#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:40:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179256 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317645.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4317645
loop_
_publ_author_name
'Dana C. Haagenson'
'Daniel F. Moser'
'Lothar Stahl'
'Richard J. Staples'
_publ_section_title
;
 Syntheses and Structures of P-Anilino-P-chalcogeno- and
 P-Anilino-P-iminodiazasilaphosphetidines and Their Group 12 and 13 Metal
 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1245
_journal_page_last               1253
_journal_paper_doi               10.1021/ic010973f
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C18 H35 Al N3 P S Si'
_chemical_formula_weight         411.59
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.131(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.916(2)
_cell_length_b                   8.8658(8)
_cell_length_c                   18.1284(16)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      2.69
_cell_volume                     2461.4(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5446
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rhombic_rods
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.4_mm
_exptl_crystal_size_mid          0.7_mm
_exptl_crystal_size_min          0.5_mm
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0673P)²+0.8055P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                3500
_reflns_number_total             4310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010973f_5.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317645
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'
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 0.22728(6) 0.59884(8) -0.03149(5) 0.0659(2) Uani 1 1 d . . .
S1 S 0.25567(5) 0.56217(7) 0.10599(4) 0.0661(2) Uani 1 1 d . . .
P1 P 0.30285(4) 0.36956(6) 0.08058(3) 0.04688(17) Uani 1 1 d . . .
Si1 Si 0.37094(5) 0.15858(8) 0.17932(4) 0.0583(2) Uani 1 1 d . . .
N1 N 0.40327(12) 0.3206(2) 0.14404(11) 0.0515(4) Uani 1 1 d . . .
N2 N 0.26862(12) 0.2088(2) 0.10327(12) 0.0566(5) Uani 1 1 d . . .
N3 N 0.28090(13) 0.4043(2) -0.01386(11) 0.0511(4) Uani 1 1 d . . .
C1 C 0.4165(2) -0.0225(3) 0.16416(19) 0.0844(9) Uani 1 1 d . . .
H10A H 0.3833 -0.1045 0.1713 0.127 Uiso 1 1 calc R . .
H10B H 0.4762 -0.0310 0.2032 0.127 Uiso 1 1 calc R . .
H10C H 0.4134 -0.0258 0.1101 0.127 Uiso 1 1 calc R . .
C2 C 0.3824(2) 0.1721(4) 0.28506(18) 0.0908(9) Uani 1 1 d . . .
H20A H 0.3547 0.2627 0.2912 0.136 Uiso 1 1 calc R . .
H20B H 0.4432 0.1744 0.3219 0.136 Uiso 1 1 calc R . .
H20C H 0.3553 0.0863 0.2970 0.136 Uiso 1 1 calc R . .
C3 C 0.2982(3) 0.7553(3) -0.0504(2) 0.0979(11) Uani 1 1 d . . .
H3A H 0.3507 0.7705 -0.0015 0.147 Uiso 1 1 calc R . .
H3B H 0.2658 0.8479 -0.0651 0.147 Uiso 1 1 calc R . .
H3C H 0.3131 0.7244 -0.0936 0.147 Uiso 1 1 calc R . .
C4 C 0.1024(2) 0.6034(5) -0.1026(2) 0.1133(13) Uani 1 1 d . . .
H4A H 0.0929 0.5743 -0.1567 0.170 Uiso 1 1 calc R . .
H4B H 0.0804 0.7035 -0.1036 0.170 Uiso 1 1 calc R . .
H4C H 0.0725 0.5344 -0.0823 0.170 Uiso 1 1 calc R . .
C10 C 0.48570(17) 0.4081(3) 0.17206(17) 0.0684(7) Uani 1 1 d . . .
C11 C 0.4872(2) 0.4999(5) 0.1024(2) 0.1169(14) Uani 1 1 d . . .
H11A H 0.4796 0.4342 0.0577 0.175 Uiso 1 1 calc R . .
H11B H 0.5423 0.5511 0.1200 0.175 Uiso 1 1 calc R . .
H11C H 0.4408 0.5727 0.0850 0.175 Uiso 1 1 calc R . .
