# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Norbert Mitzel'
'Ina Kamps'
'Irina Langlitz'
'Andreas Mix'
'Beate Neumann'
'Hans-Georg Stammler'

_publ_contact_author_name        'Norbert Mitzel'
_publ_contact_author_email       MITZEL@UNI-BIELEFELD.DE

_publ_section_title              
;
Transmetallation and silylation products of aminal carbanions
;

# Attachment 'Compound_all.CIF'

data_ina01
_database_code_depnum_ccdc_archive 'CCDC 736454'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
'TMTAC-AlMe2 dimer'
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H40 Al2 N6'
_chemical_formula_weight         370.50

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.664(2)
_cell_length_b                   9.184(3)
_cell_length_c                   9.832(4)
_cell_angle_alpha                75.64(3)
_cell_angle_beta                 72.48(3)
_cell_angle_gamma                73.10(3)
_cell_volume                     540.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      4.81
_cell_measurement_theta_max      25.59

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             204
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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  'STOE IPDS-1'
_diffrn_measurement_method       '\phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7096
_diffrn_reflns_av_R_equivalents  0.1095
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.81
_diffrn_reflns_theta_max         25.59
_reflns_number_total             1838
_reflns_number_gt                1655
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE IPDS-1 software package'
_computing_cell_refinement       'STOE IPDS-1 softawre package'
_computing_data_reduction        'STOE X-Area'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.2970P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1838
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0935
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.146
_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
Al1 Al -0.16487(9) 1.15738(6) 0.60283(5) 0.01359(18) Uani 1 1 d . . .
N1 N 0.0410(2) 0.80766(16) 0.61496(15) 0.0143(3) Uani 1 1 d . . .
N2 N 0.0062(3) 0.92678(18) 0.82796(16) 0.0184(4) Uani 1 1 d . . .
N3 N 0.1318(3) 0.65147(18) 0.83661(17) 0.0224(4) Uani 1 1 d . . .
C1 C 0.0307(3) 0.95340(19) 0.67214(18) 0.0138(4) Uani 1 1 d . . .
H1A H 0.1798 0.9716 0.6302 0.020(5) Uiso 1 1 calc R . .
C2 C 0.1539(3) 0.7881(2) 0.8784(2) 0.0239(4) Uani 1 1 d . . .
H2A H 0.1246 0.7726 0.9852 0.024(6) Uiso 1 1 calc R . .
H2B H 0.3043 0.8003 0.8370 0.039(7) Uiso 1 1 calc R . .
C3 C 0.1909(3) 0.6715(2) 0.6794(2) 0.0198(4) Uani 1 1 d . . .
H3A H 0.1867 0.5772 0.6497 0.023(6) Uiso 1 1 calc R . .
H3B H 0.3407 0.6858 0.6422 0.023(6) Uiso 1 1 calc R . .
C4 C -0.1755(3) 0.7731(2) 0.6517(2) 0.0191(4) Uani 1 1 d . . .
H4A H -0.1676 0.6917 0.6007 0.029 Uiso 1 1 calc R . .
H4B H -0.2804 0.8666 0.6222 0.029 Uiso 1 1 calc R . .
H4C H -0.2211 0.7382 0.7564 0.029 Uiso 1 1 calc R . .
C5 C -0.2116(3) 0.9463(2) 0.9238(2) 0.0254(4) Uani 1 1 d . . .
H5A H -0.2045 0.9463 1.0219 0.038 Uiso 1 1 calc R . .
H5B H -0.2736 0.8611 0.9256 0.038 Uiso 1 1 calc R . .
H5C H -0.3028 1.0447 0.8882 0.038 Uiso 1 1 calc R . .
C6 C 0.2698(4) 0.5101(3) 0.8967(2) 0.0352(5) Uani 1 1 d . . .
H6A H 0.2542 0.4215 0.8653 0.053 Uiso 1 1 calc R . .
H6B H 0.2267 0.4959 1.0027 0.053 Uiso 1 1 calc R . .
H6C H 0.4210 0.5180 0.8623 0.053 Uiso 1 1 calc R . .
C7 C -0.1186(4) 1.3258(2) 0.6732(2) 0.0259(4) Uani 1 1 d . . .
H7A H -0.1576 1.4242 0.6090 0.039 Uiso 1 1 calc R . .
H7B H 0.0340 1.3052 0.6737 0.039 Uiso 1 1 calc R . .
H7C H -0.2092 1.3317 0.7717 0.039 Uiso 1 1 calc R . .
C8 C -0.4750(3) 1.1666(2) 0.6309(2) 0.0243(4) Uani 1 1 d . . .
H8D H -0.5555 1.2749 0.6179 0.036 Uiso 1 1 calc R . .
H8A H -0.5321 1.1143 0.7290 0.036 Uiso 1 1 calc R . .
H8B H -0.4910 1.1153 0.5598 0.036 Uiso 1 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
Al1 0.0150(3) 0.0142(3) 0.0115(3) -0.00336(17) -0.00213(19) -0.00367(18)
N1 0.0155(8) 0.0133(7) 0.0144(7) -0.0017(5) -0.0039(6) -0.0044(5)
N2 0.0209(8) 0.0231(8) 0.0105(7) -0.0015(5) -0.0051(6) -0.0043(6)
N3 0.0241(8) 0.0198(8) 0.0176(8) 0.0043(6) -0.0058(7) -0.0023(6)
C1 0.0158(9) 0.0162(8) 0.0110(8) -0.0028(6) -0.0031(6) -0.0061(6)
C2 0.0261(10) 0.0293(10) 0.0152(9) 0.0002(7) -0.0090(7) -0.0041(8)
C3 0.0207(9) 0.0173(8) 0.0174(9) 0.0005(7) -0.0045(7) -0.0017(7)
C4 0.0190(9) 0.0195(9) 0.0200(9) -0.0028(7) -0.0022(7) -0.0095(7)
C5 0.0264(10) 0.0318(10) 0.0132(9) -0.0039(7) 0.0000(8) -0.0049(8)
C6 0.0360(12) 0.0304(11) 0.0265(11) 0.0085(8) -0.0103(9) 0.0027(9)
C7 0.0321(11) 0.0226(9) 0.0260(10) -0.0108(8) -0.0060(8) -0.0067(8)
C8 0.0166(9) 0.0320(10) 0.0208(9) -0.0032(7) -0.0023(8) -0.0040(7)

