#------------------------------------------------------------------------------
#$Date: 2025-08-20 22:19:29 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/95/4309510.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_4309510
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_formula_moiety         'C12 H24 Cl O10 Tl'
_chemical_formula_sum            'C12 H24 Cl O10 Tl'
_chemical_formula_weight         568.13
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.50
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.477(2)
_cell_length_b                   8.6688(4)
_cell_length_c                   22.343(2)
_cell_measurement_reflns_used    37536
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      1.83
_cell_volume                     3655.7(5)
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  '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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37536
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.042
_exptl_absorpt_correction_T_max  0.3680
_exptl_absorpt_correction_T_min  0.1853
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.589
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0244P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                6418
_reflns_number_total             8090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050547ksi20050408_084135.cif
_cod_data_source_block           Tl(18crown6)ClO4
_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:

'_exptl_crystal_density_meas' value 'unknown' was changed to '?' -
the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3655.72
_cod_database_code               4309510
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl01 Tl 0.430029(8) 0.197807(18) 0.829178(8) 0.02805(5) Uani 1 1 d . . .
Tl02 Tl 0.147219(9) 0.333657(19) 0.773446(8) 0.03257(5) Uani 1 1 d . . .
Cl03 Cl 0.17094(6) 0.66214(12) 0.56472(5) 0.0337(2) Uani 1 1 d . . .
Cl04 Cl 0.33684(5) 0.40972(12) 0.89978(5) 0.0328(2) Uani 1 1 d . . .
O005 O 0.03092(16) 0.3706(4) 0.63418(14) 0.0345(7) Uani 1 1 d . . .
O006 O 0.2954(2) 0.5477(4) 0.87826(19) 0.0529(9) Uani 1 1 d . . .
O007 O 0.56940(17) 0.3524(3) 0.88113(15) 0.0357(7) Uani 1 1 d . . .
O008 O 0.33048(17) -0.0279(3) 0.74312(17) 0.0393(8) Uani 1 1 d . . .
C009 C 0.0369(3) 0.6667(5) 0.7838(3) 0.0388(11) Uani 1 1 d . . .
C010 C 0.2754(3) 0.1773(7) 0.6647(2) 0.0464(13) Uani 1 1 d . . .
O011 O 0.18195(17) 0.2136(3) 0.90263(15) 0.0354(7) Uani 1 1 d . . .
C012 C 0.3481(3) -0.1880(6) 0.7556(4) 0.0554(16) Uani 1 1 d . . .
O013 O 0.34124(16) 0.2484(4) 0.68176(15) 0.0362(7) Uani 1 1 d . . .
O014 O 0.10648(17) 0.4889(3) 0.87116(15) 0.0345(7) Uani 1 1 d . . .
O015 O 0.18990(19) 0.6385(4) 0.63499(16) 0.0479(8) Uani 1 1 d . . .
C016 C 0.6201(3) 0.1589(7) 0.9674(2) 0.0459(13) Uani 1 1 d . . .
O017 O 0.44582(17) 0.4673(3) 0.76464(15) 0.0348(7) Uani 1 1 d . . .
O018 O 0.16013(16) -0.0100(3) 0.80541(15) 0.0322(6) Uani 1 1 d . . .
O019 O 0.45576(18) -0.1437(3) 0.85824(17) 0.0390(7) Uani 1 1 d . . .
O020 O 0.3342(2) 0.3477(4) 0.95793(18) 0.0496(9) Uani 1 1 d . . .
O021 O 0.55451(17) 0.0789(4) 0.94243(15) 0.0379(7) Uani 1 1 d . . .
O022 O 0.05376(16) 0.5974(4) 0.73504(16) 0.0360(7) Uani 1 1 d . . .
O023 O 0.10990(16) 0.0959(3) 0.66870(15) 0.0345(7) Uani 1 1 d . . .
O024 O 0.2327(2) 0.6985(4) 0.5588(2) 0.0535(9) Uani 1 1 d . . .
O026 O 0.40938(17) 0.4408(4) 0.91677(17) 0.0417(8) Uani 1 1 d . . .
O027 O 0.1392(2) 0.5246(5) 0.5279(2) 0.0708(13) Uani 1 1 d . . .
