#------------------------------------------------------------------------------
#$Date: 2017-10-13 10:03:29 +0200 (vie 13 de oct de 2017) $
#$Revision: 201974 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/72/2217205.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2217205
loop_
_publ_author_name
'Bauer, Matthew'
'Groy, Thomas L.'
'Kouvetakis, John'
_publ_section_title
;
 Redetermination of tetrakis(trimethylstannyl)germane
;
_journal_coeditor_code           MG2036
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m49
_journal_page_last               m49
_journal_paper_doi               10.1107/S1600536807054724
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ge Sn4 (C H3)12]'
_chemical_formula_moiety         'C12 H36 Ge Sn4'
_chemical_formula_sum            'C12 H36 Ge Sn4'
_chemical_formula_weight         727.76
_chemical_name_systematic        tetrakis(trimethylstannyl)germane
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.033(2)
_cell_angle_beta                 90.5460(10)
_cell_angle_gamma                111.7360(10)
_cell_formula_units_Z            2
_cell_length_a                   9.1666(7)
_cell_length_b                   9.9521(7)
_cell_length_c                   14.5400(14)
_cell_measurement_reflns_used    6668
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.20
_cell_volume                     1232.06(17)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXTL (Bruker, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'ω 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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12284
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.191
_exptl_absorpt_correction_T_max  0.4599
_exptl_absorpt_correction_T_min  0.3169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.086
_refine_diff_density_min         -1.007
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         5646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0304P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                4466
_reflns_number_total             5646
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            mg2036.cif
_cod_data_source_block           I
_cod_database_code               2217205
_cod_database_fobs_code          2217205
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ge Ge1 0.75863(7) 0.73542(6) 0.75103(5) 0.04589(16) Uani d . 1
Sn Sn1 0.76633(5) 0.47736(5) 0.75113(4) 0.05566(14) Uani d . 1
Sn Sn2 0.67526(5) 0.79813(5) 0.91050(3) 0.05480(14) Uani d . 1
Sn Sn3 0.55868(5) 0.75649(5) 0.63013(3) 0.05205(13) Uani d . 1
Sn Sn4 1.03424(5) 0.92048(5) 0.70999(3) 0.05197(13) Uani d . 1
C C1A 0.5374(9) 0.3234(8) 0.7776(6) 0.084(2) Uani d . 1
H H1AA 0.5400 0.2278 0.7776 0.125 Uiso calc R 1
H H1AB 0.4659 0.3296 0.7306 0.125 Uiso calc R 1
H H1AC 0.5030 0.3432 0.8364 0.125 Uiso calc R 1
C C1B 0.9275(9) 0.4584(9) 0.8546(7) 0.092(3) Uani d . 1
H H1BA 0.9284 0.3623 0.8534 0.138 Uiso calc R 1
H H1BB 0.8949 0.4776 0.9141 0.138 Uiso calc R 1
H H1BC 1.0311 0.5270 0.8424 0.138 Uiso calc R 1
C C1C 0.8419(9) 0.4301(9) 0.6205(6) 0.084(2) Uani d . 1
H H1CA 0.8442 0.3344 0.6214 0.126 Uiso calc R 1
H H1CB 0.9451 0.4990 0.6080 0.126 Uiso calc R 1
H H1CC 0.7702 0.4355 0.5734 0.126 Uiso calc R 1
C C2A 0.8272(9) 0.7754(10) 1.0181(6) 0.088(3) Uani d . 1
H H2AA 0.7939 0.7992 1.0762 0.132 Uiso calc R 1
H H2AB 0.9332 0.8395 1.0067 0.132 Uiso calc R 1
H H2AC 0.8224 0.6774 1.0194 0.132 Uiso calc R 1
C C2B 0.6866(10) 1.0148(8) 0.9115(6) 0.087(2) Uani d . 1
H H2BA 0.6556 1.0371 0.9707 0.131 Uiso calc R 1
H H2BB 0.6172 1.0264 0.8651 0.131 Uiso calc R 1
H H2BC 0.7922 1.0790 0.8993 0.131 Uiso calc R 1