_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 C7 1.976(2) . ?
Al1 C8 1.980(2) . ?
Al1 N1 2.0295(17) 2_576 ?
Al1 C1 2.0383(19) . ?
N1 C4 1.486(2) . ?
N1 C3 1.492(2) . ?
N1 C1 1.552(2) . ?
N1 Al1 2.0295(17) 2_576 ?
N2 C2 1.445(2) . ?
N2 C1 1.456(2) . ?
N2 C5 1.462(3) . ?
N3 C3 1.453(2) . ?
N3 C6 1.461(2) . ?
N3 C2 1.471(3) . ?
C1 H1A 1.0000 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8D 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Al1 C8 112.88(9) . . ?
C7 Al1 N1 106.26(8) . 2_576 ?
C8 Al1 N1 105.37(8) . 2_576 ?
C7 Al1 C1 109.31(9) . . ?
C8 Al1 C1 118.68(9) . . ?
N1 Al1 C1 103.06(7) 2_576 . ?
C4 N1 C3 108.71(14) . . ?
C4 N1 C1 111.73(13) . . ?
C3 N1 C1 109.70(15) . . ?
C4 N1 Al1 110.58(11) . 2_576 ?
C3 N1 Al1 107.56(11) . 2_576 ?
C1 N1 Al1 108.47(10) . 2_576 ?
C2 N2 C1 112.82(14) . . ?
C2 N2 C5 112.68(15) . . ?
C1 N2 C5 118.86(16) . . ?
C3 N3 C6 109.88(16) . . ?
C3 N3 C2 108.45(15) . . ?
C6 N3 C2 111.28(18) . . ?
N2 C1 N1 113.51(14) . . ?
N2 C1 Al1 111.75(11) . . ?
N1 C1 Al1 118.25(12) . . ?
N2 C1 H1A 103.8 . . ?
N1 C1 H1A 103.8 . . ?
Al1 C1 H1A 103.8 . . ?
N2 C2 N3 111.42(17) . . ?
N2 C2 H2A 109.3 . . ?
N3 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
N3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N3 C3 N1 111.29(14) . . ?
N3 C3 H3A 109.4 . . ?
N1 C3 H3A 109.4 . . ?
N3 C3 H3B 109.4 . . ?
N1 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Al1 C7 H7A 109.5 . . ?
Al1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Al1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Al1 C8 H8D 109.5 . . ?
Al1 C8 H8A 109.5 . . ?
H8D C8 H8A 109.5 . . ?
Al1 C8 H8B 109.5 . . ?
H8D C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C1 N1 47.2(2) . . . . ?
C5 N2 C1 N1 -88.02(19) . . . . ?
C2 N2 C1 Al1 -176.00(13) . . . . ?
C5 N2 C1 Al1 48.81(19) . . . . ?
C4 N1 C1 N2 74.94(18) . . . . ?
C3 N1 C1 N2 -45.69(19) . . . . ?
Al1 N1 C1 N2 -162.91(12) 2_576 . . . ?
C4 N1 C1 Al1 -58.89(16) . . . . ?
C3 N1 C1 Al1 -179.52(11) . . . . ?
Al1 N1 C1 Al1 63.26(13) 2_576 . . . ?
C7 Al1 C1 N2 52.31(15) . . . . ?
C8 Al1 C1 N2 -79.08(15) . . . . ?
N1 Al1 C1 N2 165.01(12) 2_576 . . . ?
C7 Al1 C1 N1 -173.10(12) . . . . ?
C8 Al1 C1 N1 55.50(15) . . . . ?
N1 Al1 C1 N1 -60.41(14) 2_576 . . . ?
C1 N2 C2 N3 -55.9(2) . . . . ?
C5 N2 C2 N3 82.1(2) . . . . ?
C3 N3 C2 N2 63.2(2) . . . . ?
C6 N3 C2 N2 -175.85(16) . . . . ?
C6 N3 C3 N1 175.18(17) . . . . ?
C2 N3 C3 N1 -63.0(2) . . . . ?
C4 N1 C3 N3 -68.5(2) . . . . ?
C1 N1 C3 N3 53.93(19) . . . . ?
Al1 N1 C3 N3 171.72(12) 2_576 . . . ?

_diffrn_measured_fraction_theta_max 0.909
_diffrn_reflns_theta_full        25.59
_diffrn_measured_fraction_theta_full 0.909
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.044

#===END

data_compound1b
_database_code_depnum_ccdc_archive 'CCDC 736455'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H48 Al2 N6'
_chemical_formula_sum            'C20 H48 Al2 N6'
_chemical_formula_weight         426.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2897(7)
_cell_length_b                   9.0162(6)
_cell_length_c                   9.7438(8)
_cell_angle_alpha                99.687(4)
_cell_angle_beta                 106.821(3)
_cell_angle_gamma                110.728(4)
_cell_volume                     621.47(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12671
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       needle
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             236
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9723
_exptl_absorpt_correction_T_max  0.9946
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_exptl_special_details           
;

;

_diffrn_ambient_temperature      100(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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9581
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2810
_reflns_number_gt                2136
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.3427P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2810
_refine_ls_number_parameters     132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1113
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Al1 Al 0.26872(8) 0.38822(7) 0.34152(7) 0.02001(17) Uani 1 1 d . . .
N1 N 0.5751(2) 0.36366(19) 0.59800(18) 0.0198(3) Uani 1 1 d . . .
N2 N 0.2410(2) 0.16484(19) 0.52466(19) 0.0218(4) Uani 1 1 d . . .
N3 N 0.4881(2) 0.13755(19) 0.70795(19) 0.0220(4) Uani 1 1 d . . .
C1 C 0.3669(2) 0.3300(2) 0.5329(2) 0.0202(4) Uani 1 1 d . . .
H1 H 0.3542 0.4067 0.6118 0.024 Uiso 1 1 calc R . .
C2 C 0.2971(3) 0.1254(2) 0.6637(2) 0.0235(4) Uani 1 1 d . . .
H2A H 0.2099 0.0111 0.6514 0.028 Uiso 1 1 calc R . .
H2B H 0.2903 0.2030 0.7445 0.028 Uiso 1 1 calc R . .
C3 C 0.6145(3) 0.3097(2) 0.7358(2) 0.0224(4) Uani 1 1 d . . .
H3A H 0.7445 0.3219 0.7712 0.027 Uiso 1 1 calc R . .
H3B H 0.6022 0.3828 0.8163 0.027 Uiso 1 1 calc R . .
C4 C 0.6291(3) 0.2768(2) 0.4868(2) 0.0216(4) Uani 1 1 d . . .
H4A H 0.7638 0.3103 0.5288 0.032 Uiso 1 1 calc R . .
H4B H 0.5961 0.3069 0.3939 0.032 Uiso 1 1 calc R . .
H4C H 0.5630 0.1562 0.4648 0.032 Uiso 1 1 calc R . .
C5 C 0.1784(3) 0.0258(2) 0.3908(2) 0.0247(4) Uani 1 1 d . . .
H5A H 0.2833 0.0002 0.3888 0.037 Uiso 1 1 calc R . .
H5B H 0.1308 0.0562 0.3005 0.037 Uiso 1 1 calc R . .
H5C H 0.0793 -0.0720 0.3933 0.037 Uiso 1 1 calc R . .
C6 C 0.5360(3) 0.0905(3) 0.8461(2) 0.0275(5) Uani 1 1 d . . .
H6A H 0.6652 0.1042 0.8782 0.041 Uiso 1 1 calc R . .
H6B H 0.4526 -0.0259 0.8270 0.041 Uiso 1 1 calc R . .
H6C H 0.5221 0.1619 0.9253 0.041 Uiso 1 1 calc R . .
C7 C 0.0071(3) 0.3489(2) 0.3124(2) 0.0255(4) Uani 1 1 d . . .
H7A H -0.0698 0.2275 0.2668 0.031 Uiso 1 1 calc R . .
H7B H 0.0043 0.3779 0.4140 0.031 Uiso 1 1 calc R . .
C8 C -0.0951(3) 0.4342(3) 0.2199(3) 0.0312(5) Uani 1 1 d . . .
H8A H -0.0384 0.5536 0.2729 0.047 Uiso 1 1 calc R . .
H8B H -0.2267 0.3857 0.2067 0.047 Uiso 1 1 calc R . .
H8C H -0.0853 0.4176 0.1211 0.047 Uiso 1 1 calc R . .
C9 C 0.2994(3) 0.2855(2) 0.1582(2) 0.0244(4) Uani 1 1 d . . .
H9A H 0.4135 0.3646 0.1517 0.029 Uiso 1 1 calc R . .
H9B H 0.3170 0.1844 0.1688 0.029 Uiso 1 1 calc R . .
C10 C 0.1336(3) 0.2380(3) 0.0111(3) 0.0376(6) Uani 1 1 d . . .
H10A H 0.0182 0.1674 0.0197 0.056 Uiso 1 1 calc R . .
H10B H 0.1513 0.1772 -0.0725 0.056 Uiso 1 1 calc R . .
H10C H 0.1256 0.3391 -0.0077 0.056 Uiso 1 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
Al1 0.0164(3) 0.0186(3) 0.0228(3) 0.0075(2) 0.0046(2) 0.0068(2)
N1 0.0153(8) 0.0204(8) 0.0220(8) 0.0077(7) 0.0046(7) 0.0070(6)
N2 0.0170(8) 0.0195(8) 0.0260(9) 0.0097(7) 0.0054(7) 0.0055(7)
N3 0.0189(8) 0.0211(8) 0.0256(9) 0.0113(7) 0.0062(7) 0.0079(7)
C1 0.0149(9) 0.0179(9) 0.0262(10) 0.0076(8) 0.0052(8) 0.0069(7)
C2 0.0195(10) 0.0236(10) 0.0290(11) 0.0129(9) 0.0093(9) 0.0084(8)
C3 0.0196(10) 0.0214(9) 0.0226(10) 0.0084(8) 0.0045(8) 0.0069(8)
C4 0.0187(10) 0.0213(9) 0.0253(10) 0.0078(8) 0.0076(8) 0.0093(8)
C5 0.0190(10) 0.0199(9) 0.0295(11) 0.0082(9) 0.0046(9) 0.0054(8)
C6 0.0279(11) 0.0267(10) 0.0281(11) 0.0141(9) 0.0074(9) 0.0118(9)
C7 0.0178(10) 0.0251(10) 0.0303(11) 0.0101(9) 0.0057(9) 0.0073(8)
C8 0.0201(11) 0.0340(11) 0.0367(13) 0.0127(10) 0.0052(9) 0.0121(9)
C9 0.0233(10) 0.0217(9) 0.0247(10) 0.0067(8) 0.0070(9) 0.0075(8)
C10 0.0343(13) 0.0479(14) 0.0241(12) 0.0060(10) 0.0084(10) 0.0148(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
Al1 C7 1.994(2) . ?
Al1 C9 1.997(2) . ?
Al1 N1 2.0231(17) 2_666 ?
Al1 C1 2.042(2) . ?
N1 C3 1.491(2) . ?
N1 C4 1.494(2) . ?
N1 C1 1.550(2) . ?
N1 Al1 2.0231(16) 2_666 ?
N2 C2 1.447(2) . ?
N2 C1 1.457(2) . ?
N2 C5 1.463(3) . ?
N3 C3 1.457(2) . ?
N3 C6 1.466(2) . ?
N3 C2 1.473(2) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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 1.542(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.537(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Al1 C9 114.43(9) . . ?
C7 Al1 N1 108.36(8) . 2_666 ?
C9 Al1 N1 107.02(8) . 2_666 ?
C7 Al1 C1 105.46(8) . . ?
C9 Al1 C1 117.90(8) . . ?
N1 Al1 C1 102.78(7) 2_666 . ?
C3 N1 C4 109.49(14) . . ?
C3 N1 C1 109.78(14) . . ?
C4 N1 C1 112.23(15) . . ?
C3 N1 Al1 107.85(12) . 2_666 ?
C4 N1 Al1 109.15(12) . 2_666 ?
C1 N1 Al1 108.23(10) . 2_666 ?
C2 N2 C1 112.40(15) . . ?
C2 N2 C5 113.26(15) . . ?
C1 N2 C5 118.77(16) . . ?
C3 N3 C6 109.38(15) . . ?
C3 N3 C2 107.97(14) . . ?
C6 N3 C2 109.59(15) . . ?
N2 C1 N1 113.14(14) . . ?
N2 C1 Al1 110.87(12) . . ?
N1 C1 Al1 119.14(12) . . ?
N2 C1 H1 103.9 . . ?
N1 C1 H1 103.9 . . ?
Al1 C1 H1 103.9 . . ?
N2 C2 N3 111.61(16) . . ?
N2 C2 H2A 109.3 . . ?
N3 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
N3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N3 C3 N1 111.83(15) . . ?
N3 C3 H3A 109.2 . . ?
N1 C3 H3A 109.2 . . ?
N3 C3 H3B 109.2 . . ?
N1 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 Al1 122.53(14) . . ?
C8 C7 H7A 106.7 . . ?
Al1 C7 H7A 106.7 . . ?
C8 C7 H7B 106.7 . . ?
Al1 C7 H7B 106.7 . . ?
H7A C7 H7B 106.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 Al1 113.81(14) . . ?
C10 C9 H9A 108.8 . . ?
Al1 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
Al1 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.057

