#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:00:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179821 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/17/7011751.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_7011751
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 Al Cl3 N Si0 Sn3'
_chemical_formula_weight         638.72
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   12.6514(15)
_cell_length_b                   13.0879(16)
_cell_length_c                   12.6514(16)
_cell_measurement_reflns_used    89
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      23.7
_cell_measurement_theta_min      4.01
_cell_volume                     2094.8(4)
_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 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker axs CCD 1000'
_diffrn_measurement_method       omega-scan
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4832
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    3.959
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5345
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1208
_refine_diff_density_max         3.734
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.263
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2941
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1335P)²+22.9284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                2806
_reflns_number_total             2941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203489c.txt
_cod_data_source_block           cheng
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1335P)^2^+22.9284P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1335P)^2^+22.9284P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7011751
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.07457(8) 0.89584(6) 0.72229(10) 0.0280(3) Uani 1 d . . .
N1 N -0.0016(9) 0.7481(7) 0.7523(9) 0.017(2) Uani 1 d . . .
Sn2 Sn 0.11494(8) 0.62888(7) 0.72464(10) 0.0300(3) Uani 1 d . . .
Sn3 Sn -0.13032(8) 0.72898(7) 0.64109(10) 0.0292(3) Uani 1 d . . .
Cl2 Cl -0.1072(4) 0.8912(3) 0.9380(4) 0.0401(10) Uani 1 d . . .
Cl3 Cl -0.1765(4) 0.6376(3) 0.9052(4) 0.0422(11) Uani 1 d . . .
Cl1 Cl 0.0727(4) 0.6967(4) 0.9996(3) 0.0423(10) Uani 1 d . . .
Al1 Al -0.0504(4) 0.7439(3) 0.8919(4) 0.0256(9) Uani 1 d . . .
C1 C 0.2653(15) 0.6840(13) 0.7864(16) 0.043(4) Uani 1 d . . .
H1A H 0.3194 0.6326 0.7751 0.064 Uiso 1 calc R . .
H1B H 0.2584 0.6975 0.8615 0.064 Uiso 1 calc R . .
H1C H 0.2850 0.7465 0.7501 0.064 Uiso 1 calc R . .
C2 C 0.1856(16) 0.8738(16) 0.5939(16) 0.049(5) Uani 1 d . . .
H2A H 0.2209 0.9379 0.5786 0.073 Uiso 1 calc R . .
H2B H 0.1480 0.8506 0.5316 0.073 Uiso 1 calc R . .
H2C H 0.2376 0.8229 0.6142 0.073 Uiso 1 calc R . .
C3 C 0.1661(15) 0.9357(14) 0.8602(14) 0.041(4) Uani 1 d . . .
H3A H 0.1192 0.9454 0.9200 0.061 Uiso 1 calc R . .
H3B H 0.2047 0.9984 0.8469 0.061 Uiso 1 calc R . .
H3C H 0.2157 0.8812 0.8758 0.061 Uiso 1 calc R . .
C4 C -0.1528(19) 0.5635(12) 0.6279(17) 0.053(5) Uani 1 d . . .
H4A H -0.1752 0.5364 0.6956 0.079 Uiso 1 calc R . .
H4B H -0.0867 0.5317 0.6072 0.079 Uiso 1 calc R . .
H4C H -0.2063 0.5493 0.5751 0.079 Uiso 1 calc R . .
C5 C 0.1190(17) 0.6062(14) 0.5580(15) 0.046(6) Uani 1 d . . .
H5A H 0.1701 0.5535 0.5411 0.070 Uiso 1 calc R . .
H5B H 0.1391 0.6695 0.5235 0.070 Uiso 1 calc R . .
H5C H 0.0496 0.5854 0.5335 0.070 Uiso 1 calc R . .
C6 C -0.0847(15) 0.7958(15) 0.4931(14) 0.040(4) Uani 1 d . . .
H6A H -0.0777 0.8691 0.5014 0.059 Uiso 1 calc R . .