C028 C 0.0985(3) 0.6490(5) 0.8531(3) 0.0378(10) Uani 1 1 d . . .
C029 C 0.1126(3) -0.0631(5) 0.6868(2) 0.0365(10) Uani 1 1 d . . .
C030 C 0.1740(3) -0.0867(5) 0.7558(3) 0.0385(11) Uani 1 1 d . . .
C031 C 0.1676(3) 0.4655(6) 0.9363(2) 0.0399(11) Uani 1 1 d . . .
O032 O 0.1216(2) 0.7875(5) 0.5388(2) 0.0650(11) Uani 1 1 d . . .
C033 C 0.0543(3) 0.1266(6) 0.6014(2) 0.0390(11) Uani 1 1 d . . .
C034 C 0.0501(3) 0.2955(6) 0.5880(2) 0.0394(11) Uani 1 1 d . . .
C036 C 0.2018(3) 0.0575(6) 0.9217(2) 0.0375(11) Uani 1 1 d . . .
O037 O 0.30814(19) 0.2973(5) 0.8455(2) 0.0597(11) Uani 1 1 d . . .
C038 C 0.5537(3) 0.5124(5) 0.8661(3) 0.0430(12) Uani 1 1 d . . .
C039 C 0.6059(3) 0.3272(6) 0.9529(2) 0.0453(12) Uani 1 1 d . . .
C040 C 0.1736(3) 0.2977(6) 0.9529(2) 0.0432(12) Uani 1 1 d . . .
C041 C 0.2204(3) -0.0145(6) 0.8712(3) 0.0375(10) Uani 1 1 d . . .
C042 C 0.3343(3) 0.4105(6) 0.6697(3) 0.0451(12) Uani 1 1 d . . .
C043 C 0.5147(3) 0.5335(5) 0.7911(3) 0.0405(11) Uani 1 1 d . . .
C044 C 0.0178(3) 0.5324(6) 0.6195(2) 0.0385(11) Uani 1 1 d . . .
C045 C 0.3873(3) -0.2157(6) 0.8300(4) 0.0559(16) Uani 1 1 d . . .
C046 C 0.4924(4) -0.1542(6) 0.9313(3) 0.0555(16) Uani 1 1 d . . .
C047 C 0.4064(3) 0.4767(6) 0.6923(2) 0.0420(12) Uani 1 1 d . . .
C049 C 0.5636(3) -0.0809(6) 0.9591(3) 0.0483(14) Uani 1 1 d . . .
C050 C -0.0043(3) 0.6005(5) 0.6676(2) 0.0381(11) Uani 1 1 d . . .
C051 C 0.2853(3) 0.0069(7) 0.6722(3) 0.0503(14) Uani 1 1 d . . .
H1 H 0.400(2) 0.582(6) 0.679(2) 0.035(12) Uiso 1 1 d . . .
H2 H 0.598(3) 0.563(5) 0.887(2) 0.037(13) Uiso 1 1 d . . .
H3 H -0.021(2) 0.716(5) 0.654(2) 0.035(12) Uiso 1 1 d . . .
H4 H 0.238(2) -0.121(6) 0.885(2) 0.035(12) Uiso 1 1 d . . .
H5 H 0.431(3) 0.428(6) 0.672(2) 0.040(14) Uiso 1 1 d . . .
H6 H 0.593(3) -0.090(6) 1.013(3) 0.048(14) Uiso 1 1 d . . .
H7 H 0.010(2) 0.315(5) 0.538(2) 0.025(11) Uiso 1 1 d . . .
H8 H 0.161(2) 0.525(5) 0.967(2) 0.036(13) Uiso 1 1 d . . .
H9 H -0.020(3) 0.544(5) 0.572(2) 0.035(12) Uiso 1 1 d . . .
H10 H 0.540(2) 0.481(5) 0.764(2) 0.030(12) Uiso 1 1 d . . .
H11 H 0.217(3) 0.281(6) 0.997(3) 0.045(14) Uiso 1 1 d . . .
H12 H 0.142(3) 0.681(5) 0.853(2) 0.037(13) Uiso 1 1 d . . .
H13 H 0.243(2) 0.056(5) 0.967(2) 0.028(11) Uiso 1 1 d . . .
