#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/17/7011745.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7011745
loop_
_publ_author_name
'Q. m. Cheng'
'O. Stark'
'K. Merz'
'M. Winter'
'R. A. Fischer'
_publ_section_title
;
 Lewis base properties of tris(trimethylstannyl)amine: unusually short
 M--N bonds of the adduct compounds [X3M·N(SnMe3)3] (X = Cl, Br;
 M = Al, Ga, In) and [Cl2(CH3)M·N(SnMe3)3] (M = Al, Ga)
;
_journal_issue                   14
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              2933
_journal_page_last               2936
_journal_paper_doi               10.1039/b203489c
_journal_year                    2002
_chemical_formula_sum            'C9 H27 Br3 In N Sn3'
_chemical_formula_weight         859.94
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.989(3)
_cell_length_b                   12.989(3)
_cell_length_c                   12.989(3)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2191.4(9)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Bruker axs SHELXTL-97'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker axs CCD 1000'
_diffrn_measurement_method       \scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3882
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    9.875
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.028(17)
_refine_ls_extinction_coef       0.00083(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0141P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0440
_reflns_number_gt                1145
_reflns_number_total             1277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203489c.txt
_cod_data_source_block           md433
_cod_original_cell_volume        2191.4(8)
_cod_original_sg_symbol_H-M      P2(1)3
_cod_database_code               7011745
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.10091(3) 0.27802(3) 0.82422(4) 0.02735(14) Uani 1 1 d . . .
In1 In 0.34238(3) 0.15762(3) 0.84238(3) 0.0293(2) Uani 1 3 d S . .
Br1 Br 0.52908(5) 0.18459(6) 0.80113(6) 0.0452(2) Uani 1 1 d . . .
N1 N 0.2465(4) 0.2535(4) 0.7465(4) 0.027(2) Uani 1 3 d S . .
C1 C 0.1269(5) 0.4005(5) 0.9287(5) 0.0381(18) Uani 1 1 d . . .
H11 H 0.0631 0.4350 0.9426 0.057 Uiso 1 1 calc R . .
H12 H 0.1748 0.4484 0.8991 0.057 Uiso 1 1 calc R . .
H13 H 0.1547 0.3737 0.9917 0.057 Uiso 1 1 calc R . .
C2 C 0.0606(5) 0.1385(5) 0.8996(6) 0.0398(19) Uani 1 1 d . . .
H21 H 0.1116 0.0870 0.8850 0.060 Uiso 1 1 calc R . .
H22 H -0.0053 0.1155 0.8754 0.060 Uiso 1 1 calc R . .
H23 H 0.0574 0.1500 0.9726 0.060 Uiso 1 1 calc R . .
C3 C -0.0095(5) 0.3193(6) 0.7087(6) 0.0450(19) Uani 1 1 d . . .
H31 H -0.0778 0.3073 0.7344 0.067 Uiso 1 1 calc R . .
H32 H 0.0016 0.2783 0.6482 0.067 Uiso 1 1 calc R . .
H33 H -0.0018 0.3908 0.6916 0.067 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
Sn1 0.0246(3) 0.0292(3) 0.0283(3) 0.0008(2) 0.0018(2) 0.0032(2)
In1 0.0293(2) 0.0293(2) 0.0293(2) 0.0052(2) -0.0052(2) 0.0052(2)
Br1 0.0292(4) 0.0577(5) 0.0486(5) 0.0046(4) -0.0041(3) 0.0037(4)
N1 0.027(2) 0.027(2) 0.027(2) 0.003(2) -0.003(2) 0.003(2)
C1 0.041(5) 0.039(4) 0.033(4) -0.001(3) 0.009(3) 0.007(4)
C2 0.037(4) 0.037(5) 0.045(5) 0.008(4) 0.009(4) 0.006(3)
C3 0.035(4) 0.054(5) 0.046(5) 0.000(4) -0.009(4) 0.017(4)
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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'
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
C1 Sn1 C2 112.6(3) . . ?
C1 Sn1 C3 111.6(3) . . ?
C2 Sn1 C3 111.8(3) . . ?
C1 Sn1 N1 105.64(19) . . ?
C2 Sn1 N1 107.7(3) . . ?
C3 Sn1 N1 107.1(3) . . ?
N1 In1 Br1 110.75(2) . 6_456 ?
N1 In1 Br1 110.75(2) . . ?
Br1 In1 Br1 108.17(3) 6_456 . ?
N1 In1 Br1 110.75(2) . 12_565 ?
Br1 In1 Br1 108.17(3) 6_456 12_565 ?
Br1 In1 Br1 108.17(3) . 12_565 ?
In1 N1 Sn1 108.6(2) . 12_565 ?
In1 N1 Sn1 108.6(2) . 6_456 ?
Sn1 N1 Sn1 110.3(2) 12_565 6_456 ?
In1 N1 Sn1 108.6(2) . . ?
Sn1 N1 Sn1 110.3(2) 12_565 . ?
Sn1 N1 Sn1 110.3(2) 6_456 . ?
Sn1 C1 H11 109.5 . . ?
Sn1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
Sn1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
Sn1 C2 H21 109.5 . . ?
Sn1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
Sn1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
Sn1 C3 H31 109.5 . . ?
Sn1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
Sn1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
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
Sn1 C1 2.119(7) . ?
Sn1 C2 2.125(6) . ?
Sn1 C3 2.144(6) . ?
Sn1 N1 2.167(3) . ?
In1 N1 2.158(8) . ?
In1 Br1 2.5081(9) 6_456 ?
In1 Br1 2.5081(9) . ?
In1 Br1 2.5081(9) 12_565 ?
N1 Sn1 2.167(3) 12_565 ?
N1 Sn1 2.167(3) 6_456 ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
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
Br1 In1 N1 Sn1 -35.99(2) 6_456 . . 12_565 ?
Br1 In1 N1 Sn1 84.01(2) . . . 12_565 ?
Br1 In1 N1 Sn1 -155.99(2) 12_565 . . 12_565 ?
Br1 In1 N1 Sn1 -155.99(2) 6_456 . . 6_456 ?
Br1 In1 N1 Sn1 -35.99(2) . . . 6_456 ?
Br1 In1 N1 Sn1 84.01(2) 12_565 . . 6_456 ?
Br1 In1 N1 Sn1 84.01(2) 6_456 . . . ?
Br1 In1 N1 Sn1 -155.99(2) . . . . ?
Br1 In1 N1 Sn1 -35.99(2) 12_565 . . . ?
C1 Sn1 N1 In1 82.8(2) . . . . ?
C2 Sn1 N1 In1 -37.8(2) . . . . ?
C3 Sn1 N1 In1 -158.2(2) . . . . ?
C1 Sn1 N1 Sn1 -158.3(3) . . . 12_565 ?
C2 Sn1 N1 Sn1 81.2(4) . . . 12_565 ?
C3 Sn1 N1 Sn1 -39.2(4) . . . 12_565 ?
C1 Sn1 N1 Sn1 -36.2(4) . . . 6_456 ?
C2 Sn1 N1 Sn1 -156.7(3) . . . 6_456 ?
C3 Sn1 N1 Sn1 82.9(3) . . . 6_456 ?
