#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/84/2228446.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_2228446
loop_
_publ_author_name
'Blasberg, Florian'
'Lerner, Hans-Wolfram'
'Bolte, Michael'
_publ_section_title
;
 Tetra-μ₃-tert-butanolato-tetrathallium(I)
;
_journal_coeditor_code           KJ2165
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1621
_journal_paper_doi               10.1107/S1600536810047550
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Tl4 (C4 H9 O)4]'
_chemical_formula_moiety         'C16 H36 O4 Tl4'
_chemical_formula_sum            'C16 H36 O4 Tl4'
_chemical_formula_weight         1109.93
_chemical_name_systematic
;
Tetra-μ₃-tert-butanolato-tetrathallium(I)
;
_space_group_IT_number           218
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_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            8
_cell_length_a                   17.1500(15)
_cell_length_b                   17.1500(15)
_cell_length_c                   17.1500(15)
_cell_measurement_reflns_used    7201
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      3.4
_cell_volume                     5044.2(8)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       ω
_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  0.0839
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13612
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.492
_exptl_absorpt_correction_T_max  0.1848
_exptl_absorpt_correction_T_min  0.0754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.009
_refine_ls_abs_structure_details 'Flack (1983), 711 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1489
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0419
_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)+(0.0370P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                1226
_reflns_number_total             1489
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kj2165.cif
_cod_data_source_block           I
_cod_database_code               2228446
_cod_database_fobs_code          2228446
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y+1/2, -x+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, x+1/2, -z+1/2'
'x, -y, -z'
'-y+1/2, -x+1/2, z+1/2'
'-x, y, -z'
'y+1/2, x+1/2, z+1/2'
'z, x, y'
'x+1/2, -z+1/2, -y+1/2'
'-z, -x, y'
'-x+1/2, z+1/2, -y+1/2'
'z, -x, -y'
'-x+1/2, -z+1/2, y+1/2'
'-z, x, -y'
'x+1/2, z+1/2, y+1/2'
'y, z, x'
'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'
'y, -z, -x'
'-y, -z, x'
'-y, z, -x'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl Tl1 0.66760(4) 0.91953(4) 0.57229(3) 0.02168(17) Uani d . 1 . .
O O1 0.8130(7) 0.9310(7) 0.5635(7) 0.022(2) Uani d . 1 . .
C C1 0.8550(13) 0.8777(10) 0.6115(13) 0.029(4) Uani d . 1 . .
C C2 0.9386(12) 0.8950(18) 0.6078(19) 0.059(8) Uani d . 1 . .
H H2A 0.9478 0.9485 0.6256 0.088 Uiso calc R 1 . .
H H2B 0.9569 0.8895 0.5539 0.088 Uiso calc R 1 . .
H H2C 0.9671 0.8586 0.6414 0.088 Uiso calc R 1 . .
C C3 0.8400(19) 0.7958(10) 0.583(2) 0.059(7) Uani d . 1 . .
H H3A 0.7839 0.7853 0.5844 0.089 Uiso calc R 1 . .
H H3B 0.8669 0.7588 0.6177 0.089 Uiso calc R 1 . .
H H3C 0.8596 0.7901 0.5301 0.089 Uiso calc R 1 . .
C C4 0.8261(16) 0.8852(14) 0.6961(12) 0.041(6) Uani d . 1 . .
H H4A 0.8368 0.9380 0.7153 0.061 Uiso calc R 1 . .
H H4B 0.8533 0.8472 0.7290 0.061 Uiso calc R 1 . .
H H4C 0.7698 0.8753 0.6980 0.061 Uiso calc R 1 . .
Tl Tl1A 0.42129(4) 0.42129(4) 0.42129(4) 0.0223(2) Uani d S 1 . .
O O1A 0.5652(6) 0.4348(6) 0.4348(6) 0.020(4) Uani d S 1 . .
C C1A 0.6118(13) 0.3882(13) 0.3882(13) 0.020(7) Uani d S 1 . .
C C2A 0.6960(12) 0.3942(13) 0.4110(14) 0.035(5) Uani d U 1 . .
H H2A1 0.7125 0.4488 0.4086 0.053 Uiso calc R 1 . .
H H2A2 0.7277 0.3631 0.3751 0.053 Uiso calc R 1 . .
H H2A3 0.7027 0.3746 0.4643 0.053 Uiso calc R 1 . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Tl1 O1 14_664 12_656 81.0(4) ?
O1 Tl1 O1 14_664 . 78.3(4) ?
O1 Tl1 O1 12_656 . 77.8(4) ?
O1 Tl1 Tl1 14_664 5_576 41.8(3) ?
O1 Tl1 Tl1 12_656 5_576 41.2(3) ?
O1 Tl1 Tl1 . 5_576 84.3(2) ?
C1 O1 Tl1 . 12_656 119.7(10) ?
C1 O1 Tl1 . 14_664 119.3(11) ?
Tl1 O1 Tl1 12_656 14_664 97.0(4) ?
C1 O1 Tl1 . . 114.7(11) ?
Tl1 O1 Tl1 12_656 . 101.8(4) ?
Tl1 O1 Tl1 14_664 . 101.0(4) ?
O1 C1 C2 . . 109.8(17) ?
O1 C1 C3 . . 109.2(17) ?
C2 C1 C3 . . 110(2) ?
O1 C1 C4 . . 109.1(16) ?
