# Supplementary Material (ESI) for Perkin Transactions
# This journal is © The Royal Society of Chemistry 2001

data_apr796

_database_code_CSD	152354


_journal_coden_Cambridge      207

_publ_requested_journal       'Perkin Transactions 1'

loop_
_publ_author_name
'Boesveld, W. Marco'
'Hitchcock, P. B.'
'Lappert, M.'

_publ_contact_author_name     	'Prof M Lappert'  
_publ_contact_author_address 
;
Prof M Lappert
School of Chemistry & Molecular Science
University of Sussex
BRIGHTON
BN1 9QJ
U.K.
;
_audit_creation_date            2000-01-10T14:43:12-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.1beta5
_audit_conform_dict_location    
;
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
;
_publ_requested_category        FO

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic
;
'4-Bis(trimethylsilyl)methyl-1,4-dihydro-1,3,5-triazine'
;
_chemical_formula_sum                   'C10 H23 N3 Si2'
_chemical_formula_weight                241.49

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

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

_cell_length_a                          13.449(9)
_cell_length_b                          13.597(3)
_cell_length_c                          16.399(9)
_cell_angle_alpha                       90
_cell_angle_beta                        90
_cell_angle_gamma                       90
_cell_volume                            2999(3)
_cell_formula_units_Z                   8
_cell_measurement_temperature           173(2)

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max                 0.4
_exptl_crystal_size_mid                 0.4
_exptl_crystal_size_min                 0.4
_exptl_crystal_density_diffrn           1.07
_exptl_crystal_F_000                    1056
_exptl_special_details
;
?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION NOT APPLIED                        #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu           0.216

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature             173(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_reflns_number                   4027
_diffrn_reflns_av_R_equivalents         0
_diffrn_reflns_av_sigmaI/netI           0.0742
_diffrn_reflns_limit_h_min              0
_diffrn_reflns_limit_h_max              17
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              17
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              21
_diffrn_reflns_theta_min                2.13
_diffrn_reflns_theta_max                28.03
_reflns_number_total                    4027
_reflns_number_gt                       3212
_reflns_threshold_expression            >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement         'SHELXL-93 (Sheldrick, 1993)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details
;
H atoms on N2 and N5 were freely refined; other H atoms in riding mode.
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^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_extinction_method            none
_refine_ls_number_reflns                4027
_refine_ls_number_parameters            279
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0691
_refine_ls_R_factor_gt                  0.0474
_refine_ls_wR_factor_gt                 0.1033
_refine_ls_wR_factor_all                0.1144
_refine_ls_goodness_of_fit_gt           1.051
_refine_ls_goodness_of_fit_all          1.031
_refine_ls_restrained_S_all             1.031
_refine_ls_restrained_S_obs             1.051
_refine_ls_shift/su_max                 -0.001
_refine_ls_shift/su_mean                0
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack          0.20(17)
_refine_diff_density_max                0.287
_refine_diff_density_min                -0.283
_refine_diff_density_rms                0.06