#===END

data_compound1c
_database_code_depnum_ccdc_archive 'CCDC 736456'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H48 Ga2 N6'
_chemical_formula_sum            'C20 H48 Ga2 N6'
_chemical_formula_weight         512.08

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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5157(9)
_cell_length_b                   9.2989(7)
_cell_length_c                   9.7039(6)
_cell_angle_alpha                69.657(6)
_cell_angle_beta                 64.465(9)
_cell_angle_gamma                71.805(9)
_cell_volume                     638.02(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    40
_cell_measurement_theta_min      4.604
_cell_measurement_theta_max      20.526

_exptl_crystal_description       rhomb
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             272
_exptl_absorpt_coefficient_mu    2.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5677
_exptl_absorpt_correction_T_max  0.6756
_exptl_absorpt_process_details   'SADABS - Bruker Nonius - V2.10'

_exptl_special_details           
;

;

_diffrn_ambient_temperature      100(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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21456
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         30.00
_reflns_number_total             3712
_reflns_number_gt                3459
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        
'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.2244P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3712
_refine_ls_number_parameters     132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0172
_refine_ls_wR_factor_ref         0.0423
_refine_ls_wR_factor_gt          0.0408
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Ga1 Ga 0.505523(14) 0.404276(12) 0.703216(13) 0.00898(4) Uani 1 1 d . . .
N1 N 0.54489(11) 0.35138(9) 0.39498(10) 0.00980(15) Uani 1 1 d . . .
N2 N 0.73161(12) 0.15803(10) 0.54481(10) 0.01203(16) Uani 1 1 d . . .
N3 N 0.72976(12) 0.11350(10) 0.31438(10) 0.01282(16) Uani 1 1 d . . .
C1 C 0.64215(13) 0.31987(11) 0.50628(12) 0.01007(17) Uani 1 1 d . . .
H1 H 0.7407 0.3797 0.4431 0.012 Uiso 1 1 calc R . .
C2 C 0.83674(14) 0.09758(12) 0.40640(13) 0.01417(19) Uani 1 1 d . . .
H2A H 0.8887 -0.0141 0.4393 0.017 Uiso 1 1 calc R . .
H2B H 0.9355 0.1547 0.3391 0.017 Uiso 1 1 calc R . .
C3 C 0.66358(14) 0.27974(12) 0.26065(12) 0.01223(18) Uani 1 1 d . . .
H3A H 0.5978 0.2938 0.1926 0.015 Uiso 1 1 calc R . .
H3B H 0.7652 0.3340 0.1966 0.015 Uiso 1 1 calc R . .
C4 C 0.37627(13) 0.29083(12) 0.47397(12) 0.01298(19) Uani 1 1 d . . .
H4A H 0.3192 0.3156 0.3976 0.019 Uiso 1 1 calc R . .
H4B H 0.2968 0.3398 0.5609 0.019 Uiso 1 1 calc R . .
H4C H 0.4019 0.1773 0.5153 0.019 Uiso 1 1 calc R . .
C5 C 0.63293(15) 0.04589(12) 0.67906(13) 0.0169(2) Uani 1 1 d . . .
H5A H 0.5498 0.0194 0.6508 0.025 Uiso 1 1 calc R . .
H5B H 0.5670 0.0923 0.7696 0.025 Uiso 1 1 calc R . .
H5C H 0.7160 -0.0491 0.7066 0.025 Uiso 1 1 calc R . .
C6 C 0.83869(15) 0.04896(13) 0.17671(13) 0.0185(2) Uani 1 1 d . . .
H6A H 0.7661 0.0620 0.1161 0.028 Uiso 1 1 calc R . .
H6B H 0.8852 -0.0624 0.2117 0.028 Uiso 1 1 calc R . .
H6C H 0.9376 0.1042 0.1103 0.028 Uiso 1 1 calc R . .
C7 C 0.66657(15) 0.37024(13) 0.81706(13) 0.0173(2) Uani 1 1 d . . .
H7A H 0.6268 0.4566 0.8691 0.021 Uiso 1 1 calc R . .
H7B H 0.6505 0.2724 0.9014 0.021 Uiso 1 1 calc R . .
C8 C 0.86496(16) 0.35959(15) 0.72051(17) 0.0250(3) Uani 1 1 d . . .
H8A H 0.9050 0.2822 0.6590 0.037 Uiso 1 1 calc R . .
H8B H 0.9303 0.3279 0.7917 0.037 Uiso 1 1 calc R . .
H8C H 0.8868 0.4618 0.6490 0.037 Uiso 1 1 calc R . .
C9 C 0.26595(14) 0.35294(12) 0.84794(12) 0.01466(19) Uani 1 1 d . . .
H9A H 0.1748 0.4305 0.8089 0.018 Uiso 1 1 calc R . .
H9B H 0.2623 0.2489 0.8444 0.018 Uiso 1 1 calc R . .
C10 C 0.21899(17) 0.35172(15) 1.02016(14) 0.0234(2) Uani 1 1 d . . .
H10A H 0.3112 0.2785 1.0585 0.035 Uiso 1 1 calc R . .
H10B H 0.1047 0.3190 1.0854 0.035 Uiso 1 1 calc R . .
H10C H 0.2111 0.4569 1.0263 0.035 Uiso 1 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
Ga1 0.01008(6) 0.00808(5) 0.00982(5) -0.00266(4) -0.00484(4) -0.00080(4)
N1 0.0095(4) 0.0093(4) 0.0112(4) -0.0040(3) -0.0040(3) -0.0007(3)
N2 0.0137(4) 0.0083(4) 0.0124(4) -0.0025(3) -0.0054(3) 0.0010(3)
N3 0.0152(4) 0.0094(4) 0.0135(4) -0.0054(3) -0.0052(3) 0.0009(3)
C1 0.0112(4) 0.0085(4) 0.0119(4) -0.0028(3) -0.0061(4) -0.0006(3)
C2 0.0136(5) 0.0121(4) 0.0160(5) -0.0054(4) -0.0061(4) 0.0019(4)
C3 0.0146(5) 0.0101(4) 0.0114(4) -0.0043(3) -0.0047(4) 0.0001(3)
C4 0.0117(4) 0.0124(4) 0.0168(5) -0.0043(4) -0.0056(4) -0.0033(3)
C5 0.0206(5) 0.0108(5) 0.0160(5) -0.0012(4) -0.0066(4) -0.0011(4)
C6 0.0213(5) 0.0151(5) 0.0180(5) -0.0096(4) -0.0054(4) 0.0016(4)
C7 0.0204(5) 0.0173(5) 0.0189(5) -0.0047(4) -0.0132(4) -0.0006(4)
C8 0.0185(5) 0.0256(6) 0.0367(7) -0.0127(5) -0.0169(5) 0.0038(4)
C9 0.0152(5) 0.0137(5) 0.0144(5) -0.0035(4) -0.0030(4) -0.0054(4)
C10 0.0253(6) 0.0267(6) 0.0145(5) -0.0022(4) -0.0017(5) -0.0113(5)

