#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/17/7011750.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_7011750
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 Ga N Sn3'
_chemical_formula_weight         814.84
_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                   12.9467(10)
_cell_length_b                   12.9467(10)
_cell_length_c                   12.9467(10)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2170.1(3)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'BRUKER axs SHELXTL-PLUS'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker axs CCD 1000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5337
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    10.151
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.486
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.389
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0001P)²+195.7444P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.1921
_reflns_number_gt                1265
_reflns_number_total             1299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203489c.txt
_cod_data_source_block           md394
_cod_original_sg_symbol_H-M      P2(1)3
_cod_database_code               7011750
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 0.92217(14) 1.02577(14) 1.14592(14) 0.0265(4) Uani 1 1 d . . .
Br1 Br 0.9486(2) 0.9370(3) 0.7366(2) 0.0417(8) Uani 1 1 d . . .
Ga1 Ga 0.9120 0.9120 0.9120 0.0270(10) Uani 1 3 d S . .
N1 N 0.9992 0.9992 0.9992 0.020(7) Uiso 1 3 d S . .
C1 C 1.044(3) 1.068(2) 1.254(2) 0.042(8) Uani 1 1 d . . .
H1A H 1.0145 1.0774 1.3216 0.063 Uiso 1 1 calc R . .
H1B H 1.0754 1.1314 1.2320 0.063 Uiso 1 1 calc R . .
H1C H 1.0946 1.0144 1.2563 0.063 Uiso 1 1 calc R . .
C2 C 0.820(3) 1.155(2) 1.119(2) 0.044(8) Uani 1 1 d . . .
H2A H 0.7633 1.1333 1.0766 0.066 Uiso 1 1 calc R . .
H2B H 0.8574 1.2091 1.0844 0.066 Uiso 1 1 calc R . .
H2C H 0.7945 1.1802 1.1838 0.066 Uiso 1 1 calc R . .
C3 C 0.853(3) 0.883(3) 1.194(3) 0.061(11) Uani 1 1 d . . .
H3A H 0.7809 0.8942 1.2089 0.091 Uiso 1 1 calc R . .
H3B H 0.8871 0.8575 1.2541 0.091 Uiso 1 1 calc R . .
H3C H 0.8586 0.8330 1.1390 0.091 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 0.0259(9) 0.0285(10) 0.0251(9) -0.0038(7) 0.0016(8) -0.0033(7)
Br1 0.0437(18) 0.054(2) 0.0278(14) -0.0048(13) -0.0035(12) -0.0045(14)
Ga1 0.0270(10) 0.0270(10) 0.0270(10) -0.0027(12) -0.0027(12) -0.0027(12)
C1 0.07(2) 0.042(17) 0.017(12) -0.006(12) 0.018(13) 0.011(16)
C2 0.06(2) 0.040(18) 0.034(17) -0.006(14) -0.007(14) -0.008(15)
C3 0.05(2) 0.10(3) 0.037(18) -0.010(18) -0.017(16) 0.01(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ga Ga 0.2307 1.6083 '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'
Sn Sn -0.6537 1.4246 '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'
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'
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
C3 Sn1 C2 117.2(13) . . ?
C3 Sn1 N1 107.9(10) . . ?
C2 Sn1 N1 105.2(8) . . ?
C3 Sn1 C1 109.6(12) . . ?
C2 Sn1 C1 110.5(11) . . ?
N1 Sn1 C1 105.7(7) . . ?
N1 Ga1 Br1 111.31(8) . . ?
N1 Ga1 Br1 111.31(8) . 9 ?
Br1 Ga1 Br1 107.58(8) . 9 ?
N1 Ga1 Br1 111.31(8) . 5 ?
Br1 Ga1 Br1 107.58(8) . 5 ?
Br1 Ga1 Br1 107.58(8) 9 5 ?
Ga1 N1 Sn1 109.36(5) . 5 ?
Ga1 N1 Sn1 109.36(5) . . ?
Sn1 N1 Sn1 109.58(5) 5 . ?
Ga1 N1 Sn1 109.36(5) . 9 ?
Sn1 N1 Sn1 109.58(5) 5 9 ?
Sn1 N1 Sn1 109.58(5) . 9 ?
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 C3 2.15(4) . ?
Sn1 C2 2.16(3) . ?
Sn1 N1 2.1731(18) . ?
Sn1 C1 2.18(3) . ?
Br1 Ga1 2.342(3) . ?
Ga1 N1 1.95385(16) . ?
Ga1 Br1 2.342(3) 9 ?
Ga1 Br1 2.342(3) 5 ?
N1 Sn1 2.1731(18) 5 ?
N1 Sn1 2.1731(18) 9 ?
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 Ga1 N1 Sn1 -84.76(10) . . . 5 ?
Br1 Ga1 N1 Sn1 35.24(10) 9 . . 5 ?
Br1 Ga1 N1 Sn1 155.24(10) 5 . . 5 ?
Br1 Ga1 N1 Sn1 155.24(10) . . . . ?
Br1 Ga1 N1 Sn1 -84.76(10) 9 . . . ?
Br1 Ga1 N1 Sn1 35.24(10) 5 . . . ?
Br1 Ga1 N1 Sn1 35.24(10) . . . 9 ?
Br1 Ga1 N1 Sn1 155.24(10) 9 . . 9 ?
Br1 Ga1 N1 Sn1 -84.76(10) 5 . . 9 ?
C3 Sn1 N1 Ga1 41.2(10) . . . . ?
C2 Sn1 N1 Ga1 -84.6(9) . . . . ?
C1 Sn1 N1 Ga1 158.4(8) . . . . ?
C3 Sn1 N1 Sn1 -78.6(10) . . . 5 ?
C2 Sn1 N1 Sn1 155.5(9) . . . 5 ?
C1 Sn1 N1 Sn1 38.6(8) . . . 5 ?
C3 Sn1 N1 Sn1 161.1(10) . . . 9 ?
C2 Sn1 N1 Sn1 35.3(9) . . . 9 ?
C1 Sn1 N1 Sn1 -81.7(8) . . . 9 ?
