data_01src073
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C9 H15 Cl3 N2 Si Sn'
_chemical_formula_weight          404.36
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sn'  'Sn'  -0.6537   1.4246
 '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                    9.2498(18)
_cell_length_b                    9.7081(19)
_cell_length_c                    17.738(4)
_cell_angle_alpha                 93.62(3)
_cell_angle_beta                  90.61(3)
_cell_angle_gamma                 104.26(3)
_cell_volume                      1540.1(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     18630
_cell_measurement_theta_min       1.00
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.744
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              792
_exptl_absorpt_coefficient_mu     2.235
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6634
_exptl_absorpt_correction_T_max   0.8074
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             23521
_diffrn_reflns_av_R_equivalents   0.0809
_diffrn_reflns_av_sigmaI/netI     0.0559
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          1.15
_diffrn_reflns_theta_max          27.46
_reflns_number_total              6924
_reflns_number_gt                 5961
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'COLLECT (Hooft, 1998)' 
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' 
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'CAMERON (Watkin, Pearce 1995)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0440P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0022(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          6924
_refine_ls_number_parameters      298
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0386
_refine_ls_R_factor_gt            0.0307
_refine_ls_wR_factor_ref          0.0812
_refine_ls_wR_factor_gt           0.0769
_refine_ls_goodness_of_fit_ref    0.980
_refine_ls_restrained_S_all       0.980
_refine_ls_shift/su_max           0.043
_refine_ls_shift/su_mean          0.002
 
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
C1 C 0.0035(3) 0.2624(2) 0.26032(14) 0.0220(5) Uani 1 1 d . . .
C2 C -0.1285(3) 0.2912(3) 0.28861(16) 0.0285(6) Uani 1 1 d . . .
H2 H -0.1519 0.2828 0.3404 0.034 Uiso 1 1 calc R . .
C3 C -0.2222(3) 0.3317(3) 0.23862(18) 0.0339(7) Uani 1 1 d . . .
H3 H -0.3115 0.3523 0.2566 0.041 Uiso 1 1 calc R . .
C4 C -0.1904(3) 0.3435(3) 0.16267(18) 0.0346(7) Uani 1 1 d . . .
H4 H -0.2568 0.3721 0.1293 0.042 Uiso 1 1 calc R . .
C5 C -0.0614(3) 0.3132(3) 0.13620(16) 0.0290(6) Uani 1 1 d . . .
C6 C -0.0159(3) 0.3179(3) 0.05529(16) 0.0426(7) Uani 1 1 d . . .
H6A H 0.0866 0.3759 0.0526 0.064 Uiso 1 1 calc R . .
H6B H -0.0831 0.3598 0.0263 0.064 Uiso 1 1 calc R . .
H6C H -0.0215 0.2210 0.0341 0.064 Uiso 1 1 calc R . .
C7 C 0.0405(3) 0.2912(3) 0.45393(17) 0.0401(7) Uani 1 1 d . . .
H7A H 0.0370 0.3838 0.4361 0.060 Uiso 1 1 calc R . .
H7B H 0.0815 0.3042 0.5058 0.060 Uiso 1 1 calc R . .
H7C H -0.0605 0.2287 0.4527 0.060 Uiso 1 1 calc R . .
C8 C 0.1392(4) 0.0213(3) 0.41274(18) 0.0444(8) Uani 1 1 d . . .
H8A H 0.0336 -0.0295 0.4076 0.067 Uiso 1 1 calc R . .
H8B H 0.1751 0.0172 0.4645 0.067 Uiso 1 1 calc R . .
H8C H 0.1972 -0.0235 0.3773 0.067 Uiso 1 1 calc R . .
C9 C 0.3585(3) 0.3120(4) 0.40759(19) 0.0466(8) Uani 1 1 d . . .
H9A H 0.4251 0.2558 0.3867 0.070 Uiso 1 1 calc R . .
H9B H 0.3796 0.3330 0.4619 0.070 Uiso 1 1 calc R . .
H9C H 0.3748 0.4015 0.3825 0.070 Uiso 1 1 calc R . .
C10 C -0.6235(3) -0.2808(2) 0.23682(14) 0.0228(5) Uani 1 1 d . . .
C11 C -0.7693(3) -0.3217(3) 0.20651(17) 0.0312(6) Uani 1 1 d . . .
H11 H -0.7879 -0.3250 0.1536 0.037 Uiso 1 1 calc R . .
C12 C -0.8838(3) -0.3567(3) 0.25508(18) 0.0341(7) Uani 1 1 d . . .
H12 H -0.9833 -0.3845 0.2353 0.041 Uiso 1 1 calc R . .
C13 C -0.8591(3) -0.3528(3) 0.33282(17) 0.0339(7) Uani 1 1 d . . .
H13 H -0.9404 -0.3780 0.3657 0.041 Uiso 1 1 calc R . .