H14 H 0.062(2) 0.074(5) 0.568(2) 0.034(12) Uiso 1 1 d . . .
H15 H 0.120(3) -0.122(6) 0.654(3) 0.052(15) Uiso 1 1 d . . .
H16 H 0.648(3) 0.143(6) 1.013(3) 0.044(14) Uiso 1 1 d . . .
H17 H 0.368(3) -0.171(6) 0.859(3) 0.053(16) Uiso 1 1 d . . .
H18 H 0.088(3) 0.714(6) 0.885(3) 0.045(14) Uiso 1 1 d . . .
H19 H 0.062(3) 0.577(6) 0.621(3) 0.055(16) Uiso 1 1 d . . .
H20 H 0.496(3) -0.265(7) 0.945(3) 0.056(16) Uiso 1 1 d . . .
H21 H -0.007(2) 0.615(5) 0.782(2) 0.033(12) Uiso 1 1 d . . .
H22 H 0.222(3) -0.043(5) 0.758(2) 0.037(13) Uiso 1 1 d . . .
H23 H 0.165(3) -0.003(6) 0.923(2) 0.038(14) Uiso 1 1 d . . .
H24 H 0.308(3) -0.032(7) 0.647(3) 0.061(17) Uiso 1 1 d . . .
H25 H 0.131(3) 0.259(6) 0.956(3) 0.044(14) Uiso 1 1 d . . .
H26 H 0.576(3) 0.370(7) 0.973(3) 0.057(16) Uiso 1 1 d . . .
H27 H -0.043(3) 0.545(6) 0.667(2) 0.045(14) Uiso 1 1 d . . .
H28 H 0.391(3) -0.335(7) 0.841(3) 0.065(18) Uiso 1 1 d . . .
H29 H 0.658(3) 0.371(7) 0.980(3) 0.060(16) Uiso 1 1 d . . .
H30 H 0.185(3) -0.198(7) 0.768(3) 0.065(18) Uiso 1 1 d . . .
H31 H 0.462(3) -0.104(6) 0.949(3) 0.054(15) Uiso 1 1 d . . .
H32 H 0.521(3) 0.548(5) 0.889(2) 0.039(13) Uiso 1 1 d . . .
H33 H 0.007(3) 0.085(5) 0.595(2) 0.037(13) Uiso 1 1 d . . .
H34 H 0.027(3) 0.780(6) 0.775(2) 0.042(14) Uiso 1 1 d . . .
H35 H 0.259(3) 0.043(6) 0.872(3) 0.050(15) Uiso 1 1 d . . .
H36 H 0.211(3) 0.505(6) 0.937(2) 0.044(15) Uiso 1 1 d . . .
H37 H 0.242(3) -0.052(6) 0.656(3) 0.054(16) Uiso 1 1 d . . .
H38 H 0.095(3) 0.339(6) 0.595(3) 0.055(16) Uiso 1 1 d . . .
H39 H 0.302(3) 0.432(6) 0.622(3) 0.050(15) Uiso 1 1 d . . .
H40 H 0.378(3) -0.219(6) 0.733(3) 0.051(15) Uiso 1 1 d . . .
H41 H 0.066(3) -0.094(6) 0.684(2) 0.039(13) Uiso 1 1 d . . .
H42 H 0.650(3) 0.115(7) 0.945(3) 0.066(18) Uiso 1 1 d . . .
H43 H 0.312(3) 0.461(6) 0.696(2) 0.039(13) Uiso 1 1 d . . .
H44 H 0.307(4) -0.249(8) 0.738(3) 0.09(2) Uiso 1 1 d . . .
H45 H 0.512(3) 0.649(6) 0.779(3) 0.056(16) Uiso 1 1 d . . .
H46 H 0.590(3) -0.133(6) 0.942(3) 0.053(16) Uiso 1 1 d . . .
H47 H 0.242(3) 0.195(5) 0.618(3) 0.035(12) Uiso 1 1 d . . .
H48 H 0.257(3) 0.212(6) 0.696(3) 0.047(14) Uiso 1 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'
O O 0.0106 0.0060 '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'
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
O027 Cl03 O024 109.9(2) . . ?
O027 Cl03 O032 110.1(3) . . ?