H6B H -0.1382 0.7812 0.4403 0.059 Uiso 1 calc R . .
H6C H -0.0176 0.7672 0.4706 0.059 Uiso 1 calc R . .
C7 C -0.0418(18) 1.0057(12) 0.6845(15) 0.051(5) Uani 1 d . . .
H7A H -0.0912 1.0119 0.7429 0.076 Uiso 1 calc R . .
H7B H -0.0795 0.9845 0.6215 0.076 Uiso 1 calc R . .
H7C H -0.0082 1.0712 0.6720 0.076 Uiso 1 calc R . .
C8 C -0.264(2) 0.8081(14) 0.7018(17) 0.056(6) Uani 1 d . . .
H8A H -0.2485 0.8806 0.7054 0.084 Uiso 1 calc R . .
H8B H -0.2802 0.7828 0.7721 0.084 Uiso 1 calc R . .
H8C H -0.3241 0.7969 0.6558 0.084 Uiso 1 calc R . .
C9 C 0.0608(19) 0.4930(12) 0.8014(18) 0.055(6) Uani 1 d . . .
H9A H 0.1115 0.4385 0.7902 0.083 Uiso 1 calc R . .
H9B H -0.0071 0.4732 0.7722 0.083 Uiso 1 calc R . .
H9C H 0.0534 0.5058 0.8766 0.083 Uiso 1 calc R . .
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'
Si Si 0.0817 0.0704 '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'
Al Al 0.0645 0.0514 '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'
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 Sn1 C3 113.1(7) . . ?
C7 Sn1 C2 111.9(8) . . ?
C3 Sn1 C2 106.9(8) . . ?
C7 Sn1 N1 109.4(6) . . ?
C3 Sn1 N1 108.0(6) . . ?
C2 Sn1 N1 107.3(6) . . ?
Al1 N1 Sn3 111.2(5) . . ?
Al1 N1 Sn2 110.7(5) . . ?
Sn3 N1 Sn2 108.8(4) . . ?
Al1 N1 Sn1 109.5(5) . . ?
Sn3 N1 Sn1 108.7(5) . . ?
Sn2 N1 Sn1 107.8(5) . . ?
C9 Sn2 C1 113.1(8) . . ?
C9 Sn2 C5 110.0(9) . . ?
C1 Sn2 C5 112.3(8) . . ?
C9 Sn2 N1 107.8(6) . . ?
C1 Sn2 N1 107.3(5) . . ?
C5 Sn2 N1 106.0(5) . . ?
C8 Sn3 N1 107.9(6) . . ?
C8 Sn3 C6 109.3(7) . . ?
N1 Sn3 C6 108.5(6) . . ?
C8 Sn3 C4 113.9(8) . . ?
N1 Sn3 C4 105.1(7) . . ?
C6 Sn3 C4 111.8(8) . . ?
N1 Al1 Cl3 110.0(4) . . ?
N1 Al1 Cl2 110.0(4) . . ?
Cl3 Al1 Cl2 108.4(3) . . ?
N1 Al1 Cl1 111.5(4) . . ?
Cl3 Al1 Cl1 107.7(2) . . ?
Cl2 Al1 Cl1 109.2(3) . . ?
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 C7 2.113(19) . ?
Sn1 C3 2.159(17) . ?
Sn1 C2 2.166(19) . ?
Sn1 N1 2.194(10) . ?
N1 Al1 1.872(12) . ?
N1 Sn3 2.166(12) . ?
N1 Sn2 2.175(10) . ?
Sn2 C9 2.139(17) . ?
Sn2 C1 2.179(19) . ?
Sn2 C5 2.129(19) . ?
Sn3 C8 2.13(2) . ?
Sn3 C6 2.145(18) . ?
Sn3 C4 2.190(16) . ?
Cl2 Al1 2.138(6) . ?
Cl3 Al1 2.124(6) . ?
Cl1 Al1 2.159(6) . ?