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_group
Si1 Si 0.50441(8) 0.34478(8) 0.28974(6) 0.0275(2) Uani 1 d . .
Si4 Si 0.60089(8) 0.83326(7) 0.62354(6) 0.0268(2) Uani 1 d . .
Si3 Si 0.37237(8) 0.76319(8) 0.65393(6) 0.0264(2) Uani 1 d . .
Si2 Si 0.58328(8) 0.18810(7) 0.42279(6) 0.0251(2) Uani 1 d . .
N1 N 0.6943(2) 0.4130(2) 0.4736(2) 0.0248(7) Uani 1 d . .
N2 N 0.6106(3) 0.4990(2) 0.5755(2) 0.0276(7) Uani 1 d . .
H2N H 0.612(4) 0.533(4) 0.622(3) 0.065(16) Uiso 1 d . .
N3 N 0.5165(2) 0.3854(2) 0.5014(2) 0.0301(7) Uani 1 d . .
N4 N 0.6151(2) 0.6107(2) 0.7269(2) 0.0227(6) Uani 1 d . .
N5 N 0.6441(2) 0.6349(2) 0.8660(2) 0.0249(7) Uani 1 d . .
H5N H 0.683(3) 0.623(3) 0.899(2) 0.014(10) Uiso 1 d . .
N6 N 0.5587(2) 0.7609(2) 0.7989(2) 0.0235(6) Uani 1 d . .
C1 C 0.5936(3) 0.3998(2) 0.4390(2) 0.0228(7) Uani 1 d . .
H1 H 0.5767(3) 0.4615(2) 0.4088(2) 0.027 Uiso 1 calc R .
C2 C 0.6952(3) 0.4662(3) 0.5375(2) 0.0249(8) Uani 1 d . .
H2 H 0.7577(3) 0.4842(3) 0.5601(2) 0.03 Uiso 1 calc R .
C3 C 0.5287(3) 0.4386(3) 0.5635(2) 0.0319(9) Uani 1 d . .
H3 H 0.4790(3) 0.4372(3) 0.6046(2) 0.038 Uiso 1 calc R .
C4 C 0.5923(3) 0.3146(2) 0.3762(2) 0.0217(7) Uani 1 d . .
H4 H 0.6598(3) 0.3164(2) 0.3507(2) 0.026 Uiso 1 calc R .
C5 C 0.3831(3) 0.3927(4) 0.3284(3) 0.0453(11) Uani 1 d . .
H5A H 0.3952(3) 0.4486(4) 0.3648(3) 0.068 Uiso 1 calc R .
H5B H 0.3485(3) 0.3406(4) 0.3584(3) 0.068 Uiso 1 calc R .
H5C H 0.3421(3) 0.4140(4) 0.2823(3) 0.068 Uiso 1 calc R .
C6 C 0.5675(4) 0.4409(3) 0.2265(3) 0.0459(12) Uani 1 d . .
H6A H 0.5812(4) 0.4988(3) 0.2602(3) 0.069 Uiso 1 calc R .
H6B H 0.5242(4) 0.4596(3) 0.1810(3) 0.069 Uiso 1 calc R .
H6C H 0.6301(4) 0.4146(3) 0.2051(3) 0.069 Uiso 1 calc R .
C7 C 0.4817(3) 0.2385(3) 0.2206(2) 0.0399(10) Uani 1 d . .
H7A H 0.5454(3) 0.2135(3) 0.2003(2) 0.06 Uiso 1 calc R .
H7B H 0.4406(3) 0.2597(3) 0.1745(2) 0.06 Uiso 1 calc R .
H7C H 0.4472(3) 0.1863(3) 0.2506(2) 0.06 Uiso 1 calc R .
C8 C 0.6469(4) 0.1806(3) 0.5236(2) 0.0420(11) Uani 1 d . .
H8A H 0.6142(4) 0.2251(3) 0.5622(2) 0.063 Uiso 1 calc R .
H8B H 0.7167(4) 0.1997(3) 0.5174(2) 0.063 Uiso 1 calc R .
H8C H 0.6432(4) 0.1130(3) 0.5442(2) 0.063 Uiso 1 calc R .
C9 C 0.6509(3) 0.1012(3) 0.3542(2) 0.0335(9) Uani 1 d . .
H9A H 0.6204(3) 0.1022(3) 0.2999(2) 0.05 Uiso 1 calc R .
H9B H 0.6472(3) 0.0345(3) 0.3767(2) 0.05 Uiso 1 calc R .
H9C H 0.7207(3) 0.1212(3) 0.3499(2) 0.05 Uiso 1 calc R .
C10 C 0.4510(3) 0.1460(3) 0.4345(2) 0.0377(10) Uani 1 d . .
H10A H 0.4172(3) 0.1498(3) 0.3816(2) 0.057 Uiso 1 calc R .
H10B H 0.4167(3) 0.1884(3) 0.4738(2) 0.057 Uiso 1 calc R .
H10C H 0.4501(3) 0.0780(3) 0.4541(2) 0.057 Uiso 1 calc R .
C11 C 0.5358(3) 0.6850(3) 0.7370(2) 0.0217(7) Uani 1 d . .
H11 H 0.4749(3) 0.6494(3) 0.7558(2) 0.026 Uiso 1 calc R .
C12 C 0.6605(3) 0.5890(3) 0.7928(2) 0.0243(8) Uani 1 d . .
H12 H 0.7086(3) 0.5380(3) 0.7910(2) 0.029 Uiso 1 calc R .
C13 C 0.6066(3) 0.7291(3) 0.8597(2) 0.0243(8) Uani 1 d . .
H13 H 0.6176(3) 0.7729(3) 0.9040(2) 0.029 Uiso 1 calc R .
C14 C 0.5098(3) 0.7349(3) 0.6557(2) 0.0220(7) Uani 1 d . .
H14 H 0.5182(3) 0.6818(3) 0.6141(2) 0.026 Uiso 1 calc R .
C15 C 0.3311(3) 0.8218(3) 0.7514(2) 0.0364(10) Uani 1 d . .
H15A H 0.3657(3) 0.8847(3) 0.7585(2) 0.055 Uiso 1 calc R .