_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
Ga1 C7 1.9984(11) . ?
Ga1 C9 2.0086(11) . ?
Ga1 C1 2.0439(10) . ?
Ga1 N1 2.1197(9) 2_666 ?
N1 C3 1.4872(13) . ?
N1 C4 1.4907(13) . ?
N1 C1 1.5291(13) . ?
N1 Ga1 2.1197(9) 2_666 ?
N2 C2 1.4476(13) . ?
N2 C1 1.4571(12) . ?
N2 C5 1.4662(14) . ?
N3 C3 1.4588(13) . ?
N3 C6 1.4652(13) . ?
N3 C2 1.4746(13) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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 1.5287(17) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.5383(16) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Ga1 C9 113.14(5) . . ?
C7 Ga1 C1 109.82(4) . . ?
C9 Ga1 C1 119.76(4) . . ?
C7 Ga1 N1 105.55(4) . 2_666 ?
C9 Ga1 N1 104.76(4) . 2_666 ?
C1 Ga1 N1 102.06(4) . 2_666 ?
C3 N1 C4 109.39(7) . . ?
C3 N1 C1 109.32(7) . . ?
C4 N1 C1 113.12(8) . . ?
C3 N1 Ga1 106.25(6) . 2_666 ?
C4 N1 Ga1 110.30(6) . 2_666 ?
C1 N1 Ga1 108.22(6) . 2_666 ?
C2 N2 C1 112.41(8) . . ?
C2 N2 C5 113.26(8) . . ?
C1 N2 C5 119.08(8) . . ?
C3 N3 C6 108.94(8) . . ?
C3 N3 C2 107.78(8) . . ?
C6 N3 C2 110.53(8) . . ?
N2 C1 N1 113.88(8) . . ?
N2 C1 Ga1 111.20(6) . . ?
N1 C1 Ga1 117.03(6) . . ?
N2 C1 H1 104.4 . . ?
N1 C1 H1 104.4 . . ?
Ga1 C1 H1 104.4 . . ?
N2 C2 N3 111.72(8) . . ?
N2 C2 H2A 109.3 . . ?
N3 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
N3 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
N3 C3 N1 111.78(8) . . ?
N3 C3 H3A 109.3 . . ?
N1 C3 H3A 109.3 . . ?
N3 C3 H3B 109.3 . . ?
N1 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 Ga1 117.69(8) . . ?
C8 C7 H7A 107.9 . . ?
Ga1 C7 H7A 107.9 . . ?
C8 C7 H7B 107.9 . . ?
Ga1 C7 H7B 107.9 . . ?
H7A C7 H7B 107.2 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 Ga1 113.67(8) . . ?
C10 C9 H9A 108.8 . . ?
Ga1 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
Ga1 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.054

#===END

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 736457'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            TM-Triazin-TMS
_chemical_melting_point          275
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H23 N3 Si'
_chemical_formula_weight         201.39

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.919(3)
_cell_length_b                   8.764(3)
_cell_length_c                   10.073(4)
_cell_angle_alpha                98.46(3)
_cell_angle_beta                 111.72(3)
_cell_angle_gamma                94.88(3)
_cell_volume                     634.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'zonemelting of frozen liquid in a capillary'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             224
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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  'STOE IPDS-1'
_diffrn_measurement_method       'Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8438
_diffrn_reflns_av_R_equivalents  0.1212
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.85
_diffrn_reflns_theta_max         25.60
_reflns_number_total             2184
_reflns_number_gt                1856
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE IPDS-1'
_computing_cell_refinement       'X-AREA (STOE 2003)'
_computing_data_reduction        'X-AREA (STOE 2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL 5.01'
_computing_publication_material  'SHELXTL 5.01'