O024 Cl03 O032 109.6(2) . . ?
O027 Cl03 O015 108.7(2) . . ?
O024 Cl03 O015 109.9(2) . . ?
O032 Cl03 O015 108.6(2) . . ?
O006 Cl04 O020 109.4(2) . . ?
O006 Cl04 O026 110.6(2) . . ?
O020 Cl04 O026 109.7(2) . . ?
O006 Cl04 O037 109.5(3) . . ?
O020 Cl04 O037 108.8(2) . . ?
O026 Cl04 O037 108.8(2) . . ?
C044 O005 C034 111.8(4) . . ?
C039 O007 C038 110.8(4) . . ?
C012 O008 C051 113.2(4) . . ?
O022 C009 C028 109.0(4) . . ?
O013 C010 C051 109.2(4) . . ?
C036 O011 C040 112.6(4) . . ?
O008 C012 C045 109.4(4) . . ?
C010 O013 C042 112.1(4) . . ?
C028 O014 C031 110.6(4) . . ?
O021 C016 C039 109.2(4) . . ?
C047 O017 C043 112.7(4) . . ?
C041 O018 C030 111.3(4) . . ?
C045 O019 C046 111.2(4) . . ?
C049 O021 C016 112.6(4) . . ?
C050 O022 C009 112.7(4) . . ?
C029 O023 C033 112.2(3) . . ?
O014 C028 C009 108.7(4) . . ?
O023 C029 C030 108.8(4) . . ?
O018 C030 C029 109.1(4) . . ?
O014 C031 C040 108.6(4) . . ?
O023 C033 C034 109.6(4) . . ?
O005 C034 C033 108.1(4) . . ?
O011 C036 C041 108.7(4) . . ?
O007 C038 C043 109.2(4) . . ?
O007 C039 C016 109.8(4) . . ?
O011 C040 C031 109.3(4) . . ?
O018 C041 C036 109.2(4) . . ?
O013 C042 C047 108.4(4) . . ?
O017 C043 C038 109.5(4) . . ?
O005 C044 C050 108.5(4) . . ?
O019 C045 C012 109.7(4) . . ?
O019 C046 C049 110.1(4) . . ?
O017 C047 C042 108.7(4) . . ?
O021 C049 C046 108.6(4) . . ?
O022 C050 C044 109.7(4) . . ?
O008 C051 C010 108.4(4) . . ?
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
Cl03 O027 1.423(4) . ?
Cl03 O024 1.429(4) . ?
Cl03 O032 1.432(4) . ?
Cl03 O015 1.436(3) . ?
Cl04 O006 1.429(4) . ?
Cl04 O020 1.432(4) . ?
Cl04 O026 1.442(3) . ?
Cl04 O037 1.444(3) . ?
O005 C044 1.436(6) . ?
O005 C034 1.437(6) . ?
O007 C039 1.425(6) . ?
O007 C038 1.428(6) . ?
O008 C012 1.429(6) . ?
O008 C051 1.440(7) . ?
C009 O022 1.433(6) . ?
C009 C028 1.488(7) . ?
C010 O013 1.418(6) . ?
C010 C051 1.490(8) . ?
O011 C036 1.420(5) . ?
O011 C040 1.420(5) . ?
C012 C045 1.481(9) . ?
O013 C042 1.424(6) . ?
O014 C028 1.431(5) . ?
O014 C031 1.435(6) . ?
C016 O021 1.423(6) . ?
C016 C039 1.493(8) . ?
O017 C047 1.424(6) . ?
O017 C043 1.426(6) . ?
O018 C041 1.422(5) . ?
O018 C030 1.439(5) . ?
O019 C045 1.436(7) . ?
O019 C046 1.437(7) . ?
O021 C049 1.422(6) . ?
O022 C050 1.425(5) . ?
O023 C029 1.429(5) . ?
O023 C033 1.429(5) . ?
C029 C030 1.489(7) . ?
C031 C040 1.490(7) . ?
C033 C034 1.487(7) . ?
C036 C041 1.499(7) . ?
C038 C043 1.483(7) . ?
C042 C047 1.494(8) . ?
C044 C050 1.487(7) . ?
C046 C049 1.489(9) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139129680