C12 C 0.5609(2) 0.2973(5) 0.2038(3) 0.1239(15) Uani 1 1 d . . .
H12A H 0.5581 0.2393 0.2473 0.186 Uiso 1 1 calc R . .
H12B H 0.6151 0.3514 0.2236 0.186 Uiso 1 1 calc R . .
H12C H 0.5571 0.2310 0.1606 0.186 Uiso 1 1 calc R . .
C13 C 0.4938(3) 0.5145(5) 0.2410(3) 0.1193(13) Uani 1 1 d . . .
H13A H 0.4457 0.5841 0.2219 0.179 Uiso 1 1 calc R . .
H13B H 0.5477 0.5693 0.2591 0.179 Uiso 1 1 calc R . .
H13C H 0.4930 0.4570 0.2856 0.179 Uiso 1 1 calc R . .
C20 C 0.17906(18) 0.1485(3) 0.0775(2) 0.0745(8) Uani 1 1 d . . .
C21 C 0.1256(3) 0.1767(7) -0.0098(3) 0.190(3) Uani 1 1 d . . .
H21A H 0.1196 0.2834 -0.0195 0.285 Uiso 1 1 calc R . .
H21B H 0.0689 0.1324 -0.0258 0.285 Uiso 1 1 calc R . .
H21C H 0.1534 0.1326 -0.0410 0.285 Uiso 1 1 calc R . .
C22 C 0.1379(3) 0.2182(6) 0.1289(4) 0.165(2) Uani 1 1 d . . .
H22A H 0.1791 0.2173 0.1852 0.248 Uiso 1 1 calc R . .
H22B H 0.0871 0.1613 0.1225 0.248 Uiso 1 1 calc R . .
H22C H 0.1213 0.3204 0.1117 0.248 Uiso 1 1 calc R . .
C23 C 0.1851(3) -0.0187(5) 0.0928(4) 0.157(2) Uani 1 1 d . . .
H23A H 0.2110 -0.0662 0.0607 0.235 Uiso 1 1 calc R . .
H23B H 0.1277 -0.0590 0.0779 0.235 Uiso 1 1 calc R . .
H23C H 0.2206 -0.0378 0.1495 0.235 Uiso 1 1 calc R . .
C30 C 0.30286(15) 0.3176(3) -0.06816(13) 0.0537(5) Uani 1 1 d . . .
C31 C 0.3537(2) 0.1894(3) -0.04644(19) 0.0851(9) Uani 1 1 d . . .
H31 H 0.3741 0.1531 0.0066 0.102 Uiso 1 1 calc R . .
C32 C 0.3750(3) 0.1138(4) -0.1025(2) 0.1008(12) Uani 1 1 d . . .
H32 H 0.4101 0.0284 -0.0866 0.121 Uiso 1 1 calc R . .
C33 C 0.3446(2) 0.1643(4) -0.1809(2) 0.0934(11) Uani 1 1 d . . .
H33 H 0.3581 0.1126 -0.2187 0.112 Uiso 1 1 calc R . .
C34 C 0.2942(2) 0.2917(5) -0.20334(17) 0.0939(11) Uani 1 1 d . . .
H34 H 0.2741 0.3275 -0.2564 0.113 Uiso 1 1 calc R . .
C35 C 0.27313(18) 0.3670(4) -0.14785(15) 0.0740(8) Uani 1 1 d . . .
H35 H 0.2382 0.4527 -0.1642 0.089 Uiso 1 1 calc R . .
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'
Si Si 0.0817 0.0704 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N3 Al1 C4 115.62(14) . . ?
N3 Al1 C3 112.71(13) . . ?
C4 Al1 C3 116.25(17) . . ?
N3 Al1 S1 80.17(6) . . ?
C4 Al1 S1 112.26(12) . . ?
C3 Al1 S1 114.75(11) . . ?
N3 Al1 P1 34.67(5) . . ?
C4 Al1 P1 122.10(12) . . ?
C3 Al1 P1 121.43(12) . . ?
S1 Al1 P1 45.50(2) . . ?