_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.2781P] 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    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2184
_refine_ls_number_parameters     188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1043
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_restrained_S_all      1.165
_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
Si1 Si 1.04375(8) 0.87798(6) 0.76624(6) 0.02205(19) Uani 1 1 d . . .
N1 N 0.6770(2) 0.70032(19) 0.64123(19) 0.0213(4) Uani 1 1 d . . .
N3 N 0.9027(2) 0.61431(18) 0.84219(19) 0.0209(4) Uani 1 1 d . . .
N2 N 0.5917(2) 0.4792(2) 0.7315(2) 0.0251(4) Uani 1 1 d . . .
C2 C 0.8426(3) 0.7501(2) 0.7778(2) 0.0183(4) Uani 1 1 d . . .
C1 C 0.5318(3) 0.6146(2) 0.6700(3) 0.0249(4) Uani 1 1 d . . .
H1A H 0.490(4) 0.686(3) 0.741(3) 0.030 Uiso 1 1 d . . .
H1B H 0.424(4) 0.581(3) 0.578(3) 0.030 Uiso 1 1 d . . .
C3 C 0.7537(3) 0.5316(2) 0.8674(2) 0.0260(5) Uani 1 1 d . . .
H3A H 0.721(4) 0.608(3) 0.938(3) 0.031 Uiso 1 1 d . . .
H3B H 0.794(4) 0.444(3) 0.911(3) 0.031 Uiso 1 1 d . . .
C4 C 0.9723(3) 0.5083(2) 0.7550(3) 0.0289(5) Uani 1 1 d . . .
H4A H 1.006(4) 0.422(4) 0.804(3) 0.043 Uiso 1 1 d . . .
H4B H 1.085(4) 0.561(3) 0.752(3) 0.043 Uiso 1 1 d . . .
H4C H 0.880(4) 0.464(3) 0.651(4) 0.043 Uiso 1 1 d . . .
C8 C 1.0737(4) 0.8186(3) 0.5915(3) 0.0341(5) Uani 1 1 d . . .
H8A H 1.174(5) 0.883(4) 0.591(4) 0.051 Uiso 1 1 d . . .
H8B H 0.965(5) 0.821(4) 0.503(4) 0.051 Uiso 1 1 d . . .
H8C H 1.102(4) 0.716(4) 0.577(4) 0.051 Uiso 1 1 d . . .
C9 C 1.2558(3) 0.8644(3) 0.9241(3) 0.0345(5) Uani 1 1 d . . .
H9A H 1.356(5) 0.930(4) 0.920(4) 0.052 Uiso 1 1 d . . .
H9B H 1.290(4) 0.757(4) 0.919(4) 0.052 Uiso 1 1 d . . .
H9C H 1.243(5) 0.890(4) 1.004(4) 0.052 Uiso 1 1 d . . .
C7 C 1.0095(4) 1.0876(3) 0.7865(3) 0.0355(6) Uani 1 1 d . . .
H7A H 1.113(5) 1.151(4) 0.788(4) 0.053 Uiso 1 1 d . . .
H7B H 0.990(5) 1.122(4) 0.865(4) 0.053 Uiso 1 1 d . . .
H7C H 0.893(5) 1.108(4) 0.701(4) 0.053 Uiso 1 1 d . . .
C6 C 0.6055(4) 0.8330(3) 0.5780(3) 0.0322(5) Uani 1 1 d . . .
H6A H 0.492(5) 0.792(3) 0.488(4) 0.048 Uiso 1 1 d . . .
H6B H 0.693(4) 0.884(4) 0.543(4) 0.048 Uiso 1 1 d . . .
H6C H 0.576(4) 0.915(4) 0.654(4) 0.048 Uiso 1 1 d . . .
C5 C 0.4435(4) 0.3954(3) 0.7586(3) 0.0395(6) Uani 1 1 d . . .
H5A H 0.480(5) 0.305(4) 0.791(4) 0.059 Uiso 1 1 d . . .
H5B H 0.333(5) 0.367(4) 0.665(4) 0.059 Uiso 1 1 d . . .
H5C H 0.403(5) 0.469(4) 0.834(4) 0.059 Uiso 1 1 d . . .
H1 H 0.802(3) 0.810(3) 0.851(3) 0.022(6) Uiso 1 1 d . . .

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 0.0270(3) 0.0183(3) 0.0196(3) 0.00219(19) 0.0090(3) 0.00012(19)
N1 0.0187(8) 0.0243(8) 0.0165(9) 0.0040(6) 0.0011(8) 0.0060(6)
N3 0.0187(8) 0.0177(7) 0.0210(9) 0.0053(6) 0.0011(8) 0.0024(6)
N2 0.0181(9) 0.0263(8) 0.0258(10) 0.0038(7) 0.0046(8) -0.0028(6)
C2 0.0219(10) 0.0153(8) 0.0157(10) 0.0017(7) 0.0051(9) 0.0053(7)
C1 0.0173(10) 0.0331(11) 0.0223(12) 0.0035(8) 0.0055(10) 0.0064(8)
C3 0.0244(11) 0.0275(10) 0.0210(11) 0.0091(8) 0.0026(10) -0.0017(8)
C4 0.0249(11) 0.0200(9) 0.0384(14) 0.0045(9) 0.0076(11) 0.0089(8)
C8 0.0387(14) 0.0384(13) 0.0300(13) 0.0064(10) 0.0185(12) 0.0071(10)
C9 0.0256(12) 0.0386(13) 0.0316(14) 0.0033(10) 0.0060(12) -0.0054(9)
C7 0.0543(16) 0.0208(10) 0.0326(14) 0.0034(9) 0.0201(14) 0.0008(10)
C6 0.0317(12) 0.0347(11) 0.0294(13) 0.0143(10) 0.0057(12) 0.0157(10)
C5 0.0277(13) 0.0451(14) 0.0424(16) 0.0098(11) 0.0122(13) -0.0091(10)

_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 C9 1.864(3) . ?
Si1 C8 1.867(2) . ?
Si1 C7 1.873(2) . ?
Si1 C2 1.918(2) . ?
N1 C1 1.461(3) . ?
N1 C6 1.463(3) . ?
N1 C2 1.481(3) . ?
N3 C3 1.453(3) . ?
N3 C4 1.464(3) . ?
N3 C2 1.469(2) . ?
N2 C1 1.453(3) . ?
N2 C5 1.463(3) . ?
N2 C3 1.464(3) . ?
C2 H1 1.00(2) . ?
C1 H1A 1.04(3) . ?
C1 H1B 0.98(3) . ?
C3 H3A 1.02(3) . ?
C3 H3B 0.95(3) . ?
C4 H4A 0.96(3) . ?
C4 H4B 0.98(3) . ?
C4 H4C 1.03(3) . ?
C8 H8A 0.94(3) . ?
C8 H8B 0.99(4) . ?
C8 H8C 0.95(4) . ?
C9 H9A 0.96(3) . ?
C9 H9B 1.00(3) . ?
C9 H9C 0.84(4) . ?
C7 H7A 0.95(4) . ?
C7 H7B 0.88(4) . ?
C7 H7C 1.05(4) . ?
C6 H6A 1.00(3) . ?
C6 H6B 1.00(3) . ?
C6 H6C 1.07(3) . ?
C5 H5A 0.93(4) . ?
C5 H5B 1.00(4) . ?
C5 H5C 1.08(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
C9 Si1 C8 110.44(13) . . ?
C9 Si1 C7 106.78(13) . . ?
C8 Si1 C7 108.89(12) . . ?
C9 Si1 C2 107.64(11) . . ?
C8 Si1 C2 112.61(11) . . ?
C7 Si1 C2 110.31(11) . . ?
C1 N1 C6 107.98(17) . . ?
C1 N1 C2 109.81(16) . . ?
C6 N1 C2 112.15(17) . . ?
C3 N3 C4 110.74(17) . . ?
C3 N3 C2 109.93(16) . . ?
C4 N3 C2 113.23(17) . . ?
C1 N2 C5 110.10(19) . . ?
C1 N2 C3 108.78(17) . . ?
C5 N2 C3 110.47(19) . . ?
N3 C2 N1 110.29(15) . . ?
N3 C2 Si1 111.33(13) . . ?
N1 C2 Si1 116.36(14) . . ?
N3 C2 H1 102.9(14) . . ?
N1 C2 H1 106.7(14) . . ?
Si1 C2 H1 108.2(13) . . ?
N2 C1 N1 111.33(17) . . ?
N2 C1 H1A 109.2(15) . . ?
N1 C1 H1A 111.1(14) . . ?
N2 C1 H1B 109.8(15) . . ?
N1 C1 H1B 108.7(15) . . ?
H1A C1 H1B 107(2) . . ?
N3 C3 N2 111.18(17) . . ?
N3 C3 H3A 107.3(14) . . ?
N2 C3 H3A 109.3(15) . . ?
N3 C3 H3B 109.8(15) . . ?
N2 C3 H3B 110.0(17) . . ?
H3A C3 H3B 109(2) . . ?
N3 C4 H4A 107.5(18) . . ?
N3 C4 H4B 109.8(17) . . ?
H4A C4 H4B 107(2) . . ?
N3 C4 H4C 114.5(16) . . ?
H4A C4 H4C 108(2) . . ?
H4B C4 H4C 109(2) . . ?
Si1 C8 H8A 110(2) . . ?
Si1 C8 H8B 114.5(18) . . ?
H8A C8 H8B 109(3) . . ?
Si1 C8 H8C 114(2) . . ?
H8A C8 H8C 105(3) . . ?
H8B C8 H8C 105(3) . . ?
Si1 C9 H9A 108(2) . . ?
Si1 C9 H9B 112(2) . . ?
H9A C9 H9B 105(3) . . ?
Si1 C9 H9C 111(2) . . ?
H9A C9 H9C 111(3) . . ?
H9B C9 H9C 108(3) . . ?
Si1 C7 H7A 110(2) . . ?
Si1 C7 H7B 114(2) . . ?
H7A C7 H7B 108(3) . . ?
Si1 C7 H7C 112.9(18) . . ?
H7A C7 H7C 108(3) . . ?
H7B C7 H7C 104(3) . . ?
N1 C6 H6A 108.3(18) . . ?
N1 C6 H6B 110.2(18) . . ?
H6A C6 H6B 105(3) . . ?
N1 C6 H6C 111.7(18) . . ?
H6A C6 H6C 111(2) . . ?
H6B C6 H6C 111(2) . . ?
N2 C5 H5A 109(2) . . ?
N2 C5 H5B 108(2) . . ?
H5A C5 H5B 109(3) . . ?
N2 C5 H5C 111.5(18) . . ?
H5A C5 H5C 112(3) . . ?
H5B C5 H5C 106(3) . . ?

