#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:53:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309511.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_4309511
loop_
_publ_author_name
'Anja-Verena Mudring'
'Franziska Rieger'
_publ_contact_author_address
;
        Institut für Anorganische Chemie
        Universität zu Köln
        Greinstraße 6
        D-50939 Köln
        Germany
;
_publ_contact_author_email       a.mudring@uni-koeln.de
_publ_contact_author_fax         '+49 221 470 5083'
_publ_contact_author_name
;
        Dr. A. Mudring
;
_publ_contact_author_phone       '+49 221 470 3921'
_publ_section_title
;
Lone Pair Effect in Thallium(I) Macrocyclic Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6240
_journal_page_last               6243
_journal_paper_doi               10.1021/ic050547k
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'as described'
_chemical_formula_sum            'C12 H24 I4 O6 Tl2'
_chemical_formula_weight         1180.65
_chemical_melting_point          ?
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.968(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4090(7)
_cell_length_b                   21.104(2)
_cell_length_c                   14.6444(13)
_cell_measurement_reflns_used    5660
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      1.72
_cell_volume                     2542.4(4)
_computing_molecular_graphics    'DIAMOND (CrystalImpact'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe IPDS II'
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27992
_diffrn_reflns_theta_max         27.31
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    17.538
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    3.085
_exptl_crystal_F_000             2072
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.964
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.650
_refine_ls_goodness_of_fit_obs   0.647
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.650
_refine_ls_restrained_S_obs      0.647
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_obs          0.0388
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0734P)²+96.6910P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1046
_refine_ls_wR_factor_obs         0.0922
_reflns_number_observed          4466
_reflns_number_total             5660
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic050547ksi20050408_084146.cif
_cod_data_source_block           Tl(18crown6)TlI4
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value 'not determined' changed to '?' - value
is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+96.6910P] 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^)+(0.0734P)^2^+96.6910P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4309511
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tl1 Tl 0.04906(5) 0.91713(2) 0.70671(3) 0.03699(10) Uani 1 d . .
Tl2 Tl 0.28162(5) 0.79532(2) 0.96739(3) 0.03995(11) Uani 1 d . .
I3 I 0.35710(9) 0.94634(4) 0.68188(5) 0.0442(2) Uani 1 d . .
I4 I -0.00029(10) 0.78717(3) 0.68897(6) 0.0515(2) Uani 1 d . .
I5 I -0.18722(9) 0.98826(4) 0.59479(5) 0.0488(2) Uani 1 d . .
I6 I 0.05197(9) 0.94698(3) 0.89205(5) 0.0435(2) Uani 1 d . .
O1 O 0.6162(9) 0.8389(3) 0.9721(5) 0.043(2) Uani 1 d . .
O2 O 0.4983(8) 0.7262(4) 0.8709(5) 0.039(2) Uani 1 d . .
O3 O 0.2457(9) 0.6631(3) 0.9362(5) 0.041(2) Uani 1 d . .
O4 O 0.0242(8) 0.7277(4) 1.0250(5) 0.040(2) Uani 1 d . .
O5 O 0.1691(9) 0.8308(4) 1.1396(5) 0.044(2) Uani 1 d . .
O6 O 0.4170(9) 0.9019(4) 1.0790(5) 0.046(2) Uani 1 d . .
C1 C 0.5818(14) 0.9187(6) 1.0797(9) 0.052(3) Uani 1 d . .
C2 C 0.6143(15) 0.9061(6) 0.9843(9) 0.053(3) Uani 1 d . .
C3 C 0.6563(14) 0.8211(6) 0.8854(8) 0.047(3) Uani 1 d . .
C4 C 0.6587(12) 0.7493(6) 0.8818(8) 0.044(2) Uani 1 d . .
C5 C 0.4964(15) 0.6593(5) 0.8866(8) 0.045(2) Uani 1 d . .
C6 C 0.3213(15) 0.6375(6) 0.8666(8) 0.048(3) Uani 1 d . .
C7 C 0.0784(13) 0.6442(5) 0.9237(8) 0.044(2) Uani 1 d . .
C8 C 0.0208(13) 0.6602(5) 1.0114(7) 0.043(2) Uani 1 d . .
C9 C -0.0152(14) 0.7439(6) 1.1121(8) 0.049(3) Uani 1 d . .
C10 C -0.0008(14) 0.8138(6) 1.1240(8) 0.049(3) Uani 1 d . .
C11 C 0.1943(16) 0.8970(5) 1.1570(8) 0.050(3) Uani 1 d . .
C12 C 0.3750(17) 0.9106(6) 1.1680(7) 0.053(3) Uani 1 d . .
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'
I I -0.4742 1.8119 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I5 Tl1 I3 112.47(3) . . ?
I5 Tl1 I4 114.10(3) . . ?
I3 Tl1 I4 109.53(3) . . ?
I5 Tl1 I6 108.52(3) . . ?
I3 Tl1 I6 105.04(3) . . ?
I4 Tl1 I6 106.60(3) . . ?
C2 O1 C3 112.5(9) . . ?
C4 O2 C5 111.4(8) . . ?
C6 O3 C7 112.1(8) . . ?
C9 O4 C8 111.2(8) . . ?
C11 O5 C10 112.1(9) . . ?
C1 O6 C12 112.5(9) . . ?
O6 C1 C2 108.1(9) . . ?
O1 C2 C1 107.6(10) . . ?
O1 C3 C4 107.5(9) . . ?
O2 C4 C3 109.3(9) . . ?
O2 C5 C6 108.2(9) . . ?
O3 C6 C5 108.0(9) . . ?
O3 C7 C8 108.0(9) . . ?
O4 C8 C7 109.8(8) . . ?
O4 C9 C10 108.4(9) . . ?
O5 C10 C9 108.6(9) . . ?
O5 C11 C12 108.2(9) . . ?
O6 C12 C11 108.0(8) . . ?
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
Tl1 I5 2.7453(8) . ?
Tl1 I3 2.7590(8) . ?
Tl1 I4 2.7781(9) . ?
Tl1 I6 2.7815(8) . ?
O1 C2 1.429(13) . ?
O1 C3 1.430(13) . ?
O2 C4 1.412(12) . ?
O2 C5 1.430(12) . ?
O3 C6 1.416(13) . ?
O3 C7 1.437(13) . ?
O4 C9 1.423(12) . ?
O4 C8 1.438(13) . ?
O5 C11 1.428(14) . ?
O5 C10 1.444(14) . ?
O6 C1 1.429(14) . ?
O6 C12 1.431(13) . ?
C1 C2 1.50(2) . ?
C3 C4 1.52(2) . ?
C5 C6 1.51(2) . ?
C7 C8 1.50(2) . ?
C9 C10 1.49(2) . ?
C11 C12 1.52(2) . ?