C C2C 0.4400(9) 0.6608(10) 0.9404(6) 0.088(3) Uani d . 1
H H2CA 0.4116 0.6858 0.9996 0.132 Uiso calc R 1
H H2CB 0.4321 0.5619 0.9409 0.132 Uiso calc R 1
H H2CC 0.3703 0.6730 0.8943 0.132 Uiso calc R 1
C C3A 0.6191(9) 0.7151(9) 0.4940(5) 0.085(2) Uani d . 1
H H3AA 0.5431 0.7236 0.4509 0.128 Uiso calc R 1
H H3AB 0.6202 0.6191 0.4909 0.128 Uiso calc R 1
H H3AC 0.7212 0.7840 0.4792 0.128 Uiso calc R 1
C C3B 0.3259(8) 0.6064(8) 0.6589(6) 0.076(2) Uani d . 1
H H3BA 0.2539 0.6160 0.6134 0.115 Uiso calc R 1
H H3BB 0.2952 0.6266 0.7187 0.115 Uiso calc R 1
H H3BC 0.3247 0.5095 0.6575 0.115 Uiso calc R 1
C C3C 0.5645(8) 0.9736(8) 0.6319(6) 0.075(2) Uani d . 1
H H3CA 0.4909 0.9828 0.5874 0.112 Uiso calc R 1
H H3CB 0.6683 1.0393 0.6172 0.112 Uiso calc R 1
H H3CC 0.5371 0.9959 0.6920 0.112 Uiso calc R 1
C C4A 1.2038(8) 0.9083(9) 0.8092(6) 0.081(2) Uani d . 1
H H4AA 1.3058 0.9769 0.7938 0.121 Uiso calc R 1
H H4AB 1.2058 0.8125 0.8088 0.121 Uiso calc R 1
H H4AC 1.1756 0.9299 0.8693 0.121 Uiso calc R 1
C C4B 1.0969(8) 0.8697(9) 0.5750(5) 0.078(2) Uani d . 1
H H4BA 1.1990 0.9379 0.5593 0.117 Uiso calc R 1
H H4BB 1.0210 0.8748 0.5306 0.117 Uiso calc R 1
H H4BC 1.0986 0.7738 0.5752 0.117 Uiso calc R 1
C C4C 1.0413(9) 1.1383(7) 0.7095(6) 0.080(2) Uani d . 1
H H4CA 1.1451 1.2033 0.6940 0.120 Uiso calc R 1
H H4CB 1.0148 1.1625 0.7693 0.120 Uiso calc R 1
H H4CC 0.9674 1.1468 0.6648 0.120 Uiso calc R 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ge1 0.0459(3) 0.0435(3) 0.0477(4) 0.0158(3) 0.0020(3) 0.0011(3)
Sn1 0.0596(3) 0.0444(2) 0.0628(3) 0.0192(2) -0.0006(2) 0.0007(2)
Sn2 0.0586(3) 0.0588(3) 0.0469(3) 0.0216(2) 0.0030(2) 0.0002(2)
Sn3 0.0501(2) 0.0549(3) 0.0501(3) 0.0183(2) -0.00229(19) -0.0012(2)
Sn4 0.0469(2) 0.0507(3) 0.0549(3) 0.01392(19) 0.00327(19) 0.0024(2)
C1A 0.079(5) 0.058(4) 0.102(7) 0.012(4) 0.009(5) 0.015(4)
C1B 0.086(6) 0.081(6) 0.119(8) 0.042(5) -0.015(5) 0.022(5)
C1C 0.098(6) 0.080(5) 0.080(6) 0.039(5) 0.011(5) -0.021(4)
C2A 0.091(6) 0.110(7) 0.068(6) 0.045(5) -0.023(4) -0.006(5)
C2B 0.120(7) 0.072(5) 0.076(6) 0.041(5) 0.003(5) -0.012(4)
C2C 0.071(5) 0.105(7) 0.082(6) 0.025(5) 0.022(4) 0.018(5)
C3A 0.102(6) 0.091(6) 0.051(5) 0.022(5) 0.010(4) -0.011(4)
C3B 0.055(4) 0.082(5) 0.084(6) 0.016(4) 0.006(4) -0.003(4)
C3C 0.080(5) 0.060(4) 0.086(6) 0.028(4) 0.000(4) 0.009(4)
C4A 0.063(4) 0.102(6) 0.080(6) 0.035(4) -0.020(4) -0.016(5)
C4B 0.079(5) 0.084(5) 0.069(5) 0.026(4) 0.029(4) 0.006(4)
C4C 0.094(6) 0.049(4) 0.094(7) 0.022(4) 0.009(5) 0.009(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'
Ge Ge 0.1547 1.8001 '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
Sn4 Ge1 Sn3 108.29(3)
Sn4 Ge1 Sn1 109.08(3)
Sn3 Ge1 Sn1 111.09(3)
Sn4 Ge1 Sn2 109.91(3)
Sn3 Ge1 Sn2 107.59(3)
Sn1 Ge1 Sn2 110.83(3)
C1A Sn1 C1C 108.9(3)
C1A Sn1 C1B 109.3(3)
C1C Sn1 C1B 108.0(3)
C1A Sn1 Ge1 109.4(2)
C1C Sn1 Ge1 110.3(2)
C1B Sn1 Ge1 111.0(2)
C2B Sn2 C2C 107.9(3)
C2B Sn2 C2A 108.2(3)
C2C Sn2 C2A 108.6(3)
C2B Sn2 Ge1 110.0(2)
C2C Sn2 Ge1 110.9(3)
C2A Sn2 Ge1 111.2(2)
C3A Sn3 C3C 107.0(3)
C3A Sn3 C3B 108.5(3)
C3C Sn3 C3B 110.3(3)
C3A Sn3 Ge1 111.5(2)
C3C Sn3 Ge1 108.7(2)
C3B Sn3 Ge1 110.9(2)
C4C Sn4 C4A 108.0(3)
C4C Sn4 C4B 108.7(3)
C4A Sn4 C4B 109.4(3)
C4C Sn4 Ge1 112.1(2)
C4A Sn4 Ge1 109.6(2)
C4B Sn4 Ge1 109.0(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ge1 Sn4 2.5912(7)
Ge1 Sn3 2.5917(8)
Ge1 Sn1 2.5952(7)
Ge1 Sn2 2.5953(8)
Sn1 C1A 2.130(7)
Sn1 C1C 2.139(8)
Sn1 C1B 2.156(7)
Sn2 C2B 2.120(8)
Sn2 C2C 2.132(7)
Sn2 C2A 2.152(7)
Sn3 C3A 2.141(7)
Sn3 C3C 2.141(7)
Sn3 C3B 2.148(7)
Sn4 C4C 2.145(7)
Sn4 C4A 2.147(7)
Sn4 C4B 2.162(7)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 24730390