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
C3 N3 C2 N1 -56.9(2) . . . . ?
C4 N3 C2 N1 67.6(2) . . . . ?
C3 N3 C2 Si1 172.40(13) . . . . ?
C4 N3 C2 Si1 -63.16(19) . . . . ?
C1 N1 C2 N3 56.36(19) . . . . ?
C6 N1 C2 N3 176.43(16) . . . . ?
C1 N1 C2 Si1 -175.62(13) . . . . ?
C6 N1 C2 Si1 -55.55(19) . . . . ?
C9 Si1 C2 N3 -32.28(17) . . . . ?
C8 Si1 C2 N3 89.68(17) . . . . ?
C7 Si1 C2 N3 -148.44(15) . . . . ?
C9 Si1 C2 N1 -159.80(14) . . . . ?
C8 Si1 C2 N1 -37.83(17) . . . . ?
C7 Si1 C2 N1 84.05(16) . . . . ?
C5 N2 C1 N1 -179.79(19) . . . . ?
C3 N2 C1 N1 59.0(2) . . . . ?
C6 N1 C1 N2 179.28(18) . . . . ?
C2 N1 C1 N2 -58.1(2) . . . . ?
C4 N3 C3 N2 -67.0(2) . . . . ?
C2 N3 C3 N2 58.9(2) . . . . ?
C1 N2 C3 N3 -59.4(2) . . . . ?
C5 N2 C3 N3 179.66(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        25.60
_diffrn_measured_fraction_theta_full 0.914
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.044

_vrf_PLAT029_compound2           
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.91
RESPONSE: 1-circle goniometer of STOE diffractometer and space group
(rotation around the spindle axis only)
;

#===END

data_compound4a
_database_code_depnum_ccdc_archive 'CCDC 736458'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H28 Al N3 Si'
_chemical_formula_sum            'C11 H28 Al N3 Si'
_chemical_formula_weight         257.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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                   6.7450(3)
_cell_length_b                   19.6403(8)
_cell_length_c                   12.0390(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.308(3)
_cell_angle_gamma                90.00
_cell_volume                     1594.44(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    1024
_cell_measurement_theta_min      8.617
_cell_measurement_theta_max      139.374

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             568
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_T_max  0.9512
_exptl_absorpt_process_details   'SADABS - Bruker Nonius - V2.10'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  'goebel mirror'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8452
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0734
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.31
_diffrn_reflns_theta_max         65.99
_reflns_number_total             2717
_reflns_number_gt                1942
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1187P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2717
_refine_ls_number_parameters     152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1650
_refine_ls_wR_factor_gt          0.1469
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_restrained_S_all      0.896
_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
Al1 Al 0.62240(12) 0.24920(4) 0.23370(7) 0.0254(3) Uani 1 1 d . . .
Si1 Si 0.47533(12) 0.11891(4) 0.35153(7) 0.0263(3) Uani 1 1 d . . .
N1 N 0.5775(3) 0.16365(11) 0.13844(19) 0.0227(5) Uani 1 1 d . . .
N2 N 0.5897(3) 0.04048(11) 0.1536(2) 0.0259(6) Uani 1 1 d . . .
N3 N 0.6800(4) 0.09518(12) -0.0159(2) 0.0289(6) Uani 1 1 d . . .
C1 C 0.6168(4) 0.10416(13) 0.2152(2) 0.0230(6) Uani 1 1 d . . .
H1 H 0.7610 0.1064 0.2360 0.028 Uiso 1 1 calc R . .
C2 C 0.7213(4) 0.03823(15) 0.0590(2) 0.0308(7) Uani 1 1 d . . .
H2A H 0.8610 0.0404 0.0858 0.037 Uiso 1 1 calc R . .
H2B H 0.7020 -0.0052 0.0184 0.037 Uiso 1 1 calc R . .
C3 C 0.7111(4) 0.15892(14) 0.0428(2) 0.0269(7) Uani 1 1 d . . .
H3A H 0.6852 0.1975 -0.0084 0.032 Uiso 1 1 calc R . .
H3B H 0.8507 0.1619 0.0696 0.032 Uiso 1 1 calc R . .
C4 C 0.3669(4) 0.16387(15) 0.0973(3) 0.0292(7) Uani 1 1 d . . .
H4A H 0.3508 0.1975 0.0376 0.044 Uiso 1 1 calc R . .
H4B H 0.2798 0.1757 0.1585 0.044 Uiso 1 1 calc R . .
H4C H 0.3318 0.1186 0.0688 0.044 Uiso 1 1 calc R . .
C5 C 0.6335(5) -0.01843(15) 0.2244(3) 0.0355(8) Uani 1 1 d . . .
H5A H 0.7683 -0.0143 0.2559 0.053 Uiso 1 1 calc R . .
H5B H 0.6233 -0.0602 0.1801 0.053 Uiso 1 1 calc R . .
H5C H 0.5385 -0.0203 0.2847 0.053 Uiso 1 1 calc R . .
C6 C 0.8083(5) 0.09232(18) -0.1125(3) 0.0393(8) Uani 1 1 d . . .
H6A H 0.7793 0.1312 -0.1614 0.059 Uiso 1 1 calc R . .
H6B H 0.7837 0.0498 -0.1532 0.059 Uiso 1 1 calc R . .
H6C H 0.9475 0.0941 -0.0875 0.059 Uiso 1 1 calc R . .
C7 C 0.9096(4) 0.25653(16) 0.2673(3) 0.0409(9) Uani 1 1 d . . .
H7A H 0.9818 0.2596 0.1978 0.061 Uiso 1 1 calc R . .
H7B H 0.9541 0.2162 0.3089 0.061 Uiso 1 1 calc R . .
H7C H 0.9355 0.2974 0.3120 0.061 Uiso 1 1 calc R . .
C8 C 0.5168(5) 0.32360(16) 0.1398(3) 0.0420(9) Uani 1 1 d . . .
H8A H 0.5591 0.3675 0.1710 0.063 Uiso 1 1 calc R . .
H8B H 0.3716 0.3214 0.1371 0.063 Uiso 1 1 calc R . .
H8C H 0.5672 0.3189 0.0644 0.063 Uiso 1 1 calc R . .
C9 C 0.4665(4) 0.21342(15) 0.3592(2) 0.0301(7) Uani 1 1 d . . .
H9A H 0.5243 0.2293 0.4310 0.036 Uiso 1 1 calc R . .
H9B H 0.3275 0.2295 0.3531 0.036 Uiso 1 1 calc R . .
C10 C 0.6315(5) 0.08294(17) 0.4671(3) 0.0388(8) Uani 1 1 d . . .
H10A H 0.7630 0.1042 0.4670 0.058 Uiso 1 1 calc R . .
H10B H 0.6451 0.0337 0.4569 0.058 Uiso 1 1 calc R . .
H10C H 0.5686 0.0921 0.5381 0.058 Uiso 1 1 calc R . .
C11 C 0.2264(4) 0.07640(16) 0.3454(3) 0.0363(8) Uani 1 1 d . . .
H11A H 0.1523 0.0885 0.4117 0.054 Uiso 1 1 calc R . .
H11B H 0.2441 0.0269 0.3426 0.054 Uiso 1 1 calc R . .
H11C H 0.1528 0.0916 0.2788 0.054 Uiso 1 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
Al1 0.0284(5) 0.0168(5) 0.0310(5) -0.0008(3) 0.0037(4) 0.0005(3)
Si1 0.0286(5) 0.0236(5) 0.0269(5) 0.0008(3) 0.0033(3) -0.0031(3)
N1 0.0223(12) 0.0188(12) 0.0271(13) 0.0030(10) 0.0020(9) 0.0029(9)
N2 0.0306(14) 0.0137(12) 0.0335(14) -0.0007(10) 0.0050(10) 0.0004(10)
N3 0.0361(15) 0.0212(12) 0.0298(14) -0.0046(11) 0.0083(11) 0.0009(11)
C1 0.0225(15) 0.0168(14) 0.0298(15) 0.0008(12) 0.0018(11) 0.0014(11)
C2 0.0345(17) 0.0186(15) 0.0394(18) -0.0038(13) 0.0078(13) 0.0040(12)
C3 0.0310(16) 0.0199(15) 0.0302(16) 0.0006(13) 0.0056(12) 0.0023(12)
C4 0.0279(16) 0.0260(16) 0.0338(17) 0.0012(13) 0.0001(12) 0.0034(12)
C5 0.0436(19) 0.0177(15) 0.045(2) 0.0046(14) 0.0019(15) 0.0000(13)
C6 0.046(2) 0.0381(19) 0.0343(18) -0.0057(15) 0.0151(14) 0.0042(16)
C7 0.0334(19) 0.0333(19) 0.056(2) -0.0059(16) 0.0021(16) -0.0043(14)
C8 0.057(2) 0.0256(17) 0.044(2) 0.0011(15) 0.0057(17) 0.0038(15)
C9 0.0334(17) 0.0268(16) 0.0302(16) -0.0037(13) 0.0041(13) 0.0028(13)
C10 0.049(2) 0.0350(18) 0.0322(17) 0.0064(15) -0.0053(14) -0.0076(15)
C11 0.0307(18) 0.0357(19) 0.0427(19) 0.0018(15) 0.0086(14) -0.0070(14)