C14 C -0.7148(3) -0.3120(3) 0.36124(16) 0.0306(6) Uani 1 1 d . . .
C15 C -0.6719(4) -0.2989(3) 0.44378(16) 0.0415(7) Uani 1 1 d . . .
H15A H -0.5938 -0.3491 0.4518 0.062 Uiso 1 1 calc R . .
H15B H -0.7594 -0.3409 0.4729 0.062 Uiso 1 1 calc R . .
H15C H -0.6345 -0.1980 0.4605 0.062 Uiso 1 1 calc R . .
C16 C -0.3029(3) -0.3231(3) 0.08276(18) 0.0404(7) Uani 1 1 d . . .
H16A H -0.2145 -0.2922 0.1164 0.061 Uiso 1 1 calc R . .
H16B H -0.2733 -0.3102 0.0303 0.061 Uiso 1 1 calc R . .
H16C H -0.3496 -0.4239 0.0886 0.061 Uiso 1 1 calc R . .
C17 C -0.3524(4) -0.0234(3) 0.09754(18) 0.0433(8) Uani 1 1 d . . .
H17A H -0.4260 0.0318 0.1089 0.065 Uiso 1 1 calc R . .
H17B H -0.3192 -0.0097 0.0456 0.065 Uiso 1 1 calc R . .
H17C H -0.2666 0.0091 0.1327 0.065 Uiso 1 1 calc R . .
C18 C -0.6028(4) -0.2759(3) 0.04223(16) 0.0409(7) Uani 1 1 d . . .
H18A H -0.6517 -0.3755 0.0499 0.061 Uiso 1 1 calc R . .
H18B H -0.5704 -0.2679 -0.0101 0.061 Uiso 1 1 calc R . .
H18C H -0.6731 -0.2167 0.0523 0.061 Uiso 1 1 calc R . .
N1 N 0.1149(2) 0.2182(2) 0.29565(12) 0.0233(4) Uani 1 1 d . . .
N2 N 0.0295(2) 0.2721(2) 0.18542(12) 0.0243(4) Uani 1 1 d . . .
N3 N -0.4883(2) -0.2394(2) 0.20267(12) 0.0247(5) Uani 1 1 d . . .
N4 N -0.6020(2) -0.2777(2) 0.31259(12) 0.0244(5) Uani 1 1 d . . .
Cl1 Cl 0.14769(9) 0.01469(8) 0.09993(4) 0.0446(2) Uani 1 1 d . . .
Cl2 Cl 0.40315(8) 0.07721(8) 0.25131(5) 0.04184(18) Uani 1 1 d . . .
Cl3 Cl 0.39713(7) 0.38054(7) 0.15316(5) 0.03904(18) Uani 1 1 d . . .
Cl4 Cl -0.30297(8) -0.38795(8) 0.36123(4) 0.03809(17) Uani 1 1 d . . .
Cl5 Cl -0.12398(7) -0.11446(9) 0.24907(5) 0.04330(19) Uani 1 1 d . . .
Cl6 Cl -0.34435(8) -0.01164(8) 0.39134(4) 0.03954(18) Uani 1 1 d . . .
Sn1 Sn 0.229335(18) 0.185994(17) 0.198833(9) 0.02289(8) Uani 1 1 d . . .
Sn2 Sn -0.358360(17) -0.199702(18) 0.301483(9) 0.02414(8) Uani 1 1 d . . .
Si1 Si 0.16100(8) 0.20922(8) 0.39166(4) 0.02720(16) Uani 1 1 d . . .
Si2 Si -0.43809(8) -0.21478(7) 0.10756(4) 0.02591(16) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 N2 1.358(3) . ?
C1 N1 1.371(3) . ?
C1 C2 1.408(3) . ?
C1 Sn1 2.611(2) . ?
C2 C3 1.374(4) . ?
C3 C4 1.388(4) . ?
C4 C5 1.378(4) . ?
C5 N2 1.350(3) . ?
C5 C6 1.500(4) . ?
C7 Si1 1.856(3) . ?
C8 Si1 1.848(3) . ?
C9 Si1 1.863(3) . ?
C10 N4 1.354(3) . ?
C10 N3 1.376(3) . ?
C10 C11 1.400(4) . ?
C10 Sn2 2.612(3) . ?
C11 C12 1.363(4) . ?
C12 C13 1.392(4) . ?
C13 C14 1.375(4) . ?
C14 N4 1.353(3) . ?
C14 C15 1.502(4) . ?
C16 Si2 1.861(3) . ?
C17 Si2 1.853(3) . ?
C18 Si2 1.856(3) . ?
N1 Si1 1.764(2) . ?
N1 Sn1 2.074(2) . ?
N2 Sn1 2.224(2) . ?
N3 Si2 1.770(2) . ?
N3 Sn2 2.075(2) . ?
N4 Sn2 2.209(2) . ?
Cl1 Sn1 2.3235(11) . ?
