . ?
C5 N1 P1 120.66(12) . . ?
C5 N1 Al1 123.28(12) . . ?
P1 N1 Al1 92.52(7) . . ?
C9 N2 P1 126.39(13) . . ?
C9 N2 Al1 131.83(12) . . ?
P1 N2 Al1 93.24(7) . . ?
C4 C1 C3 109.97(18) . . ?
C4 C1 C2 109.61(17) . . ?
C3 C1 C2 107.52(17) . . ?
C4 C1 P1 114.51(13) . . ?
C3 C1 P1 107.16(13) . . ?
C2 C1 P1 107.81(14) . . ?
N1 C5 C7 112.47(16) . . ?
N1 C5 C8 111.38(15) . . ?
C7 C5 C8 108.51(17) . . ?
N1 C5 C6 107.04(16) . . ?
C7 C5 C6 107.98(17) . . ?
C8 C5 C6 109.38(18) . . ?
N2 C9 C10 114.43(17) . . ?
N2 C9 C11 109.13(17) . . ?
C10 C9 C11 109.8(2) . . ?
N2 C9 C12 107.94(17) . . ?
C10 C9 C12 108.6(2) . . ?
C11 C9 C12 106.72(19) . . ?
C15 N3 C13 108.30(18) . . ?
C15 N3 C14 108.65(19) . . ?
C13 N3 C14 108.34(17) . . ?
C15 N3 Al1 115.11(14) . . ?
C13 N3 Al1 108.66(13) . . ?
C14 N3 Al1 107.60(13) . . ?

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
N1 P1 Al1 N2 -167.14(10) . . . . ?
C1 P1 Al1 N2 -84.33(10) . . . . ?
N2 P1 Al1 N1 167.14(10) . . . . ?
C1 P1 Al1 N1 82.81(9) . . . . ?
N2 P1 Al1 N3 81.69(10) . . . . ?
N1 P1 Al1 N3 -85.45(10) . . . . ?
C1 P1 Al1 N3 -2.64(10) . . . . ?
N2 P1 N1 C5 -140.68(14) . . . . ?
C1 P1 N1 C5 112.56(14) . . . . ?
Al1 P1 N1 C5 -131.66(16) . . . . ?
N2 P1 N1 Al1 -9.03(7) . . . . ?
C1 P1 N1 Al1 -115.79(8) . . . . ?
N2 Al1 N1 C5 138.38(14) . . . . ?
N3 Al1 N1 C5 -105.40(14) . . . . ?
P1 Al1 N1 C5 129.76(16) . . . . ?
N2 Al1 N1 P1 8.62(7) . . . . ?
N3 Al1 N1 P1 124.84(8) . . . . ?
N1 P1 N2 C9 159.79(16) . . . . ?
C1 P1 N2 C9 -94.67(17) . . . . ?
Al1 P1 N2 C9 150.66(19) . . . . ?
N1 P1 N2 Al1 9.13(7) . . . . ?
C1 P1 N2 Al1 114.67(8) . . . . ?
N1 Al1 N2 C9 -156.66(18) . . . . ?
N3 Al1 N2 C9 85.11(18) . . . . ?
P1 Al1 N2 C9 -148.0(2) . . . . ?
N1 Al1 N2 P1 -8.63(7) . . . . ?
N3 Al1 N2 P1 -126.85(7) . . . . ?
N2 P1 C1 C4 -48.75(16) . . . . ?
N1 P1 C1 C4 45.27(16) . . . . ?
Al1 P1 C1 C4 -1.82(17) . . . . ?
N2 P1 C1 C3 73.50(15) . . . . ?
N1 P1 C1 C3 167.52(13) . . . . ?
Al1 P1 C1 C3 120.44(13) . . . . ?
N2 P1 C1 C2 -171.02(14) . . . . ?
N1 P1 C1 C2 -77.00(15) . . . . ?
Al1 P1 C1 C2 -124.08(13) . . . . ?
P1 N1 C5 C7 -65.79(19) . . . . ?
Al1 N1 C5 C7 177.44(13) . . . . ?
P1 N1 C5 C8 56.3(2) . . . . ?
Al1 N1 C5 C8 -60.5(2) . . . . ?
P1 N1 C5 C6 175.78(13) . . . . ?
Al1 N1 C5 C6 59.01(19) . . . . ?
P1 N2 C9 C10 -5.4(3) . . . . ?
Al1 N2 C9 C10 133.60(18) . . . . ?
P1 N2 C9 C11 -128.77(19) . . . . ?
Al1 N2 C9 C11 10.2(3) . . . . ?
P1 N2 C9 C12 115.61(17) . . . . ?
Al1 N2 C9 C12 -105.4(2) . . . . ?
N2 Al1 N3 C15 46.08(18) . . . . ?
N1 Al1 N3 C15 -50.63(18) . . . . ?
P1 Al1 N3 C15 -1.42(19) . . . . ?
N2 Al1 N3 C13 167.70(13) . . . . ?
N1 Al1 N3 C13 70.99(15) . . . . ?
P1 Al1 N3 C13 120.20(12) . . . . ?
N2 Al1 N3 C14 -75.19(16) . . . . ?
N1 Al1 N3 C14 -171.90(14) . . . . ?
P1 Al1 N3 C14 -122.69(14) . . . . ?

_diffrn_measured_fraction_theta_max    0.880
_diffrn_reflns_theta_full              28.27
_diffrn_measured_fraction_theta_full   0.880
_refine_diff_density_max    1.537
_refine_diff_density_min   -0.363
_refine_diff_density_rms    0.086