H15B H 0.3469(3) 0.7782(3) 0.7972(2) 0.055 Uiso 1 calc R .
H15C H 0.2592(3) 0.8332(3) 0.7495(2) 0.055 Uiso 1 calc R .
C16 C 0.3347(3) 0.8454(3) 0.5676(2) 0.0423(11) Uani 1 d . .
H16A H 0.3683(3) 0.9090(3) 0.5730(2) 0.063 Uiso 1 calc R .
H16B H 0.2626(3) 0.8552(3) 0.5688(2) 0.063 Uiso 1 calc R .
H16C H 0.3537(3) 0.8149(3) 0.5157(2) 0.063 Uiso 1 calc R .
C17 C 0.3063(3) 0.6432(3) 0.6404(3) 0.0421(11) Uani 1 d . .
H17A H 0.3279(3) 0.6124(3) 0.5893(3) 0.063 Uiso 1 calc R .
H17B H 0.2344(3) 0.6546(3) 0.6385(3) 0.063 Uiso 1 calc R .
H17C H 0.3220(3) 0.5996(3) 0.6862(3) 0.063 Uiso 1 calc R .
C18 C 0.5777(4) 0.9538(3) 0.6745(3) 0.0424(11) Uani 1 d . .
H18A H 0.5090(4) 0.9744(3) 0.6643(3) 0.064 Uiso 1 calc R .
H18B H 0.6234(4) 1.0033(3) 0.6525(3) 0.064 Uiso 1 calc R .
H18C H 0.5884(4) 0.9470(3) 0.7333(3) 0.064 Uiso 1 calc R .
C19 C 0.7323(3) 0.7950(3) 0.6436(3) 0.0418(11) Uani 1 d . .
H19A H 0.7453(3) 0.7317(3) 0.6171(3) 0.063 Uiso 1 calc R .
H19B H 0.7428(3) 0.7885(3) 0.7025(3) 0.063 Uiso 1 calc R .
H19C H 0.7778(3) 0.8448(3) 0.6218(3) 0.063 Uiso 1 calc R .
C20 C 0.5895(4) 0.8508(4) 0.5101(2) 0.0505(12) Uani 1 d . .
H20A H 0.6015(4) 0.7880(4) 0.4825(2) 0.076 Uiso 1 calc R .
H20B H 0.6385(4) 0.8993(4) 0.4918(2) 0.076 Uiso 1 calc R .
H20C H 0.5224(4) 0.8742(4) 0.4970(2) 0.076 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
Si1 0.0299(6) 0.0313(5) 0.0212(5) 0.0018(4) -0.0023(5) 0.0025(5)
Si4 0.0320(6) 0.0276(5) 0.0209(5) 0.0024(4) 0.0056(4) 0.0021(5)
Si3 0.0273(5) 0.0260(5) 0.0257(5) 0.0016(4) -0.0081(5) 0.0010(4)
Si2 0.0355(6) 0.0215(5) 0.0184(4) 0.0004(4) -0.0001(4) -0.0022(4)
N1 0.027(2) 0.026(2) 0.0214(15) -0.0057(13) 0.0034(13) -0.0033(14)
N2 0.037(2) 0.025(2) 0.0205(15) -0.0060(13) 0.0043(15) 0.0014(15)
N3 0.028(2) 0.036(2) 0.026(2) -0.0081(14) 0.0095(14) -0.003(2)
N4 0.030(2) 0.0187(14) 0.0192(14) -0.0001(11) -0.0021(13) 0.0038(13)
N5 0.025(2) 0.032(2) 0.0176(15) 0.0002(13) -0.0070(14) 0.0060(14)
N6 0.030(2) 0.0232(15) 0.0172(13) -0.0033(12) -0.0018(13) 0.0036(13)
C1 0.027(2) 0.020(2) 0.021(2) -0.0017(13) 0.005(2) 0.000(2)
C2 0.029(2) 0.022(2) 0.024(2) 0.0003(15) 0.002(2) -0.002(2)
C3 0.033(2) 0.035(2) 0.028(2) -0.006(2) 0.008(2) 0.003(2)
C4 0.027(2) 0.022(2) 0.0163(14) -0.0010(14) 0.0011(15) 0.0018(15)
C5 0.034(2) 0.066(3) 0.036(2) -0.006(2) -0.003(2) 0.014(2)
C6 0.055(3) 0.045(3) 0.038(2) 0.016(2) -0.007(2) 0.003(2)
C7 0.046(3) 0.047(2) 0.027(2) -0.001(2) -0.012(2) -0.001(2)
C8 0.062(3) 0.034(2) 0.030(2) 0.010(2) -0.013(2) -0.001(2)
C9 0.041(2) 0.022(2) 0.038(2) -0.001(2) 0.004(2) 0.001(2)
C10 0.043(2) 0.037(2) 0.033(2) -0.002(2) 0.010(2) -0.013(2)
C11 0.025(2) 0.023(2) 0.0168(15) 0.0016(14) -0.0026(14) 0.0022(15)
C12 0.029(2) 0.019(2) 0.025(2) 0.001(2) -0.002(2) 0.003(2)
C13 0.028(2) 0.027(2) 0.018(2) -0.0028(14) 0.0003(15) -0.001(2)
C14 0.028(2) 0.023(2) 0.0150(14) -0.0010(14) -0.0011(15) 0.005(2)
C15 0.030(2) 0.042(2) 0.037(2) -0.003(2) 0.000(2) 0.010(2)
C16 0.045(3) 0.045(2) 0.037(2) 0.011(2) -0.014(2) 0.012(2)
C17 0.036(2) 0.037(2) 0.053(3) 0.002(2) -0.015(2) -0.006(2)
C18 0.053(3) 0.028(2) 0.046(2) -0.001(2) 0.015(2) -0.006(2)
C19 0.032(2) 0.049(3) 0.045(3) 0.005(2) 0.010(2) -0.001(2)
C20 0.060(3) 0.066(3) 0.026(2) 0.015(2) 0.009(2) 0.004(3)


