#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:51:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179427 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/24/4332408.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332408
loop_
_publ_author_name
'Eichler, Jack F.'
'Just, Oliver'
'Rees, William S.'
_publ_section_title
;
 Synthesis and Characterization of Imidocubanes with Exocube GeIVand
 SnIVSubstituents:  [M(μ3-NGeMe3)]4(M = Sn, Ge, Pb);
 [Sn(μ3-NSnMe3)]4
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6706
_journal_page_last               6712
_journal_paper_doi               10.1021/ic060331y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C12 H36 N4 Sn8'
_chemical_formula_weight         1185.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           217
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_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            2
_cell_length_a                   11.6106(14)
_cell_length_b                   11.6106(14)
_cell_length_c                   11.6106(14)
_cell_measurement_temperature    193(2)
_cell_volume                     1565.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4478
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    6.276
_exptl_absorpt_correction_T_max  0.5669
_exptl_absorpt_correction_T_min  0.4823
_exptl_crystal_density_diffrn    2.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0291P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0480
_reflns_number_gt                394
_reflns_number_total             405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060331ysup6.cif
_cod_data_source_block           jfe30
_cod_database_code               4332408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, 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
Sn1 Sn 0.09975(2) 0.09975(2) 0.09975(2) 0.02780(15) Uani 1 6 d S
Sn2 Sn 0.19030(2) 0.19030(2) -0.19030(2) 0.03178(16) Uani 1 6 d S
N1 N 0.0887(3) 0.0887(3) -0.0887(3) 0.0290(12) Uani 1 6 d S
C1 C 0.3636(5) 0.1461(4) -0.1461(4) 0.0508(12) Uani 1 2 d S
H1A H 0.3677 0.1277 -0.0656 0.042(16) Uiso 0.50 1 calc PR
H1B H 0.4134 0.2101 -0.1623 0.042(16) Uiso 0.50 1 calc PR
H1C H 0.3875 0.0806 -0.1906 0.042(16) Uiso 0.50 1 calc PR
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 0.02780(15) 0.02780(15) 0.02780(15) -0.00286(11) -0.00286(11) -0.00286(11)
Sn2 0.03178(16) 0.03178(16) 0.03178(16) 0.00494(11) 0.00494(11) -0.00494(11)
N1 0.0290(12) 0.0290(12) 0.0290(12) 0.0009(14) 0.0009(14) -0.0009(14)
C1 0.034(2) 0.059(2) 0.059(2) 0.006(3) 0.0038(16) -0.0038(16)
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'
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
N1 Sn1 N1 83.1(2) 4 3
N1 Sn1 N1 83.1(2) 4 .
N1 Sn1 N1 83.1(2) 3 .
N1 Sn1 Sn1 85.27(15) 4 3
N1 Sn1 Sn1 41.76(10) 3 3
N1 Sn1 Sn1 41.76(10) . 3
N1 Sn1 Sn1 41.76(10) 4 4
N1 Sn1 Sn1 85.27(15) 3 4
N1 Sn1 Sn1 41.76(10) . 4
Sn1 Sn1 Sn1 60.0 3 4
N1 Sn1 Sn1 41.76(10) 4 2
N1 Sn1 Sn1 41.76(10) 3 2
N1 Sn1 Sn1 85.27(15) . 2
Sn1 Sn1 Sn1 60.0 3 2
Sn1 Sn1 Sn1 60.0 4 2
N1 Sn2 C1 105.43(19) . 11
N1 Sn2 C1 105.43(19) . .
C1 Sn2 C1 113.20(16) 11 .
N1 Sn2 C1 105.43(19) . 8
C1 Sn2 C1 113.20(16) 11 8
C1 Sn2 C1 113.20(16) . 8
Sn2 N1 Sn1 120.54(15) . .
Sn2 N1 Sn1 120.54(15) . 4
Sn1 N1 Sn1 96.5(2) . 4
Sn2 N1 Sn1 120.54(15) . 3
Sn1 N1 Sn1 96.5(2) . 3
Sn1 N1 Sn1 96.5(2) 4 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 N1 2.196(3) 4
Sn1 N1 2.196(3) 3
Sn1 N1 2.196(3) .
Sn1 Sn1 3.2757(9) 3
Sn1 Sn1 3.2757(9) 4
Sn1 Sn1 3.2757(9) 2
Sn2 N1 2.043(7) .
Sn2 C1 2.139(5) 11
Sn2 C1 2.139(5) .
Sn2 C1 2.139(5) 8
N1 Sn1 2.196(3) 4
N1 Sn1 2.196(3) 3