Cl2 Sn1 2.3441(9) . ?
Cl3 Sn1 2.3256(11) . ?
Cl4 Sn2 2.3279(9) . ?
Cl5 Sn2 2.3464(10) . ?
Cl6 Sn2 2.3244(10) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N2 C1 N1 110.4(2) . . ?
N2 C1 C2 118.8(2) . . ?
N1 C1 C2 130.7(2) . . ?
N2 C1 Sn1 58.44(12) . . ?
N1 C1 Sn1 52.13(12) . . ?
C2 C1 Sn1 173.70(18) . . ?
C3 C2 C1 117.6(3) . . ?
C2 C3 C4 122.0(3) . . ?
C5 C4 C3 119.3(3) . . ?
N2 C5 C4 118.5(3) . . ?
N2 C5 C6 116.9(2) . . ?
C4 C5 C6 124.6(3) . . ?
N4 C10 N3 109.8(2) . . ?
N4 C10 C11 119.0(2) . . ?
N3 C10 C11 131.2(2) . . ?
N4 C10 Sn2 57.70(13) . . ?
N3 C10 Sn2 52.14(12) . . ?
C11 C10 Sn2 176.35(19) . . ?
C12 C11 C10 118.1(3) . . ?
C11 C12 C13 121.9(3) . . ?
C14 C13 C12 118.9(3) . . ?
N4 C14 C13 118.8(3) . . ?
N4 C14 C15 116.6(2) . . ?
C13 C14 C15 124.6(3) . . ?
C1 N1 Si1 132.69(17) . . ?
C1 N1 Sn1 96.42(15) . . ?
Si1 N1 Sn1 130.56(11) . . ?
C5 N2 C1 123.8(2) . . ?
C5 N2 Sn1 145.79(18) . . ?
C1 N2 Sn1 90.22(15) . . ?
C10 N3 Si2 132.88(18) . . ?
C10 N3 Sn2 96.30(16) . . ?
Si2 N3 Sn2 130.69(11) . . ?
C14 N4 C10 123.3(2) . . ?
C14 N4 Sn2 145.54(19) . . ?
C10 N4 Sn2 91.09(15) . . ?
N1 Sn1 N2 62.73(8) . . ?
N1 Sn1 Cl1 127.00(6) . . ?
N2 Sn1 Cl1 91.64(6) . . ?
N1 Sn1 Cl3 118.44(7) . . ?
N2 Sn1 Cl3 95.51(6) . . ?
Cl1 Sn1 Cl3 108.99(4) . . ?
N1 Sn1 Cl2 98.93(6) . . ?
N2 Sn1 Cl2 161.00(6) . . ?
Cl1 Sn1 Cl2 96.43(4) . . ?
Cl3 Sn1 Cl2 98.05(3) . . ?
N1 Sn1 C1 31.45(8) . . ?
N2 Sn1 C1 31.34(8) . . ?
Cl1 Sn1 C1 110.47(6) . . ?
Cl3 Sn1 C1 110.88(6) . . ?
Cl2 Sn1 C1 130.00(6) . . ?
N3 Sn2 N4 62.76(8) . . ?
N3 Sn2 Cl6 126.03(6) . . ?
N4 Sn2 Cl6 92.58(6) . . ?
N3 Sn2 Cl4 119.98(6) . . ?
N4 Sn2 Cl4 94.28(6) . . ?
Cl6 Sn2 Cl4 108.33(3) . . ?
N3 Sn2 Cl5 98.82(6) . . ?
N4 Sn2 Cl5 161.45(6) . . ?
Cl6 Sn2 Cl5 97.40(4) . . ?
Cl4 Sn2 Cl5 97.33(4) . . ?
N3 Sn2 C10 31.56(8) . . ?
N4 Sn2 C10 31.20(8) . . ?
Cl6 Sn2 C10 111.25(6) . . ?
Cl4 Sn2 C10 110.03(6) . . ?
Cl5 Sn2 C10 130.32(6) . . ?
N1 Si1 C8 109.66(13) . . ?
N1 Si1 C7 110.85(13) . . ?
C8 Si1 C7 109.75(15) . . ?
N1 Si1 C9 107.12(14) . . ?
C8 Si1 C9 110.61(16) . . ?
C7 Si1 C9 108.82(14) . . ?
N3 Si2 C17 109.02(12) . . ?
N3 Si2 C18 111.36(12) . . ?
C17 Si2 C18 109.63(16) . . ?
N3 Si2 C16 108.36(13) . . ?
C17 Si2 C16 110.46(15) . . ?
C18 Si2 C16 108.00(14) . . ?
 
_diffrn_measured_fraction_theta_max    0.984
_diffrn_reflns_theta_full              27.46
_diffrn_measured_fraction_theta_full   0.984
_refine_diff_density_max    0.736
_refine_diff_density_min   -1.075
_refine_diff_density_rms    0.116