_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 C8 1.971(3) . ?
Al1 C7 1.976(3) . ?
Al1 C9 1.989(3) . ?
Al1 N1 2.053(2) . ?
Si1 C9 1.859(3) . ?
Si1 C10 1.865(3) . ?
Si1 C11 1.875(3) . ?
Si1 C1 1.940(3) . ?
N1 C3 1.481(3) . ?
N1 C4 1.494(3) . ?
N1 C1 1.509(3) . ?
N2 C1 1.463(3) . ?
N2 C5 1.463(4) . ?
N2 C2 1.461(3) . ?
N3 C3 1.450(4) . ?
N3 C2 1.459(4) . ?
N3 C6 1.467(3) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 Al1 C7 113.79(15) . . ?
C8 Al1 C9 120.50(14) . . ?
C7 Al1 C9 113.77(15) . . ?
C8 Al1 N1 103.86(13) . . ?
C7 Al1 N1 107.79(12) . . ?
C9 Al1 N1 93.53(11) . . ?
C9 Si1 C10 111.05(14) . . ?
C9 Si1 C11 114.62(14) . . ?
C10 Si1 C11 110.53(15) . . ?
C9 Si1 C1 102.03(12) . . ?
C10 Si1 C1 107.12(14) . . ?
C11 Si1 C1 110.97(14) . . ?
C3 N1 C4 109.5(2) . . ?
C3 N1 C1 109.0(2) . . ?
C4 N1 C1 110.9(2) . . ?
C3 N1 Al1 113.65(17) . . ?
C4 N1 Al1 108.05(16) . . ?
C1 N1 Al1 105.68(16) . . ?
C1 N2 C5 111.1(2) . . ?
C1 N2 C2 110.5(2) . . ?
C5 N2 C2 108.2(2) . . ?
C3 N3 C2 109.7(2) . . ?
C3 N3 C6 109.8(2) . . ?
C2 N3 C6 110.7(2) . . ?
N2 C1 N1 109.5(2) . . ?
N2 C1 Si1 119.87(18) . . ?
N1 C1 Si1 108.63(17) . . ?
N2 C1 H1 106.0 . . ?
N1 C1 H1 106.0 . . ?
Si1 C1 H1 106.0 . . ?
N3 C2 N2 110.4(2) . . ?
N3 C2 H2A 109.6 . . ?
N2 C2 H2A 109.6 . . ?
N3 C2 H2B 109.6 . . ?
N2 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N3 C3 N1 110.4(2) . . ?
N3 C3 H3A 109.6 . . ?
N1 C3 H3A 109.6 . . ?
N3 C3 H3B 109.6 . . ?
N1 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Al1 C7 H7A 109.5 . . ?
Al1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Al1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Al1 C8 H8A 109.5 . . ?
Al1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Al1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 Al1 107.25(14) . . ?
Si1 C9 H9A 110.3 . . ?
Al1 C9 H9A 110.3 . . ?
Si1 C9 H9B 110.3 . . ?
Al1 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        65.99
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.085

#===END

data_compound4b
_database_code_depnum_ccdc_archive 'CCDC 736459'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H28 Ga N3 Si'
_chemical_formula_sum            'C11 H28 Ga N3 Si'
_chemical_formula_weight         300.17

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'
Ga Ga 0.2307 1.6083 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   6.69260(10)
_cell_length_b                   19.4695(5)
_cell_length_c                   12.1088(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9260(15)
_cell_angle_gamma                90.00
_cell_volume                     1577.59(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30021
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       fragment
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    1.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6924
_exptl_absorpt_correction_T_max  0.8995
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_exptl_special_details           
;

;