#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Si1 C7 1.862(4) . ?
Si1 C5 1.867(4) . ?
Si1 C6 1.872(4) . ?
Si1 C4 1.890(4) . ?
Si4 C18 1.866(4) . ?
Si4 C19 1.872(4) . ?
Si4 C20 1.881(4) . ?
Si4 C14 1.889(4) . ?
Si3 C17 1.871(4) . ?
Si3 C15 1.870(4) . ?
Si3 C16 1.874(4) . ?
Si3 C14 1.887(4) . ?
Si2 C8 1.864(4) . ?
Si2 C9 1.869(4) . ?
Si2 C10 1.878(4) . ?
Si2 C4 1.887(3) . ?
N1 C2 1.274(4) . ?
N1 C1 1.479(5) . ?
N2 C2 1.371(5) . ?
N2 C3 1.388(5) . ?
N3 C3 1.260(5) . ?
N3 C1 1.471(4) . ?
N4 C12 1.275(4) . ?
N4 C11 1.478(4) . ?
N5 C12 1.371(4) . ?
N5 C13 1.380(5) . ?
N6 C13 1.263(4) . ?
N6 C11 1.480(4) . ?
C1 C4 1.550(4) . ?
C11 C14 1.536(5) . ?

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
C7 Si1 C5 109.5(2) . . ?
C7 Si1 C6 106.2(2) . . ?
C5 Si1 C6 109.9(2) . . ?
C7 Si1 C4 113.0(2) . . ?
C5 Si1 C4 111.5(2) . . ?
C6 Si1 C4 106.5(2) . . ?
C18 Si4 C19 108.9(2) . . ?
C18 Si4 C20 108.5(2) . . ?
C19 Si4 C20 106.6(2) . . ?
C18 Si4 C14 112.8(2) . . ?
C19 Si4 C14 111.5(2) . . ?
C20 Si4 C14 108.2(2) . . ?
C17 Si3 C15 109.4(2) . . ?
C17 Si3 C16 107.6(2) . . ?
C15 Si3 C16 108.2(2) . . ?
C17 Si3 C14 106.8(2) . . ?
C15 Si3 C14 111.3(2) . . ?
C16 Si3 C14 113.4(2) . . ?
C8 Si2 C9 106.0(2) . . ?
C8 Si2 C10 109.1(2) . . ?
C9 Si2 C10 109.3(2) . . ?
C8 Si2 C4 112.3(2) . . ?
C9 Si2 C4 107.6(2) . . ?
C10 Si2 C4 112.3(2) . . ?
C2 N1 C1 113.2(3) . . ?
C2 N2 C3 113.7(3) . . ?
C3 N3 C1 113.2(3) . . ?
C12 N4 C11 114.1(3) . . ?
C12 N5 C13 114.5(3) . . ?
C13 N6 C11 114.2(3) . . ?
N3 C1 N1 113.2(3) . . ?
N3 C1 C4 110.8(3) . . ?
N1 C1 C4 110.9(3) . . ?
N1 C2 N2 123.4(4) . . ?
N3 C3 N2 123.9(4) . . ?
C1 C4 Si2 114.4(2) . . ?
C1 C4 Si1 110.1(2) . . ?
Si2 C4 Si1 117.5(2) . . ?
N4 C11 N6 113.8(3) . . ?
N4 C11 C14 111.7(3) . . ?
N6 C11 C14 109.6(3) . . ?
N4 C12 N5 124.1(3) . . ?
N6 C13 N5 124.3(3) . . ?
C11 C14 Si3 109.1(2) . . ?
C11 C14 Si4 114.0(2) . . ?
Si3 C14 Si4 119.1(2) . . ?