P1 S1 Al1 78.34(3) . . ?
N3 P1 N2 118.63(10) . . ?
N3 P1 N1 119.44(9) . . ?
N2 P1 N1 88.02(10) . . ?
N3 P1 S1 98.34(7) . . ?
N2 P1 S1 117.24(7) . . ?
N1 P1 S1 116.87(7) . . ?
N3 P1 Si1 136.59(7) . . ?
N2 P1 Si1 44.16(7) . . ?
N1 P1 Si1 44.16(7) . . ?
S1 P1 Si1 125.08(3) . . ?
N3 P1 Al1 42.17(7) . . ?
N2 P1 Al1 135.44(8) . . ?
N1 P1 Al1 136.02(7) . . ?
S1 P1 Al1 56.17(3) . . ?
Si1 P1 Al1 178.72(3) . . ?
N1 Si1 N2 82.04(9) . . ?
N1 Si1 C2 114.47(13) . . ?
N2 Si1 C2 115.70(13) . . ?
N1 Si1 C1 116.29(12) . . ?
N2 Si1 C1 115.98(13) . . ?
C2 Si1 C1 110.09(14) . . ?
N1 Si1 P1 41.16(6) . . ?
N2 Si1 P1 41.16(6) . . ?
C2 Si1 P1 120.45(11) . . ?
C1 Si1 P1 129.45(10) . . ?
C10 N1 P1 129.68(16) . . ?
C10 N1 Si1 134.22(16) . . ?
P1 N1 Si1 94.68(9) . . ?
C20 N2 P1 130.63(17) . . ?
C20 N2 Si1 133.78(17) . . ?
P1 N2 Si1 94.68(10) . . ?
C30 N3 P1 128.41(16) . . ?
C30 N3 Al1 128.23(15) . . ?
P1 N3 Al1 103.16(9) . . ?
N1 C10 C11 110.0(2) . . ?
N1 C10 C12 107.8(2) . . ?
C11 C10 C12 110.9(3) . . ?
N1 C10 C13 110.4(2) . . ?
C11 C10 C13 109.0(3) . . ?
C12 C10 C13 108.8(3) . . ?
C21 C20 N2 110.8(2) . . ?
C21 C20 C23 109.2(4) . . ?
N2 C20 C23 108.5(3) . . ?
C21 C20 C22 111.1(4) . . ?
N2 C20 C22 109.6(3) . . ?
C23 C20 C22 107.6(4) . . ?
C31 C30 C35 117.7(2) . . ?
C31 C30 N3 124.4(2) . . ?
C35 C30 N3 117.9(2) . . ?
C30 C31 C32 120.9(3) . . ?
C33 C32 C31 120.3(3) . . ?
C32 C33 C34 119.4(3) . . ?
C33 C34 C35 120.4(3) . . ?
C34 C35 C30 121.2(3) . . ?
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 N3 1.9116(19) . ?
Al1 C4 1.953(4) . ?
Al1 C3 1.958(3) . ?
Al1 S1 2.3518(10) . ?
Al1 P1 2.7728(9) . ?
S1 P1 2.0193(8) . ?
P1 N3 1.6198(18) . ?
P1 N2 1.6546(18) . ?
P1 N1 1.6546(19) . ?
P1 Si1 2.5056(8) . ?
Si1 N1 1.7515(19) . ?
Si1 N2 1.752(2) . ?
Si1 C2 1.847(3) . ?
Si1 C1 1.851(3) . ?
N1 C10 1.484(3) . ?
N2 C20 1.483(3) . ?
N3 C30 1.417(3) . ?
C10 C11 1.512(4) . ?
C10 C12 1.514(4) . ?
C10 C13 1.525(4) . ?
C20 C21 1.474(5) . ?
C20 C23 1.503(5) . ?
C20 C22 1.513(5) . ?
C30 C31 1.378(4) . ?
C30 C35 1.383(3) . ?
C31 C32 1.386(4) . ?
C32 C33 1.366(5) . ?
C33 C34 1.369(5) . ?
C34 C35 1.375(4) . ?