_diffrn_ambient_temperature      100(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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30750
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3617
_reflns_number_gt                3084
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.4766P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3617
_refine_ls_number_parameters     152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0683
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.002
_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
Ga1 Ga 0.61436(3) 0.252839(8) 0.238750(14) 0.01952(7) Uani 1 1 d . . .
Si1 Si 0.46837(6) 0.11769(2) 0.35119(4) 0.02012(11) Uani 1 1 d . . .
N1 N 0.56851(19) 0.16288(7) 0.13866(10) 0.0183(3) Uani 1 1 d . . .
N2 N 0.5851(2) 0.03907(7) 0.15428(11) 0.0209(3) Uani 1 1 d . . .
N3 N 0.6764(2) 0.09468(7) -0.01449(11) 0.0220(3) Uani 1 1 d . . .
C1 C 0.6102(2) 0.10376(8) 0.21517(13) 0.0190(3) Uani 1 1 d . . .
H1 H 0.7555 0.1068 0.2351 0.023 Uiso 1 1 calc R . .
C2 C 0.7191(2) 0.03761(8) 0.05982(13) 0.0227(3) Uani 1 1 d . . .
H2A H 0.8595 0.0404 0.0864 0.027 Uiso 1 1 calc R . .
H2B H 0.7019 -0.0063 0.0195 0.027 Uiso 1 1 calc R . .
C3 C 0.7045(2) 0.15908(8) 0.04426(13) 0.0209(3) Uani 1 1 d . . .
H3A H 0.6777 0.1980 -0.0065 0.025 Uiso 1 1 calc R . .
H3B H 0.8446 0.1627 0.0711 0.025 Uiso 1 1 calc R . .
C4 C 0.3572(2) 0.16360(8) 0.09904(13) 0.0220(3) Uani 1 1 d . . .
H4A H 0.3412 0.1977 0.0401 0.033 Uiso 1 1 calc R . .
H4B H 0.2699 0.1755 0.1604 0.033 Uiso 1 1 calc R . .
H4C H 0.3210 0.1181 0.0706 0.033 Uiso 1 1 calc R . .
C5 C 0.6318(3) -0.02023(9) 0.22465(14) 0.0261(4) Uani 1 1 d . . .
H5A H 0.6205 -0.0625 0.1810 0.039 Uiso 1 1 calc R . .
H5B H 0.5378 -0.0220 0.2858 0.039 Uiso 1 1 calc R . .
H5C H 0.7684 -0.0159 0.2542 0.039 Uiso 1 1 calc R . .
C6 C 0.8076(3) 0.09213(9) -0.10993(14) 0.0284(4) Uani 1 1 d . . .
H6A H 0.9471 0.0962 -0.0849 0.043 Uiso 1 1 calc R . .
H6B H 0.7748 0.1301 -0.1602 0.043 Uiso 1 1 calc R . .
H6C H 0.7888 0.0483 -0.1487 0.043 Uiso 1 1 calc R . .
C7 C 0.9059(3) 0.25806(9) 0.26837(16) 0.0305(4) Uani 1 1 d . . .
H7A H 0.9761 0.2632 0.1984 0.046 Uiso 1 1 calc R . .
H7B H 0.9507 0.2159 0.3054 0.046 Uiso 1 1 calc R . .
H7C H 0.9351 0.2977 0.3159 0.046 Uiso 1 1 calc R . .
C8 C 0.5036(3) 0.32586(9) 0.14198(15) 0.0306(4) Uani 1 1 d . . .
H8A H 0.5465 0.3708 0.1698 0.046 Uiso 1 1 calc R . .
H8B H 0.3573 0.3234 0.1415 0.046 Uiso 1 1 calc R . .
H8C H 0.5520 0.3195 0.0667 0.046 Uiso 1 1 calc R . .
C9 C 0.4540(2) 0.21257(8) 0.36121(13) 0.0227(3) Uani 1 1 d . . .
H9A H 0.5082 0.2281 0.4336 0.027 Uiso 1 1 calc R . .
H9B H 0.3132 0.2278 0.3545 0.027 Uiso 1 1 calc R . .
C10 C 0.6289(3) 0.08194(10) 0.46503(14) 0.0293(4) Uani 1 1 d . . .
H10A H 0.7591 0.1049 0.4654 0.044 Uiso 1 1 calc R . .
H10B H 0.6476 0.0326 0.4534 0.044 Uiso 1 1 calc R . .
H10C H 0.5641 0.0895 0.5360 0.044 Uiso 1 1 calc R . .
C11 C 0.2187(2) 0.07395(9) 0.34768(14) 0.0265(4) Uani 1 1 d . . .
H11A H 0.1485 0.0836 0.4164 0.040 Uiso 1 1 calc R . .
H11B H 0.2378 0.0243 0.3401 0.040 Uiso 1 1 calc R . .
H11C H 0.1395 0.0911 0.2848 0.040 Uiso 1 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
Ga1 0.01957(11) 0.01678(11) 0.02218(11) -0.00096(7) -0.00017(7) 0.00053(6)
Si1 0.0200(2) 0.0209(2) 0.0195(2) 0.00037(17) 0.00056(16) -0.00116(17)
N1 0.0182(6) 0.0185(7) 0.0181(6) 0.0007(5) 0.0003(5) 0.0011(5)
N2 0.0229(7) 0.0167(7) 0.0231(7) -0.0007(5) 0.0016(5) 0.0008(5)
N3 0.0242(7) 0.0210(7) 0.0208(6) -0.0026(5) 0.0044(5) 0.0011(5)
C1 0.0177(7) 0.0155(7) 0.0236(8) 0.0014(6) -0.0017(6) 0.0002(6)
C2 0.0227(8) 0.0192(8) 0.0262(8) -0.0025(6) 0.0019(6) 0.0022(6)
C3 0.0223(8) 0.0191(8) 0.0214(8) -0.0010(6) 0.0019(6) 0.0005(6)
C4 0.0190(8) 0.0230(8) 0.0239(8) -0.0016(6) -0.0026(6) 0.0022(6)
C5 0.0313(9) 0.0174(8) 0.0296(9) 0.0030(7) -0.0006(7) 0.0016(7)
C6 0.0307(9) 0.0306(9) 0.0240(8) -0.0032(7) 0.0082(7) 0.0018(7)
C7 0.0218(9) 0.0281(10) 0.0415(12) -0.0048(8) -0.0019(8) -0.0023(7)
C8 0.0392(10) 0.0235(9) 0.0291(9) 0.0031(7) 0.0013(8) 0.0062(7)
C9 0.0238(8) 0.0227(9) 0.0217(8) -0.0033(6) 0.0010(6) -0.0007(6)
C10 0.0322(10) 0.0308(9) 0.0248(9) 0.0039(7) -0.0045(7) -0.0056(7)
C11 0.0227(8) 0.0289(9) 0.0281(9) 0.0005(7) 0.0029(7) -0.0031(7)

_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
Ga1 C8 1.9789(17) . ?
Ga1 C7 1.9808(18) . ?
Ga1 C9 2.0042(16) . ?
Ga1 N1 2.1492(13) . ?
Si1 C9 1.8539(17) . ?
Si1 C10 1.8684(17) . ?
Si1 C11 1.8751(17) . ?
Si1 C1 1.9333(16) . ?
N1 C3 1.4742(19) . ?
N1 C4 1.486(2) . ?
N1 C1 1.501(2) . ?
N2 C2 1.465(2) . ?
N2 C5 1.466(2) . ?
N2 C1 1.468(2) . ?
N3 C3 1.452(2) . ?
N3 C2 1.455(2) . ?
N3 C6 1.463(2) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 Ga1 C7 115.40(8) . . ?
C8 Ga1 C9 121.28(7) . . ?
C7 Ga1 C9 115.08(8) . . ?
C8 Ga1 N1 101.70(7) . . ?
C7 Ga1 N1 105.97(6) . . ?
C9 Ga1 N1 91.44(6) . . ?
C9 Si1 C10 110.66(8) . . ?
C9 Si1 C11 114.01(8) . . ?
C10 Si1 C11 110.42(8) . . ?
C9 Si1 C1 102.84(7) . . ?
C10 Si1 C1 106.97(8) . . ?
C11 Si1 C1 111.49(7) . . ?
C3 N1 C4 110.26(12) . . ?
C3 N1 C1 109.23(12) . . ?
C4 N1 C1 111.89(12) . . ?
C3 N1 Ga1 113.19(9) . . ?
C4 N1 Ga1 107.50(9) . . ?
C1 N1 Ga1 104.68(9) . . ?
C2 N2 C5 108.13(13) . . ?
C2 N2 C1 110.02(12) . . ?
C5 N2 C1 111.24(13) . . ?
C3 N3 C2 109.51(12) . . ?
C3 N3 C6 109.99(13) . . ?
C2 N3 C6 110.38(13) . . ?
N2 C1 N1 109.23(12) . . ?
N2 C1 Si1 119.65(11) . . ?
N1 C1 Si1 109.24(10) . . ?
N2 C1 H1 105.9 . . ?
N1 C1 H1 105.9 . . ?
Si1 C1 H1 105.9 . . ?
N3 C2 N2 110.59(13) . . ?
N3 C2 H2A 109.5 . . ?
N2 C2 H2A 109.5 . . ?
N3 C2 H2B 109.5 . . ?
N2 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N3 C3 N1 110.28(12) . . ?
N3 C3 H3A 109.6 . . ?
N1 C3 H3A 109.6 . . ?
N3 C3 H3B 109.6 . . ?
N1 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Ga1 C7 H7A 109.5 . . ?
Ga1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Ga1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Ga1 C8 H8A 109.5 . . ?
Ga1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Ga1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 Ga1 108.20(8) . . ?
Si1 C9 H9A 110.1 . . ?
Ga1 C9 H9A 110.1 . . ?
Si1 C9 H9B 110.1 . . ?
Ga1 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.065

#===END