C2 C1 C4 . . 110(2) ?
C3 C1 C4 . . 109(2) ?
C1 C2 H2A . . 109.5 ?
C1 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
C1 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
C1 C3 H3A . . 109.5 ?
C1 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C1 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C1 C4 H4A . . 109.5 ?
C1 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C1 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
O1A Tl1A O1A . 7_656 78.9(6) ?
O1A Tl1A O1A . 3_665 78.9(6) ?
O1A Tl1A O1A 7_656 3_665 78.9(6) ?
C1A O1A Tl1A . 7_656 117.7(11) ?
C1A O1A Tl1A . 3_665 117.7(11) ?
Tl1A O1A Tl1A 7_656 3_665 100.1(5) ?
C1A O1A Tl1A . . 117.7(11) ?
Tl1A O1A Tl1A 7_656 . 100.1(5) ?
Tl1A O1A Tl1A 3_665 . 100.1(5) ?
O1A C1A C2A . 11_665 111.4(15) ?
O1A C1A C2A . 24_656 111.4(15) ?
C2A C1A C2A 11_665 24_656 107.4(16) ?
O1A C1A C2A . . 111.4(15) ?
C2A C1A C2A 11_665 . 107.4(16) ?
C2A C1A C2A 24_656 . 107.4(16) ?
C1A C2A H2A1 . . 109.5 ?
C1A C2A H2A2 . . 109.5 ?
H2A1 C2A H2A2 . . 109.5 ?
C1A C2A H2A3 . . 109.5 ?
H2A1 C2A H2A3 . . 109.5 ?
H2A2 C2A H2A3 . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Tl1 O1 14_664 2.463(12) ?
Tl1 O1 12_656 2.493(11) ?
Tl1 O1 . 2.506(12) ?
O1 C1 . 1.42(2) ?
O1 Tl1 12_656 2.463(12) ?
O1 Tl1 14_664 2.492(11) ?
C1 C2 . 1.47(3) ?
C1 C3 . 1.51(3) ?
C1 C4 . 1.54(3) ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 H2C . 0.9800 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
Tl1A O1A . 2.490(8) ?
Tl1A O1A 7_656 2.490(8) ?
Tl1A O1A 3_665 2.490(8) ?
O1A C1A . 1.38(4) ?
O1A Tl1A 7_656 2.490(8) ?
O1A Tl1A 3_665 2.490(8) ?
C1A C2A 11_665 1.50(2) ?
C1A C2A 24_656 1.50(2) ?
C1A C2A . 1.50(2) ?
C2A H2A1 . 0.9800 ?
C2A H2A2 . 0.9800 ?
C2A H2A3 . 0.9800 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 Tl1 O1 C1 14_664 . . . -137.9(13) ?
O1 Tl1 O1 C1 12_656 . . . 139.0(13) ?
Tl1 Tl1 O1 C1 5_576 . . . -179.8(12) ?
O1 Tl1 O1 Tl1 14_664 . . 12_656 91.4(5) ?
O1 Tl1 O1 Tl1 12_656 . . 12_656 8.2(4) ?
Tl1 Tl1 O1 Tl1 5_576 . . 12_656 49.5(3) ?
O1 Tl1 O1 Tl1 14_664 . . 14_664 -8.2(4) ?
O1 Tl1 O1 Tl1 12_656 . . 14_664 -91.4(5) ?
Tl1 Tl1 O1 Tl1 5_576 . . 14_664 -50.1(3) ?
Tl1 O1 C1 C2 12_656 . . . -53(2) ?
Tl1 O1 C1 C2 14_664 . . . 66(2) ?
Tl1 O1 C1 C2 . . . . -174.2(19) ?
Tl1 O1 C1 C3 12_656 . . . -173.5(18) ?
Tl1 O1 C1 C3 14_664 . . . -55(2) ?
Tl1 O1 C1 C3 . . . . 65(2) ?
Tl1 O1 C1 C4 12_656 . . . 67.6(19) ?
Tl1 O1 C1 C4 14_664 . . . -173.7(14) ?
Tl1 O1 C1 C4 . . . . -53.8(18) ?
O1A Tl1A O1A C1A 7_656 . . . 139.7(13) ?
O1A Tl1A O1A C1A 3_665 . . . -139.7(13) ?
O1A Tl1A O1A Tl1A 7_656 . . 7_656 10.8(5) ?
O1A Tl1A O1A Tl1A 3_665 . . 7_656 91.49(15) ?
O1A Tl1A O1A Tl1A 7_656 . . 3_665 -91.49(15) ?
O1A Tl1A O1A Tl1A 3_665 . . 3_665 -10.8(5) ?
Tl1A O1A C1A C2A 7_656 . . 11_665 68.4(10) ?
Tl1A O1A C1A C2A 3_665 . . 11_665 -171.6(10) ?
Tl1A O1A C1A C2A . . . 11_665 -51.6(10) ?
Tl1A O1A C1A C2A 7_656 . . 24_656 -171.6(10) ?
Tl1A O1A C1A C2A 3_665 . . 24_656 -51.6(10) ?
Tl1A O1A C1A C2A . . . 24_656 68.4(10) ?
Tl1A O1A C1A C2A 7_656 . . . -51.6(10) ?
Tl1A O1A C1A C2A 3_665 . . . 68.4(10) ?
Tl1A O1A C1A C2A . . . . -171.6(10) ?
